JP3685436B2 - Method for producing electrophotographic photosensitive member, method for forming coating film, and coating solution - Google Patents
Method for producing electrophotographic photosensitive member, method for forming coating film, and coating solution Download PDFInfo
- Publication number
- JP3685436B2 JP3685436B2 JP00623098A JP623098A JP3685436B2 JP 3685436 B2 JP3685436 B2 JP 3685436B2 JP 00623098 A JP00623098 A JP 00623098A JP 623098 A JP623098 A JP 623098A JP 3685436 B2 JP3685436 B2 JP 3685436B2
- Authority
- JP
- Japan
- Prior art keywords
- coating
- alcohol
- organic compound
- coating film
- coating solution
- 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.)
- Expired - Lifetime
Links
Description
【０００１】
【発明の属する技術分野】
本発明は、塗布膜の形成方法及び電子写真感光体の製造方法に関するものである。詳しくは、特定の塗布液を施すことを特徴とする塗膜の形成方法及び特定の下引き塗布液を施すことを特徴とする電子写真感光体の製造方法に関するものである。
【０００２】
【従来の技術】
アルコール可溶性樹脂を含有する塗布膜を形成する方法は、アルコールのみに可溶する樹脂の場合は、当然溶媒としてアルコールを主とする溶媒が用いられるが、アルコール以外の溶媒にも溶解する樹脂についても、コスト及び安全性、更に特性向上のために、金属酸化物粒子等が含有する場合が多く、そして、その金属酸化物粒子の分散性等の理由で、溶媒として低級アルコールを主成分とする塗布液により形成されるのが一般的であった。
【０００３】
更に、その金属酸化物粒子も、更なる特性向上のために、有機化合物或いは金属原子を有する有機化合物で処理されたものも使用されるようになってきた。
尚、本明細書中で、低級アルコールとは、炭素数が８以下の直鎖及び分岐を有するアルコールを表す。
電子写真感光体分野においては、感光波長域の選択容易性、製造の容易性（塗布による製造が可能）、安全性の面でも無公害な材料を選択出来る点などから有機光導電体（ＯＰＣ）が、感光体の主流になってきた。このＯＰＣの構成も電荷発生材料、電荷輸送材料をバインダー中に分散した単層型や電荷発生層、電荷輸送層と機能を分離した積層型など、種々の構成のものが開発されているが、基体の上に電荷発生層、電荷輸送の順に積層された積層型が一般的である。
【０００４】
更に、近年では、電気特性、画像特性、機械特性の向上を図るために、基体上に下引き層を形成し、その後感光層を形成するものが、最も主流となってきている。
下引き層のバインダー樹脂としては、基体との接着性、耐溶剤性（電荷発生層及び電荷輸送の溶剤）、塗工性、電気的バリア性といった点で、アルコール可溶性樹脂、特にアルコール可溶性ポリアミド樹脂が好ましい樹脂として検討、使用されることが多い。
【０００５】
更に、下引き層としての要求特性を満足させるために、下引き層に、金属酸化物粒子等の無機粒子、特に酸化チタン粒子等が含有されていることが多い。更に、下引き層としての性能を向上させるために、該金属酸化物粒子が有機化合物処理されているのが一般的になってきている。特に、有機珪素化合物のように、金属原子を含有する有機化合物で処理されているのが一般的になりつつある。
このような少なくともアルコール可溶性樹脂及び有機化合物処理された金属酸化物粒子を含有する下引き層を有する電子写真感光体を製造する場合は、溶媒として、低級アルコールを主成分とした塗布液で塗布を行い、下引き層を形成し、更に感光層を塗布することにより一般的には製造されていた。
【０００６】
【発明が解決しようとする課題】
ところで、有機化合物処理された金属酸化物粒子を含む下引き塗布液を作製する場合は、一般的には、分散処理及び加熱処理等を行うため、金属酸化物に処理を施している有機化合物が塗布液中に遊離してくる。
また、作製後も経時とともに、金属酸化物に処理を施している有機化合物が塗布液中に遊離してくる。現状では、有機化合物処理剤の遊離を完全に抑制するのは、困難である。また、特性を向上させる有機化合物処理剤は、一般的には、低級アルコールや水との相溶性が悪いものが多い。それ故に、有機化合物処理された金属酸化物粒子とアルコール可溶性樹脂を含む下引き層の製造方法において、溶媒として低級アルコールを主成分とした塗布液を用いた場合、金属酸化物から遊離してきた有機化合物の処理剤が、塗布液中で会合しやすく、そのため塗布時にハジキ等の塗布欠陥が発生しやすく、良好な塗布膜が形成されにくいという問題があった。特に電子写真感光体の場合は、これらの下引き層のハジキ等の欠陥は、画像欠陥に繋がることが多く、歩留まりの低下に繋がり、大きな問題となる。
【０００７】
【課題を解決するための手段】
以下に、対策及び効果として、電子写真感光体の製造方法に限定して記述するが、他の塗膜形成においても、必然的に同様の効果が得られる。本発明者らは、上記問題を解決するため鋭意検討した結果、アルコール可溶性樹脂と、有機化合物で処理された金属酸化物粒子を少なくとも含有する下引き層を有する電子写真感光体の製造方法において、該有機化合物としてポリシロキサン化合物を用い、かつ、溶媒として、低級アルコールと芳香族炭化水素を混合した下引き層形成用塗布液にすることにより、下引き層塗布時の塗布性の改善，塗布液の保存安定性向上に特に有効であることを見出し、本発明を完成させた。
【０００８】
すなわち、本発明の要旨は、アルコール可溶性樹脂と、有機化合物で処理された金属酸化物粒子を少なくとも含有する下引き層を有する電子写真感光体の製造方法において、該有機化合物がポリシロキサン化合物であり、かつ、該下引き層を、低級アルコールと芳香族炭化水素の混合溶媒を主成分とする溶媒組成の下引き層形成用塗布液を塗布し、乾燥することにより形成することを特徴とする電子写真感光体の製造方法、に存する。
また、本発明の要旨は、アルコール可溶性樹脂と、有機化合物で処理された金属酸化物粒子を少なくとも含有する塗布膜を形成する方法において、該有機化合物がポリシロキサン化合物であり、かつ、該塗布膜を、低級アルコールと芳香族炭化水素の混合溶媒を主成分とする溶媒組成の塗布膜形成用塗布液を塗布し、乾燥することにより形成することを特徴とする塗布膜を形成する方法、及び、アルコール可溶性樹脂とポリシロキサン化合物で処理された金属粒子化合物を含有し、溶媒組成が低級アルコールと芳香族炭化水素の混合溶媒を主成分とすることを特徴とする塗布液、に存する。
【０００９】
芳香族炭化水素を混合することにより、塗布性が改善される理由は定かではないが以下のように考えられる。前述したように、一般的に、下引き層としての特性を向上させるための金属酸化物粒子の有機化合物処理剤は、極性が小さく低級アルコールとの相溶性が小さいため、低級アルコール溶媒では会合しやすい。逆に、芳香族炭化水素溶媒とは、相溶性が大きい場合が多く、そのため、芳香族炭化水素溶媒が一定量混合されていると、有機化合物の処理剤が遊離しても、会合する度合いが小さく、塗布液中に均一な状態で存在し易くなるため、ハジキ等の塗布欠陥が減少するものと考えられる。
【００１０】
【発明の実施の形態】
以下、本発明を詳細に説明する。
本発明において作製される下引き層のアルコール可溶性樹脂としては、ポリビニルブチラール等のポリビニルアセタール、セルロース、ポリアミド等が挙げられるが、基体との接着性、耐溶剤性、電気的バリア性、塗工性等から、ポリアミド樹脂が好ましい。その中でも下引き層としての性能及び塗布液の安定性の面で、下記一般式（Ｉ）で示されるジアミン成分を構成成分として有する共重合ポリアミド樹脂が特に好ましい樹脂である。
【００１１】
【化１】
（式中、環Ａ、環Ｂはそれぞれ独立して置換基を有していても良いシクロヘキシル基を表し、Ｒ1 、Ｒ2 はそれぞれ独立して水素原子、アルキル基、アルコキシ基、アリール基を表す。）
もう一方の構成成分である金属酸化物粒子は、有機化合物処理されているが、好ましくは、金属原子を含有する有機化合物で処理されていることが好ましい。その中でも、有機珪素化合物が一般的で有り、特にジメチルポリシロキサン及びメチル水素ポリシロキサン等のポリシロキサン化合物が好ましい。金属酸化物粒子としては、酸化チタンがより好ましい例として挙げられる。
【００１３】
下引き層塗布液の溶媒としては、低級アルコールと炭化水素の混合溶媒が主成分として用いられるが、低級アルコールとしては、特に炭素数４以下のアルコールがバインダー樹脂の溶解性から一般的に用いられ、メタノール，エタノール，ｎ−プロパノール，イソプロパノール，ｎ−ブタノールが好ましい。炭化水素としては、芳香族炭化水素及び炭素数が５から８の脂肪族炭化水素が好ましい例であり、より好ましくは芳香族炭化水素であり、その中でも、トルエンが処理剤との相溶性及び乾燥性及び安全性等の面から最も好ましい例である。
【００１４】
主成分以外の溶媒としては、それらの溶媒の役割に応じて、任意の溶媒を選択することが出来るが、炭素数９以上のアルコール，ケトン類，エーテル類等が好ましい。
低級アルコールと炭化水素の混合比は、任意に選ぶことが出来るが、炭化水素が３重量％から５０重量％が好ましい範囲である。炭化水素が、３重量％より少ない場合は、塗布時のハジキ欠陥の抑制に対して不十分であり、逆に５０重量％を超えると、バインダー樹脂の溶解性が悪くなる。より好ましい範囲としては、１０重量％から４０重量％である。
【００１５】
有機化合物処理された金属酸化物粒子と、アルコール可溶性樹脂の比は任意に選択できるが、特性及び塗布液の安定性の面から、重量比で、０．５／１から１０／１の範囲が好ましく、より好ましくは、２／１から５／１の範囲である。
更に、塗布性、分散粒子の分散性を改良する目的で、各種の界面活性剤を添加しても良い。その他、レベリング剤や酸化防止剤を含んでいても良い。
【００１６】
上記、下引き塗布液は、下記のように作製される。有機化合物処理された金属酸化物粒子をボールミル、コボールミル、サンドミル等で分散処理を行った後、適度な濃度に希釈してスラリーを作製する。上記スラリーに、予め溶媒で溶解しておいたバインダー溶解液を加えて混合し、下引き塗布液を作製する。又は、上記スラリーにバインダーペレット及び粉末を直接添加し、混合、攪拌し、上記バインダーを溶解し、下引き塗布液とする。また、逆に、バインダー溶解液に有機化合物処理の金属酸化物粒子を添加し、上記分散処理を行うことでも作製できる。これらの製造過程において、各種添加物は、任意に添加できる。また、必要に応じて、加熱処理、超音波処理等が加えられても良い。
このようにして作製された下引き塗布液は、基体上に塗布され、乾燥することにより下引き層が形成されるが、この時の塗布方法としては、スプレー塗布，ノズル塗布，ブレード塗布，スピンコート，浸漬塗布等いずれの方法を用いても良いが、電子写真感光体の塗布については、浸漬塗布が一般的に用いられる。
【００１７】
【実施例】
以下、実施例、比較例により本発明を更に具体的に説明するが、本発明はその要旨を越えない限り、これらに限定されるものでは無い。なお、実施例中及び比較例中及び参考例中で用いる「部」は断りがない限り、「重量部」を示す。
尚、各実施例、比較例とも、バインダー樹脂として、下記の構造式を持つ共重合ポリアミドＡを用いた。
【００１８】
【化２】
分散液（Ｐ）の調液
酸化チタンとして、石原産業（株）製：商品名ＴＴＯ５５Ｎを用い、ＴＴＯ５５Ｎに、メチル水素ポリシロキサンを３重量％処理したチタニアを予めボールミルにより分散し、その酸化チタンスラリーに、共重合ポリアミドＡ溶解液を混合し、更に超音波分散処理を行い、溶媒組成が、メタノール／ｎ−プロパノール／トルエン＝７／１／２で、酸化チタン／ナイロン＝３／１で、固形分濃度１６重量％の分散液を調整し、これを分散液（Ｐ）とした。
【００２０】
分散液（Ｑ）の調液
酸化チタンとして、石原産業（株）製：商品名ＴＴＯ５５Ｎを用い、ＴＴＯ５５Ｎに、メチル水素ポリシロキサンを３重量％処理したチタニアを予めボールミルにより分散し、その酸化チタンスラリーに、共重合ポリアミドＡ溶解液を混合し、更に超音波分散処理を行い、溶媒組成が、メタノール／ｎ−プロパノール＝７／３で、酸化チタン／ナイロン＝３／１で、固形分濃度１６重量％の分散液を調整し、これを分散液（Ｑ）とした。
【００２１】
実施例１
分散液（Ｐ）に、表面が鏡面仕上げされた外径６０ｍｍ、長さ３５０ｍｍ、肉厚１．０ｍｍのアルミニウム製シリンダーを浸漬塗布し、その乾燥膜厚が、０．７５μｍとなるように下引き層を設けた。このようにして、ドラムを２本作製し、そのドラムに発生したハジキ欠陥の数を数えたところ、１本あたりの平均として、６８個のハジキ欠陥が発生していた。
【００２２】
比較例１
分散液（Ｑ）に、表面が鏡面仕上げされた外径６０ｍｍ、長さ３５０ｍｍ、肉厚１．０ｍｍのアルミニウム製シリンダーを浸漬塗布し、その乾燥膜厚が、０．７５μｍとなるように下引き層を設けた。このようにして、ドラムを２本作製し、そのドラムに発生したハジキ欠陥の数を数えたところ、１本あたりの平均として、６６４個のハジキ欠陥が発生していた。
以上の結果から、本発明の電子写真感光体の製造方法は、塗布時のハジキ発生の抑制に効果が有り、その結果、電子写真感光体の製造時の歩留まりが向上し、生産コストの低減に繋がる。よって、本発明の電子写真感光体の製造方法は、非常に優れた方法であるといえる。
【００２３】
【発明の効果】
本発明の電子写真感光体の製造方法によれば、従来の炭化水素を含まない下引き塗布液と比べ、下引き層塗布時のハジキ等の塗布欠陥が減少し、歩留まり向上に効果が有り、優れた電子写真感光体の製造方法を提供出来る。尚、本明細書では、電子写真感光体の製造方法について、実施例を挙げて説明したが、他の用途の塗布膜の形成においても、同様な効果が得られる。[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a method for forming a coating film and a method for producing an electrophotographic photosensitive member. More specifically, the present invention relates to a method for forming a coating film characterized by applying a specific coating solution and a method for producing an electrophotographic photoreceptor characterized by applying a specific undercoat coating solution.
[0002]
[Prior art]
As a method of forming a coating film containing an alcohol-soluble resin, in the case of a resin that is soluble only in alcohol, naturally a solvent mainly composed of alcohol is used as a solvent, but a resin that is soluble in a solvent other than alcohol is also used. In order to improve cost, safety, and characteristics, metal oxide particles are often contained, and for reasons such as dispersibility of the metal oxide particles, a coating mainly containing a lower alcohol as a solvent. It was generally formed by a liquid.
[0003]
Further, the metal oxide particles have been used which are treated with an organic compound or an organic compound having a metal atom in order to further improve the characteristics.
In the present specification, the lower alcohol represents a linear and branched alcohol having 8 or less carbon atoms.
In the field of electrophotographic photoreceptors, organic photoconductors (OPCs) can be selected because of the ease of selection of the photosensitive wavelength range, ease of manufacture (manufacturing by coating), and safety-friendly materials can be selected. However, it has become the mainstream of photoconductors. Various OPC configurations have been developed, such as a charge generation material, a single layer type in which a charge transport material is dispersed in a binder, a charge generation layer, and a stacked type in which the function is separated from the charge transport layer. A stacked type in which a charge generation layer and a charge transport layer are stacked in this order on a substrate is generally used.
[0004]
Further, in recent years, in order to improve electrical characteristics, image characteristics, and mechanical characteristics, an undercoat layer is formed on a substrate, and then a photosensitive layer is formed mainly.
The binder resin for the undercoat layer is an alcohol-soluble resin, particularly an alcohol-soluble polyamide resin, in terms of adhesion to the substrate, solvent resistance (charge generation layer and charge transport solvent), coating properties, and electrical barrier properties. Is often studied and used as a preferred resin.
[0005]
Furthermore, in order to satisfy the required characteristics as the undercoat layer, the undercoat layer often contains inorganic particles such as metal oxide particles, particularly titanium oxide particles. Furthermore, in order to improve the performance as the undercoat layer, the metal oxide particles are generally treated with an organic compound. In particular, it is becoming common to treat with an organic compound containing a metal atom, such as an organosilicon compound.
When producing an electrophotographic photosensitive member having an undercoat layer containing at least an alcohol-soluble resin and an organic compound-treated metal oxide particle, the coating is performed with a coating solution mainly composed of a lower alcohol as a solvent. In general, it has been produced by forming an undercoat layer and further applying a photosensitive layer.
[0006]
[Problems to be solved by the invention]
By the way, in the case of preparing an undercoating coating solution containing metal oxide particles that have been treated with an organic compound, generally, an organic compound that has been treated with a metal oxide is used to perform a dispersion treatment, a heat treatment, and the like. Releases into the coating solution.
Further, with the passage of time even after the production, the organic compound that is treating the metal oxide is released into the coating solution. At present, it is difficult to completely suppress the release of the organic compound treating agent. In general, many organic compound treating agents that improve the properties have poor compatibility with lower alcohols and water. Therefore, in a method for producing an undercoat layer containing metal oxide particles treated with an organic compound and an alcohol-soluble resin, when a coating liquid containing a lower alcohol as a main component is used as a solvent, the organic released from the metal oxide The compound treating agent is likely to associate in the coating solution, so that coating defects such as repelling are likely to occur during coating, and a good coating film is difficult to form. In particular, in the case of an electrophotographic photosensitive member, defects such as repelling in the undercoat layer often lead to image defects, leading to a decrease in yield, which is a serious problem.
[0007]
[Means for Solving the Problems]
In the following, as a countermeasure and an effect, the description is limited to the production method of the electrophotographic photosensitive member, but the same effect is inevitably obtained in the formation of other coating films. The present inventors have made intensive studies for solving the above problems, and A alcohol-soluble resin, in the manufacturing method of the electrophotographic photosensitive member having an undercoat layer containing at least a metal oxide particles treated with an organic compound By using a polysiloxane compound as the organic compound and by using a coating solution for forming an undercoat layer in which a lower alcohol and an aromatic hydrocarbon are mixed as a solvent, the coating property at the time of applying the undercoat layer is improved. The present invention was completed by finding that it is particularly effective for improving the storage stability of the liquid.
[0008]
That is, the gist of the present invention, the A alcohol-soluble resin, in the manufacturing method of the electrophotographic photosensitive member having an undercoat layer containing at least a metal oxide particles treated with an organic compound, the organic compound is polysiloxane compound There, and the undercoat layer, an undercoat layer coating liquid for forming the solvent composition mainly containing a mixed solvent of a lower alcohol and an aromatic hydrocarbon is applied, and forming by drying The present invention relates to a method for producing an electrophotographic photoreceptor.
The gist of the present invention is a method for forming a coating film containing at least an alcohol-soluble resin and metal oxide particles treated with an organic compound, wherein the organic compound is a polysiloxane compound, and the coating film A method for forming a coating film, characterized in that the coating film is formed by applying and drying a coating film-forming coating solution having a solvent composition mainly composed of a mixed solvent of a lower alcohol and an aromatic hydrocarbon, and The coating liquid contains a metal particle compound treated with an alcohol-soluble resin and a polysiloxane compound, and the solvent composition is mainly composed of a mixed solvent of a lower alcohol and an aromatic hydrocarbon.
[0009]
The reason why the coating property is improved by mixing the aromatic hydrocarbon is not clear, but is considered as follows. As described above, generally, the organic compound treating agent for metal oxide particles for improving the properties of the undercoat layer has low polarity and low compatibility with the lower alcohol. Cheap. On the other hand, the aromatic hydrocarbon solvent is often highly compatible. Therefore, when a certain amount of the aromatic hydrocarbon solvent is mixed, the degree of association even if the treating agent of the organic compound is liberated. Since it is small and tends to exist in a uniform state in the coating solution, it is considered that coating defects such as cissing are reduced.
[0010]
DETAILED DESCRIPTION OF THE INVENTION
Hereinafter, the present invention will be described in detail.
Examples of the alcohol-soluble resin for the undercoat layer produced in the present invention include polyvinyl acetal such as polyvinyl butyral, cellulose, polyamide, etc., but adhesion to the substrate, solvent resistance, electrical barrier properties, and coating properties. From the above, a polyamide resin is preferable. Among them, a copolymerized polyamide resin having a diamine component represented by the following general formula (I) as a constituent component is a particularly preferable resin in terms of performance as an undercoat layer and stability of a coating solution.
[0011]
[Chemical 1]
(In the formula, ring A and ring B each independently represent a cyclohexyl group which may have a substituent, and R 1 and R 2 each independently represents a hydrogen atom, an alkyl group, an alkoxy group or an aryl group. Represents.)
The metal oxide particles as the other constituent component are treated with an organic compound, but are preferably treated with an organic compound containing a metal atom. Among these, organosilicon compounds are common, and polysiloxane compounds such as dimethylpolysiloxane and methylhydrogen polysiloxane are particularly preferable. As a metal oxide particle, a titanium oxide is mentioned as a more preferable example.
[0013]
As a solvent for the undercoat layer coating solution, a mixed solvent of a lower alcohol and a hydrocarbon is used as a main component. As the lower alcohol, an alcohol having 4 or less carbon atoms is generally used because of the solubility of the binder resin. Methanol, ethanol, n-propanol, isopropanol, and n-butanol are preferred. Preferred examples of the hydrocarbon include aromatic hydrocarbons and aliphatic hydrocarbons having 5 to 8 carbon atoms, and more preferred are aromatic hydrocarbons. Among them, toluene is compatible with the treatment agent and is dried. This is the most preferable example in terms of safety and safety.
[0014]
As the solvent other than the main component, any solvent can be selected according to the role of the solvent, but alcohols, ketones, ethers and the like having 9 or more carbon atoms are preferable.
The mixing ratio of the lower alcohol and the hydrocarbon can be arbitrarily selected, but the range of 3 to 50% by weight of the hydrocarbon is preferable. When the amount of hydrocarbon is less than 3% by weight, it is insufficient for suppressing repelling defects during coating. Conversely, when the amount exceeds 50% by weight, the solubility of the binder resin becomes poor. A more preferred range is from 10% to 40% by weight.
[0015]
The ratio between the metal oxide particles treated with the organic compound and the alcohol-soluble resin can be arbitrarily selected. However, in terms of characteristics and stability of the coating solution, the weight ratio ranges from 0.5 / 1 to 10/1. Preferably, it is in the range of 2/1 to 5/1.
Furthermore, various surfactants may be added for the purpose of improving coating properties and dispersibility of dispersed particles. In addition, a leveling agent and an antioxidant may be included.
[0016]
The above undercoat coating solution is prepared as follows. The metal oxide particles treated with the organic compound are subjected to a dispersion treatment with a ball mill, a coball mill, a sand mill or the like, and then diluted to an appropriate concentration to prepare a slurry. A binder solution previously dissolved in a solvent is added to the slurry and mixed to prepare an undercoat coating solution. Alternatively, binder pellets and powder are directly added to the slurry, mixed and stirred, and the binder is dissolved to form an undercoat coating solution. Conversely, it can also be produced by adding organic compound-treated metal oxide particles to the binder solution and carrying out the dispersion treatment. In these production processes, various additives can be arbitrarily added. Moreover, heat processing, ultrasonic processing, etc. may be added as needed.
The undercoat coating solution thus prepared is applied onto a substrate and dried to form an undercoat layer. At this time, spray coating, nozzle coating, blade coating, spin coating, etc. Although any method such as coating or dip coating may be used, dip coating is generally used for coating the electrophotographic photosensitive member.
[0017]
【Example】
EXAMPLES Hereinafter, although an Example and a comparative example demonstrate this invention further more concretely, this invention is not limited to these, unless the summary is exceeded. In the examples, comparative examples and reference examples, “parts” means “parts by weight” unless otherwise specified.
In each Example and Comparative Example, copolymer polyamide A having the following structural formula was used as the binder resin.
[0018]
[Chemical formula 2]
As the preparation titanium oxide of the dispersion (P), Ishihara Sangyo Co., Ltd. product name: TTO55N, titania treated with 3% by weight of methylhydrogenpolysiloxane in TTO55N is dispersed in advance by a ball mill, and the titanium oxide slurry The solution is mixed with a copolymerized polyamide A solution, further subjected to ultrasonic dispersion treatment, and the solvent composition is methanol / n-propanol / toluene = 7/1/2, titanium oxide / nylon = 3/1, solid A dispersion having a partial concentration of 16% by weight was prepared, and this was designated as dispersion (P).
[0020]
Titanium treated with 3% by weight of methylhydrogenpolysiloxane was previously dispersed in a TTO55N with a ball mill using Ishihara Sangyo Co., Ltd. product name: TTO55N as the preparation titanium oxide of the dispersion (Q), and the titanium oxide slurry In addition, the copolymerized polyamide A solution is mixed, further subjected to ultrasonic dispersion treatment, the solvent composition is methanol / n-propanol = 7/3, titanium oxide / nylon = 3/1, and the solid content concentration is 16 wt. % Dispersion liquid was prepared, and this was designated as dispersion liquid (Q).
[0021]
Example 1
An aluminum cylinder having an outer diameter of 60 mm, a length of 350 mm, and a wall thickness of 1.0 mm is dip-coated on the dispersion liquid (P), and the coating is subbed so that the dry film thickness becomes 0.75 μm. A layer was provided. In this way, when two drums were produced and the number of cissing defects generated on the drums was counted, 68 cissing defects occurred as an average per one drum.
[0022]
Comparative Example 1
An aluminum cylinder having an outer diameter of 60 mm, a length of 350 mm, and a wall thickness of 1.0 mm is dip-applied to the dispersion liquid (Q), and the coating is subbed so that the dry film thickness becomes 0.75 μm. A layer was provided. In this way, when two drums were produced and the number of cissing defects generated on the drum was counted, 664 cissing defects occurred as an average per one drum.
From the above results, the method for producing an electrophotographic photosensitive member of the present invention is effective in suppressing the occurrence of repelling during coating, and as a result, the yield during production of the electrophotographic photosensitive member is improved and the production cost is reduced. Connected. Therefore, it can be said that the method for producing an electrophotographic photoreceptor of the present invention is a very excellent method.
[0023]
【The invention's effect】
According to the method for producing an electrophotographic photosensitive member of the present invention, coating defects such as repellency during coating of the undercoat layer are reduced compared to a conventional undercoating solution that does not contain hydrocarbons, which is effective in improving yield. An excellent method for producing an electrophotographic photoreceptor can be provided. In the present specification, the method for producing an electrophotographic photosensitive member has been described with reference to examples, but the same effect can be obtained in the formation of a coating film for other purposes.
Claims (4)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP00623098A JP3685436B2 (en) | 1998-01-16 | 1998-01-16 | Method for producing electrophotographic photosensitive member, method for forming coating film, and coating solution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP00623098A JP3685436B2 (en) | 1998-01-16 | 1998-01-16 | Method for producing electrophotographic photosensitive member, method for forming coating film, and coating solution |
Related Child Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2004243380A Division JP2004326134A (en) | 2004-08-24 | 2004-08-24 | Method for manufacturing electrophotographic photoreceptor as well as method for forming coating film and coating liquid |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH11202519A JPH11202519A (en) | 1999-07-30 |
| JP3685436B2 true JP3685436B2 (en) | 2005-08-17 |
Family
ID=11632725
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP00623098A Expired - Lifetime JP3685436B2 (en) | 1998-01-16 | 1998-01-16 | Method for producing electrophotographic photosensitive member, method for forming coating film, and coating solution |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3685436B2 (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101587309B (en) | 2004-11-19 | 2012-01-25 | 三菱化学株式会社 | Coating liquid for undercoating layer formation, and electrophotographic photoreceptor |
| WO2007135987A1 (en) | 2006-05-18 | 2007-11-29 | Mitsubishi Chemical Corporation | Electrographic photoreceptor, image forming apparatus, and electrographic cartridge |
| EP2019338B1 (en) | 2006-05-18 | 2013-07-03 | Mitsubishi Chemical Corporation | Electrophotographic photosensitive body, image forming device, and electrophotographic cartridge |
| WO2007135986A1 (en) | 2006-05-18 | 2007-11-29 | Mitsubishi Chemical Corporation | Coating liquid for undercoating layer formation, process for producing coating liquid for undercoating layer formation, electrophotographic photoreceptor, apparatus for image formation, and electrophotographic cartridge |
| TWI452449B (en) | 2006-05-18 | 2014-09-11 | Mitsubishi Chem Corp | Electrophotographic photosensitive body, method for producing conductive case, and electrophotographic cartridge |
| TW200807189A (en) | 2006-05-19 | 2008-02-01 | Mitsubishi Chem Corp | Coating liquid for forming foundation layer, photosensitive body having foundation layer obtained through application of the coating liquid, image forming device and electrophotographic cartridge using the photosensitive body |
-
1998
- 1998-01-16 JP JP00623098A patent/JP3685436B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH11202519A (en) | 1999-07-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US6960247B2 (en) | Chromium-free water reducible rust inhibitive paint for metals | |
| JP3685436B2 (en) | Method for producing electrophotographic photosensitive member, method for forming coating film, and coating solution | |
| JP3722839B2 (en) | Crosslinkable conductive composition, conductor and method for forming the same | |
| JP2000103620A (en) | Electrophotographic photosensitizer and its production and titanium dioxide used therefor | |
| JP3624713B2 (en) | Electrophotographic photoreceptor and method for producing the same | |
| FR2738836A1 (en) | New photo-catalytic coatings based on titanium di:oxide in a mineral or organic dispersion | |
| MX2022004440A (en) | Nir light scattering coatings and compositions for preparing them. | |
| JP3612977B2 (en) | Method for producing electrophotographic photosensitive member and method for forming coating film | |
| JP2009198808A (en) | Application liquid for electrophotographic photoreceptor undercoating layer, manufacturing method therefor, electrophotographic photoreceptor, and image forming device | |
| FR2630124A1 (en) | POLYORGANOSILSESQUIOXANNE FINE POWDER SURFACE-TREATED | |
| JP2009288629A (en) | Method for manufacturing electrophotographic photoreceptor and electrophotographic photoreceptor | |
| JP2000137344A (en) | Production of electrophotographic photoreceptor | |
| JP2004326134A (en) | Method for manufacturing electrophotographic photoreceptor as well as method for forming coating film and coating liquid | |
| JPH0151183B2 (en) | ||
| KR102054684B1 (en) | Microcapsules | |
| WO2019106041A1 (en) | Dehydrated coating compositions in solid form, production method thereof, and method for rehydrating same | |
| JPS59221361A (en) | Heat-resistant corrosion-proofing paint | |
| JP2774065B2 (en) | Anti-sagging composition for paint and paint composition | |
| JPS6180158A (en) | Photosensitive body | |
| JP2005134924A (en) | Electrophotographic photoreceptor and image forming apparatus using the same | |
| KR102266248B1 (en) | Particulate composition, liquid composition, method for producing particulate composition, surface modifier, method for improving water dispersibility | |
| JP3981161B2 (en) | Surface-treated silica for paints | |
| JP3791277B2 (en) | Electrophotographic photoreceptor | |
| JP2001194809A (en) | Producing method of electrophotographic sensitive body and electrophotographic sensitive body | |
| JP2007264663A (en) | Method for manufacturing electrophotographic photoreceptor |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| A977 | Report on retrieval |
Free format text: JAPANESE INTERMEDIATE CODE: A971007 Effective date: 20040603 |
|
| A131 | Notification of reasons for refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A131 Effective date: 20040706 |
|
| A521 | Written amendment |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20040902 |
|
| A131 | Notification of reasons for refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A131 Effective date: 20041012 |
|
| RD02 | Notification of acceptance of power of attorney |
Free format text: JAPANESE INTERMEDIATE CODE: A7422 Effective date: 20050118 |
|
| RD02 | Notification of acceptance of power of attorney |
Free format text: JAPANESE INTERMEDIATE CODE: A7422 Effective date: 20041215 |
|
| A072 | Dismissal of procedure |
Free format text: JAPANESE INTERMEDIATE CODE: A073 Effective date: 20050428 |
|
| A01 | Written decision to grant a patent or to grant a registration (utility model) |
Free format text: JAPANESE INTERMEDIATE CODE: A01 Effective date: 20050519 |
|
| A61 | First payment of annual fees (during grant procedure) |
Free format text: JAPANESE INTERMEDIATE CODE: A61 Effective date: 20050527 |
|
| R150 | Certificate of patent or registration of utility model |
Free format text: JAPANESE INTERMEDIATE CODE: R150 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20080610 Year of fee payment: 3 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20090610 Year of fee payment: 4 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20100610 Year of fee payment: 5 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20100610 Year of fee payment: 5 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20110610 Year of fee payment: 6 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20120610 Year of fee payment: 7 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20130610 Year of fee payment: 8 |
|
| EXPY | Cancellation because of completion of term |