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Article(id=1199640630298247234, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1199640628146565556, articleNumber=null, orderNo=null, doi=10.16790/j.cnki.1009-9239.im.2023.08.006, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1665331200000, receivedDateStr=2022-10-10, revisedDate=1670774400000, revisedDateStr=2022-12-12, acceptedDate=null, acceptedDateStr=null, onlineDate=1763946214507, onlineDateStr=2025-11-24, pubDate=1692460800000, pubDateStr=2023-08-20, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1763946214507, onlineIssueDateStr=2025-11-24, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1763946214507, creator=13701087609, updateTime=1763946214507, updator=13701087609, issue=Issue{id=1199640628146565556, tenantId=1146029695717560320, journalId=1149653034449285133, year='2023', volume='56', issue='8', pageStart='1', pageEnd='118', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1763946213995, creator=13701087609, updateTime=1766563621744, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1210618832004190662, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1199640628146565556, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1210618832004190663, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1199640628146565556, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=37, endPage=44, ext={EN=ArticleExt(id=1199640630566682691, articleId=1199640630298247234, tenantId=1146029695717560320, journalId=1149653034449285133, language=EN, title=Space charge characteristics of nano-MgO/epoxy composites, columnId=1190369066675179686, journalTitle=Insulating Materials, columnName=Material Research, runingTitle=null, highlight=null, articleAbstract=

Epoxy composite is easy to accumulate space charge under high temperature and high electirc field condition, which would lead to local electirc field distort, and in severe case, partial discharge would produce and insulation would break down. Nano-MgO/EP composites with different doping rate were prepared by mixing nano-MgO particles into epoxy resin. Their glass transition temperature was measured by differential scanning calorimetry (DSC). Their trap characteristics were calculated by thermal stimulation depolarization current method (TSDC). Their space charge characteristics were measured by pulse electroacoustic (PEA) method. The results show that the addition of nano-MgO particles can increase the glass transition temperature of epoxy resin and inhibit the space charge accumulation in epoxy resin. With the increase of nano-MgO doping rate, the glass transition temperature of epoxy composite increases at first and then decreases, the deep trap energy level and density of nano-MgO/EP composite increase at first and then decrease, the space charge density of nano-MgO/EP composite decreases at first and then increases, and the electric field distortion trend is similar with that of space charge. When the doping rate of nano-MgO is 3%, the glass transition temperature of the nano-MgO/epoxy composite reaches the maximum value, and the ability to inhibit the space charge accumulation and electric field distortion is the best.

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环氧复合材料在高温高场等复杂的工况下易积聚空间电荷，造成局部场强畸变，严重时将引发局部放电乃至绝缘击穿。通过纳米MgO颗粒与环氧树脂（EP）混合制备不同掺杂率的纳米MgO/EP复合电介质，采用差示扫描量热分析（DSC）测试环氧复合电介质的玻璃化转变温度；采用热刺激去极化电流法（TSDC）拟合计算环氧复合电介质的陷阱特性；采用电声脉冲法（PEA）测试环氧复合电介质的空间电荷特性。结果表明：纳米MgO颗粒的添加可以提高环氧树脂的玻璃化转变温度，抑制环氧树脂内空间电荷积聚。随着纳米MgO掺杂率的增加，纳米MgO/EP复合电介质的玻璃化转变温度先上升后下降，深陷阱能级和密度均先增大后减小；空间电荷密度先下降后上升，电场畸变的变化趋势与空间电荷的变化趋势相似。当纳米MgO掺杂率为3%时，纳米MgO/EP复合电介质的玻璃化温度达到最大值，抑制空间电荷积聚和场强畸变的能力最好。

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吴鹏（1980-），男（汉族），山东济宁人，高级工程师，主要从事交直流特高压运检技术的研究；

庞曦（1997-），女（汉族），江苏宿迁人，博士生，主要从事电工环氧基聚合物空间电荷输运机理与多物理场仿真计算的研究。

, authorsList=吴鹏, 庞曦, 雷战斐, 柴斌, 许天蕾, 秦有苏, 刘鹏, 彭宗仁)}, authors=[Author(id=1211277135243776194, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1199640630298247234, orderNo=0, firstName=null, middleName=null, lastName=null, nameCn=null, orcid=null, stid=null, country=null, authorPic=null, dead=0, email=null, emailSecond=null, emailThird=null, correspondingAuthor=0, authorType=1, ext={EN=AuthorExt(id=1211277135377993925, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1199640630298247234, authorId=1211277135243776194, language=EN, stringName=Peng WU, firstName=Peng, middleName=null, lastName=WU, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=1, address=1State Grid Ningxia Electric Power Co., Ltd. Ultra High Voltage Company, Yinchuan 750011, China, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null), CN=AuthorExt(id=1211277135487045838, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1199640630298247234, authorId=1211277135243776194, language=CN, stringName=吴鹏, firstName=鹏, middleName=null, lastName=吴, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=1, address=1国网宁夏电力有限公司超高压公司,宁夏 银川 750011, bio={"content":"

吴鹏（1980-），男（汉族），山东济宁人，高级工程师，主要从事交直流特高压运检技术的研究；

"}, bioImg=null, bioContent=

吴鹏（1980-），男（汉族），山东济宁人，高级工程师，主要从事交直流特高压运检技术的研究；

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庞曦（1997-），女（汉族），江苏宿迁人，博士生，主要从事电工环氧基聚合物空间电荷输运机理与多物理场仿真计算的研究。

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庞曦（1997-），女（汉族），江苏宿迁人，博士生，主要从事电工环氧基聚合物空间电荷输运机理与多物理场仿真计算的研究。

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figureFileBig=null, tableContent=
试样玻璃化转变温度/℃
纯EP122.34
0.1% MgO/EP125.25
1% MgO/EP125.58
3% MgO/EP128.17
5% MgO/EP127.00
10% MgO/EP123.67
), ArticleFig(id=1211277140495045028, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1199640630298247234, language=CN, label=表1, caption=

不同掺杂率的纳米MgO/EP复合电介质的玻璃化转变温度

, figureFileSmall=null, figureFileBig=null, tableContent=
试样玻璃化转变温度/℃
纯EP122.34
0.1% MgO/EP125.25
1% MgO/EP125.58
3% MgO/EP128.17
5% MgO/EP127.00
10% MgO/EP123.67
), ArticleFig(id=1211277140570542507, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1199640630298247234, language=EN, label=Tab.2, caption=Trap characteristics of nano MgO/EP composites with different doping rate, figureFileSmall=null, figureFileBig=null, tableContent=
试样陷阱能级/eV陷阱密度/m-3
纯EP1.461.04×1016
0.1% MgO/EP1.574.97×1016
1% MgO/EP1.605.18×1016
3% MgO/EP1.665.32×1016
5% MgO/EP1.583.33×1016
10% MgO/EP1.533.08×1016
), ArticleFig(id=1211277140675400109, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1199640630298247234, language=CN, label=表2, caption=

不同掺杂率的纳米MgO/EP复合电介质的陷阱特性

, figureFileSmall=null, figureFileBig=null, tableContent=
试样陷阱能级/eV陷阱密度/m-3
纯EP1.461.04×1016
0.1% MgO/EP1.574.97×1016
1% MgO/EP1.605.18×1016
3% MgO/EP1.665.32×1016
5% MgO/EP1.583.33×1016
10% MgO/EP1.533.08×1016
), ArticleFig(id=1211277140759286189, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1199640630298247234, language=EN, label=Tab.3, caption=The average space charge density of nano MgO/EP composites with different doping rate, figureFileSmall=null, figureFileBig=null, tableContent=
试样60℃/(C/m3)80℃/(C/m3)
去极化2 s去极化1 h去极化2 s去极化1 h
纯EP1.560.631.811.09
0.1% MgO/EP0.940.311.540.84
1% MgO/EP0.720.281.040.62
3% MgO/EP0.570.180.890.49
5% MgO/EP0.750.190.960.54
10% MgO/EP0.940.201.180.65
), ArticleFig(id=1211277140843172273, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1199640630298247234, language=CN, label=表3, caption=

不同掺杂率的纳米MgO/EP复合电介质的平均空间电荷密度

, figureFileSmall=null, figureFileBig=null, tableContent=
试样60℃/(C/m3)80℃/(C/m3)
去极化2 s去极化1 h去极化2 s去极化1 h
纯EP1.560.631.811.09
0.1% MgO/EP0.940.311.540.84
1% MgO/EP0.720.281.040.62
3% MgO/EP0.570.180.890.49
5% MgO/EP0.750.190.960.54
10% MgO/EP0.940.201.180.65
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纳米MgO/环氧复合电介质的空间电荷特性研究
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吴鹏 1 , 庞曦 2 , 雷战斐 1 , 柴斌 1 , 许天蕾 2 , 秦有苏 1 , 刘鹏 2 , 彭宗仁 2
绝缘材料 | 材料研究 2023,56(8): 37-44
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绝缘材料 | 材料研究 2023, 56(8): 37-44
纳米MgO/环氧复合电介质的空间电荷特性研究
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吴鹏1, 庞曦2, 雷战斐1, 柴斌1, 许天蕾2, 秦有苏1, 刘鹏2, 彭宗仁2
作者信息
  • 1国网宁夏电力有限公司超高压公司,宁夏 银川 750011
  • 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

    • 吴鹏（1980-），男（汉族），山东济宁人，高级工程师，主要从事交直流特高压运检技术的研究；

    庞曦（1997-），女（汉族），江苏宿迁人，博士生，主要从事电工环氧基聚合物空间电荷输运机理与多物理场仿真计算的研究。

Space charge characteristics of nano-MgO/epoxy composites
Peng WU1, Xi PANG2, Zhanfei LEI1, Bin CHAI1, Tianlei XU2, Yousu QIN1, Peng LIU2, Zongren PENG2
Affiliations
  • 1State Grid Ningxia Electric Power Co., Ltd. Ultra High Voltage Company, Yinchuan 750011, China
  • 2State Key Laboratory of Electrical Insulation and Power Equipment, Xi′an Jiaotong University, Xi′an 710049, China
出版时间: 2023-08-20 doi: 10.16790/j.cnki.1009-9239.im.2023.08.006
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摘要
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环氧复合材料在高温高场等复杂的工况下易积聚空间电荷，造成局部场强畸变，严重时将引发局部放电乃至绝缘击穿。通过纳米MgO颗粒与环氧树脂（EP）混合制备不同掺杂率的纳米MgO/EP复合电介质，采用差示扫描量热分析（DSC）测试环氧复合电介质的玻璃化转变温度；采用热刺激去极化电流法（TSDC）拟合计算环氧复合电介质的陷阱特性；采用电声脉冲法（PEA）测试环氧复合电介质的空间电荷特性。结果表明：纳米MgO颗粒的添加可以提高环氧树脂的玻璃化转变温度，抑制环氧树脂内空间电荷积聚。随着纳米MgO掺杂率的增加，纳米MgO/EP复合电介质的玻璃化转变温度先上升后下降，深陷阱能级和密度均先增大后减小；空间电荷密度先下降后上升，电场畸变的变化趋势与空间电荷的变化趋势相似。当纳米MgO掺杂率为3%时，纳米MgO/EP复合电介质的玻璃化温度达到最大值，抑制空间电荷积聚和场强畸变的能力最好。

纳米MgO  /  环氧  /  深陷阱特性  /  空间电荷特性

Epoxy composite is easy to accumulate space charge under high temperature and high electirc field condition, which would lead to local electirc field distort, and in severe case, partial discharge would produce and insulation would break down. Nano-MgO/EP composites with different doping rate were prepared by mixing nano-MgO particles into epoxy resin. Their glass transition temperature was measured by differential scanning calorimetry (DSC). Their trap characteristics were calculated by thermal stimulation depolarization current method (TSDC). Their space charge characteristics were measured by pulse electroacoustic (PEA) method. The results show that the addition of nano-MgO particles can increase the glass transition temperature of epoxy resin and inhibit the space charge accumulation in epoxy resin. With the increase of nano-MgO doping rate, the glass transition temperature of epoxy composite increases at first and then decreases, the deep trap energy level and density of nano-MgO/EP composite increase at first and then decrease, the space charge density of nano-MgO/EP composite decreases at first and then increases, and the electric field distortion trend is similar with that of space charge. When the doping rate of nano-MgO is 3%, the glass transition temperature of the nano-MgO/epoxy composite reaches the maximum value, and the ability to inhibit the space charge accumulation and electric field distortion is the best.

nano-MgO  /  epoxy  /  deep trap characteristics  /  space charge characteristics
吴鹏, 庞曦, 雷战斐, 柴斌, 许天蕾, 秦有苏, 刘鹏, 彭宗仁. 纳米MgO/环氧复合电介质的空间电荷特性研究. 绝缘材料, 2023 , 56 (8) : 37 -44 . DOI: 10.16790/j.cnki.1009-9239.im.2023.08.006
Peng WU, Xi PANG, Zhanfei LEI, Bin CHAI, Tianlei XU, Yousu QIN, Peng LIU, Zongren PENG. Space charge characteristics of nano-MgO/epoxy composites[J]. Insulating Materials, 2023 , 56 (8) : 37 -44 . DOI: 10.16790/j.cnki.1009-9239.im.2023.08.006
正文
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0 引言
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环氧树脂因其优异的粘接性[1-2]、耐腐蚀性[3]、阻燃性[4]、绝缘性能[5]和力学性能[6]，已被广泛应用于电力设备（变压器[7]、气体绝缘开关设备（GIS）[8]、干式套管[9]、平滑电抗器[10]）和电子器件（半导体粘接和封装[4]）。近年来，随着我国特高压输电工程向大容量、长距离、高电压和大电流的方向发展，对环氧树脂复合电介质的电、热、力学性能提出了更高的要求。
电力设备长期在高温高场等复杂的工况下运行可能存在安全隐患，其中环氧复合电介质材料中积聚的空间电荷可能导致电力设备局部电场畸变，严重时将引起电介质材料劣化，甚至引发局部放电和绝缘故障[11-13]。因此，开发热稳定性好、抑制空间电荷积聚的环氧复合电介质材料对提高特高压电力设备的电性能和热性能、保障特高压输电工程的安全稳定运行具有重要意义。
“纳米电介质”的概念由T J LEWIS[15]于1994年首次提出，指的是与电介质基体具有类似电学性能的特殊纳米复合电介质，之后纳米电介质引起了大量学者的关注。近十余年，国内外学者对环氧基纳米复合电介质的热学性能和介电性能进行了大量研究，发现相比传统的环氧电介质，纳米粒子的添加使复合电介质的热稳定性、局部放电、介电性能和击穿强度等性能有了很大的改善[16-19]。添加少量纳米BN可以有效增强环氧复合电介质的电气强度，降低平均电荷密度[20]。添加较低含量的纳米SiO2时，环氧复合电介质的介电性能和空间电荷性能均得到提高[21]。在众多纳米填料中，MgO作为一种成本低廉且比较常见的无机纳米材料，其化学性质较稳定，具有较好的电气性能[22]，被认为是一种可以广泛应用且前景广阔的聚合物补强填料。K J MAJEED等[23]研究发现掺杂纳米MgO能有效提高环氧树脂的相对介电常数、介质损耗因数和热导率。刘衍等[24]研究发现随着纳米MgO掺杂量的增加，环氧复合电介质的介电常数先下降后上升。T ANDRITSCH等[25-26]对不同掺杂率的纳米MgO和Al2O3的环氧复合电介质空间电荷特性进行研究，发现纳米颗粒作为电子和空穴的复合中心，是影响空间电荷分布的主要原因。目前关于环氧复合电介质空间电荷的研究主要针对不同温度[27]、极性反转电压[28]、紫外线照射[29]等外界条件的影响，对于纳米粒子影响复合材料空间电荷特性的机理研究较少，且针对不同掺杂率试样陷阱参数的变化缺乏实验验证与定量化结论。
本研究通过制备不同掺杂率的纳米MgO/EP复合电介质，研究纳米MgO掺杂率对环氧复合电介质玻璃化转变温度、陷阱特性和空间特性的影响，通过分析陷阱特性参数深入研究不同掺杂率纳米MgO抑制空间电荷的机理。
1 试验
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1.1 主要原材料
环氧树脂为双酚A二缩水甘油醚（E51），南通星辰合成材料有限公司；固化剂为甲基六氢邻苯二甲酸酐（MeHHPA），广州深创化工有限公司；促进剂为N,N-二甲基苄胺，国药集团化学试剂有限公司。纳米MgO，宁波贝伽尔新材料有限公司，平均粒径为20 nm，白色球状粉末，未处理前呈亲水性。
1.2 试样制备
为了改善MgO纳米粒子在环氧树脂基体中的团聚现象，首先用γ-氨丙基三乙氧基硅烷偶联剂（KH550）对纳米MgO进行表面改性。然后利用磁力搅拌器将纳米MgO颗粒与环氧树脂、无水乙醇混合，用超声探头进行30 min的超声处理，将混合液置于恒温油浴蒸发锅，蒸出烧杯内残留的无水乙醇。之后按比例加入适量的固化剂和促进剂，通过机械搅拌将其与MgO/EP混合物混合30 min。将搅拌均匀的溶液脱气4 h后浇注到夹片模具中，根据以下固化程序制备出不同掺杂率的薄片方形试样：65℃/10 h+80℃/6 h+110℃/4 h+135℃/6 h+110℃/6 h+80℃/4 h+50℃/4 h。最终制得纯环氧以及掺杂率分别为0.1%、1%、3%、5%和10%的纳米MgO/EP复合电介质，试样尺寸为40 mm×40 mm，平均厚度为0.24 mm。
1.3 测试方法
扫描电子显微镜测试：使用日本KEYENCE公司VE9800S型扫描电子显微镜（SEM）对纳米MgO/EP复合电介质的内部微观结构进行表征测试。所有复合电介质试样均在液氮温度下脆断，再使用英国Quorum公司Q150TES型真空离子溅射仪在断面处溅射一层很薄的金膜，以防止电荷积聚。
差示扫描量热测试：使用德国METTLER公司822e型差示扫描量热仪（DSC）对纳米MgO/EP复合电介质的玻璃化转变温度进行测试。所有测试样品在测试前均进行预烘干处理，测试均在氮气环境下进行，氮气流速约为20 mL/min，温度范围为30～180℃，升温速率为10℃/min。
介电性能测试：使用Novocontrol Concept 80型宽频介电谱对纳米MgO/EP复合电介质的介电性能进行测试，测试频率范围为10-1～106 Hz，测试温度为30℃。为保证试样与系统电极间的良好接触，试样两面溅射直径为30 mm的金电极。
热刺激去极化电流（TSDC）测试：使用Keithley 6517B静电计测量。实验前，试样两面溅射金电极，且经真空干燥（105℃、50 Pa）处理13 h，以尽量除去所含水分。实验时，首先在140℃的温度下对试样施加0.8 kV/mm的直流极化电场40 min。然后快速降温至-120℃，撤去外加电压，将试样两面短路 3 min，直至短路电流衰减到1 pA以内。最后以 3℃/min的速率将试样加热到140℃，线性升温过程中，采用Keithley 6517B型静电计测量外电路通过的电流。
空间电荷测试：使用电声脉冲系统（PEA）测量纳米MgO/EP复合电介质的空间电荷分布[30-31]，脉冲宽度为5 ns，测量场强为30 kV/mm，测试温度分别为60℃和80℃，极化时间和去极化时间均为1 h。
2 结果与分析
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2.1 纳米MgO/EP复合电介质的微观形貌
图1为不同掺杂率的纳米MgO/EP复合电介质的断面扫描电子显微镜（SEM）图。从图1可以看出，随着纳米颗粒的加入，环氧基体中出现一些颜色偏亮的纳米颗粒；随着掺杂率的增加，纳米颗粒的分布密度逐渐增大，但未出现明显团聚现象。
2.2 纳米MgO掺杂率对玻璃化转变温度的影响
玻璃化转变温度（Tg）是材料耐热特性的一个重要指标，与聚合物材料的交联密度紧密相关[32]。本研究以DSC曲线上以等距法确定的中点温度作为材料的玻璃化转变温度。
图2为不同掺杂率的纳米MgO/EP复合电介质的DSC曲线，不同掺杂率的纳米MgO/EP复合电介质的玻璃化转变温度列于表1。从表1可以看出，纯环氧的玻璃化转变温度为122.34℃，随着纳米MgO掺杂率的增加，环氧复合电介质的玻璃化温度先上升再下降，且均高于纯环氧。其中3%掺杂率的纳米MgO/EP复合电介质玻璃化转变温度最高，相较于纯环氧提高了4.77%。这是由于纳米粒子的增加，使纳米粒子与环氧大分子链段间形成界面区，在掺杂阈值内（本研究为≤3%），界面区的形成限制了环氧大分子链段的运动，使环氧大分子的松弛过程发生在更高温度区间，导致环氧复合电介质的玻璃化转变温度上升。随着纳米MgO掺杂率的继续增加，超过掺杂阈值（本研究为>3%），导致界面区发生重叠。界面区重叠区域为环氧基体引入更多的自由体积，为环氧大分子链段运动提供更多空间，降低了环氧复合电介质的玻璃化转变温度。
2.3 纳米MgO掺杂率对介电性能的影响
为了研究掺杂率对纳米MgO/EP复合电介质介电性能的影响，对不同掺杂率的纳米MgO/EP复合电介质进行介电性能测试。图3为室温下纳米MgO/EP复合电介质的介电谱图。
从图3(a)可以看出，随着纳米MgO掺杂率的增加，环氧复合电介质在10-1～106 Hz内的介电常数先下降后上升。随着纳米MgO掺杂率的增加，纳米粒子与环氧大分子形成界面区，导致该区域的分子链段转向困难，抑制环氧树脂分子的极化，从而降低了环氧复合电介质的介电常数。当纳米MgO的掺杂率大于3%时，界面区发生重叠，引入更多自由体积，为环氧大分子链段运动提供了更多空间[24]，从而提高了环氧复合电介质的介电常数。此外，纳米MgO粒子的加入均降低了环氧树脂的介电常数。
从图3(b)可以看出，随着纳米MgO掺杂率的增加，环氧复合电介质在中低频下的介质损耗因数先下降后上升。这是由于纳米MgO粒子的增加使环氧复合电介质中的陷阱能级先增大后减小，陷阱能级的变化使载流子的迁移率先降低后上升，进而使环氧复合电介质的电导率先降低后上升，导致环氧复合电介质的介质损耗因数先降低后上升，其中掺杂率为3%的纳米MgO/EP复合电介质介质损耗因数最小。
2.4 纳米MgO掺杂率对陷阱特性的影响
为了研究纳米MgO掺杂率对环氧基体陷阱特性的影响，对不同掺杂率的纳米MgO/EP复合电介质进行TSDC测试。热刺激去极化电流I满足动力学方程，如式（1）所示。
I(t)=n0sexp(-EkBT)⋅exp-sβ∫T0Texp(-EkBT)dT
式（1）中：n0为初始入陷电荷浓度，C·m-3；s是频率因子，s-1；E是陷阱能级，eV；kB是玻尔兹曼常数；T是绝对温度，K；T0是升温过程的起始温度，K；β是升温速率，K/min。
通过对式（1）的拟合，TSDC曲线可以分解为不同温度下的弛豫峰。图4为不同掺杂率的纳米MgO/EP复合电介质TSDC曲线及分解的弛豫峰。纳米MgO/EP复合电介质的玻璃化转变温度在125℃左右，因此图4中最高温度的热刺激电流峰（约120℃）认为是由玻璃化转变时分子链段运动引发的α峰。α峰可以反映深陷阱的特性如陷阱密度和陷阱能级[33]。与其他拟合的弛豫峰相比（峰2～峰5），认为峰1对电荷入陷和脱陷的影响较大，因此本文主要研究纳米MgO掺杂率对峰1的影响。
表2总结了根据TSDC测试曲线计算出的峰1的陷阱参数。从表2可以看出，随着纳米MgO粒子掺杂率的增加，深陷阱的能级不断增加，从1.46 eV（纯EP）到1.57 eV（0.1%）、1.60 eV（1%）和1.66 eV（3%），这是由于纳米粒子与环氧基体形成的界面区会增大体系的陷阱能级或引入深陷阱。随着纳米MgO掺杂率的进一步增加，深陷阱能级逐渐下降，由1.66 eV（3%）下降至1.58 eV（5%）和1.53 eV（10%），这是界面区域重叠导致的。计算得到的深陷阱密度随掺杂率的变化趋势与深陷阱能级的变化趋势相似，随着纳米MgO掺杂率的增加，深陷阱密度在3%掺杂率时出现拐点，3%掺杂率的纳米MgO/EP复合电介质具有最大的深陷阱密度。
2.5 纳米MgO掺杂率对空间电荷的影响
在高温、高场等复杂的工程环境中，环氧复合电介质中更容易产生和积聚空间电荷[34]。空间电荷的积聚会导致材料发生严重的局部电场畸变，进而引发材料劣化、局部放电甚至绝缘失效[11-13]。图5和图6为不同掺杂率的纳米MgO/EP复合电介质分别在60℃和80℃下加压1 h和去压1 h的彩图。从图5可以看出，随着纳米MgO掺杂率的增加，环氧复合电介质中积聚的电荷量先减小后增大。在3%纳米MgO/EP复合电介质中积聚的空间电荷主要分布在电极与试样界面处，而0.1%和10%纳米MgO/EP复合电介质中积聚的空间电荷逐渐深入试样内部。由此可知，适量的纳米掺杂不仅有利于抑制空间电荷积聚，也能在一定程度上抑制电荷向试样内部注入，避免引起试样电场畸变、材料劣化。由图5还可知，高温（80℃）下的电荷积聚量大于低温（60℃），且高温下的电荷积聚位置靠近试样内部，这是因为高温下电荷更容易从电极注入。从图6可以看出，经过去极化1 h后，高温（80℃）下的积聚电荷量仍大于低温（60℃），这可能是由于高温下电荷量较多，1 h内无法完全消散。
图7和图8分别是不同掺杂率的纳米MgO/EP复合电介质在60℃和80℃下的平均空间电荷密度变化趋势。由图7～8可知，随着掺杂率的增加，空间电荷密度先减小后增大。在60℃下去极化2 s后，纯环氧的平均电荷密度为1.56 C/m3，随着纳米MgO的掺杂率从0.1%增加到3%，试样的平均空间电荷密度由0.94 C/m3降至0.57 C/m3。当纳米MgO的掺杂率由3%增加到10%时，试样的平均空间电荷密度由0.57 C/m3增加到0.94 C/m3。当温度为80℃时，不同掺杂率的纳米MgO/EP复合电介质平均空间电荷密度的变化规律与60℃一致，掺杂率为3%的纳米MgO/EP复合电介质平均空间电荷密度最小，抑制空间电荷积聚能力最强，其具体数值如表3所示。这是因为环氧基体与掺杂的纳米MgO颗粒形成了界面区域，从而引入了更多更深的陷阱捕获移动的载流子。被捕获的载流子与电极相邻的区域形成反向电场，抑制空间电荷向试样内部移动和积聚。当掺杂率较小（≤3%）时，掺杂率越大，深陷阱能级越高，深陷阱密度越大。当掺杂率较大 （>3%）时，界面区重叠并形成传导通道，且陷阱能级变小，导致更多载流子向试样内部迁移并积聚。除此之外，温度对积聚的空间电荷量也有影响。如图7和8所示，随着温度升高，环氧复合电介质的平均空间电荷密度增加。根据肖特基注入理论，电极中的载流子在较高温度下更容易获得能量，因此注入载流子的数量随着温度的升高而增加，进一步导致环氧复合电介质中的电荷积聚量增多。
积聚的空间电荷会导致电场畸变，60℃和80℃下不同掺杂率的纳米MgO/EP复合电介质的场强分布分别如图9和图10所示。从图9～10可以看出，随着掺杂率的增加，局部电场强度最大值先减小后增大，与空间电荷的变化趋势一致。
3 结论
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（1）随着纳米MgO掺杂率的增加，纳米MgO/EP复合电介质的玻璃化转变温度先上升后下降，且均大于纯环氧的玻璃化转变温度，其中3%掺杂率的纳米MgO/EP复合电介质玻璃化转变温度最高，相较于纯环氧提高了4.77%。
（2）随着纳米MgO掺杂率的增加，纳米MgO/EP复合电介质的介电常数和介质损耗因数先下降后上升，且均低于纯环氧，其中3%掺杂率的纳米MgO/EP复合电介质介质损耗因数最小。
（3）纳米MgO/EP复合电介质的深陷阱密度和深陷阱能级随着纳米MgO粒子掺杂率的增加先上升后下降，在3%掺杂率时出现拐点，使得3%掺杂率的纳米MgO/EP复合电介质具有最大的深陷阱能级和密度。
（4）随着纳米MgO掺杂率的增加，纳米MgO/EP复合电介质的空间电荷密度先减小后增大，电场强度最大值与空间电荷的变化趋势一致。当掺杂率为3%时，纳米MgO/EP复合电介质抑制空间电荷积聚和场强畸变的效果最好。
基金
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  • 宁夏自然科学基金资助项目(2021AAC03492)
  • 国网宁夏电力有限公司科技项目(SGNXJX00LZJS2100466)
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2023年第56卷第8期
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doi: 10.16790/j.cnki.1009-9239.im.2023.08.006
  • 接收时间：2022-10-10
  • 首发时间：2025-11-24
  • 出版时间：2023-08-20
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  • 收稿日期：2022-10-10
  • 修回日期：2022-12-12
基金
宁夏自然科学基金资助项目(2021AAC03492)
国网宁夏电力有限公司科技项目(SGNXJX00LZJS2100466)
作者信息
    1国网宁夏电力有限公司超高压公司,宁夏 银川 750011
    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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