JPH06208238A - Electrophotographic receptor and electrophotographic device using the same - Google Patents
Electrophotographic receptor and electrophotographic device using the sameInfo
- Publication number
- JPH06208238A JPH06208238A JP5276936A JP27693693A JPH06208238A JP H06208238 A JPH06208238 A JP H06208238A JP 5276936 A JP5276936 A JP 5276936A JP 27693693 A JP27693693 A JP 27693693A JP H06208238 A JPH06208238 A JP H06208238A
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- Prior art keywords
- layer
- photosensitive member
- electrophotographic photosensitive
- coating layer
- weight
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- Photoreceptors In Electrophotography (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は電子写真感光体及びこの
電子写真感光体を用いた電子写真装置に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an electrophotographic photosensitive member and an electrophotographic apparatus using this electrophotographic photosensitive member.
【０００２】[0002]
【従来の技術】電子写真感光体は基本的には支持体と支
持体上に形成された光導電層とから成っている。しか
し、支持体の欠陥の被覆、光導電層の塗工性向上、光導
電層と支持体との接着性改良、光導電層の電気的破壊に
対する保護、帯電性の向上、支持体から光導電層への電
荷注入性の改良などのために光導電層と支持体との間に
中間層を設けることが有効である。したがって、電子写
真感光体における中間層は被覆性、接着性、機械的強
度、適当な導電性と電気的バリア性などの多くの機能が
要求される。2. Description of the Related Art An electrophotographic photosensitive member basically comprises a support and a photoconductive layer formed on the support. However, it covers the defects of the support, improves the coating property of the photoconductive layer, improves the adhesion between the photoconductive layer and the support, protects the photoconductive layer from electrical damage, improves the charging property, and improves the photoconductivity from the support. It is effective to provide an intermediate layer between the photoconductive layer and the support in order to improve the charge injection property to the layer. Therefore, the intermediate layer in the electrophotographic photosensitive member is required to have many functions such as covering property, adhesive property, mechanical strength, appropriate conductivity and electric barrier property.
【０００３】従来から中間層としては、以下のタイプの
ものが提案されている。 （ｉ）導電性フィラーの含有しない樹脂薄膜。 （ｉｉ）導電性フィラーの含有した樹脂薄膜。 （ｉｉｉ）上記（ｉｉ）の薄膜の上に、上記（ｉ）の薄
膜を積層したもの。Conventionally, the following types of intermediate layers have been proposed. (I) A resin thin film containing no conductive filler. (Ii) A resin thin film containing a conductive filler. (Iii) A thin film of (i) above laminated on the thin film of (ii) above.
【０００４】上記（ｉ）の薄膜は導電性フィラーを含有
しないため膜の抵抗が高く、しかも支持体上の欠陥を被
覆するために厚膜にして用いなければならない。そのた
めに、初期および繰り返し使用時の残留電位が高くなる
という欠点をもっており、上記（ｉ）の薄膜の実用化の
ためには支持体上の欠陥を小さくし、中間層の膜厚を非
常に薄くする必要がある。Since the thin film of (i) above does not contain a conductive filler, the resistance of the film is high, and it must be used as a thick film to cover defects on the support. Therefore, it has a drawback that the residual potential becomes high at initial and repeated use. In order to put the thin film of (i) into practical use, defects on the support are reduced and the thickness of the intermediate layer is made extremely thin. There is a need to.
【０００５】一方、上記（ｉｉ）及び（ｉｉｉ）の薄膜
は、導電性フィラーを分散することによって適当な導電
性を付与できる利点はあるが、導電性フィラーの分散性
が悪いと、中間層の抵抗や誘電率などの電気特性が変化
し、電位特性や画像性に大きな影響を与える。また、フ
ィラーの分散性が悪いと、膜の表面平滑性が悪くなり、
塗工欠陥の原因になる。さらに、フィラーの分散が悪い
と支持体との密着性や機械的強度も低下する。On the other hand, the thin films of (ii) and (iii) above have the advantage that suitable conductivity can be imparted by dispersing the conductive filler, but if the dispersibility of the conductive filler is poor, the intermediate layer of the intermediate layer Electrical characteristics such as resistance and permittivity change, and have a great influence on potential characteristics and image quality. Also, if the dispersibility of the filler is poor, the surface smoothness of the film becomes poor,
It causes coating defects. Further, if the dispersion of the filler is poor, the adhesion to the support and the mechanical strength will also decrease.
【０００６】これまでに中間層の導電性フィラーとし
て、金属（特開昭５８−１８１０５４号公報）や金属酸
化物（特開昭５４−１５１８４３号公報）、金属窒化物
（特開平１−１１８８４８号公報）などが報告されてい
る。So far, as conductive fillers for the intermediate layer, metals (JP-A-58-181054), metal oxides (JP-A-54-151843), and metal nitrides (JP-A-1-1184848). Gazette) etc. have been reported.
【０００７】[0007]
【発明が解決しようとする課題】しかしながら、従来の
導電性フィラーを中間層のフィラーとして用いた電子写
真感光体では、温度、湿度などの環境依存性が大きく、
低温低湿から高温高湿下での全環境に対して常に安定し
た電位特性および画像特性を有する感光体を作成するこ
とが困難であった。たとえば、中間層の抵抗の増大を招
く低温低湿下では、感光体を繰り返し使用した場合、中
間層に電荷が蓄積され残留電位および明部電位が上昇し
た。一方、中間層の抵抗低下を招く高温高湿下において
は、中間層の電気的バリア能が低下し、支持体からキャ
リア注入が加速され、繰り返し使用時における暗部電位
の低下が観測された。その結果、高温高湿下で画像濃度
の低下が起こる他に、反転現像を行う電子写真方式のプ
リンターの場合は、画像に不要な黒点（黒ポチ）が発生
したり、カブリを生じやすくなった。However, in the electrophotographic photosensitive member using the conventional conductive filler as the filler of the intermediate layer, the environmental dependence such as temperature and humidity is large,
It has been difficult to produce a photoconductor having stable potential characteristics and image characteristics in all environments from low temperature and low humidity to high temperature and high humidity. For example, under low temperature and low humidity, which causes an increase in the resistance of the intermediate layer, when the photoconductor was repeatedly used, charges were accumulated in the intermediate layer and the residual potential and the bright part potential increased. On the other hand, under high temperature and high humidity which causes a decrease in the resistance of the intermediate layer, the electrical barrier ability of the intermediate layer was decreased, carrier injection from the support was accelerated, and a decrease in the dark area potential was observed during repeated use. As a result, in addition to a decrease in image density under high temperature and high humidity, in the case of an electrophotographic printer that performs reversal development, unnecessary black spots (black spots) and fogging tend to occur in the image. .
【０００８】このように、環境の変化によって感光体の
特性が変化してしまうのは、導電性フィラーの分散性が
悪いためと考えられる。すなわち、中間層内部における
導電性フィラーの分散性低下によって局所的な抵抗変化
が生じ、そのために電位特性や画像特性が環境変化に受
けやすくなるものと考えられる。As described above, it is considered that the characteristics of the photoconductor are changed due to the change of environment because the dispersibility of the conductive filler is poor. That is, it is considered that a local resistance change occurs due to a decrease in the dispersibility of the conductive filler inside the intermediate layer, which makes the potential characteristics and the image characteristics susceptible to environmental changes.
【０００９】本発明の目的は低温低湿から高温高湿下に
至る全環境下に対して安定した電位特性と画像特性を有
する電子写真感光体を提供すること及びこの電子写真感
光体を用いた電子写真装置を提供することである。An object of the present invention is to provide an electrophotographic photoreceptor having stable potential characteristics and image characteristics under all environments from low temperature and low humidity to high temperature and high humidity, and an electron using this electrophotographic photoreceptor. It is to provide a photographic device.
【００１０】[0010]
【課題を解決するための手段】本発明の電子写真感光体
は、支持体と、前記支持体側から順に中間層と感光層と
を有し、前記中間層に、被覆層を有する硫酸バリウム微
粒子からなる粉体を含有し、かつ前記被覆層を酸化スズ
で形成したものである。The electrophotographic photoreceptor of the present invention comprises a support, an intermediate layer and a photosensitive layer in this order from the support side, and barium sulfate fine particles having a coating layer in the intermediate layer. And a coating layer formed of tin oxide.
【００１１】本発明の電子写真装置は、上記の電子写真
感光体と、前記電子写真感光体を帯電させる帯電手段
と、帯電した前記電子写真感光体に対し像露光を行ない
静電潜像を形成する像露光手段と、静電潜像の形成され
た前記電子写真感光体をトナーで現像する現像手段とを
有するものである。The electrophotographic apparatus of the present invention forms the electrostatic latent image by performing image exposure on the electrophotographic photosensitive member, charging means for charging the electrophotographic photosensitive member, and the charged electrophotographic photosensitive member. And an image exposing unit for developing the electrophotographic photosensitive member on which the electrostatic latent image is formed with a toner.
【００１２】本発明の電子写真感光体は、支持体上に支
持体側から順に中間層と感光層とを有する。中間層には
フィラーとして、導電性被覆層を有する硫酸バリウム微
粒子からなる粉体を含有する。The electrophotographic photosensitive member of the present invention has an intermediate layer and a photosensitive layer on a support in order from the support side. The intermediate layer contains, as a filler, a powder composed of barium sulfate fine particles having a conductive coating layer.
【００１３】硫酸バリウム微粒子は、分散性が非常に優
れている。また、硫酸バリウム微粒子の屈折率は、バイ
ンダー樹脂の屈折率にほぼ等しいため、中間層の光透過
性が低下しない。The barium sulfate fine particles have excellent dispersibility. Moreover, since the refractive index of the barium sulfate fine particles is substantially equal to the refractive index of the binder resin, the light transmittance of the intermediate layer does not decrease.
【００１４】本発明においては、硫酸バリウム微粒子に
導電性被覆層を設けることにより、フィラーとして適切
な比抵抗としている。被覆層としては酸化スズで形成さ
れた被覆層を使用する。被覆層を有する硫酸バリウムか
らなる粉体の比抵抗は０．１〜１０００Ωｃｍ、更には
１〜１０００Ωｃｍが好ましい。In the present invention, by providing a conductive coating layer on the barium sulfate fine particles, a specific resistance suitable as a filler is obtained. A coating layer formed of tin oxide is used as the coating layer. The specific resistance of the powder of barium sulfate having a coating layer is preferably 0.1 to 1000 Ωcm, more preferably 1 to 1000 Ωcm.
【００１５】本発明において、粉体比抵抗は三菱油化製
の抵抗測定装置ロレスタＡＰ（Ｌｏｒｅｓｔａ Ａｐ）
を用いて測定した。測定対象の粉体は、５００ｋｇ／ｃ
ｍ2の圧力でかためてコイン状のサンプルとして上記測
定装置に装着した。In the present invention, the powder resistivity is the resistance measuring device Loresta AP manufactured by Mitsubishi Yuka.
Was measured using. The powder to be measured is 500 kg / c
The sample was attached to the above measuring device as a coin-shaped sample which was warmed up under a pressure of m 2 .
【００１６】被覆層の被覆率は１０〜８０重量％、更に
は３０〜６０重量％が好ましい。被覆層の被覆率とは被
覆層を有する微粒子からなる粉体の重量に対する、この
粉体に使用されている被覆層の全重量の割合である。被
覆層を有する硫酸バリウム微粒子の平均粒径は０．０５
〜１．０μｍ、更には０．０７〜０．７μｍが好まし
い。本発明において、微粒子の平均粒径は遠心沈降法に
より測定した値である。The coverage of the coating layer is preferably 10 to 80% by weight, more preferably 30 to 60% by weight. The coverage of the coating layer is the ratio of the total weight of the coating layer used for this powder to the weight of the powder of fine particles having the coating layer. The average particle diameter of the barium sulfate fine particles having a coating layer is 0.05
.About.1.0 .mu.m, more preferably 0.07 to 0.7 .mu.m. In the present invention, the average particle size of the fine particles is a value measured by the centrifugal sedimentation method.
【００１７】一般に、フィラーの平均粒径が小さくなる
と、分散が難しくなり再凝集しやすくなるが、本発明で
使用するフィラーは、分散性に優れるものである。フィ
ラーの含有量は、中間層に対して１．０〜９０重量％、
更には５．０〜８０重量％が好ましい。Generally, when the average particle size of the filler becomes small, it becomes difficult to disperse and re-aggregate easily, but the filler used in the present invention has excellent dispersibility. The content of the filler is 1.0 to 90% by weight with respect to the intermediate layer,
Further, 5.0 to 80% by weight is preferable.
【００１８】被覆層には、必要に応じてフッ素あるいは
アンチモンを含有してもよい。フッ素あるいはアンチモ
ンを含有させることにより、被覆層の比抵抗を低下させ
ることができる。フッ素あるいはアンチモンを含有した
酸化スズの被覆層は、酸化スズの結晶格子にフッ素原子
あるいはアンチモン原子がとり込まれた固溶体である。
フッ素あるいはアンチモンの含有量は、被覆層に対して
０．０１〜３０重量％、更には０．１〜１０重量％が好
ましい。The coating layer may contain fluorine or antimony, if necessary. By containing fluorine or antimony, the specific resistance of the coating layer can be reduced. The tin oxide coating layer containing fluorine or antimony is a solid solution in which fluorine atoms or antimony atoms are incorporated into the crystal lattice of tin oxide.
The content of fluorine or antimony is preferably 0.01 to 30% by weight, more preferably 0.1 to 10% by weight, based on the coating layer.
【００１９】また、還元法により酸化スズの酸素を欠損
させることによっても、被覆層の比抵抗を低下させるこ
とができる。The specific resistance of the coating layer can also be reduced by depleting the oxygen of tin oxide by the reduction method.
【００２０】本発明の中間層に用いられる結着樹脂とし
ては、例えばフェノール樹脂、ポリウレタン、ポリアミ
ド、ポリイミド、ポリアミドイミド、ポリアミド酸、ポ
リビニールアセタール、エポキシ樹脂、アクリル樹脂、
メラミン樹脂あるいはポリエステルなどが好ましい。こ
れらの樹脂は単独でも、二種以上を組み合わせて用いて
もよい。これらの樹脂は、支持体に対する接着性が良好
であると共に、本発明で使用するフィラーの分散性を向
上させ、かつ成膜後の耐溶剤性が良好である。上記樹脂
の中でも特にフェノール樹脂、ポリウレタン及びポリア
ミド酸が好ましい。Examples of the binder resin used in the intermediate layer of the present invention include phenol resin, polyurethane, polyamide, polyimide, polyamideimide, polyamic acid, polyvinyl acetal, epoxy resin, acrylic resin,
Melamine resin or polyester is preferable. These resins may be used alone or in combination of two or more. These resins have good adhesion to the support, improve the dispersibility of the filler used in the present invention, and have good solvent resistance after film formation. Among the above resins, phenol resin, polyurethane and polyamic acid are particularly preferable.
【００２１】中間層は、例えば浸漬あるいはマイヤーバ
ー等による溶剤塗布で形成することができる。The intermediate layer can be formed, for example, by dipping or solvent coating with a Meyer bar or the like.
【００２２】フィラーの分散性を向上させるために、フ
ィラー表面をカップリング剤（シランカップリング剤や
チタンカップリング剤など）あるいはシリコンオイルな
どの処理剤で処理してもよい。また、上記処理剤を中間
層のバインダー中に含有させてもよい。In order to improve the dispersibility of the filler, the filler surface may be treated with a coupling agent (such as a silane coupling agent or a titanium coupling agent) or a treating agent such as silicone oil. Moreover, you may make the said processing agent contain in the binder of an intermediate | middle layer.
【００２３】中間層の厚みは０．１〜３０μｍ、更には
０．５〜１０μｍが好ましい。また、中間層の体積抵抗
率は１０13Ωｃｍ以下、更には１０12Ωｃｍ以下１０Ω
ｃｍ以上が好ましい。本発明において、体積抵抗率はア
ルミニウム板上に測定対象の中間層を塗布し、更にこの
中間層上に金の薄膜を形成して、アルミニウム板と金薄
膜の両電極間を流れる電流値を pＡメーターで測定して
求めた。The thickness of the intermediate layer is preferably 0.1 to 30 μm, more preferably 0.5 to 10 μm. The volume resistivity of the intermediate layer is 10 13 Ωcm or less, and further 10 12 Ωcm or less 10 Ω.
cm or more is preferable. In the present invention, the volume resistivity is obtained by applying an intermediate layer to be measured on an aluminum plate, further forming a gold thin film on this intermediate layer, and measuring the current value flowing between both electrodes of the aluminum plate and the gold thin film by p It was determined by measuring with an A meter.
【００２４】中間層には、被覆層を有する硫酸バリウム
微粒子からなる粉体以外に、酸化亜鉛や酸化チタン等の
粉体からなるフィラーを含有してもよい。更に、中間層
の表面性を高めるためにレベリング剤を添加してもよ
い。The intermediate layer may contain a filler made of powder of zinc oxide, titanium oxide or the like, in addition to the powder made of barium sulfate fine particles having a coating layer. Furthermore, a leveling agent may be added to enhance the surface properties of the intermediate layer.
【００２５】本発明の感光層は単一層でもよいし、少な
くとも電荷発生層及び電荷輸送層で構成される積層構造
でもよい。The photosensitive layer of the present invention may be a single layer or a laminated structure composed of at least a charge generation layer and a charge transport layer.
【００２６】感光層が単一層の場合、電荷発生物質、電
荷輸送物質を同一層に含有して、同一層内で光キャリア
の生成および移動を行う。When the photosensitive layer is a single layer, a charge generating substance and a charge transporting substance are contained in the same layer to generate and move photocarriers in the same layer.
【００２７】感光層が積層構造の場合、電荷発生物質を
含有する電荷発生層と電荷輸送物質を含有する電荷輸送
層との積層順は、支持体側から電荷発生層、電荷輸送層
の順でもよいし、その逆でもよい。When the photosensitive layer has a laminated structure, the charge generating layer containing the charge generating substance and the charge transporting layer containing the charge transporting substance may be laminated in the order of the charge generating layer and the charge transporting layer from the support side. And vice versa.
【００２８】電荷発生物質としては、例えばアゾ系顔料
（例えばモノアゾ、ビスアゾ、トリスアゾなど）、金属
および無金属のフタロシアニン系顔料、インジゴ系顔料
（例えばインジゴ、チオインジゴなど）、キノン系顔料
（例えばアントアントロン、ピレンキノンなど）、ペリ
レン系顔料（例えばペリレン酸無水物、ペリレン酸イミ
ドなど）、スクワリウム系色素、ピリリウム、チアピリ
リウム塩類、トリフェニルメタン系色素などが挙げられ
る。また、セレン、セレン−テルルあるいはアモルファ
スシリコンなどの無機材料も、発荷発生物質として使用
することができる。Examples of the charge generating substance include azo pigments (eg, monoazo, bisazo, trisazo, etc.), metal and metal-free phthalocyanine pigments, indigo pigments (eg, indigo, thioindigo), quinone pigments (eg, anthanthrone). , Pyrenequinone, etc.), perylene pigments (eg, perylene anhydride, perylene imide, etc.), squalium dyes, pyrylium, thiapyrylium salts, triphenylmethane dyes, and the like. Further, an inorganic material such as selenium, selenium-tellurium, or amorphous silicon can also be used as the charge generation substance.
【００２９】電荷輸送物質としては、電子輸送物質と正
孔輸送物質がある。電子輸送物質と正孔輸送物質として
は、たとえば２，４，７−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、クロラニ
ル、テトラシアノキノジメタンなどが挙げられる。正孔
輸送物質としては、たとえば多環芳香族化合物（例えば
ピレン、アントラセンなど）、複素環化合物（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、トリアゾールなど）、ヒドラ
ゾン系化合物（例えばｐ−ジエチルアミノベンズアルデ
ヒド−Ｎ、Ｎ−ジフェニルヒドラゾン、Ｎ，Ｎ−ジフェ
ニルヒドラジノ−３−メチリデン−９−エチルカルバゾ
ールなど）、スチリル系化合物（例えばα−フェニル−
４′−Ｎ，Ｎ−ジアミノスチルベン、５−［４−（ジ−
ｐ−トリルアミノ）ベンジリデン］−５Ｈ−ジベンゾ
［ａ，ｄ］ジシクロヘプテンなど）、ベンジジン系化合
物、トリアリールアミン系化合物などが挙げられる。The charge transport material includes an electron transport material and a hole transport material. Examples of the electron transporting material and the hole transporting material include 2,4,7-trinitrofluorenone,
2,4,5,7-tetranitrofluorenone, chloranil, tetracyanoquinodimethane and the like can be mentioned. Examples of the hole-transporting substance include polycyclic aromatic compounds (such as pyrene and anthracene) and heterocyclic compounds (such as carbazole, indole, imidazole, oxazole, thiazole, oxadiazole, pyrazole, pyrazoline, thiadiazole, and triazole), Hydrazone compounds (for example, p-diethylaminobenzaldehyde-N, N-diphenylhydrazone, N, N-diphenylhydrazino-3-methylidene-9-ethylcarbazole, etc.), styryl compounds (for example, α-phenyl-
4'-N, N-diaminostilbene, 5- [4- (di-
(p-tolylamino) benzylidene] -5H-dibenzo [a, d] dicycloheptene), benzidine compounds, triarylamine compounds and the like.
【００３０】感光層が単一層の場合感光層の厚みは５〜
１００μｍが好ましく、更には１０〜６０μｍが好まし
い。単一層の感光層には、電荷発生物質及び電荷輸送物
質を各々の１０〜７０重量％、更には２０〜７０重量％
含有するのが好ましい。When the photosensitive layer is a single layer, the thickness of the photosensitive layer is 5 to
The thickness is preferably 100 μm, more preferably 10 to 60 μm. In the single photosensitive layer, the charge generating material and the charge transporting material are respectively 10 to 70% by weight, and further 20 to 70% by weight.
It is preferably contained.
【００３１】感光層が積層構造の場合、電荷発生層の厚
みは０．００１〜５μｍ、更には０．０５〜２μｍが好
ましく、電荷輸送層の厚みは１〜４０μｍ、更には１０
〜３０μｍが好ましい。電荷発生層には、電荷発生物質
を１０〜１００重量％、更には４０〜１００重量％含有
するのが好ましい。電荷輸送層には、電荷輸送物質を２
０〜８０重量％、更には３０〜７０重量％含有するのが
好ましい。When the photosensitive layer has a laminated structure, the thickness of the charge generation layer is preferably 0.001 to 5 μm, more preferably 0.05 to 2 μm, and the thickness of the charge transport layer is 1 to 40 μm, more preferably 10 μm.
-30 μm is preferable. The charge generation layer preferably contains 10 to 100% by weight, and more preferably 40 to 100% by weight of the charge generation substance. The charge transport layer contains 2 charge transport materials.
The content is preferably 0 to 80% by weight, more preferably 30 to 70% by weight.
【００３２】本発明の電子写真感光体は、感光層に使用
する材料を真空蒸着あるいは適当な結着樹脂と組み合わ
せて支持体上に成膜して得られる。The electrophotographic photosensitive member of the present invention can be obtained by forming a film on a support by using the material used for the photosensitive layer in combination with vacuum vapor deposition or an appropriate binder resin.
【００３３】感光層の結着樹脂としては、例えばポリビ
ニルアセタール、ポリカーボネート、ポリスチレン、ポ
リエステル、ポリ酢酸エステル、ポリメタクリル酸エス
テル、アクリル樹脂、セルロース系樹脂などが好ましく
用いられる。As the binder resin for the photosensitive layer, for example, polyvinyl acetal, polycarbonate, polystyrene, polyester, polyacetic acid ester, polymethacrylic acid ester, acrylic resin, cellulose resin and the like are preferably used.
【００３４】感光層の材料の種類によっては中間層から
感光層にフリーキャリアが注入されることがあり、感光
体の帯電能が低下し、画像特性に大きな影響を及ぼす。
この様な場合には、必要に応じて中間層と感光層との間
に電気的バリア性を有するバリア層（たとえば適当な樹
脂薄膜）を設けることによってこのフリーキャリアの注
入を効果的に抑制することができる。バリア層として
は、たとえばポリビニルアルコール、ポリビニルメチル
エーテル、ポリアクリル酸類、メチルセルロース、エチ
ルセルロース、ポリグルタミン酸、カゼイン、でんぷん
などの水溶性樹脂や、ポリアミド、ポリイミド、ポリア
ミドイミド、ポリアミド酸、メラミン樹脂、エポキシ樹
脂、ポリウレタンやポリグルタミン酸エステルなどの樹
脂を用いることができる。特に、塗工性、密着性、耐溶
剤性および電気的バリア性、抵抗などの点でポリアミド
がバリア層として好ましい。ポリアミドとしては、溶液
状態で塗布できるような低結晶性もしくは非結晶性の共
重合ナイロンなどが適当である。バリア層の厚みは、
０．１〜２μｍが好ましい。Free carriers may be injected from the intermediate layer into the photosensitive layer depending on the type of the material of the photosensitive layer, which reduces the charging ability of the photosensitive member and greatly affects the image characteristics.
In such a case, if necessary, a barrier layer having an electric barrier property (for example, a suitable resin thin film) is provided between the intermediate layer and the photosensitive layer to effectively suppress the injection of this free carrier. be able to. The barrier layer, for example, polyvinyl alcohol, polyvinyl methyl ether, polyacrylic acid, methyl cellulose, ethyl cellulose, polyglutamic acid, casein, water-soluble resins such as starch, polyamide, polyimide, polyamideimide, polyamic acid, melamine resin, epoxy resin, Resins such as polyurethane and polyglutamic acid ester can be used. In particular, polyamide is preferable as the barrier layer in terms of coatability, adhesion, solvent resistance, electric barrier property, resistance and the like. As the polyamide, low crystalline or non-crystalline copolymerized nylon that can be applied in a solution state is suitable. The thickness of the barrier layer is
0.1 to 2 μm is preferable.
【００３５】本発明の電子写真感光体においては、感光
層上に保護層を設けてもよい。保護層は主に樹脂で構成
される。保護層を構成する材料としては、例えばポリエ
ステル、ポリウレタン、ポリアリレート、ポリエチレ
ン、ポリスチレン、ポリブタジエン、ポリカーボネー
ト、ポリアミド、ポリプロピレン、ポリイミド、ポリア
ミドイミド、ポリサルホン、ポリアリルエーテル、ポリ
アセタール、ナイロン、フェノール樹脂、アクリル樹
脂、シリコーン樹脂、エポキシ樹脂、ユリア樹脂、アリ
ル樹脂、アルキッド樹脂、ブチラール樹脂などが挙げら
れる。保護層の膜厚は０．０５〜１５μｍ、更には１〜
１０μｍが好ましい。In the electrophotographic photoreceptor of the present invention, a protective layer may be provided on the photosensitive layer. The protective layer is mainly composed of resin. Examples of the material forming the protective layer include polyester, polyurethane, polyarylate, polyethylene, polystyrene, polybutadiene, polycarbonate, polyamide, polypropylene, polyimide, polyamideimide, polysulfone, polyallyl ether, polyacetal, nylon, phenolic resin, acrylic resin, Examples thereof include silicone resin, epoxy resin, urea resin, allyl resin, alkyd resin, butyral resin and the like. The thickness of the protective layer is 0.05 to 15 μm, and further 1 to
10 μm is preferable.
【００３６】支持体はアルミニウム、アルミニウム合
金、銅、チタン、ステンレスなどの金属や合金、また
は、ポリエチレンテレフタレート、ポリブチレンテレフ
タレート、フェノール樹脂、ポリプロピレン、ポリスチ
レンなどの高分子材料、更には、硬質紙などの材料を用
いて製造することができる。支持体の形状は、円筒状、
ベルト状あるいはシート状が好ましい。支持体を構成す
る材料の体積抵抗が高い場合には、導電処理をする必要
がある。導電処理は、支持体上に導電性薄膜を形成した
り、あるいは支持体内に導電性物質を分散させて行なう
ことができる。The support may be a metal or alloy such as aluminum, aluminum alloy, copper, titanium or stainless steel, or a polymer material such as polyethylene terephthalate, polybutylene terephthalate, phenol resin, polypropylene or polystyrene, and further hard paper or the like. It can be manufactured using the material. The shape of the support is cylindrical,
A belt shape or a sheet shape is preferable. When the material constituting the support has a high volume resistance, it is necessary to conduct a conductive treatment. The conductive treatment can be performed by forming a conductive thin film on the support or by dispersing a conductive substance in the support.
【００３７】本発明の電子写真感光体は、電子写真複写
機に利用されるだけでなく、レーザービームプリンタ
ー、ＣＲＴプリンター、ＬＥＤプリンター、液晶プリン
ター、ファクシミリ、レーザー製版などの電子写真応用
技術に広く用いることができる。The electrophotographic photoconductor of the present invention is not only used in electrophotographic copying machines, but also widely used in electrophotographic application techniques such as laser beam printers, CRT printers, LED printers, liquid crystal printers, facsimiles, and laser plate making. be able to.
【００３８】本発明による電子写真感光体は、低温低湿
から高温高湿に至る全環境下に対して、安定した電位特
性と良好な画像形成を実現することができる。The electrophotographic photosensitive member according to the present invention can realize stable potential characteristics and good image formation in all environments from low temperature and low humidity to high temperature and high humidity.
【００３９】次に、本発明の電子写真感光体を備えた電
子写真装置について説明する。図１に本発明のドラム型
感光体を用いた転写式電子写真装置の概略構成を示し
た。図において、１は本発明のドラム型感光体であり、
軸１ａを中心に矢印方向に所定の周速度で回転駆動す
る。該感光体１はその回転過程で帯電手段２によりその
周面に正または負の所定電位の均一帯電を受け、次いで
露光部３にて不図示の像露光手段により光像露光Ｌ（ス
リット露光あるいはレーザービーム走査露光など）を受
ける。これにより感光体周面に露光像に対応した静電潜
像が順次形成されていく。その静電潜像は、次いで現像
手段４でトナー現像され、そのトナー現像像が転写手段
５により不図示の給紙部から感光体１と転写手段５との
間に感光体１の回転と同期取りされて給送された記録材
Ｐの面に順次転写されていく。像転写を受けた記録材Ｐ
は感光体面から分離されて像定着手段８へ導入されて像
定着を受けて複写物（コピー）として機外へプリントア
ウトされる。像転写後の感光体１の表面はクリーニング
手段６にて転写残りトナーの除去を受けて清浄面化さ
れ、前露光手段７により除電処理がされて繰り返して像
形成に使用される。感光体１の均一帯電手段２としては
コロナ帯電装置が一般に広く使用されている。また、転
写装置５もコロナ転写手段が一般に広く使用されてい
る。電子写真装置として、上述の感光体や現像手段、ク
リーニング手段などの構成要素のうち、複数のものを装
置ユニットとして一体に結合して構成し、このユニット
を装置本体に対して着脱自在に構成しても良い。例え
ば、感光体１とクリーニング手段６とを一体化してひと
つの装置ユニットとし、装置本体のレールなどの案内手
段を用いて着脱自在の構成にしてもよい。このとき上記
の装置ユニットのほうに帯電手段および／または現像手
段を伴って構成してもよい。また、光像露光Ｌは、電子
写真装置を複写機やプリンターとして使用する場合に
は、原稿からの反射光や透過光を用いる、あるいは、原
稿を読み取り信号化し、この信号に従ってレーザービー
ムの走査、発光ダイオードアレイの駆動、または液晶シ
ャッターアレイの駆動などを行うことにより行われる。Next, an electrophotographic apparatus provided with the electrophotographic photosensitive member of the present invention will be described. FIG. 1 shows a schematic structure of a transfer type electrophotographic apparatus using the drum type photoreceptor of the present invention. In the figure, 1 is a drum type photoreceptor of the present invention,
It is rotationally driven around the shaft 1a in the arrow direction at a predetermined peripheral speed. In the course of its rotation, the photosensitive member 1 is uniformly charged at its peripheral surface by a predetermined positive or negative potential by a charging means 2, and then at an exposure section 3 an optical image exposure L (slit exposure or slit exposure by an image exposure means not shown). Laser beam scanning exposure). As a result, electrostatic latent images corresponding to the exposed image are sequentially formed on the peripheral surface of the photoconductor. The electrostatic latent image is then toner-developed by the developing means 4, and the toner-developed image is synchronized with the rotation of the photoconductor 1 between the photoconductor 1 and the transfer means 5 from a paper feeding portion (not shown) by the transfer means 5. The images are sequentially transferred onto the surface of the recording material P that has been taken and fed. Recording material P that has received image transfer
Is separated from the surface of the photoconductor and introduced into the image fixing means 8 to undergo image fixing, and is printed out as a copy. After the image transfer, the surface of the photoconductor 1 is cleaned by the cleaning unit 6 to remove the transfer residual toner, and the pre-exposure unit 7 removes the charge to repeatedly use the image. As a uniform charging means 2 for the photoconductor 1, a corona charging device is generally widely used. Also, as the transfer device 5, corona transfer means is generally widely used. The electrophotographic apparatus is configured by integrally combining a plurality of constituent elements such as the photoconductor, the developing unit, and the cleaning unit described above as an apparatus unit, and the unit is configured to be detachable from the apparatus body. May be. For example, the photosensitive member 1 and the cleaning means 6 may be integrated into one device unit, and may be detachably configured by using guide means such as a rail of the device body. At this time, the above-mentioned apparatus unit may be provided with a charging means and / or a developing means. Further, when the electrophotographic apparatus is used as a copying machine or a printer, the light image exposure L uses reflected light or transmitted light from an original, or makes the original read into a signal, and scans a laser beam according to the signal. This is performed by driving the light emitting diode array or the liquid crystal shutter array.
【００４０】[0040]
実施例１ 酸化スズの被覆層を有する硫酸バリウム微粒子からなる
粉体（被覆率５０重量％、粉体比抵抗７００Ωｃｍ）１
２０重量部とレゾール型フェノール樹脂（プライオーフ
ェン Ｊ−３２５、大日本インキ化学工業製、固形分７
０％）７０重量部と、２−メトキシ−１−プロパノール
１００重量部とからなる溶液を約２０時間、ボールミル
で分散した。この分散液に含有するフィラーの平均粒径
は、０．２２μｍであった。Example 1 Powder composed of barium sulfate fine particles having a coating layer of tin oxide (coverage 50% by weight, powder specific resistance 700 Ωcm) 1
20 parts by weight and resol type phenol resin (Priofen J-325, manufactured by Dainippon Ink and Chemicals, solid content 7
0%) 70 parts by weight and 2-methoxy-1-propanol 100 parts by weight were dispersed in a ball mill for about 20 hours. The average particle size of the filler contained in this dispersion was 0.22 μm.
【００４１】このようにして調合した分散液を外径３０
ｍｍ、長さ３６０ｍｍのアルミニウムシリンダー（表面
の粗さＲmax５μｍ）上に浸漬法によって塗布し、１４
０℃で３０分間加熱硬化することにより、厚み１７μｍ
の中間層を形成した。中間層のこの時の表面粗さＲmax
を測定したところ０．５μｍであった。尚、粗さＲmax
はＪＩＳ Ｂ０６０１によるものである。The dispersion prepared in this manner was used to prepare an outer diameter of 30
14 mm, the aluminum cylinder having a length of 360 mm (surface roughness R max 5 μm) was applied by the dipping method, and 14
By heating and curing at 0 ° C for 30 minutes, the thickness is 17 μm.
Was formed. Surface roughness R max of the intermediate layer at this time
Was 0.5 μm. The roughness R max
Is based on JIS B0601.
【００４２】次に、共重合ナイロン樹脂（アミランＣＭ
８０００、東レ製）１０重量部をメタノール６０重量部
とブタノール４０重量部の混合液に溶解した溶液を、前
記中間層の上に浸漬塗布し、９０℃で１０分間加熱乾燥
して厚み０．５μｍのバリア層を形成した。Next, a copolymer nylon resin (Amilan CM
(8000, manufactured by Toray) 10 parts by weight dissolved in a mixed solution of 60 parts by weight of methanol and 40 parts by weight of butanol is dip-coated on the intermediate layer, and dried by heating at 90 ° C. for 10 minutes to give a thickness of 0.5 μm. Barrier layer was formed.
【００４３】次に、オキシチタニウムフタロシアニン顔
料４重量部、ポリビニルブチラール樹脂（ＢＸ−１、積
水化学工業製）２重量部、シクロヘキサノン３４重量部
からなる溶液をサンドミルで８時間分散した後、テトラ
ヒドロフラン６０重量部を加えて電荷発生層用の分散液
を調合した。この分散液を上記のバリア層の上に浸漬塗
布し、８０℃で１０分間加熱乾燥することにより、電荷
発生層を形成した。電荷発生層の膜厚は０．２μｍであ
った。Next, a solution consisting of 4 parts by weight of oxytitanium phthalocyanine pigment, 2 parts by weight of polyvinyl butyral resin (BX-1, manufactured by Sekisui Chemical Co., Ltd.) and 34 parts by weight of cyclohexanone was dispersed in a sand mill for 8 hours, and then 60 parts by weight of tetrahydrofuran. Parts were added to prepare a dispersion liquid for the charge generation layer. This dispersion was applied onto the above barrier layer by dip coating, and dried by heating at 80 ° C. for 10 minutes to form a charge generation layer. The film thickness of the charge generation layer was 0.2 μm.
【００４４】次いで、下記構造で示されるトリアリール
アミン化合物５０重量部と、Then, 50 parts by weight of a triarylamine compound represented by the following structure:
【００４５】[0045]
【外１】 ポリカーボネート樹脂（ユーピロン Ｚ−２００、三菱
瓦斯化学製）５０重量部をモノクロルベンゼン４００重
量部に溶解した溶液を、前記電荷発生層の上に浸漬塗布
し、１２０℃で１時間加熱乾燥して厚み２０μｍの電荷
輸送層を形成した。[Outer 1] A solution prepared by dissolving 50 parts by weight of a polycarbonate resin (Iupilon Z-200, manufactured by Mitsubishi Gas Chemical Co., Ltd.) in 400 parts by weight of monochlorobenzene is dip-coated on the charge generation layer and heated and dried at 120 ° C. for 1 hour to give a thickness of 20 μm. Was formed on the charge transport layer.
【００４６】このようにして作成した本発明の電子写真
感光体を、正現像の電子写真方式の複写機に装着して、
帯電−露光−現像−転写−クリーニングのプロセスを
０．８秒サイクルで繰り返した。この感光体について低
温低湿（１５℃、１５％ＲＨ）および高温高湿（３０
℃、８５％ＲＨ）の環境下で電子写真特性を評価した。
この結果、この感光体は、表１に示すように低温低湿お
よび高温高湿のどちらにおいても、暗部電位（ＶD ）と
明部電位（ＶL ）との間に大きな差を形成することがで
きて十分なコントラストを得ることができた。更に、連
続して１００００枚の記録紙に画像を出したところ、い
ずれの環境でも暗部電位及び明部電位のどちらもほとん
ど変化せず、非常に優れた画質の画像も安定して得られ
た。The electrophotographic photosensitive member of the present invention thus prepared was mounted in a positive development electrophotographic copying machine,
The process of charging-exposure-developing-transfer-cleaning was repeated with a 0.8 second cycle. About this photoreceptor, low temperature and low humidity (15 ° C., 15% RH) and high temperature and high humidity (30
The electrophotographic characteristics were evaluated under the environment of (° C., 85% RH).
As a result, as shown in Table 1, this photoreceptor can form a large difference between the dark portion potential (V D ) and the light portion potential ( VL ) at both low temperature and low humidity and high temperature and high humidity. It was possible to obtain sufficient contrast. Further, when images were continuously printed on 10000 sheets of recording paper, both the dark portion potential and the light portion potential were hardly changed in any environment, and an image of extremely excellent image quality was stably obtained.
【００４７】[0047]
【表１】 [Table 1]
【００４８】実施例２ アルミニウムシリンダーを外径３０ｍｍ、長さ２６０ｍ
ｍのものに代え、その他は、実施例１と同様にして本発
明の電子写真感光体を作成した。得られた電子写真感光
体を、反転現像の電子写真方式のプリンターに装着して
帯電−露光−現像−転写−クリーニングのプロセスを６
秒サイクルで繰り返した。この感光体に対して低温低湿
（１５℃、１５％ＲＨ）および高温高湿（３０℃、８５
％ＲＨ）の環境下で電子写真特性の評価を行った。その
結果、この感光体は、表２に示すように低温低湿および
高温高湿においても、暗部電位（ＶD ）と明部電位（Ｖ
L）との間に大きな差を形成させることができて十分な
コントラストを得ることができた。更に、連続して５０
００枚の記録紙に画像を出したところ、いずれの環境で
も暗部電位及び明部電位のどちらもほとんど変化せず、
また、不要な黒点画像やカブリのない非常に優れた画質
の画像が安定して得られた。Example 2 An aluminum cylinder having an outer diameter of 30 mm and a length of 260 m
An electrophotographic photosensitive member of the present invention was prepared in the same manner as in Example 1 except that m was replaced by m. The obtained electrophotographic photosensitive member is attached to an electrophotographic printer of reversal development, and the charging-exposure-developing-transfer-cleaning process is performed.
Repeated every second cycle. For this photoreceptor, low temperature and low humidity (15 ° C, 15% RH) and high temperature and high humidity (30 ° C, 85%
% RH) and electrophotographic characteristics were evaluated. As a result, as shown in Table 2, this photoconductor has a dark portion potential (V D ) and a light portion potential (V
It was possible to form a large difference with L ) and obtain sufficient contrast. Furthermore, 50 consecutively
When an image was printed on 00 sheets of recording paper, both the dark potential and the bright potential did not change in any environment,
In addition, an image with excellent image quality without unnecessary black spot images or fog was stably obtained.
【００４９】[0049]
【表２】 [Table 2]
【００５０】実施例３〜６ 実施例１の中間層を、下記の塗工液を用いて形成した中
間層にかえ、その他は実施例１と同様にして、実施例３
〜６のそれぞれの電子写真感光体を作成した。実施例３
の中間層用塗工液に含有するフィラーの平均粒径は０．
２７μｍであった。また、実施例４の中間層用塗工液に
含有するフィラーの平均粒径は０．２５μｍであった。Examples 3 to 6 The intermediate layer of Example 1 was replaced with an intermediate layer formed by using the following coating liquid, and otherwise the same as in Example 1 except that Example 3 was used.
Each of the electrophotographic photoconductors Nos. 6 to 6 was produced. Example 3
The average particle size of the filler contained in the coating liquid for the intermediate layer is 0.
It was 27 μm. The average particle size of the filler contained in the coating liquid for intermediate layer of Example 4 was 0.25 μm.
【００５１】こうして作成した各電子写真感光体につい
て、実施例１と同様にして評価した。その結果、これら
の感光体は、表３に示すように低温低湿および高温高湿
のどちらにおいても、暗部電位（ＶD ）と明部電位（Ｖ
L ）との間に大きな差を形成することができて十分なコ
ントラストを得ることができた。更に、連続して１００
００枚の記録紙に画像を出したところ、いずれの環境で
も暗部電位及び明部電位のどちらもほとんど変化せず、
非常に優れた画質の画像も安定して得られた。The electrophotographic photosensitive members thus prepared were evaluated in the same manner as in Example 1. As a result, as shown in Table 3, these photoconductors have a dark portion potential (V D ) and a light portion potential (V D ) at both low temperature and low humidity and high temperature and high humidity.
It was possible to form a large difference with L ) and obtain a sufficient contrast. In addition, 100 consecutively
When an image was printed on 00 sheets of recording paper, both the dark potential and the bright potential did not change in any environment,
Images of excellent quality were also stably obtained.
【００５２】実施例３の塗工液 ・フッ素含有の酸化スズ被覆層を有する硫酸バリウム微
粒子からなる粉体（被覆率５０重量％、被覆層における
フッ素含有率９重量％、粉体比抵抗４０Ωｃｍ）１５０
重量部 ・実施例１と同様のレゾール型フェノール樹脂 ７０重
量部 ・２−メトキシ−１−プロパノール １００重量部 Coating liquid of Example 3 Powder containing barium sulfate fine particles having a fluorine-containing tin oxide coating layer (coating rate 50% by weight, fluorine content in coating layer 9% by weight, powder specific resistance 40 Ωcm) 150
Parts by weight-70 parts by weight of resol-type phenol resin similar to Example 1-100 parts by weight of 2-methoxy-1-propanol
【００５３】実施例４の塗工液 ・アンチモン含有の酸化スズ被覆層を有する硫酸バリウ
ム微粒子からなる粉体（被覆率５０重量％、被覆層にお
けるアンチモン含有率９重量％、粉体比抵抗３０Ωｃ
ｍ） １００重量部 ・実施例１と同様のレゾール型フェノール樹脂 ７０重
量部 ・２−メトキシ−１−プロパノール ８０重量部Powder of barium sulfate fine particles having an antimony-containing tin oxide coating layer of the coating liquid of Example 4 (covering rate 50% by weight, antimony content in coating layer 9% by weight, powdery specific resistance 30 Ωc
m) 100 parts by weight-Resole type phenolic resin similar to that of Example 1 70 parts by weight-2-Methoxy-1-propanol 80 parts by weight
【００５４】実施例５の塗工液 ・実施例１と同様の硫酸バリウム微粒子からなる粉体
１２０重量部 ・ポリエステルポリウレタン（ニッポラン２３０４、日
本ポリウレタン製） ７０重量部 ・２−メトキシ−１−プロパノール １００重量部 Coating liquid of Example 5 : Powder containing barium sulfate fine particles similar to that of Example 1
120 parts by weight Polyester polyurethane (Nipporan 2304, made by Nippon Polyurethane) 70 parts by weight 2-Methoxy-1-propanol 100 parts by weight
【００５５】実施例６の塗工液 ・実施例３と同様の硫酸バリウム微粒子からなる粉体
１００重量部 ・下記構造式のポリアミド酸樹脂（重量平均分子量８５
００） ５０重量部 Coating liquid of Example 6・ Powder made of barium sulfate fine particles similar to that of Example 3
100 parts by weight Polyamic acid resin having the following structural formula (weight average molecular weight 85
00) 50 parts by weight
【００５６】[0056]
【外２】 ・Ｎ，Ｎ−ジメチルアセトアミド １７０重量部[Outside 2] -N, N-dimethylacetamide 170 parts by weight
【００５７】[0057]
【表３】 [Table 3]
【００５８】比較例１および２ 実施例１の中間層を、下記の塗工液を用いて形成した中
間層にかえ、その他は実施例１と同様にして、比較例１
および２のそれぞれの電子写真感光体を作成した。比較
例１の中間層用塗工液に含有するフィラーの平均粒径は
０．２５μｍであった。また、比較例２の中間層用塗工
液に含有するフィラーの平均粒径は０．２０μｍであっ
た。Comparative Examples 1 and 2 The intermediate layer of Example 1 was replaced with an intermediate layer formed by using the following coating liquid, and otherwise the same as in Example 1 and Comparative Example 1
Electrophotographic photoreceptors of 2 and 2 were prepared. The average particle size of the filler contained in the coating liquid for intermediate layer of Comparative Example 1 was 0.25 μm. The average particle size of the filler contained in the coating liquid for intermediate layer of Comparative Example 2 was 0.20 μm.
【００５９】こうして作成した各電子写真感光体につい
て、実施例１と同様にして評価した。その結果、表４に
示すようにいずれの感光体も初期においては暗部電位
（ＶD）と明部電位（ＶL ）との間に大きな差を形成す
ることができて十分なコントラストを得られたが、連続
して１００００枚の記録紙に画像形成したところ、いず
れの電子写真感光体も低温低湿の環境下で暗部電位の降
下および明部電位の上昇が見られた。Each electrophotographic photosensitive member thus prepared was evaluated in the same manner as in Example 1. As a result, as shown in Table 4, any of the photoconductors can form a large difference between the dark portion potential (V D ) and the light portion potential ( VL ) in the initial stage, and sufficient contrast can be obtained. However, when images were continuously formed on 10000 sheets of recording paper, a drop in dark part potential and a rise in light part potential were observed in all electrophotographic photoconductors under a low temperature and low humidity environment.
【００６０】比較例１の塗工液 ・アンチモン含有の酸化スズの被覆層を有する酸化チタ
ン微粒子からなる粉体（ＥＣＴＴ−１、チタン工業製）
１５０重量部 ・実施例１と同様のレゾール型フェノール樹脂 ７５重
量部 ・メチルセロソルブ ６０重量部 ・メタノール １５重量部Powder of fine particles of titanium oxide having a coating layer of the coating liquid of Comparative Example 1 and antimony-containing tin oxide (ECTT-1, manufactured by Titanium Industry Co., Ltd.)
150 parts by weight-Resol type phenolic resin similar to Example 1 75 parts by weight-Methylcellosolve 60 parts by weight-Methanol 15 parts by weight
【００６１】比較例２の塗工液 ・アンチモン含有の酸化スズ微粒子からなる粉体（Ｔ−
１、三菱マテリアル製）１００重量部 ・実施例５と同様のポリエステルポリウレタン ７０重
量部 ・２−メトキシ−１−プロパノール ８０重量部Powder of the coating solution of Comparative Example 2 and tin oxide fine particles containing antimony (T-
100 parts by weight of Mitsubishi Materials) 70 parts by weight of the same polyester polyurethane as in Example 5 80 parts by weight of 2-methoxy-1-propanol
【００６２】[0062]
【表４】 [Table 4]
【００６３】実施例７〜１０ アルミニウムシリンダーを外径３０ｍｍ、長さ２６０ｍ
ｍのものに代えその他は、実施例３〜６と同様にして、
実施例７（実施例３の中間層を使用）、実施例８（実施
例４の中間層を使用）、実施例９（実施例５の中間層を
使用）及び実施例１０（実施例６の中間層を使用）の電
子写真感光体を作成した。Examples 7 to 10 Aluminum cylinders having an outer diameter of 30 mm and a length of 260 m
Other than m, the same as in Examples 3 to 6, except that
Example 7 (using the intermediate layer of Example 3), Example 8 (using the intermediate layer of Example 4), Example 9 (using the intermediate layer of Example 5) and Example 10 (using the intermediate layer of Example 6). An electrophotographic photosensitive member (using an intermediate layer) was prepared.
【００６４】こうして作成した各電子写真感光体につい
て、実施例２と同様に評価した。その結果、これらの感
光体は表５に示すように低温低湿および高温高湿におい
ても暗部電位（ＶD ）と明部電位（ＶL ）との間に大き
な差を形成させることができて十分なコントラストを得
ることができた。更に、連続して５０００枚の記録紙に
画像を出したところ、いずれの環境でも暗部電位及び明
部電位のどちらもほとんど変化せず、また、不要な黒点
画像やカブリのない非常に優れた画質の画像が安定して
得られた。The electrophotographic photosensitive members thus prepared were evaluated in the same manner as in Example 2. As a result, as shown in Table 5, these photoreceptors can form a large difference between the dark portion potential (V D ) and the light portion potential ( VL ) even at low temperature and low humidity and high temperature and high humidity. It was possible to obtain a good contrast. Furthermore, when images were continuously printed on 5000 sheets of recording paper, both the dark part potential and the light part potential hardly changed in any environment, and the image quality was excellent without unnecessary black spot images or fog. The image of was stably obtained.
【００６５】[0065]
【表５】 [Table 5]
【００６６】比較例３および４ アルミニウムシリンダーを外径３０ｍｍ、長さ２６０ｍ
ｍのものに代えその他は、比較例１および２と同様にし
て、比較例３（比較例１の中間層を使用）及び比較例４
（比較例２の中間層を使用）の電子写真感光体を作成し
た。Comparative Examples 3 and 4 An aluminum cylinder having an outer diameter of 30 mm and a length of 260 m.
Comparative Example 3 (using the intermediate layer of Comparative Example 1) and Comparative Example 4 in the same manner as in Comparative Examples 1 and 2 except that m was replaced by m.
An electrophotographic photosensitive member (using the intermediate layer of Comparative Example 2) was prepared.
【００６７】こうして作成した各電子写真感光体につい
て、実施例２と同様に評価した。その結果、表６に示す
ようにいずれの感光体も初期においては暗部電位（Ｖ
D ）と明部電位（ＶL ）との間に大きな差を形成するこ
とができて十分なコントラストを得ることができたが、
連続して５０００枚の記録紙に画像形成したところ、い
ずれの電子写真感光体についても高温高湿の環境下で暗
部電位の降下が見られた。また、高温高湿の環境下では
初期から記録紙上に不要な黒点が認められた。The electrophotographic photosensitive members thus prepared were evaluated in the same manner as in Example 2. As a result, as shown in Table 6, all the photoconductors initially have a dark part potential (V
It was possible to form a large difference between D ) and the bright part potential ( VL ) and obtain a sufficient contrast.
When images were continuously formed on 5,000 sheets of recording paper, a drop in the dark area potential was observed in any of the electrophotographic photoreceptors under a high temperature and high humidity environment. In the high temperature and high humidity environment, unnecessary black dots were observed on the recording paper from the beginning.
【００６８】[0068]
【表６】 [Table 6]
【００６９】実施例１１ 実施例１で用いた中間層用分散液を、実施例１と同様の
アルミニウムシリンダー上に浸漬法によって塗布し、１
４０℃で３０分乾燥硬化することにより、厚み５μｍの
中間層を形成した。Example 11 The intermediate layer dispersion liquid used in Example 1 was applied onto the same aluminum cylinder as in Example 1 by a dipping method, and 1
By drying and curing at 40 ° C. for 30 minutes, an intermediate layer having a thickness of 5 μm was formed.
【００７０】次に下記構造式のビスアゾ顔料５重量部
に、Next, to 5 parts by weight of a bisazo pigment having the following structural formula,
【００７１】[0071]
【外３】 テトラヒドロフラン９０重量部加えて２０時間サンドミ
ルで分散した。この液にブチラール樹脂（ＢＬＳ、積水
化学工業製）２．５重量部をテトラヒドロフラン２０重
量部に溶かした溶液を加えて更に２時間分散した。この
分散液にシクロヘキサノン１００重量部とテトラヒドロ
フラン１００重量部を加えて希釈し、前記中間層の上に
膜厚が０．２μｍになるようにマイヤーバーで塗布して
電荷発生層を形成した。[Outside 3] 90 parts by weight of tetrahydrofuran was added and dispersed by a sand mill for 20 hours. A solution of 2.5 parts by weight of butyral resin (BLS, manufactured by Sekisui Chemical Co., Ltd.) in 20 parts by weight of tetrahydrofuran was added to this liquid, and the mixture was further dispersed for 2 hours. To this dispersion, 100 parts by weight of cyclohexanone and 100 parts by weight of tetrahydrofuran were added for dilution, and the intermediate layer was coated with a Mayer bar to a thickness of 0.2 μm to form a charge generation layer.
【００７２】次いで、下記構造式のスチリル化合物５０
重量部と、Then, a styryl compound 50 having the following structural formula
Parts by weight,
【００７３】[0073]
【外４】 ポリカーボネート樹脂（ユーピロン Ｚ−２００、三菱
瓦斯化学製）５０重量部をモノクロルベンゼン４００重
量部に溶解した溶液を、前記電荷発生層の上に浸漬塗布
し、１２０℃で１時間加熱乾燥して厚み２０μｍの電荷
輸送層を形成して本発明の電子写真感光体を作成した。[Outside 4] A solution prepared by dissolving 50 parts by weight of a polycarbonate resin (Iupilon Z-200, manufactured by Mitsubishi Gas Chemical Co., Ltd.) in 400 parts by weight of monochlorobenzene is dip-coated on the charge generation layer and heated and dried at 120 ° C. for 1 hour to give a thickness of 20 μm. The charge transporting layer was formed to prepare an electrophotographic photoreceptor of the present invention.
【００７４】こうして作成した電子写真感光体につい
て、実施例１と同様にして評価した。その結果、これら
の感光体は、表７に示したように低温低湿および高温高
湿のどちらにおいても、暗部電位（ＶD ）と明部電位
（ＶL ）との間の大きな差を形成することができて十分
なコントラストを得ることができた。更に、連続して１
００００枚記録紙に画像を出したところ、いずれの環境
でも暗部電位及び明部電位のどちらもほとんど変化せ
ず、非常に優れた画質の画像も安定して得られた。The electrophotographic photosensitive member thus prepared was evaluated in the same manner as in Example 1. As a result, these photoreceptors form a large difference between the dark potential (V D ) and the light potential ( VL ) at both low temperature and low humidity and high temperature and high humidity, as shown in Table 7. It was possible to obtain sufficient contrast. Furthermore, 1 in succession
When an image was printed on 0000 sheets of recording paper, both the dark portion potential and the light portion potential were hardly changed in any environment, and an image of extremely excellent image quality was stably obtained.
【００７５】[0075]
【表７】 [Table 7]
【００７６】実施例１２ 中間層用分散液として、実施例３で用いたものを用い、
その他は実施例１１と同様にして本発明の電子写真感光
体を作成した。Example 12 As the dispersion liquid for the intermediate layer, the one used in Example 3 was used.
An electrophotographic photosensitive member of the present invention was prepared in the same manner as in Example 11 except for the above.
【００７７】こうして作成した電子写真感光体につい
て、実施例１と同様に評価した。その結果、この感光体
は表８で示したように、低温低湿および高温高湿におい
ても暗部電位（ＶD ）と明部電位（ＶL ）との間の大き
な差を形成することができて十分なコントラストを得る
ことができた。更に、連続して１００００枚記録紙に画
像を出したところ、いずれの環境でも暗部電位及び明部
電位のどちらもほとんど変化せず、非常に優れた画質の
画像も安定して得られた。The electrophotographic photosensitive member thus prepared was evaluated in the same manner as in Example 1. As a result, as shown in Table 8, this photosensitive member was able to form a large difference between the dark portion potential (V D ) and the light portion potential ( VL ) even at low temperature and low humidity and high temperature and high humidity. We were able to obtain sufficient contrast. Further, when images were continuously printed on 10000 sheets of recording paper, neither the dark portion potential nor the light portion potential changed substantially in any environment, and an image of extremely excellent image quality was stably obtained.
【００７８】[0078]
【表８】 [Table 8]
【図１】本発明の電子写真感光体を用いた電子写真装置
の一例を示す側面図である。FIG. 1 is a side view showing an example of an electrophotographic apparatus using an electrophotographic photosensitive member of the present invention.
１ 電子写真感光体 ２ 帯電手段 ３ 露光部 ４ 現像手段 ５ 転写手段 ６ クリーニング手段 ７ 前露光手段 ８ 像定着手段 DESCRIPTION OF SYMBOLS 1 Electrophotographic photosensitive member 2 Charging means 3 Exposure part 4 Developing means 5 Transfer means 6 Cleaning means 7 Pre-exposure means 8 Image fixing means
───────────────────────────────────────────────────── フロントページの続き (72)発明者 島田 明 東京都大田区下丸子３丁目30番２号キヤノ ン株式会社内 (72)発明者 佐藤 一馬 東京都大田区下丸子３丁目30番２号キヤノ ン株式会社内 ─────────────────────────────────────────────────── ─── Continuation of front page (72) Akira Shimada 3-30-2 Shimomaruko, Ota-ku, Tokyo Canon Inc. (72) Inventor Kazuma Sato 3-30-2 Shimomaruko, Ota-ku, Tokyo Canon Within the corporation
Claims (10)
感光層とを有し、前記中間層に、被覆層を有する硫酸バ
リウム微粒子からなる粉体を含有し、かつ前記被覆層を
酸化スズで形成したことを特徴とする電子写真感光体。1. A support, an intermediate layer and a photosensitive layer in this order from the support, wherein the intermediate layer contains a powder of barium sulfate fine particles having a coating layer, and the coating layer is oxidized. An electrophotographic photoconductor characterized by being formed of tin.
％である請求項１記載の電子写真感光体。2. The electrophotographic photosensitive member according to claim 1, wherein the coating rate of the coating layer is 10 to 80% by weight.
求項２記載の電子写真感光体。3. The electrophotographic photosensitive member according to claim 2, wherein the coverage is 30 to 60% by weight.
ンを含有する請求項１記載の電子写真感光体。4. The electrophotographic photosensitive member according to claim 1, wherein the coating layer contains fluorine or antimony.
有量が、前記被覆層に対して０．０１〜３０重量％であ
る請求項４記載の電子写真感光体。5. The electrophotographic photosensitive member according to claim 4, wherein the content of the fluorine or the antimony is 0.01 to 30% by weight based on the coating layer.
請求項５記載の電子写真感光体。6. The electrophotographic photosensitive member according to claim 5, wherein the content is 0.1 to 10% by weight.
ル樹脂、ポリウレタン、ポリアミド、ポリイミド、ポリ
アミドイミド、ポリアミド酸、ポリビニールアセター
ル、エポキシ樹脂、アクリル樹脂、メラミン樹脂および
ポリエステルからなる群から選ばれたものを用いる請求
項１記載の電子写真感光体。7. The binder resin for the intermediate layer is selected from the group consisting of phenol resin, polyurethane, polyamide, polyimide, polyamideimide, polyamic acid, polyvinyl acetal, epoxy resin, acrylic resin, melamine resin and polyester. The electrophotographic photosensitive member according to claim 1, wherein the electrophotographic photosensitive member is used.
ポリウレタン及び、ポリアミド酸のうちから選ばれたも
のを用いる請求項７記載の電子写真感光体。8. A phenol resin as the binder resin,
The electrophotographic photosensitive member according to claim 7, wherein one selected from polyurethane and polyamic acid is used.
ア層を有する請求項１記載の電子写真感光体。9. The electrophotographic photosensitive member according to claim 1, further comprising a barrier layer between the intermediate layer and the photoconductive layer.
記電子写真感光体を帯電させる帯電手段と、帯電した前
記電子写真感光体に対し像露光を行ない静電潜像を形成
する像露光手段と、静電潜像の形成された前記電子感光
体をトナーで現像する現像手段とを有することを特徴と
する電子写真装置。10. The electrophotographic photosensitive member according to claim 1, charging means for charging the electrophotographic photosensitive member, and image exposure for forming an electrostatic latent image by performing image exposure on the charged electrophotographic photosensitive member. An electrophotographic apparatus comprising: a developing unit and a developing unit that develops the electrophotographic photosensitive member on which the electrostatic latent image is formed with toner.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP05276936A JP3118129B2 (en) | 1992-11-06 | 1993-11-05 | Electrophotographic photoreceptor, apparatus unit using the electrophotographic photoreceptor, and electrophotographic apparatus |
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP29724992 | 1992-11-06 | ||
| JP4-297249 | 1992-11-06 | ||
| JP05276936A JP3118129B2 (en) | 1992-11-06 | 1993-11-05 | Electrophotographic photoreceptor, apparatus unit using the electrophotographic photoreceptor, and electrophotographic apparatus |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH06208238A true JPH06208238A (en) | 1994-07-26 |
| JP3118129B2 JP3118129B2 (en) | 2000-12-18 |
Family
ID=26552170
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP05276936A Expired - Fee Related JP3118129B2 (en) | 1992-11-06 | 1993-11-05 | Electrophotographic photoreceptor, apparatus unit using the electrophotographic photoreceptor, and electrophotographic apparatus |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3118129B2 (en) |
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| US7135261B2 (en) | 2002-08-26 | 2006-11-14 | Fuji Electric Imaging Device Co., Ltd. | Multi-layered organic electrophotographic photoconductor |
| US7371491B2 (en) | 2003-09-30 | 2008-05-13 | Ricoh Company Limited | Electrophotographic photoreceptor, method for manufacturing the electrophotographic photoreceptor, and image forming apparatus and process cartridge using the electrophotographic photoreceptor |
| US7442479B2 (en) | 2004-07-08 | 2008-10-28 | Ricoh Company, Limited | Electrophotographic photoreceptor, and image forming apparatus and process cartridge using the electrophotographic photoreceptor |
| US7507511B2 (en) | 2005-01-14 | 2009-03-24 | Ricoh Company Ltd. | Electrophotographic photoreceptor, and image forming apparatus and process cartridge therefor using the electrophotographic photoreceptor |
| US7534537B2 (en) | 2005-04-12 | 2009-05-19 | Canon Kabushiki Kaisha | Electrophotographic photosensitive member, process cartridge and electrophotographic apparatus |
| US7537872B2 (en) | 2005-04-13 | 2009-05-26 | Ricoh Company Limited | Image bearing member with charge blocking layer and moire prevention layer, and image forming apparatus and process cartridge using the same |
| US7560203B2 (en) | 2003-12-01 | 2009-07-14 | Ricoh Company, Ltd. | Electrophotographic photoreceptor, method of image formation, image formation apparatus and process cartridge for image formation apparatus |
| US7670743B2 (en) | 2005-03-04 | 2010-03-02 | Ricoh Company, Ltd. | Image forming method |
| US7732113B2 (en) | 2005-03-28 | 2010-06-08 | Canon Kabushiki Kaisha | Electrophotographic photosensitive member, process cartridge and electrophotographic apparatus, and process for producing electrophotographic photosensitive member |
| JP2010191373A (en) * | 2009-02-20 | 2010-09-02 | Sharp Corp | Coating solution for intermediate layer of electrophotographic photoreceptor having organic photosensitive layer and application for the same |
| WO2012118230A1 (en) | 2011-03-03 | 2012-09-07 | Canon Kabushiki Kaisha | Electrophotographic photosensitive member, process cartridge and electrophotographic apparatus, and method of manufacturing electrophotographic photosensitive member |
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- 1993-11-05 JP JP05276936A patent/JP3118129B2/en not_active Expired - Fee Related
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| JP3118129B2 (en) | 2000-12-18 |
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