JPS621873A - Washing method for deposit film-forming device - Google Patents
Washing method for deposit film-forming deviceInfo
- Publication number
- JPS621873A JPS621873A JP60140400A JP14040085A JPS621873A JP S621873 A JPS621873 A JP S621873A JP 60140400 A JP60140400 A JP 60140400A JP 14040085 A JP14040085 A JP 14040085A JP S621873 A JPS621873 A JP S621873A
- Authority
- JP
- Japan
- Prior art keywords
- deposited film
- cleaning
- gases
- washing
- gas
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Light Receiving Elements (AREA)
- Photoreceptors In Electrophotography (AREA)
- Chemical Vapour Deposition (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は堆積膜形成装置、とシわけプラズマCVD法、
グロー放電法、アーク放電法等(以下、これらを気相法
と総称する)により堆積膜を形成する装置の洗浄方法に
関する、
〔従来の技術〕
気相法によって基体上に機能性堆積膜を形成する技術は
、電子写真における光導電性部材を均一にドラム上に成
膜する場合などに既に広く採用されている。かかる気相
法による堆積膜形成に際して、反応生成物の一部が目的
とする基体以外の部分、即ち反応槽等の内壁に被膜又は
粉末として付着することは避けることができない。付着
したこれら被膜又は粉末は、剥離し易く、剥離した小片
や粉は反応槽内を飛翔して機能性堆積膜を形成すべき基
体上に付着し、これらが堆積膜にピンホール等の膜欠陥
を生ずる原因の1つとなる。[Detailed Description of the Invention] [Industrial Application Field] The present invention relates to a deposited film forming apparatus, a plasma CVD method,
[Conventional technology] Forming a functional deposited film on a substrate by a vapor phase method, regarding a cleaning method for an apparatus that forms a deposited film by a glow discharge method, an arc discharge method, etc. (hereinafter collectively referred to as a vapor phase method) This technique has already been widely used in electrophotography to uniformly form a photoconductive member on a drum. When forming a deposited film by such a vapor phase method, it is unavoidable that a part of the reaction product adheres as a film or powder to a portion other than the intended substrate, that is, to the inner wall of a reaction tank or the like. These adhered coatings or powders are easily peeled off, and the peeled off pieces and powder fly inside the reaction tank and adhere to the substrate on which the functional deposited film is to be formed, causing film defects such as pinholes in the deposited film. This is one of the causes of this.
従来、気相法によ多形成される堆積膜の例として、例え
ばシラン系化合物を用いてプラズマ反応によ多形成され
る、ケイ素原子を主成分とする光導電性部材用の堆積膜
がある。この堆積膜を形成した反応槽内には、基体以外
の部分にシランの重複合物(/リシランと呼ばれている
)が副生じ、これを洗浄除去する方法として、従来例え
ばCF4と02の混合ガスを用いてプラズマ反応により
洗浄する方法が用いられている。この方法により、堆積
膜形成と洗浄とを交互に行なうことにより、生産能率を
挙げることができる。Conventionally, as an example of a deposited film formed by a vapor phase method, there is a deposited film for a photoconductive member whose main component is silicon atoms, which is formed by a plasma reaction using a silane compound. . In the reaction tank in which this deposited film was formed, a heavy composite of silane (called /resilane) was generated as a by-product in parts other than the substrate, and conventional methods for cleaning and removing this were, for example, a mixture of CF4 and 02. A method of cleaning by plasma reaction using gas is used. With this method, production efficiency can be increased by alternately performing deposited film formation and cleaning.
しかしながら、述上の方法によりポリシランが取除かれ
るが、これによ、9810.が残渣として残シ、また0
2.1分子等が吸着物として残留し、次回の堆積膜形成
時に堆積膜中にとシ込まれ、例えば光背電性部材として
の使用特性劣化(帯電能の低下、画像流れ等)、乃至は
光導電特性劣化〔光導電率(σph)/暗導電率(σ、
)の低下、モビリティ−の低下〕の原因となる。However, the method described above removes the polysilane, which results in 9810. remains as a residue, and 0
2.1 molecules, etc. remain as adsorbents and are injected into the deposited film during the next deposited film formation, resulting in, for example, deterioration of the characteristics of use as a photobackable member (decrease in charging ability, image blurring, etc.), or Deterioration of photoconductive properties [photoconductivity (σph)/dark conductivity (σ,
) and mobility.
従って、前述した堆積膜形成と洗浄を繰返しサイクルで
行なりと、次第に特性劣化が嵩じ、比較的短期間で製品
としての品質許容限度を逸脱してしまう。従ってこれ迄
は、数サイクル毎に、前記洗浄のほかに反応槽分解清掃
作業が必要となシ、生産性の低下を招いた。Therefore, if the above-mentioned deposited film formation and cleaning are repeated in cycles, the characteristics gradually deteriorate, and the product quality exceeds the allowable limit in a relatively short period of time. Therefore, until now, in addition to the above-mentioned cleaning, it has been necessary to disassemble and clean the reaction tank every few cycles, resulting in a decrease in productivity.
本発明は、従来の問題点を解決し、気相法により堆積膜
を形成する反応槽内を効率よく洗浄することができ、且
つ形成される堆積膜の品質を高水準に維持することので
きる堆積膜形成装置の洗浄方法を提供すべくなされたも
のである。The present invention solves the conventional problems, makes it possible to efficiently clean the inside of a reaction tank in which a deposited film is formed by a vapor phase method, and maintains the quality of the deposited film formed at a high level. This invention was made to provide a method for cleaning a deposited film forming apparatus.
上記問題点を解決する手段として見出された本発明の堆
積膜形成装置の洗浄方法は、気相法により堆積膜を形成
するための反応槽内を気相を含む反応により洗浄する方
法において、それぞれ反応性の異なる複数の気体を用い
て複数回の反応操作を行なうことを特徴とするものであ
る。The method for cleaning a deposited film forming apparatus of the present invention, which was discovered as a means to solve the above problems, is a method for cleaning the inside of a reaction tank by a reaction including a gas phase for forming a deposited film by a gas phase method. This method is characterized by performing multiple reaction operations using multiple gases each having a different reactivity.
本発明の洗浄方法において使用する前記気体は、洗浄除
去対象となる物質との反応性、洗浄用気体同志の反応性
等を考慮して適宜組合せることができるが、同時に、気
相反応後の反応槽内への残留性、乃至は残留した場合の
堆積膜への影響等を総合的に判断する必要がある。The gases used in the cleaning method of the present invention can be appropriately combined in consideration of the reactivity with the substance to be cleaned and the reactivity of the cleaning gases, etc. It is necessary to comprehensively judge whether the substance remains in the reaction tank or, if it remains, the influence on the deposited film.
具体的には、例えば前述したプラズマ反応により形成さ
れるケイ素原子を主成分とする光導電性部材用の堆積膜
を形成する場合に副生するシランの重複合物を洗浄除去
対象とする場合、プラズマ反応による第1回目の反応操
作には、前述したCF4と02の混合ガスを選択するの
が好ましい。フッ化アンモニウム等を用いることも知ら
れているが、反応進行中に反応槽内壁面に5INxが生
成、付着し、被洗浄面を覆い、洗浄能率を低下させる。Specifically, for example, when cleaning and removing a heavy composite of silane that is produced as a by-product when forming a deposited film for a photoconductive member mainly composed of silicon atoms formed by the above-mentioned plasma reaction, For the first reaction operation using plasma reaction, it is preferable to select the above-mentioned mixed gas of CF4 and 02. Although it is known to use ammonium fluoride or the like, 5INx is generated and adheres to the inner wall surface of the reaction tank during the progress of the reaction, covers the surface to be cleaned, and reduces the cleaning efficiency.
この様な選択を行なった場合、第2回目以降の反応操作
には、8102等の固体残渣や0□、1分子等の吸着物
と気相反応を起して反応槽内に残留することのない化合
物を生成し得る気体を選択するのは勿論であるが、併せ
て洗浄用気体自体が残留した場合の、次回の堆積膜形成
への影響をも考慮して選択する必要がある。そこで、第
2回目以降の洗浄操作に使用する気体としては、例えば
CF4とH2の混合ガス、ArとH2の混合ガス等を選
択するのが好ましい。場合によっては、これらの気体を
用いて複数の反応操作を行なうことができ、例えばCF
4とH2の混合がスを用いる洗浄操作と、ArとH2の
混合ガスを用いる洗浄操作とを相前後して行なうことが
できる。このうち、第2回目にCF4とH2の混合がス
、第3回目にArとH2の混合ガスを用いて洗浄を行な
うのが、特に望ましい。If such a selection is made, in the second and subsequent reaction operations, it is necessary to prevent gas phase reactions from occurring with solid residues such as 8102 and adsorbates such as 0□, 1 molecule, etc., and remaining in the reaction tank. Of course, it is necessary to select a gas that can generate a compound that is not present, but it is also necessary to select a gas that takes into account the effect on the next deposited film formation if the cleaning gas itself remains. Therefore, as the gas used for the second and subsequent cleaning operations, it is preferable to select, for example, a mixed gas of CF4 and H2, a mixed gas of Ar and H2, or the like. In some cases, multiple reaction operations can be performed using these gases, e.g.
A cleaning operation using a mixed gas of Ar and H2 and a cleaning operation using a mixed gas of Ar and H2 can be performed one after the other. Of these, it is particularly desirable to use a mixed gas of CF4 and H2 for the second cleaning, and to use a mixed gas of Ar and H2 for the third cleaning.
以下、本発明の効果を実証するための具体的実施例を説
明する。Hereinafter, specific examples for demonstrating the effects of the present invention will be described.
実施例1、比較例1
第1図に示した装置を用い、プラズマCVD法により、
下記作製条件により光導電性部材用堆積膜を形成し、こ
れと併せて下記洗浄条件により本発明方法を実施し、反
応槽内をプラズマ反応によυ洗浄し、堆積膜形成と洗浄
とを連続して繰返し行なったO
〔炸裂条件〕
堆積膜の積層順序 使用原料ガス 膜厚(μm)電
荷注入阻止層 SiH4、B2H60,6光導電層
S lH420
表面保護層 SiH4、C2H40,1基体(ア
ルミニウムシリンダー)5の温度:250M5℃に制御
堆積膜形成時の堆積室内内圧: 0.3 Torr放電
周波数: 13.56 MH嶌
堆積膜形成速度: 20 i/sec
放電電カニ 0.18 W/crtt”がス流速: 2
00 m/畠
ガス流量:電荷注入阻止層 5iH4200SCCMB
2H65IH4に対し200ppm
光導電層 5iH4200SCCM表面保護層
5iH410SCCMCH4200SCCM
〔洗浄条件〕
実施例1:第1回目 CF4(流量1000 SCCM
)と02(流量200SCCM)
の混合ガス、
第2回目 CF4(流量500SCCM)とH2(流量
101005CC
の混合ガス。Example 1, Comparative Example 1 Using the apparatus shown in FIG. 1, by plasma CVD method,
A deposited film for a photoconductive member is formed under the following production conditions, and in conjunction with this, the method of the present invention is carried out under the following cleaning conditions, the inside of the reaction tank is cleaned by plasma reaction, and deposited film formation and cleaning are performed continuously. [Explosion conditions] Lamination order of deposited film Raw material gas used Film thickness (μm) Charge injection blocking layer SiH4, B2H60,6 photoconductive layer S lH420 Surface protective layer SiH4, C2H40,1 substrate (aluminum cylinder) Temperature of 5: Control at 250M5℃ Internal pressure in deposition chamber during deposited film formation: 0.3 Torr Discharge frequency: 13.56 MH deposited film formation rate: 20 i/sec Discharge electric crab 0.18 W/crtt" Flow rate: 2
00 m/Hata Gas flow rate: Charge injection blocking layer 5iH4200SCCMB
200ppm for 2H65IH4 Photoconductive layer 5iH4200SCCM surface protective layer
5iH410SCCMCH4200SCCM [Cleaning conditions] Example 1: First CF4 (flow rate 1000 SCCM
) and 02 (flow rate 200SCCM), 2nd time CF4 (flow rate 500SCCM) and H2 (flow rate 101005CC gas mixture).
比較例1:実施例工の第1回目のみ。Comparative Example 1: Only the first run of the example process.
かくして、堆積膜形成と洗浄とをそれぞれ20サイクル
繰返した後の光導電部材の帯電能(初期帯電能を1.0
とした場合の比率)、及び画像ぎケの評価(画像状態の
優良なものをAとし、A、B。In this way, the charging ability of the photoconductive member after repeating 20 cycles of deposited film formation and cleaning (initial charging ability of 1.0
Ratio), and evaluation of image sharpness (A indicates excellent image condition; A, B).
C,D、Eの5段階で評価)を行なった。結果を第1表
に示した。Evaluation was made on a 5-grade scale of C, D, and E. The results are shown in Table 1.
第 1 表
第1表から、本発明方法により洗浄を行なうことにより
、堆積膜特性の変動がなく、品質の再現性が維持される
。Table 1 From Table 1, it can be seen that by cleaning according to the method of the present invention, there is no change in the characteristics of the deposited film and the reproducibility of quality is maintained.
実施例2〜5、比較例2
第2表に示した洗浄条件により、実施例1と同様に堆積
膜形成と洗浄とを20サイクル連続して繰返し、20サ
イクル後に得られた光導電性部材の特性を評価した。結
果を第2表に示した。Examples 2 to 5, Comparative Example 2 Under the cleaning conditions shown in Table 2, deposited film formation and cleaning were repeated 20 times in a row in the same manner as in Example 1. After 20 cycles, the resulting photoconductive member Characteristics were evaluated. The results are shown in Table 2.
第2表からも分る様に、本発明方法により、堆積膜特性
が安定し、膜中へのコンタミネーションを防止し、均一
な成膜が行なえるため、高水準の品質を維持することが
でき、しかも反応槽の分解清浄等を必要としない。As can be seen from Table 2, the method of the present invention stabilizes the characteristics of the deposited film, prevents contamination into the film, and allows uniform film formation, making it possible to maintain a high level of quality. Moreover, it does not require decomposition and cleaning of the reaction tank.
本発明によれば、気相法により堆積膜を形成する反応槽
内を効率よく洗浄することができ、且つ形成される堆積
膜の品質を高水準に維持することができる。According to the present invention, the interior of a reaction tank in which a deposited film is formed by a vapor phase method can be efficiently cleaned, and the quality of the deposited film formed can be maintained at a high level.
第1図は本発明に用いることのできる堆積膜形成装置の
構成を示した模式図である。
1・・・灰石槽容器、3・・・容器底板、4・・・基体
受は台、5・・・円筒状導電性基体、6・・・上蓋又は
グー)、8.8・・・ガス導入管、9,9.9・・・ガ
ス導入孔、12・・・高周波マツチングデックス、13
・・・ガス排気管・、14・・・抵抗発熱体。
代理人 弁理士 山 下 積 平
第1図FIG. 1 is a schematic diagram showing the configuration of a deposited film forming apparatus that can be used in the present invention. DESCRIPTION OF SYMBOLS 1... Ashstone tank container, 3... Container bottom plate, 4... Base support is a stand, 5... Cylindrical conductive base, 6... Top lid or goo), 8.8... Gas introduction pipe, 9, 9.9...Gas introduction hole, 12...High frequency matching index, 13
...Gas exhaust pipe...14...Resistance heating element. Agent Patent Attorney Sekihei Yamashita Figure 1
Claims (1)
含む反応により洗浄する方法において、それぞれ反応性
の異なる複数の気体を用いて複数回の反応操作を行なう
ことを特徴とする堆積膜形成装置の洗浄方法。In a method of cleaning the inside of a reaction tank by a reaction involving a gas phase for forming a deposited film by a gas phase method, a deposition method is characterized in that reaction operations are performed multiple times using multiple gases each having a different reactivity. Method for cleaning film forming equipment.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP60140400A JPS621873A (en) | 1985-06-28 | 1985-06-28 | Washing method for deposit film-forming device |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP60140400A JPS621873A (en) | 1985-06-28 | 1985-06-28 | Washing method for deposit film-forming device |
Publications (1)
Publication Number | Publication Date |
---|---|
JPS621873A true JPS621873A (en) | 1987-01-07 |
Family
ID=15267899
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP60140400A Pending JPS621873A (en) | 1985-06-28 | 1985-06-28 | Washing method for deposit film-forming device |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPS621873A (en) |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH03153485A (en) * | 1989-11-08 | 1991-07-01 | Yoshigai Kikai Kinzoku Kk | Braking device for two wheeler |
US5064027A (en) * | 1989-10-23 | 1991-11-12 | Maeda Industries, Ltd. | Brake shoe for bicycles |
DE4417205A1 (en) * | 1993-05-18 | 1994-11-24 | Mitsubishi Electric Corp | Production instrument for semiconductor devices and cleaning method for the instrument |
US5655630A (en) * | 1994-08-24 | 1997-08-12 | Shimano, Inc. | Bicycle brake device |
EP0940333A2 (en) | 1998-03-02 | 1999-09-08 | Shimano Industrial Co., Ltd. | Bicycle brake device |
-
1985
- 1985-06-28 JP JP60140400A patent/JPS621873A/en active Pending
Cited By (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5064027A (en) * | 1989-10-23 | 1991-11-12 | Maeda Industries, Ltd. | Brake shoe for bicycles |
JPH03153485A (en) * | 1989-11-08 | 1991-07-01 | Yoshigai Kikai Kinzoku Kk | Braking device for two wheeler |
DE4417205A1 (en) * | 1993-05-18 | 1994-11-24 | Mitsubishi Electric Corp | Production instrument for semiconductor devices and cleaning method for the instrument |
US5584963A (en) * | 1993-05-18 | 1996-12-17 | Mitsubishi Denki Kabushiki Kaisha | Semiconductor device manufacturing apparatus and cleaning method for the apparatus |
DE4417205C2 (en) * | 1993-05-18 | 1998-10-08 | Mitsubishi Electric Corp | Manufacturing device for semiconductor devices and cleaning method for the device |
US5655630A (en) * | 1994-08-24 | 1997-08-12 | Shimano, Inc. | Bicycle brake device |
EP0940333A2 (en) | 1998-03-02 | 1999-09-08 | Shimano Industrial Co., Ltd. | Bicycle brake device |
US6003638A (en) * | 1998-03-02 | 1999-12-21 | Shimano Inc. | Bicycle brake device |
US6089356A (en) * | 1998-03-02 | 2000-07-18 | Shimano Inc. | Bicycle brake device |
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