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Article(id=1241795751546782518, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1241795749348967189, articleNumber=null, orderNo=null, doi=10.16790/j.cnki.1009-9239.im.2021.08.007, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1601222400000, receivedDateStr=2020-09-28, revisedDate=1604332800000, revisedDateStr=2020-11-03, acceptedDate=null, acceptedDateStr=null, onlineDate=1773996778618, onlineDateStr=2026-03-20, pubDate=1629388800000, pubDateStr=2021-08-20, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1773996778618, onlineIssueDateStr=2026-03-20, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1773996778618, creator=13701087609, updateTime=1773996778618, updator=13701087609, issue=Issue{id=1241795749348967189, tenantId=1146029695717560320, journalId=1149653034449285133, year='2021', volume='54', issue='8', pageStart='1', pageEnd='114', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1773996778094, creator=13701087609, updateTime=1773997690758, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1241799577397953390, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1241795749348967189, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1241799577397953391, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1241795749348967189, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=39, endPage=44, ext={EN=ArticleExt(id=1241795751924269893, articleId=1241795751546782518, tenantId=1146029695717560320, journalId=1149653034449285133, language=EN, title=DC Surface Flashover Voltage of Epoxy Nano-composites in Vacuum Improved by TiO2-MWCNTs Nanofillers, columnId=1190369066675179686, journalTitle=Insulating Materials, columnName=Material Research, runingTitle=null, highlight=null, articleAbstract=

Two kinds of nano-fillers nano-tiania (TiO2) and muti-wall carbon nanotubes (MWCNTS) were selected. Sixteen different epoxy nanocomposite dielectrics were prepared by adding two kinds of nanofiller alone or simultaneously to the epoxy resin. The influence of nanoparticles on the surface flashover characteristics of epoxy nanocomposite dielectrics was explored through the volume resistivity test, surface potential decay and vacuum DC surface flashover experiment. The results show that the surface flashover voltage of epoxy nano-composite is related to the mass fraction of filler, and an appropriate amount of filler can enhance the flashover voltage effectively. Comparing with adding TiO2 (improving 14.49%) and MWCNTS alone (improving 23.11%), adding TiO2 and MWCNT simultaneously can further improve the surface flashover voltage up to 44.99 kV (improving 36.06%). The surface trap characteristics of the material are calculated by the surface potential decay curve. By analyzing the relationship between deep trap and surface flashover voltage, it is found that the flashover voltage is linearly correlated with the deep trap energy level, and the deeper the trap energy, the higher the flashover voltage. The depth of surface deep trap energy is improved by adding two kinds of nanoparticle into epoxy composites, thus the electron emission and charge transport processes are suppressed, and the surface flashover voltage increases.

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选用两种纳米填料：纳米氧化钛（TiO2）和多壁羟基碳纳米管（MWCNTS），向环氧树脂中单独或同时加入两种粒子，制备16种不同的环氧纳米复合电介质。通过体积电阻率测试、表面电位衰减试验与真空直流沿面闪络试验，探究纳米粒子对环氧纳米复合电介质沿面闪络特性的影响。结果表明：环氧纳米复合电介质的沿面闪络电压与填料的质量分数有关，适量的纳米填料会提升复合电介质的沿面闪络电压。单独加入纳米TiO2与MWCNTS分别将闪络电压提升了14.49%和23.11%，同时加入两种填料可进一步将闪络电压提升至44.99 kV，提升幅度高达36.06%。通过表面电位衰减曲线计算了材料的表面陷阱特性。分析深陷阱与沿面闪络电压的关系发现，闪络电压与深陷阱能级线性相关，陷阱能级越深，闪络电压越高。同时添加两种纳米粒子可以提高材料的深陷阱深度，从而抑制材料表面电子发射和电荷输运过程，提高沿面闪络电压。

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申巍（1983-），男（汉族），河北石家庄人，高级工程师，主要从事高电压绝缘技术与电力设备状态评估领域的研究。

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申巍（1983-），男（汉族），河北石家庄人，高级工程师，主要从事高电压绝缘技术与电力设备状态评估领域的研究。

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申巍（1983-），男（汉族），河北石家庄人，高级工程师，主要从事高电压绝缘技术与电力设备状态评估领域的研究。

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纳米TiO2-MWCNTs掺杂提升环氧绝缘材料真空直流沿面闪络性能
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申巍 1 , 李明儒 2 , 李枕 2 , 李盛涛 2
绝缘材料 | 材料研究 2021,54(8): 39-44
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绝缘材料 | 材料研究 2021, 54(8): 39-44
纳米TiO2-MWCNTs掺杂提升环氧绝缘材料真空直流沿面闪络性能
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申巍1, 李明儒2, 李枕2, 李盛涛2
作者信息
  • 1国网陕西省电力公司电力科学研究院，陕西 西安 710199
  • 2西安交通大学 电力设备电气绝缘国家重点实验室，陕西 西安 710049

    • 申巍（1983-），男（汉族），河北石家庄人，高级工程师，主要从事高电压绝缘技术与电力设备状态评估领域的研究。

DC Surface Flashover Voltage of Epoxy Nano-composites in Vacuum Improved by TiO2-MWCNTs Nanofillers
Wei SHEN1, Mingru LI2, Zhen LI2, Shengtao LI2
Affiliations
  • 1Electric Power Research Institute of State Grid Shaanxi Electric Power Company, Xi'an 710199, China
  • 2State Key Laboratory of Electrical Insulation and Power Equipment, Xi'an Jiaotong University, Xi'an 710049, China
出版时间: 2021-08-20 doi: 10.16790/j.cnki.1009-9239.im.2021.08.007
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摘要
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选用两种纳米填料：纳米氧化钛（TiO2）和多壁羟基碳纳米管（MWCNTS），向环氧树脂中单独或同时加入两种粒子，制备16种不同的环氧纳米复合电介质。通过体积电阻率测试、表面电位衰减试验与真空直流沿面闪络试验，探究纳米粒子对环氧纳米复合电介质沿面闪络特性的影响。结果表明：环氧纳米复合电介质的沿面闪络电压与填料的质量分数有关，适量的纳米填料会提升复合电介质的沿面闪络电压。单独加入纳米TiO2与MWCNTS分别将闪络电压提升了14.49%和23.11%，同时加入两种填料可进一步将闪络电压提升至44.99 kV，提升幅度高达36.06%。通过表面电位衰减曲线计算了材料的表面陷阱特性。分析深陷阱与沿面闪络电压的关系发现，闪络电压与深陷阱能级线性相关，陷阱能级越深，闪络电压越高。同时添加两种纳米粒子可以提高材料的深陷阱深度，从而抑制材料表面电子发射和电荷输运过程，提高沿面闪络电压。

沿面闪络  /  陷阱特性  /  纳米复合材料  /  环氧树脂

Two kinds of nano-fillers nano-tiania (TiO2) and muti-wall carbon nanotubes (MWCNTS) were selected. Sixteen different epoxy nanocomposite dielectrics were prepared by adding two kinds of nanofiller alone or simultaneously to the epoxy resin. The influence of nanoparticles on the surface flashover characteristics of epoxy nanocomposite dielectrics was explored through the volume resistivity test, surface potential decay and vacuum DC surface flashover experiment. The results show that the surface flashover voltage of epoxy nano-composite is related to the mass fraction of filler, and an appropriate amount of filler can enhance the flashover voltage effectively. Comparing with adding TiO2 (improving 14.49%) and MWCNTS alone (improving 23.11%), adding TiO2 and MWCNT simultaneously can further improve the surface flashover voltage up to 44.99 kV (improving 36.06%). The surface trap characteristics of the material are calculated by the surface potential decay curve. By analyzing the relationship between deep trap and surface flashover voltage, it is found that the flashover voltage is linearly correlated with the deep trap energy level, and the deeper the trap energy, the higher the flashover voltage. The depth of surface deep trap energy is improved by adding two kinds of nanoparticle into epoxy composites, thus the electron emission and charge transport processes are suppressed, and the surface flashover voltage increases.

flashover voltage  /  trap characteristic  /  nano-composites  /  epoxy resin
申巍, 李明儒, 李枕, 李盛涛. 纳米TiO2-MWCNTs掺杂提升环氧绝缘材料真空直流沿面闪络性能. 绝缘材料, 2021 , 54 (8) : 39 -44 . DOI: 10.16790/j.cnki.1009-9239.im.2021.08.007
Wei SHEN, Mingru LI, Zhen LI, Shengtao LI. DC Surface Flashover Voltage of Epoxy Nano-composites in Vacuum Improved by TiO2-MWCNTs Nanofillers[J]. Insulating Materials, 2021 , 54 (8) : 39 -44 . DOI: 10.16790/j.cnki.1009-9239.im.2021.08.007
正文
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0 引言
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环氧树脂因具有良好的电气性能、优异的力学性能和易塑性等优势，广泛应用于气体绝缘开关、干式变压器、电抗器等高压电力设备[1-8]。随着社会经济发展，输电线路电压等级日益提升，电力设备气/固界面的沿面闪络问题成为制约输变电技术发展的关键壁垒。为了提升环氧电介质的沿面闪络性能，研究人员先后将非导电的TiO2、Al2O3和半导电的SiO2等纳米填料掺入环氧树脂中[9-14]，发现制备出的环氧纳米复合电介质沿面闪络电压与陷阱特性有关，其闪络电压均值提升幅度可达20%，但沿面闪络电压仍需进一步提高。部分学者通过表面氟化、臭氧氧化、表面涂覆等方式[15-16]提升绝缘材料的沿面闪络电压，但这些方法会产生有害气体危及环境及实验人员健康，或因处理条件苛刻、适用范围有限难以应用于大规模工业生产，因此有必要通过纳米改性的方式在现有研究基础上进一步提升绝缘材料的沿面闪络电压。
多壁羟基碳纳米管（MWCNTS）自1991年被发现以来，其优异的介电性能引起了广泛的关注[17]，其巨大的纵横比使粒子具有很大的比表面积，为纳米粒子改性进一步提升材料沿面闪络性能提供了一种新的可能。
通过纳米掺杂提升绝缘材料沿面闪络电压的传统方法通常为单独添加非导电、半导电或导电的纳米填料[9-14]，而较少关注同时掺入两种或多种导电性能完全不同的纳米填料对绝缘材料表面放电性能的影响。在现有纳米掺杂改善电介质沿面性能的方法无法满足进一步提升环氧纳米复合电介质沿面闪络性能需求的情况下，同时加入两种或多种导电性不同的纳米填料，是探寻进一步通过纳米掺杂提升绝缘材料沿面闪络性能的一条新路径。
本研究选择TiO2和MWCNTS两种纳米填料，制备了16种含有不同质量分数纳米填料的环氧基纳米复合电介质，分别测试它们的表面电位衰减特性（SPD）和真空直流沿面闪络电压，通过拟合SPD曲线计算试样的表面陷阱特性，建立真空直流沿面闪络电压与表面陷阱参数之间的联系。
1 试验
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1.1 试样的制备
环氧树脂为液态E51双酚A环氧树脂，南通星辰合成材料有限公司；固化剂为甲基四氢苯酐（GH9303），促进剂为二甲氨基甲基（DMP-30），阿拉丁化学试剂；MWCNTS粒径为10～30 nm，长度为20～30 μm，北京德科岛金纳米技术有限公司；纳米TiO2粒径为10～30 nm，北京德科岛金纳米技术有限公司。试验前将MWCNTS和纳米TiO2放入80℃的烘箱干燥12 h以上。使用前用硅烷偶联剂（KH560）对纳米填料表面进行改性。
制样前将模具清洗干净，均匀喷涂脱模剂（佳丹909）后放入80℃烘箱备用。将纳米TiO2与固化剂在容器中混合，然后用高速剪切机（IKAT25型）进行高速剪切处理，剪切速度为5 200 r/min，剪切时间为15 min。使用THINKY离心搅拌机将剪切后的混合物先离心搅拌10 min，转速为2 000 r/min，再离心脱气10 min，转速为2 200 r/min。然后，使用超声设备（ICQ100KDE型）用最大功率将混合物超声分散10 min，之后将环氧树脂、促进剂和MWCNTS添加到装有混合物的容器中，重复离心搅拌、脱气及超声处理过程。将新得到的混合物倒入模具中进行固化，固化程序为80℃/4 h+120℃/8 h。试样制好后用无水乙醇清洗，然后放入恒温干燥箱备用。样品命名为CaTb（C和T分别代表MWCNT和TiO2，a和b分别为MWCNT和纳米TiO2的填料质量分数，a分别为0.05%、0.10%、0.15%，b分别为1%、2%、5%）。
1.2 表面电位衰减试验
表面电位衰减（SPD）检测系统如图1所示，系统由充电电极、检测器及数据采集模块组成。测试前，先对试样表面充电，充电电压为针电极-10 kV、栅电极-6 kV，充电时间为2 min，然后将检测器的探头迅速移动到试样表面正上方。SPD的采样间隔为1 s，测量时间为10 000 s，试验在60℃下进行。
文献[18-19]详细阐述了通过SPD测试结果计算表面陷阱参数的方法。陷阱特性曲线中有两个峰，分别称为浅陷阱和深陷阱。最大值的水平和垂直坐标被认为是陷阱参数，即陷阱能级和陷阱密度。
1.3 体积电阻率测试
电阻测试采用的是三电极系统，其原理图如图2所示。采用的试验仪器为6517B高阻计。测试样品为直径为100 mm、厚度为1 mm的圆片，测试电压为800 V，重复测量8次，系统自动计算测试误差。
1.4 沿面闪络试验
沿面闪络测试在真空环境下进行，腔体为JTK-200 kV真空腔体，试验装置示意图如图3所示。
从图3可以看出，试样为直径为50 mm、厚度为1 mm的圆片。试验前，将试样及电极放置好，然后分别使用机械泵和分子泵将气体抽离腔体。当腔体内真空度小于3×10-3 Pa，关闭真空泵，静置10 min以确保腔体内气压稳定。试验所用电极为指型电极，电极末端直径为20 mm，电极间距为5 mm。采用步进法升压，升压速率为2 kV/s，记录闪络发生时的电压，每种纳米复合材料至少重复测量18次，闪络电压取测试电压的平均值。
2 结果与讨论
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2.1 试样微观形貌
图4(a)、(b)分别为样品C0.05T0和样品C0.1T2的扫描电子显微镜（SEM）截面图。从图4可以看出，纳米粒子在环氧基体中分散均匀，未发生团聚现象。
2.2 表面陷阱特性
图5为环氧及环氧纳米TiO2复合电介质的SPD曲线和计算得到的深陷阱特性。从图5可以看出，加入纳米粒子后，环氧绝缘材料表面电位的衰减速率发生了变化。聚合物的表面电位的衰减与其深陷阱特性密切相关。通过计算得到表面陷阱特性参数，如图6所示。从图6可以看出，随着粒子质量分数的增加，环氧纳米复合电介质的深陷阱能级先增大后减小，深陷阱密度持续上升，导致表面电位衰减能力发生变化。
根据纳米粒子多层结构模型[20-21]，最接近纳米粒子表面区域的为键合层，纳米粒子表面存在很多不饱和化学键，即为深陷阱。当电子经过纳米粒子时，这些不饱和化学键会吸附附近的电子，使得纳米粒子表面带电，并在纳米粒子附近形成势垒，直到这个势垒与不饱和化学键对电子的吸附作用达到平衡。当纳米粒子的质量分数较低时，单个纳米粒子间距较大，具有吸附能力的不饱和化学键持续增多，使得环氧纳米电介质的陷阱能级随着纳米粒子质量分数的增加而提升，表现为图6(a)的曲线左侧；当纳米粒子质量分数较大时，聚合物中纳米粒子的间距较小，界面区出现重叠，使得单一纳米粒子达到平衡时所需吸附的电子减少，即纳米粒子吸附电子的能力下降，表现为图6(a)的曲线右侧。纳米粒子表面的不饱和化学键是深陷阱的主要来源，随着纳米粒子质量分数的增加，深陷阱密度呈稳定的上升趋势，如图6(b)所示。
2.3 体积电阻率特性
图7为纳米填料质量分数与体积电阻率的关系。从图7可以看出，当纳米粒子加入后，环氧纳米复合电介质的体积电阻率先增大后减小，与图6(a)中深陷阱能级保持相同的变化趋势。
电介质的体积电阻率与其对体内电荷输运的阻碍能力有关。陷阱会捕获其周围的带电粒子，当电子在外电场作用下迁移经过深陷阱附近，会受到深陷阱的吸引作用而入陷，从而降低电子的迁移率及浓度。当深陷阱能级上升时，表明其对电子的捕获及束缚能力增强，电子的迁移率及浓度持续下降，表现为图7各条曲线左侧体积电阻率随着纳米粒子质量分数的增加而上升；当粒子质量分数超过某一极限后，陷阱能级下降，陷阱对电子的吸附能力下降，即为图7曲线右侧描述的体积电阻率在上升到一定程度后反而下降。
2.4 沿面闪络特性
图8为真空环境下环氧纳米复合电介质直流沿面闪络试验结果。从图8可以看出，纳米粒子改变了材料的沿面闪络性能，随着粒子质量分数的增加，闪络电压的平均值先增大后减小，纯环氧材料的直流闪络电压平均值为33.07 kV。当单独加入TiO2、单独加入MWCNTS及同时加入TiO2和MWCNTS时，环氧纳米复合电介质的直流闪络电压平均值最大分别可达37.85、40.70、44.99 kV，较纯环氧材料分别提高了14.49%、23.11%和36.06%。
从图8可知，环氧纳米绝缘材料的闪络电压随粒子质量分数的变化趋势与深陷阱能级随粒子质量分数的变化十分类似，因此沿面闪络电压与深陷阱能级可能存在某种关系。以深陷阱能级为横轴，沿面闪络电压为纵轴，做出深陷阱能级与沿面闪络电压关系图（图9）。如图9所示，随着陷阱能级的变深，沿面闪络电压不断上升，表明深陷阱能级与沿面闪络电压正相关。
2.5 讨论
目前学术界较为认可的沿面闪络理论模型有两个：二次电子发射模型（SEEA）和电子触发松弛极化模型（EPTR）。SEEA理论认为表面陷阱对沿面闪络有着重要的影响[22-24]。
根据SEEA模型，沿面闪络始发于阴极三结合点处的电子发射。当电子从阴极三结合点射出后，会受到介质表面正电荷的吸引作用，直至与介质表面发生碰撞。碰撞时，若入射电子的能量适中，会促进介质表面电子发射，从表面再激发出一个或多个新的电子（二次电子），碰撞同时也会使材料表面吸附的气体分子发生解吸附。二次电子从介质表面射出后，一方面会做与初始电子类似的运动，与介质表面碰撞激发更多的二次电子，导致电子倍增；另一方面会与解吸附的气体分子碰撞，使气体分子电离出正、负电荷，电离的正、负电荷在外电场作用下定向迁移，最终在表层的气体层发生闪络。在电子与介质表面发生碰撞时，深陷阱会捕获入射的电子，电子入陷后形成入陷电子。入陷电子必须从外界获得足够的能量才能从陷阱中脱离，即电子脱陷。电子脱陷的难易程度取决于陷阱能级的大小[25]，陷阱能级大，电子需从外界获得更大的能量克服陷阱对其的束缚作用，进而从陷阱发射出去，因此陷阱能级的增大会降低二次电子发射系数，进而提升沿面闪络电压。
如图9所示，环氧纳米复合电介质的沿面闪络电压与深陷阱能级线性相关。当掺入2%TiO2和0.1%MWCNTS时，深陷阱能级最大为1.14 eV。如前所述，当从电极发射的初始电子撞击到试样表面时，由于电介质的深陷阱能级较大，需要更多的能量才能使介质表面发生碰撞电离，造成材料表面二次电子难以激发，进而阻止了沿面闪络的发生[25]；当进一步增加MWCNTS和TiO2的质量分数时，环氧纳米复合电介质的深陷阱能级下降，初始电子撞击电介质表面后，较容易产生二次电子，使电子在表面发生碰撞电离，进而降低了沿面闪络电压。
3 结论
收起
（1）单独添加纳米TiO2、MWCNTS和同时加入纳米TiO2及MWCNTS可分别使材料的沿面闪络电压提升了14.49%、23.11%和36.06%。
（2）纳米粒子界面效应是导致环氧纳米电介质陷阱特性变化的主要原因，随着纳米填料质量分数的增加，表面深陷阱能级先上升后下降，表面深陷阱密度持续上升，深陷阱能级的变化是体积电阻率变化的主要原因，二者随纳米粒子浓度的改变保持相同的变化趋势。
（3）环氧纳米电介质的真空直流沿面闪络电压与深陷阱能级线性相关，深陷阱能级上升，降低了材料表面发射二次电子的能力，从而增大了沿面闪络电压。
基金
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  • 国网陕西省电力公司项目(5226SX1800FB)
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2021年第54卷第8期
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doi: 10.16790/j.cnki.1009-9239.im.2021.08.007
  • 接收时间：2020-09-28
  • 首发时间：2026-03-20
  • 出版时间：2021-08-20
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  • 收稿日期：2020-09-28
  • 修回日期：2020-11-03
基金
国网陕西省电力公司项目(5226SX1800FB)
作者信息
    1国网陕西省电力公司电力科学研究院，陕西 西安 710199
    2西安交通大学 电力设备电气绝缘国家重点实验室，陕西 西安 710049
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