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Article(id=1235553555348779344, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1235553554455392591, articleNumber=null, orderNo=null, doi=10.16790/j.cnki.1009-9239.im.2021.05.004, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1595520000000, receivedDateStr=2020-07-24, revisedDate=1597852800000, revisedDateStr=2020-08-20, acceptedDate=null, acceptedDateStr=null, onlineDate=1772508523069, onlineDateStr=2026-03-03, pubDate=1621440000000, pubDateStr=2021-05-20, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1772508523069, onlineIssueDateStr=2026-03-03, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1772508523069, creator=13701087609, updateTime=1772508523069, updator=13701087609, issue=Issue{id=1235553554455392591, tenantId=1146029695717560320, journalId=1149653034449285133, year='2021', volume='54', issue='5', pageStart='1', pageEnd='108', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1772508522857, creator=13701087609, updateTime=1773989531393, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1241765354544890513, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1235553554455392591, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1241765354544890514, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1235553554455392591, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=27, endPage=33, ext={EN=ArticleExt(id=1235553556124725588, articleId=1235553555348779344, tenantId=1146029695717560320, journalId=1149653034449285133, language=EN, title=Effect of Ratio of Alicyclic Amine to Polyether Amine in Curing Agent on Energy Storage Properties of Epoxy Film, columnId=1190369066675179686, journalTitle=Insulating Materials, columnName=Material Research, runingTitle=null, highlight=null, articleAbstract=

Curing agent acts as a link of epoxy resin molecular chains, its molecular structure will affect the various properties of epoxy resin. In this paper, the influence of curing agent molecular structure on the thermal properties, polarization properties, charge transport properties, and energy storage properties of epoxy films were comprehensively discussed by adjusting the ratio of alicyclic amine to polyether amine in curing agent. The results show that with the increase of proportion of rigid alicyclic amine in curing agent, the thermal stability of epoxy resin is significantly enhanced, and the dielectric loss is greatly reduced. This is mainly because the increase of rigid groups can effectively restrict the turning of molecular segments and the transporting of charge. Meanwhile, with the increase of ratio of alicyclic amine, the electric strength and charge-discharge efficiency of the epoxy film increase at first and then decrease. The F51/AP1.6 has the most excellent electric strength, energy density, and charge-discharge efficiency under four different ratios of curing agent. This is related to its stable molecular structure, low dielectric loss, and extremely high deep traps density.

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固化剂作为连接环氧树脂分子链的纽带，其分子结构会影响环氧树脂的各项性能。本文通过调控固化剂中脂环胺与聚醚胺的比例，综合探究了固化剂分子结构对环氧薄膜热学性能、极化特性、电荷输运特性及储能性能的影响规律。结果表明：随着固化剂中刚性脂环胺比例的增加，环氧树脂的热稳定性显著增强，介质损耗降低，这主要是因为刚性基团的增加能有效限制分子链段的转向过程和载流子迁移过程。同时，随着脂环胺比例的增大，环氧薄膜的电气强度及充放电效率先提升后下降，其中F51/AP1.6的电气强度、储能密度与充放电效率最高，这与其较为稳定的分子结构、较低的介质损耗以及极高的深陷阱密度有关。

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孟永鹏（1976-），男（汉族），陕西西安人，讲师，博士，研究方向为功能电介质材料、绝缘材料检测新技术。
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孔波（1996-），男（汉族），湖南长沙人，硕士生，主要从事储能电介质材料的研究。

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孔波（1996-），男（汉族），湖南长沙人，硕士生，主要从事储能电介质材料的研究。

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孔波（1996-），男（汉族），湖南长沙人，硕士生，主要从事储能电介质材料的研究。

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样品浅陷阱参数深陷阱参数
E/eVQ/nCE/eVQ/nC
F51/AP10.6153.81.0995.4
F51/AP1.30.67146.81.17192.0
F51/AP1.60.67128.41.32217.4
F51/AP20.67111.61.09123.0
), ArticleFig(id=1243118820131455585, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1235553555348779344, language=CN, label=表1, caption=

环氧薄膜的陷阱参数

, figureFileSmall=null, figureFileBig=null, tableContent=
样品浅陷阱参数深陷阱参数
E/eVQ/nCE/eVQ/nC
F51/AP10.6153.81.0995.4
F51/AP1.30.67146.81.17192.0
F51/AP1.60.67128.41.32217.4
F51/AP20.67111.61.09123.0
), ArticleFig(id=1243118820206953060, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1235553555348779344, language=EN, label=Tab.2, caption=Weibull parameters of electric strength ofepoxy films, figureFileSmall=null, figureFileBig=null, tableContent=
样品类型威布尔参数（室温）威布尔参数（70℃）
Eb/(MV/m)βEb/(MV/m)β
F51/AP14269.53147.8
F51/AP1.35359.83818.4
F51/AP1.650711.244313.5
F51/AP245414.535510.8
), ArticleFig(id=1243118820286644838, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1235553555348779344, language=CN, label=表2, caption=

环氧薄膜电气强度的威布尔参数

, figureFileSmall=null, figureFileBig=null, tableContent=
样品类型威布尔参数（室温）威布尔参数（70℃）
Eb/(MV/m)βEb/(MV/m)β
F51/AP14269.53147.8
F51/AP1.35359.83818.4
F51/AP1.650711.244313.5
F51/AP245414.535510.8
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固化剂中脂环胺与聚醚胺比例对环氧薄膜储能性能的影响
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孔波 , 孟永鹏 , 马延昊 , 陈思宇 , 高宇栓 , 王若丞 , 成永红
绝缘材料 | 材料研究 2021,54(5): 27-33
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绝缘材料 | 材料研究 2021, 54(5): 27-33
固化剂中脂环胺与聚醚胺比例对环氧薄膜储能性能的影响
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孔波, 孟永鹏, 马延昊, 陈思宇, 高宇栓, 王若丞, 成永红
作者信息
  • 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

    • 孔波（1996-），男（汉族），湖南长沙人，硕士生，主要从事储能电介质材料的研究。

通讯作者:

孟永鹏（1976-），男（汉族），陕西西安人，讲师，博士，研究方向为功能电介质材料、绝缘材料检测新技术。
Effect of Ratio of Alicyclic Amine to Polyether Amine in Curing Agent on Energy Storage Properties of Epoxy Film
Bo KONG, Yongpeng MENG, Yanhao MA, Siyu CHEN, Yushuan GAO, Ruocheng WANG, Yonghong CHENG
Affiliations
  • State Key Laboratory of Electrical Insulation and Power Equipment, Xi'an Jiaotong University, Xi'an 710049, China
出版时间: 2021-05-20 doi: 10.16790/j.cnki.1009-9239.im.2021.05.004
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摘要
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固化剂作为连接环氧树脂分子链的纽带，其分子结构会影响环氧树脂的各项性能。本文通过调控固化剂中脂环胺与聚醚胺的比例，综合探究了固化剂分子结构对环氧薄膜热学性能、极化特性、电荷输运特性及储能性能的影响规律。结果表明：随着固化剂中刚性脂环胺比例的增加，环氧树脂的热稳定性显著增强，介质损耗降低，这主要是因为刚性基团的增加能有效限制分子链段的转向过程和载流子迁移过程。同时，随着脂环胺比例的增大，环氧薄膜的电气强度及充放电效率先提升后下降，其中F51/AP1.6的电气强度、储能密度与充放电效率最高，这与其较为稳定的分子结构、较低的介质损耗以及极高的深陷阱密度有关。

环氧薄膜  /  介电性能  /  储能密度  /  充放电效率

Curing agent acts as a link of epoxy resin molecular chains, its molecular structure will affect the various properties of epoxy resin. In this paper, the influence of curing agent molecular structure on the thermal properties, polarization properties, charge transport properties, and energy storage properties of epoxy films were comprehensively discussed by adjusting the ratio of alicyclic amine to polyether amine in curing agent. The results show that with the increase of proportion of rigid alicyclic amine in curing agent, the thermal stability of epoxy resin is significantly enhanced, and the dielectric loss is greatly reduced. This is mainly because the increase of rigid groups can effectively restrict the turning of molecular segments and the transporting of charge. Meanwhile, with the increase of ratio of alicyclic amine, the electric strength and charge-discharge efficiency of the epoxy film increase at first and then decrease. The F51/AP1.6 has the most excellent electric strength, energy density, and charge-discharge efficiency under four different ratios of curing agent. This is related to its stable molecular structure, low dielectric loss, and extremely high deep traps density.

epoxy film  /  dielectric properties  /  energy density  /  charge-discharge efficiency
孔波, 孟永鹏, 马延昊, 陈思宇, 高宇栓, 王若丞, 成永红. 固化剂中脂环胺与聚醚胺比例对环氧薄膜储能性能的影响. 绝缘材料, 2021 , 54 (5) : 27 -33 . DOI: 10.16790/j.cnki.1009-9239.im.2021.05.004
Bo KONG, Yongpeng MENG, Yanhao MA, Siyu CHEN, Yushuan GAO, Ruocheng WANG, Yonghong CHENG. Effect of Ratio of Alicyclic Amine to Polyether Amine in Curing Agent on Energy Storage Properties of Epoxy Film[J]. Insulating Materials, 2021 , 54 (5) : 27 -33 . DOI: 10.16790/j.cnki.1009-9239.im.2021.05.004
正文
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0 引言
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储能电介质材料作为薄膜电容器的核心材料，因其轻便、经济以及极高的能量密度等优点，在新能源汽车、智能配电网等领域备受关注[1]。储能密度与充放电效率是衡量电介质材料储能特性的两个重要参数，其计算方法如式（1）～（2）所示。
Ud=∫EdD
η=UdUc
式（1）～（2）中：Ud为放电能量密度，即储能密度（单位为J/cm3）；Uc为充电能量密度（单位为J/cm3）；E为电场强度；D为电位移；η为充放电效率。其中，D=εE，ε为绝对介电常数。所以，储能密度的大小受到材料的介电常数、电气强度（Eb）以及充放电效率的影响。对于线性电介质，充放电效率主要与材料的介质损耗及电导损耗有关[2]。
目前应用最广泛的有机电容器薄膜——双向拉伸聚丙烯（BOPP）薄膜，一方面由于介电常数较低而限制了其储能密度，另一方面因耐高温性能不好而限制了其在高温储能领域的使用[3]，如在电动汽车中用于交直流变换的储能电容器的应用温度为120℃，而BOPP薄膜无法在此温度下正常工作[4]。因此具有良好高温储能特性的聚合物受到了国内外学者的广泛关注。LI Q等[5]制备了交联苯并环丁烯薄膜，其在150℃的高温下储能密度为0.4 J/cm3，充放电效率达到了85%。ZHOU Y等[6]利用等离子体增强气相沉积法将二氧化硅喷覆到不同聚合物的表面，实现了充放电效率的大幅提高。
然而，上述提及的材料或方法成本昂贵，难以满足大规模的工业化生产需求。环氧树脂是被广泛应用的一种电介质材料，具有价格低廉、热稳定性良好、绝缘性能好、介质损耗较低等优点。更好的热稳定性使其适用于更广泛的工作温度，较低的介质损耗与良好的绝缘性能有利于高充放电效率的实现。较BOPP薄膜具有更高的介电常数（环氧树脂介电常数一般为3～5，BOPP介电常数为2.2），有利于实现更高的储能密度，实现薄膜电容器的小型化与轻量化[2]。CHEN S Y等[7]基于双酚A环氧树脂制备了高性能、低成本的环氧薄膜，其不仅在室温下实现了高达9.12 J/cm3的储能密度，还能耐受120℃的高温。作为传统电介质材料，环氧树脂虽然应用广泛，但目前国内外针对其在储能领域的研究还有所欠缺。众所周知，环氧树脂的各项性能，如热性能、介电性能、击穿性能等，受固化剂结构的影响很大，而固化剂结构对环氧树脂储能性能的影响规律及机理尚不明确。
本研究通过曼尼希反应制备脂环胺与聚醚胺物质的量之比不同的4种胺类固化剂，并分别与酚醛环氧树脂进行反应，通过热压工艺制备4种环氧薄膜，对环氧薄膜的玻璃化转变温度、介电性能、电气强度以及储能性能等进行测试，研究固化剂分子链结构对环氧树脂介电及储能性能的影响，为环氧树脂材料的改性与在储能领域的应用提供技术基础。
1 试验
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1.1 主要原材料
本研究选用的环氧树脂为酚醛环氧树脂，型号为F51，上海国药集团化学试剂有限公司，环氧值为0.51～0.54 mol/100 g，黏度为15 000～20 000 mPa·s，软化点为20～30℃，图1为F51型环氧树脂的结构示意图。脂环胺（ACA）为异佛尔酮二胺，型号为IPDA，上海阿拉丁试剂有限公司；聚醚胺（PEA）型号为TTD，德国巴斯夫有限公司。图2为ACA与PEA的结构示意图。
1.2 环氧薄膜的制备方法
将脂环胺（ACA）与聚醚胺（PEA）作为原料，与甲醛及苯酚通过曼尼希反应制备了4种改性脂肪胺固化剂，其中脂环胺与聚醚胺的比例分别为1∶1、1.3∶1、1.6∶1、2∶1，固化剂命名为AP1、AP1.3、AP1.6和AP2。图3为固化剂的结构示意图。固化剂的制备过程及结构表征可参考本课题组之前的工作[7]。将4种固化剂分别与酚醛环氧树脂进行交联反应制备环氧薄膜。制备过程中，预先称取2 g环氧树脂，置于60℃真空烘箱中2 h以去除气泡。同样，称取合适质量的固化剂并在60℃下抽真空15 min。将环氧树脂与固化剂按质量比为3∶1进行共混，在80℃下预热5 min后，脱泡搅拌6 min，均匀共混后在80℃下进行热压，经过80℃/2 h+130℃/1 h+150℃/ 1 h的固化过程后得到环氧薄膜。
1.3 测试方法
采用扫描电子显微镜（SEM）对环氧薄膜的断面形貌进行表征，测试设备型号为VE9800，基恩士有限公司生产。
通过差示扫描量热分析（DSC）仪对环氧树脂的熔融过程进行表征，测试设备型号为TGA/SDTA851，梅特勒-托利多仪器有限公司生产，样品质量约为10 mg，升温速率为10℃/min。
电学测试前预先在薄膜上下表面喷覆圆形金电极，电极面积为0.035 2 cm2。
采用介电分析仪对环氧薄膜的介电频谱和温谱进行测试，测试设备型号为Techologies Concept 80，德国Novocontrol公司生产，其中介电频谱测试在室温（25℃）下进行，测试频率为10-1～106 Hz；介电温谱的测试温度为25～180℃，测试频率分别为10、102、103、104、105、106 Hz。
采用极化电滞回线及高压介电击穿测试系统对环氧薄膜的电滞回线进行测试，测试频率为100 Hz，同时采用该测试系统的击穿模块对环氧薄膜的直流击穿电压进行测试，每组环氧薄膜测试10个样品，并用威布尔分布分析。
采用热刺激去极化电流测量系统对环氧薄膜的热刺激电流（TSDC）进行测试，测试设备型号为Techologies Concept 90，德国Novocontrol公司生产。极化电压为250 V，保压时间为30 min，测试温度为-45～150℃，升温速率为3℃/min。并通过半峰宽法分析热刺激电流曲线，由式（3）～（4）求得环氧薄膜的陷阱电荷量及陷阱能级[8]。
Q=60β∫T0T1I(T)dT
E=2.47Tm2kΔT
式（3）～（4）中：Q为陷阱电荷量，单位为nC；β为升温速率，单位为K/min；T0和T1分别为起始温度和终止温度，单位为K；I(T)为热刺激电流，单位为pA；E为活化能，单位为J；Tm为峰值电流对应的温度，单位为K；ΔT为半峰值对应的温度差，单位为K；k为玻尔兹曼常数，k=1.380 65×10-23 J/K。
2 结果与讨论
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固化后的环氧树脂虽然是热固性材料，但固化剂分子中大量的线性聚醚结构单元使分子链具有较大的空间自由度，增强了大分子的柔顺性。图4为环氧薄膜的实物图。由图4可以看出，所制备的环氧薄膜具备良好的柔韧性，该环氧薄膜的厚度为15 μm，可以实现弯曲和卷绕，能满足薄膜电容器的卷绕工艺要求。图5为环氧薄膜的断面SEM图。从图5可以看出，环氧薄膜的厚度较为均匀，且未观测到明显的气泡和微孔等缺陷。
2.1 DSC分析
高分子聚合物的玻璃化转变温度（Tg）是耐热性的重要反映参数之一。对4种固化后的环氧树脂进行DSC测试，结果如图6所示。从图6可以看出，F51/AP1、F51/AP1.3、F51/AP1.6、F51/AP2的Tg分别为130、147、155、170℃。这表明固化剂中脂环胺比例的增加有利于提升环氧树脂的Tg。环氧树脂的Tg与其分子结构和交联结构密切相关[9]，饱和的脂环结构有利于增加聚合物分子结构的稳定性与刚性，提升环氧树脂的热稳定性。
2.2 介电特性分析
介电常数与介质损耗很大程度上会影响储能电介质的储能密度与充放电效率，环氧薄膜的介电频谱测试结果如图7所示。
从图7可以看出，固化剂中脂环胺比例越大，环氧薄膜的介电常数与介质损耗越小。在频率为 1 kHz时，F51/AP2的介电常数仅为4.1，介质损耗因数为0.01；而F51/AP1的介电常数达到4.56，介质损耗因数为0.015。环氧树脂的极化主要由位移极化与转向极化两部分形成。聚醚胺结构中额外的极性醚键结构有利于介电常数的增大。此外，高分子的介电性能还与其链段的运动能力密切相关[10]。刚性脂环基团的增多会使得固化物中分子运动受阻，极性基团的转向过程受到束缚，从而导致环氧薄膜的介电常数减小。而室温下的介质损耗主要来源于极性基团转向过程中造成的松弛损耗，因此脂环胺比例增大还会导致环氧薄膜的介质损耗减小。
固化剂分子结构对环氧薄膜高温介电性能的影响与室温时类似，如图8所示。从图8可以看出，脂环胺比例的增加导致环氧薄膜的介电常数与介质损耗同时减小。F51/AP2在高温下保持了最低的介质损耗因数，其介质损耗因数直到160℃左右才发生明显变化。F51/AP2在160℃、1 kHz情况下介质损耗因数仅为0.048，而F51/AP1.6为0.086，F51/AP1.3为0.093，F51/AP1则达到了0.22。高温下环氧薄膜的介质损耗主要由泄漏电流造成，这说明脂环胺稳定的分子结构不仅能束缚极性基团的转向，还可以有效地限制载流子的迁移。
2.3 TSDC分析
图9为4种环氧薄膜的TSDC测试曲线及分峰、拟合曲线。使用两个高斯峰对实际测量曲线进行拟合，其中实线为实际测量曲线，点划线为采用高斯拟合法的分离峰，虚线为高斯拟合结果。从图9可以看到，4种环氧薄膜均在100～120℃附近出现了一个宽峰，F51/AP1、F51/AP1.3、F51/AP1.6、F51/AP2出现峰值电流的温度分别为91、92、106、103℃，峰值电流分别为229、531、537、310 pA。
表1为通过式（3）～（4）分析分离峰求得的深陷阱与浅陷阱参数。从表1可以看出，固化剂中聚醚胺与脂肪胺的比例对浅陷阱能级的影响较小，在F51/AP1.3取得了最大的浅陷阱电荷量，达到146.8 nC。而深陷阱能级与深陷阱电荷量随脂肪胺比例的增大呈先上升后下降的趋势。其中，F51/AP1.6的深陷阱能级与电荷量最大，分别达到1.32 eV与217.4 nC。而F51/AP2的两项参数均有明显下降，分别为1.09 eV与123 nC。
2.4 电气强度分析
除了介电常数，电介质的电气强度也是影响其储能密度的重要参数。同时，薄膜电容器的大部分应用环境都对聚合物薄膜的电气强度有较高的要求[11]。
分别在室温和70℃下对环氧薄膜（厚度为12 μm）的电气强度进行测试，并通过双参数威布尔分布模型分析环氧薄膜的直流电气强度，如式（5）所示，表2为4种环氧薄膜直流击穿特性的威布尔参数[8]。
P(E)=1-exp (-(E/Eb)β)
式（5）中：P(E)为失效概率或击穿概率；E为电场强度；Eb为电气强度，也是威布尔分布模型中的尺度参数；β为威布尔分布模型中的形状参数。
图10为在室温及70℃下4种环氧薄膜的电气强度威布尔分布图。从表2可以看出，室温下F51/AP1、F51/AP1.3、F51/AP1.6、F51/AP2的Eb分别为426、535、507、454 MV/m。70℃下F51/AP1.6的电气强度在4种环氧薄膜中最高，其Eb达到443 MV/m，而F51/AP1、F51/AP1.3、F51/AP2的Eb分别为314、381、355 MV/m。可见随着固化剂中脂环胺比例的增加，室温与70℃下环氧薄膜的电气强度均呈先上升后下降的趋势。不同的是，室温下F51/AP1.3的电气强度在4种环氧薄膜中最高，而70℃下F51/AP1.6的电气强度最高。
众所周知，聚合物的电气强度与其电荷输运过程密切相关[12]。在室温条件下，F51/AP1.3极高的浅陷阱密度使其取得了最大的电气强度。浅陷阱虽然对载流子的捕获作用有限，但通过载流子的入陷与脱陷过程，能大幅降低载流子的动能，从而限制碰撞电离过程的发生[13]。在高温条件下，浅陷阱对于载流子的束缚能力不够，深陷阱在此时占据了主要作用。F51/AP1.6拥有4种环氧薄膜中最高的深陷阱能级与最大的深陷阱电荷量，这是其在70℃下保持最优异电气性能的重要因素。深陷阱的增多意味着载流子被捕获的概率增加，载流子的平均自由程减小，电子雪崩过程受到限制[14]。而深陷阱能级的提升意味着电子入陷后需要克服更大的势垒才能脱陷，载流子的迁移过程受到极大的限制[13]。
拥有更多刚性脂环胺结构单元与更稳定空间网络结构的F51/AP2的电气强度未能得到进一步提升，这可能是因为其深陷阱能级过低（仅为1.09 eV，接近深陷阱与浅陷阱的分界能级1 eV），且其深陷阱电荷量相比F51/AP1.6也有所下降（仅为123.0 nC），这使其在高温下对载流子的束缚能力大幅减弱，电子在高场强下极易通过加速过程引发碰撞电离，从而导致介质内载流子数量倍增以及聚合物最终击穿[15]。
2.5 储能性能分析
图11为4种环氧薄膜在室温下的储能密度及充放电效率。由图11可以看出，室温下4种环氧薄膜均保持了很高的充放电效率，在电场强度为400 MV/m时，充放电效率均在90%以上。其中F51/AP1.6在490 MV/m的电场强度下，不仅充放电效率达到90%，还实现了6.92 J/cm3的放电能量密度，几乎是BOPP薄膜放电能量密度的6倍（1.2 J/cm3）[16]。这与其较高的介电常数和较低的介质损耗有关。
一般来说，随着温度的提高，环氧薄膜的充放电效率与放电能量密度会呈明显下降趋势，这是因为温度的升高会造成泄漏电流迅速增大，使得η急剧下降，同时这一部分能量会以热的形式损耗掉，造成Ud的下降[5]。为探究4种环氧薄膜在高温下储能性能的差异，分别在同一电场强度下与同一效率下对4种环氧薄膜的高温储能性能进行比较。
目前电动汽车中用于交直流变换的储能电容器的工作电场强度为200 MV/m，因此这一电场强度下的储能性能非常值得关注[16]。图12为4种环氧薄膜在200 MV/m下的储能密度及充放电效率。从图12可以看出，在室温时，4种环氧薄膜在该电场强度下均保持了100%的充放电效率与1 J/cm3左右的放电能量密度。在70℃时，4种环氧薄膜在该电场强度下的充放电效率虽然有所下降，但都保持在90%以上。随着温度的进一步提升，F51/AP1在该电场强度下的充放电效率恶化得最为剧烈，在100℃时在该电场强度下的η仅为76%，在120℃时仅为54%。而F51/AP1.6环氧薄膜在100℃、200 MV/m条件下还能保持90%的效率，120℃时该场强下的η依然超过了80%。
过低的充放电效率不仅会影响储能密度的大小，而且会限制电容器储能薄膜的实际应用。充放电效率太低会造成能量损失，而且损失的能量以热的形式散发出来，造成设备局部过热，引起薄膜的提前击穿与加速老化[17]。本文着重研究了环氧薄膜在不同温度下充放电效率在80%以上时的最大放电能量密度，结果如图13所示。从图13可以看出，在70℃下，4种环氧薄膜在充放电效率为80%以上时均能达到高于3 J/cm3的放电能量密度，其中F51/AP1.6的放电能量密度达到了3.64 J/cm3。温度升高后，F51/AP1.6也依然保持了该效率下最优异的放电能量密度，在120℃时仍能达到1.04 J/cm3，是F51/AP1（同温度与同效率下仅为0.37 J/cm3）的2.8倍。
比较4种环氧薄膜的储能性能可以看出，环氧薄膜的储能性能，特别是高温下的充放电效率，随着固化剂中脂环胺比例的增加呈明显的先上升后下降的趋势。这主要与环氧薄膜的深陷阱分布有关。高温或高场强条件下，环氧薄膜的介质损耗主要由泄漏电流造成，是充放电效率下降的主要原因，而深陷阱能级及密度的增加能有效限制载流子的迁移过程。因此4种薄膜中深陷阱密度最大的F51/AP1.6具有最优异的储能性能。
3 结论
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（1）环氧树脂的玻璃化转变温度随固化剂中脂环胺比例的增加而显著提升，环氧薄膜的介电常数与介质损耗均随脂环胺比例的增加而减少。
（2）随着固化剂中脂环胺比例的增加，环氧薄膜的深陷阱密度、电气强度、储能密度、充放电效率均呈先上升后下降的趋势。其中，F51/AP1.6的电气强度与储能性能最为优异，其在120℃、80%充放电效率条件下的储能密度是F51/AP1的约3倍。
（3）适当提高固化剂中脂环胺的比例能够提升环氧薄膜的储能性能。另外，通过合理调控固化剂的分子结构，尤其是刚性基团与柔性基团的比例，可以综合优化环氧薄膜的各项性能。
基金
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  • 国家自然科学基金资助项目(51677143)
文献
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参考文献 引证文献
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2021年第54卷第5期
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doi: 10.16790/j.cnki.1009-9239.im.2021.05.004
  • 接收时间：2020-07-24
  • 首发时间：2026-03-03
  • 出版时间：2021-05-20
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  • 收稿日期：2020-07-24
  • 修回日期：2020-08-20
基金
国家自然科学基金资助项目(51677143)
作者信息
    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

通讯作者:

孟永鹏（1976-），男（汉族），陕西西安人，讲师，博士，研究方向为功能电介质材料、绝缘材料检测新技术。
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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
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红菇科 Russulaceae 3 23 11.00 小皮伞属 Marasmius 6 2.87
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光柄菇属 Pluteus 5 2.39
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