JPH07331420A - Vacuum deposition method and device therefor - Google Patents
Vacuum deposition method and device thereforInfo
- Publication number
- JPH07331420A JPH07331420A JP12231694A JP12231694A JPH07331420A JP H07331420 A JPH07331420 A JP H07331420A JP 12231694 A JP12231694 A JP 12231694A JP 12231694 A JP12231694 A JP 12231694A JP H07331420 A JPH07331420 A JP H07331420A
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- Japan
- Prior art keywords
- evaporation
- raw material
- vacuum
- temperature
- vapor deposition
- Prior art date
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- Physical Vapour Deposition (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、食品包装，医薬品包
装，電子機器部品包装，たばこ包装，写真製版，感光性
写真材料などの分野に利用可能な各種機能を有したフレ
キシブルプラスチックフィルムの真空蒸着加工に好適に
用いられる真空蒸着方法および真空蒸着装置に関する。FIELD OF THE INVENTION The present invention relates to a vacuum deposition of a flexible plastic film having various functions, which can be used in the fields of food packaging, pharmaceutical packaging, electronic device component packaging, tobacco packaging, photoengraving, photosensitive photographic materials and the like. TECHNICAL FIELD The present invention relates to a vacuum vapor deposition method and a vacuum vapor deposition apparatus suitably used for processing.
【０００２】[0002]
【従来の技術】近年、真空蒸着法によりフレキシブルプ
ラスチックフィルムの表面に金属または金属酸化物をコ
ーティングし、装飾性、ガスバリヤ性、耐薬品性、濡れ
特性、磁気特性、電導性、寸法安定性などの機能性を付
与し、食品包装，医薬品包装，電子機器部品包装，たば
こ包装，写真製版及び感光性写真材料などの分野に利用
されるようになった。特にアルミニウム蒸着フィルム
は、装飾、包装用途に広くに利用されるようになってい
る。また、最近では環境汚染の少ない透明ハイバリヤー
素材として珪素酸化物蒸着フィルムの研究開発も盛んに
行われ広く、普及することも期待されるなど金属酸化物
の蒸着技術の開発に対する要求も日増しに強くなってい
る。2. Description of the Related Art In recent years, the surface of a flexible plastic film is coated with a metal or a metal oxide by a vacuum vapor deposition method to improve decorative properties, gas barrier properties, chemical resistance, wetting properties, magnetic properties, electrical conductivity, dimensional stability, etc. With added functionality, it has come to be used in fields such as food packaging, pharmaceutical packaging, electronic device component packaging, tobacco packaging, photoengraving and photosensitive photographic materials. In particular, aluminum vapor-deposited films have come to be widely used for decoration and packaging. Recently, silicon oxide vapor deposition film has been actively researched and developed as a transparent high barrier material with little environmental pollution, and it is expected that it will be widely spread, and demand for the development of metal oxide vapor deposition technology will increase day by day. It's getting stronger.
【０００３】これらの用途の広がりに対応し、大量生産
および加工コストの低減が必要となった。そのため、蒸
発温度を高温にして加工速度を高速化することによる加
工時間の短縮、装着するフィルム幅を広くすることによ
る１回の加工工程で生産可能な面積の拡大、加工長の延
長などが実用化され、結果として蒸着機が大型化してき
た。加工長を延長するためには、蒸発原料を１回に大量
に仕込めるように蒸発原料るつぼの大型化をはかった
り、真空槽内に蒸発原料の保存スペースを設けてそれを
連続供給できるよう工夫されてきた。アルミニウムのよ
うな溶融性蒸発原料を連続供給する場合には、図４に示
すように抵抗加熱方式により蒸発原料が蒸発する温度以
上に加熱されたボート状の蒸発源（蒸発原料を蒸発させ
る加熱部）にワイヤー状に加工された蒸発原料を連続供
給する方法が欧米では広く普及している。また、珪素酸
化物のような昇華性蒸発原料を使用する場合には、図５
に示すように電子線加熱方式により昇華温度以上に加熱
された蒸発原料をゆっくりと移動させることにより連続
供給する方法や、図６に示すような装置（特開平１−２
５２７６８号、特開平２−２７７７７４号に開示）を用
い蒸発原料を連続供給する方法がとられてきた。In response to the spread of these applications, it has become necessary to reduce mass production and processing costs. Therefore, it is practical to reduce the processing time by increasing the evaporation temperature to increase the processing speed, widen the width of the film to be mounted to increase the area that can be produced in one processing step, and extend the processing length. As a result, vapor deposition machines have become larger. In order to extend the processing length, the evaporation material crucible must be enlarged so that a large amount of evaporation material can be charged at one time, or a storage space for evaporation material can be provided in the vacuum chamber so that it can be continuously supplied. It has been. In the case of continuously supplying a meltable evaporation material such as aluminum, as shown in FIG. 4, a boat-shaped evaporation source (heating unit for evaporating the evaporation material is heated by a resistance heating method to a temperature at which the evaporation material is evaporated or more). The method of continuously supplying the evaporation raw material processed into a wire is widely used in Europe and America. Further, when a sublimable evaporation material such as silicon oxide is used, as shown in FIG.
As shown in FIG. 6, a method for continuously supplying an evaporating raw material heated to a sublimation temperature or higher by an electron beam heating method to continuously supply it, or an apparatus as shown in FIG.
No. 52768, disclosed in JP-A-2-277774), a method of continuously supplying an evaporation raw material has been adopted.
【０００４】しかしながら、どの方法も蒸発原料を予め
加熱することなく蒸発源（蒸発原料を蒸発させる加熱
部）である原料加熱ヒーターに供給しているため、蒸発
原料は室温に近い温度から蒸発温度まで急激に加熱され
る。そのため蒸発原料の加熱が不十分となり、十分な蒸
発速度（蒸着加工速度）を得ることが難しい。蒸発原料
が複合組成物の場合はその組成物自体が破損したりす
る。また、不足した蒸発速度を補うため蒸発源のヒータ
ーや電子線に投入するパワーを大きくすると、蒸発原料
の温度分布に大きな偏差が生じる。この結果、アルミニ
ウムのような溶融性原料の場合、突沸によるスプラッシ
ュ（蒸発飛沫）の発生を招く。このスプラッシュは、蒸
着フィルムに到達し蒸着膜の欠陥、基材フィルムの損
傷、異物の混入現象等のトラブルの原因となる問題点が
あった。また、珪素酸化物のような昇華性原料の複合組
成物（特に粉体成形物）の場合、やはりスプラッシュの
発生や急激なガス放出（粉体成形原料の場合または低蒸
発温度の不純物を含む場合）、さらには蒸発原料である
複合組成物（特に成形原料）が割れ、真空槽内圧力の上
昇，不純物の混入や蒸発速度の変動を招いていた。However, in any of the methods, the evaporation raw material is supplied to the raw material heater which is the evaporation source (heating part for evaporating the evaporation raw material) without preheating it, so that the evaporation raw material is heated from a temperature close to room temperature to an evaporation temperature. It is heated rapidly. Therefore, heating of the evaporation raw material becomes insufficient, and it is difficult to obtain a sufficient evaporation rate (vapor deposition processing rate). When the evaporation raw material is a composite composition, the composition itself may be damaged. Further, if the power supplied to the heater of the evaporation source or the electron beam is increased in order to compensate for the insufficient evaporation rate, a large deviation will occur in the temperature distribution of the evaporation raw material. As a result, in the case of a fusible raw material such as aluminum, splash (evaporative splash) is caused by bumping. This splash has a problem that it reaches the vapor deposition film and causes troubles such as defects of the vapor deposition film, damage of the base film, and a phenomenon of mixing of foreign matter. Moreover, in the case of a composite composition of sublimable raw materials such as silicon oxide (particularly powder molding), the occurrence of splash and rapid gas release (in the case of powder molding raw materials or when impurities of low evaporation temperature are included) ), And further, the composite composition (particularly the forming raw material) which is the evaporation raw material is cracked, which causes rise in the pressure in the vacuum chamber, mixing of impurities and fluctuations in the evaporation rate.
【０００５】その結果として、真空槽内圧力が上昇する
と、珪素酸化物蒸着フィルムの品質は低下し、蒸発速度
（結果として蒸着加工速度）も低下する。また、スプラ
ッシュの発生は、前述のように蒸着膜の欠陥、基材フィ
ルムの損傷や異物の混入現象としてトラブルの原因とな
り、蒸発原料である複合組成物の割れは、連続供給蒸着
用ヒーターの中で「詰まり」現象を発生し、蒸発原料の
連続供給による長時間蒸着加工の妨げとなる。蒸発速度
の変動は、複数並ぶ蒸発源の加熱ヒーター毎に不規則に
生じるため、蒸着膜厚等の制御を不安定にし、結果とし
て蒸着フィルムの品質が低下する。前述のように、従来
の蒸発原料を連続供給可能な蒸着方式には、生産性と蒸
着フィルムの品質の両立が難しいという問題点があっ
た。As a result, when the pressure in the vacuum chamber rises, the quality of the silicon oxide vapor deposition film deteriorates, and the evaporation rate (as a result, the vapor deposition processing rate) also decreases. Further, the occurrence of splash causes troubles such as defects in the vapor deposition film, damage to the base film and the phenomenon of mixing of foreign matter as described above, and cracking of the composite composition, which is the evaporation raw material, occurs in the heater for continuous supply vapor deposition. In this case, a "clogging" phenomenon occurs, which hinders long-time vapor deposition processing due to continuous supply of evaporation raw materials. Fluctuations in the evaporation rate occur irregularly for each heater of the evaporation sources arranged in a line, which makes control of the vapor deposition film thickness and the like unstable, resulting in deterioration of the quality of the vapor deposition film. As described above, the conventional vapor deposition method capable of continuously supplying the evaporation raw material has a problem that it is difficult to achieve both productivity and vapor deposition film quality.
【０００６】[0006]
【発明が解決しようとする課題】本発明は、大量生産を
実現するために蒸発原料を連続供給する真空蒸着方法に
おいて、高い蒸発速度（結果として蒸着加工速度）と安
定した品質の両立を実現する真空蒸着方法を提供するこ
とにある。DISCLOSURE OF THE INVENTION The present invention realizes both high evaporation rate (as a result, evaporation processing rate) and stable quality in a vacuum evaporation method for continuously supplying evaporation raw materials for realizing mass production. It is to provide a vacuum deposition method.
【０００７】[0007]
【課題を解決するための手段】本発明の目的は、蒸発原
料を実質的に連続供給する真空蒸着方法において、蒸発
原料を蒸発させる前に予め加熱することを特徴とする真
空蒸着方法によって達成することができる。本発明の目
的は更に、蒸発原料を実質的に連続供給する真空蒸着装
置において、蒸発原料を蒸発させる前に予め加熱する予
備加熱部を有することを特徴とする真空蒸着装置によっ
て達成することができる。The object of the present invention is achieved by a vacuum vapor deposition method in which an evaporation raw material is substantially continuously supplied, in which the evaporation raw material is preheated before being vaporized. be able to. The object of the present invention can be further achieved by a vacuum vapor deposition apparatus, which is a vacuum vapor deposition apparatus for substantially continuously supplying an evaporation raw material, having a preheating unit for preheating the evaporation raw material before vaporizing. .
【０００８】本発明において、蒸発原料を実質的に連続
供給する真空蒸着装置としては、図４に示すように抵抗
加熱方式により蒸発原料が蒸発する温度以上に加熱され
たボート状の蒸発源にワイヤー状に加工された蒸発原料
を連続供給する装置，図５に示すように電子線加熱方式
により昇華温度以上に加熱された蒸発原料をゆっくりと
移動させることにより連続供給する装置や、図６に示す
ような特開平１−２５２７６８号や特開平２−２７７７
７４号公報に記載された装置が挙げられる。本発明にお
いて、連続供給される蒸発原料を予備加熱部で予め加熱
する方法としては、真空状態で使用でき、且つ蒸発原料
を所定の時間内に所定の温度に昇温可能な方法で有れば
特に制限は無く、直接抵抗加熱、間接抵抗加熱、直接高
周波誘導加熱、間接高周波誘導加熱、輻射加熱、電子線
加熱など従来公知の方法を用いることができる。In the present invention, as a vacuum vapor deposition apparatus for substantially continuously supplying an evaporation raw material, as shown in FIG. 4, a wire is applied to a boat-shaped evaporation source heated by a resistance heating method to a temperature at which the evaporation raw material is evaporated or higher. Device for continuously feeding the vaporized raw material processed into a shape, a device for continuously feeding the vaporized raw material heated above the sublimation temperature by an electron beam heating system as shown in FIG. As described in JP-A-1-252768 and JP-A-2-2777.
The device described in Japanese Patent Publication No. 74 is cited. In the present invention, as a method of preliminarily heating the continuously supplied evaporation raw material in the preheating unit, if the method can be used in a vacuum state and the evaporation raw material can be heated to a predetermined temperature within a predetermined time There is no particular limitation, and conventionally known methods such as direct resistance heating, indirect resistance heating, direct high frequency induction heating, indirect high frequency induction heating, radiation heating, and electron beam heating can be used.
【０００９】予備加熱部については直接的に温度制御し
ても良いが、特にしなくても良い。予備加熱部を直接的
に温度制御する場合、その制御方法はＰＩＤ制御、比例
制御、ファジィー制御などの方法が挙げられる。そのた
めの温度計測方法も熱電対温度計、放射温度計などの従
来公知の温度計を用いた方法が使用できる。図２に、直
接抵抗加熱の蒸発源（蒸発原料を蒸発させる加熱部）と
直接抵抗加熱の予備加熱部を放射温度計でＰＩＤ制御し
たシステムの模式図を示す。また、図３に、直接抵抗加
熱の蒸発源（蒸発原料を蒸発させる加熱部）と高周波誘
導加熱の予備加熱部を放射温度計でＰＩＤ制御したシス
テムの模式図を示す。予備加熱部を直接的に温度制御し
ない場合は、図１に示すように、蒸発源（蒸発原料を蒸
発させる加熱部）と予備加熱部を一体化する方法が挙げ
られる。蒸発源と予備加熱部を一体化する方法は、装置
を簡便かつ安価にできることから好ましい方法である。
この方法を用いた場合でも、蒸発源の温度は制御される
ため、蒸発源の温度と予備加熱部の温度差を正しく把握
することにより、事実上、予備加熱部の温度制御が実現
する。The temperature of the preheating section may be directly controlled, but it is not necessary to do so. When the temperature of the preheating unit is directly controlled, the control method includes PID control, proportional control, fuzzy control and the like. As a temperature measuring method therefor, a method using a conventionally known thermometer such as a thermocouple thermometer and a radiation thermometer can be used. FIG. 2 shows a schematic diagram of a system in which a direct resistance heating evaporation source (a heating unit for evaporating an evaporation material) and a direct resistance heating preheating unit are PID-controlled by a radiation thermometer. Further, FIG. 3 shows a schematic diagram of a system in which a direct resistance heating evaporation source (a heating unit for evaporating evaporation material) and a preheating unit for high-frequency induction heating are PID-controlled by a radiation thermometer. When the temperature of the preheating unit is not directly controlled, a method of integrating the evaporation source (heating unit for evaporating the evaporation raw material) and the preheating unit as shown in FIG. 1 can be mentioned. The method of integrating the evaporation source and the preheating unit is a preferable method because the apparatus can be simple and inexpensive.
Even when this method is used, the temperature of the evaporation source is controlled. Therefore, the temperature difference between the evaporation source and the temperature of the preheating unit can be grasped correctly, so that the temperature of the preheating unit can be effectively controlled.
【００１０】本発明においては、蒸発原料を円滑にかつ
連続的に供給することは必須条件であり、それを妨げな
いよう蒸発原料を予め加熱しなければならない。つま
り、予備加熱部の温度は、蒸発原料の特性（溶融性／昇
華性），蒸発原料の熱容量，熱伝導度及び蒸発原料の供
給速度等を考慮し、設定するべきである。具体的には、
蒸発原料が溶融性原料の場合、予備加熱部の温度は、原
料の溶融温度より２００℃低い温度以上、溶融温度未満
でなければならない。予備加熱部の温度が蒸発原料の溶
融温度以上の場合、蒸発原料が蒸発源（蒸発原料を蒸発
させる加熱部）に到達する前に、予備加熱部で溶融，液
化してしまい、蒸発源で適正な蒸発ができなくなり、蒸
発原料の供給が事実上円滑に行われなくなる。また、蒸
発原料が珪素酸化物のような熱伝導度の低い昇華性原料
の場合、予備加熱部の温度は、原料の昇華温度より２０
０℃低い温度以上、昇華温度より５０℃高い温度以下で
なければならない。予備加熱部の温度がこの範囲より高
い場合、蒸発原料が蒸発源に到達する前に、予備加熱部
で大量に昇華してしまうため、蒸発原料自体が減量し、
効率の良い蒸発が行われなくなる。In the present invention, it is an essential condition to supply the evaporation raw material smoothly and continuously, and the evaporation raw material must be preheated so as not to disturb it. That is, the temperature of the preheating unit should be set in consideration of the characteristics (meltability / sublimability) of the evaporation material, the heat capacity of the evaporation material, the thermal conductivity, the supply rate of the evaporation material, and the like. In particular,
When the evaporation raw material is a meltable raw material, the temperature of the preheating section must be equal to or higher than the melting temperature of the raw material by 200 ° C. and lower than the melting temperature. If the temperature of the preheating unit is higher than the melting temperature of the evaporation source, the evaporation source will melt and liquefy in the preheating unit before reaching the evaporation source (heating unit that evaporates the evaporation source) As a result, the evaporation material cannot be smoothly supplied. Further, when the evaporation raw material is a sublimable raw material having a low thermal conductivity such as silicon oxide, the temperature of the preheating portion is 20 ° C. lower than the sublimation temperature of the raw material.
It must be above 0 ° C lower and below 50 ° C above sublimation temperature. If the temperature of the preheating unit is higher than this range, the evaporation raw material is sublimated in a large amount before reaching the evaporation source, so the evaporation raw material itself is reduced,
Efficient evaporation will not occur.
【００１１】蒸発原料を予め加熱する予備加熱部の温度
は、蒸発源で蒸発する蒸発速度をできるだけ高くし、本
発明が目的とする課題解決の効果をより大きくするため
には、条件範囲内で可能な限り高い温度であることが好
ましい。予備加熱部の温度は、溶融性原料であるアルミ
ニウムを真空蒸着する場合は、７３３〜９３３℃、さら
には８５０〜９３３℃が好ましい。熱伝導度の低い昇華
性原料である一酸化珪素を１×１０-2Ｐａの圧力下で真
空蒸着する場合は、６７３〜９２３℃、さらには９０３
〜９２３℃が好ましい。また、珪素と熱伝導度の低い二
酸化珪素の混合物を１×１０-2Ｐａの圧力下で真空蒸着
する場合は９２３〜１１７３℃、さらには１１５３〜１
１７３℃が好ましい。蒸発原料として熱伝導度の低い昇
華性原料であるＳｉＯ2 を含む場合、予め加熱する昇温
速度が急激であると、結果としてスプラッシュの発生，
急激なガス放出，蒸発原料の割れ，真空槽内圧力の上
昇，不純物の混入，蒸発速度の変動等を引き起こす。そ
のため、蒸発原料としてＳｉＯ2 を含む場合、蒸発材料
を予備加熱する際の昇温速度は、１００〜３００℃／分
程度が好ましい。The temperature of the preheating section for preheating the evaporation raw material is within the range of conditions in order to increase the evaporation rate of evaporation by the evaporation source as much as possible and to further enhance the effect of solving the problem to be solved by the present invention. It is preferable that the temperature is as high as possible. The temperature of the preheating part is preferably 733 to 933 ° C., and more preferably 850 to 933 ° C. when vacuum-depositing aluminum, which is a meltable raw material. When silicon monoxide, which is a sublimable raw material having low thermal conductivity, is vacuum-deposited under a pressure of 1 × 10 −2 Pa, the temperature is 673 to 923 ° C., and further 903.
〜923 ° C. is preferable. When a mixture of silicon and silicon dioxide having low thermal conductivity is vacuum-deposited under a pressure of 1 × 10 -2 Pa, the temperature is 923 to 1173 ° C., and further 1153 to 1: 1.
173 ° C is preferred. When SiO 2 which is a sublimable raw material having low thermal conductivity is included as the evaporation raw material, if the temperature rising rate for preheating is rapid, as a result, splash occurs,
It causes sudden gas release, cracking of evaporation material, increase of pressure in vacuum chamber, mixing of impurities, fluctuation of evaporation rate, etc. Therefore, when the evaporated raw material containing SiO 2, heating rate at the time of pre-heating the evaporation material is preferably 100 to 300 ° C. / minute degree.
【００１２】蒸発原料としては、連続的に原料を供給す
る真空蒸着装置に使用される原料であれば特に制限はな
く、溶融性原料としては、アルミニウム，銅，銀等の金
属が挙げられる。また、昇華性原料としては、Ｓｉ及び
ＳｉＯ，Ｓｉ3 Ｏ4 ，Ｓｉ2 Ｏ3 ，ＳｉＯ2 を含むＳｉ
Ｏｘ（Ｘ＝１〜２）等の珪素及び珪素酸化物から選ばれ
る１種または２種以上の物質の混合物や、珪素及びまた
は珪素酸化物と金属及びまたは金属化合物との混合物や
化学結合物が挙げられる。この中でＳｉＯ2 等の珪素酸
化物は結晶性でも非晶性でも構わない。金属化合物とし
ては金属酸化物や金属フッ化物が挙げられる。金属酸化
物としては、マグネシウム酸化物，カルシウム酸化物，
バリウム酸化物，アルミニウム酸化物，チタン酸化物，
ジルコニア酸化物，ナトリウム酸化物，カリウム酸化
物，錫酸化物，インジウム酸化物，酸化マグネシウム−
二酸化珪素共酸化物（フォルステライト，ステアタイ
ト），酸化アルミニュウム−二酸化珪素共酸化物（ムラ
イト）等が挙げられる。また金属フッ化物としては、ア
ルカリ土類金属のフッ化物，例えばフッ化マグネシウム
やフッ化カルシウム，フッ化バリウムや、アルカリ金属
のフッ化物，例えばフッ化ナトリウムやフッ化カリウム
等が挙げられる。The evaporation raw material is not particularly limited as long as it is a raw material used in a vacuum vapor deposition apparatus for continuously supplying the raw material, and examples of the fusible raw material include metals such as aluminum, copper and silver. Further, as the sublimable raw material, Si and Si containing SiO, Si 3 O 4 , Si 2 O 3 and SiO 2 are used.
A mixture of one or more substances selected from silicon and silicon oxides such as Ox (X = 1 to 2), a mixture of silicon and / or silicon oxide and a metal and / or a metal compound, and a chemical bond. Can be mentioned. Among them, silicon oxide such as SiO 2 may be crystalline or amorphous. Examples of the metal compound include metal oxides and metal fluorides. Metal oxides include magnesium oxide, calcium oxide,
Barium oxide, aluminum oxide, titanium oxide,
Zirconia oxide, sodium oxide, potassium oxide, tin oxide, indium oxide, magnesium oxide-
Examples thereof include silicon dioxide co-oxide (forsterite, steatite), aluminum oxide-silicon dioxide co-oxide (mullite) and the like. Examples of the metal fluorides include alkaline earth metal fluorides such as magnesium fluoride, calcium fluoride, and barium fluoride, and alkali metal fluorides such as sodium fluoride and potassium fluoride.
【００１３】[0013]
【実施例】以下、実施例に基づいて本発明をさらに詳細
に説明するが、本発明はその要旨をこえない限り、以下
の実施例に限定されるものではない。なお実施例で得ら
れた蒸着フィルムの試験方法は以下のとおりである。 酸素バリヤー性：ＡＳＴＭ Ｄ ３９８５に準拠し、米
国モダンコントロールズ社のＯＸＴＲＡＮ−ＴＷＩＮを
用いて酸素ガス透過率を測定した。 外観：得られた蒸着フィルムの蒸着膜の欠陥，異物混入
について、目視にて評価した。The present invention will be described in more detail based on the following examples, but the invention is not intended to be limited to the following examples without departing from the gist thereof. The test method for the vapor-deposited film obtained in the examples is as follows. Oxygen barrier property: According to ASTM D 3985, the oxygen gas permeability was measured using OXTRAN-TWIN manufactured by Modern Controls, Inc., USA. Appearance: Defects in the deposited film of the obtained deposited film and inclusion of foreign matter were visually evaluated.
【００１４】〔実施例１〕図１に示すように、特開平１
−２５２７６８号公報に記載された真空蒸着装置に、蒸
発源と一体となっている予備加熱部（ちっ化ほう素複合
焼結体製）を設けた。予備加熱部の加熱方法は、蒸発源
の加熱方法と同じ抵抗加熱方式である。なお、予備加熱
部の温度制御は独自に行わず、蒸発源の放射温度計によ
る温度制御に依存する方法をとった。次に、珪素と二酸
化珪素（非晶質）との等モル混合物を圧縮成形し、直径
４０ｍｍ，高さ３５ｍｍの円柱状成形物を得た。得られ
た成形物を、蒸発原料供給機構から５ｍｍ／分間の供給
速度で、蒸発源と一体となっている予備加熱部に連続供
給し、１×１０-2Ｐａの真空下で蒸発源を抵抗加熱によ
り１３５０℃に加熱し、（その時予備加熱部の温度を放
射温度計を用いて測定したところ、１１７０℃であっ
た。）厚さ１２μｍのポリエチレンテレフタレートフィ
ルムに珪素酸化物を真空蒸着した。その条件のまま加工
速度は５０ｍ／分で、１時間真空蒸着加工を行った。な
お、１時間の真空蒸着加工中には、スプラッシュの発生
は認められなかった。蒸着膜の厚みは、水晶式膜厚モニ
ターを用いて測定したところ、約１０００オングストロ
ームであった。[Example 1] As shown in FIG.
The vacuum vapor deposition apparatus described in Japanese Patent Publication No. 252768 has a preheating unit (made of a boron nitride composite sintered body) integrated with an evaporation source. The heating method of the preheating unit is the same resistance heating method as the heating method of the evaporation source. Note that the temperature control of the preheating unit was not performed independently, but the method that relied on the temperature control by the radiation thermometer of the evaporation source was adopted. Next, an equimolar mixture of silicon and silicon dioxide (amorphous) was compression molded to obtain a cylindrical molded product having a diameter of 40 mm and a height of 35 mm. The obtained molded product is continuously supplied to the preheating section integrated with the evaporation source at a supply rate of 5 mm / minute from the evaporation source supply mechanism, and the evaporation source is resisted under a vacuum of 1 × 10 -2 Pa. The film was heated to 1350 ° C. by heating (at that time, the temperature of the preheating part was measured by using a radiation thermometer and found to be 1170 ° C.), and silicon oxide was vacuum-deposited on a polyethylene terephthalate film having a thickness of 12 μm. Under the conditions, the processing speed was 50 m / min, and vacuum deposition processing was performed for 1 hour. No splash was observed during the vacuum deposition process for 1 hour. The thickness of the vapor-deposited film was about 1000 Å when measured using a quartz-type film thickness monitor.
【００１５】〔実施例２〕図３に示すように、特開平１
−２５２７６８号公報に記載される真空蒸着装置に、蒸
発源と別体となっている予備加熱部（グラファイト製）
を設けた。予備加熱部の加熱方法は、高周波誘導加熱方
式である。なお、予備加熱部の温度制御は、蒸発源とは
別に、放射温度計により行った。次に、一酸化珪素と酸
化マグネシウムの混合物（混合比９０モル％：１０モル
％）圧縮成形し、直径４０ｍｍ，高さ３５ｍｍの円柱状
成形物を得た。得られた成形物を、蒸発原料供給機構か
ら１０ｍｍ／分間の供給速度で、蒸発源と別体となって
いる予備加熱部に連続供給し、１×１０-2Ｐａの真空下
で蒸発源を抵抗加熱方式により１３００℃に加熱し、ま
た同時に予備加熱部を９２０℃に加熱した。厚さ１２μ
ｍのポリエチレンテレフタレートフィルムに珪素−マグ
ネシウム複合酸化物を真空蒸着した。その条件のまま加
工速度は５０ｍ／分で、１時間真空蒸着加工を行った。
なお、１時間の真空蒸着加工中には、スプラッシュの発
生は認められなかった。蒸着膜の厚みは、水晶式膜厚モ
ニターを用いて測定したところ、約１０００オングスト
ロームであった。[Embodiment 2] As shown in FIG.
In the vacuum vapor deposition apparatus described in Japanese Patent Publication No. 252768, a preheating unit (made of graphite) that is separate from the evaporation source.
Was set up. The heating method of the preheating section is a high frequency induction heating method. The temperature control of the preheating unit was performed by a radiation thermometer separately from the evaporation source. Next, a mixture of silicon monoxide and magnesium oxide (mixing ratio 90 mol%: 10 mol%) was compression molded to obtain a cylindrical molded product having a diameter of 40 mm and a height of 35 mm. The obtained molded product is continuously supplied from the evaporation material supply mechanism to the preheating section which is a separate body from the evaporation source at a supply rate of 10 mm / minute, and the evaporation source is supplied under a vacuum of 1 × 10 -2 Pa. It was heated to 1300 ° C. by the resistance heating method, and at the same time, the preheating part was heated to 920 ° C. Thickness 12μ
m-polyethylene terephthalate film was vacuum-deposited with a silicon-magnesium composite oxide. Under the conditions, the processing speed was 50 m / min, and vacuum deposition processing was performed for 1 hour.
No splash was observed during the vacuum deposition process for 1 hour. The thickness of the vapor-deposited film was about 1000 Å when measured using a quartz-type film thickness monitor.
【００１６】〔実施例３〕珪素と二酸化珪素等モル混合
物を圧縮成形し、直径４０ｍｍ，高さ３５ｍｍの円柱状
成形物を得た。得られた成形物を、実施例２と同様の真
空蒸着装置の蒸発原料供給機構から１０ｍｍ／分の供給
速度で、蒸発源と別体となっている予備加熱部に連続供
給し、１×１０-2Ｐａの真空下で蒸発源を抵抗加熱によ
り１３００℃に加熱し、また同時に予備加熱部を１１６
５℃に加熱した。予備加熱部の温度と蒸発源の温度から
蒸発原料成形物の昇温速度を計算したところ、２００℃
／分間であった。厚さ１２μｍのポリエチレンテレフタ
レートフィルムに珪素酸化物を真空蒸着し、その条件の
まま加工速度は５０ｍ／分で、１時間真空蒸着加工を行
った。なお、１時間の真空蒸着加工中には、スプラッシ
ュの発生は認められなかった。蒸着膜の厚みは、水晶式
膜厚モニターを用いて測定したところ、約１０００オン
グストロームであった。Example 3 An equimolar mixture of silicon and silicon dioxide was compression molded to obtain a cylindrical molded product having a diameter of 40 mm and a height of 35 mm. The obtained molded product was continuously supplied from the evaporation source supply mechanism of the vacuum evaporation apparatus similar to that of Example 2 to the preheating unit which was separate from the evaporation source at a supply rate of 10 mm / min, and 1 × 10 5. The evaporation source was heated to 1300 ° C. by resistance heating under a vacuum of −2 Pa, and at the same time, the preheating section was heated to 116 ° C.
Heated to 5 ° C. From the temperature of the preheating part and the temperature of the evaporation source, the temperature rise rate of the evaporation raw material molding was calculated to be 200 ° C.
/ Minute. Silicon oxide was vacuum-deposited on a polyethylene terephthalate film having a thickness of 12 μm, and vacuum deposition was performed for 1 hour at the processing speed of 50 m / min under the conditions. No splash was observed during the vacuum deposition process for 1 hour. The thickness of the vapor-deposited film was about 1000 Å when measured using a quartz-type film thickness monitor.
【００１７】〔実施例４〕予備加熱部を６００℃に加熱
した以外は実施例３と同様にして、厚さ１２μｍのポリ
エチレンテレフタレートフィルムに珪素酸化物を真空蒸
着した。予備加熱部及び蒸発源の温度から蒸発原料成形
物の昇温速度を計算したところ、７００℃／分間であっ
た。その条件のまま加工速度は５０ｍ／分で、１時間真
空蒸着加工を行った。しかし、１時間の真空蒸着加工中
に、スプラッシュの発生が認められた。蒸着膜の厚み
は、水晶式膜厚モニターを用いて測定したところ、約１
０００オングストロームであった。Example 4 Silicon oxide was vacuum-deposited on a polyethylene terephthalate film having a thickness of 12 μm in the same manner as in Example 3 except that the preheating section was heated to 600 ° C. The temperature rising rate of the evaporation raw material molded product was calculated from the temperatures of the preheating part and the evaporation source, and it was 700 ° C./minute. Under the conditions, the processing speed was 50 m / min, and vacuum deposition processing was performed for 1 hour. However, generation of splash was observed during the vacuum deposition process for 1 hour. The thickness of the vapor-deposited film was about 1 when measured using a quartz-type film thickness monitor.
It was 000 angstroms.
【００１８】〔比較例１〕予備加熱部を加熱しない以外
は実施例２と同様にして、厚さ１２μｍのポリエチレン
テレフタレートフィルムに珪素−マグネシウム複合酸化
物を真空蒸着した。真空蒸着加工時の蒸発源の温度は実
施例２と同じ１３００℃であるが、その時の予備加熱部
は加熱を行っていないため、熱電対温度計で測定したと
ころ、６０℃であった。その条件のまま加工速度は５０
ｍ／分間で真空蒸着加工を続けたところ、スプラッシュ
の発生が認められ、約３０分後に蒸発原料である成形物
が破損して原料の連続供給ができなくなった為、真空蒸
着加工を中止した。Comparative Example 1 A silicon-magnesium composite oxide was vacuum-deposited on a polyethylene terephthalate film having a thickness of 12 μm in the same manner as in Example 2 except that the preheating section was not heated. The temperature of the evaporation source at the time of vacuum deposition processing was 1300 ° C., which was the same as that in Example 2, but the preheating part at that time did not perform heating, and it was 60 ° C. when measured with a thermocouple thermometer. Machining speed is 50 under that condition
When the vacuum vapor deposition process was continued at m / min, generation of splash was observed, and after about 30 minutes, the molded material as the evaporation raw material was damaged and continuous supply of the raw material was impossible, so the vacuum vapor deposition process was stopped.
【００１９】実施例および比較例で得られた蒸着フィル
ムの蒸着加工の最後の部分について、酸素バリヤー性と
外観を評価した。結果を表１に示す。The oxygen barrier properties and the appearance of the last portion of the vapor deposition process of the vapor deposition films obtained in the examples and comparative examples were evaluated. The results are shown in Table 1.
【表１】 [Table 1]
【００２０】[0020]
【発明の効果】本発明により、蒸発原料の不十分な加
熱，蒸発速度の低下，原料成形物自体が破損，突沸によ
るスプラッシュの発生，急激なガス放出，真空槽内圧力
の上昇，不純物の混入や蒸発速度の変動等のトラブル無
く真空蒸着でき、高品質の蒸着フィルムを得ることがで
きる。EFFECTS OF THE INVENTION According to the present invention, insufficient heating of the evaporation raw material, decrease in evaporation rate, damage to the raw material molding itself, generation of splash due to bumping, rapid gas release, pressure increase in vacuum chamber, inclusion of impurities Vacuum deposition can be performed without troubles such as fluctuation of evaporation rate and evaporation rate, and a high quality vapor deposition film can be obtained.
【００２１】[0021]
【図１】本発明の蒸発源と一体となった予備加熱部と蒸
発源の側面図。FIG. 1 is a side view of a preheating unit and an evaporation source integrated with the evaporation source of the present invention.
【図２】本発明の蒸発源と別体となった予備加熱部と蒸
発源の側面図。FIG. 2 is a side view of a preheating unit and an evaporation source which are separate from the evaporation source of the present invention.
【図３】本発明の蒸発源と別体となった予備加熱部と蒸
発源の側面図。FIG. 3 is a side view of a preheating unit and an evaporation source which are separate from the evaporation source of the present invention.
【図４】従来のボート状の蒸発源の斜視図。FIG. 4 is a perspective view of a conventional boat-shaped evaporation source.
【図５】従来の電子線加熱方式の蒸発源の側面図。FIG. 5 is a side view of a conventional electron beam heating evaporation source.
【図６】従来の蒸発源の側面図。FIG. 6 is a side view of a conventional evaporation source.
１：蒸発源 ２：蒸発原料
３：蒸発原料供給機構 ４：電子銃 ５：電子線
６：電極 ７：予備加熱部 ８：放射温度計
９：ＰＩＤ温調計 10：高周波誘導コイル1: evaporation source 2: evaporation material
3: Evaporation material supply mechanism 4: Electron gun 5: Electron beam
6: Electrode 7: Preheating part 8: Radiation thermometer
9: PID temperature controller 10: High frequency induction coil
Claims (2)
方法において、蒸発原料を蒸発させる前に予め加熱する
ことを特徴とする真空蒸着方法。1. A vacuum vapor deposition method for substantially continuously supplying an evaporation raw material, wherein the evaporation raw material is preheated before being vaporized.
装置において、蒸発原料を蒸発させる前に予め加熱する
予備加熱部を有することを特徴とする真空蒸着装置。2. A vacuum vapor deposition apparatus for supplying an evaporation raw material substantially continuously, comprising a preheating unit for preheating the evaporation raw material before vaporizing it.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP12231694A JP3453190B2 (en) | 1994-06-03 | 1994-06-03 | Vacuum evaporation method and vacuum evaporation apparatus |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP12231694A JP3453190B2 (en) | 1994-06-03 | 1994-06-03 | Vacuum evaporation method and vacuum evaporation apparatus |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH07331420A true JPH07331420A (en) | 1995-12-19 |
| JP3453190B2 JP3453190B2 (en) | 2003-10-06 |
Family
ID=14832943
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP12231694A Expired - Fee Related JP3453190B2 (en) | 1994-06-03 | 1994-06-03 | Vacuum evaporation method and vacuum evaporation apparatus |
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| Country | Link |
|---|---|
| JP (1) | JP3453190B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010229531A (en) * | 2009-03-30 | 2010-10-14 | Toppan Printing Co Ltd | Vapor deposition apparatus |
-
1994
- 1994-06-03 JP JP12231694A patent/JP3453190B2/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010229531A (en) * | 2009-03-30 | 2010-10-14 | Toppan Printing Co Ltd | Vapor deposition apparatus |
Also Published As
| Publication number | Publication date |
|---|---|
| JP3453190B2 (en) | 2003-10-06 |
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