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Article(id=1198665393033278328, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1198665390676083408, articleNumber=null, orderNo=null, doi=10.16790/j.cnki.1009-9239.im.2023.03.002, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1646841600000, receivedDateStr=2022-03-10, revisedDate=1650297600000, revisedDateStr=2022-04-19, acceptedDate=null, acceptedDateStr=null, onlineDate=1763713699825, onlineDateStr=2025-11-21, pubDate=1679241600000, pubDateStr=2023-03-20, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1763713699825, onlineIssueDateStr=2025-11-21, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1763713699825, creator=13701087609, updateTime=1763713699825, updator=13701087609, issue=Issue{id=1198665390676083408, tenantId=1146029695717560320, journalId=1149653034449285133, year='2023', volume='56', issue='3', pageStart='1', pageEnd='121', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1763713699263, creator=13701087609, updateTime=1766563510720, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1210618366327386648, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1198665390676083408, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1210618366327386649, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1198665390676083408, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=9, endPage=13, ext={EN=ArticleExt(id=1198665393494651773, articleId=1198665393033278328, tenantId=1146029695717560320, journalId=1149653034449285133, language=EN, title=Surface modification of nano-silica and preparation of corona resistant wire enamel, columnId=1190369066675179686, journalTitle=Insulating Materials, columnName=Material Research, runingTitle=null, highlight=null, articleAbstract=

The problem of nanoparticle agglomeration in wire enamel can be solved by modification and gradual dispersion of nanoparticles. Five modifiers, emulsifier OP-10, silane coupling agent AP1231, silane coupling agent A112, γ-propyl trimethoxysilane (KH560), and N-[3-(trimethoxysilyl) propyl] ethylenediamine (KH-792), were used to modify the surface of nano silica particles. The effects of modifier type, modifier dosage, modification temperature and time on the modification effect of nano-SiO2 particles were explored. The effects of nano-SiO2 particles before and after modification on the performance of corona resistant wire enamel were compared by corona resistance test, and the dispersion of nano-SiO2 particles before and after modification was observed by transmission electron microscopy (TEM). The results indicate that the nanoparticles modified by KH-560 have the best dispersion in wire enamel, and the best process conditions are as follows: the dosage of KH-560 is 1.5wt%, the modification temperature is 90℃, and the modification time is 4 h. The wire enamel with high stability and higher than 50 h of corona resistance time can be obtained by gradually dispersing modified nanoparticles into the wire enamel, and the appropriate addition amount of nanoparticles is 13.5wt%.

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采用纳米粒子改性、逐步分散的方法解决漆包线漆中纳米粒子团聚的难题。分别用乳化剂OP-10、硅烷偶联剂AP1231、硅烷偶联剂A112、γ-丙基三甲氧基硅烷（KH-560）和N-[3-(三甲氧基硅基)丙基]乙二胺（KH-792）5种改性剂对纳米SiO2粒子表面进行改性，研究改性剂种类、改性剂用量、改性温度及改性时间对纳米SiO2粒子改性效果的影响，通过耐电晕性能测试对比了改性前后的纳米SiO2粒子对耐电晕漆包线漆性能的影响，并用透射电子显微镜（TEM）观察改性前后纳米SiO2粒子的分散状况。结果表明：经KH-560改性后的纳米SiO2在漆包线漆中分散性最好，其最佳工艺条件为：KH-560质量分数为1.5%，改性温度为90℃，改性时间为4 h。将改性后的纳米SiO2逐步均匀分散到漆包线漆中，可以得到高稳定性、耐电晕时间＞50 h的漆包线漆，适宜的纳米SiO2添加量为13.5%。

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周剑林（1982-），男（汉族），湖南常德人，讲师，主要从事纳米材料、绝缘材料的应用研究。
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成昊霖（2000-），男（汉族），湖南湘潭人，硕士生，主要从事高分子材料及纳米SiO2表面改性的研究。

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成昊霖（2000-），男（汉族），湖南湘潭人，硕士生，主要从事高分子材料及纳米SiO2表面改性的研究。

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成昊霖（2000-），男（汉族），湖南湘潭人，硕士生，主要从事高分子材料及纳米SiO2表面改性的研究。

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纳米SiO2表面改性及耐电晕漆包线漆的制备
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成昊霖 1 , 周剑林 2, 3 , 曾荣今 1
绝缘材料 | 材料研究 2023,56(3): 9-13
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绝缘材料 | 材料研究 2023, 56(3): 9-13
纳米SiO2表面改性及耐电晕漆包线漆的制备
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成昊霖1, 周剑林2, 3, 曾荣今1
作者信息
  • 1湖南科技大学，化学化工学院，湖南 湘潭 411201
  • 2湖南科技大学，煤炭资源清洁利用与矿山环境保护湖南省重点实验室，湖南 湘潭 411201
  • 3湖南科技大学，资源环境与安全工程学院，湖南 湘潭 411201

    • 成昊霖（2000-），男（汉族），湖南湘潭人，硕士生，主要从事高分子材料及纳米SiO2表面改性的研究。

通讯作者:

周剑林（1982-），男（汉族），湖南常德人，讲师，主要从事纳米材料、绝缘材料的应用研究。
Surface modification of nano-silica and preparation of corona resistant wire enamel
Haolin CHENG1, Jianlin ZHOU2, 3, Rongjin ZENG1
Affiliations
  • 1College of Chemistry and Chemical Engineering, Environment and Safety Engineering, Environment and Safety Engineering, Hunan University of Science and Technology, Xiangtan 411201, China
  • 2Hunan Provincial Key Laboratory of Coal Resources Clean Utilization and Mine Environment Protection, Environment and Safety Engineering, Environment and Safety Engineering, Hunan University of Science and Technology, Xiangtan 411201, China
  • 3School of Resources, Environment and Safety Engineering, Hunan University of Science and Technology, Xiangtan 411201, China
出版时间: 2023-03-20 doi: 10.16790/j.cnki.1009-9239.im.2023.03.002
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摘要
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采用纳米粒子改性、逐步分散的方法解决漆包线漆中纳米粒子团聚的难题。分别用乳化剂OP-10、硅烷偶联剂AP1231、硅烷偶联剂A112、γ-丙基三甲氧基硅烷（KH-560）和N-[3-(三甲氧基硅基)丙基]乙二胺（KH-792）5种改性剂对纳米SiO2粒子表面进行改性，研究改性剂种类、改性剂用量、改性温度及改性时间对纳米SiO2粒子改性效果的影响，通过耐电晕性能测试对比了改性前后的纳米SiO2粒子对耐电晕漆包线漆性能的影响，并用透射电子显微镜（TEM）观察改性前后纳米SiO2粒子的分散状况。结果表明：经KH-560改性后的纳米SiO2在漆包线漆中分散性最好，其最佳工艺条件为：KH-560质量分数为1.5%，改性温度为90℃，改性时间为4 h。将改性后的纳米SiO2逐步均匀分散到漆包线漆中，可以得到高稳定性、耐电晕时间＞50 h的漆包线漆，适宜的纳米SiO2添加量为13.5%。

纳米SiO2  /  改性  /  漆包线漆  /  耐电晕性

The problem of nanoparticle agglomeration in wire enamel can be solved by modification and gradual dispersion of nanoparticles. Five modifiers, emulsifier OP-10, silane coupling agent AP1231, silane coupling agent A112, γ-propyl trimethoxysilane (KH560), and N-[3-(trimethoxysilyl) propyl] ethylenediamine (KH-792), were used to modify the surface of nano silica particles. The effects of modifier type, modifier dosage, modification temperature and time on the modification effect of nano-SiO2 particles were explored. The effects of nano-SiO2 particles before and after modification on the performance of corona resistant wire enamel were compared by corona resistance test, and the dispersion of nano-SiO2 particles before and after modification was observed by transmission electron microscopy (TEM). The results indicate that the nanoparticles modified by KH-560 have the best dispersion in wire enamel, and the best process conditions are as follows: the dosage of KH-560 is 1.5wt%, the modification temperature is 90℃, and the modification time is 4 h. The wire enamel with high stability and higher than 50 h of corona resistance time can be obtained by gradually dispersing modified nanoparticles into the wire enamel, and the appropriate addition amount of nanoparticles is 13.5wt%.

nano-silica  /  modification  /  wire enamel  /  corona resistance
成昊霖, 周剑林, 曾荣今. 纳米SiO2表面改性及耐电晕漆包线漆的制备. 绝缘材料, 2023 , 56 (3) : 9 -13 . DOI: 10.16790/j.cnki.1009-9239.im.2023.03.002
Haolin CHENG, Jianlin ZHOU, Rongjin ZENG. Surface modification of nano-silica and preparation of corona resistant wire enamel[J]. Insulating Materials, 2023 , 56 (3) : 9 -13 . DOI: 10.16790/j.cnki.1009-9239.im.2023.03.002
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0 引言
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新能源汽车是《中国制造2025》指出的重点发展领域。新能源汽车的核心部件是变频驱动电机，而电机绕组匝间的绝缘漆包线在高频脉冲电压作用下产生的强烈局部放电，是目前导致变频电机绝缘破坏的主要原因[1]。变频驱动电机脉冲电压的迅速翻转，在电磁线表面形成较强的反向电场叠加，并且同时存在切向电场，使空间电荷在介质内部逐渐贯穿，导致高分子绝缘层老化。为了适应高瞬时功率、高功率密度、变速工况、强过载能力和大启动转矩等要求，对漆包线的耐电晕性能提出了更高的要求[2]。漆包线的耐电晕能力是由绝缘层材料的耐电晕性能决定的，提升绝缘层材料的耐电晕性能是解决变频电机技术难题的关键[3]。
对于绝缘材料耐电晕性能的研究国外开展较早。1994年，Dupont公司研制出聚酰亚胺（PI）薄膜Kapton 100CR，在20 kV/mm场强下其耐电晕时间是原始薄膜100HN的10倍以上[4]。由Amoco公司最早研制的聚酰胺酰亚胺（PAI）材料，在保留了PI优异性能的基础上，还具有更好的耐磨性而被广泛应用于漆包线漆[5-6]。1994年，T J LWEIS[7]首次提出纳米介质的概念，随后CAO Y等[8]研究表明，相较于传统介质，纳米复合介质具有更优良的耐电晕性能。基于以上研究，易建英[9]采用纳米SiO2粒子与PAI漆共混制备出耐电晕性较好的SiO2复合漆包线漆。但由于纳米SiO2粒子表面含有大量羟基，而羟基具有亲水性，对于漆包线漆来说，大部分分散介质为有机溶剂，因此纳米SiO2粒子表面羟基越多，其在漆包线漆中的分散性和稳定性越不理想[10-11]。为了提高纳米SiO2粒子在漆包线漆中的分散性和稳定性，需要对纳米SiO2粒子进行改性。刘彦生等[12]采用硅烷偶联剂对纳米SiO2粒子进行表面改性，结果发现纳米SiO2在有机材料中的分散性显著提升。尽管目前针对纳米SiO2在有机材料中的分散性研究取得了一定进展，但目前研究对于适宜改性剂的筛选还涉及较少，国内绿色高效的改性工艺也尚未成熟，给国内纳米SiO2改性漆包线漆技术的实际应用带来一定困难。
本研究采用乳化剂OP-10、氨基硅烷低聚物（AP1231）、N-(2-氨乙基)-3-氨丙基三甲氧基硅烷（A112）、γ-丙基三甲氧基硅烷（KH-560）和N-[3-(三甲氧基硅基)丙基]乙二胺（KH-792）5种改性剂分别改性纳米SiO2，比较不同改性剂对纳米SiO2的改性效果，并对改性后的纳米SiO2表面羟基及掺杂纳米SiO2改性后的漆包线漆耐电晕性进行检测，对改性工艺和漆包线漆纳米SiO2添加工艺的相关参数进行优化探究。
1 实验
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1.1 试剂与仪器
纳米SiO2（粒径为20～50 nm，比表面积为200～300 m2/g），AP1231、A112、KH-560、KH-792、乳化剂OP-10，均为纳新化工有限公司生产；二甲苯，分析纯，天津市科密欧化学试剂有限公司；盐酸、氢氧化钠，分析纯，上海麦克林生化科技有限公司；聚酰胺酰亚胺（PAI）漆，艾维特电气绝缘材料（常州）有限公司。
DHG-9030A型电热鼓风干燥箱，上海一恒科学仪器有限公司；CL-4型恒温加热磁力搅拌器，巩义市予华仪器有限责任公司；LAN-10-L型理化分析型超纯水机，重庆力德高端水处理设备研发有限公司；KQ-500DE型数控超声波清洗器，昆山市超声仪器有限公司；DPT-1000S型漆包线耐电晕测试仪，上海迪安电工器材有限公司。
1.2 材料制备
纳米SiO2的改性：按照一定比例称取纳米SiO2和二甲苯溶液，倒入锥形瓶中，在室温下磁力搅拌，30 min后再加入一定量改性剂到溶液中，在室温下继续搅拌，再用乙酸或氨水调节pH至一定值，然后将混合液置于恒温加热磁力搅拌器中，90℃条件下搅拌反应一定时间。待混合液冷却至室温时进行抽滤，对滤饼用无水乙醇洗涤多次，然后将滤饼置于110℃烘箱中烘干，磨碎后备用。
纳米SiO2改性耐电晕漆的制备：称取一定量改性前后的纳米SiO2粒子超声分散在二甲苯溶液中，然后将分散均匀的纳米SiO2浆液逐步滴加到聚酰胺酰亚胺漆中，获得耐电晕漆，备用。
耐电晕漆的涂装：采用3涂层的绝缘结构，底层涂覆2道聚酯漆打底，中间涂覆7道添加了纳米SiO2粒子的聚酰胺酰亚胺耐电晕漆，外层涂覆2道聚酰胺酰亚胺漆。漆包线耐电晕漆的涂装工艺：车速为15 m/min，进口炉温为430℃，中间炉温为480℃，出口炉温为460℃，主循环/排废风机的转速为2 000/1 000 r/min。
1.3 测试方法
纳米SiO2表面羟基数的测定：参考T/FSI 049—2020《气相二氧化硅表面硅羟基含量的测定方法》[13]，称取2 g改性后的纳米SiO2样品于烧杯中，加入25 mL无水乙醇和75 mL的20% NaCl溶液，在25℃下搅拌均匀后用0.1 mol/L的盐酸调节溶液pH为4.0，随后缓慢加入0.1 mol/L氢氧化钠溶液使pH值上升至9.0，并保持30 s稳定不变。记录NaOH消耗的体积V1，此时纳米SiO2表面积上的羟基个数N可由式（1）计算。
N=cV1NA×10-3Sm
式（1）中：c为NaOH的浓度，mol/L；V1为pH值从4.0升到9.0时所消耗的NaOH体积，mL；NA为阿伏伽德罗常数；S为纳米SiO2的比表面积，nm2/g；m为纳米SiO2的质量，g。
耐电晕性能的测试：扁线测试样品的制备参照GB/T 4074.5—2008[14]，取扁线弯曲成有效直线长度为12 cm、两端夹角为60°、两端长度为4 cm的试样，取与试样相同形状规格的裸线，再把裸线与所要测试的扁线试样用聚酰亚胺薄膜粘带缠紧，随后在一定条件下采用脉冲电流测试试样绝缘层被击穿所用的时间。测试相关参数参照GB/T 21707—2008[15]设定，电压为3 kV（薄膜测试电压为2 kV），脉冲频率为20 kHz，脉冲占空比为50%，脉冲波形为方波，脉冲极性为双极，试验温度为（155±2）℃。
2 结果与讨论
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2.1 改性剂种类对纳米SiO2表面羟基的影响
改性剂的种类对纳米SiO2分散性的改性结果有较大差异。图1为相同条件下经KH-560、KH-792、AP1231、A112、乳化剂OP-10 5种不同改性剂改性后纳米SiO2的分散度，并与未改性前（Blank）的分散度进行了比较。
从图1可知，在二甲苯溶液中，用KH-560改性后的纳米SiO2表面羟基数最少，分散性最好。这是由于KH-560非极性基团较长，其疏水能力强，并且由于烷氧基官能团度较高，在纳米SiO2表面形成化学键的强度和水解稳定性也较高[16]。当KH-560与纳米SiO2加入到二甲苯溶液中时，KH-560的分子空间构型在纳米SiO2表面反应下发生改变，形成曲折结构，它的硅醇基把其他基团包在里面，使整个硅醇基处于外面，而纳米SiO2表面的羟基以氢键的形式与硅醇基连接，形成非常稳定且疏水的Si-O-Si键，大量减少了SiO2表面亲水性羟基的数量[17-18]，因此使用KH-560改性后的纳米SiO2在有机相中分散性较好，即改性效果最好。
2.2 改性剂用量对纳米SiO2表面羟基的影响
以KH-560作为改性剂，在反应温度为90℃、反应时间为4 h、溶液pH值为5的条件下研究改性剂用量（改性剂与纳米SiO2质量比）对改性后纳米SiO2分散度的影响，结果如图2所示。
由图2可知，当改性剂用量较低时，随着改性剂用量的增加，纳米SiO2表面羟基个数显著减少。当改性剂质量分数达到1.5%时，改性效果达到最佳。此时若继续增加改性剂用量，纳米SiO2表面的大部分羟基已完成接枝，由于纳米SiO2表面羟基减少及空间位阻增大，大多数改性剂分子难以与纳米SiO2表面羟基发生有效接触而只能发生物理吸附[19]。此外，改性剂浓度过高容易发生自身聚合，产生絮凝物，导致改性效果反而下降。因此，1.5%为KH-560的最适宜用量。
2.3 改性温度对纳米SiO2表面羟基的影响
在反应时间为4 h、溶液pH值为5、选用改性剂为KH-560、质量分数为1.5%的条件下研究改性温度对分散度的影响，结果如图3所示。
由图3可知，当温度低于90℃时，纳米SiO2表面羟基数随着温度升高而减小，这是因为温度升高增大了改性剂的分子活性，改性剂分子在纳米SiO2表面从物理吸附变为与表面上的自由羟基发生有效化学反应，导致表面羟基数下降。当温度超过90℃时，纳米SiO2表面羟基数开始随温度上升而增加，其原因主要是当温度过高时，分子运动加剧，导致纳米SiO2表面不稳定的羟基自身发生缩合[20]，与改性反应产生竞争；此外，温度过高也会引起改性剂本身发生自聚或分解[21]，从而使改性效果变差。因此90℃为适宜反应温度。
2.4 改性时间对纳米SiO2表面羟基的影响
在KH-560改性剂质量分数为1.5%，反应温度为90℃、溶液pH值为5的条件下研究改性时间对改性纳米SiO2分散度的影响，结果如图4所示。
由图4可知，纳米SiO2表面羟基数随改性时间延长逐渐下降，在4 h后下降趋势逐渐缓慢，进入平缓区。这是因为当反应刚开始时，纳米SiO2表面羟基数量较多，与改性剂反应较快。随着反应的进行，纳米SiO2表面羟基数量减少，偶联剂接枝在纳米SiO2表面后增加了空间位阻，使得反应逐渐减缓。此外，反应时间过长，对分散性效果影响不大，但增加了后处理的难度[22-23]。因此，适宜的反应时间为4 h。
2.5 纳米SiO2改性前后的形貌分析
图5为纳米SiO2改性前后的透射电镜图。由图5可以看出，未经改性的纳米SiO2粒子有较为明显的团聚现象，而经过KH-560改性后的纳米SiO2粒子团聚现象得到明显改善。纳米SiO2经过改性后，接枝在纳米粒子表面改性剂的自由基会发生聚合，在粒子表面形成一层或多层的预聚体，使单个纳米SiO2粒径变大的同时增大了纳米粒子之间的空间位阻，能够有效降低纳米粒子间的团聚程度[24]，使其在有机相中的分散性更好。
2.6 纳米粒子改性对PAI漆耐电晕性的影响
纳米SiO2掺杂含量对PAI漆的耐电晕性结果有较大影响[25]。为了研究纳米SiO2在PAI漆中适宜的掺杂量，在3 kV（薄膜实验电压为2 kV）、20 kHz的脉冲电压下对不同纳米SiO2粒子掺杂量的PAI漆进行耐电晕性能检测，结果如图6所示。
由图6可知，PAI漆的耐电晕时间随纳米SiO2添加量的增加而增加，结合T TANAKA多核模型理论[26]可以解释为：由于纳米SiO2粒子具有较大的比表面积和较强的稳定性，可以在PAI漆膜耐电晕性最差的无定形聚合物表层形成一层有利于电荷弥散的保护层，削弱局部放电强度，从而增强材料的耐电晕性能[27]。当纳米粒子添加质量分数达到12%时，PAI漆的耐电晕时间>50 h，已满足目前新能源汽车行业相关标准。当纳米粒子添加质量分数达到13.5%时，继续增加纳米SiO2的添加量将显著降低PAI漆膜的柔韧性和稳定性[28-29]。从工艺效果考虑，13.5%为较为适宜的纳米SiO2粒子添加量。
3 结论
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（1）在KH-560、KH-792、AP1231，A112、乳化剂OP-10中，改性剂KH-560改性后的纳米SiO2表面羟基数最少，即改性效果最好。
（2）在二甲苯体系中，KH-560改性纳米SiO2的最优条件为：KH-560质量分数为1.5%，反应温度为90℃，反应时间为4 h。
（3）改性后的纳米SiO2能够有效改善PAI漆的耐电晕性能，当纳米SiO2质量分数为13.5%时，PAI漆的耐电晕性能可以满足新能源汽车变频驱动电机漆包线漆的行业标准要求，继续增加添加纳米粒子将显著降低漆包线的柔韧性与稳定性，因此13.5%为较适宜的添加量。
基金
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  • 湖南省重点研发项目(2019GK2237)
  • 湖南省科技特派员项目(2021GK5048)
  • 湖南省自然科学基金资助项目(2021JJ50124)
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2023年第56卷第3期
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doi: 10.16790/j.cnki.1009-9239.im.2023.03.002
  • 接收时间：2022-03-10
  • 首发时间：2025-11-21
  • 出版时间：2023-03-20
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  • 收稿日期：2022-03-10
  • 修回日期：2022-04-19
基金
湖南省重点研发项目(2019GK2237)
湖南省科技特派员项目(2021GK5048)
湖南省自然科学基金资助项目(2021JJ50124)
作者信息
    1湖南科技大学，化学化工学院，湖南 湘潭 411201
    2湖南科技大学，煤炭资源清洁利用与矿山环境保护湖南省重点实验室，湖南 湘潭 411201
    3湖南科技大学，资源环境与安全工程学院，湖南 湘潭 411201

通讯作者:

周剑林（1982-），男（汉族），湖南常德人，讲师，主要从事纳米材料、绝缘材料的应用研究。
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https://castjournals.cast.org.cn/joweb/jycl/CN/10.16790/j.cnki.1009-9239.im.2023.03.002
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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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