JPS5964847A - Production of electrophotographic receptor - Google Patents

Production of electrophotographic receptor

Info

Publication number
JPS5964847A
JPS5964847A JP17404482A JP17404482A JPS5964847A JP S5964847 A JPS5964847 A JP S5964847A JP 17404482 A JP17404482 A JP 17404482A JP 17404482 A JP17404482 A JP 17404482A JP S5964847 A JPS5964847 A JP S5964847A
Authority
JP
Japan
Prior art keywords
coating
viscosity
charge transfer
charge
transfer layer
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
JP17404482A
Other languages
Japanese (ja)
Other versions
JPH05701B2 (en
Inventor
Yuichi Yashiki
雄一 矢敷
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.)
Canon Inc
Original Assignee
Canon Inc
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 Canon Inc filed Critical Canon Inc
Priority to JP17404482A priority Critical patent/JPS5964847A/en
Publication of JPS5964847A publication Critical patent/JPS5964847A/en
Publication of JPH05701B2 publication Critical patent/JPH05701B2/ja
Granted legal-status Critical Current

Links

Classifications

    • GPHYSICS
    • G03PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03GELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
    • G03G5/00Recording members for original recording by exposure, e.g. to light, to heat, to electrons; Manufacture thereof; Selection of materials therefor
    • G03G5/02Charge-receiving layers
    • G03G5/04Photoconductive layers; Charge-generation layers or charge-transporting layers; Additives therefor; Binders therefor
    • G03G5/05Organic bonding materials; Methods for coating a substrate with a photoconductive layer; Inert supplements for use in photoconductive layers
    • G03G5/0525Coating methods

Landscapes

  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Photoreceptors In Electrophotography (AREA)

Abstract

PURPOSE:To obtain an electrophotographic receptor of a function snpn. type having a charge transfer layer wherein the surface characteristic is satisfactory by using a polymer contg. styrene or methyl methacrylate and coating the same at a specific soln. concn. and coating speed thereby forming the charge transfer layer. CONSTITUTION:The viscosity of a soln. prepd. by dissolving a polymer or copomer contg. styrene or methyl methacrylate and a charge transferrable material is adjusted to 50-300cP viscosity and is coated on the charge generation layer of an electrophotographic receptor of a function sepn. type having the charge transfer layer and the charge generating layer at <=40cm/min coating speed to form the charge transfer layer in a stage for dip coating said soln. on the charge transfer layer of said photoreceptor. The viscosity N (cP) and pulling speed S(cm/m) are related to each other inversely proportionally and a specified thickness of the film is obtd. at S=A/N (A is a constant ranging 300-3,000). A is the constant determined by the kind of the resin and charge transfer material used and a desired film thickness.

Description

【発明の詳細な説明】 本発明は電子写真感光体の製造方法に関し、更に詳しく
は、電荷輸送層と電荷発生層とを有する機能分離型電子
写真感光体の電荷輸送層の塗布方法に関するものである
DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for manufacturing an electrophotographic photoreceptor, and more particularly, to a method for coating a charge transport layer of a functionally separated electrophotographic photoreceptor having a charge transport layer and a charge generation layer. be.

有機光導電物質は、無機光導電物質に比べて、無公害性
、高生産性などの利点があるが、感度が低いため実用化
はむずかしかった。そのため、いくつかの増感方法が提
案されているが、効果的な方法としては電荷発生層と電
荷輸送層を積層した機能分離型感光体を用いることが知
られている。
Organic photoconductive materials have advantages over inorganic photoconductive materials, such as being non-polluting and highly productive, but their low sensitivity has made it difficult to put them into practical use. For this reason, several sensitization methods have been proposed, but it is known that an effective method is to use a functionally separated photoreceptor in which a charge generation layer and a charge transport layer are laminated.

電荷発生層は、スーダンレッド、グイアンプル−、ジェ
ナスグリーンBなどのアゾ顔料、アルゴールイエロー、
ヒレンキノン、インダンスレンブリリアントバイオレッ
トRRPなどのキノン顔料、キノシアニン顔料、はリレ
ン顔料、インジゴ、チオインジゴ等のインジゴ顔料、イ
ンドファーストオレンジトナーなどのビスベンゾイミダ
ゾール顔料、銅フタロシアニンなどのフタロシアニン顔
料、キナクリドン顔料等の電荷発生物質をポリエステル
、ポリスチレン、脂肪酸セルロースエステル、ポリ酢酸
ビニル、アクリル、ポリビニルピロリドン、メチルセル
ロース、ヒドロキシプロピルメチルセルロース、ボリビ
ニルブチラールなどの結着剤樹脂に分散させて、基体上
に塗布して形成される。
The charge generation layer is made of azo pigments such as Sudan Red, Guianpuru, and Jenas Green B, Algol Yellow,
Quinone pigments such as hillenquinone and indanthrene brilliant violet RRP, quinocyanine pigments, rylene pigments, indigo pigments such as indigo and thioindigo, bisbenzimidazole pigments such as India Fast Orange toner, phthalocyanine pigments such as copper phthalocyanine, quinacridone pigments, etc. It is formed by dispersing a charge-generating substance in a binder resin such as polyester, polystyrene, fatty acid cellulose ester, polyvinyl acetate, acrylic, polyvinylpyrrolidone, methylcellulose, hydroxypropylmethylcellulose, or polyvinyl butyral, and coating it on a substrate. .

電荷発′生層の上に設ける電荷輸送層は、主鎖又は側鎖
にアントラセン、ピレン、フェナントレン、コロネンな
どの多環芳香族化合物又はインドール、カルバゾール、
オキサゾール、イソオキサゾール、チアゾール、イミダ
ゾール、ピラゾール、オキサジアゾール、ピラゾリン、
チアジアゾール、トリアゾール彦どの含窒素環式化合物
を有する化合物、ヒドラゾン化合物、等の電荷輸送性物
質を成膜性のある樹脂に溶解させて形成される。とれは
電荷輸送性物質が一般的に低分子量で、それ自身では成
膜性に乏しいためである。このような樹脂としてはポリ
エステル、ポリサルホン、ポリカーボネート、ポリメタ
クリル酸エステル類、ポリスチレン、スチレン−アクリ
ロニトリル共重合体等が挙げられる。これらの樹脂のう
ち、成膜性や電位、感度、光メモリー効果等の電子写真
的特性を考慮すると、スチレン、またはメタクリル酸メ
チルの重合体もしくは共重合体を用いることが好ましい
The charge transport layer provided on the charge generation layer contains a polycyclic aromatic compound such as anthracene, pyrene, phenanthrene, coronene, or indole, carbazole, etc. in the main chain or side chain.
Oxazole, isoxazole, thiazole, imidazole, pyrazole, oxadiazole, pyrazoline,
It is formed by dissolving a charge-transporting substance such as a compound having a nitrogen-containing cyclic compound such as thiadiazole or triazole, or a hydrazone compound in a resin that has film-forming properties. This is because the charge transporting substance generally has a low molecular weight and has poor film-forming properties by itself. Examples of such resins include polyester, polysulfone, polycarbonate, polymethacrylic acid esters, polystyrene, and styrene-acrylonitrile copolymer. Among these resins, it is preferable to use styrene or a polymer or copolymer of methyl methacrylate in consideration of electrophotographic properties such as film-forming properties, potential, sensitivity, and photomemory effect.

例エバ、ポリスチレン、ポリメタクリル酸メチル、スチ
レンメタクリル酸メチル共重合体、スチレンアクリロニ
トリル共重合体、スチレンブタジェン共重合体、メタク
リル酸メチルメタクリル酸ブチル共重合体などである。
Examples include EVA, polystyrene, polymethyl methacrylate, styrene methyl methacrylate copolymer, styrene acrylonitrile copolymer, styrene butadiene copolymer, methyl methacrylate butyl methacrylate copolymer.

また、電荷輸送層を形成する方法としてはスプレー、ロ
ールコータ−、バーコーター、ナイフコーター、ブレー
ドコーター、浸漬などの塗布による方法が挙げられるが
、これらのうち、円筒状基体に、継ぎ目がなく、平滑な
表面が得られ、簡便な塗布方法として浸漬塗布方法が好
適である。塗布のようすを添付図面に示す。
Methods for forming the charge transport layer include coating methods such as spraying, roll coater, bar coater, knife coater, blade coater, and dipping. A dip coating method is suitable as a simple coating method that provides a smooth surface. The application process is shown in the attached drawing.

本発明は浸漬塗布方法によって電荷輸送層を塗布する際
において塗液の粘度と引き上げ塗布速度の関係において
、最も良好な表面性が得られる条件を設定することを目
的とするものであるO 電荷輸送層の膜厚は、受容電位や感度等に寄与し、通常
は10〜20μ程度の範囲に選ばれるが、この膜厚を得
るように浸漬塗布するには、粘度と引き上げ塗布速度に
は一定の関係がある。
The purpose of the present invention is to set conditions that will provide the best surface properties in terms of the relationship between the viscosity of the coating liquid and the lifting coating speed when applying a charge transport layer by a dip coating method. The thickness of the layer contributes to acceptance potential, sensitivity, etc., and is usually selected in the range of about 10 to 20μ, but in order to achieve this thickness by dip coating, the viscosity and pull-up coating speed must be kept at a certain level. There is a relationship.

すなわち、粘度、塗布速度はいずれも値が大きいほど膜
厚は厚くなり、膜厚をT1粘度をN1塗布速度を8とす
るとTccN8の関係があることがわかった。そこで所
定の膜厚を得るためには、塗液の粘4度が低い場合には
塗布速度を速く、粘度が高い場合には塗布速度をお干〈
すればよい。
That is, it was found that the larger the values of both viscosity and coating speed, the thicker the film becomes.If the film thickness is T1, the viscosity is N1, and the coating speed is 8, it was found that there is a relationship of TccN8. Therefore, in order to obtain the desired film thickness, increase the coating speed when the viscosity of the coating liquid is low, and decrease the coating speed when the viscosity is high.
do it.

ところが本発明者の実験の結果、スチレン、またはメタ
クリル酸メチルの重合体もしくは共重合体を含む塗液の
場合は、粘度が50cP(センチポアズ)より低い場合
には、塗布速度f40crn/分にしたくてはならず、
このような条件で塗布すると、塗膜の膜厚の上下むらが
2μ以上となり、感光体の電位むらが大きくなり、実用
に適しないことがわかった。さらに溶剤の比率が多いの
で、引き上げ中に塗膜からの溶剤の乾燥によって結露す
ることもあった。
However, as a result of the inventor's experiments, in the case of a coating liquid containing a polymer or copolymer of styrene or methyl methacrylate, if the viscosity is lower than 50 cP (centipoise), it is necessary to set the coating speed to f40 crn/min. Not,
It was found that when applied under these conditions, the vertical unevenness of the coating film thickness was 2 μ or more, and the potential unevenness of the photoreceptor became large, making it unsuitable for practical use. Furthermore, since the proportion of solvent was high, dew condensation could occur due to drying of the solvent from the coating film during pulling.

また粘度が300 cPより高い場合には、塗布速度を
いくら遅くしても膜厚が厚くなりすぎて、 5− これも実用に適しないことがわかった。
It was also found that when the viscosity is higher than 300 cP, the film thickness becomes too thick no matter how slow the coating speed is, and this is also not suitable for practical use.

本発明は、電荷輸送層を浸漬塗布する際に、塗液の粘度
を50〜300 cPの範囲圧調整し、塗布速度を40
1yR/分以下で塗布することを特徴とする。なお塗布
速度は401M/分以下とし生産性との兼ね合いで定め
られる。
In the present invention, when dip coating the charge transport layer, the viscosity of the coating liquid is adjusted to a pressure range of 50 to 300 cP, and the coating speed is adjusted to 40 cP.
It is characterized by coating at a rate of 1yR/min or less. The coating speed is determined to be 401 M/min or less in consideration of productivity.

また、TOCNEIであるから一定の膜厚を得るためK
は、NとSは反比例する関係にあシ、S=Δで表わされ
る。ここでAは300〜3000の範囲の定数であり、
これは使用する樹脂や電荷輸送物質の種類、および希望
膜厚によって定まることがわかった。これらの数値につ
いては実施例によって説明する。
Also, since it is TOCNEI, in order to obtain a constant film thickness, K
Since N and S are inversely proportional, it is expressed as S=Δ. Here A is a constant in the range of 300 to 3000,
It was found that this is determined by the type of resin and charge transport material used, and the desired film thickness. These numerical values will be explained using examples.

電荷輸送層の形成は、本発明による如く、スチレン、ま
たはメタクリル酸メチル含有重合体を用い、溶液粘度5
0〜300 cP、引き上げ塗布速度40(7)7分以
下、S=A/N (A=300〜3000)の関係で塗
布することによって、平滑で一様な表面性で特性も良好
な電荷輸送層の形成に奏功した。
According to the present invention, the charge transport layer is formed using a styrene- or methyl methacrylate-containing polymer with a solution viscosity of 5.
0 to 300 cP, pulling coating speed of 40(7) or less than 7 minutes, and coating with the relationship S=A/N (A=300 to 3000) provides a smooth and uniform surface with good charge transport properties. The layer was successfully formed.

 6− 実施例 1 添付図面に示されるような一方が閉じた円筒状の80φ
X 300+nmのアルミニウムシリンダーを基体とし
た。これにポリアミド樹脂(商品名:アミランC’M8
00[1、東し製)の4%メタノール溶液を浸漬法によ
JIDcm/分の引き上げ塗布速度で塗布し、80℃1
0分間の加熱乾燥を施して0.6μ厚の下引き層をもう
けた。
6- Example 1 Cylindrical 80φ with one end closed as shown in the attached drawings
The substrate was an aluminum cylinder of x 300+nm. This is made of polyamide resin (product name: Amilan C'M8
A 4% methanol solution of 00 [1, Toshi Co., Ltd.] was applied by the dipping method at a pull-up coating speed of JID cm/min, and the temperature was 80°C.
Heat drying was performed for 0 minutes to form an undercoat layer with a thickness of 0.6 μm.

次に下記構造式のビスアゾ顔料を10部(重量部、以下
同様)、 ポリビニルブチラール樹脂(商品名:エスレツクBXL
 、種水化学■製)8部およびシクロヘキサ2フ60部
を1φガラスピーズを用いたサンドミル装置で20時間
にわたり分散した。この分散液にメチルエチルケトン(
MKK)を100部加えて、塗液とした。これを浸漬塗
布法により、10crn/分の引き上げ速度で塗布し、
80°e10分間の乾燥をして0.07μの電荷発生層
を形成した。
Next, 10 parts (parts by weight, the same shall apply hereinafter) of a bisazo pigment with the following structural formula were added to polyvinyl butyral resin (trade name: Eslec BXL).
, manufactured by Tanemizu Kagaku ■) and 60 parts of cyclohexane 2F were dispersed over 20 hours using a sand mill apparatus using 1φ glass beads. Add methyl ethyl ketone (
100 parts of MKK) were added to prepare a coating liquid. This was applied using a dip coating method at a pulling rate of 10 crn/min.
A charge generation layer of 0.07 μm was formed by drying at 80° e for 10 minutes.

で示される構造式のヒドラゾン化合物7部、ポリスチレ
ン樹脂(商品名:ダイヤレックスH,F −55;三菱
モンサンド化成製)10部をモノクロルベンゼンに溶解
した。モノクロルベンゼンの重量部と溶液粘度の関係を
第1表に示す。
7 parts of a hydrazone compound having the structural formula represented by and 10 parts of a polystyrene resin (trade name: Dialex H, F-55; manufactured by Mitsubishi Monsando Kasei) were dissolved in monochlorobenzene. Table 1 shows the relationship between parts by weight of monochlorobenzene and solution viscosity.

第1表 これらの液を用い、乾燥後の膜厚が16μとなるよう浸
漬法で塗布した。引き上げ速度との関係を第2表に示す
Table 1 Using these solutions, coating was performed by dipping so that the film thickness after drying was 16 μm. Table 2 shows the relationship with the pulling speed.

第2表 このように粘度が250.120.6Q (cP)のと
ころで良い結果が得られた。なお、この時のへの値は1
5DOであった。
As shown in Table 2, good results were obtained when the viscosity was 250.120.6Q (cP). In addition, the value of at this time is 1
It was 5DO.

第2表に示された条件で電荷発生層上に電、荷輸送層を
塗布し、100℃で1時間乾燥して電子写真感光体とし
た。
A charge transport layer was coated on the charge generation layer under the conditions shown in Table 2, and dried at 100° C. for 1 hour to obtain an electrophotographic photoreceptor.

こうして製造した電子写真感光体を、5.6KVコロナ
帯電、画像露光、乾式トナー現像、普通紙へのトナー転
写、ウレタンゴムブレード(硬度70°、圧力5gw/
cm、感光体に対する角度20’) 9− によるクリーニング工程等を有する電子写真複写機に取
り付けてみたところ、粘度350F以外のものは良質の
コピー画像が得られたが、粘度35cPのものは、画像
濃度のむらが見られた。
The thus produced electrophotographic photoreceptor was subjected to 5.6KV corona charging, image exposure, dry toner development, toner transfer to plain paper, and urethane rubber blade (hardness 70°, pressure 5gw/
cm, angle to the photoconductor (20') 9- When I installed it in an electrophotographic copying machine that has a cleaning process, etc., I was able to obtain good quality copy images with the viscosity other than 350F, but with the viscosity of 35cP, the image quality was poor. Unevenness in concentration was observed.

実施例 2 電荷発生層までは実施例1と同様に基体上に塗布した。Example 2 The layers up to the charge generation layer were coated on the substrate in the same manner as in Example 1.

さらに実施例1と同じヒドラゾン化合物7部と、スチレ
ン−メタクリル酸メチル共重合樹脂(商品名:MS20
0、製鉄化学制)10部をトルエンに溶解した。トルエ
ンの量と粘度、および膜厚が16μとなる塗布速度の関
係を第10− このように粘度は220.150.100cPのところ
で良い結果が得られ、Aの値は2400であった。
Furthermore, 7 parts of the same hydrazone compound as in Example 1 and styrene-methyl methacrylate copolymer resin (trade name: MS20
0, Steel Manufacturing Chemical System) was dissolved in toluene. The relationship between the amount of toluene, the viscosity, and the coating speed at which the film thickness is 16 μm is shown in Figure 10. Thus, good results were obtained when the viscosity was 220.150.100 cP, and the value of A was 2400.

得られた電子写真感光体を用いてコピー画像をとると、
粘度が220.150.100cPのものけ良質の画像
が得られたが、5[1cPのものはむらが大きかった。
When a copy image is taken using the obtained electrophotographic photoreceptor,
Images with a viscosity of 220, 150, and 100 cP were of good quality, but those with a viscosity of 5 [1 cP were highly uneven.

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

図は浸漬塗布について装置の一例を挙げたものである。 図中の符号は、1・・・塗膜、2・・・液槽、3・・・
塗液、4・・・一端が閉じた円筒状基体、5・・・支持
部、6・・・駆動モーター(この回転により7・・・昇
降ねじを回転させ、基体を引き上げる。)、8・・・通
気管、9・・・ゴム製空気室(8と9により基体内部に
閉じ込められた空気の一部をとり出す。)を示す。 特許出願人  キ ヤ ノ ン株′、弐会狂代 埋 人
  弁理士 狩  野   有1 l−
The figure shows an example of equipment for dip coating. The symbols in the diagram are 1...paint film, 2...liquid tank, 3...
Coating liquid, 4... Cylindrical base with one end closed, 5... Support part, 6... Drive motor (this rotation rotates 7... the lifting screw and lifts up the base), 8... ...Vent pipe, 9... Rubber air chamber (8 and 9 take out part of the air trapped inside the base body). Patent applicant: Canon Co., Ltd., Kyoyoshi Nikai Patent attorney: Yu Kano

Claims (2)

【特許請求の範囲】[Claims] (1)  スチレンまたはメタクリル酸メチルを含有す
る重合体もしくは共重合体、および電荷輸送性物質を溶
解した溶液を浸漬塗布する工程において、該溶液の粘度
を50〜300 cPに調整し、塗布速度を40crn
/分以下で塗布して電荷輸送層を形成することを特徴と
する機能分離型電子写真感光体の製造方法。
(1) In the step of dip coating a solution containing a polymer or copolymer containing styrene or methyl methacrylate and a charge transporting substance, the viscosity of the solution is adjusted to 50 to 300 cP and the coating speed is adjusted. 40crn
1. A method for producing a functionally separated electrophotographic photoreceptor, characterized in that a charge transport layer is formed by coating at a rate of 1/min or less.
(2)粘度N (cP)と引き上げ塗布速度5(crn
Z分)の関係がS=A/N (Aは500〜3000の
範囲の定数)である特許請求の範囲第1項記載の機能分
離型電子写真感光体の製造方法。
(2) Viscosity N (cP) and pulling application speed 5 (crn
2. The method for manufacturing a functionally separated electrophotographic photoreceptor according to claim 1, wherein the relationship S=A/N (A is a constant in the range of 500 to 3000).
JP17404482A 1982-10-05 1982-10-05 Production of electrophotographic receptor Granted JPS5964847A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP17404482A JPS5964847A (en) 1982-10-05 1982-10-05 Production of electrophotographic receptor

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP17404482A JPS5964847A (en) 1982-10-05 1982-10-05 Production of electrophotographic receptor

Publications (2)

Publication Number Publication Date
JPS5964847A true JPS5964847A (en) 1984-04-12
JPH05701B2 JPH05701B2 (en) 1993-01-06

Family

ID=15971636

Family Applications (1)

Application Number Title Priority Date Filing Date
JP17404482A Granted JPS5964847A (en) 1982-10-05 1982-10-05 Production of electrophotographic receptor

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01124859A (en) * 1987-11-10 1989-05-17 Minolta Camera Co Ltd Production of photosensitive body
JPH02124576A (en) * 1988-11-02 1990-05-11 Fuji Xerox Co Ltd Production of electrophotographic sensitive body

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS4918131A (en) * 1972-06-12 1974-02-18
JPS5610368A (en) * 1979-07-09 1981-02-02 Mitsubishi Rayon Co Ltd Method and device for immersion coating
JPS57122444A (en) * 1981-01-23 1982-07-30 Canon Inc Electrophotographic receptor

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS4918131A (en) * 1972-06-12 1974-02-18
JPS5610368A (en) * 1979-07-09 1981-02-02 Mitsubishi Rayon Co Ltd Method and device for immersion coating
JPS57122444A (en) * 1981-01-23 1982-07-30 Canon Inc Electrophotographic receptor

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01124859A (en) * 1987-11-10 1989-05-17 Minolta Camera Co Ltd Production of photosensitive body
JPH02124576A (en) * 1988-11-02 1990-05-11 Fuji Xerox Co Ltd Production of electrophotographic sensitive body

Also Published As

Publication number Publication date
JPH05701B2 (en) 1993-01-06

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