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Article(id=1242756977798000709, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1242756974576775191, articleNumber=null, orderNo=null, doi=10.16790/j.cnki.1009-9239.im.2021.11.018, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1608480000000, receivedDateStr=2020-12-21, revisedDate=1611244800000, revisedDateStr=2021-01-22, acceptedDate=null, acceptedDateStr=null, onlineDate=1774225952776, onlineDateStr=2026-03-23, pubDate=1637510400000, pubDateStr=2021-11-22, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1774225952776, onlineIssueDateStr=2026-03-23, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1774225952776, creator=13701087609, updateTime=1774225952776, updator=13701087609, issue=Issue{id=1242756974576775191, tenantId=1146029695717560320, journalId=1149653034449285133, year='2021', volume='54', issue='11', pageStart='1', pageEnd='139', issueExtLink='null', onlineDate='null', pubDate='1637510400000', pubDateStr='2021-11-22', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1774225952044, creator='13701087609', updateTime=1774226047274, updator='13701087609', preIssue=null, nextIssue=null, articleTotal=null, ext={EN=IssueExt(id=1242757374059066044, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1242756974576775191, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1242757374059066045, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1242756974576775191, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null, downloadFileDto=null}, startPage=126, endPage=129, ext={EN=ArticleExt(id=1242756980767568015, articleId=1242756977798000709, tenantId=1146029695717560320, journalId=1149653034449285133, language=EN, title=Preparation and Properties of GO/PI Composite Film, columnId=1198664996516360309, journalTitle=Insulating Materials, columnName=Polyimide Film Special Issue, runingTitle=null, highlight=null, articleAbstract=

A graphene oxide (GO) was synthesized by modified Hummers’ method, and a graphene oxide/polyimide (GO/PI) composite film was prepared by solution blending method. The structure and the properties of the composite film were analyzed by XRD, TMA, TGA. The results show that compared with the PI film without GO, when the mass fraction of GO in composite film is 0.2%, the mechanical properties of the composite film increase obviously, the tensile strength increases by 26.77%, the elongation at break increases by 76.47%, and the elastic modulus changes little basically. When the mass fraction of GO is 0.1%, the maximum value of T5 and T10 of the composite film are 587.3℃ and 603.3℃, which increase by 2.44% and 1.69% compared with that of the PI film without GO, respectively. It is indicated that the addition of GO with appropriate amount can enhance the mechanical properties and thermal properties of PI films.

, authors=null, authorsList=Songfeng HAN, Bilian TANG, Bing ZHANG, Chuanguo MA, Shuanggui QING, authorCompany=null, correspAuthors=null, authorNote=null, correspAuthorsNote=null, copyrightStatement=null, copyrightOwner=null, extLink=null, articleAbsUrl=null, sourceXml=null, magXml=null, pdfUrl=null, pdf=null, pdfFileSize=null, pdfExtLink=null, richHtmlUrl=null, mobilePdfUrl=null, reviewReport=null, pdfFirstPage=null, abstractGraph=null, abstractGraphContent=null, abstractVideo=null, citation=null, cebUrl=null, magXmlContent=null, mapNumber=null, fund=null), CN=ArticleExt(id=1242756984974455152, articleId=1242756977798000709, tenantId=1146029695717560320, journalId=1149653034449285133, language=CN, title=GO/PI复合薄膜的制备及性能研究, columnId=1198664997682376829, journalTitle=绝缘材料, columnName=聚酰亚胺薄膜专题, runingTitle=null, highlight=null, articleAbstract=

利用改进Hummers法制备氧化石墨烯（GO），再通过溶液共混法制备氧化石墨烯/聚酰亚胺（GO/PI）复合薄膜，采用XRD、TMA、TGA等对其结构和性能进行表征。结果表明：相对于不添加GO的PI薄膜而言，当复合薄膜中的GO质量分数为0.2%时，复合薄膜的力学性能得到很大提升，其中拉伸强度提高了26.77%，断裂伸长率提高了76.47%，弹性模量基本不变。当GO质量分数为0.1%时，复合薄膜的T5、T10最大值分别为587.3℃、603.3℃，相对于未添加GO的PI薄膜分别提高了2.44%、1.69%。说明适量GO的加入可以显著增强复合薄膜的力学性能和热学性能。

, authors=

韩松锋（1991-），男（汉族），河南驻马店人，结构工程师，主要从事高分子材料加工工艺与装备研究。

, authorsList=韩松锋, 唐必连, 张冰, 马传国, 青双桂, authorCompany=null, correspAuthors=null, authorNote=null, correspAuthorsNote=
马传国（1978-），男（汉族），山东临清人，教授，博士，主要从事高分子复合材料及功能材料研究。
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韩松锋（1991-），男（汉族），河南驻马店人，结构工程师，主要从事高分子材料加工工艺与装备研究。

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韩松锋（1991-），男（汉族），河南驻马店人，结构工程师，主要从事高分子材料加工工艺与装备研究。

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样品CTE/(10-6 K-1)T5/℃T10/℃Tmax/℃拉伸强度/MPa断裂伸长率/%弹性模量/GPa
PI-0%17.61573.3593.3618.3198175.3
PI-0.1%17.26587.3603.3614.2217175.5
PI-0.2%16.13577.7598.2613.2251305.5
PI-0.3%17.32569.2589.0610.5223205.4
PI-0.4%17.73563.1588.1610.5215155.6
PI-0.5%17.30576.0595.1623.120195.7
PI-1%17.74577.6597.2617.719265.7
), ArticleFig(id=1245100050188189813, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756977798000709, language=CN, label=表1, caption=

不同GO含量的GO/PI薄膜的热重分析结果和力学性能

, figureFileSmall=null, figureFileBig=null, tableContent=
样品CTE/(10-6 K-1)T5/℃T10/℃Tmax/℃拉伸强度/MPa断裂伸长率/%弹性模量/GPa
PI-0%17.61573.3593.3618.3198175.3
PI-0.1%17.26587.3603.3614.2217175.5
PI-0.2%16.13577.7598.2613.2251305.5
PI-0.3%17.32569.2589.0610.5223205.4
PI-0.4%17.73563.1588.1610.5215155.6
PI-0.5%17.30576.0595.1623.120195.7
PI-1%17.74577.6597.2617.719265.7
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GO/PI复合薄膜的制备及性能研究
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韩松锋 1 , 唐必连 2 , 张冰 1 , 马传国 3 , 青双桂 2
绝缘材料 | 聚酰亚胺薄膜专题 2021,54(11): 126-129
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绝缘材料 |聚酰亚胺薄膜专题 2021 , 54 (11) : 126 -129
GO/PI复合薄膜的制备及性能研究
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韩松锋1, 唐必连2, 张冰1, 马传国3, 青双桂2
作者信息
  • 1郑州凯雪冷链股份有限公司，河南 郑州 450000
  • 2桂林电器科学研究院有限公司， 广西 桂林 541004
  • 3桂林电子科技大学 材料科学与工程学院，广西 桂林 541004
通讯作者:
马传国（1978-），男（汉族），山东临清人，教授，博士，主要从事高分子复合材料及功能材料研究。
Preparation and Properties of GO/PI Composite Film
Songfeng HAN1, Bilian TANG2, Bing ZHANG1, Chuanguo MA3, Shuanggui QING2
Affiliations
  • 1Zhengzhou Kaixue Cold Chain Co., Ltd., Zhengzhou 450000, China
  • 2Guilin Electrical Equipment Scientific Research Institute Co., Ltd., Guilin 541004, China
  • 3School of Material Science and Engineering, Guilin University of Electronic Technology, Guilin 541004, China
出版时间: 2021-11-22 doi: 10.16790/j.cnki.1009-9239.im.2021.11.018
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利用改进Hummers法制备氧化石墨烯（GO），再通过溶液共混法制备氧化石墨烯/聚酰亚胺（GO/PI）复合薄膜，采用XRD、TMA、TGA等对其结构和性能进行表征。结果表明：相对于不添加GO的PI薄膜而言，当复合薄膜中的GO质量分数为0.2%时，复合薄膜的力学性能得到很大提升，其中拉伸强度提高了26.77%，断裂伸长率提高了76.47%，弹性模量基本不变。当GO质量分数为0.1%时，复合薄膜的T5、T10最大值分别为587.3℃、603.3℃，相对于未添加GO的PI薄膜分别提高了2.44%、1.69%。说明适量GO的加入可以显著增强复合薄膜的力学性能和热学性能。

溶液共混法  /  氧化石墨烯  /  聚酰亚胺  /  复合薄膜

A graphene oxide (GO) was synthesized by modified Hummers’ method, and a graphene oxide/polyimide (GO/PI) composite film was prepared by solution blending method. The structure and the properties of the composite film were analyzed by XRD, TMA, TGA. The results show that compared with the PI film without GO, when the mass fraction of GO in composite film is 0.2%, the mechanical properties of the composite film increase obviously, the tensile strength increases by 26.77%, the elongation at break increases by 76.47%, and the elastic modulus changes little basically. When the mass fraction of GO is 0.1%, the maximum value of T5 and T10 of the composite film are 587.3℃ and 603.3℃, which increase by 2.44% and 1.69% compared with that of the PI film without GO, respectively. It is indicated that the addition of GO with appropriate amount can enhance the mechanical properties and thermal properties of PI films.

solution blending method  /  graphene oxide  /  polyimide  /  composite film
韩松锋, 唐必连, 张冰, 马传国, 青双桂. GO/PI复合薄膜的制备及性能研究. 绝缘材料, 2021 , 54 (11) : 126 -129 . DOI: 10.16790/j.cnki.1009-9239.im.2021.11.018
Songfeng HAN, Bilian TANG, Bing ZHANG, Chuanguo MA, Shuanggui QING. Preparation and Properties of GO/PI Composite Film[J]. Insulating Materials, 2021 , 54 (11) : 126 -129 . DOI: 10.16790/j.cnki.1009-9239.im.2021.11.018
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0 引言
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聚酰亚胺（PI）凭借自身优异的力学、热学、电学等性能，被广泛应用于各大先进行业中。为满足不同领域中的性能需求，针对聚酰亚胺方面的改性工作始终在进行，目前按类型主要分为填料改性和聚合改性。
石墨烯凭借自身独特的单层碳二维结构，以及优异的力学、电学、热学性能，成为复合材料界的理想填料。但作为填料应用于复合材料的过程中，由于石墨烯表面没有官能基团，并且具有比表面积大、比表面能高等特点，使其在有机溶剂中极易团聚，很难与复合材料基体发生化学反应生成均匀分散的悬浮液[1]。氧化石墨烯（GO）作为实验室制备石墨烯的中间产物，其表面含有丰富的含氧基团，如羟基、羧基、羰基和环氧基等，使其更容易与复合材料基体发生反应，形成分散均匀的聚合物。
目前，通过引入较低含量的GO对PI进行改性的研究报道并不多见，且研究内容主要以均苯型PI为主，对联苯型PI的研究还未见报道。本研究将实验室制备的GO作为填料，通过溶液混合的方式对PI树脂进行改性，制备成GO/PI复合薄膜，主要研究GO含量的变化对复合薄膜的CTE、力学、热学性能的影响。
1 实验
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1.1 原材料
二酐：3,3′,4,4′-联苯四甲酸二酐（s-BPDA）（纯度为99%），干燥处理后再使用；二胺：对苯二胺（PDA）（纯度为99.5%）、4,4′-二氨基二苯醚（ODA）（纯度为99.5%），干燥处理后再使用；溶剂：二甲基乙酰胺（DMAc），蒸馏处理后再使用。上述原材料均购于国药集团化学试剂有限公司。制备GO的原材料：鳞片石墨（325目），购于南京先丰纳米科技有限公司；无水乙醇（AR）、高锰酸钾（AR）、硝酸钠（AR）、稀盐酸（AR），购于西陇化工股份有限公司；浓硫酸（纯度为98%）、双氧水（纯度为30%），购于廉江市爱廉化试剂有限公司。
1.2 试样制备
（1）含DMAc溶剂的GO悬浮液的制备
采用改进Hummers法[2]制备GO。称取2.0 g鳞片石墨、1.0 g NaNO3加入到250 mL三口烧瓶中，整个装置置于冰浴中，量取50 mL H2SO4缓慢加入三口烧瓶中，充分搅拌30 min。待温度降至5℃以下，将0.3 g KMnO4加入到三口烧瓶中并充分搅拌30 min，在1 h内将7.0 g KMnO4分3次加入到三口烧瓶中，整个加料过程控制反应体系温度在20℃以下。然后将实验装置放入（35±3）℃的水浴中搅拌处理2 h。将90 mL去离子水缓慢滴加到三口烧瓶中，温度控制在70～100℃，搅拌反应15 min。将7 mL浓度为30%的过氧化氢和55 mL温度为45℃的去离子水混合液滴加到三口烧瓶中。将悬浮液趁热过滤，用150 mL浓度为3%的稀盐酸反复洗涤滤饼3次后，将其分散在600 mL纯水中，离心即得凝胶状的氧化石墨。用DMAc溶剂对上述凝胶状氧化石墨进行分散、离心，重复该步骤至少3次，最后进行超声处理，得到含DMAc溶剂的GO悬浮液。
（2）PAA树脂的合成
将称量好的ODA、PDA、含DMAc溶剂的GO悬浮液溶解在相应量的DMAc中，待溶解完全后，分多次少量缓慢加入20 g s-BPDA，每次加料后均反应1 h，得到s-BPDA/ODA/PDA/GO型聚酰胺酸（PAA）树脂。
（3）GO/PI复合薄膜的制备
采用数控涂布机将上述PAA树脂在玻璃板上刮膜，然后放入烘箱中进行亚胺化，处理条件为60℃/1 h+100℃/0.5 h+150℃/1 h+200℃/1 h+250℃/1 h+300℃/0.5 h+380℃/0.5 h，最终得到GO/PI复合薄膜。s-BPDA/ODA/PDA的分子链结构式如图1所示，GO的结构如图2所示。
在联苯型s-BPDA/ODA/PDA三元体系中引入GO，以GO悬浮液的固含量为变量，制备6个配方的PAA树脂，其中GO的质量分数分别为0.1%、0.2%、0.3%、0.4%、0.5%、1%，按照上述比例制备的GO/PI复合薄膜分别命名为PI-0.1%、PI-0.2%、PI-0.3%、PI-0.4%、PI-0.5%、PI-1%。GO/PI复合薄膜实物如图3所示，从图3中可以看出，GO在PI基体中分散性良好，色泽度均匀。
1.3 测试方法
采用X-射线衍射仪（XRD/PIXCED3D型，荷兰帕拉克公司）测试GO/PI复合薄膜的聚集态结构；采用静态热机械分析仪（TMA/SDTA840型，梅特勒-托利多公司）测试CTE，升温速率为10℃/min；采用热失重分析仪（TGA/NETZSCH STA 449F3型，德国耐驰公司）测试热分解温度（Td），升温速率为10℃/min；采用电子万能拉力机（KD111-0.2型，深圳市凯强利试验仪器有限公司）按照GB/T 13542.6—2009测试力学性能。
2 结果与讨论
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2.1 XRD分析
采用广角X射线衍射仪对PI薄膜的聚集态结构进行分析，结果如图4所示。从图4可以看出，与未添加GO的PI-0%薄膜XRD测试曲线相比，微量GO的加入对GO/PI复合薄膜的聚集态结构几乎没有影响。这是由于加入的GO不会改变PI分子链原有的结构，这与大多数文献的报道结果一致[3-4]。
2.2 热膨胀系数
对PI薄膜采用TMA测试，分析GO含量变化对CTE的影响，测试曲线如图5所示，具体数值见表1。
从图5及表1的CTE数据可以看出，GO含量的变化没有明显影响复合薄膜的CTE数值。PI的CTE与分子链的面内取向有很大关系，面内取向度的增加可使CTE数值呈下降趋势，存在刚性、直线型特征的主链结构是PI发生面内取向的必要条件[5]。虽然GO片层表面丰富的含氧基团可与PI基体之间反应形成氢键或其他配位键，但该体系中GO的质量分数最高仅为1%，可能对二胺和二酐之间的环化反应影响不大，未能在一定程度上改变原有分子链的结构和聚集态，未得到分子链排列有序度更高的紧密堆砌状态。
2.3 热稳定性
采用热失重分析仪在Ar气氛下以10℃/min的升温速率从室温升至900℃，对GO/PI复合薄膜进行热失重测试，结果如图6所示，具体数据列于表1。
从表1中数据可以看出，相对于未加入GO的PI-0%薄膜而言，当GO质量分数为0.1%时，复合薄膜的热失重温度得到了最大程度上的提高，T5、T10提高率分别为2.44%、1.69%。当GO质量分数再增加时，复合薄膜的热失重温度基本与PI-0%薄膜相差不大。一方面是因为GO的添加量较少，其在低温范围内的失重行为微乎其微，对复合薄膜热稳定性的影响较小；另一方面GO比表面积大，同时表面含有较多的含氧基团，这些基团的存在使GO具有一定的亲水性[6]，容易在PI树脂基体中均匀分散，此外PI分子链可以与GO表面富集的羧基、羰基等基团形成氢键或其他配位键，客观上限制了PI的热振动，因而增大了聚合物链分解时所需要的能量，这种相互作用弥补了GO稍差的热稳定性，在一定程度上提高了复合薄膜的热稳定性[7]。
2.4 力学性能
不同GO含量GO/PI复合薄膜的力学性能如表1所示。从表1可以看出，随着GO含量的增加，GO/PI复合薄膜的拉伸强度和断裂伸长率均呈现出先增大后减小的趋势，而弹性模量基本不变。当GO质量分数为0.2%时，拉伸强度和弹性模量均达到最高，分别为251 MPa和30%，相对于PI-0%薄膜分别提高了26.77%、76.47%。这是由于GO与PI之间的共价键结合作用，使两者之间产生了较强的界面结合作用，因此在拉伸过程中应力能够得到有效转移，避免应力集中[8]。而随着GO含量的继续增加，GO/PI复合薄膜的拉伸强度和断裂伸长率又同时下降，其原因可能在于虽然GO片层表面含有较多含氧基团，可以和PI基体之间生成较强的界面结合，但在高温热亚胺化处理阶段也容易团聚[9]，团聚的产生极易在复合薄膜中形成暗斑、孔洞等缺陷，导致复合薄膜的力学性能下降。
3 结论
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通过在s-BPDA/ODA/PDA型PI薄膜中引入实验室自制含有DMAc溶剂的GO分散液，通过改变GO的添加量，制备出一系列综合性能优异的GO/PI复合薄膜。当GO质量分数为0.2%时，复合薄膜的拉伸强度最大，为251 MPa，断裂伸长率最大，为30%，相对于未添加GO的PI-0%薄膜分别提高了26.77%和76.47%；当GO质量分数为0.1%时，T5、T10最大值分别为587.3℃、603.3℃，相对于未添加GO的PI-0%薄膜分别提高了2.44%、1.69%。微量GO的加入对GO/PI复合薄膜的CTE几乎没有影响，当加入的GO质量分数适量时，能够明显提高复合薄膜的热学性能和力学性能。
基金
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  • 国家自然科学基金资助项目(51363003)
  • 广西自然科学基金资助项目(2016JJA160040)
  • 桂林市科学研究与技术开发计划项目(2016010705)
  • 桂林电子科技大学研究生教育创新计划项目(2017YJCX121)
文献
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参考文献 引证文献
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闵春英,聂鹏,刘颖,等.耐高温GO/聚酰亚胺复合材料的制备及摩擦性能[J].固体火箭技术,2014(4):569-573.
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TRAN D N H, KABIRI S, LOSIC D. A green approach for the reduction of graphene oxide nanosheets using non-aromatic amino acids[J]. Carbon,2014,76(18):193-202.
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何刘成.氧化石墨烯的硅氧烷化及其增强聚酰亚胺的研究[D].苏州:苏州大学,2015.
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彭思敏,王世敏,万丽,等.原位聚合制备氧化石墨烯/聚酰亚胺纳米复合薄膜[C]//第七届中国功能材料及其应用学术会议论文集(第4分册).2010.
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马鹏常,杨正华,姬相玲,等.单向拉伸聚酰亚胺薄膜[J].应用化学,2007,24(3):331-334.
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赵浩然,吕生华.氧化石墨烯及其聚合物复合材料制备的研究进展[J].高分子材料科学与工程,2016,32(3):184-190.
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麻琪.氧化石墨烯纳米复合膜研究[D].天津:天津大学,2008.
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ZAMAN I, PHAN T T, KUAN H C, et al. Epoxy/graphene platelets nanocomposites with two levels of interface strength[J]. Polymer,2011,52(7):1603-1611.
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2021年第54卷第11期
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文章信息
doi: 10.16790/j.cnki.1009-9239.im.2021.11.018
  • 接收时间：2020-12-21
  • 首发时间：2026-03-23
  • 出版时间：2021-11-22
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出版历史
  • 收稿日期：2020-12-21
  • 修回日期：2021-01-22
基金
国家自然科学基金资助项目(51363003)
广西自然科学基金资助项目(2016JJA160040)
桂林市科学研究与技术开发计划项目(2016010705)
桂林电子科技大学研究生教育创新计划项目(2017YJCX121)
作者信息
    1郑州凯雪冷链股份有限公司，河南 郑州 450000
    2桂林电器科学研究院有限公司， 广西 桂林 541004
    3桂林电子科技大学 材料科学与工程学院，广西 桂林 541004

通讯作者:

马传国（1978-），男（汉族），山东临清人，教授，博士，主要从事高分子复合材料及功能材料研究。
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https://castjournals.cast.org.cn/joweb/jycl/CN/10.16790/j.cnki.1009-9239.im.2021.11.018
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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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