JPH0726023A - Production of thin organic polymer film - Google Patents
Production of thin organic polymer filmInfo
- Publication number
- JPH0726023A JPH0726023A JP5197865A JP19786593A JPH0726023A JP H0726023 A JPH0726023 A JP H0726023A JP 5197865 A JP5197865 A JP 5197865A JP 19786593 A JP19786593 A JP 19786593A JP H0726023 A JPH0726023 A JP H0726023A
- Authority
- JP
- Japan
- Prior art keywords
- film
- substrate
- carrier gas
- thin film
- raw material
- 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.)
- Pending
Links
Landscapes
- Polyurethanes Or Polyureas (AREA)
- Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
- Other Resins Obtained By Reactions Not Involving Carbon-To-Carbon Unsaturated Bonds (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、表面保護膜、非線形光
学膜、液晶配向膜、分離膜等に用いられる有機高分子薄
膜の作製方法に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing an organic polymer thin film used for a surface protective film, a non-linear optical film, a liquid crystal alignment film, a separation film and the like.
【０００２】[0002]
【従来の技術】従来、この種の有機高分子薄膜の作製方
法としては、高分子材料の原料モノマーを適当な溶媒に
溶かしてこれを基板上に滴下し重合させて、高分子薄膜
を得る所謂湿式法や、高分子材料そのものを真空容器中
で加熱し、基板上に蒸着する蒸着法や、プラズマ中に有
機モノマーを入れプラズマ重合により、基板上に高分子
薄膜を得るプラズマ重合法などが知られている。しか
し、前記湿式法の場合は、極めて薄い膜が得られ難く、
また、基板に対する皮膜の密着性が不十分で、しかも溶
媒を用いるため添加、除去、回収等の工程が入るために
不純物の混入を避けることが困難であるという欠点があ
る。また、蒸着法は、高分子材料が熱分解を起こし、得
られる高分子の分子量が小さくなるという欠点がある。
また、プラズマ重合法の場合には、モノマーが一旦分解
したりして分子設計が困難で、しかも架橋構造を含むた
め、比較的に剛直な皮膜しか得られないといった欠点が
あった。2. Description of the Related Art Conventionally, as a method for producing such an organic polymer thin film, a so-called polymer thin film is obtained by dissolving a raw material monomer of a polymer material in an appropriate solvent and dropping it on a substrate for polymerization. Wet method, vapor deposition method of heating polymer material itself in a vacuum container and depositing it on the substrate, plasma polymerization method of obtaining a polymer thin film on the substrate by plasma polymerization by putting organic monomer in plasma are known. Has been. However, in the case of the wet method, it is difficult to obtain an extremely thin film,
Further, there is a drawback that it is difficult to avoid mixing of impurities because the adhesion of the film to the substrate is insufficient, and since a solvent is used, steps such as addition, removal and recovery are required. In addition, the vapor deposition method has a drawback that the polymer material undergoes thermal decomposition, and the molecular weight of the obtained polymer becomes small.
Further, in the case of the plasma polymerization method, there is a drawback in that the monomer is once decomposed so that the molecular design is difficult, and since the monomer contains a crosslinked structure, only a relatively rigid film can be obtained.
【０００３】ところで、例えば、特開昭６１−７８４６
３号、特開昭６３−６２８６９号、特開平１−２３８９
８５号、特開平２−６６７１９号等の公報に開示されて
いるように、最近、所謂、蒸着重合に関する技術開発が
されつつある。即ち、図２は従来の蒸着重合により高分
子皮膜を形成するための装置の一例断面図で、図中、Ａ
は処理室で、該処理室内を外部の真空ポンプその他の真
空排気系Ｂに接続すると共に、前記処理室Ａ内に基板Ｃ
が基板ホルダーＤによって下向きに保持され、前記基板
Ｃは、前記基板ホルダーＤの背面に設けたヒーターＥに
よって所定の温度に加熱できるようにされている。処理
室Ａ内下位には、前記基板Ｃに対向させて原料モノマー
７ａ、７ｂを蒸発させるためのガラス製の蒸発用管Ｆが
配置され、該蒸発用管Ｆは、その周囲に巻回されたヒー
ターＥによって所定の温度に加熱できるようにされてい
る。また、図中Ｈは、ヒーターＥの電源、Ｇは基板Ｃと
前記蒸発用管Ｆとの間に介在されるシャッターである。By the way, for example, Japanese Patent Laid-Open No. 61-7846.
3, JP-A-63-62869, JP-A-1-2389.
As disclosed in Japanese Patent Laid-Open No. 85-66719 and Japanese Patent Application Laid-Open No. 2-66719, technical development on so-called vapor deposition polymerization has recently been underway. That is, FIG. 2 is a cross-sectional view of an example of a conventional apparatus for forming a polymer film by vapor deposition polymerization.
Is a processing chamber, the processing chamber is connected to an external vacuum pump or other vacuum exhaust system B, and the substrate C is placed in the processing chamber A.
Are held downward by the substrate holder D, and the substrate C can be heated to a predetermined temperature by the heater E provided on the back surface of the substrate holder D. A glass evaporation tube F for evaporating the raw material monomers 7a and 7b is arranged in the lower part of the processing chamber A so as to face the substrate C, and the evaporation tube F is wound around it. The heater E can be heated to a predetermined temperature. Further, in the figure, H is a power source of the heater E, and G is a shutter interposed between the substrate C and the evaporation tube F.
【０００４】このような装置を用いての有機高分子薄膜
の作製は、まず、一種類あるいは数種類の重合性モノマ
ーを、それぞれの蒸発源より処理室Ａ中の基板Ｃ上に蒸
着させ、その後、必要に応じて、形成した蒸着膜に熱ま
たは紫外線等のエネルギーを加えることにより重合反応
を起こさせて、基板Ｃ上にポリマーの薄膜を形成すると
いうものであり、例えば、ポリイミド薄膜を作製する場
合、原料であるピロメリット酸二無水物（ＰＭＤＡ）と
４，４, −ジアミノジフェニルエーテル（ＯＤＡ）とを
蒸着し、基板上にポリイミド薄膜を形成するといったも
のである。この蒸着重合法によれば、緻密で高純度、か
つ均一な膜厚の有機高分子薄膜を基板に対して良好な密
着性をもって所望厚さに形成でき、更に原料モノマーの
選択によって種々に分子設計された有機高分子薄膜の形
成が行えるものである。In the production of an organic polymer thin film using such an apparatus, first, one or several kinds of polymerizable monomers are vapor-deposited from the respective evaporation sources on the substrate C in the processing chamber A, and thereafter, If necessary, energy such as heat or ultraviolet rays is applied to the formed vapor deposition film to cause a polymerization reaction to form a polymer thin film on the substrate C. For example, when a polyimide thin film is produced. The raw materials pyromellitic dianhydride (PMDA) and 4,4 , -diaminodiphenyl ether (ODA) are vapor-deposited to form a polyimide thin film on the substrate. According to this vapor deposition polymerization method, it is possible to form a dense, high-purity, uniform-thickness organic polymer thin film to a desired thickness with good adhesion to the substrate. Furthermore, various molecular designs can be made by selecting raw material monomers. The formed organic polymer thin film can be formed.
【０００５】[0005]
【発明が解決しようとする課題】しかし、前記公報記載
の方法では、処理室中の蒸発源では比較的蒸気圧の低い
固体モノマーしか用いることができず、蒸発量を制御す
ることも困難であり、また、処理室外の蒸発源では、蒸
気圧の高い固体モノマーや液体モノマーを用いることが
できるが、その蒸発量の制御はかなり困難であるという
問題があった。However, in the method described in the above publication, only the solid monomer having a relatively low vapor pressure can be used in the evaporation source in the processing chamber, and it is difficult to control the evaporation amount. Also, in the evaporation source outside the processing chamber, a solid monomer or a liquid monomer having a high vapor pressure can be used, but there is a problem that it is quite difficult to control the evaporation amount.
【０００６】[0006]
【課題を解決するための手段】本発明は、上記の如き蒸
着重合法にみられた問題点に着目し、鋭意研究した結
果、重合性原料モノマーが固体の場合、液体の場合を問
わず、その蒸発量を精度良く制御でき、より純度の高い
有機高分子薄膜を得ることができる方法を確立したもの
である。即ち、本発明の有機高分子薄膜の作製方法は、
２種以上の重合性原料モノマーを真空容器中に導入し、
前記真空容器中の基体上で蒸着重合させて有機高分子薄
膜を作製する方法において、一定温度に保って密閉容器
に収容された前記重合性原料モノマーのそれぞれの中
を、一定流量のキャリアガスを通過させた後、それぞれ
の重合性原料モノマーガスを含有したキャリアガスを真
空容器中に導入することを特徴とするものである。Means for Solving the Problems The present invention focused on the problems found in the vapor deposition polymerization method as described above, and as a result of earnest research, as a result, regardless of whether the polymerizable raw material monomer is a solid or a liquid, The inventors have established a method capable of controlling the amount of evaporation with high precision and obtaining a highly pure organic polymer thin film. That is, the method for producing an organic polymer thin film of the present invention is
Introducing two or more polymerizable raw material monomers into a vacuum container,
In the method for producing an organic polymer thin film by vapor deposition polymerization on a substrate in the vacuum container, each of the polymerizable raw material monomers stored in a closed container while maintaining a constant temperature is charged with a constant flow rate of a carrier gas. After passing through, the carrier gas containing each polymerizable raw material monomer gas is introduced into the vacuum container.
【０００７】本発明において用いる有機高分子の重合性
原料モノマーとしては、加熱することにより重合してポ
リイミド、ポリアミド、ポリアミドイミド、ポリエステ
ル、ポリウレタン、ポリ尿素、ポリアゾメチンなどを生
成する種々の原料化合物、例えばジアミン化合物、二塩
基酸化合物、ジオール、ビスフェノール、またはグリコ
ール化合物、ジイソシアネート化合物などが好ましく使
用できる。例えば、ジアミン化合物としては、フェニレ
ンジアミン、フェニレンテトラミン、４，４, −ジアミ
ノジフェニルエーテル、４，４, −ジアミノジフェニル
メタンなどが好ましく使用できる。二塩基酸化合物とし
ては、ピロメリット酸、トリメリット酸、ベンゾフェノ
ンテトラカルボン酸、テレフタル酸、イソフタル酸およ
びこれらの酸無水物、酸塩化物などが好ましく使用でき
る。ジオール、ビスフェノール、またはグルコール化合
物としては、ビスフェノール、ビスフェノールジアセテ
ート、キシリレングリコール、シクロヘキサンジメタノ
ールなどを、また、ジイソシアネート化合物としては、
フェニレンジイソシアネート、ビフェニレンジイソシア
ネート、４，４, −ジフェニルメタンジイソシアネート
などが好ましく用いられる。本発明にて用いられるキャ
リアガスとしては、ヘリウム、ネオン、アルゴン、窒素
などの不活性ガスが、少なくとも１種類以上にて通常用
いられる。As the polymerizable raw material monomer of the organic polymer used in the present invention, various raw material compounds which are polymerized by heating to produce polyimide, polyamide, polyamideimide, polyester, polyurethane, polyurea, polyazomethine, etc., For example, diamine compounds, dibasic acid compounds, diols, bisphenols, glycol compounds and diisocyanate compounds can be preferably used. For example, as the diamine compound, phenylenediamine, phenylenetetramine, 4,4 , -diaminodiphenyl ether, 4,4 , -diaminodiphenylmethane and the like can be preferably used. As the dibasic acid compound, pyromellitic acid, trimellitic acid, benzophenonetetracarboxylic acid, terephthalic acid, isophthalic acid and acid anhydrides and acid chlorides thereof can be preferably used. As the diol, bisphenol, or glycol compound, bisphenol, bisphenol diacetate, xylylene glycol, cyclohexanedimethanol, etc., and as the diisocyanate compound,
Phenylene diisocyanate, biphenylene diisocyanate, 4,4 , -diphenylmethane diisocyanate and the like are preferably used. As the carrier gas used in the present invention, at least one kind of inert gas such as helium, neon, argon and nitrogen is usually used.
【０００８】以下、本発明方法を図を用いて説明する。
図１は、本発明の有機高分子薄膜の作製方法を説明する
ための一実施例装置の概略図で、図中１は真空容器、２
は有機高分子薄膜を形成せしめる基板、３は基板２を保
持すると共に基板２を所望温度に加熱できるヒーター１
２を備えた基板ホルダー、４は基板ホルダー３内のヒー
ター１２の温度調節器を備えた電源、５は真空容器１を
真空引きするための真空ポンプ、６は真空容器１内の真
空度を測定するための真空計、７ａ、７ｂは有機高分子
薄膜を形成するための重合性原料モノマー、８は重合性
原料モノマー７ａ、７ｂを加熱するための密閉された容
器、９はキャリアガス源、１０はキャリアガスの流量を
制御するための流量計、１１は重合性原料モノマー７
ａ、７ｂを真空容器１内に導くためのノズル、１６は密
閉された容器８および、ノズル１１を加熱するための温
度調節器付き電源（図示せず）を備えたヒーター、１３
は容器８とノズル１１との間に接続された流量を調節す
ることのできるバルブ、１４は基板２とノズル１１との
間に介在するシャッター、１５は作製された蒸着重合膜
の膜厚、蒸着レートなどを測定するための膜厚モニター
である。The method of the present invention will be described below with reference to the drawings.
FIG. 1 is a schematic view of an apparatus for one embodiment for explaining the method for producing an organic polymer thin film of the present invention, in which 1 is a vacuum container and 2
Is a substrate on which an organic polymer thin film is formed, 3 is a heater 1 which holds the substrate 2 and can heat the substrate 2 to a desired temperature
Substrate holder with 2; power source with temperature controller for heater 12 in substrate holder 3; 5; vacuum pump for evacuating the vacuum container 1; 6; vacuum degree in the vacuum container 1; A vacuum gauge for heating, 7a and 7b are polymerizable raw material monomers for forming an organic polymer thin film, 8 is a closed container for heating the polymerizable raw material monomers 7a and 7b, and 9 is a carrier gas source. Is a flow meter for controlling the flow rate of the carrier gas, 11 is the polymerizable raw material monomer 7
Nozzles for introducing a and 7b into the vacuum container 1, 16 is a sealed container 8 and a heater equipped with a power source (not shown) with a temperature controller for heating the nozzle 11, 13
Is a valve connected between the container 8 and the nozzle 11 and capable of adjusting the flow rate, 14 is a shutter interposed between the substrate 2 and the nozzle 11, 15 is the thickness of the vapor-deposited polymer film thus prepared, vapor deposition It is a film thickness monitor for measuring the rate.
【０００９】本発明の有機高分子薄膜の作製方法では、
上記のような装置を用いて、まず、真空容器１内を真空
ポンプ５を用いて真空引きし、基板２を基板ホルダー３
によって所望の温度に維持しておく。一方、密閉された
容器８内に重合性原料モノマー７ａ、７ｂをそれぞれ入
れ、重合性原料モノマーが適当な蒸気圧を有するように
ヒーター１２によって加熱しておく。ここで重合性原料
モノマーが固体状のものであるときには加熱することに
より液化させるか、あるいは液化せず昇華するものであ
るときは適当な昇華圧になるような温度に加熱してお
く。その後、流量計１０を介してキャリアガス源９より
キャリアガスをそれぞれ重合性原料モノマー中を通して
流し、このモノマーガスを含有したキャリアガスを密閉
された容器８とノズル１１との間に接続されたバルブ１
３を調節して真空容器１内に化学量論比になるように導
入する。真空容器１内に導入されるガスが安定したとこ
ろで、基板２とノズル１１との間に介在するシャッター
１４を開け、基板２上に蒸着重合により有機高分子薄膜
を作製させる。なお、基板２上に作製される蒸着重合膜
の膜厚は、膜厚モニター１５によって観測し、所望の膜
厚に達したところで前記シャッター１４を閉じて製膜を
終了させるものである。In the method for producing an organic polymer thin film of the present invention,
Using the apparatus as described above, first, the inside of the vacuum container 1 is evacuated using the vacuum pump 5, and the substrate 2 is moved to the substrate holder 3
To maintain the desired temperature. On the other hand, the polymerizable raw material monomers 7a and 7b are placed in the closed container 8 and heated by the heater 12 so that the polymerizable raw material monomers have an appropriate vapor pressure. Here, when the polymerizable raw material monomer is solid, it is liquefied by heating, or when it is sublimated without being liquefied, it is heated to a temperature at which an appropriate sublimation pressure is obtained. Then, a carrier gas is supplied from a carrier gas source 9 through a flow meter 10 through each polymerizable raw material monomer, and a carrier gas containing the monomer gas is connected between a sealed container 8 and a nozzle 11. 1
3 is adjusted and introduced into the vacuum container 1 so as to have a stoichiometric ratio. When the gas introduced into the vacuum container 1 becomes stable, the shutter 14 interposed between the substrate 2 and the nozzle 11 is opened, and an organic polymer thin film is formed on the substrate 2 by vapor deposition polymerization. The film thickness of the vapor-deposited polymerized film formed on the substrate 2 is observed by the film thickness monitor 15, and when the desired film thickness is reached, the shutter 14 is closed to complete the film formation.
【００１０】[0010]
【作用】一定温度に保って密閉容器に収容された重合性
原料モノマーのそれぞれの中に、流量を制御されたキャ
リアガスを通し、この重合性原料モノマーを含有したキ
ャリアガスを真空容器内に導入するので、安定的に重合
性原料モノマーを真空容器中に導入することができる。[Function] A carrier gas whose flow rate is controlled is passed through each of the polymerizable raw material monomers stored in a hermetically sealed container at a constant temperature, and the carrier gas containing the polymerizable raw material monomer is introduced into a vacuum container. Therefore, the polymerizable raw material monomer can be stably introduced into the vacuum container.
【００１１】[0011]
【実施例】以下、本発明の実施例を示す。 （実施例１）図１に示す装置を用いて、原料モノマー７
ａとしてピロメリット酸二無水物（ＰＭＤＡ）、７ｂと
して４，４, −ジアミノジフェニルエーテル（ＯＤＡ）
を用い、キャリアガスとしてアルゴンを用いてポリイミ
ド薄膜を作製した。即ち、真空ポンプ５により真空容器
１内を約１０-3Ｐａに排気し、基板温度を３０℃に設定
し、ＰＭＤＡの入った密閉された容器８を１１０℃、Ｏ
ＤＡの入った密閉された容器８を１００℃に加熱し、両
方の容器８に流すキャリアガスの流量を１０ｓｃｃｍと
して、蒸着時間を１時間として製膜を行った。蒸着重合
中の製膜レートは安定していた。蒸着重合終了後、真空
容器１内で基板２を３００℃に加熱し、１時間保持して
イミド化処理を行ってポリイミド薄膜を得た。得られた
ポリイミド薄膜の膜厚は約１μｍであり、均一性が良
く、基板との密着性も良好であった。なお、得られたポ
リイミド薄膜は、ＦＴ−ＩＲにより、モノマーの吸収の
ない純粋なポリイミド薄膜であることが判った。EXAMPLES Examples of the present invention will be shown below. (Example 1) Using the apparatus shown in FIG.
Pyromellitic dianhydride (PMDA) as a and 4,4 , -diaminodiphenyl ether (ODA) as 7b
Was used to prepare a polyimide thin film using argon as a carrier gas. That is, the inside of the vacuum container 1 was evacuated to about 10 −3 Pa by the vacuum pump 5, the substrate temperature was set to 30 ° C., and the sealed container 8 containing PMDA was heated to 110 ° C.
The sealed container 8 containing DA was heated to 100 ° C., the flow rate of the carrier gas flowing in both containers 8 was 10 sccm, and the deposition time was 1 hour to form a film. The film formation rate during vapor deposition polymerization was stable. After completion of the vapor deposition polymerization, the substrate 2 was heated to 300 ° C. in the vacuum container 1 and held for 1 hour to perform imidization treatment to obtain a polyimide thin film. The thickness of the obtained polyimide thin film was about 1 μm, the uniformity was good, and the adhesion to the substrate was good. The obtained polyimide thin film was found by FT-IR to be a pure polyimide thin film having no monomer absorption.
【００１２】（実施例２）図１に示す装置を用いて、原
料モノマー７ａとして４，４, −ジフェニルメタンジイ
ソシアネート、７ｂとして４，４, −ジアミノジフェニ
ルエーテルを用い、キャリアガスとして窒素を用いてポ
リ尿素薄膜を作製した。即ち、真空ポンプ５により真空
容器１内を約１０-3Ｐａに排気し、基板温度を３０℃に
設定し、４，４, −ジフェニルメタンジイソシアネート
の入った密閉された容器８を７０℃、ＯＤＡの入った密
閉された容器８を９０℃にそれぞれ加熱し、両方の容器
８に流すキャリアガスの流量を１０ｓｃｃｍとして、蒸
着時間を１時間として製膜を行った。蒸着重合中の製膜
レートは安定していた。得られたポリ尿素薄膜の膜厚は
約１μｍであり、均一性が良く、基板との密着性も良好
であった。なお、得られたポリ尿素薄膜は、ＦＴ−ＩＲ
により、モノマーの吸収のない純粋なポリ尿素薄膜であ
ることが判った。[0012] Using the apparatus shown in (Example 2) 1, 4,4 as a raw material monomer 7a, - diphenylmethane diisocyanate, 4,4 as 7b, - using diaminodiphenyl ether, polyurea using nitrogen as a carrier gas A thin film was prepared. That is, by the vacuum pump 5 to evacuate the vacuum vessel 1 to about 10 -3 Pa, the substrate temperature is set to 30 ° C., 4, 4, - sealed container 8 70 ° C. containing the diphenylmethane diisocyanate, the ODA Each of the sealed containers 8 contained therein was heated to 90 ° C., the flow rate of the carrier gas flowing in both containers 8 was set to 10 sccm, and the deposition time was set to 1 hour to perform film formation. The film formation rate during vapor deposition polymerization was stable. The thickness of the obtained polyurea thin film was about 1 μm, and the uniformity and the adhesion to the substrate were good. The obtained polyurea thin film was FT-IR.
It was found from the above that it was a pure polyurea thin film with no absorption of monomers.
【００１３】（比較例１）図２に示す装置を用いて、原
料モノマー７ａとしてＰＭＤＡ、７ｂとしてＯＤＡを用
い、ＰＭＤＡの入った蒸着源の温度を１４０℃、ＯＤＡ
の入った蒸着源の温度を１２０℃にそれぞれ加熱し、蒸
着時間を１時間として製膜を行った。蒸着重合中の製膜
レートは時々不安定になることがあった。蒸着重合終了
後、真空容器１内で基板２を３００℃に加熱し、１時間
保持してイミド化処理を行ってポリイミド薄膜を得た。
得られたポリイミド薄膜の膜厚は約１μｍであったが、
膜中に白い粉状のものが混入していた。この白い粉状の
ものを分析したところ、モノマーの１つであるＰＭＤＡ
であることが判った。(Comparative Example 1) Using the apparatus shown in FIG. 2, PMDA was used as the raw material monomer 7a and ODA was used as 7b, the temperature of the vapor deposition source containing PMDA was 140 ° C., and ODA was used.
The temperature of the vapor deposition source containing was heated to 120 ° C., and the vapor deposition time was set to 1 hour to form a film. The film formation rate during vapor deposition polymerization sometimes became unstable. After completion of the vapor deposition polymerization, the substrate 2 was heated to 300 ° C. in the vacuum container 1 and held for 1 hour to perform imidization treatment to obtain a polyimide thin film.
The thickness of the obtained polyimide thin film was about 1 μm,
White powder was mixed in the film. Analysis of this white powder showed that PMDA, which is one of the monomers
Was found.
【００１４】[0014]
【発明の効果】以上、説明した如く、本発明方法によれ
ば、蒸着重合法において、重合性原料モノマーが固体の
場合、液体の場合を問わず、キャリアガスの流量調整に
より重合性原料モノマーの蒸発量を精度良く制御できる
ことから、より純度の高い有機高分子薄膜を作製できる
ものである。As described above, according to the method of the present invention, in the vapor deposition polymerization method, regardless of whether the polymerizable raw material monomer is solid or liquid, the flow rate of the carrier gas can be adjusted to adjust the amount of the polymerizable raw material monomer. Since the amount of evaporation can be controlled with high precision, a higher purity organic polymer thin film can be produced.
【図１】本発明方法を実施するための一実施例装置の概
略図である。FIG. 1 is a schematic view of an embodiment of an apparatus for carrying out the method of the present invention.
【図２】従来の方法を実施するための一実施例装置の概
略図である。FIG. 2 is a schematic diagram of an example apparatus for performing a conventional method.
１ 真空容器 ２ 基板 ３ 基板ホルダー ４ 温度調節器を備えた電源 ５ 真空ポンプ ６ 真空計 ７ａ 重合性原料モノマー ７ｂ 重合性原料モノマー ８ 密閉された容器 ９ キャリアガス源 １０ 流量計 １１ ノズル １２ ヒーター １３ バルブ １４ シャッター １５ 膜厚モニター １６ ヒーター Ａ 処理室 Ｂ 真空排気系 Ｃ 基板 Ｄ 基板ホルダー Ｅ ヒーター Ｆ 蒸発用管 Ｇ シャッター Ｈ ヒーターの電源 1 Vacuum Container 2 Substrate 3 Substrate Holder 4 Power Supply with Temperature Controller 5 Vacuum Pump 6 Vacuum Gauge 7a Polymerizable Raw Material Monomer 7b Polymerizable Raw Material Monomer 8 Sealed Container 9 Carrier Gas Source 10 Flowmeter 11 Nozzle 12 Heater 13 Valve 14 Shutter 15 Film thickness monitor 16 Heater A Processing chamber B Vacuum exhaust system C Substrate D Substrate holder E Heater F Evaporation tube G Shutter H Heater power supply
Claims (1)
器中に導入し、前記真空容器中の基体上で蒸着重合させ
て有機高分子薄膜を作製する方法において、一定温度に
保って密閉容器に収容された前記重合性原料モノマーの
それぞれの中を、一定流量のキャリアガスを通過させた
後、それぞれの重合性原料モノマーガスを含有したキャ
リアガスを真空容器中に導入することを特徴とする有機
高分子薄膜の作製方法。1. A method for producing an organic polymer thin film by introducing two or more kinds of polymerizable raw material monomers into a vacuum container and vapor-depositing and polymerizing the monomers on a substrate in the vacuum container, which is kept closed at a constant temperature. In each of the polymerizable raw material monomer contained in, after passing a constant flow rate of the carrier gas, carrier gas containing the respective polymerizable raw material monomer gas is introduced into the vacuum container Method for producing organic polymer thin film.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5197865A JPH0726023A (en) | 1993-07-14 | 1993-07-14 | Production of thin organic polymer film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5197865A JPH0726023A (en) | 1993-07-14 | 1993-07-14 | Production of thin organic polymer film |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0726023A true JPH0726023A (en) | 1995-01-27 |
Family
ID=16381624
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP5197865A Pending JPH0726023A (en) | 1993-07-14 | 1993-07-14 | Production of thin organic polymer film |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0726023A (en) |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2001023077A1 (en) * | 1999-09-28 | 2001-04-05 | Toray Industries, Inc. | Process for producing composite semipermeable membrane |
| EP1167040A1 (en) * | 2000-06-26 | 2002-01-02 | Toshiba Tec Kabushiki Kaisha | Ink jet printer head and method for manufacturing the same |
| WO2007111098A1 (en) | 2006-03-24 | 2007-10-04 | Konica Minolta Medical & Graphic, Inc. | Transparent barrier sheet and method for producing same |
| WO2007111074A1 (en) | 2006-03-24 | 2007-10-04 | Konica Minolta Medical & Graphic, Inc. | Transparent barrier sheet and method for producing transparent barrier sheet |
| WO2007111092A1 (en) | 2006-03-24 | 2007-10-04 | Konica Minolta Medical & Graphic, Inc. | Transparent barrier sheet and method for producing transparent barrier sheet |
| WO2007111075A1 (en) | 2006-03-24 | 2007-10-04 | Konica Minolta Medical & Graphic, Inc. | Transparent barrier sheet and method for producing transparent barrier sheet |
| WO2007111076A1 (en) | 2006-03-24 | 2007-10-04 | Konica Minolta Medical & Graphic, Inc. | Transparent barrier sheet and method for producing transparent barrier sheet |
| EP2322688A1 (en) | 2009-10-15 | 2011-05-18 | Kojima Press Industry Co., Ltd. | Method of forming organic polymer thin film and an appartus for forming the organic polymer thin film |
| JP2019183115A (en) * | 2018-03-30 | 2019-10-24 | 株式会社カネカ | Polyamic acid manufacturing system and manufacturing method, and polyimide manufacturing system and manufacturing method |
-
1993
- 1993-07-14 JP JP5197865A patent/JPH0726023A/en active Pending
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2001023077A1 (en) * | 1999-09-28 | 2001-04-05 | Toray Industries, Inc. | Process for producing composite semipermeable membrane |
| US6521130B1 (en) * | 1999-09-28 | 2003-02-18 | Toray Industries, Inc. | Process for producing composite semipermeable membrane |
| EP1167040A1 (en) * | 2000-06-26 | 2002-01-02 | Toshiba Tec Kabushiki Kaisha | Ink jet printer head and method for manufacturing the same |
| US6547374B2 (en) | 2000-06-26 | 2003-04-15 | Toshiba Tec Kabushiki Kaisha | Ink jet printer head and method for manufacturing the same |
| WO2007111098A1 (en) | 2006-03-24 | 2007-10-04 | Konica Minolta Medical & Graphic, Inc. | Transparent barrier sheet and method for producing same |
| WO2007111074A1 (en) | 2006-03-24 | 2007-10-04 | Konica Minolta Medical & Graphic, Inc. | Transparent barrier sheet and method for producing transparent barrier sheet |
| WO2007111092A1 (en) | 2006-03-24 | 2007-10-04 | Konica Minolta Medical & Graphic, Inc. | Transparent barrier sheet and method for producing transparent barrier sheet |
| WO2007111075A1 (en) | 2006-03-24 | 2007-10-04 | Konica Minolta Medical & Graphic, Inc. | Transparent barrier sheet and method for producing transparent barrier sheet |
| WO2007111076A1 (en) | 2006-03-24 | 2007-10-04 | Konica Minolta Medical & Graphic, Inc. | Transparent barrier sheet and method for producing transparent barrier sheet |
| EP2322688A1 (en) | 2009-10-15 | 2011-05-18 | Kojima Press Industry Co., Ltd. | Method of forming organic polymer thin film and an appartus for forming the organic polymer thin film |
| US9290837B2 (en) | 2009-10-15 | 2016-03-22 | Kojima Press Industry Co., Ltd. | Method of forming organic polymer thin film and an apparatus for forming the organic polymer thin film |
| JP2019183115A (en) * | 2018-03-30 | 2019-10-24 | 株式会社カネカ | Polyamic acid manufacturing system and manufacturing method, and polyimide manufacturing system and manufacturing method |
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