European Space Agency (ESA), ESTEC (European Space Research and Technology Centre) (1) Materials Space Evaluation and Radiation Effects Section (3)

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1 Elastosil S 69 A Space Qualified European Silicone Material C.O.A. Semprimoschnig (1), D. Pueyo (2), J.R. Williamson (1), C. Mooney (1), C. Zimmermann (2), M. v. Eesbeek (1), S. Taylor (3) European Space Agency (ESA), ESTEC (European Space Research and Technology Centre) (1) Materials Space Evaluation and Radiation Effects Section (3) Solar Generator Section PO BOX 299, Keplerlaan 1, NL - 22 AG Noordwijk, The Netherlands (2) EADS Astrium GmbH, Mϋnchen, Germany Keywords: Silicone Adhesive, Solar Cells, Space environmental effects ABSTRACT Triggered by the interest of European spacecraft manufacturers a new material has been developed and space qualified by ESA and its industrial partners. The material is produced by WACKER Chemie in Burghausen, Germany and is available under the tradename Elastosil S 69. It is a transparent Silicone adhesive and is an improved development of the already space established Elastosil S 695. Potential applications are soft structural bonds such as solar cell coverglass adhesives, high quality pottings and encapsulations as well as transparent bonds for detectors and sensors. ESTEC has carried out an intensive test programme characterising the materials performance with regards to its resistance to UV, temperature and particle radiation. UV testing has been carried out up to 12 e.s.h., particle testing has been done to simulate a 15 year GEO application and thermal endurance has been performed at 2 C for 3 days. At several intermediate points the transmission stability in the UV/VIS/NIR range (2 nm to 25 nm) was measured with a CARY 5 photospectrometer. Finally thermal analysis was performed on BOL materials and after UV, electron radiation exposure and thermal ageing Four different thermal techniques were utilised; TGA, DSC, TMA and DMA across a temperature range of -15 up to 1 (for TGA) to assess the physico-chemical stability of the material. The measurement campaign was performed to compare the performance of Elastosil S 69 to two other space grade materials: Elastosil S 695 and DC93-5 from Dow Corning (USA). Since 27 Elastosil S 69 is considered as space qualified for the herein described application as a coverglass adhesive as well as for high quality pottings qualified in a different ESA programme with Thales Electron Devices. 1. INTRODUCTION Silicone materials find several applications in space programmes due to their attractive properties such as a wide operational temperature range (down to cryogenic temperatures) and high radiation and thermal stability [1][2]. Typical applications are high quality pottings and encapsulations, bonding of detectors, sensors and other parts that do not carry high structural loads. Other uses include as an adhesive to optically couple a coverglass onto a solar cell. This applications is essential as the coverglass needs to protect the solar cell from energetic particle radiation. Therefore the adhesive itself needs to be radiation stable against particles as well as against the part of the UV radiation that can pass through the coverglass. In addition it needs to possess an excellent outgassing behaviour. Recently ESA has been working together with EADS Astrium Ottobrunn to qualify the adhesive for an intended solar cell coverglass adhesive application as well as with Thales Electron Devices in France and Germany to assess the suitability of the material for high quality pottings [1]. This paper will only present the work performed for the first application. 2. EXPERIMENTAL TEST PROGRAMME For solar cell coverglass adhesive applications ESTEC have performed an intensive test programme characterising the materials optical and thermomechanical performance with regards to its resistance

2 to UV, temperature and particle radiation. At the beginning of the test campaign it was decided to include two reference materials for comparison. Elastosil S the previous material available from Wacker - and DC 93-5 from Dow Corning were utilized as the reference materials.. In order to evaluate the effects on optical performance, samples were prepared in a sandwich configuration where the Silicones were cured between two fused silica glass pieces of 1 mm thickness and 19 mm x 19 mm size. The nominal adhesive thickness was 25 µm, which represents a typical thickness used in space. To reach a typical configuration for a coverglass a CMX window from QioptiQ (UK) - typically used on solar cell coverglasses - was placed on top of the Quartz window during the UV irradiation. As the CMX coverglass has a 5% cut-off around 35 nm the hardest UV radiation is therefore shielded from the adhesive. In addition several experimental configurations were evaluated with different filters in order to understand the resistance of the Silicone materials below 4 nm. The emphasis of the results in this paper is however on the CMX configuration as used for solar generators. Furthermore, to evaluate the effects on mechanical performance, tiles of bulk adhesive of 3 mm x 3 mm x 2 mm were prepared. A CMX window from QioptiQ was also placed on top of the tiles during the UV irradiation. UV testing was carried out in ESTEC s SUV facility up to a simulated UV dose of 12 esh (esh = equivalent sun hours) with intermediate inspection points as shown in table. 1. Test temperature on the samples was maintained at 8 C (+3 C/-1 C). The facility is equipped with a LN2 cooled shroud to trap possible contamination. At each test point the transmission stability in the UV/VIS/NIR range (2 nm to 25 nm) was measured with a CARY 5 photospectrometer ex-situ. During intermediate measurements, the exposure of the samples to air was minimized by storing them in a N 2 atmosphere. Table 1. Summary of Test points Test n UV exposure Time [hrs] UV acceleration Accumulated e.s.h. BOT N/A EOT EOT EOT EOT EOT Analysis UV-VIS-NIR, Thermal Analysis UV-VIS-NIR UV-VIS-NIR UV-VIS-NIR UV-VIS-NIR UV-VIS-NIR, Thermal Analysis The dose accumulated during 15 years in a geostationary orbit amounts to 1.8 MGy, with little variation as a function of depth in the adhesive. The main contribution for the total dose are electrons trapped in the radiation belts. The contribution of solar protons is about three orders of magnitude smaller. Therefore electrons are considered the most representative particle for irradiation of the silicone,. Including a 2% margin. Particle testing was carried out up to a total dose of 2.2 MGy by using an electron fluence of e - /cm 2 of 1 MeV electrons and a current of approximately 66 μa. Three identical samples were included for each silicone. The sample temperature was again maintained at around 8 (± 1) and a special enclosure was built to perform the irradiation in a N 2 atmosphere. Thermal endurance has been performed in ESTEC s HITES 2 facility where samples were aged up to 3 days at 2. The samples were enclosed inside a temperature controlled box and a large liquid nitrogen cooled area acted as a cold shroud to limit internal cross contamination. Molecular contamination was monitored with the help of a CaF 2 window according to [4]. After 9, 19 and 3 days intermediate inspections were carried out measuring mass loss as well as transmission stability. Finally, on pristine samples and after UV exposure, electron radiation testing and thermal ageing a full set of thermo-mechanical analysis was performed. Different techniques were used to characterise the adhesive; hardness, TGA, DSC, TMA and DMA. TGA tests were performed in accordance with ISO specification 11358[6] with a heating rate of 1.min -1 and in the temperature range between -15 up to 1. DSC tests were done in accordance with ISO specification 11357[7] with a heat-cool-heat cycle

3 between -15 and 2 and a ramp rate of 1.min -1. TMA tests were performed in accordance with ISO specification [8] between -15 and 2 using a heating rate of 1.min -1. DMA tests were performed in accordance with specification ISO 6721[9] between -15 and 2 and were conducted in a shear mode with a heating rate of 3.min -1. Rubber hardness measurements were performed on samples of the rubber using a Wallace H12/1 Microhardness Tester. Results for microhardness were obtained in International Rubber Hardness Degrees (IRHD). Samples are automatically tested by applying a dead load to the specimen followed by applying a vibrator for 3 seconds before the measurement is taken. This procedure conforms to Method M of reference [5]. In this way a comprehensive assessment of the physico-chemical stability of the material was conducted. 3. RESULTS & DISCUSSION 3.1 UV RESISTANCE The UV-VIS-NIR transmission for all three materials (S 69, S 695 and DC93-5) is shown in Fig. 1 to 3. These samples were irradiated with a CMX coverglass in front of the quartz sandwich; however during transmission measurements the CMX coverglass was removed in order to study the transmission performance down to 2 nm. As expected the degradation of the transmission caused by the formation of radicals and chromospheres is most dominant in the UV and visible region. In order to study the stability in more detail, several approaches were followed. For instance, various individual wave length analyses have been carried out. This showed that for the CMX coverglass configuration no discernable difference can be found at 6, 5 and 4 nm. A small but noticeable difference is however seen when the samples are probed at the 5% cutoff of the CMX coverglass (see Fig. 4). Even though small, it is believed that this is caused by an increased absorption of phenyl-methyl moieties which are present in the Elastosil materials. It should be noted howeverthat DC 93-5 also loses some transmission capability at 35 nm but it is the most stable in this range of wavelengths. Transmission (%) Fig.1: UV-VIS-NIR transmission of S 69 during UV testing campaign Transmission (%) Fig. 2: UV-VIS-NIR transmission of S 695 during UV testing campaign Transmission (%) Normal Transmission sandwich 27 - BOL 6 sandwich 27 - EOT1 5 sandwich 27 - EOT2 4 sandwich 27 - EOT3 3 sandwich 27 - EOT4 sandwich 27 - EOT (nm) Normal Transmission sandwich BOL 6 sandwich EOT1 5 sandwich EOT2 4 sandwich EOT3 3 sandwich EOT4 sandwich EOT (nm) Normal Transmission sandwich BOL 6 sandwich EOT1 5 sandwich EOT2 4 sandwich EOT3 3 sandwich EOT4 sandwich EOT (nm) Fig. 3: UV-VIS-NIR transmission of DC 93-5 during UV testing campaign

4 [%] [%] Table 2: Evolution of sun power intensity (P) as function of UV exposure BOL EOT1 EOT2 EOT3 EOT4 EOT5 [W/m 2 ] [%] [%] [%] [%] [%] S S DC Table 3: Evolution of first junction power loss (I) as function of UV exposure Fig. 4: UV-VIS-NIR transmission of S 69 (blue), S 695 (pink) and DC93-5 (yellow) at 35 nm during UV testing campaign, 3 samples each. To quantify the UV resistance we have calculated the integrated sun power variation as well as the integrated power variation of the first junction in a triple junction solar cell as shown in Fig. 5. Both represent a worst case as the first junction, with an efficiency between 3 nm and 7 nm, is the only one affected by a transmission loss in the UV range. The results are shown in table 2 and table 3. I [esh] 6 [esh] P = 25 2 Fig. 5: ( T T E S ) dλ CMX adhesive ( T T E ) dλ 25 (2 25nm) = CMX adhesive 2 SUN 1st jnnction I: Intensity produced by the first junction. T CMX : spectral CMX transmission T adhesive : spectral adhesive transmission E sun : spectral sun irradiance S 1st junction : spectral first junction response in a GaAs triple junction solar cell Definition: Sun power intensity (P) as well as first junction power loss (I) SUN BOL EOT1 EOT2 EOT3 EOT4 EOT5 [A/m 2 ] [%] [%] [%] [%] [%] S S DC Even though the real power loss of a triple junction solar cell will be much smaller and therefore this is a worst case analysis, all three materials show a rather small predicted power loss of the first junction after 1 e.s.h. Analysing the obtained UV transmission data with a different methodology and extrapolating the predicted power loss to a 15 years lifetime as described in [1], it was estimated that Elastosil S 69 gives comparable power losses to the two reference materials. The maximum predicted power loss is estimated to be less than 2% after 15 years in orbit. 3.2 PARTICLE RESISTANCE The UV-VIS/NIR analysis after electron exposure revealed that both CMX coverglasses and bare fused silica windows are somewhat degraded with electron exposure at low wavelengths. For the CMX coverglasses the degradation is located between cut-off (32 nm) and 45 nm. For the fused silica windows the degradation in the measured range is located between 2 and 35 nm. On this basis, the impact of any degradation of the coverglass adhesive, among the three adhesives studied, due to electron radiation should have no impact on the performance of a solar cell if a CMX coverglass is used. Indeed any possible degradation of the adhesive due to electron radiation would be below the cut-off wavelength of the CMX coverglass. Therefore we can conclude that the impact of the UV-VIS-NIR transmission change after electron irradiation of all three adhesives is negligible.

5 1 Thermal Endurance S695 S695 Transmission [%] Bare CMX - BOL Bare CMX EOT6 CMX sandwiches BOL & CMX sandwich non-e - exposed EOT6 CMX sandwiches e - exposed EOT6 Mass value w.r.t BOT 1,% S695 S69 DC935 DC935 99,5% 99,% 98,5% 98,% 97,5% C Fig. 6: Wavelength [nm] UV-VIS-NIR transmission after electron testing with 1 MEV and 4 x 1 EXP 15 e/cm TEMPERATURE RESISTANCE Initial vacuum screening tests showed that Elastosil S 69 also satisfies the routine outgassing requirement as per [3] in which a total mass loss of less than 1% and a collected volatile condensable materials content of less than.1 % is required. Prolonged thermal exposure ageing of silicone adhesives revealed some degradation in the physical properties and weight loss of the adhesives, although these appear to be quite low. As shown in Fig. 7, S 69 showed the lowest percentage weight loss (about.6%) after 3 days whilst S 695 showed approximately 1 % of mass loss and DC 93-5 showed the highest mass loss (about 2.4%). Visual inspections as well as UV-VIS-NIR transmission indicated negligible changes for S 69 and S 695. Some batch to batch variability was noticed on DC No discolouration was noticed after 3 days and 2 ºC for all three adhesives. From these tests we can conclude that Elastosil S 69 shows a good temperature resistance. Fig. 7: Mass loss as function of time at 2 ºC for S 69 (in blue), S 695 (in pink) and DC 93-5 (in green). 3.4 PHYSICO-CHEMICAL ANALYSIS The first and simplest analysis was to assess the hardness of the three materials after the various experiments. UV exposure (behind a CMX coverglass) results in a larger increase of IRHD than the 2 ºC thermal exposure. Electron irradiation shows the most significant effects in hardness change which suggests that radiation assisted cross-linking is taking place. It is also worthwhile to note that electron irradiation on S 695 was the only experiment where a sufficiently large increase in hardness resulted in the value being measured. Changes of S 69 and DC 93-5 were similar with DC 93-5 giving the highest hardness values after exposure. Table 2: IRHD measured after various exposure conditions. A comparison of the various mass loss curves obtained by TGA analysis is given in Fig. 8, following adjustment to remove the effects of the initial water loss effect. It can be seen that Elastosil S 69 performs well when compared with the other two silicone adhesives. It has a similar onset for mass loss as Elastosil S 695 and shows a slightly higher onset temperature than DC Further it can be seen that following exposure, the changes in the low mass loss region is relatively small and primarily results in a shift in onset to higher temperatures. For all three materials the onset of mass loss is associated with the degradation of the organic

6 components within the silicone elastomer. The relative level of total mass loss (not shown here) is significantly lower for Elastosil S 69 than for either of the other two adhesives both before and after environmental exposure. BOL 2 exposed UV exposed Elastosil S-69 DC 935 Elastosil S-695 highest CTE at around 35 ppm. -1 with DC 93-5 and Elastosil S 69 displaying similar CTE values of around 28-3 ppm. -1 above the glass transition temperature. After electron exposure no change in the Tg as determined by DSC and TMA were observed. However, an apparent decrease of the CTE values was noticed. The decrease is approximately 3-5 ppm. -1 for both S 69 and DC 93-5 with S 695 showing a drop of around 5-8 ppm -1. ppm^-1.2 % Elastosil S-69 DC 935 Elastosil S Fig. 8: Overlay of mass loss as measured by TGA for various exposures, S 69 in green, DC 93-5 in black and S 695 in red. Table 3 shows that all three glass transition temperatures are present in the typical range for silicone materials. Whilst DC 93-5 has the lowest glass transition temperature the differences between all three materials is negligible and unlikely to result in significant performance differences. The glass transition temperatures of the two Elastosil materials are essentially identical. Exposure to the two environments (UV and temperature) resulted in no change in either the position or intensity of the glass transition temperatures for all three materials. Table 3: Tg as measured by DSC of exposed and unexposed materials. Material 1 st Heat Glass Transition 2 nd Heat Glass Transition Elastosil S 69 BOL Elastosil S 69 / Elastosil S 69 / UV -116/ /-117 DC 93-5 BOL DC 93-5 / DC 93-5 / UV -121/ Elastosil S 695 BOL Elastosil S 695 / 2-116/ /-117 Elastosil S 695 / UV A comparison of the three materials CTE values with respect to temperature is given in Fig. 9. As can be seen Elastosil S 695 has the Fig. 9: CTE values at BOL of S 69 (black), DC 93-5 (red) and S 695 (green) as determined by TMA. A comparison of the three materials and the environmental effects on their storage modulus as measured by DMA curves is given in Figure 1 where it can be seen that the three materials have different dynamic moduli values above their glass transition temperature. DC 93-5 has the highest modulus and similarly displays the highest absolute change following UV exposure. However all three undergo a similar relative change in modulus following environmental exposure with each seeing an approximate doubling of the BOL value. Despite the changes observed in all three materials it should be noted that they all retained some elasticity after environmental exposure. After electron exposure an appreciable change in the mechanical behaviour of the two Elastosil materials has been observed by DMA. Both materials display an appreciable increase in storage modulus (by around a factor of 2-3 in both cases). This results in a similar increase in the dynamic modulus which will equate to an approximately equal change to the static or E- modulus. This would normally result in a stiffer material which will be more susceptible to the effects of applied strain e.g. from CTE effects. A note of interest is that the storage modulus curves of the electron beam exposed materials show an upward trend with respect to temperature. This behaviour is counter to the effects that would intuitively be associated with temperature

7 i.e. that the material becomes softer with increasing temperature. DMA analysis for DC 93-5 is given in Figure 12. Whilst there in an appreciable increase in the storage modulus values this is in line with the values observed for the ultraviolet and thermal environments. However it should be noted that whilst the relative increase is approximately the same as for the other environmental conditions with respect to the other silicones the DC 93-5 shows the highest absolute change. MPa DC 935/BOL DC 935/UV 61 DC 935/UV 66 DC 935/2 CROSS MPa Elastosil S-69 DC 935 Elastosil S-695 Curve after UV exposure BOL Curve Fig. 12: E (Storage modulus) for DC 93-5 as determined by DMA after electron exposure (red) and at BOL and after UV exposure (black) 4. Summary and Conclusion 4 2 Fig. 1: E (Storage modulus) values at BOL & after UV exposure of S 69 (green), DC93-5 (black) and S 695 (red) as determined by TMA. MPa Elastosil S-69 E-beam Elastosil S69 BOL Elastosil S69/UV 66 Elastosil S69/UV 64 Elastosil S69/2 CROSS Fig. 11: E (Storage modulus) for S 69 as determined by DMA after electron exposure (blue) and at BOL and after UV exposure (black) For the application as a solar cell coverglass adhesive we have investigated the materials performance with regards to its resistance to UV, temperature and particle radiation. UV testing has been carried out up to 12 e.s.h., particle testing has been done simulating a 15 year GEO application and thermal endurance has been done at 2 C for 3 days. At each point the transmission stability in the UV/VIS/NIR range (2 nm to 25 nm) was measured with a CARY 5 photospectrometer. Finally, on the pristine materials, after the UV and electron radiation testing as well as after the thermal ageing a full set of thermal analysis has been carried out. Techniques such as hardness, TGA, DSC, TMA and DMA analysis were performed to assess the physico-chemical stability of the material. The whole measurement campaign has been conducted comparing the performance of Elastosil S 69 to two other space grade materials: Elastosil S 695 also from Wacker Chemie (Germany) and DC 93-5 from Dow Corning (USA). A coverglass like CMX will protect the adhesive and the solar cell from the most damaging forms of UV and energetic particle radiations and Elastosil S 69 shows acceptable resistance for that application. Thermomechanical analysis before and after UV radiation, particle radiation and thermal ageing 3 days at 2 showed stable properties of Elastosil S 69. Following the intensive test programme characterising the newly developed Elastosil S 69 from Wacker Chemie in Burghausen, Germany, we consider Elastosil S 69 as a suitable alternative to DC 93-5 and a suitable replacement for Elastosil S 695.

8 Since 27 Elastosil S 69 is therefore considered space qualified for the herein described application as a coverglass adhesive as well as for high quality pottings qualified in a different ESA programme with Thales Electron Devices [1]. REFERENCES [1] Introduction and Qualification of Elastosil S69 as a New High Voltage Encapsulant for Travelling Wave Tubes for Space Application, H.G. Seidel, B. Graf, N.T. Nguyen, 11 th ISMSE, Aix en Provence, France 29 [2] ECSS Q 7 71, Data for the selection of space materials, ESA/ESTEC, The Netherlands, February 24 [3] ECSS-Q-ST-7-2C Thermal vacuum outgassing test for the screening of space materials, ESA/ESTEC, The Netherlands, Nov. 28 [4] ECSS-Q-ST-7-5C Detection of organic contamination of surfaces by IR spectroscopy ESA/ESTEC, The Netherlands, March 29 [5] ISO Specification 48 Rubber, vulcanized or thermoplastic - Determination of hardness (hardness between IO IRHD and I IRHD). [6] ISO Specification 11358, Plastics Thermogravimetry (TG) of Polymers General Principles, International Standards Organisation, [7] ISO Specification 11357, Plastics Differential Scanning Calorimetry (DSC), International Standards Organisation, [8] ISO Specification , Plastics Plastics Thermomechanical analysis (TMA) - Part 1: General principles, International Standards Organisation, [9] ISO Specification 6721, Plastics Determination of dynamic mechanical properties, International Standards Organisation, 21. [1] END-OF-LIFE PERFORMANCE EVALUATION OF A NEW COVERGLASS ADHESIVE, C. Zimmermann, D. Pueyo, C. Semprimoschnig and S. Taylor, 8 th ESPC, Konstanz/Germany, 28

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