JP2010016130A - 多孔質膜の作製方法、多孔質膜、及び多孔質膜の前駆体組成物の溶液 - Google Patents
多孔質膜の作製方法、多孔質膜、及び多孔質膜の前駆体組成物の溶液 Download PDFInfo
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- JP2010016130A JP2010016130A JP2008173910A JP2008173910A JP2010016130A JP 2010016130 A JP2010016130 A JP 2010016130A JP 2008173910 A JP2008173910 A JP 2008173910A JP 2008173910 A JP2008173910 A JP 2008173910A JP 2010016130 A JP2010016130 A JP 2010016130A
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- ZNOCGWVLWPVKAO-UHFFFAOYSA-N trimethoxy(phenyl)silane Chemical compound CO[Si](OC)(OC)C1=CC=CC=C1 ZNOCGWVLWPVKAO-UHFFFAOYSA-N 0.000 description 1
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Landscapes
- Paints Or Removers (AREA)
- Formation Of Insulating Films (AREA)
- Silicon Compounds (AREA)
Abstract
【解決手段】式:Si(OR1)4及びRa(Si)(OR2)4−a(式中、R1は1価の有機基を表し、Rは水素原子、フッ素原子又は1価の有機基を表し、R2は1価の有機基を表し、aは1〜3の整数であり、R、R1及びR2は同一であっても異なっていてもよい)で示される化合物から選ばれた化合物と、熱分解性有機化合物とを含む多孔質膜の前駆体組成物の溶液であって、pHが5〜9である溶液を基板上に塗布し、所定の温度範囲で焼成させ、得られた多孔質膜に対する紫外線照射後、ヘキサメチルジシラザン、ビス(トリメチルシリル)アセトアミド、トリメチルシリルイミダゾール及びトリメチルアミンジメチルアミンから選ばれた疎水性化合物を所定の温度で気相反応させ、疎水化された多孔質膜を作製する。
【選択図】なし
Description
次の一般式(1):
Si(OR1)4 (1)
で示される化合物(A)、及び次の一般式(2):
Ra(Si)(OR2)4−a (2)
で示される化合物(B)
から選ばれた少なくとも1種の化合物と、250℃以上で熱分解する熱分解性有機化合物(C)とを含有している多孔質膜の前駆体組成物の溶液であって、pHが5〜9である溶液を基板上に塗布し、100〜400℃の温度範囲で乾燥、焼成させ、基板上に形成された多孔質膜に対して、波長157nm〜344nmの紫外線を照射した後、ヘキサメチルジシラザン、ビス(トリメチルシリル)アセトアミド、トリメチルシリルイミダゾール及びトリメチルシリルジメチルアミンから選ばれた有機ケイ素化合物である疎水性化合物を、100〜600℃の温度範囲で気相反応させ、疎水化された多孔質膜を作製することを特徴とする。
Si(OR1)4 (1)
で示される化合物(A)、及び次の一般式(2):
Ra(Si)(OR2)4−a (2)
で示される化合物(B)
から選ばれた少なくとも1種の化合物と、250℃以上で熱分解する熱分解性有機化合物(C)とを含有し、pHが5〜9であることを特徴とする。
Si(OR1)4 (1)
で示される化合物(A)、及び次の一般式(2):
Ra(Si)(OR2)4−a (2)
で示される化合物(B)
加水分解せしめるための弱酸性触媒あるいは弱塩基性触媒を加え、20〜80℃の範囲で30分〜5時間攪拌し、一般式(1)及び(2)で示される化合物を加水分解させ、溶液を調製する。次いで、この溶液を攪拌しながら、界面活性剤を1秒間に100万分の1モルから100分の1モルの範囲内で少量ずつ滴下する。この時、界面活性剤は直接滴下しても有機溶媒等で希釈したものを滴下しても良く、界面活性剤の単位時間あたりの滴下量は界面活性剤の分子量に依存するが、多すぎると界面活性剤の分散が不十分となり、最終的に得られる溶液に不均一が生じる。以上の各原料の混合比は目的とする比誘電率によって適宜決定すればよい。
(アルコキシシラン類)
(有機溶媒)
(触媒)
(界面活性剤)
(上記一般式中、aは0〜2の整数であり、bは0〜4の整数であり、nは8〜24の整数であり、mは0〜12の整数であり、Lは1〜24の整数であり、Xは1価の有機アニオンを表す。)で示されるアルキルアンモニウム塩の使用が好ましい。a、b、n、m、Lがこの範囲内であり、Xがこのようなイオンであれば、形成される孔が適当な大きさとなり、孔形成後の気相反応において対象化合物が十分に孔内へ浸透し、目的とする重合反応が生じる。
(疎水性化合物)
(比較例1)
Claims (9)
- 次の一般式(1):
Si(OR1)4 (1)
で示される化合物(A)、及び次の一般式(2):
Ra(Si)(OR2)4−a (2)
で示される化合物(B)
(上記式(1)及び(2)中、R1は1価の有機基を表し、Rは水素原子、又は1価の有機基を表し、R2は1価の有機基を表し、aは1〜3の整数であり、R、R1及びR2は同一であっても異なっていてもよい。)
から選ばれた少なくとも1種の化合物と、250℃以上で熱分解する熱分解性有機化合物(C)とを含有している多孔質膜の前駆体組成物の溶液であって、pHが5〜9である溶液を基板上に塗布し、100〜400℃の温度範囲で乾燥、焼成させ、基板上に形成された多孔質膜に対して、波長157nm〜344nmの紫外線を照射した後、ヘキサメチルジシラザン、ビス(トリメチルシリル)アセトアミド、トリメチルシリルイミダゾール及びトリメチルシリルジメチルアミンから選ばれた有機ケイ素化合物である疎水性化合物を、100〜600℃の温度範囲で気相反応させ、疎水化された多孔質膜を作製することを特徴とする多孔質膜の作製方法。 - 前記熱分解性有機化合物(C)が、分子量200〜5000の界面活性剤を少なくとも1種含んでいることを特徴とする請求項1記載の多孔質膜の作製方法。
- 前記前駆体組成物中に含まれる金属イオン不純物が、10ppb以下であることを特徴とする請求項1又は2に記載の多孔質膜の作製方法。
- 前記前駆体組成物の溶液が、弱塩基性触媒、又は有機酸及び過酸化物から選ばれた弱酸性触媒を含んでいることを特徴とする請求項1〜3のいずれかに記載の多孔質膜の作製方法。
- 請求項1〜4のいずれかに記載の多孔質膜の作製方法に従って得られたことを特徴とする多孔質膜。
- 次の一般式(1):
Si(OR1)4 (1)
で示される化合物(A)、及び次の一般式(2):
Ra(Si)(OR2)4−a (2)
で示される化合物(B)
(上記式(1)及び(2)中、R1は1価の有機基を表し、Rは水素原子、又は1価の有機基を表し、R2は1価の有機基を表し、aは1〜3の整数であり、R、R1及びR2は同一であっても異なっていてもよい。)
から選ばれた少なくとも1種の化合物と、250℃以上で熱分解する熱分解性有機化合物(C)とを含有し、pHが5〜9であることを特徴とする多孔質膜の前駆体組成物の溶液。 - 前記前駆体組成物の溶液が、弱塩基性触媒、又は有機酸及び過酸化物から選ばれた弱酸性触媒を含んでいることを特徴とする請求項6記載の多孔質膜の前駆体組成物の溶液。
- 前記熱分解性有機化合物(C)が、分子量200〜5000の界面活性剤を少なくとも1種含んでいることを特徴とする請求項6又は7記載の多孔質膜の前駆体組成物の溶液。
- 前記前駆体組成物中に含まれる金属イオン不純物が、10ppb以下であることを特徴とする請求項5〜8のいずれかに記載の多孔質膜の前駆体組成物の溶液。
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