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Article(id=1210613545268547611, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1210613541111984320, articleNumber=null, orderNo=null, doi=10.16790/j.cnki.1009-9239.im.2024.11.006, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1716912000000, receivedDateStr=2024-05-29, revisedDate=1815235200000, revisedDateStr=2027-07-11, acceptedDate=null, acceptedDateStr=null, onlineDate=1766562361303, onlineDateStr=2025-12-24, pubDate=1732032000000, pubDateStr=2024-11-20, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1766562361303, onlineIssueDateStr=2025-12-24, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1766562361303, creator=13701087609, updateTime=1766562361303, 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=59, endPage=64, ext={EN=ArticleExt(id=1210613545536983078, articleId=1210613545268547611, tenantId=1146029695717560320, journalId=1149653034449285133, language=EN, title=Preparation and application of epoxy potting materials for thin film capacitors in new energy vehicles, columnId=1210613542542241998, journalTitle=Insulating Materials, columnName=Special Issue on Key Materials and Technology for New Energy Vehicles, runingTitle=null, highlight=null, articleAbstract=

Using bisphenol A and bisphenol F epoxy resin as main resin, aluminum hydroxide and spherical silicon micro powder as fillers, combined with anhydride curing agent and epoxy toughening agent, a film capacitor epoxy potting material for new energy vehicle was prepared, and the effects of each component on the properties of potting materials were analyzed. The results show that the film capacitor epoxy potting material for new energy vehicles prepared by optimized formula has high glass transition temperature, good mechanical properties, good adhesion performance, small linear expansion coefficient, and the performances of capacitors are excellent. The prepared potting material has comparable performance levels to similar potting materials abroad and is suitable for thin film capacitors used in new energy vehicles.

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以双酚A型环氧树脂和双酚F型环氧树脂为主体树脂，氢氧化铝和球形硅微粉为填料，配合酸酐类固化剂和环氧增韧剂，制备了新能源汽车用薄膜电容环氧灌封材料，并分析了各组份对灌封材料性能的影响。结果表明：采用优化配方制备的新能源汽车用薄膜电容环氧灌封材料玻璃化转变温度高、力学性能好、粘接性能佳、线膨胀系数小、制作的电容器各项性能优异。所制备的灌封材料与国外同类灌封材料的各项性能水平相当，适用于新能源汽车用薄膜电容。

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蒋寅（1986-），男（汉族），江苏宜兴人，工程师，主要从事环氧树脂在电容电机方面的研究。

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蒋寅（1986-），男（汉族），江苏宜兴人，工程师，主要从事环氧树脂在电容电机方面的研究。

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蒋寅（1986-），男（汉族），江苏宜兴人，工程师，主要从事环氧树脂在电容电机方面的研究。

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Polymer Materials Science & Engineering,2000,16(1):70-73., articleTitle=Studies on effectiveness-losing mechanism of liquid filling sealed high voltage energy-storing capacitor, refAbstract=null), Reference(id=1218964284848128579, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210613545268547611, doi=null, pmid=null, pmcid=null, year=2019, volume=40, issue=3, pageStart=74, pageEnd=78, url=null, language=null, rfNumber=[22], rfOrder=41, authorNames=黄云锴, 储松潮, 潘焱尧, journalName=电力电容器与无功补偿, refType=null, unstructuredReference=黄云锴,储松潮,潘焱尧,等.树脂灌封电力电子电容器耐湿热性能的研究[J].电力电容器与无功补偿,2019,40(3):74-78., articleTitle=树脂灌封电力电子电容器耐湿热性能的研究, refAbstract=null), Reference(id=1218964284944597576, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210613545268547611, doi=null, pmid=null, pmcid=null, year=2019, volume=40, issue=3, pageStart=74, pageEnd=78, url=null, language=null, rfNumber=[22], rfOrder=42, authorNames=HUANGY K, CHUS C, PANY R, journalName=Power Capacitor & Reactive Power Compensation, refType=null, unstructuredReference=HUANGY K, CHUS C, PANY R, et al. Study on humidity resistance performance resin encapsulated power electric capacitor[J]. Power Capacitor & Reactive Power Compensation,2019,40(3):74-78., articleTitle=Study on humidity resistance performance resin encapsulated power electric capacitor, refAbstract=null)], funds=null, companyList=[AuthorCompany(id=1218964271795454042, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210613545268547611, xref=1, ext=[AuthorCompanyExt(id=1218964271803842651, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210613545268547611, companyId=1218964271795454042, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1Pulitai Electronic Materials Jiangsu Co., Ltd., Huaian 211600, China), AuthorCompanyExt(id=1218964271808036956, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210613545268547611, companyId=1218964271795454042, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1普利泰电子材料江苏有限公司，江苏 淮安 211600)]), AuthorCompany(id=1218964273120854114, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210613545268547611, xref=2, ext=[AuthorCompanyExt(id=1218964273129242723, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210613545268547611, companyId=1218964273120854114, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=2Jiangnan University, Wuxi 214122, China), AuthorCompanyExt(id=1218964273137631332, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210613545268547611, companyId=1218964273120854114, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=2江南大学，江苏 无锡 214122)])], figs=[ArticleFig(id=1218964275444498680, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210613545268547611, language=EN, label=Fig.1, caption=Viscosity curve of component A, figureFileSmall=Jnvk/00L/cQ0MLAz2Vkm6g==, figureFileBig=srv9AHtg9Vs2brsA0AJNog==, tableContent=null), ArticleFig(id=1218964275603882243, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210613545268547611, language=CN, label=图1, caption=组份A黏度变化曲线, figureFileSmall=Jnvk/00L/cQ0MLAz2Vkm6g==, figureFileBig=srv9AHtg9Vs2brsA0AJNog==, tableContent=null), ArticleFig(id=1218964275733905676, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210613545268547611, language=EN, label=Fig.2, caption=Viscosity curve of component B, figureFileSmall=uf95Ab6h3t2MHUoXFSz8jw==, figureFileBig=W4lta5rSRMeOBFw8LUD4qw==, tableContent=null), ArticleFig(id=1218964275821986066, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210613545268547611, language=CN, label=图2, caption=组份B黏度变化曲线, figureFileSmall=uf95Ab6h3t2MHUoXFSz8jw==, figureFileBig=W4lta5rSRMeOBFw8LUD4qw==, tableContent=null), ArticleFig(id=1218964275901677849, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210613545268547611, language=EN, label=Table 1, caption=Preparation formula of component A, figureFileSmall=null, figureFileBig=null, tableContent=
编号850SNPEF-170MX154氢氧化铝球形微硅粉
A128.07.00560
A224.06.05560
A320.05.010560
A426.13.95560
A525.05.05560
A623.16.95560
A720.05.05565
A816.04.05570
), ArticleFig(id=1218964275998146847, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210613545268547611, language=CN, label=表1, caption=

组份A的制备配方

, figureFileSmall=null, figureFileBig=null, tableContent=
编号850SNPEF-170MX154氢氧化铝球形微硅粉
A128.07.00560
A224.06.05560
A320.05.010560
A426.13.95560
A525.05.05560
A623.16.95560
A720.05.05565
A816.04.05570
), ArticleFig(id=1218964276098810150, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210613545268547611, language=EN, label=Table 2, caption=Preparation formula of component B, figureFileSmall=null, figureFileBig=null, tableContent=
编号MeTHPABDMA氢氧化铝球形硅微粉
B129.50.5565
B224.50.5570
B319.50.5575
), ArticleFig(id=1218964276228833581, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210613545268547611, language=CN, label=表2, caption=

组份B的制备配方

, figureFileSmall=null, figureFileBig=null, tableContent=
编号MeTHPABDMA氢氧化铝球形硅微粉
B129.50.5565
B224.50.5570
B319.50.5575
), ArticleFig(id=1218964276346274097, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210613545268547611, language=EN, label=Table 3, caption=The effect of epoxy toughening agent dosage on the properties of encapsulating materials, figureFileSmall=null, figureFileBig=null, tableContent=
组份A1-B1A2-B1A3-B1
MX154质量分数/%02.55
Tg/℃120118115
拉伸强度/MPa526864
剪切强度/MPa10.210.210.4
线膨胀系数/(×10-5 K-1)2.702.702.72
恒高温试验未发现异常未发现异常未发现异常
恒低温试验胶体开裂未发现异常未发现异常
高低温冲击试验胶壳/胶体均开裂胶壳开裂胶壳开裂
抗湿热性试验△C/C=10.4%△C/C=5.0%△C/C=5.2%
), ArticleFig(id=1218964277684257076, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210613545268547611, language=CN, label=表3, caption=

环氧增韧剂用量对灌封材料的性能影响

, figureFileSmall=null, figureFileBig=null, tableContent=
组份A1-B1A2-B1A3-B1
MX154质量分数/%02.55
Tg/℃120118115
拉伸强度/MPa526864
剪切强度/MPa10.210.210.4
线膨胀系数/(×10-5 K-1)2.702.702.72
恒高温试验未发现异常未发现异常未发现异常
恒低温试验胶体开裂未发现异常未发现异常
高低温冲击试验胶壳/胶体均开裂胶壳开裂胶壳开裂
抗湿热性试验△C/C=10.4%△C/C=5.0%△C/C=5.2%
), ArticleFig(id=1218964277852029247, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210613545268547611, language=EN, label=Table 4, caption=The effect of bisphenol F epoxy resin dosage on the properties of encapsulating materials, figureFileSmall=null, figureFileBig=null, tableContent=
组份A4-B1A5-B1A2-B1A6-B1
m(850S)∶m(NPEF-170)100∶15100∶20100∶25100∶30
Tg/℃117118118117
拉伸强度/MPa62686868
剪切强度/MPa10.110.410.210.4
线膨胀系数/(×10-5K-1)2.712.702.702.72
恒高温试验未发现异常未发现异常未发现异常未发现异常
恒低温试验未发现异常未发现异常未发现异常未发现异常
高低温冲击试验胶壳开裂胶壳开裂胶壳开裂胶壳开裂
抗湿热性试验△C/C=4.5%△C/C=4.7%△C/C=5.0%△C/C=6.2%
), ArticleFig(id=1218964277990441288, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210613545268547611, language=CN, label=表4, caption=

双酚F环氧树脂用量对灌封材料的性能影响

, figureFileSmall=null, figureFileBig=null, tableContent=
组份A4-B1A5-B1A2-B1A6-B1
m(850S)∶m(NPEF-170)100∶15100∶20100∶25100∶30
Tg/℃117118118117
拉伸强度/MPa62686868
剪切强度/MPa10.110.410.210.4
线膨胀系数/(×10-5K-1)2.712.702.702.72
恒高温试验未发现异常未发现异常未发现异常未发现异常
恒低温试验未发现异常未发现异常未发现异常未发现异常
高低温冲击试验胶壳开裂胶壳开裂胶壳开裂胶壳开裂
抗湿热性试验△C/C=4.5%△C/C=4.7%△C/C=5.0%△C/C=6.2%
), ArticleFig(id=1218964278103687500, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210613545268547611, language=EN, label=Table 5, caption=The effect of filler dosage on properties of encapsulating materials, figureFileSmall=null, figureFileBig=null, tableContent=
组份A5-B1A7-B2A8-B3
填料占比/%67.572.577.5
Tg/℃118117111
拉伸强度/MPa686658
剪切强度/MPa10.410.07.2
线膨胀系数/(×10-5 K-1)2.702.001.80
恒高温试验未发现异常未发现异常未发现异常
恒低温试验未发现异常未发现异常未发现异常
高低温冲击试验胶壳开裂未发现异常胶壳开裂
抗湿热性试验△C/C=4.7%△C/C=1.2%△C/C=4.2%
), ArticleFig(id=1218964278258876756, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210613545268547611, language=CN, label=表5, caption=

填料用量对灌封材料的性能影响

, figureFileSmall=null, figureFileBig=null, tableContent=
组份A5-B1A7-B2A8-B3
填料占比/%67.572.577.5
Tg/℃118117111
拉伸强度/MPa686658
剪切强度/MPa10.410.07.2
线膨胀系数/(×10-5 K-1)2.702.001.80
恒高温试验未发现异常未发现异常未发现异常
恒低温试验未发现异常未发现异常未发现异常
高低温冲击试验胶壳开裂未发现异常胶壳开裂
抗湿热性试验△C/C=4.7%△C/C=1.2%△C/C=4.2%
), ArticleFig(id=1218964278430843231, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210613545268547611, language=EN, label=Table 6, caption=Suggested formula of encapsulating materials, figureFileSmall=null, figureFileBig=null, tableContent=
组份原材料名称质量份组份原材料名称质量份
A850S20MeTHPA24.5
NPEF-1705BDMA0.5
MX-1545B氢氧化铝5
氢氧化铝5球形硅微粉70
球形硅微粉65KS-6030.2～0.3
KH-5800.2～0.3
KS-6030.2～0.3
), ArticleFig(id=1218964278569255265, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210613545268547611, language=CN, label=表6, caption=

灌封材料的建议配方

, figureFileSmall=null, figureFileBig=null, tableContent=
组份原材料名称质量份组份原材料名称质量份
A850S20MeTHPA24.5
NPEF-1705BDMA0.5
MX-1545B氢氧化铝5
氢氧化铝5球形硅微粉70
球形硅微粉65KS-6030.2～0.3
KH-5800.2～0.3
KS-6030.2～0.3
), ArticleFig(id=1218964278657335657, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210613545268547611, language=EN, label=Table 7, caption=Curing conditions and processes, figureFileSmall=null, figureFileBig=null, tableContent=
项目内容固化条件真空度/MPa
第1道灌注物料浸没至电容内芯4/5处90℃/2 h≥-0.1
第2道灌注物料浸没至电容边缘90℃/2 h+110℃/2 h≥-0.1
), ArticleFig(id=1218964278799942002, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210613545268547611, language=CN, label=表7, caption=

固化条件与工艺

, figureFileSmall=null, figureFileBig=null, tableContent=
项目内容固化条件真空度/MPa
第1道灌注物料浸没至电容内芯4/5处90℃/2 h≥-0.1
第2道灌注物料浸没至电容边缘90℃/2 h+110℃/2 h≥-0.1
), ArticleFig(id=1218964278917382522, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210613545268547611, language=EN, label=Table 8, caption=Test data and contrast of encapsulating materials, figureFileSmall=null, figureFileBig=null, tableContent=
序号测试项目试验产品测试结果国外品牌产品测试结果测试标准
1邵氏硬度93D92DGB/T 2411—2008
2Tg/℃117117GB/T 1634—2004
3线膨胀系数(23～80℃)/(×10-5K-1)2.00×10-51.98×10-5GB/T 1036—2008
4拉伸强度/MPa6668.3GB/T1040.1—2006
5伸长率/%1.81.7GB/T1040.1—2006
6弯曲强度/MPa165150GB/T 9341—2008
7剪切强度(PPS)/MPa10.010.0GB/T 6396—2018
8吸水率(100℃/4 h)/%0.120.14—
9导热系数(23℃)/(W/(m·K))0.650.62GB/T 10295—2008
10介质损耗因数(1 MHz)0.017 590.018 64GB/T 1409—2006
11介电常数(1 MHz)3.64.0GB/T 1409—2006
12体积电阻率/(Ω·m)3.7×10143.6×1014GB/T 1410—2006
13表面电阻率/Ω5.7×10125.5×1012GB/T 1410—2006
14绝缘电阻/Ω8.9×10108.5×1010GB/T 10064—2006
15恒高温试验合格合格—
16恒低温试验合格合格—
17高低温冲击试验合格合格—
18抗湿热性试验△C/C=1.2%△C/C=2.3%—
), ArticleFig(id=1218964279009657217, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210613545268547611, language=CN, label=表8, caption=

灌封材料测试数据与对比

, figureFileSmall=null, figureFileBig=null, tableContent=
序号测试项目试验产品测试结果国外品牌产品测试结果测试标准
1邵氏硬度93D92DGB/T 2411—2008
2Tg/℃117117GB/T 1634—2004
3线膨胀系数(23～80℃)/(×10-5K-1)2.00×10-51.98×10-5GB/T 1036—2008
4拉伸强度/MPa6668.3GB/T1040.1—2006
5伸长率/%1.81.7GB/T1040.1—2006
6弯曲强度/MPa165150GB/T 9341—2008
7剪切强度(PPS)/MPa10.010.0GB/T 6396—2018
8吸水率(100℃/4 h)/%0.120.14—
9导热系数(23℃)/(W/(m·K))0.650.62GB/T 10295—2008
10介质损耗因数(1 MHz)0.017 590.018 64GB/T 1409—2006
11介电常数(1 MHz)3.64.0GB/T 1409—2006
12体积电阻率/(Ω·m)3.7×10143.6×1014GB/T 1410—2006
13表面电阻率/Ω5.7×10125.5×1012GB/T 1410—2006
14绝缘电阻/Ω8.9×10108.5×1010GB/T 10064—2006
15恒高温试验合格合格—
16恒低温试验合格合格—
17高低温冲击试验合格合格—
18抗湿热性试验△C/C=1.2%△C/C=2.3%—
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新能源汽车用薄膜电容环氧灌封材料的制备和应用
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蒋寅 1 , 顾铖 1 , 顾域轩 2 , 庄雪峰 1
绝缘材料 | 新能源汽车用关键材料与技术专题 2024,57(11): 59-64
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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): 59-64
新能源汽车用薄膜电容环氧灌封材料的制备和应用
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蒋寅1, 顾铖1, 顾域轩2, 庄雪峰1
作者信息
  • 1普利泰电子材料江苏有限公司，江苏 淮安 211600
  • 2江南大学，江苏 无锡 214122

    • 蒋寅（1986-），男（汉族），江苏宜兴人，工程师，主要从事环氧树脂在电容电机方面的研究。

Preparation and application of epoxy potting materials for thin film capacitors in new energy vehicles
Yin JIANG1, Cheng GU1, Yuxuan GU2, Xuefeng ZHUANG1
Affiliations
  • 1Pulitai Electronic Materials Jiangsu Co., Ltd., Huaian 211600, China
  • 2Jiangnan University, Wuxi 214122, China
出版时间: 2024-11-20 doi: 10.16790/j.cnki.1009-9239.im.2024.11.006
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摘要
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以双酚A型环氧树脂和双酚F型环氧树脂为主体树脂，氢氧化铝和球形硅微粉为填料，配合酸酐类固化剂和环氧增韧剂，制备了新能源汽车用薄膜电容环氧灌封材料，并分析了各组份对灌封材料性能的影响。结果表明：采用优化配方制备的新能源汽车用薄膜电容环氧灌封材料玻璃化转变温度高、力学性能好、粘接性能佳、线膨胀系数小、制作的电容器各项性能优异。所制备的灌封材料与国外同类灌封材料的各项性能水平相当，适用于新能源汽车用薄膜电容。

新能源汽车  /  薄膜电容  /  环氧树脂

Using bisphenol A and bisphenol F epoxy resin as main resin, aluminum hydroxide and spherical silicon micro powder as fillers, combined with anhydride curing agent and epoxy toughening agent, a film capacitor epoxy potting material for new energy vehicle was prepared, and the effects of each component on the properties of potting materials were analyzed. The results show that the film capacitor epoxy potting material for new energy vehicles prepared by optimized formula has high glass transition temperature, good mechanical properties, good adhesion performance, small linear expansion coefficient, and the performances of capacitors are excellent. The prepared potting material has comparable performance levels to similar potting materials abroad and is suitable for thin film capacitors used in new energy vehicles.

new energy vehicles  /  thin film capacitor  /  epoxy resin
蒋寅, 顾铖, 顾域轩, 庄雪峰. 新能源汽车用薄膜电容环氧灌封材料的制备和应用. 绝缘材料, 2024 , 57 (11) : 59 -64 . DOI: 10.16790/j.cnki.1009-9239.im.2024.11.006
Yin JIANG, Cheng GU, Yuxuan GU, Xuefeng ZHUANG. Preparation and application of epoxy potting materials for thin film capacitors in new energy vehicles[J]. Insulating Materials, 2024 , 57 (11) : 59 -64 . DOI: 10.16790/j.cnki.1009-9239.im.2024.11.006
正文
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0 引言
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薄膜电容是一种常见的现代电子元器件，主要应用于电子、家电、通讯、电力、电气化铁路、混合动力汽车、风力发电、太阳能发电等领域，具有良好的电气性能和可靠性[1-3]。在新能源汽车领域，干式直流滤波薄膜电容是核心元器件之一，其应用于新能源汽车HEV/EV电驱控制器中，为不同功率等级电驱提供解决方案，广泛作用于DC-LINK电路中，做直流滤波储能之用。干式直流滤波薄膜电容的主要特点包括：①采用特殊结构材料设计、自愈性好、介质损耗因数低、等效串联电阻低、温升低[4-6]；②由叠式母排引出，杂散电感低[7]；③采用高温高导材料灌注，在高温高湿复杂的应用环境下，可长期稳定工作[8-10]。
目前干式直流滤波薄膜电容的灌封主要使用环氧-酸酐体系材料，该材料具有低膨胀系数、高拉伸强度、耐高低温、耐高低温冲击、耐湿热、与电容外壳（PPS）粘接力强等特点[11]。长期以来，这类灌封材料一直被日本企业垄断。为应对潜在的技术封锁，响应国产化替代趋势，本文旨在研究一种同样具有以上特点，且能满足新能源车用薄膜电容灌封要求的材料。以本次研究为始，经系列研究，国内率先制备了新能源汽车用薄膜电容灌封材料[12]，其主要性能与国外同类产品水平相当，在本领域实现下游客户覆盖。
1 试验
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1.1 主要原材料
双酚A型环氧树脂850S（环氧当量为184～194 g/eq），南通星辰合成材料有限公司；双酚F型环氧树脂NPEF-170（环氧当量为160～180 g/eq），南亚环氧树脂（昆山）有限公司；环氧增韧剂MX154，钟渊化学工业株式会社；氢氧化铝（1 200目），新乡市锦盛新材料有限公司；球形硅微粉（800～1 000目），上海巴萱贸易有限公司；甲基四氢邻苯二甲酸酐（MeTHPA），濮阳惠成电子材料股份有限公司；苄基二甲胺（BDMA），杭州施特安化工有限公司；γ-巯丙基三乙氧基硅烷KH-580，丹阳多利新材料有限公司；消泡剂KS-603，信越化学工业株式会社。
1.2 胶样的制备
1.2.1 组份A的制备
按一定的质量比将850S、NPEF-170、MX154、氢氧化铝、球形硅微粉、KH-580和KS-603混合，在80℃条件下高速分散搅拌均匀后，在-0.1 MPa/110℃条件下脱泡2 h制得灌封材料的组份A，按表1配方分别标注。
1.2.2 组份B的制备
按一定的质量比将MeTHPA、BDMA、氢氧化铝、球形硅微粉和KS-603混合，在常温（23～25℃）下高速分散搅拌均匀后，在-0.1 MPa/90℃条件下脱泡1 h制得灌封材料的组份B，按表2配方分别标注。
1.3 性能测试
（1）旋转黏度：使用旋转黏度计（型号为NDJ-79B，上海昌吉地质仪器有限公司）测试，温度为40℃，转子为100#，转速为75 r/min，参考GB/T 1632—2008相关要求进行测试。
（2）拉伸强度：使用万能拉力机（型号为TY-8000，江苏天源试验设备有限公司）测试，温度为25℃，速度为20 mm/min。
（3）剪切强度：使用万能拉力机（型号为TY-8000，江苏天源试验设备有限公司）测试，温度为25℃，速度为20 mm/min，垂直拉伸，粘接基材为聚苯硫醚（PPS），粘接面积为100 mm2。
（4）线膨胀系数：使用高温卧式膨胀仪（型号为PCY-1700，湖南湘科仪器设备有限公司）测试，升温速率为5℃/min，测试温度为23～80℃。
（5）玻璃化转变温度（Tg）：使用DSC差示扫描量热仪（型号为7020，日本日立金属株式会社）测试，升温速率为10℃/min，测试温度为30～160℃。
（6）电容器性能测试：测试选用的电容器参数为MODULAR DCR 670μF/2 300 V/105 A，尺寸为220 mm×115 mm。性能测试包括恒高温、恒低温、高低温冲击和抗湿热性试验。其中恒高温试验条件为105℃/96 h；恒低温试验条件为-40℃/96 h。高低温冲击试验温度为-40～120℃，升/降温速率均为4℃/min，保持时间为30 min，切换时间为1 min，循环次数为500次。合格标准为灌封材料与外壳无开裂现象（也称“胶壳开裂”）和灌封材料自身未发现开裂现象（也称“胶体开裂”）。抗湿热性试验是在温度为85℃，湿度为85%下以UN连续运行1 000 h。合格标准为电容量损耗△C/C≤3%，时间常数RC≥5 000 s，串联电阻ESR≤2ESR0（鉴于非电力电子专业实验室，仅测试△C/C作为评判标准；C为电容；R为电阻；ESR为等效串联电阻）[13-15]。
2 结果与讨论
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2.1 环氧增韧剂用量对灌封材料性能的影响
将A1～A3分别与B1按质量比为100∶100混合搅拌均匀后制备成各类样块并灌注薄膜电容，固化条件为90℃/2 h+110℃/2 h。各灌封材料试样的性能测试数据见表3。从表3可以看出，以MX154作为增韧剂，850S和NPEF-170按质量比为100∶25复配时，随着MX154占比的增加，灌封材料的玻璃化转变温度逐渐下降，拉伸强度先增大后减小。这是由于MX154为核壳类粒子，在一定添加量下可以提高固化物的拉伸强度，但是其作为非反应型物质，添加过量会导致环氧基与酸酐的交联密度减小，降低玻璃化转变温度和拉伸强度。各试样的剪切强度和线膨胀系数并无明显差异，这是由于剪切强度的影响因素主要是粘接基材、反应物基团和偶联剂；而线膨胀系数的影响因素主要是填料的种类和添加量与增韧剂的用量关系不大。在进行一定的增韧且剪切强度优异的情况（一般要求≥8 MPa）下[16-18]，电容器胶体和胶壳依旧出现不同程度的开裂现象，可以考虑继续增大拉伸强度和减小线膨胀系数（目前结果略大于PPS的线膨胀系数2.4×10-5 K-1[19-20]）。由于出现开裂现象，水汽进入电容器内部会对内芯金属化聚丙烯膜造成破坏[21-22]，导致薄膜电容的电容量损耗△C/C均不合格，但对比发现胶体开裂对电容量损耗的影响更大。
2.2 双酚F环氧树脂用量对灌封材料性能的影响
将A2、A4、A5、A6与B1分别按质量比为100∶100混合搅拌均匀后制备成各类样块并灌注薄膜电容，固化条件为90℃/2 h+110℃/2 h。各类灌封材料试样的性能测试数据见表4。从表4可以看出，当MX154添加量为5份、850S和NPEF-170按一定质量比复配时，随着NPEF-170含量的增加，灌封材料的拉伸强度增大至68 MPa后保持不变，这是由于NPEF-170作为双酚F型环氧树脂，其每个聚合单元比850S少两个甲基，刚性较弱，故灌封材料的拉伸强度增大。当m(850S)∶m(NPEF-170)≥100∶20后，灌封材料的刚性不足以影响交联结构和密度，故拉伸强度趋于稳定。而各试样的玻璃化转变温度、剪切强度和线膨胀系数等未有明显差异。虽然添加增韧剂和双酚F型环氧树脂后灌封材料的拉伸强度较高且剪切强度优异，但电容器胶壳仍出现不同程度的开裂现象，可考虑减小线膨胀系数。由于出现开裂现象，水汽进入电容器内部会对内芯金属化聚丙烯膜造成破坏，导致薄膜电容的电容量损耗△C/C均不合格。由于双酚F型环氧树脂甲基的缺失，耐水性不如双酚A型环氧树脂，故随NPEF-170含量的增加，△C/C呈不断上升趋势。
2.3 填料用量对灌封材料性能的影响
将A5、A7、A8分别与B1、B2、B3按质量比为100∶100搅拌混合均匀后制备成各类样块并灌注薄膜电容，固化条件为90℃/2 h+110℃/2 h。各类灌封材料试样的性能测试数据见表5。从表5可以看出，当MX154添加量为5份，850S与NPEF-170按质量比100：25复配时，随着填料（氢氧化铝加球形微硅粉）占比的增加，灌封材料的拉伸强度和玻璃化转变温度逐渐下降，这是由于填料的存在阻碍了有机分子间的运动交联成形。剪切强度在填料占比增大时急剧减小，这是由于填料挤占了有机组份的运动空间，导致有机组份相关基团在PPS基材表面含量过少，影响了灌封材料的剪切强度。填料占比的增加使灌封材料的线膨胀系数逐渐减小，当填料占比为72.5%时，灌封材料的线膨胀系数小于PPS，且在拉伸强度、剪切强度和线膨胀系数等因素综合作用下，灌封材料未出现开裂现象，电容器性能测试均合格，△C/C=1.2%。
2.4 新能源汽车用薄膜电容灌封材料的建议配方
通过试验确定灌封材料的配方如表6所示。由于不同的客户在电容器性能测试的要求方面不尽相同，如德国某公司要求高低温冲击循环次数为1 000次，可在此配方上进行改进。
2.5 新能源汽车用薄膜电容灌封材料的黏度曲线
为应对不同客户的灌封材料预处理工艺，如厦门某公司采用温度为70～80℃预热工艺，深圳某公司采用温度为80～90℃的预热工艺，故对组份A和B在不同温度下的黏度进行测试，结果如图1和图2所示。从图1和图2可以看出，当温度超过80℃时，组份A和B的黏度基本趋于平稳，故建议下游客户的预处理工艺选择80℃预热。
2.6 新能源汽车用薄膜电容灌封材料的固化条件和工艺
通过试验确定灌封材料的固化条件和工艺，如表7所示。
新能源汽车用薄膜电容灌封材料的固化工艺一般采用两道真空灌注工艺，第1道真空灌注工艺的目的是固定电容内芯，消除搅拌气泡；第2道真空灌注工艺采用两段加温方式进行固化，前段目的是控制凝胶时间，以便于消除气泡和防止局部应力过大而产生微小裂缝；后段目的是使组份B固化。为了防止高温下环氧-酸酐体系的过高放热对电容内芯造成伤害，固化温度控制在110℃以下。
2.7 新能源汽车用薄膜电容灌封材料的性能
将本试验所述灌封材料与国外品牌灌封材料进行性能测试与对比，结果如表8所示。从表8可以看出，本试验所述灌封材料各项性能与国外产品水平相当，适用于新能源汽车用薄膜电容。
3 结论
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以双酚A型环氧树脂850S、双酚F型环氧树脂NPEF-170、环氧增韧剂MX154、氢氧化铝、球形硅微粉按质量比为20∶5∶5∶5∶65制备的组份A7和以甲基四氢邻苯二甲酸酐、苄基二甲胺、氢氧化铝、球形硅微粉按质量比为24.5∶0.5∶5∶70制备的组份B2，按质量比为100∶100进行，制备了一种新能源车用薄膜电容灌封材料，其玻璃化转变温度为117℃，线膨胀系数为2.0×10-5 K-1，拉伸强度为66 MPa，弯曲强度为165 MPa，PPS剪切强度为10.0 MPa，吸水率为0.12%，其所灌注的直流滤波薄膜电容通过了恒高温、恒低温、高低温冲击和抗湿热性试验，同时经与国外品牌材料性能进行对比，表明本次试验所制备的新能源汽车用薄膜电容灌封材料在主要性能上与国外品牌同类产品相当，可满足新能源汽车用薄膜电容的使用要求。
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2024年第57卷第11期
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doi: 10.16790/j.cnki.1009-9239.im.2024.11.006
  • 接收时间：2024-05-29
  • 首发时间：2025-12-24
  • 出版时间：2024-11-20
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  • 收稿日期：2024-05-29
  • 修回日期：2027-07-11
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    1普利泰电子材料江苏有限公司，江苏 淮安 211600
    2江南大学，江苏 无锡 214122
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2种不同金属材料的力学参数
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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
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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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