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Article(id=1241795756147937618, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1241795749348967189, articleNumber=null, orderNo=null, doi=10.16790/j.cnki.1009-9239.im.2021.08.004, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1598112000000, receivedDateStr=2020-08-23, revisedDate=1603123200000, revisedDateStr=2020-10-20, acceptedDate=null, acceptedDateStr=null, onlineDate=1773996779715, onlineDateStr=2026-03-20, pubDate=1629388800000, pubDateStr=2021-08-20, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1773996779715, onlineIssueDateStr=2026-03-20, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1773996779715, creator=13701087609, updateTime=1773996779715, updator=13701087609, issue=Issue{id=1241795749348967189, tenantId=1146029695717560320, journalId=1149653034449285133, year='2021', volume='54', issue='8', 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=1773996778094, creator=13701087609, updateTime=1773997690758, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1241799577397953390, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1241795749348967189, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1241799577397953391, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1241795749348967189, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=24, endPage=30, ext={EN=ArticleExt(id=1241795756567368032, articleId=1241795756147937618, tenantId=1146029695717560320, journalId=1149653034449285133, language=EN, title=Effect of Size Distribution and Content of Barium Titanate on Properties of Polyvinylidene Fluoride Based Composites, columnId=1190369066675179686, journalTitle=Insulating Materials, columnName=Material Research, runingTitle=null, highlight=null, articleAbstract=

A barium titanate/polyvinylidene fluoride (BT/PVDF) composites was prepared by solution blending method, and the effect of size distribution and content of BT particles on the dielectric properties, electric strength, energy storage properties, and thermal stability of the composites were investigated. The results show that compared with single particle size BT, the synergistic effect of double particle size BT filler makes the composites have more excellent comprehensive properties, and the synergistic effect is the most remarkable when the mass ratio of BT with double size is equal to 1. With the increase of filler content, the dielectric constant and thermal stability of the composites increase, and the dielectric loss factor of the composites maintains at the relative low level. When the mass fraction of BT is 60%, and the mass ratio of BT with double size is 5∶5, the dielectric constant of BT/PVDF composites reaches 46.5 at 100 Hz, which is 5 times bigger than that of pure PVDF; the energy storage density and polarization are 0.18 J/cm3 and 0.011 9 C/m2, respectively, which are 176% and 310% higher than those of pure PVDF; the decomposition temperature corresponding to 5% of weight loss reaches 478.4℃, which is 1.3℃ and 30.3℃ higher than that of PVDF composites filled with S-BT and L-BT, respectively.

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采用溶液共混法制备了钛酸钡/聚偏氟乙烯（BT/PVDF）复合材料，研究了BT粒度分布及含量对复合材料介电性能、电气强度、储能性能和热稳定性的影响。结果表明：相较于单一粒径BT，双粒径BT共同填充的协同作用使复合材料具有更加优异的综合性能，且协同作用在两种粒径的BT等质量比时表现最为显著。随着填料含量的增加，复合材料的介电常数增大，热稳定性提升，介质损耗因数保持在相对较低的水平。当BT质量分数为60%，两种粒径BT的质量比为5∶5时，复合材料在100 Hz的介电常数达到46.5，是纯PVDF的5倍；其储能密度与极化强度分别为0.18 J/cm3和0.0119 C/m2，相比纯PVDF分别提高了176%和310%。热失重5%的分解温度达到478.4℃，分别比S-BT和L-BT单独填充的PVDF基复合材料提高了1.3℃和30.3℃。

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邓伟（1980-），女（汉族），黑龙江哈尔滨人，副教授，博士，主要从事聚合物基复合电介质材料及功能性聚合物微球的研究。
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周明（1993-），女（汉族），黑龙江佳木斯人，硕士生，主要从事高分子复合材料的研究。

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周明（1993-），女（汉族），黑龙江佳木斯人，硕士生，主要从事高分子复合材料的研究。

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周明（1993-），女（汉族），黑龙江佳木斯人，硕士生，主要从事高分子复合材料的研究。

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journalId=1149653034449285133, articleId=1241795756147937618, language=CN, orderNo=4, keyword=粒度分布), Keyword(id=1245062202714075935, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1241795756147937618, language=CN, orderNo=5, keyword=性能)], refs=[Reference(id=1245062205004165994, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1241795756147937618, doi=null, pmid=null, pmcid=null, year=2020, volume=51, issue=5, pageStart=469, pageEnd=483, url=null, language=null, rfNumber=[1], rfOrder=0, authorNames=成桑, 李雨抒, 梁家杰, journalName=高分子学报, refType=null, unstructuredReference=成桑,李雨抒,梁家杰,等.介电高分子及其纳米复合材料的电容储能应用[J].高分子学报,2020,51(5):469-483., articleTitle=介电高分子及其纳米复合材料的电容储能应用, refAbstract=null), Reference(id=1245062205113217901, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1241795756147937618, doi=null, pmid=null, pmcid=null, year=2018, volume=167, issue=null, pageStart=497, pageEnd=506, url=null, language=null, rfNumber=[2], 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钛酸钡粒度分布及含量对聚偏氟乙烯基复合材料性能的影响
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周明 1 , 邓伟 1, 2 , 王文琪 1 , 任冠纶 1 , 崔巍巍 1
绝缘材料 | 材料研究 2021,54(8): 24-30
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绝缘材料 | 材料研究 2021, 54(8): 24-30
钛酸钡粒度分布及含量对聚偏氟乙烯基复合材料性能的影响
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周明1, 邓伟1, 2, 王文琪1, 任冠纶1, 崔巍巍1
作者信息
  • 1哈尔滨理工大学 材料科学与工程学院，黑龙江 哈尔滨 150040
  • 2哈尔滨理工大学 工程电介质及其应用教育部重点实验室，黑龙江 哈尔滨 150080

    • 周明（1993-），女（汉族），黑龙江佳木斯人，硕士生，主要从事高分子复合材料的研究。

通讯作者:

邓伟（1980-），女（汉族），黑龙江哈尔滨人，副教授，博士，主要从事聚合物基复合电介质材料及功能性聚合物微球的研究。
Effect of Size Distribution and Content of Barium Titanate on Properties of Polyvinylidene Fluoride Based Composites
Ming ZHOU1, Wei DENG1, 2, Wenqi WANG1, Guanlun REN1, Weiwei CUI1
Affiliations
  • 1School of Material Science and Engineering, Harbin University of Science and Technology, Harbin 150040, China
  • 2Key Laboratory of Engineering Dielectrics and Its Application, Ministry of Education, Harbin University of Science and Technology, Harbin 150080, China
出版时间: 2021-08-20 doi: 10.16790/j.cnki.1009-9239.im.2021.08.004
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摘要
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采用溶液共混法制备了钛酸钡/聚偏氟乙烯（BT/PVDF）复合材料，研究了BT粒度分布及含量对复合材料介电性能、电气强度、储能性能和热稳定性的影响。结果表明：相较于单一粒径BT，双粒径BT共同填充的协同作用使复合材料具有更加优异的综合性能，且协同作用在两种粒径的BT等质量比时表现最为显著。随着填料含量的增加，复合材料的介电常数增大，热稳定性提升，介质损耗因数保持在相对较低的水平。当BT质量分数为60%，两种粒径BT的质量比为5∶5时，复合材料在100 Hz的介电常数达到46.5，是纯PVDF的5倍；其储能密度与极化强度分别为0.18 J/cm3和0.0119 C/m2，相比纯PVDF分别提高了176%和310%。热失重5%的分解温度达到478.4℃，分别比S-BT和L-BT单独填充的PVDF基复合材料提高了1.3℃和30.3℃。

聚偏氟乙烯  /  钛酸钡粒子  /  复合材料  /  粒度分布  /  性能

A barium titanate/polyvinylidene fluoride (BT/PVDF) composites was prepared by solution blending method, and the effect of size distribution and content of BT particles on the dielectric properties, electric strength, energy storage properties, and thermal stability of the composites were investigated. The results show that compared with single particle size BT, the synergistic effect of double particle size BT filler makes the composites have more excellent comprehensive properties, and the synergistic effect is the most remarkable when the mass ratio of BT with double size is equal to 1. With the increase of filler content, the dielectric constant and thermal stability of the composites increase, and the dielectric loss factor of the composites maintains at the relative low level. When the mass fraction of BT is 60%, and the mass ratio of BT with double size is 5∶5, the dielectric constant of BT/PVDF composites reaches 46.5 at 100 Hz, which is 5 times bigger than that of pure PVDF; the energy storage density and polarization are 0.18 J/cm3 and 0.011 9 C/m2, respectively, which are 176% and 310% higher than those of pure PVDF; the decomposition temperature corresponding to 5% of weight loss reaches 478.4℃, which is 1.3℃ and 30.3℃ higher than that of PVDF composites filled with S-BT and L-BT, respectively.

polyvinylidene fluoride  /  barium titanate particle  /  composites  /  size distribution  /  property
周明, 邓伟, 王文琪, 任冠纶, 崔巍巍. 钛酸钡粒度分布及含量对聚偏氟乙烯基复合材料性能的影响. 绝缘材料, 2021 , 54 (8) : 24 -30 . DOI: 10.16790/j.cnki.1009-9239.im.2021.08.004
Ming ZHOU, Wei DENG, Wenqi WANG, Guanlun REN, Weiwei CUI. Effect of Size Distribution and Content of Barium Titanate on Properties of Polyvinylidene Fluoride Based Composites[J]. Insulating Materials, 2021 , 54 (8) : 24 -30 . DOI: 10.16790/j.cnki.1009-9239.im.2021.08.004
正文
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0 引言
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随着储能技术的进步和电子元件向小型轻质化的发展，对电介质材料的要求不断提高[1]。具有高介电常数的电介质材料是电容器实现小尺寸、高储能密度的关键，同时较低的介质损耗可以减小使用过程中的放热和能量损失，提高器件的使用寿命和安全性[2-4]。因此，研发高介电常数、低介质损耗的电介质材料以适应电容器的发展需求，受到广泛关注。
聚合物材料由于加工性能好、介质损耗低、电气强度高、力学性能优良而广泛应用于电子、电力领域。但是，聚合物材料普遍介电常数较低。虽然陶瓷材料具有较高的介电常数，但存在介质损耗大、成型温度高、抗冲击性差、不易加工等不可忽视的缺点。陶瓷与聚合物进行复合，将二者优势互补，是目前获得性能优异的电介质材料的主要策略之一[5]。
聚合物和陶瓷填料的复合方法包括熔融共混法[6-8]、溶液共混法[9-10]和原位聚合法[11-13]等，其中溶液共混法因体系黏度低，更有利于陶瓷填料在聚合物基体中的良好分散，提升复合材料性能。为有效增强陶瓷填料与聚合物基体的相容性，对填料进行表面改性[14-16]、包覆壳层[17-19]或者多种填料共填充[20-21]，都是有效提高复合材料介电常数的方法。即使是同一种填料，形貌不同也会影响其与聚合物基体之间的界面相互作用和界面面积，表现出不同的性能变化。如LI Z Y等[22]对比了钛酸钡（BT）颗粒与BT纤维对聚偏氟乙烯-六氟丙烯共聚物（P(VDF-HFP)）性能的影响，发现在相同的填料含量下，具有高长径比的BT纤维能够有效提高复合材料的介电常数。SONG Z J等[23]为研究硫化锌（ZnS）粒径对复合材料储能性能的影响，分别制备了100 nm、500 nm和3 µm三种尺寸的ZnS粒子并与聚偏氟乙烯（PVDF）基体进行复合。结果表明，填充100 nm-ZnS的复合材料具有更高的电气强度，当100 nm-ZnS 填充量为3%时，复合材料的电气强度达到496.6 kV/mm，能量密度为6.47 J/cm3。JIANG Z H等[24]将两种不同粒径的二氧化硅（SiO2）共混物填充到聚四氟乙烯（PTFE）中，发现通过调节SiO2的粒度分布可以提高其在基体中的分散性，进而改善复合材料的介电性能和热性能。党智敏[25]制备了微-纳米BT共同填充PVDF的高介电复合材料，研究结果表明，当微-纳米BT填充量高于40%时，微-纳米BT之间的协同作用可使复合材料的介电性能和击穿性能远高于同含量单一粒径BT填充时的复合材料。
本文选用聚合物中介电常数较高的PVDF作为基体，典型的钙钛矿型陶瓷材料BT作为填料，通过改变两种粒径BT的质量配比，研究BT粒度分布及含量对BT/PVDF复合材料微观结构、介电性能、储能性能和热稳定性的影响。提出了双粒径BT共同作用的机理，提供通过控制同一填料双粒径协同作用获得综合性能优异的聚合物基复合材料的思路和方法。
1 实验
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1.1 原材料
聚偏氟乙烯（PVDF），东莞市展阳高分子材料有限公司；700 nm钛酸钡（L-BT），分析纯，上海杳田新材料科技有限公司；100 nm钛酸钡（S-BT），分析纯，上海阿拉丁生化科技股份有限公司；N,N-二甲基甲酰胺（DMF），分析纯，天津市富宇精细化工有限公司。
1.2 BT/PVDF复合材料的制备
称取10 g PVDF溶于30 mL DMF，在80℃下搅拌30 min至PVDF完全溶解。同时，按比例称取一定质量的S-BT和L-BT加入到30 mL DMF中，超声分散30 min。然后将分散均匀的BT溶液倒入PVDF溶液中，恒温搅拌3 h，流延成膜，在真空烘箱中于80℃烘干至恒重，即得到BT/PVDF复合薄膜。
将BT/PVDF复合薄膜于200℃、10 MPa下热压1 h，冷却脱模后得到BT/PVDF复合材料。固定S-BT与L-BT的质量比为5∶5，改变填料含量重复上述过程，其中BT质量分数分别为10%、20%、30%、40%、50%、60%。固定BT的质量分数为60%，改变S-BT与L-BT的质量比分别为10∶0、9∶1、7∶3、5∶5、3∶7、1∶9、0∶10。S-BT、L-BT和双粒径BT粒子共填充PVDF复合材料分别记为S-BT/PVDF、L-BT/PVDF和D-BT/PVDF。
1.3 测试方法
采用扫描电子显微镜（SEM，SU8020型，日本Hitachi公司）观察形貌，将BT/PVDF复合材料制成20 mm×2 mm的样条，在液氮中脆断后粘于样品台上进行喷金处理，加速电压为20 kV；采用X-射线衍射仪（XRD，D/MAX-3BX型，日本Rigaku公司）表征晶型，将BT/PVDF复合材料制备成15 mm×15 mm的正方形薄片，管电流为30 mA，管电压为40 kV，射线源为CuKα，波长λ为0.154 nm，扫描速率为 5°/min，扫描范围为10°～80°；采用宽频介电阻抗谱仪（HIOKI3532-50 LCR型，日置电机株式会社）测试介电性能，测试频率为102～107 Hz；采用击穿测试仪（HT-100型，机械工业电工材料产品质量监督检测中心）进行击穿性能测试，升压速率为1 kV/s，电气强度为样品被击穿时的电压与样品厚度的比值；采用热重分析仪（TGA，Pyris-Diamond型，Perkin-Elmer公司）进行热重分析，氮气保护，升温速率为10℃/min，测试温度范围为50～750℃。
2 结果与讨论
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2.1 XRD分析
PVDF和BT均具有同质多晶的性质，各晶相在电场下的极化程度不同，表现出不同的介电性能[26-28]。对纯PVDF、不同粒径的BT以及BT/PVDF复合材料进行XRD表征，结果如图1所示。
从图1可以看到，PVDF在2θ为18.4°和19.5°的衍射峰分别对应PVDF的α和β相[29]。BT颗粒具有典型的钙钛矿相结构，但两种粒径的BT表现出不同的晶相。粒径为700 nm的L-BT粒子在2θ为45°时出现双峰结构，此为｛200｝的分裂峰，即为BT晶面（200）和（002）的双峰结构，由单位晶格变形引起，是四方相BT的明显特征峰。粒径为100 nm的S-BT粒子在2θ为45°处的（200）晶面对应峰为单峰，表现为立方相结构[30]。由XRD局部放大图可以清晰看出，在D-BT/PVDF复合材料中PVDF特征峰强度随BT含量增加而减弱，当BT含量为60%时，S-BT/PVDF、L-BT/PVDF和D-BT/PVDF复合材料中的PVDF特征峰强度均明显降低，这是因为BT的加入破坏了PVDF分子链的有序排列。
2.2 形貌分析
图2为纯PVDF和BT/PVDF复合材料的断面SEM图。从图2可以看到，纯PVDF薄膜断面形貌均匀，无明显缺陷；D-BT/PVDF（m(S-BT)∶m(L-BT)=5∶5）复合材料中，填料分布较为均匀，分散性良好。在填料添加量均为60%时，对比采用不同粒径BT填充的复合材料发现，S-BT/PVDF复合材料中出现明显填料团聚现象（图2(e)）；L-BT则与聚合物基体间存在明显的空隙（图2(f)）；而D-BT/PVDF复合材料中，双粒径共同填充减少了复合材料界面缺陷，填料表现较为紧密的粒子堆积（图2(d)）。
图3为不同粒径BT填充PVDF的复合材料结构示意图。从图3(a)可以看出，S-BT粒径小，具有较大的比表面积，因而在聚合物基体中易团聚，分散性差；从图3(b)可以看出，L-BT由于粒径的增大和晶体的不规则形状与聚合物基体相容性较差，界面松散存在空隙；从图3(c)可以看出，S-BT与L-BT共填充则产生良好的协同作用，一方面L-BT在一定程度上缓解了S-BT的团聚，另一方面S-BT可填充至L-BT与聚合物基体间的空隙和缺陷中，且这种对空隙和缺陷的弥补随着填料含量的增加而变得明显，如图2(b)～(d)所示。
图4为固定BT质量分数为60%，改变BT粒度分布，即S-BT与L-BT不同质量配比获得的D-BT/PVDF复合材料的断面SEM图。从图4(a)和(b)可以看到，当100 nm的S-BT用量较少时，700 nm的L-BT与聚合物基体之间存在明显的空隙；从图4(e)可以看出，随着S-BT的占比增多，空隙被有效填充，但过多的S-BT导致团聚发生；从图4(c)和(d)可以看出，S-BT和L-BT的质量配比为5∶5和7∶3时，填料分散性良好且没有明显的界面分离。
2.3 介电性能
S-BT/PVDF、L-BT/PVDF和D-BT/PVDF复合材料的介电常数随BT含量、粒度分布和频率的变化关系如图5所示。
从图5(a)可知，无论采用何种粒径BT单独填充或双粒径共同填充，复合材料的介电常数均随填料含量的增加而增大，随频率的增大而减小，表现出典型的界面极化特性。填料用量低于50%时，在相同填料用量和频率下，相较于立方相的S-BT，四方相的L-BT更容易在电场下被极化并拥有高介电常数。随着填料用量的增加，S-BT与聚合物基体之间形成的界面增多，界面极化增强，成为复合材料介电常数提升的主要因素，故填料用量在50%以上时，S-BT/PVDF复合材料的介电常数大于L-BT/PVDF复合材料。双粒径BT共同填充体系在高填料含量下，粒径质量比为5∶5时，对复合材料介电常数提升的协同作用表现最为明显，与前文复合材料结构的SEM分析结果一致。复合材料在100 Hz下的介电常数随填料含量和粒径的变化对比列于图5(b)。从图5(b)可以看到，双粒径共同填充体系在填料含量较高时发挥明显的协同作用，填料含量为60%时，D-BT/PVDF（m(S-BT)∶m(L-BT)=5∶5）复合材料的介电常数为46.5，比S-BT/PVDF和L-BT/PVDF分别提高了50.1%和68.2%，是纯PVDF的5倍。
图6显示了BT/PVDF复合材料的介质损耗因数随BT含量、粒度分布和频率的变化关系。
从图6(a)可以看出，S-BT、L-BT和双粒径共填充的PVDF复合材料的介质损耗因数均保持较低的水平。低频下，复合材料的介质损耗因数略高于纯PVDF，此时复合材料的介质损耗因数主要源于填料与基体间的界面极化及空间电荷等引起的介电松弛，载流子在电场作用下被材料中的缺陷和界面所捕获，形成空间电荷的局部积累，造成介质损耗增大[31]。BT填料的加入使得聚合物基体相对含量减小，导致聚合物分子偶极运动引起的介质损耗被显著抑制，因此在高频下，复合材料的介质损耗因数明显降低，低于纯PVDF的介质损耗因数[32]。图6(b)为复合材料在100 Hz、100 kHz下的介质损耗因数随填料含量和粒径的变化对比。从图6(b)可以看到，复合材料的介质损耗因数具有较强的频率依赖性，随BT粒度分布和含量变化相对较小。100 Hz下，D-BT/PVDF（m(S-BT)∶m(L-BT)=5∶5）在填料含量为60%时的介质损耗因数为0.266，纯PVDF的介质损耗因数为0.035；100 kHz下D-BT/PVDF的介质损耗因数降为0.039 4，纯PVDF的介质损耗因数为0.073。
2.4 电气强度和储能性能
为探讨粒度分布对BT/PVDF复合材料击穿性能的影响，固定填料含量为60%，对S-BT、L-BT和不同质量比的复合材料进行工频耐击穿测试，采用Weibull分布对击穿数据进行处理，击穿概率为63.2%对应值为电气强度特征值，结果如图7所示。
从图7可以看出，载流子浓度和界面缺陷的增加导致复合材料的电气强度相较纯PVDF都有所下降。当S-BT与L-BT的质量比为5∶5、7∶3、9∶1时，D-BT/PVDF复合材料的电气强度相比于单一粒径BT填充的复合材料有所提升，这是双粒径BT协同作用的结果。当填料中S-BT占比较多时，能够有效减少L-BT与聚合物基体间的介电常数失配和空隙现象，降低界面处的电场畸变，抑制电树枝的发展。同时，基体中分散较为均匀的填料，使得电树枝的发展通道更为曲折，从而提高了复合材料的电气强度。如前所述，当S-BT与L-BT质量比为5∶5时，填料间的协同效应最为显著，此时复合材料的电气强度达到最大值29.60 kV/mm。
图8为PVDF、BT/PVDF复合材料储能密度和极化强度随粒度分布的变化图。储能密度和极化强度的计算公式如式（1）、（2）所示[33]。
Ue=0.5E2ε'ε0
P=Eε0(ε'-1)
式（1）～（2）中：Ue为储能密度，单位为J/cm3；P为极化强度，单位为C/m2；E为电气强度，单位为kV/mm；ε′为介电常数；ε0为真空介电常数（8.85×10-12 F/m）。根据式（1）～（2）可以看出，复合材料的储能密度和极化强度受介电常数和电气强度的共同影响。相比于纯PVDF，复合材料因介电常数较大，使其储能密度和极化强度均有所提高。从图8可以看出，在BT填充量为60%的D-BT/PVDF复合材料中，当S-BT与L-BT的质量比为5∶5、7∶3、9∶1时，复合材料的介电常数和电气强度均大于单一粒径BT填充的PVDF基复合材料，因此其储能密度和极化强度也相对较高。当S-BT与L-BT的质量比为5∶5时，复合材料的储能密度和极化强度达到最大值，分别为0.18 J/cm3和0.011 9 C/m2，相比纯PVDF提高了约176%和310%。
2.5 热稳定性
选取填料含量为20%、40%、60%的D-BT/PVDF（m(S-BT)∶m(L-BT)=5∶5）复合材料和60%的S-BT/PVDF、L-BT/PVDF复合材料进行热稳定性测试，结果如图9所示，内嵌图为温度在400～500℃的局部放大图。从图9可以看出，相比于纯PVDF，D-BT/PVDF复合材料的热分解出现明显的滞后现象，随着填料含量的增加热分解温度逐渐升高，一方面是由于BT的加入限制了PVDF分子链的运动，另一方面BT含量的增加也减少了复合材料中聚合物的占比，即减少了材料可分解的实际重量。当BT质量分数为60%时，S-BT/PVDF、L-BT/PVDF和D-BT/PVDF复合材料在热失重5%时的分解温度分别为477.1、448.1、478.4℃。L-BT粒径较大，形状不规则，与PVDF相容性差，除了不能有效限制聚合物分子链的运动外，还在复合材料中引入较多缺陷，导致填充L-BT的复合材料热稳定性较差。
3 结论
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（1）双粒径BT共同填充PVDF基体时，L-BT可以缓解S-BT的团聚；同时，S-BT可以填充到L-BT与PVDF基体之间的空隙缺陷中。双粒径共同填充的协同作用能够改善BT在PVDF中的分散性，增强BT/PVDF复合材料结构的致密性。
（2）BT/PVDF复合材料的介电常数随BT含量增加而增大，双粒径BT的协同作用在S-BT和L-BT等质量比时最为显著。频率为100 Hz，填料质量分数为60%时，D-BT/PVDF（m(S-BT)∶m(L-BT)=5∶5）复合材料介电常数为46.5，比S-BT/PVDF和L-BT/PVDF复合材料分别提高了50.1%和68.2%，是纯PVDF的5倍。在此填料含量和粒度分布下，D-BT/PVDF复合材料的电气强度为29.60 kV/mm，储能密度和极化强度分别达到0.18 J/cm3和0.011 9 C/m2，相比纯PVDF提高了176%和310%。
（3）相较于单一粒径BT填充PVDF，D-BT/PVDF复合材料表现出更优异的热稳定性，且热稳定性随着填料含量增加而增强。填料质量分数为60%时，D-BT/PVDF（m(S-BT)∶m(L-BT)=5∶5）复合材料热失重5%的分解温度为478.4℃，比S-BT和L-BT单独填充的PVDF基复合材料分别提高了1.3℃和30.3℃。
基金
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  • 黑龙江省自然科学基金联合引导项目(LH2019E059)
  • 哈尔滨理工大学理工英才计划项目(LGYC2018JC031)
文献
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2021年第54卷第8期
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doi: 10.16790/j.cnki.1009-9239.im.2021.08.004
  • 接收时间：2020-08-23
  • 首发时间：2026-03-20
  • 出版时间：2021-08-20
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  • 收稿日期：2020-08-23
  • 修回日期：2020-10-20
基金
黑龙江省自然科学基金联合引导项目(LH2019E059)
哈尔滨理工大学理工英才计划项目(LGYC2018JC031)
作者信息
    1哈尔滨理工大学 材料科学与工程学院，黑龙江 哈尔滨 150040
    2哈尔滨理工大学 工程电介质及其应用教育部重点实验室，黑龙江 哈尔滨 150080

通讯作者:

邓伟（1980-），女（汉族），黑龙江哈尔滨人，副教授，博士，主要从事聚合物基复合电介质材料及功能性聚合物微球的研究。
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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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