JPH09160266A - Production of electrophotographic photoreceptor - Google Patents

Production of electrophotographic photoreceptor

Info

Publication number
JPH09160266A
JPH09160266A JP32167495A JP32167495A JPH09160266A JP H09160266 A JPH09160266 A JP H09160266A JP 32167495 A JP32167495 A JP 32167495A JP 32167495 A JP32167495 A JP 32167495A JP H09160266 A JPH09160266 A JP H09160266A
Authority
JP
Japan
Prior art keywords
coating
substrate
forming
layer
charge generation
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.)
Granted
Application number
JP32167495A
Other languages
Japanese (ja)
Other versions
JP3562078B2 (en
Inventor
Takashi Koyanagi
崇 小柳
Takaharu Nakayama
隆治 中山
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Mitsubishi Chemical Corp
Original Assignee
Mitsubishi Chemical Corp
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Mitsubishi Chemical Corp filed Critical Mitsubishi Chemical Corp
Priority to JP32167495A priority Critical patent/JP3562078B2/en
Publication of JPH09160266A publication Critical patent/JPH09160266A/en
Application granted granted Critical
Publication of JP3562078B2 publication Critical patent/JP3562078B2/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

Links

Landscapes

  • Photoreceptors In Electrophotography (AREA)

Abstract

PROBLEM TO BE SOLVED: To provide a process for producing an electrophotographic photoreceptor which is free from coating defects and has good electrical characteristics and image characteristics and excellent sensitivity and printing resistance. SOLUTION: This process comprises forming a charge generating layer and a charge transfer layer in this order on a substrate 3 for the electrophotographic photoreceptor. In dip-coating the substrate 3 for the electrophotographic photoreceptor with the charge generating layer, the average flow velocity at which a coating material for forming the charge generating layer rises in the gap between the substrate 3 for the electrophotographic photoreceptor and a coating vessel 6 is kept in a range from 0.1 to 0.5m/min.

Description

【発明の詳細な説明】Detailed Description of the Invention

【0001】[0001]

【発明の属する技術分野】本発明は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、塗布欠陥がな
く、且つ良好な電気特性及び画像特性を有する感度、耐
刷性に優れた機能分離型電子写真感光体の製造方法に関
する。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for manufacturing an electrophotographic photosensitive member. More specifically, the present invention relates to a method for producing a function-separated electrophotographic photosensitive member which has no coating defects, has excellent electrical characteristics and image characteristics, and has excellent sensitivity and printing durability.

【0002】[0002]

【従来の技術】近年、電子写真感光体は安全性、生産プ
ロセスの容易さ、生産コスト等の多くの面での利点を有
するために、今まで用いられてきたセレン、硫化カドミ
ウム、酸化亜鉛等の無機物質を光導電体として用いた無
機系電子写真感光体に代わって広く使用されるようにな
ってきている。
2. Description of the Related Art In recent years, electrophotographic photoreceptors have advantages in many aspects such as safety, easiness of a production process, and production costs. Therefore, selenium, cadmium sulfide, zinc oxide, etc. Inorganic electrophotographic photoreceptors using inorganic materials as photoconductors have been widely used.

【0003】電子写真感光体は、一般に単層型と機能分
離型(積層型)に分類されるが、機能分離型電子写真感
光体の方が感度に優れているために現在の主流となって
いる。機能分離型の層構成としてはまず感光体基体上に
電荷発生層、電荷輸送層を順に形成する。必要に応じて
基体表面にはアンダーコート層を設ける場合もあり、更
に必要に応じて電荷輸送層上にオーバーコート層を形成
する場合もある。
Electrophotographic photoreceptors are generally classified into a single-layer type and a function-separated type (multilayer type), but the function-separated type electrophotographic photoreceptor is the mainstream at present because of its superior sensitivity. There is. In the layer structure of the function separation type, first, a charge generation layer and a charge transport layer are sequentially formed on a photoreceptor substrate. An undercoat layer may be provided on the surface of the substrate as needed, and an overcoat layer may be formed on the charge transport layer as needed.

【0004】近年は複写機、レーザープリンター等の高
機能化が著しいため、その主要部品を構成する電子写真
感光体にも大幅な高感度化が求められている。電子写真
感光体の高感度化の方法論としては以下の2つの方法が
考えられる。即ち、 (1)電荷発生層の量子効率の向上 (2)電荷輸送層の電荷輸送能の向上 である。
In recent years, since the functions of copying machines, laser printers, etc. have been remarkably enhanced, electrophotographic photoreceptors constituting the main parts thereof are also required to be highly sensitive. The following two methods can be considered as the methodology for increasing the sensitivity of the electrophotographic photosensitive member. That is, (1) improvement of quantum efficiency of the charge generation layer and (2) improvement of charge transport ability of the charge transport layer.

【0005】前者について、量子効率は電荷発生材料の
固有の特性であるため、電子写真感光体の製造条件等を
変更することでは、量子効率を向上させて高感度化を計
ることは困難である。しかし後者の方法については、電
子写真感光体上の電荷発生層を薄膜化することで、電子
写真プロセスにおいて、電荷発生層から電子が電子写真
感光体基体へ移動する速度を高速化し、電子写真感光体
の感度を向上させるといった検討が行われ、実際に実用
化されている。
Regarding the former, since quantum efficiency is a characteristic peculiar to the charge generating material, it is difficult to improve quantum efficiency and increase sensitivity by changing the manufacturing conditions of the electrophotographic photosensitive member. . However, regarding the latter method, by thinning the charge generation layer on the electrophotographic photosensitive member, in the electrophotographic process, the speed at which electrons move from the charge generation layer to the electrophotographic photosensitive member substrate is increased, and Studies have been conducted to improve the sensitivity of the body, and they have been put to practical use.

【0006】また電子写真感光体を製造する場合、電子
写真感光体形成用塗料を用いて円筒状支持基体上に塗膜
を形成する方法としては、浸漬塗布法、スプレー塗布
法、ノズル塗布法、カーテン塗布法、ロール塗布法、ブ
レード塗布法、スパイラル塗布法及びリング塗布法等が
知られている。これらの中でも浸漬塗布法は電子写真感
光体形成用塗料を満たした塗工槽の中に、電子写真感光
体用基体を一定速度又は逐次変化する速度或いは一定速
度と逐次変化する速度の組み合わせ等で浸漬した後に、
この感光体基体を一定速度又は逐次変化する速度或いは
一定速度と逐次変化する速度の組み合わせ等で引き上げ
ることによって感光体基体表面に感光層形成用塗料を塗
布し、感光層を形成する方法である。
Further, in the case of producing an electrophotographic photosensitive member, as a method for forming a coating film on a cylindrical supporting substrate using a coating material for forming an electrophotographic photosensitive member, a dip coating method, a spray coating method, a nozzle coating method, Curtain coating method, roll coating method, blade coating method, spiral coating method, ring coating method and the like are known. Among these, the dip coating method is a method in which a substrate for an electrophotographic photosensitive member is placed in a coating tank filled with a coating material for forming an electrophotographic photosensitive member at a constant speed or a sequentially changing speed or a combination of a constant speed and a sequentially changing speed. After soaking
This is a method of forming a photosensitive layer by applying a coating for forming a photosensitive layer on the surface of the photosensitive body substrate by pulling up the photosensitive body substrate at a constant speed or a speed that changes sequentially or a combination of a constant speed and a speed that sequentially changes.

【0007】この浸漬塗布法は複雑な設備を必要とせ
ず、また生産性及びコストの面でも他の方法よりも優れ
ているために、電子写真感光体の製造に広く用いられて
いる。浸漬塗布法を使用する生産ラインでの連続塗布の
際には、電子写真感光体表面に形成する感光層、即ち電
荷発生層及び電荷輸送層等の膜厚制御方法としては通常
以下の2つの方法が行われる。
Since this dip coating method does not require complicated equipment and is superior in productivity and cost to other methods, it is widely used in the production of electrophotographic photoreceptors. In continuous coating in a production line using the dip coating method, the following two methods are usually used as a method for controlling the film thickness of the photosensitive layer formed on the surface of the electrophotographic photosensitive member, that is, the charge generation layer and the charge transport layer. Is done.

【0008】(1)電子写真感光体基体の引き上げ速度
を変化させる方法 (2)電荷発生層又は電荷輸送層形成用塗料の濃度を変
化させる方法 これらの方法の根拠としては、浸漬塗布法により基体表
面に形成される各感光層の膜厚と引き上げ速度及び感光
層形成用塗料の濃度の間には以下に示す関係の成立する
ことが挙げられる。
(1) Method of changing the pulling rate of the electrophotographic photosensitive member substrate (2) Method of changing the concentration of the coating material for forming the charge generating layer or the charge transport layer The basis of these methods is that the substrate is formed by the dip coating method. The following relationship may be established between the film thickness of each photosensitive layer formed on the surface, the pulling rate, and the concentration of the coating material for forming the photosensitive layer.

【0009】[0009]

【数1】 [Equation 1]

【0010】 μ :形成された感光層の膜厚 k,α:定数 C :感光層形成用塗料の濃度(wt%) η :感光層形成用塗料の粘度 Vc :感光体基体の引き上げ速度Μ: Film thickness of the formed photosensitive layer k, α: Constant C: Concentration (wt%) of coating material for forming photosensitive layer η: Viscosity of coating material for forming photosensitive layer Vc: Lifting speed of photoreceptor substrate

【0011】式[1]より感光層の膜厚を変化させるた
めには感光層形成用塗料の濃度又は粘度、或いは感光体
基体の引き上げ速度を変化させれば良い。しかしなが
ら、感光層形成用塗料の濃度又は粘度を変化させた場合
には、感光層の形成に悪影響が出る場合がある。例え
ば、生産ラインでの連続運転中に電荷発生層形成用塗料
の濃度又は粘度を低下させた場合には、塗布ムラの発生
や顔料の過分散又は凝集が起こる場合が有る。電荷輸送
層形成用塗料の濃度又は粘度を低下させた場合には、電
荷輸送層の膜厚形状の不均一化又は電子写真感光体のド
ロップゾーンが大きくなり、画像領域が制限されてしま
うといった問題が発生する。また反対に、感光層形成用
塗料の濃度又は粘度を上昇させた場合には、感光体基体
の引き上げ速度を低下させなければ同じ感光層膜厚を維
持することが出来ないため生産性が低下する。
From the formula [1], the film thickness of the photosensitive layer can be changed by changing the concentration or viscosity of the coating material for forming the photosensitive layer, or the pulling rate of the photosensitive substrate. However, if the concentration or viscosity of the photosensitive layer-forming coating material is changed, the formation of the photosensitive layer may be adversely affected. For example, when the concentration or viscosity of the charge generation layer-forming coating material is reduced during continuous operation on a production line, coating unevenness or pigment overdispersion or aggregation may occur. When the concentration or viscosity of the coating material for forming the charge transport layer is reduced, the thickness of the charge transport layer becomes non-uniform or the drop zone of the electrophotographic photoreceptor becomes large, and the image area is limited. Occurs. Conversely, when the concentration or viscosity of the coating material for forming a photosensitive layer is increased, the same photosensitive layer thickness cannot be maintained unless the pulling speed of the photosensitive member substrate is reduced, thereby lowering productivity. .

【0012】そのために、通常前記(2)の膜厚制御方
法は生産ラインでの連続運転中では実施されることはな
く、主に(1)の方法で感光層の膜厚制御が為される。
この浸漬塗布法は塗工層への感光層形成用塗料の供給方
法によって幾つかの方法が存在する。ここでは感光層形
成用塗料の供給方法に注目して、以下にそれぞれの方法
を説明する。
Therefore, the above-mentioned method (2) for controlling the film thickness is usually not carried out during continuous operation on the production line, and the method (1) is mainly used for controlling the film thickness of the photosensitive layer. .
There are several dip coating methods depending on the method of supplying the coating material for forming the photosensitive layer to the coating layer. Here, each method will be described below, focusing on the method of supplying the coating material for forming the photosensitive layer.

【0013】(1)一回の塗布工程で使用した分だけの
感光層形成用塗料を塗工槽へ逐次追加する方法(非オー
バーフロー方式)。 (2)塗布工程中、感光体基体の浸漬・引き上げ工程以
外の工程に於いて、塗工槽へ連続的に一定量又は逐次変
化する量の感光層形成用塗料を補給する方法(一時オー
バーフロー方式)。 (3)塗布工程を通して塗工槽へ一定量又は逐次変化す
る量の感光層形成用塗料を供給し続け、常に塗工槽から
塗料をオーバーフローさせる方法(常時オーバーフロー
方式)。 これら3つの方法に於いて、感光体基体を塗工槽に浸漬
する事によって塗工槽より溢れ出た感光層形成用塗料
は、一旦ホールドタンクに集められ、溶剤等の補給を行
った後、十分に攪拌を行うことで一定濃度・粘度且つ均
質な感光層形成用塗料に調整されてから塗工槽へ供給さ
れる。
(1) A method (non-overflow method) in which the coating material for forming the photosensitive layer, which is used in one coating step, is sequentially added to the coating tank. (2) During the coating step, in a step other than the step of dipping / pulling up the photoconductor substrate, a method of continuously replenishing the coating tank with a constant amount or a variable amount of the photosensitive layer-forming coating material (temporary overflow method) ). (3) A method in which a constant amount or a continuously changing amount of the photosensitive layer-forming coating material is continuously supplied to the coating tank through the coating step to constantly overflow the coating material (constant overflow method). In these three methods, the photosensitive layer-forming coating material overflowing from the coating tank by immersing the photosensitive substrate in the coating tank is once collected in a hold tank and replenished with a solvent or the like. It is supplied to the coating tank after being sufficiently stirred to prepare a photosensitive layer-forming coating material having a uniform concentration and viscosity and uniform.

【0014】しかしながら、(1)、(2)の供給方法
は塗工槽の内壁、配管内面、溢れ出た感光層形成用塗料
をホールドタンクへ導くインレットの部分等で、感光層
形成用塗料がある程度乾燥してしまうために、感光層形
成用塗料に濃度ムラが生じたり、感光層形成用塗料中に
乾燥した塗膜又は微小なダストが混入することが避けら
れず、微小なダストの除去や感光層形成用塗料の均一化
のための攪拌・循環系に多大な設備的負担が必要とな
り、又品質、品質管理や生産効率の面でも(3)の方法
に比べて劣っていることが分かっている。
However, the supply methods (1) and (2) are the inner wall of the coating tank, the inner surface of the pipe, the inlet portion for guiding the overflowed photosensitive layer forming coating material to the hold tank, and the like. Since it is dried to a certain extent, uneven density occurs in the photosensitive layer-forming coating material, and it is unavoidable that a dried coating film or minute dust is mixed in the photosensitive layer-forming coating material, and it is possible to remove minute dust particles. It was found that a large facility burden was required on the stirring / circulation system for uniformizing the coating for forming the photosensitive layer, and it was also inferior to the method of (3) in terms of quality, quality control and production efficiency. ing.

【0015】そして(3)の供給方法では浸漬・塗布工
程に於いても塗工槽に感光層形成用塗料を供給し続ける
ため、供給ポンプの能力(定量性、無脈動性)、塗工槽
内での流れのパターン、流速・流量、塗工槽の形状、塗
工槽内の整流方法等の影響が製品の品質に大きく反映さ
れることが知られている。特に(3)の方法では、電子
写真感光体基体上へ電荷発生層を形成する工程(浸漬・
塗布工程)に於いて、電荷発生層にドラムの長手方向に
伸びる筋状の塗布欠陥が発生するという現象が認められ
た。
In the supply method of (3), since the photosensitive layer forming coating material is continuously supplied to the coating tank even in the dipping / coating process, the capacity of the supply pump (quantitative, non-pulsating), the coating tank It is known that the quality of the product is largely influenced by the flow pattern inside, the flow velocity / flow rate, the shape of the coating tank, the rectification method in the coating tank, and the like. Particularly, in the method (3), the step of forming the charge generation layer on the electrophotographic photosensitive member substrate (immersion /
In the coating step), a phenomenon that streak-shaped coating defects extending in the longitudinal direction of the drum were generated in the charge generation layer was observed.

【0016】一般的に、この現象は電荷発生層の膜厚が
薄いほど発生し易いことが分かっており、従来は電荷発
生層の膜厚を厚くする方法でこの塗布欠陥を防止する方
法が行われてきた。電荷発生層の乾燥膜厚を1.2μm
以上に設定した場合にはこの様な塗布ムラは殆ど発生し
ないことが分かっている。しかしながら前述したよう
に、電子写真感光体の高感度化の手段として電荷発生層
の薄膜化が提案され、実用化されているためにこれらの
塗布欠陥の発生を防止する対策が求められている。
It is generally known that this phenomenon is more likely to occur as the film thickness of the charge generation layer is smaller, and conventionally, a method of preventing this coating defect is performed by increasing the film thickness of the charge generation layer. I've been told. Dry film thickness of charge generation layer is 1.2μm
It is known that such coating unevenness hardly occurs when the above setting is made. However, as described above, the thinning of the charge generation layer has been proposed as a means for increasing the sensitivity of the electrophotographic photosensitive member, and since it has been put into practical use, measures for preventing the occurrence of these coating defects are required.

【0017】[0017]

【発明が解決しようとする課題】先にも述べたように常
時オーバーフロー方式は、電子写真感光体基体上へ電荷
発生層を形成する工程(浸漬・塗布工程)に於いて、高
感度化のために電荷発生層の膜厚を薄く形成する場合に
は、電荷発生層に感光体基体の長手方向(浸漬及び塗布
方向)に伸びる筋状の塗布欠陥が発生し易いといった問
題があった。これは浸漬・塗布工程に於いて電子写真感
光体基体を、塗工槽に満たした感光層形成用塗料中へ浸
漬する際、塗工槽と感光体基体とが成す空隙に感光層形
成用塗料の上昇する流れが生ずるが、この上昇流に不均
一な流れが発生し、この不均一な流れが感光体基体表面
に、流れの方向に痕跡として残ってしまうことが原因で
ある。これら筋状の塗布欠陥は電子写真感光体表面に於
いて正常部よりも白い筋状のムラとして表れる。
As described above, the constant overflow method is used to increase the sensitivity in the step (immersion / coating step) of forming the charge generation layer on the electrophotographic photoreceptor substrate. When the film thickness of the charge generation layer is thin, there is a problem that streak-shaped coating defects extending in the longitudinal direction (immersion and coating direction) of the photoconductor substrate are likely to occur in the charge generation layer. This is a coating for forming a photosensitive layer in the gap between the coating tank and the photosensitive substrate when the electrophotographic photosensitive substrate is immersed in the coating for forming a photosensitive layer in the dipping / coating process. However, a non-uniform flow is generated in the upward flow, and the non-uniform flow remains on the surface of the photoconductor substrate as a trace in the flow direction. These streak-shaped coating defects appear as white streak unevenness on the surface of the electrophotographic photosensitive member as compared with the normal portion.

【0018】これに対して、非オーバーフロー方式や一
時オーバーフロー方式では、浸漬工程及びそれに続いて
行われる感光体基体の引き上げによる塗布工程に於い
て、感光層形成用塗料の供給を行わない。従って、感光
体基体を引き上げるにつれて、塗工槽と感光体基体とが
成す空隙に、感光層形成用塗料の溶剤蒸気を多量に含む
領域が必然的に形成され、感光体基体表面に形成された
電荷発生層はこれら溶剤蒸気を多量に含む領域でのレベ
リング効果によって、電子写真感光体基体を塗工槽に満
たした感光層形成用塗料中へ浸漬する際に、不均一な上
昇流による筋状の塗布欠陥が発生した場合でもこれら塗
布欠陥は緩和されてしまう。このために、非オーバーフ
ロー方式や一時オーバーフロー方式では、感光体基体の
長手方向に伸びる筋状の塗布欠陥は発生し難いことが分
かっている。しかしこれらの方法でも感光体基体の塗布
上端部は、溶剤蒸気を多量に含む領域を通過する時間が
短いために筋状の塗布欠陥が完全に緩和されないことも
判明している。
On the other hand, in the non-overflow method and the temporary overflow method, the coating for forming the photosensitive layer is not supplied in the dipping step and the subsequent coating step by pulling up the photoreceptor substrate. Therefore, as the photosensitive body substrate is pulled up, a region containing a large amount of solvent vapor of the photosensitive layer-forming coating material is inevitably formed in the void formed by the coating tank and the photosensitive body substrate, and is formed on the surface of the photosensitive body substrate. Due to the leveling effect in the area containing a large amount of these solvent vapors, the charge generation layer is streaked due to non-uniform upward flow when the electrophotographic photoreceptor substrate is dipped in the coating solution for forming the photosensitive layer. Even when the coating defects described above occur, these coating defects are alleviated. For this reason, it has been known that the non-overflow method and the temporary overflow method are unlikely to cause streak-shaped coating defects extending in the longitudinal direction of the photoreceptor substrate. However, even with these methods, it has been found that the stripe-shaped coating defects cannot be completely alleviated because the coating upper end portion of the photoreceptor substrate passes through a region containing a large amount of solvent vapor for a short time.

【0019】以上の知見より、この問題を解決するため
のアプローチとして以下に示す2つの方法が考えられ
る。即ち、 (1)不均一な上昇流が発生し、感光体基体表面に筋状
の塗布欠陥が発生しても溶剤蒸気によるレベリング効果
で消してしまう方法を開発する。 (2)不均一な上昇流が発生しない浸漬方式を開発する
Based on the above knowledge, the following two methods are conceivable as approaches for solving this problem. That is, (1) a method is developed in which even if streaky coating defects occur on the surface of the photoreceptor substrate due to nonuniform upflow, they are eliminated by the leveling effect of the solvent vapor. (2) Develop an immersion method that does not generate uneven upflow

【0020】まず(1)の方法についてであるが、これ
は常時オーバーフロー方式であっても塗工槽上部に感光
体形成用塗料の溶剤蒸気を充満させた部分を設けたなら
ば、レベリング効果によって、感光体基体の長手方向に
伸びる筋状の塗布欠陥を含めた様々な塗布欠陥を緩和す
ることが可能であると推論されることに根拠を置いてい
る、又この様な塗布欠陥対策の例も存在する。(特開平
4−255858号公報参照)。しかし、それらの方法
は設備的にも負担を大きくし、溶剤蒸気槽内の溶剤蒸気
濃度の制御、気流の制御等を行う必要もあるため好まし
い方法とは考えにくい。そこで次の(2)の方法につい
て、不均一な上昇流による筋状の塗布欠陥のみに的を絞
り、(1)の方法とは異なった、その他の塗布ムラに対
する効果は考えない代わりに、設備的な負担増や新たな
管理項目の追加による煩雑化をできる限り回避する方向
で検討を行った。
First of all, regarding the method (1), even if the method is always the overflow method, if a portion filled with the solvent vapor of the photoconductor-forming paint is provided in the upper part of the coating tank, the leveling effect will result. , Is based on the assumption that it is possible to mitigate various coating defects including streak-shaped coating defects extending in the longitudinal direction of the photoreceptor substrate, and an example of such coating defect countermeasures. Also exists. (See Japanese Patent Laid-Open No. 4-255858). However, it is difficult to think that these methods are preferable because they require a large facility burden and require the control of the solvent vapor concentration in the solvent vapor tank and the control of the air flow. Therefore, in the following method (2), only the streak-like coating defects due to the non-uniform upward flow are focused, and the effect on the other coating unevenness different from the method (1) is not considered. The study was conducted in the direction of avoiding complications due to the increase in the workload and the addition of new management items as much as possible.

【0021】[0021]

【課題を解決するための手段】本発明者等は上記筋状の
塗布欠陥の発生を防止すべく種々検討の結果、電子写真
感光体基体を電荷発生層形成用塗料に浸漬する際に、電
子写真感光体基体と塗工槽の間の空隙を電荷発生層形成
用塗料が上昇する平均流速を、特定の範囲に保つことに
よって、電子写真感光体基体の長手方向(浸漬又は塗布
方向)に発生する筋状の塗布欠陥を防止する効果が得ら
れたことを知得して、本発明に到達した。即ち、本発明
の要旨は、導電性の電子写真感光体用基体上に電荷発生
層と電荷輸送層をこの順に有する電子写真感光体の製造
方法において、電子写真感光体基体上に電荷発生層を浸
漬塗布する際に、電子写真感光体基体と塗工槽の間の空
隙を電荷発生層形成用塗料が上昇する平均流速を、0.
1〜0.5m/minまでの範囲に保つことを特徴とす
る電子写真感光体の製造方法に存する。
As a result of various investigations by the present inventors to prevent the occurrence of the above-mentioned streak-shaped coating defects, when the electrophotographic photoreceptor substrate is dipped in a charge generation layer forming coating material, Generated in the longitudinal direction (immersion or coating direction) of the electrophotographic photoreceptor substrate by keeping the average flow velocity of the charge generation layer forming paint rising in the gap between the photographic photoreceptor substrate and the coating tank within a specific range. The present invention has been achieved by knowing that the effect of preventing streaky coating defects is obtained. That is, the gist of the present invention is a method for producing an electrophotographic photoreceptor having a charge generation layer and a charge transport layer in this order on a conductive electrophotographic photoreceptor substrate, in which the charge generation layer is provided on the electrophotographic photoreceptor substrate. At the time of dip coating, the average flow rate at which the charge generation layer-forming coating material rises in the space between the electrophotographic photoreceptor substrate and the coating tank is 0.
A method for producing an electrophotographic photosensitive member is characterized by maintaining the range of 1 to 0.5 m / min.

【0022】[0022]

【発明の実施の形態】以下に本発明を詳細に説明する。
図1は本発明の一例である常時オーバーフロー方式の浸
漬塗布法の説明図である。塗布機1の感光体基体把持装
置2によって垂直に懸吊されている感光体基体3は、昇
降モーター4の回転によって垂直に上下動可能なアーム
5を下降させることによって、塗工槽6に満たされた感
光層形成用塗料7に浸漬される(浸漬工程)。ここで塗
工槽6上端よりオーバーフローして塗料受け部8に流下
した感光層形成用塗料7は配管を通ってホールドタンク
9に集められる。浸漬工程に続いて、アーム5を昇降モ
ーター4の回転で垂直に引き上げることによって塗布が
行われる(塗布工程)。この間、感光層形成用塗料7は
感光層形成用塗料供給ポンプ10によって常に供給され
続けるために、塗工槽6の液面は下降することがない。
従って、塗工槽6上端端面、塗工槽6内面、塗料受け部
8及び配管の塗料接触部は乾燥することがなく、乾燥し
た塗膜片が感光層形成用塗料7に混入することは防がれ
る。ホールドタンク9に集められた感光層形成用塗料7
は揮発分のごく少量の溶剤の添加後、ホールドタンク9
内の攪拌装置を用いて均一に攪拌・混合により均一化さ
れ、感光層形成用塗料供給ポンプ10を通過したところ
で混入したダストを除去するためのフィルター11を通
して塗工槽6の底部より供給される。
DESCRIPTION OF THE PREFERRED EMBODIMENTS The present invention will be described below in detail.
FIG. 1 is an explanatory diagram of a dip coating method of a constant overflow method which is an example of the present invention. The photoconductor substrate 3 vertically suspended by the photoconductor substrate holding device 2 of the coating machine 1 is filled in the coating tank 6 by lowering the vertically movable arm 5 by the rotation of the lifting motor 4. It is dipped in the photosensitive layer forming coating material 7 thus prepared (immersing step). Here, the photosensitive layer forming paint 7 overflowing from the upper end of the coating tank 6 and flowing down to the paint receiving portion 8 is collected in a hold tank 9 through a pipe. Subsequent to the dipping process, the arm 5 is vertically lifted by the rotation of the lifting motor 4 to perform the coating (coating process). During this time, since the photosensitive layer forming coating material 7 is continuously supplied by the photosensitive layer forming coating material supply pump 10, the liquid level in the coating tank 6 does not descend.
Therefore, the upper end surface of the coating tank 6, the inner surface of the coating tank 6, the paint receiving portion 8 and the paint contacting portion of the pipe are not dried, and the dried coating film pieces are prevented from being mixed in the photosensitive layer forming paint 7. Get off. Paint 7 for forming photosensitive layer collected in hold tank 9
Hold tank 9 after adding a very small amount of volatile solvent
The mixture is uniformly stirred and mixed by using the internal stirring device, and is supplied from the bottom of the coating tank 6 through a filter 11 for removing dust mixed in when passing through the photosensitive layer forming paint supply pump 10. .

【0023】本発明の特徴は、塗工槽に満たされた感光
層形成用塗料中に感光体基体を浸漬する際に、押し出さ
れる感光層形成用塗料が塗工槽内壁と感光体基体とが成
す空隙を上昇する平均流速を0.1〜0.5m/mi
n、より好ましくは0.2〜0.4m/minの範囲に
保つことで、塗工槽上部より溢れ出る感光層形成用塗料
の流れをほぼ均一にして、筋状塗布欠陥の原因となる特
定の不均一で強い流れを発生させないことにある。
The feature of the present invention is that when the photosensitive body substrate is immersed in the photosensitive layer-forming coating material filled in the coating tank, the photosensitive layer-forming coating material that is extruded is separated from the inner wall of the coating tank and the photosensitive body substrate. The average flow velocity that rises through the voids is 0.1 to 0.5 m / mi
n, more preferably in the range of 0.2 to 0.4 m / min, to make the flow of the photosensitive layer-forming coating material overflowing from the upper part of the coating tank substantially uniform, and to identify the cause of streaky coating defects. The non-uniform and strong flow of is not generated.

【0024】ここで塗工槽上部より溢れ出る感光層形成
用塗料の流れを均一にする方法としては、 (1)感光体基体を浸漬する速度を低下させる。 (2)感光体基体の断面積に対して十分に大きな開口面
積を有する塗工槽を使用する。 (3)感光体基体を浸漬する工程において、塗工槽底部
より感光層形成用塗料の供給を停止する又は感光層形成
用塗料を徐々に排出する。等の手段又はこれらの手段の
組み合わせが挙げられる。
Here, as a method for uniformizing the flow of the coating material for forming the photosensitive layer overflowing from the upper part of the coating tank, (1) the immersion speed of the photosensitive substrate is reduced. (2) Use a coating tank having an opening area sufficiently large with respect to the cross-sectional area of the photoreceptor substrate. (3) In the step of immersing the photoconductor substrate, the supply of the photosensitive layer forming coating material is stopped from the bottom of the coating tank or the photosensitive layer forming coating material is gradually discharged. And the like or a combination of these means.

【0025】上記(1)の方法は生産性の問題から考え
た場合、好ましい方法ではない。また(2)の方法も、
感光体基体の断面積と塗工槽の開口面積との比が一定限
度の値を超えた場合には、その過剰の値に応じて、特定
の塗布欠陥の発生する傾向にある。従って、実際には
(1)〜(3)の方法を組み合わせることが好ましい。
The method (1) is not a preferable method from the viewpoint of productivity. In addition, the method of (2)
When the ratio between the cross-sectional area of the photoconductor substrate and the opening area of the coating tank exceeds a certain limit value, a specific coating defect tends to occur depending on the excess value. Therefore, it is actually preferable to combine the methods (1) to (3).

【0026】本発明における電子写真感光体用の基体と
しては、導電性であれば、周知の電子写真感光体に採用
されているものがいずれも使用できる。具体的に挙げれ
ば、アルミニウム、ニッケル、ステンレス、銅等の金属
製円筒状基体、シートあるいはこれら金属箔をラミネー
トしたもの、またガラス、プラスティック、紙等からな
る基体にこれらの金属を蒸着させ導電性を持たせたもの
等が挙げられる。更に金属粉末、カーボンブラック、ヨ
ウ化銅、高分子電解質等の導電性物質を適当なバインダ
ーと共に表面塗布を行うことで導電処理を行った又は金
属粉末、カーボンブラック、炭素繊維などを含有し導電
性を有したプラスティック、紙等からなる円筒状又はフ
ィルム状基体等が挙げられる。
As the substrate for the electrophotographic photosensitive member in the present invention, any of those which are adopted in known electrophotographic photosensitive members can be used as long as they are conductive. Specifically, a metal cylindrical substrate made of aluminum, nickel, stainless steel, copper or the like, a sheet or a laminate of these metal foils, or a substrate made of glass, plastic, paper or the like is vapor-deposited with these metals so as to have conductivity. And the like. Further, a conductive material such as metal powder, carbon black, copper iodide, or a polymer electrolyte is surface-coated with an appropriate binder to perform a conductive treatment, or a conductive material containing metal powder, carbon black, carbon fibers, or the like is used. And a cylindrical or film-like substrate made of paper or the like.

【0027】電子写真感光体用基体としては、特に、ア
ルミニウムを主成分とする様々なものが好ましい。例え
ばアルミニウムを主成分とするものの材質としては、J
IS1050,JIS1070,JIS1080等の純
アルミニウムまたはAl−Mg系合金、Al−Cu系合
金、Al−Si系合金、Al−Mg−Si系合金、Al
−Cu−Si系合金等種々のアルミニウム合金、より好
ましくはAl−Mn系合金であるJIS3003、Al
−Si系合金であるJIS6063等が挙げられる。
As the electrophotographic photoreceptor substrate, various substrates containing aluminum as a main component are particularly preferable. For example, as a material of a material mainly containing aluminum, J
Pure aluminum such as IS1050, JIS1070, JIS1080 or Al-Mg alloy, Al-Cu alloy, Al-Si alloy, Al-Mg-Si alloy, Al
-Cu-Si alloys and other various aluminum alloys, more preferably Al-Mn alloys JIS3003, Al
JIS6063 etc. which are -Si type alloys are mentioned.

【0028】上記アルミニウムからなる感光体基体は、
表面切削処理またはしごき加工等によって成型される。
更にこれら感光体基体を加熱処理した後、アルマイト処
理したものも例示される。電子写真感光体の感光層とし
ては、電荷発生層と電荷輸送層が積層された構造の機能
分離型感光層を用いる。
The photoreceptor base made of aluminum is
It is molded by surface cutting or ironing.
Further, those obtained by subjecting these photoreceptor substrates to heat treatment and then alumite treatment are also exemplified. As the photosensitive layer of the electrophotographic photosensitive member, a function separation type photosensitive layer having a structure in which a charge generation layer and a charge transport layer are laminated is used.

【0029】本発明における電子写真感光体形成用塗料
としては電荷発生材料及び/または電荷輸送材料を含む
感光層形成用塗料が使用される。通常機能分離型感光層
の場合は上記の電子写真感光体基体上に電荷発生層及び
電荷輸送層が順次形成されるが、必要に応じて感光体基
体上にはアンダーコート層が設けられる。アンダーコー
ト層の形成用塗料は、例えば、ポリビニルアルコール、
カゼイン、ポリビニルピロリドン、ポリアクリル酸、セ
ルロース類、ゼラチン、でんぷん、ポリウレタン、ポリ
イミド、ポリアミド、ポリビニルブチラール、フェノキ
シ樹脂、ポリカーボネート、ポリビニルカルバゾール等
の高分子材料単独、またはこれらの共重合体等を適切な
溶媒、即ち水、各種アルコール、エーテル、ケトン、炭
化水素類等に溶解することで調製される。これらアンダ
ーコート層形成用塗料を感光体基体上に塗布・乾燥する
ことで下引き層が形成される。又アンダーコート層中に
は必要に応じてシリカ、アルミナ、酸化亜鉛、酸化チタ
ン、酸化インジウム、酸化スズ等の各種無機酸化物や各
種有機顔料が添加される。
As the electrophotographic photosensitive member-forming coating material in the present invention, a photosensitive layer-forming coating material containing a charge generating material and / or a charge transporting material is used. In the case of a function-separated type photosensitive layer, a charge generation layer and a charge transport layer are sequentially formed on the above electrophotographic photosensitive substrate, but an undercoat layer is provided on the photosensitive substrate as required. The coating material for forming the undercoat layer is, for example, polyvinyl alcohol,
Polymeric materials such as casein, polyvinylpyrrolidone, polyacrylic acid, celluloses, gelatin, starch, polyurethane, polyimide, polyamide, polyvinyl butyral, phenoxy resin, polycarbonate, polyvinylcarbazole alone, or copolymers thereof are suitable solvents. That is, it is prepared by dissolving in water, various alcohols, ethers, ketones, hydrocarbons and the like. The undercoat layer is formed by applying and drying the undercoat layer forming paint on the photoreceptor substrate. If necessary, various inorganic oxides such as silica, alumina, zinc oxide, titanium oxide, indium oxide, tin oxide and various organic pigments are added to the undercoat layer.

【0030】上記電荷発生層に用いられる電荷発生材料
としては、アゾ系顔料、ビスアゾ系顔料、トリスアゾ系
顔料、テトラキスアゾ系顔料、シアニン系顔料、スクエ
アリリウム系顔料、ペリノン系顔料、ペリレン系顔料、
アントラキノン系顔料、多環キノン系顔料、インジゴイ
ド系顔料、フタロシアニン系顔料、カルボニウム系顔
料、キノンイミン系顔料、メチン系顔料、キノリン系顔
料、ニトロ系顔料、ニトロソ系顔料、ベンゾキノン及び
ナフトキノン系顔料、ナフタルイミド系顔料、ビスベン
ズイミダゾール系顔料等公知の電荷発生材料が挙げられ
る。これら電荷発生材料は公知の各種バインダー樹脂、
増感剤等を含む適切な有機溶媒中へ分散することで電荷
発生層形成用塗料が得られる。これら電荷発生層形成用
塗料を先に述べた方法で塗布を行い、電荷発生層を形成
する。
As the charge generating material used in the charge generating layer, azo pigments, bisazo pigments, trisazo pigments, tetrakisazo pigments, cyanine pigments, squarylium pigments, perinone pigments, perylene pigments,
Anthraquinone pigment, polycyclic quinone pigment, indigoid pigment, phthalocyanine pigment, carbonium pigment, quinoneimine pigment, methine pigment, quinoline pigment, nitro pigment, nitroso pigment, benzoquinone and naphthoquinone pigment, naphthalimide Known charge generating materials such as pigments and bisbenzimidazole pigments can be used. These charge generation materials are various known binder resins,
By dispersing in a suitable organic solvent containing a sensitizer and the like, a charge generation layer forming coating material can be obtained. These charge generation layer forming paints are applied by the method described above to form a charge generation layer.

【0031】電荷輸送材料としては特に限定されず、電
子の輸送媒体或いはホールの輸送媒体を使用することが
でき、またその混合物も使用できる。電子の輸送媒体と
してはニトロ基、シアノ基、エステル基等の電子吸引性
基を有する電子吸引性化合物、例えば2,4,6−トリ
ニトロフルオレノン、2,4,5,7−テトラニトロフ
ルオレノン等のニトロ化フルオレノン類或いはテトラシ
アノキノジメタン、ジフェノキノン誘導体等が挙げられ
る。また、ホールの輸送媒体としては電子供与性の有機
光導電性化合物、例えば、カルバゾール、インドール、
イミダゾール、オキサゾール、チアゾール、オキサジア
ゾール、ピラゾール、ピラゾリン、チアジアゾール等の
複素環化合物、トリフェニルメタンとその誘導体、トリ
フェニルアミンとその誘導体、フェニレンジアミン誘導
体、N−フェニルカルバゾール誘導体、スチルベン誘導
体、ヒドラゾン誘導体或いはこれらの構造を主鎖又は側
鎖に有する高分子材料等が挙げられる。そしてこれら電
荷輸送材料は公知の各種バインダー樹脂、その他添加剤
等を含む適切な有機溶媒中へ分散又は溶解することによ
って電荷輸送層形成用塗料が得られる。これら電荷輸送
層形成用塗料を先に述べた方法で塗布を行い、電荷輸送
層を形成する。
The charge transport material is not particularly limited, and an electron transport medium or a hole transport medium can be used, and a mixture thereof can also be used. As an electron transport medium, an electron-withdrawing compound having an electron-withdrawing group such as a nitro group, a cyano group, an ester group, for example, 2,4,6-trinitrofluorenone, 2,4,5,7-tetranitrofluorenone, etc. Examples thereof include nitrated fluorenones, tetracyanoquinodimethane, and diphenoquinone derivatives. Further, as a hole transport medium, an electron-donating organic photoconductive compound, for example, carbazole, indole,
Heterocyclic compounds such as imidazole, oxazole, thiazole, oxadiazole, pyrazole, pyrazoline, thiadiazole, triphenylmethane and its derivatives, triphenylamine and its derivatives, phenylenediamine derivatives, N-phenylcarbazole derivatives, stilbene derivatives, hydrazone derivatives Alternatively, polymer materials having these structures in the main chain or side chain may be mentioned. These charge transporting materials are dispersed or dissolved in a suitable organic solvent containing various known binder resins and other additives to obtain a coating material for forming a charge transporting layer. These charge transport layer forming paints are applied by the method described above to form a charge transport layer.

【0032】上記電荷発生層又は電荷輸送層形成用塗料
を調製するための溶媒としては、N,N−ジメチルホル
ムアミド、アセトン、メチルエチルケトン、シクロヘキ
サノン、4−メトキシ−4−メチルペンタノン−2、ジ
メトキシメタン、ジメトキシエタン、ベンゼン、トルエ
ン、キシレン、クロロホルム、ジクロロメタン、1,2
−ジクロロエタン、テトラヒドロフラン、1,4−ジオ
キサン、メタノール、エタノール、2−プロパノール、
酢酸エチル、酢酸ブチル、ジメチルスルホキシド、2,
4−ペンタンジオン、3−オキソブタン酸メチル等が挙
げられる。上述の本発明を利用した電子写真感光体の製
造方法は、常時オーバーフロー方式での浸漬塗布法によ
る電荷発生層の形成の際、塗布欠陥の発生を抑制する効
果が非常に顕著である。従って、塗布ムラや感度のばら
つきが少なくかつ良好な画像特性を有する電子写真感光
体を製造することが可能である。
Solvents for preparing the above-mentioned coating material for forming the charge generating layer or the charge transporting layer include N, N-dimethylformamide, acetone, methyl ethyl ketone, cyclohexanone, 4-methoxy-4-methylpentanone-2 and dimethoxymethane. , Dimethoxyethane, benzene, toluene, xylene, chloroform, dichloromethane, 1,2
-Dichloroethane, tetrahydrofuran, 1,4-dioxane, methanol, ethanol, 2-propanol,
Ethyl acetate, butyl acetate, dimethyl sulfoxide, 2,
4-pentanedione, methyl 3-oxobutanoate and the like can be mentioned. The above-described method of manufacturing an electrophotographic photosensitive member according to the present invention has a very remarkable effect of suppressing the occurrence of coating defects when the charge generation layer is formed by the dip coating method using the always overflow method. Therefore, it is possible to manufacture an electrophotographic photoreceptor having good image characteristics with less coating unevenness and variation in sensitivity.

【0033】[0033]

【実施例】以下、実施例によって本発明を更に詳細に説
明する。なお、以下において「部」は「重量部」を表わ
す。 実施例1 電子写真感光体用基体としてアルミニウムからなる導電
性円筒状基体を用意し、この表面に、以下のようにして
作成した電荷発生層形成用塗料及び電荷輸送層形成用塗
料を順次塗布、乾燥を行い、電子写真感光体を作成し
た。まず電荷発生層形成用塗料は以下の様に作成した。
即ち、下記構造式(1)で表されるフタロシアニン化合
物4部、ポリビニルブチラール樹脂(電気化学工業
(株)製、商品名#6000−C)1部、フェノキシ樹
脂(ユニオンカーバイト社製、商品名PKHH)1部、
ジメトキシエタン360部、および、4−メトキシ−4
−メチルペンタノン−2 40部
The present invention will be described in more detail with reference to the following examples. In the following, “parts” means “parts by weight”. Example 1 A conductive cylindrical substrate made of aluminum was prepared as a substrate for an electrophotographic photoreceptor, and a charge generating layer forming coating material and a charge transporting layer forming coating material prepared in the following manner were sequentially applied to this surface. It was dried to prepare an electrophotographic photoreceptor. First, a paint for forming a charge generation layer was prepared as follows.
That is, 4 parts of a phthalocyanine compound represented by the following structural formula (1), 1 part of polyvinyl butyral resin (manufactured by Denki Kagaku Kogyo KK, trade name # 6000-C), phenoxy resin (manufactured by Union Carbide Co., trade name PKHH) 1 copy,
360 parts of dimethoxyethane and 4-methoxy-4
-Methylpentanone-2 40 parts

【0034】[0034]

【化1】 Embedded image

【0035】をサンドグラインダーミルにて分散処理及
び混合溶解し、約2.0センチポアズの粘度を有する電
荷発生層形成用塗料を作成した。この電荷発生層形成用
塗料を導電性円筒状基体の外周面に、乾燥膜厚が0.1
0μmになるように後記条件で浸漬塗布を行って電荷発
生層を形成した。続いて、電荷輸送層形成用塗料の1例
を以下に挙げる。
Dispersion treatment and mixing and dissolution were carried out with a sand grinder mill to prepare a charge generation layer-forming coating material having a viscosity of about 2.0 centipoise. The charge generation layer-forming coating material is applied to the outer peripheral surface of the conductive cylindrical substrate so that the dry film thickness is 0.1.
The charge generation layer was formed by performing dip coating under the conditions described below so as to have a thickness of 0 μm. Next, an example of the charge transport layer forming coating material will be given below.

【0036】下記構造式(2)で表されるヒドラゾン化
合物76部、下記構造式(3)で表されるヒドラゾン化
合物19部、下記構造式(4)で表されるポリカーボネ
ート樹脂100部、下記構造式(5)で表される化合物
1.5部、テトラヒドロフラン70部、および1,4−
ジオキサン30部
76 parts of the hydrazone compound represented by the following structural formula (2), 19 parts of the hydrazone compound represented by the following structural formula (3), 100 parts of the polycarbonate resin represented by the following structural formula (4), and the following structure 1.5 parts of the compound represented by the formula (5), 70 parts of tetrahydrofuran, and 1,4-
30 parts dioxane

【0037】[0037]

【化2】 Embedded image

【0038】[0038]

【化3】 Embedded image

【0039】[0039]

【化4】 Embedded image

【0040】[0040]

【化5】 Embedded image

【0041】をセパラブルフラスコ中で混合溶解し、2
50センチポアズの粘度を有する電荷輸送層形成用塗料
を得た。そしてこの電荷輸送層形成用塗料を電荷発生層
表面に乾燥膜厚が22μmになるように浸漬塗布を行っ
た後、125℃、48分間の乾燥を行って電子写真感光
体を形成した。
Mix and dissolve in a separable flask to
A charge transport layer-forming coating material having a viscosity of 50 centipoise was obtained. Then, this charge transport layer-forming coating material was applied on the surface of the charge generation layer by dip coating so that the dry film thickness was 22 μm, and then dried at 125 ° C. for 48 minutes to form an electrophotographic photoreceptor.

【0042】前記電荷発生層の塗布条件は以下の通りで
ある。 ・感光体基体の外径 :150(mm) ・塗工層の内径 :195(mm) ・感光体基体の浸漬速度:3.3(mm/sec) ・感光体基体の浸漬時、電荷発生層形成用塗料の供給は
行わない。 以上の条件で浸漬塗布を行ったところ、電荷発生層に筋
状の塗布欠陥の無い、均一な電子写真感光体が得られ
た。これを実際の複写機に搭載し、コピープロセスを繰
り返し行った。その結果、筋状塗布欠陥由来の画像ムラ
の少ない良好な画像が得られた。
The coating conditions for the charge generation layer are as follows. -Outer diameter of photoconductor substrate: 150 (mm) -Inner diameter of coating layer: 195 (mm) -Dip speed of photoconductor substrate: 3.3 (mm / sec) -Charge generation layer during dipping of photoconductor substrate No forming paint is supplied. When the dip coating was performed under the above conditions, a uniform electrophotographic photosensitive member having no streak-shaped coating defects in the charge generation layer was obtained. This was installed in an actual copying machine and the copying process was repeated. As a result, a good image with less image unevenness due to streak application defects was obtained.

【0043】実施例2、比較例1〜3 感光体基体の浸漬速度の条件を変化させることによっ
て、感光体基体と塗工槽の間の空隙を電荷発生層形成用
塗料が上昇する平均流速を変化させる以外は実施例1と
同様に行なった。その結果を実施例1と併せて以下に示
す。
Example 2, Comparative Examples 1 to 3 By changing the condition of the dipping speed of the photoconductor substrate, the average flow velocity at which the charge generation layer forming coating material rises in the gap between the photoconductor substrate and the coating tank is set. The same procedure as in Example 1 was carried out except that it was changed. The results are shown below together with Example 1.

【0044】[0044]

【表1】 [Table 1]

【0045】本発明で規定した流速、即ち、感光体基体
浸漬時の基体と塗工槽の間の電荷発生層形成用塗料の平
均流速が0.1〜0.5(m/min)であるという条
件を満たす場合、筋状の塗布欠陥は発生せず、良好な画
像特性を有する電子写真感光体が得られるのに対して、
条件から外れる場合には筋状の塗布欠陥及びその他の形
状を示す不均一な流れの発生に起因する塗布欠陥が発生
し、歩留りが低下したのみならず、良好な画像特性を有
する電子写真感光体はほとんど得られなかった。
The flow velocity specified in the present invention, that is, the average flow velocity of the charge generation layer forming coating material between the substrate and the coating tank when the photoreceptor substrate is immersed is 0.1 to 0.5 (m / min). When the condition is satisfied, no streak-shaped coating defects occur and an electrophotographic photosensitive member having good image characteristics can be obtained.
If the conditions are not satisfied, streak-shaped coating defects and coating defects due to the generation of non-uniform flow showing other shapes occur, and not only the yield is lowered but also an electrophotographic photoreceptor having good image characteristics. Was hardly obtained.

【0046】実施例3 実施例1と同様に、電子写真感光体基体としてアルミニ
ウムからなる導電性円筒状基体を用意し、この表面に、
以下のようにして作成した電荷発生層形成用塗料及び電
荷輸送層形成用塗料を順次塗布、乾燥を行い、電子写真
感光体を作成した。まず電荷発生層形成用塗料は以下の
様に作成した、即ち、下記構造式(6)で表されるビス
アゾ化合物4部、ポリビニルブチラール樹脂(電気化学
工業(株)製、商品名#6000−C)2部、フェノキ
シ樹脂(ユニオンカーバイト社製、商品名PKHH)1
部、ジメトキシエタン360部、および4−メトキシ−
4−メチルペンタノン−2 40部
Example 3 In the same manner as in Example 1, a conductive cylindrical substrate made of aluminum was prepared as an electrophotographic photosensitive substrate, and on the surface of this, a conductive cylindrical substrate was prepared.
The charge generation layer-forming coating material and the charge transport layer-forming coating material prepared as described below were sequentially applied and dried to prepare an electrophotographic photoreceptor. First, the charge generation layer-forming coating material was prepared as follows, that is, 4 parts of a bisazo compound represented by the following structural formula (6), polyvinyl butyral resin (trade name # 6000-C manufactured by Denki Kagaku Kogyo KK). ) 2 parts, phenoxy resin (manufactured by Union Carbide Co., trade name PKHH) 1
Parts, 360 parts of dimethoxyethane, and 4-methoxy-
4-methylpentanone-2 40 parts

【0047】[0047]

【化6】 [Chemical 6]

【0048】をサンドグラインダーミルにて分散処理及
び混合溶解し、約2.0センチポアズの粘度を有する電
荷発生層形成用塗料を作成した。この電荷発生層形成用
塗料を導電性円筒状基体の外周面に、乾燥膜厚が0.1
8μmになるように後記条件で浸漬塗布を行って電荷発
生層を形成した。
Dispersion treatment and mixing and dissolution were carried out with a sand grinder mill to prepare a charge generation layer forming coating having a viscosity of about 2.0 centipoise. The charge generation layer-forming coating material is applied to the outer peripheral surface of the conductive cylindrical substrate so that the dry film thickness is 0.1.
The charge generation layer was formed by performing dip coating under the conditions described below so as to have a thickness of 8 μm.

【0049】続いて電荷輸送層形成用塗料の1例を以下
に挙げる。下記構造式(7)で表されるヒドラゾン化合
物110部、前記構造式(4)で表されるポリカーボネ
ート樹脂100部、下記構造式(8)で表される化合物
1.5部、下記構造式(9)で表される酸化防止剤2
部、テトラヒドロフラン70部、および1,4−ジオキ
サン30部
Next, one example of the coating material for forming the charge transport layer will be described below. 110 parts of the hydrazone compound represented by the following structural formula (7), 100 parts of the polycarbonate resin represented by the structural formula (4), 1.5 parts of the compound represented by the following structural formula (8), and the following structural formula ( Antioxidant 2 represented by 9)
Parts, tetrahydrofuran 70 parts, and 1,4-dioxane 30 parts

【0050】[0050]

【化7】 Embedded image

【0051】[0051]

【化8】 Embedded image

【0052】[0052]

【化9】 Embedded image

【0053】をセパラブルフラスコ中で混合溶解し、約
250センチポアズの粘度を有する電荷輸送層形成用塗
料を得た。そしてこの電荷輸送層形成用塗料を電荷発生
層表面に乾燥膜厚が35.0μmになるように浸漬塗布
を行った後、130℃、48分間の乾燥を行って電子写
真感光体を形成した。
The above components were mixed and dissolved in a separable flask to obtain a charge transport layer-forming coating material having a viscosity of about 250 centipoise. Then, the coating material for forming a charge transport layer was applied by dip coating on the surface of the charge generation layer so that the dry film thickness became 35.0 μm, and then dried at 130 ° C. for 48 minutes to form an electrophotographic photosensitive member.

【0054】電荷発生層の塗布条件は以下の通りであ
る。 ・感光体基体の外径 :100(mm) ・塗工層の内径 :155(mm) ・感光体基体の浸漬速度:5.0(mm/sec) ・感光体基体の浸漬時、電荷発生層形成用塗料の供給は
行わない。 以上の条件で浸漬塗布を行ったところ、電荷発生層に筋
状の塗布欠陥の無い、均一な電子写真感光体が得られ
た。これを実際の複写機に搭載し、コピープロセスを繰
り返し行った。その結果、筋状塗布欠陥由来の画像ムラ
の少ない良好な画像が得られた。
The coating conditions for the charge generation layer are as follows. -Outer diameter of photoconductor substrate: 100 (mm) -Inner diameter of coating layer: 155 (mm) -Dip rate of photoconductor substrate: 5.0 (mm / sec) -Charge generation layer when dipping the photoconductor substrate No forming paint is supplied. When the dip coating was performed under the above conditions, a uniform electrophotographic photosensitive member having no streak-shaped coating defects in the charge generation layer was obtained. This was installed in an actual copying machine and the copying process was repeated. As a result, a good image with less image unevenness due to streak application defects was obtained.

【0055】実施例4、比較例4、5 感光体基体の浸漬速度の条件を変化させることによっ
て、感光体基体と塗工槽の間の空隙を電荷発生層形成用
塗料が上昇する平均流速を変化させる以外は実施例3と
同様に行なった。その結果を実施例3と併せて以下に示
す。
Examples 4, Comparative Examples 4 and 5 By changing the conditions of the immersion speed of the photoconductor substrate, the average flow velocity at which the paint for forming the charge generation layer rises in the gap between the photoconductor substrate and the coating tank is set. The same procedure as in Example 3 was carried out except that it was changed. The results are shown below together with Example 3.

【0056】[0056]

【表2】 [Table 2]

【0057】この結果からも、浸漬塗布の際に、本発明
で規定する条件を満たす場合には、塗布欠陥が発生せ
ず、これに対して、条件を満たさない場合は、筋状の塗
布欠陥が発生したため著しく歩留りを低下させたことが
理解される。
Also from this result, when the conditions prescribed in the present invention are satisfied during the dip coating, coating defects do not occur. On the other hand, when the conditions are not satisfied, streak-shaped coating defects occur. It is understood that the yield was significantly reduced due to the occurrence of.

【0058】[0058]

【発明の効果】本発明で規定する塗布工程に於ける浸漬
時の条件を使用することにより、塗布欠陥が無く、良好
な電気特性及び画像特性を有し、且つ感度・耐刷性に優
れた機能分離型電子写真感光体の製造方法を提供するこ
とが可能である。
EFFECTS OF THE INVENTION By using the conditions at the time of dipping in the coating process defined by the present invention, there are no coating defects, good electric characteristics and image characteristics, and excellent sensitivity and printing durability. It is possible to provide a method for producing a function-separated electrophotographic photoreceptor.

【図面の簡単な説明】[Brief description of the drawings]

【図1】本発明の一例の説明図。FIG. 1 is an explanatory diagram of an example of the present invention.

【符号の説明】[Explanation of symbols]

1 塗布機 3 電子写真感光体用基体 6 塗工槽 7 感光層形成用塗料 1 Coating Machine 3 Electrophotographic Photosensitive Body Substrate 6 Coating Tank 7 Photosensitive Layer Forming Paint

Claims (2)

【特許請求の範囲】[Claims] 【請求項1】 導電性の電子写真感光体用基体上に電荷
発生層と電荷輸送層をこの順に有する電子写真感光体の
製造方法において、電子写真感光体基体上に電荷発生層
を浸漬塗布する際に、電子写真感光体基体と塗工槽の間
の空隙を電荷発生層形成用塗料が上昇する平均流速を
0.1〜0.5m/minまでの範囲に保つことを特徴
とする電子写真感光体の製造方法。
1. A method for producing an electrophotographic photoreceptor having a charge generation layer and a charge transport layer in this order on a conductive electrophotographic photoreceptor substrate, wherein the charge generation layer is dip-coated on the electrophotographic photoreceptor substrate. At this time, the electrophotography characterized by maintaining the average flow velocity of the charge generation layer forming coating in the space between the electrophotographic photoreceptor substrate and the coating tank within a range of 0.1 to 0.5 m / min. Manufacturing method of photoconductor.
【請求項2】 常に電荷発生層形成用塗料を塗工槽から
オーバーフローさせながら電荷発生層を塗布させること
を特徴とする請求項1記載の電子写真感光体の製造方
法。
2. The method for producing an electrophotographic photoreceptor according to claim 1, wherein the charge generation layer is applied while the coating material for forming the charge generation layer is always overflowed from the coating tank.
JP32167495A 1995-12-11 1995-12-11 Manufacturing method of electrophotographic photoreceptor Expired - Fee Related JP3562078B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP32167495A JP3562078B2 (en) 1995-12-11 1995-12-11 Manufacturing method of electrophotographic photoreceptor

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP32167495A JP3562078B2 (en) 1995-12-11 1995-12-11 Manufacturing method of electrophotographic photoreceptor

Publications (2)

Publication Number Publication Date
JPH09160266A true JPH09160266A (en) 1997-06-20
JP3562078B2 JP3562078B2 (en) 2004-09-08

Family

ID=18135157

Family Applications (1)

Application Number Title Priority Date Filing Date
JP32167495A Expired - Fee Related JP3562078B2 (en) 1995-12-11 1995-12-11 Manufacturing method of electrophotographic photoreceptor

Country Status (1)

Country Link
JP (1) JP3562078B2 (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002214810A (en) * 2001-01-23 2002-07-31 Mitsubishi Chemicals Corp Electrophotographic photoreceptor, coating liquid for electric charge transport layer and method for producing the electrophotographic photoreceptor

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002214810A (en) * 2001-01-23 2002-07-31 Mitsubishi Chemicals Corp Electrophotographic photoreceptor, coating liquid for electric charge transport layer and method for producing the electrophotographic photoreceptor

Also Published As

Publication number Publication date
JP3562078B2 (en) 2004-09-08

Similar Documents

Publication Publication Date Title
JP2008046494A (en) Tube stock for electrophotographic photoreceptor, electrophotographic photoreceptor using the same and method for manufacturing the same
JP3562078B2 (en) Manufacturing method of electrophotographic photoreceptor
JPH1026835A (en) Production of electrophotographic photoreceptor
JP6945989B2 (en) Immersion coating device and method for manufacturing electrophotographic photosensitive member
JP2002049162A (en) Coating applicator for electrophotographic photoreceptor and method for manufacturing the same
JP3728952B2 (en) Method for producing electrophotographic photosensitive member
JPH10337514A (en) Dip coating device and device for manufacturing electrophotography photosensitive body
JP4568674B2 (en) Electrophotographic photoreceptor manufacturing apparatus and manufacturing method
JP2006337926A (en) Electrophotographic photoreceptor, method for manufacturing electrophotographic photoreceptor, process cartridge and electrophotographic apparatus
JP3412301B2 (en) Manufacturing method of electrophotographic photoreceptor
JPH01119373A (en) Coating method
JP2000325863A (en) Coating material applying method on cylindrical base body and production of electrophotographic photoreceptor drum
JP4470516B2 (en) Immersion coating method
JP2013134490A (en) Method for manufacturing electrophotographic photoreceptor and electrophotographic photoreceptor manufactured by manufacturing method
JP2003076042A (en) Method for manufacturing electrophotographic photoreceptor
JP2014178365A (en) Electrophotographic photoreceptor and method for manufacturing the same
JP3943265B2 (en) Immersion coating method
JP3980389B2 (en) Method for producing seamless flexible endless metal sheet
JP2001066802A (en) Apparatus for production of electrophotographic photoreceptor, and production of electrophotographic photoreceptor
JPH1172931A (en) Apparatus for production of photoreceptor
JP3266952B2 (en) Manufacturing method of cylindrical coated body
JPH10207089A (en) Production of electrophotographic photoreceptor
JPH0651545A (en) Production of organic electrophotographic sensitive body
JPH11216405A (en) Method and device for applying paint to cylindrical base body and manufacture of electrophotographic sensitive drum
JP2003270804A (en) Method for manufacturing electrophotographic photoreceptor

Legal Events

Date Code Title Description
A131 Notification of reasons for refusal

Free format text: JAPANESE INTERMEDIATE CODE: A131

Effective date: 20040210

A521 Written amendment

Free format text: JAPANESE INTERMEDIATE CODE: A523

Effective date: 20040409

TRDD Decision of grant or rejection written
A01 Written decision to grant a patent or to grant a registration (utility model)

Free format text: JAPANESE INTERMEDIATE CODE: A01

Effective date: 20040511

A61 First payment of annual fees (during grant procedure)

Free format text: JAPANESE INTERMEDIATE CODE: A61

Effective date: 20040524

FPAY Renewal fee payment (prs date is renewal date of database)

Free format text: PAYMENT UNTIL: 20080611

Year of fee payment: 4

FPAY Renewal fee payment (prs date is renewal date of database)

Free format text: PAYMENT UNTIL: 20090611

Year of fee payment: 5

FPAY Renewal fee payment (prs date is renewal date of database)

Free format text: PAYMENT UNTIL: 20100611

Year of fee payment: 6

FPAY Renewal fee payment (prs date is renewal date of database)

Free format text: PAYMENT UNTIL: 20100611

Year of fee payment: 6

FPAY Renewal fee payment (prs date is renewal date of database)

Free format text: PAYMENT UNTIL: 20110611

Year of fee payment: 7

FPAY Renewal fee payment (prs date is renewal date of database)

Free format text: PAYMENT UNTIL: 20120611

Year of fee payment: 8

FPAY Renewal fee payment (prs date is renewal date of database)

Free format text: PAYMENT UNTIL: 20130611

Year of fee payment: 9

LAPS Cancellation because of no payment of annual fees