JPS60208760A - Manufacture of electrophotographic sensitive fluid - Google Patents

Manufacture of electrophotographic sensitive fluid

Info

Publication number
JPS60208760A
JPS60208760A JP6490584A JP6490584A JPS60208760A JP S60208760 A JPS60208760 A JP S60208760A JP 6490584 A JP6490584 A JP 6490584A JP 6490584 A JP6490584 A JP 6490584A JP S60208760 A JPS60208760 A JP S60208760A
Authority
JP
Japan
Prior art keywords
photosensitive
alumina
plates
charge
fluid
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
JP6490584A
Other languages
Japanese (ja)
Inventor
Susumu Nakazawa
中沢 享
Masahiro Tsutsumi
真洋 堤
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.)
Kyocera Mita Industrial Co Ltd
Original Assignee
Mita Industrial Co Ltd
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 Mita Industrial Co Ltd filed Critical Mita Industrial Co Ltd
Priority to JP6490584A priority Critical patent/JPS60208760A/en
Publication of JPS60208760A publication Critical patent/JPS60208760A/en
Pending 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
    • 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
    • G03G5/0528Macromolecular bonding materials
    • G03G5/0557Macromolecular bonding materials obtained otherwise than by reactions only involving carbon-to-carbon unsatured bonds
    • G03G5/056Polyesters
    • 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
    • G03G5/06Photoconductive layers; Charge-generation layers or charge-transporting layers; Additives therefor; Binders therefor characterised by the photoconductive material being organic
    • G03G5/0622Heterocyclic compounds
    • G03G5/0644Heterocyclic compounds containing two or more hetero rings
    • G03G5/0646Heterocyclic compounds containing two or more hetero rings in the same ring system
    • G03G5/0657Heterocyclic compounds containing two or more hetero rings in the same ring system containing seven relevant rings

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  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Photoreceptors In Electrophotography (AREA)

Abstract

PURPOSE:To form a photosensitive layer superior in mechanical strength by dispersing a photosensitive fluid essentially consisting of an electrostatic charge transfer medium and a charge generating pigment by using a dispersing machine composed of a vessel and a ball mill both made of alumina. CONSTITUTION:A photosensitive fluid is prepared by mixing 12pts.wt. of N,N'- di(3,5-dimethylphenyl)perylene-3,4,9,10-tetracarboxylic acid diimide, 100pts.wt. of poly-N-vinylcarbazole, 10pts.wt. of a polyester resin ''Bairon 200'' made by TOYO BOSEKE KK, and 150pts.wt. of tetrahydrofuran, and alumina balls are placed into a mill pot made of alumina in an apparent volume of 200ml, and 100ml of said fluid mixture is introduced, and dispersion operations are executed at a revolution of 70rpm for 6, 12, 24, 45hr to prepare 4 kinds of photosensitive fluids. They are applied to aluminum plates each 80mum thick with a wire bar so as to form each 14mum dried thickness, and dried at 100 deg.C for 1hr to form photosensitive plates. The pencil hardness of the obtained plates are 3H in the cases of >=12hr drying times, and it is found in actual tests to have superior mechanical strength as compared with the case of 2H obtained by using an ultrasonic dispersing machine.

Description

【発明の詳細な説明】 (技術分野) 本発明は、電子写真用感光液の製造方法に関する。[Detailed description of the invention] (Technical field) The present invention relates to a method for producing a photosensitive liquid for electrophotography.

(従来技術) 鮮明な電子写真を得るためには、電子写真用感光液は均
一に帯電されねばならない。そのためには感光層が導電
性基体表面に平滑でかつ均等厚に形成されていることが
必須の要件である。感光層の形成にあたり無機・有機の
各種の感光材料が知られているが、その中で電荷発生顔
料、電荷輸送媒質を主成分としてなる感光層は、その感
光液調製において、ボールミルなどを用いて顔料などの
粒子を微細状に粉砕する手段がとられている。上記感光
層は無機系の感光層に比較して機械的強度に乏しい。そ
の強度を高めるために、従来から。
(Prior Art) In order to obtain clear electrophotography, electrophotographic photosensitive liquids must be uniformly charged. For this purpose, it is essential that the photosensitive layer be formed on the surface of the conductive substrate to be smooth and to have a uniform thickness. Various inorganic and organic photosensitive materials are known for forming photosensitive layers. Among them, photosensitive layers containing charge-generating pigments and charge-transporting media as main components are prepared using a ball mill or the like in the preparation of photosensitive liquids. Measures have been taken to pulverize particles such as pigments into fine particles. The photosensitive layer described above has poor mechanical strength compared to inorganic photosensitive layers. Conventionally to increase its strength.

例えば、径が1μm以下のシリカ、四フッ化炭素。For example, silica and carbon tetrafluoride with a diameter of 1 μm or less.

アルミナなどの無機微粉粒子を補強粉体として感光層内
に混入させることが行われている。微粉粒子の感光層内
への分散方法としては、微粉粒子を感光液の処方秤量段
階で混入させたり、予め分散させた分散液中に混入させ
る方法などが採用されている。混入される微粉粒子は感
光液■の1%以下という微量であるため、感光液中での
均一分散が非常に難しく、微粉粒子は感光層内で局在化
する傾向にある。また、このようにして?A J’A粒
子を混入させた感光液は、感光層形成段階で凝集をおこ
しやすくこれが感光体表面を粗面にする。
Inorganic fine powder particles such as alumina are mixed into the photosensitive layer as reinforcing powder. As a method for dispersing the fine powder particles into the photosensitive layer, a method is adopted in which the fine powder particles are mixed in at the stage of prescribing and weighing the photosensitive liquid, or mixed in a dispersion liquid in which the fine powder particles are dispersed in advance. Since the fine powder particles mixed are in a very small amount, less than 1% of the photosensitive liquid (1), uniform dispersion in the photosensitive liquid is very difficult, and the fine powder particles tend to be localized within the photosensitive layer. Also, in this way? A photosensitive liquid mixed with AJ'A particles tends to cause aggregation during the photosensitive layer formation stage, which makes the surface of the photoreceptor rough.

(発明の目的) 本発明の目的は、感光層補強用微粉粒子を外部から投入
することな(9機械的強度に優れた感光層を形成しうる
電子写真用感光液の製造方法を提供することにある。本
発明の他の目的は、均質かつ平滑な感光層表面を形成し
うる感光液の製造方法を提供することにある。
(Object of the Invention) An object of the present invention is to provide a method for producing an electrophotographic photosensitive liquid that can form a photosensitive layer with excellent mechanical strength without introducing fine powder particles for reinforcing the photosensitive layer from the outside. Another object of the present invention is to provide a method for producing a photosensitive liquid that can form a homogeneous and smooth surface of a photosensitive layer.

(発明の構成) 本発明の電子写真用感光液の製造方法は、アルミナ製容
器およびアルミナ製ボールでなる分散機を用い、主とし
て電荷輸送媒質と電荷発生顔料とを含有する感光液を分
散処理することを包含し。
(Structure of the Invention) The method for producing a photosensitive liquid for electrophotography of the present invention uses a dispersing machine comprising an alumina container and an alumina ball to disperse a photosensitive liquid mainly containing a charge transport medium and a charge generating pigment. It encompasses things.

そのことにより上記目的が達成される。Thereby, the above objective is achieved.

本発明に用いられる分散機は、アルミナ製容器とアルミ
ナ製ボールでなるボールミル分散機であることが必要で
ある。その構成には特に制限はない。このボールミル分
散機内で、ホールが容器壁と衝突することにより生ずる
アルミナの超微わ〕粒子が感光液中に混入し、これが感
光層の補強用微粉粒子として機能する。容器およびボー
ルに使用されるアルミナは焼結して形成されるため非常
に堅牢である。したがって、容器あるいはボールのうち
いずれかがアルミナ以外の材質で構成されると、いずれ
かが破壊されてしまい所望のアルミナ微粉粒子が発生し
えなくなり本発明の効果が達成されない。
The dispersing machine used in the present invention needs to be a ball mill dispersing machine consisting of an alumina container and an alumina ball. There are no particular restrictions on its configuration. In this ball mill dispersion machine, ultrafine alumina particles generated by the collision of the holes with the container wall are mixed into the photosensitive liquid, and these serve as fine powder particles for reinforcing the photosensitive layer. The alumina used in the container and bowl is sintered and is therefore very strong. Therefore, if either the container or the ball is made of a material other than alumina, either of them will be destroyed and the desired alumina fine particles will not be generated, making it impossible to achieve the effects of the present invention.

感光液を効率よく分散させるための条件としてはボール
が見掛容積でボールミル分敵機容器の内容積の50%量
で、かつ分散液が内容積の15〜30%量が好ましい。
In order to efficiently disperse the photosensitive liquid, it is preferable that the apparent volume of the balls be 50% of the internal volume of the ball mill container, and that the dispersion liquid be 15 to 30% of the internal volume.

さらにボールミル分散機の好適な回転数N (rPm)
は容器の内径Rに依存し、下記式(1)で決定される。
Furthermore, the suitable rotation speed N (rPm) of the ball mill dispersion machine
depends on the inner diameter R of the container and is determined by the following equation (1).

N −(37−3,3R) /fF ・・・(1)(R
:単位はフィート) 弐(11によれば2例えば、内径13cmの分散機を用
いる場合は回転数は70 rpmと算出することができ
る。
N - (37-3, 3R) /fF ... (1) (R
2 (according to 11) For example, when using a disperser with an inner diameter of 13 cm, the rotation speed can be calculated as 70 rpm.

本発明においては上記の条件下のもとに12〜24蒔間
分散を行うことにより、顔料粒子などの分散が好適にな
され゛るとともに所望量のアルミナ微粉粒子が感光液中
に混入し分散される。この感光液を用いて形成される感
光体の機械的強度は増大する。しかも、感光体の電気的
特性には何らの悪影響も及ばない。分散時間が12時間
未満のときは。
In the present invention, by carrying out dispersion between 12 and 24 hours under the above conditions, pigment particles and the like are suitably dispersed, and a desired amount of fine alumina particles are mixed into the photosensitive liquid and dispersed. Ru. The mechanical strength of a photoreceptor formed using this photoreceptor increases. Furthermore, there is no adverse effect on the electrical characteristics of the photoreceptor. When the dispersion time is less than 12 hours.

感光液の分散が不充分であるうえに混入すべきアルミナ
微粉粒子の量が少ない。それゆえ、この分散感光液を用
いて感光体にした場合、感光液の残留電位は上昇し、感
度が低下する。分散時間が24時間を超えると3分散液
中にアルミナ微粉粒子が過剰量混入することになる。こ
れが汚染物と、して感光体表面に付着し、残留電位の上
昇をきたし。
Dispersion of the photosensitive liquid is insufficient, and the amount of alumina fine powder particles to be mixed is small. Therefore, when this dispersed photosensitive liquid is used to make a photoreceptor, the residual potential of the photosensitive liquid increases and the sensitivity decreases. If the dispersion time exceeds 24 hours, an excessive amount of alumina fine powder particles will be mixed into the 3 dispersion liquid. This becomes a contaminant and adheres to the surface of the photoreceptor, causing an increase in residual potential.

同じく感光体の感度を低下させる。It also reduces the sensitivity of the photoreceptor.

感光液としては、あらゆる種類の有機光導電体感光層用
の分散液が使用されうる。感光層とじては、導電性基体
表面に電荷発生顔料の層とその上に電荷輸送媒質の層を
設けた機能分散型の有機感光層や、基体表面に電荷発生
顔料の電荷輸送媒質への分散体の層を設けてなる有機感
光層がある。
As photosensitive liquids, all kinds of dispersions for organic photoconductor photosensitive layers can be used. Photosensitive layers include functionally dispersed organic photosensitive layers, which have a charge-generating pigment layer on the surface of a conductive substrate and a charge-transporting medium layer thereon, and functionally dispersed organic photosensitive layers, which have a charge-generating pigment layer on the surface of a conductive substrate and a charge-transporting medium layer thereon, as well as functionally dispersed organic photosensitive layers in which a charge-generating pigment layer is disposed on the substrate surface and a charge-transporting medium layer. There is an organic photosensitive layer provided with a body layer.

電荷発生顔料としては、ペリレン系顔料、キナクリドン
系顔料、ピラントロン系顔料、フタロシアニン系顔料、
ジスアゾ系顔料、トリスアゾ系顔料等の光導電性有機顔
料が使用される。電荷輸送媒質としては、ポリビニルカ
ルバゾールのような電荷輸送性樹脂を単独もしくは他の
それ自体光導電性を有しない樹脂1例えば、ポリエステ
ル樹脂。
Examples of charge-generating pigments include perylene pigments, quinacridone pigments, pyranthrone pigments, phthalocyanine pigments,
Photoconductive organic pigments such as disazo pigments and trisazo pigments are used. As the charge transport medium, a charge transport resin such as polyvinylcarbazole or other resins which do not themselves have photoconductivity may be used, such as polyester resin.

エポキシ樹脂、ポリカーボネート樹脂、アクリル樹脂な
どと組合わせたものや、ヒドラジノ基Bn &体、ピラ
ゾリン型誘導体等の低分子電荷輸送媒質を樹脂中に分散
させたものが使用される。
A combination with an epoxy resin, a polycarbonate resin, an acrylic resin, etc., or a resin in which a low-molecular charge transport medium such as a hydrazino group Bn & form or a pyrazoline type derivative is dispersed is used.

(実施例) 以下に本発明を実施例について述べる。(Example) The present invention will be described below with reference to examples.

N、N’ −ジ (3,5−シメチ1トフェニル) ペ
リレン−3,4,9,10−テトラカルネン 1貨ジイ
ミド 12ffiffi部ポll−N−ビニ11カルバ
シー+L 100重唱1部ボ9 ’L ステ11樹脂(
バイuン200.東洋紡績に、に製)10重量部テトラ
ヒト■フラン lsomi部 上記処方を混合した。次に、アルミナ製ミルボット(内
径3cm、内容積400mn)へアルミナボールを見掛
容積で200m1入れ、さらに上記の混合液を100m
j2入れて分散を行った。分散は回転数7Orpmで1
分散時間を6.12.24.45時間と変えたものをそ
れぞれ作成し、4種の感光液を作製した。
N,N'-di (3,5-cymethy1tophenyl) perylene-3,4,9,10-tetracarnene 1 unit diimide 12ffiffi part Poll-N-vini 11 carbacy + L 100 duet 1 part Bo 9 'L Ste 11 resin(
Buy-un 200. 10 parts by weight of tetrahydrofuran (manufactured by Toyobo Co., Ltd.) and lsomi parts of the above formulation were mixed. Next, put an apparent volume of 200 ml of alumina balls into an alumina millbot (inner diameter 3 cm, internal volume 400 m), and then add 100 ml of the above mixed solution.
j2 was added for dispersion. The dispersion is 1 at a rotation speed of 7 Orpm.
Four types of photosensitive solutions were prepared by changing the dispersion time to 6, 12, 24, and 45 hours.

上記感光液をそれぞれ厚さ80μmのアルミニウム板上
に乾燥後の厚さが14μmになるようにワイヤーバーに
て塗布し、100℃で1時間の乾燥を行い、感光板を得
た。
Each of the above photosensitive solutions was coated onto an 80 μm thick aluminum plate using a wire bar so that the dried thickness would be 14 μm, and dried at 100° C. for 1 hour to obtain a photosensitive plate.

この感光液の静電特性(帯電量、残留電位)および表面
硬度(鉛筆硬度測定方法: JIS K 5400に準
する)を測定した。
The electrostatic properties (charge amount, residual potential) and surface hardness (pencil hardness measurement method: according to JIS K 5400) of this photosensitive liquid were measured.

その結果を表に示す。The results are shown in the table.

なお、静電特性については、エレクトロスタティックペ
ーパーアナライザー(川口型iKK製)により測定した
The electrostatic properties were measured using an electrostatic paper analyzer (manufactured by Kawaguchi type iKK).

比較例 実施例での未分散の混合液をボールミル分散する代わり
に超音波分散機を用いて150 (5ec)分散を行い
、さらに実施例と同様にして感光板を作製した。
Comparative Example Instead of dispersing the undispersed liquid mixture using a ball mill, an ultrasonic dispersion machine was used to perform dispersion for 150 (5 ec), and a photosensitive plate was produced in the same manner as in the example.

実施例と同様に各測定を行ったところ表面電位は600
 (V) 、残留電位100(V)であり、鉛筆硬度は
2Hであった。
When each measurement was carried out in the same manner as in the example, the surface potential was 600.
(V), the residual potential was 100 (V), and the pencil hardness was 2H.

(発明の効果) 本発明方法によれば、このように、アルミナ製のボール
ミル分散機を用い、これを所定時間駆動させるだけで機
械的強度に優れた感光層を形成しうる感光液が得られる
。この感光液で形成される感光層表面は均質かつ平滑で
もあるため、優れた電子写真を供給しうる。
(Effects of the Invention) According to the method of the present invention, a photosensitive liquid capable of forming a photosensitive layer with excellent mechanical strength can be obtained simply by using an alumina ball mill dispersion machine and driving it for a predetermined period of time. . Since the surface of the photosensitive layer formed with this photosensitive liquid is homogeneous and smooth, excellent electrophotography can be provided.

出願人 三田工業株式会社 代理人 弁理士 山本秀策Applicant: Sanda Kogyo Co., Ltd. Agent: Patent Attorney Shusaku Yamamoto

Claims (1)

【特許請求の範囲】 1、アルミナ製容器およびアルミナ製ボールでなる分散
機を用い、主として電荷輸送媒質と電荷発生顔料とを含
有する感光液を分散処理することを包含する電子写真用
感光液の製造方法。 2、前記分散処理は、前記分散機をアルミナ製容器の内
径をR9回転板をN(rplll)としたときN= (
37−3,3R)/(Wの条件下で12〜24時間駆動
させて行われる特許請求の範囲第1項に記載の製造方法
。 3、前記電荷輸送媒質がポリビニルカルバゾール系樹脂
を特徴とする特許請求の範囲第1項に記載の製造方法。 4、前記電荷発生顔料がペリレン系顔料である特許請求
の範囲第1項に記載の製造方法。
[Claims] 1. A photosensitive liquid for electrophotography, which involves dispersing a photosensitive liquid mainly containing a charge transport medium and a charge-generating pigment using a dispersing machine comprising an alumina container and an alumina ball. Production method. 2. In the dispersion process, when the inner diameter of the alumina container of the dispersion machine is R9 and the rotary plate is N (rpllll), N = (
37-3,3R)/(W) for 12 to 24 hours. 3. The charge transport medium is a polyvinylcarbazole resin. The manufacturing method according to claim 1. 4. The manufacturing method according to claim 1, wherein the charge-generating pigment is a perylene pigment.
JP6490584A 1984-03-31 1984-03-31 Manufacture of electrophotographic sensitive fluid Pending JPS60208760A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP6490584A JPS60208760A (en) 1984-03-31 1984-03-31 Manufacture of electrophotographic sensitive fluid

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP6490584A JPS60208760A (en) 1984-03-31 1984-03-31 Manufacture of electrophotographic sensitive fluid

Publications (1)

Publication Number Publication Date
JPS60208760A true JPS60208760A (en) 1985-10-21

Family

ID=13271539

Family Applications (1)

Application Number Title Priority Date Filing Date
JP6490584A Pending JPS60208760A (en) 1984-03-31 1984-03-31 Manufacture of electrophotographic sensitive fluid

Country Status (1)

Country Link
JP (1) JPS60208760A (en)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS62127843A (en) * 1985-11-29 1987-06-10 Mita Ind Co Ltd Electrophotographic organic sensitive body
JPH02144550A (en) * 1988-11-28 1990-06-04 Canon Inc Electrophotographic sensitive body
JPH04223472A (en) * 1990-12-26 1992-08-13 Fuji Xerox Co Ltd Production of electrophotographic sensitive body
JP2008107618A (en) * 2006-10-26 2008-05-08 Ricoh Co Ltd Method for manufacturing coating liquid for electrophotographic photoreceptor, and electrophotographic photoreceptor using the method, and electrophotographic device and process cartridge for electrophotographic device using the photoreceptor

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS62127843A (en) * 1985-11-29 1987-06-10 Mita Ind Co Ltd Electrophotographic organic sensitive body
JPH0555036B2 (en) * 1985-11-29 1993-08-16 Mita Industrial Co Ltd
JPH02144550A (en) * 1988-11-28 1990-06-04 Canon Inc Electrophotographic sensitive body
JPH04223472A (en) * 1990-12-26 1992-08-13 Fuji Xerox Co Ltd Production of electrophotographic sensitive body
JP2008107618A (en) * 2006-10-26 2008-05-08 Ricoh Co Ltd Method for manufacturing coating liquid for electrophotographic photoreceptor, and electrophotographic photoreceptor using the method, and electrophotographic device and process cartridge for electrophotographic device using the photoreceptor

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