CN115449223B - 高导热界面材料的制备方法 - Google Patents
高导热界面材料的制备方法 Download PDFInfo
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- CN115449223B CN115449223B CN202211109454.3A CN202211109454A CN115449223B CN 115449223 B CN115449223 B CN 115449223B CN 202211109454 A CN202211109454 A CN 202211109454A CN 115449223 B CN115449223 B CN 115449223B
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- 239000000463 material Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000011521 glass Substances 0.000 claims abstract description 70
- 239000011324 bead Substances 0.000 claims abstract description 69
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 68
- 238000003756 stirring Methods 0.000 claims abstract description 42
- 239000011787 zinc oxide Substances 0.000 claims abstract description 34
- -1 polydimethylsiloxane Polymers 0.000 claims abstract description 28
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000001035 drying Methods 0.000 claims abstract description 24
- 229910052709 silver Inorganic materials 0.000 claims abstract description 23
- 239000004332 silver Substances 0.000 claims abstract description 23
- 239000000945 filler Substances 0.000 claims abstract description 21
- 239000001257 hydrogen Substances 0.000 claims abstract description 21
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 21
- 239000007788 liquid Substances 0.000 claims abstract description 19
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229920002545 silicone oil Polymers 0.000 claims abstract description 17
- 239000004205 dimethyl polysiloxane Substances 0.000 claims abstract description 13
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 12
- 238000007747 plating Methods 0.000 claims abstract description 10
- 206010070834 Sensitisation Diseases 0.000 claims abstract description 8
- 230000008313 sensitization Effects 0.000 claims abstract description 8
- 230000004913 activation Effects 0.000 claims abstract description 4
- 239000000126 substance Substances 0.000 claims abstract description 4
- 238000004073 vulcanization Methods 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 53
- 239000000243 solution Substances 0.000 claims description 53
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 30
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 26
- 239000000741 silica gel Substances 0.000 claims description 26
- 229910002027 silica gel Inorganic materials 0.000 claims description 26
- 239000008367 deionised water Substances 0.000 claims description 24
- 229910021641 deionized water Inorganic materials 0.000 claims description 24
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 24
- 238000005406 washing Methods 0.000 claims description 24
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 20
- 239000012065 filter cake Substances 0.000 claims description 19
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 17
- 238000000967 suction filtration Methods 0.000 claims description 16
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 12
- 229910052697 platinum Inorganic materials 0.000 claims description 12
- 239000003112 inhibitor Substances 0.000 claims description 11
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 10
- 239000003054 catalyst Substances 0.000 claims description 10
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 10
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 6
- 238000013007 heat curing Methods 0.000 claims description 6
- 238000009210 therapy by ultrasound Methods 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 claims description 5
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims description 5
- 238000011049 filling Methods 0.000 claims description 5
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 claims description 5
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 5
- 239000011780 sodium chloride Substances 0.000 claims description 5
- 239000011775 sodium fluoride Substances 0.000 claims description 5
- 235000013024 sodium fluoride Nutrition 0.000 claims description 5
- 239000001119 stannous chloride Substances 0.000 claims description 5
- 235000011150 stannous chloride Nutrition 0.000 claims description 5
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 4
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 238000007605 air drying Methods 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- 235000019441 ethanol Nutrition 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 3
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 2
- QYLFHLNFIHBCPR-UHFFFAOYSA-N 1-ethynylcyclohexan-1-ol Chemical group C#CC1(O)CCCCC1 QYLFHLNFIHBCPR-UHFFFAOYSA-N 0.000 claims description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 2
- 238000010790 dilution Methods 0.000 claims description 2
- 239000012895 dilution Substances 0.000 claims description 2
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 2
- 229920002554 vinyl polymer Polymers 0.000 claims description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims 2
- 230000010355 oscillation Effects 0.000 claims 1
- 150000003378 silver Chemical class 0.000 claims 1
- 230000004048 modification Effects 0.000 abstract description 11
- 238000012986 modification Methods 0.000 abstract description 11
- 239000011159 matrix material Substances 0.000 abstract description 7
- 230000008569 process Effects 0.000 abstract description 2
- 238000007788 roughening Methods 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 16
- 239000011231 conductive filler Substances 0.000 description 9
- 230000001965 increasing effect Effects 0.000 description 9
- 239000000047 product Substances 0.000 description 7
- 230000015556 catabolic process Effects 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 238000001723 curing Methods 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 239000011256 inorganic filler Substances 0.000 description 3
- 229910003475 inorganic filler Inorganic materials 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000017525 heat dissipation Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 238000007551 Shore hardness test Methods 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- PLKATZNSTYDYJW-UHFFFAOYSA-N azane silver Chemical compound N.[Ag] PLKATZNSTYDYJW-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/40—Compounds of aluminium
- C09C1/407—Aluminium oxides or hydroxides
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Abstract
本发明涉及一种高导热界面材料的制备方法,通过粗化、敏化、活化、烘干、制备银液和还原液、玻璃微珠表面化学镀银等一系列操作得到自制镀银玻璃微珠。以端乙烯基聚二甲基硅氧烷和甲基含氢硅油为有机基体,以上述自制镀银玻璃微珠和球形氧化铝、氧化锌作为导热填料,通过导热填料改性—真空搅拌—平板硫化—烘干等一系列工序,制备了一种导热性能高、柔韧性好、绝缘性佳、重量轻的高导热界面材料。
Description
技术领域
本发明涉及一种高导热界面材料的制备方法,该材料用于增强电子发热元器件与散热器件之间的接触和热量传递。
背景技术
目前,随着电力电子行业及能源等领域的快速发展,电子集成电路、电子器件与电子设备等的功率密度越来越大,带来的散热问题日益突出。电子器件与设备工作时产生的热量会导致其工作温度升高,并对其性能及寿命造成严重的影响。
近年来,导热界面材料的市场规模持续扩大,但是目前现有的导热界面材料仍然存在导热性能低、填充量过大、性能不稳定等问题。例如中国专利 CN202011428667.3所述,无机填料的重量百分数占到样品的90%以上,高填充量的产品会降低产品的柔顺性和粘弹性。一些采用金属粉末作为导热填料的产品也面临着高填充量、绝缘性能差、价格高昂等问题。例如中国专利 CN202110876637.7所述,使用铜粉作为导热填料,这不利于产品的绝缘性能,同时进一步提高了成本。如何提高复合材料的导热、绝缘、力学等综合性能,同时制备的产品具有导热性能好,柔性好等优点,这是一个十分重大的挑战。
基于此,本发明以端乙烯基聚二甲基硅氧烷和甲基含氢硅油为有机基体,以自制的镀银玻璃微珠、不同尺寸的球形氧化铝和球形氧化锌作为导热填料,利用不同尺寸的粒子进行复配,在有机基体中构建有效的导热通路。通过填料改性—真空搅拌—平板硫化—烘干等一系列工序,制备了一种高导热、低填充量、低成本的高导热界面材料。
发明内容
本发明针对上述技术问题,提供了一种金属包覆中空玻璃微珠填充的高导热界面材料及其制备方法,兼顾高导热、柔韧性、绝缘性、重量轻等优点。本发明所要解决的技术问题可以通过以下技术方案来实现:
一种高导热界面材料的制备方法,
首先制备镀银玻璃微珠
步骤1:粗化:在粗化之前先将准备好的玻璃微珠放入丙酮中超声,抽滤洗涤干净,去除表面油污;取氟化钠溶于去离子水中,搅拌均匀;再加入盐酸,搅拌均匀,配制成粗化液;将预处理的玻璃微珠加入粗化液中超声,抽滤后用去离子水重复洗涤一次以上备用;
步骤2:敏化、活化:取氯化钯和盐酸,加去离子水稀释;取氯化钠溶于水中,搅拌均匀,将上述两种溶液混合搅拌,得到溶液A;取氯化亚锡溶于水中,搅拌均匀后,加入到溶液A中,然后加入去离子水,搅拌均匀后得到敏化液;将上述制备的敏化液倒入到粗化后的玻璃微珠中,超声分散,静置抽滤后,用去离子水重复洗涤一次以上;
步骤3:烘干:将敏化后的玻璃微珠,进行烘干处理;
步骤4:制备银液和还原液:称取硝酸银溶液于去离子水中,充分溶解,量取适量氨水,倒入上述溶液中,并不断搅拌,直至溶液澄清,最后,用稀硝酸溶液调节溶液的pH值,配制成银液;取甲醛和乙醇,加入到烧杯中,充分搅拌,再加入去离子水,混合均匀,配制得到还原液;
步骤5:玻璃微珠表面化学镀银:将步骤3中预处理后的玻璃微珠,先进行磁力搅拌和超声波分散;取还原液加入到处理后的玻璃微珠中,充分搅拌混合均匀;将银液缓慢倒入到还原液中,在超声波发生器中反应,抽滤后,用去离子水重复洗涤一次以上,烘干后,得到表面镀银玻璃微珠;
其次再制备高导热界面材料
步骤6:改性,向烧杯中加入适量KH-570和无水乙醇,配制成KH-570的无水乙醇溶液,再加入自制镀银玻璃微珠,超声震荡后,使填料均匀分散在无水乙醇中,加热搅拌,冷却抽滤后,用无水乙醇反复洗涤滤饼若干次,放入烘箱烘干。得到改性的镀银玻璃微珠;
球形氧化铝和球形氧化锌的改性,向烧杯中加入适量KH-550和无水乙醇,配制成KH-550的无水乙醇溶液,再加入适量的球形氧化铝和球形氧化锌,超声震荡,使填料均匀分散在无水乙醇中,加热搅拌,冷却抽滤后,用无水乙醇重复洗涤一次以上,放入烘箱烘干,得到改性的球形氧化铝和球形氧化锌;
步骤7:真空搅拌,称取适量的端乙烯基聚二甲基硅氧烷、甲基含氢硅油、卡斯特铂金催化剂、抑制剂,将上述改性的镀银玻璃微珠、球形氧化铝和球形氧化锌依照粒径从小到大依次加入到上述混合物中,进行真空搅拌一定时间,得到硅胶预聚体;
步骤8:平板硫化,将上述硅胶预聚体填入到模具中,在平板硫化仪上进行热固化,并进行烘干,得到高导热界面材料。
优选的,步骤1中氟化钠含量为0.1~0.5g,盐酸浓度为20~50%。
优选的,步骤2中氯化钯的含量为0.2~0.8g,盐酸浓度为30~40%,氯化钠的含量为100~200g,氯化亚锡含量为20~40g。
优选的,步骤3中放入鼓风干燥烘箱,设定温度120烘干℃,时间为1h。
优选的,步骤4中硝酸银含量为5~8g,pH值为10~13;甲醛含量为1~4mL。
优选的,步骤7中按照质量百分比,所述端乙烯基聚二甲基硅氧烷 30%~50%,甲基含氢硅油0.4%~0.8%,镀银玻璃微珠20%~40%、球形氧化铝 10%~15%、球形氧化锌5%~10%,卡斯特铂金催化剂0.03%~0.7%,填料和硅烷偶联剂的质量比例为1:0.02~0.05、抑制剂为端乙烯基硅油和甲基含氢硅油质量之和的0.05%~1%。
优选的,端乙烯基聚二甲基硅氧烷的粘度范围在500~30000mPa·s;甲基含氢硅油的粘度范围在50~600mPa·s,含氢量在0.05%~1.5%。
优选的,镀银玻璃微珠平均粒径为10~20μm;球形氧化铝的平均粒径为 8~12μm;球形氧化锌平均粒径为200~500nm。
优选的,KH-570为γ-丙基三甲氧基硅烷,KH-550为γ-氨丙基三乙氧基硅烷。
优选的,卡斯特铂金催化剂的含铂有效浓度在0.5%~1.0%;抑制剂为1-乙炔基环己醇。
采用上述技术特征,与现有技术相比,本发明的有益效果为
一、本发明采用自制的镀银玻璃微珠作为导热填料,将玻璃微珠的质量轻、成本低廉的优点和金属银的高导热特性结合在一起,在提高产品导热性的基础上,进一步减轻了产品的重量、同时大大降低了生产成本。
二、本发明根据自制镀银玻璃微珠和球形氧化铝、球形氧化锌的表面化学特性,分别选择了KH-570和KH-550作为硅烷偶联剂,增强了无机导热填料与有机基体的相容性,有利于无机填料在有机基体的分散,构建均匀、有效的导热网络。
三、玻璃微珠表面化学镀银过程中,制备的敏化液可以循环利用,与传统的制备过程相比,提高了镀银玻璃微珠的循环再生产能力,同时避免将有害废液直接排入环境,加工工艺绿色环保。
附图说明
图1是本发明各个实施例对比参数图;
图2是本发明制备方法流程框图。
具体实施方式
以下给出的实施例对本发明作进一步详细的说明。
实施例1
参见图2所示,(一)镀银玻璃微珠的制备
步骤1:粗化。在粗化之前先将准备好的玻璃微珠放入丙酮中超声10min,抽滤洗涤干净,去除表面油污。取0.2g氟化钠溶于50mL的去离子水中,搅拌均匀。再加入2mL浓度为40%的盐酸,搅拌均匀,配制成粗化液体。将预处理的玻璃微珠加入粗化液中,超声10min,抽滤后用去离子水洗涤三次以备用。
步骤2:敏化、活化。取0.5g的氯化钯、60mL浓度为37%的盐酸,加去离子水稀释至100mL;取160g的氯化钠溶于500mL水中,搅拌均匀。将上述两种溶液混合搅拌,得到溶液A;取30g的氯化亚锡溶于300mL水中,搅拌均匀后,缓慢加入到溶液A中,然后加入去离子水至1000mL,搅拌均匀后的到敏化液;将上述制备的敏化液倒入到粗化后的玻璃微珠中,超声分散10min,静置抽滤后,用去离子水洗涤三次。
步骤3:烘干。将敏化后的玻璃微珠,放入鼓风干燥烘箱,设定120℃,烘干时间为1h。
步骤4:制备银液和还原液。称取7g硝酸银溶液于160g去离子水中,充分溶解。量取40mL的氨水,缓慢倒入上述溶液中,并不断搅拌,直至溶液澄清。最后,用稀硝酸溶液调节溶液的pH值在12.4左右,配制成银液;量取3mL的甲醛和200mL的乙醇中,加入到烧杯中,充分搅拌。再加入10mL的去离子水,混合均匀,配制得到还原液。
步骤5:玻璃微珠表面化学镀银。将预处理后的玻璃微珠,先进行10min 的磁力搅拌和10min的超声波分散。取50mL的还原液加入到处理后的玻璃微珠中,充分搅拌混合均匀。将50mL银氨溶液缓慢倒入到还原液中,在超声波发生器中反应1.5h。抽滤后,用去离子水洗涤三次,放入烘箱中,设定温度为120℃,烘干3h,得到表面镀银的玻璃微珠。
实施例1应用
(一)导热填料的改性
步骤1:镀银玻璃微珠改性。向烧杯中加入1.5g的KH-570和100mL的无水乙醇,制成KH-570的无水乙醇溶液,放入30g镀银玻璃微珠,超声震荡5min。然后升温至60℃,持续搅拌3h。抽滤后,用无水乙醇反复洗涤滤饼3次,再经 80℃真空烘箱烘干,得到改性的镀银玻璃微珠。
步骤2:球形氧化铝和球形氧化锌的改性。向烧杯中加入1.5g的KH-550和 100mL无水乙醇,配制成KH-550的无水乙醇溶液,再加入30g的球形氧化铝和球形氧化锌,超声震荡10min,使填料均匀分散在无水乙醇中。加热搅拌2h,温度为80℃;冷却抽滤后,用无水乙醇反复洗涤滤饼3次,放入烘箱烘干1h,温度为85℃。得到改性的球形氧化铝和球形氧化锌。
(二)高导热界面材料的制备
步骤1:取端乙烯基聚二甲基硅氧烷30g,粘度为2000mPa·s;取甲基含氢硅油8g,含氢量在0.25-0.35%;将步骤1和2改性好的镀银玻璃微珠30g、球形氧化铝10g、球形氧化锌6g、卡斯特铂金催化剂0.35g和抑制剂0.38g投入到上述混合物中,启动双行星搅拌机,真空搅拌1h,得到硅胶预聚体。
步骤2:将步骤1所得的硅胶预聚体倒入到模具中,在平板硫化仪中进行热固化处理,设定压力为15MPa,温度为155℃,固化时间为10min,得到导热硅胶垫片。
步骤3:将步骤2得到的导热硅胶垫片放入烘箱中烘干,温度设定为85℃,时间为0.5h。在烘干后的硅胶垫片两面贴上离型纸,得到成品的高导热界面材料。
实施例2
(一)镀银玻璃微珠的制备:同实施例1
实施例1应用
(一)导热填料的改性
步骤1:取1.8g的KH-570溶于100mL的无水乙醇中,配制KH-570的无水乙醇溶液,放入36g镀银玻璃微珠。超声震荡5min。然后升温至60℃,持续搅拌3h。抽滤后,用无水乙醇反复洗涤滤饼3次,再经80℃真空烘箱烘干,得到改性的镀银玻璃微珠。
步骤2:球形氧化铝和球形氧化锌的改性。向烧杯中加入1.5g的KH-550 和100mL无水乙醇,配制成KH-570的无水乙醇溶液,再加入30g的球形氧化铝和球形氧化锌,超声震荡10min,使填料均匀分散在无水乙醇中。加热搅拌 2h,温度为80℃;冷却抽滤后,用无水乙醇反复洗涤滤饼3次,放入烘箱烘干 1h,温度为85℃。得到改性的球形氧化铝和球形氧化锌。
(二)高导热界面材料的制备
步骤1:取端乙烯基聚二甲基硅氧烷30g,粘度为2000mPa·s;取甲基含氢硅油5g,含氢量在0.025-0.035%;将步骤1和2改性好的镀银玻璃微珠36g、球形氧化铝12g、球形氧化锌8g、卡斯特铂金催化剂0.35g和抑制剂0.35g投入到上述混合物中,启动双行星搅拌机,真空搅拌1h,得到硅胶预聚体。
步骤2:将步骤1所得的硅胶预聚体倒入到模具中,在平板硫化仪中进行热固化处理,设定压力为15MPa,温度为155℃,固化时间为10min,得到导热硅胶垫片。
步骤3:将步骤2得到的导热硅胶垫片放入烘箱中烘干,温度设定为85℃,时间为0.5h。在烘干后的硅胶垫片两面贴上离型纸,得到成品的高导热界面材料。
实施例3
(一)镀银玻璃微珠的制备:同实施例1
实施例3应用
(一)导热填料的改性
步骤1:取1.8g的KH-570溶于100mL的无水乙醇中,配制KH-570的无水乙醇溶液,放入36g镀银玻璃微珠。超声震荡5min。然后升温至60℃,持续搅拌3h。抽滤后,用无水乙醇反复洗涤滤饼3次,再经80℃真空烘箱烘干,得到改性的镀银玻璃微珠。
步骤2:球形氧化铝和球形氧化锌的改性。向烧杯中加入1.5g的KH-550 和100mL无水乙醇,配制成KH-550的无水乙醇溶液,再加入30g的球形氧化铝和球形氧化锌,超声震荡10min,使填料均匀分散在无水乙醇中。加热搅拌 2h,温度为80℃;冷却抽滤后,用无水乙醇反复洗涤滤饼3次,放入烘箱烘干 1h,温度为85℃。得到改性的球形氧化铝和球形氧化锌。
(二)高导热界面材料的制备
步骤1:取端乙烯基聚二甲基硅氧烷35g,粘度为2000mPa·s;取甲基含氢硅油5g,含氢量在0.025-0.035%;将步骤1和2改性好的镀银玻璃微珠42g、球形氧化铝15g、球形氧化锌9g、卡斯特铂金催化剂0.41g和抑制剂0.4g投入到上述混合物中,启动双行星搅拌机,真空搅拌1h,得到硅胶预聚体。
步骤2:将步骤1所得的硅胶预聚体倒入到模具中,在平板硫化仪中进行热固化处理,设定压力为15MPa,温度为155℃,固化时间为10min,得到导热硅胶垫片
步骤3:将步骤2得到的导热硅胶垫片放入烘箱中烘干,温度设定为85℃,时间为0.5h。在烘干后的硅胶垫片两面贴上离型纸,得到成品的高导热界面材料。
实施例4
(一)镀银玻璃微珠的制备:同实施例1
实施例4应用
(一)导热填料的改性
步骤1:取1.8g的KH-570溶于100mL的无水乙醇中,配制KH-570的无水乙醇溶液,放入36g镀银玻璃微珠。超声震荡5min。然后升温至60℃,持续搅拌3h。抽滤后,用无水乙醇反复洗涤滤饼3次,再经80℃真空烘箱烘干,得到改性的镀银玻璃微珠。
步骤2:球形氧化铝和球形氧化锌的改性。向烧杯中加入1.5g的KH-550 和100mL无水乙醇,配制成KH-550的无水乙醇溶液,再加入30g的球形氧化铝和球形氧化锌,超声震荡10min,使填料均匀分散在无水乙醇中。加热搅拌 2h,温度为80℃;冷却抽滤后,用无水乙醇反复洗涤滤饼3次,放入烘箱烘干 1h,温度为85℃。得到改性的球形氧化铝和球形氧化锌。
(二)高导热界面材料的制备
步骤1:取端乙烯基聚二甲基硅氧烷35g,粘度为2000mPa·s;取甲基含氢硅油6g,含氢量在0.025-0.035%;将步骤1和2改性好的镀银玻璃微珠25g、球形氧化铝10g、球形氧化锌5g、卡斯特铂金催化剂0.41g和抑制剂0.38g投入到上述混合物中,启动双行星搅拌机,真空搅拌1h,得到硅胶预聚体。
步骤2:将步骤1所得的硅胶预聚体倒入到模具中,在平板硫化仪中进行热固化处理,设定压力为15MPa,温度为155℃,固化时间为10min,得到导热硅胶垫片
步骤3:将步骤三得到的导热硅胶垫片放入烘箱中烘干,温度设定为85℃,时间为0.5h。在烘干后的硅胶垫片两面贴上离型纸,得到成品的高导热界面材料。
对比实施例
与实施例1相比,将镀银玻璃微珠替换成同体积的银粉,其余条件保持不变。
实施例2与实施例1相比,提高了镀银玻璃微珠、球形氧化铝和球形氧化锌的用量。根据测试结果分析可知,实施例2相比于实施例1样品的密度和硬度都有所提高,得益于导热填料用量的增加,实施例2样品的导热系数有所提高,相应的击穿电压有所下降。
实施例3与实施例2相比,继续提高镀银玻璃微珠、球形氧化铝和球形氧化锌的用量。根据测试结果分析。实施例3相比于实施例1,密度和硬度有所提高,得益于导热填料用量的增加,实施例3相比于实施例2样品的导热系数进一步提高,相应的击穿电压有所下降。
实施例4与实施例1相比,实施例减少了镀银玻璃微珠、球形氧化铝和球形氧化锌填料的用量,增加了端乙烯基聚二甲基硅氧烷和甲基含氢硅油的用量,使实施例1与实施例4的质量基本相同。根据测试结果分析,实施例4相比于实施例1,硬度有所下降,这符合预期结果。因为减少了导热填料的用量,实施例4相比于实施例1的导热系数有所下降,但同时击穿电压有所提高。
对比实施例与实施例1相比,把实施例1所使用的镀银玻璃微珠替换为同体积的银粉,其余条件保持不变。根据测试结果分析,对比实施例相比于实施例1样品的密度大幅提升,这是由于银粉的密度远超过镀银玻璃微珠的密度。与此同时,对比实施例的样品硬度更高,柔韧性变差。对比实施例相比实施例1 样品的导热系数有所提高,同时由于银粉的高导电性,样品的击穿电压大幅下降。
最后介绍上述实施例的材料根据下述测试方法得出参见附图1中参数。
导热性能测定采用保护热板法导热仪,测试采用ASTM D5470标准,试样为厚度3mm,直径100mm的圆形样品,重复测试三次,取平均值。
密度测试采用天平法测量,测试采用GB4472-84标准,试样为厚度为3mm,边长50mm的正方形样品,重复测试三次,取平均值。
邵氏硬度测试采用邵氏硬度计,测试采用ASTM D2240标准,试样为厚度为5mm,边长50mm的正方形样品,重复测试三次,取平均值。
击穿电压采用电气强度测试仪测试,测试采用ASTM D149标准,测试样品为厚度为1mm,直径25mm的圆形样品。测量8~10个测试点取平均值。
本发明采用自制的镀银玻璃微珠作为导热填料,在降低导热硅胶垫片密度的同时,保持了优异的导热性能和较高的击穿电压,同时大大降低了生产成本;通过对不同的导热填料选择性的使用相应的硅烷偶联剂,增强了无机导热填料与有机硅基体的相容性,有利于无机填料在有机基体的分散,构建均匀、有效的导热网络。根据测试结果显示,在最优的配方下,所制备的导热硅胶垫片的导热系数可以达到10.2W/mk。
上述实施例中的KH-570和KH-550为偶联剂的代号,是本领域常用代号。
以上所述仅是本发明的优选实施方式,应当指出、本技术领域的普通技术人员来说,在不脱离本发明原理的前提下,凡在本发明所涉及到的填料配比及加工方式,任何修改、等同、替换改进等,均包含在本发明的保护范围之内。
Claims (10)
1.一种高导热界面材料的制备方法,其特征在于,
首先制备镀银玻璃微珠
步骤1:粗化:在粗化之前先将准备好的玻璃微珠放入丙酮中超声,抽滤洗涤干净,去除表面油污;取氟化钠溶于去离子水中,搅拌均匀;再加入盐酸,搅拌均匀,配制成粗化液;将预处理的玻璃微珠加入粗化液中超声,抽滤后用去离子水重复洗涤一次以上备用;
步骤2:敏化、活化:取氯化钯和盐酸,加去离子水稀释;取氯化钠溶于水中,搅拌均匀,将上述两种溶液混合搅拌,得到溶液A;取氯化亚锡溶于水中,搅拌均匀后,加入到溶液A中,然后加入去离子水,搅拌均匀后得到敏化液;将上述制备的敏化液倒入到粗化后的玻璃微珠中,超声分散,静置抽滤后,用去离子水重复洗涤一次以上;
步骤3:烘干:将敏化后的玻璃微珠,进行烘干处理;
步骤4:制备银液和还原液:称取硝酸银溶液于去离子水中,充分溶解,量取适量氨水,倒入上述溶液中,并不断搅拌,直至溶液澄清,最后,用稀硝酸溶液调节溶液的pH值,配制成银液;取甲醛和乙醇,加入到烧杯中,充分搅拌,再加入去离子水,混合均匀,配制得到还原液;
步骤5:玻璃微珠表面化学镀银:将步骤3中预处理后的玻璃微珠,先进行磁力搅拌和超声波分散;取还原液加入到处理后的玻璃微珠中,充分搅拌混合均匀;将银液缓慢倒入到还原液中,在超声波发生器中反应,抽滤后,用去离子水重复洗涤一次以上,烘干后,得到表面镀银玻璃微珠;
其次再制备高导热界面材料
步骤6:改性,向烧杯中加入适量KH-570和无水乙醇,配制成KH-570的无水乙醇溶液,再加入自制镀银玻璃微珠,超声震荡后,使填料均匀分散在无水乙醇中,加热搅拌,冷却抽滤后,用无水乙醇反复洗涤滤饼若干次,放入烘箱烘干,得到改性的镀银玻璃微珠;
球形氧化铝和球形氧化锌的改性,向烧杯中加入适量KH-550和无水乙醇,配制成KH-550的无水乙醇溶液,再加入适量的球形氧化铝和球形氧化锌,超声震荡,使填料均匀分散在无水乙醇中,加热搅拌,冷却抽滤后,用无水乙醇重复洗涤一次以上,放入烘箱烘干,得到改性的球形氧化铝和球形氧化锌;
步骤7:真空搅拌,称取适量的端乙烯基聚二甲基硅氧烷、甲基含氢硅油、卡斯特铂金催化剂、抑制剂,将上述改性的镀银玻璃微珠、球形氧化铝和球形氧化锌依照粒径从小到大依次加入到上述混合物中,进行真空搅拌一定时间,得到硅胶预聚体;
步骤8:平板硫化,将上述硅胶预聚体填入到模具中,在平板硫化仪上进行热固化,并进行烘干,得到高导热界面材料。
2.根据上述权利要求1所述的高导热界面材料的制备方法,其特征在于,步骤1中氟化钠含量为0.1~0.5g,盐酸浓度为20~50%。
3.根据上述权利要求1所述的高导热界面材料的制备方法,其特征在于,步骤2中氯化钯的含量为0.2~0.8g,盐酸浓度为30~40%,氯化钠的含量为100~200g,氯化亚锡含量为20~40g。
4.根据上述权利要求1所述的高导热界面材料的制备方法,其特征在于,步骤3中放入鼓风干燥烘箱,设定温度120烘干℃,时间为1h。
5.根据上述权利要求1所述的高导热界面材料的制备方法,其特征在于,步骤4中硝酸银含量为5~8g,pH值为10~13;甲醛含量为1~4mL。
6.根据上述权利要求1所述的高导热界面材料的制备方法,其特征在于,步骤7中按照质量百分比,所述端乙烯基聚二甲基硅氧烷30%~50%,甲基含氢硅油0.4%~0.8%,镀银玻璃微珠20%~40%、球形氧化铝10%~15%、球形氧化锌5%~10%,卡斯特铂金催化剂0.03%~0.7%,填料和硅烷偶联剂的质量比例为1:0.02~0.05、抑制剂为端乙烯基硅油和甲基含氢硅油质量之和的0.05%~1%。
7.根据上述权利要求1所述的高导热界面材料,其特征在于,端乙烯基聚二甲基硅氧烷的粘度范围在500~30000mPa·s;甲基含氢硅油的粘度范围在50~600mPa·s,含氢量在0.05%~1.5%。
8.根据上述权利要求1所述的高导热界面材料的制备方法,其特征在于,镀银玻璃微珠平均粒径为10~20μm;球形氧化铝的平均粒径为8~12μm;球形氧化锌平均粒径为200~500nm。
9.根据上述权利要求1所述的高导热界面材料的制备方法,其特征在于,KH-570为γ-丙基三甲氧基硅烷,KH-550为γ-氨丙基三乙氧基硅烷。
10.根据上述权利要求1所述的高导热界面材料的制备方法,其特征在于,卡斯特铂金催化剂的含铂有效浓度在0.5%~1.0%;抑制剂为1-乙炔基环己醇。
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