Walter E. C. Pritzkow Spezialkeramik

Keramik für technische Anwendungen

Adam-Opel-Straße 6

D-70794 Filderstadt

Tel.: +49 7158 9157090

Fax: +49 7158 9157099

pritzkow-wps@keramikblech.com

www.keramikblech.com

Walter Pritzkow *

Kurosch Rezwan **

Kamen Tushtev **

* Walter E.C. Pritzkow Spezialkeramik

** Advanced Ceramics, University of Bremen

All-oxide ceramic matrix composites (OCMC)

based on low cost 3M™ Nextel™ 610 fabrics

HT-CMC 10, 22.-26.09.2019, Bordeaux, France

Introduction

• Overview on production and characteristics of OCMC‘s based on

3M™ Nextel™ fabric Type DF11

• What happens with fiber and fabric during the production process

• Experimental 3M™ Nextel™ 610 fabrics

• OCMC‘s based on experimental 3M™ Nextel™ 610 fabrics and a

matrix Al2O3/ZrO2 (FW12), production and characterisation

• Complex parts made of OCMC

• Cost reduction using the new fabrics

• Summary

2

3

Overview of companies working since more than 10 years on

OCMC‘s based on 3M™ Nextel™ 610 fabric Type DF11

Company COI Ceramics

(COIC)

Composites

Horizons Inc.

(CHI)

Walter E.C. Pritzkow

Spezialkeramik

(WPS)

Process technology Autocalve Autoclave Open laminated

press technology

Matrix Al2O3/SiO2 Al2O3/SiO2 Al2O3/ZrO2 (FW12)

Sintering temperature Unknown Unknown 1200 ºC

Literature:

• 3M™ Nextel™ Spread tow: enabling automated processing methods and unique composite construction

Aaron Beaber et al., USACA Jan 23, 2018

• Oxide-Oxide Ceramic Matrix Composites – Enabling Widespread Industry Adoption

Barrett Jackson et al, HTCMC 9, 2016

• Designing with oxide-oxide CMCs: Understanding the price-performance relationship in new fabric designs

Aaron Beaber et al., USACA Jan 24, 2017

Processing of OCMC‘s at WPS

4

Standard layup with

3M™ Nextel™ 610 fabric DF11

Characteristics of OCMC (1)

5

0

100

200

300

400

WPS pressed COIC CHI

tensile

str

ength

[M

Pa]

Tensile strength

0

20

40

60

80

100

120

WPS pressed COIC CHI

tensile

modulu

s [

GP

a]

Tensile modulus

0

100

200

300

400

WPS open WPSpressed

COIC CHI

bendin

g s

trength

[M

Pa]

Bending strength

0

20

40

60

80

100

120

WPS open WPSpressed

COIC CHIbendin

gm

odulu

s[G

Pa]

Bending modulus

6

Characteristics of OCMC (2)

0

5

10

15

20

25

WPS pressed COIC CHI

ILS

S [M

Pa

]

ILSS (SBB)

7

Tensile strength and bending strength

dependent upon the fiber volume content

0

100

200

300

400

38 40 42 44 46

tensile

str

ength

(MP

a)

fiber volume content calc. (vol%)

OCMC based on DF11

WPSopen

WPSpressed

COIC

CHI

0

100

200

300

400

38 40 42 44 46

bendin

g s

trength

(M

Pa)

fiber volume content calc. (vol%)

OCMC based on DF11

WPSopen

WPSpressed

COIC

CHI

8

What happens when a fabric layup filled with powder

is pressed to high fiber volume content?

As received Pressed to 1,5 mm Pressed to 1,25 mm

0

100

200

300

30 35 40 45 50

tensile

str

ess [N

/cm

]

fiber volume content [%]

Nextel 610 fabric type DF11 warp/fill with powder, tensile stress at 1% hits

as received

pressed to 1,5 mm

pressed to 1,25 mm

Warp-fill Warp-fill

filled

with powder

9

0,00

50,00

100,00

150,00

200,00

250,00

300,00

350,00

400,00

0,00

10,00

20,00

30,00

40,00

50,00

60,00

70,00

Lot 95GTW FW12with Lot 95GTW Lot JHDV9 FW12 with Lot JHDV9

bendin

g s

trength

[M

Pa]

tensile

str

ength

[kg/c

m]

Tensile strength fabric (DITF) [kg/cm] Bending strength FW12 [MPa]

Tensile strength of fabric 3M™ Nextel™ 610 type DF11

compared with bending strength of the composite FW12

10

Experimental 3M™ Nextel™ 610 fabrics

Fabric type DF11-

3000 5HS

DF13-

4500 5HS

DF13-

4500 4HS

DF13-

4500 Twill

DF19-

4500 8HS

10.000

Semi Uni

20.000

Semi Uni

Yarn type

Nextel 610

3000

Denier

4500

Denier

4500

Denier

4500

Denier

4500

Denier

10000/1500

Denier

20000/1500

Denier

Weaving 5HS 5HS 4HS Twill 8HS UD UD

Areal weight

[g/m²]

390 500 496 501 682 393 590

Thickness

heat cleaned

[mm]

0,28 0,33 0,33 0,33 0,43 0,26 0,48

11

Composites with matrix Al2O3/ZrO2 and

experimental 3M™ Nextel™ 610 fabrics

Fabric type DF11-

3000 5HS

DF13-

4500 5HS

DF13-

4500 4HS

DF13-

4500 Twill

DF19-

4500 8HS

10.000

Semi Uni

20.000

Semi Uni

Number of

plies

10 10 8 8 6 12 8

Fiber volume

content [%]

38,5 41,4 39,6 40,0 39,9 39,0 37,5

Matrix volume

[%]

33,1 30,6 29,8 27,8 32,1 30,8 30,7

Porosity

volume [%]

28,2 28,0 30,6 32,2 28,0 30,2 31,8

Density [g/cm³] 2,74 2,75 2,69 2,75 2,83 2,79 2,78

Laminate

thickness [mm]

2,63 3,1 2,57 2,6 2,57 3,3 3,17

Thickness per

ply [mm]

0,263 0,31 0,32 0,325 0,428 0,275 0,396

12

SEM-micrographs of composites with

experimental 3M™ Nextel™ 610 fabrics (1)

FW12-DF11-3000 5HS FW12-DF13-4500 4HS FW12-DF13-4500 5HS

13

SEM-micrographs of composites with

experimental 3M™ Nextel™ 610 fabrics (2)

FW12-DF13-3000 Twill FW12-DF19-4500 8HS

14

FW12-10.000 Semi Uni FW12-20.000 Semi Uni

SEM-micrographs of composites with

experimental 3M™ Nextel™ 610 fabrics (3)

15

Tensile tests on

composites with matrix Al2O3/ZrO2 and

experimental 3M™ Nextel™ 610 fabrics

0

50

100

150

tensile

mo

du

lus [

GP

a]

0

100

200

300

400

tensile

str

eng

th [M

Pa

]

16

4-Point-bending tests on

composites with matrix Al2O3/ZrO2 and

experimental 3M™ Nextel™ 610 fabrics

0

100

200

300

400

500

600

ben

din

g s

tre

ng

th [M

Pa

]

0

50

100

150

bendin

g m

odulu

s [G

Pa]

17

4-Point-bending on edge tests on

composites with matrix Al2O3/ZrO2 and

experimental 3M™ Nextel™ 610 fabrics

0

100

200

300

400

500

600

ben

din

g s

tre

ng

th [M

Pa

]

0

50

100

150

ben

din

g m

odu

lus [G

Pa

]

18

Stress intensity factor and notch sensitivity on

composites with matrix Al2O3/ZrO2 and

experimental 3M™ Nextel™ 610 fabrics

0

5

10

15

20

25

30

str

ess in

ten

sity f

acto

r [M

Pa

* m

^0,5

] Single-Edge Notch Beam SENB [MPa]

0

0,2

0,4

0,6

0,8

1

1,2

notc

hsensitiv

ity

facto

r[-

]

notched strength / unnotched strength

19

Short beam bending / interlaminar shear tests on

composites with matrix Al2O3/ZrO2 and

experimental 3M™ Nextel™ 610 fabrics

0

5

10

15

20

25

ILS

S [M

Pa

]

20

Complex structures made of oxide-oxide CMC

Static mixer

Development and production done

by COIC and CHI

Picture source:

aviation international news

Thrusters for a

Fluidic Propulsion System™

for unmanned aerial

vehicles from the company

Jetoptera Inc.

Picture source:

Jetoptera Inc. (left), WPS (right)

21

Cost reduction possibilities using experimental

3M™ Nextel ™ 610 fabrics

11 o

z/yd

2

11 o

z/yd

2

15 o

z/yd

2

19 o

z/yd

2

20 o

z/y

d2

12 o

z/yd

2

0%

20%

40%

60%

80%

100%

120%

% P

rice o

fD

F11-1

500

Est. Baseline Cost [%] (wt. basis)

Data bases: 3M

12

Plie

s

11

Plie

s 9 P

lies

6 P

lies

7 P

lies

10

Plie

s

0%

20%

40%

60%

80%

100%

120%

% p

rice o

f D

F11

-1500

Est. Baseline Cost [%] (Ply Count of 2,8mm panel)

22

Summary

• Tensile strength and bending strength are independent of the fiber

volume content when producing OCMC within the range of 38-46%

• Pressing to higher fiber volume content with powder based slurries

will damage the fibers

• Fabrics based on higher denier rovings can be well infiltrated with

the Al2O3/ZrO2 (FW12) slurry

• With some of the experimental 3M™ Nextel™ 610 fabrics better

characteristics in comparison to DF11 based OCMC‘s can be

realized

• Estimated cost reduction using the experimental fabrics is more than

20%

23

Acknowledgement

3M:

• Peter Dietrich, Germany

• Larry Visser, USA (retired)

• Andrew d‘Souza, USA

• Stan Fast, USA

Advanced Ceramics, University of Bremen

• Renato Almeida

• Luisa Bastos Mateus

• Kürsat Cihan

• Vincent Conrads

• Liesa Kelling

• Igor Myskin

Walter E.C. Pritzkow Spezialkeramik

• Robert da Silva

• Adriana Conrad

• Frank Wehner

24

Thanks for your attention

OCMC-Thrusters for

the „Fluidic Propulsion System™

from Jetoptera Inc.