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AD-A168 611 THERMAL AND MECHANICAL PROPERTIES OF CALCIUM LANTHANUM It/iSULFIDE(U)'SOUTHERN RESEARCH INST BIRMINGHAM ALJ R KOENIG APR 85 SORI-EAS-85-401-5267-l-F N
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MICROCOPY RESOLUTION TEST CHART
NATIONAL BUREAU OF STANDARDS-1963-A
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SO I-8I--401 5267-1-F
"1EBNAL AND NECHANICAL PROPERTIES;,-'-'. G~F CALCIUMI LANITHANUM SULFIDEr.L-
Final Report to
OFFICE OF NAVAL YSEARCHDepartment of the Navy800 North Quincy StreetArlington, Virginia 22217
Contract number NO014-83-K-0195
April, 1905
S ELECTEOCT 28 MS
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SoRI-EAS-85-401-5267-I-F
THERMAL AND MECHANICAL PROPERTIESOF CALCIUM LANTHANUM SULFIDE
Final Report to
OFFICE OF NAVAL RESEARCHDepartment of the Navy800 North Quincy Street
Arlington, Virginia 22217
Contract Number N00014-83-K-0195
PREPARED BY:
April, 1985* . Koenig, Head Date
T e physical Divisi4
APPROVED BY:
C. D. Pears, DirectorMechanical and Material Engineering DI
Department D I(IELECTE
Southern Research Institute 0C2000 Ninth Avenue, SouthPost Office Box 55305
Birmingham, Alabama 35255-5305B
Apptvedtat public 161MI
,. triui.o Uuhzuit*.*..*
LO "i~.IV-7
TABLE OF CONTENTS
Page
1.0 INTRODUCTION 1
2.0 APPARATUSES AND PROCEDURES 3
2.1 Flexure 3
2.2 Thermal Conductivity 5
2.3 Thermal Expansion 7
2.4 Heat Capacity 8
2.5 Bulk Density 10
2.6 Ultrasonic Velocity 10
3.0 DATA AND DISCUSSION 11
3.1 NonDestructive Characterization 11
3.2 Flexure 11
3.3 Thermal Expansion 13
3.4 Specific Heat 13
3.5 Thermal Conductivity 13
4.0 SUMMARY OF THE DATA 14
5.0 REFERENCES 15
Appendices
A - Flexural Load/Deflection Curves A- 1
B - Sensitivity Studies B-23
ii
LIST OF ILLUSTRATIONS
Figure Page
1 Schematic of High Temperature Flexural Apparatus 16
2 Flexural Four-Point Loading Set-up 17
3 Schematic of Comparative Rod Thermal Conductivity Apparatus 18
4 Assembly of Quartz Tube Dilatometer for Thermal ExpansionMeasurements 19
5 Block Diagram of Ultrasonic Velocity Measuring Apparatus 20
6 Flexural Specimen Configuration 21
7 Flexural Moduli of CaLa2S4 as a Function of Temperature 22
8 Strength versus Temperature for CaLa2S4 23
9 EDS Scan of CaLa2S4 Specimen Fracture Face 24
10 Failure Surface of F-10 25
11 Probable Initiation Site in F-10 26
12 Higher Magnification of Probable Initiation Site in F-10 27
13 Structure in "Hackle" seen in Figure 10 28
14 Thermal Specimen Configurations 29
15 Thermal Expansion of CaLa2S4 30
16 Enthalpy Plot for CaLa2S4 31
17 Specific Heat of CaLa2S4 32
18 Thermal Conductivity of CaLa2S4 33
Accessic ,)SNTIS G ';:
DTIC T'
Jf Lhot, .
Di .'. "~~~Avail'.O AW' 1 ,.Dist
iii A S
LIST OF TABLES
Table Page
1 Test Matrix for CaLa2S4 34
2 Density and Velocity of CaLaS Specimens 35
3 Flexural Properties of CaLa2S4 IR Window Material 36
4 Thermal Expansion of CaLa2S4 - Encl 4 Measured in Quartz Dilatometer 37 -.
5 Thermal Expansion of CaLa2S4 - Encl 4 Measured in Quartz Dilatometer 38 A6 Enthalpy of CaLa2S4 Measured in the Adiabatic Calorimeter 39
7 Enthalpy of CaLa2S Measured in the Ice Calorimeter 40
8 Thermal Conductivity of CaLa2S - Encl 6 using Comparative RodApparatus with TM-Silica References 41
9 Thermal Conductivity of CaLa2S4 - Encl 6 using Comparative RodApparatus with TM-Silica References 42
10 Thermal Conductivity of CaLa2S4 - Encl 6 using Comparative RodApparatus with TM-Silica References 43
11 Thermal Conductivity of CaLa2S4 - Encl 6 using Comparative RodApparatus with TM-Silica References 44
12 Summary of CaLa2S4 Mechanical and Thermal Data 45
iv
Ia I
IA-
THERMAL AND MECHANICAL PROPERTIES
OF CALCIUM LANTHANIUM SULFIDE
1.0 INTRODUCTION
This is the final report of the effort conducted at Southern
Research Institute for the Office of Nav~L Research, Arlington, Virginia,
under contract number NOOO14-83-K-O195. 4'The purpose of this effort was
the determination of the mechanical and thermal properties of specimens
fabricated from calcium lanthanium sulfide (CaLaS,) by Raytheon Company,
Research Division.
The CaLa S, was reported by Raytheon to have initial (slow)
decomposition occur/ing at 700 to 800 °C. They suggested 1000 OC as an
effective use temperature. It melts at 1800 OC. It is further reported to
have favorable transmission properties in the 8-12 micron range and twice the
hardness of ZnS.1
\KThe test matrix used s shown in Table 1. It is essentially
identical to the test matrix ut ized for the evaluation of ZnS and ZnSe under
NWC contract number N6053 -C-0031 and reported in SoRI-EAS-84-1096, Thermal
aid_-ehanioal Properties of Candidate Optical Materials for IR windows. It
was designed to obtain sufficient information 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 thermal stress resistance was investigated using thermal
expansion, thermal conductivity, specific heat and flexure. Sensitivity .
_ . ,
-- studies conducted on this class of materials -reference 2, see Appendix B)
show the critical properties which control the thermal stress reponse 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
temperature 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 other critical responses./<For example, the thermal
conductivity and specific heat, in addition to being necessary to predict the
thermal 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. In addition to these
properties, nondestructive measurements (NDC) were made to aid the
interpretation of the data and fractographic studies were made of the tested
specimens to aid in the understanding of the results.
Tensile and compressive tests, which were planned in the initial
matrix, were not conducted as specimens were not received. This is
unfortunate, particularly for the tensile tests, as these are more directly
related to the response of the material as a dome under thermostructural
loading than are the flexural results.
The flexure tests were conducted at a series of temperatures
providing both flexural modulus and strength. Tests were conducted at 70,
500, 1000, 1500 and 1800 OF. (20, 260, 538, 816 and 982 0C). Thermal
expansion and specific heat were measured up to the material limit (-1000 0C).
Thermal conductivity was measured up to about 650 0C at which temperature the
degradation of the material poisoned the thermocouples and additional data
could not be taken. Several attempts to extend that range meet with limited
success as will be discussed later.
2
vU. 1
L
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
microscopy was used for the fractography.
C
2.0 APPARATUSES AND PROCEDURES
2.1 Flexure
Beam flexural evaluations were performed in the flexural apparatus
shown in Figure 1 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 deflection. 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 extending down to a differential
transformer. The differential transformer is supported by a tube that
attaches to the support bar eliminating load train motion from the deflection
measurement. A new molybdinum loading system was designee and fabricated for
this effort.
From the plot of load versus midpoint deflection, the values of
modulus of rupture and flexural measured. The ultimate strength is calculated
from the equation:
McI
3
Vi.
which simplifies to
PLS =-
bh
II 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
specimen span length. The four point loading system is shown schematically in
Figure 2. In these equations:
S - modulus of rupture
I.V' P = maximum applied load
L - span length
b = width of specimen
h = height of the specimen
The initial modulus in flexure was calculated from the equation:
Ef = 6P [a3 3 + ac/2 (a + c/4]
6 bh~where
wr Ef - elastic modulus in flexure
P/6 - 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
V.h
4
The above equation neglects the deformation due to shear and
assumes that the neutral axis coincides with the center of the cross-section.
2.2 Thermal Conductivity
The apparatus used for the evaluation of the thermal conductivity
of these materials through 1800 OF was the comparative rod apparatus (CRA).
The CRA compares the conductivity of the specimen being characterized to the
known conductivity of a reference piece. Several types of references are
available and their conductivities are traceable to NBS data or other reliable
sources. In this effort references of Pyroceram and slipcast fused silica
were used.
The CRA consists of a series of cylindrical pieces stacked in a
vertical column as illustrated in Figure 3. 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 thermal gradient
in the experiment. 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 insul tor,
another steel rod, and a cooling sink, if required. The entire column is
supported upon a steel ball for elimination of lateral forces that Lould
deform the structure.
In assembling the apparatus, a large annular shell of alumina 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, each
separately controlled to match the temperature gradient through the stacked
column, thereby controlling radial heat losses or shunting.
5 4
NOV.,
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. In this case the insulation was thermatomic
carbon.
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-OF, 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 ecuation for one dimensional
heat flow:
q" = 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 drops and gage
D6
""J"V, V
: '-. , ,' .. , . .... -' - . . , ... .-,,. ..- - ... ... .. .. . ..
." '-. ..4-'[ 4 [.'[ ) ,..... . '', '/ ' ---. -
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.
2.3 Thermal Expansion
Thermal expansion measurements were made using quartz tube
dilatometers modified from the Bureau of Standards design for measurements up
to 1800 OF. Improvements have been made to prevent lateral movement of the
quartz tube, thus eliminating possible erroneous readings.
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, and the dial gage piston
• 'to register a displacement on the gage. The quartz tube and specimen are
located within a cylindrical electrical heater and can be heated to 1800 OF in
the apparatus. The dial gage is calibrated in 0.0001 inch displacements and
has an accuracy of ±0.0001 inch at any point in its range (0.5 inches).
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.
7
z' -
This facility is shown schematically in Figure 4.
2.4 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 furnace was used to bring the specimen to temperature.
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 temperature,
and following a stabilization period, are dropped into the calorimeter cup.
Adiabatic conditions are maintained during each run by manually adjusting 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 immersed in the liquid. A double bladed stirrer
8
X21
maintains uniform bath temperature.
In the calorimeter six copper-constantan thermocouples,
differentially connected between calorimeter cup and jacket, indicate
temperature difference between the cup and bath. The six thermocouples allow
a difference of 0.03 OF to be detected. This difference is maintained to
within 0.15 OF. During the run, absolute temperature measurements of the cup
are determined by means of the three thermocouple junctions, series connected,
in the bottom of the calorimeter cup.
The enthalpy of the specimen at any initial temperature is
calculated from the equation:
h = K/Ws (t2 - t1 )
where h = enthalpy above t2
K - calorimeter constant, 0.2654 Btu/OF
Ws - sample weight in lbs
t, = initial cup temperature in OF
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 linear
interpolation. The enthalpy-temperature curve established is used to
9'ak I
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 measuring the
enthalpy of sapphire (SRM 734 from NBS) and other data which indicate that the
overall uncertainty of the apparatus is ±3 percent.
2.5 Bulk Density
The bulk density of the specimens was measured on the specimens
by gravimetric techniques. The specimens were measured with micrometers and
weighed on a Mettler balance. The reported density is simply the mass, in
grams, divided by the calculated volume in cubic centimeters.
2.6 Ultrasonic Velocity
The ultrasonic velocity was measured on each of the specimens in
the direction of test. The measurement was made using a through transmission
technique. The setup is shown schematically in Figure 5.
The basic apparatuses used for measuring ultrasonic velocity were
a Sperry UM 721 Reflectoscope and a Tektronix oscilloscope. In using the
through transmission, 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 this sound beam was the reference point on the time base of
the oscilloscope which was used as a high speed stop watch. When the leading
10
-6- .
edge of this pulse of energy 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.
3.0 DATA AND DISCUSSION
3.1 NonDestructive Characterization
Table 2 shows the bulk density and ultrasonic velocity of each of
the specimens tested under this effort. Note that some of the specimens
received earlier (thermal specimens) were of slightly lower density than the
bulk of the specimens. The average density was 4.611 gms/cc. The sonic
velocity was typically 0.201 in./usec. From these data a sonic modulus
(neglecting Poisson's effect) can be calculated. It was typically 17.5 x 106
psi. Visual inspect saw no obvious defects except a few chips previously
noted by Raytheon.
3.2 Flexure
The flexural test results are provided in Table 3. The tests were
run on specimens as shown in Figure 6 with a 1.25 inch inner span and a 3.75
inch outer span. As requested the tensile face was opposite the marked face.
This face was reported to have the better finish.
The 70 OF flexural strength was not very high, averaging 7240 psi.
This was less than the value reported by Raytheon of about 14000 psi. A large
portion of that difference may be attributable to specimen size, the Raytheon
data having been generated on miniature specimens. The average 700
iwag
flexural modulus was 13.57 x 10' psi. Note that prior to every test a
nondestructive mechanical (low stress loading, 1200 psi) test was run at 700
4to get an initial modulus). The average value for all the NDM tests was
13.48 x 106 psi, in good agreement with the average of the five 708 tests.
The modulus is also in fair agreement with the calculated sonic modulus. The
elevated temperature moduli show a steady decrease as a function of
temperature. This is shown in Figure 7. At 1500 and 1800 OF the data became
somewhat nonlinear and were represented by a bilinear fit. The secondary
slope is shown as solid symbols on Figure 7 and an effective yield point
provided in Table 3. The ultimate flexural strength as a function of
temperature is shown in Figure 8. The strength drops slightly or is almost
constant (eliminating the weakest specimen brings the average 5000 strength to
6750 psi) through 1000 OF then has higher strengths at 1500 and 1800 OF. The
higher strengths at 1500 and 1800 OF are concurrent with the nonlinearity of
the flexural response curve.
The failures occurred at relatively low levels giving poorly
defined fracture patterns. There were zones in the material which gave the
appearance of being a visually more absorptive precipitate. These were
present in all specimens but became more distinctive as the specimens had seen
temperatures of 10000 and over. Also, specimens of that temperature range
emitted a distinctive sulphurous order. EDS scans showed these "precipitate"
zones to have the same elemental components as the other zones of the
specimens. Only calcium, lanthanum and sulfur were detected as illustrated in
Figure 9. Figures 10 through 13 show scanning electron microscopy
documentation of the fracture initiation site in FS 10, one of the weaker
70 OF flexure tests. Most but not all of the specimens were even less
definitive. There is the appearance of a mirror zone and some hackle in the
left tensile corner of the specimen seen in Figure 10. The initiation site
12
PA
4..
(Figures 11 and 12) does not show any defect structure. It was in a
"precipitate" zone. Figure 13 shows the structure in the hackle.
The raw load deflection curves are given in Appendix A.
3.3 Thermal Expansion
Figure 14 shows the specimen used for measuring the thermal
expansion of the CaLa 2S,. The measured response is shown in Figure 15 and the
data given in Tables 4 and 5. The thermal expansion is higher than 00
sapphire which is shown as a reference. Above 10000 a sulfur odor was noted.
There was also a slight deviation between the specimens at that temperature
range. The two specimens both returned to near zero residual change after
cooldown to room temperature. No significant weight loss was noted.
3.14 Specific Heat
Figure 16 shows the enthalpy plot generated for the CaLa2S1
specimens. Higher scatter than normal was seen above 1100 OF. Also the
specimens tended to shatter due to thermal stresses when dropped from the
higher temperatures. The calculated specific heat (slope of the curve in
Figure 16) is shown in Figure 17. The material has a remarkably low specific
heat typical of lanthanum compounds. It rises gradually through about 1200 OF
then somewhat more rapidly thereafter. Tables 6 and 7 show the data obtained.
3.5 Thermal Conductivity
The thermal conductivity data generated on the CaLa2 S, material
are shown in Figure 18. The initial data were well behaved at low
13
li - %j . .
temperatures. However, at about 1000 OF on the first run the measured
conductivity climbed dramatically and became erratic. Upon return to about
200 OF the data repeated fairly well for the one, lower temperature, specimen.
- Thermocouples could not be read on the other specimen and upon inspection it
was seen that the thermocouples had been destroyed. New thermocouples were
installed and cemented in place to protect them. The runs were repeated with
similar results, this time obtaining an apparently valid data point at just in
excess of 1000 OF. Again the thermocouples were destroyed. As with the
expansion, a sulfurous order was detected. It was still present on the
specimens after cooldown. No significant weight change was noted.
A third attempt was made this time changing to Pyroceram
references with large (10 mil) thermocouple wire. It was planned to
extrapolate surface temperatures as a backup after the failure of the internal
thermocouples. The results showed permanent change in the conductivity of the
material even at room temperature. Again the thermocouples were destroyed
including those in the Pyroceram hot reference. Additional data were obtained
by extrapolating temperatures to the surface for calculation of the
temperature drop across the specimen. Figure 18 shows the apparently valid
data only. A line value through the data up to 1000 OF is provided. Tables 8
through 11 provide the measured data.
4.0 SUMMARY OF THE DATA
Table 12 gives a summary of the data and compares the data with
ZnS and ZnSe data from NWC Contract N60530-83-C-0031. The strength was
somewhat lower and the modulus slightly higher than the ZnS. The comparison
to ZnSe was similar except that at 70 OF the strength of the CaLaS, was
14'X6%
1+ ...... . ... . . ... .N . ... . . . ..
slightly higher. Specific heat was slightly lower than the comparison
materials but all had low specific heats, the density was intermediate and, as
expected from the moduli and densities, the sonic velocity was similar. The
• =most remarkable differences were in the thermal conductivity and thermal
expansion. The thermal conductivity is dramatically lower (a factor of about
five) than either of the materials and the thermal expansion was a factor of
about two higher.
This combination of properties will give a material that is not
very good in thermostructural response, as was indicated by the fracturing of
the heat capacity specimens, and therefore probably not a good candidate for
high velocity IR dome applications. The reported optical and hardness
properties may make this appropriate for a low velocity 8-12 micron window
application where rain erosion is a concern.
5.0 REFERENCES
1. Personal Communication, R. Gentilman to J. R. Koenig, 1984
2. Koenig, J. R., Presentation to AMRAAM JSPO, 1980
*414,
15
4. V
Graphite Pushrod
Graphite ResistanceFurnace . raphite Load Bar
Test Specimen ahtsuprBr
Graphite SumpportiBar
Graphite Deflection -Tubape Cmestn
Rod- Graphite Support Rod
- DifferentialTrransformer
- Figure 1. Schematic of High Temperature Flexural Apparatus
16
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40,4
1: I
I 4)
C14
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(44
170
Zircn'iaDiatomaceous
Reference 4
optional ThermocoupleHeater(Typ)
Aluminum CoigCoilHousing for Cold Sink
Figure 3. Schematic of Comparative Rod Thermal Conductivity Apparatus
* 18
Dial Gagecooling coils
Piston Brass Dial and LVDT Housing (Brass)
LVDT Sleeve (Brass)
LVDT Adjusting Lever
LVDT Lead Wire
Invar Insert
Support Plate(Steel)
. . . . . .
S.NBS Quartz Dilatomfeter Tubes hro
I couple Lead Wire
Invarcement
1 I Joint
SpecimenI
Specimen Support Fixture
Thermocouple Location(Typical of two places)
Approximate Location-
of Heating Element1 1 Furnace
I Support\M~ate te
Figure 4. Assembly of Quartz Tube Dilatometer for Thermal Expansion
Measurements
19
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0i cn -. x -
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.., ...., ....... .., .. ....,. , .. .... , . , ,_ : , .._ _, _,.. ,.. ., .., ... .. ..., o , ... .., .... .,.. .. .., .,-.u%
0. 250"
1s..0. 500"
*4'1
4L
4%*'
Notes: 1. Break corners on all edges
2. Surfaces to be ground parallel to length
~Figure 6. Flexural Specimen Configuration
* .- 4 ,... .. . . *
! " , ,', ,' .""- "'.,'.,""-.'" .''." ,' -.. .. . " .'',". '.', " ," " " ,".,"., . .. ''...'',, ... ', " '.", ", ., : ,," .,'',' ,'4 * ''4
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18 24
24
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;-:'-. - ...:" i , .,' , -- ":' "' " .(:- ;* V . ";' ' ' ' i
Figure 10. Failure Surface of F-10
25
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Fiue1.Poal ntainSt nF1
42
%
.5%
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9''
,o.
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- ' Figure 12. Higher Magnification of Probable Initiation Site in F-IO
".I.
I1 27
-.•4.. , ,,,_,-;, . '' . ', , - ,, ;" . -' . '". ,,.,"./ ' - ". -""C ' '.,. ' ""
-II
Figure 13. Structure in "Hackle" seen in Figure 10.
28
% I 4% I;
0.100 m-0 .300- * 0.100
______________ . -0.750 nia.
II 0.500
___ __ __ __ __ Heat Capacity Specimen
*s4~ 0.500
0. 5004 i-Thermal Conductivity Specimen
3.000
V3.000 Spherical
Radius Both Ends
Thermal Expansion Specimen
Figure 14. Thermal Specimen configurations
29
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Table 1. Test Matrix for CaLa2S4
Temperature OF
70 500 100G. 1500 1800
Flexural Strengthand Modulus 5 4 4 4 2
Thermal Expansion 2
Specific Heat 2
Thermal Conductivity 2
Density X
Sonic Velocity X
U 34
Table 2. Density and Velocity of CaLa 2S4 Specimens
Density Velocity pV2
Specimen Number (gm/cc) (in./psec) (106 psi)
RHP-145-HVl-26 #22 (TE) 4.591 0.201 17.46
RHP-220-HVI-47 #31 (TE) 4.558 0.201 17.33
RHP-155-HVI-30 #22-1 (TC) 4.591 0.204 18.05 -
RHP-207-HVI-41 #32 (TC) 4.608 0.202 17.69
RHP-155-HVI-30 #22-2 (SH) 4.604 0.202 17.68
RHP-155-HVI-30 #29 (SH) 4.609 0.204 18.05
F-I 4.616 0.201 17.55
F-2 4.631 0.201 17.61
F-3 4.632 0.201 17.62
F-4 4.643 0.201 17.66
F-5 4.641 0.201 17.65
F-6
F-7 4.621 0.201 17.66
F-8 4.621 0.201 17.66
F-9 4.619 0.201 17.57
F-10 4.619 0.201 17.57
F-I 4.611 0.201 17.54
F-12 4.619 0.201 17.57
F-13 4.608 0.201 17.52
F-14 4.610 0.201 17.53
F-15 4.618 0.201 17.39
F-16 4.603 0.201 17.50
F-17 4.597 0.201 17.48
F-18
F-19 4.603 0.201 17.50
F-20 4.588 0.200 17.27
F-21 4.602 0.200 17.33
F-23 4.586 0.201 17.44 L
35
...................................................................................
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APPENDIX A
FLEXURAL LOAD -DEFLECTION CURVES
A-
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~ APPENDIX B
SENSITIVITY STUDIES
B- 23
Sensitivity Studies
The sensitivity studies in Reference I were conducted on
Pyroceram)using nominal properties available prior to the data set
4developed 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
* Vspecimens 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 1.
The sensitivity studies were conducted by varying the prop-
erties listed in Table 1 one at a time. As can be seen the most sensitive
parameters in terms of stress generation were the stiffnesses and thermal
expansion.
I
B-24
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12-85
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