JP2001356505A - Method for manufacturing electrophotographic photoreceptor - Google Patents

Method for manufacturing electrophotographic photoreceptor

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Publication number
JP2001356505A
JP2001356505A JP2000180984A JP2000180984A JP2001356505A JP 2001356505 A JP2001356505 A JP 2001356505A JP 2000180984 A JP2000180984 A JP 2000180984A JP 2000180984 A JP2000180984 A JP 2000180984A JP 2001356505 A JP2001356505 A JP 2001356505A
Authority
JP
Japan
Prior art keywords
dispersion
temperature
layer
type
electrophotographic photoreceptor
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
JP2000180984A
Other languages
Japanese (ja)
Other versions
JP3743268B2 (en
Inventor
Yutaka Iwahashi
豊 岩橋
Kazuhiko Matsui
数彦 松井
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
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Mitsubishi Chemical Corp
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Priority to JP2000180984A priority Critical patent/JP3743268B2/en
Publication of JP2001356505A publication Critical patent/JP2001356505A/en
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Publication of JP3743268B2 publication Critical patent/JP3743268B2/en
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Expired - Lifetime legal-status Critical Current

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  • Photoreceptors In Electrophotography (AREA)

Abstract

PROBLEM TO BE SOLVED: To produce so-called Y-type titanyl oxyphthalocyanine with good reproducibility. SOLUTION: The method for manufacturing an electrophotographic photoreceptor features that when the Y-type titanyl oxyphthalocyanine is dispersed, the temperature of the dispersion liquid is maintained in the range from -10 deg.C to 3 deg.C with fluctuation of the temperature of the dispersion liquid controlled to within 4 deg.C.

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】本発明は特定のオキシチタニ
ウムフタロシアニンの結晶を電荷発生剤として用いた電
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 producing an electrophotographic photosensitive member using a specific oxytitanium phthalocyanine crystal as a charge generating agent.

【0002】[0002]

【従来の技術】近年、従来の白色光の変わりにレーザー
光を露光光源とし、高速化、高画質化、高精細化、ノン
インパクト化をメリットとしたレーザープリンターが広
く普及するに至り、その要求に耐えうる高感度で、応答
性も良好な感光体の開発が盛んである。
2. Description of the Related Art In recent years, laser printers which use laser light as an exposure light source in place of conventional white light and have the advantages of high speed, high image quality, high definition and non-impact have become widespread. The development of photoreceptors with high sensitivity and good responsiveness that can withstand odors has been actively pursued.

【0003】このような高感度かつ応答性も良好な感光
体を得るためには、ブラッグ角(2θ±0.2°)9.
2°、14.3°、24.0°、及び27.3°に回折
ピークを有するオキシチタニウムフタロシアニン(以
下、単に「Y型TiOPc」という。)の結晶を電荷発
生剤として用いることが有効である。例えば、特開平3
−257458号公報には、10℃以下で分散処理する
とY型TiOPcを結晶型を安定に製造することができ
るとの記載がある。
In order to obtain such a photosensitive member having high sensitivity and good responsiveness, a Bragg angle (2θ ± 0.2 °) 9.
It is effective to use a crystal of oxytitanium phthalocyanine (hereinafter simply referred to as “Y-type TiOPc”) having diffraction peaks at 2 °, 14.3 °, 24.0 °, and 27.3 ° as a charge generating agent. is there. For example, Japanese Unexamined Patent Publication
JP-A-257458 discloses that a crystal form of Y-type TiOPc can be stably produced by a dispersion treatment at 10 ° C. or lower.

【0004】[0004]

【発明が解決しようとする課題】しかしながら、Y型T
iOPcはその結晶型が準安定型であるので、分散液を
作成する際、安定型(例えば、α型やβ型のTiOP
c)に変化しやすい。このため、特開平3−25745
8号公報に記載されているように分散液の温度を10℃
以下として分散処理を施した場合、ある程度Y型TiO
Pcが安定に製造できるものの、一部安定型のTiOP
cが生成する場合があるという問題点があった。
However, the Y-type T
Since iOPc has a metastable crystal form, a stable (for example, α-type or β-type TiOP
It is easy to change to c). For this reason, Japanese Unexamined Patent Publication No.
No. 8, the temperature of the dispersion is 10 ° C.
When the dispersion treatment is performed as follows, to some extent Y-type TiO
Although Pc can be manufactured stably, a partially stable type of TiOP
There is a problem that c may be generated.

【0005】[0005]

【課題を解決するための手段】Y型TiOPcの結晶型
を保持したまま安定な分散液を再現性よく作成するため
に、分散条件を検討したところ、分散液中で分散処理す
る際の分散液温度を低温にするだけではなく、温度変化
(ΔT)にも十分配慮することが重要であることを見い
だし本発明に至った。
Means for Solving the Problems In order to prepare a stable dispersion with good reproducibility while maintaining the crystal type of Y-type TiOPc, the dispersion conditions were examined. The present inventors have found that it is important not only to lower the temperature but also to sufficiently consider the temperature change (ΔT), and have reached the present invention.

【0006】すなわち、本発明の要旨は、Y型TiOP
cを分散処理する際に、分散液温度は−3℃〜10℃、
より好ましくは、−3℃〜3℃に設定すると同時に、分
散処理中の液温度変化(ΔT)を4℃以内、より好まし
くは2℃以内に制御する電子写真感光体の製造方法に存
する。Y型TiOPcは、温度変化の少ない状態で分散
処理を施した方が、安定結晶への結晶型変化が起こりに
くい。このため、単に低温で分散処理するだけではな
く、更に温度変化を少なくすれば、Y型TiOPcの結
晶型を変えずに分散処理を施すことがより効果的になる
のである。
That is, the gist of the present invention is to provide a Y-type TiOP
When performing dispersion treatment of c, the dispersion temperature is -3C to 10C,
More preferably, the present invention is directed to a method for producing an electrophotographic photoreceptor in which the temperature is set at −3 ° C. to 3 ° C. and the change in liquid temperature (ΔT) during the dispersion treatment is controlled within 4 ° C., more preferably within 2 ° C. In the case of Y-type TiOPc, when the dispersion treatment is performed in a state where the temperature change is small, the crystal type change to a stable crystal is less likely to occur. For this reason, it is more effective to perform the dispersion treatment without changing the crystal form of the Y-type TiOPc if the temperature change is further reduced, not only at a low temperature.

【0007】[0007]

【発明の実施の形態】以下、本発明を詳細に説明する。
本発明の電子写真感光体は、導電性支持体と、導電性支
持体上に形成された感光層とを具備する。感光層は、電
荷発生層と電荷移動層の2層を含むいわゆる積層型であ
っても、1層のみからなる単層型であっても良い。ま
た、導電性支持体と感光層の間には、中間層が設けられ
ても良い。さらに、感光層の表面には保護層が設けられ
ても良い。
BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, the present invention will be described in detail.
The electrophotographic photoreceptor of the present invention includes a conductive support and a photosensitive layer formed on the conductive support. The photosensitive layer may be of a so-called stacked type including two layers of a charge generation layer and a charge transfer layer, or may be a single layer type including only one layer. Further, an intermediate layer may be provided between the conductive support and the photosensitive layer. Further, a protective layer may be provided on the surface of the photosensitive layer.

【0008】導電性支持体としては、アルミニウム、ス
テンレス鋼、銅、ニッケル及びこれらの合金等の金属材
料、表面にアルミニウム、銅、パラジウム、酸化スズ、
酸化インジウム等の導電性層を例えば蒸着して作成され
たポリエステルフィルム、紙、ガラス等の絶縁性支持体
が使用される。電荷発生層は、電荷発生材としてのY型
TiOPcと結着樹脂とを具備する。Y型TiOPcの
結晶は公知な製造方法により製造することができる。
As the conductive support, metal materials such as aluminum, stainless steel, copper, nickel and alloys thereof, and aluminum, copper, palladium, tin oxide,
For example, an insulating support such as a polyester film, paper, or glass prepared by depositing a conductive layer of indium oxide or the like is used. The charge generation layer includes Y-type TiOPc as a charge generation material and a binder resin. The Y-type TiOPc crystal can be produced by a known production method.

【0009】通常の場合、Y型TiOPcは、27.3
°以外、9.5°、14.3°、及び24.0°付近に
も比較的明瞭な回折ピークを示す。製造条件の細かな差
により、ピーク強度の相対関係も微妙に振れることもあ
る。結着樹脂としては、ポリビニルブチラール、ポリビ
ニルアセタール、ポリエステル、ポリカーボネート、ポ
リスチレン、ポリエステルカーボネート、ポリスルフォ
ン、ポリイミド、ポリメチルメタクリレート、ポリ塩化
ビニル等のビニル重合体、及びその共重合体、フェノキ
シ、エポキシ、シリコーン樹脂、等又はこれらの部分的
架橋硬化物等単独あるいは2種以上用いる事もできる。
In the normal case, Y-type TiOPc is 27.3.
In addition to °, relatively clear diffraction peaks are also shown at around 9.5 °, 14.3 °, and 24.0 °. Due to small differences in the manufacturing conditions, the relative relationship between the peak intensities may slightly fluctuate. Examples of the binder resin include polyvinyl butyral, polyvinyl acetal, polyester, polycarbonate, polystyrene, polyester carbonate, polysulfone, polyimide, polymethyl methacrylate, and vinyl polymers such as polyvinyl chloride, and copolymers thereof, phenoxy, epoxy, and silicone. Resins, etc., or partially crosslinked and cured products thereof can be used alone or in combination of two or more.

【0010】Y型TiOPcと結着樹脂との割合は電子
写真感光体としての特性を発揮できる限り特に限定され
るものではない。一般的には、樹脂100重量部に対し
てY型TiOPcが5〜500重量部の範囲で使用され
る。また、電荷発生層は、必要に応じ、酸化防止剤、増
感剤、滑剤他を含んでいても良い。
The ratio between the Y-type TiOPc and the binder resin is not particularly limited as long as the characteristics as an electrophotographic photosensitive member can be exhibited. Generally, Y type TiOPc is used in a range of 5 to 500 parts by weight based on 100 parts by weight of the resin. Further, the charge generation layer may contain an antioxidant, a sensitizer, a lubricant, and the like, if necessary.

【0011】Y型TiOPcは、分散処理を施した後、
結着樹脂等と混合され調液された後導電性支持体上に塗
布される。Y型TiOPcが、分散媒体中で分散処理す
る際に、分散液の温度は10℃〜−3℃に維持され、か
つ分散液の温度変化(ΔT)は、4℃以内、更に好まし
くは分散液温度が3℃〜−3℃に維持され、最も好まし
くは、ΔTが2℃以内に制御される様、冷却される。
The Y-type TiOPc is subjected to a dispersion treatment,
After mixing with a binder resin or the like to prepare a solution, it is applied on a conductive support. When Y-type TiOPc is subjected to dispersion treatment in a dispersion medium, the temperature of the dispersion is maintained at 10 ° C. to −3 ° C., and the temperature change (ΔT) of the dispersion is within 4 ° C., more preferably the dispersion. The temperature is maintained between 3 ° C. and −3 ° C., and most preferably is cooled such that ΔT is controlled within 2 ° C.

【0012】上記分散処理に用いる分散媒体としては、
原材料として用いるY型TiOPcの結晶型を変化させ
ない限り、種々の溶媒を用いても良い。かかる分散溶媒
としては、例えば、ジエチルエーテル、ジメトキシメタ
ン、テトラヒドロフラン、1,2−ジメトキシエタン等
の直鎖状、環状エーテル類、アセトン、メチルエチルケ
トン、シクロヘキサノン等の直鎖状、環状ケトン類、酢
酸メチル、酢酸エチル等のエステル類、メタノール、エ
タノール、プロパノール等のアルコール類等を単独ある
いは2種以上混合しても使用することができる。
[0012] The dispersion medium used in the above dispersion processing includes:
Various solvents may be used as long as the crystal form of Y-type TiOPc used as a raw material is not changed. Such a dispersion solvent, for example, diethyl ether, dimethoxymethane, tetrahydrofuran, linear such as 1,2-dimethoxyethane, cyclic ethers, acetone, methyl ethyl ketone, linear such as cyclohexanone, cyclic ketones, methyl acetate, methyl acetate, Esters such as ethyl acetate and alcohols such as methanol, ethanol and propanol can be used alone or in combination of two or more.

【0013】用いる分散媒の量は、分散が十分行え、且
つ、分散液中に有効量のオキシチタニウムフタロシアニ
ンが含まれる限りいかなる量でもよく、通常は分散時の
分散液中のY型TiOPcの濃度にして3〜20重量
%、より好ましくは、4〜20重量%程度が好ましい。
分散処理する方法としては、公知の方法例えば、ボール
ミル、サンドグラインドミル、ロールミル等の方法を用
いることができる。これらの中でも、サンドグラインド
ミルを用いる方法が、分散効率等の観点から特に好まし
い。
The amount of the dispersion medium used may be any amount as long as the dispersion can be sufficiently performed and the dispersion contains an effective amount of oxytitanium phthalocyanine. Usually, the concentration of the Y-type TiOPc in the dispersion at the time of dispersion is used. It is preferably about 3 to 20% by weight, more preferably about 4 to 20% by weight.
As a method of performing the dispersion treatment, a known method, for example, a method such as a ball mill, a sand grind mill, and a roll mill can be used. Among these, a method using a sand grind mill is particularly preferable from the viewpoint of dispersion efficiency and the like.

【0014】分散溶液を保持する容器を冷媒により一定
の温度下、制御冷却する方法としては、公知の方法が用
いられる。例えば、ドライアイスによる直接冷却、水、
氷、食塩等寒剤を使用した冷媒、メタノール、ブタノー
ル、グリセリン等を併用した冷媒等も有効である。分散
液の液温度を一定温度に制御維持するためには、分散液
温度管理装置を用いることが好ましい。分散液温度管理
装置は、分散処理中の温度を測定する分散液温度測定手
段と、得られた温度データに基づき、前記分散液保持装
置を冷却する冷媒の流量を制御する冷媒制御手段とを具
備する。分散液温度測定手段としては、分散液中に挿入
された電子温度計等で計測され、同時に冷媒流量制御装
置に信号が送られて流量制御される事により、分散処理
工程が一定の温度下、温度変化(ΔT)も極めて狭い範
囲でなされる。
As a method for controlling and cooling the container holding the dispersion solution with a refrigerant at a constant temperature, a known method is used. For example, direct cooling with dry ice, water,
A refrigerant using a cryogen such as ice and salt, a refrigerant using methanol, butanol, glycerin and the like in combination are also effective. In order to control and maintain the temperature of the dispersion liquid at a constant temperature, it is preferable to use a dispersion liquid temperature management device. The dispersion liquid temperature management device includes a dispersion liquid temperature measurement unit that measures the temperature during the dispersion process, and a refrigerant control unit that controls the flow rate of the refrigerant that cools the dispersion liquid holding device based on the obtained temperature data. I do. As the dispersion liquid temperature measuring means, the dispersion processing step is measured at an electronic thermometer or the like inserted into the dispersion liquid, and simultaneously, a signal is sent to the refrigerant flow control device to control the flow rate, so that the dispersion processing step is performed at a constant temperature. The temperature change (ΔT) is also made in a very narrow range.

【0015】次に、ここで得られた分散液は、塗布する
のに適した液物性にするために、Y型TiOPcの結晶
型を変化させない限り、種々の溶剤を用いて希釈しても
構わない。このような溶剤としては、例えば、前記分散
溶媒として例示した溶媒を使用することができる。結着
樹脂とオキシチタニウムフタロシアニン粒子との混合方
法は例えば、オキシチタニウムフタロシアニン粒子を分
散処理中に結着樹脂を粉末のままあるいはそのポリマー
溶液を加え、同時に分散する方法、分散液を結着樹脂の
ポリマー溶液中に混合する方法、あるいは逆に分散液中
にポリマー溶液を混合する方法等いずれの方法を用いて
も構わない。
Next, in order to obtain liquid properties suitable for coating, the dispersion obtained here may be diluted with various solvents unless the crystal form of Y-type TiOPc is changed. Absent. As such a solvent, for example, the solvents exemplified as the dispersion solvent can be used. The method of mixing the binder resin and the oxytitanium phthalocyanine particles is, for example, a method of dispersing the oxytitanium phthalocyanine particles in a powdery state or adding a polymer solution of the binder resin as it is, and simultaneously dispersing the oxytitanium phthalocyanine particles. Any method such as a method of mixing in a polymer solution or a method of mixing a polymer solution in a dispersion may be used.

【0016】このようにして電荷発生層塗布液が調整さ
れるのである。電荷発生層塗布液を導電性支持体に塗布
する方法としては、公知の塗布方法を用いることができ
る。例えば、浸漬塗布、スプレー塗布、リング塗布等を
用いることができる。この中でも、Y型TiOPcの安
定性や、塗布のし易さ等の観点からは浸漬塗布が望まし
い。
Thus, the coating solution for the charge generation layer is prepared. As a method for applying the charge generation layer coating solution to the conductive support, a known coating method can be used. For example, dip coating, spray coating, ring coating, or the like can be used. Of these, dip coating is desirable from the viewpoint of the stability of Y-type TiOPc and the ease of coating.

【0017】電荷発生層の膜厚としては、0.1μm〜
10μmであることが好ましく、0.5μm〜2μmで
あれば、感度や製造コスト等の観点から特に好ましい。
なお、電荷発生層のみの単層構造で感光層を形成する場
合の電荷発生層の膜厚は5μm〜40μmが好適であ
る。電荷移動層は、電荷移動材と、結着樹脂とを具備す
る。結着樹脂は、電荷発生層と同様のものを用いること
が可能である。
The thickness of the charge generation layer is 0.1 μm to
It is preferably 10 μm, and particularly preferably from 0.5 μm to 2 μm from the viewpoint of sensitivity, manufacturing cost and the like.
When the photosensitive layer is formed with a single layer structure including only the charge generation layer, the thickness of the charge generation layer is preferably 5 μm to 40 μm. The charge transfer layer includes a charge transfer material and a binder resin. As the binder resin, the same resin as the charge generation layer can be used.

【0018】電荷移動材としては公知なものを用いるこ
とができる。例えば、2,4,7−トリニトロフルオレ
ノン、テトラシアノキノジメタン、クロラニル、ジシア
ノビニル−ニトロ−ベンゼン誘導体等の電子吸引性化合
物、カルバゾール、インドール、イミダゾール、オキサ
ゾール、ピラゾール、オキサジアゾール、チアゾール、
ピラゾリン等の複素環化合物、ジアルキルアニリン、ジ
アリールアニリン、ジアリルアニリン、トリフェニルア
ミン等の芳香族アミン誘導体、ヒドラゾン化合物、スチ
ルベン化合物、スチリル系化合物あるいはこれらの構成
要素を主鎖、側鎖に組み込んだ重合体等の電子供与性化
合物を用いることができる。
As the charge transfer material, known materials can be used. For example, electron-withdrawing compounds such as 2,4,7-trinitrofluorenone, tetracyanoquinodimethane, chloranil, dicyanovinyl-nitro-benzene derivative, carbazole, indole, imidazole, oxazole, pyrazole, oxadiazole, thiazole,
Heterocyclic compounds such as pyrazoline, aromatic amine derivatives such as dialkylaniline, diarylaniline, diallylaniline, and triphenylamine, hydrazone compounds, stilbene compounds, styryl compounds, and heavy compounds in which these components are incorporated in the main chain or side chain. An electron donating compound such as a coalescence can be used.

【0019】電荷移動材と結着樹脂との混合割合は、結
着樹脂100重量部に対して、電荷移動材が5〜500
重量部の範囲より使用される。また、電荷移動層は、必
要に応じ、塗布防止剤、増感剤、滑剤他を含んでいても
よい。電荷移動層塗布液は公知の方法を用いて調整する
ことが可能である。
The mixing ratio of the charge transfer material to the binder resin is such that the charge transfer material is 5 to 500 parts per 100 parts by weight of the binder resin.
Used from parts by weight. Further, the charge transfer layer may contain, if necessary, an application inhibitor, a sensitizer, a lubricant and the like. The charge transfer layer coating solution can be adjusted using a known method.

【0020】電荷発生層を形成した後に、電荷移動層塗
布液を塗布する。塗布方法としては、電荷発生層を塗布
する方法と同様の方法を採用することができる。電荷移
動層の膜厚としては10μm〜40μmが好ましく、1
5μm〜30μmであれば、耐刷性等の観点からより好
ましい。中間層は、陽極酸化被膜、酸化アルミニウム、
水酸化アルミニウム等の無機層、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、デンプン、ポリイミド、
ポリアミド等の有機層、酸化チタン、酸化ジルコニウム
等を樹脂中に微分散したハイブリッド材料からなる層な
どが使用される。
After the formation of the charge generation layer, a coating solution for the charge transfer layer is applied. As a coating method, a method similar to the method of coating the charge generation layer can be employed. The thickness of the charge transfer layer is preferably from 10 μm to 40 μm,
A thickness of 5 μm to 30 μm is more preferable from the viewpoint of printing durability and the like. The intermediate layer is an anodized film, aluminum oxide,
Inorganic layers such as aluminum hydroxide, polyvinyl alcohol, casein, polyvinylpyrrolidone, polyacrylic acid, celluloses, gelatin, starch, polyimide,
An organic layer such as polyamide, a layer made of a hybrid material in which titanium oxide, zirconium oxide, or the like is finely dispersed in a resin is used.

【0021】中間層の膜厚は0.1μm〜20μm、好
ましくは0.1μm〜10μmの範囲が好ましい。保護
層は、電子写真感光体の特性を損なわない限り特に限定
されるものではなく、公知の保護層を用いることができ
る。
The thickness of the intermediate layer is in the range of 0.1 μm to 20 μm, preferably 0.1 μm to 10 μm. The protective layer is not particularly limited as long as the characteristics of the electrophotographic photoreceptor are not impaired, and a known protective layer can be used.

【0022】[0022]

【実施例】以下、実施例を用いて本発明電子写真感光体
を具体的に説明する。 実施例1 オキシチタニウムフタロシアニン10重量部に1,2−
ジメトキシエタン140重量部を加え分散溶液とし、該
分散溶液を保持する容器の周囲に冷媒を循環させ、該容
器に取り付けられた電子温度計で分散溶液の温度を測定
し、冷媒制御装置により冷媒の流量を制御することによ
り分散溶液の液温を3℃〜−1℃に維持しながら、サン
ドグラインドミルで5時間、分散処理を行った。次にポ
リビニルブチラール(電気化学工業(株)製、商品名デ
ンカブチラール#6000C)50重量部の10%1,
2−ジメトキシエタン溶液と混合し分散液を作製した。
The electrophotographic photoreceptor of the present invention will be specifically described below with reference to examples. Example 1 To 10 parts by weight of oxytitanium phthalocyanine, 1,2-
140 parts by weight of dimethoxyethane was added to form a dispersion solution, a refrigerant was circulated around a container holding the dispersion solution, and the temperature of the dispersion solution was measured with an electronic thermometer attached to the container. While controlling the flow rate to maintain the liquid temperature of the dispersion solution at 3 ° C. to −1 ° C., dispersion treatment was performed for 5 hours using a sand grind mill. Next, 50% by weight of polyvinyl butyral (manufactured by Denki Kagaku Kogyo Co., Ltd., trade name: Denka butyral # 6000C),
A dispersion was prepared by mixing with a 2-dimethoxyethane solution.

【0023】次にこの分散液をポリエステルフィルム上
に蒸着したアルミニウム蒸着面の上にバーコーターによ
り乾燥後の膜厚が0.4μmとなるように電荷発生層を
設けた。次にこの電荷発生層の上に、次に示すヒドラゾ
ン化合物56重量部と
Next, a charge generation layer was provided on an aluminum-deposited surface on which the dispersion was deposited on a polyester film so that the film thickness after drying was 0.4 μm by a bar coater. Next, 56 parts by weight of a hydrazone compound shown below was placed on the charge generation layer.

【0024】[0024]

【化1】 次に示すヒドラゾン化合物14重量部Embedded image 14 parts by weight of the following hydrazone compound

【0025】[0025]

【化2】 及び下記のシアノ化合物1.5重量部Embedded image And 1.5 parts by weight of the following cyano compound

【0026】[0026]

【化3】 及びポリカーボネート樹脂(三菱化学(株)製、商品名
ノバレックス7030A)100重量部をテトラヒドロ
フラン100重量部に溶解させた液をフィルムアプリケ
ーターにより塗布し、乾燥後の膜厚が17μmとなるよ
うに電荷移動層を設けた。このようにして得られた感光
体を感光体Aとする。
Embedded image And a solution prepared by dissolving 100 parts by weight of a polycarbonate resin (manufactured by Mitsubishi Chemical Corporation, trade name NOVAREX 7030A) in 100 parts by weight of tetrahydrofuran is applied by a film applicator, and charge transfer is performed so that the film thickness after drying becomes 17 μm. Layers were provided. The photoreceptor thus obtained is referred to as photoreceptor A.

【0027】同様にして感光体を5本作成した。これら
の感光体群をA−1〜A−5とする。この感光体の初期
電気特性として帯電圧、半減露光感度及び残留電位を静
電複写紙試験装置(川口電気製作所製、モデルSP−4
28)により測定した。すなわち、暗所でコロナ電流が
22μAになるように設定した印加電圧によるコロナ放
電により感光体を負帯電したときの帯電圧Vo、次いで
1.0luxの照度の白色光を連続的に露光し、表面電
位が−450V〜−90Vに減少するのに要した露光量
(E1/5)、および露光から10秒後の残留電位Vrを
測定した。
Similarly, five photosensitive members were prepared. These photoconductor groups are referred to as A-1 to A-5. As the initial electrical characteristics of the photoreceptor, a charged voltage, half-life exposure sensitivity, and residual potential were measured using an electrostatic copying paper tester (Model SP-4, manufactured by Kawaguchi Electric Works, Ltd.).
28). That is, a charged voltage Vo when the photoreceptor is negatively charged by corona discharge with an applied voltage set so that a corona current is set to 22 μA in a dark place, and then white light having an illuminance of 1.0 lux is continuously exposed, The exposure amount (E1 / 5) required for the potential to decrease from -450 V to -90 V and the residual potential Vr 10 seconds after the exposure were measured.

【0028】実施例2 実施例1において液温を3℃〜−1℃に維持するかわり
に、3℃〜1℃に維持した以外はすべて実施例1と同様
に行い、感光体B(B−1〜B−5)を作製した。 比較例1 実施例1において液温を3℃〜−1℃に維持するかわり
に、室温とし、温度を制御しなかった以外はすべて実施
例1と同様に行い、感光体C(C−1〜C−5)を作製
した。
Example 2 The procedure of Example 1 was repeated, except that the liquid temperature was maintained at 3 ° C. to -1 ° C. instead of 3 ° C. to -1 ° C. 1 to B-5). Comparative Example 1 The procedure of Example 1 was repeated except that the temperature of the solution was kept at 3 ° C. to −1 ° C., and the temperature was not controlled. C-5) was produced.

【0029】比較例2 実施例1において液温を3℃〜−1℃に維持するかわり
に、液温を10度以下−3℃以上とし、温度を制御しな
かった以外はすべて実施例1と同様に行い、感光体D
(D−1〜D−5)を作製した。次に電気特性の測定結
果を表1に示す。
COMPARATIVE EXAMPLE 2 Instead of maintaining the liquid temperature in the range of 3 ° C. to −1 ° C. in Example 1, the liquid temperature was set to 10 ° C. or lower and −3 ° C. or higher and the temperature was not controlled. The same operation is performed, and the photosensitive member D
(D-1 to D-5) were produced. Next, Table 1 shows the measurement results of the electrical characteristics.

【0030】[0030]

【表1】 表1から、明らかな通り、実施例1では特性が良好で優
れ、実施例2では特性かつその再現性も十分満足できる
電子写真感光体が得られた。比較例1、比較例2では特
性がややおとり且つ、再現性にもやや問題があった。こ
れから、Y型TiOPcの分散処理の分散液の温度を一
定に制御することが重要であることがわかる。
[Table 1] As is evident from Table 1, the electrophotographic photoreceptor obtained in Example 1 had good and excellent characteristics, and in Example 2 the characteristics and the reproducibility were sufficiently satisfactory. In Comparative Examples 1 and 2, the characteristics were slightly decoy and the reproducibility had some problems. This indicates that it is important to control the temperature of the dispersion liquid in the dispersion treatment of Y-type TiOPc to be constant.

【0031】[0031]

【発明の効果】本発明によれば、電子写真感光体用の電
荷発生材料として高特性を有するY型TiOPcを用い
た塗布液を安定型結晶型に変化することなく工業生産レ
ベルで製造でき、高感度かつ均質な電子写真感光体を得
ることが可能となる。
According to the present invention, a coating liquid using Y-type TiOPc having high characteristics as a charge generating material for an electrophotographic photosensitive member can be manufactured at an industrial production level without changing to a stable crystal form. A highly sensitive and uniform electrophotographic photosensitive member can be obtained.

Claims (3)

【特許請求の範囲】[Claims] 【請求項1】 X線回折スペクトルにおいて、ブラッグ
角(2θ±0.2°)9.2°、14.3°、24.0
°、及び27.3°に回折ピークを示すオキシチタニウ
ムフタロシアニン結晶を分散媒体中で分散処理させてな
る分散液を用いて感光層を形成させてなる電子写真感光
体の製造方法において、 前記分散処理中の分散液の温度が−3℃〜10℃に維持
され、 かつ、前記分散処理中の分散液の温度変化が4℃以内で
あることを特徴とする電子写真感光体の製造方法。
1. In an X-ray diffraction spectrum, Bragg angles (2θ ± 0.2 °) 9.2 °, 14.3 °, 24.0.
° and 27.3 °, wherein the oxytitanium phthalocyanine crystal having a diffraction peak at 27.3 ° is dispersed in a dispersion medium to form a photosensitive layer using a dispersion liquid. A method for producing an electrophotographic photoreceptor, wherein the temperature of the dispersion in the dispersion is maintained at −3 ° C. to 10 ° C., and the temperature change of the dispersion during the dispersion treatment is within 4 ° C.
【請求項2】 前記分散液の温度が−3℃〜3℃に維持
されている請求項1に記載の電子写真感光体の製造方
法。
2. The method according to claim 1, wherein the temperature of the dispersion is maintained at −3 ° C. to 3 ° C.
【請求項3】 前記分散液の温度変化が2℃以内である
請求項1、または請求項2に記載の電子写真感光体の製
造方法。
3. The method according to claim 1, wherein a temperature change of the dispersion is within 2 ° C.
JP2000180984A 2000-06-16 2000-06-16 Method for producing electrophotographic photosensitive member Expired - Lifetime JP3743268B2 (en)

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Application Number Priority Date Filing Date Title
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JP3743268B2 JP3743268B2 (en) 2006-02-08

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ID=18681977

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Country Link
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2009093024A (en) * 2007-10-10 2009-04-30 Mitsubishi Chemicals Corp Electrophotographic photoreceptor, electrophotographic photoreceptor cartridge and image forming apparatus provided with the photoreceptor

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2009093024A (en) * 2007-10-10 2009-04-30 Mitsubishi Chemicals Corp Electrophotographic photoreceptor, electrophotographic photoreceptor cartridge and image forming apparatus provided with the photoreceptor

Also Published As

Publication number Publication date
JP3743268B2 (en) 2006-02-08

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