117
Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares Pinto Leite Dissertação para obtenção do Grau de Mestre em Engenharia Aeroespacial Júri Presidente: Fernando José Parracho Lau Orientador: Luís Rego da Cunha de Eça Vogal: Filipe Szolnoky Ramos Pinto Cunha Novembro de 2012

Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

Embed Size (px)

Citation preview

Page 1: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

Development of Testing Conditions forGas/Surface Interaction Studies inAtmospheric Reentry Simulations

José Pedro Soares Pinto Leite

Dissertação para obtenção do Grau de Mestre emEngenharia Aeroespacial

Júri

Presidente: Fernando José Parracho Lau

Orientador: Luís Rego da Cunha de Eça

Vogal: Filipe Szolnoky Ramos Pinto Cunha

Novembro de 2012

Page 2: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares
Page 3: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

Acknowledgments

⋆ To my parents that always supported me.

⋆ To Prof. Olivier Chazot for all the help, hints, coaching and the basic idea for this work.

⋆ To Francesco Panerai for his unmeasurable help for this work. My research without is PhD

Thesis and his expertise as background would have been much more darker. Sorry for all the

things I did in the wrong way and infinite amount of stupid questions.

⋆ To Pascal Collin, the super-technician, because He Is The Man.

⋆ To Bernd Helber for all the help and patience in the processing of the spectrometry results.

⋆ To Prof. Luis Eça for all the help and coaching before, during and after my stay in VKI.

⋆ To Prof. João Teixeira Borges, Prof. Luis Eça, Prof. Fernando Lau, Prof. Pedro Serrão,

Prof. Ferry Schrijer and Prof. Fluvio Scarano from IST and TUDelft for those great first courses

in Mechanics, Fluid Mechanics and Aerodynamics.

⋆ To all my friends and colleagues at the von Kármán Institute because the great environment

was a big help for the development of this work.

iii

Page 4: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

iv

Page 5: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

Abstract [English]

Since the beginning of the space exploration that the design of the thermal protection system (“heat

shield”) of a planetary reentry vehicle (a vehicle that enters the atmosphere of a planet coming from

the outer space) had been a challenge for the design engineers. Problems arise because of the lack of

a fully comprehension of the physico-chemical processes involved, specifically Aerothermodynamics

and Gas/Surface Interactions. In this thesis, the Local Heat Transfer Simulation methodology is used

to fully reproduce the aerothermochemical conditions in the nose stagnation point of a reentry vehicle

in a ICP Plasma Windtunnel, the Plasmatron, installed at the von Kármán Institute and capable of

produce high enthalpy flows.

Using the the LHTS methodology, the oxidation of Silicon Carbide based thermal protective

materials is investigated and both the passive-to-active transition and the operational limits of these

materials are accessed. The materials tested are going to be used in the IXV mission under project

by the European Space Agency.

A pioneer testing methodology was developed to be used in high enthalpy facilities in order to un-

derstand the effect of surface temperature in surface recombination coefficient (catalycity) and heat

flux from the plasma to the wall. Preliminary data was obtained and a sensitivity analysis were done

to access the reliability of the method. Plus, is proposed a method to construct an computationsly

efficient AeroThermodynamic DataBase for emissivity, catalycity and heat flux to be used in design

and CFD codes and applicable both for passive and active concepts of thermal protective systems.

Keywords: Thermal Protective Systems, Ground Testing, Gas/Surface Interactions, Aerothermo-

dynamics, Oxidation, Catalycity

Resumo [Português]

Desde o início da exploração do espaço que o design do sistema de protecção térmica (“escudo tér-

mico”) de um veículo espacial de reentrada planetária, ou seja, que entra na atmosfera de um planeta

vindo do espaço exterior, tem sido um desafio para os projectistas. Os problemas surgem por causa da

falta de uma boa compreensão dos processos físico-químicos envolvidos, especificamente fenómenos

aerotermodinâmicos e interacções gás/superfície. Nesta tese, a metodologia de Simulação Local de

v

Page 6: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

vi Abstract/Resumo

Transmissão de Calor (LHTS) é utilizada para reproduzir totalmente as condições aerotermoquímicas

no ponto de estagnação do nariz de um veículo espacial de reentrada dentro de um túnel de plasma, o

Plasmatron, instalado no Instituto von Kármán e capaz de produzir jactos de muito elevada entalpia.

Utilizando a metodologia de LHTS, a oxidação e limites operacionais de materiais de protecção

térmica baseados em Carboneto de Silício são investigados. Estes materiais vão ser utilizados na

missão IXV, da responsabilidade da Agência Espacial Europeia.

Uma metodologia de teste foi desenvolvida para ser utilizada em instalações de entalpia elevada,

a fim de compreender o efeito da temperatura da superfície no coeficiente de recombinação (catalici-

dade) e no fluxo de calor do plasma para a parede. Dados preliminares foram obtidos e uma análise

de sensibilidade foi feita para testar a fiabilidade do método. Para além disso, é proposta uma me-

todologia para construir uma Base de Dados Aerotermodinâmica computacionalmente eficiente para

utilização em codigos de design e CFD e empregável em conceitos passivos e activos de sistemas de

protecção térmica.

Palavras-Chave: Sistemas de Protecção Térmica, Ensaios em Solo, Interacções Gás/Superfície,

Aerotermodinâmica, Oxidação, Coeficiente de Recombinação

Page 7: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

Contents

List of Figures xi

List of Tables xv

List of Symbols xvii

1 Introduction 11.1 Hypersonic Flows and Atmospheric Reentry . . . . . . . . . . . . . . . . . . . . . . . . 1

1.1.1 The Hypersonic Flow Regime . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11.1.2 The Atmospheric Reentry . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2

1.2 Families of Thermal Protection Systems . . . . . . . . . . . . . . . . . . . . . . . . . . 21.3 Aim of This Project . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3

2 Catalycity and Oxidation Research - A Bibliographical Review 72.1 Gas Surface Interaction and Catalycity . . . . . . . . . . . . . . . . . . . . . . . . . . . 7

2.1.1 Principles of Catalycity . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 72.1.2 Catalycity, Heat Shield Design and Simulation . . . . . . . . . . . . . . . . . . 8

2.2 Passive-to-Active Oxidation Transition in TPM . . . . . . . . . . . . . . . . . . . . . . 9

3 Experimental Facilities and the LHTS Methodology 133.1 Plasmatron: The VKI’s ICP Windtunnel . . . . . . . . . . . . . . . . . . . . . . . . . . 133.2 The Local Heat Transfer Simulation method in VKI . . . . . . . . . . . . . . . . . . . 14

3.2.1 Experimental Methods for Reentry Simulation in Plasmatrons . . . . . . . . . 183.3 Recalling the Abacus – The Temperature Problem . . . . . . . . . . . . . . . . . . . . 193.4 Sample Holders . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 203.5 Intrusive Measurement Techniques . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20

3.5.1 Heat Flux Probes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 203.5.2 Pitot Probes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22

3.6 Optical Measurement Techniques . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 233.6.1 Two-Colour Pyrometer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23

vii

Page 8: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

viii Table of contents

3.6.2 Broadband Infrared Radiometer . . . . . . . . . . . . . . . . . . . . . . . . . . . 24

3.6.3 In-Situ Emissivity Determination Method . . . . . . . . . . . . . . . . . . . . . 24

3.6.4 Optical Emission Spectroscopy . . . . . . . . . . . . . . . . . . . . . . . . . . . 25

3.7 New Techniques Developed in the Context of this Work . . . . . . . . . . . . . . . . . 25

3.7.1 Cooled Sample Setup . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25

3.7.2 New Correlation for Dynamic Pressure Estimation . . . . . . . . . . . . . . . . 29

3.8 Brief Note on the Computational Methods Used . . . . . . . . . . . . . . . . . . . . . 30

3.8.1 The heat1D script . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 30

3.8.2 The ICP code and NDPs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 32

3.8.3 The CERBOULA code . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 34

3.8.4 The Complete Experimental-Numerical Frame . . . . . . . . . . . . . . . . . . 35

4 Numerical Simulations 37

4.1 Cooled Sample Setup Simulation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37

4.1.1 ST Sample Holder Without Cooling . . . . . . . . . . . . . . . . . . . . . . . . 38

4.1.2 ST Sample Holder With Cooling . . . . . . . . . . . . . . . . . . . . . . . . . . 38

4.1.3 ST Sample Holder With Cooling and Insulation . . . . . . . . . . . . . . . . . 40

4.2 Calorimeter Adapter . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 40

5 Oxidation Campaign 43

5.1 Testing Procedures . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 43

5.2 Results . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 44

5.2.1 General Results (ST geometry) . . . . . . . . . . . . . . . . . . . . . . . . . . . 45

5.2.2 Passive-to-Active Oxidation Transition Line . . . . . . . . . . . . . . . . . . . . 48

5.2.3 Visual Inspection of the Samples . . . . . . . . . . . . . . . . . . . . . . . . . . 48

5.2.4 The Temperature Jump . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 52

5.2.5 Optical Spectrometry Results . . . . . . . . . . . . . . . . . . . . . . . . . . . . 54

5.2.6 Frozen Geometry Tests . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 54

6 Temperature Campaign 57

6.1 Testing Procedures . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 57

6.2 Results . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 58

6.2.1 Catalycity . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 62

7 Discussion of Results 67

7.1 Analysis of the Numerical Simulations . . . . . . . . . . . . . . . . . . . . . . . . . . . 67

7.2 Analysis of the Oxidation Campaign . . . . . . . . . . . . . . . . . . . . . . . . . . . . 68

7.2.1 Sensitivity Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 68

7.2.2 Flight Extrapolation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 68

Page 9: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

Table of contents ix

7.3 Analysis of the Temperature Campaign . . . . . . . . . . . . . . . . . . . . . . . . . . . 707.3.1 Sensitivity Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 707.3.2 Flight Extrapolation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 74

7.4 Stagnation Point ATDB Algorithm . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 74

8 Conclusions and Future Work 778.1 Conclusions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 778.2 Recommendations for Future Work . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 77

References 79

A Appendix A 85

B Appendix B 89

C Appendix C 93

Page 10: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

x

Page 11: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

List of Figures

1.1 Thermal Protection System Concepts . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3

1.2 Artist’s Impression of Different Vehicles During Reentry . . . . . . . . . . . . . . . . . 5

2.1 Limit Cases for Surface Catalycity . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8

2.2 IXV Surface Temperature and PA Transition Lines . . . . . . . . . . . . . . . . . . . . 11

3.1 Plasmatron Facility . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14

3.2 ICP Torch - VKI Minitorch Facility . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15

3.3 Plasmatron Operation Envelope . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15

3.4 Ground Testing in Plasmatron Facility under LHTS conditions . . . . . . . . . . . . . 17

3.5 Example of an Heat Flux Abacus . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20

3.6 Sample Holders . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21

3.7 Sample Holder - Radiative Equilibrium Setup . . . . . . . . . . . . . . . . . . . . . . . 21

3.8 Water-Cooled Copper Calorimeter . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22

3.9 Heat Flux Probe with Water-Cooled Calorimeter . . . . . . . . . . . . . . . . . . . . . 23

3.10 Pitot Probe . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23

3.11 Optical Setup . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25

3.12 High Temperature Calorimeter . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27

3.13 CO2 Absorption Spectrum . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28

3.14 Sample Holder - Cooled Sample Setup . . . . . . . . . . . . . . . . . . . . . . . . . . . 28

3.15 pd Data and Correlation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29

3.16 Correlation Relative Error [%] . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 30

3.17 Example of an output from heat1D . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 32

3.18 The Complete Experimental-Numerical Frame . . . . . . . . . . . . . . . . . . . . . . . 35

4.1 Example of the Mesh . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 38

4.2 HF Field - Cond. I . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 39

4.3 HF Field - Cond. II . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 39

4.4 HF Field - Cond. I . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 40

xi

Page 12: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

xii Table of contents

4.5 HF Field - Cond. II . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 41

4.6 Temperature Field - 5mm adapter . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 41

4.7 Temperature Field - 3mm adapter . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 42

5.1 Mass Loss Rate - HER . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 47

5.2 Mass Loss Rate - MTA . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 47

5.3 Evolution of γ with He . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 48

5.4 Passive-to-Active Transition - HER . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 49

5.5 Passive-to-Active Transition - MTA . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 49

5.6 Examples of HER samples tested with ps=5000Pa . . . . . . . . . . . . . . . . . . . . 50

5.7 Examples of MTA samples tested with ps=5000Pa . . . . . . . . . . . . . . . . . . . . 51

5.8 Temperature History During Two Different Tests - HER . . . . . . . . . . . . . . . . . 52

5.9 Temperature History During Two Different Tests - MTA . . . . . . . . . . . . . . . . . 53

5.10 Integrated Spectral Radiance and Emissivity History . . . . . . . . . . . . . . . . . . . 53

5.11 Temperature Jump - Evolution in Time . . . . . . . . . . . . . . . . . . . . . . . . . . 53

5.12 Spectra took during Test 21 (Active Oxidation) . . . . . . . . . . . . . . . . . . . . . . 55

5.13 Emission Line Si288 Intensity Evolution During a Temperature Jump . . . . . . . . . 56

6.1 Geometry tested and Simulated . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 60

6.2 Steady State Temperature Simulation . . . . . . . . . . . . . . . . . . . . . . . . . . . 60

6.3 Steady State Heat Flux Simulation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 61

6.4 Heat Flux History of Test T1 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 61

6.5 Abacus of test T1 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 62

6.6 Abacus of test T2 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 63

6.7 Abacus of test T3 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 63

6.8 γ as function of the BL edge parameters . . . . . . . . . . . . . . . . . . . . . . . . . . 64

6.9 Experimental HF as function of the BL edge parameters . . . . . . . . . . . . . . . . . 65

7.1 Abacus from Test 1 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 69

7.2 Abacus from Test 28 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 69

7.3 Extrapolated Fight Conditions - Oxidation Campaign . . . . . . . . . . . . . . . . . . . 71

7.4 Extrapolated Velocity Gradient - Oxidation Campaign . . . . . . . . . . . . . . . . . . 72

7.5 Mass Fractions at the BL Edge . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 72

7.6 Temperature Evolution Inside the Boundary Layer - Test T1 . . . . . . . . . . . . . . 73

7.7 Heat Flux to the Wall . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 73

7.8 Extrapolated Flight Conditions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 74

7.9 Flowchart for ATDB Algorithms - Hot or Insulated Structure TPS . . . . . . . . . . . 76

7.10 Flowchart for ATDB and Algorithms - Generic TPS . . . . . . . . . . . . . . . . . . . 76

Page 13: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

Table of contents xiii

A.1 Temperature Field - Section 4.1.1 - Condition I . . . . . . . . . . . . . . . . . . . . . . 85A.2 Temperature Field - Section 4.1.1 - Condition II . . . . . . . . . . . . . . . . . . . . . 86A.3 Temperature Field - Section 4.1.2 - Condition I . . . . . . . . . . . . . . . . . . . . . . 86A.4 Temperature Field - Section 4.1.2 - Condition II . . . . . . . . . . . . . . . . . . . . . 87A.5 Temperature Field - Section 4.1.3 - Condition I . . . . . . . . . . . . . . . . . . . . . . 87A.6 Temperature Field - Section 4.1.3 - Condition II . . . . . . . . . . . . . . . . . . . . . 88

B.1 Temperature vs. Time - Section 4.1.1 - Condition I . . . . . . . . . . . . . . . . . . . . 89B.2 Temperature vs. Time - Section 4.1.1 - Condition II . . . . . . . . . . . . . . . . . . . 90B.3 Temperature vs. Time - Section 4.1.2 - Condition I . . . . . . . . . . . . . . . . . . . . 90B.4 Temperature vs. Time - Section 4.1.2 - Condition II . . . . . . . . . . . . . . . . . . . 91B.5 Temperature vs. Time - Section 4.1.3 - Condition I . . . . . . . . . . . . . . . . . . . . 91B.6 Temperature vs. Time - Section 4.1.3 - Condition II . . . . . . . . . . . . . . . . . . . 92

Page 14: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

xiv

Page 15: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

List of Tables

3.1 Plasmatron Probes Dimensions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 203.2 Test Cases Used in the Design Process . . . . . . . . . . . . . . . . . . . . . . . . . . . 263.3 Operational Map for the High Temperature Calorimeter . . . . . . . . . . . . . . . . . 283.4 Constants for the NDPs Correlations . . . . . . . . . . . . . . . . . . . . . . . . . . . . 33

5.1 Test Conditions for HER samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 445.2 Test Conditions for MTA samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 455.3 Summarized Test Results - HER . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 455.4 Summarized Test Results - MTA . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 46

6.1 Test Conditions for the Temperature Campaign . . . . . . . . . . . . . . . . . . . . . . 586.2 Test Results From the Experiments . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 59

7.1 Temperature results in the setup without insulation - ANSYS vs. heat1D . . . . . . . 687.2 Temperature results in the setup with insulation - ANSYS vs. heat1D . . . . . . . . . 687.3 Sensitivity Analysis for Test T1 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 707.4 Extrapolated Flight Conditions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 74

C.1 NDPs and Rebuilt Quantities - Oxidation Campaign (HER) . . . . . . . . . . . . . . . 94C.2 NDPs and Rebuilt Quantities - Oxidation Campaign (MTA) . . . . . . . . . . . . . . . 95C.3 NDPs and Rebuilt Quantities - Temperature Campaign . . . . . . . . . . . . . . . . . 95

xv

Page 16: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

xvi

Page 17: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

List of Symbols

Acronyms

AP Active-to-Passive

ARD Atmospheric Reentry Demonstrator

ATDB AeroThermodynamic DataBase

BL Boundary Layer

CERBERE Catalycity and Enthalpy ReBuilding for a REference probe

CERBOULA CERBERE + NEBOULA

CFD Computational Fluid Dynamics

CMC Ceramic Matrix Composite

CS Cooled Sample setup

C/SiC CMC with SiC matrix and Carbon fibre reinforcement

DAC Data Acquisition Card

ESA European Space Agency

FEA Finite Element Analysis

GSI Gas-Surface Interaction

HF Heat Flux

HFreq High Frequency

HER Herakles - A Safran Group Company (Previously SPS)

ICBM Inter-Continental Ballistic Missile

ICIASF International Congress on Instrumentation in Aerospace Simulation Facilities

ICP Inductively-Coupled Plasma

IPM-RAS Institute for Problems in Mechanics of the Russian Academy of Sciences

(in russian: ИПМех РАН - Институт проблем механики РАН )

IR Infrared

IST Instituto Superior Técnico - Faculty of UTL

IXV Intermediate eXperimental Vehicle

LHTS Local Heat Transfer Simulation

LTE Local Thermo-chemical Equilibrium

xvii

Page 18: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

xviii List of Symbols

MESOX Moyen d’Essai et de DIagnostic en Ambiance Spatiale

MLR Mass Loss Rate

MTA MT Aerospace

NASA National Aeronautics and Space Administration

NDP Non-Dimensional Parameter

NEBOULA NonEquilibrium BOUndary LAyer

PA Passive-to-Active

PEGASE PErfect GAS Equation Solver

PLC Power Line Communication

PROMES Le Laboratoire PROcédés, Matériaux et Energie Solaire

RS Radiative equilibrium Sample setup

SEM Scanning Electron Microscopy

SPS Snecma Propulsion Solide - Previous name of HER

SSO Space Shuttle Orbiter

TPM Thermal Protection Material

TPS Thermal Protection System

TRP Technology Research Programme

UQ Uncertainty Quantification

UTL Technical University of Lisbon

VKI von Kármán Institute for Fluid Dynamics

Roman symbols

A Area m2

cp Specific Heat J kg−1 K−1

cp Frozen Specific Heat = ∑ yicp,i J kg−1 K−1

D Dissociation Energy of the Recombining Molecule J

D Diameter m

D Diffusion Coefficient -

Da Damköhler number = τfl/τch -

E Energy J

H Specific Total Enthalpy J kg−1

h Specific Enthalpy J kg−1

h Convection Coefficient W m−2 K−1

I Intensity a.u.

J Mass Flux kg m−2 s−1

k Catalytic Reaction Rate m s−1

Le Lewis Number = ρDcp/λ -

Page 19: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

List of Symbols xix

M Mass Flux (atoms) kg m−2 s−1

m Mass or Particle Mass kg

m Mass Flow Rate kg s−1

NS Number of Species i -

Nu Nusselt Number = hD/λ -

n Number Density m−3

n Normal to the Wall (oriented: gas to wall) -

p Pressure Pa = kg m−1 s−2

Q Heat J

Q Heat Rate W = J s−1

q Heat Flux W m−2

R Radius m

Re Reynolds Number = ρV D/µ -

Sc Schmidt Number = µ/(ρD) -

T Temperature K

V Velocity m s−1

v Freestream Plasma Velocity m s−1

W Spectral Radiance W m−2 sr−1 µm−1

Wλ1→λ2 Integrated Spectral Radiance between λ1 and λ2 W m−2 sr−1

w Reaction Rate kg m−3 s−1

yi Mass Fraction -

y Atom Mass Fraction -

Greek symbols

B Energy Accommodation Coefficient -β Velocity Gradient s−1

γ Catalycity -∆ Boundary Layer Thickness mδ Uncertainty -ε Emissivity -λ Wavelength mλ Thermal Conductivity W kg−1 K−1

µ Viscosity kg m−1 s−1

ρ Density kg m−3

τ Characteristic Time s

Page 20: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

xx List of Symbols

Subscripts

amb ambientapp apparentcond conductivecal calorimetercat due to catalycitych chemical reactioncw cold wallD dissociationd dynamicdiff diffusivee boundary layer outer edgeeff effectiveel electric - imposed on the HFreq generatorexp experimentalF formationfl flowgeo geometrici relative to specie iint intrinsicm modelpj post-jumppost after testpre before testrec recombinations staticsol solidt totalw wallwet wetted∞ freestream

Page 21: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

List of Symbols xxi

Superscripts

0 blackbodyF relative to flightGT relative to the ground test(n) iteration n↓ impinging on the surface« transferred to the surface© leaving the surface

Constants

c Speed of Light 299792458 m s−1

e Base of the Natural Logarithm 2.718281 -h Planck’s Constant 6.6260693 × 1034 J skB Boltzmann’s constant 1.380658 × 10−23 J K−1

π Pi 3.14159265 -σ Stefan-Boltzmann constant 5.670373 × 10−8 W m−2 K−4

Page 22: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

xxii

Page 23: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

Chapter 1

Introduction

1.1 Hypersonic Flows and Atmospheric Reentry

With the birth of “faster than sound” aircrafts with the flight of Charles “Chuck” Yeager in October

14th, 1947, new and challenging problems arise and countless generations of scientists and engineers

had been fighting to break the frontiers of the human knowledge and provide safer, faster and cheaper

ways to travel around the world and beyond. But the “brand new world” of supersonic and specially

hypersonic flow showed that Socrates was more than right: “I know one thing, that I know nothing”.

Along the years, specially during the firsts flights of hypersonic vehicles, the X-15 flight tests [1],

scientists discovered several new phenomena that were not predicted by the theories at the time and

the same still keep happening today. But, before further development it is important to give the

description of what is hypersonic flow.

1.1.1 The Hypersonic Flow Regime

In fact, there isn’t an universally accepted concept that could tell us what is an hypersonic flow but

is usually accepted that it is a flow with a free stream Mach number grater than 5. Although, this is

not totally accepted by the scientific community as we can read in the citation presented in the next

page.

For the proposes of this work and simplicity, hypersonic flow will be considered a flow with a free

stream Mach number grater than 5 and in which the high temperature gas properties play a non

negligible roll. One of the fields were the hypersonic flow regime play an important roll is the so

called Atmospheric Reentry.

1

Page 24: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

2 Introduction

1.1.2 The Atmospheric Reentry

The history of Atmospheric Reentry (also called Planetary Reentry) begins in the Cold War between

USA and USSR with scientists from both sides trying to understand the new phenomena arising from

the hypersonic flight conditions. These concerns have arisen from the design of new weapons, the

ICBMs and their reentry warheads, and consequently the investigations on these matters were also

propagated to the Space Race during the second half of the twentieth-century.

Nowadays reentry still represents one of the most fascinating challenges for scientific research in

the space technology context and both for atmospheric reentry and hypersonic cruise vehicles the

aerothermochemical environment is still the least known constrain for the design of such machines.

This is result of the extremely complicated coupled physical phenomena involved.

Reentry is defined as the trajectory of a celestial body (asteroid, spacecraft, etc.) between the

moment in which it first “fells” the planet atmosphere and the the moment in which it touches the

ground. These two limits are not absolutely fixed and usually vary according to the problem. For the

“upper” limit on Earth, for example, the altitude of 120km is usually accepted, despite the fact that

the official limit for space is the Kármán line at 100km altitude. The lower limit is more variable, and

can be defined as the moment in which the vehicle touches the ground, opens a parachute or changes

in flight condition “mode” (for example, for the Space Shuttle the hypersonic reenty is defined until

the moment in which a condition of Mach⩽ 2.5 is reached)[2].

During reentry, the spacecraft travels in a speed much higher than the speed of sound. Because

of it, a bow shock wave is formed in the front of the vehicle. In the nose stagnation point region, the

shock wave is almost a normal shock wave and through it the flow is decelerated to subsonic speeds

and both pressure and temperature increase by several orders of magnitude. In a reentry from earth

orbit the temperature is usually high enough to promote dissociation in the gas and for a spacecraft

returning from the moon or Mars it is usually enough to promote ionization [3].

Reentry can be divided in two groups, low-speed reentry and high-speed reentry. Low-speed

reentry corresponds to a reentry in which the initial speed is bellow the corresponding orbital speed

and a high-speed reentry to one in which the initial speed is in the order of magnitude of the escape

velocity. It can be also divided into ballistic or gliding reentry according to the lisft-over-drag ratio

of the vehicle. Examples of such vehicles are presented in figure 1.2. IXV, the base vehicle for this

work, can be classified as gliding reentry vehicle.

1.2 Families of Thermal Protection Systems

Thermal protection systems can be divided in 3 main groups: Active, Passive and Semi-Passive.

Figure 1.1 represents most of the current concepts for TPS and detailed information about each one

can be found in [1, 4, 5].

1Extracted form [3]

Page 25: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

Introduction 3

Almost everyone has their own definition of the term hypersonic. If we wereto conduct something like a public opinion poll among those present, and askedeveryone to name a Mach number above which the flow of a gas should properly bedescribed as hypersonic there would be a majority of answers around five or six, butit would be quite possible for someone to advocate, and defend, numbers as small astree, or as high as 12.

P. L. Roe, comment made in a lecture atthe Von Kármán Institute, Belgium, January 1970 1

Figure 1.1: Thermal Protection System Concepts (extracted from [5])

It is important to notice that until now the samples tested in the VKI Plasmatron were always

tested according to the concept of Hot Structure or highly Insulated Structures because the samples

were in radiative equilibrium with the environment without allowing conductive heat loss [6, 7]. The

new method developed in this work (see section 3.7.1) allow the determination of the aerothemo-

chemical environment, surface catalycity and heat transfer for several different TPS concepts like

Convective Cooling, Heat Pipe, Heat Sink Structure and Insulated Structure (for insulation types in

which the conductive HF is not negligible).

1.3 Aim of This Project

The aim of this work is to further continue the work developed all over the years in VKI about

aerothermodynamics of reentry vehicles.

In this framework, as collaborator of Francesco Panerai, Post-Doc Fellow in VKI, I actively partic-

Page 26: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

4 Introduction

ipate in the experimental TRP Oxidation campaign and in a substantial part of the post-processing

of the results. The results of this campaign is presented in chapter 5.

The development of a new experimental method to increase the Plasmatron operations capabili-

ties, including new methods for GSI research are presented in chapter 4 and 6 and are almost exclusive

responsibility of the author (except some already referenced acknowledgements).

Page 27: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

Introduction 5

(a) Apollo Command Module - A Typical Ballistic Reentry Vehicle

(b) Space Shuttle Orbiter - A Typical Gliding Reentry Vehicle

Figure 1.2: Artist’s Impression of Different Vehicles During Reentry

Page 28: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

6

Page 29: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

Chapter 2

Catalycity and Oxidation Research -

A Bibliographical Review

2.1 Gas Surface Interaction and Catalycity

2.1.1 Principles of Catalycity

As we saw in section 1.1.2 the aerothermochemical environment around a reentry body in a low

speed reentry is dominated by phenomena such as chemical reactions in the flow and wall and heat

transfer by conduction, convection, recombination and radiation. All this mechanisms play a role in

the heat flux balance at the wall. This has important implications on the final surface temperature

and conduction heat flux into the wall which will be the main parameters that drive the selection of

the TPS for the mission. This selection is very complicated because the TPS itself will play a roll in

the final picture because of the chemical characteristics of the surface. This coupling between the

surface and the flow itself is usually called Gas/Surface Interaction or GSI. When dealing with the

effect of the surface in the flow several problems arise basically because of lack of knowledgeable in

this kind of phenomena at high temperature and low pressure, despite all the efforts conducted in

solving that problems since the 50s [1].

One of the factors that contribute more for the heat transfer to the wall is the exothermic reactions

occurring there. The reactants for this reactions are the dissociated and ionized atoms generated by

the bow shock wave in the front of the vehicle. These atoms eventually reach the surface which acts as

a catalyst and promotes the exothermic recombination reactions. This process is called heterogeneous

catalycity.

But not all the atoms that reach the wall undergo the recombination process into molecules.

The probability that this reaction occour is defined as the recombination coefficient or catalycity.

Catalicity can than be defined as the ratio between the flux of recombined atoms over the flux of

7

Page 30: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

8 A Bibliographical Review

Figure 2.1: Limit Cases for Surface Catalycity

impinging atoms on the surface for a certain specie i.

γ =Mi,rec

M↓

i

(2.1)

In this work, only 2 recombination reactions were considered: O+OÐ→ O2 and N+NÐ→ N2 and

the same recombination coefficient is used for both. Some recent investigations [8, 9] shown that the

production of NO (N +OÐ→ NO) can be so important as the reactions above, but the mechanism

for its formation is not yet completely understood. In chapter 5 is also referred that the reaction

Si +OÐ→ SiO should also be taken into account due to its highly exothermic nature.

The 2 limit cases for catalicity are the fully-catalytic wall (γ = 1) and the non-catalytic wall (γ = 0)

that are represented in figure 2.1.

Following the same approach of Panerai [7], we can define the experimental values of γ as effective,

apparent catalycity, which relates with the true catalycity by the formula

γ = γapp,eff = B ⋅ γapp =E«

D⋅ γapp =

D

SwetSgeo

γint (2.2)

in which γint is the true microscopic catalycity in a multi-temperature model (temperature of the flow

different from the temperature of the wall). For more information the reader is advised to consult

Thoemel [10], Barbante [11] and Panerai [7].

2.1.2 Catalycity, Heat Shield Design and Simulation

One of the biggest unknowns when designing a new hypersonic vehicle is the surface catalycity.

Usually designers assume a fully-catalytic wall1 because that’s the “worst case scenario” for surface

heating but experiences in very different facilities had proved that for common TPM the value can

1And sometimes even Super Catalytic Wall

Page 31: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

Catalycity and Oxidation Research 9

be 3 orders of magnitude lower [12, 13, 7]. Classical references like Anderson [3] usually admit that,

for common reentry scenarios, the heat flux to a fully-catalytic wall is approx. twice the one to a

non-catalytic wall. This puts a lot of weight penalty in an “end of line” space application because a

reentry vehicle should always do the complete mission, from Earth to Earth (generally speaking: from

planet to planet). This “dead weight” (= “dead budget”) can be avoided with a better knowledge of

the reentry conditions in general and GSI phenomena in particular.

Catalycity is also a fundamental parameter that need to be accurately introduced in CFD codes

in order to correctly “connect” the flow to the surface. To complicate a little bit, usually catalycity

isn’t a single number but, instead, a variable dependent on surface temperature and boundary layer

edge parameters. This is referenced in several works like [7, 14, 15, 16] and again proved in this work

(see chapter 6). That’s why a correct ATDB, both in data and concept, is very important for the

design of future space missions.

2.2 Passive-to-Active Oxidation Transition in TPM

Since the first heat shields designed for reentry applications, reusability is an important concern for

the design engineers. For high speed reentry ablative heat shields are necessary so reusability is out of

question. On the other hand, for low speed reentry, specially when large gliding and skipping reentry

vehicles are used, reusability is a main concern, for economic reasons. We all remember the financial

disaster of the US Space-Shuttle Program, primary due to the expensive maintenance of the SSO

between flights.

So, it is essential for future designs to know if a certain material will be preserved or degraded

during a reentry maneuver. Used in the SSO and Buran (Буран), Silicon Carbide (SiC) composites

or coatings are one of the main material in study for future missions and many investigations about

it were already done in the past. It is known [7, 17, 18, 19, 20] that for high pressures and low

temperatures, SiC undergoes in a passive oxidation process that generates a net mass gain due to the

creation of a protective layer of Silica (SiO2) in the exposed surface of the material. The chemical

reaction occurring is

SiC(s) + 32O2(g)Ð→ SiO2(s) + CO(g) in a molecular oxygen atmosphere

or

SiC(s) + 3O(g)Ð→ SiO2(s) + CO(g) in a atomic oxygen atmosphere

For higher temperatures/lower pressures, the material go through an active oxidation process

which conducts to a net mass loss and degradation of the material. The chemical reaction is

SiC(s) +O2(g)Ð→ SiO(g) + CO(g) in a molecular oxygen atmosphere

or

Page 32: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

10 A Bibliographical Review

SiC(s) + 2O(g)Ð→ SiO(g) + CO(g) in a atomic oxygen atmosphere

The frontier between this two regimes is called Passive-to-Active (PA) transition.

Despite the fact that it only became a primary issue with the start of the space-shuttle program,

the first studies about oxidation transition in SiC based materials date from the 50s, when Wagner

proposed a model that relates the transition with the partial pressure of oxygen in the mixture bulk

and surface temperature [21]. Later Turkdogan et al. [22] developed the “smoke theory” for the

vaporization of Si.

Later also Gulbransen and Jansson [23], Singhal [24], Hinze and Graham [25], Nickel [26], Keys

[27], Narushima et al. [28], Heuer and Lou [29] and Balat [17, 18], among others, also published

studies about this topic.

Particularly, Gulbransen and Jansson provided 3 possible thermodynamic equilibrium equations for

the transition:

SiC(s) + 2 SiO2(s)Ð→ 3 SiO(g) + CO(g)

SiC(s) + SiO2(s)Ð→ 2 SiO(g) + C(s)

2 SiC(s) + 2 SiO2(s)Ð→ 3 Si(g) + 2CO(g)

Laboratory tests indicated the third equation as the one that best fits the results.

Balat [17, 18], based on the work of Wagner [21], developed a model that predicts the transition

partial pressures of oxygen as function of the diffusion coefficients Di.

As we can see in figure 2.2, it is difficult to find results in accordance between the different research

groups. This is why research programs about this topic are still going on, like the one that supported

part of this work.

Page 33: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

Catalycity and Oxidation Research 11

- 1 0 - 9 - 8 - 7 - 6 - 5 - 41 0 0

1 0 1

1 0 2

1 0 3

1 0 4

1 0 5

OXYG

EN PA

RTIAL

PRES

SURE

, Pa

- 1 0 4 / T E M P E R A T U R E , K - 1

I X V B a l a t , T h e o r y B a l a t , C V D C S i C s t a n d a r d a i r B a l a t , C V D C S i C e x c i t e d a i r G u l b r a n s e n H e u e r e t a l . , H e r d r i c h , a c t i v e - l i m i t H e u e r e t a l . , H e r d r i c h , p a s s i v e - l i m i t

Figure 2.2: IXV Surface Temperature and PA Transition Lines. The solid line represent theevolution in the temperature of the most heated point in the windward side of the vehicle.

Page 34: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

12

Page 35: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

Chapter 3

Experimental Facilities and the

LHTS Methodology

3.1 Plasmatron: The VKI’s ICP Windtunnel

The Plasmatron facility was designed in the early 90s in order to support the design process of Hermes,

a spacecraft also known at the time as the European Space-Shuttle. Although the main project got

cancelled, the Plasmatron project continued in order to reinforce the european knowledge in the the

fields of reentry aerothermodynamics and plasma physics. The facility was first ignited in July 18th,

1997 and it’s still the most powerful of its kind in the world. Figure 3.1 presents the complete facility

system.

Since then, a long list of lessons were learned by all the people that worked in this facility and the

most important was that nothing is easy in a Plasmatron experiment, mainly because of the extreme

temperatures and complexity of the facility. The facility and the experimental setups are continuously

being updated in order to increase the Plasmatron capabilities and the results’ quality.

To produce plasma, this facility uses a physical principle called inductive-coupled plasma generation

(ICP). Conceptually it consists in a quartz tube surrounded by a coil in which a gas is injected. The

coil is connected to a high power generator that provides high alternate voltage with an high frequency.

The current in the coil induces a powerful oscillatory electro-magnetic field inside the tube with the

field lines coaxial it. The residual charged particles in the gas are than accelerated because of the

magnetic field and additional Foucault currents appear.

This makes the gas to heat up because of Joule’s effect promoting an increase on the gas ionisation

degree, increasing the Foucault currents and making the flow entering into an heating “snowball” effect

that results in high temperature, highly ionized gas (plasma) that exits the torch in form of a jet (see

figure 3.1).

13

Page 36: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

14 Experimental Facilities and the LHTS Methodology

Water tanks

Rotating vanesvacuum pumpsBy-pass valve

HP water pumps

Water pumps

Roots vacuum pump

Heat exchanger

ICP torch

Impe

danc

e m

atch

Test chamber

Test model

1.2 MW400 kHz

MOS inverter

12-pulse thyristor rectifier

1700 kVATransformer

Exhaust

Gas supply

200 V dc 11 kV

1050 kW air-water cooler

Figure 3.1: Plasmatron Facility

The high power generator is capable of providing 1.2MW at 2kV and 400kHz and it’s a solid

state MOS technology generator. The torch as 160mm of diameter and exits to a test chamber at

low pressure with 2.5m long and 1.4m diameter and the whole facility is cooled by deionized water

in a close circuit. The facility is computer controlled using a 719 I/O lines PLC and two PC’s for

monitoring the operation. The envelope of operation of the facility is presented in figure 3.3.

3.2 The Local Heat Transfer Simulation method in VKI

In order to correctly duplicate the reentry flight conditions in a ground test facility it’s mandatory

to use similitude relations. It is known that practical ground test facilities can’t totally reproduce

the freestream of flight conditions with Mach numbers higher than 8 [30]. In order to overcome this

problem, several different types of facilities were developed to address different parts of the problem.

For the Mach number simulation Blow-Down windtunnels and Shock Tubes are used. Blow-Down

windtunnels are cold gas facilities so no chemistry can be reproduced but Shock Tubes can actually

reproduce the complete aerothermodynamic environment for reentry vehicles. The problem with these

facilities is that they only allow testing for a fraction of second. This short amount of time is not

Page 37: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

Experimental Facilities and the LHTS Methodology 15

Figure 3.2: ICP Torch - VKI Minitorch Facilitya

aThis facility was the Plasmatron pilot facility

0 2 4 6 8 1 00

2 0

4 0

6 0

8 0

1 0 0

1 2 0 0 2 8 1 8 3 2 5 0

P l a s m a t r o nE n v e l o p e

E X P E R T

E N T H A L P Y , M J / k g

ALTIT

UDE,

km

V E L O C I T Y , k m / s

A P O L L O

I X VS H U T T L E

S P A C E L I N E R

Figure 3.3: Plasmatron Operation Envelope

Page 38: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

16 Experimental Facilities and the LHTS Methodology

enough to properly test TPM due to thermal inertia.

To solve this problem, high enthalpy facilities were developed and in the western countries and

the most used were diffusion reactors [31, 32, 17, 18] and Arc-Jet facilities [13, 33, 34, 35]. Arc-Jets

provide the correct testing setup but several problems arise from their operation like jet instability,

flow contamination and lack of an exact knowledge of the operation conditions. Meanwhile in Soviet

Union, at IPM-RAS, Kolesnikov and his colleges developed the LHTS methodology based on ICP

plasma generators. This method allows to know with accuracy the boundary layer edge conditions

and those condition can then be used to extrapolate the test to a flight condition.

The base for the LHTS method are the analytical formulas developed in the 50s by Fay & Riddell

[36] and Goulard [12]. Both based their work in the pioneer work of Lees [37].

Fay & Riddell proposed the following formula for the stagnation point heat transfer on the nose

of a hypersonic vehicle with a fully-catalytic surface.

q«w = 0.763Pr−0.6(ρeµe)

0.4(ρwµw)

0.1β0.5e (He − hw)[1 + (Leα − 1)(hD,e/He)] (3.1)

were

hD,e =NS

∑ yi,ehF,e (3.2)

and α is 0.63 for frozen boundary layer and equal to 0.52 for equilibrium boundary layer.

Goulard proposed a similar formula, more simplified and applicable only to frozen boundary layers,

but it allows to study walls with an arbitrary catalycity, using the factor φ.

q«w = 0.664Pr−23 (βeρeµe)

0.5He[1 + (Le23φ − 1)(hD,eye/He)] (3.3)

φ =1

1 +0.47Sc−2/3

2βeµeρeρwkw

Analysing these two formulas, Kolesnikov [38] concluded that to simulate the reentry aerother-

mochemical environment at the stagnation point only three parameters at the boundary layer edge

need to be equal to the flight condition: total enthalpy, total pressure and velocity gradient.

HFe =HGT

e pFt,e = pGTt,e βFe = βGTe (3.4)

Conceptually, these 3 parameters represent the conditions behind the bow shock wave that appears

in the front of an hypersonic vehicle (see figure 3.4).

Than, using the 3 parameters, it is possible to extrapolate the ground test to the hypersonic flight

of a vehicle with certain geometric characteristics using the Kolesnikov’s method [30, 38]. It uses the

following formulas:

Page 39: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

Experimental Facilities and the LHTS Methodology 17

Figure 3.4: Ground Testing in Plasmatron Facility under LHTS conditions

HGTe =�

��0

hF∞+

1

2(V F

∞)

2⇔ V F

∞=√

2HGTe (3.5)

pGTe =���

0

pF∞+ ρFe ⋅ (V

F∞

)2⇔ ρFe =

pGTe2HGT

e

(3.6)

The hF∞

and pF∞

can be neglected because we are dealing only with hypersonic speeds, so (V F∞

)2>>

hF∞

and ρFe ⋅ (VF∞

)2>> pF

∞.

At this point, the density can be used to, through an atmospheric model, know all the remaining

parameters in flight like altitude, static pressure, static temperature and speed of sound and through

that also the flight Mach number. In this work the U.S. 1976 Standard Atmosphere model [39] was

used.

Then the boundary layer edge velocity gradient (βGTe ) can be determined using Π2 (NDP2, see

section 3.8.2) together with model radius and, using the thin shock layer theory [40], we can relate

it with flight conditions1:

βGTe =1

RFeff

¿ÁÁÀ8

3

pFe − pF∞

ρFe=V F∞

RFeff

¿ÁÁÀ8

3

ρF∞

ρFe(3.7)

Knowing that ρe can be considered a function of He [30] we can substitute ρFe by ρGTe , which is

a result of the enthalpy rebuilding process and the formula comes:

1An alternative to the thin shock layer theory is to use the modified Newtonian theory, in which the factor8/3 in equation 3.7 is substituted by 2 [3].

Page 40: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

18 Experimental Facilities and the LHTS Methodology

RFeff =V F∞

βGTe

¿ÁÁÀ8

3

ρF∞

ρGTe(3.8)

To know the test parameters in the Plasmatron chamber, also the methods presented by Kolesnikov

are used in VKI but with some differences introduced in-house. The general methodology is address

next in section 3.2.1 and again in 3.8.4 and the differences between the methods used in IPM-RAS

and VKI are described in [41].

3.2.1 Experimental Methods for Reentry Simulation in Plasmatrons

To extrapolate the test of a TPM sample exposed to plasma to a flight condition a multi-step

methodology is used.

First, after the test and knowing m, ps and PWel is possible to calculate the corresponding

Non-Dimensional Parameters (NDPs, see section 3.8.2).

During the test, a calorimeter (see section 3.5.1) is injected into the jet and the heat flux and

surface temperature are recorded, being the surface catalycity estimated by the Minimax method in

a different experiment [6, 42, 43, 7].

With all these results, we can than use the the CERBOULA code (see section 3.8.3) in order to

calculate the boundary layer edge enthalpy (He) and other relevant properties in the boundary layer

and in its edge.

At this point, we can extrapolate the results to flight conditions using equations 3.5, 3.6 and 3.8.

If one is also interested in the TPM catalycity, the process can than be reversed: The boundary

layer edge parameters are now known, plus the surface temperature and heat flux (by optical methods,

see section 3.6) so the CERBOULA code can be run in order to determine the surface catalycity. Also

the famous Kolesnikov’s abacus (see section 3.3) can be calculated and used for the same propose.

An important remark should be done about the way how the transferred heat flux is calculated.

It is done by performing an energy balance at the surface of the sample:

q«w = q©w (3.9)

qcond + qdiff + qrad,in = qrad,out + qloss (3.10)

(−λ∂T

∂y)w,fl

+NS

∑hiJi ● nw + qrad,in = σεT4w + (−λ

∂T

∂y)w,sol

(3.11)

In which the term qrad,in is usually neglected based on the previous experiences and the term qloss

can be neglected [6, 7] in the experiments presented in chapter 5 but is measured by a calorimeter in

the experiments presented in chapter 6.

Page 41: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

Experimental Facilities and the LHTS Methodology 19

The term qrad,out can be calculated using the Stephan-Boltzmann law (qrad = εσT 4w) being Tw

measured by the pyrometer and ε calculated form the comparison of the pyrometer data with the

radiometer data (see section 3.6.3).

At the wall, Ji,w ● nw = wi and the catalytic boundary condition is written as:

wi,cat =miMi,cat =miγiM↓

i (3.12)

If a Maxwellian distribution with the Chapman-Enskog perturbation term is used, the result for

the impinging flux of atoms comes:

M↓

i = ni

√kBTw2πmi

+1

2miJi,w ● nw (3.13)

Applying equation 3.13 in equation 3.12 the final expression comes [11]:

wi,cat =2γi

2 − γimini

√kBTw2πmi

(3.14)

A complete and comprehensive picture of the complete methodology is presented in section 3.8.4.

3.3 Recalling the Abacus – The Temperature Problem

The Heat Flux Abacus for catalycity determination come originally from the work of Kolesnikov [38]

and it is well known as a method for catalycity determination in Plasmatrons. A typical abacus can

be seen in figure 3.5. Nevertheless, it is usually misunderstood as a general picture for the behaviour

of catalycity as a function of temperature. In fact, people sometimes think that when the surface

temperature changes, the point of determined catalycity moves inside the graphic to another point

and that’s not true at all.

In fact, in all the experiments made so far, the temperature of the sample was only determined for

an unique condition: the radiative equilibrium case. So we can’t compare results from tests at two

different temperatures because the free-stream conditions, and so the boundary layer edge conditions,

are different and for different conditions we have different abacus! Also, heat flux can change due to

emissivity changes and/or aerothermodynamic factors like catalycity differences and all that must be

taken into account.

The main propose of this work is to determine the catalycity for two different temperatures and

for the same boundary edge conditions in order to plot, in the same abacus, two temperature points

and then extract information that will hopefully help the design and selection of different types of

TPS in the future, as explained in section 1.2. Results are presented in chapter 6.

As a final remark for this section the author would like to remember again that the abacus

never closes a loop: For a given flight condition/boundary layer edge condition, a specific abacus is

addressed and it allow us to relate three parameters: Tw, γ and q«w. Knowing two of them, we can

know a third.

Page 42: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

20 Experimental Facilities and the LHTS Methodology

Figure 3.5: Example of an Heat Flux Abacus

Probe Name Symbol Rb, mm Rc, mm

Standard ST 25 10Equilibrium EQ 57.5 5

Frozen FR 15 15

Table 3.1: Plasmatron Probes Dimensions

3.4 Sample Holders

The sample holders are presented in figure 3.6. Three different shapes (FR, ST and EQ) are available

in VKI and their dimensions are presented in table 3.1. The difference in shape allow us to address

different velocity gradients keeping all the remaining test conditions constant. This difference in

velocity gradients is equivalent to changing the Damköhler number of the test Da = τfl/τch and

that’s why this probes are also called Damköhler probes. In figure 3.7 is possible to see the old

location of the calorimeter that read the qloss term (see section 3.2.1) in the classical setup.

Previous experiments [6] show that this quantity is negligible thanks to the thick layer of Procelit™

180 placed in the back of the sample, so the calorimeter wasn’t used in this setup for the test campaigns

presented in this work.

A new setup for the sample holder is presented in section 3.7.1.

3.5 Intrusive Measurement Techniques

3.5.1 Heat Flux Probes

Copper heat flux calorimeters have been used for years in high enthalpy facilities in order to precisely

measure the heat flux to an high catalytic surface. In fact, despite the first experiments using the

LHTS principle used the assumption of a fully catalytic surface for copper, later on it was concluded

Page 43: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

Experimental Facilities and the LHTS Methodology 21

(a) FR Holder (b) ST Holder (c) EQ Holder

Figure 3.6: Sample Holders (Extracted from [7])

Figure 3.7: Sample Holder - Radiative Equilibrium Setup

Page 44: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

22 Experimental Facilities and the LHTS Methodology

Figure 3.8: Cross-section of the classical water-cooled copper calorimeter for heat flux measure-ments. Dimensions in mm.

that this isn’t a corrected assumption. Several campaigns were conducted in VKI to estimate the

true copper catalycity for the different test conditions and nowadays it is possible to use catalycity

tables to correct the copper catalycity used in the enthalpy rebuilding process [6, 7, 42, 43]. Some

extensive information about this topic can be found in [7].

There are two types of calorimeters available in VKI: the water cooled calorimeter and the slug

calorimeter. The later one was used in the past as reference and validator of the water cooled one [6]

and it wasn’t used in this work. From now on, the water cooled calorimeter will be just referenced as

calorimeter. The calorimeter work with a steady-state energy balance principle:

qcw =Q

A=m ⋅ cp ⋅ (Tout − Tin)

A(3.15)

In reference [44] an abacus is provided for the mass flow rate necessary in order to avoid water

boiling. In [44] and [45] uncertainty quantifications are done for the probe and the latter one proposes

the following formula for the relative error:

δqcwqcw

=

¿ÁÁÀ

(δm

m)

2

+ (δcp

cp)

2

+ (δ(Tout − Tin)

(Tout − Tin))

2

+ (δA

A)

2

(3.16)

According to the uncertainties presented in [7], for typical values of qcw (100 ∼ 2000 kW m−2) the

error vary between 7% and 12%.

3.5.2 Pitot Probes

A Pitot probe with the same geometry of the heat flux probe is used to perform stagnation pressure

measurements. The Plasmatron chamber is equipped with an absolute pressure transducer (Member-

anovac DM 12, Leybold Vacuum, OC Oerlikon Corporation AG, Pfäffikon, Switzerland) that measures

the static pressure with ±0.7 hPa accuracy. The Pitot line is connected to a Validyne variable reluc-

tance pressure transducer (DP15, Validyne Engineering Corp., Northridge, CA, USA) and the output

is amplified and corrected by a voltage demodulator (CD-15, Validyne Engineering Corp., Northridge,

CA, USA). Validyne and amplifier are calibrated by means of a Betz water manometer, leading to an

Page 45: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

Experimental Facilities and the LHTS Methodology 23

Figure 3.9: Heat Flux Probe with Water-Cooled Calorimeter

Figure 3.10: Pitot Probe

uncertainty of ±0.2% in the dynamic pressure (information extracted from [7]). In figure 3.10 one

can see an example of a pitot probe used in the Plasmatron.

3.6 Optical Measurement Techniques

3.6.1 Two-Colour Pyrometer

The two-colour pyrometers had proven to be one of the most reliable methods for practical radiative

temperature measurement. They measure the spectral radiance in two different, but close, wave-

lengths. Is allowed to assume that, between the two wavelengths, the body emissivity does not

change (gray body assumption). Then, the ratio between the spectral intensities allow to calculate

the temperature independently from the emissivity.

In the Plasmatron equipment, two two-color IR pyrometers (Marathon Series MR1SB and MR1SC,

Raytek Corp., Santa Cruz, CA) are available. They are selected according to the expected measured

Page 46: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

24 Experimental Facilities and the LHTS Methodology

temperature: the MR1SB operate between 700 and 1800°C and the MR1SC operate between 1000 and

3000°C. They work around 1µm wavelength, with a view angle of ∼35° relative to the sample normal

and through a 1cm thick quartz window. The acquisition rate is 1Hz and the overall uncertainty is

estimated to be ±10K. More information about these equipments and a mathematical description of

the working principle of a two-colour pyrometer can be found in [7].

3.6.2 Broadband Infrared Radiometer

A broadband IR radiometer (KT19, HEITRONICS Infrarot Masstechnik GmbH, Wiesbaden, Germany)

is placed with a view angle of ∼47° relative to the sample normal and it’s in front of a 1.8cm thick

window made of KRS-5. This material provides a 70% transparency over the whole range of the

operating waveband (0.6-39 µm). More information about this material can be found in [7]. The

output is the integrated thermal radiation over the operational spectrum, within a temperature range

of 0 to 3000°C and an acquisition rate of 1Hz was selected.

3.6.3 In-Situ Emissivity Determination Method

The in-situ emissivity measurement method currently used in the Plasmatron was introduced by

Panerai [7, 19] inspired on the work of Balat at al. [46].

In essence, the method is very simple. The out-coming radiation from the sample is measured by

the radiometer between the wavelengths 0.6µm and 39µm.

This radiation is than divided by the integrated blackbody radiation over the same wavelength

interval (the temperature is known from the Pyrometer reading) and the result is emissivity.

ε ≡ ε(T ) ≡ ε0.6-39µm(T ) =W0.6→39µm(T )

W 00.6→39µm(T )

(3.17)

The Planck’s law, equation 3.18, gives the spectral radiance as function of temperature and

corresponding wavelength and is integrated using the method proposed by Widger and Woodall [47]

that results in equation 3.19 with W 00→λ coming in W m−2 sr−1.

W 0(λ) =

2hc2

λ5 (e(

hckBλT

)

− 1)(3.18)

W 00→λ = 2

k4BT

4

h3c2

∑n=1

(ζ3

n+

3ζ2

n2+

n3+

6

n4) e−nζ with ζ =

2πhc

λkBT(3.19)

For the numerical calculation of the series, ∞ is substituted by nmax and using the relation

nmax = min (2 + 2/ζ,512) one can guaranty, at least, a 10 digit precision in the integration.

Page 47: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

Experimental Facilities and the LHTS Methodology 25

Figure 3.11: Optical Setup

3.6.4 Optical Emission Spectroscopy

The equipment for optical emission spectroscopy is described in [7] and following information is

adapted from there.

Optical emission spectroscopy is used to obtain qualitative information on the gas phase com-

position in front of the samples and detect the presence of relevant chemical species compared to

freestream conditions. The emitted light is collected through a variable aperture and focused by a

300 mm focal length converging lens (LA4579, Thorlabs GmbH, Munich, Germany) into the entry of

a 600 µm diameter optical fiber (Premium Fiber, Ocean Optics, Dunedin, FL). This lead to a broad

range (200-1100 nm) spectrometer (HR-4000, Ocean Optics, Dunedin, FL). An acquisition rate of

about 1 Hz provides real time acquisition spectra. In the present campaign the line of sight is main-

tained fixed in the stagnation line in 3 locations between 1mm and 9mm from the sample surface.

The calibration of the system in relative intensity is performed with a deuterium lamp in the UV range

(< 400 nm) and with a ribbon tungsten lamp in the visible (> 400 nm). The repeatability of the

measurements has been checked, ensuring the relative uncertainty on the total integrated emission

of the radiative signature to be less than 10%.

3.7 New Techniques Developed in the Context of this Work

3.7.1 Cooled Sample Setup

To achieve the objective of study the wall temperature effect on the catalycity of a TPS sample, a

new experimental setup was developed to be used in the Plasmatron. Recalling the equation 3.10

that is repeated were for commodity

qcond + qdiff + qrad,in = qrad,out + qloss

Page 48: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

26 Experimental Facilities and the LHTS Methodology

Condition I Condition II

Material SPS C/SiC SPS C/SiCTest S5 S23(a)qcw 160 1540ε 0.72 0.79Tw 1200 2000ps 5000 3000pd 25 165qexp 85 717γ 0.00264 0.0184

Table 3.2: Test Cases Used in the Design Process (data from [7])

we can conclude that in order to change the surface temperature without changing the aerother-

mochemical environment we must change the amount of incoming radiation (3rd term in LHS) or

change the conductive loss term (2nd term in RHS).

Reducing the amount of the incoming radiation will not allow reducing the wall temperature

because the incoming radiation effects are already negligible and it’s very difficult to achieve in a

practical way (probably only with help of cryogenic cooling). Besides all that, changes in the plasma

properties could happen because, above a certain temperature, plasma can be considered a radiative

participating medium. Any of the points listed above are enough to discard the incoming radiation

option. However, to increase the wall temperature this method is applicable but a super-heated

surface doesn’t have any real interest in the current frame of research. The remaining option is

changing the qloss term.

Almost since the beginning, the idea for cooling the sample was to use a calorimeter in the back of

the sample. The calorimeter serves two proposes: First it acts as an heat sink allowing the reduction

of the sample surface temperature through thermal conduction across the sample. Second because

it allows the measurement of the amount of qloss which is necessary to rebuild the surface catalycity.

The initial target was to use the same setup to cover the complete range of temperatures from the

radiative equilibrium temperature (the highest possible) to a temperature near the cold wall calorimeter

temperature (approx. 350K). Another requirement was to do it with the technical solutions available

because of the short calendar for testing and budget limitations.

In order to simulate the envelope of operation of the calorimeter, a small 1D simulator, called

heat1D, was programmed using the MATLAB™ environment. This program basically receives as

input the geometry, the working fluid, the Nu = f(Re,Pr, geometry) correlations and the boundary

conditions used and it allows to investigate the range of temperatures experienced by the different

components of the calorimeter cooling system. More details about this program can be found in

section 3.8.1.

Two test cases were selected from the data available in [7]: one representing an high HF environ-

ment and another representing a low HF environment. Details can be found in table 3.2.

The first working fluid tested was water because it has been used for years in the calorimeters

used in VKI and so the technical readiness level of such setup is quite high. The problem faced

Page 49: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

Experimental Facilities and the LHTS Methodology 27

Figure 3.12: High Temperature Calorimeter

was that it basically only allows a very narrow range for the wall temperature around 400K due to

the excellent properties of water as cooling fluid. This lead to the simulation of several different

alternative configuration by varying mass flow rate, inlet pipe diameter, materials and working fluids

in order to acess to different temperature levels. Also the idea of using a thin layer of high temperature

insulation in the back of the sample was introduced. This allow temperature levels that would be

impossible to achieve otherwise.

This finally conducted to a multi-mode solution that appears to be the optimal considering all

the constrains. An example of an operational map for this setup can be found in table 3.3. The final

design for the calorimeter is presented in figure 3.12.

Besides Water, also Air, Argon, Helium and Carbon Dioxide were tested as working fluids. Air

revealed to be the best in performance and technical simplicity for the situations were water is not

functional. Helium revealed to be an extremely good cooling fluid for this kind of applications but

in this particular case it is just “to good” because will conduct to results similar to water but with

technical and economical disadvantages. Carbon Dioxide as properties similar to air but it is interesting

for applications around 800K of calorimeter inner wall temperature because it has an abortion window

coincident with the radiative peak of a blackbody at the same temperature (approx. 4µm, see figure

3.13). Argon presents weak properties for this kind of application. In the end, Air and Water were

selected as working fluids.

The design of this calorimeter was quite challenging because of all constrains applied like maximum

metallurgic temperature, maximum outlet temperature and constructibility of all the components. For

future developments, the author recommends the reading the work of Zuckerman & Lior [48] because

of the very complete set of correlations available for jet impingement heat transfer.

Because of a heavy load of work in the VKI workshop, it was impossible in practical time to

prepare the new calorimeters needed for the original planed experience. The solution to overcome

this problem was to create an adapter to transfer the heat from the sample to an existent calorimeter

with the lowest temperature gradients in the sample as possible. The existent calorimeter can only

be used with water because of metallurgical constrains.

The final apparatus used in chapter 6 is presented in figure 3.14.

Page 50: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

28 Experimental Facilities and the LHTS Methodology

Figure 3.13: CO2 Absorption Spectrum in Absorption Length Unit

Wall Temperature [K]

<400 400 600 800 900 1200 1900 2000

Condition I Water Air Air -Water + Radiative

- -Thin Insulation Equilibrium

Condition II Water Air Air Air - -Water + Radiative

Thin Insulation Equilibrium

Table 3.3: Example of an operational map for the High Temperature Calorimeter for the twotest cases from table 3.2

Figure 3.14: Sample Holder - Cooled Sample Setup

Page 51: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

Experimental Facilities and the LHTS Methodology 29

50

100

150

200

200400

600800

10001200

14001600

1800

0

50

100

150

200

250

300

350

400

ps [hPa]q

cw [kW/m2]

p d [Pa]

Figure 3.15: pd Data and Correlation

3.7.2 New Correlation for Dynamic Pressure Estimation

Continuing the work of Marotta in VKI [15] it was noticed that the static pressure influence on dynamic

pressure was not explicit in the previous available correlations. To avoid time lost when post-processing

long lists of data with linear interpolations that can’t even guarantee a correct representation of the

static pressure effect, it was decided to crate a “single” formula of the type pd = f(qcw, ps) using

the previous database compiled by Marotta and also including some Plasmatron data that wasn’t

included in the previous work.

A non-linear least squares surface fit was done with help of a MATLAB™ script and several

different formulas were tested in order to achieve the best possible fit on the data. The data and the

fitted surface is represented in figure 3.15 and the final formula in equation 3.20. In this formula, qcwshould be introduced in kW m−2.

pd = A(1 +Bqcw)pCs +D

A = 31877.02

B = 0.004857

C = −0.935972

D = −0.832394

(3.20)

A study of the errors involved in the process was done and the conclusions are summarized in

figure 3.16. Despite some punctual measurements which have high relative deviations with respect

to the correlation (some times higher than 90%), one can see that the average relative error is

lower than 15% and the average absolute error is lower than 10 Pa. The r2 factor in this fit is

Page 52: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

30 Experimental Facilities and the LHTS Methodology

0 50 100 150 2000

200

400

600

800

1000

1200

1400

1600

1800

2000

ps [hPa]

q cw [k

W/m

2 ]

RELATIVE ERROR [%] Average Relative Error = 14%

Average Absolute Error = 7.1 Pa

0

10

20

30

40

50

60

70

80

90

100

Figure 3.16: Correlation Relative Error [%]

> 0.998. This is considered acceptable considering the experimental problems in the acquisition of

this data and fluctuations on the jet. According to Panerai [7], the typical uncertainty for the dynamic

pressure measurement in the Plasmatron is 20%, so the average error in the correlation is inside the

experimental uncertainty.

3.8 Brief Note on the Computational Methods Used

3.8.1 The heat1D script

This program was created to simulate the temperature of the sample, calorimeter, intermediate

insulation and coolant fluid inside the calorimeter, as a first approximation to check if the idea of

cooling a sample was possible or not. With the idea of simplicity in mind, the big challenge was to

create a easy method to have, at least, approximate values for the boundary conditions at the sample.

In this case, even the most complete methods can’t be trusted because the boundary conditions at

the wall of the sample exposed to plasma are in fact the ultimate target of this experiments.

A first rough method was tried by using convection coefficients between plasma and sample but

the final solution was found by analysing the work of Panerai [7]. In the experiments conducted

there, the heat flux transferred to the wall (q«w) was determined with precision through a radiative

equilibrium method2. In this method the terms qrad,in and qloss from equation 3.10 are neglected:

the first because of the low temperature of the test chamber and the second because of the thick

Procelit™ insulation placed in the back of the sample [6]. So lets consider that at the edge of the

2In reference [7], q«w is called qw

Page 53: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

Experimental Facilities and the LHTS Methodology 31

boundary layer the conditions (He, pe, βe i.e. the test conditions) remain constant with respect to the

radiative equilibrium test, ideally by submitting the two samples, in radiative equilibrium and cooled

configurations, to the same plasma jet and with the same probe geometry.

For this kind of testing, only the conditions at the wall and inside the boundary layer will change.

Lets then analyse the conditions one by one. At the wall, the variables playing are three: Temperature,

Catalycity and Emissivity. Temperature influence directly the conductive (qcond) and the “loss” (qloss)

terms as it can be checked in equation 3.11 and in combination with catalycity also the diffusion term

(qdiff ) through the species production rate at a catalytic wall (equation 3.14).

Temperature also influences the radiative heat flux (qrad,out) in combination with emissivity.

Emissivity is known to be a weak function of temperature [7, 49] but for this approximation it was

considered constant and equal to 0.8.

The main point of the approximation done was to consider that q«w does not change with wall

temperature. This is of course false but gives the “worst case scenario” for a first dimensioning of

the experience. What happens is that the qdiff term decreases with the reduction of wi,cat which

decreases with the reduction√Tw and γ. γ itself appears also to decreases with temperature which

was reported by different authors like Panerai [7] or Fourmond et al. [16].

Despite the fact that the decreasing of the wall temperature increases the conductive term (qcond)

it is known, specially for walls with an high catalycity, that this term is smaller compared with the

qdiff term so a global reduction of q«w is expected or at least a no increase of it.

The first step done in the program is to calculate the qloss term. That is made, using the

hypothesis explained above, simply by subtracting qrad,out = εσT 4w from q«w.

Then, using simple relations for 1D conduction and convection in the sample and in the calorimeter

(from Incropera et al. [49]) and imposing the calorimeter bulk temperature, all the temperatures can

be calculated.

To calculate the Nusselt number, three different correlations were used: The first come from an

old technical report written during the design phase of the Plasmatron equipment [44]. It was result

of numerical simulations and has the advantage that it was created directly for application at the

problem in study but it is only available for water. The other two are design correlations for confined

jets available in Li & Garimella [50], which result from experiments and are available for a wide range

of fluids. These last two correlations were preferred but the results from the first one are very similar.

The formula extracted from [44] is:

Nu = 2.047Re0.5(µwµin

)0.1

+ 5.848 (3.21)

The formulas extracted from [50] are:

Page 54: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

32 Experimental Facilities and the LHTS Methodology

Figure 3.17: Example of an output from heat1D

Nu = 0.676Re0.555Pr0.441(l/d)−0.071

(De/d)−0.276Ar

+ 1.133Re0.637Pr0.441(De/d)

−1.062(1 −Ar) for Water

(3.22)

Nu = 1.826Re0.473Pr0.441(l/d)−0.071

(De/d)−0.312Ar

+ 0.501Re0.724Pr0.441(De/d)

−1.062(1 −Ar) for Air

(3.23)

where l is the length of the inlet pipe, d is the inner pipe diameter, De is the diameter of the area

cooled by the confined jet and Ar is the area of the jet impingement region normalized with the total

area and is calculated using Ar = (1.9d/De)2.

A typical output of the code is presented in figure 3.17.

3.8.2 The ICP code and NDPs

As explained before in section 3.2.1, after the test being complete, a lot of information is still

missing and we need a “bridge” that is provided by CFD. Knowing the operation conditions of the

Plasmatron, one can than use the VKI ICP code to know the non-dimensional parameters (NDPs)

for the corresponding test. This solver will not be discussed in detail in this work but it is important

to say that it is a viscous reactive flow solver coupled with an electro-magnetic solver. It uses a

second-order accurate pressure-stabilized discretization on a collocated mesh that simulates the ICP

Page 55: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

Experimental Facilities and the LHTS Methodology 33

NDP C0 C1 C2 C3 C4 C5

Π1 +5.295E − 01 +2.005E − 07 −2.249E − 03 −3.637E − 08 +4.790E − 11 +9.125E − 06

Π2 +7.799E − 01 −1.724E − 05 −8.034E − 03 +9.231E − 08 +2.824E − 11 +3.521E − 05

Π3 +1.320E + 00 −3.090E − 05 −1.263E − 02 +1.824E − 07 +4.679E − 10 +5.528E − 05

Π4 +9.241E − 01 −1.815E − 05 −1.024E − 02 +6.531E − 08 +3.473E − 10 +4.486E − 05

Π5 +5.563E − 01 +2.126E − 06 −2.092E − 03 −7.657E − 09 −6.877E − 01 +8.847E − 06

Table 3.4: Constants for the NDPs Correlations

torch and part of the test chamber. For more details about this solver the reader is addressed to

specific literature [51, 52].

The solution depends on the power transmitted to the coil, static pressure, mass flow and swirl

angle (being this usually fixed). The power transmitted to the coil (also called ICP value) is related

with the power imposed on the High Frequency Generator by the generator efficiency. The generator

efficiency was estimated in the past as 50% [53] and recent sensitivity analysis shown that efficiencies

between 40% and 60% give a maximum difference in He with respect to the nominal efficiency bellow

0.6% [7].

To save CPU time and results processing time, the solutions for the ICP code are in a database.

Currently, solutions are available for mass flows of 16 g/s and 8 g/s. Only 16 g/s conditions were

used all along this work. The solutions for each NDP for all pairs (PW,ps) calculated in the past

were fit with polynomials. These correlations are valid for power values between 60 and 120 kW,

ICP value, and static pressures between 1500 Pa and 20000 Pa [7]. For all the NDPs, the regression

formula is

Πi = C0 +C1 ⋅ ps +C2 ⋅ PW +C3 ⋅ ps ⋅ PW +C4 ⋅ p2s +C5 ⋅ PW

2 (3.24)

Notice that in this formula the power should be in kW and the constants Ci are available in table

3.43.

Each NDP as a physical meaning that is explained in the following list4:

− Non-dimensional Thickness: Π1 =∆Rm

− Non-dimensional Velocity Gradient: Π2 = (dudx

)eRmv

− Non-dimensional Velocity Gradient Derivative: Π3 =ddy

(dudx

)e

R2m

v

− Non-dimensional Velocity: Π4 =Vev

− Modified Non-dimensional Velocity: Π5 =VeVe,d

3In fact, thanks to this correlations, the author never had to “lose” time running the ICP code in the clusteror studding it.

4Recently, the values used in the adimensionalization of NDPs have changed slightly so the following formulasshould be used very carefully.

Page 56: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

34 Experimental Facilities and the LHTS Methodology

3.8.3 The CERBOULA code

The code CERBOULA is in fact a code in two distinct parts: CERBERE and NEBOULA5. The

program that is executed is CERBERE and this one iteratively calls NEBOULA. Each one of them

will be shortly described in the next sections.

NEBOULA

This code is a solver for stagnation point axisymmetric boundary layers under the assumption of

thermal equilibrium and chemical nonequilibrium. It is assumed that the flow is laminar and only

steady-state is considered.

It was developed by Barbante [11] and it uses the PEGASE library developed by Bottin [54] for

thermodynamic and transport properties. The equations are discretized by Hermitian polynomials

and thanks to that the solution is forth order accurate. No more detailing about this code will be

done in this work being the reader advised to consult specific literature [11, 7].

Nevertheless, is important to say that the primary inputs for the program are the conditions at

the BL edge (He,pe,βe,ci,e,µe,etc.) plus the conditions at the wall (Tw,γ) and the main outputs are

qcond, qloss and q«w plus the temperature and species distribution inside the boundary layer.

This program is written in C and during all this work a seven species Air mixture model (Air-7)6

was used for the flow. For the gas phase reaction constants, the Dunn & Kang chemistry model [55]

was used for all the calculations except in the sensitivity analysis in section 7.2.1.

CERBERE

This code acts essentially as a pre and post processor for NEBOULA.

The user has several options available like, for example, enthalpy rebuilding, catalycity rebuilding

or abacus plotting, among others [56].

For enthalpy rebuilding the user gives all the BL edge parameters available (NDPs, pd and ps)

plus the probe radius, wall conditions at the calorimeter and the measured heat flux (qcw). The code

will than iterate the BL edge temperature (and consequentially also He) with a Newton loop until

the numerical heat flux calculated by NEBOULA (that is executed in each iteration) matches the

experimental one.

For catalycity rebuilding, the process is similar but instead of He (that is now known), the iterated

variable is γ.

To plot the heat flux abacus, the user just need to input the BL edge conditions and the NEBOULA

will calculate, for user selected pairs (Tw,γ), the corresponding heat flux.

5Sometimes this code is referred in the literature as “VKI Boundary Layer Code”6This model include the following species: O2, N2, NO, NO+, O, N and e–

Page 57: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

Experimental Facilities and the LHTS Methodology 35

NEBOULA

NDP1 …… NDP5

He , vs , ρe , βe , …

ps Rm pd

Operational Parameters

Geometry

Probe Measurements

Te(n+1)

Heat Flux Abacus

Sample Measurements

ICP Code

qcw(n) =qcw

(exp)

Tw

No

Yes

γ Catalycity

Flight

Conditions

ps m PWel Swirl ηgen

.

qcw

CERBERE

CERBOULA

PLA

SMA

TRO

N

Radiation

qloss

ε

qexp

CERBOULA

qexp(n) =qexp

(exp)

NEBOULA

NDPs

No γ(n+1)

Yes

CERBERE

Geometry

+

or

γref

Tcw

Figure 3.18: The Complete Experimental-Numerical Frame

3.8.4 The Complete Experimental-Numerical Frame

In figure 3.18 we try to give a complete view of how the data from the experiments is processed until

the final results are obtained, as explained in the previous sections.

Page 58: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

36

Page 59: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

Chapter 4

Numerical Simulations

In order to have a first feeling on the 2D effects in the cooled sample experiment a series of ther-

mal simulations were done using ANSYS™. It uses the finite element method and the element type

chosen for this work was a quadratic triangle and a serendipity quadratic quadrilateral. No further

considerations will be done about this method being the reader addressed to specialized literature

like Reddy [57]. The simulations were done in 2D axisymmetric mode and the symmetry axis is the

left vertical on the images. Because of the fallback of the original planed temperature campaign (see

section 3.7.1) also a quick simulation of the calorimeter adapter was made.

4.1 Cooled Sample Setup Simulation

As already explained in section 3.7.1, two different test cases were studied: one corresponding to low

HF and the other corresponding to high HF, respectively Condition I and Condition II. For simplicity,

the emissivity was considered always equal to 0.8 for the reasons already explained in section 3.8.1.

These two conditions were used to test three configurations of sample holders: without cooling, with

cooling and with cooling and intermediate insulation.

In figure 4.1 we can see an example of a mesh for the configuration with cooling. The meshes for

the other configurations are equivalent. The boundary conditions used were a convective surface in

the back with a bulk fluid temperature of 350K and a convection coefficient1 of 7000 W m−2 K−1, the

sample and cover being submitted to a constant HF and radiating to an enclosure at 400K. The initial

temperature was set to 300K. Details and results for the different configurations will be presented next.

Temperature fields for all the simulations are presented in Appendix A and Temperature vs. Time

graphics can be found in Appendix B and are from points along the symmetry axis.

1A value typical for the water calorimeters was used because no data is available for the cooling system of theholder itself.

37

Page 60: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

38 Numerical Simulations

Figure 4.1: Example of the Mesh

4.1.1 ST Sample Holder Without Cooling

This configuration was tested to access the validity of the approximations made in section 3.8.1. The

cover material used was the same used in the tests, Silicon Carbide (SiC).

4.1.2 ST Sample Holder With Cooling

The main objective of these simulations was to find if the lateral heat flux to the calorimeter could

“polute” the measured heat flux across the sample. The Temperature vs. Time graphics show that

the steady state for the sample area is achieved in less than 10 s. The holder in general only achieve

steady state after 75 s. Heat Flux fields can be found in figures 4.2 and 4.3.

The geometry simulated is very rough because, at this point, the final experimental setup was not

it fully defined/known which lead to the need of an extra simulation presented in section 6.2. Also a

small insulation was planed to be placed between the sample and the cover but it does not exist in

the final setup.

The conclusions for these simulation are that the lateral heat flux only has a negligible effect on

the final measurement for the two conditions.

Page 61: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

Numerical Simulations 39

Figure 4.2: HF Field - Cond. I

Figure 4.3: HF Field - Cond. II

Page 62: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

40 Numerical Simulations

Figure 4.4: HF Field - Cond. I

4.1.3 ST Sample Holder With Cooling and Insulation

In the same way as the simulations in the previous section, the objective of these simulations was to

find the lateral heat flux to the calorimeter. According to the Temperature vs. Time graphics, the

steady state for the sample area is also achieved in less then 80 s. Heat flux fields are presented in

figures 4.4 and 4.5.

The conclusion for these simulation are equal to the ones in section 4.1.2.

4.2 Calorimeter Adapter

As explained in section 3.7.1 there was the need of designing a calorimeter adapter.

The simulations done were similar to the simulations in section 4.1 with the exception that only

the sample and the adapter were simulated for simplicity and lack of time for modelling. Simulations

were made first for pure copper (λ = 400 W kg−1 K−1) and then for commercial bronze (λ = 50 W

kg−1 K−1) and for thicknesses of 5 and 3 mm. The results show that with 5 mm it’s possible to obtain

a maximum surface temperature difference lower then 4K for an adapter made of commercial bronze

with 5mm thickness for condition I which is more than acceptable for the proposed experiments.

Page 63: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

Numerical Simulations 41

Figure 4.5: HF Field - Cond. II

Figure 4.6: Temperature Field - 5mm adapter

Page 64: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

42 Numerical Simulations

Figure 4.7: Temperature Field - 3mm adapter

Page 65: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

Chapter 5

Oxidation Campaign

The objective of this campaign of tests was to establish the transition between Passive and Active

Oxidation in C/SiC TPM and also the identification of the operational limits of such material through

the investigation of the phenomena known as “temperature jump”.

The tests were done under the framework of the IXV project for the expansion of the ATDB

in order to help the design phase of this vehicle and were financed through an ESA’s Technology

Research Programme (TRP).

5.1 Testing Procedures

The testing procedure were similar for all the samples tested. Inside the Plasmatron test chamber

were installed a Pitot probe, an HF probe and the sample holder. Most of the tests were done using

the ST geometry for Pitot, HF probe and sample holder, but in the end of the test campaign some

were done using the FR geometry. These last tests are described in section 5.2.6.

The measurements with the intrusive probes were acquired before the sample injection into the

plasma and used to calibrate the jet. Afterwords, the optic instruments allow the measurement of the

sample temperature and emitted radiation. Besides that, also optical spectrometry data was acquired

from 3 points in or near the boundary layer region and the test was recorded with an High Definition

Camera. All the steps of the tests are listed below:

→ Chamber vacuum and pressure stabilization;

→ Plasma and data recording start-up;

→ Standard heat flux probe injection and power adjustment to the target heat flux;

→ Heat flux probe retraction and Pitot probe injection;

→ Pitot probe retraction and sample holder injection;

43

Page 66: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

44 Oxidation Campaign

Test Sample Tw Tw,pj qcw∗ ps pd mpre Time PWel

K K kW m−2 Pa Pa g s kW

16 HER-A16 1917 - 1021 2000 154 2.028 600 26415 HER-A15 1928 - 998 2000 151 1.996 600 26817 HER-A17 1973 - 1099 2000 164 2.031 600 2864 HER-A4 2065 - 1215 2000 178 2.085 600 3211 HER-A1 2077 - 1283 2000 187 2.083 600 3237 HER-A7 2115** 2512 1304 2000 189 2.039 200 322

5 HER-A5 1942 - 1194 5000 74 2.070 600 2702 HER-A2 1960 - 1230 5000 76 2.018 600 2838 HER-A8 1997 - 1304 5000 80 1.985 600 2919 HER-A9 2030 - 1404 5000 85 1.973 600 30410 HER-A10 2090 - 1417 5000 86 2.024 600 33111 HER-A11 2157 - 1501 5000 90 2.053 200 35213 HER-A13 2180*** 2734 1587 5000 95 2.047 130 384

3 HER-A3 1965 - 1320 6000 68 2.010 600 3026 HER-A6 1967 - 1345 6000 69 2.038 600 29918 HER-A18 1998 - 1392 6000 71 2.018 600 30319 HER-A19 2063 - 1499 6000 76 1.956 600 328

* Preliminary data to be verified** Jump temperature. Before jump, steady state was achieve with Tw=2095K*** Jump temperature

Table 5.1: Test Conditions for HER samples

→ Sample exposure to plasma for 10 minutes at stationary temperature (possible earlier interrup-

tion of a test in presence of very high temperatures and/or cooling issues in the system);

→ Plasma off and chamber ventilation;

→ Stop of data recording;

→ Samples recovery after system cooling;

Two different kinds of TPM were tested. Both are CMC C/SiC manufactured by Herakles and

MT Aerospace, that will be referred from now on as HER for the material manufactured by Herakles

and MTA for the one from MT Aerospace. Both are identical materials and they consist in a Silicon

Carbide matrix reinforced with Carbon Fiber so they can be classified as CMC. MTA also owns an

extra SiC layer coating the surface, deposited by chemical vaporization methods. HER will be used

to construct the nose and windward side of IXV and MTA will be used for the construction of the

control flaps of the same vehicle.

The test conditions are presented in the tables 5.1 and 5.2.

5.2 Results

The results of this testing campaign will be presented in this section together with results from

literature for comparison.

In this section, the notation qw will be used to represent qexp (= q«w).

Page 67: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

Oxidation Campaign 45

Test Sample Tw Tw,pj qcw∗ ps pd mpre Time PWel

K K kW m−2 Pa Pa g s kW

20 MTA-A1 1870 - 963 2000 146 3.623 600 26022 MTA-A3 1982 - 1122 2000 166 3.663 600 28321 MTA-A2 2014 - 1196 2000 176 3.711 600 30430 MTA-A11 2070** 2589 1237 2000 181 3.513 120 340

23 MTA-A4 1853 - 1210 5000 75 3.619 600 26024 MTA-A5 1956 - 1398 5000 85 3.701 600 29125 MTA-A6 2119 - 1575 5000 94 3.710 600 34831 MTA-A12 2060** 2542 1403 5000 85 3.501 120 283

26 MTA-A7 1981 - 1399 6000 71 3.645 600 32628 MTA-A9 2105 - 1497 6000 76 3.766 400 36232 MTA-A13 2130** 2593 1394 6000 71 3.701 120 320

* Preliminary data to be verified** Jump temperature

Table 5.2: Test Conditions for MTA samples

Test pO2 mpost rm/m Mass Loss Rate ε qw Te He γ OxidationPa g % mg cm−2 min−1 kW m−2 K MJ kg−1

16 452 2.0116 -0.814 0.297 0.747 571 5556 21.92 0.03081 P15 452 1.9453 -2.550 0.916 0.750 588 5534 21.50 0.03500 P17 454 1.9926 -1.900 0.695 0.735 631 5631 23.35 0.03531 P4 457 1.8430 -11.594 4.349 0.718 741 5739 25.47 0.04501 A1 459 1.8870 -9.418 3.531 0.696 735 5802 26.70 0.03972 A7 460 1.1751 -42.358 - 0.604* 760**|1364 5824 27.11 0.04217** J

5 1066 2.0644 -0.275 0.103 0.747 602 5826 22.65 0.01089 P2 1066 2.0098 -0.416 0.151 0.752 629 5857 23.20 0.01164 P8 1067 1.9639 -1.043 0.372 0.751 678 5920 24.33 0.01289 P9 1068 1.9470 -1.333 0.473 0.744 716 6004 25.87 0.01313 P/A10 1068 1.9139 -5.449 1.985 0.765 828 6011 25.99 0.01939 A11 1069 2.0197 -1.636 1.814 0.698 847 6077 27.19 0.01887 A13 1070 0.9123 -55.424 - 0.630 1996 6130 28.13 - J

6 1274 2.0287 -0.432 0.158 0.749 637 5985 24.61 0.00824 P18 1275 2.0060 -0.604 0.220 0.736 665 6024 25.31 0.00884 P19 1276 1.9016 -2.781 0.979 0.771 791 6109 26.83 0.01257 A

* During the steady state, the value is equal to 0.696** During the steady state. Calculated using Tw=2095K and ε =0.696

Table 5.3: Summarized Test Results - HER

5.2.1 General Results (ST geometry)

First, in tables 5.3 and 5.4, we present the rebuilt quantities calculated using the LHTS methodology,

more specifically using the ICP code results and running the CERBOULA code, and also some other

important quantities as, for example, mass loss rate. At the end of each table the estimated oxidation

regime is presented. The complete rebuilding results, including the NDPs used and the species

concentration at the boundary layer edge are presented in Appendix C.

To determine the oxidation regime, 3 criteria were used: visual inspection, mass loss rate (MLR)

and presence of a Silica layer detected using Scanning Electron Microscopy (SEM).

As a first approach, the visual appearance of the samples allow to roughly say if a sample went

through a passive, active regime or a temperature jump. The previous work of Panerai [7, 19] was

used as reference.

Description of the samples and images are presented in section 5.2.3. In the future, this is will

Page 68: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

46 Oxidation Campaign

Test pO2 mpost rm/m Mass Loss Rate ε qw Te He γ OxidationPa g % mg cm−2 min−1 kW m−2 K MJ kg−1

20 451 3.6028 -0.5548 0.3617 0.900* 624 5499 20.87 0.043771 P22 455 3.6018 -1.6654 1.0977 0.728 637 5655 23.81 0.034667 A21 457 3.5471 -4.4114 2.9457 0.737 688 5722 25.14 0.037660 A30 458 2.4481 -30.3092 - 0.617 1572 5755 25.79 - J

23 1066 3.6130 -0.1686 0.1098 0.907 606 5838 22.87 0.010231 P24 1068 3.6897 -0.3053 0.2033 0.852 706 5998 25.76 0.012318 P25 1070 3.5547 -4.1911 2.7982 0.755 863 6140 28.31 0.017719 A31 1068 2.4330 -30.5016 0.627 1484 6003 25.85 - J

26 1275 3.6476 0.0713 -0.0468 0.875 763 6030 25.42 0.012558 P28 1276 3.7446 -0.5682 0.5776 0.733 817 6097 26.62 0.014016 P/A32 1275 2.6605 -28.1043 - 0.616 1579 6025 25.33 - J

* Estimated. Radiometer failure during experiment.

Table 5.4: Summarized Test Results - MTA

probably be helpful for spacecraft maintenance routine checks.

The MLR allow a more scientific approach. It is known, from previous experiments which used a

real-time weight measurement, like the work done by Jacobson & Myers [20], that the mass loss rate

varies dramatically between passive and active oxidation and that fact is used as transition criteria.

Results are presented in figures 5.1 and 5.2. The letter A mark the samples that were submitted to

active oxidation.

We can clearly see a large increase in the MLR of the samples subjected to active oxidation with

respect to the ones subjected to the passive regime. One can also see that lower static pressures are

more destructive for the samples.

The SEM was used as a verification measurement, which allowed to confirm the presence/absence

of a glassy silica layer over the exposed surface, hence, cross-checking the predicted regime by the

other methods. The SEM analysis were preformed at PROMES, France.

An uncertainty analysis was done for the MLR determination. Knowing that the MLR is given by

the formula

MLR =mpost −mpre

A ∆t(5.1)

than it can be deducted that the relative uncertainty is given by

δMLRMLR

=

¿ÁÁÀδmpost

2+ δmpre

2

(mpost +mpre)2+ (

δ∆t

∆t)

2

+ (2πδD

4D)

2

(5.2)

The uncertainty for the temperature is given by the pyrometer specifications and it is equal to ±10K.

The observation, using SEM, of samples without a SiO2 layer which didn’t went through a tem-

perature jump, together with the analysis of the results of the visual inspection and the MLR, can

be used to declare, with relative confidence, that the temperature jump can’t be used as a marker of

the transition.

An interesting result can be found plotting the surface catalycity as function of the boundary layer

edge enthalpy. It can be observed in figure 5.3 that the catalycity has a relative increase during the

Page 69: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

Oxidation Campaign 47

1900 1950 2000 2050 2100 2150 22000

0.5

1

1.5

2

2.5

3

3.5

4

4.5

A

A

AA

A

Mass Loss Rate vs. Surface Temperature − HER

Surface Temperature [K]

Mas

s Lo

ss R

ate

[mg

cm−

2 min

−1 ]

HER, p

s=2000Pa

HER, ps=5000Pa

HER, ps=6000Pa

Figure 5.1: Mass Loss Rate - HER

1800 1850 1900 1950 2000 2050 2100 2150−0.5

0

0.5

1

1.5

2

2.5

3

3.5

A

A

A

A

Mass Loss Rate vs. Surface Temperature − MTA

Surface Temperature [K]

Mas

s Lo

ss R

ate

[mg

cm−

2 min

−1 ]

MTA, p

s=2000Pa

MTA, ps=5000Pa

MTA, ps=6000Pa

Figure 5.2: Mass Loss Rate - MTA

transition and such result goes in the same direction as the theory: active oxidation is equivalent to

a more reactive wall.

This sudden increase in γ can be used for determination of the PA transition but is not recom-

mended by the author. It implicate a very long measurement chain, subjected to several different

errors, which in the end conducts to an high uncertainty. In fact, previous UQ studies done by Vil-

ladieu et al. [58] and Panerai [7] point to uncertainties that can be bigger than the vertical range of

this graph. Plus, chemistry models involving Si in the gas phase are still missing in the code, including

the important exotermic reaction Si + OÐ→ SiO. Nevertheless, this method is valid but needs an

higher number of tests to guarantee its validity.

Page 70: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

48 Oxidation Campaign

22 23 24 25 26 27 28 290.01

0.011

0.012

0.013

0.014

0.015

0.016

0.017

0.018

0.019

0.02γ vs. BL Edge Enthalpy

BL Edge Enthalpy [MJ/Kg]

γ

Active

Passive

HER, ps=5000Pa

MTA, ps=5000Pa

Figure 5.3: Catalycity Coefficient γ evolution through the PA transition. One should note thatγ also depends on βe that is varying for each test condition, so the dash-doted line should notbe strictly interpreted as the evolution of γ with He. For more information, the author advisethe reader to consult [14].

5.2.2 Passive-to-Active Oxidation Transition Line

In this section we present our results together with our propose for a PA oxidation transition line,

based on the same trending of the result from the experiments done at PROMES using the MESOX

set-up using CVD SiC on C/SiC composits under microwave-excited air and presented by Balat (fig.

11 in [18]).

As we can see, our results are in very good agreement with the reference. The results are presented

in figures 5.4 and 5.5 as function of the oxygen partial pressure and reciprocal wall temperature. The

differences in the results can be attributed to the uncertainties and differences in the tested samples.

5.2.3 Visual Inspection of the Samples

Despite that the samples were submitted to scanning electron microscopy (SEM), a simple visual

inspection of them can deliver interesting information. In figure 5.6 we can see pictures of samples

that undergone different oxidation regimes for the same static pressure level (in this case 5000 Pa).

For the sample that undergone passive oxidation a yellow/brown/blue appearance can be observed

and it is associated to the existence of a thin silica layer in the surface. The colours change according

to the thickness of the silica layer. After active oxidation, the surface as a shiny look and one can

notice the reduction of the coating protection that makes the carbon fibres more exposed. After a

temperature jump, the surface is completely eroded and the black appearance is due to the residuals

of the carbon combustion. Also an appreciable reduction in thickness is noticeable.

Similar conclusions can be extracted for the MTA samples, with the pictures presented in figure

5.7.

Page 71: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

Oxidation Campaign 49

Figure 5.4: Passive-to-Active Transition - HER

Figure 5.5: Passive-to-Active Transition - MTA

Page 72: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

50 Oxidation Campaign

(a) Virgin Sample (b) After Passive Regime - Test 5

(c) After Active Regime - Test 10 (d) After Temperature Jump - Test 13

Figure 5.6: Examples of HER samples tested with ps=5000Pa

Page 73: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

Oxidation Campaign 51

(a) Virgin Sample (b) After Passive Regime - Test 24

(c) After Active Regime - Test 25 (d) After Temperature Jump - Test 31

Figure 5.7: Examples of MTA samples tested with ps=5000Pa

Page 74: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

52 Oxidation Campaign

0 100 200 300 400 500 600 7001400

1600

1800

2000

2200

2400

2600

T w, K

, sec

HER 1

(a) TEST 1 - No Jump

0 40 80 120 160 200 2401400

1600

1800

2000

2200

2400

2600

T w, K

, sec

HER 7

(b) TEST 7 - Temperature Jump

Figure 5.8: Temperature History During Two Different Tests - HER

5.2.4 The Temperature Jump

The temperature jump is a phenomena observed in TPM containing SiC and submitted to extreme

reentry environments. It was first reported by Lacombe & Lacoste [59] and after by other scientists

[60, 61].

More recently, I. Sakraker et al. [62], Marshall et al. [63] and Panerai [7] found the same phe-

nomena in experiments done in the Plasmatron at VKI. In this work we are going to avoid detailed

comments or explanations on this topic being the reader advised to consult Hald [64] or Marshall et

al. [63].

In figures 5.8 and 5.9 one can observe the difference in temperature evolution between a test

without jump and one with the jump. One should also notice that after the jump the temperature

is several hundreds of Kelvin above the cases without jump. These extreme temperatures, in an

enough long reentry manoeuvre would conduct to the destruction of the TPM and consequently of

the spacecraft.

In figure 5.10 we can see the evolution of emissivity for the two jump examples presented in figures

5.8 and 5.9. One can notice that after the jump, emissivity is reduced with respect to the condition

pre-jump. This was noticed to be a common behaviour for all jump cases.

The emissivity peaks that appear in the graphics are just an artefact generated by the measurement

system. The pyrometer is measuring the temperature in a circle with a diameter of ∼ 3mm concentric

with the sample. On the order hand, the radiometer is measuring the radiation from almost all the

sample. This correspond to an advance/delay in the two measurements due to the slow propagation

of the “jump front” across the sample.

In figure 5.11 one can see the visual recording of the “jump front” and the corresponding temper-

ature evolution.

Only when the surface is completely immersed into the jump state, the emissivity measurement

is reliable again. In conclusion, the emissivity data recorded during the jump should be ignored.

Page 75: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

Oxidation Campaign 53

0 100 200 300 400 5001400

1600

1800

2000

2200

2400

2600

2800T w

, K

MTA 28

(a) TEST 28 - No Jump

0 25 50 75 100 1251400

1600

1800

2000

2200

2400

2600

2800

T w, K

MTA 32

(b) TEST 32 - Temperature Jump

Figure 5.9: Temperature History During Two Different Tests - MTA

0250500750

1000

0 25 50 75 100 125 150 175 200 2250.50

0.75

1.00

W0.

6>39

m, k

W m

-2 s

r-1

Sample Blackbody

, sec

(a) TEST 7 - HER

0250500750

1000

0 25 50 75 100 1250.50

0.75

1.00

W0.

6>39

m, k

W m

-2 s

r-1

Sample Blackbody

, sec

(b) TEST 32 - MTA

Figure 5.10: Integrated Spectral Radiance and Emissivity History

Figure 5.11: Temperature Jump - Evolution in Time

Page 76: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

54 Oxidation Campaign

5.2.5 Optical Spectrometry Results

As referred before, optical spectrometry data was took during the tests. The spectrometers were

aligned in order to record the emission from 3 points in the boundary layer, at 2mm, 5.5mm and

9mm from the sample along the stagnation point axis. In figure 5.12 one can see the spectra recorded

with the flow already calibrated for the desired conditions with and without the sample in place. The

data was obtained with the same spectrometer, pointed 1.5mm away from the sample.

5.2.6 Frozen Geometry Tests

This tests, presented in figure 5.13, show the evolution of one Si emission line (with λ=288nm)

during a temperature jump. One can observe that the increase in emission starts before the measured

temperature jump because of the diffusion of Si in the boundary layer during the jump evolution and

the fact that the spectrometer doesn’t measure the emission in a single point but instead in a line

in front of the sample. In the last image we can see that in the last 20 sec. a jump started but the

jump front didn’t reach the centre of the sample before the end of the test.

Page 77: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

Oxidation Campaign 55

250 300 350 400 450 500 550 600 650 7000

1

2

3

4

5

6

7

8

9

10Spectra from Test 21, lower wavelengths

Wavelenghth [nm]

Inte

nsity

[a.u

.]

Si 251

Si 288

Si 391

Na 589FreestreamWith Sample, 1.5 mm

700 720 740 760 780 800 820 840 860 880 9000

10

20

30

40

50

60

Spectra from Test 21, higher wavelengths

Wavelenghth [nm]

Inte

nsity

[a.u

.]

O 777

N 742,744,746

N 818,821,824 O 844

N 868

← ←

FreestreamWith Sample, 1.5 mm

Figure 5.12: Spectra took during Test 21 (Active Oxidation). One should also notice the Sipeaks that appear in the presence of the sample. The arrows in the bottom figure indicate thereduction in intensity due to the recombination of the species in the BL and/or temperaturereduction.

Page 78: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

56 Oxidation Campaign

0 20 40 60 80 100 120 1401250

1500

1750

2000

2250

2500

T w [K

]

Temperature

0 20 40 60 80 100 120 1400

50

100

150

200

250

300 1.5 mm 5.5 mm 9.0 mm

I, a.

u.

Time

(a) Test M2 – ps = 2000 Pa, qcw = 1.1 MW m−2

0 20 40 60 80 100 120 140 160 1801250

1500

1750

2000

2250

2500

Temperature

0 20 40 60 80 100 120 140 160 1800

50

100

150

200

250 1.5 mm 5.5 mm 9.0 mm

Time

(b) Test M3 – ps = 2000 Pa, qcw = 1.0 MW m−2

0 20 40 60 80 100 120 140 160 180 2001250

1500

1750

2000

2250

2500

T w [K

]

Temperature

0 20 40 60 80 100 120 140 160 180 2000

15

30

45

60

75 1.5 mm 5.5 mm 9.0 mm

I, a.

u.

Time

(c) Test M4 – ps = 2000 Pa, qcw = 0.9 MW m−2

Figure 5.13: Emission Line Si288 Intensity Evolution During a Temperature Jump

Page 79: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

Chapter 6

Temperature Campaign

This campaign had the objective of investigate the effect of temperature in surface catalycity and heat

transfer on C/SiC TPM. The experience consist in fixing all the parameters in the BL edge (He, pe, βe)

and change only the surface temperature. This allow us to “isolate” the surface temperature effects.

On the original test campaign was programmed to investigate several temperature levels but in

consequence of issues in the manufacturing of the lab equipment1, only 2 temperature levels were

investigated as explained in section 6.1. The samples tested were manufactured by Snecma Propulsion

Solide.

6.1 Testing Procedures

Three tests were done in this experiment and all followed the same testing sequence which is described

below. In each test two samples were tested: one with the cooled setup, already described in

section 3.7.1 and one with the conventional insulated setup (see section 3.4). From now on the

sample installed in the cooled setup will be referred as cooled sample (CS) and the other as radiative

equilibrium sample (RS). In all the tests the geometries of the sample holder and the heat flux probe

were the ST one. Each test correspond to a different pair of (pe, βe) because we tried to keep He

constant and equal to 10MJ/kg.

→ Chamber vacuum and pressure stabilization;

→ Plasma generator and data recording start-up;

→ Heat flux probe injection and power adjustment to the target heat flux;

→ Heat flux probe retraction and cooled sample injection;

→ Cooled sample exposure to plasma for approx. 8 minutes;1One of the drawbacks of doing an experimental simulation is that it doesn’t depend only of our will

57

Page 80: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

58 Temperature Campaign

Test Sample qcw ps pd PWelkW m−2 Pa Pa kW

T1-CS S4 343 1440 93 138T1-RS S1 343 1440 93 138S6 [7] - 360 1300 83 99

T2-CS S5 381 5000 31 149T2-RS S2 381 5000 31 149S10 [7] - 390 5000 27 130

T3-CS S6 303 10000 13 142T3-RS S3 303 10000 13 142C2a [7] - 315 10000 11.8 137

Table 6.1: Test Conditions for the Temperature Campaign and Reference [7]

→ Cooled sample retraction and radiative equilibrium sample injection;

→ Radiative equilibrium sample exposure to plasma for approx. 8 minutes;

→ Plasma off and chamber ventilation;

→ Stop of data recording;

→ Samples recovery after system cooling;

In table 6.1 the test conditions are presented as well as some reference results extracted from [7].

The target HF was calculated before the tests using the NEBOULA code in order to match a BL

edge enthalpy of 10MJ/kg. Unfortunately, it is always impossible to match exactly the the desired

condition as consequence of uncertainties in the HF measurement, because the power is “tuned” in

real time but the real average value of HF is only acquired in post-processing and also because in

the preparation only an approximate value for the power was used. Nevertheless, the difference with

respect to the target He obtained in tests T1 and T2 was 6% and in test T3 was 13%. The error in T3

is higher because of lack of accurate power estimations during the preparation of the test campaign,

which was caused by a “last-moment” change in the test condition related with Plasmatron operation

constrains.

6.2 Results

The results of the campaign are summarized in table 6.2. As for the oxidation campaign, the complete

rebuilding results are presented in Appendix C and some considerations on the degree of dissociation

of the flow and on the temperature profile across the BL are presented on section 7.3.

During the experiments was noted that the HF measurement of qloss recorded by the DAC was

much higher than expected. It was found that there was two reasons for that. First there was a

question of concept in the the HF determination: the calorimeter probe doesn’t measure directly the

HF, it measures the heat rate, this value is then divided by the area of the calorimeter and the result

is the output value of the DAC. But, in fact, the area of the sample is higher than the area of the

Page 81: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

Temperature Campaign 59

Test βe Tw ε qrad qloss qexp Te pe He ρe γref γ

s−1 K kW m−2 kW m−2 kW m−2 K Pa MJ kg−1 kg m−3

T1-CS 6925.0 1375 0.82 167 43.7 210 4223 1440 9.3777 0.0009677418 0.10 0.026205T1-RS 6925.0 1513 0.86 257 0.0 257 4223 1440 9.3777 0.0009677418 0.10 0.079643S6 [7] 7277.0 1400 0.79 172 0.0 172 4440 1300 10.2487 0.0008190640 0.10 0.007280

T2-CS 2168.5 1374 0.78 157 52.8 210 4354 5000 9.4236 0.0032728925 0.10 0.005751T2-RS 2168.5 1528 0.82 254 0.0 254 4354 5000 9.4236 0.0032728925 0.10 0.018183S10 [7] 2097.8 1400 0.86 187 0.0 187 4485 5000 9.8197 0.0031588285 0.10 0.002204

T3-CS 935.2 1367 0.79 157 40.2 197 4085 10000 8.6575 0.0070697653 0.01 0.004082T3-RS 935.2 1449 0.94 235 0.0 235 4085 10000 8.6575 0.0070698046 0.01 0.011544C2a [7] 916.7 1515 0.90 269 0.0 269 4306 10000 9.1462 0.0066631346 0.01 0.023190

Table 6.2: Test Results From the Experiments and Reference [7]

calorimeter but the heat rate that crosses the surface of the sample is the same that crosses the

surface of the calorimeter (conservation of energy principle), than the heat rate should be divided

by the sample area, because that is the input for the 1D catalycity rebuilding process used in the

CERBOULA code (see section 3.8.3).

Second, it was found that the SiC sample holder was exchanging a huge amount of heat with the

sample (Qlat), i.e., the insulation created by the surface contact was to low to properly insulate the

sample, as it was expected prior to the experiment. In order to overcome this issue, a new numerical

simulation of the experiment was done, this time using the exact geometry tested2. A sketch of the

simulated geometry is presented in figure 6.1.

The calculation of the heat rates was done performing the heat flux integration over the area using

the HF results from the FEA considering cylindrical coordinates. The imposed heat flux in the wall

was the value obtained by measuring the radiative equilibrium sample. The final formula to correct

the measured heat flux at the calorimeter surface3 was again based on the conservation of energy

principle and it is

Qloss = Qcal − Qlat⇔

⇔Qloss = Qcal (1 −Qlat

Qcal)⇔

⇔qloss = qcalAcal

Asample(1 − F )

(6.1)

in which F is equal to 0.6894 and the numerical simulations shown that this value is a weak function

of the imposed heat flux for the ranges of this experiment. Using this method it is possible to obtain

a corrected value for the qloss term.

In figure 6.4 one can see the heat flux history graphic of test T1. The graphs for the other

experiments are similar.

2During the design phase simulations, presented in chapter 4, there were several unknowns like the exactsamples to be tested and the exact way the sample and the calorimeter would be installed.

3Output of the DAC.

Page 82: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

60 Temperature Campaign

Figure 6.1: Geometry tested and Simulated

Figure 6.2: Steady State Temperature Simulation

Page 83: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

Temperature Campaign 61

Figure 6.3: Steady State Heat Flux Simulation

600 800 1000 1200 1400 1600 18000

50

100

150

200

250

300Measured Heat Fluxes vs. Time − T1

Time [s]

Hea

t Flu

x [k

W/m

2 ]

CS RS

qexp

qrad

qloss

Figure 6.4: Heat Flux History of Test T1

Page 84: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

62 Temperature Campaign

300 400 500 600 700 800 900 1000 1100 1200 1300 1400 1500 16000

50

100

150

200

250

300

350

400HF Abacus − T1

Temperature [K]

Exp

erim

enta

l Hea

t Flu

x [k

W/m

2 ]

γ = 1

γ = 0.1

γ = 0.05

γ = 0.03

γ = 0.02

γ = 0.01

γ = 0.005

γ = 0

Reference (Copper)Cooled Sample (CS)Rad. Eq. Sample (RS)Cooled Sample (Rad. Only)Radiative HF (CS)Radiative HF (RS)

Figure 6.5: Abacus of test T1

6.2.1 Catalycity

The final output of the rebuilding process can than be obtained using the CERBOULA code and/or

the HF Abacus. The graphics are presented in figures 6.5, 6.6 and 6.7 and in the abacus of T2 (figure

6.6) one can observe some important HF quantities. These quantities are also presented in section

7.3.

We can also plot the result in a 3D graphic including all the boundary condition variables (except

enthalpy that is considered constant) and the result is presented in figure 6.8 together with the results

from [7]. A 2D version of the graph can be also plotted to increase the readability but one should

remember that pe and βe are independent parameters [14] and in order create the plot the βe values

were approximated (the approximation error is around 10%).

Appears that the slope of γ vs. Tw in a log scale doesn’t evolve with (pe,βe), which means that

γ is more sensible to Tw for (low pe, high βe) values. On the other hand, the slope of HF vs. Twseams to be independent of (pe,βe).

Page 85: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

Temperature Campaign 63

300 400 500 600 700 800 900 1000 1100 1200 1300 1400 1500 1600 17000

50

100

150

200

250

300

350

400HF Abacus − T2

Temperature [K]

Exp

erim

enta

l Hea

t Flu

x [k

W/m

2 ]

← q

loss →←

(a) →

γ = 1

γ = 0.1

γ = 0.05

γ = 0.03

γ = 0.02

γ = 0.01

γ = 0.005

γ = 0

Reference (Copper)Cooled Sample (CS)Rad. Eq. Sample (RS)Cooled Sample (Rad. Only)Radiative HF (CS)Radiative HF (RS)

Figure 6.6: Abacus of test T2 - (a): Reduction on the experimental heat flux due to the reductionon the surface temperature

300 400 500 600 700 800 900 1000 1100 1200 1300 1400 1500 16000

50

100

150

200

250

300

350HF Abacus − T3

Temperature [K]

Exp

erim

enta

l Hea

t Flu

x [k

W/m

2 ]

γ = 1γ = 0.08

γ = 0.03γ = 0.02

γ = 0.01

γ = 0.005

γ = 0

Reference (Copper)Cooled Sample (CS)Rad. Eq. Sample (RS)Cooled Sample (Rad. Only)Radiative HF (CS)Radiative HF (RS)

Figure 6.7: Abacus of test T3

Page 86: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

64 Temperature Campaign

13601380

14001420

14401460

14801500

15201540

01000

20003000

40005000

60007000

800010

−3

10−2

10−1

Tw

[K]

γ vs. BL edge Parameters − He ≈ 10MJ/kg

βe [s−1]

γ

pe = 1300 Pa

pe = 1440 Pa

pe = 5000 Pa

pe = 10000 Pa

(a) Complete Plot

1360 1380 1400 1420 1440 1460 1480 1500 1520 154010

−3

10−2

10−1

γ vs. BL edge Parameters − He ≈ 10MJ/kg

Tw

[K]

γ

p

e = 1300 Pa, β

e = 7277 s−1

pe = 1440 Pa, β

e = 6925 s−1

pe = 5000 Pa, β

e ≈ 2100 s−1

pe = 10000 Pa, β

e ≈ 920 s−1

(b) Approximate Plot

Figure 6.8: γ as function of the BL edge parameters

Page 87: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

Temperature Campaign 65

13601380

14001420

14401460

14801500

15201540

01000

20003000

40005000

60007000

8000150

200

250

300

Tw

[K]

HF vs. BL edge Parameters − He ≈ 10MJ/kg

βe [s−1]

q exp [k

W m

−2 ]

pe = 1300 Pa

pe = 1440 Pa

pe = 5000 Pa

pe = 10000 Pa

1360 1380 1400 1420 1440 1460 1480 1500 1520 1540170

180

190

200

210

220

230

240

250

260

270

HF vs. BL edge Parameters − He ≈ 10MJ/kg

Tw

[K]

q exp [k

W m

−2 ]

p

e = 1300 Pa, β

e = 7277 s−1

pe = 1440 Pa, β

e = 6925 s−1

pe = 5000 Pa, β

e ≈ 2100 s−1

pe = 10000 Pa, β

e ≈ 920 s−1

Figure 6.9: Experimental HF as function of the BL edge parameters

Page 88: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

66

Page 89: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

Chapter 7

Discussion of Results

7.1 Analysis of the Numerical Simulations

Taking into account the assumptions and approximations done for the boundary conditions and

material properties, it is clear that very good results in terms of temperature values can be obtained

using a finite element analysis specially for steady state.

Looking to the results of the simulation of the holder without cooling for condition I we can

observe that the holder reaches steady state after approx. 150s and the maximum temperature is

about 1070K. Considering that the time for steady state observed in the experiment was around 1min

and the temperature recorded was 1200K we can see that the numerical results are not in perfect

agreement with the experiment. Anyway, for steady state, the temperature relative error is 11%,

which is acceptable for this preliminary analysis.

The same doesn’t happen for condition II were the values are much more close to the experimental

values: time for steady state around 50s and temperature with a relative error of 0.7%. Specially for

steady state conditions, the approximation seems to give better results for higher heat flux.

For the simulation with cooling a comparison was done between the steady state results from

ANSYS™ and the results from heat1D. The values taken from the 2D simulation are from the sym-

metry axis. The results can be found in tables 7.1 and 7.2 and one can conclude that there is a good

agreement between the two methods, despite the fact that in the ANSYS™ simulations the materials

are non linear and, surfaces exchange heat through radiation with an enclosure at 400K instead of

deep space (0K) in heat1D and the convection coefficient is fixed.

67

Page 90: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

68 Results Discussion

Condition I Condition II

Outer wall Inner wall Outer wall Inner wall

ANSYS™ 363.8 363.4 464 460.2heat1D 367.9 362.2 501.6 454.1

Rel. Error [%] 1.13 0.32 8.11 1.33

a Values adimensionalized by the result of ANSYS

Table 7.1: Temperature results in the setup without insulation - ANSYS vs. heat1D

Condition I Condition II

Outer wall Interface Inner wall Outer wall Interface Inner wall

ANSYS™ 913.3 912.5 356.8 1832.2 1818.6 378.6heat1D 906 902.3 358 1880 1870 372

Rel. Error [%] 0.8 1.12 0.33 2.61 2.82 1.75

a Values adimensionalized by the result of ANSYS

Table 7.2: Temperature results in the setup with insulation - ANSYS vs. heat1D

7.2 Analysis of the Oxidation Campaign

7.2.1 Sensitivity Analysis

To access the reliability of the method, a sensitivity analysis was done in the catalycity determination

process. That was done by calculating the HF Abacus using three different sources for the gas reaction

constants: Dunn & Kang [55], Gupta et al. [65] and Park [66]1.

Two tests were selected (Test 1 and Test 28) and the results are presented in figures 7.1 and

7.2. One can notice that, for the temperatures and HF, the differences in the catalycity results are

negligible.

7.2.2 Flight Extrapolation

Using the LHTS methodology (see section 3.2), it is possible to extrapolate the tests done in the

Plasmatron to actual flight conditions. In figure 7.3 one can see the trajectory of the IXV vehicle and

the reconstructed tests. The IXV trajectory was obtained from [7, 67]. It appears that the vehicle

starts in an active oxidation region and than evolves to an passive region but that’s only an illusion.

In fact, in the experiments we simulate a steady-state condition, what would be equivalent to a

cruise condition at the same speed and altitude. A reentry manoeuvre is typically a transient condition

and as we can see in figure 2.2 the temperature in the surface starts by being relatively low due to the

fact that the spacecraft comes from the “outer space”. Afterwords, during the surface warming up, the

pressure is also increasing keeping the vehicle in a passive oxidation regime. After critical conditions

being achieve, it goes into an active oxidation region and finally, with the increasing pressure, back

to passive again.

1The BL edge condition were rebuilt using always the Dunn & Kang reaction constants.

Page 91: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

Results Discussion 69

300 550 800 1050 1300 1550 1800 2050 2300 2550 28000

125

250

375

500

625

750

875

1000

1125

1250

1375

1500

Temperature [K]

Wal

l Hea

t Flu

x [k

W m

−2 ]

γ = 1

γ = 0.1

γ = 0.05

γ = 0.03

γ = 0.02

γ = 0.01

γ = 0.005

γ = 0

Dunn & KangGupta et al.ParkReference (Cu)Experiment

Figure 7.1: Abacus from Test 1

300 550 800 1050 1300 1550 1800 2050 2300 2550 28000

125

250

375

500

625

750

875

1000

1125

1250

1375

1500

Temperature [K]

Wal

l Hea

t Flu

x [k

W m

−2 ]

γ = 1

γ = 0.1

γ = 0.05

γ = 0.03

γ = 0.02

γ = 0.01

γ = 0.005

γ = 0

Dunn & KangGupta et al.ParkReference (Cu)Experiment

Figure 7.2: Abacus from Test 28

Page 92: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

70 Results Discussion

Variation in qloss qloss [kW m−2] γ γ Rel. Error [%]

-50% 21.9 0.01562 40.40% 43.7 0.02621 -

+10% 48.1 0.02877 9.8+50% 65.6 0.04109 56.8+100% 87.4 0.06349 142.3

Table 7.3: Sensitivity Analysis for Test T1

Besides, one should take into attention that the BL edge velocity gradient is not the same that in

the IXV flight condition as it can be seen in figure 7.4, so some of the tests correspond to a vehicle

with a different effective nose radius. The effective nose radius can be calculated using equation 3.8.

One should also note that the tests simulate better the IXV case for the higher pressures. In [7],

Panerai showed that the EQ geometry is better for IXV simulations at low pressure.

Future work should be directed into the development of “transient flight extrapolation” capabilities

for the Plasmatron.

7.3 Analysis of the Temperature Campaign

In this section, some considerations on the boundary layer of the samples tested in this campaign will

be made.

First, lets look into the species present at the BL edge (figure 7.5). One can observe that almost

all the O2 is dissociated and also that small quantities of atomic N appear, specially for low pressures.

Looking now to the differences between the temperature profiles in the BL (figure 7.6), one can

notice that the difference in the shape of the curves is small near the wall, despite the difference in

the wall temperature. This only results in a tiny increase in the qcond term (figure 7.7).

In figure 7.7, one can also see that the behaviour predicted in section 3.8.1 was correct: Cooling

the sample (reducing Tw) conducts to an increase in the qcond term but also to a major decrease in

the qdiff term, due to catalycity decrease, which results in a global reduction of q«w.

7.3.1 Sensitivity Analysis

A sensitivity analysis on the catalycity rebuilding process was done considering that errors on qlossmeasurement and correction can occur. Experiment T1 was selected for the sensitivity study and the

results are presented in table 7.3. One should note that even if the qloss term had been underestimated

by half of its value, the value of γ would still be lower than the value measured in the RS.

A complete UQ of the experiments was impossible in practical time because of the complexity

of the software DAKOTA+CERBOULA [7] together with the need of modifications to accommodate

the latest version of the CERBOULA code developed in the context of this work. Nevertheless the

author consider that it is a mandatory step in future work.

Page 93: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

Results Discussion 71

0 1000 2000 3000 4000 5000 6000 7000 8000 9000

30

40

50

60

70

80

90

100

110

120

Flight Velocity [m/s]

Alti

tude

[km

]

IXV trajectoryTests − Passive Ox.Tests − Active Ox.Tests − Temp. JumpMach = 15Mach = 20Mach = 25

5500 6000 6500 7000 7500 800065

66

67

68

69

70

71

72

73

74

75

76

Flight Velocity [m/s]

Alti

tude

[km

]

IXV trajectoryTests − Passive Ox.Tests − Active Ox.Tests − Temp. Jump

Figure 7.3: Extrapolated Fight Conditions - Oxidation Campaign

Page 94: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

72 Results Discussion

0 5 10 15 20 25 300

2000

4000

6000

8000

10000

12000

BL Edge Enthalpy [kJ/kg]

BL

Edg

e V

eloc

ity G

radi

ent [

s−1 ]

IXVTests − p

s = 2000

Tests − ps = 5000

Tests − ps = 6000

Figure 7.4: Extrapolated Velocity Gradient - Oxidation Campaign

0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1

T1

T2

T3

Mass Fractions at the BL Edge

O

2

N2

NO

NO+

ON

e−

Figure 7.5: Mass Fractions at the BL Edge

Page 95: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

Results Discussion 73

y-coordinate [m]

Tem

pera

ture

[K]

0 0.002 0.004 0.006 0.008 0.010

500

1000

1500

2000

2500

3000

3500

4000

4500

Temp. - CSTemp. - RS

Figure 7.6: Temperature Evolution Inside the Boundary Layer - Test T1

T1cs T1rs T2cs T2rs T3cs T3rs0

50

100

150

200

250

300

Wal

l Hea

t Flu

x [k

W m

−2 ]

q

cond

qdiff

Figure 7.7: Heat Flux to the Wall

Page 96: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

74 Results Discussion

Velocity [m/s] Mach Altitude [km] Static Pressure [Pa] Static Temperature [K] Effective Nose Radius [m]

4331 14.6 69.8 4.8 218 0.294341 13.9 60.6 18.6 244 0.934161 12.8 54.4 43.3 261 2.08

Table 7.4: Extrapolated Flight Conditions

0 1000 2000 3000 4000 5000 6000 7000 8000

30

40

50

60

70

80

90

100

110

120

Flight Velocity [m/s]

Alti

tude

[km

]

IXV trajectoryT1T2T3Mach = 13Mach = 14Mach = 15

Figure 7.8: Extrapolated Flight Conditions

7.3.2 Flight Extrapolation

In figure 7.8 and table 7.4 one can see the reconstructed flight conditions and the values of the

effective nose radius of an hypothetical cruise vehicle which nose stagnation point would be subjected

to the same aerothermodynamic environment as the tested samples.

7.4 Stagnation Point ATDB Algorithm

The ultimate target of TPS testing is to help the decision process and dimensioning of the TPS to

be installed in future space missions.

Nowadays, very old and conservative formulas to estimate the heat transfer to the wall are still in

use (see section 2.1.2). This happens because design engineers like to have very simple formulas in

order to introduce them in the fast optimization loops used during the preliminary-design phase of a

project. The objective is always to know the heat flux from the plasma to the wall and it’s known

that it depends on 4 parameters: He,pe,βe,Tw besides surface material and gas mixture. In fact, for

a given material and gas mixture the HF dependencies can be summarized in the following formulas.

Page 97: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

Results Discussion 75

q«w = q©w (7.1)

q«w = f(He, pe, βe, Tw) (7.2)

q©w = f (Tw,(−λ∂T

∂y)w,sol

, ε(Tw)) (7.3)

In equation 7.2 we can also include the term γ = f(Tw, ...) but it is a characteristic of the material

Using the current setup in the Plasmatron, it is possible to make complete reconstruction of

stagnation point boundary layer of a body immersed in an hypersonic flow. Then, knowing the

conditions in the boundary layer edge, it is possible to obtain all the other relevant properties.

One should remember that the cooled setup allows to define the surface temperature and also that

catalycity depends on wall temperature.

With all this in mind, the correct way to construct a steady-state ATDB seems to be the one

presented in the figures 7.9 and 7.10. For each flight condition, should be done a set of tests to access

different velocity gradients (it varies with nose radius and flight conditions). For radiative equilibrium

TPS types this is enough and the wall temperature is also a result but for active-passive or active

TPS types (see section 1.2), additional tests for several wall temperatures must be conducted.

All the information can then be stored in tables and allow a fast and easy method to know heat

flux or catalycity to be implemented in future design or CFD codes.

In the figures, the thick boxes represent the inputs for the ATDB and the thick dashed boxes the

results from the ATDB.

Page 98: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

76 Results Discussion

Figure 7.9: Flowchart for ATDB Algorithms - Hot or Insulated Structure TPS

Figure 7.10: Flowchart for ATDB and Algorithms - Generic TPS

Page 99: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

Chapter 8

Conclusions and Future Work

8.1 Conclusions

In this work, the Passive-to-Active oxidation transition of C/SiC TPM in Earth’s reentry aerothermo-

chemical environment was determined by experimental methods and the results are in good agreement

with the data available in literature. Also it was proved that the temperature jump phenomena can’t

be considered a indicator of the PA transition.

Also the method used to estimate the heat flux to cooled walls presented in section 3.8.1 and

its applicability to 2D thermal simulations, without direct fluid simulation, proved to be a valuable

method for quick estimation of heat transfer rates for Plasmatron equipment or even for reentry

spacecraft design whenever data for the TPM in radiative equilibrium conditions is available.

A new method for TPS testing was developed, allowing now the tests of Convective Cooling,

Heat Pipe and Heat Sink Structure TPS in the VKI’s Plasmatron. This new method also allows

the correctly study of the wall temperature effect on catalycity for fixed flight conditions. With this

method it was discovered that both catalicity and heat flux to the wall decrease by decreasing the

surface temperature. It was also discovered that γ is more sensible to variations in Tw for (low pe,

high βe) values and that the sensitivity of the heat flux to variations on Tw seems to independent of

(pe,βe).

Efficient computational methods for construction and use of stagnation point aerothermodynamic

databases are also presented.

8.2 Recommendations for Future Work

Further theoretical investigations must be done to understand better the temperature jump phenom-

ena and it’s causes. Introduction of more chemical reactions and models is also important, specially

in the boundary layer code (NEBOULA).

77

Page 100: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

78 Conclusions

A redesign of the sample holders is mandatory to decrease the errors associated with the lateral

heat flux in the cooled sample configuration. Expanding the Temperature Campaign to different

velocity gradients by using the frozen and equilibrium holders in a cooled sample configuration could

be also an important improvement.

Also, further improvements are necessary to correctly simulate reentry conditions in terms of

velocity gradient and transient effects. New probes are necessary to achieve a time continuous

complete simulation of TPS in the Plasmatron.

Careful radiation analysis are also important for future work. Inside the test chamber the sample

faces the torch gas which irradiates large amounts of energy because of it’s high temperature. This

doesn’t happen in flight so must be taken into account during the calculation of the experimental

heat flux. Maps for the incoming radiation could maybe be constructed using the radiation transport

capabilities of the ICP code.

Page 101: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

References

[1] J. J. Bertin and R. M. Cummings, “Fifty years of hypersonics: where we’ve been, where we’re

going,” Progress in Aerospace Sciences, vol. 39, pp. 511–536, August-October 2003.

[2] E. Mooij, “Re-entry systems course notes.” Delft University of Technology, 2011.

[3] J. D. Anderson, Hypersonic and High Temperature Gas Dynamics. New York: AIAA, 2nd ed.,

2006.

[4] D. E. Glass, “Ceramic Matrix Composite (CMC) Thermal Protection Systems (TPS) and Hot

Structures for Hypersonic Vehicles,” in 15th AIAA International Space Planes and Hypersonic

Systems and Technologies Conference, AIAA 2008-2682, (Dayton, OH, USA), April-May 2008.

[5] H. N. Kelly and M. L. Blosser, “Active Cooling From The Sixties to NASP,” in Current Tech-

nology for Thermal Protection Systems, NASA CP 3157, 1992.

[6] O. Chazot, “Hypersonic Stagnation Point Aerothermodynamics in Plasmatron Facilities,” in

Course on Hypersonic Entry and Cruise Vehicles, Stanford University and NASA Ames Research

Center (in collaboration with von Karman Institute for Fluid Dynamics), 2008.

[7] F. Panerai, Aerothermochemistry Caracterization of Thermal protection Systems. PhD thesis,

Università degli Studi di Perugia, von Kármán Institute for Fluid Dynamics, February 2012.

[8] D. A. Pejaković, J. Marschall, L. Duan, and M. P. Martin, “Nitric Oxide Production from Surface

Recombination of Oxygen and Nitrogen Atoms,” Journal of Thermophysics and Heat Transfer,

vol. 22, pp. 178–186, 2008.

[9] D. A. Pejaković, J. Marschall, L. Duan, and M. P. Martin, “Direct Detection of NO Produced

by High-Temperature Surface-Catalyzed Atom Recombination,” Journal of Thermophysics and

Heat Transfer, vol. 24, no. 3, pp. 603–611, 2010.

[10] J. Thoemel, Heterogeneous Catalysis in High Enthalpy Flows. PhD thesis, RWTH Aachen

University, von Karman Institute for Fluid Dynamics, 2011. To be published.

79

Page 102: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

80 References

[11] P. F. Barbante, Accurate and Efficient Modelling of High Temperature Nonequilibrium Air Flows.

PhD thesis, Université Libre de Bruxelles, von Kármán Institute for Fluid Dynamics, 2001.

[12] R. Goulard, “On Catalytic Recombination Rates in Hypersonic Stagnation Heat Transfer,” Jet

Propulsion, vol. 28, no. 11, pp. 737–745, 1958.

[13] L. A. Anderson, “Effect of surface catalytic activity on stagnation heat-transfer rates.,” AIAA

Journal, vol. 11, pp. 649–656, May 1973.

[14] O. Chazot, F. Panerai, and M. Marotta, “Ground testing for gsi database, what do we deter-

mine?,” in 7th European Aerothermodynamics Symposium, (Brugge, Belgium), 2011.

[15] M. Marotta, “Investigation on the Driving Phenomena Characterizing Gas/Surface Interactions

in Plasmatron Facility,” VKI Project Report 2011-17, von Karman Institute for Fluid Dynamics,

2011.

[16] C. Fourmond, G. D. Rold, F. Rousseau, C. Guyon, S. Cavadias, D. Morvan, and R. Mévrel,

“Characterisation of thermal barrier coatings and ultra high temperature composites deposited

in a low pressure plasma reactor,” Journal of the European Ceramic Society, vol. 31, no. 13,

pp. 2295 – 2302, 2011.

[17] M. Balat, G. Flamant, G. Male, and G. Pichelin, “Active to Passive Transition in the Oxidation

of Silicon Carbide at High Temperature and Low Pressure in Molecular and Atomic Oxygen,”

Journal of Materials Science, vol. 27, no. 3, pp. 697–703, 1992.

[18] M. J. H. Balat, “Determination of the Active-to-Passive Transition in the Oxidation of Silicon

Carbide in Standard and Microwave-Excited Air,” Journal of the European Ceramic Society,

vol. 16, no. 1, pp. 55–62, 1996.

[19] F. Panerai and O. Chazot, “Characterization of gas/surface interactions for ceramic matrix

composites in high enthalpy, low pressure air flow,” Materials Chemistry and Physics, vol. 134,

no. 2-3, pp. 597 – 607, 2012.

[20] N. Jacobson and D. Myers, “Active Oxidation of SiC,” Oxidation of Metals, vol. 75, no. 1-2,

pp. 1–25, 2011.

[21] C. Wagner, “Passivity during the Oxidation of Silicon at Elevated Temperatures,” Journal of

Applied Physics, vol. 29, no. 9, pp. 1295–1297, 1958.

[22] E. T. Turkdogan, P. Grieveson, and L. S. Darken, “Enhacement of Diffusion-Limited Rates of

Vaporization of Metals,” The Journal of Physical Chemistry, vol. 67, no. 8, pp. 1647–1654,

1963.

Page 103: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

References 81

[23] E. A. Gulbransen and S. A. Jansson, “The High-Temperature Oxidation, Reduction, and

Volatilization Reactions of Silicon and Silicon Carbide,” Oxidation of Metals, vol. 4, no. 3,

pp. 181–201, 1972.

[24] S. C. Singhal, “Thermodynamic Analysis of the High-Temperature Stability of Silicon Nitride

and Silicon Carbide,” Ceramurgia International, vol. 2, no. 3, pp. 123–130, 1976.

[25] J. W. Hinze and H. C. Graham, “The Active Oxidation of Si and SiC in the Viscous Gas-Flow

Regime,” Journal of The Electrochemical Society, vol. 123, no. 7, pp. 1066–1073, 1976.

[26] K. G. Nickel, “The Role of Condensed Silicon Monoxide in the Active-to-Passive Oxidation

Transition of Silicon Carbide,” Journal of the European Ceramic Society, vol. 9, no. 1, pp. 3–8,

1992.

[27] L. H. Keys, “The Oxidation of Silicon Carbide,” in Properties of High Temperature Alloys with

Emphasis on Environmental Effects (Z. A. Foroulis and P. F. S., eds.), vol. 77, (Princeton, NJ,

USA), The Electrochemical Society, 1977.

[28] T. Narushima, T. Goto, and T. Hirai, “High-Temperature Passive Oxidation of Chemically Vapor

Deposited Silicon Carbide,” Journal of the American Ceramic Society, vol. 72, no. 8, pp. 1386–

1390, 1989.

[29] A. H. Heuer and V. L. K. Lou, “Volatility Diagrams for Silica, Silicon Nitride, and Silicon

Carbide and Their Application to High-Temperature Decomposition and Oxidation,” Journal of

the American Ceramic Society, vol. 73, no. 10, pp. 2789–2803, 1990.

[30] A. F. Kolesnikov, “Combined Measurements and Computations of High Enthalpy and Plasma

Flows for Determination of TPM Surface Catalycity,” in Educational Notes RTO-EN-AVT-008,

RTO, 1999.

[31] D. A. Stewart, “Surface Catalysis and Characterization of Proposed Candidate TPS for Access-

to-Space Vehicles,” Technical Memorandum 112206, NASA Ames Reasearch Center, Moffett

Field, CA, USA, July 1997.

[32] J. Marschall, “Experimental Determination of Oxygen and Nitrogen Recombination Coefficients

at Elavated Temperatures Using Laser-Induced Fluorescence,” in 1997 National Heat Transfer

Conference, (Baltimore, MD), 1997.

[33] D. A. Stewart, J. V. Rakich, and M. J. Lanfranco, “Catalytic Surface Effects Experiment on the

Space Shuttle,” in 31st AIAA Thermophysics Conference, AIAA 1981-1143, (Palo Alto, CA),

1981.

[34] D. A. Stewart and S. Bouslog, “Surface Characterization of Candidate Metallic TPS for RLV,”

in 33rd AIAA Thermophysics Conference, AIAA 1999-3458, (Norfolk, VA, USA), 1999.

Page 104: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

82 References

[35] C. D. Scott, “Catalytic Recombination of Nitrogen and Oxygen on High-Temperature Reusable

Surface Insulation,” in 15th AIAA Thermophysics Conference, AIAA 1980-1477, (Snowmass, CO,

USA), July 1980.

[36] J. A. Fay and F. R. Riddell, “Theory of Stagnation Point Heat Transfer in Dissociated Air,”

Journal of Aeronautical Science, vol. 25, no. 2, pp. 73–85, 1958.

[37] L. Lees, “Laminar Heat Transfer Over Blunt-Nosed Bodies at Hypersonic Flight Speeds,” Jet

Propulsion, vol. 26, no. 4, pp. 259–269, 274, 1956.

[38] A. F. Kolesnikov, “Conditions of Simulation of Stagnation Point Heat Transfer from a High-

enthalpy Flow,” Fluid Dynamics, vol. 28, no. 1, pp. 131–137, 1993.

[39] COESA: US Commission/Stand Atmosphere (Compiler), Natl. Oceanic & Atmospheric Admin

(Collaborator), Natl. Aeronautics & Space Admin (Collaborator), United States Air Force (Col-

laborator), U.S. Standard Atmosphere, 1976 (NOAA Document S/T 76-1562). NOAA, NASA,

USAF, 1st ed., 1976.

[40] V. V. Lunev, Hypersonic Aerodynamics. Moscow, Russia: Maschinostroenie, 1975. (in Russian).

[41] G. Degrez, P. Barbante, M. de la Llave, T. Magin, and O. Chazot, “Determination of the

Catalytic Properties of TPS Materials in the VKI ICP Facilities,” in European Congress on

Computational Methods in Applied Sciences and Engineering, ECCOMAS Computational Fluid

Dynamics Conference, (Swansea, Wales, UK), September 2001.

[42] H.-W. Krassilchikoff, “Procedures for the Determination of the Cold Copper Catalycity,” VKI

Project Report 2006-18, von Karman Institute for Fluid Dynamics, 2006.

[43] H. W. Krassilchikoff, O. Chazot, and J. Thoemel, “Procedure for the Determination of Cold Cop-

per Recombination Efficiency,” in 2nd European Conference for Aero-Space Sciences (EUCASS),

(Bruxelles, Belgium), July 2007.

[44] J. F. Lumens, B. Bottin, and M. Carbonaro, “Design of a Steady-State Heat Flux Probe for

Measurements in an Induction-Heated Plasma Flow,” in ICIASF ’97 Record (F. K. Owen, ed.),

(Pacific Grove, CA), IEEE Publication 97CH36121, Septemebr-October 1997.

[45] B. Bottin, O. Chazot, M. Carbonaro, V. van der Haegen, and S. Paris, “The VKI Plasmatron

Characteristics and Performance,” in Educational Notes RTO-EN-AVT-008, RTO, 1999.

[46] M. Balat-Pichelin, J. F. Robert, and J. L. Sans, “Emissivity Measurements on Carbon Carbon

Composites at High Temperature under High Vacuum,” Applied Surface Science, vol. 253, no. 2,

pp. 778–783, 2006.

[47] W. K. Widger and M. P. Woodall, “Integration of the Planck Blackbody Radiation Function,”

Bulletin of the American Meteorological Society, vol. 57, no. 10, pp. 1217–1219, 1976.

Page 105: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

References 83

[48] N. Zuckerman and N. Lior, “Jet impingement heat transfer: physics, correlations, and numerical

modeling,” in Advances in heat transfer, vol. 39, pp. 565–631, Elsevier - Academic Press, 2006.

[49] F. P. Incropera, DeWitt, Bergman, and Lavine, Fundamentals of Heat and Mass Transfer. John

Wiley & Sons, 2006.

[50] C.-Y. Li and S. V. Garimella, “Prandtl-number effects and generalized correlations for confined

and submerged jet impingement,” International Journal of Heat and Mass Transfer, vol. 44,

no. 18, pp. 3471–3480, 2001.

[51] P. Rini, Analysis of Differential Diffusion Phenomena in High Enthalpy Flows, with Application to

Thermal Protection Material Testing in ICP Facilities. PhD thesis, Université Libre de Bruxelles,

von Karman Institute for Fluid Dynamics, 2006.

[52] G. Degrez, D. P. Vanden Abeele, P. F. Barbante, and B. Bottin, “Numerical Simulation of

Inductively Coupled Plasma Flows under Chemical Non-equilibrium,” International Journal of

Numerical Methods for Heat & Fluid Flow, vol. 14, no. 4, pp. 538–558, 2004.

[53] M. de la Llave Plata, “Analysis and Application of a Methodology for the Determination of TPS

Material Catalycity,” VKI Project Report 2000-04, von Karman Institute for Fluid Dynamics,

2000.

[54] B. Bottin, D. P. Vanden Abeele, M. Carbonaro, G. Degrez, and G. S. R. Sarma, “Thermodynamic

and Transport Properties for Inductively Plasma Modeling,” Journal of Thermophysics and Heat

Transfer, vol. 13, no. 3, pp. 343–350, 1999.

[55] M. G. Dunn and K. S.-W., “Theoretical and Experimental Studies of Reentry Plasmas,” Con-

tractor Report 2232, NASA Langley Research Center, Hampton, VA, USA, 1973. Prepared by

Cornell Aeronautical Laboratory, Inc., Buffalo, NY,14221.

[56] H. W. Krassilchikoff, “User’s guide for CERBERE 2.0,” tech. rep., von Karman Institute for Fluid

Dynamics, August 2006.

[57] J. Reddy, An Introduction to the Finite Element Method. McGraw-Hill Series in Mechanical

Engineering, McGraw-Hill, 2006.

[58] N. Villedieu, F. Panerai, T. E. Magin, and O. Chazot, “Uncertainty Quantification for Gas-

Surface Interation in the VKI Plasmatron,” in 7th European Aerothermodynamics Symposium,

(Brugge, Belgium), 2011.

[59] A. Lacombe and M. Lacoste, “Investigation of C/SiC Breaking-Point Under Arc Jet Environment

at NASA-JSC,” High Temperature Chemical Processes, vol. 3, pp. 285–296, 1994.

Page 106: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

84 References

[60] T. Laux, G. Herdrich, and M. Auweter-Kurtz, “Oxidation Behavior of Sintered Silicon Carbide

in Various Plasma Wind Tunnels,” in 4th European Workshop on Hot Structures and Thermal

Protection Systems for Space Vehicles, (Palermo, Italy), November 2003.

[61] G. Herdrich, M. Fertig, S. L’ole, S. Pidan, , M. Auweter-Kurtz, and T. Laux, “Oxidation Behavior

of Siliconcarbide-Based Materials by Using New Probe Techniques,” Journal of Spacecraft and

Rockets, vol. 42, no. 5, pp. 817–824, 2005.

[62] I. Sakraker, C. O. Asma, and F. Panerai, “Experimental Study on the Passive-Active Oxida-

tion Transition of the FAST 20XX SpaceLiner Thermal Protection System,” in 4th European

Conference for Aero-Space Sciences (EUCASS), (San Petersburg, Russia), 2011.

[63] J. Marschall, D. A. Pejaković, W. Fahrenholtz, G. Hilmas, F. Panerai, and O. Chazot, “Tem-

perature Jump Phenomenon during Plasmatron Testing of ZrB2−SiC Ultra-High-Temperature

Ceramics,” Journal of Thermophysics and Heat Transfer (On Press), 2012.

[64] H. Hald, “Operational Limits for Reusable STS due to Physical Boundaries of C/SiC Materias,”

in Structure and Technologies Challenges for future Launchers, 3rd European Conference on

Launcher Technology, December 2001.

[65] R. N. Gupta, J. M. Yos, R. A. Thompson, and K.-P. Lee, “A Review of Reaction Rates and

Thermodynamic and Transport Properties for an 11-Species Air Model for Chemical and Thermal

Nonequilibrium Calculations to 30 000 K,” Reference Publication 1232, NASA Scientific and

Technical Information Division, Washington, DC, USA, 1990.

[66] C. Park, “On Convergence of Computation of Chemically Reacting Flows,” in 23rd AIAA

Aerospace Sciences Meeting, AIAA 1985-0247, (Reno, NV, USA), 1985.

[67] G. Tumino, “IXV: the Intermadiate eXperimental Vehicle,” ESA Bulletin 128, November 2006.

Page 107: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

Appendix A

Figure A.1: Temperature Field - Section 4.1.1 - Condition I

85

Page 108: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

86 Temperature Fields

Figure A.2: Temperature Field - Section 4.1.1 - Condition II

Figure A.3: Temperature Field - Section 4.1.2 - Condition I

Page 109: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

Numerical Simulations 87

Figure A.4: Temperature Field - Section 4.1.2 - Condition II

Figure A.5: Temperature Field - Section 4.1.3 - Condition I

Page 110: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

88 Temperature Fields

Figure A.6: Temperature Field - Section 4.1.3 - Condition II

Page 111: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

Appendix B

Figure B.1: Temperature vs. Time - Section 4.1.1 - Condition I

89

Page 112: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

Figure B.2: Temperature vs. Time - Section 4.1.1 - Condition II

Figure B.3: Temperature vs. Time - Section 4.1.2 - Condition I

90

Page 113: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

Figure B.4: Temperature vs. Time - Section 4.1.2 - Condition II

Figure B.5: Temperature vs. Time - Section 4.1.3 - Condition I

91

Page 114: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

Figure B.6: Temperature vs. Time - Section 4.1.3 - Condition II

92

Page 115: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

App

endi

xC

93

Page 116: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

Test

NDP1

NDP2

NDP3

NDP4

NDP5

Te

pe

µe

[O2]

[N2]

[NO]

[NO+]

[O]

[N]

[e–]

hw

Vs

γref

KPa

kgs−

1m−1

×1010

Jkg−1

ms−

1

16

0.3826

0.3229

0.6043

0.3364

0.4363

5556

2000

0.000173

1.34E-05

4.46E-01

1.48E-03

3.69E-04

2.32E-01

3.20E-01

67

4.37E+06

587

0.1

15

0.3828

0.3259

0.6091

0.3400

0.4368

5534

2000

0.000173

1.41E-05

4.57E-01

1.53E-03

3.57E-04

2.32E-01

3.09E-01

65

3.88E+06

578

0.1

17

0.3847

0.3431

0.6366

0.3609

0.4398

5631

2000

0.000175

1.12E-05

4.09E-01

1.33E-03

4.09E-04

2.32E-01

3.58E-01

75

4.35E+06

618

0.1

40.3925

0.3927

0.7155

0.4222

0.4500

5739

2000

0.000177

8.77E-06

3.54E-01

1.14E-03

4.71E-04

2.32E-01

4.13E-01

86

4.12E+06

661

0.1

10.3931

0.3962

0.7211

0.4266

0.4507

5802

2000

0.000178

7.64E-06

3.21E-01

1.03E-03

5.09E-04

2.32E-01

4.45E-01

93

4.86E+06

689

0.1

70.3928

0.3945

0.7183

0.4244

0.4503

5824

2000

0.000178

7.29E-06

3.11E-01

9.97E-04

5.22E-04

2.32E-01

4.56E-01

95

3.89E+06

696

0.1

50.3698

0.3138

0.6027

0.3213

0.4389

5826

5000

0.000180

1.96E-05

4.37E-01

1.94E-03

4.44E-04

2.32E-01

3.29E-01

81

4.67E+06

264

0.1

20.3704

0.3279

0.6259

0.3375

0.4409

5857

5000

0.000180

1.83E-05

4.22E-01

1.86E-03

4.62E-04

2.32E-01

3.44E-01

84

4.63E+06

270

0.1

80.3712

0.3380

0.6425

0.3493

0.4425

5920

5000

0.000182

1.61E-05

3.93E-01

1.71E-03

4.99E-04

2.32E-01

3.73E-01

91

4.63E+06

281

0.1

90.3730

0.3569

0.6733

0.3716

0.4458

6004

5000

0.000183

1.35E-05

3.53E-01

1.53E-03

5.52E-04

2.32E-01

4.13E-01

101

5.03E+06

296

0.1

10

0.3793

0.4056

0.7520

0.4301

0.4550

6011

5000

0.000183

1.33E-05

3.50E-01

1.51E-03

5.56E-04

2.32E-01

4.16E-01

102

3.76E+06

298

0.1

11

0.3865

0.4523

0.8272

0.4868

0.4643

6077

5000

0.000184

1.17E-05

3.20E-01

1.38E-03

5.99E-04

2.32E-01

4.47E-01

110

4.12E+06

309

0.1

13

0.4014

0.5385

0.9652

0.5924

0.4823

6130

5000

0.000185

1.05E-05

2.95E-01

1.28E-03

6.33E-04

2.32E-01

4.71E-01

116

4.34E+06

322

0.1

30.3679

0.3508

0.6700

0.3635

0.4455

5963

6000

0.000183

1.79E-05

3.98E-01

1.84E-03

5.09E-04

2.32E-01

3.68E-01

93

3.72E+06

237

0.1

60.3675

0.3461

0.6624

0.3580

0.4447

5985

6000

0.000183

1.71E-05

3.88E-01

1.79E-03

5.22E-04

2.32E-01

3.78E-01

96

5.52E+06

240

0.1

18

0.3681

0.3524

0.6726

0.3653

0.4457

6024

6000

0.000184

1.58E-05

3.70E-01

1.70E-03

5.47E-04

2.32E-01

3.96E-01

100

5.51E+06

246

0.1

19

0.3732

0.3977

0.7464

0.4192

0.4539

6109

6000

0.000185

1.33E-05

3.31E-01

1.51E-03

6.01E-04

2.32E-01

4.35E-01

110

4.70E+06

259

0.1

Tab

leC.1:NDPsan

dRebuiltQua

ntities-Oxida

tion

Cam

paign(H

ER)

94

Page 117: Development of Testing Conditions for Gas/Surface ... · Development of Testing Conditions for Gas/Surface Interaction Studies in Atmospheric Reentry Simulations José Pedro Soares

Test

NDP1

NDP2

NDP3

NDP4

NDP5

Te

pe

µe

[O2]

[N2]

[NO]

[NO+]

[O]

[N]

[e–]

hw

Vs

γref

KPa

kgs−

1m−1

×1010

Jkg−1

ms−

1

20

0.3825

0.3202

0.5998

0.3331

0.4358

5499

2000

0.000172

1.53E-05

4.74E-01

1.60E-03

3.40E-04

2.32E-01

2.93E-01

62

3.17E+06

564

0.1

22

0.3843

0.3398

0.6314

0.3569

0.4392

5655

2000

0.000175

1.06E-05

3.97E-01

1.29E-03

4.23E-04

2.32E-01

3.69E-01

77

4.53E+06

625

0.1

21

0.3880

0.3659

0.6730

0.3890

0.4444

5722

2000

0.000177

9.11E-06

3.62E-01

1.16E-03

4.61E-04

2.32E-01

4.04E-01

84

4.62E+06

655

0.1

30

0.3991

0.4287

0.7726

0.4670

0.4577

5755

2000

0.000177

8.46E-06

3.45E-01

1.11E-03

4.81E-04

2.32E-01

4.21E-01

88

4.23E+06

670

0.1

23

0.3699

0.3050

0.5881

0.3114

0.4378

5838

5000

0.000180

1.91E-05

4.31E-01

1.91E-03

4.51E-04

2.32E-01

3.35E-01

83

4.96E+06

267

0.1

24

0.3712

0.3380

0.6425

0.3493

0.4425

5998

5000

0.000183

1.37E-05

3.56E-01

1.54E-03

5.48E-04

2.32E-01

4.10E-01

100

5.25E+06

295

0.1

25

0.3850

0.4428

0.8119

0.4753

0.4624

6140

5000

0.000185

1.03E-05

2.91E-01

1.26E-03

6.40E-04

2.32E-01

4.75E-01

117

4.60E+06

321

0.1

31

0.3704

0.3279

0.6259

0.3375

0.4409

6003

5000

0.000183

1.35E-05

3.54E-01

1.53E-03

5.51E-04

2.32E-01

4.12E-01

101

4.29E+06

296

0.1

26

0.3727

0.3937

0.7399

0.4143

0.4532

6030

6000

0.000184

1.56E-05

3.67E-01

1.69E-03

5.50E-04

2.32E-01

3.99E-01

101

4.32E+06

246

0.1

28

0.3848

0.4771

0.8745

0.5148

0.4694

6097

6000

0.000185

1.37E-05

3.36E-01

1.54E-03

5.94E-04

2.32E-01

4.30E-01

109

4.30E+06

259

0.1

32

0.3713

0.3820

0.7209

0.4004

0.4510

6025

6000

0.000184

1.58E-05

3.69E-01

1.70E-03

5.48E-04

2.32E-01

3.97E-01

100

3.20E+06

246

0.1

Tab

leC.2:NDPsan

dRebuiltQua

ntities-Oxida

tion

Cam

paign(M

TA)

Test

NDP1

NDP2

NDP3

NDP4

NDP5

Te

pe

µe

[O2]

[N2]

[NO]

[NO+]

[O]

[N]

[e–]

hw

Vs

γref

KPa

kgs−

1m−1

×1010

Jkg−1

ms−

1

T1-C

S0.4177

0.3930

0.7115

0.4309

0.4541

4223

1440

0.000139

4.12E-04

7.49E-01

5.83E-03

2.60E-05

2.29E-01

1.54E-02

52.08E+06

418

0.10

T1-R

S0.4177

0.3930

0.7115

0.4309

0.4541

4223

1440

0.000139

4.12E-04

7.49E-01

5.83E-03

2.60E-05

2.29E-01

1.54E-02

51.17E+06

418

0.10

S6[7]

0.4385

0.4521

0.8026

0.5083

0.4766

4440

1300

0.000145

1.80E-04

7.33E-01

4.32E-03

4.68E-05

2.30E-01

3.18E-02

93.59E+06

429

0.10

T2-C

S0.4125

0.3763

0.6850

0.4095

0.4496

4354

5000

0.000142

9.04E-04

7.50E-01

9.33E-03

2.67E-05

2.27E-01

1.25E-02

52.32E+06

131

0.10

T2-R

S0.4125

0.3763

0.6850

0.4095

0.4496

4354

5000

0.000142

9.04E-04

7.50E-01

9.33E-03

2.67E-05

2.27E-01

1.25E-02

51.34E+06

131

0.10

S10[7]

0.4123

0.3510

0.6491

0.3872

0.4641

4485

5000

0.000146

5.96E-04

7.45E-01

8.11E-03

3.72E-05

2.28E-01

1.85E-02

73.15E+06

125

0.10

T3-C

S0.3968

0.2829

0.5692

0.3228

0.4613

4085

10000

0.000135

4.37E-03

7.55E-01

1.75E-02

1.06E-05

2.19E-01

3.65E-03

21.76E+06

58

0.01

T3-R

S0.3968

0.2829

0.5692

0.3228

0.4613

4085

10000

0.000135

4.37E-03

7.55E-01

1.75E-02

1.06E-05

2.19E-01

3.64E-03

21.10E+06

58

0.01

C2a[7]

0.4001

0.2884

0.5770

0.3311

0.4636

4306

10000

0.000141

2.07E-03

7.53E-01

1.37E-02

1.97E-05

2.24E-01

7.61E-03

48.18E+05

57

0.01

Tab

leC.3:NDPsan

dRebuiltQua

ntities-Tem

perature

Cam

paign

95