2020年聚酰亚胺薄膜和尺寸稳定及其制备工艺精品版.pdf
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1、精选文档 United States PatentUnited States Patent Kumagawa ,Kumagawa , et al. et al. 4,725,4844,725,484 February 16, 1988February 16, 1988 Dimensionally stablepolyimide filmpolyimide filmand process for preparation thereof AbstractAbstract A dimensionally stable polyimidefilmfilm and processes for the p
2、reparation thereof. The polyimidefilmfilmis composed of an aromatic polyimide obtained from a solution of a polymer formed by polymerization of a biphenyl-tetracarboxylic acid and a phenylene diamine, wherein the average linear expansion coefficient of the polyimidefilmfilm in the temperature range
3、of from 50.degree. C. to 300.degree. C. is 0.1.times.10.sup.-5 to 2.5.times.10.sup.-5 cm/cm.degree.C., the ratio of the linear expansion coefficient in the machine direction of thefilmfilm to the linear expansion coefficient in the transverse direction of the filmfilmis in the range of from 1/5 to 4
4、, and the thermal dimension stability expressed by the ratio of the change of the size of thefilmfilm at normal temperature after the heat treatment where the temperature is elevated to 400.degree. C. from normal temperature and thefilmfilm is maintained at 400.degree. C. for 2 hours is less than 0.
5、3%. Kumagawa; KiyoshiKumagawa; Kiyoshi (Ube, JPJP), Kuniyasu; Kenji, Kuniyasu; Kenji (Ube, JPJP), , Inventors: Nishino; ToshiyukiNishino; Toshiyuki (Ube, JPJP), Matsui; Yuji, Matsui; Yuji (Ube, JPJP) Assignee: Ube Industries, Ltd.Ube Industries, Ltd. (Yamaguchi, JPJP) Appl. No.: 06/864,29906/864,299
6、 Filed:May 16, 1986May 16, 1986 Foreign Application Priority DataForeign Application Priority Data 精选文档 精选文档 May 17, 1985 JP May 17, 1985 JP Current U.S. Class:Current U.S. Class: 60-103674 60-103675 428/220428/220 ; 428/473.5; 428/901; 528/353 CurrentCurrent InternationalInternational Class:Class:C
7、08J 5/18(20060101); B32B 027/28(); B32B 027/34(); C08G 069/26() Field of Search:Field of Search:428/473.5,220,901 528/353 264/212 References CitedReferences Cited Referenced ByReferenced By Foreign Patent DocumentsForeign Patent Documents Jan., 1980 Jan., 1980 007805 0007805 JP JP Primary Examiner:
8、Herbert; Thomas J. Attorney, Agent or Firm: Burgess, Ryan cm/cm/.degree.C.)wasdetermined according to the following procedures. Namely, a test piece (5 mm.times.20 mm) was set at a thermal mechanical analysis apparatus (supplied by Rigaku Denki K. K.) adopting the tensile load method, and the temper
9、ature was elevated at a rate of 10.degree. C./min to 300.degree. C. from normal temperature. The test piece was maintained at 300.degree. C. for 1 minute, and the temperature was lowered to normal temperature at a rate of 5.degree. to 20.degree. C./min. The average linear expansion coefficient calcu
10、lated from the change (.DELTA.L.sub.1) of the length observed when the temperature was lowered from 300.degree. C. to 50.degree. C. and the original length (L.sub.1 ; 10 mm) of the test piece according to the following calculation formula: The thermal dimension stability was determined according to
11、the following procedures. A dehydrated test piece (5 mm.times.20 mm) was set at the same thermal mechanical analysis apparatus as described above, and the temperature was elevated at a rate of 10.degree. C./min from normal 精选文档 精选文档 temperature to 400.degree. C. The test piece was maintained at 400.
12、degree. C. for 2 hours and the temperature was lowered at a rate of 5.degree. to 20.degree. C./min to normal temperature. The thermal dimension stability was calculated from the difference (.DELTA.L.sub.2) between the length of the test piece at normal temperature before the heating and the length o
13、f the test piece at normal temperature after the heating and the original length (L.sub.2 ; 10 mm) of the test piece according to the following calculation formula: EXAMPLE 1 (Preparation of Dope) A cylindrical polymerization tank having an inner capacity of 50 l was chargedwith38.1kgofN,N-dimethyla
14、cetamide,and5.2959kgof 3,3,4,4-biphenyltetracarboxylic dianhydride was added and 1.9466 kg of p-phenylene diamine was gradually added with stirring. The reaction liquid was stirred at 30.degree. C. for about 10 hours to effect polymerization between both the components and form a polyamic acid. The
15、logarithmic viscosity number (as determined at 30.degree. C.) of the polyamic acid formed by the polymerization reaction was 3.10, and the rotation viscosity (as determined at 30.degree. C.) of the solution of the polyamic acid was 25,000 poise. (Formation of theFilmFilm) The solution of thepolyamic
16、 acid wasused as thefilmfilm-forming dope. The dope was extruded at 30.degree. C. in the form of a thin layer through a slit of T-die (lip distance =0.5 mm, lip width =650 mm), and the thin layer of the dopewas continuously supplied onto a smooth metalbelt and was subjected to the drying of the firs
17、t stage on the belt by hot air maintained at about 120.degree. C. to form a solidifiedfilmfilmmember. Then, the solidifiedfilmfilm member was peeled from the belt and was cut into a square piece having a side of 200 mm. One side of the square piece of the filmfilm member was secured to a frame by a
18、pin sheet, and a load of about 35 g was uniformly applied to the opposite sides of the square piece along the entire width thereof by dancers to place the square piece under a low tension (a tension of 7.0 g/mm.sup.2 with respect to the machine direction of the solidifiedfilmfilmmember). In this sta
19、te, the temperature was elevated to 190.degree. C. over a period of about 30 seconds and the drying of the second stage was carried out at 190.degree. C. for 5 minutes to form a solidifiedfilmfilm. The four sides of the square piece of the solidifiedfilmfilm were held and fixed by pin tenter, and th
20、e temperature 精选文档 精选文档 of the solidifiedfilmfilm was elevated at a rate of about10.degree. C./min and thefilmfilmwas dried and heat-treated (imidized) at 450.degree. C. for 30 minutes to form an aromatic polyimidefilmfilm having a thickness of 25 .mu.m. The contents of the volatile components such
21、as the solvent and formed water in the solidifiedfilmfilm member after the drying ofthe first stage, the solidifiedfilmfilm after the drying of the second stage under a low tension and the aromatic polyimidefilm,film,and the properties of the obtained aromatic polyimidefilmfilm are shown in Table 1.
22、 COMPARATIVE EXAMPLE 1 An aromatic polyimidefilmfilm was prepared in the same manner as described in Example 1 except that the square piece of the solidifiedfilmfilm member was not subjected tc the drying of the second stage but was directly dried and heat-treated in the high-temperature heat treatm
23、ent apparatus. The obtained results are shown in Table 1. EXAMPLE 2 A solution of a polyamic acid prepared in the same manner as described in Example 1 was used as thefilmfilm-forming dope, and the dope was extruded at about 30.degree. C. in the form of a thin layer through a slip of a T-die (lip di
24、stance =0.5 mm, lip width =650 mm) and the thin layer of the dope was continuously placed on a smooth metal belt. Thefilmfilmwas subjected to the drying of the first stage on the belt by hot air maintained at about 120.degree. C. to form a solidifiedfilmfilm member continuously. Then, the solidified
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