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Article(id=1242757051722612887, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1242757048333611957, articleNumber=null, orderNo=null, doi=10.16790/j.cnki.1009-9239.im.2021.12.007, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1612108800000, receivedDateStr=2021-02-01, revisedDate=1614009600000, revisedDateStr=2021-02-23, acceptedDate=null, acceptedDateStr=null, onlineDate=1774225970440, onlineDateStr=2026-03-23, pubDate=1639929600000, pubDateStr=2021-12-20, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1774225970440, onlineIssueDateStr=2026-03-23, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1774225970440, creator=13701087609, updateTime=1774225970440, updator=13701087609, issue=Issue{id=1242757048333611957, tenantId=1146029695717560320, journalId=1149653034449285133, year='2021', volume='54', issue='12', pageStart='1', pageEnd='114', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1774225969632, creator=13701087609, updateTime=1774226074518, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1242757488324494073, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1242757048333611957, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1242757488324494074, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1242757048333611957, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=38, endPage=47, ext={EN=ArticleExt(id=1242757053014458531, articleId=1242757051722612887, tenantId=1146029695717560320, journalId=1149653034449285133, language=EN, title=Research on Preparation of Nano ZnO-RTV Composite Material and Its Ultraviolet Resistance, columnId=1190369066675179686, journalTitle=Insulating Materials, columnName=Material Research, runingTitle=null, highlight=null, articleAbstract=

To improve the UV resistance of room temperature vulcanized silicone rubber (RTV), we used titanate coupling agent (PN) to modify nano zinc oxide (ZnO), and then nano ZnO-RTV composites were prepared by doping different mass fraction of modified nano ZnO into RTV. The ultraviolet accelerated ageing experiments were conducted on pure RTV and nano ZnO-RTV composites, and the effect of nano ZnO on the ultraviolet resistance of RTV was compared and analyzed. The results show that nano ZnO can effectively improve the UV shielding performance of RTV, and the UV shielding rate of nano ZnO-RTV composite with 1.0% of ZnO can increase by 72.63%; after adding nano ZnO, the electrical strength of RTV is slightly improved. After UV ageing for 2 500 hours, the decreasing amplitude of static con-tact angle and the ageing degree which reflected by surface micro-morphology of pure RTV are far greater than that of nano ZnO-RTV composite, it is verified by the changes of Si-(CH3)2, Si-CH3, and C=O of RTV molecular chains before and after ageing. At the same time, after UV ageing for 2500 hours, the thermal stability of nano ZnO-RTV composite is significantly better than that of pure RTV.

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为了提高室温硫化硅橡胶（RTV）抗紫外性能，本文通过钛酸酯偶联剂（PN）对纳米氧化锌（ZnO）进行改性，将其作为填料掺入RTV制备得到不同质量分数的纳米ZnO-RTV复合材料，对纯RTV和纳米ZnO-RTV复合材料进行紫外光加速老化实验，并对比分析纳米ZnO对RTV抗紫外性能的影响。结果表明：纳米ZnO能有效改善RTV的紫外光屏蔽性能，质量分数为1.0%的纳米ZnO-RTV复合材料紫外光屏蔽率的提升幅度高达72.63%；添加纳米ZnO后，RTV的电气强度略微提高；2 500 h紫外老化后，纯RTV表面静态接触角的下降幅度、表面微观形貌所反映的老化程度都远大于纳米ZnO-RTV复合材料，这与老化前后RTV分子链Si-(CH3)2、Si-CH3和C=O的变化情况相印证。同时，2 500 h紫外老化后，纳米ZnO-RTV复合材料的热稳定性明显优于纯RTV。

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谢从珍（1973-），女（汉族），陕西安康人，教授，主要从事新型功能电介质材料研发及测试、电力大数据及输配电线路防灾减灾技术的研究。
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骆守康（1995-），男（汉族），广东河源人，硕士生，主要从事新型功能电介质材料研发及测试的研究。

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骆守康（1995-），男（汉族），广东河源人，硕士生，主要从事新型功能电介质材料研发及测试的研究。

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骆守康（1995-），男（汉族），广东河源人，硕士生，主要从事新型功能电介质材料研发及测试的研究。

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暴露周期紫外灯型号辐照度/(W/m2×nm)波长/nm黑板温度/℃

8h干燥

4h冷凝

UVA-340

0.76±0.02

0

340

60±3

50±3

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荧光紫外灯暴露实验条件

, figureFileSmall=null, figureFileBig=null, tableContent=
暴露周期紫外灯型号辐照度/(W/m2×nm)波长/nm黑板温度/℃

8h干燥

4h冷凝

UVA-340

0.76±0.02

0

340

60±3

50±3

), ArticleFig(id=1245106611421819597, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242757051722612887, language=EN, label=Tab.2, caption=The electric strength of nano ZnO-RTV composite, figureFileSmall=null, figureFileBig=null, tableContent=
质量分数/%电气强度/(kV/mm)
017.06
0.518.96
1.019.33
2.019.52
), ArticleFig(id=1245106611505705679, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242757051722612887, language=CN, label=表2, caption=

纳米ZnO-RTV复合材料的电气强度

, figureFileSmall=null, figureFileBig=null, tableContent=
质量分数/%电气强度/(kV/mm)
017.06
0.518.96
1.019.33
2.019.52
), ArticleFig(id=1245106611585397457, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242757051722612887, language=EN, label=Tab.3, caption=The characteristic absorption peak and corresponding group of RTV, figureFileSmall=null, figureFileBig=null, tableContent=
吸收峰波数/(cm-1)基团
717～846Si-(CH3)2
1 200～1 300Si-CH3
916～1 212Si-O-Si
1 563～1 707C=O
), ArticleFig(id=1245106611690255059, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242757051722612887, language=CN, label=表3, caption=

RTV特征吸收峰及对应基团

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吸收峰波数/(cm-1)基团
717～846Si-(CH3)2
1 200～1 300Si-CH3
916～1 212Si-O-Si
1 563～1 707C=O
), ArticleFig(id=1245106611757363925, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242757051722612887, language=EN, label=Tab.4, caption=Thermal properties of pure RTV under different ageing time, figureFileSmall=null, figureFileBig=null, tableContent=
老化时间/hTmax/℃
第1阶段第2阶段第3阶段
0423.15521.37—
1 000411.13517.61558.27
2 000408.02487.92535.68
2 500420.46491.16540.31
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纯RTV在不同老化时间下的热性能

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老化时间/hTmax/℃
第1阶段第2阶段第3阶段
0423.15521.37—
1 000411.13517.61558.27
2 000408.02487.92535.68
2 500420.46491.16540.31
), ArticleFig(id=1245106611920941785, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242757051722612887, language=EN, label=Tab.5, caption=Thermal properties of nano ZnO-RTV composite with different mass fraction after ageing for 2 500 h, figureFileSmall=null, figureFileBig=null, tableContent=
质量分数/%Tinitial/℃Tmax/℃M%
第1阶段第2阶段第3阶段
0415.91420.46491.16540.311.618
0.5422.20461.00536.26—2.182
1.0432.47485.33548.65—2.052
2.0435.69495.57542.60—2.802
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不同质量分数的纳米ZnO-RTV复合材料老化2 500 h后的热性能

, figureFileSmall=null, figureFileBig=null, tableContent=
质量分数/%Tinitial/℃Tmax/℃M%
第1阶段第2阶段第3阶段
0415.91420.46491.16540.311.618
0.5422.20461.00536.26—2.182
1.0432.47485.33548.65—2.052
2.0435.69495.57542.60—2.802
), ArticleFig(id=1245106612092908252, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242757051722612887, language=EN, label=Tab.6, caption=The chemical bond energy of polydimethylsiloxane, figureFileSmall=null, figureFileBig=null, tableContent=
化学键键能/(kJ/mol)
Si-O447
O-H463
C-H413
Si-C318
), ArticleFig(id=1245106612172600029, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242757051722612887, language=CN, label=表6, caption=

聚二甲基硅氧烷化学键能

, figureFileSmall=null, figureFileBig=null, tableContent=
化学键键能/(kJ/mol)
Si-O447
O-H463
C-H413
Si-C318
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纳米ZnO-RTV复合材料的制备与抗紫外性能研究
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骆守康 1 , 谢从珍 1 , 王瑞 1 , 李立浧 1 , 杨杰 2
绝缘材料 | 材料研究 2021,54(12): 38-47
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绝缘材料 | 材料研究 2021, 54(12): 38-47
纳米ZnO-RTV复合材料的制备与抗紫外性能研究
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骆守康1, 谢从珍1, 王瑞1, 李立浧1, 杨杰2
作者信息
  • 1华南理工大学，广东 广州 510641
  • 2广东电网有限责任公司 广州供电局电力试验研究院，广东 广州 510410

    • 骆守康（1995-），男（汉族），广东河源人，硕士生，主要从事新型功能电介质材料研发及测试的研究。

通讯作者:

谢从珍（1973-），女（汉族），陕西安康人，教授，主要从事新型功能电介质材料研发及测试、电力大数据及输配电线路防灾减灾技术的研究。
Research on Preparation of Nano ZnO-RTV Composite Material and Its Ultraviolet Resistance
Shoukang LUO1, Congzhen XIE1, Rui WANG1, Licheng LI1, Jie YANG2
Affiliations
  • 1South China University of Technology, Guangzhou 510641, China
  • 2Electric Power Test Research Institute of Guangzhou Power Supply Burecus, Guangdong Power Grid Co., Ltd., Guangzhou 510410, China
出版时间: 2021-12-20 doi: 10.16790/j.cnki.1009-9239.im.2021.12.007
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摘要
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为了提高室温硫化硅橡胶（RTV）抗紫外性能，本文通过钛酸酯偶联剂（PN）对纳米氧化锌（ZnO）进行改性，将其作为填料掺入RTV制备得到不同质量分数的纳米ZnO-RTV复合材料，对纯RTV和纳米ZnO-RTV复合材料进行紫外光加速老化实验，并对比分析纳米ZnO对RTV抗紫外性能的影响。结果表明：纳米ZnO能有效改善RTV的紫外光屏蔽性能，质量分数为1.0%的纳米ZnO-RTV复合材料紫外光屏蔽率的提升幅度高达72.63%；添加纳米ZnO后，RTV的电气强度略微提高；2 500 h紫外老化后，纯RTV表面静态接触角的下降幅度、表面微观形貌所反映的老化程度都远大于纳米ZnO-RTV复合材料，这与老化前后RTV分子链Si-(CH3)2、Si-CH3和C=O的变化情况相印证。同时，2 500 h紫外老化后，纳米ZnO-RTV复合材料的热稳定性明显优于纯RTV。

纳米ZnO  /  室温硫化硅橡胶  /  纳米复合材料  /  抗紫外性能

To improve the UV resistance of room temperature vulcanized silicone rubber (RTV), we used titanate coupling agent (PN) to modify nano zinc oxide (ZnO), and then nano ZnO-RTV composites were prepared by doping different mass fraction of modified nano ZnO into RTV. The ultraviolet accelerated ageing experiments were conducted on pure RTV and nano ZnO-RTV composites, and the effect of nano ZnO on the ultraviolet resistance of RTV was compared and analyzed. The results show that nano ZnO can effectively improve the UV shielding performance of RTV, and the UV shielding rate of nano ZnO-RTV composite with 1.0% of ZnO can increase by 72.63%; after adding nano ZnO, the electrical strength of RTV is slightly improved. After UV ageing for 2 500 hours, the decreasing amplitude of static con-tact angle and the ageing degree which reflected by surface micro-morphology of pure RTV are far greater than that of nano ZnO-RTV composite, it is verified by the changes of Si-(CH3)2, Si-CH3, and C=O of RTV molecular chains before and after ageing. At the same time, after UV ageing for 2500 hours, the thermal stability of nano ZnO-RTV composite is significantly better than that of pure RTV.

nano ZnO  /  RTV  /  nano composites  /  ultraviolet resistance
骆守康, 谢从珍, 王瑞, 李立浧, 杨杰. 纳米ZnO-RTV复合材料的制备与抗紫外性能研究. 绝缘材料, 2021 , 54 (12) : 38 -47 . DOI: 10.16790/j.cnki.1009-9239.im.2021.12.007
Shoukang LUO, Congzhen XIE, Rui WANG, Licheng LI, Jie YANG. Research on Preparation of Nano ZnO-RTV Composite Material and Its Ultraviolet Resistance[J]. Insulating Materials, 2021 , 54 (12) : 38 -47 . DOI: 10.16790/j.cnki.1009-9239.im.2021.12.007
正文
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0 引言
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室温硫化硅橡胶（room temperature vulcanized silicone rubber，RTV），以其优异的憎水性和憎水恢复迁移特性，常作为防污闪涂料被广泛应用于电力系统[1-4]。然而在实际服役过程中，涂覆于瓷绝缘子、玻璃绝缘子以及输变电设备的RTV材料受热、电、酸雨以及紫外辐射的影响，运行寿命严重缩短[5-6]。在我国南方地区，高湿热和强紫外辐射气候容易使RTV材料发生老化脱落，进而引发污闪事故[7]。因此，提高RTV材料的抗紫外性能对延长RTV材料紫外老化寿命尤为重要。
研究发现，纳米氧化锌（ZnO）作为一种带隙值约为3.37 eV的宽带隙半导体材料，具有优良的紫外线屏蔽效应[8-11]，与其他紫外光屏蔽剂相比，纳米ZnO不仅对中长波紫外线均有屏蔽作用，而且兼具良好的热稳定性。因此，纳米ZnO常作为紫外光屏蔽剂广泛应用于高分子材料中。近年来，为探究纳米ZnO对紫外光的屏蔽效应，国内外学者在纳米ZnO/有机高分子复合材料领域开展了大量研究[12-15]。XU B等[15]通过对纳米ZnO-PP复合材料进行紫外老化实验，发现纳米ZnO对聚丙烯材料有显著的抗紫外老化和成核作用；ZHANG C H等[16]研究了纳米ZnO-EP复合涂料对PBO纤维抗紫外老化性能的影响，发现相同紫外老化时间下，PBO复合纤维的抗张强度是纯PBO纤维的两倍；CUI C W等[17]制备了一种紫外光高屏蔽的纳米ZnO-PMMA复合材料，研究发现紫外老化200 h后，纯PMMA的断裂伸长率降幅高达52%，而纳米ZnO-PMMA复合材料只下降了3%，依旧保持良好的力学性能。然而目前关于利用纳米ZnO提高RTV抗紫外性能的研究鲜见报道。
本研究以纳米ZnO作为无机填料，利用钛酸酯偶联剂进行表面化学修饰后添加到RTV基质中，制备得到质量分数为0、0.5%、1.0%、2.0%的纳米ZnO-RTV复合材料，并对各试样开展紫外光加速老化实验。对比不同含量的纳米ZnO-RTV复合材料的表面静态接触角、红外特征吸收峰、表面微观形貌及热分解特性随老化时间的变化规律，研究纳米ZnO对RTV抗紫外性能的影响机理。
1 实验
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1.1 主要原材料
107胶（SR，107#B2000），深圳市红叶杰科技有限公司；二丁基二月硅酸锡（工业级），济南铭宇化工有限公司；正硅酸乙酯（分析纯）、纳米ZnO（粒径为30±10 nm），阿拉丁试剂有限公司；钛酸酯偶联剂（PN-105，工业级），常州久隆助剂有限公司；丙酮（分析纯），广州市同源化工科技有限公司；无水乙醇（分析纯）、去离子水，麦克林试剂有限公司。
1.2 纳米ZnO-RTV复合材料的制备
称取10 g纳米ZnO干燥处理后，超声分散于200 mL丙酮中。将丙酮与去离子水以体积比3∶1混合，称取1 g钛酸酯偶联剂倒入其中，混合均匀后加入纳米ZnO超声分散液中，再超声20 min。将上述混合溶液在70℃下搅拌回流反应8 h后于室温静置24 h，再依次使用无水乙醇、丙酮和去离子水反复洗涤，最后在100℃下真空干燥12 h，得到的改性纳米ZnO记为PN-ZnO。
为使纳米颗粒在RTV中分散均匀，先将RTV基体稀释于适量的丙酮中，再将PN-ZnO加入其中，在40℃下机械搅拌6 h。随后将上述混合物真空加热以除去丙酮，待其冷却至室温后，在氮气氛围下滴加4.0%正硅酸乙酯以及0.5%二丁基二月硅酸锡，真空搅拌均匀后迅速倒入模具，静置8 h后制得纳米ZnO-RTV复合材料。在性能测试前，使用无水乙醇清洗试样，然后置于25℃的干燥器中干燥24 h。
1.3 紫外光加速老化实验
为尽可能模拟RTV的户外曝晒过程[18]，本研究选用QUV型紫外加速老化试验机，美国Q-Lab公司，并根据GB/T 14522—2008试验方法，选用UVA-340灯管（辐照波长为290～400 nm）进行试验，具体实验条件如表1所示。
1.4 性能测试
采用VERTEX 70型傅里叶红外光谱（FTIR）装置，德国Bruker公司，测试纳米ZnO改性前后的化学结构，波数范围为400～4 000 cm-1。通过Merlin型场发射扫描电镜（SEM），德国Carl Zeiss AG公司，观察纳米ZnO在RTV基质中的分散情况。利用Lambda 950型紫外-可见光分光光度计（UV-Vis），美国PerkinElmer公司，检测试样在紫外-可见光区的吸收特征光谱，扫描波长范围为200～400 nm。采用自行搭建的交流电气强度测试平台对试样进行检测，将试样浸泡于变压器油中，以0.5 kV/s的升压速率对每种试样分别进行7次击穿实验。
紫外光加速老化实验完成后，对各试样老化前后的表面进行FTIR测试，以表征其特征基团的变化情况，波数范围为500～3 750 cm-1。通过SEM观察各试样老化前后的表面微观形貌。利用OCA 40 Micro型表面张力表面接触角测试仪，德国Dataphysics公司，检测各试样老化前后表面的静态接触角。采用TG 209F1 Libra型热重分析仪，德国NETZSCH公司，测试样品的热失重曲线，氮气氛围，升温速率为10℃/min，温度范围为室温～800℃，样品质量为10 mg。
2 复合材料的性能分析
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2.1 纳米ZnO化学结构
傅里叶红外光谱（FTIR）常用于化学官能团的表征分析，本文利用FTIR检测对纳米ZnO表面接枝效果进行研究。图1为纳米ZnO、纳米ZnO-PN及钛酸酯偶联剂（PN）的红外光谱曲线。
从图1可以看出，纳米ZnO分别在480 cm-1、 3 435cm-1处出现Zn-O和-OH特征吸收峰。经过PN改性后，纳米ZnO-PN的Zn-O吸收峰强度保持不变，但-OH吸收峰明显削弱，与此同时，还出现PN的特征吸收峰Ti-O-P（1 028 cm-1）、-CH3（2 963 cm-1、2 870 cm-1）和-CH2-伸缩振动峰（2 926 cm-1），表明纳米ZnO表面成功接枝上PN。这是因为PN水解生成的烷羟基与纳米ZnO表面发生羟基反应，最终实现了纳米ZnO与PN的化学接枝。考虑到制备过程中，改性后的纳米颗粒用无水乙醇多次清洗，并在100℃下真空干燥24 h，因此可忽略改性后纳米颗粒表面物理吸附的偶联剂。
2.2 复合材料的微观形貌分析
采用SEM观察纳米ZnO-RTV复合材料液氮脆断面的微观形貌，以判断纳米ZnO是否均匀分散于RTV基质，测试结果如图2所示。从图2可以看出，经改性后的纳米ZnO均匀分散在RTV基质中，粒径为20～40 nm。在图2(c)中，质量分数为1.0%的ZnO绝大部分颗粒粒径在纳米级别范围内，并未出现团聚现象，颗粒形貌为不规则球状。纳米ZnO质量分数增大至2.0%后（图2(d)），部分颗粒会发生明显的团聚现象，此时团聚颗粒的粒径已达微米级别。总体上来说，在低填充量下，改性后的纳米ZnO能均匀分散于RTV基质中，但填充量持续增大后，纳米颗粒又难以避免发生团聚。
2.3 复合材料的紫外屏蔽性能
为表征纳米ZnO-RTV复合材料的紫外光屏蔽性能，利用紫外-可见光分光光度计（UV-Vis）对各试样进行检测，所得紫外光透射光谱图如图3所示。此外，为进一步量化试样的紫外屏蔽率，利用式（1）～（2）求解试样在紫外光加速老化实验辐照波段（290～400 nm）的透射比算术平均值。
T(UV)i=1m∑λ=290400Ti(λ)
A(UV)=1-T(UV)
式（1）～（2）中：m为290～400 nm波段间的测定次数；Ti(λ)为试样i在波长λ时的光谱透射比；T(UV)为紫外光透射比；A(UV)为紫外光屏蔽率。
根据式（1）～（2），可得各填充量纳米ZnO-RTV复合材料的紫外光屏蔽率变化规律，如图4所示。
从图4可以看出，纯RTV的紫外光屏蔽率仅为25.22%，随着纳米ZnO填充量的增大，试样的紫外光屏蔽率迅速提高，并在质量分数为1.0%时，试样的屏蔽率达到最大值，即97.85%，随后又出现下降趋势。可见，纳米ZnO的加入能显著提升RTV对紫外光的屏蔽效率，提升幅度高达72.63%。分析认为，纳米ZnO-RTV之所以能表现出显著的紫外屏蔽性能，主要是因为纳米ZnO对紫外光具有强吸收、易折射和散射作用。一方面，纳米ZnO作为宽带隙半导体材料，在室温下的带隙宽度约为3.37 eV，激子束缚能高达60 meV，与之对应的自由激子的响应吸收带始于387 nm，有利于吸收紫外光[19]。另一方面，纳米ZnO粒径极小且具有优良的界面反射性能。入射光照射到纳米ZnO时，在纳米ZnO-RTV基体的界面会不断产生漫反射现象[20]。此外，纳米ZnO尺寸小于紫外光波长，因此紫外光绕过粒子朝各个方向发生散射，进一步削弱了入射紫外光强度。然而当纳米ZnO的质量分数达到2.0%时，纳米ZnO-RTV的紫外光屏蔽率不升反降，这可能是由于纳米ZnO团聚成微米颗粒而无法有效吸收或散射紫外光，这一点与上述SEM测试结果相一致。
2.4 复合材料的电气强度
利用纳米改性技术对RTV填充纳米ZnO以增强RTV紫外屏蔽性能的同时，也需要探究纳米ZnO对RTV电气强度的影响，以确保纳米ZnO-RTV复合材料适用于电力系统。因此，对试样进行电气强度测试，并结合威布尔统计[21-23]（（3）～（4））对电气强度数据进行拟合分析，得到如图5所示的电气强度威布尔分布图。
F(U;α,β)=1-exp-(Uα)β
式（3）中：U为试样的电气强度；α、β分别为威布尔分布曲线的尺度参数和形状参数。
F(i,n)=i-0.44n+0.25×100%
式（4）中：i为试样的测试序号；n为试样测试次数。
根据威布尔统计分布，常以F(t)=63.2%作为试样的电气强度，具体数据如表2所示。
由表2可以看出，纯RTV的电气强度为17.06 kV/mm，纳米ZnO-RTV的电气强度随纳米ZnO填充量的增加而逐步增大，且在质量分数为2.0%时，达到最大值，即19.52 kV/mm。分析认为，可能是纳米ZnO作为RTV预聚体固化过程中的促进剂[24]，使得纳米ZnO-RTV复合材料形成更为致密的交联体系，而且纳米ZnO在RTV中分散较为均匀，因此，复合材料中的电子需要克服更高的势垒才能发生跃迁，其载流子定向迁移活动受到约束，进而表现为更大的电气强度。由此可见，适量的纳米ZnO填充，可以增大RTV的电气强度。
3 老化实验结果与分析
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3.1 老化试样的FTIR分析
为研究紫外老化对纳米ZnO-RTV复合材料表层化学结构的影响，采用FTIR对老化前后纳米ZnO-RTV复合材料表层的重要特征官能团进行表征分析。图6～7为各老化试样的全波段FTIR光谱，因为各曲线波形较为相似而难以直观比较，所以将老化后RTV的特征官能团图单独放大进行对比分析，其中RTV特征吸收峰及其对应基团如表3所示。
在图6的部分基团放大光谱图中，可知纯RTV在老化0～2 000 h过程中，所有特征官能团均未发生明显变化。然而，在老化2 500 h后，纯RTV的Si-(CH3)2吸收峰强度明显变弱。此外，与其他老化阶段不同的是，老化2 500 h的纯RTV试样红外光谱图出现C=O吸收峰，这反映了氧气参与到RTV老化过程中，与紫外光辐射引发生成的RTV碳链自由基发生氧化反应。单从分子链上的官能团变化情况来看，纯RTV在2 500 h时的紫外老化效应最为明显。
从图7可以看出，经过2 500 h紫外老化后，不同质量分数的纳米ZnO-RTV复合材料表层的红外特征吸收峰强度有所差异。其中，Si-(CH3)2和Si-CH3吸收峰强度随着纳米ZnO填充量的增大而增强，且在质量分数为1.0%时，吸收率最强。分析认为，虽然紫外光能使Si-C键发生断裂，但纳米ZnO吸收了大部分紫外光，一定程度上避免紫外光直接辐照RTV，从而抑制了侧甲基Si-C的脱落。此外，老化2 500 h后，不同质量分数的纳米ZnO-RTV复合材料的Si-O-Si特征吸收峰强度几乎相同，分析认为紫外光加速老化实验的紫外光主波峰（340 nm）能量为352 kJ/mol，低于RTV中Si-O的平均键能（447 kJ/mol），导致紫外光无法切断RTV主链的Si-O。与此同时，对比4种试样在2 500 h紫外老化后的C=O变化情况，发现随着纳米ZnO填充量增大，试样的C=O峰强度呈现减弱趋势，这说明纳米ZnO可有效地抑制RTV碳链自由基的产生，进而削弱RTV的光氧老化效应。
综上可见，RTV在紫外老化过程中，不仅会发生侧甲基Si-(CH3)2、Si-CH3脱落现象，还会因氧化反应产生C=O，而纳米ZnO的添加能明显抑制上述的紫外老化效应，使纳米ZnO-RTV复合材料表现出优异的抗紫外性能。
3.2 老化试样的SEM分析
利用SEM对不同质量分数的纳米ZnO-RTV复合材料表层微观形貌进行检测，以探究紫外老化对各组试样表层微观形貌的影响，并验证纳米ZnO对RTV表面紫外老化效应的削弱作用。
在0～2 500 h紫外老化条件下，纯RTV表层微观形貌图如图8所示。从图8可以看出，未老化的RTV表面较为平整光滑，但存在少许微米级别的团状物，可能是在RTV制备过程中，附着在试样表面的灰尘。紫外老化1 000 h后，纯RTV试样表面开始出现少许凸起的片状硅橡胶，但该现象不是特别明显。当紫外老化时间达2 000 h时，试样表面不仅出现块状硅橡胶脱落，还有蜷缩的条状硅橡胶，表明RTV紫外老化效应更为明显。直至老化时间达到2 500 h时，试样表面裸露着更多细碎的块状物。分析认为，长时间的紫外光辐射是造成RTV试样表层脱落老化现象的根本原因，这与FTIR表征中RTV侧甲基的断键与脱落解释相符。
老化2 500 h后，不同质量分数的纳米ZnO-RTV复合材料表层微观形貌如图9所示。从图9可以看出，与纯RTV试样表面形貌不同的是，质量分数为0.5%的纳米ZnO-RTV试样表面块状脱落物有所减少，并出现少许裸露的纳米颗粒。当纳米ZnO的质量分数增大至1.0%和2.0%时，试样微观表面的块状物与球状纳米颗粒均逐渐减少。总体上看，在2 500 h老化时间下，随着纳米ZnO填充量的增大，RTV表面微观形貌的老化效应逐渐减弱，这与3.1节FTIR测试中，纳米ZnO-RTV复合材料的Si-(CH3)2和C=O含量的变化规律相印证。
3.3 老化试样的表面静态接触角分析
为研究紫外老化对不同质量分数的纳米ZnO-RTV复合材料表面憎水性的影响，对各组试样进行表面静态接触角测试，结果如图10所示。
从图10可知，未老化的纳米ZnO-RTV复合材料表面憎水性优良，其静态接触角均在107°左右；经紫外老化后，各组试样表面静态接触角均有不同程度的下降。其中，纯RTV下降趋势最为明显，紫外老化2 500 h后，其静态接触角减小至74°，比初始状态的静态接触角小了30%；紫外老化2 500 h后，各组纳米ZnO-RTV复合材料试样的静态接触角分别为93°、96°、100°，仍保持较为良好的憎水性。总体而言，紫外老化后，纯RTV憎水性的丧失程度远大于纳米ZnO-RTV复合材料。
分析认为，RTV分子链上的侧甲基Si-(CH3)2作为强极性基团，对主链具有屏蔽作用，赋予了RTV优异的憎水性能。然而Si-(CH3)2中的C-H键能较小，长时间紫外辐射导致C-H键容易发生断裂生成CH2·等自由基，并进一步与氧气反应产生C=O等亲水基团，导致其对主链的屏蔽效应逐渐丧失，进而宏观表现为RTV静态接触角大幅减小，憎水性能显著削弱，这与3.1节FTIR分析中纯RTV的侧甲基Si-(CH3)2和C=O特征基团含量的变化规律相佐证。此外，紫外老化2 500 h后，各组纳米ZnO-RTV复合材料的表面静态接触角均远高于纯RTV，与3.2节SEM测试结果相吻合，这是因为纳米ZnO作为紫外光屏蔽剂，能够吸收或散射部分紫外光，这不仅削弱了紫外光直接辐射对RTV侧甲基的破坏，还抑制了亲水基团C=O的生成。
3.4 老化试样的热性能
采用热重分析法对不同质量分数的纳米ZnO-RTV复合材料的热降解性能进行检测分析，以研究紫外老化对各组试样热稳定性能的影响。其中， Tinitial为初始裂解温度（即10%质量损失对应的温度），Tmax为最大降解速率时的温度，M%为热重测试后试样的残留率。
0～2 500 h紫外老化过程中，纯RTV的热失重（TGA）曲线与微分热重（DTG）曲线如图11所示，表4为对应的数据。
由图11和表4可知，未老化的纯RTV试样热降解过程可分为两个阶段，第1阶段（300～430℃）主要是交联副产物和残余催化剂的裂解释放，并在相应DTG曲线中出现一个小驼峰（423.15℃），随后第2阶段在521.37℃出现最大降解速率，对应的降解物是RTV分子链。与未老化RTV试样热失重特性不同，紫外老化后RTV试样的热分解过程可分为3个阶段，分析认为长时间紫外光辐射作用，能使RTV制备过程中所残余的副产物几乎完全分解，因此第1阶段对应RTV紫外老化产生的小分子链段的热分解，第2阶段和第3阶段对应RTV长链自由基交联产物的分解释放。此外，随着老化时间的延长，3个阶段的Tmax均有所下降，但老化2 500 h试样的Tmax略微上升，这可能是因为2 500 h紫外辐射会使小分子自由基进一步聚合成较大分子量的硅氧烷。
经2 500 h紫外老化后，不同质量分数的纳米ZnO-RTV复合材料的TGA与DTG曲线如图12所示，表5为相应的数据。从表5可知，与纯RTV热失重特性不同的是，纳米ZnO-RTV复合材料的热分解过程只有两个阶段，且对应的Tmax随着纳米ZnO填充量的增大而升高，这说明纳米ZnO-RTV复合材料因紫外老化生成的小分子链段含量较低，因此其老化程度弱于纯RTV。此外，纳米ZnO-RTV复合材料的Tinitial、M%均比纯RTV高，且随着纳米ZnO填充量的增大而有所升高，这是因为纳米ZnO具备屏蔽紫外光的作用，从而抑制紫外光辐射对RTV分子链的切断，削弱纳米ZnO-RTV复合材料的紫外老化效应。
综上所述，紫外老化会破坏RTV的热稳定性能，且随着老化时间的延长，RTV的Tmax下降；但纳米ZnO的添加提高了RTV的热稳定性，且同在2 500 h紫外老化时间下，RTV的Tinitial、Tmax以及M%随纳米ZnO填充量的增大而明显提升，可见纳米ZnO-RTV复合材料具有良好的抗紫外性能。
3.5 纳米ZnO-RTV复合材料的紫外老化机理探讨
RTV的主要成分是聚二甲基硅氧烷（PDMS），其分子结构如图13所示，相对应的化学键能如表6所示。在紫外光加速老化实验后，RTV发生了不同程度的光氧老化，其根本原因是紫外线能量大于许多化学键能而切断PDMS的化学键，产生不同类型的自由基，并在氧气的作用下，发生进一步的自由基反应而生成新的化学态物质，具体老化反应式如图14所示。
320～400 nm紫外线的光子能量为380～299 kJ/mol（波长越短，光子能量越大），且照射光主波峰340 nm光子能量为352 kJ/mol，根据表6可知，紫外老化实验的辐射波段能量与Si-C、C-H和O-H的键能相近，因此长时间的紫外辐照可以切断PDMS分子链上的Si-C和C-H。
图14的光引发反应中，紫外光会引发RTV主链的自由基反应。随着自由基反应的触发，上述化学键逐渐减弱甚至断裂，PDMS分子链发生部分裂解，生成活泼自由基团～Si-CH2·、～Si·、H·和CH3·，这在侧甲基Si-(CH3)2、Si-CH3红外特征吸收峰强度明显减弱的结论中得到验证。此外，在CH3·夺取PDMS侧甲基的氢原子生成～Si-CH2·时，还会产生硅氧烷小分子链段和CH4气体，导致RTV微观形貌发生变化，如试样表面出现诸多块状脱落物，这一点在3.2节SEM分析中得到充分证明。
图14反映了自由基引发的一系列反应。自由基反应初始阶段积累的长链自由基首先发生交联反应，该反应生成的～Si-CH2-Si～低分子量聚合物不仅拓宽了RTV的分子量分布，还降低了RTV主链的平均分子量，最终导致RTV热稳定性下降，这与3.4节热稳定性能分析结论相一致。此外，～Si-CH2·在紫外辐照条件下与氧气继续发生光氧化反应，生成C=O亲水基团，微观表现为RTV表层红外特征吸收峰C=O显著增强，宏观表现为RTV表面接触角明显下降，这已在3.1节FTIR和3.3节静态接触角分析中得到相应证明。
图15为纳米ZnO-RTV复合材料抗紫外辐射机理示意图。如图15所示，纳米ZnO能够吸收紫外光并以热量形式发散，减少了紫外光对RTV主链的直接辐射，从而抑制了图14中的自由基反应。与此同时，纳米ZnO还能清除RTV主链自由基反应产生的光反应自由基，抑制主链的进一步光反应。因此，纳米ZnO的填充能够显著增强RTV的抗紫外性能。
4 结论
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针对电力设备中RTV涂料抗紫外性能差的问题，本文利用钛酸酯偶联剂对纳米ZnO进行表面改性，成功制备纳米ZnO-RTV复合材料，并进行了紫外光加速老化实验，从试样的红外特征吸收峰、表面微观形貌、表面静态接触角以及热稳定性方面，研究了纳米ZnO对RTV性能的影响，主要有以下结论：
（1）纳米ZnO能有效改善RTV的紫外光屏蔽性能，质量分数为1.0%的纳米ZnO-RTV复合材料的紫外光屏蔽率的提升幅度高达72.63%；复合材料的紫外光屏蔽率随纳米ZnO填充量的增加先升高后下降；而且掺杂适量的纳米ZnO有助于提高RTV的电气强度。
（2）长时间紫外老化后，RTV的疏水基团Si-(CH3)2、Si-CH3不仅会发生断裂，还会进一步氧化成亲水基团C=O，这导致RTV表层脱落块状物，最终宏观表现为RTV憎水性显著下降；而纳米ZnO的添加能明显削弱纳米ZnO-RTV复合材料的老化特征吸收峰强度，抑制RTV表层老化脱落，并使纳米ZnO-RTV复合材料的表面静态接触角仍保持在90°以上。
（3）紫外老化后，纳米ZnO-RTV复合材料的热稳定性明显优于纯RTV，且复合材料的初始裂解温度、最大裂解速度时温度以及残留率随着纳米ZnO填充量的增大而升高。
基金
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  • 国家自然科学基金资助项目(51977084)
  • 南方电网公司重点科技项目(080037KK52190040)
文献
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2021年第54卷第12期
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doi: 10.16790/j.cnki.1009-9239.im.2021.12.007
  • 接收时间：2021-02-01
  • 首发时间：2026-03-23
  • 出版时间：2021-12-20
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  • 收稿日期：2021-02-01
  • 修回日期：2021-02-23
基金
国家自然科学基金资助项目(51977084)
南方电网公司重点科技项目(080037KK52190040)
作者信息
    1华南理工大学，广东 广州 510641
    2广东电网有限责任公司 广州供电局电力试验研究院，广东 广州 510410

通讯作者:

谢从珍（1973-），女（汉族），陕西安康人，教授，主要从事新型功能电介质材料研发及测试、电力大数据及输配电线路防灾减灾技术的研究。
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https://castjournals.cast.org.cn/joweb/jycl/CN/10.16790/j.cnki.1009-9239.im.2021.12.007
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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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