JPH05281755A - Method for washing base body - Google Patents
Method for washing base bodyInfo
- Publication number
- JPH05281755A JPH05281755A JP7722792A JP7722792A JPH05281755A JP H05281755 A JPH05281755 A JP H05281755A JP 7722792 A JP7722792 A JP 7722792A JP 7722792 A JP7722792 A JP 7722792A JP H05281755 A JPH05281755 A JP H05281755A
- Authority
- JP
- Japan
- Prior art keywords
- base body
- cleaning
- washing
- substrate
- methylene chloride
- 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
- Photoreceptors In Electrophotography (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は表面に鏡面が要求される
基体の洗浄方法に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for cleaning a substrate which requires a mirror surface on its surface.
【０００２】[0002]
【従来の技術】近時、成膜用の表面に厳しい鏡面が要求
される技術分野が出てきており、例えば、アモルファス
シリコンから成る電子写真感光体においては、その被成
膜面の平滑性を高めるとともに、その面の脱脂のために
洗浄剤をスプレーするという液噴射洗浄が行われてい
る。一般的には、この液噴射洗浄は、被洗浄用基体の溝
や窪み等が形成されている場合、もしくはブラシスクラ
ビング等の接触洗浄法を用いることができない場合に有
効である。2. Description of the Related Art Recently, a technical field in which a strict mirror surface is required for a film-forming surface is emerging. For example, in an electrophotographic photosensitive member made of amorphous silicon, the smoothness of the film-forming surface is required. Liquid jet cleaning is performed in which the cleaning agent is sprayed to degrease the surface as well as to raise the surface. Generally, this liquid jet cleaning is effective when the substrate to be cleaned has grooves or depressions formed therein or when a contact cleaning method such as brush scrubbing cannot be used.
【０００３】[0003]
【発明は解決しようとする問題点】この液噴射洗浄にお
いては、その洗浄剤として塩化メチレンが用いられてお
り、そのままで塩化メチレンが使用されると、光、熱、
水分、金属粉、溶解物等の存在下で酸化熱分解、加水分
解等の劣化をおこし、安定性に問題がある。この問題点
に対してメタノール、エタノール、プロパノール等の低
級アルコールが添加されるが、これらが添加された塩化
メチレンで液噴射洗浄を行った場合、その洗浄直後もし
くは乾燥後にしみ（液だれの輪郭に青白く残渣がある状
態）が基体の表面に発生するという問題点がある。DISCLOSURE OF THE INVENTION Problems to be Solved by the Invention In this liquid jet cleaning, methylene chloride is used as a cleaning agent. If methylene chloride is used as it is, light, heat,
In the presence of water, metal powder, dissolved substances, etc., deterioration due to oxidative thermal decomposition, hydrolysis, etc. occurs and there is a problem in stability. To this problem, lower alcohols such as methanol, ethanol and propanol are added, but when liquid jet cleaning is performed with methylene chloride to which these are added, stains (immediately after the cleaning or after drying, There is a problem in that a bluish-white residue exists on the surface of the substrate.
【０００４】[0004]
【問題点を解決するための手段】本発明の基体洗浄方法
は、気化熱が１３０ｃａｌ／ｇ以下のエーテル類が添加
された塩化メチレンを含有する洗浄剤を被洗浄用基体に
対して液噴射（スプレー）させて該被洗浄用基体の表面
を洗浄することを特徴とする。In the substrate cleaning method of the present invention, a cleaning agent containing methylene chloride to which ethers having a heat of vaporization of 130 cal / g or less is added is sprayed onto a substrate to be cleaned ( The surface of the substrate to be cleaned is cleaned by spraying.
【０００５】上記エーテル類には例えばジエチルエーテ
ル、エチルエーテル、プロピレンオキシド、エチレンオ
キシド、１，４−ジオキサンなどがあり、これらのエー
テルの気化熱は１３０ｃａｌ／ｇ以下と小さく、これに
より、液噴射後に被洗浄用基体の表面に残留せず、更に
塩化メチレンの蒸発後でも、その表面に残留せず、その
結果、被洗浄用基体の表面にしみが発生しない。このエ
ーテルの気化熱は好ましくは１００ｃａｌ／ｇ以下がよ
い。因みにジエチルエーテルの気化熱は８４ｃａｌ／
ｇ、エチルエーテルの気化熱は９３．５ｃａｌ／ｇ、
１，４−ジオキサンの気化熱は９８．６ｃａｌ／ｇ、プ
ロピレンオキシドの気化熱は８９ｃａｌ／ｇであり、こ
れに対比してｎ−プロピレンアルコールの気化熱は１６
３ｃａｌ／ｇ、エチルアルコールの気化熱は２００ｃａ
ｌ／ｇ、メチルアルコールの気化熱は２６３ｃａｌ／ｇ
である。The above ethers include, for example, diethyl ether, ethyl ether, propylene oxide, ethylene oxide, 1,4-dioxane, etc., and the heat of vaporization of these ethers is as small as 130 cal / g or less. It does not remain on the surface of the substrate for cleaning, and does not remain on the surface even after evaporation of methylene chloride, and as a result, stains do not occur on the surface of the substrate for cleaning. The heat of vaporization of this ether is preferably 100 cal / g or less. By the way, the heat of vaporization of diethyl ether is 84 cal /
g, the heat of vaporization of ethyl ether is 93.5 cal / g,
The heat of vaporization of 1,4-dioxane is 98.6 cal / g, and the heat of vaporization of propylene oxide is 89 cal / g. In contrast, the heat of vaporization of n-propylene alcohol is 16
3cal / g, heat of vaporization of ethyl alcohol is 200ca
1 / g, the heat of vaporization of methyl alcohol is 263 cal / g
Is.
【０００６】また、上記の目的を達成するためには、エ
ーテル類の添加量を少なくとも０．０１重量％とし、更
には０．０１〜５重量％、好適には０．０１〜２重量％
がよい。To achieve the above object, the amount of ethers added is at least 0.01% by weight, more preferably 0.01 to 5% by weight, and preferably 0.01 to 2% by weight.
Is good.
【０００７】[0007]
【実施例】以下、本発明の実施例をアモルファスシリコ
ンから成る電子写真感光体の成膜用基体の表面を洗浄す
る場合を例にとって詳述する。Embodiments of the present invention will be described in detail below by taking as an example the case of cleaning the surface of a film-forming substrate of an electrophotographic photosensitive member made of amorphous silicon.
【０００８】図１はこの成膜用基体の洗浄を示す説明図
である。FIG. 1 is an explanatory view showing the cleaning of the film-forming substrate.
【０００９】同図において、１は円筒形状の成膜用基
体、２は洗浄器であり、この洗浄器２は基体１の内面を
洗浄するための内面ノズル３と基体１の外面を洗浄する
ための外面ノズル４とからなり、これらのノズル３、４
が一体化されて洗浄器２は回転しながら基体１に入り、
これらノズル３、４から上述した洗浄剤が噴出して、こ
の基体１の内面と外面とが同時に洗浄される。また、５
は洗浄室、６と７はポンプ、８はフィルター、９は使用
洗浄液タンクであり、洗浄室５における液噴射洗浄が行
われた後には、使用洗浄液タンク９に入り、その後ポン
プ６とフィルター８にてろ過する。このろ過された洗浄
液をタンク１０に貯蔵し、そして、その洗浄液をポンプ
７にて内面・外面ノズル３、４へ送られる。In the figure, 1 is a cylindrical film forming substrate, 2 is a cleaning device, and this cleaning device 2 is for cleaning the inner surface nozzle 3 for cleaning the inner surface of the substrate 1 and the outer surface of the substrate 1. And the outer surface nozzle 4 of
Are integrated, the washer 2 enters the base 1 while rotating,
The above-mentioned cleaning agent is jetted from these nozzles 3 and 4, and the inner surface and the outer surface of the substrate 1 are simultaneously cleaned. Also, 5
Is a cleaning chamber, 6 and 7 are pumps, 8 is a filter, and 9 is a cleaning liquid tank used. After the liquid jet cleaning in the cleaning chamber 5, the cleaning liquid tank 9 is used, and then the pump 6 and the filter 8 are connected. And filter. The filtered cleaning liquid is stored in the tank 10, and the cleaning liquid is sent to the inner and outer surface nozzles 3 and 4 by the pump 7.
【００１０】本例によれば、上記円筒形状の成膜用基体
１は、電子写真感光体の製作工程中、次の段階で液噴射
洗浄が行われる。According to this example, the cylindrical film-forming substrate 1 is subjected to liquid jet cleaning at the next stage in the process of manufacturing the electrophotographic photosensitive member.
【００１１】この液噴射洗浄には高圧スプレーと低圧ス
プレーとの２種類があり、前者の高圧スプレーは次のよ
うに使用される。即ち、感光体用の成膜用基体は先ず切
削加工によりその基体の表面を精密仕上げを行うが、そ
の切削加工により基体表面には切粉、オイルミスト等が
付着したり、また微小なバリが発生しており、その除去
には浸漬超音波洗浄を行う。しかし、その浸漬超音波洗
浄で除去できない一部の切粉やバリの除去には高圧スプ
レー洗浄を行う。There are two types of liquid jet cleaning, high pressure spray and low pressure spray, and the former high pressure spray is used as follows. That is, the film-forming substrate for the photoconductor is first subjected to a cutting process to precisely finish the surface of the substrate. It has been generated, and immersion ultrasonic cleaning is performed to remove it. However, high pressure spray cleaning is used to remove some chips and burrs that cannot be removed by the immersion ultrasonic cleaning.
【００１２】また、低圧スプレーについては、上記の浸
漬超音波洗浄を行うと、その浸漬洗浄後の引き上げ時に
液中の異物が同時に基体表面に付着するために、その付
着物を除去するために行う。本発明者はこの異物を未だ
十分に解明している訳ではないが、油分、水分、有機物
等であると推測する。With respect to the low-pressure spray, when the above-mentioned immersion ultrasonic cleaning is carried out, foreign substances in the liquid are simultaneously adhered to the surface of the substrate at the time of pulling up after the immersion cleaning, so that the adhered substances are removed. . Although the present inventor has not fully clarified this foreign substance, it is presumed to be oil, water, organic matter and the like.
【００１３】かくして感光体用の成膜用基体は、切削加
工、浸漬超音波洗浄、低圧スプレー、高圧スプレーを順
次行った後に蒸気乾燥を行い、アモルファスシリコン膜
の成膜に供される。この蒸気乾燥は、液噴射洗浄にて使
用した洗浄液と同一の塩化メチレン蒸気を用いて、８ｍ
ｍ／秒の速度で引き上げることにより行う。Thus, the film-forming substrate for the photoconductor is subjected to cutting, immersion ultrasonic cleaning, low-pressure spraying and high-pressure spraying in sequence, and then steam-dried to be used for forming an amorphous silicon film. This vapor drying is performed using the same methylene chloride vapor as the cleaning liquid used for liquid jet cleaning,
It is performed by pulling up at a speed of m / sec.
【００１４】上記構成の基体洗浄方法においては、高圧
スプレーと低圧スプレーの各液噴射洗浄に用いる洗浄剤
には、気化熱が１３０ｃａｌ／ｇ以下のエーテル類が添
加された塩化メチレンを用いており、これにより、液噴
射後に基体の表面に残留せず、更に塩化メチレンの蒸発
後でも、その表面に残留せず、その結果、被洗浄用基体
の表面にしみが発生しないことが判った。この結果は次
に述べる実験例からも明らかである。In the method of cleaning a substrate having the above-mentioned structure, methylene chloride to which ethers having a heat of vaporization of 130 cal / g or less is added is used as the cleaning agent used for the high pressure spray and the low pressure spray. As a result, it was found that after spraying the liquid, it did not remain on the surface of the substrate, and even after evaporation of methylene chloride, it did not remain on the surface, and as a result, no stain was generated on the surface of the substrate to be cleaned. This result is also clear from the experimental example described below.
【００１５】（実験例）円筒形状の成膜用基体１には、
Φ１０８ｍｍ×３５８ｍｍの寸法のアルミニウム製を用
いて、その内外周面にスプレーするノズル３、４の径は
３ｍｍΦであり、そのノズル３、４より塩化メチレンの
添加剤を７種類にも変えて、それぞれ１５リットル／分
の流速にて３０秒噴射させて洗浄を行った。その後のし
みの発生状態を目視により観察し、更にその後塩化メチ
レンによる蒸気乾燥を行って、そのしみの発生状態も目
視により観察した。これらの結果は表１に示す通りであ
る。同表にて、×はしみが確認された場合であり、○は
しみが確認されなかった場合である。Experimental Example The cylindrical film-forming substrate 1 was
The diameter of the nozzles 3 and 4 for spraying on the inner and outer peripheral surfaces is 3 mmΦ using aluminum made of aluminum having a size of 108 mm × 358 mm, and the methylene chloride additive is changed to 7 kinds from the nozzles 3 and 4, respectively. Cleaning was performed by jetting for 30 seconds at a flow rate of 15 liters / minute. After that, the generation state of stains was visually observed, and then steam drying with methylene chloride was performed, and the generation state of the stains was also visually observed. The results are shown in Table 1. In the same table, x indicates that stains were confirmed, and ○ indicates that stains were not confirmed.
【００１６】[0016]
【表１】 [Table 1]
【００１７】この結果から明らかなように、（例２）、
（例３）、（例６）はいずれも添加剤の気化熱が１３０
ｃａｌ／ｇ以下のエーテル類であり、スプレー後及び蒸
気乾燥後でしみの発生が認められなかった。尚、（例
６）では液中水分が３００ｐｐｍ以上になるとスプレー
後、水分によるしみが発生したが、これも蒸気乾燥後で
しみの発生が認められなかった。As is clear from this result, (Example 2),
In both (Example 3) and (Example 6), the heat of vaporization of the additive was 130.
It was an ether of cal / g or less, and no stain was observed after spraying and after steam drying. In (Example 6), when the water content in the liquid was 300 ppm or more, stains due to water were generated after spraying, but no stain was observed after steam drying.
【００１８】これに対して、（例１）、（例４）、（例
５）、（例７）はいずれもスプレー後及び蒸気乾燥後
で、液だれの輪郭に青白く残渣がある状態が認められ
た。尚、（例４）、（例５）、（例７）ではエーテル類
とアルコール類との組合せであるが、メチルアルコール
を含み、その気化熱は２６３ｃａｌ／ｇである。On the other hand, in each of (Example 1), (Example 4), (Example 5) and (Example 7), after spraying and after steam drying, it was recognized that the outline of the dripping had a pale residue. Was given. In addition, in (Example 4), (Example 5), and (Example 7), a combination of ethers and alcohols is included, but methyl alcohol is included, and the heat of vaporization is 263 cal / g.
【００１９】[0019]
【発明の効果】以上のように、本発明の基体洗浄方法
は、気化熱が１３０ｃａｌ／ｇ以下のエーテル類が添加
された塩化メチレンを含有する洗浄剤を被洗浄用基体に
対して液噴射（スプレー）させて洗浄しており、これに
より、液噴射後に被洗浄用基体の表面に残留せず、更に
塩化メチレンの蒸発後でも、その表面に残留せず、その
結果、被洗浄用基体の表面にしみが発生しなくなり、高
い品質の成膜製品やガラスレンズ、ウエハー、ポリゴン
ミラー等が提供できる。As described above, according to the method of cleaning a substrate of the present invention, a cleaning agent containing methylene chloride to which ethers having a heat of vaporization of 130 cal / g or less is added is sprayed onto a substrate to be cleaned ( It is sprayed and washed so that it does not remain on the surface of the substrate to be cleaned after liquid injection, and does not remain on the surface even after evaporation of methylene chloride, and as a result, the surface of the substrate to be cleaned. It is possible to provide high-quality film-formed products, glass lenses, wafers, polygon mirrors, etc., without causing stains.
【図１】実施例における基体の洗浄を示す説明図であ
る。FIG. 1 is an explanatory diagram showing cleaning of a substrate in an example.
１・・・成膜用基体 ２・・・洗浄器 ３・・・内面ノズル ４・・・外面ノズル 1 ... Film forming substrate 2 ... Cleaning device 3 ... Inner surface nozzle 4 ... Outer surface nozzle
Claims (1)
類が添加された塩化メチレンを含有する洗浄剤を被洗浄
用基体に対して液噴射させ、該被洗浄用基体の表面を洗
浄することを特徴とする基体洗浄方法。1. A cleaning agent containing methylene chloride to which ethers having a heat of vaporization of 130 cal / g or less is sprayed onto a substrate to be cleaned to clean the surface of the substrate to be cleaned. A method for cleaning a substrate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7722792A JPH05281755A (en) | 1992-03-31 | 1992-03-31 | Method for washing base body |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7722792A JPH05281755A (en) | 1992-03-31 | 1992-03-31 | Method for washing base body |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH05281755A true JPH05281755A (en) | 1993-10-29 |
Family
ID=13627972
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP7722792A Pending JPH05281755A (en) | 1992-03-31 | 1992-03-31 | Method for washing base body |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH05281755A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08232089A (en) * | 1995-01-10 | 1996-09-10 | Elf Atochem Sa | Composition mainly comprising stabilized methylene chloride and usable for degreasing metal |
| US6277203B1 (en) | 1998-09-29 | 2001-08-21 | Lam Research Corporation | Method and apparatus for cleaning low K dielectric and metal wafer surfaces |
-
1992
- 1992-03-31 JP JP7722792A patent/JPH05281755A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08232089A (en) * | 1995-01-10 | 1996-09-10 | Elf Atochem Sa | Composition mainly comprising stabilized methylene chloride and usable for degreasing metal |
| JP2955225B2 (en) * | 1995-01-10 | 1999-10-04 | エルフ・アトケム・エス・アー | A stabilized methylene chloride-based composition that can be used for degreasing metals |
| US6277203B1 (en) | 1998-09-29 | 2001-08-21 | Lam Research Corporation | Method and apparatus for cleaning low K dielectric and metal wafer surfaces |
| US6319330B1 (en) | 1998-09-29 | 2001-11-20 | Lam Research Corporation | Method and apparatus for cleaning low K dielectric and metal wafer surfaces |
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