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Article(id=1193556934142948296, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1193556932167431095, articleNumber=null, orderNo=null, doi=10.16790/j.cnki.1009-9239.im.2025.04.003, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1724083200000, receivedDateStr=2024-08-20, revisedDate=1728835200000, revisedDateStr=2024-10-14, acceptedDate=null, acceptedDateStr=null, onlineDate=1762495748314, onlineDateStr=2025-11-07, pubDate=1745078400000, pubDateStr=2025-04-20, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1762495748314, onlineIssueDateStr=2025-11-07, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1762495748314, creator=13701087609, updateTime=1762495748314, updator=13701087609, issue=Issue{id=1193556932167431095, tenantId=1146029695717560320, journalId=1149653034449285133, year='2025', volume='58', issue='4', pageStart='1', pageEnd='144', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1762495747843, creator=13701087609, updateTime=1762498255746, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1193567451108573868, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1193556932167431095, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1193567451112768173, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1193556932167431095, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=16, endPage=23, ext={EN=ArticleExt(id=1193556934428160970, articleId=1193556934142948296, tenantId=1146029695717560320, journalId=1149653034449285133, language=EN, title=Study on energy storage performance of polyvinylidene fluoride based dielectric thin films modified by doping voltage stabilizers, columnId=1193556932997903294, journalTitle=Insulating Materials, columnName=Advanced Energy Storage Dielectric Special Issue, runingTitle=null, highlight=null, articleAbstract=

The ternary copolymer of polyvinylidene fluoride, poly (vinylidene fluoride trifluoroethylene chlorofluoro-ethylene) (P(VDF-TrFE-CFE), abbreviated as PVTC) is expected to be used as a new type of capacitor film material due to its high relative dielectric constant. In this paper, the crystal phase structure of PVTC was regulated by optimizing the hot pressing process of thin film preparation, and the influence of different hot pressing temperatures on the crystal phase structure of PVTC thin films was discussed. Then, PVTC composite films doped with low content voltage stabilizer aromatic ketone small molecule 4-acryloxy-2-hydroxyphenylketone (ALRB) were prepared by solution casting method, and the influence law and mechanism of ALRB doping content on the electrical properties of the composite films were studied systematically. The results show that when the hot pressing temperature is 180℃, a multiphase structure coexisting with α phase, β phase, and γ phase is formed inside the PVTC film, which has significant improvement effect on its dielectric properties and energy storage properties. Appropriate amount of voltage stabilizer ALRB can dissipate high-energy electron energy and improve the insulation performance of PVTC films. When the mass fraction of ALRB is 0.5%, the electric strength of PVTC/ALRB composite film reaches 485.7 kV/mm, and the discharge energy density and charge discharge efficiency are 12.12 J/cm3 and 64.4%, respectively.

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聚偏氟乙烯的三元共聚物聚（偏氟乙烯-三氟乙烯-氯氟乙烯）（P(VDF-TrFE-CFE)，简称PVTC）因具有较高的相对介电常数而有望作为新型电容器薄膜材料。本文首先通过优化薄膜制备的热压工艺来调控PVTC的晶相结构，探讨不同热压温度对PVTC薄膜晶相结构的影响；然后利用溶液流延法制备掺杂低含量电压稳定剂芳香酮类小分子4-丙烯氧基-2-羟基二苯甲酮（ALRB）的PVTC复合薄膜，系统研究ALRB掺杂含量对复合薄膜电学性能的影响规律及机制。结果表明：结果表明：当热压温度为180℃时，PVTC薄膜内部形成了α晶相、β晶相和γ晶相共存的多相结构，对其介电性能和储能性能提升效果显著。适量的电压稳定剂ALRB能够耗散高能电子能量，提高PVTC薄膜的绝缘性能。当ALRB质量分数为0.5%时，PVTC/ALRB复合薄膜的电气强度达到了485.7 kV/mm，储能密度和充放电效率分别为12.12 J/cm3和64.4%。

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张天栋（1987-），男（汉族），黑龙江大庆人，教授，主要从事先进电工绝缘材料与绝缘技术的研究。
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李琳（1986-），女（汉族），黑龙江哈尔滨人，高级工程师，主要从事高电压与绝缘技术的研究。

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李琳（1986-），女（汉族），黑龙江哈尔滨人，高级工程师，主要从事高电压与绝缘技术的研究。

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李琳（1986-），女（汉族），黑龙江哈尔滨人，高级工程师，主要从事高电压与绝缘技术的研究。

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Study on the influence and mechanism of voltage stabilizers on the AC and DC insulation performance of XLPE[D]. Harbin: Harbin University of Science and Technology,2019., articleTitle=Study on the influence and mechanism of voltage stabilizers on the AC and DC insulation performance of XLPE, refAbstract=null), Reference(id=1195072453144749015, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1193556934142948296, doi=null, pmid=null, pmcid=null, year=2014, volume=5, issue=21, pageStart=3677, pageEnd=3687, url=null, language=null, rfNumber=[20], rfOrder=22, authorNames=ZHU L, journalName=The Journal of Physical Chemistry Letters, refType=null, unstructuredReference= ZHU L. Exploring strategies for high dielectric constant and low loss polymer dielectrics[J]. 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掺杂电压稳定剂改性聚偏氟乙烯基介电薄膜的储能性能研究
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李琳 1 , 郑楷川 2 , 马海鑫 2 , 牛晟堃 2 , 于浩 1 , 张健 1 , 邢照亮 3 , 张天栋 2 , 迟庆国 2
绝缘材料 | 先进储能电介质专题 2025,58(4): 16-23
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绝缘材料 | 先进储能电介质专题 2025, 58(4): 16-23
掺杂电压稳定剂改性聚偏氟乙烯基介电薄膜的储能性能研究
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李琳1, 郑楷川2, 马海鑫2, 牛晟堃2, 于浩1, 张健1, 邢照亮3, 张天栋2, 迟庆国2
作者信息
  • 1 国网黑龙江省电力有限公司电力科学研究院，黑龙江 哈尔滨 150030
  • 2 哈尔滨理工大学 工程电介质及其应用教育部重点实验室，黑龙江 哈尔滨 150080
  • 3 中国电力科学研究院有限公司，北京 102209

    • 李琳（1986-），女（汉族），黑龙江哈尔滨人，高级工程师，主要从事高电压与绝缘技术的研究。

通讯作者:

张天栋（1987-），男（汉族），黑龙江大庆人，教授，主要从事先进电工绝缘材料与绝缘技术的研究。
Study on energy storage performance of polyvinylidene fluoride based dielectric thin films modified by doping voltage stabilizers
Lin LI1, Kaichuan ZHENG2, Haixin MA2, Shengkun NIU2, Hao YU1, Jian ZHANG1, Zhaoliang XING3, Tiandong ZHANG2, Qingguo CHI2
Affiliations
  • 1 Electric Power Research Institute of State Grid Heilongjiang Electric Power Co., Ltd., Harbin 150030, China
  • 2 Key Laboratory of Engineering Dielectrics and Its Application, Ministry of Education, Harbin University of Science and Technology, Harbin 150080, China
  • 3 China Electric Power Reserch Institute, Beijing 102209, China
出版时间: 2025-04-20 doi: 10.16790/j.cnki.1009-9239.im.2025.04.003
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摘要
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聚偏氟乙烯的三元共聚物聚（偏氟乙烯-三氟乙烯-氯氟乙烯）（P(VDF-TrFE-CFE)，简称PVTC）因具有较高的相对介电常数而有望作为新型电容器薄膜材料。本文首先通过优化薄膜制备的热压工艺来调控PVTC的晶相结构，探讨不同热压温度对PVTC薄膜晶相结构的影响；然后利用溶液流延法制备掺杂低含量电压稳定剂芳香酮类小分子4-丙烯氧基-2-羟基二苯甲酮（ALRB）的PVTC复合薄膜，系统研究ALRB掺杂含量对复合薄膜电学性能的影响规律及机制。结果表明：结果表明：当热压温度为180℃时，PVTC薄膜内部形成了α晶相、β晶相和γ晶相共存的多相结构，对其介电性能和储能性能提升效果显著。适量的电压稳定剂ALRB能够耗散高能电子能量，提高PVTC薄膜的绝缘性能。当ALRB质量分数为0.5%时，PVTC/ALRB复合薄膜的电气强度达到了485.7 kV/mm，储能密度和充放电效率分别为12.12 J/cm3和64.4%。

聚（偏氟乙烯-三氟乙烯-氯氟乙烯）  /  复合薄膜  /  电压稳定剂  /  储能性能

The ternary copolymer of polyvinylidene fluoride, poly (vinylidene fluoride trifluoroethylene chlorofluoro-ethylene) (P(VDF-TrFE-CFE), abbreviated as PVTC) is expected to be used as a new type of capacitor film material due to its high relative dielectric constant. In this paper, the crystal phase structure of PVTC was regulated by optimizing the hot pressing process of thin film preparation, and the influence of different hot pressing temperatures on the crystal phase structure of PVTC thin films was discussed. Then, PVTC composite films doped with low content voltage stabilizer aromatic ketone small molecule 4-acryloxy-2-hydroxyphenylketone (ALRB) were prepared by solution casting method, and the influence law and mechanism of ALRB doping content on the electrical properties of the composite films were studied systematically. The results show that when the hot pressing temperature is 180℃, a multiphase structure coexisting with α phase, β phase, and γ phase is formed inside the PVTC film, which has significant improvement effect on its dielectric properties and energy storage properties. Appropriate amount of voltage stabilizer ALRB can dissipate high-energy electron energy and improve the insulation performance of PVTC films. When the mass fraction of ALRB is 0.5%, the electric strength of PVTC/ALRB composite film reaches 485.7 kV/mm, and the discharge energy density and charge discharge efficiency are 12.12 J/cm3 and 64.4%, respectively.

P(VDF-TrFE-CFE)  /  composite film  /  voltage stabilizer  /  energy storage performance
李琳, 郑楷川, 马海鑫, 牛晟堃, 于浩, 张健, 邢照亮, 张天栋, 迟庆国. 掺杂电压稳定剂改性聚偏氟乙烯基介电薄膜的储能性能研究. 绝缘材料, 2025 , 58 (4) : 16 -23 . DOI: 10.16790/j.cnki.1009-9239.im.2025.04.003
Lin LI, Kaichuan ZHENG, Haixin MA, Shengkun NIU, Hao YU, Jian ZHANG, Zhaoliang XING, Tiandong ZHANG, Qingguo CHI. Study on energy storage performance of polyvinylidene fluoride based dielectric thin films modified by doping voltage stabilizers[J]. Insulating Materials, 2025 , 58 (4) : 16 -23 . DOI: 10.16790/j.cnki.1009-9239.im.2025.04.003
正文
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0 引言
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电介质电容器因具有充放电速率快、功率密度大、可靠性和安全性高等优点，已在高压直流换流阀、配电网无功补偿系统、新能源汽车电驱动系统、电磁能武器装备等电能传输与转换等领域得到广泛应用[1-3]。目前，双向拉伸聚丙烯（BOPP）薄膜作为应用最广泛的电容器薄膜材料，以其低介质损耗和高电气强度而受到青睐。然而，BOPP薄膜的相对介电常数仅为2.2，室温储能密度也仅为2 J/cm³，为满足实际工程对电容器大容量的需求，只能增加薄膜电容器的体积，这会导致其占据的工程物理空间增大[4-6]。因此提高电容器容积比是当前该领域发展的重要方向[7]。基于此，开发具有高相对介电常数、高电气强度、低能量损耗且易于制备的聚合物储能电介质薄膜成为当前电工绝缘材料领域的研究重点之一[8-10]。
聚偏氯乙烯（PVDF）是一种典型的铁电聚合物，自20世纪40年代末首次合成以来，PVDF及其共聚物在多个领域获得了广泛应用[11]。然而，尽管PVDF具有较高的相对介电常数，但其电气强度较低，且由于偶极子间的极化耦合带来巨大的能量损耗，严重影响薄膜的充放电效率[12]，限制了PVDF作为电容器储能介质薄膜材料的应用。目前提升PVDF基聚合物介电性能与储能特性常用的方法有晶相调控优化与填料掺杂。LIU H等[6]通过退火和淬火处理对PVDF中α晶相、β晶相和γ晶相的比例进行调整，当α晶相、β晶相、γ晶相比例为2∶3∶5时， PVDF薄膜获得了19.66 J/cm3的超高能量密度，表明晶相结构与薄膜的介电性能和储能性能密切相关。
纳米填料掺杂是提升聚合物储能性能的一种普遍手段。刘喆[13]研究了SnO2/PVDF、钛酸钠纳米管/PVTC以及Ag@SiO2/PVDF-TrFE薄膜中有机-无机界面性质及纳米填料对复合薄膜介电性能的影响，成功设计并制备了具有高储能密度和低介质损耗特性的介电复合材料。LUO H B等[14]将SiO2纳米球与二硫化钼（MoS2）复合，并将MoS2@SiO2掺杂到PVDF中，得到具有较高相对介电常数和较高电气强度的PVDF聚合物复合薄膜。此外，电压稳定剂在纳米填料中也有广泛应用，研究者们深入研究了电压稳定剂对聚合物击穿性能的影响，发现电压稳定剂可以显著增强聚合物的抗电树枝特性和电气强度，具有一定的应用前景。
本文以PVDF的三元共聚物聚（偏氟乙烯-三氟乙烯-氯氟乙烯）（P(VDF-TrFE-CFE)，简称PVTC）作为研究对象，探究不同热压温度对PVTC薄膜晶相结构的影响机制。利用电压稳定剂芳香酮类小分子4-丙烯氧基-2-羟基二苯甲酮（ALRB）作为功能填料，采用溶液流延法制备复合薄膜，探讨ALRB掺杂含量对复合薄膜介电性能和储能性能的影响，为开发具有高储能密度的电容器薄膜材料提供参考。
1 实验
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1.1 主要原材料
P(VDF-TrFE-CFE)（产品型号为6833M）购于美国杜邦公司；ALRB购于Aladdin公司；N,N-二甲基甲酰胺（DMF）溶剂购于国药集团化学试剂有限公司。
1.2 PVTC薄膜的制备
称取1 g PVTC粉末溶于10 mL DMF溶剂中，利用磁力搅拌器搅拌12 h，待PVTC粉末充分溶解并形成稳定的胶体后将胶体溶液置于真空箱中除气12 h，然后将胶体溶液倾倒在洁净玻璃基板上，并用涂膜机进行刮涂，形成连续均匀的PVTC薄膜。将基板转移到80℃的烘箱中以去除溶剂，取下薄膜再将其放到80℃的真空烘箱中干燥12 h后放置在平板硫化机中，分别在140、160、180、200℃下进行热压处理，时间为10 min，压强为15 MPa，随后保持压力冷却降温，最终得到PVTC薄膜试样。
1.3 PVTC/ALRB复合薄膜的制备
图1为ALRB分子结构。首先将不同质量分数（0.1%、0.3%、0.5%、0.7%、0.9%）的有机填料ALRB掺入PVTC粉末中混合并溶于DMF溶剂中，重复1.2步骤，热压温度选择180℃，制备一系列不同ALRB掺杂含量的PVTC/ALRB复合薄膜。将质量分数为20%的ALRB加入PVTC粉末中并重复上述操作，热压温度选择180℃，得到对照组薄膜样品。制备过程如图2所示。
1.4 表征与性能测试
使用日本日立公司生产的SU8020型扫描电子显微镜（SEM）表征薄膜的断面微观结构；使用瑞士MettlerToledo公司生产的DSC-1型差示扫描量热仪（DSC）对薄膜进行热性能分析；使用荷兰P Analytical公司生产的XRD-600型X射线衍射仪（XRD）表征薄膜的物相结构；使用德国Bruker公司生产的EQUINOX 55型傅里叶变换红外光谱仪（FTIR）分析薄膜的分子结构；使用北京泰诺科技有限公司生产的ZHD-400型高真空电阻蒸发镀膜设备在薄膜两面分别蒸镀铝电极用于后续介电性能及储能性能的测试；使用德国Novocontrol公司生产的Alpha-A型宽频介电谱仪对薄膜进行介电特性测试；使用Radiant Technologies公司生产的Radiant Premier II型铁电测试仪测试薄膜的电气强度、漏电流密度和储能性能，升压速率设定为400 V/s。
2 结果与讨论
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2.1 PVTC薄膜的晶相结构与储能性能
2.1.1 晶相结构表征
图3为未处理和140、160、180、200℃热压处理后PVTC薄膜的DSC表征结果。从图3(a)可以看出，PVTC在约166℃处有1个熔融峰，该峰对应的温度代表聚合物的熔融转变温度。值得注意的是，随着热压温度的升高，该熔融峰逐渐向更高温度方向移动。这一现象可以归因于PVTC薄膜的结晶相变行为，由于γ晶相的熔融温度高于α晶相，α晶相的熔融温度高于β晶相，随着热压温度的升高，当热压温度接近或高于熔融温度时，α晶相转变为γ晶相，因此PVTC的熔融峰逐渐向更高温度方向移动。从图3(b)可以看出，在降温曲线中，PVTC的结晶峰随热压温度升高的变化趋势和升温曲线相同。在熔融重结晶过程中β晶相含量减少，α晶相的含量逐渐增多，同时在α晶相熔融温度附近，α晶相会转化为γ晶相[15]，因此PVTC的结晶峰向更高温度方向偏移。
图4为未处理及经不同热压温度处理PVTC薄膜的XRD图。从图4可以看出，PVTC薄膜的α晶相衍射峰分别位于18.3°（020）和19.9°（110）；γ晶相衍射峰分别位于18.5°（020）、20.26°（002）和26.6°（022）；β晶相衍射峰位于20.26°（200）[16]。在180℃和200℃下热压处理后，PVTC薄膜位于19.9°（110）处的α晶相衍射峰增强，同时在26.6°（022）处观察到γ晶相衍射峰，这是因为热压温度高于α晶相的熔融温度时，α晶相在其熔融温度附近会转化为γ晶相。
2.1.2 薄膜的介电性能
图5为不同热压温度处理后PVTC薄膜的介电频谱。从图5可以看出，当热压温度为140℃和160℃时，由于温度未达到PVTC的熔融温度，随着热压温度升高，β晶相含量会逐渐增多，而β晶相是极性相，因此随着热压温度升高薄膜的相对介电常数增大[17]。当热压温度为180℃和200℃时，热压温度高于α晶相、β晶相和γ晶相的熔融温度，PVTC中β晶相含量逐渐减少，α晶相含量逐渐增多。当热压温度接近且高于α晶相熔融温度时，α晶相会转变为γ晶相，形成了α晶相、β晶相和γ晶相共存的多晶相结构，多晶相接触界面有利于界面极化，从而提升薄膜的相对介电常数。尽管β晶相含量减少会降低薄膜的相对介电常数，但是界面极化的贡献更大，促使了相对介电常数的提高。在测试频率范围内，PVTC薄膜的介质损耗因数表现出先降低后上升的变化趋势。在低频区域（＜102 Hz）和高频区域（＞105 Hz）均观察到介质损耗因数的提升，这些趋势分别与PVTC材料的α晶相弛豫和β晶相弛豫介质损耗峰相一致。
2.1.3 薄膜的击穿性能
图6为不同热压温度处理后PVTC薄膜的电气强度威布尔分布。从图6可以看出，相较于未处理的PVTC薄膜，140、160、180、200℃热压处理后PVTC薄膜的电气强度明显提升，这是因为热压处理后，薄膜内部结构更加致密，微孔等缺陷更少。经180℃和200℃热压处理的PVTC薄膜电气强度提升幅度更大，这归因于热压处理过程中β晶相含量减少和γ晶相产生，β晶相具有较高的极化强度，其相对介电常数要高于α晶相和γ晶相，施加强电场时，容易在晶相界面产生严重的电场畸变。随着β晶相含量减少，具有介电错配的界面区击穿概率降低，有利于提高电气强度。此外，γ晶相的电气强度也要高于β晶相，这也进一步提升了薄膜的电气强度。
2.1.4 薄膜的储能性能
图7为不同热压温度处理后PVTC薄膜的储能性能。从图7可以看出，热压处理对薄膜的储能性能提升显著，其中经过180℃热压后PVTC薄膜的放电能量密度达到了10.26 J/cm3，充放电效率为52.5%，与未处理的PVTC薄膜相比，分别提升了71.9%和37.8%，这是因为热压减少了介质内部产生缺陷的概率，且热压处理后，β晶相含量减少，α晶相含量增多和γ晶相的产生，有助于提高PVTC薄膜的电气强度和充放电效率。值得注意的是，随着电场的增大，充放电效率呈现先降低再升高的趋势，这是由于，当施加电场大于350 kV/mm时，薄膜内会发生从α晶相到γ晶相的转变，导致其充放电效率出现回升趋势[18]。
综上可知，热压处理会诱导PVTC薄膜的晶相发生转变。当热压温度为180℃时，PVTC薄膜的晶相结构对其整体的介电性能及储能性能有较好的提升效果。
2.2 PVTC/ALRB复合薄膜的测试结果与分析
2.2.1 PVTC/ALRB复合薄膜的微观形貌结构
图8为掺杂ALRB质量分数分别为0.1%、0.3%、0.5%、0.7%、0.9%的PVTC/ALRB复合薄膜的断面形貌。从图8可以看出，掺杂不同质量分数ALRB复合薄膜的厚度为10～12 μm。与经过180℃热压处理的原始PVTC薄膜相比，PVTC/ALRB复合薄膜未见明显的气隙、孔洞或裂纹等缺陷。这一结果表明，ALRB与PVTC之间有良好的界面相容性。
为了验证ALRB掺杂是否成功，采用傅里叶变换红外光谱（FTIR）对复合薄膜进行表征，结果如图9(a)所示。从图9(a)可以看出，PVTC薄膜α晶相的特征吸收峰位于766 cm-1和976 cm-1处；β晶相的特征吸收峰位于840 cm-1和1 073 cm-1处；γ晶相的特征吸收峰位于766 cm-1、812 cm-1和840 cm-1处，这表明ALRB的引入并未影响PVTC薄膜的晶相结构，同时发现当ALRB质量分数较低时 （≤0.9%），PVTC/ALRB复合薄膜未检测到ALRB的FTIR吸收峰。考虑可能是由于ALRB掺杂含量过低，红外吸收峰强度不足导致的，因此对高掺杂含量（ALRB质量分数为20%）PVTC/ALRB复合薄膜进行测试分析，结果如图9(b)所示。从图9(b)可以看出，掺杂ALRB质量分数为20%的复合薄膜具有ALRB的特征峰：936 cm-1处是C-H键的面外摇摆振动特征峰；1 578 cm-1处是ALRB分子的苯环特征峰；1 597 cm-1处是ALRB分子乙烯基中C=C双键的伸缩振动特征峰；1 625 cm-1处是ALRB分子芳香酮C=O双键的伸缩振动特征峰[19]。证明在图9(a)中PVTC/ALRB复合薄膜观察不到ALRB独有的特征峰是因为ALRB掺杂含量过小，同时验证ALRB成功掺入PVTC基体中。
2.2.2 PVTC/ALRB复合薄膜的介电性能
图10(a)为不同ALRB掺杂含量复合薄膜的介电频谱。从图10(a)可以看出，掺杂ALRB复合薄膜的相对介电常数有所增加。这一现象归因于ALRB作为极性分子，其固有的偶极矩在被引入PVTC基体后，受到外加电场的作用而参与到材料的极化过程中，进而导致复合薄膜的相对介电常数得到提升[19]。在测试频率范围内，复合薄膜的介质损耗因数表现出先降低后升高的变化趋势，该趋势与PVTC材料的α晶相弛豫和β晶相弛豫介质损耗峰相一致[20]。
图10(b)总结了频率为103 Hz时，不同ALRB掺杂含量复合薄膜的相对介电常数和介质损耗因数。从图10(b)可以看出，与未掺杂ALRB的PVTC薄膜相比，添加不同质量分数的ALRB后，复合薄膜的相对介电常数和介质损耗因数在103 Hz时差异不明显。整体而言，在频率为100～106 Hz内，由于掺杂ALRB的含量极少，其对复合薄膜相对介电常数和介质损耗因数的影响较为有限。
2.2.3 PVTC/ALRB复合薄膜的击穿性能
图11为PVTC/ALRB复合薄膜的击穿性能测试结果。从图11可以看出，掺杂一定含量电压稳定剂ALRB后，复合薄膜的电气强度得到一定程度的增大。当ALRB的质量分数为0.1%、0.3%、0.5%、0.7%、0.9%时，PVTC/ALRB复合薄膜电气强度分别达到了472.3、479.9、485.7、480.2、483.1 kV/mm，对应的形状因子β值都大于10，这表明所制备的复合薄膜具有很好的绝缘可靠性，证明掺杂ALRB对提升复合薄膜的电气强度有积极影响。
在电荷注入与加速运动过程中，ALRB发挥了关键作用，其通过捕获高能电子并利用自激发或电离机制来耗散具有高动能的电子，有效地降低高能电子的动能并减少其数量，显著减轻对聚合物分子链的冲击作用，对于提高复合薄膜的电气强度具有积极影响。通过引入ALRB，复合薄膜的内部电场分布得到优化，从而降低局部高电场畸变的可能性。此外，ALRB的耗散作用还有助于缓解电荷在聚合物基体中的累积。但是，当ALRB的质量分数大于0.5%时，复合薄膜的电气强度却表现出下降的趋势，这是由于ALRB属于具有高电子亲和能的分子半导体材料，随着ALRB含量增加，其自身半导电特性会提供更多载流子[21]，从而导致复合薄膜的电气强度降低。在利用ALRB调控薄膜击穿特性时，其亲电子特性（限制电荷输运，提高电气强度）与其自身半导电特性（提供额外载流子，降低电气强度）之间存在一定矛盾，因此需调控ALRB在复合薄膜中的掺杂含量。
图12为PVTC/ALRB复合薄膜的漏电流密度测试结果。在100 kV/mm的电场范围内，探究ALRB掺杂含量对复合薄膜的漏电流密度的影响，结果如图12(a)所示。从图12(a)可以看出，在电场为0～60 kV/mm时，相较于PVTC薄膜，掺杂ALRB的复合薄膜漏电流密度有所增大。而在电场为60～100 kV/mm时，由于ALRB纳米片可以捕获高能电子，通过激发或电离的手段使其消散，相较PVTC薄膜，复合薄膜的漏电流密度相对减小。从图12(b)可以看出，100 kV/mm电场下PVTC/ALRB复合薄膜的漏电流密度相比PVTC薄膜明显减小。
2.2.4 PVTC/ALRB复合薄膜的储能性能
图13(a)为不同ALRB掺杂含量PVTC/ALRB复合薄膜的单边电位移-电场强度（D-E）曲线。从图13(a)可以看出，与PVTC薄膜相比，PVTC/ALRB复合薄膜的最大电位移强度变化不大，但剩余极化强度有所下降。可见，掺杂ALRB对于降低复合薄膜在高电场作用下的能量损耗起到积极作用，有助于提高复合薄膜的储能性能。
图13(b)为不同ALRB掺杂含量复合薄膜的储能性能，并在图13(c)中总结了不同ALRB掺杂含量复合薄膜在电场强度下的储能密度和充放电效率。从图13(b)和13(c)图可以看出，掺杂适量的ALRB对复合薄膜储能性能的提升效果显著。当ALRB质量分数为0.5%时，复合薄膜在490 kV/mm下的储能密度达到了12.12 J/cm³，充放电效率达到了64.4%，与PVTC薄膜相比，分别提升了31.6%和15.2%。
3 结论
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本文首先探究了不同热压温度对PVTC薄膜晶相结构的影响，并选择有机电压稳定剂ALRB为填充相，使用溶液流延法结合热压工艺制备了不同掺杂含量的PVTC/ALRB复合薄膜，探究了ALRB含量对PVTC/ALRB复合薄膜微观结构与介电及储能性能的影响机理，得到以下结论：
（1）综合比较不同热压温度热处理后PVTC薄膜晶相结构的变化，发现当热压温度为180℃时，PVTC中α晶相和γ晶相可显著抑制极化损耗，提高电气强度，有助于改善薄膜的储能性能。
（2）电压稳定剂ALRB具有高电子亲和能，能够捕获电荷并降低电导损耗。当ALRB的质量分数为0.5%时，PVTC/ALRB复合薄膜的电气强度为485.7 kV/mm，储能密度和充放电效率分别达到了12.12 J/cm3和64.4%，显著提升了复合薄膜的介电性能和储能性能。
基金
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  • 国家电网有限公司科技项目(5500-202430125A-1-1-ZN)
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2025年第58卷第4期
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doi: 10.16790/j.cnki.1009-9239.im.2025.04.003
  • 接收时间：2024-08-20
  • 首发时间：2025-11-07
  • 出版时间：2025-04-20
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  • 收稿日期：2024-08-20
  • 修回日期：2024-10-14
基金
国家电网有限公司科技项目(5500-202430125A-1-1-ZN)
作者信息
    1 国网黑龙江省电力有限公司电力科学研究院，黑龙江 哈尔滨 150030
    2 哈尔滨理工大学 工程电介质及其应用教育部重点实验室，黑龙江 哈尔滨 150080
    3 中国电力科学研究院有限公司，北京 102209

通讯作者:

张天栋（1987-），男（汉族），黑龙江大庆人，教授，主要从事先进电工绝缘材料与绝缘技术的研究。
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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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