JPH04356055A - electrophotographic photoreceptor - Google Patents
electrophotographic photoreceptorInfo
- Publication number
- JPH04356055A JPH04356055A JP19661191A JP19661191A JPH04356055A JP H04356055 A JPH04356055 A JP H04356055A JP 19661191 A JP19661191 A JP 19661191A JP 19661191 A JP19661191 A JP 19661191A JP H04356055 A JPH04356055 A JP H04356055A
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- Japan
- Prior art keywords
- weight
- pigment
- intermediate layer
- titanium
- parts
- 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.)
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- Photoreceptors In Electrophotography (AREA)
Abstract
Description
【0001】0001
【産業上の利用分野】本発明は、電子写真感光体に関す
る。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an electrophotographic photoreceptor.
【0002】0002
【従来の技術】従来、中間層を有する電子写真感光体が
あるが、この中間層の機能として
(1)優れた帯電安定性
(2)低残留電位
(3)干渉縞の防止(可干渉光を書込み光源とする電子
写真プロセスの場合)
(4)厚膜化が可能であり、粗悪表面基体の使用可能化
(5)高感度化等が挙げられる。[Prior Art] Conventionally, there is an electrophotographic photoreceptor having an intermediate layer.The functions of this intermediate layer are (1) excellent charging stability, (2) low residual potential, (3) prevention of interference fringes (coherent light In the case of an electrophotographic process using a writing light source as a writing light source) (4) It is possible to make a thick film, and it is possible to use a substrate with a poor surface. (5) It is possible to increase sensitivity.
【0003】これらの機能の実現のため、多くの中間層
が提案されている。例えば、
(a)樹脂のみからなる薄い層
この場合は、上記(1)、(2)の機能に対してある程
度の効果がある。[0003] Many intermediate layers have been proposed to realize these functions. For example, (a) A thin layer made only of resin. In this case, this has a certain degree of effect on the functions (1) and (2) above.
【0004】(b)樹脂に顔料を分散した層。(b) A layer in which a pigment is dispersed in a resin.
【0005】この場合は、(2)の機能に対してはある
程度の効果があり、さらに使用する顔料の種類によって
は(3)、(5)に対しても効果がある。すなわち、屈
折率と顔料粒径が大きければ(3)に効果があり、書込
み光波長における反射率が大きければ基体の種類に関係
なく(5)の効果が期待できる。In this case, there is a certain degree of effect on function (2), and depending on the type of pigment used, there is also an effect on function (3) and (5). That is, if the refractive index and pigment particle size are large, the effect (3) is obtained, and if the reflectance at the writing light wavelength is large, the effect (5) can be expected regardless of the type of substrate.
【0006】(c)樹脂に導電性顔料を分散した層の上
に、樹脂のみの層を設ける。(c) A layer made only of resin is provided on a layer in which a conductive pigment is dispersed in resin.
【0007】この場合には(1)〜(4)の効果が期待
できる。In this case, the effects (1) to (4) can be expected.
【0008】しかしながら、(a)の場合、一般には比
較的抵抗の低い樹脂を用いる必要があり、これらの樹脂
は一般に吸湿性が高い。従って(a)の中間層を用いた
感光体は、環境依存性が大きく、低湿時に残留電位が上
昇し、高湿時には帯電性が低下する。However, in the case of (a), it is generally necessary to use a resin with relatively low resistance, and these resins are generally highly hygroscopic. Therefore, a photoreceptor using the intermediate layer (a) has a large environmental dependence, and the residual potential increases when the humidity is low, and the charging property decreases when the humidity is high.
【0009】(b)の場合、使用する顔料の特性に感光
体の特性が大きく影響され、特に帯電安定性と低残留電
位を両立させる顔料は単独ではほとんど存在せず、実用
上、中間層として十分とは言えない。In the case of (b), the characteristics of the photoreceptor are greatly influenced by the characteristics of the pigment used, and in particular, there are almost no pigments that can achieve both charging stability and low residual potential on their own, and in practice, they are not suitable for use as an intermediate layer. I can't say it's enough.
【0010】(c)の場合、二層構成であり製造工程が
多くなり、コスト的に不利である。また樹脂のみの層が
あるため、(a)の場合と同様の欠点がある。In the case of (c), it has a two-layer structure and requires many manufacturing steps, which is disadvantageous in terms of cost. Furthermore, since there is a layer made only of resin, there are the same drawbacks as in case (a).
【0011】以上、述べたように従来技術の中間層は機
能が不十分であり、かつ欠点を有している。As described above, the intermediate layer of the prior art has insufficient functionality and has drawbacks.
【0012】0012
【発明が解決しようとする課題】本発明は、こうした実
状の下に干渉縞の防止をはじめ上記中間層に要求される
機能の全てを満足する電子写真感光体を提供することを
目的とするものである。SUMMARY OF THE INVENTION Under these circumstances, it is an object of the present invention to provide an electrophotographic photoreceptor that satisfies all of the functions required of the intermediate layer, including the prevention of interference fringes. It is.
【0013】[0013]
【課題を解決するための手段】本発明者らは、鋭意検討
した結果、中間層にチタンエロー等特定の顔料を使用す
ることが有効であることを知見し、本発明に至った。[Means for Solving the Problems] As a result of extensive studies, the present inventors have found that it is effective to use a specific pigment such as titanium yellow in the intermediate layer, and have arrived at the present invention.
【0014】すなわち、本発明は、(1)導電性支持体
上に中間層、光導電層を順に設けた電子写真感光体にお
いて、前記中間層は結着樹脂中に平均粒径0.3μm以
上の粒径を有するチタンエロー顔料を含む電子写真感光
体、(2)導電性支持体上に中間層、光導電層を順に設
けた電子写真感光体において、前記中間層は結着樹脂中
に平均粒径0.3μm以上の粒径を有するチタンエロー
顔料及び二酸化チタン顔料を含む電子写真感光体、(3
)導電性支持体上に中間層、光導電層を順に設けた電子
写真感光体において、前記中間層は結着剤樹脂中に平均
粒径が0.3μm以上のチタンエロー顔料、二酸化チタ
ン顔料、及び酸化第2スズ(SnO2)粉体を含み、か
つ二酸化チタンの添加量はチタンエロー1重量部に対し
、0.1〜10重量部の範囲であり、酸化第2スズの添
加量はチタンエロー顔料と二酸化チタン顔料の合計重量
に対し、3〜30重量%であることを特徴とする電子写
真感光体、(4)導電性支持体上に中間層、光導電層を
順に設けた電子写真感光体において、前記中間層は結着
剤樹脂中に平均粒径が0.3μm以上のチタンエロー顔
料、二酸化チタン顔料、及び酸化インジウム(In2O
3)粉体を含み、かつ二酸化チタンはチタンエロー1重
量部に対し、0.1〜10重量部の範囲であり、酸化イ
ンジウムの添加量はチタンエロー顔料と二酸化チタン顔
料の合計重量に対し、3〜30重量%であることを特徴
とする電子写真感光体である。That is, the present invention provides (1) an electrophotographic photoreceptor in which an intermediate layer and a photoconductive layer are sequentially provided on a conductive support, wherein the intermediate layer has an average particle size of 0.3 μm or more in a binder resin; (2) An electrophotographic photoreceptor comprising a titanium yellow pigment having a particle size of An electrophotographic photoreceptor containing a titanium yellow pigment and a titanium dioxide pigment having a particle size of 0.3 μm or more, (3
) An electrophotographic photoreceptor in which an intermediate layer and a photoconductive layer are sequentially provided on a conductive support, and the intermediate layer contains a titanium yellow pigment, a titanium dioxide pigment, and a titanium dioxide pigment having an average particle size of 0.3 μm or more in a binder resin. Contains stannic oxide (SnO2) powder, and the amount of titanium dioxide added is in the range of 0.1 to 10 parts by weight per 1 part by weight of titanium yellow, and the amount of stannic oxide added is equal to the amount of titanium yellow pigment and An electrophotographic photoreceptor characterized in that the amount of titanium pigment is 3 to 30% by weight based on the total weight of the titanium pigment, (4) an electrophotographic photoreceptor in which an intermediate layer and a photoconductive layer are sequentially provided on a conductive support, The intermediate layer contains a titanium yellow pigment with an average particle size of 0.3 μm or more, a titanium dioxide pigment, and indium oxide (In2O) in a binder resin.
3) Contains powder, and titanium dioxide is in the range of 0.1 to 10 parts by weight per 1 part by weight of titanium yellow, and the amount of indium oxide added is 3 to 10 parts by weight with respect to the total weight of titanium yellow pigment and titanium dioxide pigment. This is an electrophotographic photoreceptor characterized by having a content of 30% by weight.
【0015】上記本発明の第1発明における中間層は顔
料として、チタンエローを含有した樹脂層から成る。チ
タンエローは黄色顔料の一種でTiO2−NiO−Sb
2O5の3成分よりなり、1000℃前後の温度で発色
させたものである。The intermediate layer in the first aspect of the present invention comprises a resin layer containing titanium yellow as a pigment. Titanium yellow is a type of yellow pigment made from TiO2-NiO-Sb.
It consists of three components, 2O5, and develops color at a temperature of around 1000°C.
【0016】この3成分組成物は塩酸や硫酸などで煮沸
しても、NiやSbは抽出されず、変化もしないので、
Ni、Sb原子が酸化チタンのルチル結晶格子中のTi
原子と置換固溶していると見なされる。したがって化学
的にも、物理的にもルチル形TiO2にある程度類似し
、きわめて安定である。Even if this three-component composition is boiled with hydrochloric acid or sulfuric acid, Ni and Sb are not extracted or changed.
Ni and Sb atoms are Ti in the rutile crystal lattice of titanium oxide
It is considered to be in solid solution by substitution with atoms. Therefore, it is chemically and physically similar to rutile TiO2 to some extent and is extremely stable.
【0017】また、その平均粒径は白色酸化チタンより
大きなもの(0.4〜1.2μm程度)が市販されてお
り、これを用いることで近赤外光の場合でも乱反射能が
高く、かつ静電特性の優れた感光体を得ることができる
。[0017] In addition, particles with an average particle size larger than that of white titanium oxide (approximately 0.4 to 1.2 μm) are commercially available, and by using them, even in the case of near-infrared light, the diffused reflection ability is high, and A photoreceptor with excellent electrostatic properties can be obtained.
【0018】本発明の第2発明における中間層はチタン
エローの他に二酸化チタンを含有する。この二酸化チタ
ンは、塗布液中のチタンエローの分散状態を安定化する
作用を有し、好ましくは0.2〜0.3μmの平均粒径
のものが用いられる。The intermediate layer in the second aspect of the present invention contains titanium dioxide in addition to titanium yellow. This titanium dioxide has the effect of stabilizing the dispersion state of titanium yellow in the coating liquid, and preferably has an average particle size of 0.2 to 0.3 μm.
【0019】二酸化チタンの使用量は、そのグレードに
もよるが、チタンエロー1に対しておおよそ重量で0.
1〜10の範囲がよい。0.1未満ではその効果が小さ
く、また10を越えると干渉縞防止効果がなくなる。The amount of titanium dioxide to be used depends on its grade, but it is approximately 0.00% by weight per 1 part of titanium yellow.
A range of 1 to 10 is preferable. If it is less than 0.1, the effect will be small, and if it exceeds 10, the interference fringe prevention effect will be lost.
【0020】又、本発明の第3発明における中間層はチ
タンエローの他に、さらに二酸化チタン、酸化第2スズ
を含有する。又、本発明の第4発明においては前記第3
発明における酸化第2スズに代えて、酸化インジウム(
In2O3)を含有する。これらの発明において二酸化
チタンは、前記第2発明と同様に塗布液中のチタンエロ
ーの分散状態を安定化する作用を有し、好ましくは0.
2〜0.3μmの平均粒径のものが用いられる。The intermediate layer in the third aspect of the present invention further contains titanium dioxide and stannic oxide in addition to titanium yellow. Further, in the fourth aspect of the present invention, the third aspect of the present invention
In place of stannic oxide in the invention, indium oxide (
In2O3). In these inventions, titanium dioxide has the effect of stabilizing the dispersion state of titanium yellow in the coating liquid, as in the second invention, and preferably 0.
Those having an average particle size of 2 to 0.3 μm are used.
【0021】そして、その使用量は二酸化チタンのグレ
ードにもよるが、チタンエロー1に対して、おおよそ重
量で0.1〜10の範囲がよい。0.1未満ではその効
果が小さく、また10を越えると干渉縞防止効果がなく
なる。[0021] The amount used depends on the grade of titanium dioxide, but it is preferably in the range of approximately 0.1 to 10 by weight per 1 of titanium yellow. If it is less than 0.1, the effect will be small, and if it exceeds 10, the interference fringe prevention effect will be lost.
【0022】また粗い表面形状をした基体上に感光体を
設けるためには、中間層の膜厚を厚くする必要があるが
、この場合、残留電位の上昇を抑制する為に導電性の顔
料を加える事が望ましい。しかしながら金属粉末、カー
ボンブラック等の導電性粉体を用いた場合、反転現像方
式を用いたプロセスでは地肌部に砂目状の地肌汚れが発
生する。この様な欠点が無く、かつ高感度を維持するた
めに半導体レーザによる書き込み光の波長である近赤外
光の吸収が小さい導電性粉体はほとんど無いが、酸化第
2スズあるいは酸化インジウムが以上の条件を満足する
ことを確認した。従ってチタンエロー、二酸化チタン、
二酸化第2スズあるいは酸化インジウムを加えることで
、前記(1)〜(5)の全ての機能を満足する中間層を
得ることができる。Furthermore, in order to provide a photoreceptor on a substrate with a rough surface, it is necessary to increase the thickness of the intermediate layer, but in this case, a conductive pigment is added to suppress the increase in residual potential. It is desirable to add. However, when a conductive powder such as metal powder or carbon black is used, a grain-like background stain occurs in the background part in a process using a reversal development method. There are almost no conductive powders that do not have such drawbacks and have low absorption of near-infrared light, which is the wavelength of writing light from a semiconductor laser, in order to maintain high sensitivity. It was confirmed that the following conditions were satisfied. Therefore, titanium yellow, titanium dioxide,
By adding stannic dioxide or indium oxide, an intermediate layer that satisfies all of the functions (1) to (5) above can be obtained.
【0023】酸化第2スズあるいは酸化インジウムの添
加量はチタンエロー顔料と二酸化チタン顔料の合計重量
に対し3〜30重量%程度が望ましい。3%未満では酸
化第2スズの添加効果が無く、30%を越えた場合、感
光体の帯電安定性が悪くなる。The amount of stannic oxide or indium oxide added is preferably about 3 to 30% by weight based on the total weight of the titanium yellow pigment and the titanium dioxide pigment. If it is less than 3%, there is no effect of adding stannic oxide, and if it exceeds 30%, the charging stability of the photoreceptor will deteriorate.
【0024】又、チタンエロー顔料、二酸化チタン顔料
及び酸化第二スズ粉体あるいは酸化インジウム粉体の合
計(P)と結着剤樹脂(R)との比P/Rは体積比で1
/1〜3/1が好ましい。中間層のP/R体積比が1未
満であると中間層は結着剤樹脂の特性に左右され、特に
温湿度の変化で感光体特性は変化する。又、P/R比が
3を越えると中間層は層中に空隙が多くなり、空気がた
まる。これが光導電層の塗布乾燥時に気泡となり、塗膜
欠陥を生ずる。[0024] Furthermore, the ratio P/R of the sum of the titanium yellow pigment, titanium dioxide pigment, and stannic oxide powder or indium oxide powder to the binder resin (R) is 1 in terms of volume ratio.
/1 to 3/1 is preferred. When the P/R volume ratio of the intermediate layer is less than 1, the intermediate layer is influenced by the properties of the binder resin, and in particular, the characteristics of the photoreceptor change with changes in temperature and humidity. Furthermore, if the P/R ratio exceeds 3, the intermediate layer will have many voids and air will accumulate therein. These become bubbles when the photoconductive layer is applied and dried, resulting in coating film defects.
【0025】本発明の電子写真感光体は、導電性基体上
に上記の中間層を設け、さらにその上の感光層から構成
される。The electrophotographic photoreceptor of the present invention comprises the above-mentioned intermediate layer provided on a conductive substrate and a photosensitive layer thereon.
【0026】導電性基体としてはアルミニウム、ニッケ
ル、ステンレスなどの金属;カーボン等の導電性顔料を
分散したプラスチック;絶縁性支持体(プラスチック又
はプラスチックフィルムのごときもの)上に金属を蒸着
したもの、または導電性塗料を塗工したもの等が例示で
きる。[0026] As the conductive substrate, metals such as aluminum, nickel, and stainless steel; plastics in which conductive pigments such as carbon are dispersed; metals deposited on insulating supports (such as plastics or plastic films), or Examples include those coated with conductive paint.
【0027】中間層に用いる樹脂としては適宜のものを
用いることができるが、その上に感光層を溶剤で塗布す
ることを考え合わせると、一般の有機溶剤に対して耐溶
剤性の高い樹脂が望ましい。このような樹脂としては、
ポリビニルアルコール、カゼイン、ポリアクリル酸ナト
リウム等の水溶性樹脂;共重合ナイロン、メトキシメチ
ル化ナイロン等のアルコール可溶性樹脂;ポリウレタン
、メラミン樹脂、エポキシ樹脂等の三次元網目構造を形
成する硬化型樹脂などが挙げられる。Any suitable resin can be used for the intermediate layer, but considering that the photosensitive layer will be coated on top of it with a solvent, it is recommended to use a resin that has high solvent resistance to common organic solvents. desirable. As such resin,
Water-soluble resins such as polyvinyl alcohol, casein, and sodium polyacrylate; Alcohol-soluble resins such as copolymerized nylon and methoxymethylated nylon; Curable resins that form three-dimensional network structures such as polyurethane, melamine resin, and epoxy resin. Can be mentioned.
【0028】中間層を導電性基体上に得るには、チタン
エロー、又はチタンエローと二酸化チタン、及び酸化ス
ズあるいは酸化インジウムを前記樹脂の溶液中に分散し
浸漬塗布法等の手段で塗布乾燥すれば良い。[0028] To obtain the intermediate layer on the conductive substrate, titanium yellow, or titanium yellow and titanium dioxide, and tin oxide or indium oxide may be dispersed in a solution of the above resin, and the mixture may be coated and dried by a dip coating method or the like. .
【0029】中間層の膜は0.3〜30μm程度が望ま
しい。0.3μm未満では成膜性が悪く、30μmを越
えた場合は帯電安定性と低残留電位の両立が難しくなる
。The thickness of the intermediate layer is preferably about 0.3 to 30 μm. If the thickness is less than 0.3 μm, film forming properties are poor, and if it exceeds 30 μm, it becomes difficult to achieve both charging stability and low residual potential.
【0030】本発明に用いる光導電層としては(1)電
子供与性化合物と電子受容性化合物との組合せにより電
荷移動錯体を形成したもの(USP3484237に記
載)、(2)有機光導電体に染料を添加して増感したも
の(特公昭48−25658号公報に記載)、(3)正
孔あるいは電子活性マトリックスに顔料を分散したもの
(特開昭47−30328号、特開昭47−18545
号などの公報に記載)、(4)電荷発生層と電荷輸送層
とに機能分離したもの(特開昭49−105537号公
報に記載)、(5)染料及び樹脂からなる共晶錯体を主
成分とするもの(特開昭47−10785号公報に記載
)、(6)電荷移動錯体中に有機顔料ないしは無機電荷
発生材料を添加したもの(特開昭49−91648号公
報に記載)など従来から知られている有機光導電体のい
ずれで形成されていてもかまわない。The photoconductive layer used in the present invention includes (1) a charge transfer complex formed by a combination of an electron-donating compound and an electron-accepting compound (described in US Pat. No. 3,484,237), and (2) a dye in an organic photoconductor. (described in Japanese Patent Publication No. 48-25658); (3) pigments dispersed in a hole- or electron-active matrix (Japanese Patent Application Laid-open Nos. 47-30328 and 18545-1982);
(4) functionally separated charge generation layer and charge transport layer (described in JP-A-49-105537), (5) mainly composed of a eutectic complex consisting of a dye and a resin. Conventional methods such as those in which an organic pigment or an inorganic charge generating material is added to a charge transfer complex (described in Japanese Patent Application Laid-open No. 49-91648) It may be formed of any organic photoconductor known from .
【0031】しかし、これらの中でも特に(4)のタイ
プの積層型感光体は高感度であり、かつ、機能にあわせ
て多様に材料が選択できる等から有利である。However, among these, the laminated photoreceptor of type (4) is particularly advantageous because it has high sensitivity and a variety of materials can be selected depending on the function.
【0032】電荷発生層はアゾ系顔料、フタロシアニン
系顔料、スクエアリック顔料、インジゴ系顔料、ペリレ
ン系顔料、セレン粉末、セレン合金粉末、アモルファス
シリコン粉末、酸化亜鉛粉末、硫化カドミウム粉末のご
とき電荷発生物質をポリエステル、ポリカーボネート、
ポリビニルブチラール、アクリル樹脂などの結着樹脂溶
液中に分散し、これを中間層上に塗工することにより形
成される。電荷発生層の厚さは0.01〜2μmくらい
が適当である。The charge generating layer is made of a charge generating substance such as an azo pigment, a phthalocyanine pigment, a square pigment, an indigo pigment, a perylene pigment, a selenium powder, a selenium alloy powder, an amorphous silicon powder, a zinc oxide powder, or a cadmium sulfide powder. polyester, polycarbonate,
It is formed by dispersing in a solution of a binder resin such as polyvinyl butyral or acrylic resin and coating it on the intermediate layer. The appropriate thickness of the charge generation layer is about 0.01 to 2 μm.
【0033】電荷輸送層はα−フェニルスチルベン化合
物(特開昭58−198043公報に記載)、ヒドラゾ
ン化合物(特開昭55−46760号公報に記載)など
の電荷輸送性物質を成膜性のある樹脂例えばポリエステ
ル、ポリサルホン、ポリカーボネート、ポリメタクリル
酸エステル類、ポリスチレンなどに溶解させ、これを電
荷発生層上に厚さ10〜40μm程度に塗工すればよい
。ここで成膜性樹脂が用いられるのは、電荷輸送性物質
が一般に低分子量でそれ自身では成膜性に乏しいためで
ある。The charge transporting layer is made of a charge transporting substance such as an α-phenylstilbene compound (described in JP-A-58-198043) or a hydrazone compound (described in JP-A-55-46760) that has film-forming properties. It may be dissolved in a resin such as polyester, polysulfone, polycarbonate, polymethacrylic acid ester, polystyrene, etc., and coated on the charge generation layer to a thickness of about 10 to 40 μm. The film-forming resin is used here because the charge transporting substance generally has a low molecular weight and has poor film-forming properties by itself.
【0034】[0034]
実施例1
アルコール可溶性ポリアミド樹脂{アミランCM−80
00(東レ製)}1重量部をメタノール8重量部、n−
ブタノール5重量部の混合溶媒に溶解した。これにチタ
ンエロー粉末{タイペークイエローTY−50(石原産
業製)}1重量部を加え、ボールミルで12時間分散し
、中間層用塗布液を作成した。これを表面を鏡面に仕上
げた外径80mm、長さ359mmのアルミシリンダー
に、乾燥後の膜厚が1.5μmになるように塗布乾燥し
、中間層を形成した。Example 1 Alcohol-soluble polyamide resin {Amilan CM-80
00 (manufactured by Toray)} 1 part by weight, 8 parts by weight of methanol, n-
It was dissolved in a mixed solvent containing 5 parts by weight of butanol. To this was added 1 part by weight of titanium yellow powder {Typaque Yellow TY-50 (manufactured by Ishihara Sangyo)}, and the mixture was dispersed in a ball mill for 12 hours to prepare a coating liquid for an intermediate layer. This was applied to an aluminum cylinder having a mirror-finished surface and having an outer diameter of 80 mm and a length of 359 mm, and was dried to form an intermediate layer so that the film thickness after drying was 1.5 μm.
【0035】次にブチラール樹脂{エスレックBLS(
積水化学製)}5重量部をシクロヘキサノン150重量
部に溶解し、これに下記構造式のトリスアゾ顔料10重
量部を加えボールミルにて48時間分散した。Next, butyral resin {S-LEC BLS (
Sekisui Chemical Co., Ltd.)} was dissolved in 150 parts by weight of cyclohexanone, 10 parts by weight of a trisazo pigment having the following structural formula was added thereto, and the mixture was dispersed in a ball mill for 48 hours.
【0036】[0036]
【化1】[Chemical formula 1]
【0037】更にシクロヘキサノン210重量部を加え
、3時間分散を行った。これを固形分が1.5wt%に
なるように、撹拌しながらシクロヘキサノンで希釈した
。こうして得られた電荷発生層用塗布液を前記中間層上
に塗布乾燥し、厚さ約0.2μmの電荷発生層を形成し
た。Further, 210 parts by weight of cyclohexanone was added and dispersion was carried out for 3 hours. This was diluted with cyclohexanone while stirring so that the solid content was 1.5 wt%. The charge generation layer coating liquid thus obtained was applied onto the intermediate layer and dried to form a charge generation layer having a thickness of about 0.2 μm.
【0038】更に下記構造式の電荷輸送物質6重量部、
ポリカーボネート樹脂{パンライトK−1300(帝人
化成製)}10重量部、シリコンオイル{KF−50(
信越化学工業製)}0.002重量部を90重量部の塩
化メチレンに溶解した。こうして得られた電荷輸送層用
塗布液を前記電荷発生層上に塗布乾燥し厚さ23μmの
電荷輸送層を形成し、電子写真用感光体を作成した。Furthermore, 6 parts by weight of a charge transport substance having the following structural formula,
Polycarbonate resin {Panlite K-1300 (manufactured by Teijin Chemicals)} 10 parts by weight, silicone oil {KF-50 (
Shin-Etsu Chemical Co., Ltd.)} 0.002 parts by weight was dissolved in 90 parts by weight of methylene chloride. The charge transport layer coating liquid thus obtained was applied onto the charge generation layer and dried to form a charge transport layer having a thickness of 23 μm, thereby producing an electrophotographic photoreceptor.
【0039】[0039]
【化2】[Case 2]
【0040】比較例1
実施例1の中間層のチタンエローを除き、ポリアミド樹
脂のみの厚さ0.5μmの中間層を設けた以外は実施例
1と同様に電子写真感光体を作成した。Comparative Example 1 An electrophotographic photoreceptor was prepared in the same manner as in Example 1 except that the titanium yellow in the intermediate layer of Example 1 was removed and an intermediate layer of 0.5 μm thick made of polyamide resin was provided.
【0041】以上得られた感光体をデジタル複写機{イ
マジオ420(リコー製)}に装着し、オレンジ色の紙
を原稿として、文字写真モードを選択しコピーを取った
ところ、実施例1においては均一な中間調の画像が得ら
れたが、比較例1においては明らかに干渉縞と考えられ
る画像の濃淡ムラが確認された。The photoreceptor obtained above was installed in a digital copying machine {Imagio 420 (manufactured by Ricoh)}, and a copy was made by selecting the text photo mode using orange paper as a document. Although an image with uniform halftones was obtained, in Comparative Example 1, unevenness in density of the image, which was clearly considered to be interference fringes, was observed.
【0042】実施例2
アクリル樹脂{アクリディックA−460−60(大日
本インキ化学工業製)}15重量部、メラミン樹脂{ス
パーベッカミンL−121−60(大日本インキ化学工
業製)}10重量部をメチルエチルケトン100重量部
に溶解した。これにチタンエロー粉末{タイペークイエ
ローTY−70S(石原産業製)}50重量部を加え、
ボールミルで12時間分散し、中間層用塗布液を作成し
た。これを実施例1と同様のアルミシリンダーに乾燥後
の膜厚が2.0μmになるように塗布乾燥し、中間層を
形成した。Example 2 Acrylic resin {Acrydic A-460-60 (Dainippon Ink & Chemicals)} 15 parts by weight, melamine resin {Superbeckamine L-121-60 (Dainippon Ink & Chemicals)} 10 Part by weight was dissolved in 100 parts by weight of methyl ethyl ketone. Add 50 parts by weight of titanium yellow powder {Typeque Yellow TY-70S (manufactured by Ishihara Sangyo)} to this,
The mixture was dispersed in a ball mill for 12 hours to prepare a coating solution for an intermediate layer. This was coated and dried on the same aluminum cylinder as in Example 1 so that the film thickness after drying was 2.0 μm to form an intermediate layer.
【0043】次に実施例1と同様の電荷発生層を前記中
間層上に形成した。Next, a charge generation layer similar to that in Example 1 was formed on the intermediate layer.
【0044】更に下記構造式の電荷輸送物質Furthermore, a charge transport substance having the following structural formula:
【0045
】0045
]
【化3】[Chemical formula 3]
【0046】
8重量部 ポリカ
ーボネート樹脂{パンライトK−1300(帝人化成製
)}
10重量部 シリコンオ
イル{KF−50(信越化学工業製)
0.002重量部 ブチルヒドロキシトルエン
0.04重量部を86重量部の塩化メチレンに
溶解した。こうして得られた電荷輸送層用塗布液を前記
電荷発生層上に塗布乾燥し、厚さ20μmの電荷輸送層
を形成し、電子写真用感光体を作成した。[0046]
8 parts by weight Polycarbonate resin {Panlite K-1300 (manufactured by Teijin Kasei)}
10 parts by weight Silicone oil {KF-50 (manufactured by Shin-Etsu Chemical)
0.002 parts by weight Butylated hydroxytoluene
0.04 parts by weight was dissolved in 86 parts by weight of methylene chloride. The charge transport layer coating liquid thus obtained was applied onto the charge generation layer and dried to form a charge transport layer with a thickness of 20 μm, thereby producing an electrophotographic photoreceptor.
【0047】比較例2
実施例2の中間層のチタンエローに変えて、酸化チタン
粉末{タイペークR−680(石原産業製)を用いた以
外は実施例2と同様に電子写真感光体を作成した。Comparative Example 2 An electrophotographic photoreceptor was prepared in the same manner as in Example 2, except that titanium oxide powder {Tiepeke R-680 (manufactured by Ishihara Sangyo) was used instead of titanium yellow in the intermediate layer of Example 2.
【0048】以上得られた感光体を実施例1と同様にイ
マジオ420で評価したところ実施例2においては均一
な中間調の画像が得られたが、比較例2においてはわず
かではあるが、干渉縞と考えられる画像の濃淡ムラが確
認された。The photoreceptor obtained above was evaluated using Imageo 420 in the same manner as in Example 1. In Example 2, an image with uniform halftones was obtained, but in Comparative Example 2, although there was slight interference, Uneven shading in the image, which is considered to be stripes, was confirmed.
【0049】実施例3〜5比較例3,4アクリル樹脂{
アクリル樹脂A460−60(大日本インキ化学工業製
)}15重量部、メラミン樹脂{スーパーベッカミンL
−121−60(大日本インキ化学工業製)}10重量
部をメチルエチルケトン100重量部に溶解した。これ
にチタンエロー粉末{タイペークイエローTY−70(
石原産業製)}と二酸化チタン粉末{タイペークA−1
00(石原産業製)}とを表1に示した量で、それぞれ
加えボールミルで6時間分散し、中間層用塗布液を作成
した。これを実施例1と同様のアルミシリンダーに乾燥
後の膜厚が2.0μmになるよう、浸漬塗工法で塗布し
、130℃20分間乾燥し、中間層を形成した。Examples 3 to 5 Comparative Examples 3 and 4 Acrylic resin {
Acrylic resin A460-60 (manufactured by Dainippon Ink and Chemicals) 15 parts by weight, melamine resin {Super Beckamine L
-121-60 (manufactured by Dainippon Ink & Chemicals)}10 parts by weight were dissolved in 100 parts by weight of methyl ethyl ketone. Add titanium yellow powder {Type Yellow TY-70 (
Ishihara Sangyo)} and titanium dioxide powder {Tiepeke A-1
00 (manufactured by Ishihara Sangyo)} in the amounts shown in Table 1, and dispersed in a ball mill for 6 hours to prepare an intermediate layer coating solution. This was applied to the same aluminum cylinder as in Example 1 by dip coating so that the film thickness after drying was 2.0 μm, and dried at 130° C. for 20 minutes to form an intermediate layer.
【0050】[0050]
【表1】[Table 1]
【0051】次に実施例1と同様の電荷発生層を形成し
た。Next, a charge generation layer similar to that in Example 1 was formed.
【0052】更に下記IIの電荷輸送物質Furthermore, the following charge transport substance II
【0053】[0053]
【化4】[C4]
【0054】
8重量部 ポリカーボ
ネート樹脂{パンライトK−1300(帝人化成製)}
10重量部 シリコンオイル{K
F−50
(信越化学工業製)}
0.00
2重量部 ブチルヒドロキシトルエン
0.04重量部を86重量部の塩化メチレンに溶解した
。[0054]
8 parts by weight Polycarbonate resin {Panlite K-1300 (manufactured by Teijin Kasei)}
10 parts by weight silicone oil {K
F-50 (manufactured by Shin-Etsu Chemical)
0.00
2 parts by weight Butylated hydroxytoluene
0.04 parts by weight was dissolved in 86 parts by weight of methylene chloride.
【0055】こうして得られた電荷輸送層用塗布液を前
記電荷発生層上に塗布乾燥し、厚さ20μmの電荷輸送
層を形成し、電子写真用感光体を作成した。The charge transport layer coating liquid thus obtained was coated on the charge generation layer and dried to form a charge transport layer with a thickness of 20 μm, thereby producing an electrophotographic photoreceptor.
【0056】以上得られた感光体をディジタル複写機{
イマジオ420(リコー製)}に装着し、オレンジ色の
紙を原稿として、文字写真モードを選択し、コピーを取
ったところ表2に示した結果を得た。[0056] The photoreceptor obtained above was used in a digital copying machine {
Imagio 420 (manufactured by Ricoh)], the text photo mode was selected using orange paper as the original, and copies were made, and the results shown in Table 2 were obtained.
【0057】[0057]
【表2】[Table 2]
【0058】実施例6〜8、比較例5,6アルコール可
溶性ポリアミド樹脂{アミランCM−8000(東レ製
)}20重量部をメタノール160重量部、n−ブタノ
ール80重量部の混合溶媒に溶解した。
これにチタンエロー粉末{タイペークイエローTY−5
0(石原産業製)}と二酸化チタン粉末{タイペークC
R−EL(石原産業製)}とを{表3}に示した量でそ
れぞれ加え、ボールミルで6時間分散し中間層用塗布液
を作成した。Examples 6 to 8, Comparative Examples 5 and 6 Twenty parts by weight of alcohol-soluble polyamide resin {Amilan CM-8000 (manufactured by Toray Industries, Ltd.)} were dissolved in a mixed solvent of 160 parts by weight of methanol and 80 parts by weight of n-butanol. Add to this titanium yellow powder {Typaque Yellow TY-5
0 (manufactured by Ishihara Sangyo)} and titanium dioxide powder {Tipeque C
R-EL (manufactured by Ishihara Sangyo)} were added in the amounts shown in Table 3, and dispersed in a ball mill for 6 hours to prepare an intermediate layer coating solution.
【0059】[0059]
【表3】[Table 3]
【0060】これを実施例3〜5と同様のアルミシリン
ダーに乾燥後の膜厚が3.5μmになるよう浸漬塗工法
で塗布し120℃で15分間乾燥し、中間層を形成した
。[0060] This was coated on the same aluminum cylinder as in Examples 3 to 5 by dip coating so that the film thickness after drying was 3.5 μm, and dried at 120° C. for 15 minutes to form an intermediate layer.
【0061】次に、ブチラール樹脂{エスレックBLS
(積水化学製)}2重量部をシクロヘキサノン60重量
部に溶解し、これにチタニルフタロシアニン3重量部を
加え、ボールミルにて24時間分散した。更にシクロヘ
キサノン80重量部を加え、3時間分散をした。これを
固形分が2.5wt%になるように撹拌しながらメチル
エチルケトンで希釈した。Next, butyral resin {S-LEC BLS
(manufactured by Sekisui Chemical)} was dissolved in 60 parts by weight of cyclohexanone, 3 parts by weight of titanyl phthalocyanine was added thereto, and the mixture was dispersed in a ball mill for 24 hours. Furthermore, 80 parts by weight of cyclohexanone was added and the mixture was dispersed for 3 hours. This was diluted with methyl ethyl ketone while stirring so that the solid content was 2.5 wt%.
【0062】こうして得られた電荷発生層用塗布液を前
記中間層上に塗布乾燥し、厚さ約0.4μmの電荷発生
層を形成した。The charge generation layer coating liquid thus obtained was applied onto the intermediate layer and dried to form a charge generation layer having a thickness of about 0.4 μm.
【0063】
更に下記III の電荷輸送物質
8重量部[0063] Furthermore, the following charge transport material III
8 parts by weight
【0064】[0064]
【化5】[C5]
【0065】
ポリカーボネート樹脂{パンライトK−130
0(帝人化成製)}
10重量部
シリコンオイル{KF−50(信越化学工業製)}
0.002重量部 ブチルヒドロキ
シトルエン
0.04重量部を88重量部の塩
化メチレンに溶解した。Polycarbonate resin {Panlite K-130
0 (made by Teijin Chemicals)}
10 parts by weight
Silicone oil {KF-50 (manufactured by Shin-Etsu Chemical)}
0.002 parts by weight Butylated hydroxytoluene
0.04 parts by weight was dissolved in 88 parts by weight of methylene chloride.
【0066】こうして得られた電荷輸送層用塗布液を前
記電荷発生層上に塗布乾燥し、厚さ20μmの電荷輸送
層を形成し、電子写真用感光体を作成した。The charge transport layer coating liquid thus obtained was coated on the charge generation layer and dried to form a charge transport layer with a thickness of 20 μm, thereby producing an electrophotographic photoreceptor.
【0067】以上得られた感光体をディジタル複写機{
イマジオ420(リコー製)}に装着し、オレンジ色の
紙を原稿として、文字写真モードを選択し、コピーを取
ったところ表4に示した結果を得た。[0067] The photoreceptor obtained above was used in a digital copying machine {
Imagio 420 (manufactured by Ricoh)], the text photo mode was selected using orange paper as the original, and copies were made, and the results shown in Table 4 were obtained.
【0068】[0068]
【表4】[Table 4]
【0069】実施例9〜11、比較例7〜9 ア
クリル樹脂{アクリディックA−460−60(大日本
インキ化学工業製)}
18重量部
メラミン樹脂{スーパーベッカミンL−121−
60(大日本インキ化学工業製)}
12重量部をメチルエチルケトン60重量部に溶解し、
これにチタンエロー顔料{タイペークイエローTY−5
0(石原産業製)}、二酸化チタン顔料{タイペークA
−100(石原産業製)}、酸化スズ粉末(三菱金属製
)を表5に示した量をそれぞれ加え、ボールミルで8時
間分散し、中間層塗布液を作成した。Examples 9 to 11, Comparative Examples 7 to 9 Acrylic resin {Acridic A-460-60 (manufactured by Dainippon Ink and Chemicals)}
18 parts by weight
Melamine resin {Super Beckamine L-121-
60 (manufactured by Dainippon Ink and Chemicals)
Dissolve 12 parts by weight in 60 parts by weight of methyl ethyl ketone,
This is titanium yellow pigment {Typaque Yellow TY-5
0 (manufactured by Ishihara Sangyo)}, titanium dioxide pigment {Tiepeque A
-100 (manufactured by Ishihara Sangyo)} and tin oxide powder (manufactured by Mitsubishi Metals) were added in the amounts shown in Table 5, and dispersed in a ball mill for 8 hours to prepare an intermediate layer coating solution.
【0070】[0070]
【表5】[Table 5]
【0071】これを実施例1と同様のアルミシリンダー
に浸漬塗布し、140℃で20分間乾燥し、中間層を形
成した。[0071] This was coated by dip coating on the same aluminum cylinder as in Example 1, and dried at 140°C for 20 minutes to form an intermediate layer.
【0072】次に実施例1同様の電荷発生層を形成した
。Next, a charge generation layer similar to that in Example 1 was formed.
【0073】更に下記式IVの電荷輸送物質6重量部、
ポリカーボネート樹脂{パンライトK−1300(帝人
化成製)}10重量部、シリコンオイル{KF−50(
信越化学工業製)}0.002重量部、ブチルヒドロキ
シトルエン(BHT)0.06重量部を90重量部の塩
化メチレンに溶解した。こうして得られた電荷輸送層用
塗布液を前記電荷発生層上に塗布乾燥し、厚さ23μm
の電荷輸送層を形成し、電子写真用感光体を作成した。Furthermore, 6 parts by weight of a charge transport material of the following formula IV,
Polycarbonate resin {Panlite K-1300 (manufactured by Teijin Chemicals)} 10 parts by weight, silicone oil {KF-50 (
(manufactured by Shin-Etsu Chemical Co., Ltd.)} and 0.06 parts by weight of butylated hydroxytoluene (BHT) were dissolved in 90 parts by weight of methylene chloride. The charge transport layer coating solution thus obtained was applied onto the charge generation layer and dried to a thickness of 23 μm.
A charge transport layer was formed to produce an electrophotographic photoreceptor.
【0074】[0074]
【化6】[C6]
【0075】以上得られた感光体をディジタル複写機{
イマジオ420(リコー製)}に装置しオレンジ色の紙
を原稿にし、文字写真モードでコピーを得たところ表6
の結果を得た。[0075] The photoreceptor obtained above was used in a digital copying machine {
Imagio 420 (manufactured by Ricoh)] was used as an original on orange paper, and a copy was obtained in text photo mode. Table 6
I got the result.
【0076】[0076]
【表6】[Table 6]
【0077】実施例12〜14、比較例10,11
アルキッド樹脂{ベッコゾール1307−60EL
、固形分60重量%(大日本インキ化学製)}
45重量部
メラミン樹脂{スーパーベッカミンL−121−6
0固形分60重量%(大日本インキ化学製)}
30重量部をメ
チルエチルケトン150重量部に溶解し、これにチタン
エロー顔料{タイペークイエローTY−70(石原産業
製)}、二酸化チタン顔料{タイペークCR−EL(石
原産業製)}酸化スズ粉末(三菱金属製)を表7に示し
た量をそれぞれ加え、ボールミルで8時間分散し、中間
層用塗布液を作成した。この時のそれぞれの粉体(P)
と結着剤樹脂(R)の体積比P/Rも表7に示した(材
料の密度はTY−70が4.4、CR−EL4.2、酸
化スズ7.0、アルキッドメラミン樹脂1.3である)
。Examples 12 to 14, Comparative Examples 10 and 11
Alkyd resin {Beccosol 1307-60EL
, solid content 60% by weight (manufactured by Dainippon Ink Chemical)}
45 parts by weight
Melamine resin {Super Beckamine L-121-6
0 solid content 60% by weight (manufactured by Dainippon Ink Chemical)}
Dissolve 30 parts by weight in 150 parts by weight of methyl ethyl ketone, and add titanium yellow pigment {Typeque Yellow TY-70 (manufactured by Ishihara Sangyo)}, titanium dioxide pigment {Typek CR-EL (manufactured by Ishihara Sangyo)} and tin oxide powder (Mitsubishi). (metal) were added in the amounts shown in Table 7, and dispersed in a ball mill for 8 hours to prepare a coating solution for an intermediate layer. Each powder (P) at this time
The volume ratio P/R of binder resin (R) and binder resin (R) is also shown in Table 7 (the density of the materials is 4.4 for TY-70, 4.2 for CR-EL, 7.0 for tin oxide, and 1.0 for alkyd melamine resin). 3)
.
【0078】[0078]
【表7】[Table 7]
【0079】これを実施例1と同様のアルミシリンダー
に浸漬塗布し、150℃で20分間乾燥し、厚さ13μ
mの中間層を形成した。次に実施例9と同様の電荷発生
層と電荷輸送層を形成し、電子写真用感光体を作成した
。この結果比較例11においては電荷輸送層の乾燥時に
気泡を発生し、評価に値する感光体が得られなかった。[0079] This was coated by dip coating on the same aluminum cylinder as in Example 1, and dried at 150°C for 20 minutes to give a thickness of 13μ.
An intermediate layer of m was formed. Next, a charge generation layer and a charge transport layer similar to those in Example 9 were formed to produce an electrophotographic photoreceptor. As a result, in Comparative Example 11, bubbles were generated during drying of the charge transport layer, and a photoreceptor worthy of evaluation was not obtained.
【0080】以上得られた感光体を実施例9と同様に評
価し、結果を表8に示した。The photoreceptor obtained above was evaluated in the same manner as in Example 9, and the results are shown in Table 8.
【0081】[0081]
【表8】[Table 8]
【0082】実施例15
実施例12の中間層用塗布液を直径が80mm、長さ3
59mmで表面を最大表面粗さが7μmに加工したアル
ミシリンダーに浸漬塗布し、150℃で20分間乾燥し
、厚さ15μmの中間層を形成した。これに実施例9と
同様の電荷発生層、電荷輸送層を形成し、電子写真感光
体を得た。Example 15 The intermediate layer coating solution of Example 12 was coated with a diameter of 80 mm and a length of 3 mm.
The coating was applied by dip coating onto an aluminum cylinder whose surface was processed to have a maximum surface roughness of 7 μm with a diameter of 59 mm, and dried at 150° C. for 20 minutes to form an intermediate layer with a thickness of 15 μm. A charge generation layer and a charge transport layer similar to those in Example 9 were formed on this to obtain an electrophotographic photoreceptor.
【0083】これを実施例9と同様に評価した所、50
枚コピー後においても良好な画像が得られた。[0083] When this was evaluated in the same manner as in Example 9, 50
Good images were obtained even after copying.
【0084】実施例16〜18、比較例12〜15
アクリル樹脂{アクリディックA−460−60
(大日本インキ化学工業製)}
18重量部
メラミン樹脂{スーパーベッカミンL−121
−60 (大日本インキ化学工業製)}
1
2重量部をメチルエチルケトン60重量部に溶解し、こ
れにチタンエロー顔料{タイペークイエローTY−50
(石原産業製)}、二酸化チタン顔料{タイペークA−
100(石原産業製)}、酸化インジウム粉末(三菱金
属製)を表9に示した量をそれぞれ加え、ボールミルで
8時間分散し、中間層用塗布液を作成した。Examples 16 to 18, Comparative Examples 12 to 15
Acrylic resin {Acrydic A-460-60
(Manufactured by Dainippon Ink and Chemicals)
18 parts by weight Melamine resin {Super Beckamine L-121
-60 (Dainippon Ink & Chemicals)}
1
Dissolve 2 parts by weight in 60 parts by weight of methyl ethyl ketone, and add titanium yellow pigment {Typaque Yellow TY-50
(manufactured by Ishihara Sangyo)}, titanium dioxide pigment {Tiepeque A-
100 (manufactured by Ishihara Sangyo)} and indium oxide powder (manufactured by Mitsubishi Metals) were added in the amounts shown in Table 9, and dispersed in a ball mill for 8 hours to prepare an intermediate layer coating solution.
【0085】[0085]
【表9】[Table 9]
【0086】これを直径80mm、長さ360mmの表
面を鏡面加工したアルミドラムに浸漬塗布し、140℃
で20分間乾燥し、中間層を形成した。[0086] This was applied by dip coating onto an aluminum drum with a mirror-finished surface, 80 mm in diameter and 360 mm in length, and heated at 140°C.
The mixture was dried for 20 minutes to form an intermediate layer.
【0087】次にブチラール樹脂{エスレックBLS(
積水化学製)}5重量部をシクロヘキサノン150重量
部に溶解し、これに下記構造式のトリスアゾ顔料10重
量部を加えボールミルにて48時間分散した。Next, butyral resin {S-LEC BLS (
Sekisui Chemical Co., Ltd.)} was dissolved in 150 parts by weight of cyclohexanone, 10 parts by weight of a trisazo pigment having the following structural formula was added thereto, and the mixture was dispersed in a ball mill for 48 hours.
【0088】[0088]
【化7】[C7]
【0089】更にシクロヘキサノン210重量部を加え
、3時間分散を行った。これを固形分が1.5wt%に
なるように、撹拌しながらシクロヘキサノンで希釈した
。こうして得られた電荷発生層用塗布液を前記中間層上
に塗布乾燥し、厚さ約0.2μmの電荷発生層を形成し
た。Further, 210 parts by weight of cyclohexanone was added and dispersion was carried out for 3 hours. This was diluted with cyclohexanone while stirring so that the solid content was 1.5 wt%. The charge generation layer coating liquid thus obtained was applied onto the intermediate layer and dried to form a charge generation layer having a thickness of about 0.2 μm.
【0090】更に下記構造式の電荷輸送物質6重量部、
ポリカーボネート樹脂{パンライトK−1300(帝人
化成製)}10重量部、シリコンオイル{KF−50(
信越化学工業製)]0.002重量部、ブチルヒドロキ
シトルエン(BHT)0.06重量部を90重量部の塩
化メチレンに溶解した。こうして得られた電荷輸送層用
塗布液を前記電荷発生層上に塗布乾燥し厚さ23μmの
電荷輸送層を形成し、電子写真用感光体を作成した。Furthermore, 6 parts by weight of a charge transport substance having the following structural formula,
Polycarbonate resin {Panlite K-1300 (manufactured by Teijin Chemicals)} 10 parts by weight, silicone oil {KF-50 (
Shin-Etsu Chemical Co., Ltd.)] and 0.06 parts by weight of butylated hydroxytoluene (BHT) were dissolved in 90 parts by weight of methylene chloride. The charge transport layer coating liquid thus obtained was applied onto the charge generation layer and dried to form a charge transport layer having a thickness of 23 μm, thereby producing an electrophotographic photoreceptor.
【0091】[0091]
【化8】[Chemical formula 8]
【0092】以上得られた感光体をデジタル複写機{イ
マジオ420(リコー製)}に装着し、オレンジ色の紙
を原稿にて、文字写真モードでコピーを得たところ以下
の結果を得た。The photoreceptor obtained above was installed in a digital copying machine {Imagio 420 (manufactured by Ricoh)}, and copies were made in the text/photo mode using orange paper as the original, and the following results were obtained.
【0093】[0093]
【表10】[Table 10]
【0094】実施例19〜21
アルキッド樹脂{ベッコゾール1307−60
EL、 固形分60重量%(大日本インキ化学製)}
重量部
メラミン樹脂{スパーベッカミンL−121−
60 固形分60重量%(大日本インキ化学工業製)
} 重量部をメチ
ルエチルケトン 重量部に溶解し、これにチ
タンエロー顔料{タイペークイエローTY−70S(石
原産業製)}、二酸化チタン顔料{タイペークCR−E
L(石原産業製)}、酸化インジウム粉末(三菱金属製
)を表11に示した量をそれぞれ加え、ボールミルで8
時間分散し、中間層用塗布液を作成した。この時のそれ
ぞれの粉体(P)と結着剤樹脂(R)の体積比P/Rも
表−3に示した(材料の密度はTY−70が4.4、C
R−EL4.2、酸化インジウム7.2、アルキッドメ
ラミン樹脂1.3である)。Examples 19-21 Alkyd resin {Beccosol 1307-60
EL, solid content 60% by weight (Dainippon Ink Chemical)}
Part by weight Melamine resin {Super Beckamine L-121-
60 Solid content 60% by weight (manufactured by Dainippon Ink and Chemicals)
} Dissolve parts by weight in parts by weight of methyl ethyl ketone, and add titanium yellow pigment {Tiepeke Yellow TY-70S (manufactured by Ishihara Sangyo)} and titanium dioxide pigment {Tiepeke CR-E].
L (manufactured by Ishihara Sangyo)} and indium oxide powder (manufactured by Mitsubishi Metals) were added in the amounts shown in Table 11, and milled with a ball mill.
A coating solution for an intermediate layer was prepared by dispersing the mixture over time. The volume ratio P/R of each powder (P) and binder resin (R) at this time is also shown in Table 3 (the density of the material is 4.4 for TY-70, C
R-EL: 4.2, indium oxide: 7.2, alkyd melamine resin: 1.3).
【0095】[0095]
【表11】[Table 11]
【0096】これを実施例16と同様のアルミシリンダ
ーに浸漬塗布し、150℃で20分間乾燥し、厚さ13
μmの中間層を形成した。次に実施例16と同様の電荷
発生層と電荷輸送層を形成し、電子写真用感光体を作成
した。この結果比較例17においては電荷輸送層の乾燥
時に気泡を発生し、評価に値する感光体が得られなかっ
た。以上得られた感光体を実施例16と同様に評価し、
結果を表12に示した。[0096] This was coated by dip coating on the same aluminum cylinder as in Example 16, and dried at 150°C for 20 minutes to a thickness of 13.
An intermediate layer of .mu.m was formed. Next, a charge generation layer and a charge transport layer similar to those in Example 16 were formed to produce an electrophotographic photoreceptor. As a result, in Comparative Example 17, bubbles were generated during drying of the charge transport layer, and a photoreceptor worthy of evaluation was not obtained. The photoreceptor obtained above was evaluated in the same manner as in Example 16,
The results are shown in Table 12.
【0097】[0097]
【表12】[Table 12]
【0098】実施例22
実施例19の中間層用塗布液を直径が80mm、長さ3
60mmで表面を最大表面粗さを7μmに加工したアル
ミシリンダーに浸漬塗布し、150℃で20分間乾燥し
、厚さ15μmの中間層を形成した。これに実施例1と
同様の電荷発生層、電荷輸送層を形成し、電子写真感光
体を得た。これを実施例16と同様に評価したところ5
0枚コピー後においても良好な画像が得られた。Example 22 The intermediate layer coating solution of Example 19 was coated with a diameter of 80 mm and a length of 3
The coating was applied by dip coating onto an aluminum cylinder whose surface was processed to a maximum surface roughness of 7 μm with a thickness of 60 mm, and dried at 150° C. for 20 minutes to form an intermediate layer with a thickness of 15 μm. A charge generation layer and a charge transport layer similar to those in Example 1 were formed on this to obtain an electrophotographic photoreceptor. When this was evaluated in the same manner as in Example 16, it was found to be 5.
Good images were obtained even after 0 copies were made.
【0099】0099
【発明の効果】以上説明したように、本発明によれば特
定の中間層の採用により画像特性の優れた電子写真画像
を形成することができる。As explained above, according to the present invention, an electrophotographic image with excellent image characteristics can be formed by employing a specific intermediate layer.
Claims (6)
順に設けた電子写真感光体において、前記中間層は結着
樹脂中に平均粒径0.3μm以上の粒径を有するチタン
エロー顔料を含むことを特徴とする電子写真感光体。1. An electrophotographic photoreceptor comprising an intermediate layer and a photoconductive layer provided in this order on a conductive support, wherein the intermediate layer comprises a titanium yellow pigment having an average particle size of 0.3 μm or more in a binder resin. An electrophotographic photoreceptor comprising:
順に設けた電子写真感光体において、前記中間層は結着
樹脂中に平均粒径が0.3μm以上のチタンエロー顔料
、及び二酸化チタン顔料を含むことを特徴とする電子写
真感光体。2. An electrophotographic photoreceptor in which an intermediate layer and a photoconductive layer are sequentially provided on a conductive support, wherein the intermediate layer contains a titanium yellow pigment having an average particle size of 0.3 μm or more in a binder resin, and carbon dioxide. An electrophotographic photoreceptor characterized by containing a titanium pigment.
順に設けた電子写真感光体において、前記中間層は結着
剤樹脂中に平均粒径が0.3μm以上のチタンエロー顔
料、二酸化チタン顔料、及び酸化第二スズ(SnO2)
粉体を含み、かつ二酸化チタンの添加量はチタンエロー
1重量部に対し、0.1〜10重量部の範囲であり、酸
化第2スズの添加量はチタンエロー顔料と二酸化チタン
顔料の合計重量に対し、3〜30重量%であることを特
徴とする電子写真感光体。3. An electrophotographic photoreceptor in which an intermediate layer and a photoconductive layer are sequentially provided on a conductive support, wherein the intermediate layer contains a titanium yellow pigment having an average particle size of 0.3 μm or more and a titanium dioxide pigment in a binder resin. Titanium pigment and stannic oxide (SnO2)
Contains powder, and the amount of titanium dioxide added is in the range of 0.1 to 10 parts by weight per 1 part by weight of titanium yellow, and the amount of stannic oxide added is based on the total weight of titanium yellow pigment and titanium dioxide pigment. , 3 to 30% by weight.
、二酸化チタン顔料及び酸化第二スズ粉体の合計(P)
と結着剤樹脂(R)との比P/Rは体積比で1/1〜3
/1であることを特徴とする電子写真感光体。4. The total amount (P) of titanium yellow pigment, titanium dioxide pigment, and stannic oxide powder in claim 3.
The ratio P/R of and binder resin (R) is 1/1 to 3 in terms of volume ratio.
An electrophotographic photoreceptor characterized in that: /1.
順に設けた電子写真感光体において、前記中間層は結着
剤樹脂中に平均粒径が0.3μm以上のチタンエロー顔
料、二酸化チタン顔料、及び酸化インジウム(In2O
3)粉体を含み、かつ二酸化チタンはチタンエロー1重
量部に対し、0.1〜10重量部の範囲であり、酸化イ
ンジウムの添加量はチタンエロー顔料と二酸化チタン顔
料の合計重量に対し、3〜30重量%であることを特徴
とする電子写真感光体。5. An electrophotographic photoreceptor in which an intermediate layer and a photoconductive layer are sequentially provided on a conductive support, wherein the intermediate layer contains a titanium yellow pigment having an average particle size of 0.3 μm or more, and a titanium dioxide pigment in a binder resin. Titanium pigment, and indium oxide (In2O
3) Contains powder, and titanium dioxide is in the range of 0.1 to 10 parts by weight per 1 part by weight of titanium yellow, and the amount of indium oxide added is 3 to 10 parts by weight with respect to the total weight of titanium yellow pigment and titanium dioxide pigment. An electrophotographic photoreceptor characterized in that the content is 30% by weight.
二酸化チタン顔料、及び酸化インジウム粉体の合計(P
)と結着剤樹脂(R)との比(P/R比)が体積比で1
/1〜3/1の範囲であることを特徴とする電子写真感
光体。6. A titanium yellow pigment according to claim 5,
Total of titanium dioxide pigment and indium oxide powder (P
) and the binder resin (R) (P/R ratio) is 1 in volume ratio.
1. An electrophotographic photoreceptor characterized in that the photoreceptor has a photoreceptor having a photoresistance of 1/1 to 3/1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19661191A JPH04356055A (en) | 1990-11-27 | 1991-08-06 | electrophotographic photoreceptor |
Applications Claiming Priority (5)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP32081490 | 1990-11-27 | ||
| JP2-320814 | 1990-11-27 | ||
| JP3-37768 | 1991-02-08 | ||
| JP3776891 | 1991-02-08 | ||
| JP19661191A JPH04356055A (en) | 1990-11-27 | 1991-08-06 | electrophotographic photoreceptor |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH04356055A true JPH04356055A (en) | 1992-12-09 |
Family
ID=27289582
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP19661191A Pending JPH04356055A (en) | 1990-11-27 | 1991-08-06 | electrophotographic photoreceptor |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH04356055A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2014171338A1 (en) * | 2013-04-16 | 2014-10-23 | Canon Kabushiki Kaisha | Electrophotographic photosensitive member, method for manufacturing the same, process cartridge, and electrophotographic apparatus |
-
1991
- 1991-08-06 JP JP19661191A patent/JPH04356055A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2014171338A1 (en) * | 2013-04-16 | 2014-10-23 | Canon Kabushiki Kaisha | Electrophotographic photosensitive member, method for manufacturing the same, process cartridge, and electrophotographic apparatus |
| JP2014209153A (en) * | 2013-04-16 | 2014-11-06 | キヤノン株式会社 | Electrophotographic photoreceptor, manufacturing method of electrophotographic photoreceptor, process cartridge, and electrophotographic device |
| CN105143988A (en) * | 2013-04-16 | 2015-12-09 | 佳能株式会社 | Electrophotographic photosensitive member, manufacturing method thereof, process cartridge, and electrophotographic apparatus |
| US9557664B2 (en) | 2013-04-16 | 2017-01-31 | Canon Kabushiki Kaisha | Electrophotographic photosensitive member, method for manufacturing the same, process cartridge, and electrophotographic apparatus |
| CN105143988B (en) * | 2013-04-16 | 2019-10-22 | 佳能株式会社 | Electrophotographic photosensitive member, manufacturing method thereof, process cartridge, and electrophotographic apparatus |
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