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Article(id=1210613542311555272, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1210613541111984320, articleNumber=null, orderNo=null, doi=10.16790/j.cnki.1009-9239.im.2024.11.003, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1718121600000, receivedDateStr=2024-06-12, revisedDate=1722700800000, revisedDateStr=2024-08-04, acceptedDate=null, acceptedDateStr=null, onlineDate=1766562360599, onlineDateStr=2025-12-24, pubDate=1732032000000, pubDateStr=2024-11-20, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1766562360599, onlineIssueDateStr=2025-12-24, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1766562360599, creator=13701087609, updateTime=1766562360599, updator=13701087609, issue=Issue{id=1210613541111984320, tenantId=1146029695717560320, journalId=1149653034449285133, year='2024', volume='57', issue='11', pageStart='1', pageEnd='143', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1766562360313, creator=13701087609, updateTime=1766564044072, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1210620603392987671, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1210613541111984320, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1210620603392987672, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1210613541111984320, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=34, endPage=39, ext={EN=ArticleExt(id=1210613542621933775, articleId=1210613542311555272, tenantId=1146029695717560320, journalId=1149653034449285133, language=EN, title=Preparation and performance analysis of ANF/mica composite insulating paper, columnId=1210613542542241998, journalTitle=Insulating Materials, columnName=Special Issue on Key Materials and Technology for New Energy Vehicles, runingTitle=null, highlight=null, articleAbstract=

An ANF/mica composite insulating paper was prepared by vacuum assisted filtration and hot pressing technology taking aramide nanofiber (ANF) as matrix and natural mica (mica) as filler. The microscopic morphology, tensile strength, electrical insulation properties, and temperature resistance of the composite insulating paper were studied systematically. The results show that the mica and ANF are superimposed in order during vacuum filtration process, and the mica fragments fill the gaps in paper effectively, creating a dense "brick-and-mortar structure", which significantly enhances the electric strength and insulating properties of the composite insulating paper. Furthermore, the glass transition temperatures of pure ANF insulating paper and ANF/mica-10 composite insulating paper are higher than 300℃, exhibiting excellent thermal stability. Although the addition of mica slightly reduces the tensile properties of pure ANF insulating paper, its insulation strength and tensile performance remain superior to traditional mica paper.

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以芳纶纳米纤维（ANF）为基体，天然云母（mica）为填料，通过真空辅助抽滤和热压技术制备了ANF/mica复合绝缘纸，并系统研究了复合绝缘纸的微观形貌、拉伸特性、电绝缘性能以及耐温性能。结果表明：mica与ANF在真空抽滤过程中有序叠加，mica碎片有效填补了纸张中的空隙，形成致密的“砖泥结构”，显著提高了复合绝缘纸的电气强度和绝缘性能。此外，纯ANF绝缘纸和ANF/mica-10复合绝缘纸的玻璃化转变温度均高于300℃，展现出优异的热稳定性。虽然mica的加入稍微降低了纯ANF绝缘纸的拉伸性能，但其绝缘强度和拉伸性能仍明显优于传统云母纸。

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任俊文（1987-），男（汉族），四川成都人，副研究员，主要从事高电压与绝缘技术的研究。
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赵莉华（1968-），女（汉族），四川成都人，副教授，主要从事变压器绝缘及状态检测技术的研究。

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赵莉华（1968-），女（汉族），四川成都人，副教授，主要从事变压器绝缘及状态检测技术的研究。

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赵莉华（1968-），女（汉族），四川成都人，副教授，主要从事变压器绝缘及状态检测技术的研究。

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ANF/mica复合绝缘纸的制备及性能分析
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赵莉华 1 , 滕富莉 1 , 魏佳 1 , 高萌 2 , 卞超 1 , 卓然 2 , 卿湫惋喻 1 , 任俊文 1
绝缘材料 | 新能源汽车用关键材料与技术专题 2024,57(11): 34-39
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绝缘材料 | 新能源汽车用关键材料与技术专题 2024, 57(11): 34-39
ANF/mica复合绝缘纸的制备及性能分析
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赵莉华1, 滕富莉1, 魏佳1, 高萌2, 卞超1, 卓然2, 卿湫惋喻1, 任俊文1
作者信息
  • 1四川大学 电气工程学院，四川 成都 610065
  • 2南方电网公司电力科学研究院有限公司，广东 广州 510623

    • 赵莉华（1968-），女（汉族），四川成都人，副教授，主要从事变压器绝缘及状态检测技术的研究。

通讯作者:

任俊文（1987-），男（汉族），四川成都人，副研究员，主要从事高电压与绝缘技术的研究。
Preparation and performance analysis of ANF/mica composite insulating paper
Lihua ZHAO1, Fuli TENG1, Jia WEI1, Meng GAO2, Chao BIAN1, Ran ZHUO2, Qiuwanyu QING1, Junwen REN1
Affiliations
  • 1College of Electrical Engineering, Sichuan University, Chengdu 610065, China
  • 2Electric Power Research Institute of CSG, Guangzhou 510623, China
出版时间: 2024-11-20 doi: 10.16790/j.cnki.1009-9239.im.2024.11.003
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摘要
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以芳纶纳米纤维（ANF）为基体，天然云母（mica）为填料，通过真空辅助抽滤和热压技术制备了ANF/mica复合绝缘纸，并系统研究了复合绝缘纸的微观形貌、拉伸特性、电绝缘性能以及耐温性能。结果表明：mica与ANF在真空抽滤过程中有序叠加，mica碎片有效填补了纸张中的空隙，形成致密的“砖泥结构”，显著提高了复合绝缘纸的电气强度和绝缘性能。此外，纯ANF绝缘纸和ANF/mica-10复合绝缘纸的玻璃化转变温度均高于300℃，展现出优异的热稳定性。虽然mica的加入稍微降低了纯ANF绝缘纸的拉伸性能，但其绝缘强度和拉伸性能仍明显优于传统云母纸。

芳纶纳米纤维  /  天然云母  /  复合绝缘纸  /  拉伸特性  /  电气强度

An ANF/mica composite insulating paper was prepared by vacuum assisted filtration and hot pressing technology taking aramide nanofiber (ANF) as matrix and natural mica (mica) as filler. The microscopic morphology, tensile strength, electrical insulation properties, and temperature resistance of the composite insulating paper were studied systematically. The results show that the mica and ANF are superimposed in order during vacuum filtration process, and the mica fragments fill the gaps in paper effectively, creating a dense "brick-and-mortar structure", which significantly enhances the electric strength and insulating properties of the composite insulating paper. Furthermore, the glass transition temperatures of pure ANF insulating paper and ANF/mica-10 composite insulating paper are higher than 300℃, exhibiting excellent thermal stability. Although the addition of mica slightly reduces the tensile properties of pure ANF insulating paper, its insulation strength and tensile performance remain superior to traditional mica paper.

aramid nanofibers  /  natural mica  /  composite insulating paper  /  tensile properties  /  electric strength
赵莉华, 滕富莉, 魏佳, 高萌, 卞超, 卓然, 卿湫惋喻, 任俊文. ANF/mica复合绝缘纸的制备及性能分析. 绝缘材料, 2024 , 57 (11) : 34 -39 . DOI: 10.16790/j.cnki.1009-9239.im.2024.11.003
Lihua ZHAO, Fuli TENG, Jia WEI, Meng GAO, Chao BIAN, Ran ZHUO, Qiuwanyu QING, Junwen REN. Preparation and performance analysis of ANF/mica composite insulating paper[J]. Insulating Materials, 2024 , 57 (11) : 34 -39 . DOI: 10.16790/j.cnki.1009-9239.im.2024.11.003
正文
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0 引言
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近些年，随着新能源汽车对电机系统性能要求的不断提高，电机系统朝着高速高效、轻量化和高可靠性方向发展，相应地对绝缘材料的性能要求也不断提高[1-3]。在此背景下，为满足安全性、稳定性和耐用性的需求，新型绝缘材料应运而生，成为推动电机技术进步的关键。
云母作为一种无机耐高温绝缘材料，具有优异的电性能、耐热性能、耐化学性能、耐电晕性和低成本等特点，在绝缘系统中被广泛应用[4-5]。纯云母纸虽具有优异的电性能，但云母片（mica）之间范德华力较弱且界面作用差，制成的纯云母纸力学特性差，纸张非常脆且易碎[6]。芳纶纤维（AF）具有优异的拉伸强度、模量和耐高温性能[7-8]，常被用作补强材料来提高云母纸的韧性和拉伸强度，芳纶云母纸就是基于云母纸和芳纶绝缘纸的发展趋势而出现的新型复合材料，已经应用在建材、航空、国防等多个领域[9-11]。现有研究大多着眼于利用AF作为力学增韧剂来改善芳纶云母纸的力学性能，H MITSUI等[12]研究发现加入少量AF可以提高纸张的剪切强度、透气性及热稳定性，但降低了纸张的电气强度。张翼等[13]研究发现天然纤维与mica复合可以改善纸张的拉伸强度，但纸张的电气性能降低。王腊梅等[14]研究发现芳纶短切纤维和芳纶浆粕的加入改善了芳纶云母纸的力学性能、耐温性等，但在一定程度上降低了芳纶云母纸的绝缘性能。从上述研究成果可以看出，通过添加AF可以增强芳纶云母纸的韧性和强度，但芳纶云母纸整体的韧性和强度仍较低，且随着纤维的加入，芳纶云母纸的电气强度遭到破坏，无法充分发挥芳纶云母纸的高绝缘特性。
将AF进行剥离制成的芳纶纳米纤维（ANF）不仅具有AF的优异性能，并且拥有超高的长径比（径向尺寸为纳米级，长度为微米级）和丰富的活性基团（如酰胺基团等），有效解决了AF反应活性能和表面光滑等问题，成为制备高性能绝缘纸的理想选择[15-16]。TAN J J等[17]发现相较于传统芳纶绝缘纸，ANF绝缘纸具有更加致密的结构，更加优异的力学性能、电气性能和耐高温性能。进一步地，ANF展现出的优异特性不仅有利于提升ANF之间的相互作用，形成致密网络结构，也为灵活设计功能芳纶绝缘纸提供了基础。例如，研究者利用氮化硼纳米片作为导热基元与ANF共同构筑了一系列兼具高力学强度、高导热特性的ANF复合绝缘纸[18-19]。由此可得，利用ANF作为构筑单元可以改善云母纸的力学强度和绝缘特性。然而，传统的云母复合绝缘纸是以ANF为填充材料，虽然可以在一定程度上改善纯云母纸的力学性能，但会破坏纯云母纸的绝缘性能。因此，如何有效地将ANF和mica进行复合，解决它们在结合过程中可能出现的问题，如相容性、界面效应等，是当前亟需解决的瓶颈问题之一。
天然珍珠母贝壳以其高度有序的“砖泥结构”和精细的界面分子设计，实现了高强度与高韧性的协同提升，成为学者们广泛研究和模仿的模型[20]。LI Y J等[21]通过分子内氢键作用在介质薄膜内形成致密的层状微结构，从而显著提升薄膜的电气强度和热稳定性。CHEN J等[22]通过将BNNS与聚合物纳米纤维结合，构建了仿珍珠母贝壳结构的三维高效导热网络，获得高热导率与高力学强度的绝缘介质材料。
综上，本文以ANF为基体，mica为填料，通过真空辅助抽滤及热压的方式制备具有“砖泥结构”的ANF/mica复合绝缘纸，并研究mica含量对复合绝缘纸微观形貌、拉伸强度以及击穿特性的影响规律。
1 实验
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1.1 主要原材料
凯夫拉尔纤维（Kevlar 29®纤维），黄色，400D，平均直径为12 μm，东莞市索维特特殊线带有限公司；天然云母，透明浅银色，100目，宁波双洋电工材料有限公司；十六烷基三甲基溴化铵，白色，上海阿拉丁生化科技公司；其他试剂，均为分析纯，中国成都科龙化学试剂有限公司。
1.2 ANF/mica复合绝缘纸的制备
（1）称取1 g mica和1 g十六烷基三甲基溴化铵分散在无水乙醇中，充分搅拌后超声处理30 min，随后用无水乙醇反复彻底清洗，在45℃真空环境下干燥24 h后得到干净的mica粉末备用。称取适量mica粉末，加入20 g二甲基亚砜（DMSO），经超声处理30 min，制得mica/DMSO分散液。
（2）将Kevlar 29®纤维剪碎至长度为0.5 cm的小段，利用丙酮浸泡，辅以超声清洗，过滤掉丙酮后在45℃真空环境下干燥，密封储存。称取处理过的Kevlar 29®纤维（1 g）加入到KOH浓碱溶液（2 g KOH和10 mL去离子水）和二甲基亚砜（DMSO）（500 mL）的混合溶液中，室温下避光搅拌7天，得到暗红色的ANF/DMSO分散液。
（3）称取20 g ANF/DMSO分散液，加入60 g的DMSO进行稀释处理，加入Mica/DMSO分散液与之混合，并加入DMSO总体积的4%的去离子水进行质子化处理，然后将混合溶液进行水浴超声、乳化剪切后得到复合浆料，将复合浆料转移至抽滤瓶中，真空抽滤成膜，并依次浸入乙醇、去离子水中，通过溶胶凝胶法去除残留的DMSO、十六烷基三甲基溴化铵，最后热压、干燥得到ANF/mica复合绝缘纸，其中mica质量分数分别为0%、5%、10%、15%、20%的样品分别命名为纯ANF绝缘纸、ANF/Mica-5、ANF/Mica-10、ANF/Mica-15、ANF/Mica-20。
1.3 测试方法
采用扫描电子显微镜（FEI公司，型号为Quanta 250 FEG）观察ANF、mica及复合绝缘纸的微观结构；采用透射电子显微镜（JEOL公司，型号为JEM-2100F）分析ANF的局部微观形貌；使用电子万能试验机（英斯特朗试验设备贸易有限公司，型号为 Instron 2340）测试复合绝缘纸的拉伸性能；利用电击穿试验机（北京科朗测量仪器有限公司，型号为DDJ50kV）测定复合绝缘纸的电气强度及体积电阻率；借助差示扫描量热仪（美国TA公司，型号为Q2000）测试复合绝缘纸的耐温性能，并绘制DSC曲线。
2 结果与讨论
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2.1 微观形貌结构分析
2.1.1 Kevlar 29®纤维、ANF及mica微观形貌
图1为Kevlar 29®纤维、ANF及mica的微观形貌图。
从图1(a)可以看出，单根Kevlar 29®纤维的直径约为12 μm，表面光滑无破损，呈化学惰性，与填充物之间界面作用差；而经过浓碱去质子化制备的ANF呈细长弯曲的网丝状，其相互缠绕呈网状结构，如图1(b)所示。ANF直径约为30 nm，长度达几微米以上，具有较高的长径比。从图1(c)可以看出，处理后的mica呈片状结构，且表面光滑平整无杂物，径厚比较大。另外，在十六烷基三甲基溴化铵和超声波共同作用下，mica产生轻微细碎化，出现小粒径鳞片，在一定程度上起到填充纸张空隙的作用。但大量mica碎片的出现会削弱其本身的绝缘性能，影响其综合利用价值[23]。
2.1.2 ANF/Mica复合绝缘纸微观形貌
图2为不同mica含量复合绝缘纸和ANF/mica-10溶液的SEM表征结果。
从图2(a)可以看出，纯ANF绝缘纸的纤维之间紧密结合，形成致密的结构，但无明显的层状结构。从图2(b)～(e)可以看出，随着Mica的加入，在真空辅助抽滤过程中，片状mica的堆积减少了细微ANF通过微孔滤膜的损失，二者有序叠加，辅之以溶胶凝胶法改善真空抽滤带来的两面差，形成致密的“砖泥结构”。从图2(c)可以看出，当mica质量分数为10%时，mica平整地嵌入ANF之间，mica碎片填补了ANF中的空隙，弥补了纯ANF绝缘纸的缺陷，表现出高度致密的层状结构，有利于提高复合绝缘纸的整体性能。图2(f)为ANF/mica-10溶液的SEM图，从图中可以看出mica被ANF紧密缠绕、包覆，直观地表现出ANF的“泥”与片状mica的“砖”之间的紧密结构。
2.2 拉伸特性
ANF/mica复合绝缘纸的应力-应变关系、弹性模量及拉伸强度测试结果如图3所示。
由于ANF表面具有丰富的活性基团，分子内能形成广泛的氢键作用和苯环的π-π共轭作用，因此纤维之间结合紧密，纯ANF绝缘纸表现出优异的拉伸特性。从图3可以看出，纯ANF绝缘纸的拉伸强度、拉伸应变和弹性模量分别达到了265.33 MPa、17.5%、5.76 GPa，ANF/mica的拉伸强度、拉伸应变和弹性模量随着mica含量的增加而逐渐降低。虽然mica的加入有助于在ANF/mica复合绝缘纸内部构筑“砖泥结构”，但也在一定程度上带来了界面效应，导致应力分布不均匀，多数集中在复合绝缘纸界面薄弱处，从而劣化复合绝缘纸的力学性能，最终使材料损伤断裂。虽然mica的加入劣化了纯ANF绝缘纸的拉伸特性，但相对于纯云母纸以及利用AF作为补强材料的芳纶云母纸[13-14]，ANF/mica-10复合绝缘纸的拉伸特性仍较好，拉伸强度、应变和弹性模量分别为171.41 MPa、11.81%、4.89 GPa。
2.3 绝缘性能
绝缘纸的电绝缘性能对于电气设备的正常运行至关重要，对纯ANF绝缘纸和ANF/mica复合绝缘纸在500 V/s的高直流电压升压速率下的电气强度和直流1 000 V下的体积电阻率进行测试，结果如图4和图5所示。
从图4可以看出，ANF/mica-10复合绝缘纸的电气强度为247.14 kV/mm，相较于纯ANF绝缘纸（187.45 kV/mm）提升了31.8%。这主要得益于mica本身优异的电气强度，mica的加入显著改善了ANF/mica复合绝缘纸的电气强度。ANF/mica-10复合绝缘纸具有致密的“砖泥结构”，且适量的mica碎片填补了纸张中的空隙，从而促进了电荷的横向耗散，为电树枝的发展提供了曲折的路径。然而，随着mica含量的进一步增加，ANF/mica复合绝缘纸出现结构缺陷，并且mica碎片的增加不利于发挥其优异的电绝缘特性，导致复合绝缘纸的电气强度下降。
从图5可以看出，纯ANF绝缘纸和ANF/mica复合绝缘纸均具有较高体积电阻率（>1012 Ω·cm），表明它们都具有优良的电绝缘性能。其中，纯ANF绝缘纸的体积电阻率为5.1×1013 Ω·cm，而ANF/mica-20复合绝缘纸的体积电阻率为5.6×1012 Ω·cm。这一体积电阻率的略微下降是由于高含量mica的团聚导致的，并且在复合绝缘纸中引入了空隙和缺陷。
2.4 耐温性能
纯ANF绝缘纸和ANF/mica-10复合绝缘纸的DSC曲线如图6所示。
从图6可以看出，纯ANF绝缘纸和ANF/mica-10复合绝缘纸在温度为100～300℃内未出现明显的吸收峰，说明其玻璃化转变温度高于300℃。纯ANF绝缘纸因其内部存在强氢键作用和苯环π-π共轭作用，展现出优异的热稳定性[24]。引入mica后，绝缘纸内部形成“砖泥结构”，这限制了大分子链的流动，增强了材料内部的作用力，使得ANF/mica-10复合绝缘纸同样具有优异的热稳定性。
3 结论
收起
本文通过复合ANF和mica，制备出具有“砖泥结构”的ANF/mica复合绝缘纸，并对其微观结构、拉伸特性、绝缘性能以及耐温性能进行了深入研究，主要得到以下结论：
（1）十六烷基三甲基溴化铵和超声处理的共同作用有利于提升mica表面活性，增强其在ANF基体间的界面粘结力，同时产生mica碎片。
（2）在真空辅助抽滤下，mica与ANF有序堆叠，而Mica碎片可以填补复合绝缘纸内部的空隙，有利于形成致密的“砖泥结构”。
（3）虽然mica在复合绝缘纸内部产生界面效应导致复合绝缘纸的拉伸性能下降，但ANF/mica-10复合绝缘纸的拉伸特性仍相对较好。
（4）mica为电树枝的发展提供了曲折的路径，显著改善ANF/mica复合绝缘纸的电气强度。然而，高含量mica不仅使绝缘纸出现结构缺陷，而且带来更多的mica碎片，不利于发挥其优异的电绝缘特性，导致复合绝缘纸电气强度和体积电阻率的下降。
（5）纯ANF绝缘纸和ANF/mica-10复合绝缘纸均展现出优异的热稳定性，其玻璃化转变温度均高于300℃。
基金
收起
  • 国家自然科学基金资助项目(52107020)
  • 四川省重点研发项目(2023YFG0236)
  • 电力设备电气绝缘国家重点实验室开放基金项目(EIPE23210)
文献
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2024年第57卷第11期
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doi: 10.16790/j.cnki.1009-9239.im.2024.11.003
  • 接收时间：2024-06-12
  • 首发时间：2025-12-24
  • 出版时间：2024-11-20
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  • 收稿日期：2024-06-12
  • 修回日期：2024-08-04
基金
国家自然科学基金资助项目(52107020)
四川省重点研发项目(2023YFG0236)
电力设备电气绝缘国家重点实验室开放基金项目(EIPE23210)
作者信息
    1四川大学 电气工程学院，四川 成都 610065
    2南方电网公司电力科学研究院有限公司，广东 广州 510623

通讯作者:

任俊文（1987-），男（汉族），四川成都人，副研究员，主要从事高电压与绝缘技术的研究。
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2种不同金属材料的力学参数
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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
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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
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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