Phase appearance during polymerization of fluorinated polyimide monomers and deposition into the microscopic‐scale trenches in supercritical carbon dioxide

Phase appearance during polymerization of fluorinated polyimide monomers and deposition into the microscopic‐scale trenches in supercritical carbon dioxide
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DOI:
10.1002/app.43334
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发表时间:
2016-05
影响因子:
3
通讯作者:
Masashi Haruki;A. Oda;Atsuhiko Wasada;Y. Hasegawa;S. Kihara;Shigeki Takishima
Masashi Haruki;A. Oda;Atsuhiko Wasada;Y. Hasegawa;S. Kihara;Shigeki Takishima
中科院分区:
化学3区
文献类型:
--
作者:
Masashi Haruki;A. Oda;Atsuhiko Wasada;Y. Hasegawa;S. Kihara;Shigeki Takishima

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研究了2,2-二(3,4-脱水二羧基苯基)-六氟丙烷(6 FDA)和2,2 ′-二(三氟甲基)-4,4 ′-二氨基联苯(TFDB)在超临界CO2中合成含氟聚酰胺酸(PAA)的相态,为超临界CO2沉积含氟聚酰亚胺(PI)提供了基础数据.所有聚合反应均在30 MPa下进行60 min。实验温度范围为50 - 70 °C,各单体浓度范围为0.67 × 10−5 - 3.3 × 10−5 mol cm−3。透明相的保持时间,即从聚合开始到出现混浊相的时间,随着聚合温度的降低或初始单体浓度的降低而增加。氟化PAA的保持时间比Kapton型PAA的单体的保持时间长。在scCO 2中,将PI沉积到已经形成在硅晶片上的微观尺度沟槽中是成功的。© 2016 Wiley Periodicals,Inc. J.应用聚合物Sci. 2016,133,43334。
The phase appearance during the synthesis of fluorinated polyamic acid (PAA) from 2,2-bis(3,4-anhydrodicarboxyphenyl)-hexafluoropropane (6FDA) and 2,2′-bis(trifluoromethyl)−4,4′-diaminobiphenyl (TFDB) in supercritical carbon dioxide (scCO2) was investigated to obtain fundamental data for the deposition of fluorinate polyimides (PI) using scCO2. All polymerizations were carried out at 30 MPa for 60 min. The experimental temperatures ranged from 50 to 70 °C, and each of the monomer concentrations ranged from 0.67 × 10−5 to 3.3 × 10−5 mol cm−3. The holding time of the transparent phases, which was the time from the beginning of the polymerization to the appearance of a turbid phase, was increased with either a decrease in the polymerization temperature or a decrease in the initial monomer concentration. The holding time of the fluorinated PAA was longer than that of the monomers of Kapton-type PAA. The deposition of PI into the microscopic-scale trenches that had formed on the silicon wafer was successful in scCO2. © 2016 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2016, 133, 43334.