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REPORT NO.NASA-CR- 54354

WESTINGHOUSEWAED 65.17EMARCH 1965

DEVELOPMENT AND EVALUATION OF MAGNETIC ANDELECTRICAL MATERIALS CAPABLE OF OPERATINGIN THE 800° TO 1600°F TEMPERATURE RANGE

Fi rs t Q u a r t e r l y Repor t

byP. E. Kueser et al

prepared for

NATIONAL AERONAUTICS AND SPACE ADMINISTRATIONLEWIS RESEARCH CENTER

UNDER CONTRACT NAS3-6465

¥55-34731(ACCESSION UUMBERI

IPAOJSI

•NASA CR OR TMXOR AD DUMBER/

(THRUt

I

(COBLE)

•CATEGORY)

Westinghouse Electric CorporationAEROSPACE ELECTRICAL DIVISION

LIMA. OHIO

https://ntrs.nasa.gov/search.jsp?R=19650024630 2020-07-12T19:16:03+00:00Z

NOTICE

This report was prepared as an account of Government-sponsoredwork. Neither the United States nor the National Aeronautics andSpace Administration (NASA), nor any person acting on behalf ofNASA:

A). Makes any warranty or representation, expressed or implied,with respect to the accuracy, completeness, or usefulness ofthe information contained in this report, or that the use of anyinformation, apparatus, method, or process disclosed in thisreport may not infringe privately-owned rights; or

\

B) Assumes any liabilities with respect to the use of, or fordamages resulting from the use of any information, apparatusmethod or process disclosed in this report.

As used above, "person acting on behalf of NASA" includes anyemployee or contractor of NASA, or employee of such contractor,to the extent that such employee or contractor of NASA or employeeof such contractor prepares, disseminates, or provides access1

to, any information pursuant to his employment or contract withNASA, or his employment with such contractor.

AVAILABILITY NOTICE

Qualified requestors may obtain copies of this report from:

National Aeronautics and Space AdministrationOffice of Scientific and Technical InformationWashington 25, D. C.Attn: AFSS-A

Report No. 65.17E

March 1965

DEVELOPMENT AND EVALUATION OF MAGNETIC ANDELECTRICAL MATERIALS CAPABLE OF OPERATING

IN THE 800° TO 1600°F TEMPERATURE RANGE

FIRST QUARTERLY REPORT(NOVEMBER 12, 1964 - FEBRUARY 28, 1965)

NAS3-6465

sponsored by

NATIONAL AERONAUTICS AND SPACE ADMINISTRATIONCONTRACT NAS3-6465

Project ManagementNASA - Lewis Research CenterSpace Power Systems Division

R. A. Lindberg

Prepared by: Approved by:

P. E. Kueser, et al N. W. Bucci, Jr.,Manager, NASA Materials Study Manager, Engineeringand Research Program Systems Research and

Development Department

Westinghouse Electric CorporationAerospace Electrical Division

Lima, Ohio

PREFACE

The work reported here was sponsored by the Space Power Systems Divisionof the NASA Lewis Research Center under contract NAS3-6465. Mr. R. A.Lindberg of NASA has provided the Project Management for the program.His review and suggestions as well as those of Mr. T. A. Moss, also ofNASA, are gratefully acknowledged. The Westinghouse Aerospace ElectricalDivision (WAED) is responsible for the Technical Direction of the program.The Westinghouse Research and Development Center (WR&D) is conductingTasks 2, 3 and 4 of Program 1 on Optimized Magnetic Materials for Appli-cation in the 1000 to 1200°F Range, the Investigation for Raising the Alphato Gamma Transformation, and Creep Testing of Rotor Materials. Eitel-McCullough (EIMAC) is responsible for the Bore Seal Development, Task1 of Program III. All other tasks are being conducted at the WestinghouseAerospace Electrical Division (WAED).

In a program of this magnitude a large group of engineers and scientists areinvolved in its progress. An attempt to recognize those who are contributingdirectly, together with their area of endeavor, follows:

Program I - Magnetic Materials for High Temperature Operation

Task 1 - Optimized Precipitation Hardened Magnetic Materials for Appli-cation in the 1000 to 1200°F Range.

Dr. K. Detert (WR&D); J. W. Toth (WAED)

Task 2 - Investigation for Raising the Alpha to Gamma TransformationTemperature in Cobalt-Iron Alloys.

Dr. K. Detert (WR&D); J. W. Toth (WAED)

Task 3 - Dispersion-strengthened Magnetic Materials for Applicationin the 1200-1600°F Range.

Dr. R. J. Towner (WAED)

Task 4 - Creep Testing.

M. Spewpck (WR&D); D. H. Lane (WAED)

11

Program II - High Temperature Capacitor Feasibility

R. E. Stapleton (WAED)

Program III - Bore Seal Development and Combined Material InvestigationUnder a Space Simulated Environment

Task 1 - Bore Seal Development

R. C. McRae, Dr. L. Reed (EIMAC); J. W. Toth (WAED)

Tasks 2, 3,4 - Stator and Bore Seal, Transformer and Solenoid

W. L. Grant, H. .E. Keneipp, D. H. Lane, R. P. Shumate,J. W. Toth (WAED)

Dr. A. C. Beiler (WAED) and Dr. G. W. Weiner (WR&D) are acting asconsultants on Program I.

111

ABSTRACT

This is the first quarterly report on Contract NAS3-6465 for the Develop-ment and Evaluation of Magnetic and Electrical Materials Capable of Op-erating in the Temperature Range from 800 °F to 1600°F. Advanced spaceelectric power systems are the area of eventual application.

Program I is directed at developing high-temperature magnetic materialwith satisfactory strength for rotor use. The ternary alloy systems of co-balt-nickel-iron are under study with the cobalt and iron corners of thephase diagram. Thirty to forty per cent cobalt gives the greatest satura-tion at 600°C. The additions of beryllium to a composition of 15% nickel-25% cobalt-balance iron improves the stability of the alpha phase. Eighteenpre-alloyed atomized powders and 12 composite powders have been ex-amined for use as dispersion-strengthened magnetic materials.

Program 11 will determine the feasibility of a high-temperature capacitorusing high quality dielectric materials. Pyrolytic boron-nitride has beenprepared in thicknesses of 0.0015 ± 0.0005 inches; Lucalox alumina rodsto 0.006 inches thick.

Program III incorporates combinations of materials into a stator with boreseal, a transformer, and a solenoid for investigations of compatibility underelectrical stress and space-simulated conditions of elevated temperature. Asystem for loading and sealing alkali-metals in vacuum is in the progress ofassembly. The stator, transformer and solenoid designs for use in space-simulated testing have been completed.

IV

TABLE OF CONTENTS

Section Page

PREFACE iiABSTRACT iv

I INTRODUCTION 1

II PROGRAM I - MAGNETIC MATERIALS FOR HIGH-TEMPERATURE OPERATION 3

A. Task 1 - Optimized Precipitation-HardenedMaterials For High-Temperature Application .. 41. Summary of Technical Progress 42. Discussion 4

a. Experimental Procedure 8b. Results 9

3. Program for the Next Quarter 16

B. Task 2 - Investigation For Raising the Alphato Gamma Transformation Temperature inCobalt-Iron Alloys 171. Summary of Technical Progress 172. Discussion 17

a. Background 17b. Experimental Procedure 19c. Results 19

3. Program for the Next Quarter 19

C. Task 3 - Dispersion-Strengthened MagneticMaterials For Application in the 1200-1600 °FRange 201. Summary of Technical Progress 202. Discussion 20

a. Prealloyed Atomized Powders 20b. Composite Powders 22c. Extrusions of Dispersion-Strength-

ened Cobalt and Cobalt-Iron Alloys . 243. Program for the Next Quarter 25

TABLE OF CONTENTS (Cont.)

Section Page

D. Task 4 - Creep Testing 261. Summary of Technical Progress 262. Discussion 263. Program for the Next Quarter 28

III PROGRAM II - HIGH TEMPERATURE CAPACITORFEASIBILITY 29

A. Summary of Technical Progress 29B. Discussion 31

1. Dielectric Materials Selection 312. Single Wafer Fabrication 313. Wafer Slicing 35

a. Mounting For Slicing Operations ... 35b. Slicing 35

4. Lapping Procedures and Results 375. Dielectric Measurements 40

C. Program For Next Quarter 43

IV PROGRAM 111 - BORE SEAL DE VE LOPMENT ANDCOMBINED MATERIAL INVESTIGATIONS UNDER ASPACE-SIMULATED ENVIRONMENT 44

A. Task 1 - Bore Seal Development 451. Summary of Technical Progress 452. Discussion 45

a. Facility Design 45b. Bore Seal Materials and Sealing

Study 45c. Ceramic Materials 51

3. Program for Next Quarter 52

B. Task 2 - Stator and Bore Seal 551. Summary of Technical Progress 552. Discussion 553. Program for Next Quarter 59

VI

TABLE OF CONTENTS (Cont.)

Section Page

C. Task 3 - Transformer 601. Summary of Technical Progress 602. Discussion 603. Program for Next Quarter 62

D. Task 4 - Solenoid 631. Summary of Technical Progress 632. Discussion 633. Program for Next Quarter 63

APPENDIX A A-l

APPENDDC B B-l

APPENDIX C C-l

vn

LIST OF FIGURES

Figure Title Page

II-l Influence of Cobalt Content on Saturation in a TernaryAlloy With 12 Percent Nickel in Iron 13

11-2 Hardness and Coercive Force of Alloy l-A-2 (58Fe-15Ni-25Co-2Nb) at Room Temperature After AgingOne Hour at Temperature 15

11-3 Encapsulated Vacuum Creep Specimen 27

I II-l Preparation and Evaluation of Single LayerCapacitors 32

111-2 Lucalox Rod Stock With 10 Mil Sliced Wafer Held inLOC-Wax 20 36

III-3 Dielectric Materials 38

I V-l Schematic of the Capsule Fabrication and LoadingEquipment 46

IV-2 Schematic of Dual Vacuum Furnace ModificationsUsing Ion Pumping 47

IV-3 Cutaway View of Vacuum Furnace Showing theStator Test Specimen Installed 57

IV-4 Details of Thermocouple Feedthrough Flange on theVacuum Furnace Chamber 58

IV-5 Cutaway View of Transformer ,. 61IV-6 Cutaway View of Solenoid 64

viii

LIST OF TABLES

Number Title Page

II-l Group A - Precipitation-Hardening Alloys 611-2 Group B - Precipitation-Hardening Alloys 711-3 Transformation Temperature in Degrees Fahrenheit

and Centigrade of Fe-15Ni-25Co Alloys WithModifiers 10

11-4 Transformation Temperature in Degrees Fahrenheitand Centigrade of Iron - 12 Nickel Alloys WithVarying Cobalt Content 11

11-5 Saturation Magnetic Moment (emu/g) at RoomTemperature Annealed at 1832°F (1000 °C) for30 Minutes, No Aging 12

11-6 Maximum Hardness Obtained by Isochronal Aging 1411-7 Alloys Selected for Alpha-Gamma Transformation

Study 18II-8 Atomized Powders 21II-9 Composite Powders 2311-10 Supplier Extrusions 25

I II-l Tabulation of Dielectric Properties andPresent Status 33

111-2 Spectrochemical Analysis of Candidate Dielectrics 34III-3 Lapping and Polishing Operations 39111-4 Possible Causes of Grain Pull Outs in Machined

Lucalox Wafers 41

IV-1 Spectrographic Silica Analyses of SelectedCeramics 53

IX

SECTION I

INTRODUCTION

This is the first quarterly report on Contract NAS3-6465 for the Develop-ment and Evaluation of Magnetic and Electrical Materials Capable of Oper-ating in the Temperature Range from 800°F to 1600T. The period of per-formance is from November 12, 1964 through February 28, 1965. Theprogram consists of three Programs with their related tasks as follows:

Program I -

Task 1 -

Task 2 -

Task 3 -

Task 4 -

Program II -

Program III -

Task 1 -

Task 2 -

Task 3 -

Task 4 -

Magnetic Materials for High-Temperature Operation

Optimized Precipitation Hardened Magnetic Materials forApplication in the 1000 to 1200°F Range

Investigation for Raising the Alpha to Gamma Transforma-tion Temperature in Cobalt-Iron Alloys

Dispersion-Strengthened Magnetic Materials for Applica-tion in the 1200 to 1600°F Range

Creep Testing

High-Temperature Capacitor Feasibility

Bore Seal Development and Combined Material InvestigationsUnder a Space Simulated Environment

Bore Seal Development

Stator and Bore Seal

Transformer

Solenoid

In Program I, limitations in magnetic material performance at elevated temper-ature have been recognized from Contract NAS3-4162 and the development ofmaterials incorporating improved magnetic and mechanical properties is be-ing pursued. In most cases, high-strength compromises the magnetic proper-ties; therefore, a balance between these two variables is sought.

Program II is directed at determining the feasibility of applying high-qualitydielectric materials and their processes to a high-temperature (HOOT)capacitor which is lightweight and suitable for static power conditioning ap-paratus used in space applications.

Program III incorporates combinations of materials previously evaluatedunder Contract NAS3-4162 into a stator with a bore seal, a transformer, anda solenoid; all of which will be evaluated under space-simulated conditions atelevated temperature.

The three Programs will be reported consecutively in Sections II, III and IV.Each of these Sections is further subdivided into a summary of the technicalprogress, a discussion, and the program for the next quarter.

SECTION II

PROGRAM I - MAGNETIC MATERIALS FORHIGH-TEMPERATURE OPERATION

Program I is directed at the improvement and further understanding ofmagnetic materials suitable for application in the rotor of an alternatoror motor in advanced space electric power systems.

Task 1 is concerned with precipitation-hardened magnetic materials in the1000 to 1200°F range. These materials are of the iron-cobalt-nickel ternarysystem. The two specific areas of interest are the iron and cobalt cornersof the ternary system.

Task 2 is a small research investigation for determining the feasibility ofraising the alpha to gamma transformation temperature in the iron-cobaltsystem; thereby increasing the useful magnetic temperature of this system.

Task 3 is directed at applying dispersion-strengthening mechanisms tomagnetic materials to achieve useful and invariant mechanical and magneticproperties in the 1200 to 1600°F range. Because both variables are in-fluenced differently by particle size and spacing, a compromise is soughtthereby tailoring the materials to the need of dynamic electric machines.

Task 4 is a creep program on Nivco alloy (approximately 72% cobalt, 23%nickel and certain other elements) which will generate 5000 hour designdata in a vacuum environment (1 x 10" torr). This material representsa presently available magnetic material with the highest useful applicationtemperature.

TASK 1 - OPTIMIZED PRECIPITATION-HARDENED MATERIALFOR HIGH-TEMPERATURE APPLICATION.

1. Summary of Technical Progress

a.) Twenty ferritic and twenty cobalt base alloys were selectedand approved for evaluation as high-strength magnetic alloys.

b.) All of the ferritic alloys and most of the cobalt-base alloyshave been melted.

c.) Transformation temperatures of ten ferritic alloys weredetermined during fast and slow cooling. Several of these alloyswere subjected to isochronal aging between 842 °F (450 °C) and1202°F (650°C). Hardness and coercivity were tested at roomtemperature.

d.) Magnetic saturation measurements at room temperaturewere made on all of the ferritic alloys.

e.) Three of the cobalt base alloys have been subjected toisochronal aging between 932°F (500"C) and 1382°F (15Q°C).Hardness and coercivity were determined at room temperature.

2. Discussion

A suitable alloy composition must be found which gives good strengthat elevated temperatures combined with good magnetic properties.The target ultimate tensile strength for the alloy at 1100°F is 125,000psi or better. The target stress to produce 0. 40% creep strain in 1000hours atl!00°Fis76,000 psi or greater. The 10,000 hour stress targetat 1100°F is 80to 90% of that at 1000 hours. The target magnetic satura-tion for the developmental alloy is 13,000 gauss or better at 1100 °Fand a coercive force less than 25 oersteds. In order to screen a var-iety of compositions, the Vickers hardness, coercivity, magneticsaturation, and temperature stability of the magnetic phase were se-lected as suitable parameters to evaluate the different alloy compo-sitions.

Two general areas of basic alloy composition are regarded as mosthopeful. First, body- centered ferritic alloys of iron and cobalt usingadditional components for obtaining high strengths by a precipitationhardening mechanism (Group A). Second, cobalt base alloys withalloying additions to obtain precipitation strengthening (Group B).

In the ferritic alloys, the maraging treatment gives high strengthcompared to highly alloyed carbon steels. The maraging treatmentrequires a certain amount of nickel present (15% - 25%) in the al-loy. One goal of the screening program will be to find a suitablecomposition which can make use of a maraging treatment applied toa Fe-Co alloy with sufficient temperature stability of the alpha phase.

In the cobalt base alloys, another strengthening mechanism will betried. This mechanism gives rise to considerable strengths innickel-cobalt alloys by the formation of the face centered, orderedcubic phase (NisAl) designated gamma prime. The formation ofgamma prime, however, requires the presence of a certain amountof nickel in the alloy.

The Group A alloys 1-A-l to l-A-10 (Table II-l) were selected basedon a review of literature and on results available from previous studiesby Westinghouse. The composition, 15 nickel and 25 cobalt, will al-low a martensitic transformation which is a prerequisite for maragingtreatment. Furthermore, it has been established that stability of thealpha phase can be expected up to 1202 °F (650°C) for 500 to 1000 hours.The influence of titanium, molybdenum and tantalum has been recog-nized as suitable for maraging treatment. W, Nb, V, Cr, Al, Be, Sb,Sn, Si and Mn will be evaluated for their potential to exert a strength-ening influence on a maraging treatment. The effect of alloying on thetemperature of transformation will be checked to determine whetherthe martensitic transformation can be applied and whether the marten-sitic phase is sufficiently stable at temperature.

Tests on the Group A alloys 1-A-ll to l-A-20 (Table II-l) will definea suitable composition which is lower in nickel (12%). It is expectedthat saturation will be increased compared to the 15 nickel contain-ing alloys. However, there is some doubt whether a martensitictransformation will occur during cooling.

In the cobalt-base alloys, the series 1-B-l to l-B-12 (Table 11-2)will produce some information as to the region in which high satura-tion is attained and what portion will be sacrificed when nickel isadded to obtain a suitable strength by gamma prime formation. Thealloys l-B-13 to l-B-15 were selected to define the role of nickelin achieving strength by the formation of gamma prime.

TABLE II-l. Group A - Precipitation-Hardening Alloys

Number

1-A-l

l-A-2

l-A-3

l-A-4

l-A-5

l-A-6

l-A-7

l-A-8

l-A-9

l-A-10

1-A-ll

l-A-12

1-A-l 3

l-A-14

l-A-15

l-A-16

l-A-17

l-A-18

l-A-19

l-A-20

Nominal Alloy Composition(Weight Percent)

55

58

58

58

59.

58

58

58

58

58

88

83

78

73

68

63

58

53

48

43

Fe

Fe

Fe

Fe

5 Fe

Fe

Fe

Fe

Fe

Fe

Fe

Fe

Fe

Fe

Fe

Fe

Fe

Fe

Fe

Fe

- 15

- 15

- 15

- 15

- 15

- 15

- 15

- 15

- 15

- 15

- 12

- 12

- 12

- 12

- 12

- 12

- 12

- 12

- 12

- 12

Ni -

Ni -

Ni-

Ni-

Ni-

Ni-

Ni-

Ni-

Ni-

Ni-

Ni

Ni-

Ni-

Ni-

Ni-

Ni-

Ni-

Ni-

Ni -

Ni-

25

25

25

25

25

25

25

25

25

25

Co- 5

Co- 2

Co- 2

Co- 2

Co- 0.

Co- 2

Co- 2

Co- 2

Co- 2

Co- 2

W

Nb

V

Cr

5 Al

Be

Sb

Sn

Si

Mn

5 Co

10

15

20

25

30

35

40

45

Co

Co

Co

Co

Co

Co

Co

Co

6

TABLE 11-2. Group B - Precipitation-Hardening Alloys

Number

1-B-l

l-B-2

l-B-3

l-B-4

l-B-5

l-B-6

l-B-7

l-B-8

l-B-9

l-B-10

1-B-ll

l-B-12

1.-B-13

l-B-14

l-B-15

l-B-16

l-B-17

l-B-18

l-B-19

l-B-20

Nominal Alloy Composition(Weight Percent)

95 Co - 5 Fe

90 Co - 5 Fe - 5 Ni

85 Co - 5 Fe - 10 Ni

80 Co - 5 Fe - 15 Ni

75 Co - 5 Fe - 20 Ni

70 Co - 5 Fe - 25 Ni

65 Co - 5 Fe - 30 Ni

85 Co - 10 Fe - 5 Ni

80 Co - 15 Fe - 5 Ni

75 Co - 20 Fe - 5 Ni

70 Co - 25 Fe - 5 Ni

65 Co - 30 Fe - 5 Ni

86 Co - 5 Fe - 5 Ni - 3 Ti - 1

81 Co - 5 Fe - 10 Ni - 3 Ti -

76 Co - 5 Fe - 15 Ni - 3 Ti -

81 Co - 10 Fe - 5 Ni - 3 Ti -

76 Co - 15 Fe - 5 Ni - 3 Ti -

71 Co - 20 Fe - 5 Ni - 3 Ti -

66 Co - 25 Fe - 5 Ni - 3 Ti -

61 Co - 30 Fe - 5 Ni - 3 Ti -

Al

1 Al

1 Al

1 Al

1 Al

1 Al

1 Al

1 Al

a. EXPERIMENTAL PROCEDURE

All of the alloys were prepared by the levitation melting tech-nique. In general, about 20 grams of the pure constituents,present as tiny chips and in powder form, were compacted ata pressure of 220,000 psi applied for one minute. High puritymaterials were used. Iron and cobalt of electrolytic grade,better than 99. 9 percent pure, and nickel in the powder form,with a purity of 99.98 percent, were used. The levitationmelting was performed in a funnel-shaped coil with five wind-ings. The frequency used was in the range of 550 kc; the inputof energy was in the range of 3 to 5 KW. The melting was donein a chamber which was evacuated to 1 x 10" torr, then back-filled using argon (10 ppm 03 maximum, 5 ppm H2, 40 ppm N2)with a dewpoint of -85°F under reduced pressure on the orderof 75 mm Hg. The material was held for about eight secondsin the molten state and then dropped into a copper mold bycutting the power. The mold was slightly tapered to provide abar shaped ingot with a 9/32 inch diameter on one end and 5/16inch diameter on the upper end. The length was 1-7/8 inches.Dilatometer test specimens were machined from the ingot. Thespecimens were one inch long, 1/4 inch in diameter and con-tained a hole for inserting a thermocouple. The samples forsaturation measurements were small cylinders with a 1/10 inchdiameter and 1/10 inch in length. The dilatometer tests weremade under argon by heating up to 1832°F (1000°C), then coolingwhile recording the change in length at temperature. The heat-ing rate applied was of the order of 90°F/min (50°C/min) and 1. 8to 3. 6°F/min (1 to 2°C/min. ).The cooling rate was 90°F/min(50°C/min) and 9°F/min (5°C/min). After the samples had beentested in the dilatometer, the samples were cold rolled to flatstrips of 95 mil thickness. The samples were homogenized andaustenitized in an argon flushed tube furnace at 1832°F (1000 °C)for 30 minutes. Then the samples underwent isochronal annealas follows. The samples were held for one hour at temperaturewith intermittent increases of 90 °F (50 <€) between 842°F (450 °C)and 1382°F (750 C). Aging at these temperatures was done in asalt bath. * Hardness and coercivity were measured on these

*Thermosalt No. 311 was used for aging treatments in the range of 842^(450^0)to 1022°F (550°C).Thermosalt No. 914 was used for aging treatments in the range of 11120F(600°C)to 1292°F (700°C).Thermosalt No. 1018 was used for aging treatments at 1382 °F (750°C).All designations are those of the Carmac Chemical Co.

8

samples. The Vickers hardness was measured at room temper-ature with a load of 50 kilograms. Coercivity was measured ina Forster probe. The magnetizing field was 1300 oersteds.

Saturation was measured in a magnetic field with a gradient of980 oersteds per centimeter. The mean value of the appliedfield was on the order of 10,000 oersteds. For measuring thesaturation at high temperature, a small electric resistance fur-nace was placed into the gap of the magnet which was doublewound to avoid any additional field by the electric current passingthrough the windings. This technique reduced the residual fieldbelow 100 millioersteds.

b. RESULTS

Testing of the alloys 1-A-l to l-A-20 was undertaken. The alloys1-A-l, l-A-5, l-A-6, l-A-7, l-A-8, l-A-9 broke during coldrolling. Further investigations will be made to determine modifi-cations needed to permit rolling. Dilatometer measurementswere made on alloys 1-A-l to l-A-20. The results of the dila-tometer tests are listed in Tables 11-3 and 11-4. The room tem-perature saturation measurements of the samples 1-A-l to l-A-10are listed in Table 11-5. Saturation curves at room temperatureand at 1112°F (600°C) for samples 1-A-ll to l-A-20 are shown inFigure II-l. The approximate saturation in gauss may be ob-tained by multiplying the cgs magnetic moment by one hundred.In Table 11-6, the maximum hardness which could be obtained bythe isochronal anneal is listed for several alloys at the particularaging temperature. Coercivity is also listed. Isochronal anneal-ing has shown that only the l-A-2 alloy showed considerablestrengths after maraging treatment. Figure 11-2 shows coercivityand hardness as a function of aging temperature for this alloy.

Testing of all the additions to the alloy composition of 15 nickel,25 cobalt balance iron (Alloys 1-A-l to l-A-10) had shown thatberyllium was the only element which would increase the stabil-ity of the alpha phase considerably. The addition of 5% tungsten(1-A-l), 2% chromium (l-A-4), 2% manganese (l-A-10), 2% tin(l-A-8) and 2% vanadium (l-A-3) decreased the temperaturestability sufficiently that one cannot expect adequate stabilityat 1112 °F (600°C). All the additions except beryllium decreasedthe transformation temperature into alpha phase during the cool-ing (See Table 11-4). The influence of silicon was very pro-nounced.

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TABLE 11-5. Saturation Magnetic Moment (emu/g) at Room TemperatureAnnealed at 1832°F (1000°C) for 30 Minutes, No Aging

AlloyDesignation

1-A-l

l-A-2

l-A-3

l-A-4

l-A-5

l-A-6

l-A-7

l-A-8

l-A-9

l-A-10

Nominal Alloy Composition(Weight Percent)

55 Fe - 15 Ni - 25 Co - 5 W

58 Fe - 15 Ni - 25 Co - 2 Mb

58 Fe - 15 Ni - 25 Co - 2V

58 Fe - 15 Ni - 25 Co - 2 Cr

Saturation(emu/g)

197.6

208.4

206.4

204.8

59. 5 Fe - 15 Ni - 25 Co - 0. 5 Al 212. 0

58 Fe - 15 Ni - 25 Co - 2 Be

58 Fe - 15 Ni - 25 Co - 2 Sb

58 Fe - 15 Ni - 25 Co - 2 Sn

58 Fe - 15 Ni - 25 Co - 2 Si

58 Fe - 15 Ni - 25 Co - 2 Mn

60 Fe - 15 Ni - 25 Co

194.8

210.8

210.8

202.0

214.0

215.2

Change inSaturation vs.60Fe-15Ni-25

Co (emu/g)

-17.6

-6.8

-8.8

-10.4

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15

The saturation measurements showed that all additions de-creased the saturation at room temperature compared to aternary alloy of 15 nickel and 25 cobalt, balance iron (Table11-5).

From the alloys tested for response to maraging treatment(Table 11-6), it is seen that the effect of niobium addition (Al-loy l-A-2) is similar to the addition of titanium in maragingsteels if atomic percent additions are compared. Vanadiumand chromium apparently have no effect on strengthening. Theother series A alloying additions have not been tested.

Testing the series of alloys containing 12 nickel (Alloys 1-A-llto l-A-20) showed the influence of cobalt on saturation (FigureII-l). Thirty to forty percent cobalt give the highest satura-tion at 1112 °F (600 °C). Alloys with twenty to thirty percent co-balt show slightly reduced values of saturation. The dilatometertest showed that, with the exception of the binary alloy (88 Fe -12 Ni) and the alloy with 45 Co, all alloys appear to have suf-ficient stability of the alpha phase (Table 11-4).

The testing of the cobalt base alloys is in its initial stage. Onecould generally see that the strengths will not reach comparablelevels to the alloys where maraging can be applied. (Compari-son of hardness of alloys are shown in Table 11-6.) By the samereason, the obtained values of the coercivity are considerablylower. The three alloys (l-B-13 through l-B-15) tested showthat increase in the nickel content will lead to increased strength-ening if the same amount of aluminum and titanium are added.

3. Program for the Next Quarter

The tests of the alloys already melted will be completed. The phasesformed in the precipitation hardening process must be identified andtheir stability must be ascertained during isochronal aging at a suitabletemperature. After completing the results, and pending approval, anew series of alloys will be started. The tests of the new alloys shallfulfill two different goals. One will be to determine the suitablecomposition range of the primary components and the second is to findthe best combination of suitable alloying elements to obtain the de-sired magnetic and mechanical properties.

16

B. TASK 2 - INVESTIGATION FOR RAISING THE ALPHA TO GAMMATRANSFORMATION TEMPERATURE IN COBALT-IRON ALLOYS.

1. Summary of Technical Progress

a.) Eighteen cobalt-iron alloys were selected for evaluation(Table 11-7).

b.) Eight alloys have been melted in the form of ingots bythe levitation melting technique.

2. Discussion

a. BACKGROUND

Evaluating the results of previous research work, includingthat performed at the Westinghouse Research Laboratories,and a survey of the binary cobalt-iron phase diagram led to theselection of the basic alloy compositions shown in Table 11-7.

The highest transformation temperature of 1805 °F (985 °C) willbe obtained with an alloy containing 45 Co. The highest valueof saturation (Bs) at temperatures above 1292 °F (700°C) aremeasured in Fe-50 Co (Bs = 10,000 gauss at 1742°F (950°C).So a basic composition Fe:Co at 1:1 appears most suitable forinitial efforts to raise the transformation temperature by ad-dition of alloying elements.

Addition of one weight percent of the elements known to raisethe alpha to gamma transformation temperature in pure ironwill be checked for their influence on transformation tempera-ture and saturation of the 1:1 cobalt-iron alloy. The first 12alloys were selected based on this argument. The alloys withcolumbium and tantalum contain only 0. 5 weight percent of thealloying elements because it is questionable whether the solu-bility limit will extend above this value in the temperatureregion to be tested.

Chromium and zinc close the gamma region of iron, althoughthe transformation temperature of iron will initially be loweredby the addition of either element. The addition of gold to irondecreases the transformation temperature but slightly.

17

TABLE 11-7. Alloys Selected for Alpha-Gamma Transformation Study

Number

2-0

2-1

2-2

2-3

2-4

2-5

2-6

2-7

2-8

2-9

2-10

2-11

2-12

2-13

2-14

2-15

2-16

2-17

2-18

Nominal Alloy Composition(Weight Percent)

50.

49.

49.

49.

49.

49.

49.

49.

49.

49.

49.

49.

49.

49.

49.

49.

49.

49.

49.

0

5

5

5

5

5

5

5

5

5

5

5

5

Fe-

Fe -

Fe-

Fe -

Fe-

Fe-

Fe -

Fe -

Fe -

Fe -

Fe -

Fe -

Fe -

75 Fe

75 Fe

5

5

5

5

Fe -

Fe -

Fe -

Fe -

50.

49.

49.

49.

49.

49.

49.

49.

49.

49.

49.

49.

49.

0

5

5

5

5

5

5

5

5

5

5

5

5

- 49.

- 49.

49.

49.

49.

49.

5

5

5

5

Co

Co-

Co-

Co-

Co-

Co-

Co-

Co-

Co-

Co-

Co-

Co-

Co-

75 Co

75 Co

Co-

Co-

Co-

Co-

1

1

1

1

1

1

1

1

1

1

1

1

-

-

1

1

1

1

Al

As

Be

Ge

Mo

P

Sb

Si

Sn

Ti

V

W

0.5 Nb

0.5 Ta

Cr

Zn

Au

Mn

18

In the case that all alloys tested do not indicate a potential forextending the temperature range where an alloy with magnetiza-tion saturation superior to pure cobalt can be used, a secondseries may be suggested.

It is anticipated that a second series of alloys would include ad-ditions of 0. 5 weight percent rare earth elements. It is notknown whether alloying is possible and what effect it might haveon transformation temperature and saturation. It is known thatthe number of Bohr magnetons in some of these alloys are veryhigh. Gadolinium, terbium, dysprosium, holmium, erbium,and thulium have effective Bohr magneton numbers of eight orhigher. A unique kind of interaction of the electrons might beexpected if these elements prove soluble in the Fe-Co matrix.

b. EXPERIMENTAL PROCEDURE: (See Section 11. A. 2. a.)

c. RESULTS

The alloys numbered 2-0, 2-1, 2-3, 2-5, 2-7, 2-17, and 2-18were melted as 15 gram ingots by the levitation melting tech-nique described in Section II. A.

The melting of alloys 2-2, 2-6, and 2-16 has been postponeduntil master melts are available because of the difficultiesanticipated during melting of compounds having high-vaporpressures at the melting temperatures.

Alloys 2-3 and 2-17 will be remelted. There are indicationsthat splashes during casting may have caused inhomogeneitiesin these ingots.

Testing of alloys on this program has not started.

3. Program for Next Quarter

Dilatometer tests to define the transformation temperature will beconducted.

19

C. TASK 3 - DISPERSION-STRENGTHENED MAGNETIC MATERIALSFOR APPLICATION IN THE 1200-1600 °F RANGE.

1. Summary of Technical Progress

a.) Purchase Orders for 18 prealloyed cobalt base and cobalt-iron base atomized powders were completed and submitted forapproval to the NASA Contracting Officer prior to placing theorders with suppliers.

b.) Specifications for cobalt and cobalt-iron base compositepowders containing dispersions of alumina and thoria, and asummary of quotations received were prepared and submittedfor review to the NASA Project Manager before preparing Pur-chase Orders. Later these will require approval by the NASAContracting Officer.

c.) Specifications for cobalt and cobalt-iron base extrusionscontaining dispersions of alumina and thoria, and a summary ofquotations received were prepared before writing Purchase Orders.

d.) A number of discussions were held with possible suppliersand various reports reviewed. Dr. F. R. Morrall of the CobaltInformation Center visited Westinghouse to discuss projects onthe dispersion-strengthening of cobalt which his organizationhad sponsored elsewhere.

2. Discussion

a. PREALLOYED ATOMIZED POWDERS

The 18 prealloyed atomized powders to be used in the programare listed in Table 11-8. The end product which will be fabri-cated from each powder and tested is extruded rod. In the firstphase of this task, which involves an initial evaluation of variouscompositions, the amount of dispersed phase is of the order of10 percent by volume.

The atomizing process will provide an extremely rapid quench ofthe molten powder particles to the solid state ^'. This insuresthat the constituent particles of high-melting point, which solidifyfirst, will be dispersed and not have time to grow above submicronsize before the cobalt or cobalt-iron matrix has solidified.

(1) - Towner, R. J., "Atomized Powder Alloys of Aluminum", Metal Progress,May 1958, p. 70

20

TABLE 11-8. Atomized Powders

AtomizedPowderNumber

Nominal Composition(Weight Percent)

1

2

3

4

5

6

7

8

9

10

11

12

13

14

15

16

17

18

Pure cobalt

Pure cobalt -2 .0 boron

Pure cobalt -1.0 boron - 2 . 2 titanium

Pure cobalt -1.0 boron - 4.2 zirconium

Pure cobalt -1.0 boron - 4.2 columbium

Pure cobalt -1.0 boron - 8. 3 tantalum

Pure cobalt - 4.0 cerium

Pure cobalt - 2.5 aluminum

Pure cobalt -1.3 beryllium

27 cobalt - 73 iron

26.5 cobalt - 71.5 iron -2 .0 boron

26.1 cobalt - 70. 7 iron -1.0 boron - 2 . 2 titanium

25. 6 cobalt - 69.2 iron -1.0 boron - 4.2 zirconium

25. 6 cobalt - 69.2 iron -1.0 boron - 4.2 columbium

24. 5 cobalt - 66.2 iron -1.0 boron - 8. 3 tantalum

25.9 cobalt - 70.1 iron - 4.0 cerium

26. 3 cobalt - 71.0 iron - 2. 7 aluminum

26. 6 cobalt - 72.0 iron -1.4 beryllium

21

Powder Nos. 1 and 10, pure cobalt and 27 percent cobalt-73percent iron, do not contain alloy additions and will serve asbases for comparison with the other compositions. The twopercent boron additions in powder Nos. 2 and 11 will be presentpartially in solid solution and partially as dispersed particlesof metal boride compound. The change in solid solubility ofboron with temperature is slight, so that the amount of metalboride particles out of solution will be approximately the sameat room and elevated temperatures.

The boron additions in powder Nos. 3 through 6 and 12 through15 are for the purpose of formation of submicron boride particlescontaining titanium, zirconium, columbium, and tantalum whichare stable at high temperatures and resist agglomeration. Pow-der Nos. 7 and 16 contain cerium and will provide another dis-persion-hardening agent, the intermetallic compound CeCos.The aluminum and beryllium containing powders, Nos. 8, 9, 17,and 18, will be given internal oxidation treatments to form Al£O3and BeO dispersed particles at elevated temperatures where thealuminum and beryllium are in solid solution. Also, the ceriumcontaining alloys Nos. 7 and 16 may be considered for internaloxidation treatments.

Based on technical capability for meeting our specifications,the number of compositions quoted on, price, and delivery time,purchase orders were prepared for buying 14 powders fromHoeganaes Sponge Iron Corporation and four powders fromDomtar Chemicals Ltd. All four vendors who quoted wouldundertake to atomize these compositions on an experimentaleffort basis. Discussions were held with suppliers concern-ing ways of insuring homogeneity of composition of powderparticles from start to end of a run. Homogeneity is assuredby the following production methods the vendors will use: (1)induction melting and holding which exerts a stirring action onthe melt, and (2) the short production time (about 5 minutes)to atomize a 100 Ib. melt. Sampling of the powder stream dur-ing atomizing to check composition is not possible in the supplier'sequipment.

b. COMPOSITE POWDERS

The compositions of the powders for which quotations were solicitedfrom suppliers are listed in Table 11-9. The amount of dispersedoxide is constant, 10 percent by volume. The iron powders Nos.5 through 8 can be mixed with the cobalt powders to produce cobalt-iron base compositions. Another approach is to purchase cobalt-

22

TABLE 11-9. Composite Powders

CompositePowderNumber

1

2

3

4

5

6

7

8

9

10

11

12

Nominal Composition(Weight Percent)

95. 25 Co + 4. 75 A12O3

95. 25 Co + 4. 75 A12O3

88. 8 Co + 11.2 ThC>2

88. 8 Co + 11.2 ThO2

94. 7 Fe + 5. 30 A12O3

94. 7 Fe + 5. 30 A12O3

87. 6 Fe + 12. 4 ThCfe

87.6 Fe + 12.4ThO2

25. 6 Co + 69. 2 Fe + 5. 20 A12O3

25. 6 Co + 69. 2 Fe + 5. 20 A12O3

23. 7 Co + 64. 2 Fe + 12. 1 ThO2

23. 7 Co + 64. 2 Fe + 12. 1 ThO2

ParticleSize ofOxide

(Microns)

0.01-0.06

0. 1-0. 6

0.01-0.06

0.1-0.6

0.01-0.06

0.1-0.6

0.01-0.06

0.1-0.6

0.01-0.06

0.1-0.6

0.01-0.06

0.1-0.6

23

iron powders Nos. 9 through 12 directly. Selection of thefinal approach and compositions to be purchased will be justi-fied in terms of the technical capability of the supplier, pro-cessing technique used to make the material, price and deliverytime.

The oxide particles will be dispersed in metal particles or theoxide and metal phases will be intermixed so that when the pow-ders are fabricated into extrusions an even distribution of thesubmicron oxide particles in the metal matrix will result.

The summary of quotations received on composite powders inaccordance with our specifications shows that four vendors cansupply some or all of the powders made by the following pro-cesses: (1) coating of suspended oxide core particles by pre-cipitation of metal from aqueous solution, (2) high intensityarc co-vaporization of mixed oxides of cobalt or cobalt-iron,aluminum, and thorium followed by hydrogen reduction of cobaltor cobalt-iron oxides to metal, (3) a proprietary semi-metallicpowder process, and (4) mechanical mixing of metal and aluminapowders, and thermal decomposition of thorium salt on metalpowder to introduce thoria.

c. EXTRUSIONS OF DISPERSION-STRENGTHENED COBALTAND COBALT-IRON ALLOYS

Quotations from suppliers have been received on the composi-tions listed in Table 11-10. All compositions contain 10 percentby volume of oxide with the exception of No. 9 which containstwo percent by volume. Selection of the final compositions willbe based on technical capability of the vendor and processingtechnique used to make the material.

Suppliers of extrusions of dispersion-strengthened cobalt andcobalt-iron have proposed the following processes in accordancewith our specifications: (1) mechanical mixing of metal andalumina powders, and thermal decomposition of a thorium salton metal powder, and (2) co-dissolving the desired elementsin a volatile solvent, flash-drying, grinding and reduction ofmatrix oxides. After the above powders are prepared, com-pacting, sintering, and extrusion are performed.

24

TABLE 11-10. Supplier Extrusions

ExtrusionNumber

1

2

3

4

5

6

7

8

9

Nominal Composition(Weight Percent)

95. 25 Co + 4. 75 A12O3

95. 25 Co + 4. 75 A12O3

88.8 Co + 11.2 ThO2

88.8 Co+ 11.2 ThO2

25. 6 Co + 69. 2 Fe + 5. 20 A12O3

25. 6 Co + 69. 2 Fe + 5. 20 A12O3

23. 7 Co + 64. 2 Fe + 12. 1 ThO2

23. 7 Co + 64. 2 Fe + 12. 1 ThO2

97. 74Co + 2.26ThO2

ParticleSize ofOxide

(Microns)

0.01-0.06

0.1-0.6

0.01-0.06

0.1-0.6

0.01-0.06

0.1-0.6

0.01-0.06

0.1-0.6

0.01-0.06

3. Program for Next Quarter

a.) After purchase orders for prealloyed atomized powdershave been approved by the NASA Contracting Officer, the orderswill be placed with vendors.

b.) Purchase orders for composite powders and extrusionsof dispersion-strengthened cobalt and cobalt-iron alloys willbe submitted for approval to the NASA Contracting Officer.

c.) Once purchased materials are received, processing andtesting will be initiated.

25

D. TASK 4 - CREEP TESTING.

1. Summary of Technical Progress

a.) A reliable vacuum-creep capsule design previously devel-oped by Westinghouse was modified and the design improvedfor use on NAS 3-6465.

b.) Nivco alloy (72Co-23Ni and other elements) was se-lected for the 5,000 to 10,000-hour vacuum creep tests.

c.) Sufficient Nivco bar was obtained from Westinghouse pro-grams to conduct the vacuum creep tests. Official approval totest Nivco alloy was obtained from NASA. Creep test data willbe included in subsequent reports as it becomes available afterthe start of testing.

2. Discussion

Figure 11-3 represents the vacuum creep capsule design to be used inthe elevated temperature tests on magnetic materials for rotor appli-cation. The design was the result of a Westinghouse program wherevarious vacuum chamber designs, pumping systems, and extensometerswere evaluated to determine a system which could provide meaningfuldata at reasonable cost. Included in the extensometer evaluation weremeasurements of strain using mechanical methods located at variouspositions along the specimen and the use of strain gages. A slab ofNivco alloy bar was obtained from Westinghouse programs for testingon NAS 3-6465. The composition of the alloy to be tested is listed be-low in weight percent.

C Co Ni Mn Si Ti Al Zr Ingot No.

0.01 Bal 22.5 0.32 0.15 2.15 0.28 0.95 AC-232

Creep sample blanks were cut from the slab which had been solutionannealed at 1725°F in air for one hour and water quenched. Theblanks were rough machined and will be aged for 25 hours at 1225°±5°F.

As part of the program, a series of vacuum measurements were madeon the proposed capsule configuration to evaluate pressure losses inthe design. These included both hot and cold capsule vacuum measure-

26

SPECIMEN

EXTENSOMETERMOUNTING HOLES

ELECTRON BEAMWELDED

ELECTRON BEAMWELDED

BELLOWS(304 STAINLESS STEEL)

ELECTRON BEAMiWELDED

ELECTRON BEAMWELDED

TO VACUUM PUMP

FIGURE 11-3. Encapsulated Vacuum Creep Specimen

27

ments at a position on the upper end of the capsule (position ofhighest pressure) as well as at a position upstream from the vacuumpumps. Because the total capsule is heated, the ionization gage couldnot be located at the capsule top end; therefore, data were obtained bybrazing a 12-inch extension onto the capsule and locating the ioniza-tion gage at the top of this extension outside of the hot zone. After a48-hour bakeout, a cold-trapped, oil diffusion pumped capsule at 860 °Fachieved a pressure of 8.2 x 10~ ? torr at the capsule extensions.

A similar series of vacuum measurements were made using a fourliter per second ion pump. After 22 hours at 570 °F. the pressure atthe capsule extension was observed to be 6.1 x 10" ' torr and at thepumping port it was observed as 2.1 x 1.0"? torr. After 23 hours andan increase in temperature to 1050°F, the pressure was 5.5 x 10"?torr at the pump port and 3 x 10~ 6 torr at the top of the capsule ex-tension. A new ion-pumping system of twice the capacity is being pro-cured and will be available by April 1 to use in the test program. Itshould allow improved vacuum conditions during testing over that ob-served with the older ion pump. In addition, the removal of the cap-sule extension will reduce the chamber volume being pumped.

As part of a Westinghouse program to determine bellows reliability,one type of 304 stainless steel bellows has been held at 1350°F in airfor more than 4000 hours. Twice monthly the bellows is removedfrom the furnace and leak checked using a mass spectrometer. Asof this date, the bellows has remained leak tight. A second bellowswas removed from an actual creep test capsule at 2056 hours formetallographic examination. An examination failed to reveal any de-gree of deterioration in the bellows. No evidence of intergranularpenetration by oxygen was present.

3. Program for Next Quarter

a.) Creep testing at 1000°F and 1100 °F will be initiated.

28

SECTION III

PROGRAM II - HIGH TEMPERATURECAPACITOR FEASIBILITY

This program will study the feasibility of building a lightweight capacitorsuitable for operation up to 1100°F. It will utilize high-purity dielectricmaterials and specialized fabrication methods. The ultimate application isin lightweight, high-temperature, power-conditioning equipment suitable forspace application. The design goal is a capacitor of 100 to 200 microfaradvolts per cubic inch. This range is comparable with conventional low-temper-ature capacitors.

A. SUMMARY OF TECHNICAL PROGRESS.

1.) Major equipment items purchased by Westinghouse for machiningand electroding single wafer capacitors are operating satisfactorily.The items include a precision watering machine, an ultrasonic cutterand machine tool, a vibratory lapping/polishing machine, an ultra-sonic cleaner and a three electrode or "triode" sputtering system.

2.) Lucalox rods have been reproducibly sliced to a thickness of 10mils. These wafers were lapped and polished to 6 mils. Grain pullouts have not been completely eliminated and represent a potentialproblem area particularly for wafers lapped to thicknesses less than6 mils.

3.) A one inch square wafer of pyrolytic boron nitride (Boralloy,High Temperature Materials, Inc.) sliced from a 1 x 1 x 1/8 inchblock of "as received" material was lapped to a thickness of 1.5 mils.In this thickness range, the material is very flexible, translucent andfree of pin holes or pull outs.

4.) An order has been placed for six groupings of differently pro-cessed BeO wafers lapped to 10 mils. The vendor, ConsolidatedCeramics and Metallizing Corp., will machine the wafers from com-mercial stock ranging in purity from 99. 8 to 99% BeO and one groupof wafers will be hot pressed. The other materials are sintered fromdry pressed and isostatically pressed BeO.

29

5.) Five suppliers are being contacted concerning the availabilityof ultra high purity sputtering target materials of rhodium and platinum(for capacitor electrodes).

6.) A wafer holding fixture is being fabricated for sputtering nobelmetal electrodes through glass masks. Preliminary designs weremade for a small vacuum test furnace with tantalum radiation shields.The furnace will be set up in the CV-18 evaporator (Consolidated VacuumCorporation) which has been evacuated to about 5 x 10~8 torr with aliquid nitrogen cooled baffle.

30

B. DISCUSSION.

1. Dielectric Materials Selection

Four dielectric materials are presently being considered for singlelayer capacitor evaluation in terms of fabricability and electricalproperties. Based on these results, a final selection will be made.It is planned to obtain actual chemical analysis on the material se-lected for preparing multi-layer and monolithic type capacitors.

Included in the group of materials initially selected are aluminumoxide (single crystal and polycrystalline), pyrolytic boron nitrideand beryllium oxide. It will be necessary to perform precisionmachining, lapping and polishing operations on these as receivedmaterials to achieve the desired test capacitor thicknesses and sur-face finishes for comparative evaluation. Electrical data will be ob-tained on single wafer capacitors electroded by sputtering platinumand/or rhodium films on opposing surfaces. A flow diagram is shownin Figure III-l to illustrate this approach.

A tabulation of significant properties for a total of ten different mater-ials considered as possible candidates is shown in Table III-l. In-cluded in the table are all of the materials which are known to be avail-able commercially that have superior electrical properties at elevatedtemperatures. Table II1-2 shows a typical spectrochemical analysisfor each specific material selected for preliminary study. It is note-worthy that although all the materials listed have very low impuritycontents, pyrolytic boron nitride (Boralloy, High Temperature Mater-ials, Inc.) has a total metal impurity level of less than 0.0003%. The oxygencontent of this material is not given; however, it is generally consideredthat the oxygen as 6203 in pyrolytically deposited boron nitride is sub-stantially lower than it is for the hot pressed material.

2. Single Wafer Fabrication

In addition to a materials property tabulation, Table III-l summarizesthe present status of the program as indicated in the appropriate col-umns.i

The major equipment items obtained for preparing single wafercapacitors are:

a.) WMSA Precision Wafering Machine manufactured by Micro-mesh Manufacturing Corporation. The machine is equipped witha variable spindle speed motor and two variable longitudinal tablespeed ranges (0 to 1/4 and 0 to 3 inches per minute).

31

Material Selection

Mount Stock Materialfor Wafering

Slice Material(Diamond Wafering Machine)

Clean,

Ir^Mount & Lap Side 1

Inspection,Thickness. Storage

IPolish Side 1

Mount and Lap Side 2to Final Thickness

Polish Side 2Measure Thickness

Remove FromMeasure Thickness

Mount, Clean &

Final CleaningInspection, Storage

Mask - Sputter Electrodes(Triode Sputtering System)

Qualification Tests @ Room Temp.Inspection, Storage

Dielectric Constant &Tan a 1 KC

Voltage Test500-1000 VDC Insulation Resistance

J

Selection

High Temperature ElectricalMeasurements to 1100°F

Final Selection_L

Approval ofNASA Project Mgr.

FIGURE III-l. Preparation and Evaluation of Single Layer Capacitors

32

TABLE III-l. Tabulation of Dielectric Material Propertiesand Present Status

Material

A1203

A12°36* v>

A1203

BN

BN

BN

BeO

BeO

BeO

MgO

i

Microstructure

Single Crystal

Polycrystallme

Polycrystalhne

Hexagonal layerHigh degree oforientation

Polycrystallme

Polycrystallme

Polycrystalline

Polycrystallme

Polycrystalline

SingleCrystal

ProcessMethod

Verne ulUlampfusion)

Pressedand

Sintered

HotPressed

Pyrolyticdecompo-sition ofBC13 andNH3

HotPressed

HotPressed

Pressedand

Sintered

Pressedand

Sintered

HotPressed

CooledMelt

Mfg. orSource andTrade Name

Ljnde Div.UnionCarbideCorp.

GeneralElectric' Lucalox"

(W)AED(experi-mental)

HighTempera-ture Mater-ials Inc."Bor alloy"

CarborundumCompany

NationalCarbonCompany

CoorsBD 99. 5

AmericanLava Corp.Alsimag 754

AtomicsInter-national(experi-mental)

Norton Co."Magnorite"

Form( As Received

"Boule"- 3/4 '

Diameterx 3" long

Rods 3/4to 1-1/4"diameter

Disks

Plates 1 X1 X l/8r2 X 2 X 1/4"

NoneOrdered

NoneOrdered

(1)

(1)

Not knownat present

NoneOrdered

Purity

< 100 ppmimpurities

(2)

99.9%A1203 (2)

StartingMaterial< 100 ppmimpurities

Totalimpurities3 100 ppm

(2)

97% BN

~ 95 to97% BN

99. 5% BeO

99. 5% BeO

Startingmaterial -MinoxAAA

(2)

99. 9% MgO

Density -^of

Theoretical

-100

-100 .

-100

~ 98

>93.4

-90

-95

-99.7

-100

PreseiStatus

Twobouleson hand

0. 006"thickwafers •sliced,lapped £polished

Several0. 370 X0. 010"disksavailable

0. 001 to0. 002"wafers -sliced,lapped &polished

Not se-lected ascandidalmaterial

Not se-lected ascandidatimaterial

(1)

(1)

Samplerequestei

Not se-lected ascandidatematerial

1. An order has been placed with Consolidated Ceramics Inc. for machined disks of2 See Table 111-2 for spectrochemical analysis of materials.

33

ELECTRICAL PROPERTIES

DC ResistivityOhm -Cm

(Approximate Values)

400°C - 7 X 1012

600°C - 7 X 1010

400°C - 1 X 1013

600<C - 3 X 1010

i

1400-C 5 X 1012

600°C - 9 X 1010

400<C - 1014

eoo-c - io13

420°C- 1. 7X IO11

550"C - 8. 3 X 10°660°C - 3. 4 X IO7

482<C - 5 X IO8

1000°C'- 1 X IO7

300°C - MO*5

500-O - 5 X IO13

700=0 - 1. 5 X IO10

(

I

400°C - IO}3

600"C - 10l*

No measurements

600-C - 1. 6 X IO12

1000 °C - IO8

Tan 8

@ IO5 cps JL tooptic axis400 =C- 0.0002600°C- 0.001

@ 9720 me20°C - 0. 000025

Not Measured

@ 4kmc, "a"direction RTto 649 °C, ap-proximate0. 0004 over thetemperaturerange

@ IO3 cps400«C- 0.012600°C - 0. 14

§ IO3 cpssoot:- o.ois575-^- 1.0

No lowfrequency datagiven

No lowfrequency datagiven

No measurement!

@ 100 cps25 °C- 0.0003

DielectricConstant

@ IO5 cps 60=to optic axisK@20*C - 9K@900<C - 10

@ 9720 me20°C - 9. 9

Not Measured

K3.4"c"direction @RT, notmeasuredat elevatedtemperature

@ IO3 cps400°C- 4.5600°C - 6. 5

@ IO3 cps21<C- 4.4300-0 - 4. 52

@ 1 me6.7

~7

Nomeasure-ments

@ 100 cps25-C- 9.65

Electric Strength/ Voltage \\ Breakdown /

1700 volts/mil@ 60 cps, 20mil thick sample(Room temper-ature)

1700 volts/mil§20<C, 20 milthick sample

Not Measured

4000 volts/milin "c" direction,d-c 10 to 20 milsample (notmeasured atelevated temper-ature)

1450 volts/mil@ RT, sample10 mils thick

500-1000 volts/mil, thicknessnot known

700 volts/milaverage RMSat RT, 10 milsample thickness

None given

Nomeasurements

No data given

Remarks

No electrical breakdownstrength at elevated temper-ature. Tan 4 and dielectricconstant data not given for 60cps to 50 kc freq. vs. temp.

Low frequency (60 cps to 50kc) Tan J and dielectric con-stant not given. High temper-ature voltage breakdown notgiven.

Low frequency data not avail-able (vs. temperature) (60cps to 50 kc)

Not selected as candidatematerial because of lowdensity.

Not selected as candidatematerial because of lowdensity.

Sample requested.

Not selected as candidatematerial because of hydro-scopic characteristics.

DataReference

Lmde IndustrialCrystals Bulletin

F-814-CF-917-B

Company DataBulletin

AF33(615)1360

Materials in De-sign Eng. , Feb1964 (M. Bosche& D. Schiff)

Company DataBulletin

Company DataBulletin H-8745

Company DataBulletin

Company DataBulletin

Private com-municationfrom R. L.McKisson

Norton Co.Memo Feb. 1,1963

O from various commercial sources

TABLE III-2. Spectrochemical Analysis of Candidate Dielectrics

AMTFRLAL

L,'°.,ilo\(GeneralEleitr ic Co.)

Linde Sapphire(dingle Crystal

A1203)

Boralloy BoronNitride (3)(Pyrolytic Bn)(High Temper-ature MaterialsInc.)

Minox AAABeO powderused to preparehot pressedmaterials byAtomicsInternational

ELEMEN

Al Fe Mg Ti Mn V Na Cu Ni Ca Cr Ga

Percent |

Major 0.002 0 15 (1) (U (1) (1) (1) (1) 0.004 (1) (1)

Parts Per Millio

(U

(1)

< 2

(1)

<2 (2) (2)

~

(2)

(1) (1) (1) (1)

(2) (2) (2) 9 (2) (2)

Percent (%)

(1)

75 35 50 1 1 -- 75

0. 0001 (1) 0. 0001 (1) (1)

Parts Per Million

1 7 80 15 ..

(1) Not detected.

(2) These elements not listed.

(3) Total impurities less than 0. 003%. Thirty-four additionalelements listed as not detected.

34

Si '. Mo B Zr Cd Pb Ba Bi Co Sm 1 la

).03 (2) (2) (2) (2) (2) (2) (2) (2) (2) (2)

>pm)

6 (2) (2) (2) (2) (2)

--

(2) (2) (2) (2) (2)

9. 0001 (1) Major (1) (1) (1) (1) (1) (1) (1) (1)

m)

25 <3 <1 <30 < l <2 <5 <5 < 1 <5 <5

REFERENCE SOURCE

ASDTR-61-628,Part 1 1 Studiesof the BrittleBehavior of CeramicMaterials, April1963 - ContractAF33(616)7465

Letter fromMr. B G Benak(Lmde Co )

Company DatasheetDated February 1,1965

Letter fromR. L. McKisson(AtomicsInternational)

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TRANSFORMER MATERIALS SUMMARY

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SOLENOID MATERIALS SUMMARY

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b.) Model 602, Mazur Lapping/Polishing Machine manu-factured by Westinghouse Scientific Equipment Division. Themachine is equipped with a variable vibrational speed controland timer.

c.) Model 200 B-5 Bench Type Ultrasonic Machine Toolmanufactured by Sheffield Corporation.

d.) Model F, Industrial Abrasive Unit manufactured byS. S. White Co.

e.) Model L-300 Ultrasonic Cleaner manufactured by Lands-verk Electrometer Co.

f.) Model AST-100 Low Energy Sputtering System (Plasmavac)including a CV-18 Vacuum Evaporator manufactured by Consoli-dated Vacuum Corporation. The system has an ultimate vacuumof 3. 5 x 10~8 torr. Sputtering operations are performed usinga novel three electrode technique.

3. Wafer Slicing

The Lucalox rod was sliced into wafers ranging in thickness from 8 to15 mils. Six wafers were sliced in the 10 mil thickness range.Pyrolytic boron nitride was wafered into 10 to 12 mil thick slices.A yield of five wafers per 1/8 inch thick block was obtained.

Lucalox rod stock and a 1 x 1 x 1/8 inch block of pyrolytic boron nitridewas mounted and sliced as follows:

a. MOUNTING FOR SLICING OPERATIONS

A 3/4 inch diameter x 3 inch long Lucalox rod was cemented to aglass plate with LOG-Wax 20 (Geoscience Instrument Co.) andsliced as shown in Figure III-2. A 1 x 1 x 1/8 inch block ofpyrolytic boron nitride was also mounted and sliced in a similarmanner.

b. SLICING

Slicing Machine: WMSA Precision Watering Machine

Diamond Wheel: Metal Bonded Diamond Wheel manufacturedby Norton Co., Abrasives Div.Wheel Diameter - 5 inches

35

10 mil w a f e r

FIGURE 111-2. Lucalox Rod Stock With 10 Mil SlicedWafer Held in LOC-Wax 20

(Geoscience Instrument Co.)

36

Wheel Thickness - 0. 017 inchesManufacturer's Identification 1-5 x 0. 015 x 5/8,D220-N100M-1/8, ME 73082

Travel Speed: Wafers were cut at longitudinal table speedsin the range from 0. 059 to 0. Ill inches per minute.

Coolant & Wheel RPM : Water was used as a coolant. Thewheel was rotated at 3800 rpm during all cuttingoperations.

4. Lapping Procedures & Results

The sliced wafers were bonded to a 3 x 3 inch piece of plate glass witha lightly frosted surface to improve adhesion. A black, low meltingpoint wax (Pyseal, Fisher Scientific Co.) was used. The glass platewas heated on a hot plate to the flow temperature of the wax ~158°F( ~ 70 °C). After applying a thin coating of wax, the preheated waferswere positioned on the plate and the excess wax was then squeezed outfrom under the wafers by applying light and uniform pressure to eachindividual wafer.

Controlled wafer thickness were achieved by cementing metal (steel)shim strips along two edges of the glass. An epoxy cement was usedto permanently bond the shim strips to the glass. A series of glassplates with different thickness shims were made ranging from 2 to 10mils. Each set of wafers were sequencially lapped by transferringthem to thinner shimmed plates until the desired thickness was ob-tained (2 to 6 mils). Figure 111-3 shows two sliced Lucalox waferslapped to 6 mils. In addition, a 10 mil hot pressed A^C^ disk is alsoshown. All thickness measurements were made with a hand heldmicrometer.

Lapping and polishing operations were performed with a Mazur Lapping/Polishing Machine manufactured by Westinghouse Scientific EquipmentDepartment. The machine operation is based on a variable-speed,eccentrically-rotating plate with interchangeable trays that containdifferent grades of abrasives. Each tray has a plate glass removablebase. Lapping and polishing can be done directly on the glass plateor the plate can be covered with a variety of bonded surfacing materials.

Table III-3 shows a lapping and polishing sequence which was found toyield the least number of grain pull outs in Lucalox wafers. In manyinstances, large areas of the Lucalox wafer surfaces were free from

37

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A & B - 6 Mil Lucalox Wafer Cut and LappedFrom 3/4 Inch Rod Stock

C - 10 Mil Hot Pressed Al2O3 PreparedUnder WAED Contract AF33(615)360

Note the Translucence of the Materials.

FIGURE 111-3. Dielectric Materials

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pull outs; however, occasional grain voids were found in all waferswhen their surfaces were completely scanned at high magnification.In general, the highest concentration of voids or pull outs were foundin the central area of a wafer. Wafers that were lapped to 2 mils hadvoids that penetrated the entire thickness of the wafer resulting in pinholes. It appears, at present, that 5 to 6 mil wafers can be producedfree of pin holes and these wafers could be electroded and tested.

Although the measured thickness of these wafers is in the range of 5to 6 mils their effective thicknesses (due to large grain pull outs)after electroding might be in the 4 to 5 mil range. In addition, sur-face voids would contribute to high voltage stress concentrations duringelectric strength tests causing premature breakdown.

A pyrolytic boron nitride wafer has been lapped and polished with rela-tive ease to a measured thickness that varied from 1 to 2 mils acrossthe wafer surface (Table 111-3 shows the lapping sequence). Thiswafer exhibited an unusually high degree of flexibility (about equivalentto mica sheet or paper in the same thickness range). No visible pinholes or pull outs could be seen. At this stage, pyrolytic boron nitrideappears very promising.

Mechanical stresses that occur during machining of brittle materialscannot be entirely eliminated but they can be minimized. Table 111-4contains a listing of possible causes of grain pull outs together withappropriate corrective actions.

5. Dielectric Measurements

It is not planned to make extensive high-temperature dielectric meas-urements until an inventory of qualified, single-wafer capacitors areaccumulated. Room temperature measurements will be made to deter-mine test sample qualification as follows:

a.) Dielectric constant and Tan 6 @ 1 KG

b.) Insulation resistance

c.) Voltage Test: 500 to 1000 VDC

Preliminary designs are being considered for constructing a small cold-wall vacuum furnace capable of heating test specimens to HOOT in a

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vacuum in the lO'7 - 10"8 torr range. The vacuum pumping unit(Model CV18) presently combined with our sputtering unit can evacuatean 18-inch glass bell jar into the 10-8 torr range.

42

C. PROGRAM FOR NEXT QUARTER.

1.) Fabrication of single crystal sapphire wafers will be started.

2.) Lucalox and pyrolytic boron nitride machining and polishingstudies will be continued.

3.) Sputtered rhodium and platinum electrodes will be applied tolapped and polished wafers of the candidate dielectric materials.

4.) Dielectric tests will be started including qualification tests andhigh temperature dielectric measurements;

43

SECTION IV

PROGRAM III - BORE SEAL DEVELOPMENTAND COMBINED MATERIAL INVESTIGATIONSUNDER A SPACE SIMULATED ENVIRONMENT

The bore seal effort under Task 1 will evaluate promising ceramic-metalsealing systems in potassium and lithium vapor at temperatures to 1600°Ffor 2000 hours. Elevated temperature seal strength and vacuum tightnesswill be determined. A four-inch diameter bore seal loaded with potassiumwill be used in a 5000-hour stator endurance evaluation at temperature andin a high-vacuum environment to confirm data determined on smallergeometries.

Two five-thousand hour tests will be run under Task 2 on a stator which typifiesthe construction of an inductor alternator or a motor. The first will be runbetween 800 - 1100°F temperature. The second test will be run with a boreseal at temperatures between 1100 - 1600°F. All will be tested at high vac-uum (greater than 10"^ torr) under electric and magnetic stresses.

A transformer and two solenoids under Tasks 3 and 4 will be similarlytested under high-vacuum and at elevated temperature. The purpose willbe to evaluate the combined effects of electric and magnetic stresses, andhigh vacuum on combinations of materials suitable for application to advancedspace electric power systems. One solenoid test will be under d-c excitationand the other under intermittent excitation so the effects of an invariant elec-tric stress can be investigated.

44

TASK 1 - BORE SEAL DEVELOPMENT.

1. Summary of Technical Progress

a.) The alkali metal loading facility has been undergoing modi-fication to make provisions for manipulative controls through thevacuum chamber walls and for the electron-beam welder whichwill be used in final closure of the alkali metal corrosion testcapsules.

b.) Microhardness surveys were completed across the metal-braze alloy-ceramic seals which survived alkali metal exposureon a previous bore seal program conducted on NAS 3-4162.

c.) Two additional ceramics and six braze alloys have beenordered. Delivery is scheduled for the second quarter.

d.) Tentative design of the model four-inch diameter bore sealhas been completed.

2. Discussion

a. FACILITY DESIGN

The chamber which was utilized in performance of the previouscontract NAS 3-4162 is being modified to include provisions forloading test capsules with alkali metal in a vacuum of 1 x 10"5torr and for electron-beam welding of the final closure. Thisrequires manipulative control through the vacuum chamber walls.A schematic layout of the loading chamber is shown in Figure IV-1.The capsule loading techniques which are to be used with the modi-fied equipment have been evaluated. The manipulators for theloading chamber and the electron-beam welder have been delivered.A 1500 jH/sec diffusion pump is on order.

The present vacuum system for alkali metal loaded capsule testingfurnace is being converted to ion pumps to achieve a vacuum of10~9 torr. The modifications associated with this change areshown in Figure IV-2. The 400 I/sec ion pump and power sup-ply for the dual vacuum environmental test furnaces are on order.

b. BORE SEAL MATERIALS AND SEALING STUDY

The ceramic bodies (low silica 99.8% beryllia and low silica yttria),refractory metal member (low oxygen columbium-1% zirconium),

45

TO:

BTI #1615.06 KW POWER SUPPLY

ELECTRON BEAM WELDERBTI #785

GUN BOOMBTI #215-7

TURNTABLEBTI #1920-12

MANIPULATORMRC #V4-120

ARGONSYSTEM

(NO CHANGE)WELCH13978

CVC#BCRU

NRC#HKG1500

ALKALI METAL"HOT TRAP"

FREON 12REFRIGER-ATIONUNIT

FIGURE IV-1. Schematic of the Capsule Fabricationand Loading Equipment

46

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FIGURE IV-2. Schematic of Dual Vacuum Furnace ModificationsUsing Ion Pumping

47

and special braze alloys required in the bore seal test programare all long lead-time items. Delivery of most of these mater-ials is scheduled in the second quarter. A discussion of thehigh-temperature seal fabrication program follows.

1) Active Metal Brazing

The evaluation of ceramic-to-metal seals which withstood500 hour alkali metal exposure at 1600°F on Contract NAS3-4162 was continued.

Thermalox 998 (99. 8% BeO ceramic made by Brush Beryl-lium Co.) joined to columbium-1% zirconium alloy withactive metal braze of composition 56Zr-28V-16Ti ex-hibited a modulus of rupture strength averaging 11,800psi after exposure at 1600°F for 500 hours in potassiumvapor. This seal system also exhibited a similar strengthafter exposure to lithium at 1000 °F for 500 hours. Thisseal system will be tested for a period of 2000 hours inhigh purity potassium and lithium at 1600 °F on this program.

Variable joint micro structure of the seals previouslytested was attributed primarily to brazing parameters andaging rather than alkali metal exposure. &)

The effects of 500 hour aging on the active-metal-brazedseals is being determined by microhardness surveys andelectron microprobe analyses. Since the ceramic-to-brazeinterface region is most susceptible to aging effects, em-phasis is being placed on the study of this area.

In addition to the 56Zr-28V-16Ti, seals made with 75Zr-19Cb-6Be and 48Zr-48Ti-4Be retained strength afterexposure in previous tests. (2) These and several other high-temperature, low-oxygen active metal-braze alloys will bescreened.

' ' - Kueser, P. E., et al, Bore Seal Technology, NASA-CR-54093, Contract NAS 3-4162.

W -Ibid.

48

The yttrium-columbium and yttrium-beryllium alloysystems will also be investigated. The Cb - Y alloysare markedly softer than pure Cb; even small additionsof Y ( < 1%) produce significant reduction in hardness andincreases the cold workability of columbium. This effectmay be caused by the impurity scavenging of yttrium. ™)

Since corrosion of the active-metal-braze joint proceedsat the ceramic-to-braze interface by reaction with the oxideswhich are formed, it is desirable to have braze systemswhich produce reacted oxides having maximum thermo-dynamic stability. Yttrium oxide and beryllium oxide havesuch stability. Potential suppliers, including BattelleMemorial Institute, Materials Research Corporation andRodney Metals, have been contacted to obtain pure, low-oxygen yttrium metal for the braze alloy investigation.

Ceramic-to-metal seals will be made using braze alloys infoil form, when practicable, to minimize oxygen contamina-tion.

Battelle Memorial Institute which supplied active-metal-braze alloys on NAS 3-4162 will supply active braze alloysin the form of foil for those useful compositions which areductile enough to roll.

2) Alternate Seals

A limited number of seals will be made as a back-up forthe active-metal-sealing systems. Ceramic-to-metal sealswill be fabricated by utilizing several of the following alter-nate approaches:

a) Pressure seals or diffusion bonding

b) Evaporated metallizing

c) Gradient seals

Spedding, F. H. and A. H. Daane, The Rare Earths, John Wiley &Sons, Inc., N. Y. C. 1961.

49

d) Ion sputtering

e) Combinations of ion sputtering or evaporatedmetallizing, chemical vapor deposition, andbrazing.

In pressure bonding, a metal diffusion plating or washer isbonded at temperature to a metallized ceramic. Pressuremay be applied externally or generated through thermal mis-match of ceramic and metal members. The coating on theceramic is an alkali metal resistant metallizing.

Evaporated metallizings showed nrpmise in the work com-pleted on the previous program. ™ Chemical vapordeposited columbium-1% zirconium or other alkali-metal-resistant deposits will be used. This approach appearsmost promising as a wetting aid for active-metal brazingof large surface areas.

A gradient seal consists of an integrally bonded compositestructure of metal and ceramic which varies from nearly100 percent ceramic to 100 percent metal in a continuouslygraduated manner. The metal end (or ends) may then bejoined to the electrical apparatus frame by conventionalmethods. Combinations of ceramic and metal will be chosenfrom rhenium, columbium, alumina or beryllia, or otherappropriate materials.

Ion sputtering of molybdenum or Cb - 1 Zr onto a ceramicsubstrate (5» «) followed by a thicker coating of metal (i. e.Cb - 1 Zr ) applied by chemical vapor deposition C') andbrazing to a metal member appears promising for seal

*- Kueser, P. E. , et al, Bore Seal Technology, NASA-CR-54093, ContractNAS 3-4162.

(5>- Mattox, D. M. , Sandia Corporation, Reprint, SC-R-64-1330, September

f*\ 1964>

I8'- Maisset, L. I. , and P. M. Schailbe, "Thin Films Deposited by Bias Sputter-ing", Journal of Applied Physics, Vol. 36, No. 1, p. 237, Jan. 1965.

CO- Reed, L. and R. McRae, "Evaporated Metallizing", American CeramicSociety Bulletin, January 1965.

50

fabrication. This method offers the possibility of a clean,highly adherent interface. The system limits oxygen con-centration to one highly polarized Be-O-Cb or Be-O-Molayer v^> 9) which is immune to solution by potassium.

At the present time, methods b, d, and e are preferred andeffort on supplementary seal systems will be emphasized inthese areas.

c. CERAMIC MATERIALS

The ceramic bodies which survived the 500 hour, 1600°F potassiumexposure on the previous program (NAS 3-4162) were:

Thermalox 998 - 99. 8% beryllium oxide by Brush Beryllium Co.

Sapphire - 100% alumina by Linde Co.

Lucalox - 99. 8% aluminum oxide by General Electric Co.

Experimental results established the desirability of low silicacontent ( < 0.05%) in ceramics intended for potassium exposureat 1600°F.

Sapphire and Lucalox are useful for feedthrough geometries butare not available in large sizes (greater than four-inch diameter)for actual bore seal construction. Coors Porcelain Co., WesternGold and Platinum Co., General Electric Co., Linde Co., CorningGlass Co., Alite Div., and U. S. Stoneware Co. were contactedto determine the availability of fabricable, low-silica ( < 0. 05%)alumina. Such bodies are not available at the present time. How-ever, several experimental bodies are being developed by CoorsPorcelain Co.

^ ' - DiStefano, J. R. and A. P. Litman "Effects of Impurities in Some Re-fractory Metal-Alkali Metal Systems", Corrosion, Vol. 20, No. 12,p. 392, Dec. 1964.

(9) - Weyl, W. A., Coloured Glasses, p. 343, Society of Glass Technology,Sheffield, Rp. Dawson, London.

51

Table I V-l shows the spectrographic silica analyses ofseveral Coors experimental alumina bodies, and the U. S.Stoneware (Alite Division) alumina body No. 610. Theanalyses of several bodies which were used on the previousprogram are also shown. The results indicate that anumber of the Coors alumina bodies have the desirablelow-silica content. When available, they will be consideredfor use as a back-up ceramic.

Two new ceramic bodies will be tested in potassium on thepresent program. These have been selected as

a) 99.9% beryllium oxide or low silica ( < SOppmSiOo) 99. 8% beryllium oxide (Brush BerylliumCo.)

b) 99+% yttrium oxide (Coors Porcelain Co.)

The rare earth oxides possess good thermodynamic proper-ties. However, experience in fabricating bodies is limited(10 and 11)

The Brush 99. 8% beryllia body has been ordered for use onceramic outgassing and braze alloy screening investigations.In addition, ceramics which survived exposure on theprevious program and the new ceramic bodies which with-stand 500 hour exposure at 1600°F will be subjected to 2000hour tests.

3. Program for the Next Quarter

a.) Complete design and construction of loading and test facility.

* '- Ploetz, G. L., C. W. Krystyniak, H. E. Dumas, "Sintering Character-istics of Rare Earth Oxides", Journal of American Ceramic Society,Vol. 41, No. 12, p. 550, 1958.

- Perez, M., Y. Gorba, F. Queryroux, and R. Collorieques, Bull. Soc.Franc. Min. Crist., Vol. 84 (4), pp. 401-402, 1961.

52

TABLE I V-l. Spectrographic Silica Analyses of Selected Ceramics

SupplierDesignationof Ceramic

BodyNominal

CompositionSiO2 Content(Weight Percent)

Alite #610 Alumina

Ei3-3 Alumina(Wesgo)

Thermalox 998Beryllia (BrushBeryllium Co.)

Lucalox Alumina(a E. )

Sapphire Alumina(Linde)

Coors #1 Alumina

Coors #2 Alumina

Coors ATD 995Alumina

Coors X Alumina

Coors Y Alumina

(c)

99. 7 A12O3-0.1 SiO2-0.1 MgO

99. 8% BeO

99. 7% A12O3-0. 25 MgO

100% A12O3

(c)

(c)

(c)

(c)

(c)

1.5

0.2

0.015

0.02

0.015

0.005

0.03

0.04

0.02

0.025

^

(a) Eitel-McCullough, Inc. All data ± 200%

(b) American Spectrographic Laboratories, San Francisco

(c) Compositions were not given by supplier; all are "high alumina".

53

b.) Complete ordering of materials for screening of ceramicand brazes.

c.) Initiate ceramic outgassing study.

d.) Start experimental work on screening of braze alloys andalternate seals.

54

B. TASK 2 - STATOR AND BORE SEAL.

1. Summary of Technical Progress

a.) A stator design for the first 5000-hour test has beencompleted. All long lead time materials are on order.

b.) The two vacuum environmental test furnaces and associatedcontrol equipment were ordered. Both furnaces are now underconstruction and should be delivered by the 3rd week in April.

c.) A design for vacuum furnace test specimen thermocouplefeedthroughs which are compatible with special shielded thermo-couples has been completed.

d.) A test specimen thermocouple design specification hasbeen released for quotations. (This thermocouple design willbe used on Tasks 2, 3, and 4.)

2. Discussion

The assembly and detail drawings which define the components and as-semblies that make up the stator are given in Appendix A. A summaryof the major materials used in the constructions are also shown in theAppendix. The sequence of drawings begins with the stator assembly,followed by stack assembly drawings, details (several parts to a draw-ing, identified as items and assemblies) and component parts. Twostator stack drawings are included. EDSK 326602 shows a practicewinding stack using plain copper conductors and steel punchings. Thisassembly will be used to develop coil forming procedures and coilinstallation techniques before working with the high-temperature con-ductors.

In some cases the detail drawings show parts that apply to the trans-former or solenoid models. In such cases the same drawings are re-peated in the drawings covering the subject models.

The stator design is based on the solid-rotor, inductor generator con-cept using one stack of laminations. It also typifies a motor construc-tion. The excitation coils found in an inductor generator have beeneliminated from the design since the winding is similar to the solenoidwinding used in Task 4. The stack is made up of Hiperco 27 (27 Co-Fe)laminations, 0. 008 inch thick, which are held in place in a Hiperco 27frame by a bolted and pinned retaining ring. The laminations will be

55

annealed in a hydrogen atmosphere for one hour minimum at a tem-perature of 1492 to 1672 °F. Forgings will be annealed in a roughmachined condition in an exotherm gas atmosphere for one hour mini-mum at a temperature of 1492 to 1672°F.

Ceramic slot liners insulate the conductors from the laminations andfrom each other. Non-magnetic end bells are attached to each end ofthe magnetic frame.

The stator windings consist of three 12-turn coils which are installedin the frame in the same manner as in a standard three-phase machine.Thermocouples are located in two of the 12 slots filled by each winding.Additional thermocouples are positioned in the laminations; at the outeredge (OD) of the laminations, and attached to the outside of the magneticframe and to coil end-turns.

The high-temperature stator to be used in conjunction with the boreseal will be of the same design except that additional members will berequired to support the bore seal in position in the stator cavity. Inaddition, a special high-temperature stator winding and insulation sys-tem capable of extended operation at approximately HOOT has beenspecified for the bore seal stator. The first stator will operate at1100°F and will utilize a modified Anaconda Anadur (refractory oxidefilled fiber glass) high-temperature insulation system evaluated underNAS 3-4162.

Figure IV- 3 is a cutaway drawing of the vacuum furnace which showsthe stator installed in the furnace hot zone. Stator thermocouple leadsand winding leads are brought up through holes in the top heat shieldsto their respective feedthroughs in the chamber wall. The chamber isof double wall construction with baffles between the walls to channelcooling water flow. The chamber top cover is also double walled toprovide a path for cooling water.

Figure IV- 4 is a sketch showing the details of the vacuum furnacethermocouple feedthroughs. The thermocouples pass through the hollowtubes and are brazed to the tubes outside the chamber to form a vacuum-tight seal. An inner ceramic disc provides mechanical support andacts as a thermal radiation shield.

The thermocouple construction consists of two wires in an inconelsheath with Al2O% powder (99%) insulating the wires from each otherand from the sheath. The wire system is Platinel II (platinum -rhodium - gold) made by Engelhardt. Final sizing (OD) is done bydrawing the complete assembly.

56

•e0)

CO

HH

eo>s

Hfe2

0)o

3

E*0)

IU

•CO

I57

MODIFIED OCTALTUBULAR FEEDTHROUGH

OUTSIDE OFCHAMBER

CERAMIC TOMETAL JOINT(8 PLACES)

METAL TOMETAL JOINT

NICKEL TUBES(8)

CHAMBER WALL

INSIDE OFCHAMBER

CERAMIC DISC

FLARE NICKELTUBING(8 PLACES)

CLIPS

FIGURE IV-4. Details of Thermocouple Feedthrough Flangeon the Vacuum Furnace Chamber

58

3. Program for the Next Quarter

a.) Expedite the procurement of long lead time materials.

b. ) Coordinate vacuum furnace delivery, installation andcheck-out.

c.) Build a practice stator assembly as a check on coil form-ing techniques.

d. ) Continue the manufacture of stator detail parts and begintest specimen assembly.

e.) Evaluate a new high temperature plasma arc sprayed in-sulation system. The insulation is high purity Linde A

f. ) Evaluate Handy & Harmon lithobraz 'BT' and Braze 360brazing alloys for thermocouple feedthrough brazing.

g.) Continue the 1500°F, 5000-hour vacuum stability tests onInconel-clad silver.

59

C. TASK 3 - TRANSFORMER.

1. Summary of Technical Progress

a.) A transformer design has been completed and all long leadtime materials are on order.

b.) An engineering model release has been prepared to manu-facture the parts in the shop.

2. Discussion

The assembly and detail drawings which define the components and as-semblies that make up the transformer are shown in Appendix B. Asummary of the major materials used in the constructions are also shownin the Appendix. The sequence of drawings begins with the transformerassembly, followed by the winding assembly, details (several parts toa drawing, identified as items) and component parts.

In some cases the detail drawings show parts that apply to the statorand solenoid models. In such cases the same drawings are repeatedin the drawings covering the subject models.

Figure IV-5 is a view of the transformer assembly showing the locationof the winding leads and thermocouple leads. This design is rated at1 KVA with 600 volts on the primary winding and approximately 30volts at the secondary winding. The core is made from E-I styleHiperco 27 laminations 0.008 inch thick. Evaluation of plasma-arcsprayed insulation is required to confirm the inter laminar insulationsystem that will be used. The windings are formed around a ceramicspool which provides insulation between the windings and the centerleg of the core. Ceramic endplates and channels provide insulationbetween the winding ends and sides respectively and the laminations.

Pairs of thermocouples are installed between the primary winding andceramic spool and between the two windings. The core has been dividedinto two halves by ceramic strip spacers so that four thermocouplescan be buried in the core.

Non-magnetic alloy strips are used outside the laminations to providelamination support. The laminations and support strips are held to-gether by through studs, ceramic washers and lock nuts.

60

(HV

ISfi

gin

ai

61

3. Program for the Next Quarter

a.) Expedite the procurement of long lead time items.

b.) Continue the manufacture of transformer detail parts andbegin test specimen assembly.

c.) Evaluate a plasma-arc sprayed ALjC^ lamination insulationsystem.

62

D. TASK 4 - SOLENOID.

1. Summary of Technical Progress

a.) A solenoid design has been completed and all long lead timematerials are on order.

b.) An engineering model release has been prepared to initiatemanufacture of the parts.

2. Discussion

Appendix C shows the drawings which define the assemblies and compo-nents which make up the solenoid. A summary of the major materialsused in the constructions are also given in the Appendix. The sequenceof drawings begin with the solenoid assembly, followed by the windingassembly, details (several parts to a drawing, identified as items andassemblies) and component parts.

Figure IV-6 is a view of the external configuration of the solenoidshowing the location of the coil leads and thermocouple leads. Aweight of approximately three pounds is suspended on the plunger,and when the solenoid is actuated the weight is lifted approximately0.050 inches and held in that position.

The magnetic solenoid housing, cover and plunger are made from aHiperco 27 forging. The coil is wound on a ceramic spool which pro-vides insulation between the winding and the plunger and housing centercore. Ceramic end plates insulate the sides of the winding from theHiperco 27 housing and cover. Bearing surfaces for the plunger con-sist of a ceramic guide rod at one end of the plunger and a ceramicbushing at the opposite end.

Pairs of thermocouples are installed between the coil and the ceramiccoil spool, midway between the coil ID and OD, between the coil ODand the housing, and on the outside of the housing.

3. Program for the Next Quarter

a.) Expedite the procurement of long lead time items.

b.) Complete the manufacture of solenoid detail parts and be-gin test specimen assembly.

c.) Carry out a heat transfer calculation from the inside to theoutside of the coil.

63

THERMOCOUPLES

CERAMIC END PLATE

CERAMICGUIDE ROD

CERAMIC SPOOL

COIL

CERAMICEND PLATE

PLUNGERSTOP PLATE

WEIGHT

COIL LEADS

GUIDE RODRETAINER

MAGNETICHOUSING

POTTINGCOMPOUND

PLUNGER

MAGNETICCOVER

POTTINGCOMPOUND

CERAMIC BUSHING

METAL"0" RING

FIGURE IV-6. Cutaway View of Solenoid

64