Author's personal copy Cryogenics 48 (2008) 497–510 Contents lists available at ScienceDirect Cryogenics journal homepage: www.elsevier.com/locate/cryogenics Measurement of mechanical properties of electronic materials at temperatures down to 4.2 K M. Fink a,*, Th. Fabing a, M. Scheerer a, E. Semerad a, B. Dunn b a b ARC Seibersdorf Research GmbH, 2444 Seibersdorf, Austria ESA/ESTEC, 2200 AG Noordwijk, The Netherlands a r t i c l e i n f o Article history: Received 30 October 2007 Received in revised form 25 June 2008 Accepted 16 July 2008 Keywords: Solder PCB Conformal coating Material characterisation Tensile test a b s t r a c t Operating temperatures of spacecraft components in the ‘subzero’ range are encountered during solar eclipse periods or when voyaging on deep-space missions. Moreover some spacecraft instruments or parts of them, e.g. sensors, have to be cooled to obtain an improved performance, e.g. in spacecraft missions like the infrared space observatory (ISO) and CryoSat. Materials utilized in the assembly of electronic circuits can be subjected to mechanical loading at cryogenic temperatures. [Semerad E, Scholze P, Schmidt M, Wendrinsky W. Effect of new cleaning liquids on electronic materials and parts. ESA metallurgy report no. 3275; January 2002, [1]]. Within the present work the mechanical properties of electronic materials at cryogenic temperatures down to liquid helium temperature were analysed. Specifically the tensile properties of solders (63Sn37Pb, 62Sn36Pb2Ag, 60Sn40Pb, 96Sn4Ag, 50In50Pb, 70Pb30In, 96.8Pb1.5Ag1.7Sn, 96.5Sn3Ag0.5Cu), PC boards (MLB polyimide glass fibre, MLB epoxy glass fibre, MLB Thermount), conformal coatings (Arathane 5750, Sylgard 184, Scotchcast 280, Solithane 113, CV-1144-0, Mapsil 213, Conathane EN4/EN11) as well as OFE Cu were characterised at room temperature, at liquid nitrogen and at liquid helium temperature by tensile tests. The fracture surface of tested samples was examined by means of optical microscope and if necessary with scanning electron microscope. Ó 2008 Elsevier Ltd. All rights reserved. 1. Introduction The objective of the present work was to check the reliability of OFE Cu, solders, PC boards, and conformal coatings at low operating temperatures. Specifically the temperature dependence from room temperature (RT) down to 4.2 K (LHe) of following materials properties was characterised Young’s modulus. Proof stress. Elongation at rupture. Ultimate tensile strength. OFE copper was delivered from Goodfellow GmbH [12] in form of an as drawn rod (diameter: 12.7 mm, length: 1000 mm, purity: better than 99.95%). The rod was cut into pieces of about 80 mm. These specimens were machined according to ASTM-E8. The round tensile specimen had a reduced length of 30 mm with a diameter * Corresponding author. Tel.: +43 505503384; fax: +43 505503366. E-mail address: markus.fi[email protected] (M. Fink). 0011-2275/$ - see front matter Ó 2008 Elsevier Ltd. All rights reserved. doi:10.1016/j.cryogenics.2008.07.006 of 5 mm and threaded ends of M9x1.5. The single specimens were taken arbitrarily for the tests at room temperature, at LN2- and at LHe temperature. The solders (except of 96.5Sn3Ag0.5Cu) delivered from JL Goslar GmbH had a length of about 400 mm and a triangle profile. To get samples having the same geometry like the OFE copper specimens, the raw solder bars had to be melt to a rod with a length of at least 70 mm. The raw solder materials were squeezed to a roughly round form that fits in glass tubes with an inner diameter of 10 mm and a length of 100 mm. To avoid hollows in the casted solder rods and to get comparable results with previous investigations [2,3], the melting process took place under vacuum (10E-2 mbar) at casting temperatures shown in Table 1. The melting temperatures of the solders are also given in this table. The parameters for casting were chosen in accordance to previous investigations [2] and [3] to ensure comparable results. In Fig. 1 a typical solder rod after casting is shown. The cast rods were cleaned, identified as well as end trimmed and machined according to ASTM-E8. The round tensile test specimens had a reduced length of 30 mm with a diameter of 5 mm and threaded ends of M9x1.5 like the OFE Cu samples. The solder 96.5Sn3Ag0.5Cu was delivered in form of a bar (48 4 2 cm3). From this bar the round tensile test samples Author's personal copy 498 M. Fink et al. / Cryogenics 48 (2008) 497–510 Table 1 Solder Melting range (°C) Solid 63Sn37Pb 62Sn36Pb2Ag 60Sn40Pb 96Sn4Ag 50In50Pb 70Pb30In 96.8Pbl.5Agl.7Sn 96.5Sn3Ag0.5Cu Casting temperature (°C) Liquid 183 183 240 180 190 240 183 190 240 221 221 240 180 209 240 220 255 270 304 310 340 Tested in as-received condition! Fig. 3. Taped PCB samples. Fig. 1. Vacuum casted solder rod. could be cut directly. Thus, a direct comparison of the measured values of 96.5Sn3Ag0.5Cu with the other solders should be regarded carefully. In Fig. 2 a solder tensile test specimen is shown. The tensile specimens were checked by means of ultrasonic inspection. Samples with any hollows were rejected. The PCB’s were delivered from GPV Printca A/S. The dimensions of all specimens were nearly identical, i.e. approx. 200 mm in length, 20 mm in width and 1.6 mm in thickness. The core material is 0.2 mm thick. It is pressed into a 1.6 mm sandwich (due to a real board contain several layers). For clamping in the specimen holder the thickness of the samples should be about 8 mm. Due to the thickness of the samples of 1.6 mm and to assure that they are not harmed when clamping them, their ends were taped with a 40 mm long glass fibre reinforced polymer. In Fig. 3 a sample of every PCB material prepared for tensile test is shown. The conformal coatings consisted of three silicones, three polyurethanes and one epoxy system, which where evaluated for spacecraft applications in previous technical notes [4]. These conformal coatings have either an extensive usage in the fabrication of spacecraft or are expected to pass the ESA requirements for outgassing, offgassing, toxicity and flammability. The materials delivered from ESA had a form of 20 20 cm2. Fig. 2. Solder tensile test specimen. Fig. 4. Conformal Coating tensile test specimen. The samples had to be trumped by means of a special formed cutter. A photo of a Solithane 113 tensile specimen is shown in Fig. 4. Before clamping the specimens in the sample holder, they were taped with spare material of Solithane 113 to assure that they are not harmed when clamping. 2. Experimental details The tests included Ultrasonic Inspection of the samples. Tensile tests at room temperature as well as at cryogenic temperatures down to 4.2 K. Visual inspection and surface analysis by optical microscope and scanning electron microscope (SEM). Before tensile tests started, all samples were checked with ultrasonic inspection which was done by means of a automated scanning ultrasonic testing facility type panametrics multiscan with an immersion tank using a 20 MHz focused immersion transducer type: V317/188237 with a focal length of 28 mm in impulseecho mode. For scanning the transducer was placed 23 mm above the surface of the sample – that means the focal point of the transducer was adjusted to the axis of the sample. The samples were rotated around their axis and the transducer was moved along the axis giving a rectangular winding-up c-scan of the whole cylindrical part of the sample. To prove the detectable pore size, holes of different diameters were drilled in the samples and the pre-damaged samples were inspected. Defects > 0.4 mm could be detected. Samples with any failure larger than the minimum detectable size were rejected. The test campaigns were carried out on a class I universal testing machine. The load cells and the extensometers have been calibrated on site by the certified calibration service of Messphysik Laborgeräte GmbH/Austria based on standards issued by BEF, the supreme Austrian authority for standards and calibration. The calibration certificates state accuracies of ±0.5% of the selected load Author's personal copy M. Fink et al. / Cryogenics 48 (2008) 497–510 499 Fig. 5. Arrangement for tensile testing at 4.2 K in LHe featuring the 4 column testing machine, the LHe – cryostat containing the specimen (black cylindrical object). range, ±0.005 mm of the machines stroke indicator and ±0.5% of the extensometers gauge length. Tests were performed with a constant cross-head speed of 1 mm/min and a tensile preload of 10–20 N. The extensometer was calibrated and ‘‘zeroed” at preload level prior of each test. The mechanical properties calculated after completion of each test were based on the recorded signals of the load cell, the cross-head position sensor and the extensometer. Measurements at room temperature were performed with a video extensometer. Tensile tests at 77 K (LN2 temperature) were performed by means of a liquid nitrogen bath mounted in the tensile test machine. Measurements at cryogenic temperature were made with a special low temperature extensometer. Tensile properties at 4.2 K (LHe temperature) were measured by means of a LHe – cryostat mounted in a mechanical testing machine (Fig. 5). The cryostat is described in detail in [5]. By means of this experimental setup tensile measurements with a maximum load of 200 kN at cryogenic temperatures down to 4.2 K can be per- Fig. 6. Stress/strain diagram as recorded by means of a PC. Fig. 7. Solder sample before and after tensile test at 4.2 K. Author's personal copy 500 M. Fink et al. / Cryogenics 48 (2008) 497–510 3. Test results At least 3 tensile specimens of each material and each temperature were tested. In Fig. 7 a solder sample, in Fig. 8 a PCB sample, and in Fig. 9 a conformal coating sample mounted in sample holder before and after tensile test at 4.2 K are shown. The data are given in Tables 2–20. In Figs. 10–13 the average values of the temperature dependence of Young’s modulus E, ultimate tensile strength Rm, proof stress Rp0.2, and elongation at rupture A are plotted. An exception is the elongation at rupture of OFE Cu at room temperature (Fig. 13). Due to fracture outside of the extensometer of Test Nos. 24 and 26, it is expected that only the elongation of test 147 is a valid factor. So, this value is shown in Fig. 13. For this reason the A-values of Test Nos. 24 and 26 in Table 2 are marked with a red exclamation mark. Before each tensile test, the samples were measured by means of a micrometer screw (accuracy: +/ 0.01 mm). Applying the low Table 2 OFE Cu E (kN/ mm2) Fmax (N) Rm (N/ mm2) Rp0.2 (N/ mm2) A (%) RT 24 1-1 26 1-3 147 1-7 Average Standard deviation 108.024 109.649 108.284 108.652 0.873 7287.6 7317.0 7528.0 7377.530 131.138 388.00 381.80 389.61 386.470 4.124 386.79 381.03 388.14 385.320 3.776 0.255 0.453 15.876 5.528 8.962 77 K 50 1-4 51 1-5 52 1-6 Average Standard deviation 123.700 121.900 124.600 123.400 1.375 9939.0 9872.0 98200 9877.000 59.657 508.20 515.00 5124.0 511.867 3.431 456.50 464.20 452.90 457.867 5.773 16.750 11.760 12.330 13.613 2.731 4.2 K 18 1-1 19 1-2 82 1-3 Average Standard deviation 137.200 129.500 127.200 131.300 5237 9472.0 9315.0 11259.0 10015.333 1079.904 490.20 488.00 582.70 520.300 54.051 298.70 307.90 494.30 366.967 110.370 24.850 28.340 44.760 32.650 10.632 ChNo E (kN/ mm2) Fmax (N) Rm (N/ mm2) Rp0.2 (N/ mm2) A (%) RT 32 2–3 34 2–5 35 2–6 Average Standard deviation 16.120 18.997 20.584 18.567 2.263 562.0 559.4 553.3 558.233 4.466 28.74 28.60 28.29 28.543 0.230 27.38 27.75 27.56 27.563 0.185 73.741 57.628 24.650 52.006 25.024 77 K 56 2–7 57 2–8 58 2–9 Average Standard deviation 38.820 35.970 38.930 37.907 1.678 2210.0 2179.0 1923.0 2104.000 157.515 115.80 113.30 101.60 110.233 7.580 87.85 83.08 93.36 88.030 5.151 1.083 1.189 0.408 0.893 0.424 4.2 K 21 2–1 23 2–3 87 2–5 Average Standard deviation 43.820 41.440 43.410 42.890 1.272 2698.0 2753.0 2497.0 2649.333 134.760 138.00 140.80 129.00 135.933 6.165 122.10 111.50 115.10 116.233 5.390 0.262 0.413 0.267 0.314 0.086 Test no. Fig. 8. PCB sample before and after tensile test at 4.2 K. ChNo Table 3 63Sn 37Pb Test no. Fig. 9. Conformal Coating sample before and after tensile test at 4.2 K. formed. A special top loading mechanism enables a quick change of the samples. Therefore, no heating up of the cryostat between the tests is warranted and so, the cooling down time of specimen is less than 2 h (big samples, like PCB’s) and less than 1 h (smaller samples, like OFE copper, solders and conformal coatings). During each tensile test a stress/strain diagram is plotted, from which the tensile properties were evaluated. Fig. 6 shows a typical one. Author's personal copy 501 M. Fink et al. / Cryogenics 48 (2008) 497–510 Table 4 62Sn 36Pb 2Ag Table 6 96Sn 4Ag ChNo E (kN/ mm2) Fmax (N) Rm (N/ mm2) Rp0.2 (N/ mm2) A (%) RT 15 3-1 16 3-2 17 3-3 Average Standard deviation 38.517 39.164 32.640 36.774 3.594 838.5 853.9 798.4 830.267 28.651 43.05 43.84 41.00 42.630 1.466 40.69 42.30 39.30 40.763 1.501 8.142 5.871 10.340 8.118 2.235 77 K 38 3-4 39 3-5 40 3-6 Average Standard deviation 41.230 38.560 38.830 39.540 1.470 2065.0 2067.0 2186.0 2106.000 69.289 105.60 105.70 112.20 107.833 3.782 80.67 83.77 87.64 84.027 3.492 4.2 K 24 3-1 25 3-2 26 3-3 Average Standard deviation 39.650 38.630 30.840 36.373 4.819 3187.0 2598.0 2815.0 2833.667 297.880 164.90 134.40 145.10 148.133 15.475 109.00 120.10 106.60 111.900 7.202 Test no. E (kN/ mm2) Fmax (N) Rm (N/ mm2) Rp0.2 (N/ mm2) A (%) RT 67 5-7 69 5-9 151 5-10 Average Standard deviation 58.346 57.020 66.432 60.599 5.095 590.6 656.2 636.0 627.590 33.593 30.94 33.83 32.52 32.430 1.447 18.97 32.51 26.73 26.070 6.794 29.830 2.011 44.326 25.389 21.504 1.024 0.522 0.682 0.743 0.256 77 K 59 5-1 60 5-2 61 5-3 Average Standard deviation 33.420 35.550 34.280 34.417 1.072 1477.0 1455.0 1346.0 1426.000 70.150 76.43 75.33 70.23 73.997 3.308 50.37 60.05 62.48 57.633 6.406 0.912 0.507 0.295 0.571 0.313 0.507 0.388 0.774 0.556 0.198 4.2 K 16 5-2 38 5-5 44 5-6 Average Standard deviation 46.480 42.380 42.600 43.820 2.306 1615.0 1563.0 1609.0 1595.667 28.449 84.24 79.61 82.27 82.040 2.324 n.a. n.a. n.a. 0.100 0.011 0.056 0.056 0.045 E (kN/ mm2) Fmax (N) Rm (N/ mm2) Rp0.2 (N/ mm2) A (%) Table 5 60Sn 40Pb Test no. ChNo Table 7 50In 50Pb ChNo E (kN/ mm2) Fmax (N) Rm (N/ mm2) Rp0.2 (N/ mm2) A (%) RT 21 4-1 22 4-2 23 4-3 Average Standard deviation 25.050 25.980 25.690 25.573 0.476 832.3 820.4 807.3 820.000 12.505 42.73 42.46 41.78 42.323 0.490 39.61 39.73 38.99 39.443 0.397 11.530 15.180 21.590 16.110 5.093 RT 12 6-1 14 6-3 87 6-11 Average Standard deviation 7.361 7.860 6.197 7.139 0.853 635.3 639.3 556.4 610.333 46.750 33.69 33.08 28.91 31.893 2.602 21.03 22.61 19.48 21.040 1.585 8.869 8.837 9.319 9.008 0.270 77 K 47 4-4 48 4-5 49 4-6 Average Standard deviation 42.770 40.470 38.070 40.437 2.350 2030.0 2100.0 1908.0 2012.667 97.167 105.10 109.10 99.14 104.447 5.012 75.68 74.62 81.09 77.130 3.470 1.377 2.263 1.050 1.563 0.628 77 K 42 6-7 43 6-8 153 6-12 Average Standard deviation 11.590 10.320 14.524 12.145 2.156 1145.0 1126.0 1142.4 1137.800 10.301 58.76 58.29 59.89 58.980 0.822 34.05 31.96 33.40 33.137 1.070 25.150 34.070 41.100 33.440 7.994 4.2 K 28 4-2 29 4-3 88 4-4 Average Standard deviation 42.500 42.730 44.560 43.263 1.129 2708.0 2735.0 2697.0 2713.333 19.553 143.60 144.40 139.00 142.333 2.914 119.70 108.70 115.70 114.700 5.568 0.529 0.773 0.882 0.728 0.181 4.2 K 31 6-1 33 6-3 85 6-5 Average Standard deviation 14.440 14.720 13.400 14.187 0.696 1329.0 1331.0 1735.0 1465.000 233.829 69.07 70.00 88.38 75.817 10.890 37.77 39.80 21.41 32.993 10.083 26.720 22.950 12.730 20.800 7.239 Test no. of error propagation a deviation of the measurements of +/ 5% is roughly estimated. The Young’s modulus of OFE Cu is superior to all other tested materials. For the conformal coatings the lowest values were found. The temperature dependence of the elastic modulus is for all tested PCB’s the same. The Young’s modulus increases at lower temperatures. PCB 2301 MLB epoxy glass fibre has the highest Young’s modulus of the PC boards, PCB Thermount the lowest one at all temperatures investigated. The Young’s modulus of the conformal coatings increases from a few thousandth GPa at RT to a few GPa at low temperatures. An exception is Arathane 5750 as well as Scotchcast 280. Their stiffness is at RT not so low. At 4.2 K the elastic modulus of Solithane 113 is superior to the rest of the tested conformal coatings. The In-based solders have the lowest elastic modulus of all tested solders. Test no. ChNo OFE Cu- and PCB-values of the ultimate tensile strength are superior to all tested solders and conformal coatings. The Sn-based solders show relative high Rm-values, accept of the Ag-doted materials, their strength is in the range of 50In50Pb. 96.5Sn3Ag0.5Cu is an exception, probably due to the Cu-content. At RT and at 77 K (=LN2) the strength of PCB 2301 MLB epoxy glass fibre is the highest one of the tested PC boards, at 4.2 K PCB 2302 MLB polyimide glass fibre shows the highest ultimate tensile strength of the 3 PCB’s. The tensile strength of PCB Thermount is at all temperatures investigated the lowest one compared with the other 2 PCB’s. The temperature dependence of the tensile strength of Arathane 5750, Sylgard 284, Scotchcast 280, Solithane 113 and Conathane EN4/EN11 shows a maximum at 77 K and a minimum at RT. This devolution is in high gear with Conathane EN4/EN11 and not so strong with Sylgard 184. The strength of CV-1144-0 and Mapsil 213 increases clearly at 4.2 K. For low temperatures the strength Author's personal copy 502 M. Fink et al. / Cryogenics 48 (2008) 497–510 Table 8 70Pb 30In Table 10 96.5Sn 3Ag 0.5Cu ChNo E (kN/ mm2) Fmax (N) Rm (N/ mm2) Rp0.2 (N/ mm2) A (%) RT 71 7-4 72 7-5 88 7-7 Average Standard deviation 12.170 11.063 12.663 11.965 0.819 508.0 431.0 473.0 470.667 38.553 26.29 22.30 23.99 24.193 2.003 21.50 n.a. 19.98 20.740 1.075 3.502 0.171 4.654 2.776 2.328 77 K 62 7-1 63 7-2 73 7-6 Average Standard deviation 20.110 19.450 17.580 19.047 1.312 528.8 727.8 865.8 707.467 169.418 27.15 37.67 44.99 36.603 8.968 21.10 26.66 25.89 24.550 3.012 4.2 K 34 7-1 35 7-2 43 7-4 Average Standard deviation 11.510 13.560 12.740 12.603 1.032 687.6 856.6 710.8 751.667 91.612 36.02 45.43 36.79 39.413 5.225 ChNo E (kN/ mm2) Fmax (N) RT 18 8-1 20 8-3 154 8-3 Average Standard deviation 22.665 18.554 22.490 21.233 2.330 549.6 466.6 606.8 540.987 70.476 77 K 44 8-4 45 8-5 46 8-6 Average Standard deviation 37.770 38.910 35.560 37.413 1.703 1033.0 1015.0 1071.0 1039.667 28.589 52.62 52.34 54.98 53.313 1.450 19.18 17.27 16.80 17.750 1.261 11.330 12.060 25.050 16.147 7.719 4.2 K 41 8-2 42 8-3 46 8-4 Average Standard deviation 32.150 29.980 30.610 30.913 1.116 1405.0 1643.0 2020.0 1689.333 310.107 71.28 83.34 104.50 86.373 16.816 17.42 19.08 17.47 17.990 0.944 16.080 17.030 16.660 16.590 0.479 Test no. E (kN/ mm2) Fmax (N) Rm (N/ mm2) Rp0.2 (N/ mm2) A (%) RT 89 19-7 148 19-8 149 19-9 Average Standard deviation 15.484 15.207 14.626 15.106 0.438 564.2 594.1 656.3 604.837 46.962 29.20 20.38 33.29 27.623 6.598 25.92 25.35 28.51 26.593 1.684 48.270 46.875 42.245 45.797 3.154 4.531 7.130 27.060 12.907 12.326 77 K 53 19-4 54 19-5 55 19-6 Average Standard deviation 34.960 34.700 29.020 32.893 3.357 2440.0 2126.0 2672.0 2412.667 274.024 128.30 110.50 138.30 125.700 14.081 92.97 84.76 88.68 88.803 4.106 0.711 0.535 0.916 0.721 0.191 30.63 35.75 35.08 33.820 2.783 6.407 6.715 0.423 4.515 3.547 4.2 K 12 19-1 13 19-2 83 19-5 Average Standard deviation 41.770 39.730 41.590 41.030 1.129 1951.0 2892.0 3156.0 2666.333 633.404 99.36 146.10 160.70 135.387 32.043 n.a. 132.50 151.20 141.850 13.223 0.012 0.314 0.218 0.181 0.154 Rm (N/ mm2) Rp0.2 (N/ mm2) A (%) 28.21 23.95 31.40 27.853 3.738 20.53 12.10 22.87 18.500 5.665 34.610 39.310 23.716 32.545 7.999 Table 9 96.8Pb 1.5Ag 1.7Sn Test no. Test no. Table 11 PCB 2302 MLB polyimide glass fibre Test no. of Solithane 113 is superior to the other conformal coatings and it is in the range of the values found for most solders. The proof stress of OFE Cu is superior to all other materials tested. The Sn-based solders show similar temperature dependence. The proof stress of 96Sn4Ag was not detectable at 4.2 K because of its peculiar stress/strain diagram. The proof stress at low temperatures, particularly at 4.2 K, of 96.5Sn3Ag0.5Cu is superior to the rest of the solders. The proof stress of PCB 2302 MLB polyimide glass fibre is the same for RT and low temperatures, PCB 2301 MLB epoxy glass fibre has the highest proof stress of the three tested PCB’s, particularly at 4.2 K. The proof stress of PCB Thermount is in the range of PCB 2302 MLB polyimide glass fibre. The proof stress at room temperature is very low (between 0.1 and 1 MPa) for all conformal coatings tested. It has a clear maximum value at 77 K (between 41 and 83 MPa). The values found ChNo RT 1 4 142 Ch-No E (kN/ mm2) Fmax (N) Rm (N/ mm2) Rp0.2 (N/ mm2) A (%) PCB 9/1 PCB 9/3 PCB 9/ 10 23.510 22.960 22.614 8682.0 8268.0 8243.1 242.30 223.90 216.02 159.00 154.20 168.14 0.642 0.549 0.416 23.028 0.452 8397.700 246.526 227.407 13.486 160.447 7.082 0.536 0.114 25.940 25.860 25.878 15458.0 15732.0 15381.0 397.80 403.40 392.52 154.10 160.10 166.16 3.719 3.546 2.135 25.893 0.042 15523.667 184.484 397.907 5.441 160.120 6.030 3.133 0.869 30.520 31.490 28.320 30.110 1.624 14910.0 15127.0 16012.0 15349.667 583.769 398.60 413.30 417.20 409.700 9.809 158.30 165.20 158.10 160.533 4.043 1.484 1.350 1.997 1.610 0.342 Average Standard deviation 77 K 130 131 159 PCB 9/4 PCB 9/5 PCB 9/63 Average Standard deviation 4.2 K 1 PCB 9/7 2 PCB 9/8 3 PCB 9/9 Average Standard deviation at 4.2 K are in between. At 4.2 K the proof stress of Solithane 113 is superior to the rest of the tested conformal coatings. The elongation at rupture of all Sn-based solders is at low temperatures very low. OFE Cu and the Pb-based solders show a higher elongation at rupture at cryogenic temperatures. For the PC boards the elongation is in the range of a few p.c. At room temperature the elongation of PCB 2301 MLB epoxy glass fibre is superior to the rest of the PCB’s. At low temperatures the elongation of PCB 2302 MLB polyimide glass fibre is the highest one of all tested PC boards. The conformal coatings show very high elongations at RT, at low temperatures the elongation decreases rapidly. At 77 K Mapsil 213 has the highest elongation, at 4.2 K the elongation of Arathane 5750 is superior to the rest of the conformal coatings. Author's personal copy 503 M. Fink et al. / Cryogenics 48 (2008) 497–510 Table 12 PCB 2301 MLB epoxy glass fibre Table 14 Arathane 5750 Rm (N/ mm2) Rp0.2 (N/ mm2) A (%) 11890.0 11802.0 12403.0 12031.667 324.580 348.00 333.80 367.10 349.633 16.710 223.71 208.10 232.90 221.570 12.538 1.952 1.893 2.033 1.959 0.070 27.270 26.734 22528.0 18943.0 609.10 513.20 302.80 320.40 3.833 2.709 26.149 21359.0 563.70 311.30 1.401 Average Standard deviation 26.718 0.561 20943.333 1828.289 562.000 47.973 311.500 8.802 2.648 1.217 4.2 K 4 5 11 PCB 10/7 PCB 10/8 PCB 10/ 11 33.180 33.400 34.300 14684.0 12842.0 11755.0 398.40 352.40 319.0 304.40 331.00 314.80 0.648 0.315 0.207 Average Standard deviation 33.627 0.593 13093.667 1480.629 356.600 39.866 316.733 13.405 0.390 0.230 Ch-No E (kN/ mm2) Fmax (N) Rm (N/ mm2) Rp0.2 (N/ mm2) A (%) PCB 11/1 PCB 11/2 PCB 11/3 16.090 17.080 14.870 16.013 1.107 7472.0 7825.0 8039.0 7778.667 286.326 194.70 205.80 207.40 202.633 6.917 187.20 159.90 179.10 175.400 14.021 1.439 1.559 1.670 1.556 0.116 16.210 16.200 16.750 16.387 0.315 7345.0 8553.0 8218.0 8038.667 623.648 178.30 213.20 200.10 197.200 17.630 151.90 n.a. n.a. 151.900 1.264 1.331 0.934 1.176 0.213 PCB 11/7 PCB 11/8 PCB 11/ 11 25.530 22.070 23.090 8791.0 9089.0 9000.0 223.50 225.10 225.70 194.00 193.00 203.80 0.438 0.393 0.326 Average Standard deviation 23.563 1.778 8960.000 152.974 224.767 1.137 196.933 5.968 0.386 0.056 Test no. RT 5 6 7 Average Standard 77 K 135 138 160 E (kN/ mm2) Fmax (N) 22.629 23.350 23.818 23.266 0.599 PCB 10/5 PCB 10/ 6-1 PCB 10/ 6-4 Ch-No PCB 10/1 PCB 10/2 PCB 10/3 deviation eB (%) rM (N/ mm2) rS0.2 (N/ 27.8 23.1 20.3 2.07 1.95 1.71 0.43 0.29 0.39 170.000 146.5000 134.500 3.000 0.000 23.753 3.807 1.910 0.183 0.368 0.074 150.333 18.058 77 K 83 12-5 84 12-6 90 12-7 Average Standard deviation 4.160 3.894 4.002 4.019 0.134 1723.0 1493.0 1637.0 1617.667 116.212 132.40 118.80 125.80 125.667 6.801 72.90 64.41 73.90 70.403 5.214 4.197 4.312 3.975 4.161 0.171 4.2 K 49 12-1 56 12-2 67 12-4 Average Standard deviation 1.830 1.983 1.786 1.866 0.103 1253.0 1085.0 670.0 1002.667 300.094 98.33 95.07 69.16 87.520 15.984 21.16 18.47 18.67 19.433 1.499 8.018 8.850 8.093 8.320 0.460 E (kN/ mm2) Fmax (N) rM (N/ rS0.2 (N/ mm2] eB (%) mm2) RT 110 13-6 111 13-7 112 13-6 Average Standard deviation 0.001 0.001 0.001 0.001 0.000 19.4 21.9 19.8 20.370 1.318 2.19 2.54 2.36 2.363 0.175 0.36 0.34 0.27 0.325 0.045 100.400 103.500 102.700 102.200 1.609 77 K 80 13-3 81 13-4 82 13-5 Average Standard deviation 3.468 3.018 3.501 3.329 0.270 494.7 474.5 477.4 482.200 10.922 60.66 55.92 55.90 57.493 2.742 58.98 53.53 51.76 54.757 3.763 2.150 2.227 2.224 2.200 0.044 4.2 K 58 13-3 66 13-4 80 13-7 Average Standard deviation 2.880 2.221 3.058 2.720 0.441 429.0 499.0 467.0 465.000 35.043 49.57 53.01 53.33 51.970 2.085 20.62 17.70 14.55 17.623 3.036 3.61 4.39 2.07 3.355 1.183 Test no. RT 75 76 143 ChNo E (kN/ mm2) Fmax (N) 12-2 12-3 1211 3.000 3.000 3.000 Average Standard deviation mm2) Table 13 PCB Thermount Test no. RT 8 9 10 Average Standard 77 K 136 137 141 Average Standard 4.2 K 6 7 8 deviation PCB 11/4 PCB 11/5 PCB 11/6 deviation For PCB bare materials and conformal coatings we found the following: In Fig. 14 the decomposition of the PCB 2302 MLB polyimide glass fibre-sandwich in its single layers after tensile test particularly at cryogenic temperatures is shown. PCB 2301 MLB epoxy glass fibre is by far not so decomposited, but several cracks are found after tensile tests (Fig. 15). The fracture surface is smooth compared to PCB Thermount and looks similar at all temperatures investigated (Fig. 16). The specimens of PCB Thermount looks similar to those of PCB 2301 MLB epoxy glass fibre after tensile tests but fewer cracks were found. At room temperature and at 77 K the singular strings can be seen in the fracture surfaces. At 4.2 K the fracture is a little bit smoother, comparable with the fracture surfaces of PCB 2301 MLB epoxy glass fibre. The reason could be that the Young’s modulus of PCB Thermount is at 4.2 K in the range of PCB 2301 MLB epoxy glass fibre, at RT and 77 K it is clearly lower. At room temperature the fracture surface of all conformal coatings investigated is very smooth; at low temperatures it is more Table 15 Sylgard 184 Test no. ChNo and more brittle. In Fig. 17 photos taken with optical microscope and in Fig. 18a–c SEM pictures of the fracture surface of Solithane 113 after tensile tests performed at room temperature, at 77 K and at 4.2 K are shown. For all comparison with data from literature it should be considered that the grain size of the solder influences the flow stress as outlined in [6]. For OFE Cu and the solders investigated we found in detail: 3.1. OFE copper (after [12]: CV007960) No thermal treatment was applied, but the variety of the mechanical properties of drawn wires, rolled foils or galvanic films should be considered. Aloud [12] the used Cu was delivered in form of a drawn rod and has a purity of better than 99.95%. Author's personal copy 504 M. Fink et al. / Cryogenics 48 (2008) 497–510 Table 16 Scotchcast 280 Table 18 CV-1144-0 rS0.2 (N/ mm2) eB (%) mm2) 70.7 66.8 57.6 64.997 6.728 10.00 11.02 10.69 10.570 0.520 0.74 0.73 0.83 0.769 0.057 105.500 91.660 93.810 96.990 7.448 4.239 4.053 4.932 4.408 0.463 600.4 597.0 464.1 553.833 77.730 98.46 108.80 113.60 106.953 7.737 81.74 78.02 88.87 82.877 5.514 2.900 3.090 3.198 3.063 0.151 554.1 956.0 503.0 671.033 248.107 64.56 98.59 81.50 81.550 17.015 25.33 26.83 27.39 26.517 1.065 E (kN/ mm2) Fmax (N) RT 113 14-4 114 14-5 115 14-6 Average Standard deviation 0.199 0.261 0.321 0.260 0.061 77 K 91 14-1 92 14-2 93 14-3 Average Standard deviation 4.2 K 51 14-1 69 14-4 81 14-5 Average Standard deviation Test no. ChNo rM (N/ 0.39 0.46 0.58 0.477 0.096 0.11 0.12 0.18 0.137 0.038 93.860 106.400 155.100 118.453 32.350 3.050 3.574 2.792 3.139 0.398 398.5 467.8 423.4 429.00 35.104 48.26 53.69 42.70 48.217 5.495 47.49 50.70 41.04 46.410 4.920 1.765 2.026 1.983 1.925 0.140 2.376 2.394 2.754 2.508 0.213 535.9 462.7 1012.0 670.200 298.262 65.96 56.92 126.60 83.160 37.891 24.70 26.17 22.13 24.333 2.045 5.977 4.224 4.747 4.983 0.900 E (kN/ mm2) Fmax (N) rM (N/ rS0.2 (N/ mm2) eB(%) mm2) RT 117 16-4 119 16-6 120 16-7 Average Standard deviation 0.001 0.001 0.001 0.001 0.000 2.718 3.220 2.659 2.866 0.0308 77 K 99 16-1 100 16-2 101 16-3 Average Standard deviation 2.75 2.43 2.72 2.631 0.174 4.2 K 57 16-2 65 16-3 77 16-5 Average Standard deviation ChNo rM (N/ Table 19 Mapsil 213 eB (%) Test no. ChNo rM (N/ mm2) rS0.2(N/ 13.5 16.6 14.1 14.703 1.638 1.62 1.73 1.51 1.620 0.110 0.24 0.40 0.31 0.314 0.078 61.420 65.610 54.650 60.560 5.530 RT 121 17-4 122 17-5 156 17-9 Average Standard deviation 0.001 0.001 0.001 0.001 0.000 9.8 11.9 7.8 9.833 2.035 1.46 1.76 0.73 1.317 0.530 0.16 0.26 0.21 0.210 0.047 169.300 199.100 82.760 150.387 60.432 4.097 4.102 4.165 4.121 0.038 1386.0 1199.0 1119.0 1234.667 137.027 161.10 146.60 132.20 146.633 14.450 94.54 59.04 61.06 71.547 19.938 5.464 5.793 5.410 5.556 0.207 77 K 102 17-1 103 17-2 104 17-3 Average Standard deviation 3.411 3.402 2.918 3.244 0.282 283.9 395.4 307.0 328.767 58.851 43.25 48.59 37.79 43.210 5.400 43.18 45.97 36.38 41.843 4.933 11.100 2.761 14.880 9.580 6.201 4.216 4.459 4.946 4.540 0.372 872.1 1104.0 1389.0 1121.700 258.904 84.31 111.30 100.50 98.703 13.584 41.79 46.85 43.24 43.960 2.606 6.659 6.824 3.333 5.605 1.970 4.2 K 54 17-1 71 17-3 90 17-4 Average Standard deviation 3.436 3.605 3.506 3.516 0.085 424.4 677.0 1007.0 702.800 292.156 61.12 70.98 107.00 79.700 24.151 21.57 20.99 20.10 20.887 0.740 2.849 2.950 3.182 2.994 0.171 E (kN/ mm2) Fmax (N) RT 116 15-6 127 15-7 128 15-8 Average Standard deviation 0.004 0.004 0.004 0.004 0.000 77 K 94 15-1 97 15-4 98 15-5 Average Standard deviation 4.2 K 48 15-1 62 15-2 89 15-3 Average Standard deviation ChNo 3.5 4.4 4.9 4.260 0.740 Fmax (N) Table 17 Solithane 113 Test no. rS0.2 (N/ mm2) eB (%) mm2) E (kN/ mm2) Test no. mm2) The ultimate tensile strength continually increases at lower temperature which is in good comparison with [13]; the proof stress remains approximately constant with temperature with a maximum value at 77 K. The values of the proof stress measured at room temperature and at 77 K are in good comparison with [13], the value measured at 4.2 K is lower. At room temperature, we have only one valid value of the elongation at rupture. As mentioned above, fracture outside of the extensometer occurred during Test Nos. 24 and 26. Thus, it is expected that only the elongation of Test No. 147 is valid. The measured value of 15.9% is somewhat lower compared with [13] and somewhat higher compared with [3]. The elastic modulus measured at room temperature (109 GPa) is lower compared with [3] (154.7 GPa). The E-Modulus measured at 77 K (123.4 GPa) is also lower than the value measured in [3] (158.6 GPa). The E-Modulus measured at 4.2 K (131.3 GPa) is higher compared with [3] (109.5 GPa). It has to be considered that with pure Cu a continuous increase of the Young’s Modulus with decreasing temperature is expected. The strength and elasticity is superior to all solders at all temperatures. The material shows ductile behaviour down to 4.2 K, the measured elongation even increases at low temperatures. 3.2. 63Sn37Pb (inspection certificate: DIN 50049/EN 10204-3.1) There is an increase of the ultimate tensile strength, the Young’s modulus and the stress at the limit of proportionality at low temperatures. The temperature dependence of these values is in good comparison with previous investigations [2,3]. At 4.2 K and 77 K the solder is brittle, with low elongation. For high temperatures the highest ductility of all tested solders was found. Also a large reduction in the cross sectional area was found at RT. Author's personal copy M. Fink et al. / Cryogenics 48 (2008) 497–510 505 Table 20 Conathane EN4/EN11 E (kN/ mm2) Fmax (N) rM (N/ mm2) rS0.2 (N/ mm2) eB(%) RT 124 18-4 125 18-5 126 18-6 Average Standard deviation 0.003 0.003 0.003 0.003 0.000 22.6 16.9 13.7 17.749 4.485 2.88 2.37 2.07 2.440 0.410 0.49 0.36 0.42 0.423 0.065 259.400 184.200 161.400 201.667 51.282 77 K 105 18-1 106 18-2 107 18-3 Average Standard deviation 4.100 4.046 3.955 4.034 0.073 894.0 790.4 947.8 877.400 80.002 114.80 114.90 113.70 114.467 0.666 80.91 92.18 69.83 80.973 11.175 5.475 5.505 5.027 5.336 0.268 4.2 K 55 18-1 61 18-2 79 18-3 Average Standard deviation 1.708 1.648 1.546 1.634 0.082 794.2 179.9 232.0 402.033 340.624 85.96 18.28 28.60 44.280 36.463 6.74 6.93 7.78 7.148 0.559 6.121 1.459 2.077 3.219 2.532 Test no. ChNo 3.3. 62Sn36Pb2Ag (inspection certificate: DIN 50049/EN 10204-3.1) The silver content improves the strength of the solder with respect to 63Sn37Pb for a little bit. The temperature dependence is similar to 63Sn37Pb. Also for 4.2 K and 77 K a brittle fracture with low elongation and for RT dimple fracture with higher elongation was found. Compared with data of [3] the values of Young’s modulus are about the same. Those of the ultimate tensile strength, the proof stress as well as the total elongation are a little bit lower. 3.4. 60Sn40Pb (inspection certificate: DIN 50049/EN 10204-3.1) Generally the tensile properties are similar to those of the eutectic composition 63Sn37Pb. Small elongations and brittle fractures are obtained at 4.2 K and 77 K. At higher temperatures the solder is ductile with high elongation ratios. Compared with [7] the proof stress, the ultimate tensile strength and the elongation at rupture are somewhat lower at cryogenic temperature. Compared with [8] and [9] the ultimate tensile strength is somewhat lower at room temperature and same at cryogenic temperatures. The elongation is lower at cryogenic temperature; nevertheless this is in good comparison with previous investigations [2,3]. 3.5. 96Sn4Ag (inspection certificate: DIN 50049/EN 10204-3.1) At room temperature the modulus of elasticity is superior to the rest of the solders. The proof stress is at RT and at 77 K somewhat lower than the values found for the rest of the Sn-based solders. At 4.2 K no proof stress could be found because of its peculiar stress/ strain diagram. The fracture of the solder is brittle at low temperatures with low elongations. At RT the solder is ductile and the fracture shows a high reduction in area. 3.6. 50In50Pb (inspection certificate: DIN 50049/EN 10204-3.1) At 4.2 K the solder remains extremely soft with a very low Young’s modulus and high ductility compared with the other Fig. 10. Elastic Modulus at room temperature, 77 K and 4.2 K. solders. The fracture surfaces of this ductile solder are shown in Fig. 19 (photos taken after tensile test at different temperatures). 3.7. 70Pb30In (inspection certificate: DIN 50049/EN 10204-3.1) Generally, this solder shows similar strength and elastic properties as the 50Pb 50In solder. The elongation is somewhat lower compared with the 50Pb 50In solder. The fracture shows a little reduction area at RT, at low temperatures the fracture is not so brittle compared with the other tested solders. Author's personal copy 506 M. Fink et al. / Cryogenics 48 (2008) 497–510 Fig. 11. Ultimate tensile strength at room temperature, 77 K and 4.2 K. 3.8. 96.8Pb1.5Ag1.7Sn (inspection certificate: DIN 50049/EN 102043.1) Beside the high melting point which makes the solder suitable for sequential soldering the solder shows interesting mechanical properties. The stiffness lies in between the Sn-based and In/Pb solders. The ultimate tensile strength is in the area of the In/Pb sol- Fig. 12. Proof stress at room temperature, 77 K and 4.2 K. ders, at 4.2 K somewhat higher. Compared with [10,11] the measured values are lower. The proof stress is the lowest one of all solders investigated at all temperatures. The elongation is the highest one beside 50In50Pb at low temperatures. It is in good comparison with [10,11] at room temperature, at cryogenic temperature the elongation is lower. The fracture shows a high reduction area at RT and at 77 K, at 4.2 K the fracture shows also a reduction. Author's personal copy M. Fink et al. / Cryogenics 48 (2008) 497–510 507 Fig. 14. PCB 2302 MLB polyimide glass fibre - samples after tensile test at room temperature, 77 K, 4.2 K. Fig. 15. PCB 2301 MLB epoxy glass fibre - samples after tensile test at room temperature, 77 K, 4.2 K. this brittle solder are shown in Fig. 20 (photos taken after tensile test at different temperatures). As mentioned above, this solder could be tested in the as-received condition. Thus, a direct comparison of the measured values with the other solders should be regarded carefully. 4. Conclusions 4.1. Solder alloys Fig. 13. Elongation at rupture at room temperature, 77 K and 4.2 K. 3.9. 96.5Sn3Ag0.5Cu (inspection certificate: DIN 50049/EN 10204-3.1) The temperature dependence of the ultimate tensile strength is similar to the other Sn-based solders, except of 96Sn4Ag. The stress at the limit of proportionality is superior to the rest of the solders at 4.2 K. The temperature dependence of the Young’s modulus as well as of the elongation is similar to 63Sn37Pb. In the cross sectional area a reduction was found. For 4.2 K and 77 K brittle fracture with low elongation were found. The fracture surfaces of The measurements of the tensile properties of bulk solder depend greatly on conditions of casting (getting pore-free samples). With decreasing temperature, Sn-based solders show a strong increase in tensile strength (Rm 135–149 MPa) and proof stress (Rp0.2 112–142 MPa), they are brittle with small elongations. Among them 96.5Sn3Ag0.5Cu shows the highest proof stress. For 77 K and 4.2 K this solders are brittle with small elongations (A 0.2–1.5 p.c.). Comparing the Cu-content solder with 96Sn4Ag, for room temperature nearly the same tensile strength and proof stress are found. The elongation is clearly higher; the Young’s modulus is clearly lower. For low temperatures the elongation is nearly the same. The values found for the tensile strength and Author's personal copy 508 M. Fink et al. / Cryogenics 48 (2008) 497–510 Fig. 16. PCB Thermount fracture surfaces after tensile test at room temperature, 77 K, 4.2 K. Fig. 17. Fracture surfaces of Solithane 113 - samples after tensile test at room temperature, 77 K, 4.2 K. the proof stress are clearly higher. The proof stress of 96Sn4Ag at 4.2 K could not be investigated. The Young’s modulus is somewhat lower. In/Pb solders remain soft (E 12–14 GPa) and ductile (A 4.5– 20 p.c.) at 4.2 K, but they have low strength (Rm 29–76 MPa) and low proof stress (Rp0.2 33 MPa). The Pb-based solder combines medium strength with good stiffness at superior ductility, but low proof stress. At room temperature the fracture surface of all investigated conformal coatings is very smooth with extremely high elongation (up to 200 p.c. for Conathane EN4/EN11), at low temperatures it is brittle, the elongation decreases to less than 10 p.c. At 4.2 K the elongation of Arathane 5750 (8.3 p.c.) is superior to the rest of the conformal coatings. 4.2. PCB–bare materials At cryogenic temperatures the proof stress, the elasticity and the ductility of OFE Cu is superior to all other materials tested. At 4.2 K the elasticity (E 33 GPa) and the proof stress (Rp0.2 317 MPa) of PCB 2301 MLB epoxy glass fibre are superior to the other tested PCB’s. PCB Thermount has the lowest elasticity and strength, its elongation is at low temperatures the smallest one of the tested PCB’s. 4.3. Conformal coatings At cryogenic temperatures all tested conformal coatings show a strong increase of strength, proof stress and elasticity, their elongation decreases very strong. An exception is Arathane 5750 which has a high elasticity at all temperatures. The Young’s modulus, the strength and the proof stress of Solithane 113 is superior to the other tested conformal coatings. 4.4. OFE copper 4.5. Overall findings The selection of a solder for use at cryogenic temperatures will depend on its mechanical properties, fatigue and the specific application like soldering temperature, possible dissolution of Au or Ag from plated components or wires, etc. The mechanical properties of the tested solders offer a wide range from stiff and brittle to soft and ductile materials. The differences in the strength and stiffness of the solders increase at low temperatures so the mechanical properties should be considered carefully for the selection of one material. The elasticity of all PCB materials is for all temperatures from the same order of magnitude like the values found for the solders. Author's personal copy M. Fink et al. / Cryogenics 48 (2008) 497–510 Fig. 18. Solithane 113 fracture surfaces (SEM). Strength and proof stress of the PCB materials is always higher than those of the solders. Generally, at room temperature the elongation of solders is higher than the elongation of PC boards, at 4.2 K only the elongation of the In/Pb as well as the Pb-based solders is higher. For all temperatures the modulus of elasticity, the strength and the proof stress of PCB materials is higher compared with the values found for conformal coatings. At all temperatures the elongation of the conformal coatings is superior to the elongation 509 Fig. 19. Fracture surfaces of ductile solder (50In50Pb) performed with optical microscope. of the PCB’s, but the relative differences diminish with respect to 4.2 K. At 77 K the tensile strength of Solithane 113 exceeds those of the solders; at 4.2 K it is lower. The stiffness of most conformal coatings increases relatively to the solders (typically 1/20 at 4.2 K, 1/5000 at room temperature). In combination with the large thermal expansion of the conformal coating the coating will impose considerable loads to the solder joints and have to be avoided at cryogenic temperatures. An exception is Arathane 5750, its stiffness is at all temperatures investigated in the same order of magnitude (1.9–4 GPa). Author's personal copy 510 M. Fink et al. / Cryogenics 48 (2008) 497–510 References [1] Semerad E, Scholze P, Schmidt M, Wendrinsky W. Effect of new cleaning liquids on electronic materials and parts. ESA metallurgy report no 3275; January 2002. [2] Dunn BD. The properties of near-eutectic tin/lead solder alloys tested between +70 and 60 °C and the use of such alloys in spacecraft electronics. ESA TM162 1975. [3] Semerad E, Reithmayr P, Hahn P, Scholze P. Mechanical testing at cryogenic temperatures. WO 1990;7(July). [4] Dunn BD, Desplat P. Evaluation of conformal coatings for future spacecraft applications. ESA SP-1173 1994. August. [5] Tschegg E, Kubasta E, Steiner W. A top loading 200 kN tensile testing cryostat. Cryogenics 1979. May. [6] Rack HJ, Maurin JK. Mechanical properties of const tin-lead solder. J Test Evaluat 1974;2(5):351–3. September. [7] Fast RW, Craddock WW, Kobayashi M, Mruzek MT. Electrical and mechanical properties of lead/tin solders and splices for superconducting cables. Cryogenics 1988;28(1):7–9. [8] Metals handbook, vol. 9, American Society for Metals; 1985. [9] C. Lea. A scientific guide to surface mount technology, Electrochemical Publications Ltd., 1988 Referenced: M.H. Manko; ‘‘Solders and soldering”. New York: McGraw-Hill; 1979. [10] Ainsworth PA. The formation and properties of soft soldered joints. Metals and Materials 1979:374–9. [11] Ainsworth PA. Soft Soldering Gold Coated Surfaces, ITRI; 1971. pp. 1–4. [12] <www.goodfellow.com>. [13] Material data sheet of ‘‘Deutsches Kupferinstitut e.V., Am Bonneshof 5, D40474 Düsseldorf”: <http://www.kupfer-institut.de/front_frame/pdf/Cu-OFE. pdf>. Fig. 20. Fracture surfaces of brittle solder (96.5Sn3Ag0.5Cu) performed with optical microscope.
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