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Article(id=1199644782915056221, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1199644777219191267, articleNumber=null, orderNo=null, doi=10.16790/j.cnki.1009-9239.im.2023.12.001, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1680969600000, receivedDateStr=2023-04-09, revisedDate=1685635200000, revisedDateStr=2023-06-02, acceptedDate=null, acceptedDateStr=null, onlineDate=1763947204569, onlineDateStr=2025-11-24, pubDate=1703001600000, pubDateStr=2023-12-20, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1763947204569, onlineIssueDateStr=2025-11-24, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1763947204569, creator=13701087609, updateTime=1763947204569, updator=13701087609, issue=Issue{id=1199644777219191267, tenantId=1146029695717560320, journalId=1149653034449285133, year='2023', volume='56', issue='12', pageStart='1', pageEnd='135', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1763947203211, creator=13701087609, updateTime=1766563728010, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1210619277716099586, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1199644777219191267, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1210619277716099587, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1199644777219191267, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=1, endPage=8, ext={EN=ArticleExt(id=1199644783242211941, articleId=1199644782915056221, tenantId=1146029695717560320, journalId=1149653034449285133, language=EN, title=Research on high temperature and thermal ageing insulation properties of silicone gel material for high voltage IGBT packaging, columnId=1199644778280350182, journalTitle=Insulating Materials, columnName=Advanced Electrical Materials for Large Capacity Offshore Wind Power Transmission, runingTitle=null, highlight=null, articleAbstract=

In high-voltage insulated gate bipolar transistor (IGBT) devices, traditional Si-based semiconductor chips are gradually replaced by emerging wide-bandgap semiconductor chips. High-power-density wide-bandgap semiconductors lead to a sharp rise of operating temperature in power electronic modules. Silicone gel is used as an insulating material for the packaging of high-voltage IGBT devices, and its insulating performance faces the challenges of high temperature and thermal ageing. In order to study the effects of high temperature and thermal ageing on the thermal stability and insulating properties of silicone gel, we studied the effects of high temperature and long-term thermal stress on the dielectric properties, volume conductivity, and breakdown strength of silicone gel by high temperature experiments and thermal ageing experiments of silicone gel materials, and analyzed the high temperature characteristics and thermal ageing characteristics of the silicone gel. The results show that with the increase of temperature, the real part of complex permittivity and breakdown strength of silicone gel decreases, and the dielectric loss and DC conductivity increases. With the increase of thermal ageing time, the real part of complex permittivity of silicone gel increases, the dielectric loss decreases at first and then increases, the DC conductivity increases at first and then decreases, and the breakdown strength decreases.

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在高压IGBT器件中，新兴的宽禁带半导体芯片逐渐代替了传统的硅基半导体芯片，其高功率密度特性会导致电力电子模块的工作温度急剧上升。硅凝胶作为高压IGBT器件的封装用绝缘材料，其绝缘性能面临高温和热老化的挑战。为了研究高温和热老化对硅凝胶材料热稳定性和绝缘性能的影响，本文基于硅凝胶材料的高温试验与热老化试验，测试了高温和长期热应力作用对硅凝胶材料介电性能、体积电导率和击穿强度的影响，对硅凝胶的高温特性和热老化特性进行分析。结果表明：随着温度的升高，硅凝胶的复介电常数实部降低、介质损耗增加、直流电导率升高、击穿强度降低；随着热老化时间的增加，硅凝胶的复介电常数实部增加、介质损耗先减小后增大、直流电导率先增大后减小、击穿强度降低。

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张博雅（1990-），男（汉族），陕西西安人，副教授，主要从事高电压与绝缘技术教学与科研工作。
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姚茗瀚（2000-），男（汉族），辽宁本溪人，硕士生，主要从事高压绝缘材料性能的研究。

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姚茗瀚（2000-），男（汉族），辽宁本溪人，硕士生，主要从事高压绝缘材料性能的研究。

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姚茗瀚（2000-），男（汉族），辽宁本溪人，硕士生，主要从事高压绝缘材料性能的研究。

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典型性能测试结果
组分A黏度/(mPa·s)450
组分B黏度/(mPa·s)425
混合后黏度/(mPa·s)475
25℃工作时间(适用期)/h>24
锥入度(0.1 mm)65
电气强度/(kV/mm)20
介电常数(100 Hz)2.85
介电常数(100 kHz)2.85
体积电阻率/(×1015 Ω·cm)0.95
介质损耗因数(100 Hz)0.001 60
介质损耗因数(100 kHz)0.000 07
热膨胀系数/(×10-6℃-1)425
25℃保质期/d180
), ArticleFig(id=1211311075493016426, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1199644782915056221, language=CN, label=表1, caption=

道康宁3-4170型硅凝胶的典型性能

, figureFileSmall=null, figureFileBig=null, tableContent=
典型性能测试结果
组分A黏度/(mPa·s)450
组分B黏度/(mPa·s)425
混合后黏度/(mPa·s)475
25℃工作时间(适用期)/h>24
锥入度(0.1 mm)65
电气强度/(kV/mm)20
介电常数(100 Hz)2.85
介电常数(100 kHz)2.85
体积电阻率/(×1015 Ω·cm)0.95
介质损耗因数(100 Hz)0.001 60
介质损耗因数(100 kHz)0.000 07
热膨胀系数/(×10-6℃-1)425
25℃保质期/d180
), ArticleFig(id=1211311075581096814, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1199644782915056221, language=EN, label=Tab.2, caption=The scale parameter and shape parameter of AC breakdown strength at different temperatures, figureFileSmall=null, figureFileBig=null, tableContent=
温度/℃尺度参数α/(kV/mm)形状参数β
3016.704.05
6013.114.37
9011.865.45
12011.8110.45
1509.5711.11
1808.047.56
), ArticleFig(id=1211311076835193713, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1199644782915056221, language=CN, label=表2, caption=

不同温度下交流击穿强度的尺度参数和形状参数

, figureFileSmall=null, figureFileBig=null, tableContent=
温度/℃尺度参数α/(kV/mm)形状参数β
3016.704.05
6013.114.37
9011.865.45
12011.8110.45
1509.5711.11
1808.047.56
), ArticleFig(id=1211311076948439926, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1199644782915056221, language=EN, label=Tab.3, caption=The scale parameter and shape parameter of AC breakdown strength at different thermal ageing time, figureFileSmall=null, figureFileBig=null, tableContent=
老化时间/h尺度参数α/(kV/mm)形状参数β
016.704.05
10014.007.04
50011.854.86
1 00011.669.45
), ArticleFig(id=1211311077028131709, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1199644782915056221, language=CN, label=表3, caption=

不同老化时间下交流击穿强度的尺度参数和形状参数

, figureFileSmall=null, figureFileBig=null, tableContent=
老化时间/h尺度参数α/(kV/mm)形状参数β
016.704.05
10014.007.04
50011.854.86
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高压IGBT封装硅凝胶材料高温和热老化绝缘特性研究
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姚茗瀚 1 , 江心宇 1 , 杨紫月 1 , 李凯旋 1 , 莫申扬 2 , 童颜 2 , 张博雅 1 , 李兴文 1
绝缘材料 | 面向大容量海上风电送出的先进电工材料 2023,56(12): 1-8
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绝缘材料 | 面向大容量海上风电送出的先进电工材料 2023, 56(12): 1-8
高压IGBT封装硅凝胶材料高温和热老化绝缘特性研究
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姚茗瀚1, 江心宇1, 杨紫月1, 李凯旋1, 莫申扬2, 童颜2, 张博雅1, 李兴文1
作者信息
  • 1西安交通大学 电气工程学院 电力设备电气绝缘国家重点实验室,陕西 西安 710049
  • 2南瑞集团有限公司,江苏 南京 211000

    • 姚茗瀚（2000-），男（汉族），辽宁本溪人，硕士生，主要从事高压绝缘材料性能的研究。

通讯作者:

张博雅（1990-），男（汉族），陕西西安人，副教授，主要从事高电压与绝缘技术教学与科研工作。
Research on high temperature and thermal ageing insulation properties of silicone gel material for high voltage IGBT packaging
Minghan YAO1, Xinyu JIANG1, Ziyue YANG1, Kaixuan LI1, Shenyang MO2, Yan TONG2, Boya ZHANG1, Xingwen LI1
Affiliations
  • 1State Key Laboratory of Electrical Insulation and Power Equipment, School of Electrical Engineering, Xi′an Jiaotong University, Xi′an 710049, China
  • 2NARI Group Co., Ltd., Nanjing 211000, China
出版时间: 2023-12-20 doi: 10.16790/j.cnki.1009-9239.im.2023.12.001
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摘要
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在高压IGBT器件中，新兴的宽禁带半导体芯片逐渐代替了传统的硅基半导体芯片，其高功率密度特性会导致电力电子模块的工作温度急剧上升。硅凝胶作为高压IGBT器件的封装用绝缘材料，其绝缘性能面临高温和热老化的挑战。为了研究高温和热老化对硅凝胶材料热稳定性和绝缘性能的影响，本文基于硅凝胶材料的高温试验与热老化试验，测试了高温和长期热应力作用对硅凝胶材料介电性能、体积电导率和击穿强度的影响，对硅凝胶的高温特性和热老化特性进行分析。结果表明：随着温度的升高，硅凝胶的复介电常数实部降低、介质损耗增加、直流电导率升高、击穿强度降低；随着热老化时间的增加，硅凝胶的复介电常数实部增加、介质损耗先减小后增大、直流电导率先增大后减小、击穿强度降低。

高压IGBT模块  /  绝缘封装  /  有机硅凝胶  /  高温  /  热老化

In high-voltage insulated gate bipolar transistor (IGBT) devices, traditional Si-based semiconductor chips are gradually replaced by emerging wide-bandgap semiconductor chips. High-power-density wide-bandgap semiconductors lead to a sharp rise of operating temperature in power electronic modules. Silicone gel is used as an insulating material for the packaging of high-voltage IGBT devices, and its insulating performance faces the challenges of high temperature and thermal ageing. In order to study the effects of high temperature and thermal ageing on the thermal stability and insulating properties of silicone gel, we studied the effects of high temperature and long-term thermal stress on the dielectric properties, volume conductivity, and breakdown strength of silicone gel by high temperature experiments and thermal ageing experiments of silicone gel materials, and analyzed the high temperature characteristics and thermal ageing characteristics of the silicone gel. The results show that with the increase of temperature, the real part of complex permittivity and breakdown strength of silicone gel decreases, and the dielectric loss and DC conductivity increases. With the increase of thermal ageing time, the real part of complex permittivity of silicone gel increases, the dielectric loss decreases at first and then increases, the DC conductivity increases at first and then decreases, and the breakdown strength decreases.

high voltage IGBT module  /  insulating package  /  silicone gel  /  high temperature  /  thermal ageing
姚茗瀚, 江心宇, 杨紫月, 李凯旋, 莫申扬, 童颜, 张博雅, 李兴文. 高压IGBT封装硅凝胶材料高温和热老化绝缘特性研究. 绝缘材料, 2023 , 56 (12) : 1 -8 . DOI: 10.16790/j.cnki.1009-9239.im.2023.12.001
Minghan YAO, Xinyu JIANG, Ziyue YANG, Kaixuan LI, Shenyang MO, Yan TONG, Boya ZHANG, Xingwen LI. Research on high temperature and thermal ageing insulation properties of silicone gel material for high voltage IGBT packaging[J]. Insulating Materials, 2023 , 56 (12) : 1 -8 . DOI: 10.16790/j.cnki.1009-9239.im.2023.12.001
正文
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0 引言
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高压大功率绝缘栅双极型晶体管（insulated gate bipolar transistor，IGBT）作为新能源的基础和关键部件，广泛应用于风电变流器、光伏逆变器、电动汽车、高铁牵引、高压直流输电等高新技术领域。随着IGBT器件向高电压、高功率密度的方向发展[1-2]，要求其绝缘封装材料具有更加优秀的电学、热学与力学性能[3]。
随着对电子封装系统小型化需求的不断提升，环氧塑封料（EMC）逐渐成为电子封装的关键材料[4]，其具有高可靠性、低成本和适合大规模自动化生产等优点，但是其散热性能受限于环氧树脂的分子结构，合成过程中也会生成有害物质[5]。聚酰亚胺（PI）作为当前热门的耐高温树脂封装材料，具有优异的绝缘性能、热性能、力学性能和化学稳定性[6]，但PI分子量刚性较强，加工性能较差。硅凝胶作为一种IGBT模块封装用绝缘材料，其固化后具有高黏度、防潮、防尘、防污、抗冲击和防振动等优点[7]，能够保护器件基板、半导体和连接处免受潮湿、污渍和振动的影响[8-11]，同时有着良好的电气绝缘性和耐高温性。
在IGBT器件中使用Si基半导体芯片工作时，内部最高结温会达到175℃[12]，而使用新一代宽禁带（wide band gap，WBG）半导体材料制造IGBT器件的芯片时，例如SiC基半导体芯片，在商业级应用方面其最高结温为225℃，在实验室中甚至可以实现在600℃条件下运行[12-16]。长期在高温环境下运行，会改变IGBT封装用有机硅凝胶的化学结构和内部成分，材料结构的变化会导致其相关特性退化[17]，从而使硅凝胶的绝缘性能发生一定程度的劣化[18-19]。M OHARA[20]发现硅凝胶在高温（200℃或更高）下受到长时间的热作用影响后会变硬变脆，完全失去弹性，最终开裂。陈庆国等[21]在120℃下对硅橡胶试样开展了人工加速热老化试验，结果表明热老化后的硅橡胶试样相对介电常数减小，随着热老化时间的增加，材料硬度逐渐增加，交联程度增大。毛塬[12]对有机硅凝胶在175℃温度下进行老化试验，并对其介电特性进行研究，发现随着热应力作用时间的延长，有机硅凝胶材料的相对介电常数减小。M T DO等[22]在宽频（10-4～103 Hz）和宽温（20～160℃）范围内研究了硅凝胶的介质损耗谱，得到其介电特性，并且特别关注了老化时间对硅凝胶介质损耗的影响。陈日荣等[23]在180℃条件下对有机硅凝胶进行了加速热氧老化试验，对发生热氧老化的机理进行了初步解释。上述文献分析了硅凝胶材料在一定温度以及一定频率范围内高温与老化性能的关系，但是缺乏对高温与热老化特性关系的表征参量研究，尤其是硅凝胶的热老化机理尚不明晰。
针对高压IGBT器件的绝缘需求，本文深入研究封装用硅凝胶材料的介电性能、电阻率以及击穿电压随频率、温度和老化时间的变化趋势，进一步阐释硅凝胶材料的热老化机理。由于硅凝胶材料应用于各种电力电子器件封装，研究高温及热老化后硅凝胶材料的电学特性，对评估电力电子器件的绝缘状态具有十分重要的意义，可为长期在热应力作用下工作的电力电子模块封装设计提供数据支撑。
1 试样制备与测试平台
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1.1 试样制备
本研究使用的原料为道康宁3-4170的A/B型硅凝胶，典型性能如表1所示。该硅凝胶具有清晰透明、快速热固化、工作时效长、黏度低的特点，其中快速热固化能够在生产中提高产品的加工速度。A、B组分均为无色无味油状液体，具体制备步骤如下：先将A胶和B胶按照质量比为1∶1配置在烧杯中，用玻璃棒对混合液体手动搅拌5 min，使组分混合均匀；然后将混合液置于真空设备中，在0.02 MPa压强下脱气20 min，之后将脱气混合液用一次性滴管转移至铺有0.1 mm厚石墨纸的培养皿上，使硅凝胶样品被培养皿定型成附着在石墨纸上的薄膜，直径同培养皿尺寸，厚度为0.1～0.5 mm；最后将培养皿置于恒温电热鼓风干燥箱中，在100℃下固化9 min，即可得到试验样品。由于硅凝胶黏度高，制备的薄膜样品操作面积较大，厚度均匀且较薄，样品可以在短时间内重复制备，批量测试。
将所制试样分为3组，未老化样品组作为对照组，其余两组分别放入恒温电热鼓风干燥箱中进行500 h与1 000 h老化，设置两组老化温度，分别为85℃和150℃，使试样暴露于空气中。为避免样品温度变化对测试的影响，每次老化周期结束后，取出样品在干燥环境放置30 min，待其温度下降到室温再进行测试。
1.2 测试平台
采用Novocontrol CONCEPT 80型宽频域介电谱测试系统测量硅凝胶的介电特性，测试电压设置为1 V AC，样品厚度为0.1～0.5 mm，测试直径为20 mm。本文选取30℃和150℃两个温度对样品进行10-1～106 Hz频段的介电测试，得到试样的频域介电谱，并对不同温度、不同老化时间下的介电特性曲线进行分析。
采用高温电阻率测试系统测量硅凝胶的体积电阻率，该测试系统由高温烘箱和内置电压源的Keithley 6517B型静电计组成。根据 IEC 62631-3-1-2016[24]，测试方法为三电极法，下平板电极直径d1=58 mm，上平板电极直径d2=50 mm，环形辅助电极内外直径d3=54 mm、d4=58 mm，测试电压为1 000 V DC。研究高温特性时样品厚度为0.16 mm，电场强度为6.25 kV/mm，温度测试范围为30～180℃。研究老化特性时样品厚度为0.3 mm±0.1 mm。传导电流在测量过程中逐渐下降并趋于稳定，待电流值稳定计算体积电阻率。
根据IEC 60243-1-2013[25]测试硅凝胶的击穿强度，测试平台如图1所示，由高压电源、千分尺和绝缘支架组成。在大气环境中使用球-板电极系统测量样品，球形电极与样品相切，测试时将石墨纸作为接地板电极。击穿实验中顶部电极为高压电极，使用50 Hz的交流电压，并以1 kV/s的速率增加。使用加热台研究高温下的击穿电压（可在室温至300℃之间调节），每次测试前对样品进行一定时间的预热，确保温度恒定且分布均匀，温度测试范围为30～180℃。试验结束后记录击穿点，用千分尺测量击穿点的厚度。为避免高压电极周边局部放电打火，排除样品界面闪络的情况，总共进行了10余次测试，保证每个测试组至少记录10个击穿点。采用双参数的Weibull分布函数对击穿数据进行处理，Weibull分布函数如式（1）所示。
F(E, α, β)=1-exp-(Eα)β
式（1）中：F(E，α，β)是击穿强度的累积概率密度分布函数；E为试验得到的击穿强度值；α是尺度参数，代表样品击穿累积概率达到63.2%的特征场强，也被称为威布尔击穿场强EBD；β为形状参数，与样品缺陷和试验条件有关。
2 硅凝胶的高温特性
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2.1 硅凝胶的介电-温度特性
材料的介电特性可以用介电函数来表示：ε*=ε′-jε″，其中ε*代表复介电常数，ε′代表复介电常数实部，ε″代表复介电常数虚部。在30℃和150℃下硅凝胶的ε′与介质损耗因数（tanδ）随频率变化曲线如图2所示。
从图2(a)可以看出，在30℃环境下，ε′基本维持在2.8左右；在高温150℃环境下，在低频区（10-1～101 Hz）ε′呈现陡坡式下降，在高频区ε′逐渐稳定在2.08左右。可以看出温度从30℃升高到150℃，在高频稳定状态下样品的ε′降低了26.1%。
对上述现象给出如下解释：硅凝胶为弱极性电介质，其在外电场作用下的主要极化形式为电子位移极化和偶极子转向极化，因此相对介电常数较小，在30℃下维持在2.8左右[26]。电子位移极化所需时间极短（10-15 s），基本不随频率变化，因此偶极子取向极化成为影响ε′变化的主要原因，随着电场频率的升高，偶极子取向极化速度低于电场交变频率，极化现象会有所衰减，此时ε′会因偶极子转向极化衰减而下降。
从30℃到高温150℃的过程中，分子的热运动随温度的升高而增强，在高温的促进作用下，分子活性迅速增强，分子热运动加剧到妨碍沿电场方向的取向程度，导致极化程度下降，高温下的ε′低于常温下的数值，这一现象也可以用硅凝胶随着温度的升高而膨胀来解释，硅凝胶体积变大，降低了电极之间恒定间隙内的材料密度[27]，从而降低了硅凝胶在高温下储存电荷的能力。
在低频（10-1～101 Hz）时，复介电常数实部会出现低频弥散现象，有机硅凝胶材料的低频弥散现象因温度的升高会更加显著。现有研究将高温下的低频弥散现象归因于界面极化和电极极化的作用[28]，界面极化和电极极化都可以解释为在材料和电极之间的界面上建立了“自由”电荷[26]。其中，界面极化在绝缘材料的掺杂研究中多有应用，而本文制备的硅凝胶样品无掺杂填料，因此低频弥散现象不属于界面极化。电极极化是电极在电场作用下产生电位跳跃、电荷积累的现象，与试验电极的材料和性能相关。本文对有机硅凝胶材料的介电特性进行测量时，由于试验电极为铜（镀金）电极，而高温会加剧电极极化，所以测试结果会受到电极极化在电场作用下积累的空间电荷的影响，从而导致高温下的低频弥散现象更加显著[29]。同时在低频区偶极子取向极化速率不低于电场交变频率，此时高温的主要贡献变成了通过加剧热运动释放更多偶极子来完成极化，使低频下的ε′相较于高频区大幅增加，相比于常温产生了更加明显的弥散现象。
如图2(b)所示，硅橡胶样品在30℃和150℃下的介质损耗因数tanδ均随频率的升高而下降，在低频段（10-1～101 Hz）下降迅速，在10 Hz处接近于0，在高频段（101～106 Hz）下降比较平缓，介质损耗因数维持在10-4量级。介质损耗包括电导损耗和极化损耗两部分，在低频下极化损耗主要取决于偶极子的取向极化损耗，电场的低交变频率给予极化时间长的偶极子足够的转向时间，为偶极子极化提供更多能量，导致介质损耗增大；随着电场交变频率的升高，偶极子尚未开始旋转，极化强度减弱，粒子极化引起的损耗减小。进一步对比高温与常温可知，二者损耗在高频段相差不大，温度带来的差异主要体现在低频区域。温度升高，导电粒子的热运动增强，其平均动能和流动性也增加，导致直流电导率增大，电导损耗增大，同时高温会使得硅凝胶材料释放更多的偶极子，导致在低频下偶极子需要更多的能量来进行取向极化，极化损耗增大。在二者的共同作用下，在低频时高温下的介质损耗远高于常温。
2.2 硅凝胶的电导-温度特性
体积电导率（σv）是表征材料导电性能的宏观参数，与体积电阻率（ρv）互为倒数关系（σv=1/ρv）[30]。通过传导电流值计算得到在30～180℃内硅凝胶的体积电阻率和电导率如图3所示。
从图3可以发现，硅橡胶的体积电导率随着温度的升高而升高，180℃下的体积电导率相比于常温提高了3个数量级。影响体积电导率的主要因素是载流子的迁移率和浓度，随着温度的升高，低温下被束缚的载流子受热激发参与导电，使得硅凝胶内部载流子的浓度升高和迁移率增大，从而导致硅凝胶试样的体积电导率升高[25]。根据载流子的性质，温度对载流子产生的影响可能有两种机制[31-32]：强场电导和弱场电导。在强电场作用下，导电性能由电子或者空穴主导，它们可能来自肖特基效应、Fowler-Nordheim效应、Poole-Frenkel效应和电子的碰撞电离。当温度升高时，肖特基效应、Poole-Frenkel效应和电子的碰撞电离会产生更多的电子。考虑到空间电荷限制电流的影响，传导电流增加，导致直流电导率增加。本文测量电导率时，样品两端的场强为6.25 kV/mm，对于硅凝胶材料而言属于弱场电导，其产生的载流子大部分是离子，它们由材料本身电离产生，而电离是一个化学过程，温度越高，化学反应越快（Arrhenius方程），载流子浓度增加，导致直流电导率增加。
2.3 硅凝胶的击穿-温度特性
图4为不同温度下硅凝胶的交流击穿强度数据的Weibull分布图，其特征参数见表2。从表2可以看出，硅凝胶的交流击穿强度随温度升高而下降。在30℃时，交流击穿强度最高在16 kV/mm以上，而在180℃时，交流击穿强度约为8 kV/mm，降低了51%。温度会影响聚合物材料的击穿强度，且在不同温度范围内击穿机理不同[33]。当温度低于聚合物的玻璃化转变温度时，击穿强度与温度无关，反之击穿强度随温度升高而降低。硅凝胶的玻璃化转变温度为-120℃，击穿测试的温度范围高于其玻璃化转变温度，因此击穿强度与温度呈负相关。同时，硅凝胶的击穿机理可以用粒子的碰撞电离使载流子数倍增加导致雪崩击穿来解释，随着温度的升高，粒子间热运动更加剧烈，碰撞电离现象加剧，导致击穿强度降低。
3 硅凝胶的热老化特性
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在热老化过程中，硅凝胶材料分子链会逐渐发生热氧化、热降解和热裂解反应[34]。热氧化、热降解和热裂解的反应方程式如图5所示。图5(a)为热氧化反应过程，硅凝胶的侧链基团在高温下发生氧化反应。图5(b)为热降解反应过程，Si-O键既是共价键也是离子键，在高温条件下Si-O结构受热分解，出现降解现象。图5(c)为热裂解反应过程，在热作用下，硅凝胶分子链断裂生成小分子，相较于热氧化和热降解反应，热裂解会在更高温度和更长老化周期下发生。
3.1 硅凝胶的介电-热老化特性
图6是在老化温度为150℃的长期热应力作用下，未老化、老化500 h和老化1 000 h硅凝胶试样在测试温度为30℃和150℃下的ε′和tanδ频谱图。
从图6(a)可以看出，经过不同时间的热老化，有机硅凝胶材料的ε′均随频率的升高而降低，在2.1中分析了频率对样品介电特性的影响，此处不再赘述。长期热应力作用下有机硅凝胶材料的ε′相比无热应力作用时明显增加，随着热应力作用时间的延长，ε′也随之增加，在测试温度为30℃时，老化500 h和1 000 h的硅凝胶样品ε′较未老化样品分别提高了32.4%和52.6%，说明有机硅凝胶内部粒子的极化现象更加剧烈。在热老化的早期，样品的交联密度由于热氧化反应而增强，但在此阶段高温促进材料产生极性偶极子对ε′起主导作用；而随着高温老化时间逐渐增加，硅凝胶材料在长时间热应力的作用下出现热降解和热裂解现象，硅凝胶结构分子式中键能较低的化学键受热断裂分解，自由基增多，使得材料的极化弛豫现象更加突出，因此ε′随热老化时间增加而增大。
从图6(b)可以看出，测试温度不影响tanδ的变化趋势，经过不同时间的热老化，有机硅凝胶材料的tanδ均随频率的升高而降低，在高频下稳定在10-4量级。频率对样品介质损耗的影响分析见2.1节。进一步分析图6(b)老化时间对介质损耗的影响可知，在低频段（10-1～101 Hz），样品的介质损耗在老化500 h后减小，而在老化1 000 h后增大。这是由于在热老化前期，硅凝胶发生交联反应，交联密度增加，侧链基团更加稳定不易断裂，介质损耗减少，而长时间热作用会破坏分子结构，极性基团密度和可动性升高，介质损耗增大。介质损耗也可以认为由交流损耗和直流损耗组成，低频下交流损耗几乎不变，直流损耗对介质损耗的影响占主导地位，而随着热作用时间的延长，直流损耗先减小后增大，进而导致低频下的介质损耗先减小后增大。
3.2 硅凝胶的电导-热老化特性
载流子的迁移率和浓度是影响体积电导率的主要因素。在85℃下对硅凝胶样品进行老化处理，测试样品在不同老化时间下的直流电导率，绘制出样品的直流电导率随老化时间的变化曲线如图7所示。从图7可以看出，硅凝胶样品的直流电导率随着老化时间的增加先减小后增大，这与3.1中热老化时间对介质损耗的影响相似，说明交联密度对直流电导率的影响更重要。硅凝胶的交联密度随着热老化时间的延长先升高后降低，短时间内热老化会进一步完善样品的交联结构，深陷阱能级与密度增大抑制了带电离子的脱陷和迁移过程，导致离子迁移率减小，交联网状结构更加致密，自由体积相对减小，载流子运动需要克服更高的势垒能级，使体积电导率略有降低[35]。而长时间热老化使样品发生了热降解和热裂解反应，破坏了分子间结构，导致交联密度下降，样品载流子浓度增多，加速离子迁移，导致体积电导率增大。
3.3 硅凝胶的击穿-热老化特性
图8为不同老化时间下硅凝胶交流击穿强度的Weibull分布图，其特征参数见表3。
从表3可以看出，硅凝胶的交流击穿强度随老化时间的延长而降低，这是因为在热老化过程中硅凝胶出现体积膨胀和热变形，单位体积内分子数减少，使电子的自由行程增加，更利于自由电子在材料中加速迁移，电子间更容易发生碰撞电离，根据雪崩击穿模型，此时载流子数迅速增加，导致样品更容易发生击穿现象。
4 结论
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本文对硅凝胶进行了高温试验与热老化试验，对不同温度和不同老化周期的样品进行介电性能、体积电导率和击穿强度测试，并分别从以上三个方面分析结果，得出以下结论：
（1）温度升高会加剧硅凝胶内部的分子热运动，阻碍粒子极化，但促进材料释放出更多的偶极子，使其复介电常数实部降低，低频下的介质损耗增加；同时温度升高会促进材料释放出更多的载流子，使载流子浓度升高，直流电导率随之升高；温度升高还会使电子的碰撞电离现象更加显著，降低样品的击穿强度。
（2）在长期的热应力作用下，硅凝胶出现热氧化、热降解和热裂解等反应，加剧了极化弛豫现象，使复介电常数实部增加；随着老化时间的增加，低频下主导介质损耗的直流损耗先减小后增大，并且硅凝胶交联密度先增大后减小，导致低频介质损耗先减小后增大；在热老化过程中，直流电导率受交联密度影响呈现出先减小后增大的趋势；老化周期延长，硅凝胶体积膨胀增加了电子的自由行程，破坏了分子结构，导致极化现象加剧，击穿强度降低。
（3）基于对硅凝胶高温特性和热老化特性的分析，老化过程中由于硅凝胶被氧化导致其绝缘性能降低，因此可以考虑在硅凝胶中加入抗氧化剂提高硅凝胶的耐热性能。
基金
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  • 国网江苏省电力有限公司电力科学研究院科技项目(5500-202240106A-1-1-ZN)
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2023年第56卷第12期
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doi: 10.16790/j.cnki.1009-9239.im.2023.12.001
  • 接收时间：2023-04-09
  • 首发时间：2025-11-24
  • 出版时间：2023-12-20
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  • 收稿日期：2023-04-09
  • 修回日期：2023-06-02
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国网江苏省电力有限公司电力科学研究院科技项目(5500-202240106A-1-1-ZN)
作者信息
    1西安交通大学 电气工程学院 电力设备电气绝缘国家重点实验室,陕西 西安 710049
    2南瑞集团有限公司,江苏 南京 211000

通讯作者:

张博雅（1990-），男（汉族），陕西西安人，副教授，主要从事高电压与绝缘技术教学与科研工作。
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2种不同金属材料的力学参数
科
Family		 属数
Number of
genus		 种数
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
species (%)
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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