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Article(id=1209928222897213940, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1209928218329616824, articleNumber=null, orderNo=null, doi=10.16790/j.cnki.1009-9239.im.2024.05.007, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1697040000000, receivedDateStr=2023-10-12, revisedDate=1701619200000, revisedDateStr=2023-12-04, acceptedDate=null, acceptedDateStr=null, onlineDate=1766398967718, onlineDateStr=2025-12-22, pubDate=1716134400000, pubDateStr=2024-05-20, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1766398967718, onlineIssueDateStr=2025-12-22, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1766398967718, creator=13701087609, updateTime=1766398967718, updator=13701087609, issue=Issue{id=1209928218329616824, tenantId=1146029695717560320, journalId=1149653034449285133, year='2024', volume='57', issue='5', pageStart='1', pageEnd='124', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1766398966629, creator=13701087609, updateTime=1766563901766, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1210620006501585415, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1209928218329616824, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1210620006501585416, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1209928218329616824, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=49, endPage=56, ext={EN=ArticleExt(id=1209928223148872190, articleId=1209928222897213940, tenantId=1146029695717560320, journalId=1149653034449285133, language=EN, title=Electric-thermal breakdown properties of core-shell structure BNNS@SiO2/epoxy composite dielectric, columnId=1209928219172671930, journalTitle=Insulating Materials, columnName=Special Issue on High-performance Transformer Insulation, runingTitle=null, highlight=null, articleAbstract=

In this paper, BNNS@SiO2/epoxy composite dielectrics with different filler content were prepared, the chemical characteristics and microscopic morphology of the composite dielectrics interface area were studied, and the trap characteristics and breakdown properties of the composite dielectrics were studied by thermal stimulation depolarization current method and breakdown test. The results show that BNNS@SiO2 has a core-shell structure and the thickness of the coated SiO2 is at the nanoscale. There is a clear chemical bonding effect on the surface of BNNS@SiO2, which can form a strong interface zone with the epoxy matrix, so as to improve its compatibility with the epoxy matrix. A small amount of BNNS@SiO2 can effectively improve the electric strength of the composite dielectric, and when the mass fraction of BNNS@SiO2 is 1%, the electric strength of the composite dielectric increases by 52.3%. When the content of BNNS@SiO2 nanoparticles is small, the deep traps in the epoxy composite dielectric increases. When content of BNNS@SiO2 nanoparticles is large, the deep traps decrease and the shallow traps increase. In addition, the thermal conductivity of the core-shell structure BNNS@SiO2/epoxy composite dielectric increases significantly, which is conducive to the heat dissipation of insulation under high electric field. Through the comprehensive effect of deep trap effect and thermal conductivity improvement, the breakdown performance of epoxy composite dielectric is improved significantly.

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本文制备不同填料含量的核壳结构BNNS@SiO2/环氧复合电介质，研究复合电介质界面区的化学特征与微观形貌，通过热刺激去极化电流法与击穿测试研究环氧复合电介质的陷阱特性与击穿性能。结果表明：BNNS@SiO2具有核壳结构，且包覆的SiO2厚度在纳米级别；BNNS@SiO2表面存在明显化学键合作用，与环氧基体可形成较强的界面区，提升其与环氧基体的相容性。少量BNNS@SiO2可有效提升复合电介质的电气强度，当BNNS@SiO2的质量分数为1%时，复合电介质的电气强度可提升52.3%。当BNNS@SiO2纳米粒子含量较少时，环氧复合电介质中的深陷阱增加，当纳米粒子含量较多时，深陷阱数量有所减少，浅陷阱数量增加。此外，核壳结构BNNS@SiO2/环氧复合电介质的热导率明显提高，有利于高电场下的绝缘散热。通过深陷阱效应与导热性能提升的综合作用，环氧复合电介质的击穿性能得到显著提升。

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徐永生（1977-），男（汉族），河北三河人，高级工程师，博士，主要从事高电压技术的研究；

王威望（1987-），男（汉族），陕西咸阳人，副教授，博士，主要从事绝缘介质理论与应用、高频磁件设计与绝缘可靠性的研究。

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徐永生（1977-），男（汉族），河北三河人，高级工程师，博士，主要从事高电压技术的研究；

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徐永生（1977-），男（汉族），河北三河人，高级工程师，博士，主要从事高电压技术的研究；

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王威望（1987-），男（汉族），陕西咸阳人，副教授，博士，主要从事绝缘介质理论与应用、高频磁件设计与绝缘可靠性的研究。

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王威望（1987-），男（汉族），陕西咸阳人，副教授，博士，主要从事绝缘介质理论与应用、高频磁件设计与绝缘可靠性的研究。

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填料质量分数/%BNNS/EPBNNS@SiO2/EP
α/(kV/mm)βα/(kV/mm)β
0242.25.63242.25.63
0.1308.54.87339.73.62
1326.85.39368.95.83
3298.54.87313.94.90
5272.23.62315.24.53
), ArticleFig(id=1217500253461332480, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209928222897213940, language=CN, label=表1, caption=

各试样Weibull分布尺度参数α和形状参数β

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填料质量分数/%BNNS/EPBNNS@SiO2/EP
α/(kV/mm)βα/(kV/mm)β
0242.25.63242.25.63
0.1308.54.87339.73.62
1326.85.39368.95.83
3298.54.87313.94.90
5272.23.62315.24.53
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核壳结构BNNS@SiO2/环氧复合电介质的电-热击穿特性
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徐永生 1 , 贺蕾 2 , 冯勇 2 , 王威望 2 , 罗兵 1 , 傅明利 1
绝缘材料 | 高性能变压器绝缘专题 2024,57(5): 49-56
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绝缘材料 | 高性能变压器绝缘专题 2024, 57(5): 49-56
核壳结构BNNS@SiO2/环氧复合电介质的电-热击穿特性
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徐永生1, 贺蕾2, 冯勇2, 王威望2, 罗兵1, 傅明利1
作者信息
  • 1南方电网科学研究院有限责任公司，广东 广州 510080
  • 2西安交通大学，陕西 西安 710049

    • 徐永生（1977-），男（汉族），河北三河人，高级工程师，博士，主要从事高电压技术的研究；

    王威望（1987-），男（汉族），陕西咸阳人，副教授，博士，主要从事绝缘介质理论与应用、高频磁件设计与绝缘可靠性的研究。

Electric-thermal breakdown properties of core-shell structure BNNS@SiO2/epoxy composite dielectric
Yongsheng XU1, Lei HE2, Yong FENG2, Weiwang WANG2, Bing LUO1, Mingli FU1
Affiliations
  • 1CSG Electric Power Research Institute, Guangzhou 510080, China
  • 2Xi′an Jiaotong University, Xi′an 710049, China
出版时间: 2024-05-20 doi: 10.16790/j.cnki.1009-9239.im.2024.05.007
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摘要
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本文制备不同填料含量的核壳结构BNNS@SiO2/环氧复合电介质，研究复合电介质界面区的化学特征与微观形貌，通过热刺激去极化电流法与击穿测试研究环氧复合电介质的陷阱特性与击穿性能。结果表明：BNNS@SiO2具有核壳结构，且包覆的SiO2厚度在纳米级别；BNNS@SiO2表面存在明显化学键合作用，与环氧基体可形成较强的界面区，提升其与环氧基体的相容性。少量BNNS@SiO2可有效提升复合电介质的电气强度，当BNNS@SiO2的质量分数为1%时，复合电介质的电气强度可提升52.3%。当BNNS@SiO2纳米粒子含量较少时，环氧复合电介质中的深陷阱增加，当纳米粒子含量较多时，深陷阱数量有所减少，浅陷阱数量增加。此外，核壳结构BNNS@SiO2/环氧复合电介质的热导率明显提高，有利于高电场下的绝缘散热。通过深陷阱效应与导热性能提升的综合作用，环氧复合电介质的击穿性能得到显著提升。

氮化硼纳米片  /  环氧复合电介质  /  核壳结构  /  击穿  /  导热  /  陷阱

In this paper, BNNS@SiO2/epoxy composite dielectrics with different filler content were prepared, the chemical characteristics and microscopic morphology of the composite dielectrics interface area were studied, and the trap characteristics and breakdown properties of the composite dielectrics were studied by thermal stimulation depolarization current method and breakdown test. The results show that BNNS@SiO2 has a core-shell structure and the thickness of the coated SiO2 is at the nanoscale. There is a clear chemical bonding effect on the surface of BNNS@SiO2, which can form a strong interface zone with the epoxy matrix, so as to improve its compatibility with the epoxy matrix. A small amount of BNNS@SiO2 can effectively improve the electric strength of the composite dielectric, and when the mass fraction of BNNS@SiO2 is 1%, the electric strength of the composite dielectric increases by 52.3%. When the content of BNNS@SiO2 nanoparticles is small, the deep traps in the epoxy composite dielectric increases. When content of BNNS@SiO2 nanoparticles is large, the deep traps decrease and the shallow traps increase. In addition, the thermal conductivity of the core-shell structure BNNS@SiO2/epoxy composite dielectric increases significantly, which is conducive to the heat dissipation of insulation under high electric field. Through the comprehensive effect of deep trap effect and thermal conductivity improvement, the breakdown performance of epoxy composite dielectric is improved significantly.

BNNS  /  epoxy composite dielectric  /  core-shell structure  /  breakdown strength  /  heat conduction  /  traps
徐永生, 贺蕾, 冯勇, 王威望, 罗兵, 傅明利. 核壳结构BNNS@SiO2/环氧复合电介质的电-热击穿特性. 绝缘材料, 2024 , 57 (5) : 49 -56 . DOI: 10.16790/j.cnki.1009-9239.im.2024.05.007
Yongsheng XU, Lei HE, Yong FENG, Weiwang WANG, Bing LUO, Mingli FU. Electric-thermal breakdown properties of core-shell structure BNNS@SiO2/epoxy composite dielectric[J]. Insulating Materials, 2024 , 57 (5) : 49 -56 . DOI: 10.16790/j.cnki.1009-9239.im.2024.05.007
正文
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0 引言
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随着电力设备不断朝着高电压、大容量和小型化方向发展，对电力设备环氧绝缘的性能与可靠性要求越来越高[1-3]。在高功率密度电力设备，如高频干式变压器的设计与应用中，环氧绝缘作为其中的主绝缘材料，需要承受高场强与高温的复杂工况，对其绝缘性能与散热性能提出了挑战[4-6]。
纳米填料可有效提升聚合物的绝缘性能，受到了人们的广泛关注与研究。在纳米尺度上，材料的物理化学特性会发生变化，出现小尺寸效应、表面/界面效应与量子效应，这些效应在粒子与聚合物基体的界面区表现尤为突出，是决定纳米复合电介质性能的关键。氮化硼纳米片（BNNS）具有优异的绝缘性能、导热性能和化学稳定性，将其与聚合物基体进行复合制备纳米复合电介质，可提升聚合物基体的绝缘与导热性能[7-9]。毕世杰等[10]研究表明，在环氧树脂中加入取向化BNNS后，所得环氧复合材料的热导率得到大幅提升，可达到纯环氧树脂的4倍；夏彦卫等[11]研究了功能化的BNNS对环氧基体电-热性能的影响，发现当BNNS质量分数为20%时，环氧复合材料的热导率达到0.51 W/(m·K)。
大量研究结果表明，提高纳米颗粒在基体中的分散性，使其混合均匀、不发生团聚，有利于改善纳米复合材料的电气性能[12-13]，而对纳米粒子进行化学修饰或功能化处理可有效改善其在基体中的分散性。此外，纳米粒子与聚合物基体形成的界面对于复合材料的绝缘性能具有重要影响。因此通过表面改性的纳米颗粒调控界面性能，可进一步提高环氧纳米复合材料的绝缘性能。M KIM等[14]研究了表面改性对环氧/纳米SiO2复合材料击穿性能的影响，发现表面改性可提高复合材料的电气强度。任俊文等[15]提出采用表面包覆介孔SiO2并接枝硅烷偶联剂功能分子的方法优化氮化硼纳米管（BNNTs）的表面特性，并将其与环氧树脂进行复合。结果表明，BNNTs的分散特性得到显著提升，所制备的环氧复合电介质热导率提升，同时具有较低的介质损耗。
目前，关于纳米填料表面改性的研究多集中于表面接枝改性[16-17]。但接枝改性方法复杂，且容易引入杂质缺陷，对复合材料的性能产生影响。为了实现更加稳定便捷的表面改性，同时制备得到高性能聚合物纳米复合材料，需要进一步探索填料的表面处理以及调控界面区的方法。研究表明，对纳米粒子进行无机材料包覆形成核壳结构，可有效改善纳米粒子表面能，提升纳米粒子在基体中的分散性，同时有助于形成较强的界面效应，进而提升复合材料的绝缘性能[18]。
本文首先制备具有核壳结构的BNNS@SiO2纳米片，然后制备得到不同填料含量的核壳结构BNNS@SiO2/环氧复合电介质。对核壳结构BNNS@SiO2纳米片进行表征，并对其在环氧基体中的分散性与表面键合作用进行分析，研究BNNS@SiO2/环氧复合电介质的击穿性能与导热性能。通过陷阱特性分析，揭示BNNS@SiO2纳米片对环氧树脂电气性能的影响机制。
1 实验
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1.1 主要原材料
双酚A型环氧树脂（E51），南通星辰合成材料有限公司；固化剂甲基四氢苯酐（MTHPA），润翔化工有限公司；促进剂2,4,6-三（二甲氨基甲基）苯酚（DMP-30）、正硅酸乙酯（TEOS），阿拉丁生化科技股份有限公司；半永久性脱模剂（JD-909A），佳丹润滑油有限公司；氮化硼纳米片（厚度小于100 nm）、硅烷偶联剂（KH560，分析纯），德科岛金有限公司；30%过氧化氢溶液（分析纯）、氨水（分析纯）、无水乙醇（分析纯）、去离子水（分析纯）。
1.2 试样制备
1.2.1 BNNS@SiO2纳米片的制备及改性
BNNS@SiO2纳米片的制备及改性过程如图1和图2所示，主要分为两步：①通过正硅酸乙酯（TEOS）的水解反应产生SiO2附着在BNNS表面得到BNNS@SiO2纳米片；②使用硅烷偶联剂KH560对BNNS@SiO2纳米片进行表面改性处理，提高纳米片在环氧基体中的分散效果。
1.2.2 BNNS@SiO2/EP复合电介质的制备
BNNS@SiO2/EP复合电介质的制备过程如图3所示。将环氧树脂基体、固化剂和促进剂按照质量比为100∶78.87∶0.6进行混合，然后分别加入质量分数为0.1%、1%、3%和5%的改性BNNS@SiO2纳米片，经过分散、脱气、固化等步骤制备得到厚度为0.2 mm的环氧复合电介质试样。根据填料的质量分数x将环氧复合电介质编号为xBNNS@SiO2/EP。采用BNNS作为填料通过相同的工艺制备BNNS/EP进行对比分析。
1.3 理化性能表征
采用Talos L120C G2型120 kV透射电子显微镜（TEM）对BNNS@SiO2纳米片进行形态观察。采用EVO10型钨丝灯扫描电子显微镜（SEM）对试样进行微观形貌观察。采用Bruker VERTEX70型显微红外光谱仪对纳米粒子的改性情况与环氧复合电介质的化学结构进行表征，采用透射模式和衰减全反射模式测试，波数为400～4 000 cm-1，扫描次数为32次。
1.4 热学与介电性能表征
采用LFA447型闪光导热分析仪测试环氧复合电介质的热扩散系数，试样尺寸为10 mm×10 mm×1 mm，测试温度为25、50、75、100℃，在每个温度点进行3次测试，比热采用系统默认值。由于试样尺寸随温度变化不大，可认为密度近似不变，则可根据式（1）计算得到热导率。
κ=αpCpρ
式（1）中：κ为热导率，W/(m·K)；αp为热扩散系数，m2/s；Cp为比热容，J/(kg·K)；ρ为密度，kg/m3。
采用极化电压范围为-1～1 kV、电流测量范围为1 fA～20 mA、温度范围为-160～400℃（±0.01℃）、升降温速率为0.5～30℃/min可调的TSDC测试系统测试环氧复合电介质的热刺激电流特性。从室温开始快速升温至极化温度（110℃），在试样上施加250 V的直流电压并维持20 min；极化过程结束后，以30℃/min的速率降温至去极化温度（-100℃）并维持10 min；去极化结束后，以5℃/min的速率线性升温，记录热刺激去极化电流的相关数据，直至升温到160℃结束实验。用“初始上升法”，根据式（2）～（3）计算陷阱参数。
IT=p0τ0exp -ETkBT-1βτ0∫T0T'exp -ETkBTdT
Nt=1βesd∫T0T'ITdT
式（2）～（3）中：I(T)为热刺激去极化电流；Nt为陷阱密度；τ0为松弛时间；β为升温速率；p0为极化强度；ET为活化能，即陷阱能级；T0、T′分别为去极化电流松弛峰的起始、终止温度；kB为玻尔兹曼常数，其值为1.38×10-23 J/K；d为试样厚度；s为试样表面积；e为电子电荷量。
1.5 直流击穿测试
击穿试验平台如图4所示，使用HJC-100kV型计算机控制电压击穿测试系统，采用直径为25 mm的铜质球-球电极作为测试电极，将试样浸入恒温的绝缘油中进行击穿测试。测试温度为室温，升压速率为1 kV/s，试样厚度约为0.2 mm，每组试样重复测试10次以上，以保证统计结果的有效性。
2 实验结果分析
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2.1 纳米片的表征结果
2.1.1 纳米片的微观形貌
图5为BNNS、BNNS@SiO2纳米片的TEM图。从图5(a)中可以看到层状堆叠的氮化硼纳米片。从图5(b)可以看到，BNNS@SiO2纳米片周围明显包覆了一层深色的物质，且包覆的壳层厚度较为均匀，包覆效果较好。
仅通过TEM观察无法判断上述深色物质是否为目标物质SiO2，故对BNNS@SiO2纳米片进行了SEM测试和能谱（EDS）分析，结果如图6所示。从图6可以看出，除BNNS中含有的B元素与N元素以外，BNNS@SiO2中还出现了两种新元素，分别是O元素和Si元素。同时从6(c)～(f)中Si、B、N、O元素的平面扫描结果可以观察到，Si、O元素分布均匀，即说明SiO2包覆在BNNS表面，且包覆效果较好。
2.1.2 纳米片的表面化学基团
对BNNS、BNNS@SiO2纳米片分别进行了FTIR分析，结果如图7所示。从图7可以看出，BNNS和BNNS@SiO2纳米片的红外光谱中均存在两个明显的特征峰，分别为1 371 cm-1附近B-N键的面内伸缩振动峰和818 cm-1处B-N-B键的面外弯曲振动峰，这两个峰是B原子和N原子相互作用的体现。而在BNNS@SiO2纳米片的红外光谱上出现了3处新的特征峰，分别为位于1 097 cm-1附近Si-O-Si的反对称伸缩振动峰、818 cm-1附近Si-O键的对称伸缩振动峰及468 cm-1处Si-O的弯曲振动峰。另外943 cm-1处的吸收峰为B取代Si后骨架局部不对称所致的特征吸收峰。综上可知，通过TEOS水解反应成功地将SiO2覆盖在BNNS表面，制备得到了BNNS@SiO2纳米片。
2.2 环氧复合电介质的表征结果
2.2.1 形貌分析
图8为纯环氧和5%BNNS@SiO2/EP复合电介质的断面SEM图。从图8(a)可以看出，纯环氧的断面呈现出一种棱壑感，并且棱壑之间的区域十分平整，表明该材料一致性很高。从图8(b)可以看出，由于经过硅烷偶联剂KH560的表面改性处理，BNNS@SiO2纳米片能够很好地融入环氧基体，环氧复合电介质的断面更加粗糙，纳米粒子在其中分散较好，团聚现象较少。
2.2.2 红外测试结果
图9为纯环氧和环氧复合电介质的红外光谱图。从图9可以看出，BNNS/EP、BNNS@SiO2/EP复合电介质的红外光谱中均出现了代表BNNS的两个特征峰，即位于1 371 cm-1附近B-N键的面内伸缩振动峰和位于818 cm-1附近B-N-B键的面外弯曲振动峰。同时，在860 cm-1处出现了KH560和环氧醚键的伸缩振动峰，说明KH560成功接枝到BNNS与BNNS@SiO2表面，并与环氧基体进行了结合。从图9(b)可以看出，BNNS@SiO2/EP复合电介质的红外光谱在1 110 cm-1处出现了Si-O键的伸缩振动峰，910 cm-1处出现了B-O键的伸缩振动峰。
2.2.3 导热性能
在不同温度下对不同填料含量的BNNS/EP、BNNS@SiO2/EP复合电介质进行热导率测试，结果如图10所示。从图10可以看出，BNNS@SiO2/EP复合电介质的热导率随着温度的升高逐渐增大。对比纯环氧树脂，掺杂了BNNS或BNNS@SiO2纳米片的环氧复合电介质导热性能均得到提升。当温度恒定时，环氧复合电介质的热导率随着纳米填料掺杂量的升高而增大。在25℃下，5%BNNS@ SiO2/EP复合电介质的热导率从纯环氧树脂的0.184 W/(m·K)提高至0.327 W/(m·K)，提升了77.7%。在100℃下，5%BNNS@SiO2/EP纳米复合电介质的热导率从纯环氧树脂的0.218 W/(m·K)提高至0.388 W/(m·K)，提升了78.0%。同时对比发现，在相同填料含量下BNNS@SiO2/EP复合电介质的热导率比BNNS/EP复合电介质高。
2.2.4 热刺激去极化电流与陷阱特性
本研究分别对纯环氧树脂和BNNS@SiO2/EP复合电介质进行热刺激去极化电流测试，通过对其去极化电流进行拟合处理，计算得到试样的陷阱能级与陷阱密度等参数。
结合热刺激去极化电流（TSDC）曲线的形状和环氧中主要的极化方式，对TSDC原始曲线进行分峰拟合，结果如图11所示。一般认为环氧介质中的TSDC电流主要由小分子链的转向极化、浅陷阱与深陷阱电荷的入陷与脱陷、大分子链的转向极化所导致。
根据不同的温度区间，划分不同的松弛区域。其中-100～0℃对应γ松弛，0～60℃对应β松弛，60℃以上对应α松弛。不同的松弛区域代表不同的陷阱能级，峰值的高低则代表陷阱密度的大小。从图11可以看出，添加BNNS@SiO2纳米片后环氧复合电介质各峰的位置与峰值均发生了较大变化。BNNS@SiO2纳米片会对γ、β和α峰的位置与峰值产生影响。在填料含量较低时，主要是α峰、β峰的峰值增大，γ峰略微增大。而当填料含量较高时，γ峰呈现增大趋势，而α峰、β峰的峰值有所减小。随着填料含量的增加，γ峰的位置向高温区移动，当BNNS@SiO2质量分数为3%和5%时，热刺激电流（TSC拟合曲线）峰变得更宽。
α峰代表深陷阱，即环氧复合电介质中的深陷阱水平数量随BNNS@SiO2含量的增加先增大后减小，并且在BNNS@SiO2质量分数为0.1%时显著增大，随后逐渐降低趋于平稳。但值得关注的是，在BNNS@SiO2质量分数为5%时，α峰出现了另一个极值，该现象可以解释为随着引入的SiO2越来越多，也引入了更多的深陷阱，导致空间电荷峰幅值增大。
2.2.5 击穿性能
对纯环氧试样、BNNS/EP、BNNS@SiO2/EP复合电介质进行直流击穿试验，取10个有效数据，采用双参数Weibull分布进行数据统计，结果如图12和表1所示。
从图12和表1可以看出，纯环氧的电气强度为242.2 kV/mm，添加BNNS和BNNS@SiO2纳米填料均能够有效提升其电气强度，当填料质量分数为1%时，1%BNNS/EP和1%BNNS@SiO2/EP的电气强度分别为326.8 kV/mm和368.9 kV/mm，比纯环氧分别提高了34.9%和52.3%。对同一种纳米填料而言，随着添加量的增加，环氧复合电介质的电气强度呈现先升高后降低的趋势。一方面，环氧树脂中积聚的正、负极性空间电荷较多，介质内部电场畸变严重，导致电气强度较低。掺杂纳米填料后增加了介质中的深陷阱，临近电极的深陷阱捕获电极注入的载流子形成同极性空间电荷，削弱了电极附近电场，抑制了后续的电极电荷注入和空间电荷积累，从而减少了试样中的空间电荷总量和介质内部的场强畸变，使环氧复合电介质的直流电气强度升高。另一方面，掺杂纳米填料将在介质中引入界面区。当纳米填料含量较低时，填料之间相距较远，相互作用弱，界面区分离，载流子在界面区中较难获得足够的能量越过键合区势垒参与电导，导致环氧复合电介质的电导率降低，电气强度升高。当填料含量较高时，填料间距离变小，作用力增强，界面区可能相互重叠而使其厚度大于载流子的平均自由行程，载流子在界面区内可以通过多次碰撞获得足够的能量越过势垒参与导电，导致环氧复合电介质的电气强度降低。
对于BNNS@SiO2/EP复合电介质的电气强度，当BNNS@SiO2的质量分数增大到5%时，引入了更多的SiO2导致深陷阱密度反而增大，使得复合电介质材料的电气强度有些许回升，但由于浅陷阱的存在，两者只是勉强抵消，并没有出现明显的上升趋势。
2.3 掺杂BNNS@SiO2对环氧复合电介质电热击穿特性的影响分析
界面区特性是影响纳米复合电介质性能的关键。研究者普遍认为界面区是一个过渡区，是一个由键合区、过渡区和正常区组成的交互区结构模型，其中存在复杂的陷阱分布与双电层结构。陷阱是指能够俘获电子或空穴的晶体缺陷或化学中心。掺杂纳米填料后，复合电介质的深陷阱能级和密度均会发生改变，从而改变材料内部电荷输运过程，进而影响材料的击穿性能[17]。
当BNNS@SiO2纳米片的含量较低时，一方面，改性后BNNS表面引入了极性基团，增加了界面区的深陷阱；另一方面，BNNS@SiO2纳米片的取向自由度大、分布范围较大及粒子间的相互作用较弱，导致环氧分子链段运动改变。BNNS的片状结构会导致径向链段分布较多，片层之间的距离限制了分子链段的转动，从而减小了片层间有效的平均自由体积长度，有利于提升复合材料的电气强度。另外，改性后BNNS@SiO2与环氧基体分子间的界面区范围变大，过渡区变宽，有利于界面区中电荷的扩散，使界面势垒区变宽，增大载流子越过势垒的能量。在界面区深陷阱增加、自由体积减小与势垒区变宽的协同作用下，BNNS@SiO2/EP的击穿性能得到了改善。
当BNNS@SiO2纳米粒子含量较高时，一方面，粒子之间的间距减小，相互作用增强，导致粒子团聚，分散性降低，从而使得环氧复合电介质内部出现缺陷与杂质；另一方面，BNNS在基体中的运动空间受限，取向运动受到影响，导致BNNS片层之间难以存在分子链段的自由运动空间，大分子链段主要沿着BNNS的横向面内运动，导致载流子运动的平均自由体积长度增大。结合高填料含量时引入的杂质与缺陷效应，环氧复合电介质的电气强度降低。
上述分析主要是针对电击穿而言。而实际高功率密度电力设备工作时其温升较高，材料本身的发热对击穿的影响也很重要。本研究制备的核壳结构BNNS@SiO2纳米片进一步提升了环氧复合材料的热导率，有利于材料在高电场下工作时的散热。考虑热击穿过程，掺杂核壳结构BNNS@SiO2纳米片有利于减少热击穿过程的热量积聚、改善材料的温度分布及提高参数稳定性，从而提升环氧复合电介质的电气强度。
目前有3种较为常见的复合材料导热性能改善机理，即导热网络理论、导热逾渗理论和热弹性系数理论。导热网络理论认为，当导热填料用量较少时，填料彼此分隔，难以形成连续的导热网络，对复合材料热导率的提升有限。本研究中环氧复合电介质的BNNS@SiO2含量不高，当BNNS@SiO2纳米片质量分数为5%时，5%BNNS@SiO2/EP的热导率为0.34 W/(m·K)，对比纯环氧树脂和5%BNNS/EP复合电介质有所提升，但仍没有显著增加。这是由于复合电介质内部可能形成了局部的导热网络，但未形成大面积的导热网络。因此，本研究中复合电介质热导率的提升主要归因于BNNS的表面处理以及界面效应。当BNNS@SiO2纳米片含量较低时，通过在BNNS表面包覆SiO2外壳，改善了其与环氧基体间的界面结合能，并降低了填料与环氧基体界面处的热阻，从而提升了环氧复合电介质的热导率。当BNNS@SiO2纳米片含量较高时，一方面界面热阻进一步下降，另一方面形成局部的导热网络延长了由无机纳米片构成的高导热路径长度，显著提升了环氧复合电介质的热导率。
综上，核壳结构BNNS@SiO2纳米片的掺杂可以增强环氧复合电介质的陷阱效应，从而影响电荷输运中载流子迁移率、电荷积聚能量等微观参数。此外，低含量BNNS@SiO2纳米片通过调节界面结合能和热阻提升复合电介质的热导率；高含量BNNS@SiO2纳米片通过形成局部导热网络进一步提升复合电介质的热导率，减少热量积聚以削弱电-热耦合应力对材料的损伤，延缓绝缘劣化过程，延长绝缘失效时间，有利于提升环氧树脂的绝缘性能和导热性能。
3 结论
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本文制备了核壳结构BNNS@SiO2/环氧复合电介质并研究了其微观理化、击穿、导热与陷阱特性，主要得到以下结论：
（1）BNNS@SiO2纳米片表面包覆情况良好，其在环氧基体中的分散效果良好。添加少量BNNS@SiO2可有效提升复合材料的直流电气强度，当BNNS@SiO2的质量分数为1%时，环氧复合电介质的电气强度最高，达到368.9 kV/mm，相比纯环氧树脂提升了52.3%。
（2）陷阱特性测试表明，添加少量BNNS @SiO2时，环氧复合电介质中的深陷阱增加，而BNNS@SiO2添加量较多时，陷阱能级有所降低，引入较多的浅陷阱。当BNNS@SiO2质量分数为0.1%时，复合电介质内深陷阱数量显著增加，随后逐渐降低并趋于平稳。通过在BNNS表面包覆SiO2外壳，有效地改善了复合电介质中的陷阱分布。当BNNS@SiO2含量较低时，界面区存在较多深陷阱，可以抑制载流子迁移，从而降低载流子输运的密度和能量，减少高电场下的碰撞电离。
（3）核壳结构BNNS@SiO2/环氧复合电介质的热导率明显提高，有利于高电场下的绝缘散热。纳米BNNS@SiO2掺杂通过改善界面结合能、构筑导热通路及网络，提高热传导效率，通过填充环氧基体间隙而减小自由空间，综合提升了环氧复合电介质的导热性能和绝缘性能。
基金
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  • 国家自然科学基金面上资助项目(52177025)
  • 南方电网科学研究院有限责任公司项目(1500002022030103GY00069)
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2024年第57卷第5期
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doi: 10.16790/j.cnki.1009-9239.im.2024.05.007
  • 接收时间：2023-10-12
  • 首发时间：2025-12-22
  • 出版时间：2024-05-20
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  • 收稿日期：2023-10-12
  • 修回日期：2023-12-04
基金
国家自然科学基金面上资助项目(52177025)
南方电网科学研究院有限责任公司项目(1500002022030103GY00069)
作者信息
    1南方电网科学研究院有限责任公司，广东 广州 510080
    2西安交通大学，陕西 西安 710049
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鹅膏菌科Amanitaceae 2 11 5.26 鹅膏菌属 Amanita 10 4.78
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