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Article(id=1210601625606026222, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1210601623135581115, articleNumber=null, orderNo=null, doi=10.16790/j.cnki.1009-9239.im.2024.10.004, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1710950400000, receivedDateStr=2024-03-21, revisedDate=1713888000000, revisedDateStr=2024-04-24, acceptedDate=null, acceptedDateStr=null, onlineDate=1766559519434, onlineDateStr=2025-12-24, pubDate=1729353600000, pubDateStr=2024-10-20, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1766559519434, onlineIssueDateStr=2025-12-24, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1766559519434, creator=13701087609, updateTime=1766559519434, updator=13701087609, issue=Issue{id=1210601623135581115, tenantId=1146029695717560320, journalId=1149653034449285133, year='2024', volume='57', issue='10', pageStart='1', pageEnd='141', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1766559518846, creator=13701087609, updateTime=1766564021205, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1210620507448275814, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1210601623135581115, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1210620507448275815, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1210601623135581115, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=26, endPage=33, ext={EN=ArticleExt(id=1210601625916403715, articleId=1210601625606026222, tenantId=1146029695717560320, journalId=1149653034449285133, language=EN, title=Preparation and properties of soluble thermoplastic polyimide films, columnId=1203281640207393262, journalTitle=Insulating Materials, columnName=Special Issue on High Performance Polyimide Materials, runingTitle=null, highlight=null, articleAbstract=

In order to improve the solution processability of traditional thermoplastic polyimide (TPI) and enhance its adhesion and heat resistance, several soluble thermoplastic polyimide (TPI) resins were prepared from different commercial dianhydride monomers and self-made diamine monomers with pyridine and diphenyl ether structures and active phenol side groups or benzene side group in the main chain through the two-step method. And then the corresponding TPI films and flexible copper clad laminates (FCCLs) were prepared. The properties of TPI resins were analyzed by solubility test and gel permeation chromatography (GPC). The structure, water absorption, mechanical properties, and dielectric properties of TPI films were tested, and the related properties of the FCCLs were also tested. The results show that all the TPI resins can dissolve in strong polar organic solvents such as NMP, and the glass transition temperature (Tg) and 5% thermal weight loss temperature (T5%) of the corresponding films are in the range of 236.8-325.6℃ and 508.7-553.7℃, respectively, and the residue rate at 800℃ (R800) is higher than 64%. The coefficient of thermal expansion (CTE), tensile strength, elongation at break, and water absorption is in the range of 56.36×10-6-78.30×10-6℃-1, 64.93-109.18 MPa, 9.09%-24.60%, and 0.74%-3.75%, respectively. The dielectric constant and dielectric loss of TPI-4 with better comprehensive properties are also lower than that of other samples, and the peeling strength of the corresponding FCCL reaches 0.95 N/mm, but it can only pass the floating welding test at 288℃ for 10 seconds. In addition, the polar phenol side group in TPI-4 not only ensures its organic solubility, but also significantly enhances its heat resistance and mechanical strength, and also reduce its CTE. The existence of reactive phenol side groups provides great convenience for the subsequent chemical modification of TPI. By adding a small amount of cyanate ester resin (CE01) to modify the TPI, the peel strength and the floating welding resistance of the responding FCCLs can be obviously improved.

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为了改善传统热塑性聚酰亚胺（TPI）的溶液加工性并提高其耐热性和粘接性，采用不同的商品化二酐单体分别与自制的主链含有吡啶和二苯醚结构及活性苯酚侧基或苯侧基的二胺单体通过两步法制备了一系列可溶解热塑性聚酰亚胺（TPI）树脂，随后制备了相应的TPI薄膜以及挠性覆铜板（FCCL）。通过溶解性试验和凝胶渗透色谱（GPC）分析TPI树脂的性能，然后测试分析了TPI薄膜的结构、吸水率、力学性能、热学性能和介电性能，并对其FCCL的相关性能进行测试。结果表明：TPI树脂均能溶解于NMP等强极性有机溶剂，相应薄膜的玻璃化转变温度（Tg）均为236.8～325.6℃，5%热失重温度（T5%）为508.7～553.7℃，800℃残留率（R800）均高于64%，热膨胀系数（CTE）为56.36×10-6～78.30×10-6℃-1，拉伸强度为64.93～109.18 MPa，断裂伸长率为9.09%～24.60%，吸水率为0.74%～3.75%。综合性能相对较优的TPI-4的介电常数和介质损耗因数也相对较低，相应FCCL的剥离强度达到0.95 N/mm，但只能通过288℃/10 s的耐浮焊测试。此外，TPI-4中极性的苯酚侧基不仅保证了其有机溶解性，对其耐热性和机械强度也有明显的增强作用，同时还降低了其CTE值。具有反应活性的苯酚侧基为TPI的后续化学改性提供了极大的便利，通过加入少量的氰酸酯树脂（CE01）对其进行改性可以明显改善其与热固性PI薄膜或铜箔的粘接性能并提高相应FCCL的耐浮焊性。

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陈文求（1982-），男（汉族），湖北黄冈人，副研究员，主要从事聚酰亚胺等高性能聚合物及其复合材料的研究，以及FCCL相关电子化学材料的开发与应用等工作。
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贺娟（1998-），女（汉族），湖南岳阳人，硕士生，研究方向为聚酰亚胺的分子设计与合成。

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贺娟（1998-），女（汉族），湖南岳阳人，硕士生，研究方向为聚酰亚胺的分子设计与合成。

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贺娟（1998-），女（汉族），湖南岳阳人，硕士生，研究方向为聚酰亚胺的分子设计与合成。

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2Haiso Technology Co., Ltd., Wuhan 430074, China
3Haiso EM (Wuhan) Ltd., Ezhou 436070, China, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null), CN=AuthorExt(id=1218266776740220999, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210601625606026222, authorId=1218266776517922876, language=CN, stringName=陈文求, firstName=文求, middleName=null, lastName=陈, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=1, 2, 3, address=1江汉大学 湖北省化学研究院，湖北 武汉 430056
2华烁科技股份有限公司， 湖北 武汉 430074
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2Haiso Technology Co., Ltd., Wuhan 430074, China
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2华烁科技股份有限公司， 湖北 武汉 430074
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Research and application progress of thermoplastic polyimide[J]. 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Design and synthesis of low thermal expansion thermoplastic polyimide resin[D]. Beijing: Beijing University of Chemical Technology, 2022., articleTitle=Design and synthesis of low thermal expansion thermoplastic polyimide resin, refAbstract=null), Reference(id=1218266787196621271, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210601625606026222, doi=null, pmid=null, pmcid=null, year=2017, volume=25, issue=12, pageStart=25, pageEnd=26, url=null, language=null, rfNumber=[23], rfOrder=30, authorNames=辜信实, journalName=印制电路信息, refType=null, unstructuredReference=辜信实.压合法二层挠性覆铜板制造技术[J].印制电路信息,2017,25(12):25-26., articleTitle=压合法二层挠性覆铜板制造技术, refAbstract=null), Reference(id=1218266787284701660, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210601625606026222, doi=null, pmid=null, pmcid=null, year=2017, volume=25, issue=12, pageStart=25, pageEnd=26, url=null, language=null, rfNumber=[23], rfOrder=31, authorNames=GUX S, journalName=Printed Circuit Information, refType=null, unstructuredReference=GUX S. Manufacturing technology of 2L-FCCL by lamination method[J]. Printed Circuit Information,2017,25(12):25-26., articleTitle=Manufacturing technology of 2L-FCCL by lamination method, refAbstract=null)], funds=[Fund(id=1218266782796796248, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210601625606026222, awardId=42000023205T000000146, language=CN, fundingSource=湖北省科技发展专项(42000023205T000000146), fundOrder=null, country=null)], companyList=[AuthorCompany(id=1218266775314158588, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210601625606026222, xref=1, ext=[AuthorCompanyExt(id=1218266775326741501, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210601625606026222, companyId=1218266775314158588, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1Hubei Chemistry Research Institute, Jianghan University, Wuhan 430056, China), AuthorCompanyExt(id=1218266775335130110, tenantId=1146029695717560320, 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remark=2华烁科技股份有限公司， 湖北 武汉 430074)]), AuthorCompany(id=1218266775645507594, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210601625606026222, xref=3, ext=[AuthorCompanyExt(id=1218266775666479116, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210601625606026222, companyId=1218266775645507594, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=3Haiso EM (Wuhan) Ltd., Ezhou 436070, China), AuthorCompanyExt(id=1218266775679062030, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210601625606026222, companyId=1218266775645507594, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=3华烁电子材料（武汉）有限公司，湖北 鄂州 436070)])], figs=[ArticleFig(id=1218266778497634499, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210601625606026222, language=EN, label=Fig.1, caption=Synthetic route of TPI, figureFileSmall=UYNoucibAQ2vH6XIyFgcnw==, figureFileBig=kYxWK9xPW8q4rR4ZUL6x5Q==, tableContent=null), ArticleFig(id=1218266778585714890, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210601625606026222, language=CN, label=图1, caption=TPI的合成路线, figureFileSmall=UYNoucibAQ2vH6XIyFgcnw==, figureFileBig=kYxWK9xPW8q4rR4ZUL6x5Q==, tableContent=null), ArticleFig(id=1218266778703155413, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210601625606026222, language=EN, label=Fig.2, caption=FT-IR spectra of TPI films, figureFileSmall=fmbBw40XUTS6y4jDRUA1mA==, figureFileBig=exEgJwpej+goUDCfxw+RPA==, tableContent=null), ArticleFig(id=1218266778791235804, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210601625606026222, language=CN, label=图2, caption=TPI薄膜的FT-IR谱图, figureFileSmall=fmbBw40XUTS6y4jDRUA1mA==, figureFileBig=exEgJwpej+goUDCfxw+RPA==, tableContent=null), ArticleFig(id=1218266778870927587, 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figureFileSmall=2KrvG1rvDOYu27Q4M6xamQ==, figureFileBig=43B6mjlfukYTB67OMO8yAQ==, tableContent=null), ArticleFig(id=1218266780666089717, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210601625606026222, language=EN, label=Fig.5, caption=TGA curves of resultingTPI films, figureFileSmall=hJBChcVxMJ0T/FPqUQ8l8Q==, figureFileBig=c8EPrL4TTaAHYkCG4HSLEQ==, tableContent=null), ArticleFig(id=1218266780762558716, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210601625606026222, language=CN, label=图5, caption=TPI薄膜的TGA图谱, figureFileSmall=hJBChcVxMJ0T/FPqUQ8l8Q==, figureFileBig=c8EPrL4TTaAHYkCG4HSLEQ==, tableContent=null), ArticleFig(id=1218266780850639106, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210601625606026222, language=EN, label=Fig.6, caption=TMA curves of TPI films, figureFileSmall=zJYF2JGGq7u0jXbkwthJAQ==, figureFileBig=dsqGEezjFfmj9Z7hB21yDw==, tableContent=null), ArticleFig(id=1218266780972273927, 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caption=Organic solubility of TPI, figureFileSmall=null, figureFileBig=null, tableContent=
试样NMPDMFDMACDMSOm-CresolCHCl3THFTL
TPI-1++-+-+-‒‒‒‒
TPI-2+++++-‒‒‒
TPI-3+++++-‒‒‒
TPI-4+++++++-‒‒
TPI-5+++++++-+-‒
), ArticleFig(id=1218266781391704344, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210601625606026222, language=CN, label=表1, caption=

TPI的有机溶解性

, figureFileSmall=null, figureFileBig=null, tableContent=
试样NMPDMFDMACDMSOm-CresolCHCl3THFTL
TPI-1++-+-+-‒‒‒‒
TPI-2+++++-‒‒‒
TPI-3+++++-‒‒‒
TPI-4+++++++-‒‒
TPI-5+++++++-+-‒
), ArticleFig(id=1218266781479784731, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210601625606026222, language=EN, label=Table 2, caption=GPC test results of PAA and TPI, figureFileSmall=null, figureFileBig=null, tableContent=
试样Mn/(×104 g/mol)Mw/(×104 g/mol)Mz/(×104 g/mol)PDI
PAA-11.652.603.511.39
PAA-21.192.404.032.02
PAA-31.943.455.271.77
PAA-41.692.884.461.71
PAA-51.562.564.181.64
TPI-44.7410.2515.842.16
TPI-53.277.5512.592.31
), ArticleFig(id=1218266781567865120, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210601625606026222, language=CN, label=表2, caption=

PAA和TPI的GPC测试结果

, figureFileSmall=null, figureFileBig=null, tableContent=
试样Mn/(×104 g/mol)Mw/(×104 g/mol)Mz/(×104 g/mol)PDI
PAA-11.652.603.511.39
PAA-21.192.404.032.02
PAA-31.943.455.271.77
PAA-41.692.884.461.71
PAA-51.562.564.181.64
TPI-44.7410.2515.842.16
TPI-53.277.5512.592.31
), ArticleFig(id=1218266781668528418, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210601625606026222, language=EN, label=Table 3, caption=Calculation results of aggregated structure of TPI films, figureFileSmall=null, figureFileBig=null, tableContent=
试样2θ/(°)d/nm
TPI-119.260.46
TPI-217.880.50
TPI-319.790.45
TPI-419.380.46
TPI-518.170.49
), ArticleFig(id=1218266781769191721, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210601625606026222, language=CN, label=表3, caption=

TPI薄膜的聚集态结构计算结果

, figureFileSmall=null, figureFileBig=null, tableContent=
试样2θ/(°)d/nm
TPI-119.260.46
TPI-217.880.50
TPI-319.790.45
TPI-419.380.46
TPI-518.170.49
), ArticleFig(id=1218266781895020845, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210601625606026222, language=EN, label=Table 4, caption=Thermal properties and dimensional stability test results of TPI films, figureFileSmall=null, figureFileBig=null, tableContent=
试样Tg(TMA)/℃T5%/℃T10%/℃R800/%LOI/%CTE/(×10-6℃-1)
TPI-1315.1553.7586.069.2145.1862.03
TPI-2301.4542.6572.768.2144.7861.03
TPI-3282.6544.4574.468.6344.9557.71
TPI-4255.1508.7529.864.4243.2756.36
TPI-5232.3521.8538.766.4044.0678.30
), ArticleFig(id=1218266782004072751, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210601625606026222, language=CN, label=表4, caption=

TPI薄膜热学性能和尺寸稳定性测试结果

, figureFileSmall=null, figureFileBig=null, tableContent=
试样Tg(TMA)/℃T5%/℃T10%/℃R800/%LOI/%CTE/(×10-6℃-1)
TPI-1315.1553.7586.069.2145.1862.03
TPI-2301.4542.6572.768.2144.7861.03
TPI-3282.6544.4574.468.6344.9557.71
TPI-4255.1508.7529.864.4243.2756.36
TPI-5232.3521.8538.766.4044.0678.30
), ArticleFig(id=1218266782121513271, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210601625606026222, language=EN, label=Table 5, caption=Test results of mechanical properties of TPI films, figureFileSmall=null, figureFileBig=null, tableContent=
试样拉伸强度/MPa弹性模量/GPa断裂伸长率/%
TPI-1104.39±1.902.09±0.109.09±0.15
TPI-2109.18±7.162.24±0.1610.32±0.86
TPI-393.03±0.792.04±0.0210.01±0.30
TPI-472.94±4.091.62±0.0910.10±1.21
TPI-564.93±6.881.52±0.0124.60±11.27
), ArticleFig(id=1218266782230565181, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210601625606026222, language=CN, label=表5, caption=

TPI薄膜的力学性能测试结果

, figureFileSmall=null, figureFileBig=null, tableContent=
试样拉伸强度/MPa弹性模量/GPa断裂伸长率/%
TPI-1104.39±1.902.09±0.109.09±0.15
TPI-2109.18±7.162.24±0.1610.32±0.86
TPI-393.03±0.792.04±0.0210.01±0.30
TPI-472.94±4.091.62±0.0910.10±1.21
TPI-564.93±6.881.52±0.0124.60±11.27
), ArticleFig(id=1218266782348005700, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210601625606026222, language=EN, label=Table 6, caption=Test results of dielectric properties and water absorption of TPI films, figureFileSmall=null, figureFileBig=null, tableContent=
试样吸水率/%DkDf
3 GHz10 GHz3 GHz10 GHz
TPI-12.36————
TPI-23.75————
TPI-32.44————
TPI-41.393.443.370.022 50.021 2
TPI-50.743.353.260.011 10.010 9
), ArticleFig(id=1218266782448669001, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210601625606026222, language=CN, label=表6, caption=

TPI薄膜的介电性能和吸水率测试结果

, figureFileSmall=null, figureFileBig=null, tableContent=
试样吸水率/%DkDf
3 GHz10 GHz3 GHz10 GHz
TPI-12.36————
TPI-23.75————
TPI-32.44————
TPI-41.393.443.370.022 50.021 2
TPI-50.743.353.260.011 10.010 9
), ArticleFig(id=1218266782532555084, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210601625606026222, language=EN, label=Table 7, caption=Test results of peeling strength and floating welding resistance of FCCL, figureFileSmall=null, figureFileBig=null, tableContent=
试样CE01加入量/份PS/(N/mm)耐浮焊性测试
288℃300℃
TPI-400.95通过不通过
TPI-501.09通过不通过
TPI-4-C111.09通过通过
TPI-4-C331.11通过通过
TPI-4-C551.08通过不通过
), ArticleFig(id=1218266782624829779, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210601625606026222, language=CN, label=表7, caption=

FCCL的剥离强度和耐浮焊性测试结果

, figureFileSmall=null, figureFileBig=null, tableContent=
试样CE01加入量/份PS/(N/mm)耐浮焊性测试
288℃300℃
TPI-400.95通过不通过
TPI-501.09通过不通过
TPI-4-C111.09通过通过
TPI-4-C331.11通过通过
TPI-4-C551.08通过不通过
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可溶解热塑性聚酰亚胺薄膜的制备和性能研究
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贺娟 1 , 牛翔 1 , 陈文求 1, 2, 3 , 范和平 1, 2, 3
绝缘材料 | 高性能聚酰亚胺材料专题 2024,57(10): 26-33
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绝缘材料 | 高性能聚酰亚胺材料专题 2024, 57(10): 26-33
可溶解热塑性聚酰亚胺薄膜的制备和性能研究
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贺娟1, 牛翔1, 陈文求1, 2, 3, 范和平1, 2, 3
作者信息
  • 1江汉大学 湖北省化学研究院，湖北 武汉 430056
  • 2华烁科技股份有限公司， 湖北 武汉 430074
  • 3华烁电子材料（武汉）有限公司，湖北 鄂州 436070

    • 贺娟（1998-），女（汉族），湖南岳阳人，硕士生，研究方向为聚酰亚胺的分子设计与合成。

通讯作者:

陈文求（1982-），男（汉族），湖北黄冈人，副研究员，主要从事聚酰亚胺等高性能聚合物及其复合材料的研究，以及FCCL相关电子化学材料的开发与应用等工作。
Preparation and properties of soluble thermoplastic polyimide films
Juan HE1, Xiang NIU1, Wenqiu CHEN1, 2, 3, Hepin FAN1, 2, 3
Affiliations
  • 1Hubei Chemistry Research Institute, Jianghan University, Wuhan 430056, China
  • 2Haiso Technology Co., Ltd., Wuhan 430074, China
  • 3Haiso EM (Wuhan) Ltd., Ezhou 436070, China
出版时间: 2024-10-20 doi: 10.16790/j.cnki.1009-9239.im.2024.10.004
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摘要
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为了改善传统热塑性聚酰亚胺（TPI）的溶液加工性并提高其耐热性和粘接性，采用不同的商品化二酐单体分别与自制的主链含有吡啶和二苯醚结构及活性苯酚侧基或苯侧基的二胺单体通过两步法制备了一系列可溶解热塑性聚酰亚胺（TPI）树脂，随后制备了相应的TPI薄膜以及挠性覆铜板（FCCL）。通过溶解性试验和凝胶渗透色谱（GPC）分析TPI树脂的性能，然后测试分析了TPI薄膜的结构、吸水率、力学性能、热学性能和介电性能，并对其FCCL的相关性能进行测试。结果表明：TPI树脂均能溶解于NMP等强极性有机溶剂，相应薄膜的玻璃化转变温度（Tg）均为236.8～325.6℃，5%热失重温度（T5%）为508.7～553.7℃，800℃残留率（R800）均高于64%，热膨胀系数（CTE）为56.36×10-6～78.30×10-6℃-1，拉伸强度为64.93～109.18 MPa，断裂伸长率为9.09%～24.60%，吸水率为0.74%～3.75%。综合性能相对较优的TPI-4的介电常数和介质损耗因数也相对较低，相应FCCL的剥离强度达到0.95 N/mm，但只能通过288℃/10 s的耐浮焊测试。此外，TPI-4中极性的苯酚侧基不仅保证了其有机溶解性，对其耐热性和机械强度也有明显的增强作用，同时还降低了其CTE值。具有反应活性的苯酚侧基为TPI的后续化学改性提供了极大的便利，通过加入少量的氰酸酯树脂（CE01）对其进行改性可以明显改善其与热固性PI薄膜或铜箔的粘接性能并提高相应FCCL的耐浮焊性。

聚酰亚胺  /  挠性覆铜板  /  可溶解  /  热塑性  /  粘接性  /  耐热性

In order to improve the solution processability of traditional thermoplastic polyimide (TPI) and enhance its adhesion and heat resistance, several soluble thermoplastic polyimide (TPI) resins were prepared from different commercial dianhydride monomers and self-made diamine monomers with pyridine and diphenyl ether structures and active phenol side groups or benzene side group in the main chain through the two-step method. And then the corresponding TPI films and flexible copper clad laminates (FCCLs) were prepared. The properties of TPI resins were analyzed by solubility test and gel permeation chromatography (GPC). The structure, water absorption, mechanical properties, and dielectric properties of TPI films were tested, and the related properties of the FCCLs were also tested. The results show that all the TPI resins can dissolve in strong polar organic solvents such as NMP, and the glass transition temperature (Tg) and 5% thermal weight loss temperature (T5%) of the corresponding films are in the range of 236.8-325.6℃ and 508.7-553.7℃, respectively, and the residue rate at 800℃ (R800) is higher than 64%. The coefficient of thermal expansion (CTE), tensile strength, elongation at break, and water absorption is in the range of 56.36×10-6-78.30×10-6℃-1, 64.93-109.18 MPa, 9.09%-24.60%, and 0.74%-3.75%, respectively. The dielectric constant and dielectric loss of TPI-4 with better comprehensive properties are also lower than that of other samples, and the peeling strength of the corresponding FCCL reaches 0.95 N/mm, but it can only pass the floating welding test at 288℃ for 10 seconds. In addition, the polar phenol side group in TPI-4 not only ensures its organic solubility, but also significantly enhances its heat resistance and mechanical strength, and also reduce its CTE. The existence of reactive phenol side groups provides great convenience for the subsequent chemical modification of TPI. By adding a small amount of cyanate ester resin (CE01) to modify the TPI, the peel strength and the floating welding resistance of the responding FCCLs can be obviously improved.

polyimide film  /  flexible copper clad laminate  /  soluble  /  thermoplasticity  /  adhesive property  /  heat resistance
贺娟, 牛翔, 陈文求, 范和平. 可溶解热塑性聚酰亚胺薄膜的制备和性能研究. 绝缘材料, 2024 , 57 (10) : 26 -33 . DOI: 10.16790/j.cnki.1009-9239.im.2024.10.004
Juan HE, Xiang NIU, Wenqiu CHEN, Hepin FAN. Preparation and properties of soluble thermoplastic polyimide films[J]. Insulating Materials, 2024 , 57 (10) : 26 -33 . DOI: 10.16790/j.cnki.1009-9239.im.2024.10.004
正文
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0 引言
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聚酰亚胺（PI）是一类处于材料金字塔顶端的聚合物，因其具有耐高温、耐辐射、耐化学腐蚀、自阻燃等优异性能，被广泛应用于微电子、复合材料、新能源、航空航天、显示等领域，其中挠性覆铜板 （FCCL）被认为是其最主要的应用之一[1-4]。PI作为FCCL生产的主要原材料之一，其本身性能对后者的质量起着重要的作用。然而，常规的芳香族PI不溶于有机溶剂和熔点高的特点导致其加工性能差，同时其独特的分子结构导致其表面自由能极低进而使其与其他材料（如铜箔）的粘接性较差。
为了克服这些问题，大量的研究工作集中在制备可溶解或可熔融加工的PI上[5]。20世纪70年代末，美国国家航空航天局（NASA）推出热塑性聚酰亚胺（TPI）LARC-TPI[6]，从那时起，TPI引起了广泛的研究关注。UltemTM是工业应用中TPI的代表，但它不能在180℃以上使用，耐热性和氧化稳定性的不足限制了其应用[7-8]。因此，研制TPI的关键不仅要保持其热塑性，同时还要保持其耐热性。无胶FCCL使用的是由粘接性相对较好的TPI薄膜以及尺寸稳定性和收缩性相对较好的热固性PI薄膜组成的复合膜，虽然无胶FCCL能够满足当前普通柔性印刷电路板（FPC）基材的使用要求，但其粘接性仍然不及一般的有胶FCCL[9-10]。因此，开发具有较大的剥离强度的无胶FCCL用PI及其薄膜材料具有极大的实际意义和应用价值。
将醚键等柔性链节和大体积的芳香侧基引入到PI分子链中，能有效地提高分子链的柔性，减小分子结构内的聚集密度，最终改善其热塑性[11-12]，并提高其在有机溶剂中的溶解度从而改善其溶液加工成型性[13]。吡啶是一种与苯结构相近的碱性杂环化合物，具有极佳的耐热性和热稳定性[14]，同时吡啶环上存在C-N极化键，将其引入PI中能增加PI与溶剂分子间的偶极子-偶极子相互作用，从而改善其溶解性[15]。此外还有研究表明，吡啶环上含有孤电子对的N原子，可与铜离子间形成配位键作用，将其引入PI分子结构中可以增强PI与铜箔之间的粘接性[10-16]。
基于此，为了制备可溶解加工、高粘接性和耐热性的TPI，本研究采用含吡啶和二苯醚结构及苯酚基或苯基的芳香二胺单体分别与4种商品化的二酐单体，通过两步法制备一系列可溶解TPI并制成相应的薄膜和FCCL。首先测试所得TPI树脂的有机溶解性和分子量，然后测试其薄膜的化学结构和聚集态结构，以及热学性能、力学性能、尺寸稳定性、吸湿性等常规性能，由此优选出综合性能较优的TPI及其薄膜。在测试其介电性能的基础之上，探索不同用量热固性氰酸酯树脂对其共混改性得到的FCCL剥离强度和耐焊性能的影响，以期为该类可溶解TPI的制备和后续的化学改性提供研究应用基础。
1 实验
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1.1 主要原材料
3,3′,4,4′-联苯甲酸二酐（BPDA）、3,3′,4,4′-二苯酮四甲酸二酐（BTDA）、3,3′,4,4′-二苯醚四甲酸二酐（ODPA）和双酚A型二醚二酐（BPADA），天津众泰材料科技股份有限公司，使用前在150℃下真空干燥12 h；4-苯基-2,6-双[4′-(4″-胺基苯氧基)苯基]吡啶、4-（对羟基苯基）-2,6-双[4′-(4″-胺基苯氧基)苯基]吡啶，参照文献[17]合成，使用前在120℃下真空干燥12 h；N-甲基吡咯烷酮（NMP），国药集团化学试剂有限公司，使用前经CaH2回流后减压蒸馏，再经450℃烧制并干燥的4Å型分子筛干燥24 h；双酚A型氰酸酯（CE01）树脂，纯度≥99%，扬州天启新材料股份有限公司；热固性PI薄膜，GF100型，热膨胀系数（CTE）（50～200℃）为17×10-6℃-1，韩国PI Advanced公司；电解铜箔（EDCu），厚度为35 μm，苏州福田金属有限公司。
1.2 TPI薄膜及相应FCCL的制备
将二胺单体溶于适量的溶剂中，在冰水浴中搅拌溶解，分3批加入相应计量的二酐单体，继续冰水浴搅拌反应6 h得到中间体聚酰胺酸（PAA）溶液，控制单体固含量为10%。然后加入适量的乙酸酐和吡啶混合溶液，在室温下搅拌1 h后升温至60℃反应1 h，再升温至100℃反应4 h，冷却后将反应液用乙醇析出，析出固体干燥后再用NMP溶解成固含量为10%的TPI溶液备用。TPI合成反应式如图1所示。
取适量上述TPI溶液在干净的玻璃板上流延成膜，在80～100℃下烘烤12 h后再按照120℃/2 h+150℃/1 h+180℃/1 h+220℃/1 h的程序处理，冷却后用热水浸泡脱膜，得到的薄膜再放入乙醇中浸泡 2 h，取出后在120℃下真空烘干即可得到TPI薄膜。
取适量TPI或改性TPI溶液涂覆于尺寸稳定性优异的商品化热固性PI膜上，控制涂膜厚度为（10±2）μm，在80℃下烘烤12 h后，再按照120℃/1 h+150℃/1 h+180℃/1 h的程序处理。然后将其涂胶面与35 μm EDCu的粗糙面相向叠放后放入夹具内，热压压力为2.5 MPa，置于高温烘箱内从室温梯度升高到预定温度（热压温度比所用TPI的Tg高100℃）并保温处理10 min，取出放入干燥箱中冷却至室温，制备出相应的FCCL。
1.3 测试与表征
以10 mg/mL浓度将TPI固体样品置于相应有机溶剂中，常温浸泡24 h或加热到80℃保温4 h后观察其有机溶解性；采用凝胶渗透色谱仪（GPC，1260型，美国Agilent公司）测试样品的分子量，流动相为四氢呋喃（THF），流速为1 mL/min，以聚苯乙烯（PS）为标样；采用傅里叶变换红外光谱仪（FTIR，TENSOR27型，德国Bruker BioSpin公司）测试样品的化学结构，扫描范围为4 000～600 cm-1；采用广角X射线衍射仪（XRD，X’ Pert Powder型，荷兰PANalytical公司）测定样品的物理聚集态结构，Cu-Kα为发射源（入射波长λ=0.154 18 nm），扫描范围为5°～60°，扫描速度为10°/min；采用差示扫描量热仪（DSC，Q-20型，美国TA公司）测试样品的热学性能，N2氛围，测试温度为室温至350℃，升温速率为10℃/min；采用热重分析仪（TGA，TG 209 F3型，德国Netzsch公司）测试样品的热稳定性，N2氛围，测试温度为室温至800℃，升温速率为20℃/min；采用静态热机械分析仪（TMA，Q-400型，美国TA公司）测试样品的尺寸稳定性，N2氛围，测试温度为室温至400℃，升温速率为10℃/min；采用电子万能试验机（UTM4204X-SUNS型，深圳三思纵横科技股份有限公司），按照GB/T 1040.3—2006测试样品的力学性能；按照IPC-TM-650 2.6.2测试样品的吸水率（WU）；采用矢量网络分析仪（N5225B型，美国Agilent公司），按照IPC-TM-650中的SPDR法测试样品的介电常数（Dk）和介质损耗因数（Df），测试频率分别为3 GHz和10 GHz；采用剥离强度测试仪（Instron H10KS型，广东正业科技股份有限公司），按照IPC-TM-650 2.4.9 Method B测试样品的剥离强度；采用可焊性测试仪（PZ-SB-18型，广东正业科技股份有限公司），按照IPC-TM-650 2.4.13 Method B测试FCCL的耐浮焊性。
2 结果与讨论
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2.1 TPI树脂的溶解性和GPC测试结果
本研究采用传统的两步法制备了含活性大体积侧基的可溶解TPI反应液，然后经析出、过滤、洗涤和干燥得到相应的TPI树脂，最后将其溶解得到的溶液经流延成膜、中高温烘除溶剂后得到相应的TPI薄膜。实验中TPI-1～TPI-5在化学亚胺化后均得到均匀的溶液，但因其中含有乙酸酐和吡啶等残余杂质对其性能和后续改性有影响，故进一步在乙醇中沉析得到相应的固体。由于所有TPI固体在室温或适当加热均可溶于NMP中得到均匀的溶液，由此可制备出相应的TPI薄膜。
表1是制得的TPI固体在不同有机溶剂中的溶解性测试结果。从表1可以看出，5种TPI的有机溶解性均较好，在室温或加热下能完全溶于NMP中。除了BPDA对应的TPI-1外，另外4种TPI在加热条件下均能完全溶于常见的极性非质子溶剂NMP、DMF、DMAC、DMSO中。总体来看，柔性最好的BPADA对应的TPI-4和TPI-5的有机溶解性相对较优，在室温下可完全溶解于NMP中，在加热条件下能完全溶解于上述强极性溶剂，且在低沸点溶剂如氯仿（CHCl3）中加热也能部分溶解。
从表1还可以看出，制得的TPI在THF中均无法直接溶解，但其前驱体PAA溶液均可直接溶解于THF中，同时由柔性最好的BPADA得到的TPI-4和TPI-5的NMP溶液也可以稀释到大量的THF中并形成透明均匀的溶液。因此对TPI-1～TPI-5的中间体PAA（分别编号为PAA-1～PAA-5），以及TPI-4和TPI-5进行了GPC测试，结果如表2所示。从表2可以看出，PAA-1～PAA-5的数均分子量（Mn）、重均分子量（Mw）、z均分子量（Mz）和分子量分布系数（PDI）均相近，这是由于所使用的二胺单体主体结构相同或类似，且所使用的二酐单体BPDA、BTDA、ODPA、BPADA分子活性也相近。此外通过对比还发现，TPI-4和TPI-5的Mn、Mw、Mz和PDI均比其对应的PAA-4和PAA-5高，这主要是由于PAA中含有大量的极性羧基或酰胺基，从而使其与流动相溶剂分子之间存在一定的相互作用，最终使得PAA的测试结果偏小。根据相关经验，TPI分子量在104 g/mol级别时就可以得到综合性能较好的薄膜。
2.2 TPI薄膜的FTIR分析
TPI薄膜的FTIR测试结果如图2所示。从图2可以看出，制得的TPI在1 774 cm-1、1 717 cm-1附近均出现了酰亚胺环上C=O的不对称和对称伸缩振动吸收峰，在1 373 cm-1附近出现了酰亚胺环中C-N的伸缩振动峰，740 cm-1附近出现了酰亚胺环中 C=O的变形振动峰，同时在1 670 cm-1处PAA中酰胺键上C=O的特征峰完全消失，说明PAA已完全亚胺化为相应的PI。此外，在3 300～3 600 cm-1出现不同程度的酚羟基特征吸收峰，表明所得TPI中含有酚羟基。
2.3 TPI薄膜的物理聚集态结构
采用XRD测试5种TPI薄膜的物理聚集态结构，结果如图3所示。从图3可以看出，5种TPI均表现出较宽的隆起衍射峰，无明显的尖锐结晶峰，说明它们主要是无定形结构。这是由于TPI分子链中柔性醚键和大体积侧基的存在导致其排列松散，同时活性酚羟基增加了聚合物分子链间或分子内的相互作用，从而破坏了聚合物的规整性，使结晶度大幅下降。一般来说，无定形聚合物相对于它们的晶体类似物具有较低的软化温度和更好的有机溶解性。
结合5种TPI薄膜的隆起衍射峰最高点的2θ值，根据布拉格方程，估算出其分子链的间距（d），结果如表3所示。从表3可以看出，5种TPI膜的d值均为0.45～0.50 nm，说明二酐单体的类型以及二胺单体侧基是否有活性均对薄膜的物理聚集态结构和d值影响不大。
2.4 TPI薄膜的热学性能
图4是TPI薄膜的DSC曲线，其中虚线为第一次升温曲线，实线为第二次升温曲线。从图4可以看出，5种TPI的玻璃化转变温度（Tg）为236.8～325.6℃。在二胺单体相同时，TPI的Tg值随二酐单体柔韧性的增加（柔韧性从小到大依次为BPDA、BTDA、ODPA、BPADA）而逐渐降低。同时，在二酐单体以及二胺单体主链结构相同时，TPI-4因其侧基中含活性的酚羟基增加了其分子链间的相互作用，导致其热运动受到限制，最终使其Tg值高于主链结构相同但侧基不含活性基团的TPI-5。此外，TPI-4消除热历史前后的Tg值差值比TPI-5略大也与此有关。
TPI薄膜的热重分析（TGA）结果如图5所示，相关数据如表4所示。从图5和表4可以看出，5种TPI薄膜在450℃以下均无明显的热失重现象，表明它们均具有较好的热稳定性。具体而言，刚性比较强的3种酐单体对应的TPI-1～TPI-3的5%热失重温度（T5%）和10%热失重温度（T10%）分别为542.6～553.7℃和572.7～586.0℃，800℃时的残碳率（R800）均超过68%。而柔性较强的二酐单体对应的TPI-4 T5%和T10%分别为508.7℃和529.8℃，R800为64.42%，均低于上述3种TPI。此外，由于含有热稳定性不佳的酚羟基，TPI-4的T5%、T10%和R800均略低于主链结构相同但侧基为苯基的TPI-5。尽管如此，TPI-4的耐热性以及热稳定性仍均高于绝大多数普通的有机聚合物，且高于UltemTM TPI[7-8]，表明主链含刚性吡啶环和柔性二苯醚结构以及大体积苯酚侧基的引入并没有对其耐热性和热稳定性产生不利的影响。
此外，根据Van Krevelen方程[18]，估算了5种TPI的极限氧指数（LOI），结果见表4。从表4可以看出，5种TPI薄膜的LOI均为43.27%～45.18%，远高于难燃材料LOI的下限（27%），表明所制备的5种TPI薄膜均为自阻燃材料。
2.5 TPI薄膜的尺寸稳定性
采用TMA测试了5种TPI薄膜的尺寸稳定性以及Tg值，结果如图6所示，具体数据见表4。从表4可以看出，由TMA法测定的5种TPI薄膜的Tg结果均略低于退火前DSC的测试结果（图4虚线），这是测试方法的不同所造成的。同时，5种TPI薄膜在100～200℃的CTE为56.36×10-6～78.30×10-6℃-1，均高于文献[19-20]报道的热固性PI薄膜，而与公开的商品化热塑性PI薄膜一致[21-22]。这是因为引入大体积侧基后破坏了分子结构的直线性，降低了聚合物分子链的堆积密度，进而对其受热后的尺寸稳定性有一定的影响。具体而言，TPI-1～TPI-3的CTE均比TPI-4的高，这是由于在二胺单体相同时，TPI-4使用了柔韧性较大的二酐单体使其分子链间的缠绕或相互作用更加明显。而主链结构相同的TPI-4的CTE比TPI-5的低，这是由于前者侧基上活性酚羟基之间的相互作用提高了其受热后的尺寸稳定性。
2.6 TPI薄膜的力学性能
TPI薄膜的典型应力-应变曲线如图7所示，相应的力学性能数据见表5。从图7和表5可以看出，二胺单体相同的4种TPI薄膜的拉伸强度、弹性模量、断裂伸长率分别为72.94～109.18 MPa，1.62～2.24 GPa，9.09%～10.10%，表明它们具有良好的机械强度和韧性。其中TPI-1和TPI-2两种薄膜的拉伸强度和拉伸模量均高于TPI-3和TPI-4，这与前二者使用了刚性较强的二酐单体有关。侧基不含酚羟基的TPI-5薄膜的拉伸强度、弹性模量均低于主链结构相同但侧基为苯酚基的TPI-4薄膜，但其断裂伸长率更高。这主要是因为TPI-4的聚合物分子链侧基上的活性酚羟基之间存在氢键等相互作用，从而提高了其机械强度。
2.7 TPI薄膜的吸水率和介电性能
TPI薄膜的吸水率测试结果如表6所示。从表6可以看出，由于含有极性的苯酚侧基，TPI-1～TPI-4薄膜的吸水率偏高，在1.39%～3.75%；同时因TPI-4分子链的柔性比TPI-1～TPI-3更好，其分子链间相互之间缠绕更紧密，故其吸水率相对较低。而TPI-5侧基为疏水的苯基，故其吸水率比主链结构相同的TPI-4更低。
进一步测试了吸水率相对较小的TPI-4和TPI-5在3 GHz和10 GHz下的介电常数（Dk）和介质损耗因数（Df），结果列于表6中。从表6可以看出，在目前5G通讯频率范围（3～5 GHz）的下限（3 GHz）时，TPI-4和TPI-5薄膜的Dk分别为3.44和3.35，Df分别为0.022 5和0.011 1；而在更高的10 GHz下，TPI-4和TPI-5薄膜的Dk分别为3.37和3.26，Df分别为0.021 2和0.010 9。对比发现，同种TPI薄膜的Dk和Df随测试频率的增加有一定程度的降低，同时TPI-4因苯基侧基上极性羟基的存在，使其Dk和Df均比主链相同但苯基侧基上不含极性基团的TPI-5略高。
2.8 FCCL的性能
根据文献[23]可知，制作无胶FCCL用TPI的Tg不能太低（<200℃），也不能太高（>300℃），最好在200～260℃。由此可知，由BPADA和二胺单体制备的TPI-4、TPI-5满足此要求，其较低的Tg有利于高温压合时对铜箔或热固性PI膜的粘接要求。基于此，将它们的溶液分别涂覆在热固性PI薄膜上并烘干，然后将其涂胶面贴合铜箔后经高温热压得到相应的FCCL样品。测试所得FCCL的剥离强度（PS）和288℃或300℃的耐浮焊性（测试时间为10 s），结果如表7所示。从表7可以看出，TPI-4和TPI-5所制得FCCL样品的PS分别为0.95 N/mm和1.09 N/mm，均满足FCCL行业相关标准（GB/T 13556—2017、IPC 4204A:2011）的要求（≥0.7 N/mm）。同时由于剥离后的热固性PI薄膜和铜箔表面均有残胶，说明以自制的主链含吡啶环和二苯醚键以及含苯酚侧基的TPI薄膜作为胶黏剂层，对热固性PI薄膜或铜箔均具有良好的粘接性能。虽然二者均通过了288℃的耐浮焊性测试，但在更高温度的无铅焊接，如300℃的耐浮焊性仍有待进一步提高。
针对带活性酚羟基的TPI-4树脂，进一步加入少量的双酚A型氰酸酯树脂（CE01）进行共混改性并制备成相应的FCCL，分别测试它们的PS和耐浮焊性，结果见表7。从表7可以看出，对于纯TPI-4，加入1～5份的CE01改性后，对应FCCL的PS先逐渐增大到1.11 N/mm后又减小到1.08 N/mm，在CE01加入量为3份时PS达到最大值。此外，加入1份和3份CE01改性的FCCL在300℃的耐浮焊性也得到改善，而加入5份CE01改性的FCCL仍不能通过300℃的耐浮焊性测试。由此说明引入少量的CE01进行共混改性可以同时改善TPI与热固性PI薄膜或铜箔的粘接性能和耐浮焊性。
3 结论
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（1）采用常规的两步法成功制备了一系列主链含吡啶和二苯醚结构以及活性苯酚侧基或苯侧基的TPI树脂，并由此制备出TPI薄膜及相应的FCCL。
（2）5种TPI树脂在常温或加热下能完全溶解于NMP中，且它们的分子量均在104 g/mol级别，满足溶液流延成膜的加工要求。
（3）FTIR和XRD分别证实了所得TPI薄膜的化学结构和物理聚集态结构。同时，通过测试发现所有TPI薄膜均具有较好的耐热性（Tg均在263.4～325.6℃）、热稳定性（T5%在508.7～553.7℃，R800均高于64%）和尺寸稳定性（CTE值在56.36×10-6～78.30×10-6℃-1），以及良好的机械强度和韧性（拉伸强度在64.93～109.18 MPa，断裂伸长率在9.09%～24.60%）。此外，具有相对较低吸水率的TPI-4和TPI-5的介电常数和介质损耗因数也相对较低，二者对应FCCL的PS分别为0.95 N/mm和1.09 N/mm，但均不能通过300℃的耐浮焊性测试。
（4）在含有活性苯酚侧基的TPI-4中加入3份CE01树脂对其进行进一步改性后，对应FCCL的PS增大到1.11 N/mm，且在300℃的耐浮焊性也得到改善。
（5）通过与主链结构相同但侧基为苯基的TPI-5薄膜进行对比测试发现，大体积的苯酚侧基对改善TPI薄膜的有机溶解性、降低CTE值以及提高耐热性、机械强度和粘接强度等作用非常明显。
基金
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  • 湖北省科技发展专项(42000023205T000000146)
文献
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2024年第57卷第10期
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doi: 10.16790/j.cnki.1009-9239.im.2024.10.004
  • 接收时间：2024-03-21
  • 首发时间：2025-12-24
  • 出版时间：2024-10-20
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  • 收稿日期：2024-03-21
  • 修回日期：2024-04-24
基金
湖北省科技发展专项(42000023205T000000146)
作者信息
    1江汉大学 湖北省化学研究院，湖北 武汉 430056
    2华烁科技股份有限公司， 湖北 武汉 430074
    3华烁电子材料（武汉）有限公司，湖北 鄂州 436070

通讯作者:

陈文求（1982-），男（汉族），湖北黄冈人，副研究员，主要从事聚酰亚胺等高性能聚合物及其复合材料的研究，以及FCCL相关电子化学材料的开发与应用等工作。
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https://castjournals.cast.org.cn/joweb/jycl/CN/10.16790/j.cnki.1009-9239.im.2024.10.004
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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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