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Article(id=1242756979559608412, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1242756974576775191, articleNumber=null, orderNo=null, doi=10.16790/j.cnki.1009-9239.im.2021.11.019, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1620662400000, receivedDateStr=2021-05-11, revisedDate=1622476800000, revisedDateStr=2021-06-01, acceptedDate=null, acceptedDateStr=null, onlineDate=1774225953232, onlineDateStr=2026-03-23, pubDate=1637510400000, pubDateStr=2021-11-22, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1774225953232, onlineIssueDateStr=2026-03-23, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1774225953232, creator=13701087609, updateTime=1774225953232, updator=13701087609, issue=Issue{id=1242756974576775191, tenantId=1146029695717560320, journalId=1149653034449285133, year='2021', volume='54', issue='11', pageStart='1', pageEnd='139', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1774225952044, creator=13701087609, updateTime=1774226047274, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1242757374059066044, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1242756974576775191, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1242757374059066045, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1242756974576775191, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=130, endPage=133, ext={EN=ArticleExt(id=1242756980436217977, articleId=1242756979559608412, tenantId=1146029695717560320, journalId=1149653034449285133, language=EN, title=Preparation and Electrical Properties of Polyimide/LDHNSs Composite Films, columnId=1198664996516360309, journalTitle=Insulating Materials, columnName=Polyimide Film Special Issue, runingTitle=null, highlight=null, articleAbstract=

LDHNSs dispersion was obtained by ultrasonic stripping of hydrotalcite assisted with intercalation agent. PI/LDHNSS composite films were prepared by in-situ polymerization, and their electrical properties were studied. The results show that the LDHNSs disperse uniformly in PI matrix without obvious agglomeration and stacking, which show good interfacial compatibility with the matrix. Compared with pure PI film, the volume resistivity and electric strength of the composite films decrease slightly to some extent with the addition of LDHNSs. However, it should be note that the corona resistance life of the composite film is improved significantly. When the mass fraction of LDHNSs is 0.5%, the corona resistance life of the composite film is the longest, which is about 8 times longer than that of pure PI, realizing the maximum improvement of corona resistance performance for composite at a relatively low addition amount.

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通过插层剂辅助超声剥离水滑石，获得剥离充分的LDHNSs分散液；采用原位聚合的方法制备PI/LDHNSs复合薄膜，并对该类复合材料的电学性能进行深入研究。结果表明：LDHNSs在PI基体中分散均匀，未出现明显的团聚和堆叠现象，与基体之间展现出比较好的界面相容性。相较于纯PI薄膜，LDHNSs的加入使复合薄膜的体积电阻率和电气强度出现一定程度的降低；但值得注意的是，复合薄膜的耐电晕寿命明显得到提升；当LDHNSs质量分数为0.5%时，复合薄膜的耐电晕寿命最长，约为纯PI薄膜的8倍，实现了在较低添加量下对复合薄膜耐电晕性能的最大提升。

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马莉莉（1987-），女（汉族），山东德州人，讲师，博士，研究方向为聚酰亚胺基复合材料的性能调控研究。
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刘会（1990-），女（汉族），山东泰安人，硕士生，研究方向为聚酰亚胺基绝缘材料的电性能研究。

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刘会（1990-），女（汉族），山东泰安人，硕士生，研究方向为聚酰亚胺基绝缘材料的电性能研究。

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刘会（1990-），女（汉族），山东泰安人，硕士生，研究方向为聚酰亚胺基绝缘材料的电性能研究。

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tableContent=null), ArticleFig(id=1245100056383173075, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756979559608412, language=CN, label=图7, caption=PI/LDHNSs复合薄膜的耐电晕时间, figureFileSmall=/MhsKVhaffwN33xVnKrdkA==, figureFileBig=6Y8b5JPoJFKFj0j8Pw8RQA==, tableContent=null), ArticleFig(id=1245100056483836379, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756979559608412, language=EN, label=Tab.1, caption=Weibull parameters of PI/LDHNSs composite films, figureFileSmall=null, figureFileBig=null, tableContent=
直流交流
E0/(kV/mm)βE0/(kV/mm)β
PI326.714.93209.413.77
PI/0.25LDHNSs229.413.28161.712.98
PI/0.5LDHNSs265.615.53192.412.11
PI/1LDHNSs289.616.32209.012.51
PI/1.5LDHNSs306.116.79162.612.70
PI/2.5LDHNSs264.512.29140.912.66
PI/5LDHNSs233.012.03147.111.61
), ArticleFig(id=1245100056567722463, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756979559608412, language=CN, label=表1, caption=

PI/LDHNSs复合薄膜的威布尔分布参数

, figureFileSmall=null, figureFileBig=null, tableContent=
直流交流
E0/(kV/mm)βE0/(kV/mm)β
PI326.714.93209.413.77
PI/0.25LDHNSs229.413.28161.712.98
PI/0.5LDHNSs265.615.53192.412.11
PI/1LDHNSs289.616.32209.012.51
PI/1.5LDHNSs306.116.79162.612.70
PI/2.5LDHNSs264.512.29140.912.66
PI/5LDHNSs233.012.03147.111.61
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PI/LDHNSs复合薄膜的制备及电性能研究
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刘会 1 , 马莉莉 1, 2 , 郭海泉 3 , 郝春成 1 , 张洪 2
绝缘材料 | 聚酰亚胺薄膜专题 2021,54(11): 130-133
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绝缘材料 | 聚酰亚胺薄膜专题 2021, 54(11): 130-133
PI/LDHNSs复合薄膜的制备及电性能研究
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刘会1, 马莉莉1, 2, 郭海泉3, 郝春成1, 张洪2
作者信息
  • 1青岛科技大学 材料科学与工程学院，山东 青岛 266042
  • 2华北电力大学 新能源电力系统 国家重点实验室，北京 102206
  • 3中国科学院长春应用化学研究所 高分子复合材料工程实验室， 吉林 长春 130022

    • 刘会（1990-），女（汉族），山东泰安人，硕士生，研究方向为聚酰亚胺基绝缘材料的电性能研究。

通讯作者:

马莉莉（1987-），女（汉族），山东德州人，讲师，博士，研究方向为聚酰亚胺基复合材料的性能调控研究。
Preparation and Electrical Properties of Polyimide/LDHNSs Composite Films
Hui LIU1, Lili MA1, 2, Haiquan GUO3, Chuncheng HAO1, Hong ZHANG2
Affiliations
  • 1College of Material Science and Engineering, Qingdao University of Science and Technology, Qingdao 266042, China
  • 2State Key Laboratory of New Energy Power System, North China Electric Power University, Beijing 102206, China
  • 3Polymer Composites Engineering Laboratory, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, Changchun 130022, China
出版时间: 2021-11-22 doi: 10.16790/j.cnki.1009-9239.im.2021.11.019
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摘要
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通过插层剂辅助超声剥离水滑石，获得剥离充分的LDHNSs分散液；采用原位聚合的方法制备PI/LDHNSs复合薄膜，并对该类复合材料的电学性能进行深入研究。结果表明：LDHNSs在PI基体中分散均匀，未出现明显的团聚和堆叠现象，与基体之间展现出比较好的界面相容性。相较于纯PI薄膜，LDHNSs的加入使复合薄膜的体积电阻率和电气强度出现一定程度的降低；但值得注意的是，复合薄膜的耐电晕寿命明显得到提升；当LDHNSs质量分数为0.5%时，复合薄膜的耐电晕寿命最长，约为纯PI薄膜的8倍，实现了在较低添加量下对复合薄膜耐电晕性能的最大提升。

聚酰亚胺  /  二维纳米材料  /  水滑石  /  耐电晕

LDHNSs dispersion was obtained by ultrasonic stripping of hydrotalcite assisted with intercalation agent. PI/LDHNSS composite films were prepared by in-situ polymerization, and their electrical properties were studied. The results show that the LDHNSs disperse uniformly in PI matrix without obvious agglomeration and stacking, which show good interfacial compatibility with the matrix. Compared with pure PI film, the volume resistivity and electric strength of the composite films decrease slightly to some extent with the addition of LDHNSs. However, it should be note that the corona resistance life of the composite film is improved significantly. When the mass fraction of LDHNSs is 0.5%, the corona resistance life of the composite film is the longest, which is about 8 times longer than that of pure PI, realizing the maximum improvement of corona resistance performance for composite at a relatively low addition amount.

polyimides  /  two-dimension nano materials  /  hydrotalcite  /  corona resistance
刘会, 马莉莉, 郭海泉, 郝春成, 张洪. PI/LDHNSs复合薄膜的制备及电性能研究. 绝缘材料, 2021 , 54 (11) : 130 -133 . DOI: 10.16790/j.cnki.1009-9239.im.2021.11.019
Hui LIU, Lili MA, Haiquan GUO, Chuncheng HAO, Hong ZHANG. Preparation and Electrical Properties of Polyimide/LDHNSs Composite Films[J]. Insulating Materials, 2021 , 54 (11) : 130 -133 . DOI: 10.16790/j.cnki.1009-9239.im.2021.11.019
正文
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0 引言
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在高功率变频电机中，绝缘材料在高频脉冲电压作用下过早电晕老化，威胁到电机的可靠运行。因此绝缘材料是保证变频电机、电器运行可靠性的关键材料，也是决定其寿命的关键材料[1-4]。聚酰亚胺（PI）作为一种性能优异的有机绝缘材料，具有非常好的耐电晕特性和热稳定性，是高频电机内部的主要绝缘材料。通过向聚酰亚胺中添加无机纳米材料得到的聚酰亚胺纳米复合材料，是目前耐电晕性能最好的绝缘材料之一[5-7]。
目前用于制备耐电晕聚酰亚胺纳米复合材料的纳米材料主要有Al2O3、SiO2、TiO2、BN、水滑石（LDHs）等[8-11]。其中LDHs具有良好的光热稳定性及紫外阻隔特性，可对层间有机分子产生抗老化作用，从而延长其使用寿命，同时主体层板可有效抑制光活性分子降解、电离等失活反应的发生，有助于解决有机功能高分子稳定性差、使用寿命短等问题[12]。
本文主要在原有的工作基础上，通过全氟辛基磺酸钾（FS）对LDHs进行深入插层剥离，从中分离出层数少、剥离效果好的水滑石纳米片（LDHNSs），并采用原位聚合的方式，将LDHNSs引入到聚酰亚胺基体，并对复合薄膜的电学性能进行研究。
1 实验
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1.1 原材料与仪器
镁铝水滑石（Mg/Al-LDHs），Sigma-Aldrich公司；全氟辛基磺酸钾（FS），纯度为98%，武汉赛沃尔化工有限公司；无水乙醇，分析纯，天津市巴斯夫化工有限公司；N,N-二甲基乙酰胺（DMAc），分析纯，阿拉丁试剂（上海）有限公司；均苯四甲酸二酐（PMDA），纯度为99%，阿拉丁试剂(上海)有限公司；4,4′-二氨基二苯醚（ODA），纯度为98%，阿拉丁试剂（上海）有限公司。
Vertex70型红外光谱仪，德国Bruker公司；D/max-2500PC型X-射线衍射仪，日本理学株式会社；SBC-12型离子溅射仪，北京中科科仪股份有限公司；Nova-Nano450型扫描电镜，美国FEI公司；ZC-90G型高阻计，上海太欧电子有限公司；MS2674型耐压测试仪，南京民盛电子仪器有限公司；JGM-3H型高频脉冲绝缘测试仪，上海申发检测仪器有限公司。
1.2 LDHNSs的制备
LDHNSs的制备过程已在前期的论文中[13]详细描述。简单来讲，将2.00 g的Mg/Al-LDHs和1.96 g的FS分散于去离子水中，室温下搅拌均匀并反应1周，将所得产物抽滤，用去离子水洗涤至中性，60℃真空干燥12 h，将所得产物LDH-FS分散到DMAc中，室温下超声48 h。取上层清液离心20 min（转速为3 500 r/min），抽滤，可得一定浓度的LDHNSs溶液。
1.3 PI/LDHNSs复合薄膜的制备
称取一定质量的LDHNSs溶液，取适量ODA加入到三口烧瓶中，超声分散后，在冰浴条件下通N2搅拌，加入适量的PMDA机械搅拌24 h，经过薄膜涂覆、热亚胺化，最终得到LDHNSs质量分数分别为0.25%、0.5%、1%、1.5%、2.5%和5%的PI/0.25LDHNSs、PI/0.5LDHNSs、PI/1LDHNSs、PI/1.5LDHNSs、PI/2.5LDHNSs及PI/5LDHNSs复合薄膜，实验过程如图1所示。
2 结果与讨论
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图2是PI/LDHNSs复合薄膜的红外光谱图。从图2可以看出，1 776、1 712、720、1 370 cm-1处的四组特征吸收峰分别对应C=O的不对称、对称和弯曲振动的特征吸收峰以及C-N键的伸缩振动吸收峰，同时在2 940 cm-1处并未观察到-COOH的伸缩振动吸收峰，证实了复合薄膜聚酰亚胺结构的形成以及亚胺化的完全。
图3为PI/LDHNSs复合薄膜的XRD图谱。从图3可以看出，随着LDHNSs填料的增加，没有观察到明显的衍射峰，这是剥离型复合薄膜中LDHs原始的有序堆叠结构被破坏所致。
图4是PI/LDHNSs复合薄膜的断面SEM图。从图4可以看出，PI/LDHNSs复合薄膜的断面整体比较平整，并且随着LDHNSs的添加量增多，在聚合物基体中未见有明显的堆叠团聚现象，仅有少数较厚的纳米片在脆断过程中被拔出聚合物基体，而层数相对较少的纳米片与聚合物基体能很好地融合在一起。说明通过深入插层剥离来获得层数少、剥离效果好的LDHNSs，可以有效地提升LDHNSs在聚酰亚胺基体中的均匀分散性以及与聚合物基体之间的界面相容性。同时，插层剂的空间位阻作用也进一步提高了LDHNSs在聚合物基体中的分散性。
图5是PI/LDHNSs复合薄膜的体积电阻率。从图5可以看出，在LDHNSs添加量较少时，复合薄膜的体积电阻率大幅降低，随着LDHNSs含量的增加，体积电阻率逐步下降。除了服从复相材料的共混原则外，LDHNSs自身带正电的属性可以结合部分负极性电荷，一定程度上延缓了电荷的积聚，同时LDHNSs在聚酰亚胺基体中的均匀分散所带来的优势得到凸显，与聚酰亚胺基体间的界面作用区域增多，在基体中连接形成的导电网络有利于电子的传输。同时相应复合薄膜的结晶化程度下降，高分子链定向趋势下降，电子迁移率增加，因而电阻率也相应降低。
图6(a)、(b)分别为PI/LDHNSs复合薄膜的直流电气强度和交流电气强度的威布尔分布图，电气强度和分布参数详见表1。整体上PI/LDHNSs复合薄膜的电气强度均低于纯聚酰亚胺薄膜的电气强度。主要原因是LDHNSs的正电性会增大电击穿的概率，剥离程度加大的同时也引入了缺陷，界面陷阱增多，导致复合薄膜的电气强度相比于纯PI有所降低。
从表1以及图6可知，随着LDHNSs含量的增加，β变化幅值较小，侧面反映了随LDHNSs含量增加所带来的分布不均现象不明显，说明插层-超声辅助剥离法是有效提高水滑石在聚酰亚胺基体中均匀分散的一种方式。
图7是PI/LDHNSs复合薄膜的耐电晕寿命曲线。从图7可以看出，LDHNSs的加入可以提高复合薄膜的耐电晕寿命。主要是因为LDHNSs具备对小分子迁移的阻隔能力，其表面的正电荷可以吸附大量阴离子，延缓电子对分子链的破坏或热降解，延长了局部放电的破坏通道，从而提高了复合薄膜的耐电晕寿命。但因为复合薄膜中LDHNSs含量均较低，所以从实验结果上看，耐电晕时间与LDHNSs含量间没有明显的依赖关系，但复合薄膜的耐电晕性能总体均得到提升。
3 结论
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LDHNSs二维纳米材料在聚合物基体中分散均匀，与聚合物基体之间表现出非常好的界面相容性。片状LDHNSs具备对小分子迁移的阻隔能力，延长了局部放电的破坏通道，从而提高了复合薄膜的耐电晕寿命，当LDHNSs质量分数为0.5%时，复合薄膜的耐电晕寿命最长，约为纯PI薄膜的8倍，实现了在较低添加量时，对复合薄膜耐电晕性能的最大提升。
基金
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  • 新能源电力系统国家重点实验室开放课题(LAPS21022)
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2021年第54卷第11期
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doi: 10.16790/j.cnki.1009-9239.im.2021.11.019
  • 接收时间：2021-05-11
  • 首发时间：2026-03-23
  • 出版时间：2021-11-22
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  • 收稿日期：2021-05-11
  • 修回日期：2021-06-01
基金
新能源电力系统国家重点实验室开放课题(LAPS21022)
作者信息
    1青岛科技大学 材料科学与工程学院，山东 青岛 266042
    2华北电力大学 新能源电力系统 国家重点实验室，北京 102206
    3中国科学院长春应用化学研究所 高分子复合材料工程实验室， 吉林 长春 130022

通讯作者:

马莉莉（1987-），女（汉族），山东德州人，讲师，博士，研究方向为聚酰亚胺基复合材料的性能调控研究。
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https://castjournals.cast.org.cn/joweb/jycl/CN/10.16790/j.cnki.1009-9239.im.2021.11.019
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2种不同金属材料的力学参数
科
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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