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Article(id=1209928222033178901, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1209928218329616824, articleNumber=null, orderNo=null, doi=10.16790/j.cnki.1009-9239.im.2024.05.006, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1687104000000, receivedDateStr=2023-06-19, revisedDate=1689696000000, revisedDateStr=2023-07-19, acceptedDate=null, acceptedDateStr=null, onlineDate=1766398967512, onlineDateStr=2025-12-22, pubDate=1716134400000, pubDateStr=2024-05-20, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1766398967512, onlineIssueDateStr=2025-12-22, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1766398967512, creator=13701087609, updateTime=1766398967512, 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=42, endPage=48, ext={EN=ArticleExt(id=1209928222725239094, articleId=1209928222033178901, tenantId=1146029695717560320, journalId=1149653034449285133, language=EN, title=Study on performance enhancement of epoxy resin for saturated reactor, columnId=1209928219172671930, journalTitle=Insulating Materials, columnName=Special Issue on High-performance Transformer Insulation, runingTitle=null, highlight=null, articleAbstract=

The epoxy resin for casting in saturated reactors is prone to ageing and cracking when subjected to electrical stress and mechanical vibration, it is necessary to improve its mechanical and thermal properties on the basis of maintaining its excellent insulating properties and corrosion resistance. In this paper, taking the functional optimization design as principle, a silicon dioxide dielectric layer was formed on the surface of silicon carbide whiskers (SiCw) by heat treatment to obtain SiCw@SiO2. Then a SiCw@SiO2/EP composite dielectric was prepared by doping modification, and its dielectric properties, mechanical properties, and thermal properties were tested. The results show that the SiCw@SiO2/EP composite dielectric has both high dielectric constant and low dielectric loss, and its toughness is also improved. Due to the continuous thermal conductivity network formed by the contact of SiCw, the thermal conductivity of the SiCw@SiO2/EP composite dielectric increases by 117% than that of pure epoxy resin.

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针对饱和电抗器浇注用环氧树脂在受到电应力及机械振动时易出现老化开裂的问题，需要在保持其优良绝缘、抗腐蚀性能的基础上改善其力学性能及热学性能。本文以功能优化设计为原则，先通过热处理在碳化硅晶须（SiCw）表面形成二氧化硅介电层得到SiCw@SiO2，然后利用掺杂改性的方法制备SiCw@SiO2/EP复合电介质，并对其介电性能、力学性能以及导热性能进行测试。结果表明：SiCw@SiO2/EP复合电介质兼具高介电常数及低介质损耗，韧性也得到改善，且由于SiCw相互接触形成了连续导热网络，SiCw@SiO2/EP复合电介质的导热系数相比纯环氧树脂提高了117%。

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任俊文（1987-），男（汉族），四川南充人，副研究员，研究方向为高电压与绝缘技术。
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廖文龙(1989-)，男（汉族），四川内江人，工程师，研究方向为高电压与绝缘技术。

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廖文龙(1989-)，男（汉族），四川内江人，工程师，研究方向为高电压与绝缘技术。

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廖文龙(1989-)，男（汉族），四川内江人，工程师，研究方向为高电压与绝缘技术。

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tableContent=null), ArticleFig(id=1217500259320779197, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209928222033178901, language=EN, label=Fig.15, caption=DMA loss factor of EP and SiCw@SiO2/EP composite dielectrics, figureFileSmall=lWgaNIKrmSKiDPscG8HJGA==, figureFileBig=tevKB5BsS7SpJiL3Xd1cDw==, tableContent=null), ArticleFig(id=1217500259454996931, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209928222033178901, language=CN, label=图15, caption=EP及SiCw@SiO2/EP复合电介质的DMA损耗因子, figureFileSmall=lWgaNIKrmSKiDPscG8HJGA==, figureFileBig=tevKB5BsS7SpJiL3Xd1cDw==, tableContent=null), ArticleFig(id=1217500260742648259, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209928222033178901, language=EN, label=Fig.16, caption=Storage modulus of SiCw@SiO2/EP composite dielectrics, figureFileSmall=JmzEVEq718N1Rf00kJyNog==, figureFileBig=u0TlI3a5uKkp3Q2mC+/i5w==, tableContent=null), ArticleFig(id=1217500260822340039, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209928222033178901, language=CN, label=图16, caption=SiCw@SiO2/EP复合电介质的储能模量, figureFileSmall=JmzEVEq718N1Rf00kJyNog==, figureFileBig=u0TlI3a5uKkp3Q2mC+/i5w==, tableContent=null), ArticleFig(id=1217500260931391947, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209928222033178901, language=EN, label=Tab.1, caption=TGA relevant data of composite dielectric, figureFileSmall=null, figureFileBig=null, tableContent=
材料类型600℃残留率/%Td/℃Tmax/℃
EP2.2368.26412.18
5%SiCw@SiO2/EP6.8369.44411.77
10%SiCw@SiO2/EP11.4372.81412.73
15%SiCw@SiO2/EP19.7376.19412.02
20%SiCw@SiO2/EP19.6376.85410.43
), ArticleFig(id=1217500261065609681, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209928222033178901, language=CN, label=表1, caption=

复合电介质热失重的相关数据

, figureFileSmall=null, figureFileBig=null, tableContent=
材料类型600℃残留率/%Td/℃Tmax/℃
EP2.2368.26412.18
5%SiCw@SiO2/EP6.8369.44411.77
10%SiCw@SiO2/EP11.4372.81412.73
15%SiCw@SiO2/EP19.7376.19412.02
20%SiCw@SiO2/EP19.6376.85410.43
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饱和电抗器用环氧树脂性能提升研究
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廖文龙 1 , 杨玥坪 1 , 魏华超 2 , 闫志江 3 , 张榆 1 , 任俊文 2
绝缘材料 | 高性能变压器绝缘专题 2024,57(5): 42-48
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绝缘材料 | 高性能变压器绝缘专题 2024, 57(5): 42-48
饱和电抗器用环氧树脂性能提升研究
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廖文龙1, 杨玥坪1, 魏华超2, 闫志江3, 张榆1, 任俊文2
作者信息
  • 1国网四川省电力公司电力科学研究院，四川 成都 610000
  • 2四川大学 电气工程学院， 四川 成都 610065
  • 3西安交通大学 电气工程学院，陕西 西安 710049

    • 廖文龙(1989-)，男（汉族），四川内江人，工程师，研究方向为高电压与绝缘技术。

通讯作者:

任俊文（1987-），男（汉族），四川南充人，副研究员，研究方向为高电压与绝缘技术。
Study on performance enhancement of epoxy resin for saturated reactor
Wenlong LIAO1, Yueping YANG1, Huachao WEI2, Zhijiang YAN3, Yu ZHANG1, Junwen REN2
Affiliations
  • 1State Grid Sichuan Electric Power Research Institute, Chengdu 610000, China
  • 2College of Electrical Engineering, Sichuan University, Chengdu 610065, China
  • 3College of Electrical Engineering, Xi′an Jiaotong University, Xi′an 710049, China
出版时间: 2024-05-20 doi: 10.16790/j.cnki.1009-9239.im.2024.05.006
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摘要
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针对饱和电抗器浇注用环氧树脂在受到电应力及机械振动时易出现老化开裂的问题，需要在保持其优良绝缘、抗腐蚀性能的基础上改善其力学性能及热学性能。本文以功能优化设计为原则，先通过热处理在碳化硅晶须（SiCw）表面形成二氧化硅介电层得到SiCw@SiO2，然后利用掺杂改性的方法制备SiCw@SiO2/EP复合电介质，并对其介电性能、力学性能以及导热性能进行测试。结果表明：SiCw@SiO2/EP复合电介质兼具高介电常数及低介质损耗，韧性也得到改善，且由于SiCw相互接触形成了连续导热网络，SiCw@SiO2/EP复合电介质的导热系数相比纯环氧树脂提高了117%。

环氧树脂  /  碳化硅晶须  /  韧性  /  热导率  /  介电性能

The epoxy resin for casting in saturated reactors is prone to ageing and cracking when subjected to electrical stress and mechanical vibration, it is necessary to improve its mechanical and thermal properties on the basis of maintaining its excellent insulating properties and corrosion resistance. In this paper, taking the functional optimization design as principle, a silicon dioxide dielectric layer was formed on the surface of silicon carbide whiskers (SiCw) by heat treatment to obtain SiCw@SiO2. Then a SiCw@SiO2/EP composite dielectric was prepared by doping modification, and its dielectric properties, mechanical properties, and thermal properties were tested. The results show that the SiCw@SiO2/EP composite dielectric has both high dielectric constant and low dielectric loss, and its toughness is also improved. Due to the continuous thermal conductivity network formed by the contact of SiCw, the thermal conductivity of the SiCw@SiO2/EP composite dielectric increases by 117% than that of pure epoxy resin.

epoxy resin  /  silicon carbide whiskers  /  toughness  /  thermal conductivity  /  dielectric properties
廖文龙, 杨玥坪, 魏华超, 闫志江, 张榆, 任俊文. 饱和电抗器用环氧树脂性能提升研究. 绝缘材料, 2024 , 57 (5) : 42 -48 . DOI: 10.16790/j.cnki.1009-9239.im.2024.05.006
Wenlong LIAO, Yueping YANG, Huachao WEI, Zhijiang YAN, Yu ZHANG, Junwen REN. Study on performance enhancement of epoxy resin for saturated reactor[J]. Insulating Materials, 2024 , 57 (5) : 42 -48 . DOI: 10.16790/j.cnki.1009-9239.im.2024.05.006
正文
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0 引言
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近年来，随着我国经济的持续稳定增长以及对电力、能源等资源需求的与日俱增，高压直流输电（HVDC）技术得到了多层次的发展和应用[1-2]。与交流输电系统相比，直流输电系统对绝缘介质表现出更高的标准与要求。HVDC系统中换流阀为核心装备，而确保其内部晶闸管正常的导通与关断是饱和电抗器的主要功能[3]。环氧树脂（EP）作为饱和电抗器的主要封装材料，起着机械支撑和绝缘的重要作用[4]。文献[5]研究表明，当换流阀处于高负载或过载工作时，饱和电抗器中的硅钢片会在短时间内产生大量热量。而EP的导热系数仅为0.204 W/(m·K)，热量会短时间在设备内部堆积，严重影响着电气设备的使用寿命。此外，EP由于本身韧性低、脆性大，在导体电应力较大的结构处热膨胀及振动作用明显。文献[6]研究表明，EP在热应力及机械应力作用下老化易形成裂纹，造成电荷积聚现象。而积聚的电荷在超/特高直流电压下不易消散，导致固体绝缘表面电场严重畸变，表现为局部绝缘失效，对整个直流输电系统的平稳运行造成威胁[7]。因此，未来的HVDC装备对饱和电抗器中封装绝缘材料的韧性及热管理能力提出了更高的要求。
为了满足小型化、高负载电气装备的使用特性需求，需要在确保EP优异电绝缘性、耐腐蚀性的基础上，对其力学性能及热学性能进行改善。而为了获得高性能环氧复合电介质，目前的研究主要集中在复合材料的本征改性和掺杂改性 [8]。前者通常由于工艺复杂、生产条件要求苛刻及成本高昂等问题，其推广使用受到限制，且EP本身具有极性，其本征介电常数相较于非极性电介质（聚四氟乙烯、聚苯乙烯等）高，非极性化处理难度较大[9]。在掺杂改性的研究中，通过在EP基体中添加不同种类、含量、尺度的无机填料可以提高EP的电学、力学和热学性能，且掺杂改性工艺简单、成本较低，无需改变树脂基体原有的物理或化学结构，因此被广泛应用于提升环氧复合材料的性能。目前国内外普遍采用在树脂基体中添加功能填料的方法来对绝缘介质进行性能提升。
碳化硅（SiC）作为一种理化性质较为理想的半导体材料，具有机械强度高、热传导性好、耐化学腐蚀性强等优点[10]。此外，其较高的介电常数有助于电场在绝缘封装中均匀分布，从而有效避免畸形电场的出现。文献[11]将SiC纳米颗粒进行高温热处理，在其表面形成了厚度可控的二氧化硅（SiO2）层，有效调控了电子传导现象，改善了复合电介质的绝缘水平。SiC晶须（SiCw）作为一维SiC纳米材料，既具有SiC优良的热学性能、介电性能，又兼具一维纳米材料优异的抗拉强度、拉伸模量等力学性能，作为复合材料的增强增韧填料具有极大的应用潜力。文献[12]将SiCw作为功能填料采用光固化快速成型技术制备了树脂基复合材料，测试结果表明加入SiCw可大幅提高复合材料的力学性能，对固化工艺几乎无影响。文献[13]利用磁场控制SiCw在EP中定向排列，增强了复合材料的热学性能。
然而，上述研究为了使聚合物复合材料具有优异的力学性能，在聚合物基体中掺杂了大量的SiCw填料，这虽然可以显著改善聚合物基体的韧性，但SiCw在基体中含量过高，导致基体材料的绝缘性能显著下降，使其在高压电器中的应用受到限制，而由文献[11]可知，SiO2作为优良的绝缘体，可以作为介电层有效抑制导电颗粒间的泄漏电流。
基于此，本研究以EP为基体，高温氧化处理后的碳化硅晶须为无机填料，制得不同填料含量的SiCw@SiO2/EP复合电介质，研究不同功能填料含量下复合电介质的微观形貌、电学性能、力学性能以及热学性能，以实现饱和电抗器用EP性能的有效提升。
1 实验
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1.1 实验原料
E-51环氧树脂（环氧当量为185～200 g/eq）、甲基六氢邻苯二甲酸酐（MHHPA）固化剂、2,4,6-三（二甲氨基甲基）-苯酚促进剂，南通星辰合成材料有限公司；碳化硅晶须，平均长度为40 μm，肯朴（厦门）新材料有限公司；丙酮，成都科隆化工有限公司。
1.2 试样制备
1.2.1 SiCw@SiO2的制备
碳化硅晶须的烧结流程如图1所示。将碳化硅晶须（SiCw）置于坩埚中，放入箱式马弗炉，以 10℃/min的升温速率对其进行加热，在600℃下烧结6 h，得到SiCw@SiO2。
1.2.2 SiCw@SiO2/EP复合电介质的制备
为使SiCw@SiO2在EP基体中均匀分散，采用超声辅助机械共混法制备复合电介质试样，SiCw@SiO2/EP复合电介质具体的制备流程如图2所示。
首先称取定量的SiCw@SiO2填料在丙酮溶液中超声分散，将E-51环氧树脂、固化剂、促进剂按100∶80∶1.6的质量比添加到单独的烧杯中进行混合，随后将EP混合物与SiCw@SiO2分散液在室温下混合。将混合体系在70℃油浴中以500 r/min的速度搅拌2 h，以除去丙酮。然后将混合体系在70℃下脱气1 h，再转移至不锈钢模具中进行固化，获得SiCw@SiO2/EP复合电介质。研究表明，两段固化已成为EP通用的固化方案[14]，故本研究选择的固化工艺为120℃/2 h+130℃/2 h。设定SiCw@SiO2的质量分数为0%、5%、10%、15%、20%，并将相应的复合电介质分别编号为EP、5%SiCw@SiO2/EP、10%SiCw@SiO2/EP、15%SiCw@SiO2/EP、20%SiCw @SiO2/EP。
1.3 表征及测试
使用美国FEI公司的Quanta 250 FEG型场发射扫描电镜表征复合电介质的微观断面形貌；使用湘潭市仪器仪表有限公司的DRL-Ⅲ高精度材料导热系数测试仪采用热流法测试复合电介质的导热系数，样品直径为30 mm，厚度为3 mm；使用美国威明顿NC公司的高分辨率TGA2950热重分析仪对复合电介质进行热失重分析（TGA），氮气氛围，升温速率为10℃/min，温度为室温～600℃；使用德国NETZSCH公司的DMA 242E型动态力学分析仪测量复合电介质的动态热力学性能，1 Hz的频率下以5℃/min的恒定加热速率运行，试样尺寸为50 mm×10 mm×5 mm；使用德国Novocontrol GmbH公司的Concept 50型宽频介电阻抗松弛谱仪对复合电介质的介电性能进行测试，频率为10-1～107 Hz。使用美国Instron公司的5967型万能试验机对复合电介质的力学特性进行测试，试样的宽度为10 mm，厚度为3.75 mm，拉伸速率为1 mm/min，标距长度为110 mm，每个试样测试5次，结果取平均值。
2 结果与讨论
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2.1 复合电介质的微观形貌
图3为EP及5%SiCw@SiO2/EP复合电介质的断面SEM图。从图3(a)可以看出，纯EP断面光滑，几乎没有杂质，呈河流状，为典型的脆性断裂特征[15]。图3(b)中SiCw@SiO2填料随机分布，复合电介质相比纯EP表现出更为粗糙的断裂截面。将图3(b)进行放大得到图3(c)，可以明显看出SiCw表面成功氧化形成了SiO2层。
分析可知，SiCw@SiO2均匀地分散在复合电介质内部，没有出现明显的团聚现象，且晶须结构在复合电介质的断面中得到了很好地保留。随着SiCw@SiO2的引入，SiCw@SiO2/EP复合电介质的断裂面变得粗糙，具有明显的剪切变形，表现出高韧性材料的断裂特征。
2.2 复合电介质的热学性能
图4为EP及不同填料质量分数SiCw@SiO2/EP复合电介质导热系数的变化规律。
从图4可以看出，随着SiCw@SiO2填料含量增加，复合电介质的导热系数随之增大。当SiCw@ SiO2的质量分数为5%和10%时，复合电介质的导热系数分别增大至0.28 W/(m·K)和0.31 W/(m·K)，相比于纯EP的导热系数（0.21 W/(m·K)）提高了33.3%和47.4%。在低填料含量下，复合电介质的导热系数增大较为缓慢。继续提高SiCw@SiO2的含量，复合电介质的导热系数增大较快，在填料质量分数为15%和20%时，复合电介质的导热系数分别为0.38 W/(m·K)和0.45 W/(m·K)，分别比纯EP提高了82.9%和117.4%。这是由于当SiCw@SiO2填充量较低时，其被大量导热系数低的EP分隔，填料彼此之间距离太远而未能相互接触，不能形成有效的导热网络，导热系数提高并不明显；随着SiCw@SiO2填充量的提升，其在EP中相互接触形成导热链，继而形成3D导热网络，声子可以在填料和基体之间自由转移，因此导热系数提升明显。
图5和图6分别为纯EP及不同填料质量分数SiCw@SiO2/EP复合电介质的热失重（TGA）曲线和热失重微分（DTG）曲线。从图5～6可以看出，由于EP的降解，复合电介质的质量损失主要发生在350～500℃。此外，复合电介质的热分解温度随填料含量的增加而略有升高，如EP的初始热分解温度为341.34℃，而15%SiCw@SiO2/EP复合电介质的初始热分解温度为355.61℃。
根据GB/T 11026.10—2019规定的耐热指数计算方法计算复合电介质的耐热指数（THRI）[16]，计算公式如式（1）所示。
THRI=0.49×[T5+0.6×(T30-T5)]
式（1）中，T5和T30分别是质量损失为5%和30%时对应的热分解温度。
根据式（1）计算得到15%SiCw@SiO2/EP复合电介质的THRI为188.11℃，相比纯EP的THRI（183.51℃）提升了4.6℃，说明SiCw@SiO2的引入对环氧复合电介质的耐热性有一定程度的提升。
选择质量损失10%时对应的温度作为热分解温度（Td）对复合电介质的热稳定性进行分析，具体数据如表1所示。从表1可以看出，EP的Td为368.26℃，随着SiCw@SiO2含量的增加，复合电介质的Td呈升高的趋势，相比于纯EP，15%SiC@SiO2/EP的Td从368.26℃提高到376.19℃，提高了7.93℃，这可归因于由“实体”结构引起的“曲折路径效应”。此外，DTG结果显示，添加了SiCw@SiO2的复合电介质的最大热分解温度（Tmax）与纯EP相近，表明SiCw@SiO2的引入对复合电介质的热稳定性影响不大。
差示扫描量热法（DSC）是通过测定材料热力学性能的变化来表征其物理或化学变化过程，从DSC图中可以得到材料的玻璃化转变温度（Tg）等信息。电介质的Tg是指其由玻璃态过渡到高弹态所对应的温度，其与交联密度具有良好的相关性。
图7为EP及SiCw@SiO2/EP复合电介质的DSC曲线。
从图7可以看出，SiCw@SiO2/EP复合电介质的Tg随着填料含量的增加呈现先升高后降低的趋势，其中15%SiCw@SiO2/EP的Tg最高为120.75℃，20% SiCw@SiO2/EP的Tg降低至108.32℃，但仍明显高于EP的Tg（104.90℃）。复合电介质的Tg主要与其分子流动性、自由体积和聚合物交联度有关。在填料含量较低时，SiCw@SiO2的加入减小了复合电介质中的自由体积，并且限制了环氧链的链段运动，导致复合电介质的Tg升高。但当填料含量过高时，填料不易分散，在基体中形成较多团聚，进而导致Tg降低。
2.3 复合电介质的介电性能
图8为EP及不同填料质量分数SiCw@SiO2/EP复合电介质介电常数的变化情况。从图8可以看出，由于SiCw@SiO2本身的相对介电常数较高，在其与EP混合后，SiCw@SiO2/EP复合电介质的相对介电常数相比纯EP显著提高。引入少量的SiCw @SiO2即可使复合电介质的相对介电常数发生较大改变。在频率为103 Hz时，纯EP的介电常数为5.03，5%SiCw@SiO2/EP复合电介质的相对介电常数增大到6.68，比纯EP增大了约33%。当填料质量分数增大到15%时，15%SiCw@SiO2/EP复合电介质的相对介电常数显著增大至12.69，相比纯EP提高了152%。随着填料质量分数进一步增加，复合电介质的相对介电常数增速减缓，20%SiCw@SiO2/EP复合电介质的相对介电常数相比纯EP仅增大了161%。
随着SiCw@SiO2质量分数的增加，SiCw@SiO2/EP复合电介质的相对介电常数呈递增趋势，这一方面是由于掺入无机填料后产生了大量的界面极化；另一方面随着SiCw@SiO2填充量的增加，由于填料颗粒之间的间距减小，材料中产生了许多以填料为电极、以EP基体为电介质的微型电容器[17]，导致复合电介质的相对介电常数显著增大。
图9为EP及不同填料质量分数下SiCw@SiO2/EP复合电介质的复介电常数虚部（ε″）随频率（f ）的变化关系。从图9可以看出，在低频区域，复合电介质的ε″-f曲线的斜率绝对值远小于1，表明在低频时，复合电介质中不存在或极少存在直流电导行为，而以松弛极化为主。
图10为EP及不同填料质量分数下SiCw@ SiO2/EP复合电介质的介质损耗因数（tanδ）随频率的变化规律。介质损耗的高低主要取决于电介质中松弛极化的建立以及直流电导的形成[18]。从图10可以看出，复合电介质的介质损耗总体上随着SiCw@SiO2含量的增加而略有提升。其主要原因是，一方面随着SiCw@SiO2含量的增加，复合电介质的电导率提升，使得电导损耗增加；另一方面SiCw@SiO2含量的增加导致复合电介质中出现更多的转向极化和界面极化等松弛过程，极化损耗增加，介质损耗因数也随之增大。
从图10还可以看出，相比于纯EP，SiCw@SiO2/EP复合电介质的介质损耗因数的变化幅度并不明显，尤其是在低频区域（f<103 Hz）时，复合电介质的介质损耗因数仍接近0.01。结合图9和图10可知，添加SiCw@SiO2可以增大复合电介质的相对介电常数，而对其介质损耗因数几乎无影响，这表明SiO2介电层可以有效地阻碍SiCw之间的电连接。SiO2层作为电屏障成功地阻止了复合电介质中导电网络的形成。相对较高的介电常数和较低的介质损耗对于复合电介质在热管理中的应用至关重要。
图11为EP及不同填料质量分数SiCw@SiO2/EP复合电介质交流电导率随频率的变化趋势。从图11可以看出，SiCw@SiO2/EP复合电介质的交流电导率随SiCw@SiO2含量的增加而增大，但低频（102 Hz）下始终保持在较低水平（10-11级）。这主要是因为界面极化相对较弱，且复合电介质内部微型电容器始终提供较大的介电常数和较低的介质损耗，同时SiO2层有效抑制了自由电荷载流子的迁移率并削弱了界面极化。
2.4 复合电介质的力学性能
图12为EP及不同填料质量分数SiCw@SiO2/EP复合电介质典型的应力-应变曲线。从图12可以看出，随着SiCw@SiO2含量的增加，SiCw@SiO2/EP复合电介质的断裂伸长率显著提高，表明SiCw @SiO2的加入提高了EP的延展性和韧性。而当SiCw@SiO2的质量分数为20%时，SiCw@SiO2/EP复合电介质的拉伸应变与拉伸应力减小，这可能是因为填料含量较大，很难分散均匀，使其在环氧基体中出现较多团聚，界面应力集中，进而导致复合电介质的拉伸性能降低。
图13为EP及不同填料质量分数SiCw@SiO2/EP复合电介质的杨氏模量。从图13可以看出，SiCw@SiO2的加入降低了复合电介质的杨氏模量，且加入量越大，降低效果越明显。杨氏模量越小，刚性越小，韧性相对较好。当SiCw@SiO2的质量分数为20%时，复合电介质的杨氏模量为2 475.41 MPa，相比纯EP的2 725.93 MPa降低了18.2%。
图14为EP及不同填料质量分数SiCw@SiO2/EP复合电介质的拉伸强度，拉伸强度从代表性应力-应变曲线的最大应力点处收集。
从图14可以看出，加入SiCw@SiO2后复合电介质的拉伸强度明显升高，纯EP的拉伸强度为38.46 MPa，SiCw@SiO2质量分数为15%的复合电介质拉伸强度最大，为54.36 MPa，比纯EP升高了41.3%。分析原因如下：一方面SiCw@SiO2本身韧性好，具有较高的拉伸强度；另一方面由于SiCw @SiO2的定向结构，当复合电介质受到拉伸力作用时，其内部的SiCw@SiO2可以发挥分散载荷的作用，并且可以有效传递应力，阻止裂纹扩展[19]。另外，经超声处理的SiCw@SiO2可以均匀地分散在基体中，使应力分布均匀，在外力作用下电介质形成的空位、裂纹等结构也会吸收一些能量，因此复合电介质的拉伸强度提高。
图15为复合电介质的DMA损耗因子随温度的变化关系，损耗因子最大时对应的温度即为复合电介质的Tg。由图15可知，当填料质量分数低于20%时，复合电介质的Tg均高于纯EP。这可归因于SiCw@SiO2的加入限制了环氧分子链段运动并且在一定程度上减小了自由体积。但当SiCw@SiO2的质量分数达到20%时，复合电介质的Tg显著降低，这可归因于填料含量太高，分散性变差，导致EP分子链所受束缚变小。
图16为SiCw@SiO2/EP复合电介质储能模量与温度的关系。储能模量反映了复合电介质在接近Tg下存储弹性变形能量的能力。从图16可以看出，复合电介质的储能模量随着SiCw@SiO2质量分数的提高而增大，这是由于SiCw@SiO2本身韧性较大，可以限制聚合物链的运动，有效吸收应力，使应力分布更加均匀。当SiCw@SiO2的质量分数为15%时，复合电介质的最大储能模量达到2 950 MPa，相比于纯EP的最大储能模量（2 324 MPa）增大了26.9%。
3 结论
收起
为满足饱和电抗器用环氧树脂的性能需求，本研究使用溶液共混法将烧结处理后的碳化硅晶须作为填料填充到EP基体中，获得了性能优异的SiCw@SiO2/EP复合电介质，得到如下结论：
（1）当SiCw@SiO2质量分数为15%时，复合电介质的综合性能最优，其导热系数为0.38 W/(m·K)，相比纯EP提升了82.9%；介电常数提高了152%，且介质损耗因数基本不发生变化。
（2）SiCw@SiO2作为功能填料使环氧复合电介质的韧性和拉伸强度得到显著提升，当SiCw@SiO2质量分数为15%时，环氧复合电介质的拉伸强度为54.36 MPa，与纯EP相比提升了41.3%。
（3）SiCw@SiO2的引入可以极大地改善环氧复合电介质的综合特性，为制备具有优异导热性能和高韧性的复合电介质提供了一种简便的方法。
基金
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  • 中国博士后科学基金项目(2018M643475)
  • 电力设备电气绝缘国家重点实验室开放基金(EIPE23210)
  • 四川省重点研发项目(2023YFG0236)
文献
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2024年第57卷第5期
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文章信息
doi: 10.16790/j.cnki.1009-9239.im.2024.05.006
  • 接收时间：2023-06-19
  • 首发时间：2025-12-22
  • 出版时间：2024-05-20
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  • 收稿日期：2023-06-19
  • 修回日期：2023-07-19
基金
中国博士后科学基金项目(2018M643475)
电力设备电气绝缘国家重点实验室开放基金(EIPE23210)
四川省重点研发项目(2023YFG0236)
作者信息
    1国网四川省电力公司电力科学研究院，四川 成都 610000
    2四川大学 电气工程学院， 四川 成都 610065
    3西安交通大学 电气工程学院，陕西 西安 710049

通讯作者:

任俊文（1987-），男（汉族），四川南充人，副研究员，研究方向为高电压与绝缘技术。
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2种不同金属材料的力学参数
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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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