CN113195607B - 热界面材料 - Google Patents
热界面材料 Download PDFInfo
- Publication number
- CN113195607B CN113195607B CN202080007088.3A CN202080007088A CN113195607B CN 113195607 B CN113195607 B CN 113195607B CN 202080007088 A CN202080007088 A CN 202080007088A CN 113195607 B CN113195607 B CN 113195607B
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- China
- Prior art keywords
- ceramic filler
- thermally conductive
- curable composition
- total weight
- filler mixture
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 239000000463 material Substances 0.000 title description 19
- 239000000203 mixture Substances 0.000 claims abstract description 100
- 239000000945 filler Substances 0.000 claims abstract description 63
- 239000000919 ceramic Substances 0.000 claims abstract description 54
- 229920013730 reactive polymer Polymers 0.000 claims abstract description 37
- 239000007788 liquid Substances 0.000 claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000003054 catalyst Substances 0.000 claims abstract description 23
- 125000001181 organosilyl group Chemical group [SiH3]* 0.000 claims abstract 8
- 229920000642 polymer Polymers 0.000 claims description 26
- 239000006254 rheological additive Substances 0.000 claims description 19
- 239000002516 radical scavenger Substances 0.000 claims description 12
- 239000003707 silyl modified polymer Substances 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- YQGOWXYZDLJBFL-UHFFFAOYSA-N dimethoxysilane Chemical group CO[SiH2]OC YQGOWXYZDLJBFL-UHFFFAOYSA-N 0.000 claims description 5
- 229910021485 fumed silica Inorganic materials 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 239000003963 antioxidant agent Substances 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 239000000049 pigment Substances 0.000 claims description 4
- 229920001296 polysiloxane Polymers 0.000 claims description 4
- QQQSFSZALRVCSZ-UHFFFAOYSA-N triethoxysilane Chemical compound CCO[SiH](OCC)OCC QQQSFSZALRVCSZ-UHFFFAOYSA-N 0.000 claims description 4
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 claims description 4
- 230000003078 antioxidant effect Effects 0.000 claims description 3
- 239000004526 silane-modified polyether Substances 0.000 claims description 2
- 125000003808 silyl group Chemical group [H][Si]([H])([H])[*] 0.000 description 25
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 14
- 239000000843 powder Substances 0.000 description 9
- 229920000570 polyether Polymers 0.000 description 8
- 239000002245 particle Substances 0.000 description 6
- 239000004014 plasticizer Substances 0.000 description 6
- 238000006460 hydrolysis reaction Methods 0.000 description 5
- 239000004721 Polyphenylene oxide Substances 0.000 description 4
- 230000007062 hydrolysis Effects 0.000 description 4
- -1 methoxy radicals Chemical class 0.000 description 4
- 150000004756 silanes Chemical class 0.000 description 4
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 125000003545 alkoxy group Chemical group 0.000 description 3
- 238000009833 condensation Methods 0.000 description 3
- 230000005494 condensation Effects 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 150000003254 radicals Chemical class 0.000 description 3
- 229910000077 silane Inorganic materials 0.000 description 3
- 239000004432 silane-modified polyurethane Substances 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- KJTZGGMVRFZKOA-UHFFFAOYSA-N 6-(7-methyloctoxy)-6-oxohexanoic acid Chemical compound CC(C)CCCCCCOC(=O)CCCCC(O)=O KJTZGGMVRFZKOA-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 description 2
- 125000001033 ether group Chemical group 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000013021 overheating Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- FTJHKZQHQDKPFJ-UHFFFAOYSA-N (carbamoylamino)carbamic acid Chemical compound NC(=O)NNC(O)=O FTJHKZQHQDKPFJ-UHFFFAOYSA-N 0.000 description 1
- VLJQDHDVZJXNQL-UHFFFAOYSA-N 4-methyl-n-(oxomethylidene)benzenesulfonamide Chemical compound CC1=CC=C(S(=O)(=O)N=C=O)C=C1 VLJQDHDVZJXNQL-UHFFFAOYSA-N 0.000 description 1
- NIYZIKWNKMOAFD-UHFFFAOYSA-N 6-octan-3-yloxy-6-oxohexanoic acid Chemical compound CCCCCC(CC)OC(=O)CCCCC(O)=O NIYZIKWNKMOAFD-UHFFFAOYSA-N 0.000 description 1
- KXDHJXZQYSOELW-UHFFFAOYSA-M Carbamate Chemical compound NC([O-])=O KXDHJXZQYSOELW-UHFFFAOYSA-M 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- CERQOIWHTDAKMF-UHFFFAOYSA-M Methacrylate Chemical compound CC(=C)C([O-])=O CERQOIWHTDAKMF-UHFFFAOYSA-M 0.000 description 1
- WYNCHZVNFNFDNH-UHFFFAOYSA-N Oxazolidine Chemical compound C1COCN1 WYNCHZVNFNFDNH-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical class OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 1
- QYKIQEUNHZKYBP-UHFFFAOYSA-N Vinyl ether Chemical compound C=COC=C QYKIQEUNHZKYBP-UHFFFAOYSA-N 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- 125000004423 acyloxy group Chemical group 0.000 description 1
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical class OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 1
- 229940045714 alkyl sulfonate alkylating agent Drugs 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 229920003086 cellulose ether Polymers 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- QYQADNCHXSEGJT-UHFFFAOYSA-N cyclohexane-1,1-dicarboxylate;hydron Chemical compound OC(=O)C1(C(O)=O)CCCCC1 QYQADNCHXSEGJT-UHFFFAOYSA-N 0.000 description 1
- AYOHIQLKSOJJQH-UHFFFAOYSA-N dibutyltin Chemical compound CCCC[Sn]CCCC AYOHIQLKSOJJQH-UHFFFAOYSA-N 0.000 description 1
- ORHSGYTWJUDWKU-UHFFFAOYSA-N dimethoxymethyl(ethenyl)silane Chemical compound COC(OC)[SiH2]C=C ORHSGYTWJUDWKU-UHFFFAOYSA-N 0.000 description 1
- 150000002009 diols Chemical class 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 description 1
- MBGQQKKTDDNCSG-UHFFFAOYSA-N ethenyl-diethoxy-methylsilane Chemical compound CCO[Si](C)(C=C)OCC MBGQQKKTDDNCSG-UHFFFAOYSA-N 0.000 description 1
- 125000001301 ethoxy group Chemical group [H]C([H])([H])C([H])([H])O* 0.000 description 1
- CWAFVXWRGIEBPL-UHFFFAOYSA-N ethoxysilane Chemical compound CCO[SiH3] CWAFVXWRGIEBPL-UHFFFAOYSA-N 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- WBJINCZRORDGAQ-UHFFFAOYSA-N formic acid ethyl ester Natural products CCOC=O WBJINCZRORDGAQ-UHFFFAOYSA-N 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 150000002688 maleic acid derivatives Chemical class 0.000 description 1
- 238000007726 management method Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 125000002524 organometallic group Chemical group 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 239000002530 phenolic antioxidant Substances 0.000 description 1
- 235000021317 phosphate Nutrition 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 125000005498 phthalate group Chemical class 0.000 description 1
- 229920006324 polyoxymethylene Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011342 resin composition Substances 0.000 description 1
- 238000007665 sagging Methods 0.000 description 1
- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical class OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 description 1
- 150000003377 silicon compounds Chemical class 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 125000001424 substituent group Chemical group 0.000 description 1
- 229940124530 sulfonamide Drugs 0.000 description 1
- 150000003456 sulfonamides Chemical class 0.000 description 1
- 125000001273 sulfonato group Chemical group [O-]S(*)(=O)=O 0.000 description 1
- 239000013008 thixotropic agent Substances 0.000 description 1
- GKASDNZWUGIAMG-UHFFFAOYSA-N triethyl orthoformate Chemical compound CCOC(OCC)OCC GKASDNZWUGIAMG-UHFFFAOYSA-N 0.000 description 1
- 125000005591 trimellitate group Chemical group 0.000 description 1
- 235000015112 vegetable and seed oil Nutrition 0.000 description 1
- 239000008158 vegetable oil Substances 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
Classifications
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- H01M2220/20—Batteries in motive systems, e.g. vehicle, ship, plane
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
本发明涉及一种导热的可固化组合物,其包含第一部分和第二部分,其中所述第一部分包含催化剂、陶瓷填料混合物、低挥发性有机液体和水,所述第二部分包含甲硅烷基改性的反应性聚合物、低挥发性有机液体和陶瓷填料混合物,并且基于所述甲硅烷基改性的反应性聚合物的总重量,所述低挥发性有机液体以大于约50wt.%的量存在于所述组合物中。
Description
背景技术
热界面材料广泛应用于电子工业中,用于将热源与散热结构(heat-sinkingstructure)耦合,以帮助从所述热源散热。通常,这些热界面材料用于发热电子组件。这些热界面材料通常通过将由热源产生的多余热能排出到散热结构来工作。
与电子产品类似,电动车辆通常配备有包含多个电池单元(battery cell)的电池,这些电池单元存储电力用于为电动车辆提供动力。这些电池单元可以在使用之前被充电并且在驾驶过程中通过再生制动或内燃发动机被再充电。电池单元在使用过程中可能会发热,因而需要使用散热结构来防止电池单元过热。在充电过程中,电池内部发生的化学反应产生热量;在理想情况下,电池的温度保持在25-30℃。然而,当进行正常或快速充电时,电池的温度远远超过这个想要的范围。另外,当外界温度本身超过这个温度范围时,不可能维持25-30℃的理想温度。即使在再充电过程中使用冷却风扇排出电池托盘内的空气,也会出现这种情况。因此,在为用于电动车辆的电池再充电时过热是一个问题。
如果电动车辆的电池过热,电池可能会变形,内部可能产生短路。这可能导致蒸发的电池气体燃烧或爆炸,从而可能导致车辆着火。因此,电动车辆电池的热管理不仅对于实现最佳的效率和寿命而言是必要的,而且对于满足电动车辆的安全标准而言也是必要的。
通常,为了使从热源到散热结构的热传递最大化,使用热界面材料来提供热源与散热结构之间的密切接触。一般来说,热界面材料应能填充与元件间高度差相对应的各种间隙。因此,想要不仅具有高热导率而且具有高柔性的热界面材料。通常用于电子设备中的热界面材料是小规模的,因为许多电子设备是手持的。迄今为止用于小型电子设备的那些热界面材料还不能用于较大的热源上。较大的热源(例如上面讨论的电动车辆电池)需要具有不同特性的不同热界面材料。例如,当与较大的热源(例如电动车辆电池)一起使用时,必须改变热界面材料的流动特性和粘度。此外,用于大热源上的热界面材料的有用分配率(useful dispense rate)不同于用于小热源上的热界面材料的有用分配率。
因此,仍然需要具有高热导率的热界面材料,该热界面材料也不含硅酮并且具有可定制的分配率用于在较大规模下——例如在电动车辆电池中——起作用。
发明内容
本文中公开了一种导热的可固化组合物,其包含第一部分和第二部分。第一部分包含催化剂、陶瓷填料混合物、低挥发性有机液体和水,并且其中第二部分包含甲硅烷基改性的反应性聚合物、低挥发性有机液体和陶瓷填料混合物。基于甲硅烷基改性的反应性聚合物的总重量,低挥发性有机液体以大于约50wt.%的量存在于组合物中。
另一实施方案公开了一种导热的可固化组合物,其包含第一部分和第二部分,其中所述第一部分包含低挥发性有机液体、水、流变添加剂、颜料、陶瓷填料混合物、热解法二氧化硅和有机锡催化剂,并且所述第二部分包含低挥发性有机液体、流变添加剂、多功能聚合物(multifunctional polymer)、陶瓷填料混合物、抗氧化剂和水清除剂。基于填料混合物的总重量,陶瓷填料混合物包含4wt.%的D50为0.3μm的陶瓷填料、36wt.%的D50为2.4μm的陶瓷填料和60wt.%的D50为40μm的陶瓷填料。
另一实施方案公开了一种制备导热的可固化组合物的方法,该方法包括:将包含催化剂、陶瓷填料混合物和水的第一部分与包含反应性聚合物、陶瓷填料混合物和水清除剂的第二部分混合,其中该混合物在固化后是固体。
另一实施方案公开了一种电池,其包含:热源、冷却装置(mechanism)和布置在它们之间的本文公开的导热的可固化组合物。
具体实施方式
本文中公开了一种两部分的导热的可固化组合物,其可在固化后用作热界面材料。本文所公开的导热的可固化组合物可用作大的(即1500mm2或更大的)表面积的热界面材料,例如电动和混合动力车辆电池中的热界面材料。这些导热的可固化组合物可在室温下固化,与环境水分无关。它们还具有快速的分配速率,在分配之后是稳定的,并且在施用过程中具有低的压缩应力。
本文所公开的导热的可固化组合物意欲以较低的粘度配制以供商业自动分配器使用,并且降低(尤其是在汽车制造中)装置装配期间引起的压缩应力,所述汽车制造需要及时输送大量材料和装配汽车装置。
本文公开的导热的可固化组合物包含两部分:第一部分和第二部分。整篇使用术语第一部分和第二部分以表示两个不同的部分,并且不限制部分的施用顺序或其它方面。
第一部分包含催化剂,第二部分包含反应性聚合物。不管第一部分和第二部分的其它组分如何,催化剂和反应性聚合物包含在分开的部分中。优选地,第一部分包含催化剂、陶瓷填料混合物、低挥发性有机液体和水,第二部分包含甲硅烷基改性的反应性聚合物、低挥发性有机液体和陶瓷填料混合物。一旦将第一部分和第二部分混合,混合物将在室温下通过甲硅烷基水解和缩合而固化为固体。
反应性聚合物
反应性聚合物可以是能够参与甲硅烷基水解反应的任何反应性聚合物。例如,反应性聚合物可选自作为具有反应性甲硅烷基的聚合物体系的宽范围的聚合物,例如甲硅烷基改性的反应性聚合物。当用于电子设备中时,甲硅烷基改性的反应性聚合物可具有非硅酮骨架以限制硅酮的释放。优选地,甲硅烷基改性的反应性聚合物具有非硅酮骨架;更优选地,这种甲硅烷基改性的反应性聚合物具有聚醚骨架。
甲硅烷基改性的反应性聚合物可通过在自由基引发剂(radical starter)的存在下使聚醚与至少一种烯键式不饱和硅烷反应而获得,其中所述烯键式不饱和硅烷在硅原子上携带至少一个可水解基团。例如,甲硅烷基改性的反应性聚合物可以是二甲氧基硅烷改性的聚合物、三甲氧基硅烷改性的聚合物或三乙氧基硅烷改性的聚合物。例如,甲硅烷基改性的反应性聚合物可以是硅烷改性的聚醚。
烯键式不饱和硅烷特别优选地选自乙烯基三甲氧基硅烷、乙烯基三乙氧基硅烷、乙烯基二甲氧基甲基硅烷、乙烯基二乙氧基甲基硅烷、反式-β-甲基丙烯酸三甲氧基甲硅烷基甲基酯和反式-β-甲基丙烯酸三甲氧基甲硅烷基丙基酯。
甲硅烷基改性的反应性聚合物优选以统计分布包含在硅原子上具有至少一个可水解基团的甲硅烷基。
例如,甲硅烷基改性的反应性聚合物可以是通式(la)的硅烷改性的聚合物:
其中R是一价至四价的聚合物自由基,R1、R2、R3独立地为具有1至8个C原子的烷基或烷氧基,A代表羧基、氨基甲酸酯、酰胺、碳酸酯、脲基、氨基甲酸酯或磺酸酯基团或者氧原子,x=1至8,n=1至4。
甲硅烷基改性的反应性聚合物也可通过具有羟基的聚醚和具有异氰酸酯基的烷氧基硅烷反应而获得。例如,甲硅烷基改性的反应性聚合物可以是二甲氧基硅烷改性的聚氨酯聚合物、三甲氧基硅烷改性的聚氨酯聚合物或三乙氧基硅烷改性的聚氨酯聚合物。
此外,甲硅烷基改性的反应性聚合物可以是平均通式(Ib)的α-乙氧基硅烷改性的聚合物:
其中R是一价至四价的聚合物残基,式(Ib)聚合物含有的残基R1、R2和R3中的最多三分之一独立地为具有1至4个碳原子的烷基,式(Ib)聚合物含有的残基R1、R2和R3中的至少四分之一独立地为乙氧基残基,其中任何的剩余自由基R1、R2和R3彼此独立为甲氧基自由基,其中n=1至4。
甲硅烷基改性的反应性聚合物为可获得的,例如可作为二甲氧基硅烷改性的MS聚合物从Kaneka获得,可作为三甲氧基硅烷改性的ST聚合物从Evonik获得,可作为三乙氧基硅烷改性的Tegopac聚合物从Evonik获得,可作为硅烷改性的Desmoseal聚合物从Covestro获得,或可作为硅烷改性的SMP聚合物从Henkel获得。优选地,甲硅烷基改性的反应性聚合物为二甲氧基硅烷封端的MS聚合物。
甲硅烷基改性的反应性聚合物存在于不含催化剂的组合物部分中。
基于包含甲硅烷基改性的反应性聚合物的组合物部分的总重量,甲硅烷基改性的反应性聚合物可以从约20wt.%至约90wt.%、例如约30wt%至约70wt.%的量存在于组合物中。
陶瓷填料混合物
陶瓷填料混合物优选包含氧化铝,并且优选等量地添加到第一部分和第二部分中的每一个中以提高热导率。基于第一部分和第二部分中的每一个的总重量,陶瓷填料混合物优选以约80wt.%至约95wt.%的量、例如约90-92wt.%的量存在于第一部分和第二部分中的每一个中。
在特别有用的实施方案中,陶瓷填料混合物包含2.4μm陶瓷填料、40μm陶瓷填料和0.3μm陶瓷填料。优选地,基于陶瓷填料混合物的总重量,2.4μm陶瓷填料以约4wt.%的量存在于组合物中;基于陶瓷填料混合物的总重量,40μm陶瓷填料以约36wt.%的量存在;基于陶瓷填料混合物的总重量,0.3μm陶瓷填料以约60wt.%的量存在。
催化剂
催化剂包含在组合物的第一部分中。特别是,催化剂可以是用于甲硅烷基水解和缩合的有机金属催化剂,例如有机锡催化剂。催化剂不应包含在包含聚合物的组合物第二部分中。优选地,催化剂是有机锡催化剂或有机铋催化剂。
低挥发性有机液体
低挥发性有机液体包含在组合物中,以在高剪切速率下降低第一部分和第二部分的粘度。低挥发性有机液体可包含在第一部分和/或第二部分中。
低挥发性有机液体具有约10-1000cPs、例如约10-100cPs的粘度。
基于聚合物的总重量,低挥发性有机液体以大于约50wt.%的量存在于第一部分和第二部分二者中。如果过多的低挥发性有机液体包含于组合物中,则该组合物将不能在室温下固化为固体,而将是高粘度液体。如果太少的低挥发性有机液体包含于组合物中,则该组合物将固化并变得太硬,并且第二部分的粘度将过高。
优选地,低挥发性有机液体可与树脂混溶并且与填料基质相容,例如,低挥发性有机液体可以是增塑剂。甚至更优选地,低挥发性有机液体选自邻苯二甲酸酯、环己烷二羧酸二异壬酯、偏苯三甲酸酯、对苯二甲酸酯、己二酸酯、癸二酸酯、顺丁烯二酸酯、柠檬酸烷基酯、环氧化植物油、烷基磺酸苯酯、磺酰胺、有机磷酸酯、二醇和聚醚,以及聚合物增塑剂。甚至更优选地,低挥发性有机液体选自己二酸乙基己酯、己二酸异壬酯及它们的组合,更优选己二酸异壬酯。
水
水也可以存在于组合物中。虽然存在的水可来自配制物的陶瓷填料和其它组分的包含物,但组合物的第一部分优选地包含添加水以促进水解和在72小时内、优选地在24小时内完成固化,即使没有外部水分的帮助。在优选实施方案中,基于第一部分的总重量,水以500ppm至5000ppm的量存在于第一部分中。
水清除剂
组合物的第二部分优选地包含用于延长罐藏期的水清除剂。水清除剂可以是例如烷基三甲氧基硅烷、噁唑烷、沸石粉、对甲苯磺酰基异氰酸酯和原甲酸乙酯。水清除剂优选为乙烯基三甲氧基硅烷。如果过多的水清除剂包含于组合物中,则固化会减慢。其量大于约1PHR且小于约5PHR,例如为约2PHR。
任选存在的组分
在另一实施方案中,组合物可任选地包含流变添加剂。这些流变添加剂可包含在第一部分中、在第二部分中、或在第一和第二部分二者中。流变添加剂可进一步包含在组合物中以防止聚合物流挂。基于组合物的总重量,流变添加剂可以少于约1wt.%、例如少于约0.5wt%的量包含。
基于组合物中反应性聚合物的总重量,流变添加剂应以约0.01-1wt.%、例如约0.1-0.2wt.%的量添加到组合物中。流变添加剂可以是,例如,热解法二氧化硅、有机粘土以及用于陶瓷填料的支化的聚合物、触变剂和分散剂。
组合物
组合物可用作热界面材料,例如用于电动车辆中的热界面材料。组合物通过将第一部分和第二部分——优选以1:1的比例——混合而制备。组合物在室温下通过硅烷水解和缩合而固化为固体。在将第一部分和第二部分混合后,组合物将在室温和任何外部湿度下固化。
第一部分和第二部分在混合前具有相似的粘度。例如,第一部分的粘度大于约300Pas,例如为在1/s时约200-1500Pas且在3000/s时小于约200Pas,例如为在1/s时约300-500Pas且在3000/s时小于约50Pas。第二部分的粘度为在1/s时约200-1500Pas并且在3000/s时小于约200Pas,例如在1/s时约300-500Pas且在3000/s时小于约50Pas。
固化后,组合物具有约2.0至约5.0W/mK——例如约2.5-3.5W/mK——的热导率。
在替代的实施方案中,本文公开了一种电池,其包含热源、冷却装置和布置在它们之间的本文公开的组合物。
为了本发明的目的,“聚醚”被理解为其重复单元通过C-O-C醚官能团结合在一起的聚合物。因此,具有侧醚基的聚合物(例如纤维素醚、淀粉醚和乙烯基醚聚合物)以及聚缩醛不为这个定义所涵盖。
“烯键式不饱和硅烷”被理解为非聚合物硅化合物,其中至少一个硅原子通过化学键合而连接到至少一个有机残基,所述有机残基包含碳-碳双键(C═C)。
在本发明的上下文中,“可水解基团”被理解为可通过与水反应而转化为羟基(OH)的取代基。可水解基团应特别理解为烷氧基(还被称为烷基氧基)和酰氧基。
实施例
实施例A是双组分导热材料,其包含第一部分和第二部分。第一部分包含少于10wt.%的粘度小于100cps的低挥发性有机液体、少于0.5wt.%的流变添加剂(热解法二氧化硅、有机粘土或液体流变添加剂)、少于0.2wt.%的有机锡催化剂、少于0.5wt.%的颜料、多于90wt.%的氧化铝粉和任选存在的少于0.5wt.%的去离子水。第二部分包含少于10wt.%的粘度低于100cps的低挥发性有机液体、少于10wt.%的烷氧基硅烷改性的聚醚、0.5wt.%的流变添加剂(热解法二氧化硅、有机粘土或液体流变添加剂)、少于0.5wt.%的抗氧化剂、少于0.5wt.%的水清除剂和多于90wt.%的氧化铝粉。组合物的固化通过将第一部分和第二部分以约1:1的体积比混合来实现,其在约24小时内变为固体。用Shore OO硬度计测得的经固化的250mm冰球(puck)的硬度在约50至约80之间。
实施例B
第一部分通过以下方式制备:将98g增塑剂、3.5g流变添加剂、63g平均粒径为0.3μm的氧化铝填料、357g平均粒径为3μm的氧化铝填料、630g平均粒径为40μm的氧化铝填料、1g二丁基锡催化剂和1g去离子水添加到0.6加仑大小的搅拌桶中,并用Flacktec DAC-5000高速混合器以800rpm搅拌两次达2分钟。第二部分通过以下方式制备:将46g增塑剂、50g甲氧基硅烷封端的聚醚、4g流变添加剂、2g受阻酚类抗氧剂、21g平均粒径为0.3μm的氧化铝填料、399g平均粒径为3μm的氧化铝填料、630g平均粒径为40μm的氧化铝填料和2g水清除剂添加到0.6加仑大小的搅拌桶中,并用Flacktec DAC-5000高速混合器以800rpm搅拌两次达2分钟。
实施例B和C在第二部分中具有不同的树脂组成,并且与实施例B相比,实施例D具有较高的填料用量。实施例A-D中的每一个以与上述实施例B相同的方法另外制备。样品组成的比较见下表1。
表1
实施例A | 实施例B | 实施例C | 实施例D | |
A部分中的组分 | PHR | PHR | PHR | PHR |
增塑剂 | 98.0 | 98.0 | 98.0 | 98.0 |
流变添加剂 | 3.5 | 3.5 | 3.5 | 3.5 |
颜料 | 2.0 | 2.0 | 2.0 | 2.0 |
2.4μm大小的氧化铝粉 | 357.0 | 357.0 | 357.0 | 560.0 |
40μm氧化铝粉 | 630.0 | 630.0 | 630.0 | 960.0 |
0.3μm氧化铝粉 | 63.0 | 63.0 | 63.0 | 80.0 |
催化剂 | 1.0 | 1.0 | 1.0 | 1.0 |
去离子水 | 1.0 | 1.0 | 1.0 | 1.0 |
B部分中的组分 | PHR | PHR | PHR | PHR |
增塑剂 | 46.0 | 76.0 | 21.0 | 46.0 |
流变添加剂 | 4.0 | 4.0 | 4.0 | 4.0 |
硅烷封端的聚醚 | 50.0 | 20.0 | 75.0 | 50.0 |
2.4μm大小的氧化铝粉 | 399.0 | 399.0 | 399.0 | 608.0 |
40μm氧化铝粉 | 630.0 | 630.0 | 630.0 | 960.0 |
0.3μm氧化铝粉 | 21.0 | 21.0 | 21.0 | 32.0 |
抗氧化剂 | 2.0 | 2.0 | 2.0 | 2.0 |
水清除剂 | 2.0 | 2.0 | 2.0 | 2.0 |
实施例A、B、C和D中所述导热组合物的粘度通过平行板流变仪以1/s剪切速率测量,和通过毛细管流变仪以3000/s剪切速率测量。组合物的硬度通过使用第一部分和第二部分的1:1混合物并在室温下固化约72小时来测量。这些组合物的特性比较见下表2。
表2
Claims (16)
1.导热的可固化组合物,其包含第一部分和第二部分,
其中所述第一部分包含有机锡催化剂、陶瓷填料混合物、低挥发性有机液体和水,
其中所述第二部分包含甲硅烷基改性的反应性聚合物、低挥发性有机液体和陶瓷填料混合物,
并且其中基于所述甲硅烷基改性的反应性聚合物的总重量,所述低挥发性有机液体以大于50wt.%的量存在于所述组合物中,
其中基于所述第一部分和所述第二部分中每一个的总重量,所述陶瓷填料混合物以80wt.%至92wt.%的量存在于所述第一部分和所述第二部分中的每一个中,
其中基于所述陶瓷填料混合物的总重量,所述陶瓷填料混合物包含4wt.%的D50为0.3μm的陶瓷填料、36wt.%的D50为2.4μm的陶瓷填料和60wt.%的D50为40μm的陶瓷填料。
2.根据权利要求1所述的导热的可固化组合物,其中所述甲硅烷基改性的反应性聚合物具有非硅酮骨架。
3.根据权利要求1所述的导热的可固化组合物,其中所述甲硅烷基改性的反应性聚合物是硅烷改性的聚醚。
4.根据权利要求1所述的导热的可固化组合物,其中所述甲硅烷基改性的反应性聚合物是二甲氧基硅烷改性的聚合物、三甲氧基硅烷改性的聚合物、三乙氧基硅烷改性的聚合物或它们的组合。
5.根据权利要求1所述的导热的可固化组合物,其中基于所述第二部分的总重量,所述甲硅烷基改性的反应性聚合物以20wt.%至50wt.%的量存在。
6.根据权利要求1所述的导热的可固化组合物,其中基于所述第一部分的总重量,水以500ppm至5000ppm的量存在于所述第一部分中。
7.根据权利要求1所述的导热的可固化组合物,其中所述第二部分进一步包含水清除剂。
8.根据权利要求1所述的导热的可固化组合物,其中所述第一部分和/或所述第二部分进一步包含流变添加剂。
9.根据权利要求1所述的导热的可固化组合物,其中所述第一部分和所述第二部分具有在1/s时高于300Pas的粘度,且具有在3000/s时低于50Pas的粘度。
10.根据权利要求1所述的导热的可固化组合物,其中基于所述第一部分和所述第二部分中每一个的总重量,所述陶瓷填料混合物以90wt.%至92wt.%的量存在于所述第一部分和所述第二部分中的每一个中。
11.导热的可固化组合物,其包含第一部分和第二部分,
其中所述第一部分包含低挥发性有机液体、水、流变添加剂、颜料、陶瓷填料混合物、热解法二氧化硅和有机锡催化剂,
其中所述第二部分包含低挥发性有机液体、流变添加剂、多功能聚合物、陶瓷填料混合物、抗氧化剂和水清除剂,并且
其中基于所述陶瓷填料混合物的总重量,所述陶瓷填料混合物包含4wt.%的D50为0.3μm的陶瓷填料、36wt.%的D50为2.4μm的陶瓷填料和60wt.%的D50为40μm的陶瓷填料,
其中基于所述第一部分和所述第二部分中每一个的总重量,所述陶瓷填料混合物以80wt.%至92wt.%的量存在于所述第一部分和所述第二部分中的每一个中。
12.制备导热的可固化组合物的方法,其包括:
将包含有机锡催化剂、陶瓷填料混合物和水的第一部分与包含反应性聚合物、陶瓷填料混合物和水清除剂的第二部分混合,
其中所述混合物在固化后为固体,
其中基于所述第一部分和所述第二部分中每一个的总重量,所述陶瓷填料混合物以80wt.%至92wt.%的量存在于所述第一部分和所述第二部分中的每一个中,
其中基于所述陶瓷填料混合物的总重量,所述陶瓷填料混合物包含4wt.%的D50为0.3μm的陶瓷填料、36wt.%的D50为2.4μm的陶瓷填料和60wt.%的D50为40μm的陶瓷填料。
13.根据权利要求12所述的方法,其中将所述混合物在室温下固化。
14.根据权利要求13所述的方法,其中固化后所述组合物具有2.0至5.0W/mK的热导率。
15.根据权利要求13所述的方法,其中将所述第一部分和所述第二部分以1:1的比例混合。
16.电池,其包含:
热源、冷却装置和布置在它们之间的根据权利要求1所述的组合物。
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