Fermilab-TM-2366-A

Measurement of mechanical properties of three epoxy adhesives at

cryogenic temperatures for CCD construction

H. Cease, P.F. Derwent, H.T. Diehl, J. Fast, D. FinleyFermi National Accelerator Laboratory

Batavia IL 60510

November 6, 2006

Abstract

Materials testing of an adhesive for bonding Silicon to a substrate is presented. Test resultsinclude Young’s Modulus, Poisson’s Ratio, and the coefficient of thermal expansion at temper-atures ranging from room temperature to 100 K. Data for 3 epoxies (Tra-Con F113, Epotek301-2, Hysol 9361) are presented.

1 Introduction

The SNAP CCD focal plane has to meet stringent performance requirements, especially onflatness. As the CCDs are manufactured at room temperature and will operate at 130 K inspace, it is necessary to characterize their behavior as a function of temperature. In addition, itis expected that the CCD focal plane will undergo thermal cycles in space. As the constructionmaterials (Si, AlN, SiC) have different coefficients of thermal expansion (CTE), there maybe stress on all of the epoxy joints. NASA has criterion on the stress/strength relation forsuch joints [1]. This note details tensile strength tests and coefficient of thermal expansionmeasurements on proposed epoxies for use in the CCD assembly.

Tensile strength tests to measure Young’s Modulus and Possion’s Ratio [2] were performedat Precision Measurements and Instruments Corporation (PMIC) [3] at 5 temperatures (295K,250K, 200K, 150K, 100K). An additional measurement was made at Fermilab at 295K. Mea-surements of the CTE from 77 K to 295 K were made at Fermilab.

Three epoxies were measured, Hysol 9361, Tra-Con F113, and Epotek 301-2. The Hysol isbeing considered for the AlN-SiC joint, the Tra-Con and Epotek for the CCD-AlN joint. InTable 1, we summarize the properties of the glue joints as reported by the manufacturer.

The Hysol sets in 24 hours, with a full cure in 7 days at room temperature. The epoxy samplesused in the tensile strength tests had a 7 day cure. For the Hysol CTE measurements, we useda sample with am accelerated 2 day cure. For the Epotek and Tra-Con CTE measurements,measurements were made with samples with both a 2 day cure and a 7 day cure. The Epotekepoxy has an additional manufacturing specification on residuals ions (salts) in the resin whichis important for silicon bonding applications.

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Epoxy Modulus Viscosity CTE @ 295 KHysol 9361 723 MPa 1000 Pa s -

Tra-Con F113 - 180 cps @25 C 55 ppm/CEpotek 301-2 - 225-425 cps 37 ppm/C

Table 1: Epoxy properties as provided by the manufacturers.

AmbientElastic Modulus (psi) 356886± 12523 3.51%

Tra-Con F113 Poisson’s Ratio 0.401±0.003 0.64%Maximum Stress (psi) 2539± 86 3.40%Elastic Modulus (psi) 531427± 6166 1.16%

Epotek 301-2 Poisson’s Ratio 0.358±0.001 0.35%Maximum Stress (psi) 3751± 45 1.21%Elastic Modulus (psi) 154678± 1526 0.99%

Hysol 9361 Poisson’s Ratio 0.433±0.007 1.67%Maximum Stress (psi) 1153± 9 0.77%

Table 2: Epoxy properties as measured at ambient temperatures.

2 Tensile Tests

Tensile tests were performed by PMIC and also the Fermilab Material Testing Group. Bothtests used samples prepared at Fermilab. The samples were dogbone shaped and machined outof cast plates of epoxy. The samples were degassed to minimize the number and size of airbubbles. We note that the Hysol samples did have visible bubbles on the machined surfaces.

PMIC measurements were performed per ASTM method D-638. Five dogbones of eachepoxy were measured at 5 temperatures (295K, 250K, 200K, 150K, 100K). The sample moduluswas calculated using the Secant Method at a 0.68% strain (or the highest strain achieved if thesample failed before that level). The Hysol samples did fail before 0.68% strain was achievedfor the lower temperature measurements. Tables 2, 3, 4, 5, and 6 summarize the measurements.The full report from PMIC is included as Appendix 1.

The Fermilab Material Testing group also performed a tensile measurement at ambient tem-perature on the three epoxies. The steepest slope over a series of ranges was used to calculated

250 KElastic Modulus (psi) 519361± 16547 3.19%

Tra-Con F113 Poisson’s Ratio 0.372 ± 0.005 1.25%Maximum Stress (psi) 3527± 120 3.41%Elastic Modulus (psi) 595903± 16547 3.19%

Epotek 301-2 Poisson’s Ratio 0.365 ± 0.004 1.05%Maximum Stress (psi) 4115± 79 1.91%Elastic Modulus (psi) 239242± 4375 1.83%

Hysol 9361 Poisson’s Ratio 0.435 ± 0.004 1.02%Maximum Stress (psi) 1736± 35 2.02%

Table 3: Epoxy properties as measured at 250 K.

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200 KElastic Modulus (psi) 615588± 26807 4.35%

Tra-Con F113 Poisson’s Ratio 0.368 ± 0.003 0.69%Maximum Stress (psi) 4272± 198 4.64%Elastic Modulus (psi) 648860± 12482 1.92%

Epotek 301-2 Poisson’s Ratio 0.349 ± 0.005 1.32%Maximum Stress (psi) 4471± 99 2.22%Elastic Modulus (psi) 560786± 11976 2.14%

Hysol 9361 Poisson’s Ratio 0.357 ± 0.005 1.27%Maximum Stress (psi) 3912± 84 2.15%

Table 4: Epoxy properties as measured at 200 K.

150 KElastic Modulus (psi) 886035± 40429 4.56%

Tra-Con F113 Poisson’s Ratio 0.367 ± 0.008 2.28%Maximum Stress (psi) 5983± 264 4.42%Elastic Modulus (psi) 833220± 14089 1.69%

Epotek 301-2 Poisson’s Ratio 0.334 ± 0.007 2.16%Maximum Stress (psi) 5681± 106 1.87%Elastic Modulus (psi) 822654± 14072 1.71%

Hysol 9361 Poisson’s Ratio 0.357 ± 0.012 3.46%Maximum Stress (psi) 4641± 79 1.71%

Table 5: Epoxy properties as measured at 150 K.

100 KElastic Modulus (psi) 1105895± 40675 3.69%

Tra-Con F113 Poisson’s Ratio 0.348 ± 0.005 1.44%Maximum Stress (psi) 7092± 649 9.15%Elastic Modulus (psi) 1014310± 14384 1.42%

Epotek 301-2 Poisson’s Ratio 0.350 ± 0.008 2.34%Maximum Stress (psi) 6783± 162 2.39%Elastic Modulus (psi) 1132056± 13051 1.19%

Hysol 9361 Poisson’s Ratio 0.353 ± 0.016 4.55%Maximum Stress (psi) 4225± 201 4.76%

Table 6: Epoxy properties as measured at 100 K.

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AmbientElastic Modulus (ksi) 384.84 ±85.7 22.2%

Tra-Con F113 Ultimate Tensile Strength (psi) 4798.2±569.1 11.9%Elastic Modulus (ksi) 650.6± 176.2 % 27.1

Epotek 301-2 Ultimate Tensile Strength (psi) 9664.2±1769.6 18.3%Elastic Modulus (ksi) 137.5± 17 12.3%

Hysol 9361 Ultimate Tensile Strength (psi) 2400.4± 190.6 7.94%

Table 7: Epoxy properties as measured at ambient temperatures by the Fermilab Ma-terial Properties Testing group.

the modulus. The crosshead pull speed was greater than 0.05 inches per minute. The resultsare summarized in Table 2.

3 Coefficient of Thermal Expansion Measurements

CTE measurements were made at Fermilab. The measurements were performed in the spirit ofASTM-E831. Samples were approximately 8 mm × 8 mm × 20 mm, machined from samplescast in a mold. Each sample was vacuum degassed during the casting to minimize the size andnumber of trapped gas bubbles.

The CTE was measured by placing the sample in a holder inside of a cryostat. Liquidnitrogen is poured into the cryostat. Once the temperature stabilized at 77 K, a heater is usedto ramp the temperature to ambient temperature with a rate of 1-2deg C/minute. An LVDT [4]at the top of the sample measured the change in sample length. The length and temperaturewere recorded during the cooldown and the warmup. In Figure 1, we show a picture of thesample in the holder. The LVDT is at the top of the picture, connected via quartz rods tothe sample holder. The sample holder is installed inside the cryostat. We report the integralfractional change in length (dL/L) of the sample as a function of temperature in Table 8. InFigures 2, 3, and 4, we show the fractional change in length as a function of temperature for onesample of Tra-Con F113, Epotek 301-2, and Hysol 9361. In Figure 5, we show a representativetime ramp for one of the measurements.

4 Stress/Strength Ratios

The NASA guideline for epoxy joints [1] is a safety margin of a factor of 2 on the stress. Withthe measured modulus and CTE, we can calculate the expected stress on the joint and compareto yield strength, using the following logic:

Modulus =StressStrain

Strain =dLL

(1)

dLL

(epoxy) = CTE (epoxy)×∆T

With the assumption that the CTE of the substrate is small compared to the epoxy, the stresson the joint is simply:

Stress = Modulus× CTE (epoxy)×∆T (2)

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Figure 1: The sample holder for use in the dL/L measurements.

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Ambient TemperatureTra-Con F113 dL/L (×10−3) – –Epotek 301-2 dL/L (×10−3) – –Hysol 9361 dL/L (×10−3) – –

250 KTra-Con F113 dL/L (×10−3) -3.27 ± 0.13 3.94%Epotek 301-2 dL/L (×10−3) -2.83 ± 0.04 1.52%Hysol 9361 dL/L (×10−3) -4.69 ± 0.04 0.8%

200 KTra-Con F113 dL/L (×10−3) -6.20 ± 0.11 1.73%Epotek 301-2 dL/L (×10−3) -5.45 ± 0.03 0.59%Hysol 9361 dL/L (×10−3) -8.69 ± 0.02 0.3%

150 KTra-Con F113 dL/L (×10−3) -8.71 ± 0.06 0.76%Epotek 301-2 dL/L (×10−3) -7.70 ± 0.11 1.37%Hysol 9361 dL/L (×10−3) -11.3 ± 0.003 0.2%

100 KTra-Con F113 dL/L (×10−3) -10.7 ± 0.08 0.72%Epotek 301-2 dL/L (×10−3) -9.66 ± 0.18 1.88%Hysol 9361 dL/L (×10−3) -13.3 ± 0.03 0.2%

Table 8: Integral dL/L for the three epoxies as measured at the 5 temperatures.

Figure 2: The integral dL/L vs temperature for a representative Tra-Con F113 sample.

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Figure 3: The integral dL/L vs temperature for a representative Epotek 301-2 sample.

Figure 4: The integral dL/L vs temperature for a representative Hysol 9361 sample.

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Figure 5: The temperature vs time for a representative CTE measurement.

Ambient 250 K 200 K 150 K 100 KTra-Con F113 – 2.8 1.1 0.76 0.65Epotek 301-2 – 5.9 2.7 1.5 1.0Hysol 9361 – 2.1 0.83 0.5 0.29

Table 9: The ratio of strain to stress as defined in equation 3.

A criterion that the yield strength must be more than twice the stress leads to the requirementthat

yield strength (epoxy)Modulus× CTE (epoxy)×∆T

> 2. (3)

The stress reported in the data sets is not the epoxy yield strength, it is the strength at0.68% strain. A conservative guideline can still be determined if the maximum stress achievedis used in the calculations as a proof stress. We will use either the room temperature ultimatestrength or the maximum stress applied to the sample at temperature, whichever is larger. Asthe strength is known to increase with decreasing temperature, this selection is a conservativeapproach. In Table 9, we show the ratio of strength over stress as defined above.

The Epotek has the lowest bond strain and, at ambient temperature, the highest ratioof maximum strength to strength at 0.68%. Although none of the epoxies meet the criteriafor temperatures below 200 K, it does not mean the joint will fail. We have chosen to take aconservative approach in the calculation of the maximum stress. In addition, the tensile strengthdata collected was taken at high pull rates (0.10 inch/minute for the PMIC tests). Epoxies, aswith most plastics, are visco-elastic materials which respond differently based on how quicklythe load is transferred to the material. The high rates of strain applied to the samples duringtesting will have a much higher modulus and stress than in the actual application. Duringflight, the CCD focal plane will have a cool down rate of 3 degrees per minute, taking at least20 minutes to achieve operating temperature and allowing the epoxy to creep and relieve some

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of the stresses.

5 Conclusions

We have presented measurements on epoxy properties for use in the SNAP CCD assembly,covering temperatures from ambient to 100 K. Test results on Young’s Modulus, Poisson’sRatio, and integral dL/L have been presented. A criterion for the epoxy has been proposed.

References

[1] NASA-STD-5001 - Structural Design and Test Factors of Safety for Spaceflight Hardware

[2] Young’s Modulus is the ratio of tensile stress to tensile strength and is a measure of howa material changes length under tension or compression. Poisson’s Ratio is defined as thestrain normal to an applied load divided by the strain in the direction of the applied loadand is a measure of the material’s tendency to get thinner as it is stretched or thicker as itis compressed.

[3] Precision Measurements and Instruments Corporation, 3665 SW Deschutes Street, Corval-lis, OR 97333

[4] LVDT stands for Linear Variable Differential Transformer, outputting a voltage dependentupon physical displacement.

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