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Article(id=1242756903479128356, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1242756895296045592, articleNumber=null, orderNo=null, doi=10.16790/j.cnki.1009-9239.im.2021.10.005, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1608739200000, receivedDateStr=2020-12-24, revisedDate=1618329600000, revisedDateStr=2021-04-14, acceptedDate=null, acceptedDateStr=null, onlineDate=1774225935096, onlineDateStr=2026-03-23, pubDate=1634659200000, pubDateStr=2021-10-20, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1774225935096, onlineIssueDateStr=2026-03-23, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1774225935096, creator=13701087609, updateTime=1774225935096, updator=13701087609, issue=Issue{id=1242756895296045592, tenantId=1146029695717560320, journalId=1149653034449285133, year='2021', volume='54', issue='10', pageStart='1', pageEnd='109', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1774225933134, creator=13701087609, updateTime=1774226018771, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1242757254517207738, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1242756895296045592, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1242757254517207739, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1242756895296045592, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=33, endPage=40, ext={EN=ArticleExt(id=1242756903944696126, articleId=1242756903479128356, tenantId=1146029695717560320, journalId=1149653034449285133, language=EN, title=Preparation and Thermal Conductivity of Carbon Nanotubes Modified Silicon-Containing Polyarylacetylene Resin, columnId=1190369066675179686, journalTitle=Insulating Materials, columnName=Material Research, runingTitle=null, highlight=null, articleAbstract=

A triethoxyacetylenic silane (TEOAS) was synthesized to treat the surface of hydroxylated multiwalled carbon nanotubes (MWCNTs), and then the MWCNTs-T was obtained and characterized. PSA/MWCNTs and PSA/MWCNTs-T composite resins were prepared using solution method by mixing silicon-containing polyarylacetylene (PSA) with MWCNTs and MWCNTs-T, respectively. The thermal conductivity, thermal stability, electric insulation, and bending properties of the PSA/MWCNTs and PSA/MWCNTs-T composites were investigated. The results show that TEOAS was grafted on the surface of MWCNTs successfully, and MWCNTs-T is compatible with PSA matrix. The thermal conductivity of the composites increases with the increase of the mass fraction of MWCNTs and MWCNTs-T. The effect of MWCNTs-T is more obvious, with the mass fraction of 2%, the thermal conductivity of PSA/MWCNTs-T reaches 0.62 W/(m·K), which is 3 times as higher as that of PSA. The introduction of MWCNTs and MWCNTs-T can decrease the thermal stability and bending properties of PSA, the effect of MWCNTs-T is smaller than that of MWCNTs. The glass transition temperature of the PSA/MWCNTs is higher than 500℃, the electrical resistivity of the composite resin decreases linearly with the increase of frequency, while is still higher than 108 Ω·cm at 106 Hz.

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合成了三乙氧基乙炔基硅烷（TEOAS），采用TEOAS表面处理羟基化多壁碳纳米管（MWCNTs）制得MWCNTs-T，并对其进行表征。分别采用MWCNTs、MWCNTs-T与含硅芳炔树脂（PSA）通过溶液法制备了PSA/MWCNTs及PSA/MWCNTs-T复合材料，并对其导热性能、热稳定性、绝缘性能和弯曲性能等进行了研究。结果表明：TEOAS接枝到了MWCNTs表面，MWCNTs-T与PSA相容性好，复合材料的导热系数随MWCNTs及MWCNTs-T质量分数的增加而升高，其中MWCNTs-T对导热系数的提高更明显，加入2%质量分数的MWCNTs-T的复合材料导热系数达到0.62 W/(m·K)，约为PSA的3倍。MWCNTs、MWCNTs-T的加入均会使PSA的热稳定性和弯曲强度降低，但MWCNTs-T的影响低于MWCNTs。PSA/MWCNTs复合材料的玻璃化转变温度高于500℃，复合材料的电阻率随频率增加而线性下降，但频率为106 Hz时仍高于108 Ω·cm。

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王玉巧（1991-），女（汉族），河南驻马店人，硕士生，主要从事高性能高分子材料制备与应用的研究。

袁荞龙（1964-），男（汉族），江苏常州人，教授，主要从事高性能树脂的制备与性能研究。

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王玉巧（1991-），女（汉族），河南驻马店人，硕士生，主要从事高性能高分子材料制备与应用的研究。

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王玉巧（1991-），女（汉族），河南驻马店人，硕士生，主要从事高性能高分子材料制备与应用的研究。

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袁荞龙（1964-），男（汉族），江苏常州人，教授，主要从事高性能树脂的制备与性能研究。

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袁荞龙（1964-），男（汉族），江苏常州人，教授，主要从事高性能树脂的制备与性能研究。

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Thermochimica Acta,2014,590(31):66-72., articleTitle=Effect of neutral nickel catalyst on cure process of silicon-containing polyarylacetylene, refAbstract=null)], funds=[Fund(id=1245097059301310587, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756903479128356, awardId=50321042017001, language=CN, fundingSource=中央高校基本科研业务费专项资金资助项目(50321042017001), fundOrder=null, country=null)], companyList=[AuthorCompany(id=1245097052120662800, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756903479128356, xref=null, ext=[AuthorCompanyExt(id=1245097052238103315, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756903479128356, companyId=1245097052120662800, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=Key Laboratory of Specially Functional Polymeric Materials and Related Technology (Ministry of Education), School of Materials Science and Engineering, East China University of Science and Technology, Shanghai 200237, China), AuthorCompanyExt(id=1245097052246491924, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756903479128356, companyId=1245097052120662800, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=华东理工大学 材料科学与工程学院 特种功能高分子材料及相关技术教育部重点实验室，上海 200237)])], figs=[ArticleFig(id=1245097054574330826, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756903479128356, language=EN, label=Fig.1, caption=Chemical structure of PSA, figureFileSmall=xOplO3wqL0KYOGNO4S4YKg==, figureFileBig=QVmeMSH1JNpvraEyuHgnRQ==, tableContent=null), ArticleFig(id=1245097054662411217, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756903479128356, language=CN, label=图1, caption=PSA的化学结构式, figureFileSmall=xOplO3wqL0KYOGNO4S4YKg==, figureFileBig=QVmeMSH1JNpvraEyuHgnRQ==, tableContent=null), 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articleId=1242756903479128356, language=CN, label=图3, caption=TEOAS改性复合材料界面机理示意图, figureFileSmall=ygJ2IomT+ZsQHIbmjylB2w==, figureFileBig=z/PcG2/hHsfj1Dw3BJPxpw==, tableContent=null), ArticleFig(id=1245097056558236658, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756903479128356, language=EN, label=Fig.4, caption=XPS spectra of MWCNTs and MWCNTs-T, figureFileSmall=D+Ldr7bqvHXhvvnpMQ1eTg==, figureFileBig=oZkGc7W6+NZeCqtXh1abkQ==, tableContent=null), ArticleFig(id=1245097056675677173, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756903479128356, language=CN, label=图4, caption=MWCNTs和MWCNTs-T的XPS谱图, figureFileSmall=D+Ldr7bqvHXhvvnpMQ1eTg==, figureFileBig=oZkGc7W6+NZeCqtXh1abkQ==, tableContent=null), ArticleFig(id=1245097056751174650, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756903479128356, language=EN, label=Fig.5, caption=Curves fitting of C1s spectra of MWCNTs-T, 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label=Fig. 10, caption=DMA curves of the cured PSA and PSA/MWCNTs composites, figureFileSmall=DH1aA/c+Topq9LqEJUy2Kg==, figureFileBig=4z3BwzNJRM+x3RTkF/Verg==, tableContent=null), ArticleFig(id=1245097057850081330, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756903479128356, language=CN, label=图10, caption=PSA及PSA/MWCNTs复合树脂固化物的DMA曲线, figureFileSmall=DH1aA/c+Topq9LqEJUy2Kg==, figureFileBig=4z3BwzNJRM+x3RTkF/Verg==, tableContent=null), ArticleFig(id=1245097057925578805, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756903479128356, language=EN, label=Tab.1, caption=Surface element analysis of MWCNTs and MWCNTs-T, figureFileSmall=null, figureFileBig=null, tableContent=
增强体含量/%
ClsOlsSi2p
MWCNTs95.334.670.00
MWCNTs-T94.334.920.75
), ArticleFig(id=1245097058005270586, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756903479128356, language=CN, label=表1, caption=

MWCNTs和MWCNTs-T的表面元素分析

, figureFileSmall=null, figureFileBig=null, tableContent=
增强体含量/%
ClsOlsSi2p
MWCNTs95.334.670.00
MWCNTs-T94.334.920.75
), ArticleFig(id=1245097058080768062, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756903479128356, language=EN, label=Tab.2, caption=Fitting spectra data of Cls, figureFileSmall=null, figureFileBig=null, tableContent=
键合能/eV官能团相对含量/%
MWCNTsMWCNTs-T
284.44-C-C-10089.01
286.28-C-O-—8.36
288.62-C≡C-—2.63
), ArticleFig(id=1245097058156265539, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756903479128356, language=CN, label=表2, caption=

C1s拟合图谱数据

, figureFileSmall=null, figureFileBig=null, tableContent=
键合能/eV官能团相对含量/%
MWCNTsMWCNTs-T
284.44-C-C-10089.01
286.28-C-O-—8.36
288.62-C≡C-—2.63
), ArticleFig(id=1245097058240151625, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756903479128356, language=EN, label=Tab.3, caption=DSC data of PSA/MWCNTs-T, figureFileSmall=null, figureFileBig=null, tableContent=
样品Ti/℃Tp/℃ΔH/(J/g)
PSA212241444
PSA/MWCNTs-T0.5197249597
PSA/MWCNTs-T1.0198249493
PSA/MWCNTs-T1.5218251490
PSA/MWCNTs-T2.0216260510
PSA/MWCNTs-T2.5217262515
), ArticleFig(id=1245097058378563663, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756903479128356, language=CN, label=表3, caption=

PSA/MWCNTs-T的DSC数据

, figureFileSmall=null, figureFileBig=null, tableContent=
样品Ti/℃Tp/℃ΔH/(J/g)
PSA212241444
PSA/MWCNTs-T0.5197249597
PSA/MWCNTs-T1.0198249493
PSA/MWCNTs-T1.5218251490
PSA/MWCNTs-T2.0216260510
PSA/MWCNTs-T2.5217262515
), ArticleFig(id=1245097058525364307, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756903479128356, language=EN, label=Tab.4, caption=Thermal conductivity of PSA/MWCNTs and PSA/MWCNTs-T composites, figureFileSmall=null, figureFileBig=null, tableContent=
填料质量分数/%导热系数/(W/(m·K))
PSA/MWCNTsPSA/MWCNTs-T
0.50.250.32
1.00.320.39
1.50.430.51
2.00.520.62
2.50.480.55
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PSA/MWCNTs和PSA/MWCNTs-T的导热系数

, figureFileSmall=null, figureFileBig=null, tableContent=
填料质量分数/%导热系数/(W/(m·K))
PSA/MWCNTsPSA/MWCNTs-T
0.50.250.32
1.00.320.39
1.50.430.51
2.00.520.62
2.50.480.55
), ArticleFig(id=1245097058760245345, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756903479128356, language=EN, label=Tab.5, caption=TGA analysis results of cured PSA/MWCNTs and PSA/MWCNTs-T composites, figureFileSmall=null, figureFileBig=null, tableContent=
样品Td5/℃Yr800℃/%样品Td5/℃Yr800℃/%
PSA62892.1PSA62892.1
PSA/MWCNTs-0.557189.7PSA/MWCNTs-T0.557089.5
PSA/MWCNTs-1.054688.5PSA/MWCNTs-T1.057788.5
PSA/MWCNTs-1.553388.0PSA/MWCNTs-T1.553088.0
PSA/MWCNTs-2.052486.8PSA/MWCNTs-T2.058189.9
PSA/MWCNTs-2.545281.4PSA/MWCNTs-T2.553488.0
), ArticleFig(id=1245097058877685863, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756903479128356, language=CN, label=表5, caption=

PSA/MWCNTs和PSA/MWCNTs-T固化物的TGA数据

, figureFileSmall=null, figureFileBig=null, tableContent=
样品Td5/℃Yr800℃/%样品Td5/℃Yr800℃/%
PSA62892.1PSA62892.1
PSA/MWCNTs-0.557189.7PSA/MWCNTs-T0.557089.5
PSA/MWCNTs-1.054688.5PSA/MWCNTs-T1.057788.5
PSA/MWCNTs-1.553388.0PSA/MWCNTs-T1.553088.0
PSA/MWCNTs-2.052486.8PSA/MWCNTs-T2.058189.9
PSA/MWCNTs-2.545281.4PSA/MWCNTs-T2.553488.0
), ArticleFig(id=1245097058974154858, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756903479128356, language=EN, label=Tab.6, caption=Flexural properties of cured PSA, PSA/MWCNTs, and PSA/MWCNTs-T composites, figureFileSmall=null, figureFileBig=null, tableContent=
样品弯曲强度/MPa弯曲模量/GPa
PSA21.73±3.232.63±0.12
PSA/MWCNTs-0.521.11±1.663.19±0.23
PSA/MWCNTs -1.022.42±1.132.97±0.28
PSA/MWCNTs -1.518.71±1.832.93±0.15
PSA/MWCNTs -2.014.67±1.502.58±0.15
PSA/MWCNTs-T0.521.37±1.563.13±0.10
PSA/MWCNTs-T1.023.18±1.433.36±0.24
PSA/MWCNTs-T1.521.13±1.933.27±0.25
PSA/MWCNTs-T2.020.51±1.543.03±0.19
), ArticleFig(id=1245097059091595377, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756903479128356, language=CN, label=表6, caption=

PSA及复合树脂浇注体的弯曲性能数据

, figureFileSmall=null, figureFileBig=null, tableContent=
样品弯曲强度/MPa弯曲模量/GPa
PSA21.73±3.232.63±0.12
PSA/MWCNTs-0.521.11±1.663.19±0.23
PSA/MWCNTs -1.022.42±1.132.97±0.28
PSA/MWCNTs -1.518.71±1.832.93±0.15
PSA/MWCNTs -2.014.67±1.502.58±0.15
PSA/MWCNTs-T0.521.37±1.563.13±0.10
PSA/MWCNTs-T1.023.18±1.433.36±0.24
PSA/MWCNTs-T1.521.13±1.933.27±0.25
PSA/MWCNTs-T2.020.51±1.543.03±0.19
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碳纳米管改性含硅芳炔树脂的制备与导热性能
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王玉巧 , 袁荞龙 , 黄发荣
绝缘材料 | 材料研究 2021,54(10): 33-40
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绝缘材料 | 材料研究 2021, 54(10): 33-40
碳纳米管改性含硅芳炔树脂的制备与导热性能
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王玉巧, 袁荞龙, 黄发荣
作者信息
  • 华东理工大学 材料科学与工程学院 特种功能高分子材料及相关技术教育部重点实验室，上海 200237

    • 王玉巧（1991-），女（汉族），河南驻马店人，硕士生，主要从事高性能高分子材料制备与应用的研究。

    袁荞龙（1964-），男（汉族），江苏常州人，教授，主要从事高性能树脂的制备与性能研究。

Preparation and Thermal Conductivity of Carbon Nanotubes Modified Silicon-Containing Polyarylacetylene Resin
Yuqiao WANG, Qiaolong YUAN, Farong HUANG
Affiliations
  • Key Laboratory of Specially Functional Polymeric Materials and Related Technology (Ministry of Education), School of Materials Science and Engineering, East China University of Science and Technology, Shanghai 200237, China
出版时间: 2021-10-20 doi: 10.16790/j.cnki.1009-9239.im.2021.10.005
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摘要
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合成了三乙氧基乙炔基硅烷（TEOAS），采用TEOAS表面处理羟基化多壁碳纳米管（MWCNTs）制得MWCNTs-T，并对其进行表征。分别采用MWCNTs、MWCNTs-T与含硅芳炔树脂（PSA）通过溶液法制备了PSA/MWCNTs及PSA/MWCNTs-T复合材料，并对其导热性能、热稳定性、绝缘性能和弯曲性能等进行了研究。结果表明：TEOAS接枝到了MWCNTs表面，MWCNTs-T与PSA相容性好，复合材料的导热系数随MWCNTs及MWCNTs-T质量分数的增加而升高，其中MWCNTs-T对导热系数的提高更明显，加入2%质量分数的MWCNTs-T的复合材料导热系数达到0.62 W/(m·K)，约为PSA的3倍。MWCNTs、MWCNTs-T的加入均会使PSA的热稳定性和弯曲强度降低，但MWCNTs-T的影响低于MWCNTs。PSA/MWCNTs复合材料的玻璃化转变温度高于500℃，复合材料的电阻率随频率增加而线性下降，但频率为106 Hz时仍高于108 Ω·cm。

含硅芳炔树脂  /  乙炔基三乙氧基硅烷  /  多壁碳纳米管  /  导热  /  热-物理性能

A triethoxyacetylenic silane (TEOAS) was synthesized to treat the surface of hydroxylated multiwalled carbon nanotubes (MWCNTs), and then the MWCNTs-T was obtained and characterized. PSA/MWCNTs and PSA/MWCNTs-T composite resins were prepared using solution method by mixing silicon-containing polyarylacetylene (PSA) with MWCNTs and MWCNTs-T, respectively. The thermal conductivity, thermal stability, electric insulation, and bending properties of the PSA/MWCNTs and PSA/MWCNTs-T composites were investigated. The results show that TEOAS was grafted on the surface of MWCNTs successfully, and MWCNTs-T is compatible with PSA matrix. The thermal conductivity of the composites increases with the increase of the mass fraction of MWCNTs and MWCNTs-T. The effect of MWCNTs-T is more obvious, with the mass fraction of 2%, the thermal conductivity of PSA/MWCNTs-T reaches 0.62 W/(m·K), which is 3 times as higher as that of PSA. The introduction of MWCNTs and MWCNTs-T can decrease the thermal stability and bending properties of PSA, the effect of MWCNTs-T is smaller than that of MWCNTs. The glass transition temperature of the PSA/MWCNTs is higher than 500℃, the electrical resistivity of the composite resin decreases linearly with the increase of frequency, while is still higher than 108 Ω·cm at 106 Hz.

silicon-containing polyarylacetylene  /  triethoxyacetylenic silane  /  multiwall carbon nanotube  /  thermal conductivity  /  thermophysical property
王玉巧, 袁荞龙, 黄发荣. 碳纳米管改性含硅芳炔树脂的制备与导热性能. 绝缘材料, 2021 , 54 (10) : 33 -40 . DOI: 10.16790/j.cnki.1009-9239.im.2021.10.005
Yuqiao WANG, Qiaolong YUAN, Farong HUANG. Preparation and Thermal Conductivity of Carbon Nanotubes Modified Silicon-Containing Polyarylacetylene Resin[J]. Insulating Materials, 2021 , 54 (10) : 33 -40 . DOI: 10.16790/j.cnki.1009-9239.im.2021.10.005
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0 引言
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含硅芳炔树脂（PSA）是芳基乙炔主链上引入硅原子的一类有机无机杂化树脂，其加工性能、力学性能和热性能等都优于芳基乙炔树脂。20世纪90年代以来，日本M ITOH等[1-4]对含硅芳炔树脂的合成、结构与性能等开展了深入研究。1998年后国内在芳基乙炔树脂研究的基础上开始研究含硅芳炔树脂的制备和性能，对不同结构的芳基二乙炔和二氯硅烷聚合的含硅芳炔树脂的性能进行了深入研究[5-10]，发现固化后含硅芳炔树脂在氮气中具有出色的热稳定性（5%热失重温度为631℃，800℃残留率为90%）[11]。含硅芳炔树脂主链上硅原子的电子轨道和碳碳三键电子轨道及芳基电子轨道间可通过(d-p)π交叠获得σ*-π超共轭而允许电荷输送，电子在主链上的传输使得含硅芳炔树脂在光电性能和辐照性能等方面有其特色[12-13]。含硅芳炔树脂在热环境中，除了原子的晶格振动形式（晶格波-声子）可传导热，主链上因共轭离域的电子也可实现热量的传输。在含硅芳炔树脂中加入无机的导热颗粒氮化铝（AlN）形成导热回路可使其导热系数由0.2 W/(m·K)提升至2.36 W/(m·K)[14]。
S LIJIMA[15]于1991年首次发现碳纳米管（CNTs），这种大长径比无缝管状结构的一维材料是由六元环构成的石墨片层结构沿一定轴向卷曲而成，其自身的特殊结构赋予了碳纳米管特殊的光、磁、电、热、化学以及力学性能等，开拓了其在结构与功能材料等方面的应用[16]。在聚合物材料中加入少量的碳纳米管，可在保持聚合物成型加工容易、密度低等优良性质的同时提高复合材料的导热导电性能[17-19]。为了减少纳米尺度的MWCNTs团聚现象，提高其与PSA树脂之间界面结合，本研究合成了三乙氧基乙炔基硅烷（TEOAS）对羟基化多壁碳纳米管（MWCNTs）进行表面改性，并采用表面改性处理的MWCNTs填充改性PSA树脂，研究改性PSA的导热性能、耐高温性能和力学性能等。
1 实验
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1.1 原材料
乙炔基溴化镁，AR，百灵威化学技术有限公司；三乙氧基氯硅烷、乙醇，AR，上海泰坦科技股份有限公司；正己烷，AR，上海阿拉丁生化科技股份有限公司；羟基化多壁碳纳米管（MWCNTs），上海麦克林生化科技有限公司；冰乙酸，AR，摩贝（上海）生物科技有限公司；液氮，纯度＞99.999%，液化空气(上海)压缩气体有限公司。三乙氧基乙炔基硅烷（TEOAS）参照文献[20]在实验室合成，产率为83%。含硅芳炔树脂（PSA），实验室自制，Mn=3380，PDI=1.63（GPC法），结构式如图1所示。
1.2 测试表征
核磁共振氢谱（1H-NMR）测试仪器为德国BRUKER公司的AVANCE 400型超导傅里叶变换核磁共振波谱仪，内标为四甲基硅烷，氘代氯仿为溶剂，工作频率为400 MHz。红外光谱（FTIR）测试仪器为美国NICOLET公司的AVATAR 360型红外光谱仪，固体样品采用KBr压片法制样，液体样品采用涂膜法制样，扫描范围为4 000～700 cm-1，分辨率为4 cm-1，对样品进行32次扫描。激光显微拉曼光谱测试仪器为英国雷尼绍公司的iuvia refl型激光显微拉曼光谱仪，光谱范围为4 000～100 cm-1，激光波长为532 nm，光谱分辨率为1 cm-1，样品用量为1～2 mg。X射线光电子能谱（XPS）测试仪器为美国ThermoFisher公司的ESCALAB 250XI型X射线光电子能谱仪，单色Al Kα（hv=1 486.6 eV），工作功率为150 W，束斑为500 μm，能量分析器透过能为30 eV，以C1s=284.6 eV为基准进行结合能校正，利用XPS Peak4.1软件进行分峰拟合。样品密度采用日本MatsuHaku公司的MH-124S型密度天平测得。样品导热系数采用德国耐驰公司的LFA447型氙灯导热仪测得，试样直径为12.5 mm，厚度为1～ 2 mm。树脂的固化采用美国TA公司的Q-2000型差示扫描量热仪（DSC）研究，在氮气氛围程序升温，氮气流量为50 mL/min，升温速率为10℃/min，温度范围为40～400℃，样品用量为1～2 mg。样品的热失重分析（TGA）测试仪器为Mettler Toledo公司的TGA/DSC 1型热重同步热分析仪，升温速率为10℃/min，温度范围为室温至1 000℃，氮气气氛，氮气流速为50 mL/min。固化树脂的动态热力学分析（DMA）测试仪器为Mettler Toledo公司的DMA1型动态热力学分析仪，用3点弯曲模式测定，升温速率为3 ℃/min，温度范围为40～500℃，振动频率为1 Hz。样品介电性能测试仪器为德国NOVOCONTROL公司的Concept 40 型宽频介电阻抗谱仪，测试频率范围为30 μHz～10 MHz，样品为光滑平整的圆片，直径为30 mm，厚度为1～2 mm。树脂浇注体的弯曲性能采用深圳新三思材料检测有限公司的SANS CMT 4204型微机调控电子万能试验机按GB/T 2567—2008在常温下进行测试，每组测试样品5～7个，结果取平均值。
1.3 MWCNTs的表面处理
以四氢呋喃（THF）为溶剂，称取一定质量的TEOAS放于四口烧瓶中，搅拌使TEOAS溶解，加入少量乙酸调节溶液呈弱酸性，在30℃下搅拌使其水解，之后加入适量MWCNTs粉末，在50℃下搅拌 2 h。冷却后进行抽滤，并用THF进行多次洗涤后，将MWCNTs放入到烘箱中真空干燥，并放在干燥器中保存备用。将处理过的羟基化碳纳米管标记为MWCNTs-T。
1.4 复合材料的制备
称取适量的MWCNTs于250 mL四口烧瓶中，加入100 mL的THF，边高速机械搅拌边超声1 h，然后加入PSA树脂，待体系均匀混合后移去超声，换上油浴加热，减压蒸馏30 min，脱除THF得到黑色的黏稠状复合材料。PSA复合材料中MWCNTs的质量分数分别为0、0.5%、1.0%、1.5%、2.0%、2.5%，分别记作PSA、PSA/MWCNTs-0.5、PSA/MWCNTs-1.0、PSA/MWCNTs-1.5、PSA/MWCNTs-2.0、PSA/MWCNTs-2.5。相应地，用质量分数分别为0.5%、1.0%、1.5%、2.0%和2.5%的MWCNTs-T改性PSA，记为PSA/MWCNTs-T0.5、PSA/MWCNTs-T1.0、PSA/MWCNTs-T1.5、PSA/MWCNTs-T2.0和PSA/MWCNTs -T2.5。
1.5 PSA/MWCNTs浇注体的制备
首先用细砂纸打磨模具，均匀喷涂脱模剂，将模具放入130℃烘箱中预热1 h。称取一定质量的PSA/MWNCTs树脂放入烘箱熔融后浇注入模具，移至真空烘箱内在120℃下真空脱泡3～5 h，然后转移至高温烘箱内进行固化，固化工艺由DSC测试分析结果确定。固化结束后自然冷却至室温并脱模得到固化物，用砂纸对浇注体进行打磨至测试标准的尺寸。
2 结果与讨论
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2.1 MWCNTs的表面改性
图2为MWCNTs的拉曼光谱图，图中1 360 cm-1处归为D峰（碳纳米管的缺陷），1 578 cm-1处是G峰（碳纳米管的石墨结构）[21]。从图2可以看出，D峰的强度（1 960.66）大于G峰的强度（1 898.22），D峰和G峰的峰强之比R为1.03，D峰面积（51.03）和G峰面积（48.97）之比为1.04，说明实验所用的MWCNTs石墨结构不是很完整，缺陷较多。
TEOAS中的乙氧基基团在酸性环境下水解后可与羟基化碳纳米管表面上的羟基形成氢键和缩合形成化学键而接枝到MWCNTs的表面。接枝在MWCNTs表面TEOAS中的乙炔基基团受热固化时可与PSA树脂中乙炔基发生一定程度的Diels-Alder化学反应、环三聚化学反应和偶合反应，使得MWCNTs表面与PSA基体间形成一定的化学桥接，从而提高MWCNTs和PSA树脂的相容性及其在PSA中的分散性。图3是TEOAS增强改性PSA/MWCNTs复合材料的界面作用。
对TEOAS改性前后的羟基化多壁碳纳米管进行XPS测试，结果如图4所示，表1是改性前后MWCNTs表面元素的含量。从图4可以明确观察到，经表面改性后MWCNTs的XPS图谱中多了100 cm-1波数处Si元素的峰位，这是少量硅烷偶联剂改性MWCNTs后在其表面存在的硅。从表1可以看出，经表面改性后MWCNTs表面中Si元素含量由0增加至0.75%，O元素含量从4.67%增加到4.92%。
图5是MWCNTs-T的C1s拟合图谱，表2为拟合图谱中基团对应的数据。从表2可以看出，改性MWCNTs的表面基团主要为-C-C-（284.44 eV）、-C-O-（286.28 eV）和-C≡C-（288.62 eV），其相对含量分别为89.01%、8.36%和2.63%。谱图中-C≡C-峰的出现说明MWCNTs表面已经接枝TEOAS。
2.2 PSA/MWCNTs-T的固化
PSA/MWCNTs-T复合材料的固化反应采用DSC进行分析，结果见图6和表3。从图6和表3可以看出，当MWCNTs-T的质量分数小于1.0%时，复合材料固化的起始温度（Ti）低于PSA树脂，当MWCNTs-T的质量分数大于1.0%时，复合材料固化的Ti稍高于PSA树脂。PSA和MWCNTs-T共混后复合材料的热固化峰值温度（Tp）都比纯PSA固化物的高，且随着MWCNTs-T质量分数的增加，固化峰值温度呈升高趋势。PSA/MWCNTs-T复合材料的放热焓（ΔH）均高于纯PSA树脂的放热焓。由DSC分析可知PSA/MWCNTs-T复合材料的总体固化参数与PSA树脂相近，因此采用PSA树脂的固化工艺，即按照170℃/2 h+210℃/2 h+250℃/4 h进行固化。
2.3 复合材料的导热性能
图7是改性前后MWCNTs质量分数对PSA/MWCNTs复合材料固化物导热系数的影响，数据列于表4中。由图7和表4可以看出，PSA树脂的导热系数为0.21 W/(m·K)，随着混入MWCNTs质量分数的增加，PSA/MWCNTs复合材料的导热系数先增大后减小。当MWCNTs质量分数为2.0%时，复合材料的导热系数可增大至0.52 W/(m·K)。当MWCNTs质量分数较少时，导热的MWCNTs之间相互接触不多，未能形成有效导热回路。随着MWCNTs质量分数的增加，碳纳米管之间接触增加，形成一定的回路，导热系数增大。当MWCNTs的质量分数继续增加时，MWCNTs的团聚使有效导热网链减少，同时造成内部缺陷，因而导热系数减小。
为了减弱纳米微粒团聚的负面影响，采用MWCNTs-T改性PSA。从图7和表4可以看出，相同填料质量分数下，PSA/MWCNTs-T的导热系数比PSA/MWCNTs有一定程度的提升。但是MWCNTs-T的质量分数对复合材料导热系数的影响与MWCNTs的影响趋势相同，PSA/MWCNTs-T2.0复合材料的导热系数最大，为0.62 W/(m·K)，约为纯PSA导热系数的3倍。说明偶联剂改性对于MWCNTs的团聚现象有一定改善作用，接枝含炔基偶联剂TEOAS的MWCNTs加入PSA树脂中可提高MWCNTs与PSA树脂间的相容性，有助于MWCNTs在PSA基体中的分散形成导热回路，界面作用的增加也有助于增加MWCNTs-T与树脂间的界面面积，从而提高热传导。
2.4 复合材料的热稳定性
对PSA/MWCNTs和PSA/MWCNTs-T复合材料固化物进行TGA测试，图8为复合材料固化物的TGA曲线，数据列于表5中。从图8和表5可以看出，复合材料的耐热性随着碳纳米管添加量的增加而降低，PSA/MWCNTs-2.5在氮气中的5%热失重温度（Td5）和800℃残留率（Yr800℃）分别为452℃和81.4%，相比PSA的Td5（628℃）和Yr800℃（92.1%），耐热性明显降低。而PSA/MWCNTs-T的热稳定性也下降，PSA/MWCNTs-T2.5的Td5和Yr800℃分别下降到534℃和88.0%，明显高于PSA/MWCNTs-2.5。说明偶联剂TEOAS对MWCNTs的表面处理可明显改善复合树脂的耐热性，也说明碳纳米管的团聚和与树脂基体的界面作用对PSA树脂热稳定性的影响显著。表面含乙炔基的MWCNTs-T与PSA相容性好，分散较匀，对PSA树脂的固化反应影响较小，且还参与PSA的固化。
2.5 复合材料的电性能
图9为PSA/MWCNTs和PSA/MWCNTs-T的电阻率随频率的变化图。从图9可以看出，PSA/MWCNTs和PSA/MWCNTs-T的电阻率均随频率的增大而降低，当频率达106 Hz时改性PSA树脂的电阻率仍有108 Ω·cm以上。PSA/MWCNTs的电阻率随MWCNTs质量分数的增加而降低，这是分散在PSA中的MWCNTs导电特性所致。PSA/MWCNTs-T的电阻率随着MWCNTs-T质量分数的增加变化不大，在MWCNTs-T质量分数达到2.0%时出现明显降低，与PSA/MWCNTs-2.5的变化相近，这也反映出MWCNTs-T在PSA中分散均匀且形成了回路，使改性PSA的电阻率下降。
2.6 复合材料的力学性能
图10为纯PSA树脂和PSA/MWCNTs复合材料固化物的动态热力学（DMA）曲线。从图10可以看出，在温度低于280℃时PSA的储能模量E′有稍微下降趋势，随后呈上升趋势。温度的升高会导致未交联部分的链段发生运动，因而其储能模量变小；温度超过280℃之后，树脂中的内炔进行固化交联，因此E′上升[22]。从图10还可以看出，不同质量分数MWCNTs改性PSA树脂固化物的储能模量随着温度的变化趋势与PSA基本相同，也是随温度升高先缓慢下降，至280℃后随内炔的进一步固化交联而上升。PSA树脂和PSA/MWCNTs树脂的损耗因子（tanδ）在温度低于500℃时基本没变化，没有出现明显的主松弛损耗峰，即与tanδ主松弛峰峰值温度对应的玻璃化转变温度未出现，说明PSA/MWCNTs的玻璃化转变温度高于500℃。
表6是PSA/MWCNTs和PSA/MWCNTs-T树脂浇注体的弯曲性能。从表6可以看出，PSA/MWCNTs-1.0树脂的弯曲性能略高于PSA树脂，其余PSA/MWCNT树脂的弯曲性能整体低于PSA树脂；PSA/MWCNTs-T树脂浇注体的弯曲强度与PSA树脂浇注体相近，弯曲模量高于PSA树脂。说明MWCNTs-T与PSA树脂的界面作用较好，不同质量分数MWCNTs-T/PSA树脂浇注体的力学性能变化不大。
3 结论
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（1）合成了含有乙炔基的硅烷偶联剂TEOAS，用于对MWCNTs进行表面处理，TEOAS成功接枝在MWCNTs表面。
（2）PSA树脂的导热系数随着MWCNTs和MWCNTs-T质量分数的增大先增大后减小，PSA/MWCNTs-T的导热系数比PSA/MWCNTs树脂的大，PSA/MWCNTs-T2.0树脂固化物的导热系数达到0.62 W/(m·K)。
（3）PSA/MWCNTs和PSA/MWCNTs-T树脂固化物的热稳定性低于纯PSA树脂，且均随填料质量分数的增加而降低，但PSA/MWCNTs-T树脂热稳定性的下降程度低于PSA/MWCNTs树脂。
（4）PSA/MWCNTs和PSA/MWCNTs-T树脂固化物的电阻率均随频率增加而线性下降，但至106 Hz时复合材料的电阻率仍高于108 Ω·cm。
（5）PSA树脂和PSA/MWCNTs树脂固化物玻璃化转变温度高于500℃，PSA/MWCNTs树脂弯曲强度相对PSA降低，仅PSA/MWCNTs-1.0浇注体的弯曲性能略有增加；PSA/MWCNTs-T树脂的弯曲强度相对PSA变化较小，而弯曲模量有所提高。
基金
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  • 中央高校基本科研业务费专项资金资助项目(50321042017001)
文献
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参考文献 引证文献
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2021年第54卷第10期
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doi: 10.16790/j.cnki.1009-9239.im.2021.10.005
  • 接收时间：2020-12-24
  • 首发时间：2026-03-23
  • 出版时间：2021-10-20
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  • 收稿日期：2020-12-24
  • 修回日期：2021-04-14
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中央高校基本科研业务费专项资金资助项目(50321042017001)
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    华东理工大学 材料科学与工程学院 特种功能高分子材料及相关技术教育部重点实验室，上海 200237
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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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