JP2004143551A - Vacuum treatment method - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To reduce the cost of equipment and to minimize the degradation in yield and operation rate without adversely affecting other reaction vessels when abnormality occurs in one reaction vessel in a vacuum treatment method and apparatus for simultaneously performing a number of vacuum treatments by using a plurality of the reaction vessels. <P>SOLUTION: The respective reaction vessels 100 internally installed with substrates are moved by movable means 104 to connect mechanisms 107 and gate valves 102. The gate valves 102, slow exhaust valves 110, etc., of the respective reaction vessels 100 are opened and the evacuation in the plurality of the reaction vessels 100 is simultaneously started. When the valves 110 are opened, the measurement of the evacuation rates are started and whether the exhaust rates are within prescribed ranges or not is discriminated. Further, the slow evacuating is carried out and when the internal pressures of the reaction vessels 100 attain prescribed values, a main evacuating valve 106 is opened to put the interior of the reaction vessels 100 further into the evacuation state. When the internal pressures of the reaction vessels 100 attain the prescribed values, the leak check of the reaction vessels 100 is started. <P>COPYRIGHT: (C)2004,JPO

Description

（反応容器１つ当たりの流量）
【００７４】
【表２】

【００７５】
［実施例２］
図２、図４に示した真空処理装置において、反応容器部１００内に設置した長さ３５８ｍｍ、外径φ１０８ｍｍの鏡面加工を施したＡｌ製シリンダー（円筒状基体１２０）上にａ−Ｓｉ膜を、高周波電源１２１の発振周波数を１０５ＭＨｚとして表１に示す条件で成膜し、電子写真感光体を作製した。
【００７６】
図２（ａ）、（ｂ）は本実施例の真空処理方法を実施する装置の一例の模式図であり、電子写真感光体の形成装置の一例を示した模式図である。図２（ａ）は、横断面図、図２（ｂ）は、上面図である。
【００７７】
本実施例による電子写真感光体の製造装置は、図２に示すように移動可能な反応容器部１００Ａ〜Ｃを備えており、反応容器部１００Ａ〜Ｃの各々は、被処理基体（図示せず）が配置される反応容器１０１と、ゲートバルブ１０２Ａ〜Ｃと、架台１０３と、移動可能手段１０４としてのキャスターとからなる。
【００７８】
反応容器１０１内を排気するために排気手段１５０，１５１が備えられており、排気手段１５０には、反応容器１０１に繋がる集合排気管１０５と、メイン排気バルブ１０６Ａ〜Ｃと、集合排気管１０５を反応容器部１００Ａ〜Ｃに接続させる接続機構１０７Ａ〜Ｃと、内圧測定器１０８Ａ〜Ｃと、反応容器部１００の内部の圧力を調整するために、排気コンダクタンス制御手段１０９Ａ〜Ｃが接続されている。また、排気手段１５１には、集合排気管１４０、スロー排気ライン１１１、スロー排気バルブ１１０、メイン排気バルブ１４１、バルブ１４２Ａ〜Ｃが接続されている。
【００７９】
反応容器部１００のガス供給及び流量制御手段１６０は、真空処理に必要となる複数のガスボンベ、レギュレータ、バルブ類、マスフローコントローラーなどを含んでいることが望ましく、所望のガスを所望の流量、混合比で供給することが出来れば、いかなる構成でも構わない。また、更に好ましくはパージ用のガスボンベ、パージラインを含んでいることが望ましく、このことによりガスを安全に運用することが可能となる。真空処理に必要な原料ガスは、ガス供給及び流量制御手段１６０より、流量可変バルブ１６１Ａ〜Ｃ、接続機構１０７Ａ〜Ｃを介し、反応容器１０１内に供給される。
【００８０】
本実施例において、電子写真感光体の作製は以下のように行った。なお、本実施例の反応容器部１００も上記の実施例１と同じで、図４に示したとおりである。
【００８１】
クリーンルームからなる基体投入エリア（図示せず）で反応容器１０１内に基体ホルダー１３０に装着された円筒状基体１２０を設置する。次に上蓋１２４を取り付け、反応容器部１００Ａ〜Ｃを作業員による手動搬送で図２の成膜エリアの接続機構１０７Ａ〜Ｃまで移動し、ゲートバルブ１０２Ａ〜Ｃと接続機構１０７Ａ〜Ｃとを接続させる。ここで接続方法は、ゲートバルブ１０２Ａ〜Ｃと接続機構１０７Ａ〜Ｃの間にＯリングを介して接続した。本実施例においては、図２に示すように３台の反応容器部１００Ａ〜Ｃを用いた。
【００８２】
３台の反応容器部１００Ａ〜Ｃの接続を終了した後、各反応容器部１００Ａ〜Ｃのゲートバルブ１０２Ａ〜Ｃ、バルブ１４２Ａ〜Ｃを開け、スロー排気バルブ１１０を開け、スロー排気ライン１１１を使用し、複数の反応容器部１００内の減圧を同時に開始する。次に本発明の特徴である工程１を実施した。前記工程１の判別基準として、スロー排気バルブ１１０を開いた後、３０分後に各内圧測定器１０８Ａ〜Ｃの値が１１０００Ｐａ以下なら異常無し、１１０００Ｐａより圧力が高い場合は異常有りとした。本実施例では、スロー排気バルブ１１０を開いた後、３０分後に各内圧測定器１０８Ａ〜Ｃの値が１００００Ｐａに達していたので、引き続きスロー排気を実施した。次に内圧測定器１０８Ａ〜Ｃの値が４００Ｐａに達した時、スロー排気バルブ１１０を閉じ、メイン排気バルブ１４１を開けて、更に反応容器内の真空度を高くした。内圧測定器１０８Ａ〜Ｃの値が０．６５Ｐａに達した時、本発明の特徴である工程２を実施した。内圧測定器１０８Ａ〜Ｃの値が０．６５Ｐａに達した時、各バルブ１４２Ａ〜Ｃを閉め、５分間放置した。５分後の各内圧測定器１０８Ａ〜Ｃの値が１．０Ｐａ以下のときは、異常無しとし、１．０Ｐａより高い場合は異常有りとした。本実施例では、５分後の各内圧測定器１０８Ａ〜Ｃの値が０．８５Ｐａだったので、次の工程に移行した。バルブ１４２Ａ〜Ｃを開け、基体加熱用ヒーター１２５を駆動させ、円筒状基体１２０を２８０℃に加熱し制御した。
【００８３】
この加熱中に、前述の高周波電極１２７、高周波シールド１２２、高周波整合器１２８を反応容器１０１の周囲に設置し、さらに高周波整合器１２８と高周波電源１２７とを同軸ケーブルで接続した。
【００８４】
円筒状基体１２０が所定の温度となったところで、バルブ１４２Ａ〜Ｃを閉じ、ゲートバルブ１０２Ａ〜Ｃを全て開けた。次に、原料ガス導入管１２６を介して、原料ガスを反応容器１０１内に導入する。原料ガスの流量が設定流量となり、また、反応容器１０１内の圧力が安定したのを確認した後、１０５ＭＨｚの高周波電源１２１より高周波整合器１２８を介して高周波電極１２７へ所定の高周波電力を供給する。これら堆積膜形成の条件は表１に示す。堆積膜形成中は、モーター１３１を駆動させ円筒状基体１２０を回転させた。
【００８５】
堆積膜形成終了後、反応容器部１００Ａ〜Ｃを接続機構１０７Ａ〜Ｃから切り離し、円筒状基体取り出しステージ（図示せず）まで移動させ、堆積膜が形成された円筒状基体１２０を取り出した。その後、反応容器１０１内の構成部品を交換し、再度堆積膜形成可能な状態としたところで一連の工程を終了した。
【００８６】
以上の様な電子写真感光体の形成を連続して、２０回実施した。
【００８７】
このとき、３回目に、前記工程１おいて、スロー排気バルブ１１０を開いて、３０分後に内圧測定器１０８Ａの値が１１０００Ｐａより圧力が高かった。そこで、バルブ１４２Ａを閉じ、反応容器１００Ａを大気圧力に戻し、接続機構１０７Ａから切り離した。そして、切り離した接続機構１０７Ａに封止フランジを取り付けた。一方、残りの２つの反応容器部１００Ｂ，１００Ｃは、内圧測定器１０８Ｂ，１０８Ｃが９０００Ｐａになった時点でバルブ１４２Ｂ，１４２Ｃを閉じ、真空保持状態を維持した。その後、バルブ１４２Ａを開け、内圧測定器１０８Ａの値が９０００Ｐａになったところで、バルブ１４２Ｂ，１４２Ｃを開け、引き続きスロー排気を実施した。その後は、前記工程２を実施し、前述のように電子写真感光体を作製した。
【００８８】
また、１０回目に前記工程２おいて、５分間真空放置後の内圧測定器１０８Ｃの値が１．０Ｐａより高かったので、反応容器１００Ｃを大気圧力に戻し、接続機構１０７Ｃから切り離した。そして、切り離した接続機構１０７Ｃにメクラ・フランジを取付けた。そして、バルブ１４２Ｃを開け、内圧測定器１０８Ｃの値が、内圧測定器１０８Ａ，１０８Ｂと同じになったところで、バルブ１４２Ａ〜Ｃを全て開け、次の工程に移行し、前述のように電子写真感光体を作製した。
【００８９】
作製した電子写真感光体に対し、実施例１と同様に評価を行ったところ、実施例１と同様、再現性良く電子写真感光体を作製できた。また、実施例１に対し、異常の検出と異常個所の特定を同時に実施可能なため、装置の稼働率を向上できることが判った。
【００９０】
［実施例３］
図３、図４に示した真空処理装置において、反応容器部１００内に設置した長さ３５８ｍｍ、外径φ１０８ｍｍの鏡面加工を施したＡｌ製シリンダー（円筒状基体１２０）上にａ−Ｓｉ膜を、高周波電源１２１の発振周波数を１０５ＭＨｚとして表１に示す条件で成膜し、電子写真感光体を作製した。
【００９１】
図３は本実施例の真空処理方法を実施する装置の一例の模式図であり、電子写真感光体の形成装置の一例を示した模式図である。
【００９２】
本実施例による電子写真感光体の製造装置は、図３に示すように移動可能な反応容器部１００Ａ〜Ｃを備えており、反応容器部１００Ａ〜Ｃの各々は、被処理基体（図示せず）が配置される反応容器１０１と、ゲートバルブ１０２Ａ〜Ｃと、架台１０３と、移動可能手段１０４としてのキャスターとからなる。
【００９３】
反応容器１０１内を排気するために排気手段１５０，２５０，２５１が備えられており、排気手段１５０には、反応容器１０１に繋がる集合排気管１０５と、メイン排気バルブ１０６と、集合排気管１０５を反応容器部１００Ａ〜Ｃに接続させる接続機構１０７Ａ〜Ｃと、内圧測定器１０８と、スロー排気ライン１１１と、スロー排気バルブ１１０とが接続されている。
【００９４】
排気手段２５０には、集合排気管２０５、メイン排気バルブ２０６Ａ〜Ｃ、接続機構２０７Ａ〜Ｃ、内圧測定器２０８Ａ〜Ｃ、反応容器部１００Ａ〜Ｃの内部の圧力を調整するために、排気コンダクタンス制御手段２０９Ａ〜Ｃが接続されている。また、排気手段２５１には、集合排気管２４０、メイン排気バルブ２４１、バルブ２４２Ａ〜Ｃが接続されている。
【００９５】
反応容器部１００のガス供給及び流量制御手段２６０は、真空処理に必要となる複数のガスボンベ、レギュレータ、バルブ類、マスフローコントローラーなどを含んでいる。真空処理に必要な原料ガスは、ガス供給及び流量制御手段２６０より、流量可変バルブ２６１Ａ〜Ｃ、接続機構２０７Ａ〜Ｃを介し、反応容器１０１内に供給される。
【００９６】
本実施例において、電子写真感光体の作製は以下のように行った。なお、本実施例の反応容器部１００も上記の実施例１と同じで、図４に示したとおりである。
【００９７】
クリーンルームからなる基体投入エリアにある、接続機構１０７Ａ〜Ｃに反応容器部１００Ａ〜Ｃを作業員による手動搬送移動し、ゲートバルブ１０２Ａ〜Ｃと接続機構１０７Ａ〜Ｃとを接続させる。そして、各反応容器１０１内に基体ホルダー１３０に装着された円筒状基体１２０を設置する。上蓋１２４を取り付けた後、各反応容器部１００Ａ〜Ｃのゲートバルブ１０２Ａ〜Ｃを開け、スロー排気バルブ１１０を開け、スロー排気ライン１１１を使用し、複数の反応容器部１００内の減圧を同時に開始する。次に本発明の特徴である工程１を実施した。
【００９８】
前記工程１の判別基準として、スロー排気バルブ１１０を開いた後、３０分後に内圧測定器１０８の値が２００００Ｐａ以下なら異常無し、２００００Ｐａより圧力が高い場合は異常有りとした。本実施例では、スロー排気バルブ１１０を開いた後、３０分後に内圧測定器１０８の値が１８０００Ｐａに達していたので、引き続きスロー排気を実施した。次に内圧測定器１０８の値が４００Ｐａに達した時、スロー排気バルブ１１０を閉じ、メイン排気バルブ１０６を開けて、更に反応容器内の真空度を高くした。内圧測定器１０８の値が０．６５Ｐａに達した時、本発明の特徴である工程２を実施した。内圧測定器１０８の値が０．６５Ｐａに達した時、メイン排気バルブ１０６を閉め、５分間放置した。５分後の内圧測定器１０８の値が１．３Ｐａ以下のときは、問題無しとし、１．３Ｐａより高い場合は異常とした。本実施例では、５分後の内圧測定器１０８の値が１．０Ｐａだったので、次の工程に移行した。
【００９９】
ゲートバルブ１０２Ａ〜Ｃ、メイン排気バルブ１０６を閉じ、リークバルブ１６１を開き、集合排気管１０５を大気圧力に戻した。その後、反応容器部１００Ａ〜Ｃを接続機構１０７Ａ〜Ｃから切り離し、成膜エリアにある、接続機構２０７Ａ〜Ｃに反応容器部１００Ａ〜Ｃを作業員による手動搬送で移動し、ゲートバルブ１０２Ａ〜Ｃと接続機構２０７Ａ〜Ｃとを接続させる。バルブ２４２Ａ〜Ｃ、メイン排気バルブ２４１を開け、ゲートバルブ１０２Ａ〜Ｃとゲートバルブ２０６Ａ〜Ｃの間を、内圧測定器２０８Ａ〜Ｃの値が０．６Ｐａに達するまで、真空引きした。その後バルブ２４２Ａ〜Ｃを閉じ、２分間真空放置試験を実施し、接続機構２０７Ａ〜Ｃとゲートバルブ１０２Ａ〜Ｃの接続に問題が無いことを確認した。そして、ゲートバルブ１０２Ａ〜Ｃ、バルブ２４２Ａ〜Ｃを開け、基体加熱用ヒーター１２５を駆動させ、円筒状基体１２０を２５０℃に加熱し制御した。
【０１００】
この加熱中に、前述の高周波電極１２７、高周波シールド１２２、高周波整合器１２８を反応容器１０１の周囲に設置し、さらに高周波整合器１２８と高周波電源１２７とを同軸ケーブルで接続した。
【０１０１】
円筒状基体１２０が所定の温度となったところで、バルブ２４２Ａ〜Ｃを閉じ、ゲートバルブ２０６Ａ〜Ｃを全て開けた。次に、原料ガス導入管１２６を介して、原料ガスを反応容器１０１内に導入する。原料ガスの流量が設定流量となり、また、反応容器１０１内の圧力が安定したのを確認した後、１０５ＭＨｚの高周波電源１２１より高周波整合器１２８を介して高周波電極１２７へ所定の高周波電力を供給する。これら堆積膜形成の条件は表１に示す。堆積膜形成中は、モーター１３１を駆動させ円筒状基体１２０を回転させた。
【０１０２】
堆積膜形成終了後、反応容器部１００Ａ〜Ｃを接続機構１０７Ａ〜Ｃから切り離し、円筒状基体取り出しステージ（図示せず）まで移動させ、堆積膜が形成された円筒状基体１２０を取り出した。その後、反応容器１０１内の構成部品を交換し、再度堆積膜形成可能な状態としたところで一連の工程を終了した。
【０１０３】
以上の様な電子写真感光体の形成を連続して、３０回実施した。
【０１０４】
また、本実施例において、減圧速度の判定、真空放置試験の判定において、異常と判定された場合は、実施例１、２と同様な対処を行い、工程を進めた。
【０１０５】
作製した電子写真感光体に対し、実施例１、２と同様に評価を行ったところ、実施例１、２と同様、再現性良く電子写真感光体を作製できた。
【０１０６】
【発明の効果】
以上説明したように、本発明によれば、排気手段、ガス供給手段を共有した複数の反応容器を用いて同時に多数の被処理物に真空処理を行う場合、ある反応容器で異常が発生した際に、この異常が発生した反応容器のみを排気手段から断絶することで、正常に真空処理を行っている反応容器内の被処理物への影響を抑制することができ、製品の歩留まり低下を最小限にくい止めることが可能となる。
また、ガス供給系を共有することで、非常に複雑で高価な付帯設備であるガス供給及び流量制御手段を反応容器毎に設ける必要がなく、設備コストを低減することが可能となる。
【０１０７】
また、本発明によれば、異常が発生した反応容器を排気手段から直ちに切り離して次の真空処理の準備などを迅速に行うことができ、生産装置のデッドタイムを最小限に抑えることが可能である。以上の点から、高品質な真空処理をより安価に供給することが可能となる。
【図面の簡単な説明】
【図１】本発明の真空処理方法を実施する装置の例であり、電子写真感光体の形成装置の一例を示した模式図であって、（ａ）は横断面図、（ｂ）は上面図である。
【図２】本発明の実施例２である、電子写真感光体の形成装置の一例を示した模式図であって、（ａ）は横断面図、（ｂ）は上面図である。
【図３】本発明の実施例３である、電子写真感光体の形成装置の一例を示した模式図であって、（ａ）は横断面図、（ｂ）は上面図である。
【図４】ＶＨＦ帯の高周波電力を好適に使用可能なプラズマＣＶＤ法を用いた電子写真感光体の製造装置の模式図である。
【符号の説明】
１００、１００Ａ〜Ｃ　　　　　　反応容器部
１０１　　　　　　反応容器
１０２、１０２Ａ〜Ｃ　　　　　　ゲートバルブ
１０３　　　　　　架台
１０４　　　　　　移動可能手段
１０５、２０５、１４０、２４０　　　　　　集合排気配管
１０６、１０６Ａ〜Ｃ、２０６Ａ〜Ｃ　　　　　　メイン排気バルブ
１０７、１０７Ａ〜Ｃ、２０７Ａ〜Ｃ　　　　　　接続機構
１０８、２０８Ａ〜Ｃ　　　　　　内圧測定器
１０９、１０９Ａ〜Ｃ、２０９Ａ〜Ｃ　　　　　　排気コンダクタンス制御手段
１１０　　　　　　スロー排気バルブ
１１１　　　　　　スロー排気ライン
１２０　　　　　　基体
１２１　　　　　　高周波電源
１２２　　　　　　高周波シールド
１２３　　　　　　反応容器支持台
１２４　　　　　　上蓋
１２５　　　　　　基体加熱用ヒーター
１２６　　　　　　原料ガス導入管
１２７　　　　　　高周波電極
１２８　　　　　　高周波整合器
１２９　　　　　　絶縁体
１３０　　　　　　基体ホルダー
１３１　　　　　　モーター
１５０、１５１、２５０、２５１　　　　　　排気手段
１６０、２６０　　　　　　ガス供給及び流量制御手段
１６１、１６１Ａ〜Ｃ　　　　　　流量可変バルブ
１４１、２４１、１４２Ａ〜Ｃ、２４２Ａ〜Ｃ、１６１、２６１　　　　　　バルブ及び真空処理装置[0001]
TECHNICAL FIELD OF THE INVENTION
The present invention relates to a vacuum processing method such as deposition film formation and etching used for forming a semiconductor device, an electrophotographic photosensitive member, an image input line sensor, a photographing device, a photovoltaic device, and the like.
[0002]
[Prior art]
Conventionally, as a vacuum processing method used for producing a semiconductor device, an electrophotographic photoreceptor, a line sensor for image input, an imaging device, a photovoltaic device, other various electronic elements, optical elements, etc., a vacuum deposition method, a sputtering method, and the like. There are many known methods, such as an ion plating method, an ion plating method, a thermal CVD method, an optical CVD method, and a plasma CVD method, and an apparatus for the method has been put to practical use. Among them, a plasma process using high-frequency power is used for various advantages such as being able to be used for forming and etching a deposited film using various materials, and also for forming an insulating material such as an oxide film and a nitride film. I have. Preferable examples of the use of the plasma process include, for example, formation of a hydrogenated amorphous silicon for electrophotography (hereinafter, referred to as a-Si: H) deposited film and the like. Various proposals have been made.
[0003]
In addition, various devices have been devised to produce a high-quality deposited film at a lower cost.
[0004]
For example, Japanese Patent Application Laid-Open No. H10-168574 discloses a technique for shortening the total time spent for manufacturing by devising a cleaning method for a deposited film forming apparatus. An example of a deposition film forming apparatus that exhausts gas by means of the exhaust means is disclosed. Japanese Patent Publication No. 7-13947 discloses a technique for producing a plurality of thin film transistor arrays using a plurality of reaction vessels in which a source gas supply unit and an exhaust unit are shared. By connecting a plurality of reaction vessels to a single exhaust unit or a single gas supply unit in this manner, it is possible to reduce capital investment in the gas supply unit and the exhaust unit.
[0005]
Further, Japanese Patent Application Laid-Open No. 10-168576 discloses details of a deposition film forming apparatus in which a vacuum vessel is connected to an exhaust unit, a source gas supply unit via a detachable connection mechanism, and an attachment / detachment mechanism. By being detachable in this way, for example, when manufacturing different types of deposited films, only the reaction container needs to be changed, which is advantageous in terms of capital investment, equipment downtime, and the like.
[0006]
[Patent Document 1]
JP-A-10-168574
[Patent Document 2]
Japanese Patent Publication No. 7-13947
[Patent Document 3]
JP-A-10-168576
[0007]
[Problems to be solved by the invention]
The conventional method and apparatus have the advantages that the number of vacuum processes that can be performed simultaneously is large, and that additional equipment such as gas flow control means and gas exhaust means can be shared, which is advantageous in cost reduction.
[0008]
However, as described above, in the case of a configuration in which ancillary equipment such as a gas flow control unit and a gas exhaust unit is shared and a large number of vacuum processes are simultaneously performed in a plurality of reaction vessels, a certain one of the plurality of reaction vessels is used. When an abnormality occurs in the reaction vessel, the related equipment may be adversely affected due to the sharing of the auxiliary equipment.
[0009]
One of the abnormalities in the vacuum processing is an external leak into the processing container. If there is an external leak during the vacuum processing, the inside of the processing container is contaminated and adversely affects the processing characteristics.
[0010]
In this case, as described above, even if an external leak occurs in one of the plurality of reaction vessels, for example, a contamination source such as oxygen diffuses through a common exhaust pipe, and the processing of the other reaction vessels proceeds. Affects properties. Further, when processing the above-described electrophotographic photoreceptor, not only during processing as described later, but also before processing is started, and further, decompression processing is started, and even if an abnormality occurs in one reaction vessel for a while, It may adversely affect other reaction vessels.
[0011]
As described above, a mass-production type apparatus capable of processing a large amount of deposited films at one time is very advantageous in terms of cost, but once a trouble occurs, in the worst case, all reactions sharing the incidental facilities are performed. There is a problem that all the vacuum-processed products performed in the container may be defective.
[0012]
An object of the present invention is to solve the above problems. In other words, in a vacuum processing method and a vacuum processing apparatus capable of simultaneously performing a large number of vacuum processes using a plurality of reaction vessels, the auxiliary equipment such as a gas supply unit and an exhaust unit is shared to greatly reduce the cost of the equipment. In addition, a vacuum processing method is provided in which, when an abnormality occurs in one reaction vessel, it does not adversely affect other normally operating reaction vessels and can minimize a decrease in yield and operation rate. It is intended to be.
[0013]
[Means for Solving the Problems]
In order to achieve the above object, the present invention provides an object to be treated is installed in a plurality of reaction vessel sections that can be decompressed, each of the reaction vessel sections is connected to a pipe connected to the same exhaust means and exhausted, In the vacuum processing method for simultaneously processing an object to be processed, when the plurality of reaction vessel sections are depressurized, the plurality of reaction vessel sections are simultaneously evacuated by the exhaust means, and a decompression rate (Δ pressure / Δ time) is within a predetermined range, and after the step 1, the plurality of reaction vessel sections are further depressurized, and the pressure in each reaction vessel section reaches a predetermined value. Then, a predetermined vacuum process is performed after at least the step 2 of simultaneously leak-checking the plurality of reaction vessel sections.
[0014]
Further, in the step 1, when the pressure reduction rate is out of the predetermined range, the step of stopping the pressure reduction processing of the plurality of reaction vessel sections and individually detecting an abnormal portion for the plurality of reaction vessel sections. It is preferable that, after the operation is performed and only the reaction vessel part in which an abnormality occurs is disconnected from the exhaust unit, the remaining reaction vessel parts are continuously shifted to the next step.
[0015]
Further, in the step 2, when an abnormality is detected, decompression processing of the plurality of reaction vessel sections is stopped, and for the plurality of reaction vessel sections, a step of individually detecting an abnormal portion is performed, After disconnecting only the reaction vessel part in which the abnormality has occurred from the exhaust means, it is preferable to continue to the next step for the remaining reaction vessel parts.
[0016]
Further, in the step 1, the detection of the decompression rate is performed individually and simultaneously on the plurality of reaction vessel parts, and after the reaction vessel parts whose decompression rate is out of a predetermined range are disconnected from the exhaust unit, the remaining pressure is reduced. It is preferable to continue to the next step for the reaction vessel section.
[0017]
Further, in the step 2, the abnormality is detected individually and simultaneously for the plurality of reaction vessel sections, and after the reaction vessel section in which the abnormality has occurred is disconnected from the exhaust means, the remaining reaction vessel sections are continued. Then, it is preferable to proceed to the next step.
[0018]
BEST MODE FOR CARRYING OUT THE INVENTION
Hereinafter, embodiments of the present invention will be described with reference to the drawings.
[0019]
The present inventors have conducted intensive studies to achieve the above object, and as a result, a vacuum processing method capable of simultaneously performing a large amount of vacuum processing by connecting a plurality of reaction vessels to the same exhaust unit and the same gas supply unit. In the event that an abnormality occurs in a certain reaction vessel, by using the vacuum processing method as described above, it is possible to prevent the problem from spreading to other reaction vessels and minimize the decrease in the product yield rate. Made it possible.
[0020]
Such an embodiment of the present invention will be described in detail below.
[0021]
FIGS. 1A and 1B are schematic views of an example of an apparatus for performing the vacuum processing method of the present invention, and are schematic views showing an example of an apparatus for forming an electrophotographic photosensitive member. FIG. 1A is a cross-sectional view, and FIG. 1B is a top view.
[0022]
An electrophotographic photoreceptor manufacturing apparatus suitable for the vacuum processing method of the present embodiment includes a movable reaction container section 100 as shown in FIG. 1, and the reaction container section 100 includes a substrate to be processed (not shown). (1), a reaction vessel 101 in which a grease is disposed, a gate valve 102, a gantry 103, and casters as movable means 104.
[0023]
The movable means 104 may be any means capable of moving the reaction container section 100, and may employ a moving method such as caster movement, belt movement, magnetic floating movement, or air floating movement. It is desirable to move the casters from.
[0024]
The exhaust means 150 for exhausting the inside of the reaction vessel 101 includes a collective exhaust pipe 105 connected to the reaction vessel 101, a main exhaust valve 106, a connection mechanism 107 for connecting the collective exhaust pipe 105 to the reaction vessel section 100, an internal pressure An exhaust conductance control unit 109, a slow exhaust valve 110, and a slow exhaust line 111 are connected to adjust the pressure inside the reaction container 100 with the measuring device 108.
[0025]
The reaction vessel section 100 is connected to an exhaust unit 150 via a connection mechanism 107, a gate valve 102, and a collective exhaust pipe 105. The pumping means 150 may be any pump, such as a rotary pump, a mechanical booster pump, an oil diffusion pump, a turbo molecular pump, or any combination thereof as long as the pumping means can obtain a desired pumping speed.
[0026]
The gas supply and flow rate control means 160 of the reaction vessel section 100 desirably includes a plurality of gas cylinders, regulators, valves, mass flow controllers, and the like required for vacuum processing. Any configuration can be used as long as it can be supplied. Further, it is more desirable to include a gas cylinder for purging and a purge line, so that the gas can be operated safely. The source gas required for the vacuum processing is supplied from the gas supply and flow rate control means 160 into the reaction vessel 101 via the variable flow rate valve 161 and the connection mechanism 107.
[0027]
Further, it is desirable to provide a gas connection mechanism between the reaction container section 100 and the variable flow rate valve 161, and the connection mechanism 107 incorporates a gas connection mechanism.
[0028]
In FIG. 1, the number of the reaction vessel portions 100 is three, but the number is determined in consideration of the exhaust capacity of the exhaust means 150 or the work efficiency at the time of attaching and detaching the reaction vessel section 100 to the exhaust means 150. May be arbitrarily determined.
[0029]
The connection mechanism 107 preferably has a flange structure for holding a vacuum, and the vacuum seal may be any of an O-ring seal, a metal seal, and the like. As a method for fixing the connection mechanism 107 and the gate valve 102, any method using a bolt, a coupler, a clamp, or the like may be used, but it is more preferable to be able to easily attach and detach.
[0030]
The vacuum processing method of the present invention using the apparatus for manufacturing an electrophotographic photoreceptor shown in FIG. 1 can be generally performed as follows.
[0031]
First, the substrate is placed in the reaction container 101 of the reaction container section 100 in a substrate charging area (not shown).
[0032]
The substrate is precisely cleaned in advance, and the substrate is installed in a dust-controlled environment such as a clean room. Next, each reaction vessel unit 100 is moved from the substrate charging area to the connection mechanism 107 by driving a caster as the movable means 104, and the connection mechanism 107 and the gate valve 102 are connected. The gate valve 102 of each reaction vessel part 100 is opened, the slow exhaust valve 110 is opened, and the pressure in the plurality of reaction vessel parts 100 is simultaneously started using the slow exhaust line 111.
[0033]
Slow exhaust is performed by opening the main exhaust valve 106 and reducing the pressure inside the reaction vessel 100 at a stretch, whereby the gas in the reaction vessel 100 is drawn at a stretch to the connection end opening of the exhaust pipe, and the reaction vessel This is because a large turbulence is generated in the inside 100 and particles deposited on the wall surface and the bottom surface in the reaction container portion 100 soar up to prevent the particles from adhering to the substrate surface.
[0034]
When the evacuation unit 150 starts evacuation of the reaction container unit 100, step 1 which is one of the features of the present invention is performed. When the slow exhaust valve 110 is opened, measurement of the pressure reduction rate (Δpressure / Δtime) is started. In measuring the pressure reduction rate, the internal pressure measuring device 108 monitors the pressure of the collective exhaust pipe 105 to which the reaction vessel section 100 is connected. Then, it is determined whether the exhaust speed is within a predetermined range. The determination is made in advance by monitoring the exhaust time and the change in pressure in a state where there is no external leak, using the monitored values as a reference (reference value), and determining the degree of deviation from the reference. . For example, the evacuation time is fixed to T, and it is determined whether or not the pressure when the time of T elapses is near the reference. Alternatively, changes in the evacuation time and pressure may be observed several times, and the average thereof may be used as a reference.
[0035]
The step 1 is performed in a state where little time has passed since the start of evacuation, that is, in a low vacuum state. The following problems occur when the time elapses in a situation where an external leak is occurring. Air is discharged from the leak location into the reaction vessel section 100, and as a result, turbulence is generated near the leak location, and particles may flow in the reaction vessel section 100. For a while after the evacuation is started, the particles float due to a low vacuum state, and eventually float to the inside of the adjacent reaction vessel part 100 via a common exhaust pipe, and may contaminate the inside of the reaction vessel part 100. . In particular, in the production of an electrophotographic photoreceptor, the rate of occurrence of defects caused by the attachment of dust and the like on a substrate greatly affects productivity. This is because, when the above-described defect occurs in the electrophotographic photosensitive member, the defect cannot be repaired, which greatly affects the yield of the electrophotographic photosensitive member. On the other hand, in a high vacuum state, the particles can no longer float, so that the particles hardly affect the adjacent reaction vessel section 100 as described above.
[0036]
In other words, even if a leak is checked in a high vacuum state and an abnormality is found, especially for defects caused by particles attached to the substrate, such as an electrophotographic photoreceptor, the defect has already been found in the reaction vessel part where the occurrence of the abnormality was found. In some cases, this has an adverse effect, so that it is very effective to perform a leak check in a low vacuum state.
[0037]
The low vacuum state in which the step 1 is performed cannot be unconditionally defined by the shape and volume of the apparatus or the connection method and length of the exhaust pipe, and furthermore, the amount of external leakage. From the atmospheric pressure, it is preferable to perform the process up to 133 Pa (1 Torr) from the atmospheric pressure, and it is more preferable to perform the process up to 13330 Pa (100 Torr) from the viewpoint of yield.
[0038]
Further, as the leak detection method in the above step 1, the method of detecting the exhaust speed of the present invention is the best. Since the step 1 is performed in a low vacuum state as described above, a Geisler tube method or a leak detection method using a helium leak detector cannot be used. Further, in the vacuum standing method, since the exhaust valve is closed in a reduced pressure state, the gas flow is eliminated in the reaction vessel, and particles are easily diffused. The exhaust speed of the present invention can be detected in a situation where particles are unlikely to be diffused into an adjacent reaction container because a gas flow always occurs from the reaction container to the exhaust unit.
[0039]
Next, after confirming that the pumping speed is within a predetermined range, the process proceeds to the step 2. Further, slow exhaust is performed, and when the internal pressure of the reaction container 100 reaches a predetermined value, the main exhaust valve 106 is opened to further reduce the pressure inside the reaction container 100. Next, when the internal pressure of the reaction container 100 reaches a predetermined value, a leak check of the reaction container 100 is started. The method of the leak check is not particularly limited, and a Geisler tube method, a leak detection method using a helium leak detector, a vacuum leaving method, or the like is used.
[0040]
Step 2 is performed in a high vacuum state, but it is preferable that the step 2 is performed at a lower pressure than the internal pressure under vacuum processing conditions (for example, during CVD).
[0041]
After confirming that there is no abnormality, the process proceeds to the next step.
[0042]
If the pumping speed is out of the predetermined range in the step 1, and if an abnormality is found in the step 2, the process is interrupted, the reaction vessel unit 100 is disconnected from the exhaust unit 150, and the next preparation is performed. Another reaction vessel unit 100 is newly connected to the exhaust unit 150, and the process is started again from the installation of the base. Further, the separated reaction container unit 100 is moved to another area, where the cause of the abnormality is specified and the abnormality is repaired.
[0043]
By performing the vacuum processing method of the present invention in this way, a plurality of vacuum processes can be simultaneously performed in a normal state at all times, and a decrease in yield can be suppressed.
[0044]
Further, as a preferred vacuum processing method of the present invention, in the step 1, when the pressure reduction rate is outside a predetermined range, the pressure reduction processing of the plurality of reaction vessel sections is stopped, and for the plurality of reaction vessel sections, The process of individually detecting an abnormal location is performed, and only the reaction vessel part in which the abnormality has occurred is disconnected from the exhaust means, and then the remaining reaction vessel parts are continuously shifted to the next step, thereby further increasing the operation rate. Can be reduced.
[0045]
As described above, when an abnormality occurs (the process is interrupted, the reaction container unit 100 is disconnected from the exhaust unit 150, and another prepared reaction container unit 100 is newly connected to the exhaust unit 150, Again, the installation is started again, and the separated reaction container 100 is moved to another area to identify the cause of the abnormality and repair the abnormality.) Is also separated from the exhaust means 150, and a certain amount of time is required to deal with the abnormality, so that the operation rate of the apparatus is reduced.
[0046]
According to the vacuum processing method of the present invention, when an abnormality is detected, a step of individually detecting an abnormal portion is performed for a plurality of reaction container portions, and only the reaction container portion where the abnormality has occurred is separated from the exhaust unit. Therefore, the normal reaction container can be used continuously, and the operation rate of the apparatus is improved. In this case, only the reaction vessel part in which the abnormality has occurred may be replaced with another reaction vessel part, and the connection part with the exhaust means to which the reaction vessel part in which the abnormality has occurred was connected may be sealed. Since the vacuum processing can be continuously performed only in the remaining normal reaction vessel section, the operation rate can be further improved.
[0047]
Further, as a preferable vacuum processing method of the present invention, when an abnormality is detected in the step 2, the decompression process of the plurality of reaction vessel sections is stopped, and the plurality of reaction vessel sections are individually abnormally treated. After performing the step of detecting the location and disconnecting only the reaction vessel part in which an abnormality has occurred from the exhaust means, the remaining reaction vessel parts are continuously shifted to the next step, so that the operation rate is the same as described above. Can be reduced.
[0048]
Further, as a preferable vacuum processing method of the present invention, in the step 1, the detection of the pressure reduction rate is performed individually and simultaneously on the plurality of reaction vessel parts, and the reaction vessel parts whose pressure reduction rate is out of a predetermined range are subjected to After disconnection from the evacuation unit, by continuing to the next step with respect to the remaining reaction vessel portions, it is possible to further suppress a decrease in the operation rate. By performing such a vacuum processing method, it is possible to simultaneously detect an abnormality and specify an abnormal location (a reaction vessel part having an abnormality), and it is possible to further improve the operation rate.
[0049]
Further, as a preferable vacuum processing method of the present invention, in the step 2, the detection of the abnormality is individually and simultaneously performed on the plurality of reaction vessel sections, and the reaction vessel section in which the abnormality has occurred is disconnected from the exhaust unit. After that, by continuing to the next step with respect to the remaining reaction vessel sections, it is possible to further suppress a decrease in the operation rate. By performing such a vacuum processing method, it is possible to simultaneously detect an abnormality and specify an abnormal location (a reaction vessel part having an abnormality), and it is possible to further improve the operation rate.
[0050]
As described above, the present invention has been described by taking the electrophotographic photoreceptor forming apparatus and the forming method as examples, but the present invention is not limited to this, and may be applied to other vacuum processing methods such as a sputtering method and a thermal CVD method. Can also be used.
[0051]
【Example】
Hereinafter, the present invention will be described in more detail with reference to Examples, but the present invention is not limited thereto.
[0052]
[Example 1]
In the vacuum processing apparatus shown in FIGS. 1 and 4, a-a cylinder is placed on a mirror-finished Al cylinder (cylindrical substrate 120) having a length of 358 mm and an outer diameter of 108 mm, which is installed in a movable reaction vessel section 100. An Si film was formed under the conditions shown in Table 1 with the oscillation frequency of the high-frequency power supply 121 set to 105 MHz, to produce an electrophotographic photosensitive member.
[0053]
1A and 1B are schematic views showing the above-described electrophotographic photoreceptor forming apparatus. FIG. 1A is a cross-sectional view, and FIG. 1B is a top view.
[0054]
FIG. 4 is a schematic diagram showing an example of an apparatus for forming an electrophotographic photosensitive member by a VHF plasma CVD method. The movable reaction vessel section 100 is provided by a movable high-frequency shield 122 made of SUS, a cylindrical reaction vessel 101 made of alumina ceramics, a reaction vessel support base 123, an upper lid 124, a gate valve 102, and a movable means 104 such as a caster. Become.
In the reaction vessel 101, three heaters 125 for heating the substrate and three source gas introduction pipes 126 are provided concentrically. Also, three SUS rod-shaped high-frequency electrodes 127 are installed concentrically at equal intervals between the high-frequency shield 122 and the reaction vessel 101, and the high-frequency power supply 121 is connected via a high-frequency matching box (matching box) 128. It is connected.
The above-mentioned rod-shaped high-frequency electrode 127 is insulated from the high-frequency shield 122 and the reaction vessel support base 123 by an insulating member 129.
[0055]
In this example, the production of the electrophotographic photosensitive member was performed as follows.
[0056]
A cylindrical substrate 120 mounted on a substrate holder 130 is set in a reaction container 101 in a substrate charging area (not shown) formed of a clean room. Next, the upper lid 124 is attached, and the reaction container unit 100 is moved to the connection mechanism 107 of the film forming stage in FIG. 1 by manual transfer by an operator, and the gate valve 102 and the connection mechanism 107 are connected. Here, the connection method was that the gate valve 102 and the connection mechanism 107 were connected via an O-ring. In the present embodiment, three reaction vessel units 100 were used as shown in FIG.
[0057]
After the connection of the three reaction container units 100 is completed, the gate valve 102 of each reaction container unit 100 is opened, the slow exhaust valve 110 is opened, and the pressure in the plurality of reaction container units 100 is reduced using the slow exhaust line 111. Start at the same time. Next, Step 1 which is a feature of the present invention was performed. As a criterion for the step 1, after 30 minutes from the opening of the slow exhaust valve 110, if the value of the internal pressure measuring device 108 was 20,000 Pa or less, there was no abnormality. In this embodiment, the value of the internal pressure measuring device 108 reached 18000 Pa 30 minutes after the slow exhaust valve 110 was opened, so that the slow exhaust was continuously performed. Next, when the value of the internal pressure measuring device 108 reached 400 Pa, the slow exhaust valve 110 was closed, the main exhaust valve 106 was opened, and the degree of vacuum in the reaction vessel was further increased. When the value of the internal pressure measuring device 108 reached 0.65 Pa, the step 2 which is a feature of the present invention was performed. When the value of the internal pressure measuring device 108 reached 0.65 Pa, the main exhaust valve 106 was closed and left for 5 minutes. When the value of the internal pressure measuring device 108 after 5 minutes was 1.3 Pa or less, no abnormality was determined, and when it was higher than 1.3 Pa, abnormality was determined. In the present embodiment, the value of the internal pressure measuring device 108 after 5 minutes was 1.0 Pa, so that the process was shifted to the next step. The main exhaust valve 106 was opened, the heater 125 for substrate heating was driven, and the cylindrical substrate 120 was heated to 230 ° C. and controlled.
[0058]
During the heating, the above-described high-frequency electrode 127, high-frequency shield 122, and high-frequency matching device 128 were installed around the reaction vessel 101, and the high-frequency matching device 128 and the high-frequency power supply 121 were connected by a coaxial cable.
[0059]
When the temperature of the cylindrical substrate 120 reaches a predetermined temperature, the source gas is introduced into the reaction vessel 101 via the source gas introduction pipe 126. After confirming that the flow rate of the raw material gas has reached the set flow rate and that the pressure in the reaction vessel 101 has been stabilized, predetermined high-frequency power is supplied from the high-frequency power supply 121 of 105 MHz to the high-frequency electrode 127 via the high-frequency matching device 128. . Table 1 shows the conditions for forming these deposited films. During the formation of the deposited film, the motor 131 was driven to rotate the cylindrical substrate 120.
[0060]
After the formation of the deposited film, the reaction container section 100 was separated from the connection mechanism 107 and moved to a cylindrical substrate take-out stage (not shown) to take out the cylindrical substrate 120 on which the deposited film was formed. Thereafter, the components in the reaction vessel 101 were replaced, and a series of steps were completed when the state in which the deposited film could be formed again was completed.
[0061]
The formation of the electrophotographic photosensitive member as described above was continuously performed 20 times.
[0062]
At this time, at the eighth time, in the above step 1, the slow exhaust valve 110 was opened, and after 30 minutes, the value of the pressure measuring device 108 was higher than 20000 Pa, so the slow exhaust valve 110 and the gate valve 102 were first opened. All three were closed at the same time, and the vacuum processing was stopped once.
Then, the internal pressure of the collective exhaust pipe 105 was adjusted to 20000 Pa by the internal pressure measuring device 108, and one gate valve 102 was opened. Then, a change in the pressure of the internal pressure measuring device 108 at that time was observed. When this inspection was performed on each of the reaction vessel parts 100, it was confirmed that, when the reaction was carried out on one of the reaction vessel parts, the pressure of the internal pressure measuring device 108 increased significantly and the reaction vessel part was abnormal. Was. Then, the reaction vessel part 100 in which the abnormality occurred was disconnected from the connection mechanism 107, and a sealing flange was attached to the connection mechanism 107 instead of the reaction vessel part 100. After that, slow exhaust was continuously performed in the remaining two reaction container sections 100. Thereafter, the above-described step 2 was performed, and an electrophotographic photosensitive member was manufactured as described above.
[0063]
In the 18th process, since the value of the internal pressure measuring device 108 after leaving for 5 minutes in vacuum in Step 2 was higher than 1.3 Pa, first, the main exhaust valve 106 and the gate valve 102 were all closed at the same time. The vacuum processing was stopped. Then, the internal pressure of the collective exhaust pipe 105 was adjusted to 1.3 Pa by the internal pressure measuring device 108, and one gate valve 102 was opened. Then, a change in the pressure of the internal pressure measuring device 108 at that time was observed. When this inspection was performed on the reaction container unit 100, it was confirmed that, when the test was performed on a certain reaction container unit, the pressure of the internal pressure measuring device increased significantly and the reaction container unit was abnormal. . Then, the reaction vessel part 100 in which the abnormality occurred was disconnected from the connection mechanism 107, and a sealing flange was attached to the connection mechanism 107 instead of the reaction vessel part 100. After that, the remaining two reactors 100 were evacuated continuously. Thereafter, an electrophotographic photosensitive member was manufactured as described above.
[0064]
Evaluations of “sensitivity”, “variation in sensitivity”, “number of spherical projections”, and “variation in number of spherical projections” were performed on the produced electrophotographic photosensitive members as follows.
[0065]
“Sensitivity” “Sensitivity variation”
The produced electrophotographic photosensitive member was installed in a Canon copier GP-605 modified for this test. A surface voltmeter set at the charger position of the electrophotographic apparatus under the conditions that the process speed is 300 mm / sec, the pre-exposure (LED with a wavelength of 680 nm), the light amount is 4 lx · s, and the image exposure (laser with a wavelength of 660 nm) is OFF. The current of the charger is adjusted by a potential sensor (TREK Model 344) so that the surface potential of the electrophotographic photosensitive member becomes 400 V. Thereafter, an image exposure is applied, the light amount of the image exposure light source is adjusted so that the surface potential becomes 50 V, and the exposure amount at that time is measured. Measurements were performed on all the produced electrophotographic photoreceptors, and the average was used as the sensitivity, and the difference between the maximum value and the minimum value was used as the sensitivity variation.
[0066]
"Number of spherical protrusions""Variation in number of spherical protrusions"
Observe the surface of the prepared electrophotographic photoreceptor with an optical microscope, ² The number of spherical protrusions having a diameter of 15 μm or more was determined. The smaller the value, the smaller the number of image defects and the higher the image quality.
[0067]
Measurements were performed on all the produced electrophotographic photoreceptors, and the average was used as the number of spherical projections, and the difference between the maximum value and the minimum value was used as the variation in the number of spherical projections.
[0068]
Relative evaluations were made on the results of Comparative Example 1 below for "sensitivity", "variation in sensitivity", "number of spherical protrusions", and "variation in number of spherical protrusions".
[0069]
[Comparative Example 1]
In this comparative example, an electrophotographic photosensitive member was produced in the same manner as in Example 1 except that Steps 1 and 2 in Example 1 were not performed, and the same evaluation was performed.
[0070]
Table 2 shows the results obtained in Example 1 and Comparative Example 1. In Table 2, relative evaluations are shown with the result of Comparative Example 1 taken as 100.
[0071]
In the comparative example, an electrophotographic photosensitive member having deteriorated sensitivity and the number of spherical protrusions was observed several times, and the photosensitive member manufactured with the same Lot as the photosensitive member had slightly deteriorated sensitivity and the number of spherical protrusions. On the other hand, according to the vacuum processing method of the present invention, an electrophotographic photoreceptor having excellent sensitivity and the number of spherical projections was produced for each Lot.
[0072]
As a result, according to the vacuum processing method of the present invention, it was found that reproducibility was improved and the yield was increased.
[0073]
[Table 1]

(Flow rate per reaction vessel)
[0074]
[Table 2]

[0075]
[Example 2]
In the vacuum processing apparatus shown in FIGS. 2 and 4, an a-Si film is formed on a mirror-finished Al cylinder (cylindrical substrate 120) having a length of 358 mm and an outer diameter of φ108 mm, which is installed in the reaction vessel unit 100. The film was formed under the conditions shown in Table 1 with the oscillation frequency of the high-frequency power supply 121 set to 105 MHz, to produce an electrophotographic photosensitive member.
[0076]
FIGS. 2A and 2B are schematic diagrams illustrating an example of an apparatus for performing the vacuum processing method of the present embodiment, and are schematic diagrams illustrating an example of an apparatus for forming an electrophotographic photosensitive member. FIG. 2A is a cross-sectional view, and FIG. 2B is a top view.
[0077]
The apparatus for manufacturing an electrophotographic photosensitive member according to the present embodiment includes movable reaction container portions 100A to 100C as shown in FIG. 2, and each of the reaction container portions 100A to 100C includes a substrate to be processed (not shown). ) Are arranged, a reaction vessel 101, gate valves 102A to 102C, a pedestal 103, and a caster as a movable means 104.
[0078]
Exhaust means 150 and 151 are provided for exhausting the inside of the reaction vessel 101. The exhaust means 150 includes a collective exhaust pipe 105 connected to the reaction vessel 101, main exhaust valves 106A to 106C, and a collective exhaust pipe 105. Connecting mechanisms 107A-C for connecting to the reaction vessels 100A-C, internal pressure measuring devices 108A-C, and exhaust conductance control means 109A-C for adjusting the pressure inside the reaction vessel 100 are connected. . The exhaust means 151 is connected to the collective exhaust pipe 140, the slow exhaust line 111, the slow exhaust valve 110, the main exhaust valve 141, and the valves 142A to 142C.
[0079]
The gas supply and flow rate control means 160 of the reaction vessel section 100 desirably includes a plurality of gas cylinders, regulators, valves, mass flow controllers, and the like required for vacuum processing. Any configuration can be used as long as it can be supplied. Further, it is more desirable to include a gas cylinder for purging and a purge line, so that the gas can be operated safely. The source gas required for the vacuum processing is supplied from the gas supply and flow control means 160 into the reaction vessel 101 via the flow rate variable valves 161A-C and the connection mechanisms 107A-C.
[0080]
In this example, the production of the electrophotographic photosensitive member was performed as follows. The reaction vessel section 100 of this embodiment is the same as that of the first embodiment, and is as shown in FIG.
[0081]
A cylindrical substrate 120 mounted on a substrate holder 130 is set in a reaction container 101 in a substrate charging area (not shown) formed of a clean room. Next, the upper cover 124 is attached, and the reaction container units 100A to 100C are moved to the connection mechanisms 107A to 107C in the film formation area in FIG. 2 by manual transfer by an operator, and the gate valves 102A to 102C are connected to the connection mechanisms 107A to 107C. Let it. Here, the connection method was that an O-ring was connected between the gate valves 102A to 102C and the connection mechanisms 107A to 107C. In the present embodiment, three reaction vessel units 100A to 100C were used as shown in FIG.
[0082]
After terminating the connection of the three reaction vessels 100A-C, the gate valves 102A-C and valves 142A-C of each reaction vessel 100A-C are opened, the slow exhaust valve 110 is opened, and the slow exhaust line 111 is used. Then, the pressure reduction in the plurality of reaction container units 100 is started at the same time. Next, Step 1 which is a feature of the present invention was performed. As a criterion in the step 1, 30 minutes after the slow exhaust valve 110 was opened, there was no abnormality if the value of each of the internal pressure measuring devices 108A to 108C was 11000 Pa or less, and there was abnormality if the pressure was higher than 11000 Pa. In this embodiment, since the values of the internal pressure measuring devices 108A to 108C reached 10000 Pa 30 minutes after the slow exhaust valve 110 was opened, slow exhaust was continuously performed. Next, when the values of the internal pressure measuring devices 108A to 108C reached 400 Pa, the slow exhaust valve 110 was closed, the main exhaust valve 141 was opened, and the degree of vacuum in the reaction vessel was further increased. When the values of the internal pressure measuring devices 108A to 108C reached 0.65 Pa, the step 2 which is a feature of the present invention was performed. When the values of the internal pressure measuring devices 108A to 108C reached 0.65 Pa, the valves 142A to 142C were closed and left for 5 minutes. When the value of each of the internal pressure measuring devices 108A to 108C after 5 minutes was 1.0 Pa or less, there was no abnormality, and when it was higher than 1.0 Pa, there was abnormality. In the present example, the values of the internal pressure measuring devices 108A to 108C after 5 minutes were 0.85 Pa, so the process was shifted to the next step. The valves 142A to 142C were opened, the substrate heating heater 125 was driven, and the cylindrical substrate 120 was heated to 280 ° C. and controlled.
[0083]
During this heating, the high-frequency electrode 127, the high-frequency shield 122, and the high-frequency matching device 128 were installed around the reaction vessel 101, and the high-frequency matching device 128 and the high-frequency power supply 127 were connected by a coaxial cable.
[0084]
When the temperature of the cylindrical substrate 120 reached a predetermined temperature, the valves 142A to 142C were closed, and all the gate valves 102A to 102C were opened. Next, the source gas is introduced into the reaction vessel 101 via the source gas introduction pipe 126. After confirming that the flow rate of the raw material gas has reached the set flow rate and that the pressure in the reaction vessel 101 has been stabilized, predetermined high-frequency power is supplied from the high-frequency power supply 121 of 105 MHz to the high-frequency electrode 127 via the high-frequency matching device 128. . Table 1 shows the conditions for forming these deposited films. During the formation of the deposited film, the motor 131 was driven to rotate the cylindrical substrate 120.
[0085]
After the formation of the deposited film, the reaction vessels 100A to 100C were separated from the connection mechanisms 107A to 107C, and moved to a cylindrical substrate take-out stage (not shown) to take out the cylindrical substrate 120 on which the deposited film was formed. Thereafter, the components in the reaction vessel 101 were replaced, and a series of steps were completed when the state in which the deposited film could be formed again was completed.
[0086]
The formation of the electrophotographic photosensitive member as described above was continuously performed 20 times.
[0087]
At this time, the third time, in the above step 1, the slow exhaust valve 110 was opened, and after 30 minutes, the pressure of the internal pressure measuring device 108A was higher than 11000 Pa. Then, the valve 142A was closed, the reaction vessel 100A was returned to the atmospheric pressure, and the reaction vessel 100A was disconnected from the connection mechanism 107A. Then, a sealing flange was attached to the disconnected connection mechanism 107A. On the other hand, when the internal pressure measuring devices 108B and 108C reach 9000 Pa, the valves 142B and 142C of the remaining two reaction container units 100B and 100C are closed, and the vacuum holding state is maintained. Thereafter, the valve 142A was opened, and when the value of the internal pressure measuring device 108A became 9000 Pa, the valves 142B and 142C were opened, and then slow exhaust was performed. Thereafter, the above-described step 2 was performed, and an electrophotographic photosensitive member was manufactured as described above.
[0088]
In addition, in Step 10 of the above, since the value of the internal pressure measuring device 108C after leaving for 5 minutes in vacuum was higher than 1.0 Pa, the reaction container 100C was returned to the atmospheric pressure and disconnected from the connection mechanism 107C. Then, a mesh flange was attached to the disconnected connection mechanism 107C. Then, the valve 142C is opened, and when the value of the internal pressure measuring device 108C becomes the same as that of the internal pressure measuring devices 108A and 108B, all the valves 142A to 142C are opened, and the process proceeds to the next step. The body was made.
[0089]
The produced electrophotographic photosensitive member was evaluated in the same manner as in Example 1. As in Example 1, the electrophotographic photosensitive member was produced with good reproducibility. Further, as compared with the first embodiment, it was found that the operation rate of the apparatus can be improved because the detection of the abnormality and the specification of the abnormal part can be performed simultaneously.
[0090]
[Example 3]
In the vacuum processing apparatus shown in FIGS. 3 and 4, an a-Si film is formed on a mirror-finished Al cylinder (cylindrical substrate 120) having a length of 358 mm and an outer diameter of φ108 mm, which is installed in the reaction vessel unit 100. The film was formed under the conditions shown in Table 1 with the oscillation frequency of the high-frequency power supply 121 set to 105 MHz, to produce an electrophotographic photosensitive member.
[0091]
FIG. 3 is a schematic view of an example of an apparatus for performing the vacuum processing method of the present embodiment, and is a schematic view showing an example of an apparatus for forming an electrophotographic photosensitive member.
[0092]
The apparatus for manufacturing an electrophotographic photoreceptor according to the present embodiment includes movable reaction container portions 100A to 100C as shown in FIG. 3, and each of the reaction container portions 100A to 100C includes a substrate to be processed (not shown). ) Are arranged, a reaction vessel 101, gate valves 102A to 102C, a pedestal 103, and a caster as a movable means 104.
[0093]
Exhaust means 150, 250, and 251 are provided for exhausting the inside of the reaction vessel 101. The exhaust means 150 includes a collective exhaust pipe 105 connected to the reaction vessel 101, a main exhaust valve 106, and a collective exhaust pipe 105. Connection mechanisms 107A to 107C to be connected to the reaction vessels 100A to 100C, an internal pressure measuring device 108, a slow exhaust line 111, and a slow exhaust valve 110 are connected.
[0094]
The exhaust means 250 includes an exhaust conductance control for adjusting the internal pressure of the collective exhaust pipe 205, the main exhaust valves 206A to 206C, the connection mechanisms 207A to 207C, the internal pressure measuring devices 208A to 208C, and the reaction vessels 100A to 100C. Means 209A to 209C are connected. The exhaust means 251 is connected to a collective exhaust pipe 240, a main exhaust valve 241, and valves 242A to 242C.
[0095]
The gas supply and flow control means 260 of the reaction container section 100 includes a plurality of gas cylinders, regulators, valves, mass flow controllers, and the like necessary for vacuum processing. The source gas required for the vacuum processing is supplied from the gas supply and flow rate control means 260 into the reaction vessel 101 via the flow rate variable valves 261A to 261C and the connection mechanisms 207A to 207C.
[0096]
In this example, the production of the electrophotographic photosensitive member was performed as follows. The reaction vessel section 100 of this embodiment is the same as that of the first embodiment, and is as shown in FIG.
[0097]
The operator manually transports and moves the reaction vessels 100A to 100C to the connection mechanisms 107A to 107C in the substrate input area formed by the clean room, and connects the gate valves 102A to 102C to the connection mechanisms 107A to 107C. Then, the cylindrical substrate 120 mounted on the substrate holder 130 is set in each reaction vessel 101. After the upper lid 124 is attached, the gate valves 102A to 102C of each of the reaction vessel parts 100A to 100C are opened, the slow exhaust valve 110 is opened, and the pressure in the plurality of reaction vessel parts 100 is simultaneously started using the slow exhaust line 111. I do. Next, Step 1 which is a feature of the present invention was performed.
[0098]
As a criterion for the step 1, after 30 minutes from the opening of the slow exhaust valve 110, if the value of the internal pressure measuring device 108 was 20,000 Pa or less, there was no abnormality. In this embodiment, after the slow exhaust valve 110 was opened, the value of the internal pressure measuring device 108 reached 18000 Pa 30 minutes after the slow exhaust valve 110 was opened. Next, when the value of the internal pressure measuring device 108 reached 400 Pa, the slow exhaust valve 110 was closed, the main exhaust valve 106 was opened, and the degree of vacuum in the reaction vessel was further increased. When the value of the internal pressure measuring device 108 reached 0.65 Pa, the step 2 which is a feature of the present invention was performed. When the value of the internal pressure measuring device 108 reached 0.65 Pa, the main exhaust valve 106 was closed and left for 5 minutes. When the value of the internal pressure measuring device 108 after 5 minutes was 1.3 Pa or less, there was no problem, and when it was higher than 1.3 Pa, it was regarded as abnormal. In the present embodiment, the value of the internal pressure measuring device 108 after 5 minutes was 1.0 Pa, so that the process was shifted to the next step.
[0099]
The gate valves 102A to 102C and the main exhaust valve 106 were closed, the leak valve 161 was opened, and the collective exhaust pipe 105 was returned to the atmospheric pressure. Thereafter, the reaction container units 100A to 100C are separated from the connection mechanisms 107A to 107C, and the reaction container units 100A to 100C are moved to the connection mechanisms 207A to 207C in the film formation area by manual conveyance by an operator, and the gate valves 102A to 102C are operated. And the connection mechanisms 207A to 207C. The valves 242A-C and the main exhaust valve 241 were opened, and the space between the gate valves 102A-C and the gate valves 206A-C was evacuated until the value of the internal pressure measuring devices 208A-C reached 0.6 Pa. Thereafter, the valves 242A to 242C were closed, and a vacuum standing test was performed for 2 minutes, and it was confirmed that there was no problem in the connection between the connection mechanisms 207A to 207C and the gate valves 102A to 102C. Then, the gate valves 102A to 102C and the valves 242A to 242C were opened, the substrate heating heater 125 was driven, and the cylindrical substrate 120 was heated to 250 ° C. and controlled.
[0100]
During this heating, the high-frequency electrode 127, the high-frequency shield 122, and the high-frequency matching device 128 were installed around the reaction vessel 101, and the high-frequency matching device 128 and the high-frequency power supply 127 were connected by a coaxial cable.
[0101]
When the temperature of the cylindrical substrate 120 reached a predetermined temperature, the valves 242A to 242C were closed, and all the gate valves 206A to 206C were opened. Next, the source gas is introduced into the reaction vessel 101 via the source gas introduction pipe 126. After confirming that the flow rate of the raw material gas has reached the set flow rate and that the pressure in the reaction vessel 101 has been stabilized, predetermined high-frequency power is supplied from the high-frequency power supply 121 of 105 MHz to the high-frequency electrode 127 via the high-frequency matching device 128. . Table 1 shows the conditions for forming these deposited films. During the formation of the deposited film, the motor 131 was driven to rotate the cylindrical substrate 120.
[0102]
After the formation of the deposited film, the reaction vessels 100A to 100C were separated from the connection mechanisms 107A to 107C, and moved to a cylindrical substrate take-out stage (not shown) to take out the cylindrical substrate 120 on which the deposited film was formed. Thereafter, the components in the reaction vessel 101 were replaced, and a series of steps were completed when the state in which the deposited film could be formed again was completed.
[0103]
The formation of the electrophotographic photosensitive member as described above was continuously performed 30 times.
[0104]
Further, in this embodiment, when it was determined that the pressure reduction rate and the vacuum standing test were abnormal, the same measures as in Examples 1 and 2 were taken, and the process was advanced.
[0105]
The produced electrophotographic photoreceptor was evaluated in the same manner as in Examples 1 and 2, and as in Examples 1 and 2, an electrophotographic photoreceptor was produced with good reproducibility.
[0106]
【The invention's effect】
As described above, according to the present invention, when performing vacuum processing on a large number of workpieces simultaneously using a plurality of reaction vessels sharing an exhaust unit and a gas supply unit, when an abnormality occurs in a certain reaction vessel In addition, by disconnecting only the reaction vessel in which this abnormality has occurred from the exhaust means, it is possible to suppress the influence on the workpiece in the reaction vessel that is normally performing vacuum processing, and to minimize the reduction in product yield. It is possible to stop it as difficult as possible.
Further, by sharing the gas supply system, it is not necessary to provide a gas supply and flow rate control means, which is an extremely complicated and expensive auxiliary equipment, for each reaction vessel, so that the equipment cost can be reduced.
[0107]
Further, according to the present invention, the reaction vessel in which an abnormality has occurred can be immediately disconnected from the exhaust means to quickly prepare for the next vacuum processing and the like, and the dead time of the production apparatus can be minimized. is there. From the above points, it is possible to supply high-quality vacuum processing at lower cost.
[Brief description of the drawings]
FIG. 1 is an example of an apparatus for performing a vacuum processing method of the present invention, and is a schematic view showing an example of an apparatus for forming an electrophotographic photosensitive member, wherein (a) is a cross-sectional view and (b) is a top view. FIG.
FIGS. 2A and 2B are schematic views showing an example of an electrophotographic photosensitive member forming apparatus according to a second embodiment of the present invention, wherein FIG. 2A is a cross-sectional view and FIG.
FIGS. 3A and 3B are schematic diagrams illustrating an example of an electrophotographic photosensitive member forming apparatus according to a third embodiment of the present invention, wherein FIG. 3A is a cross-sectional view and FIG.
FIG. 4 is a schematic diagram of an apparatus for manufacturing an electrophotographic photosensitive member using a plasma CVD method that can suitably use high-frequency power in a VHF band.
[Explanation of symbols]
100, 100A-C Reaction vessel part
101 reaction vessel
102, 102A-C Gate valve
103 stand
104 Movable means
105, 205, 140, 240 Collective exhaust piping
106, 106A-C, 206A-C Main exhaust valve
107, 107A-C, 207A-C Connection mechanism
108, 208A-C Internal pressure measuring device
109, 109A-C, 209A-C Exhaust conductance control means
110 Slow exhaust valve
111 Slow exhaust line
120 base
121 High frequency power supply
122 High frequency shield
123 Reaction vessel support base
124 top lid
125 Heater for substrate heating
126 Source gas inlet pipe
127 High frequency electrode
128 high frequency matching box
129 Insulator
130 Substrate holder
131 motor
150, 151, 250, 251 exhaust means
160, 260 Gas supply and flow control means
161, 161A-C Variable flow rate valve
141, 241, 142A-C, 242A-C, 161, 261 Valve and vacuum processing device

Claims (5)

In a vacuum processing method in which an object to be processed is installed in a plurality of reaction vessel sections that can be decompressed, and each of the reaction vessel sections is connected to a pipe connected to the same exhaust unit and evacuated, and the object to be processed is simultaneously processed. ,
When the plurality of reaction vessel sections are brought into a reduced pressure state, the plurality of reaction vessel sections are simultaneously evacuated by the exhaust means, and a decompression rate (Δpressure / Δtime) after the start of evacuation is within a predetermined range. Step 1 of determining whether
After the step 1, after further passing through the plurality of reaction vessel sections at a reduced pressure state and the step 2 of simultaneously leak-checking the plurality of reaction vessel sections when the pressure in each of the reaction vessel sections reaches a predetermined value, A vacuum processing method, wherein a predetermined vacuum processing is performed. In the step 1, when the pressure reduction rate is out of a predetermined range, a step of stopping the pressure reduction processing of the plurality of reaction vessel sections and individually detecting an abnormal portion for the plurality of reaction vessel sections is performed. 2. The vacuum processing method according to claim 1, wherein, after disconnecting only the reaction vessel part in which the abnormality has occurred from the exhaust means, the remaining reaction vessel parts are continuously shifted to the next step. In the step 2, when an abnormality is detected, the step of depressurizing the plurality of reaction container sections is stopped, and a step of individually detecting an abnormal portion is performed for the plurality of reaction container sections. 3. The vacuum processing method according to claim 1, wherein, after disconnecting only the generated reaction vessel section from the exhaust unit, the remaining reaction vessel section is continuously shifted to the next step. 4. In the step 1, the detection of the decompression rate is performed individually and simultaneously on the plurality of reaction vessel parts, and after the reaction vessel parts whose decompression rate is out of a predetermined range are disconnected from the exhaust unit, the remaining reaction vessels are removed. The vacuum processing method according to claim 1, wherein the part is continuously shifted to the next step. In the step 2, the detection of the abnormality is performed individually and simultaneously on the plurality of reaction container portions, and after the reaction container portion in which the abnormality has occurred is disconnected from the exhaust means, the remaining reaction container portions are continuously performed. The vacuum processing method according to claim 1, wherein the method proceeds to a next step.

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