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Article(id=1203281643889996038, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1203281635908231645, articleNumber=null, orderNo=null, doi=10.16790/j.cnki.1009-9239.im.2025.06.011, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1720195200000, receivedDateStr=2024-07-06, revisedDate=1726243200000, revisedDateStr=2024-09-14, acceptedDate=null, acceptedDateStr=null, onlineDate=1764814299795, onlineDateStr=2025-12-04, pubDate=1750348800000, pubDateStr=2025-06-20, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1764814299795, onlineIssueDateStr=2025-12-04, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1764814299795, creator=13701087609, updateTime=1764814299795, updator=13701087609, issue=Issue{id=1203281635908231645, tenantId=1146029695717560320, journalId=1149653034449285133, year='2025', volume='58', issue='6', pageStart='1', pageEnd='148', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=0, articleOrder=1, issueType=-1, specialIssue=null, createTime=1764814297892, creator=13701087609, updateTime=1764815002353, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1203284590690545746, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1203281635908231645, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1203284590694740051, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1203281635908231645, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=88, endPage=93, ext={EN=ArticleExt(id=1203281644401701137, articleId=1203281643889996038, tenantId=1146029695717560320, journalId=1149653034449285133, language=EN, title=Preparation of self-leveling polyaddition silicone encapsulant with outstanding thermal conductivity, columnId=1190369066675179686, journalTitle=Insulating Materials, columnName=Material Research, runingTitle=null, highlight=

A kind of silicone encapsulant with excellent thermal conductivity, self-leveling properties, mechanical properties, and flame retardancy was prepared by employing end vinyl silicone oil with different viscosity as matrix, containing hydrogen silicone oil as cross-linking agent, and spherical alumina as thermal conductive and reinforcement filler. The effects of ratio of end vinyl silicone oils with different viscosity, molar ratio of active hydrogen and vinyl, filler ratio and filling amount on the performance of silicone encapsulant were investigated. The results show that the silicone encapsulant has the best performance when the PDMS-1 and PDMS-2 vinyl end silicone oil are mixed at a mass ratio of 1∶1 as the matrix, the molar ratio of active hydrogen and vinyl is 1.2, and the ratio of spherical alumina with different particle sizes m(5 μm)∶m(15 μm)∶m(50 μm)=2∶5∶3. When the total filling amount of different sizes of spherical alumina reaches 500 parts, the silicone encapsulant has up to 1.50 W/(m·K) of thermal conductivity, up to 1.70 MPa of tensile strength, FV-0 of vertical combustion grade, and excellent operation and processing performance as well as dispersing stability, and its comprehensive performance is excellent.

, articleAbstract=

A kind of silicone encapsulant with excellent thermal conductivity, self-leveling properties, mechanical properties, and flame retardancy was prepared by employing end vinyl silicone oil with different viscosity as matrix, containing hydrogen silicone oil as cross-linking agent, and spherical alumina as thermal conductive and reinforcement filler. The effects of ratio of end vinyl silicone oils with different viscosity, molar ratio of active hydrogen and vinyl, filler ratio and filling amount on the performance of silicone encapsulant were investigated. The results show that the silicone encapsulant has the best performance when the PDMS-1 and PDMS-2 vinyl end silicone oil are mixed at a mass ratio of 1∶1 as the matrix, the molar ratio of active hydrogen and vinyl is 1.2, and the ratio of spherical alumina with different particle sizes m(5 μm)∶m(15 μm)∶m(50 μm)=2∶5∶3. When the total filling amount of different sizes of spherical alumina reaches 500 parts, the silicone encapsulant has up to 1.50 W/(m·K) of thermal conductivity, up to 1.70 MPa of tensile strength, FV-0 of vertical combustion grade, and excellent operation and processing performance as well as dispersing stability, and its comprehensive performance is excellent.

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以不同黏度的端乙烯基硅油复配为基体，含氢硅油为交联剂，球形氧化铝为导热补强填料，制备了具有优异导热性能、自流平性能、力学性能及阻燃性能的有机硅灌封胶。探究了不同黏度的端乙烯基硅油复配比例、活性氢与乙烯基的摩尔比、填料配比及填充量对有机硅灌封胶性能的影响。结果表明：PDMS-1和PDMS-2两种端乙烯基硅油按质量比1∶1混合作为基体、活性氢与乙烯基摩尔比R=1.2、不同粒径的球形氧化铝质量比m(5 μm)∶m(15 μm)∶m(50 μm)=2∶5∶3时，灌封胶性能最佳。当不同粒径的球形氧化铝总填充量达500份时，灌封胶的导热系数可达1.50 W/(m·K)，拉伸强度为1.70 MPa，垂直燃烧等级为FV-0，具有优异的操作加工性能以及分散稳定性，综合性能优异。

, articleAbstract=

以不同黏度的端乙烯基硅油复配为基体，含氢硅油为交联剂，球形氧化铝为导热补强填料，制备了具有优异导热性能、自流平性能、力学性能及阻燃性能的有机硅灌封胶。探究了不同黏度的端乙烯基硅油复配比例、活性氢与乙烯基的摩尔比、填料配比及填充量对有机硅灌封胶性能的影响。结果表明：PDMS-1和PDMS-2两种端乙烯基硅油按质量比1∶1混合作为基体、活性氢与乙烯基摩尔比R=1.2、不同粒径的球形氧化铝质量比m(5 μm)∶m(15 μm)∶m(50 μm)=2∶5∶3时，灌封胶性能最佳。当不同粒径的球形氧化铝总填充量达500份时，灌封胶的导热系数可达1.50 W/(m·K)，拉伸强度为1.70 MPa，垂直燃烧等级为FV-0，具有优异的操作加工性能以及分散稳定性，综合性能优异。

, correspAuthors=null, authorNote=null, correspAuthorsNote=
陈淑海（1983-），男（汉族），山东临沂人，教授，博士，主要从事高分子材料的研究。
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吴阳（2000-），男（汉族），宁夏中卫人，硕士生，主要从事高分子材料的研究；

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吴阳（2000-），男（汉族），宁夏中卫人，硕士生，主要从事高分子材料的研究；

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吴阳（2000-），男（汉族），宁夏中卫人，硕士生，主要从事高分子材料的研究；

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m(PDMS-1)∶m(PDMS-2)0∶103∶75∶57∶310∶0
乙烯基含量/(mol/100 g)0.0150.0190.0210.0240.027
黏度/(mPa·s)7 7735 9794 5903 7562 638
硬度/邵氏A6469727274
拉伸强度/MPa1.722.032.872.262.10
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基体的配比对灌封胶性能的影响

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m(PDMS-1)∶m(PDMS-2)0∶103∶75∶57∶310∶0
乙烯基含量/(mol/100 g)0.0150.0190.0210.0240.027
黏度/(mPa·s)7 7735 9794 5903 7562 638
硬度/邵氏A6469727274
拉伸强度/MPa1.722.032.872.262.10
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R1.01.21.41.61.8
含氢硅油用量/份12.114.516.919.321.7
硬度/邵氏A6972737374
拉伸强度/MPa2.342.872.752.672.47
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R值对有机硅灌封胶性能的影响

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R1.01.21.41.61.8
含氢硅油用量/份12.114.516.919.321.7
硬度/邵氏A6972737374
拉伸强度/MPa2.342.872.752.672.47
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氧化铝用量/份150200250300350400450
黏度/(mPa·s)1 5391 9243 0784 9007 03716 14765 009
沉降率/%48.938.431.625.312.37.91.1
阻燃等级FV-2FV-2FV-1FV-1FV-0FV-0FV-0
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球形氧化铝填充量对有机硅灌封胶性能的影响

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氧化铝用量/份150200250300350400450
黏度/(mPa·s)1 5391 9243 0784 9007 03716 14765 009
沉降率/%48.938.431.625.312.37.91.1
阻燃等级FV-2FV-2FV-1FV-1FV-0FV-0FV-0
), ArticleFig(id=1203362948732399637, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1203281643889996038, language=EN, label=Table 4, caption=Effect of different sizes of spherical alumina compound filling on the performance of silicone encapsulant, figureFileSmall=null, figureFileBig=null, tableContent=
m(5 μm)∶m(15 μm)∶m(50 μm)4∶3∶33∶4∶32∶5∶31∶6∶31∶7∶21∶8∶2
黏度/(mPa·s)3 6283 7934 0504 1234 2884 178
导热系数/(W/(m·K))0.940.940.960.840.910.93
硬度/邵氏A646464656566
拉伸强度/MPa1.551.401.331.361.311.49
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不同粒径球形氧化铝复配填充对有机硅灌封胶性能的影响

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m(5 μm)∶m(15 μm)∶m(50 μm)4∶3∶33∶4∶32∶5∶31∶6∶31∶7∶21∶8∶2
黏度/(mPa·s)3 6283 7934 0504 1234 2884 178
导热系数/(W/(m·K))0.940.940.960.840.910.93
硬度/邵氏A646464656566
拉伸强度/MPa1.551.401.331.361.311.49
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氧化铝复配填充量/份300350400450500550600
黏度/(mPa·s）4 0506 5079 00011 71023 89293 026294 213
沉降率/%19.318.818.24.53.11.00
阻燃等级FV-1FV-0FV-0FV-0FV-0FV-0FV-0
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球形氧化铝复配填充量对有机硅灌封胶性能的影响

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黏度/(mPa·s）4 0506 5079 00011 71023 89293 026294 213
沉降率/%19.318.818.24.53.11.00
阻燃等级FV-1FV-0FV-0FV-0FV-0FV-0FV-0
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自流平加成型有机硅导热灌封胶的制备
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吴阳 , 张宇 , 孙双双 , 王传增 , 蔺红桃 , 陈淑海
绝缘材料 | 材料研究 2025,58(6): 88-93
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绝缘材料 | 材料研究 2025, 58(6): 88-93
自流平加成型有机硅导热灌封胶的制备
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吴阳, 张宇, 孙双双, 王传增, 蔺红桃, 陈淑海
作者信息
  • 山东理工大学 化学化工学院，山东 淄博 255000

    • 吴阳（2000-），男（汉族），宁夏中卫人，硕士生，主要从事高分子材料的研究；

通讯作者:

陈淑海（1983-），男（汉族），山东临沂人，教授，博士，主要从事高分子材料的研究。
Preparation of self-leveling polyaddition silicone encapsulant with outstanding thermal conductivity
Yang WU, Yu ZHANG, Shuangshuang SUN, Chuanzeng WANG, Hongtao LIN, Shuhai CHEN
Affiliations
  • School of Chemistry and Chemical Engineering, Shandong University of Technology, Zibo 255000, China
出版时间: 2025-06-20 doi: 10.16790/j.cnki.1009-9239.im.2025.06.011
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摘要
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以不同黏度的端乙烯基硅油复配为基体，含氢硅油为交联剂，球形氧化铝为导热补强填料，制备了具有优异导热性能、自流平性能、力学性能及阻燃性能的有机硅灌封胶。探究了不同黏度的端乙烯基硅油复配比例、活性氢与乙烯基的摩尔比、填料配比及填充量对有机硅灌封胶性能的影响。结果表明：PDMS-1和PDMS-2两种端乙烯基硅油按质量比1∶1混合作为基体、活性氢与乙烯基摩尔比R=1.2、不同粒径的球形氧化铝质量比m(5 μm)∶m(15 μm)∶m(50 μm)=2∶5∶3时，灌封胶性能最佳。当不同粒径的球形氧化铝总填充量达500份时，灌封胶的导热系数可达1.50 W/(m·K)，拉伸强度为1.70 MPa，垂直燃烧等级为FV-0，具有优异的操作加工性能以及分散稳定性，综合性能优异。

加成型有机硅灌封胶  /  导热系数  /  球形氧化铝  /  阻燃  /  自流平

A kind of silicone encapsulant with excellent thermal conductivity, self-leveling properties, mechanical properties, and flame retardancy was prepared by employing end vinyl silicone oil with different viscosity as matrix, containing hydrogen silicone oil as cross-linking agent, and spherical alumina as thermal conductive and reinforcement filler. The effects of ratio of end vinyl silicone oils with different viscosity, molar ratio of active hydrogen and vinyl, filler ratio and filling amount on the performance of silicone encapsulant were investigated. The results show that the silicone encapsulant has the best performance when the PDMS-1 and PDMS-2 vinyl end silicone oil are mixed at a mass ratio of 1∶1 as the matrix, the molar ratio of active hydrogen and vinyl is 1.2, and the ratio of spherical alumina with different particle sizes m(5 μm)∶m(15 μm)∶m(50 μm)=2∶5∶3. When the total filling amount of different sizes of spherical alumina reaches 500 parts, the silicone encapsulant has up to 1.50 W/(m·K) of thermal conductivity, up to 1.70 MPa of tensile strength, FV-0 of vertical combustion grade, and excellent operation and processing performance as well as dispersing stability, and its comprehensive performance is excellent.

polyaddition silicone encapsulant  /  thermal conductivity  /  spherical alumina  /  flame retardance  /  self-leveling
吴阳, 张宇, 孙双双, 王传增, 蔺红桃, 陈淑海. 自流平加成型有机硅导热灌封胶的制备. 绝缘材料, 2025 , 58 (6) : 88 -93 . DOI: 10.16790/j.cnki.1009-9239.im.2025.06.011
Yang WU, Yu ZHANG, Shuangshuang SUN, Chuanzeng WANG, Hongtao LIN, Shuhai CHEN. Preparation of self-leveling polyaddition silicone encapsulant with outstanding thermal conductivity[J]. Insulating Materials, 2025 , 58 (6) : 88 -93 . DOI: 10.16790/j.cnki.1009-9239.im.2025.06.011
正文
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0 引言
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随着现代电子科学技术的快速发展，各式各样的电子器件逐渐应用于生活、军事以及航空航天等领域。随着电子元件不断地趋于微型化、高精度化和高功率化，对热释放的要求越来越高，如果不采用适当的散热技术，会大幅增加电子器件的损耗，降低使用寿命、增加安全隐患及维护成本等。有机硅灌封胶材料耐高低温，可在-60～200℃长期保持稳定的性能[1-3]，同时具有优异的耐候性、耐化学腐蚀性、电绝缘性能及高温快速固化等优点[4-8]。因此，有机硅灌封胶材料在电子元件封装及防护等领域具有广泛的研究潜力和应用前景[9-11]。
有机硅灌封胶的导热系数较低，约为0.2 W/(m·K)，无法满足实际生产生活中的散热需求，严重影响电子设备的使用寿命，且会增加安全隐患，因此需要提升其导热性能及其他各项性能。其中通过在灌封胶中添加各类功能性填料的方式可以有效提升灌封胶的各项性能，并且具有成本低廉的特点，已被广泛用于改善灌封胶导热性能的研究。刘廷铸等[12]采用γ-氨丙基三乙氧基硅烷（KH-550）作填料改性剂对石英砂进行改性处理，研究了填料粒径和填充量对有机硅灌封胶性能的影响，结果表明当20 μm石英砂填充量为200份时，灌封胶的导热系数提升至0.73 W/(m·K)；曹鹤[13]以石英砂、改性氧化铝、空心玻璃微珠为主要填料，制得了一种低密度阻燃导热型有机硅灌封胶，硫化后灌封胶的密度为1.28 g/cm3，导热系数为0.53 W/(m·K)；王宝喜等[14]以石英砂为导热填料，氢氧化铝为阻燃填料，制备了导热阻燃型灌封胶，研究了硅油黏度、填料粒径以及填料填充量对有机硅灌封胶性能的影响，结果发现灌封胶的导热系数为0.53 W/(m·K)，阻燃等级达到FV-0级；潘科学等[15]以不同黏度的复配乙烯基硅油和含氢硅油为基料，添加氧化铝作为导热填料，制备了绝缘导热型有机硅灌封胶，当氧化铝填充量为150份时，灌封胶的导热系数为0.51 W/(m·K)。目前所研究的加成型有机硅灌封胶均存在导热系数较低、力学性能欠佳、胶料流动性较差的问题，尤其是导热性能作为一直以来需要攻克的难题，限制了有机硅灌封胶材料的实际应用。
本研究以不同黏度的端乙烯基硅油复配体系为基体材料，研究基体的配比，以及球形氧化铝作为导热填料对有机硅灌封胶各项性能的影响，制备具有高导热系数、良好物料相容性、流动性、阻燃性能和力学性能等综合性能良好的有机硅导热灌封胶。
1 实验
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1.1 主要原材料及仪器设备
端乙烯基硅油：DY-V401-180，牌号PDMS-1，黏度为180 mPa·s，乙烯基含量为0.027 mol/100 g，山东大易化工有限公司；DY-V401-500，牌号PDMS-2，黏度为500 mPa·s，乙烯基含量为0.015 mol/100g，山东大易化工有限公司；含氢硅油：DY-212T，活性氢质量分数为0.35%，山东大易化工有限公司；Karstedt铂催化剂：铂含量为2 000×10-6，东莞市澳凯新材料有限公司；抑制剂乙炔基环己醇：分析纯，上海运河材料有限公司；石英砂：粒径为7.5 μm，工业级，上海博彤化工有限公司；球形氧化铝：粒径分别为5、15、50 μm，工业级，上海清北新材料科技公司。
高速分散机：QSD，天津材料试验机厂；数显黏度计：LC-NDJ-8T，上海力辰邦西仪器科技有限公司；邵氏硬度计：LX-A-1，江都天惠试验机械有限公司；导热系数测定仪：DRL-III，湘潭仪器仪表有限公司；万能试验机：CMT4303，深圳市新三思计量技术有限公司；场发射扫描电子显微镜：S-4800，日本日立公司。
1.2 成品制备
（1）基料制备：将填料在150℃烘箱中高温除湿4 h，之后自然冷却至室温备用，PDMS-1和PDMS-2按比例混合（100份），再加入相应份量的填料，将上述混料在高速分散机中混合30 min，抽真空脱泡10 min，制得基料。
（2）A组分：取100份基料、0.2份铂催化剂，在高速分散机中混合均匀，抽真空脱泡得到A组分。
（3）B组分：取100份基料、加入一定量的含氢硅油、0.05份抑制剂，在高速分散机中混合均匀，抽真空脱泡得到B组分。
（4）混合制样：将A、B组分按质量比1∶1混合均匀脱泡，倒入模具中，在90℃下硫化2 h制成试片。
1.3 性能测试
黏度：将制备的基料抽真空脱泡后在室温下静置2 h，使用LC-NDJ-8T型数显黏度计在室温下按照GB/T 2794—1995进行测定。
硬度：采用LX-A-1型邵氏硬度计按照GB/T 531.1—2008进行测试。
拉伸性能：将样品裁剪为哑铃型，厚度为2 mm，采用CMT4303型万能试验机按照GB/T 528—2009进行测试。
导热系数：将样品裁剪成直径为30 mm、厚度为2 mm的圆形样品，使用稳态法导热仪按照GB/T 11205—2009进行测试。
扫描电子显微镜（SEM）分析：将样品拉断和液氮脆断后进行喷金处理，采用扫描电子显微镜观察样品断面形貌，加速电压为20 kV。
阻燃性能：采用垂直燃烧法，按UL 94-2006进行测试。
沉降率：取适量的基料，用注射器缓缓将其注入玻璃瓶中，在室温下密封静置两个月后，测量上层清液和总液面的高度，用式（1）计算出沉降率。
沉降率=上清液高度液面总高度×100%
2 结果与讨论
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2.1 基体的配比对有机灌封胶性能的影响
为使物料具有较低黏度，同时成品拥有较好的力学性能，本研究选取了黏度为150 mPa·s（PDMS-1）和500 mPa·s（PDMS-2）的乙烯基硅油进行复配，填料为粒径为7.5 μm的石英砂，填充量为150份，研究乙烯基硅油最佳的复配比例，调节乙烯基含量使得灌封胶性能最佳。表1为两种乙烯基硅油不同复配比例对灌封胶性能的影响。
由表1可知，随着PDMS-1比例增大，乙烯基含量随之升高，物料黏度降低，灌封胶硬度升高，拉伸强度先增大后减小。其原因是在其他条件一致的情况下，随着PDMS-1比例增大，黏度较大的乙烯基硅油比例逐渐减少，物料黏度随之降低，同时乙烯基含量增大，灌封胶交联密度增大，硬度升高；当乙烯基含量由0.015 mol/100 g增加到0.021 mol/100 g时，交联密度的增大使得灌封胶内应力可以更好地释放，并均匀分散，有助于拉伸强度的提升，继续增大乙烯基含量则会导致交联密度过大，交联网络应力集中，导致拉伸强度下降，成品更易断裂。
采用合适比例的乙烯基硅油复配作为基体，通过调节基体中的乙烯基含量，使得灌封胶具有优异流动性的前提下兼顾较好的力学性能，综合考虑，实验选择m(PDMS-1)∶m(PDMS-2)=1∶1的乙烯基硅油复合体系作为基体。
2.2 R值对有机硅灌封胶性能的影响
理想状况下，乙烯基硅油中的硅乙烯基和含氢硅油中的硅氢键反应摩尔比（R）应为1∶1，但在实际反应中，会发生一定量的副反应导致分子链之间交联不充分，影响灌封胶的性能，因而实际应用中R值（R=n(Si-H)/n(Si-Vi)）需要实验来确定。固定填料为7.5 μm石英砂，填充量为150份，研究R值对灌封胶性能的影响，结果如表2所示。由表2可知，随着R值的增大，含氢硅油用量增多，交联密度逐渐增大，导致硬度也逐步增大，拉伸强度先增大后减小。这是由于适量增大R值有利于交联网络的形成，增强成品的拉伸强度，继续增大R值导致交联过度，成品变硬变脆，且过量含氢硅油残留在体系中灌封胶的力学性能反而下降。综合实验结果，选择R=1.2可使灌封胶性能最佳。
2.3 球形氧化铝用量对有机硅灌封胶性能的影响
常见的氧化铝通常为α晶型，形貌多样，如片状、不规则形状等，相较于普通氧化铝，球形氧化铝具有良好的形貌、更高的导热系数、更好的分散性等优点。本实验采用粒径为15 μm的球形氧化铝为导热补强填料，研究其填充量对有机硅灌封胶性能的影响，结果如表3所示。
由表3可知，随着球形氧化铝填充量的增加，灌封胶黏度逐渐增大，球形氧化铝填充量达到450份时，灌封胶的黏度剧增，达到65 009 mPa·s，流动阻力明显增大，流动性变差，同时沉降率逐步接近于0%，证明填料在基体中具有较好的分散稳定性，防沉降效果极佳。随着填料填充量的增加，灌封胶的阻燃性能也得到提升，在球形氧化铝填充量为350份时，灌封胶的阻燃等级为FV-0，表明球形氧化铝的添加不仅提升了灌封胶的导热性能，同时对其阻燃性能也有显著的提高。
图1为球形氧化铝填充量对有机硅灌封胶导热系数的影响。由图1可知，随着球形氧化铝填充量的增加，所形成的导热通路越来越完整，灌封胶的导热系数逐步提升，当球形氧化铝填充量由150份增加到450份时，灌封胶的导热系数从0.56 W/(m·K)提升至1.19 W/(m·K)，导热系数与填料填充量几乎成线性关系，虽在400～450份区间增幅有所下降，但上升趋势并未停止。
图2为球形氧化铝填充量对有机硅灌封胶拉伸强度和硬度的影响。由图2可知，随着球形氧化铝填充量的增加，有机硅灌封胶的硬度逐步提高，拉伸强度先增大后减小，在球形氧化铝填充量为300份时，拉伸强度达到最大值，为1.54 MPa。这是由于球形氧化铝分子与基体之间的相互作用力较小，随着氧化铝填充量的进一步增加，填料之间互相接触堆叠，基体整体强度下降，导致成品力学性能变差。
2.4 不同粒径球形氧化铝复配制备高性能有机硅灌封胶
为了进一步提升有机硅灌封胶的导热性能，形成更加完整的导热通路，同时兼顾优异的力学性能，本研究使用不同粒径的球形氧化铝复配作为导热补强填料，为探索出最佳复配比例，选取了不同氧化铝复配比例的灌封胶进行性能对比，总填充量固定为300份，测试结果如表4所示。由表4可知，当3种粒径球形氧化铝质量比m(5 μm)∶m(15 μm)∶m(50 μm)=2∶5∶3时，灌封胶的导热性能最佳，此时导热系数由单一粒径、相同填充量下的0.89 W/(m·K)提升至0.96 W/(m·K)，力学性能也同时兼顾。
选定粒径为5、15、50 μm的球形氧化铝复配质量比为2∶5∶3，研究球形氧化铝复配填充总量对灌封胶性能的影响，结果如表5所示。由表5可知，随着球形氧化铝复配填充量的增加，灌封胶各项性能相较单一粒径球形氧化铝填充时有较为明显的提升，当氧化铝复配填充量由300份增加至500份时，灌封胶黏度由4 050 mPa·s增大至23 892 mPa·s，当氧化铝复配填充量超过550份时，灌封胶黏度突增，流动性变差；当氧化铝复配填充量高于450份时，灌封胶沉降率很低，表现出良好的分散稳定性和防沉降性能；同时氧化铝自身是天然的阻燃剂，当氧化铝复配填充量达到350份后，灌封胶的阻燃等级可达到FV-0，满足实际应用中的阻燃要求，提升了灌封胶的安全系数。
图3为球形氧化铝复配填充量对有机硅灌封胶导热系数的影响。由图3可知，随着氧化铝复配填充量的增加，灌封胶的导热系数先升高后降低，由300份时的0.96 W/(m·K)增加到500份时的最大值1.50 W/(m·K)后，又逐步降低。这是由于氧化铝复配填充量较少时，填料颗粒被基体所包裹，但是由于填料填充密度很小，填料之间彼此孤立，少有相互连接，无法形成有效的导热网络。随着氧化铝复配填充量的增加，粒子之间的连接愈加紧密，通过导热颗粒间的传热路径占比增大，传热速率加快，导热系数呈上升趋势，并在氧化铝复配填充量为500份时达到最大值，导热填料对导热网络形成的贡献也达到最大。继续增加填充量，新的导热通路增加已不再明显，填料用量对导热性能无优化作用，且填充量达到一定阈值后，填料之间堆积重叠，无法均匀分散至基体中，导热通路被破坏，致使导热系数下降。
图4为球形氧化铝复配填充量对有机硅灌封胶拉伸强度和硬度的影响。由图4可知，随着氧化铝复配填充量的增加，灌封胶硬度逐渐升高，拉伸强度先增大后减小，当氧化铝复配填充量为550份时，拉伸强度达到最大值1.80 MPa，继续增加氧化铝复配填充量，灌封胶力学性能下降。相较于单一粒径球形氧化铝的填充，复配粒径氧化铝的填充具有物料黏度更低、成品导热性能更高、力学性能更佳的优点。这是由于复配粒径氧化铝填充时，小粒径能填充在大粒径之间，不同粒径协同填充使得整体结构更加稳定，有利于灌封胶力学性能的提升。
综合实验考察，采用400～500份不同粒径球形氧化铝复配作为导热补强填料，所制备的有机硅灌封胶综合性能较佳，此时灌封胶黏度低，流平性 优异，防沉降效果好，导热系数达到1.22～1.50 W/(m·K)，拉伸强度为1.44～1.70 MPa。
相较其他常见填料，球形氧化铝拥有更低的表面能，填充后物料流动阻力明显减小，黏度相对较低，从而可使填充量提高，灌封胶导热性能提升，同时流平性能、力学性能和阻燃性能也能满足使用要求。
图5为添加球形氧化铝填料的有机硅灌封胶断面SEM图。由图5可知，相较单一粒径填充样品（图5(a)、5(b)），使用不同粒径的球形氧化铝复配填充样品（图5(c)、5(d)）断面更致密，这是由于大小粒径的填料之间相互裹挟填充，物料流动阻力减小，黏度更低，使得填充密度进一步提高，同时形成了更多更加致密完整的导热通路，促进了填料之间的热流动，优化了灌封胶导热性能，同时物料具有优异的流平性能和防沉降性能，保证了其良好的操作加工性能。
图6记录了使用红外热成像摄像机拍摄得到的不同粒径球形氧化铝复配填充的有机硅灌封胶在加热过程中的表面温度随时间的变化所对应的红外热成像图，可以更加具象化表现出灌封胶导热性能的提升。由图6可知，不同粒径球形氧化铝复配的灌封胶导热效果最佳，球形氧化铝通过复配填充的方式，提高了灌封材料表面温度的升高速率和最终稳定温度。实际导热效果与测定得到的导热系数结果一致，进一步证实了实验结果的可靠性。
3 结论
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以黏度为150 mPa·s和500 mPa·s的两种端乙烯基硅油1∶1混合为基体，按R=1.2计算所需的含氢硅油用量，灌封胶基础性能达到最佳状态。以15 μm粒径球形氧化铝为填料，当填充量达到450份时，灌封胶的导热系数为1.19 W/(m·K)，黏度增大明显，流动性变差，导热性能未到极限。为进一步提升有机硅灌封胶性能，采用不同粒径的球形氧化铝复配作为导热补强填料，实验结果表明，复配粒径的方式可以有效降低物料的黏度，灌封胶的导热系数提升至1.50 W/(m·K)，拉伸强度为1.70 MPa，自流平性能良好，防沉降效果极佳，且阻燃等级达到FV-0，综合性能最佳。本研究制备的有机硅灌封胶在保证具有较佳导热阻燃性能和力学性能的基础上，阻燃性能好，具有优异的操作加工性能和防沉降效果，且成本控制较低。
基金
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  • 国家自然科学基金面上项目(22475122)
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2025年第58卷第6期
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doi: 10.16790/j.cnki.1009-9239.im.2025.06.011
  • 接收时间：2024-07-06
  • 首发时间：2025-12-04
  • 出版时间：2025-06-20
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  • 收稿日期：2024-07-06
  • 修回日期：2024-09-14
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国家自然科学基金面上项目(22475122)
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    山东理工大学 化学化工学院，山东 淄博 255000

通讯作者:

陈淑海（1983-），男（汉族），山东临沂人，教授，博士，主要从事高分子材料的研究。
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2种不同金属材料的力学参数
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Number of
species		 占总种数比例
Percentage of
total species (%)		 属
Genus		 种数
Number of
species		 占总种数比例
Percentage of total
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鹅膏菌科Amanitaceae 2 11 5.26 鹅膏菌属 Amanita 10 4.78
小菇科 Mycenaceae 2 12 5.74 丝盖伞属 Inocybe 5 2.39
多孔菌科 Polyporaceae 8 14 6.70 蜡蘑属 Laccaria 5 2.39
红菇科 Russulaceae 3 23 11.00 小皮伞属 Marasmius 6 2.87
小菇属 Mycena 11 5.26
光柄菇属 Pluteus 5 2.39
红菇属 Russula 17 8.13
栓菌属 Trametes 5 2.39
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