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Article(id=1209927350599413971, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1209927347319468160, articleNumber=null, orderNo=null, doi=10.16790/j.cnki.1009-9239.im.2022.04.006, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1622736000000, receivedDateStr=2021-06-04, revisedDate=1628092800000, revisedDateStr=2021-08-05, acceptedDate=null, acceptedDateStr=null, onlineDate=1766398759746, onlineDateStr=2025-12-22, pubDate=1650384000000, pubDateStr=2022-04-20, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1766398759746, onlineIssueDateStr=2025-12-22, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1766398759746, creator=13701087609, updateTime=1766398759746, updator=13701087609, issue=Issue{id=1209927347319468160, tenantId=1146029695717560320, journalId=1149653034449285133, year='2022', volume='55', issue='4', pageStart='1', pageEnd='120', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1766398758964, creator=13701087609, updateTime=1766563041616, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1210616398758408595, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1209927347319468160, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1210616398758408596, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1209927347319468160, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=42, endPage=47, ext={EN=ArticleExt(id=1209927350930764011, articleId=1209927350599413971, tenantId=1146029695717560320, journalId=1149653034449285133, language=EN, title=Research on Dispersing Property of Nanoparticles in HVDC Cable Insulation Materials, columnId=1190369066675179686, journalTitle=Insulating Materials, columnName=Material Research, runingTitle=null, highlight=null, articleAbstract=

The insulation master batch was prepared by twin-screw extruder and internal mixer, and then it was used to prepare HVDC cable insulation. The dispersing property of nanoparticles in insulation was quantitatively analyzed by transmission electron microscope (TEM) and Image J software, and the electrical properties of insulation were tested. The results show that it is difficult to determine the dispersion and distribution degree of nanoparticles in nano-composite DC materials by qualitative analysis through TEM, while the characteristic data of nanoparticles in TEM images can be extracted by Image J, so as to quantitatively analyze the dispersion properties of nanoparticles. Compared with DC material using the master batch prepared by internal mixer, the DC material using the master batch by twin-screw extruder have better electrical properties, and nanoparticles are more evenly distributed and better dispersed in it.

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分别采用双螺杆挤出机和密炼机制备绝缘母料，再将绝缘母料制备成高压直流电缆绝缘料，通过透射电镜（TEM）和Image J软件定量分析直流料中纳米粒子的分散性能，并测试直流料的电气性能。结果表明：通过TEM图像的定性分析难以判断纳米复合直流料中纳米粒子的分布和分散程度，采用Image J软件可以提取TEM图中纳米粒子的特征数据，从而能够定量分析纳米粒子的分散性能；与采用密炼机制备绝缘母料的直流料相比，采用双螺杆挤出机制备绝缘母料的直流料中纳米粒子分布更均匀，分散更好，其电气性能更优。

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曾浩（1988-），男（汉族），江苏南京人，高级工程师，主要从事直流电缆绝缘材料和屏蔽材料的研究。

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曾浩（1988-），男（汉族），江苏南京人，高级工程师，主要从事直流电缆绝缘材料和屏蔽材料的研究。

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曾浩（1988-），男（汉族），江苏南京人，高级工程师，主要从事直流电缆绝缘材料和屏蔽材料的研究。

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Influence of the semiconductive material on space charge build-up in extruded HVDC cables[C]//Conference Record of the IEEE International Symposium on Electrical Insulation. San Diego, USA:IEEE,2010., articleTitle=Influence of the semiconductive material on space charge build-up in extruded HVDC cables, refAbstract=null), Reference(id=1210892031384219767, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209927350599413971, doi=null, pmid=null, pmcid=null, year=2018, volume=51, issue=9, pageStart=12, pageEnd=16, url=null, language=null, rfNumber=[15], rfOrder=14, authorNames=高凯, 曾浩, 朱智恩, journalName=绝缘材料, refType=null, unstructuredReference=高凯,曾浩,朱智恩,等.超导电炭黑复合半导电屏蔽材料对直流电缆绝缘材料空间电荷注入的影响[J].绝缘材料,2018,51(9):12-16., articleTitle=超导电炭黑复合半导电屏蔽材料对直流电缆绝缘材料空间电荷注入的影响, refAbstract=null), Reference(id=1210892031501660279, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209927350599413971, doi=null, pmid=null, pmcid=null, year=2012, volume=38, issue=10, pageStart=2669, pageEnd=2674, url=null, language=null, rfNumber=[16], rfOrder=15, authorNames=周湶, 伍科, 廖瑞金, journalName=高电压技术, refType=null, unstructuredReference=周湶,伍科,廖瑞金,等.纳米碳化硅/低密度聚乙烯复合材料的空间电荷分布特性[J].高电压技术,2012,38(10):2669-2674., articleTitle=纳米碳化硅/低密度聚乙烯复合材料的空间电荷分布特性, refAbstract=null)], funds=[Fund(id=1210892029140267033, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209927350599413971, awardId=5500-201958320A-0-0-00, language=CN, fundingSource=国家电网有限公司总部科技项目(5500-201958320A-0-0-00), fundOrder=null, country=null)], companyList=[AuthorCompany(id=1210892022920114881, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209927350599413971, xref=null, ext=[AuthorCompanyExt(id=1210892022924309186, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209927350599413971, companyId=1210892022920114881, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=NARI Group Corporation (State Grid Electric Power Research Institute), Nanjing 211106, China), AuthorCompanyExt(id=1210892022928503491, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209927350599413971, companyId=1210892022920114881, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=南瑞集团有限公司（国网电力科学研究院有限公司），江苏 南京 211106)])], figs=[ArticleFig(id=1210892026019705712, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209927350599413971, language=EN, label=Fig.1, caption=Flow chart of HVDC insulation preparation, figureFileSmall=tR4cdWmQTllX7bHHaQMToA==, figureFileBig=c56vEumGOApQt9eR5Yluaw==, tableContent=null), ArticleFig(id=1210892026137146231, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209927350599413971, language=CN, label=图1, caption=直流料制备流程图, figureFileSmall=tR4cdWmQTllX7bHHaQMToA==, figureFileBig=c56vEumGOApQt9eR5Yluaw==, tableContent=null), ArticleFig(id=1210892026258781053, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209927350599413971, language=EN, label=Fig.2, caption=TEM images of insulation material A, figureFileSmall=UqLcayZcrBfvT695UvSKOw==, figureFileBig=IsDGDM6TYMCnvnMN0piDoQ==, tableContent=null), ArticleFig(id=1210892026372027270, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209927350599413971, language=CN, label=图2, caption=直流料A的TEM图, figureFileSmall=UqLcayZcrBfvT695UvSKOw==, figureFileBig=IsDGDM6TYMCnvnMN0piDoQ==, tableContent=null), ArticleFig(id=1210892026527216525, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209927350599413971, language=EN, label=Fig.3, caption=TEM images of insulation material B, figureFileSmall=dB6SCRnqNRE1c9lOj91JmQ==, figureFileBig=KeOrPeXS6yosY2bahmqA5Q==, tableContent=null), ArticleFig(id=1210892026707571603, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209927350599413971, language=CN, label=图3, caption=直流料B的TEM图, figureFileSmall=dB6SCRnqNRE1c9lOj91JmQ==, figureFileBig=KeOrPeXS6yosY2bahmqA5Q==, tableContent=null), ArticleFig(id=1210892026845983646, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209927350599413971, language=EN, label=Fig.4, caption=Distribution statistics of nanoparticles in insulation material A, figureFileSmall=6E6qGYaQj8GwasFsPTWGcA==, figureFileBig=FpnzAuVDhsyJcb6Qr0FxYA==, tableContent=null), ArticleFig(id=1210892026988589994, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209927350599413971, language=CN, label=图4, caption=直流料A中纳米粒子的粒径分布统计, figureFileSmall=6E6qGYaQj8GwasFsPTWGcA==, figureFileBig=FpnzAuVDhsyJcb6Qr0FxYA==, tableContent=null), ArticleFig(id=1210892027106030510, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209927350599413971, language=EN, label=Fig.5, caption=Distribution statistics of nanoparticles in insulation material B, figureFileSmall=+0hlwvYwDQVTq4d7rDXKew==, figureFileBig=lyatDkYaeOacLAj1t6ss8Q==, tableContent=null), ArticleFig(id=1210892027236053942, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209927350599413971, language=CN, label=图5, caption=直流料B中纳米粒子的粒径分布统计, figureFileSmall=+0hlwvYwDQVTq4d7rDXKew==, figureFileBig=lyatDkYaeOacLAj1t6ss8Q==, tableContent=null), ArticleFig(id=1210892027340911550, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209927350599413971, language=EN, label=Fig.6, caption=Average particle size of nanoparticles in two kinds of insulation material, figureFileSmall=adVhlnECOw5AWy1UYYKOjQ==, figureFileBig=Ju+kBvfly61amnieQ0jfNA==, tableContent=null), ArticleFig(id=1210892027437380546, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209927350599413971, language=CN, label=图6, caption=两种直流料中纳米粒子的平均粒径, figureFileSmall=adVhlnECOw5AWy1UYYKOjQ==, figureFileBig=Ju+kBvfly61amnieQ0jfNA==, tableContent=null), ArticleFig(id=1210892027525460935, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209927350599413971, language=EN, label=Fig.7, caption=Maximum particle size of nanoparticles in two kinds of insulation material, figureFileSmall=ozDbs5BzapBV6W0pzMLgzQ==, figureFileBig=wTESLjKRJcKEzl2DmTGoQg==, tableContent=null), ArticleFig(id=1210892027630318543, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209927350599413971, language=CN, label=图7, caption=两种直流料中纳米粒子的最大粒径, figureFileSmall=ozDbs5BzapBV6W0pzMLgzQ==, figureFileBig=wTESLjKRJcKEzl2DmTGoQg==, tableContent=null), ArticleFig(id=1210892027743564757, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209927350599413971, language=EN, label=Fig.8, caption=Minimum particle size of nanoparticles in two kinds of insulation material, figureFileSmall=X1l2TyIa0JRGKfw60b7MyA==, figureFileBig=DHx9Po3VKyV7JE2CkmLOtg==, tableContent=null), ArticleFig(id=1210892027831645149, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209927350599413971, language=CN, label=图8, caption=两种直流料中纳米粒子的最小粒径, figureFileSmall=X1l2TyIa0JRGKfw60b7MyA==, figureFileBig=DHx9Po3VKyV7JE2CkmLOtg==, tableContent=null), ArticleFig(id=1210892027940697058, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209927350599413971, language=EN, label=Fig.9, caption=Space charge density distribution of two kinds of insulation material, figureFileSmall=bbOHe56OnljZwvkc8GXUEw==, figureFileBig=kNKeJknmhC2Xce3x6taSNw==, tableContent=null), ArticleFig(id=1210892028041360364, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209927350599413971, language=CN, label=图9, caption=两种直流料的空间电荷密度分布图, figureFileSmall=bbOHe56OnljZwvkc8GXUEw==, figureFileBig=kNKeJknmhC2Xce3x6taSNw==, tableContent=null), ArticleFig(id=1210892028175578094, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209927350599413971, language=EN, label=Tab.1, caption=Statistics of nanoparticles in insulation material A, figureFileSmall=null, figureFileBig=null, tableContent=
编号图片面积/nm2粒子数量/个粒子总面积/nm2粒子平均面积/nm2
116 196×12 2462 3235 689 1822 449
217 213×13 0072 6537 786 1852 935
38 929×6 7446852 100 7572 717
43 679×2 776122291 6312 390
53 446×2 603112295 4612 638
), ArticleFig(id=1210892028293018613, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209927350599413971, language=CN, label=表1, caption=

直流料A中纳米粒子的统计数据

, figureFileSmall=null, figureFileBig=null, tableContent=
编号图片面积/nm2粒子数量/个粒子总面积/nm2粒子平均面积/nm2
116 196×12 2462 3235 689 1822 449
217 213×13 0072 6537 786 1852 935
38 929×6 7446852 100 7572 717
43 679×2 776122291 6312 390
53 446×2 603112295 4612 638
), ArticleFig(id=1210892028376904697, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209927350599413971, language=EN, label=Tab.2, caption=Statistics of nanoparticles in insulation material B, figureFileSmall=null, figureFileBig=null, tableContent=
编号图片面积/nm2粒子数量/个粒子总面积/nm2粒子平均面积/nm2
116 706×12 6111 6036 349 4113 961
28 787×6 6425332 288 0234 293
38 418×6 370343835 7262 437
43 449×2 60293228 1322 453
53 442×2 60287240 4712 764
), ArticleFig(id=1210892028481762301, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209927350599413971, language=CN, label=表2, caption=

直流料B中纳米粒子的统计数据

, figureFileSmall=null, figureFileBig=null, tableContent=
编号图片面积/nm2粒子数量/个粒子总面积/nm2粒子平均面积/nm2
116 706×12 6111 6036 349 4113 961
28 787×6 6425332 288 0234 293
38 418×6 370343835 7262 437
43 449×2 60293228 1322 453
53 442×2 60287240 4712 764
), ArticleFig(id=1210892028586618887, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209927350599413971, language=EN, label=Tab.3, caption=Calculating data of the number of nanoparticles in insulation material A and B, figureFileSmall=null, figureFileBig=null, tableContent=
编号12345
直流料A119125118114117
直流料B97917610464
), ArticleFig(id=1210892028733419528, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209927350599413971, language=CN, label=表3, caption=

直流料A和B中纳米粒子数量的计算数据

, figureFileSmall=null, figureFileBig=null, tableContent=
编号12345
直流料A119125118114117
直流料B97917610464
), ArticleFig(id=1210892028842471440, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209927350599413971, language=EN, label=Tab.4, caption=Electrical properties of two kinds of insulation at different temperatures, figureFileSmall=null, figureFileBig=null, tableContent=
项 目直流料A直流料B
体积电阻率/(Ω·m)30℃2.35×10132.22×1013
50℃1.19×10131.21×1013
70℃1.75×10121.35×1012
90℃5.01×10114.88×1011
直流电气强度/(kV/mm)30℃401366
50℃362324
70℃317296
90℃299285
), ArticleFig(id=1210892028947329043, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209927350599413971, language=CN, label=表4, caption=

两种直流料在不同温度下的电气性能

, figureFileSmall=null, figureFileBig=null, tableContent=
项 目直流料A直流料B
体积电阻率/(Ω·m)30℃2.35×10132.22×1013
50℃1.19×10131.21×1013
70℃1.75×10121.35×1012
90℃5.01×10114.88×1011
直流电气强度/(kV/mm)30℃401366
50℃362324
70℃317296
90℃299285
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高压直流电缆绝缘料中纳米粒子的分散性能研究
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曾浩 , 高凯 , 王传博 , 朱智恩 , 杨黎明
绝缘材料 | 材料研究 2022,55(4): 42-47
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绝缘材料 | 材料研究 2022, 55(4): 42-47
高压直流电缆绝缘料中纳米粒子的分散性能研究
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曾浩, 高凯, 王传博, 朱智恩, 杨黎明
作者信息
  • 南瑞集团有限公司（国网电力科学研究院有限公司），江苏 南京 211106

    • 曾浩（1988-），男（汉族），江苏南京人，高级工程师，主要从事直流电缆绝缘材料和屏蔽材料的研究。

Research on Dispersing Property of Nanoparticles in HVDC Cable Insulation Materials
Hao ZENG, Kai GAO, Chuanbo WANG, Zhien ZHU, Liming YANG
Affiliations
  • NARI Group Corporation (State Grid Electric Power Research Institute), Nanjing 211106, China
出版时间: 2022-04-20 doi: 10.16790/j.cnki.1009-9239.im.2022.04.006
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摘要
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分别采用双螺杆挤出机和密炼机制备绝缘母料，再将绝缘母料制备成高压直流电缆绝缘料，通过透射电镜（TEM）和Image J软件定量分析直流料中纳米粒子的分散性能，并测试直流料的电气性能。结果表明：通过TEM图像的定性分析难以判断纳米复合直流料中纳米粒子的分布和分散程度，采用Image J软件可以提取TEM图中纳米粒子的特征数据，从而能够定量分析纳米粒子的分散性能；与采用密炼机制备绝缘母料的直流料相比，采用双螺杆挤出机制备绝缘母料的直流料中纳米粒子分布更均匀，分散更好，其电气性能更优。

绝缘料  /  纳米粒子  /  分散性能  /  电气性能

The insulation master batch was prepared by twin-screw extruder and internal mixer, and then it was used to prepare HVDC cable insulation. The dispersing property of nanoparticles in insulation was quantitatively analyzed by transmission electron microscope (TEM) and Image J software, and the electrical properties of insulation were tested. The results show that it is difficult to determine the dispersion and distribution degree of nanoparticles in nano-composite DC materials by qualitative analysis through TEM, while the characteristic data of nanoparticles in TEM images can be extracted by Image J, so as to quantitatively analyze the dispersion properties of nanoparticles. Compared with DC material using the master batch prepared by internal mixer, the DC material using the master batch by twin-screw extruder have better electrical properties, and nanoparticles are more evenly distributed and better dispersed in it.

insulation material  /  nanoparticles  /  dispersing property  /  electrical properties
曾浩, 高凯, 王传博, 朱智恩, 杨黎明. 高压直流电缆绝缘料中纳米粒子的分散性能研究. 绝缘材料, 2022 , 55 (4) : 42 -47 . DOI: 10.16790/j.cnki.1009-9239.im.2022.04.006
Hao ZENG, Kai GAO, Chuanbo WANG, Zhien ZHU, Liming YANG. Research on Dispersing Property of Nanoparticles in HVDC Cable Insulation Materials[J]. Insulating Materials, 2022 , 55 (4) : 42 -47 . DOI: 10.16790/j.cnki.1009-9239.im.2022.04.006
正文
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0 引言
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推进传统化石能源向风电、太阳能等新能源的转变是实现“碳达峰、碳中和”的重要措施。柔性直流输电技术作为大规模新能源并网的重要手段，近些年来发展迅速[1]。直流电缆是柔性直流输电的关键装备，其可靠性影响着电网运行的稳定。直流输电早期采用的是油浸纸绝缘（MI）电缆，但因为生产MI电缆不环保，安装和维护非常困难，所以直流输电逐渐采用交联聚乙烯（XLPE）电缆[2]。
目前，国际上高压直流电缆用XLPE绝缘料的市场基本被北欧化工公司垄断，XLPE绝缘料的工作温度仅为70℃，低于交流电缆的工作温度（90℃），采用XLPE绝缘料制造的直流电缆系统输送容量较小。国内外的研究人员已逐步开展工作温度为90℃的高压直流电缆绝缘料（以下简称“直流料”）的研发。
研发90℃直流料采用最多的是纳米复合技术路线，通过添加纳米粒子可以有效地抑制材料中的空间电荷，提高材料的直流耐压水平，降低材料电阻率/电导率对温度的敏感性[3-6]。关于纳米复合直流料的研究大多是研究纳米粒子对直流料电气性能的影响，而对于直流料中纳米粒子分散性能的研究较少，特别是定量评价纳米粒子分散性能的研究更少。
本研究分别采用双螺杆挤出机和密炼机制备绝缘母料，再将绝缘母料制备成直流料，采用透射电镜（TEM）和Image J软件定量分析直流料中纳米粒子的分散性能，并测试直流料的电气性能。通过构建微观纳米粒子的分散性能与宏观材料的电气性能的关系，为纳米复合直流料的性能评价提供参考。
1 试验
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1.1 原材料
基料为扬子石化—巴斯夫公司生产的低密度聚乙烯（LDPE），密度约为0.92 g/cm3，熔体流动速率为2.0 g/10 min；空间电荷抑制剂为一种无机纳米粒子，原生粒径约为20 nm；采用的助剂为抗氧剂300，密度为1.1 g/cm3，灰分含量≤0.05%；采用的交联剂为上海高桥石油化工有限公司生产的过氧化二异丙苯（DCP）。
1.2 直流料的制备
采用双螺杆挤出机和密炼机分别制备掺杂质量分数为10%的空间电荷抑制剂的绝缘母料，并将两种绝缘母料通过往复式单螺杆挤出机按照一定比例稀释，经500目滤网过滤、水下切粒后采用后渗透法添加一定比例的交联剂，制备成直流料，其流程如图1所示，将母料采用双螺杆挤出机和密炼机制备的直流料记为A和B。
1.3 测试方法
1.3.1 TEM测试
通过超声钻石刀将直流料制成厚度为100 nm左右的超薄试片，然后将试片置于具有支持膜的铜网上。在日立公司生产的JEM2100型透射电子显微镜上，将加速电压调整为80 kV，观察试片的微观结构，放大倍数分别为10 K、20 K、50 K。
1.3.2 Image J软件处理方法
先采用Image J软件将TEM图转为8位的灰度图，然后按照图中标尺将软件默认的单位（pixels像素）转换成nm，再调节灰度图的对比度和阈值使纳米粒子能与背景较好区分，最后设置粒子尺寸范围以排除背景灰点，并统计结果。
1.3.3 体积电阻率测试
按照GB/T 1410—2006规定测试，试片厚度为1.0 mm，每组至少5个样品，试验温度分别为30、50、70、90℃。考虑到实际工程中直流电缆绝缘层的平均场强为10～20 kV/mm，因此体积电阻率测试采用20 kV作为测试电压。为了改善金属电极与试片的接触，试片表面涂覆导电银漆作为电极材料。
1.3.4 直流电气强度测试
按照GB/T 1408—2006规定测试，试片厚度为0.3 mm，每组至少10个样品，周围媒介为绝缘油，电极为球形电极，试验温度分别为30、50、70、90℃。试验采用快速升压方式，升压速度为5 kV/s。通过击穿电压除以试片厚度得到直流电气强度。
1.3.5 空间电荷测试
采用压力波法（PWP法）[7-8]开展空间电荷测试。绝缘试片的两面需热贴半导电层，其中绝缘层厚度为1 mm、直径为170 mm，半导电层厚度为0.5 mm、直径为50 mm。测试温度为40℃，对试片施加-40 kV的直流电压（平均场强为40 kV/mm），保持60 min，记录60 min时的空间电荷分布波形。
2 结果与分析
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2.1 TEM分析
图2、图3分别为直流料A和直流料B在不同放大倍数下的TEM典型图像。从图2～3可以看出，两种直流料中纳米粒子分布较为均匀，分散较好，粒径基本都在200 nm以内，但具体的分布和分散程度难以判断，特别是两种直流料的差异性更难判断。因此如何定量评价纳米粒子在聚合物基体中的分布和分散非常重要。
Image J是可以求取图片中物体的长度、面积、角度、圆度等功能的图片分析软件，运用Image J软件可以对TEM图片中的纳米粒子进行数据分析和提取[9]。由于纳米复合聚合物材料的TEM图片存在背景亮度不均匀、纳米粒子边界与图片背景灰度差小的特点，在提取TEM图片中纳米粒子数据之前，需对图像进行二值化处理和对比度调整，形成可以用Image J软件求取纳米粒子数据的图片[10]。
采用Image J软件从TEM图像中提取纳米粒子的特征数据，每种直流料选取5张图片进行提取。表1~2分别为直流料A和直流料B中纳米粒子的统计数据。
2.2 森下氏指数
森下氏指数（Morisita's Index）首先由Masaaki Morisita提出，可以应用于纳米粒子在聚合物基体中分布和分散的研究领域[11]。森下氏指数（I）的表达式如式（1）所示。
I=Q∑i=1nni(ni-1)N(N-1)
式（1）中：Q为图片数量；N为所有图片中粒子总数；ni为第i张图的粒子数量。
森下氏指数的物理意义是当纳米粒子随机分布时，森下氏指数I=1；当纳米粒子均匀分布时，I＜1，并且分布越均匀，越接近于1；当纳米粒子不均匀分布并有团聚时，I＞1，并且I越大，分布越不均匀，团聚也越大。
由于不同TEM图片的实际大小不一致，为了便于计算，统一将图片面积归一为（5 000×2 000）nm2，计算表1～2中的粒子数量，计算数据如表3所示。
根据表3的数据分别代入式（1）计算两种直流料的森下氏指数，可得IA=0.994，IB=1.019。
从计算结果可以看出，IA＜1，且非常接近于1，表明直流料A中纳米粒子的分布非常均匀，而IB＞1，说明直流料B中纳米粒子分布不均匀。
2.3 粒径分布
为了便于比较两种直流料中纳米粒子的粒径分布情况，假设所有粒子都为规则圆形，按照式（2）计算粒子的当量直径。
d=  4S π
式（2）中：d为粒子的当量直径；S为粒子的面积。
计算图2～3中粒子的当量直径，计算结果统计如图4～5所示。从图4～5可以看出，两种直流料中纳米粒子的粒径没有呈现正态分布，而是呈现正偏态分布，但两者的粒径差异难以直接对比。因此，计算两种直流料中的粒径数据，绘制粒径分布如图6～8所示。
从图6～8可以看出，两种直流料中纳米粒子的最小粒径相差不大，最小粒径平均值为21 nm左右，这是由纳米粒子的原生粒径（约20 nm）以及Image J软件的处理方法决定的，而直流料A中纳米粒子的平均粒径和最大粒径均小于直流料B，说明直流料A中纳米粒子的分散性更优。
2.4 电气性能
与交流电缆绝缘料需要考察的参数不一样，一般可以通过体积电阻率/电导率、直流电气强度、空间电荷性能来评价直流电缆绝缘料的电气性能[12-13]，表4是两种直流料在不同温度下的电气性能对比。从表4可以看出，在不同测试温度下，直流料A和直流料B的体积电阻率均非常接近，而直流料A的直流电气强度则明显大于直流料B。
图9是两种直流料试样在加压60 min时的空间电荷密度分布图。从图9可以看出，两种直流料试样在电极附近均形成少量异极性电荷。场增强因子（field enhancement factor，FEF）[14-15]可以表征空间电荷注入情况，FEF的值越大表示空间电荷注入越多。计算得到高电场下（40℃、40 kV/mm）下直流料A的FEF为1.16，小于1.2，其空间电荷抑制效果优于直流料B（FEF为1.21）。
从电气性能测试结果可以看出，直流料A的电气性能比直流料B更好，造成电气性能差异的原因是直流料A采用了双螺杆挤出机制备的绝缘母料。
双螺杆挤出机的剪切强度高于密炼机，纳米粒子在聚合物基体能够充分分散，通过双螺杆挤出机制备绝缘母料的混炼效果更优，这一点从森下氏指数和粒径分布统计的定量分析结果可以看出，与直流料B相比，直流料A中纳米粒子的分布更均匀、粒径更小、分散更好，这些分散效果优异的纳米粒子可能会增加材料中的深陷阱数量[16]，从而起到良好的空间电荷抑制效果；此外，分散较差，甚至发生团聚的纳米粒子会增加材料中的缺陷，从而导致材料的直流耐压水平下降，再加上较差的空间电荷抑制效果，因此直流料B的直流电气强度较低。
3 结论
收起
（1）通过TEM图像的定性分析难以判断纳米复合直流料中纳米粒子的分布和分散程度，采用Image J软件可以提取TEM图中纳米粒子的特征数据，从而能够定量分析纳米粒子的分散性能。
（2）与采用密炼机制备绝缘母料的直流料B相比，采用双螺杆挤出机制备绝缘母料的直流料A中纳米粒子分布更均匀，森下氏指数＜1，粒径较小，分散更好，同时直流料A的电气性能更优。
基金
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  • 国家电网有限公司总部科技项目(5500-201958320A-0-0-00)
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2022年第55卷第4期
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doi: 10.16790/j.cnki.1009-9239.im.2022.04.006
  • 接收时间：2021-06-04
  • 首发时间：2025-12-22
  • 出版时间：2022-04-20
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  • 收稿日期：2021-06-04
  • 修回日期：2021-08-05
基金
国家电网有限公司总部科技项目(5500-201958320A-0-0-00)
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    南瑞集团有限公司（国网电力科学研究院有限公司），江苏 南京 211106
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2种不同金属材料的力学参数
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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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