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AD NUMBER

ADB093690

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TOApproved for public release, distributionunlimited

FROMDistribution authorized to U.S. Gov't.agencies only; Test and Evaluation; 30 MAY1984. Other requests shall be referred toNaval Weapons Center, China Lake, CA93555-6001.

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Naval Air Warfare Center, Weapons Div,Code 4T42AOD, China Lake, CA ltr dtd 23Sep 1999

THIS PAGE IS UNCLASSIFIED

AD-B093 690 NWC TP 6539Part 2

Thermostructural Evaluation of FourInfrared Seeker Dome Materials

Part 2. Thermal andMechanical Properties

by

John R. KoenigSouthern Research Institute

for theOrdnance Systems Department

APRIL 1985

DTICELECTE

NAVAL WEAPONS CENTER •JUL 8 1985

CHINA LAKE, CA 93555-6001

S. 'B

4 Distributtor) authorized to U.S. Government

agencies onlyý test and evaluation, 30 May 1984.Other requests for this document shall be referredto the Naval Weapons Center.

Lj

C-5

4

- . - A .;

Naval Weapons CenterAN ACTIVITY OF THE NAVAL MATERIAL COMMAND

FOREWORD

This is the final report of work conducted at the Southern ResearchInstitute (SRI), Birmingham, Ala., during 1983 and 1984 under NavalWeapons Center (NWC) contract N60530-83-C-0031, as part of the MultimodeGuidance Program. This program is uider the direction of NAVSEA 62R,SEATASK 62R21003008150186.

In the interest of economy, this report is published in its originalform as submitted by SRI and does not follow the established NWC technicalpublication (TP) format. The report is published in the NWC TP series toensure accountability and retrievability of the data,

To reduce the size of this report (originally 318 pages), threeappendixes containing raw test data were omitted. These data aresummarized in the body of the report. Copies of these appendixes may beobtai:ed from the Naval Weapons Center, Attn: Don Gay, Code 3942, ChinaLake, California 93555-6001.

This report is published in two parts: Part 1 covers test andanalysis conducted at NWC; Part 2 herein covers thermal and structuralanalysis conducted at the Southern Research Institute under NWC contract.

Approved by Under authority ofC. L. SCHANIEL, ea• K. A. DICKERSONOrd:'~arw~e tiems De ,tmo t Capt., U.S. Navy

16 Aprii 1985 Commander

Released for publication byB. W. HAYST'chni7a Iireotor

NWC Technical Publication 6539, Part 2

Published by ......................... Technical Information DepartmentCollation.. ............................................ Cover, 84 leavesFirst Printing ............................................. 125 copies

DESTRUCTION NOTICE--Destrox by any method that mill prexenit disclosure of contents or

rcconstruction of the docoimnt.

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REPORT DOCUMENTATION PAGEIda REPORT SECMRITY CLASSý--CAT;ON 'b RESTRICTiVE MAR:.cNGS

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2 SSCATION AUTHORITY 3 D;STR1BUTION/AVA!.A8!,UTY OF REPORTN/ Statement B; test and evaluation;2n• L)'•C -SS!FiC•T,!O N; DOW 'N RA 'D~,14G SCH EDULE 30 May l1984N/A 4,4ldr C ,

"4 PERFORMiNG ORGAN'Z ,TION REPORT NUMBER(S) S %^orN'TO'RtNG ORGANPZAT:ON REPORT NUMBER(S)

SoRI-EAS-84-1096-5155-I-F NWC TP 6539, Part 26a NAME OF PERFORM.NG ORGANZATION Eb OF-ICE SYMB3OL 7

a NAN1ME "OF MONiTORiNG ORGANIZATION

Southern Restar.'h Institute ,if applicable)

Thermophysical [iv-_-ion N/A Naval Weapons Centerb< aiDRESS (Cry, State, aid ZIf Code) 7b ADDRESS (City, State, and ZIP Code)

Birmingham, AL China Lake, CA 93555-600132555-5305

Ba NAVE OF ,"UNDI\%G SPONSOR:NG Bb OFFICE SVMBC'' 9 PROCUREPM(ENT INSTRUMENT jDENTiFiCATiON NUMBER

OR GAVZA T ON (if applicablej NWC ContractNaval Weapons Center Code 3921 N60530-83-C-0031

68 ADDRESS (Ci, State and ZIPCooe) 10 SOURCE OF FUNDING NUMBERS

PROGRAM PRO.ECT TASK wORK ujNTChina Lake, CA 93555-6001 ELEMENT NO NO NO NO

A:- PE63318N S0186 21003 N/A-,.nclude Securty OClassification)

'THERMOSTRUCTURAL EVALUATION OF FOUR INFRARED SEEKER DOME MATERIALS.PART 2. THERMAL AND MECHANICAL PROPERTIES

'2 D4 OT.AL AUTHOR(S)John R. Koenig3,3a " OF PcOCRT '3b TIME COVERED 14 DATE Oi REPORT (Year. Month, Day) S PAGE COL•NTFinal FROM 1983 TO 1984 1985, April 158

'6 S: PEvE•TARY NOTATION

COSAT, CODES .18 SUBJFCT -ERMS (Continue on reverse if nPcessery and identify by blo'k number)E GROLP SUB-GROUP IR seeker dome materials -Dome thermostructural limits,[i- 04 04.Z Dome material properties Fractographic studies,17 Dome thermal properties - _(Contd. on back)

.9 ' GS-PA CT.Contnue on reverse if necessary and identify by blo<k number)

'U)' Four candidate IR seeker dome materials were evaluated in this study for theirthermal and mechanical properties. The materials evaluated included sapphire, spinel, zincsulfide, and zinc selenide. The mechanical properties evaluated were tension, compression,and flexure at ambient and elevated temperatures. The thermal properties evaluated werethermal expansion, thermal conductivity, and specific heat.

(U) This report is published in two parts. Part 1 covers test and analysis conducted, at the Naval Weapons Center. Part 2 herein covers thermal and structural analysis conducted

at the Southern Research Institute under NWC contract.

20 DSR3'7-ON A.JAiLABILITY OF ABSTRACT 21 A4S8 RACT SECURITY C-ASSIFCATiON-I ;%CASS-''EO3 NLM!TED C1 SAME AS RPT [OT1C uSERS UNCLASSIFIED

22a ..AM OF RESPONS.BLE .ND!V'DUAL 22b TELEPHONE (include Area Code) 722c OFFICE Sy&'Y 80LDon Gay A, 619-939-3341 NWC, Code 3942

DO FORM 1473, 84 VAR 83 ADR ed,tor' may be used unti eKha.sted SECURiTY CLASSIFICATION OF THIS PAGE

All other ed.,:o- are ý;bso ete UNCLASS IF I ED

UNCLASSIFIEDSECURITY CLASSIFICATION OF THIS PAGE

18. (Contd.)--Sapphire domes

Spinel domesZinc sulfide domesZinc selenide domes

Accesslon For

,ýTIS IT

"" stic TA)

' Diatribution/

-- : Av'4labillty Codas"' �-- AvAi11 and/or"1W -D it t Sp~ec al

UNCLASSIFIED

SECURITY CLASS;F:CAT;O\k OF -HiS PAGE

N"NWC TP 6539, Part 2

CONTENTS

Page

1.0 INTRODUCTION I

2.0 TEST MAI RICES 2

3.0 MATERIALS 4

4.C MECHANICAL PROPERTY TESTING OF BRITTLE MATERIALS 4

5.0 APPARATUSES AND PROCEDURES 7

5.1 Tension 75.2 Compression 95.3 Flexure 105.4 Thermal Conductivity 115.5 Thermal Expansion 145.6 Heat Capacity 165.7 Bulk Density 185.8 Ultrasonic Velocity 18

6.0 DATA AND DISCUSSION

6.1 Gravimetric Density 206.2 Ultrasonic Velocity 206.3 Flexure 21

6.3.1 Flexural Results for Sapphire 216.3.2 Flexural Results for Spinel 236.3.3 Flexural Results for Zinc Sulfide 236.3.4 Flexural Results for Zinc Selenide 24

6.4 Tension 24

6.4.1 Tensile Response of Sapphire 246.4.2 Tensile Response of Spinel 256.4.3 Tensile Response of Zinc Sulfide 256.4.4 Tensile Response of Zinc Selenide 26

6.5 Compression 26

6.5.1 Compressive Results for Sapphire 266.5.2 Compressive Results for Spinel 266.5.3 Compressive Results for Zinc Sulfioe 27"6.5.4 Compressive Results for Zinc Selenide 27

-. " iii

NWC TP 6539, Part 2

Page

6.6 Thermal Expansioc, 27

6.6.1 Thermal Expansion of Sapphire 27C,.6.2 Thermal Expansion of Spinel 286.6.3 Thermal Expansion of Zinc Sulfide 286.6.4 Thermal Expansion of Zinc Selenide 286.6.5 Comparison of Thermal Expansions 29

6.7 Heat Capacity of the Four Materials 29

6.8 Thermal Conductivity of Sapphire 30

6.9 Thermal Conductivity of Spinel 31

6.10 Thermal Conductivity of Zinc Sulfide (ZnS) 32

6.11 Thermal Conductivity of Zinc Selenide (ZnSe) 32

Appendix: Sensitivity Studies 155

REFERENCES 158

iv

2"-.

. . . . . . . . . . . ..-. .

. . . . . . . . .

NWC TP 6539, Part 2

LIST OF FIG Rr

Fiqcure Page

I Photograph of a Tensile Stress-Strain Facility 33

2 Schematic Arrangement of the Gas-Bearing Universals, Specimen

and Load Train 34

3 Schematic Arrangement of the Gas-Bearing Universals, Specimen

and Load Train 35

4 Tensile Specimen Configuration 36

5 Picture of the Compressive Facility with Gas Bearings and Optical

Strain Analyzer 37

6 Schematic Arrangemnent of Gas-Bearing Universals, Specimen and

Load Train 38

7 Small 5500 cF Graphite Resista,,ce Furnace 39

8 Compression Specimen Configuration 40

9 Schematic of High Temperature Flexural Apparatus 41

.0 Flexural Four-Point Loading Set-Up 42-II Schematic of Comparative Rod Thermal Conductivity Apparatus 43

12 Cross-section Schematic of an Assembled RIA Showing a Cylindrical

"Spec i men 44

, Radial Inflow Apparatus Specimen Holder and Specimen Configuration 45S14 Thermal Expansion Specimen 46

Ultrasonic Velocity-Measuring Apparatus Schematic 47

i6 Failure Surface of Sapphire Flexure Specimen F-10 (600) Showing

Typical Conchoidal Nature of Failure 48

17 Fracture Face of 0-" Oriented Flexure Specimen 49

18 Apparent Fracture Initiation Site for Specimen F-18 50

19 Flexural Modulus versus Temperature for Sapphire 51

20 Ultimate Flexural Strength versus Temperature for Sapphire 52

21 Voids in Spinel Flexural Specimen F-16 53

22 !racture Surface of Spinel Flexure Specimen F-13 54

"23 Flexural Modulus versus Temperature for Spinel 55

24 Ultimate Flexural Strength versus Temperatur?- for Spinel 56

V

1NWC TP 6539, Part 2

LIST OF FIGURES (Continued)

gure Page

25 Flexural Modulus versus Temperature for ZnS 57

26 Ultimate Flexural Strength versus Temperature for ZnS 58

27 Flexural Modulus versus Temperature for ZnSe 59

28 Ultimate Flexural Strength versus Temperature for ZnSe 60

29 Failure Surface (Head Failure) of Sapphire Tensile Specimen T-1 61

30 Fracture Surface of Sapphire Tensile Specimen T-2 62

Failure Initiatior- Site for Specimen Shown in Figure 30 63

32 Tensile Stress-Strain Curves for Sapphire Using Clip-on

Extensometers 64

33 Failure Surface of Spinel Tensile Specimen T-2 6534 Failure Surface of Spinel Tensile Specimen T-3 66

"Higher Magnification Views of Two Zones of the Spinel Tensile

Specimen T-3 Failure Surface 67

36 200X View of Fracture Surface on Spinel Tensile Specirnen T-3 68

37 Tensile Stress-Strain Curves fc- Spinil Specimens 69

38 Tensile Stress-Strain Response of Zinc Sulfide 70

39 Fracture Surface and Failure Initiation Site for ZnS Specimen T-1 71

40 Fracture Surface and Failure Initiation Site for ZnS Specimen T-2 72

41 Tensile St-ess-Strain Response for Zinc Selenide 73

42 Fracture Surface and Initiation Site for Zinc Selenide Tensile

Specimen T-2 7t,

43 10 and 5OX SEM Micrcgraphs of Zinc Selenide Tensile Fracture

Surface (Specimen T-4) 75

44 300 and 1500X SEM1 Micrographs of Zinc Selenide Tensile Fracture

Surface (Specimen T-4) 76

45 Compressive Modul; of Sapphire 77

a6 Average Compressive Modulus of Sapphire 78

47 Compressive Moduli of Spinel 79

48 Average Compressive Moduli of Spinel 80

49 Initial Compressive Elastic Modulus of ZnS 81

i~V i

N.- -"- -" v -- "-" ".-,

i 'r' TP 6539, Part 2

LIST OF FIGURES (Continued)

Figure Page

50 Average Compressive Moduli of ZnS 82'I Compressive Moduli of ZnSe 83

52 Average Compressive Modulus of ZnSe 84

53 Thermal Expansion of Sapphire - Specimens 1 and 2 85

54 Thermal Expansion of Sapphire - Specimens 3 and 4 86

55 Thermal Expansion of Spinel 87

56 Thermal Expansion of ZnS 88

5.57 Thermal Expansion of 7nSe 89

58 Composite Plot of Thermal Expansions 90

59 Enthalpy of Sapphire 91

60 Enthalpy of Spinel 92

61 Enthalpy of ZnS 9362 Enthalpy of ZnSe 94

63 Heat Capacity of ZnSe 95

64 Heat Capacity of ZnS 96

65 Heat Capacity of Sapphire 97

"66 Heat Capacity of Spinel 9867 Composite Plot of Heat Capacities 99

68 Uncorrected Thermal Conductivity of Sapphire iGO

69 Transmission Plot for 0.125-inch Sapphire Sample (30 °C -800 0C) 101

70 Transmission Plot for 0.125-inch Sapphire Sample (1000 0C -

"1400 °C) 102

71 Calculated Thermal Conductivity for Sapphire 103

72 Uncorrected Thermal Conductivity of Spinel 104

73 Transmission Plot for 0.1005-inch Spinel Sample (1000 -C -

1400 °C) 105

74 Transmission Plot for 0.1005-inch Spinel Sample (30 'C - 800 -C) 106

75 Calculated Thermal Conductivity of Spine! 107

76 Thermal Conductivity of ZnS 108

77 Thermal Conductivity of ZnSe 109

Peak Stressed Volume and Surface Area for

"Radome Discussed in Part 1. 156

.............................................-...................

Nt.WC TP 6539, Part 2

"LIST OF TABLES

TablP

1 Test Matrix for ZnS and ZnSe 110

2 Test Matrix for Spinel Ill

3 Test Matrix fc-r Sapphire 112

4 Four Point Flexure of Sapphire 113

5 Four Point Flexure of Spinel 114

6 Four Point Flexures of ZnS 115

7 Four Point Flexure of ZnSe 116

8 Tensile Pesults for Sapphire 117

9 Tensile Results for Spinel 118

10 Tensile Results for ZnS 119

11 Tensile Results for ZnSe 120

12 Initial Compressive Moduli of Sapphire (10' psi) 121

13 Initial Compressive Moduli of Spinel (106 psi) 122

"14 Initial Compressive Moduli of ZnS (106 psi) 123

15 Initial Compressive Moduli of ZnSe (106 psi) 124

16 Thermal Expansion of 60' Sapphire Measured in Quartz Dilatometer 12517 Thermal Expansion of 60 Sapphire Measured in Quartz Dilatometer 12618 Thermal Expansion of 60' Sdpphire Measured in Graphite Dilatometer 127

19 Thermal Expansion of 60 Sapphire Measured in Graphite Dilatometer 128

20 Thermal Expansion of 60 Sapphire Measured in Quartz Dilatometer 129

21 Thermal Expansion of 0' Sapphire Measured in Quartz Dilatometer 130

22 Thermal Expansion of 0' Sapphire Measured in Graphite Dilatometer 131

23 Thermal Expansion of 0' Sapphire Measured in Graphite Dilatometer 132

24 Thermal Expansion of Spinel Measured in Quartz Ditetolaleter 133

25 Thermal Expansion of Spinel Measured in Quartz Dilatometer 134

26 Thermal Expansion of Spinel Measured in Graphite Dilatometer 135

27 Thermal Expansion of Spinel Measured in Graphite Dilatometer 136

28 Thermal Expansion of Zinc Sulfide Measured in Quartz Dilatometer 137

29 Thermal Expansion of Zinc Sulfide Measured in Quartz Dilatometer 13829 Thra Expan......... io..... of ,• ,-,inc, SufdeMa ured inQarzlatometer 138

viii

, , .i-;. -;"- . :-":i " - " .' .- '- - .:T-.I $ -- _-.i ' - .I ' . I" : " ' : -I " / I " ' " " • . .

NWC TP G539, Part 2

LIST OF TABLES (Continued)

Table PaIe

31 Thermal Expansion of ZnSe Measured in Quartz Dilatometer 140

32 Enthalpy of Sapphire Measured in the Adiabatic Calorimeter 141

33 Enthaipy of Sapphire in Ice Calorimeter 142

34 Enthaipy of Spinel t-easured in the Adiabatic Calorimeter 143

35 Enthalpy of Spinel in Ice Calorimeter 144

36 Enthalpy of Zinc Sulfide tleasured in the Adiabatic Calorimeter 145

37 Enthalpy of Zinc Sulfide in Ice Calorimeter 146

38 Enthalpy of Zinc Selenide !¶easured in the Adiabatic Calorimeter 147

39 Enthalpy of Zinc Selenide in Ice Calorimeter 148

40 Sapphire Surmmary of Properties 149

41 Spinel Sumirary of Properties 150

42 Zinc Sulfide Summary of Properties 151

43 Zinc Selenide Summary of Properties 152a4 Comparison of Predicted Tensile Loads at Failure to Measured

Tensile and Flexural Strengths at 70' 153

45 Comparison of Properties of Four Optical Materials 154

A-1 Sensitivity Study Summarv 157

ix

"NWC TP 6539, Part 2

THERMAL AND MECHANICAL PROPERTIES OF

CANDIDATE OPTICAL MATERIALS FOR IR WINDOWS

1.0 INTRODUCTION

This is the final report of the effort conducted at Southern

Research for the Naval Weapons Center, China Lake, California under Contract

Number N60530-83-C-003l. The purpose of this program was to determine the

thermal and mechanical properties of several optical materials. There were

four materials evaluated in this study: Sapphire, Spinel, Zinc Selenide

(ZnSe) and Zinc Sulphide (ZnS).

The mechanical properties used in the evaluation include tension,

compression and flexure at room temperature and elevated temperatures. The

thermal properties used were thermal expansion, thermal conductivity, and

"specific heat. In addition to these properties, nondestructive measurements

(NDC) were made to aid in the interpretation of the data and fractographic

studies were made of the tested specimens to understand the results. The NDC

results provide a tool to judge typicality and variation in future materials.

Planned applications for IR seeker systems for the intermediate

and long term time frame, particularly for air to air systems, require sur-

viva] of the windows in more extreme aerodynamic heating conditions. This

requires the materials to survive more severe thermostructural loads which

exceed the capability of currently used optical materials. The materials

listed above were selected based on several criteria, including cost, optical

properties, rain erosion resistance, fabricability and, particularly, thermal

stress resistance. The -matrices selected for this program were designed to

"address, particularly, the thermal stress issue.

This report will cover the test matrices used for the charac-

terization of these materials, a discussion of some of the parameters to be

considered when conducting tests on these materials, the apparatuses and

"procedures used, the experimental results obtained and a comparison and

summary of the materials. Some of the discussion of the data reduction

techniques will be integrated with the data reduction.

NWC TP 6539, Part 2

2.0 TEST MATRICES

The test matrices used for the eval,_•tion of these materials are

presented in Tables 1 through 3.* They were designed to obtain sufficient in-

formation for comparative design studies and screening of the material with

emphasis on those properties which are anticipated to be most critical for a

thermostructural environment. The matrices for the ZnS and ZnSe are different

from the matrices for the spinel and sapphire due to anticipated differences

in the temperature limitations of the materials. These are somewhat different

from the planned matrices as shown in Tables 3 and 4 cue to the specimens

received and decisions mAde during the course of the testing to optimize the

data set.

The objective of a screening matrix is to identify promising can-

didate materiels for a given application with a minimum expenditure. This is

more straight forward in this program in that the driving load, thermal stress,

had been defined apriori. It is still somewhat of a challenge to define a

matrix which addresses the critical intrinsic properties with minimal expendi-

ture of resources.

The thermal stress resistance was investigated using thermal expan-

sion, thermal conductivity, specific heat, compression, tcqsion and flexure.

Sensitivity studies conducted on this class of materials (see Appendix) show

the critical properties which control the thermal stress response for the

general heating rates and geometries of interest here to be the thermal

expansion, tensile strength or strain to failure and the ratio of the high

temFrrature compressive modulus to low temperature tensile modulus. The

other properties measured have a second order effect on the thermal stress

response, but are important for cther critical responses. For example, the

thermal conductivity and specific heat, in adlition to being necessary to

predict the Lhermal fields for thermal stress prediction, also affect in

depth heating of other system, components and with the thermal expansion, aid

in thermal deformation compatibility design with the collar structure (the

intermediate body between the missile main body and the dome).

*All tables and figures are located at the end of the report.

2

....................................

NWC TP 6539, Part 2

The tensile tests conducted on these materials, as seen in

Tables 1 through 3, were limited to room temperature only. This was done

to limit the expenditure on fabricating these relatively complex specimens.

As will be noted later, this was perhaps an unfortunate decision. It was

also decided to machine these specimens to a fixed surface finish which

would be matched on a dedicated set of flexure specimens (discussed below).

The rest of the flexure specimens would be finished to the equivalent

level as anticipated for IR domes. The effect of surface finish (for the

spinel and sapphire) was to be accounted for by correlation between the

flexure and tensile specimens. The temperature trend was also to be

obtained from the flexure data. Five tensile tests were planned at room

temperature, sufficient to obtain a reasonable estimate of the mean.

Three compressive tests were conducted in a nondestructive

mode (loading to low stresses in the elastic response regime) at a series

of temperatures up to the limit of the material. Tests were conducted at

intervals of 200 'F. This provided a good estimate of the compressive

elastic modulus as a function of temperature. It was not deemed important

to obtain the compressive strength for these materials as compressive

failure is unlikely. Poisson's ratio was measured at room temperature on

the compressive specimens.

The flexure tests were conducted at a series of temperaturesproviding both the flexural modulus and strength. In the case of the

sapphire additional tests were conducted at room temperature and 2000

degrees to evaluate the response at the 60 degree orientation. For both

the spinel and sapphire five tests were conducted at room temperature with

the surface ground to the same finish as the tensile specimens. In each

case some latitude was taken with the number of replications at temperature

to optimize the data set.

The thermal expansion was measured up to the material limit.

The expansion of the sapphire was measured in both the 0 and 60 degree

orientation. The specific heat and thermal conductivity were both measured

up to the material limit. As will be discussed later the conductivity was

measured at different temperature gradients to inspect how to appropriately

model these materials where a significant radiation component is present.

3

NWC TP 5539, Part 2

The nondestructive tests consisted of measuring the bulk density

and sonic velocity of each specimen plus a careful visual examination. The

surface roughness was inspected using optical and SEM microscopy. SEM micro-

scopy was used for the fractography.

3.0 MATERIALS

The specimens were all received from the fabricators in final

machined condition. Each specimen was numbered by the fabricator and that

identification was maintained through the testing. There were some differ-

ences in the number of specimens received of various orientations and

finishes between what was received and what was anticipated as discussed

herein and the matrices were adjusted accordingly.

The ZnS and ZnSe were fabricated by CVD, Inc. of Woburn,

Massachusetts. Both are isotropic in nature and transparent with an amber

S.- shade. They are both fabricated using chemical vapor deposition.

The spinel (MgAI 2O) was fabricated by Coors Porcelain of

Golden, Colorado using a hot pressing technique and the sapphire was made

by growing a single crystal boule by Crystal Systems, Inc. The spinel has

a cubic structure and is isotropic while the sapphire has a hexagonal

structure.

S•4.0 MECHANICAL PROPERTY TESTING OF BRITTLE MATERIALS

The measurement of basic mechanical properties of brittle

materials, such as tensile strength, using the methods which have been

developed for ductile materials, is typically very unsatisfactory. There

is typically a wide scatter in results when apparently identical tests are

conducted on identical specimens of the same material. Some of the varia-

tion is caused by the inherent variability in the properties of the material,

-* which is a result of the sensitivity of the material to local stress concen-

trations, caused by flaws, voids, microcracks, inclusions and other defects

in the material. Part of the variability is caused by test technique due

to the sensitivity of brittle materials to local stress concentrations or

S-paraitic stresses.

4

*- fl • ". r . r -. - .-• . -. • • --- -. . -•d -flt l T * i .a-. . .-- .. .- .-- ., , -.. V . - --- .

NNC TP 6539, Part 2

Typically in the mechanical property testing of materials,

there are many effects which leao to disturbances either in what would

otherwise be a uniform or at least a simple distribution of stress across

the gage section of the test specimen, or in the magnitude of the loads

actually applied to the test section. Some of these sources of stress

variations in the tensile test are tolerances in specimen and load train

dimensions, eccentricities in the specimen and load train, kinks in the

load train, friction in the universal joints, extraneous crosshead motion

of the test machine, failure to apply load along theŽ centerline, as well

as many others. They result from the inability to carry out every step of

the test perfectly and from the practical requirement that tolerances must

be applied to every specimen, every piece of hardware and every activity

connected with the test. Some of these variations are evident, such as

the difficulty of aligning the applied load perfectly through the centroid

of the cross-section of the specimen, or the difficulty of eliminating

friction at ball joints in the load train, or the difficulty of designing

and manufacturing a specimen such that loads can be applied without stress

concentrations occurring in the gage. All of these effects, however, lead

to locaized stresses which are different from the nominal stress determined

from the load at failure, the geometry of the failed cross-section, the

specimen geometry, and assumptions of a uniform homogeneous material having

simple elastic stress-strain properties. Since the material is brittle it

will fail, generally speaking, when the peak stress reaches the limiting

stress of the material at some particular location, regardless of how

localized this location might be. A ductile material will yield locally

and will fail only when the average stress over a significant portion of

the cross-section reaches the limiting strength of the material.

There have been two btoad approaches taken in attempts to

resolve this difficulty. One method is to select the test technique for

its relative simplicity and to accept a complex stress distribution within

the specimen. Reliance is then placed on refined stress analysis to deter-

mine the maximum stresses and, hence, material strength from the measured

loads at failure. This approach may or may not be low in cost depending on

the specimen configuration which is used. Frequently a complex specimen,

such as the theta specimen, which is designed to provide areas of uniform

5

• , .- - - " - . -. .- • -. ".. - , " - " - - " • " ' " - • . • . • ,• . - ' - " . .

NWC TP 6539, Part 2

stress, is used to minimize the stress analysis problem by substitutingspecimens which are expensive to fabricate, although the test technique

is simple. Alternatively, simple low cost specimens may be used with

complete dependence on stress analysis to determine maximum stresses.

The latter type of test is frequently used for comparative data on large

numbers of specimens.

The flexural test used in this program is an example of such

"a test. In addition to its dependence on stress analysis, this approach

involves a stress gradient at the location of fracture, so that a simple

uniaxial strength is not determined. The complex stress state also

inhibits the study of basic phenomena such as volume effects, rate

dependence, or tensile stress-strain response since the flexural response

is a combination of both tension and compression. This was understood

when the matrices for this program were developed and the objective of the

effort was to understand this data by correlation to the tensile data.

As will be discussed, there was an additional problem in that the specimens

received did not have a "break" at the corners (as is standard practice),

the effect of which will be discussed later.

The other approach is to use the type of test that will producesimple stress distributions which can be readily and accurately determined

from the measured loads and geometry, and to concentrate on refinement of

technique, apparatus and specimen configuration in order to minimize the-2. effects noted earlier. This is the approach taken for the gas bearing

tensile tests reported herein and discussed in the next section. Some of

the more obvious advantages of this test are:

1. Homogeneous stress field

2. Well defined volume urder peak stress

3. Well defined surface under peak stress

4. Sufficient volume of uniform strain to allow

good strain measurements

"5. Unique fracture surface6. Ready extension of the technique to elevated

tempera tures

"7. Strain or stress rate control

6

NI-C TP 6539, Part 2

5.0 APPARATUSES AND PROCEDURES

This section of the report presents discussions of the equip-

ment and methods used for the evaluation of the properties determined in

this program. It also shows the specimen configurations selected for eachdetermination and gives the conditions under which the tests were conducted.

5.1 Tension

The tensile evaluations were performed in a gas bearing tensilefacility. This facility utilizes gas bearing universals in the load linkage

to prevent the introduction of unknown bending moments in the load train

from the crosshead motion or eccentricity and allows monitoring cf the

straightness of the load train.

A typical tensile facility is shown in Figure 1 and schemati-

cally in Figures 2 and 3. The primary components ar- the gas bearings, theload frame, the mechanical drive system, the 5500 degree furnace (not used

in this effort), the optical strain analyzers and associated instrumentation

for measurement of load and strain. The load capacity is 15,000 pounds.

The load trame and mechanical drive system are similar to thoseof many good systems. The upper crosshead is positioned by a small electric

motor connected to a precision screw jack. This crosshead is stationary

during loading and is moved only during assembly of the load train. The

lower crosshead is used to apply the load to the specimen through a precision

screw jack chain driven by a variable speed motor and gear reducer.

Nonuniaxial loading, and therefore bending stresses, may be

introduced in tensile specimens not only from (1) misalignment of the load

train at the attachment to the crossheads, but also from (2) eccentricity

or nonstraightness within the load train, (3) unbalance of the load train,

and (4) external forces applied to the load train by such items as electrical

leads or clip-on extensoneters. Although the bending moments f-om these

sources may Feem relatively slight, the resulting stresses can c, quite

significant in the eval,,ation of extremely sensitive brittle materials.

7

••-<-..-.: • .. -2 •. . L,: -:.. • - -. :.'.2 L :. - " -. • • .::• L :. . i

NWC TP 6539, Part 2

Elimination of nonuniaxial loading at the point of attachment of

the load train to the crossheads has been confirmed by measuring the torque

required to produce initial motion within the system with the bearings in

"operation under 5000 pounds load. This torque was found to be a maximum of

"0.0066 inch-pounds. The stress that could be induced in a specimen due to

this bending moment is 0.16 psi.

Emphasis in tne design of the load train is placed on (1) large

length to diameter ratios at each connection, (2) ciose sliding fits oF allmating surfaces (3) elimination of threaded connections, (4) the use of pinconnections wherever possible and (5) increasing the size of components to

permit precise machining of all mating surfaces. All members are machined

"true and concentric to within 0.0005 inches, and the entire load train is

checked regularly with an alignment bar to check overall alignment.

Strain measurements were made using an optical extensometertracking the elongation between flags mounted on both sides of the specimen.

The signals from both sides are averaged in reporting the strain values. Onsome (typically three) of the specimens of each material, strain gages were

a~so used. Load was measured with a connercial flat load cell. The cell

received a constant dc voltage input from a power supply and transmitted a

millivolt signal (directly proportional to load) to an x-y recorder. Simul-

taneously, the optica' strain analyzer measured the axial strain and trans-

mitted a millivolt signal to the recorder. Similar plots were made using the

output of the strain gages. Thus, continuous plots of stress-strain were

recorded and are presented as the raw data in the appendix of this report.

The specimen used for the tensile tests for this program is

shown in Figure 4. The spinel specimens were slightly modified for a total

length of 4.5 inches. Both the zinc sulfide and zinc selenide specimens had

a gage diameter of 0.250 inches.

.'-.

IWC TP 6539, Part 2

5.2 Compression

The compressive evaluations were performed in a gas bearing

compressive apparatus of similar design to the tensile apparatus described

above. The compressive facility is shown in a photograph in Figure 5 and

schematically in Figure 6. It consisted primarily of a load frame, gas

bearings, load train, 50 ton screw jack, variable speed mechanical drive

system, strain analyzers,5500 'F furnace, and associated instrumentation

for the measurement of load and strain.

Gas bearings were installed at each end of the .load train to

permit precise alignment of the load train to the specimen. The upper

bearing was spherical on a radius of 6.5 incheswhich is the distance from

the top of the specimen to the bearing surface. The lower bearing is flatallowing transverse alignment of the load train. The gas bearings are

floated only during the initial portion of the loading. The instrumentation

is similar to that for the tensile facility.

A sketch of the 5500 'F furnace is shown in Figure 7. The furnace

consists of a resistively heated graphite element insulated from a water

cooled shell by thermatomic carbon. The furnace and specimen were purged

in helium to provide an inert atmosphere. Temperatures were monitored with

thermocouples at lower temperatures and with optical pyrometers at higher

temperatures.

In order to obtain a good definition of the modulus-temperature

relationship with only three specimens per materialthe specimens were cycled

through load-unload sequences at temperature increments of 200 'F. This is

referred to as nondestructive mechanicals (NDM). At room temperature both

strain gages end optical techniques were used. Strain gages monitored both

the axial and lateral strains allowing measurement of the Poisson's ratio

as well as the Young's modulus. The specimen used for the compressive

evaluations is shown ii Figure 8.

S9

NWC TP 6539, Part 2

S5.3 Flexure

Beam flexural evaluatios were performed in the flexurai

apparatus shown in Figure 9 which consists of a load frame, load cell,

load train, graphite resistance furnace, deflection measurement system

and associated equipment for continuous measurement of load and deflec-

tion. Load was applied to the specimen from the lower end of the load

train, and load measurements are made by the load cell at the upper end.

As the load is applied to the specimen~midpoint deflection of the specimen

is measured by means of a rod contacting the specimen midpoint and extend-

ing down to a differential transformer. The differential transformer is

supported by a tube that attaches tu the support bar eliminating load

train motion from the deflection measurement. A new molybdenum loading

system was designed and fabricated for this effort.

From the plot of load versus midpoint deflection, the values

"of modulus of rupture and flexural modulus were measured. The ultimate

strength is calculated from the equation:S~mCSS = ---

which simplifies to

S PLbh

for a specimen with a rectangular cross-section employing the third span

loading method, and where fracture occurs within the middle one-third of

the specimeo span length. The four point loading system is shown schemati-

cally in Figure 10. In these equations:

S = modulus of rupture

P = maximum applied load

L = span length

b = width of specimen

h = height of the specimen

in = moment

c = length over which moment is measured

I = moment of inertia

10

..-.-..-. . ......-.....4-.. .--. " . f-.•"• .'- : ... .... .... .- _• _,S • _-.-:•_ -, "_.-.• •i .•3 ' -, . . _ a .• . ,•. .' ' -i•i -_ ,. - . - -

NWC TP 6539, Part2

The initial modulus in flexure was calculated from the equation:

-- 6P [a3/3 + ac/2 (a j C/41Ef 6 bh3

where

E = elastic modulus in flexure

P/3 = ratio of load to corrected midpoint deflection at any point

along the elastic portion of the curve

a and c = distances between the supports and loading points

The above equation neglects :he deformation due to shear and

assumes that the neutral axis coincides with the center of the cross-section.

5.4 Thermal Conductivity

The apparatus used for the evaluation oi the thermal conductivity

of these materials through 1800 'F is known as the comparative rod apparatus

"(CRA). The CRA compares the conductivity of the specimen being characterized

to the known conductivity of a refererce piece. Several typ,s of references

are available and their conductivities are traceable to NBS data or other

re.iablp sources. In this effort references of Pyroceram and slipcast fused

siica were used.

The CRA consists of a series of cylindrical pieces stacked in a

vertical column as illustrated in Figure 11. The specimen and reference

pieces are placed in the order reference-specimen-reference. Above the top

reference is an electric heater that serves as the heat source for the experi-

ment. AlSiMag insulators are placed above the heater and a steel rod forms

the top of the column, receiving a compaction weight through a steel ball.

Below the bottom reference is another electric heater or irsulator, another

steel rod, and a cooling sink, if required. The entire column is supported

upon a steel ball for elimination of lateral forces that could deform the

structure.

• .--.-- .'-. -. '--'°-'--'-. -.-. '.....- -.- .- .-. ..-.-- .- ..-. . . ..-.- - .. . .- ... . .- .-.. ... . L 1.'i...L i . 1'

NWC TP 6539, Part 2

in assembling the apparatus, a large annular shell of alunminum

or transite is moved down around the stacked pieces. The central core of

the shell is wound with five electric coils which are guard heaters, ea-h

separately controlled to match the temperature gradient through the stacked

column, thereby controlling radial heat losses.

"The annular space between the central core and the stacked

column is filled with diatomaceous earth, thermatomic carbon, or other

insulating material selected to be compatible with the specimen. The entire

shell is also filled with insulation.

Thermocouples are used to measure temperatures at all key points

in the apparatus, including typically three points in the references and

specimens, two points in the upper and lower guards, and one point in the

middle guard.

For specimens with a conductivity of greater than 10 Btu-in./hr-

ft -°F, the temperature gradient through the column is considered to be linear

and the radial heat losses to be negligible. The calculations are made in a

straightforward manner from Fourier's equation for one-dimensional heat flow:A t k/l

where q" = heat flow through the material

At = temperature drop across the gage section

k = conductivity of the piece

1 = gage length of the piece

The heat flow is calculated for the reference pieces directly

since their conductivities are known and the temperature draps and gage

'lengths have been measured. It is then solved for the conductivity of the

specimen using the arithmetic average of the q" of the upper and lower

"references.

The radial inflow apparatus (RIA) was used to measure the thermal

conductivity of the spinel and sapphire specimens from 1500 to up to 5500 'F.

In this apparatus a water calorimeter located at the centerline of the specimen

removes heat that flows inward from an external heat source. The heat source

12

..-.. . .

NWC TP 6539, Part 2

is a high temperature furnace, into which the entire apparatus is placed.

The water flow rate and the temperature rise give a direct measure of the

heat flow through the specimen per unit time. Temperature measurements at

two radial locations in each of the four specimen parts give the temperature

drop across the specimen. These data enable the calkiilation of the thermal

conductivity of the specimen.

A completely assembled RIA is shown schematically in Figure 12.

In this figure a cylindrical specimen is shown rather than the four piece

specimen used in this program. Figure 13 shows at, assembled four piece

specimen. Referring to Figure 12, the calorimeter water enters at 32 'F at

the bottom and passes up through the insulation, the specimen, and more

insulation, leaving the apparatus at the top. Two thermocouples placed 1/2inch apart measure the temperature rise in the water stream as it passes

through the gage secti.-n of the specimen. A flowmeter in the external water

circuit measures the flow rate, which can be adjusted by a control valve.

Vertical sight tubes are run down through the upper insulation material

and aligned witn holes in the specimen, so that thermocouple or optical pyro-

meter readings can be taken of the specimen temperature. Vertical holes are

drilled to the center of the specimen near the furnace side to determine the

high temperatureand near the calorimeter side to determine the low temperature.

The apparatus is assembled on thi Nater calorimeter tube by

sliding cylindrical pieces down into positiotv. The lower insulating pieces

are graphite tubes filled with thermator~ic carbon. The specimen holder is

also a graphite tube, but of a slightly smaller diameter, such that it fits

snugly into the lower insulating tube. The uoper insulation piece is assembled

with their vertical sight tubes in their --e--ise positions and thermatomic

packed around them. The upper insulation oiece fits snugly around the

"specimren holder so that the assembly is F:,>ically stable and properly

aligned. The position of the specimen holder is adjusted vertically so that

the two thermocouples in the calorimeter are !paced equally above and below

tne center of the specimen. A radial hole in the specimen holder tube is

aligned with an optical port ,. the side of the furnace when the apparatus

1is inserted into the furnace anI secured in place.

13

S " " = • -" "• := " . -. .- ---- . -.• " .i - I ... • , - -" ,- .:< 'Z ' 2,,- •o ' .:.-" - "._ -.

NrC TP 6539, Part 2

To perform an evaluation, the specimens are assembled around

the calorimeter, and the unit is installed in the furnace with the sight

tubes and optical port properly aligned. Thermocouples are inserted into

the sight tubes for the initial temperature measurement. The helium purge,

calorimeter water flow, and power to the furnace are then turned on. The

first temperature check is performed at approximately 1500 IF, which is

made with thermocouples. When the desired teriperature is achieved, the

thermocouple readings and water flow are recorded.

For higher temperatures, the thermocouples are removed and the

voltage to the furnace is adjusted upward. When the desired temperature is

achieved, the thermocouple readings and water flow are recorded.

Specidl modifications of this technique had to be made to

properly model the radiation effects. This was due to the material being

transmissive to the near infrared. The specimens were machined down to a

thickness of 0.25 inches and placed between two strips of graphite which

contained the holes for temperature measurement. The inner packing around

the calorimeter was varied to provide different temperature drops across

the specimen. The reduction of these data is discussed with the data

"presentation.

5.5 Thermal Expansion

Thermal expansion measurements were made using quartz tube

dilatometers modified from the Bureau of Standards design for measurements

up to 1800 °F. Improvements have been made to prevent lateral movement of

the quartz tube, thus eliminating possible erroneous readings.

14

NWC TP 6539, Part 2

The specimen was placed in a quartz tube that is firmly

secured to the body of the apparatus, which is mounted on a work bench.

A second quartz tube of slightly smaller diameter was inserted into the

outer tube such that it rests on the specimen end. A quartz rod that is

free to move vertically was then placed into the apparatus such that one

end is in contact with the dial gage piston. The body of the dial gage

was firmly attached to the apparatus. Any expansion or contraction of

the specimen is transferred through the inner quartz tube, the quartz

push rod, ana the dial gage piston to registe a displacement on the

gage. The quartz tube and specimen are located within a cylindrical

electrical heater and can be heated to 1800 °F in the apparatus. The

dial gage is calibrated in 0.0001 incn displacements and has an accuracy

of ±0.0001 inch at any point in its range (0-0.5 inch).

The use of quartz for both the fixed and movable parts of

the apparatus eliminates any difference in expansion rates and allows the

apparatus to record only the expansion or contraction of the specimen. The

recorded raw data are then corrected based on calibration data for that

dilatometer developed from regular calibration runs on traceable standards.

The specimen used for this program is illustrated in Figure 14.

For temperatures up to the maximum use temperature of thesapphire and spinelgraphite dilatometers were used which are capable of

temperatures up to 5500 °F. The graphite dilatometers used for this effort

consist of a graphite tube into which the specimen is placed and a graphite

pushrod which is in contact with both the specimen and the precision dial

gage. The entire assembly is placed in a furnace capable of elevating the

temperature of the specimen to 5500 OF. Temperature readings are made with

Chromel-Alumel thermocouples up to 2000 OF and with an optical pyrometers

through sight glasses in the furnace at higher temperatures. The valuesfrom the dial gage readings as a function of temperature, corrected for

the calibration of the dilatometer, are plotted to provide the thermal

expansion curve.

15

S.. .. . . . . .. . . . . . . . . . . . ... - o - .. . .. _.. -.. -

NWC TP 6539, Part 2

5.6 Heat Capacity

The heat capacity to 1000 OF was determined from data

obtained in an adiabatic calorimeter. in this apparatus the heated

specimen was dropped into a thermally guarded, calibrated cup, and the

enthalpy is measured as a function of the increase in temperature of the

cup. The heat capacity is the slope of the enthalpy-temperature curve.

A tubular furndce was used to bring the specimen to tempera-

ture. The furnace pivots over the cup allowing the unit also to be used

with a cold box for temperatures down to -300 OF. When the furnace is in

place and the desired temperature is reached, the specimen is released

from a suspension assembly which is triggered externally. Thermocouples

are used to measure the specimen temperature.

Specimens of the material were heated to the desired tempera-

ture, dnd following a stabilization period, are dropped into the calorimeter

cup. Adiabatic conditions are maintained during each run by manually adjust-

ing the cup guard bath temperature.

The covered cup of the calorimeter is approximately 2.5 inches

diameter by 2 inches deep. Three thermocouple wells are located in the

bottom wall of the cup. The cup is mounted on cork supports, which rest in

a silver-plated copper jacket. The jacket is immersed in a bath of ethylene

glycol which is maintained at the temperature of the cup by means of a

heater and copper cooling coils inmnersed in the liquid. A double-bladed

stirrer maintains uniform bath temperature.

In the calorimeter six copper-constantan thermocouples, differen-

Stially connected between calorimeter cup and jacket, indicate temperature

difference between the cup and bath. The six thermocouples allow a difference

o' 0.03 OF to be detected. This difference is maintained to within 0.15 0F.F •uring the run, absolute temperature measurements of the cup are determined

by means oT the three thermocouple junctions, series-connected, in the bottom

of the calorimeter cup.

16

7 - - 7 7

NWC TP 6539, Part 2

The enthalpy of tho specimen at any initial temperature is

calculated from the equation:

--h = K/Ws(t2 - ti)

where h = enthalpy above t 2

K = calorimeter constant, 0.2654 Btu/ 0 F

WS = sample weight in lbs

t -- initial cup temperature in 'F

t2 = final cup temperature in OF

The calorimeter constant of 0.2654 Btu/OF was determined by measuring the

enthalpy of an electrolytic copper specimen of known specific heat. The

enthalpy is referred to a common base temperature of 85 OF using linearinterpolation. The enthalpy-temperature curve established is used to

determine heat capacity (specific heat) by measuring its slope at different

temperatures. This is done both graphically and by analytical methods.

The accuracy of the apparatus has been confirmed by measuringthe enthalpy of sapphire (SRM 734 from NBS) and other standard specimens.

The results of the comparison on sapphire and other data indicate that the

overall uncertainty of the apparatus is ±3 percent.

The ;,eat capacity of the spinel and sapphire were measured up

to their use Lemperature using an ice calorimeter which employs the drop

technique in which the specimen is heated in a furnace and then dropped

irto the ice calorimeter. The calorimeter contains a cup surrounded by a

frozen ice mantle. Water at an inlet temperature of 32 'F is circulated

through an annulus surrounding the mantle in order to absorb heat leak

'rom the surroundings. The entire system is insulated with glass wool.

'The enthalpy of the specimen is sensed as a change in volume of the water

ice ystem of the calorimeter as the ice melts. The annulus containing the

flooded ice mantle communicates with the atmosphere through a mercury

column in order that the change in volume can be read directly in a burette.

17

... .. .. ..

............. ** ..m..t..¾..-A -

NWC TP 6539, Part 2

The specimen is placed in either a graphite or stainless steel

basket and heated in the furnace in a controlled atmosphere such as Helium.

The specimen and basket are dropped into the calorimeter and the volume

change due to the melting ice is measured. The flutter valve immediately

above the cup and the diaphragm valve immediately below the furnace are

major features of the apparatus since the first blocks off radiation gains

from the specimen up to the drop tube, and the second blocks radiation gains

from the furnace down the drop tube just prior to dropping. The volume

changes due to the baskets are measured and correction curves are established.

Separate basket calibration minimizes the radiation error accompanying drop

techniques.

The heat necessary to melt enough ice to cause a volume change

of 1 cc has been estiblished by NBS at 3.487 BTU. The correction of the

basket is subtracted from the measured mercury displacement and the result

used to calculate specimen en~halpy above 32 'F. The heat capacity, which is

by definition the slope of the enthalpy curve, is determined both graphically

and analytically.

5.7 Bulk Density

The bulk density of the specimens was measured on the regular

specimens (all but the tensile and compressive specimens) by gravimetric

techniques. The specimens were measured with micrometers and weighed on d

Mettler balance. The reported density is simply the mass, in grams, divided

by the calculated volume in cubic centimeters.

5.8 Ultrasonic Velocity

The ultrasonic velocity was measured on each of the specimens

in the direction of test. The measurement was made using a through trans-

mission technique. The setup is shown schematically in Figure 15.

18

NWC TP 6539, Part 2

The basic apparatuses used for measuring ultrasonic velocity

were a Sperry UM 721 Reflectoscope and a Tektronix oscilloscope. In using

the through-transmnission, elapsed-time technique for measuring velocity, a

short pulse of longitudinal mode sound was transmitted through the specimen.

An electrical pulse from the pulse generator was applied to the crystal in

the transducer. The pulse generated by the transducer was transmitted

through a short delay line and inserted into the specimen. The time of

insertion of the leading edge of ths sound beam was the reference point

on the time base of the oscilloscope which was "~~as a high speed stop

I watch. When the leading edge of this pulse of F.iergy reaches the second

transducer it was displayed on an oscilloscope. The difference between the

entrance and exit times was used with the specimen length to calculate the

sonic velocity.

S 19

NWC TP 6539, Part 2

6.0 DATA AND DISCUSSION

6.1 Gravimetric Density

Tne gravimetric density was measured on each of the mechanical

and thermal specimens with the exception of the tensile and compressive

specimens. The results are given on each of the mechanical data tables.

The average densities measured were:

"Sapphire - 3.97 gms/cý;

Spinel - 3.58 gms/cc

ZnSe - 5.24 gms/cc

ZnS - 4.08 gms/cc

all of which are close to the anticipated value for theoretically dense

material

6.2 Ultrasonic Velocity

The ultrasonic velocity was measured on all specimens tested,

the results given in the data tables. The average ultrasonic velocity for

each material is

Flex Specimens Tensile Specimens

Sapphire 600 0.4081 in./iisec 0.407 in./k'sec

.3apphire 0' 0.4375 in./psec

Spinel 0.3837 in./psec 0.352

ZnSe 0.1741 in./psec 0.174

ZnS 0.2121 in./ijsec 0.211

Note the distinctive lower velocity of the 600 sapphire specimens.

These data can be used, along with the density valuesto

calculate a sonic modulus for each material. The average values of sonic

modulus for the four materials, based on the velocity vaiues measured on

the tensile specimens are:

20

-. .'

NWC TP 6539, Part 2

Sapphire 61.9 x 101 psi (47.2 x 106 psi)

Spinel 41.7 x 1D6 psi (30.1 x 1 0 1 psi)

ZnS 17.1 x 10' psi ( 9.1 x 106 psi)

ZnSe 14.9 x 106 psi (13.2 x 106 psi)

The values shown are the thin rod modulus. Those values in parentheses are

are calculated according to:

v2 (I +(,o) (1 2'aEsonic = 2 (I -V)

where • is density, v is velocity, and ') is the Poisson ratio.

6.3 Flexure

The flexural tests were conducted on each material with the

surfaces mcintained as received. Care was taken to avoid contact with this

surface prior to testing. All handling was done with cloves. As mentioned

earlier, there was no definition of "breaks" in the finishing of the corners

of the ternsile surface. This should be standard practice in the testing of

brittle materials but was not called out on the specimen drawings. This will

tend togive lower ultimate flexural strength values than would otherwise be

obtained. The trends as a function of temperature will still be valid if the

modes do not change. This is not necessarily the case for these materials.

6.3.1 Flexural Results for Sapphire

The results of the flexural tests on the sapphire specimenc dr-e

given in Table 4. The first- five 70°F specimens were the zero-de-eee specimens

with the polished finish. The second five 70 F specimens had the 60/40 finish.

There is no significant difference in either the density and sonic velocity

bctw:een the two sets. As expected there was ailso no significant difference

in the measured flexural modulus. The strength showed a dramatic difference.

The averagr- of the polished finished specimens was 130,151 psi wile those

with the 0/140 finish had an average strength of 7'3,567 psi.

21

NWC TP 6539, Part 2

The next five 70 IF specimens were oriented 600 to the first

ten 70 OF specimens. The flexural moduli were much iower (52.5 versus 64.8x 106 psi). This is also reflected in the ultrasonic velocities (0.409

versus 0.438 inches/psec). The flexural strengths of these specimens was

lower than either of the 00 specimens despite the polished finish which was

equivalent to the first set. The average was 73,490 psi. The average ,modulus

was 52.47 x 106 psi, significantly lower than the 64.8 average of the first

two sets (00 orientation). The failure surfaces of these 600 specimens was

distinctly different from the 0Q specimens. A typical example of the 600

failure is shown in Figure 16 and has a conchoidal nature.

The failure surfaces on the 00 specimens are distinctly different

as seen in Figure 17, the fracture tracking cleavage planes in a step-wise

fashion.

The strength (and moduli) of the zero-degree-oriented specimens

are lower at 20000 and continuously decrease in value as a function of tem-

,-_--rature. Specimen F-18 at 2000 OF had a dramatically lower value. The

fracture initiation site is shown in Figure 18.

The F0° specimens tested at 2000 OF showed a larger decrease instrength (45 percent of room temperature values) than the 00 specimens (81

percent of room temperature,ignoring F-18). The mean value was 33,223 psi,

considerably weaxer than even the 3000 OF 00 specimens.

The trend.of the flexural moduli as a function of temperatureare shown on Figure 19. The data are relatively well grouped and showed

consistent trends. Figure 20 shows the strength as a function of temperature.

Again a consistent trend is seen although, as expected, the coefficiehT of

variation is much higher. Also, the coefficient of variation of the 9rounrd

specimens is higher (20 percent) than that of the polished specimens. F-18

is anomalously low, having a value in the range of the 600 -9necimens.

22

.- i . . - . ' -......-.-. ..... ...-.- • .-. • -. - .;. . , - - • •. .. . - -_. -..

NWC TP 6539, Part 2

6.3.2 Flexural Results for Spinel

The results of the flexural tests on spinel are shown on Table 5.

No distinction was seen between the rground" and "polished': specimens so that

these values are lumped in the 70 0F data set. The mean strenqth at 70 OF was

13460 psi and the flexural modulus was 40.2 x 106 psi. Again recall that the

corners were not "broken" on these specimens. The apparent reason for the

lack of distinction between the degrees of polish is that there was porosity

in the parts which was larger than the scratches from the grinding or polish-

ing process. An example of this is seen in Figure 21. A typical fracture

surface is shown in Figure 22 which shows the grain size, presence of voids,

and suspected initiatijn site which is, as anticipated, at a corner. Note

also that the failure appears to propagate between, rather than through,

grains.

Several specimens had chips on one surface. These were oriented

so that the chips were on the compressive face. The chips did not have any

apparent effect.

Figure 23 shows the trend of the flexural modulus as a function

of temperature. It decreases about linearly to 2000 0F then more rapidly.

Figure 24 shows the strength :alues as a function of temperature.

6.3.3 Fiexural Results for Zinc Sulfide

The results of the flexural tests on the zinc sulfide specimens

are given in Table 6. The modulus values are relatively consistent and

decrease linearly as a function of temperature. The stress strain curves

were nonlinear at 1500 and 1800 OF. This is illustrated in Figure 25. The

flexural strength, however shows an increase as a function of temperature

up to 1500 'F andat 1800 0F, the strength is at least that at room temperature.

The cause of this effect is not known. It may be that there is a process of

defect healing occurring. If so, the rate of this event would determine if

the increase would be effective in application. The flexural strength-tem-

perature relationship is shown in Figure 26.

23

NWC TP 6539, Part 2

6.3.4 Flexural Results for Zinc Selenide

The flexure properties measured on the zinc selenide specimens

are given in Table 7. The modulus, as in the ZnS results, decreases almost

linearly as a function of temperature. This is illustrated in Figure 27.

Again the stress strain curves were nonlinear at higher temperatures, being

extremely nonlinear at 1000 ' F and above with a "yield point" of about 1500

psi at 1000 "F and 1000 psi at 1500 OF and 1800 OF. Most of the 1500 and

1800 OF specimens did not provide an ultimate flexural strength because the

specimens bottomed out in the fixture. After the tests, the unfractured

specimens maintained the curved shape.

The strength increased at 500 OF over the room temperature

values and was still higher than the room tenmerature values at 1000 'F as

illustrated in Figure 28.

6.4 Tension

Tensile tests were conducted on each of the materials at room

temperature only. Strain gages were used on several of the specimens in

addition to clip-on optical extensometers. Good agreement was seen between

the two techniques. Other specimens were ungaged as a standard, making sure

that the gages did not affect ultimate values.

_6.'.1 Tensile ResPonse of Sapphire

"The results of the tensile tests on the sapphire material are

given in Table 8. The specimens were oriented in the 600 orientation. The

scnic velocities agreed well with the 600 flexspecimens. The calculated PV2

-moduluý for these specimens is 61.9 x 10" psi and, considering Poisson effects,

the bulk sonic modulus is 47.2 ,, 106 psi. These values bracket the measured

initial modulus which averaged 51.2 x 106 psi. The tensile modulus is also

il good agreement with the room temperature flexural modulus which averaged

-2.5 x 106 psi.

24

NWC TP 6539, Part 2

One of the five tensile specimens (T-1) failed in the head of

the specimen. The failure was at a low stress level as calculated in the

gage section (39,350 psi) and an even lower number value in the head, the

value of which is affected by the stress concentration at the failure

location. The failure sur-face for T-1 is shown in Figure 29.

The average tensile strength without specimen T-1 was 45,440

psi. A typical failure surface is shown in Figure 30 and the failure initia-

tion in Figure 31. The tensile stress-strain curves for the sapphire are

shown in Figure 32.

6.4.2 Tensile Response of Spinel

One of the five spinel tensile specimens was broken giving •nly

four specimens for testing. The results of these tests are given in Table 9.

Examples of the failure surfaces are shown in Figures 33 to 36. As wit;- the

flexure specimens the failure propagated between the grains; the average

strength of the four specimens was 14,200 psi. Two specimens broke at a

lower value (12,500 psi average) and two at a higher value (15,900 psi

average). No distinction was seen between the pairs in fractography. The

two lower-strength specimens did have the lower velocity measurements but

not significantly lower. The strains to failure also sorted as the moduli

were essentially the same and the stress strain curves were linear to failure

as illustrated in Figure 37. The average strain to failure was 0.00035 in./in.

6.4.3 Tensile Response of Zinz Sulfide

The results of the tensile tests for the zinc sulfide specimens

are gi'len in Table 10. The average strength of these specimens was 3565 psi.The response was very linear to failure as illustrated in Figure 38. Fracture

faces and failure initiation points for the weakest (T-l) and strongest (T-2)

specimens are shown in Figures 39 and 40. The average modulus was 11.4 x 106

psi and the strain to failure 0.00031 inches/inch. The stiffness is just

sliqhtly higher than the flexural modulus, 10.6 x 106 psi.

25

NWC TP 6539, Part 2

"6.4.4 Tensile Response of Zinc Selenide

The tensile stress-strain data for zinc selenide are given in

Table I,. The stiffness is again slightly higher than the flexural modulus

(11.5 versus 10.3 x 10 psi) probably reflecting a shear contribution in the

flexural data. The stress-strain curves were quite linear (except for T-2

eas measured by the clip-ons). This is illustrated in Figure 41, a composite

of the stress-strain curves. Specimen T-2 was linear as measured by the

strain gages. The average strength was 2665 psi and the average strain to

failure 0.00024 inches/inch. A typical tensile failure surface and initia-

tion site (specimen T-2) are shown in Figure 42. Figures 43 and 44 show

sequential magnifications of the failure surface of specimen T-4.

6.5 Compression

The compressive measurements were made by sequentially loading

the specimens at increasing temperatures as discussed in the procedures section.

The results reported for each specimen are obtained (typically averaged) from

three replications per specimen at each temperature. Measurements were made

"up until nonlinearities were noted at the low stress levels used.

6.5.1 Compressive Results for Sapphire

The results of the compressive NDM measurements for sapphire are

"given in Table 12. These are plotted in Figure 45 and the average plotted in

Figure 46. Figure 46 also shows a comparison with the tensile modulus at 70'

and the flexural modulus at 70 and 20000. There is good agreement between

them, the tensile modulus being a little low at 70 *F.

6.5.2 Compressive Results for Spinel

The results of the compressive NOM measurements for spinel are

"given in Table 13. Specimen C-3 gave dramatically softer response than the

trtwo s pec en a` i .u.st.ra.te d o n F igure 4'7 The other two specii,,ens

26

NWC TP 6539, Part 2

were averaged to obtain the curve shown on Figure 42. The curve developed

is higher (stiffer) than indicated by the tensile and fleý,xre data.

6.5.3 Compressive Results for Zinc Sulfide

The results of the compressive NDM measurements for zinc sulfideare given in Table 14 and plotted on Figure 49. The average values agree wellwith the tensile and flexure results at 700 but tend to be stiffer than theflexural moduli at higher temperatures as illustrated in Figure 50.

6.5.4 Compressive Results for Zinc Selenide

The zinc selenide NDM compressive data are provided in Table 15

and plotted on Figure 51. The average values (Figure 52) agree well with the

tensile and flexure results.

6.6 Thermal Expansion

6.6.1 Thermal Expansion of Sapphire

Figure 53 is a plot of the thermal expansion of 60' sapphire fromroom temperature to 3400 'F. The expansion was measured in a quartz dilatometer

for temperatures up to 1500 'F. For temperatures greater than 1500 'F a"graphite dilatometer was used. Again, this is good duplication of data and the

expansion appears stable throughout the tested temperature range. The maximum

expansion is 18.5 x l0-3 in./in. at 3400 °F. Tables 16 to 19 cive the measuredresults by test.

Figure 54 is the thermal expansion of 00 sapphire. Its expansion

is also stable but lower than 60' sapphire. The maximum expansion is 17.25x i0- 3 in./in. at 3400 'F. Plotted along with the 00 sapphire expansion is the

expansion data of an NBS standard sapphire. Excellent agreement was obtained.

Tables 20 to 23 give the individual test results.

27

NWC TP 6539, Part 2

6.6.2 Thermal Expansion of Spinel

Figure 55 is a plot of the thermal expansion of spinel from

room temperature to about 2900 IF. Again, both quartz and graphite dilatom-

eters were used. The expansion is stable and increases linearly to a maximum

value of 15.5 x 10-' in./in. at 2900 IF. Tables 24 to 27 give the thermal

expansion test results.

6.6.3 Thermal Expansion of Zinc Sulfide

Figure 56 is a plot of the thermal expansion of zinc sulfide

versus temperature. The expansion was measured from room temperature to

1800 IF using a quartz dilatometer (described earlier). As can be seen

there is good agreement between the specimens. The expansion is somewhat

linear attaining a maximum value of 8.4 x l10 in./in. at 1800 OF. The

tabular results are provided in Tables 28 and 29.

6.6.4 Thermal Expansion of Zinc Selenide

Figure 57 is a plot of the thermal expansion of zinc selenide

from room temperature to 1800 °F as measured in a quartz dilatometer. There

is good duplication of data. The expansion is linear up to about 1200 IF.

After 1200 °F there is a slight "hump" in the data which peaks at about

1400 'F. The "hump" is no "longer detectable after 1600 'F as the expansion

returns to its linearity. The peak expansion is 7.0 x 10-3 in./in, at

1800 °F. The "hump" in the thermal expansion data is probably due to some

phase change within the material. This change could be either recrystalli-

zation or precipitation of the parent materials. A review of the mechanical

"data shows that the I'lexural modulus, flexural strength~and compressive

modulus all decrease somewhere between 1000 IF and 1500 "F. Infrared

absorption data from Hughes (Reference 1) indicates optical degradation of the

material at about 1200 IF. The results by test are given in Tables 30 and 31.

28

NWC TP 6539, Part 2

6.6.5 Comparison of Thermial ExpLansions

Figure 58 is a composite plot of the thermal expansions of all

four materials. At 1800 OF ZnSe had the highest expansion. ZnS, spinel and

60' sapphire are all next with roughly the same expansions. 0' sapphire

had the lowest expansion.

6.7 Heat Capacity of the Four Materials

The heat capacity of the four window materials was measurea

using an adiabatic calorimeter (for temperatures less than 1000 OF) and anice calorimeter (for temperatures greater than 1000 OF). Both of thesetechniques were described earlier. To obtain heat capacity enthalpy,changes of the material are first determined. The enthalpy changes are

plotted and the slope of the enthalpy curve (heatcapacity) is determined* graphically. Figures 59 through 62 are the enthalpy curves for Sapphire,

Spinel, Zinc Sulfide and Zinc Selenide, respectively. Figures 63 through

66 are the corresponding heat capacity curves. Figure 67 is a compositeplot of the heat capacity of all four materials. Zinc Selenide had the

lowest heat capacity. The heat capacity of the Zinc Selenide increased

linearly until about 12C OF, where it began to level off. This is

probably due to material degradation as described earlier. The heat

capacity of zinc selenide increased from 0.08 Btu/Ib-F (200 'F) to 0.125

Btu/lb-F (1800 OF). Zinc sulfide had the next lowest heat capacity whichincreased from 0.115 Btu/Ib-F (200 OF) to 0.135 Btu/lb-F (1800 "F). The

heat capacity of the sapphire increased sharply from 0.215 Btu/Ib-F at

200 OF to 0.295 Btu/ib-F at 1500 OF. After 1500 OF the heat capacityincreases slightly to 0.325 Btu/lb-F at 3250 OF. The heat capacity, of

NBS sapphire increased sharply from 0.215 Btu/Ib-F at 200 % to u.29ý at

1500 OF. After 1500 'F the heat capacity increases slightly to 0.225 Btu/lb-F at 3250 OF. The heat capacity of NBS sapphire (Reference 720) is also

plotted. As can be seen there is good agreem.ent with the NBS staildardsapphire. The heat capacity of the spinel starts off about the sadnl as

. - *.€ .,

S---1I II I I I Z I-- - 11 1 .' 1-- i i. . . . ..- Ai.. .1-- -1-

PPP

iNWC TP 6539, Part. 2

the sapphire (0.215 at 200 'F). The heat capacity of the spinel is slightly

lower than the sapphire until about 1250 *F. At this point the heat capacity

of the spinel increases, exceeding the sapphire, to a maximum value of 0.37

Btu/lb-F at 3000 OF.

Tables showing the individual data points for each of the

materials are provided as Tables 32 to 39.

6.8 Thermal Conductivity of Sapphire

Sapphire absorbs signif-icant amounts of radiation at certainwavelengtns. This radiation -is then reemitted within the ~.phire providing

a radiative transport echanism within the medium. The ordinary (true)

thermal conduction is thus augmented by a radiation conduction. The apparent

measured conductivity, a combinaition of the true thermal conduction and the

radiation conduction, is termed a thermal conductance.

Figure 68 is a plot of the thermal conductance of sapphire

versus teimperature. Conductance from 250 Or to 1500 OF was measured in the

comparative rod apparatus (CP-A), discussed earlier. Conductance from 1500 O

to about 3250 OF was measured in the radial inflow apparatus (RIA), also

discussed earlier. Figure 68 shows. a difference in the values of conductance

at 1500 OF as medsured by both facilities. This difference is attributed

to radiation effects involving sppcimEn thicknesses, transmissionl coefficients

and viev: factors. Radiation effects can be r~ompensated for analytically if

one assumes that conduction and radiation ar,? independent of one another

(References 2, 3, and 4), that .s,

qtotal = conduction + qradiation (1)

Let qconduction be simple conduction governed by Fourier's law

for steady-state heat flow (Reference 5)

-cnuto (LT, - T2) (2)

and let qrdato be defined as radiant heat transfer between two flat

.i ates with some transmiL 'tI riy-absor1b-irng dainbt.e (PRefcrences G

and 7)

30

.. ~ .- . A. . . . . .~ . . . . . . .V .~ . -

N1,-C TP 6539, Part 2

i i .- N • ~(T:• T,•+-

radiation 13 (-) T D ( 3'4 D l 11 F

where the terminology is as follows:

"-T = Temperature Hot Surface

T2 = Temperature Cold Surface

K = Thermal Conductivity

0 = Specimen Thickness

S= Stefan-Boltzman Constant

- = Transmission Coefficient

F-i = Emissivity Surface I

I = Emissivity Surface 2

F = View Factor = I for RIA = 0.2 for CRA

N = Amount of Energy below Wavelength for

Blackbody at T

If the above equations are used in conjunction with the trans-

mission plots of -,apphire (Figures 69 and 70 supplied by NWC (Reference 8)), a

value of true thermal conductivity can be solved for. This is shown in

Figure 71. The dashed line represents literature values (Reference 9 and 10).

There is good agreement between data sets as shown.

The issue of the difference between the CRA results and the

RIA results is further clouded by the misorientation of the RIA specimens

which were aligned 90' to the intended orientation. The effect of this on

the values measured is unknown but, given the relatively good agreement in

the calculated values, appears to n less than 20 percent.

"6.9 Thermal Conductivity of Spinet

Figure 72 is a plot of the thermal conductance of spinel versus

temperature. Again there is disagreement at 1500 OF between facilities. If

the data are treated in the same manner as the sapphire data and the analvti-

cal equations used in conjunction with the transmission plots (Figures 73 and

74), a corrected thermal conductivity curve is obtained (Figure 75). The

"dashed line represents the average value of the data. There were no literature

values available on spinel for comparison. Data above 2500 OF is questionable

31

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.iWC TP 6539, Part 2

since 2500 OF is the approximate hot pressing temperature of the material.

6.10 Thermal Conductivity of Zinc Sulfide (ZnS)

Figure 76 is a plot of the thermal conductivity of zinc sulfide

(ZnS) as a function of temperature. The conductivity was measured in the

comparative rod apparatus only. Data above 1470 OF is questionable as this

is the reported degradation temperature of the materiais. Since the conduc-

tivilty was measured at temperatures less than 1500 ,'Fradiation effects neednot be considered. The data in Figure 76 represents the true conductivity.

The values of conductivity range from about 95 Btu-in./hr-ft 2!F at 260 °F to

45 Btu-in./hr-ft 2 !-F at 1000 OF.

6.11 Thermal Conductivity of Zinc Selenide (ZnSe)

Figure 77 is a plot of the thermal conductivity of zinc selenide

(ZnSe) as a function of temperature. The conductivity was measured in the

comparative rod apparatus only. Data above 1112 °F is questionable as this

"is the reported degradation temperature of the material 8. Since the conduc-

tivity was measured at temperatures less than 1500 OF, radiEtion effects neead

not be considered. The data in Figure 77 represents the true conductivity.

The values of conductivity range from about 93 Btu-in./hr-ft23 F at 190 OF to

40 Btu-in.!hr-ft 2 -F at 1000 'F.

7.0 SUMfARY OF PROPERTIES

Tables 40 through 43 provide a quick summary of the properties

of each of the four materials. Flexural strength values are suspect due to

' the lack of a "break" on the corners. Thermal conductivity values are

corrected for radiation where appropriate. As expected tensile values,-ather than flexure, give a good comparison to the predicted tensile ioads

. in full scale therinostructural testing as given in Part 1 of this report and

shown in Table 44. Table 45 provides a comparison of the four materials.

32

- ... ... . ..__.___ ______- - - - - - - --

-- JG TP 6539, part 2

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NWC TP 6539, Part 2

ositioning Crosshead

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Figure 2. Schematic arrangement of the gas-bearing universals, specimen andload train

34

NWC TP 6539, Part 2

)- ,• e•.Sp spherical RadiusPositioning/ .

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Figure 3. Schematic arrangement cf gas-bearing universals, specimen and

load train

35

N.C TP 6539, Part 2

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N1,O, TP 65-39, Part 2

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NWC TP 6539, Part 2

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35

SNWC TP 6539, Part 2

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40

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NWC TP 6539, Part 2

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43

NWC TP 6539, Part 2

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QiQure 12. Cross-section scheriatic of an assembled RIA showing a cylindricalspecimen

44

NWC TP 6539, Part 2

246These voids tilled2.44 /with Thermatomic

Carbon Powder

0.350 D.350

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SECTION "A-Ao

.Fi1ure 13. Radial Inflow Apparatus specimen holder and specimen configuration

45

727:

NWC TP 6539, Part 2

D 0.500-- V

0 0.500

3.000

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Notes: All dimensions in inches

Figure 14. Thermlal Expansion specimen

46

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NWC TP 6539, Part 2

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Figure 16. Failure surface of sapphire flexure specimen F-10 (60') showing_JpICuI ConCJI4laI . OZ 1C'•,U-,.

43

..-. .. . . . . .

NWC TP G539, Pdrt 2

Figure 17. Fracture face of 0' oriented flexure specimen

49

NUC TP 6539, Part 2

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50

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NWC TP 6539, Part 2

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NWC TP 6539, Part 2

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Table 12. Initial Compressive Moduli of Sapphire (106 psi)

Temperature-- O _F 0 C-I C-8 Average

S70 53.1 55.91 54.82 54.6

200 53.1 55.9 54.8 54.6

"400 54.6 55.9 54.8 55.1

600 50.0 55.9 54.8 53.6

800 48.6 - 54.8 51.7

"1000 49.8 50.61 52.0 50.8

1200 48.6 50.61 52.0 50.4

1400 48.9 50.61 52.0 50.5

1600 48.0 50.61 53.33 50.6

1800 46.9 46.5 54.05 49.1

2000 46.9 42.55 43.96 44.5

2200 41.2 28.8 40.8 36.9

2400 39.8 32.8 35.4 37.8

2600 36.4 29.2 35.4 33.6

2800 30.7 28.2 25.0 27.9

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NWC TP 6539, Part 2

Table 13. Initial Compressive Moduli of Spinel (106 psi)

Temperature

OF #3 C-S1 C-7 Average

70 46.5 48.8 47.6 47.6

200 42.1 48.8 47.6 46.1

400 36.3 48.8 44.4 43.2

600 36.4 42.5 45.4 41.4

800 38.1 45.9 45.4 43.1

1000 34.7 45.9 44.9 41.8

1200 34.1 48.7 44.4 42.4

1400 28.7 44.4 43.0 38.7

1600 26.7 47.0 45.4 39.7

1800 23.6 40.0 44.4 36.0

2000 22.2 40.0 38.8 33.7

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2400 17.2 38.5 40.0 31.9

2600 17.7 39.2 40.0 32.3

2800 12.5 30.1 35.4 26.0

3000 7.7 23.5 32.0 21.0

3200 4.6 20.6 19.7 14.9

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122

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NWC TP 6539, Part 2

Table 14. Initial Compressive Moduli of ZnS (10" psi)

Temperature

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70 11.4 10.0 10.q 10.8

200 11.1 10.0 12.0 11.0

400 11.1 9.8 1?.5 11.0

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1000 10.0 9.8 9.3 9.7

1200 10.0 9.8 7.8 9.2

1400 9.8 8.0 7.0 8.3

1600 7.3 5.2 5.7 6.1

1800 5.0 5.0 4.4 4.8

2000 4.7 5.0 4.6 4.8

2200 4.3 3.6 3.8 3.9

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'Strain Gage Modulus 1 10.9 (v 0.38?)

123

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NWC TP 6539, Part 2

Table 15. Initial Compressive Moduli of ZnSe (106 psi)

Temperature

OF C-4 C-5 Average

70 10.91 10.8 10.8

200 10.9 10.0 10.5

400 10.9 9.9 10.4

600 10.9 10.1 10.5

800 10.1 8.4 9.3

1000 9.3 7.4 8.3

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1400 8.1 7.7 7.9

1600 7.0 5.9 6.5

1800 6.7 5.1 5.9

2000 4.5 5.2 4.8

"2200 1.7 2.8 2.3

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NWC TP 6539, Part 2

Table 33. Enthalpy of Sapphire in Ice Calorimeter

Enthalpyfrom Drop

Drop Initial Final TemperatureSpecimen SRI Run Temperature Weight Weight to 32 OF

Number Number OF Grams Grams Btu/lb

HC-I 36 2541 6.3104 6.3104 681.6

HC-I 37 3270 6.3104 6.3104 922.13

HC-2 40 2014 7.4668 7.4686 493.31

HC-I 31 1529 6.3104 6.3104 378.36

142

NWC TP 6539, Part 2

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NWC TP 6539, Part 2

Table 35. Enthalpy of Spinel in Ice Calorimeter

Enthalpyfrom Drop

Drop Initial Final TemperatureSpecimen SRI Run Temperature Weight Weight to 32 OF

Number Number OF Grams Grams Btu/lb

NOC0215

HC-1 36 1679 21.3514 21.3617 421.93

HC-I 37 2448 21.3617 21.3564 688.0

HC-I 38 2992 21.3564 21.3276 894.9

HC-2 41 2032 21.6574 21.6658 534.24

HC-2 51 2765 21.6658 21.6558 798.81

144

":•WC TP 6539, Part 2

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NWC TP 6539, Part 2

Table 37. Enthalpy of Zinc Sulfide in Ice Calorimeter

Enthalpyfrom Drop

Drop Initial Final TemperatureSpecimen SRI Run Temperature Weight Weight to 32 OF

Number Number OF Grams Grams Btu/lb

NOC0215

HC-l 38 1513 16.9758 16.9748 180

HC-l 39 1813 16.9748 16.9207 222.0

146

NWC TP 6539, Part 2

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NWC TP 6539, Part 2

Table 39. Enthalpy of Zinc Selenide in Ice Calorimeter

Enthalpyfrom Drop

Drop Initial Final TemperatureSpecimen SRI Run Tempera*--c. Weight Weight to 32 OF

Number Number OF Grams Grams Btu/lb

NOC0215

HC-i 39 1598 18.4949 18.4510 151.0

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148

NWC TP 6539, Part 2

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"1,1WC TP 6539, Part 2

An.ppendi x

SENSITIVITY STUDIES

The sensitivity studies it, Reference 8 were conducted on"PYroceram( using nominal properties available prior tO the data set

developed under tiat effort. The anoiysis was conducted on a racloee

structure at aerodynamic heating condition somewhat exceeding those

anticipated for the IR windows for ,hich the materials under this

effort were evaluated. The analysis was conducted using state of tie

art aerodynamic heating codes. the Asthma code for indepth heating

anclysis and SAAS-IIi body-of-revelation finite--elemen*n structurai

analysis. The material properties were modeled as elastic with

equad tensile and compressive modul i which va ied as a function of

temperature.

Prior to initiating the testing effort, the peak stressed

volumes and areas were calculated. These were comparable to the tensile

specimens used in that effort. Note that the volume 3nd surface areas

eare about the san;.e as would be involved in the TD surface of an IR -Dome

despite the much larger size of the full radorme as shown in -igure A-1.

The sensitivitv studies were conducted by varying the prop-

erties listed in Tabic A-1 one at a time. As can he seen the most sensitive

Daramters in tcrms of stress gerneration were tha stiffnesses and trerri.i

exoanision.

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NWC TP 6539, Part 2

Appendix

SENSITIVITY STUDIES

The sensitivity studies in Reference 8 were conducted on

Pyroceram( using nominal properties available prior to the data set

developed under that effort. The analysis was conducted on a radome

structure at aerodynamic heating condition somewhat exceeding those

anticipated for the IR windows for which the materials under this

effort were evaluated. The analysis was conducted using state of the

art aerodynamic heating codes, the Asthma code for indepth heating

analysis and SAAS-III body-of-revelation finite.-element structural

analysis. The material properties were modeled as elastic with

equal tensile and compressive moduli which varied as a function of

temperature.

Prior to initiating the testing effort, the peak stressed

volumes and areas were calculated. These were comparable to the tensile

specimens used in that effort. Note that the volume and surface areas

are about the same as would be involved in the ID surface of an IR Dome

despite the much larger size of the full radome as shown in Figure A-1.

The sensitivity studies were conducted by varying the prop-

erties listed in Table A-1 one at a time. As can be seen the most sensitive

parameters in terms of stress generation were the stiffnesses and thermal

expansion.

155

".' NWC TP 6539, Part 2

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NWC TP 6539, Part 2

TABLE A-i. Sensitivity Study Summary.

'•Error Error in Error in

Parameter backface max. thetaintroduced

temp. rise, % stress,

5 Velocity 10 9

5A Thermal conductivity 1.2 1.2

5 Thickness 1.5 1.5

I00•00', Emissivity O.i 0.1

1/8 in. Strain gauge location --- 6

I /8 in. Thermocouple location 8.5

-151, baseline Modulus -15

+11 baseline Modulus +II

+111I constant f(T) Modulus +4

Linear/2nd slope Expansion -3

-30%o linear/2nd slope Expansion -34

-40., linear/2nd slope Expansion -47

.-50: linear/2nd slope Expansion -52

157

NWC TP 6539, Part 2

REFERENCES

1. Tanzilli and Bleiler. Specular Spectral Transmittance Behaviour andAbsorption Coefficient and Emittance Estimates for Five InfraredWindow Materials at Elevated Temperatures. Hughes Aircraft ReportNo. 9T21-2E6-1, Dec. 1982.

2. Siegel, Howell. Thermal Radiation Heat Transfer. New York, McGraw-Hill, 1981.

3. Condon. "Radiative Transport in Hot Glass," J. Quan._Spectrosc.& Radiat. Transfer, Vol. 8, pp. 369-385, 1968.

4. Buzoukiwa, Men. "Use of Fused Quartz as a Reference Standard inComparative Methods of Thermal Conductivity Measurements," Inzhenerno-Fizicheskii Zhurnal, Vol. 23, No. 44 (October, 1972), pp. 669-672.

5. Krieth and Black. Basic Heat Transfer. New York, Harper-Row, 1972.

6. Rosenhow and Hartnett. Handbook of Heat Transfer. New York, McGraw-Hill, 1973.

7. Sparrow and Cejs. Radiation Heat Transfer. New York, McGraw-Hill,

1978.

8. Koenig, J. R. Presentation to AMRAAM JSPO, 1980.

9. Powell, Ho, and Liley. Thermal Conductivity of Selected Materials."Washington, D.C., U.S. Dept. of Commerce, 1966. (USDC Pub.No. NSRDS-NBS-8.)

10. Goldsmith, Waterman, and Hirschhorn. Handbook of ThermophvsicalProperties of Solid Materials, Vol. 3. New York, tfacMillan, 196j.

158

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