Article(id=1209927726748799792, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1209927720432169632, articleNumber=null, orderNo=null, doi=10.16790/j.cnki.1009-9239.im.2024.03.004, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1696003200000, receivedDateStr=2023-09-30, revisedDate=1705248000000, revisedDateStr=2024-01-15, acceptedDate=null, acceptedDateStr=null, onlineDate=1766398849427, onlineDateStr=2025-12-22, pubDate=1710864000000, pubDateStr=2024-03-20, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1766398849427, onlineIssueDateStr=2025-12-22, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1766398849427, creator=13701087609, updateTime=1766398849427, updator=13701087609, issue=Issue{id=1209927720432169632, tenantId=1146029695717560320, journalId=1149653034449285133, year='2024', volume='57', issue='3', pageStart='1', pageEnd='128', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1766398847920, creator=13701087609, updateTime=1766563849864, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1210619788792033962, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1209927720432169632, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1210619788792033963, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1209927720432169632, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=29, endPage=35, ext={EN=ArticleExt(id=1209927727059178301, articleId=1209927726748799792, tenantId=1146029695717560320, journalId=1149653034449285133, language=EN, title=Study on polyimide films for novel OLED flexible substrate, columnId=1190369066675179686, journalTitle=Insulating Materials, columnName=Material Research, runingTitle=null, highlight=null, articleAbstract=
In this study, 4,4ʹ-diaminobenzanilide (DABA), 2,2ʹ-dimethyl-[1,1ʹ-biphenyl]-4,4ʹ-diamine (m-TB), dianhydrides pyromellitic dianhydride (PMDA), and 4,4ʹ-oxybisphthalic anhydride (ODPA) were used as raw materials, and a polyimide (PI) film for oganic light emitting diodes (OLED) flexible substrates was successfully synthesized. The results show that when the molar ratio of diamine to dianhydride is 0.990, the feeding time is 120 min, the reaction temperature is 0-30℃, the stirring speed is 200-250 r/min, and the reaction time is 240 min, the gel amount during the synthesis of polyamide acid is small, and viscosity can meet the requirements of industrial synthesis. After thermal imimization at 400℃, the glass transition temperature of the polyimide film is 450℃, the 1% weight loss temperature is 554℃, the thermal expansion coefficient is 4.1×10-6 K-1, the tensile strength is 326.9 MPa, the tensile modulus is 9 572.8 MPa, the electric strength is 623 kV/mm, and the dielectric constant is 3.251, which meet the industrial application requirements of OLED flexible substrate.
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本研究以4,4ʹ-二氨基苯酰替苯胺(DABA)和4,4ʹ-二氨基-2,2ʹ-二甲基联苯(m-TB)与均苯四甲酸二酐(PMDA)和4,4,-氧双邻苯二甲酸酐(ODPA)为原料,成功合成了有机发光二极管(OLED)柔性基板用聚酰亚胺(PI)薄膜。结果表明:当二胺与二酐摩尔比为0.990、加料时间为120 min、反应温度为0~30℃、搅拌速度为200~250 r/min、反应时间为240 min时,聚酰胺酸合成过程凝胶量少,黏度满足工业化合成要求。经400℃热亚胺化后,所得PI薄膜的玻璃化转变温度为450℃,1%热失重温度为554℃,热膨胀系数为4.1×10-6 K-1,拉伸强度为326.9 MPa,拉伸模量为9 572.8 MPa,电气强度为623 kV/mm,介电常数为3.251,这些参数指标满足OLED柔性基板的工业应用要求。
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李陶琦(1964-),男(汉族),陕西西安人,研究员,主要从事聚酰亚胺基复合材料的研究。
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1大同共聚(西安)科技有限公司,陕西 西安 710075
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李陶琦(1964-),男(汉族),陕西西安人,研究员,主要从事聚酰亚胺基复合材料的研究。
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李陶琦(1964-),男(汉族),陕西西安人,研究员,主要从事聚酰亚胺基复合材料的研究。
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Schematic diagram of the preparation process of PI film, figureFileSmall=wMEBvLzglg0p1H08r9j+fA==, figureFileBig=Kgf273ytZ1bad1gtaF7BRw==, tableContent=null), ArticleFig(id=1217486326522364878, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209927726748799792, language=CN, label=图1, caption=
PI薄膜制备流程示意图, figureFileSmall=wMEBvLzglg0p1H08r9j+fA==, figureFileBig=Kgf273ytZ1bad1gtaF7BRw==, tableContent=null), ArticleFig(id=1217486326648194010, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209927726748799792, language=EN, label=Fig.2, caption=
Effect of feeding time on the gel content, figureFileSmall=BeG3L2lmA4zRS37X0yw0qA==, figureFileBig=pXCnhEFMefFktXImcmgT5w==, tableContent=null), ArticleFig(id=1217486326740468703, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209927726748799792, language=CN, label=图2, caption=
加料时间对凝胶量的影响, figureFileSmall=BeG3L2lmA4zRS37X0yw0qA==, figureFileBig=pXCnhEFMefFktXImcmgT5w==, tableContent=null), ArticleFig(id=1217486326841132010, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209927726748799792, language=EN, label=Fig.3, caption=
Effect of stirring speed on the gel content, figureFileSmall=gQzglyqhYvXtWTjwnxAxmQ==, figureFileBig=h3zSkVe9lGuYezcbxj7NVw==, tableContent=null), ArticleFig(id=1217486326945989620, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209927726748799792, language=CN, label=图3, caption=
搅拌速度对凝胶量的影响, figureFileSmall=gQzglyqhYvXtWTjwnxAxmQ==, figureFileBig=h3zSkVe9lGuYezcbxj7NVw==, tableContent=null), ArticleFig(id=1217486327034070011, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209927726748799792, language=EN, label=Fig.4, caption=
Effect of reaction time on the viscosity of polyamide acid solution, figureFileSmall=ytBwFq+ucL2rUM5ww47zKQ==, figureFileBig=XVw7nEJg7JHvJspHpIYU5A==, tableContent=null), ArticleFig(id=1217486327134733312, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209927726748799792, language=CN, label=图4, caption=
反应时间对聚酰胺酸溶液黏度的影响, figureFileSmall=ytBwFq+ucL2rUM5ww47zKQ==, figureFileBig=XVw7nEJg7JHvJspHpIYU5A==, tableContent=null), ArticleFig(id=1217486327206035463, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209927726748799792, language=EN, label=Fig.5, caption=
Effect of reactant molar ratio on the viscosity of polyamide acid used in OLED flexible substrates, figureFileSmall=xns/sbnQVnIf1qYHNPEBAg==, figureFileBig=GtND8tLj4MK2qDtpahtTSA==, tableContent=null), ArticleFig(id=1217486327302504463, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209927726748799792, language=CN, label=图5, caption=
反应物摩尔比对OLED柔性基板用聚酰胺酸黏度的影响, figureFileSmall=xns/sbnQVnIf1qYHNPEBAg==, figureFileBig=GtND8tLj4MK2qDtpahtTSA==, tableContent=null), ArticleFig(id=1217486327432527894, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209927726748799792, language=EN, label=Fig.6, caption=
Molecular structure of polyimide for OLED flexible substrate with aromatic dianhydride and aromatic diamine as monomers, figureFileSmall=XAr/avXHhwJCa+GHWtRB6A==, figureFileBig=pKrlTkNyZuXTPJgFXvqlfA==, tableContent=null), ArticleFig(id=1217486327524802589, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209927726748799792, language=CN, label=图6, caption=
以芳香二酐和芳香二胺为单体的OLED柔性基板用PI分子结构(本文中x=0.445,y=0.5), figureFileSmall=XAr/avXHhwJCa+GHWtRB6A==, figureFileBig=pKrlTkNyZuXTPJgFXvqlfA==, tableContent=null), ArticleFig(id=1217486327612882981, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209927726748799792, language=EN, label=Fig.7, caption=
Effect of imide structure on the properties of polyimide films for OLED flexible substrates, figureFileSmall=lDmlJGAaMnuUdyPIHbANxg==, figureFileBig=rUDZo4BdfTSnpVi9AP+dbQ==, tableContent=null), ArticleFig(id=1217486327747100715, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209927726748799792, language=CN, label=图7, caption=
酰亚胺结构对OLED柔性基板用PI薄膜性能的影响, figureFileSmall=lDmlJGAaMnuUdyPIHbANxg==, figureFileBig=rUDZo4BdfTSnpVi9AP+dbQ==, tableContent=null), ArticleFig(id=1217486327847764019, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209927726748799792, language=EN, label=Fig.8, caption=
Effect of imidization temperature on the properties of polyimide films for OLED flexible substrates, figureFileSmall=6wXLRnHzqNqkWlBQd4puRA==, figureFileBig=qe+MTVct8m0OP8CjD7hltA==, tableContent=null), ArticleFig(id=1217486327902289978, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209927726748799792, language=CN, label=图8, caption=
亚胺化温度对OLED柔性基板PI薄膜性能的影响, figureFileSmall=6wXLRnHzqNqkWlBQd4puRA==, figureFileBig=qe+MTVct8m0OP8CjD7hltA==, tableContent=null), ArticleFig(id=1217486327990370366, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209927726748799792, language=EN, label=Tab.1, caption=
Results of calorimetry experiment for polyamide acid synthesis reaction, figureFileSmall=null, figureFileBig=null, tableContent=
| 参数 | 结果 |
|---|
| 反应过程放热量/kJ | 9.7 |
| 反应液的比热容(35℃)/(J/(g·K)) | 2.14 |
| 反应液物质总量/g | 136.83 |
| Qm(总放热量)/(J/g) | 70.9 |
| 反应绝热温升∆Tad/K | 33.1 |
), ArticleFig(id=1217486328082645063, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209927726748799792, language=CN, label=表1, caption=
聚酰胺酸合成反应量热实验结果
, figureFileSmall=null, figureFileBig=null, tableContent=
| 参数 | 结果 |
|---|
| 反应过程放热量/kJ | 9.7 |
| 反应液的比热容(35℃)/(J/(g·K)) | 2.14 |
| 反应液物质总量/g | 136.83 |
| Qm(总放热量)/(J/g) | 70.9 |
| 反应绝热温升∆Tad/K | 33.1 |
), ArticleFig(id=1217486328158142542, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209927726748799792, language=EN, label=Tab.2, caption=
Effect of temperature on the synthesis of polyamide acid, figureFileSmall=null, figureFileBig=null, tableContent=
| 温度/℃ | -10~0 | 0~10 | 10~20 | 20~30 | 30~40 | 40~50 |
|---|
| 凝胶量/g | 0 | 0 | 0 | 0 | 0.3 | 1.6 |
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温度对聚酰胺酸合成的影响
, figureFileSmall=null, figureFileBig=null, tableContent=
| 温度/℃ | -10~0 | 0~10 | 10~20 | 20~30 | 30~40 | 40~50 |
|---|
| 凝胶量/g | 0 | 0 | 0 | 0 | 0.3 | 1.6 |
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