JP3069654B2 - Method of forming polydiphenylsiloxane - Google Patents
Method of forming polydiphenylsiloxaneInfo
- Publication number
- JP3069654B2 JP3069654B2 JP9331129A JP33112997A JP3069654B2 JP 3069654 B2 JP3069654 B2 JP 3069654B2 JP 9331129 A JP9331129 A JP 9331129A JP 33112997 A JP33112997 A JP 33112997A JP 3069654 B2 JP3069654 B2 JP 3069654B2
- Authority
- JP
- Japan
- Prior art keywords
- film
- polydiphenylsiloxane
- substrate
- cyclic
- cyclic diphenylsiloxane
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
- -1 polydiphenylsiloxane Polymers 0.000 title claims description 60
- 238000000034 method Methods 0.000 title claims description 15
- 229910052751 metal Inorganic materials 0.000 claims description 20
- 239000002184 metal Substances 0.000 claims description 20
- 239000000758 substrate Substances 0.000 claims description 18
- 239000010419 fine particle Substances 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 12
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 11
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 11
- 238000007151 ring opening polymerisation reaction Methods 0.000 claims description 9
- 238000000354 decomposition reaction Methods 0.000 claims description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 6
- 229910052802 copper Inorganic materials 0.000 claims description 6
- 239000010949 copper Substances 0.000 claims description 6
- 229910052763 palladium Inorganic materials 0.000 claims description 5
- 229910052697 platinum Inorganic materials 0.000 claims description 5
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 3
- 229910052737 gold Inorganic materials 0.000 claims description 3
- 239000010931 gold Substances 0.000 claims description 3
- 229910052709 silver Inorganic materials 0.000 claims description 3
- 239000004332 silver Substances 0.000 claims description 3
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims 1
- 239000010408 film Substances 0.000 description 33
- 239000010410 layer Substances 0.000 description 12
- VCYDUTCMKSROID-UHFFFAOYSA-N 2,2,4,4,6,6-hexakis-phenyl-1,3,5,2,4,6-trioxatrisilinane Chemical compound O1[Si](C=2C=CC=CC=2)(C=2C=CC=CC=2)O[Si](C=2C=CC=CC=2)(C=2C=CC=CC=2)O[Si]1(C=1C=CC=CC=1)C1=CC=CC=C1 VCYDUTCMKSROID-UHFFFAOYSA-N 0.000 description 9
- 238000006116 polymerization reaction Methods 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 6
- 230000008018 melting Effects 0.000 description 5
- 238000002844 melting Methods 0.000 description 5
- 229920000642 polymer Polymers 0.000 description 5
- 229920006254 polymer film Polymers 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- 229910001111 Fine metal Inorganic materials 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 238000000862 absorption spectrum Methods 0.000 description 3
- 239000002923 metal particle Substances 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- 229920001296 polysiloxane Polymers 0.000 description 3
- 238000007740 vapor deposition Methods 0.000 description 3
- VSIKJPJINIDELZ-UHFFFAOYSA-N 2,2,4,4,6,6,8,8-octakis-phenyl-1,3,5,7,2,4,6,8-tetraoxatetrasilocane Chemical compound O1[Si](C=2C=CC=CC=2)(C=2C=CC=CC=2)O[Si](C=2C=CC=CC=2)(C=2C=CC=CC=2)O[Si](C=2C=CC=CC=2)(C=2C=CC=CC=2)O[Si]1(C=1C=CC=CC=1)C1=CC=CC=C1 VSIKJPJINIDELZ-UHFFFAOYSA-N 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000002861 polymer material Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- WSLDOOZREJYCGB-UHFFFAOYSA-N 1,2-Dichloroethane Chemical compound ClCCCl WSLDOOZREJYCGB-UHFFFAOYSA-N 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- 241001655798 Taku Species 0.000 description 1
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 238000007611 bar coating method Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 150000008282 halocarbons Chemical class 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 238000000608 laser ablation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 238000007142 ring opening reaction Methods 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 238000012719 thermal polymerization Methods 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
Landscapes
- Silicon Polymers (AREA)
- Coating Of Shaped Articles Made Of Macromolecular Substances (AREA)
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、耐熱性を有しかつ
溶解性の乏しいポリジフェニルシロキサン膜を基板上に
容易に構築するためのポリジフェニルシロキサンの製膜
方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for forming a polydiphenylsiloxane film having high heat resistance and poor solubility on a substrate with ease.
【０００２】[0002]
【従来の技術】高分子材料を電気素子、光素子の部材へ
の応用する際、基板上へ薄い膜（フィルム）を形成する
ことが重要な技術要素であることは周知である。溶融成
形で形成したフィルムを基体上に張り合わせるよりも、
溶媒に高分子を溶解して塗布するのが一般的である。ポ
リシロキサンは分解温度が高く、電気的性質が優れた高
分子材料として種々の用途で使用されている。ポリシロ
キサンの中でもポリジフェニルシロキサンは、高い結晶
性を有する熱可塑性高分子として知られ、耐熱性に優れ
ている。ポリジフェニルシロキサンの一つの製造方法
は、フェニル基置換環状シロキサンをアルカリ、或いは
アルカリ土類金属を触媒として開環重合する方法が取ら
れている。しかし、この方法では、不融、不溶性のポリ
ジフェニルシロキサンを与えるため、成形ができない高
分子しか得られない。近年、重合度を低く押さえ溶媒に
対する溶解性を保持させ、有機化学的に結合させうる官
能基を末端に導入して加工した後にオリゴマーを高分子
化する方法が提案されている。2. Description of the Related Art It is well known that forming a thin film (film) on a substrate is an important technical element when applying a polymer material to members of an electric element and an optical element. Rather than laminating a film formed by melt molding on a substrate,
Generally, a polymer is dissolved in a solvent and applied. Polysiloxane is used in various applications as a polymer material having a high decomposition temperature and excellent electrical properties. Among polysiloxanes, polydiphenylsiloxane is known as a thermoplastic polymer having high crystallinity and has excellent heat resistance. One method for producing polydiphenylsiloxane is to carry out ring-opening polymerization of a phenyl group-substituted cyclic siloxane using an alkali or alkaline earth metal as a catalyst. However, in this method, an infusible or insoluble polydiphenylsiloxane is provided, so that only a polymer that cannot be molded can be obtained. In recent years, a method has been proposed in which the degree of polymerization is kept low, the solubility in a solvent is maintained, and a functional group that can be chemically bonded is introduced into the terminal to process the oligomer, followed by polymerizing the oligomer.
【０００３】[0003]
【発明が解決しようとする課題】本発明は、成形加工が
極めて困難なポリジフェニルシロキサンの製膜方法を提
供することをその課題とする。SUMMARY OF THE INVENTION An object of the present invention is to provide a method for forming a polydiphenylsiloxane which is extremely difficult to mold.
【０００４】[0004]
【課題を解決するための手段】本発明者らは、前記課題
を解決すべく鋭意研究を重ねた結果、本発明を完成する
に至った。即ち、本発明によれば、基板上に環状ジフェ
ニルシロキサン膜を形成し、該膜上に金、白金、パラジ
ウム、銅及び銀からなる群から選ばれた金属からなる金
属微粒子層を形成した後、該環状ジフェニルシロキサン
膜をポリジフェニルシロキサンの分解温度未満の温度で
加熱して該環状ジフェニルシロキサンを開環重合させる
ことを特徴とするポリジフェニルシロキサンの製膜方
法。Means for Solving the Problems The present inventors have conducted intensive studies to solve the above-mentioned problems, and as a result, have completed the present invention. That is, according to the present invention, after forming a cyclic diphenylsiloxane film on a substrate and forming a metal fine particle layer made of a metal selected from the group consisting of gold, platinum, palladium, copper and silver on the film, A method for forming a film of polydiphenylsiloxane, comprising heating the cyclic diphenylsiloxane film at a temperature lower than the decomposition temperature of polydiphenylsiloxane to cause ring-opening polymerization of the cyclic diphenylsiloxane.
【０００５】[0005]
【発明の実施の形態】本発明で用いる環状ジフェニルシ
ロキサンとしては、ヘキサフェニルシクロトリシロキサ
ンや、オクタフェニルシクロテトラシロキサンが挙げら
れるが、前者の方が開環の重合に必要とされる環歪みエ
ネルギーが大きいので好ましく使用される。BEST MODE FOR CARRYING OUT THE INVENTION The cyclic diphenylsiloxane used in the present invention includes hexaphenylcyclotrisiloxane and octaphenylcyclotetrasiloxane. The former is the ring strain energy required for ring-opening polymerization. Is preferably used because it is large.
【０００６】本発明は基板上に環状ジフェニルシロキサ
ン膜を形成し、その上に所定の金属微粒子層形成し、こ
れを加熱して開環重合によりポリジフェニルシロキサン
を得るものである。前記環状ジフェニルシロキサン膜
は、好適には、蒸着法により形成される。この場合に
は、環状ジフェニルシロキサンを減圧下において加熱気
化させ、基板上に推積させる。この方法においては、基
板表面を蒸着速度を速める環状ジフェニルシロキサンの
開環反応を起こさない温度に加熱しておいても構わな
い。前記蒸着法には、スパッタ法や、ＣＶＤ法、真空蒸
着法等が包含される。また、基板上に環状ジフェニルシ
ロキサン膜を形成する他の方法としては、環状ジフェニ
ルシロキサンの有機溶媒溶液をスピンコート法やバーコ
ート法、浸漬法等によって基板上に塗布し、乾燥する方
法が挙げられる。環状ジフェニルシロキサンを溶解させ
るための有機溶媒としては、トルエン、キシレン等の芳
香族炭化水素；塩化メチレン、クロロホルム、塩化エチ
レン等のハロゲン化炭化水素等が挙げられる。その乾燥
雰囲気としては、大気、不活性ガス、真空雰囲気等が採
用される。環状ジフェニルシロキサン膜の厚さは重要で
はなく、目的、用途に応じて設定される。According to the present invention, a cyclic diphenylsiloxane film is formed on a substrate, a predetermined metal fine particle layer is formed thereon, and this is heated to obtain polydiphenylsiloxane by ring-opening polymerization. The cyclic diphenylsiloxane film is preferably formed by a vapor deposition method. In this case, the cyclic diphenylsiloxane is heated and vaporized under reduced pressure and deposited on the substrate. In this method, the substrate surface may be heated to a temperature at which the ring-opening reaction of the cyclic diphenylsiloxane that increases the deposition rate does not occur. The vapor deposition method includes a sputtering method, a CVD method, a vacuum vapor deposition method, and the like. Further, as another method of forming a cyclic diphenylsiloxane film on a substrate, a method of applying an organic solvent solution of cyclic diphenylsiloxane on a substrate by a spin coating method, a bar coating method, a dipping method, or the like, and then drying the organic solvent solution may be mentioned. . Examples of the organic solvent for dissolving the cyclic diphenylsiloxane include aromatic hydrocarbons such as toluene and xylene; and halogenated hydrocarbons such as methylene chloride, chloroform and ethylene chloride. As the drying atmosphere, air, an inert gas, a vacuum atmosphere, or the like is used. The thickness of the cyclic diphenylsiloxane film is not important and is set according to the purpose and application.
【０００７】前記基板としては、シリコンウエハー、金
属、セラミックス、プラスチック等の各種の材料からな
るものが使用される。基板の表面形状は、平面状や、曲
面状、球面状等の各種の形状であることができる。As the substrate, those made of various materials such as a silicon wafer, metal, ceramics and plastic are used. The surface shape of the substrate can be various shapes such as a flat shape, a curved shape, and a spherical shape.
【０００８】前記のようにして基板上に形成された環状
ジフェニルシロキサン膜上には、金属微粒子層を形成す
るが、このためには、蒸着法、スパッタリング法、レー
ザーアブレーション法等を用いることができる。使用さ
れる金属は、金、白金、パラジウム、銅及び銀からなる
群から選ばれる１種の金属又は２種以上の金属の組合わ
せでもよい。A fine metal particle layer is formed on the cyclic diphenylsiloxane film formed on the substrate as described above. For this purpose, an evaporation method, a sputtering method, a laser ablation method, or the like can be used. . The metal used may be one metal selected from the group consisting of gold, platinum, palladium, copper and silver, or a combination of two or more metals.
【０００９】金属微粒子層は、金属微粒子が環状ジフェ
ニルシロキサン膜に拡散し得るならば、その厚さは重要
ではなく、連続相であることもない。The thickness of the metal fine particle layer is not important and is not a continuous phase as long as the metal fine particles can diffuse into the cyclic diphenylsiloxane film.
【００１０】次に、前記のようにして基板上に形成さ
れ、表面層として金属微粒子層が形成された環状ジフェ
ニルシロキサン膜は、これをポリジフェニルシロキサン
の分解温度未満の温度で加熱する。この加熱によって、
金属微粒子は、膜中に拡散してその開環重合を誘起させ
る。これによって、基板上の環状ジフェニルシロキサン
膜は、ポリジフェニルシロキサン膜に変換される。前記
環状ジフェニルシロキサン膜の加熱温度は、それが開環
重合する温度であればよく、その融点より低い温度でも
よいが、得られる重合体膜の内部応力を除去した安定な
構造の重合膜を迅速に形成するには、その融点以上の温
度であることが好ましい。従って、前記加熱温度は、そ
の環状ジフェニルシロキサンの融点よりも３０〜５０℃
低い温度から、重合体の分解温度より低い温度であり、
好ましくは環状ジフェニルシロキサンの融点以上でその
重合体の分解温度より低い温度である。環状ジフェニル
シロキサンがヘキサフェニルシクロトリシロキサンの場
合には、その融点である１８８℃からその重合体（ポリ
ジフェニルシロキサン）の分解温度である約５００℃の
範囲の温度の使用が好ましい。さらに、重合速度の点か
らは、高い温度の使用が好ましく、特に、ポリジフェニ
ルシロキサンの相転移温度は約２５０℃であることか
ら、２００〜３００℃の温度の使用がより好ましい。加
熱雰囲気は特に制約されず、不活性ガス雰囲気、真空雰
囲気、空気雰囲気等である。Next, the cyclic diphenylsiloxane film formed on the substrate as described above and having the fine metal particle layer formed thereon as the surface layer is heated at a temperature lower than the decomposition temperature of polydiphenylsiloxane. With this heating,
The metal fine particles diffuse into the film to induce its ring-opening polymerization. Thereby, the cyclic diphenylsiloxane film on the substrate is converted into a polydiphenylsiloxane film. The heating temperature of the cyclic diphenylsiloxane film may be a temperature at which it is subjected to ring-opening polymerization, and may be a temperature lower than its melting point, but a polymer film having a stable structure in which the internal stress of the obtained polymer film has been removed is quickly obtained. It is preferable that the temperature be equal to or higher than the melting point. Therefore, the heating temperature is 30 to 50 ° C. lower than the melting point of the cyclic diphenylsiloxane.
From a lower temperature to a temperature lower than the decomposition temperature of the polymer,
Preferably, the temperature is higher than the melting point of the cyclic diphenylsiloxane and lower than the decomposition temperature of the polymer. When the cyclic diphenylsiloxane is hexaphenylcyclotrisiloxane, it is preferable to use a temperature in the range of 188 ° C, which is the melting point, to about 500 ° C, which is the decomposition temperature of the polymer (polydiphenylsiloxane). Further, from the viewpoint of the polymerization rate, it is preferable to use a high temperature. In particular, since the phase transition temperature of polydiphenylsiloxane is about 250 ° C., it is more preferable to use a temperature of 200 to 300 ° C. The heating atmosphere is not particularly limited, and may be an inert gas atmosphere, a vacuum atmosphere, an air atmosphere, or the like.
【００１１】前記加熱による環状ジフェニルシロキサン
の重合は、酸素によって禁止されない機構で重合が進行
していることを示す。加熱によって環状ジフェニルシロ
キサンの開環重合が生じ、ポリジフェニルシロキサンが
生成したことは、その赤外スペクトルを観測することに
より確認することができる。即ち、その赤外スペクトル
を測定すると、ヘキサフェニルシクロトリシロキサン構
造に由来する１０００ｃｍ-1〜１１００ｃｍ-1付近にあ
る３本のピークがブロードな１本の吸収に変化すること
から環状ジフェニルシロキサンが開環重合したことが容
易に確認される。The polymerization of cyclic diphenylsiloxane by heating indicates that the polymerization is proceeding by a mechanism not inhibited by oxygen. It can be confirmed by observing the infrared spectrum that the ring-opening polymerization of the cyclic diphenylsiloxane occurs due to the heating and the polydiphenylsiloxane is formed. In other words, the Measurement of the infrared spectrum, cyclic diphenylsiloxane since the three peaks in the vicinity 1000cm -1 ~1100cm -1 derived from hexaphenylcyclotrisiloxane structure changes in the absorption of a single broad open It is easily confirmed that ring polymerization has occurred.
【００１２】このようにして得られたポリジフェニルシ
ロキサン膜表面からは金属微粒子層が消失することが確
認されている。つまり、加熱による重合工程中に金属微
粒子が環状ジフェニルシロキサン中に拡散し、その結
果、重合膜中に分散する。ＥＳＣＡを用いて表面観測し
たとき金属原子を示すピーク強度は極端に微弱である
が、その膜をエッチングしていくと膜内部に金属が分布
していることが認められている。It has been confirmed that the fine metal particle layer disappears from the surface of the polydiphenylsiloxane film thus obtained. That is, the metal fine particles diffuse into the cyclic diphenylsiloxane during the polymerization process by heating, and as a result, are dispersed in the polymerized film. When the surface is observed using ESCA, the peak intensity indicating a metal atom is extremely weak, but it is recognized that the metal is distributed inside the film as the film is etched.
【００１３】因みに、予め本発明で使用される金属微粒
子膜を基体上に形成させておき、その上にヘキサフェニ
ルシクロトリシロキサン膜を形成させて同様の加熱条件
で処理しても、目的とするポリジフェニルシロキサンは
実質上生成しない。また、金属微粒子層を有していない
ヘキサフェニルシクロトリシロキサン膜は同一条件では
重合しない。本発明における重合機構は現時点では定か
でないが、金属微粒子が環状ジフェニルシロキサン膜中
に拡散し、酸素に影響されない機構で重合が進行するも
のと考えられている。Incidentally, even if a metal fine particle film used in the present invention is previously formed on a substrate, and a hexaphenylcyclotrisiloxane film is formed thereon and then treated under the same heating conditions, the object is achieved. Substantially no polydiphenylsiloxane is formed. The hexaphenylcyclotrisiloxane film having no metal fine particle layer does not polymerize under the same conditions. Although the polymerization mechanism in the present invention is not clear at present, it is considered that the metal fine particles diffuse into the cyclic diphenylsiloxane film and the polymerization proceeds by a mechanism not affected by oxygen.
【００１４】本発明では、金属微粒子層をパターン状に
環状ジフェニルシロキサン膜上に形成させて加熱するこ
とによって、ポリジフェニルシロキサンのパターンを容
易に作成することができる。金属微粒子層が施されてい
ない部分の環状ジフェニルシロキサン膜は、上述の温度
処理だけでは重合しないため、環状ジフェニルシロキサ
ンを溶解する溶媒で溶解除去することができる。In the present invention, a pattern of polydiphenylsiloxane can be easily formed by forming a metal fine particle layer on the cyclic diphenylsiloxane film in a pattern and heating. Since the portion of the cyclic diphenylsiloxane film on which the metal fine particle layer is not applied is not polymerized only by the above-described temperature treatment, it can be dissolved and removed with a solvent that dissolves the cyclic diphenylsiloxane.
【００１５】[0015]
【発明の効果】本発明により、基板上への薄膜形成を含
めてポリジフェニルシロキサン膜の形成が可能となり、
また、耐熱性、耐溶剤性に優れたポリジフェニルシロキ
サンパターンを形成することができる。According to the present invention, a polydiphenylsiloxane film including a thin film on a substrate can be formed.
Further, a polydiphenylsiloxane pattern having excellent heat resistance and solvent resistance can be formed.
【００１６】[0016]
【実施例】次に本発明を実施例によりさらに詳述する。Next, the present invention will be described in more detail by way of examples.
【００１７】実施例１ 再結晶したヘキサフェニルシクロトリシロキサンをシリ
コーンウエハー上に真空蒸着して厚さ１．２ミクロンの
膜を形成し、その上に白金／パラジウム（重量比＝８０
／２０）を１０-3Ｔｏｒｒの空気プラズマでスパッタし
て、４ｎｍのＰｔ／Ｐｄ微粒子層を形成した。これを真
空チャンバーから取り出し、予め２４０℃に加熱した加
熱炉で、空気中で２時間加熱した。生成した膜の赤外吸
収スペクトルを測定した。その結果、ヘキサフェニルシ
クロトリシロキサンが開環重合したことが確認された。
また、この膜については、熱重合で得たポリジフェニル
シロキサンの赤外吸収スペクトルと同じスペクトルが観
測された。このことからも、ポリジフェニルシロキサン
が生成したことが確認された。Example 1 A recrystallized hexaphenylcyclotrisiloxane was vacuum-deposited on a silicone wafer to form a film having a thickness of 1.2 μm, and platinum / palladium (weight ratio = 80) was formed thereon.
/ 20) was sputtered with 10 −3 Torr air plasma to form a 4 nm Pt / Pd fine particle layer. This was taken out of the vacuum chamber and heated in air in a heating furnace previously heated to 240 ° C. for 2 hours. The infrared absorption spectrum of the formed film was measured. As a result, it was confirmed that ring opening polymerization of hexaphenylcyclotrisiloxane was performed.
In this film, the same spectrum as the infrared absorption spectrum of polydiphenylsiloxane obtained by thermal polymerization was observed. This also confirmed that polydiphenylsiloxane was produced.
【００１８】実施例２ 実施例１において、白金／パラジウムに代えて銅を用い
た以外は同様にして実験を行い、ヘキサフェニルシクロ
トリシロキサン膜上に３ｎｍの銅微粒子層を形成した。
これを空気中、２４０℃で２時間加熱した。得られた重
合体膜の赤外吸収スペクトルを測定した。前記実施例１
の場合と同じスペクトルが観測され、ポリジフェニルシ
ロキサンの生成が確認された。Example 2 An experiment was conducted in the same manner as in Example 1 except that copper was used instead of platinum / palladium, and a 3 nm-thick copper fine particle layer was formed on a hexaphenylcyclotrisiloxane film.
This was heated in air at 240 ° C. for 2 hours. The infrared absorption spectrum of the obtained polymer film was measured. Example 1
The same spectrum as in the case of was observed, and the formation of polydiphenylsiloxane was confirmed.
【００１９】実施例３ 実施例１において、オクタフェニルシクロテトラシロキ
サンを用いたほかはまったく同様にして実験を行った。
得られた重合体膜のスペクトルを測定したところ、ポリ
ジフェニルシロキサンと同じスペクトルが観測され、ポ
リジフェニルシロキサンが生成したことが確認された。Example 3 An experiment was conducted in exactly the same manner as in Example 1 except that octaphenylcyclotetrasiloxane was used.
When the spectrum of the obtained polymer film was measured, the same spectrum as that of polydiphenylsiloxane was observed, and it was confirmed that polydiphenylsiloxane was formed.
【００２０】比較例１ 銅微粒子層をシリコン基板上に形成しておき、その上に
ヘキサフェニルシクロトリシロキサンを蒸着し、実施例
１と同じ条件で加熱したが、この場合にはポリジフェニ
ルシロキサンは生成しなかった。Comparative Example 1 A copper fine particle layer was formed on a silicon substrate, hexaphenylcyclotrisiloxane was deposited thereon, and heated under the same conditions as in Example 1. In this case, polydiphenylsiloxane was used. Did not generate.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 鈴木 正昭 北海道札幌市豊平区月寒東２条17丁目２ 番１号 工業技術院北海道工業技術研究 所内 (72)発明者 中田 善徳 北海道札幌市豊平区月寒東２条17丁目２ 番１号 工業技術院北海道工業技術研究 所内 (72)発明者 永井 秀明 北海道札幌市豊平区月寒東２条17丁目２ 番１号 工業技術院北海道工業技術研究 所内 (72)発明者 奥谷 猛 北海道札幌市豊平区月寒東２条17丁目２ 番１号 工業技術院北海道工業技術研究 所内 (72)発明者 櫛引 信男 神奈川県藤沢市辻堂元町２−21−10− 305 (72)発明者 村上 正志 神奈川県秦野市尾尻389−３ (72)発明者 小川 ▲琢▼哉 神奈川県秦野市千村286−10 審査官 原田 隆興 (56)参考文献 特開 平７−18076（ＪＰ，Ａ) (58)調査した分野(Int.Cl.7，ＤＢ名) C08G 77/06 C08J 7/04 ──────────────────────────────────────────────────続 き Continuing on the front page (72) Inventor Masaaki Suzuki 2-17-1, Tsukikan East, Toyohira-ku, Sapporo-city, Hokkaido Inside the Institute of Industrial Technology, Hokkaido Institute of Industrial Technology (72) Inventor Yoshinori Nakata Tsukikan, Toyohira-ku, Sapporo, Hokkaido Higashi 2-Jo 17-2-1, Hokkaido Institute of Industrial Technology, Hokkaido Institute of Industrial Technology (72) Inventor Hideaki Nagai Hokkaido Sapporo City, Toyohira-ku, Tsukikan Higashi 2-Jo 17-2-1, Hokkaido Institute of Technology, Hokkaido Institute of Industrial Technology (72) Inventor Takeshi Okutani 2-1-1-17 Tsukikan-Higashi, Toyohira-ku, Sapporo-city, Hokkaido In-house Hokkaido Institute of Industrial Technology (72) Inventor Nobuo Kushibiki 2-21-10-305, Tsujido Motomachi, Fujisawa-shi, Kanagawa-ken (72) Inventor Masashi Murakami 389-3 Ojiri, Hadano-shi, Kanagawa Prefecture (72) Inventor ▲ Taku ▼ ya 286-10 Chimura, Hadano-shi, Kanagawa Examiner Takayuki Harada (56 References JP-A-7-18076 (JP, A) (58) Fields investigated (Int. Cl. 7 , DB name) C08G 77/06 C08J 7/04
Claims (1)
形成し、該膜上に金、白金、パラジウム、銅及び銀から
なる群から選ばれた金属からなる金属微粒子層を形成し
た後、該環状ジフェニルシロキサン膜をポリジフェニル
シロキサンの分解温度未満の温度で加熱して該環状ジフ
ェニルシロキサンを開環重合させることを特徴とするポ
リジフェニルシロキサンの製膜方法。1. A cyclic diphenylsiloxane film is formed on a substrate, and a metal fine particle layer made of a metal selected from the group consisting of gold, platinum, palladium, copper and silver is formed on the film. A method for forming a polydiphenylsiloxane, comprising heating the siloxane film at a temperature lower than the decomposition temperature of the polydiphenylsiloxane to cause ring-opening polymerization of the cyclic diphenylsiloxane.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9331129A JP3069654B2 (en) | 1997-11-14 | 1997-11-14 | Method of forming polydiphenylsiloxane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9331129A JP3069654B2 (en) | 1997-11-14 | 1997-11-14 | Method of forming polydiphenylsiloxane |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH11147956A JPH11147956A (en) | 1999-06-02 |
| JP3069654B2 true JP3069654B2 (en) | 2000-07-24 |
Family
ID=18240200
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP9331129A Expired - Lifetime JP3069654B2 (en) | 1997-11-14 | 1997-11-14 | Method of forming polydiphenylsiloxane |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3069654B2 (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE10010461A1 (en) | 2000-03-03 | 2001-09-13 | Infineon Technologies Ag | Process for packing electronic components comprises injection molding components into ceramic substrate having conducting pathways, contact connection surfaces and pressure contacts |
| CA2488091A1 (en) * | 2002-06-05 | 2003-12-18 | Nobuo Kushibiki | Polysiloxane film and process for producing the same |
| JP6491493B2 (en) * | 2015-02-16 | 2019-03-27 | 公益財団法人相模中央化学研究所 | Method for producing linear trisiloxane compound |
-
1997
- 1997-11-14 JP JP9331129A patent/JP3069654B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH11147956A (en) | 1999-06-02 |
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