JPH04240862A - Electrophotographic sensitive body - Google Patents
Electrophotographic sensitive bodyInfo
- Publication number
- JPH04240862A JPH04240862A JP2384991A JP2384991A JPH04240862A JP H04240862 A JPH04240862 A JP H04240862A JP 2384991 A JP2384991 A JP 2384991A JP 2384991 A JP2384991 A JP 2384991A JP H04240862 A JPH04240862 A JP H04240862A
- Authority
- JP
- Japan
- Prior art keywords
- resin
- layer
- intermediate layer
- parts
- solvent
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
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- 229920005989 resin Polymers 0.000 claims description 74
- 239000011347 resin Substances 0.000 claims description 74
- 108091008695 photoreceptors Proteins 0.000 claims description 44
- 239000012046 mixed solvent Substances 0.000 claims description 14
- 150000002576 ketones Chemical class 0.000 claims description 8
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- 238000010309 melting process Methods 0.000 claims 1
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- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 abstract description 33
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- 235000000177 Indigofera tinctoria Nutrition 0.000 description 2
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- COHYTHOBJLSHDF-UHFFFAOYSA-N indigo powder Natural products N1C2=CC=CC=C2C(=O)C1=C1C(=O)C2=CC=CC=C2N1 COHYTHOBJLSHDF-UHFFFAOYSA-N 0.000 description 2
- 229910003437 indium oxide Inorganic materials 0.000 description 2
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- 238000000746 purification Methods 0.000 description 2
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- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
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Landscapes
- Photoreceptors In Electrophotography (AREA)
- Processes Of Treating Macromolecular Substances (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し
、詳しくは支持体と感光層との間に設けられた中間層を
有する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, and more particularly to an electrophotographic photoreceptor having an intermediate layer provided between a support and a photosensitive layer.
【0002】0002
【従来の技術】一般に、カールソンタイプの電子写真感
光体においては、帯電−露光を繰り返したときに一定の
画像濃度とカブリのない画像を形成するうえで、暗部電
位と明部電位の安定性が重要になっている。[Prior Art] In general, in a Carlson type electrophotographic photoreceptor, stability of dark area potential and bright area potential is required to form a constant image density and fog-free image when charging and exposure are repeated. It has become important.
【0003】このため、支持体から感光層への電荷注入
性改良、支持体から感光層との接着性改良、感光層の塗
工性向上、支持体上の欠陥の被覆などの機能を有する中
間層を支持体と感光層との間に設けることが提案されて
いる。[0003] For this reason, an intermediate having functions such as improving charge injection from the support to the photosensitive layer, improving adhesion between the support and the photosensitive layer, improving coatability of the photosensitive layer, and covering defects on the support has been developed. It has been proposed to provide a layer between the support and the photosensitive layer.
【0004】また、感光層を電荷発生層と電荷輸送層に
機能分離した積層構造を有するものが提案されているが
、一般に電荷発生層は極めて薄い層として、例えば0.
5μm程度で設けられているため、支持体表面の欠陥、
汚れ、付着物または傷などが電荷発生層の膜厚を不均一
とする原因となる。電荷発生層の膜厚が不均一であると
感光体に感度ムラを生じるので、電荷発生層をできるだ
け均一なものとすることが要求されている。[0004]Also, a layered structure in which the photosensitive layer is functionally separated into a charge generation layer and a charge transport layer has been proposed, but generally the charge generation layer is an extremely thin layer, for example, 0.0000.
Since it is provided with a thickness of about 5 μm, defects on the support surface,
Dirt, deposits, scratches, etc. cause the charge generation layer to have an uneven thickness. If the thickness of the charge generation layer is non-uniform, uneven sensitivity will occur in the photoreceptor, so it is required that the charge generation layer be made as uniform as possible.
【0005】このようなことから電荷発生層と支持体と
の間にバリヤー層としての機能、接着層としての機能お
よび支持体上の欠陥を被覆する機能を有する中間層を設
けることが提案されている。For this reason, it has been proposed to provide an intermediate layer between the charge generation layer and the support, which functions as a barrier layer, an adhesive layer, and covers defects on the support. There is.
【0006】これまで感光層と支持体との間に設ける層
として、ポリアミド(特開昭46−47344号、特開
昭52−25638号)、ポリエステル(特開昭52−
20836号、特開昭54−26738号)、ポリウレ
タン(特開昭49−10044号、特開昭53−894
35号)、カゼイン(特開昭55−103556号)、
ポリペプチド(特開昭53−48523号)、ポリビニ
ルアルコール(特開昭52−100240号)、ポリビ
ニルピロリドン(特開昭48−30936号)、酢酸ビ
ニル−エチレン共重合体(特開昭48−26141号)
、無水マレイン酸エステル重合体(特開昭52−101
38号)、ポリビニルブチラール(特開昭57−906
39号、特開昭58−106549号)、第四級アンモ
ニウム塩含有重合体(特開昭51−126149号、特
開昭56−60448号)、エチルセルロース(特開昭
55−143564号)などを用いることが知られてい
る。Up to now, polyamide (JP-A-46-47344, JP-A-52-25638) and polyester (JP-A-52-25638) have been used as a layer between the photosensitive layer and the support.
20836, JP-A-54-26738), polyurethane (JP-A-49-10044, JP-A-53-894)
No. 35), casein (JP-A-55-103556),
Polypeptide (JP-A-53-48523), polyvinyl alcohol (JP-A-52-100240), polyvinylpyrrolidone (JP-A-48-30936), vinyl acetate-ethylene copolymer (JP-A-48-26141) issue)
, maleic anhydride ester polymer (JP-A-52-101
No. 38), polyvinyl butyral (JP-A-57-906)
39, JP 58-106549), quaternary ammonium salt-containing polymers (JP 51-126149, JP 56-60448), ethyl cellulose (JP 55-143564), etc. known to be used.
【0007】特にアルコール可溶性のナイロン樹脂、好
ましくは共重合ナイロン樹脂又はアルコキシメチル化ナ
イロン樹脂は多くの溶媒に可溶でかつ成膜性に優れるこ
とから、従来より実用化されている。In particular, alcohol-soluble nylon resins, preferably copolymerized nylon resins or alkoxymethylated nylon resins, are soluble in many solvents and have excellent film-forming properties, and have thus far been put into practical use.
【0008】[0008]
【発明が解決しようとする課題】しかしながら、前述の
材料を中間層として用いた電子写真感光体では、材料中
に含まれる不純物(モノマー、オリゴマー及び重合開始
剤、重合停止剤などの残留成分など)の存在により、次
のような問題を生じることが多い。[Problems to be Solved by the Invention] However, in electrophotographic photoreceptors using the above-mentioned materials as intermediate layers, impurities contained in the materials (monomers, oligomers, residual components such as polymerization initiators, polymerization terminators, etc.) The presence of , often causes the following problems.
【0009】温湿度変化により中間層の抵抗が変化して
、低温低湿下から高温高湿下の全環境に対して常に安定
した電位特性、画質が得るのが困難であった。The resistance of the intermediate layer changes due to changes in temperature and humidity, making it difficult to always obtain stable potential characteristics and image quality in all environments, from low temperature and low humidity to high temperature and high humidity.
【0010】例えば、中間層の抵抗が高くなる低温低湿
下では感光体を繰り返し使用した場合、中間層に電荷が
残留する結果、明部電位及び、残留電位が上昇し、コピ
ーした画像にカブリを生じた。また、反転現像を行なう
電子写真方式のプリンターにこのような感光体を装着し
た場合には、画像が薄くなったり、一定の画質を有する
コピーが得られないという問題があった。For example, if a photoreceptor is used repeatedly under low temperature and low humidity conditions where the resistance of the intermediate layer increases, charges remain in the intermediate layer, resulting in an increase in bright area potential and residual potential, causing fog on copied images. occured. Further, when such a photoreceptor is installed in an electrophotographic printer that performs reversal development, there are problems in that the image becomes pale and copies with a certain image quality cannot be obtained.
【0011】また、高温高湿下になると中間層の低抵抗
化により、バリヤー機能が低下して、支持体側からのキ
ャリアー注入が増える結果、暗部電位が低下してしまう
。この原因で、高温高湿下ではコピーした画像の濃度が
低くなったり、反転現像を行なう電子写真方式のプリン
ターにこのような感光体を装着した場合には、画像に黒
点状の欠陥(黒ポチ)、およびカブリを生じ易くなると
いった問題があった。[0011] Furthermore, under high temperature and high humidity conditions, the barrier function decreases due to the lower resistance of the intermediate layer, and as a result, carrier injection from the support side increases, resulting in a decrease in dark area potential. As a result, the density of copied images becomes low under high temperature and high humidity conditions, and when such a photoreceptor is installed in an electrophotographic printer that performs reversal development, black dot-like defects (black spots) may appear on the image. ), and fogging is likely to occur.
【0012】さらに不純物の種類によってはキャリアが
トラップされて感度低下を来すといった問題があった。
中間層用樹脂中の不純物を取り除く方法としては、良溶
媒に該樹脂を完全に溶解して形成された溶液を貧溶媒中
に滴下して樹脂を再沈澱させる再沈法または樹脂を完全
には溶解せず、かつ不純物を溶出する溶媒で洗浄する洗
浄法がある。Furthermore, depending on the type of impurity, there is a problem that carriers may be trapped, resulting in a decrease in sensitivity. The impurities in the resin for the intermediate layer can be removed by the reprecipitation method, in which the resin is completely dissolved in a good solvent, and the resulting solution is dropped into a poor solvent to reprecipitate the resin, or by the reprecipitation method, in which the resin is completely dissolved. There is a cleaning method that uses a solvent that does not dissolve impurities and elutes them.
【0013】しかし、再沈法は大量の溶媒を必要とする
上に、良溶媒に溶解した樹脂を貧溶媒中に滴下する際に
沈澱した樹脂がからみつく結果、洗浄が充分に行なわれ
ず、樹脂中に不純物が残留したり、洗浄操作がバッチ式
で得られる樹脂の純度が不均一になるという問題があっ
た。However, the reprecipitation method requires a large amount of solvent, and when the resin dissolved in a good solvent is dropped into a poor solvent, the precipitated resin gets tangled, resulting in insufficient washing and There are problems in that impurities remain in the resin and that the purity of the resin obtained when the washing operation is done in batches becomes uneven.
【0014】一方、洗浄法は溶媒中に樹脂を投入及び分
散させて樹脂中の不純物を溶出することからなる樹脂の
精製法である。処が、従来はアルコール可溶性のナイロ
ン樹脂特に、共重合ナイロン樹脂又はアルコキシメチル
化ナイロン樹脂を溶解せず、かつ樹脂中の不純物のみを
効率よく溶出除去する適当な溶媒が無いことから、良好
な特性の中間層が安定して得られなかった。[0014] On the other hand, the washing method is a resin purification method that involves introducing and dispersing the resin in a solvent to elute impurities in the resin. However, conventionally, there has been no suitable solvent that does not dissolve alcohol-soluble nylon resins, especially copolymerized nylon resins or alkoxymethylated nylon resins, and that can efficiently elute and remove only impurities in the resins, so it has not been possible to obtain good properties. A stable intermediate layer could not be obtained.
【0015】したがって、本発明の目的は低温低湿下か
ら高温高湿下に至る全環境に対して安定した電位特性と
画像の得られる電子写真感光体を提供することにある。Therefore, an object of the present invention is to provide an electrophotographic photoreceptor that can provide stable potential characteristics and images in all environments from low temperature and low humidity to high temperature and high humidity.
【0016】また、本発明の別の目的は支持体上の結果
を十分に被覆できる中間層を形成させて。欠陥のない良
好な画像を形成し得る電子写真感光体を提供することに
ある。Another object of the present invention is to form an intermediate layer which can sufficiently cover the result on the support. An object of the present invention is to provide an electrophotographic photoreceptor that can form good images without defects.
【0017】[0017]
【課題を解決するための手段】すなわち、本発明の電子
写真感光体は支持体上に中間層を介して感光層を有する
電子写真感光体において、該中間層がアルコール類とケ
トン類とを含む混合溶媒中において対象樹脂を完全には
溶解せず該溶媒と接触処理されたアルコール可溶性ナイ
ロン樹脂、好ましくは共重合ナイロン樹脂又はアルコキ
シメチル化ナイロン樹脂を含有することを特徴とする電
子写真感光体である。[Means for Solving the Problems] That is, the electrophotographic photoreceptor of the present invention has a photosensitive layer on a support via an intermediate layer, and the intermediate layer contains an alcohol and a ketone. An electrophotographic photoreceptor characterized by containing an alcohol-soluble nylon resin, preferably a copolymerized nylon resin or an alkoxymethylated nylon resin, which does not completely dissolve the target resin in a mixed solvent but has been subjected to contact treatment with the solvent. be.
【0018】本発明に用いられるアルコール可溶性ナイ
ロン樹脂として好適なものは6−,11−,12−,6
,6−,6,10−などの成分を含む多元共重合ナイロ
ン樹脂又はN−アルコキシメチル化ナイロン樹脂;芳香
族成分を含むナイロン樹脂などが挙げられる。例えば下
記に示すようなものである。Preferred alcohol-soluble nylon resins used in the present invention are 6-, 11-, 12-, and 6-
, 6-, 6, 10-, or N-alkoxymethylated nylon resins; nylon resins containing aromatic components; and the like. For example, as shown below.
【0019】[0019]
【表1】
処理対象樹脂は溶媒との接触を行なう前に適当な大きさ
に粉細しておくことが好ましい。[Table 1] The resin to be treated is preferably pulverized to an appropriate size before contacting with the solvent.
【0020】本発明の中間層に用いるアルコール可溶性
ナイロン樹脂、好ましくは共重合ナイロン樹脂又はアル
コキシメチル化ナイロン樹脂を処理するために用いる溶
媒としては、樹脂中に浸透し不純物を効率よく抽出しか
つ、樹脂を溶解せず、洗浄中に溶媒中に樹脂が不均一に
存在するようなものが必要である。The solvent used for treating the alcohol-soluble nylon resin, preferably the copolymerized nylon resin or the alkoxymethylated nylon resin used in the intermediate layer of the present invention, is a solvent that penetrates into the resin and efficiently extracts impurities. What is needed is something that will not dissolve the resin and will have a non-uniform presence of the resin in the solvent during washing.
【0021】このような溶媒としてアルコール類とケト
ン類を含む混合溶媒を用いた場合特に良好な結果が得ら
れた。Particularly good results were obtained when a mixed solvent containing alcohols and ketones was used as such a solvent.
【0022】これはアルコール可溶性ナイロン樹脂、好
ましくは共重合ナイロン樹脂又はアルコキシメチル化ナ
イロン樹脂に対するアルコール類の優れた浸透性とケト
ン類の優れた抽出力の組合わせによるものと考えられる
。本発明の方法によれば他の精製法に比べ少量の溶媒で
均一かつ高純度に樹脂を洗浄することが可能である。
ケトン類の例としてはアセトン、メチルエチルケトン(
MEK)メチルイソブチルケトン(MIBK)、ジエチ
ルケトンなどがあげられる。アルコール類の例としては
メタノール、エタノール、n−ブタノール、イソプロパ
ノール、n−プロパノールなどがあげられる。ケトン類
、アルコール類それぞれ1種類または、1種類以上を選
択する。さらに必要に応じて他類溶媒(例えば、エーテ
ル類、石油類、セルソルブ類エステル類など)を加えて
もかまわない。This is believed to be due to the combination of the excellent permeability of alcohols to alcohol-soluble nylon resins, preferably copolymerized nylon resins or alkoxymethylated nylon resins, and the excellent extraction power of ketones. According to the method of the present invention, it is possible to wash the resin uniformly and with high purity using a small amount of solvent compared to other purification methods. Examples of ketones include acetone, methyl ethyl ketone (
MEK) methyl isobutyl ketone (MIBK), diethyl ketone, etc. Examples of alcohols include methanol, ethanol, n-butanol, isopropanol, n-propanol, and the like. Select one type or more than one type each of ketones and alcohols. Furthermore, other solvents (eg, ethers, petroleum, cellosolve esters, etc.) may be added as necessary.
【0023】アルコール類、ケトン類の混合比率は樹脂
が適度に膨潤し、かつ不均一になる(完全に溶解して均
一化したり、樹粉末が固まらない)ような条件を選択す
る。樹脂の一部が溶解するていどの溶解性は問題となら
ない。[0023] The mixing ratio of alcohols and ketones is selected so that the resin swells appropriately and becomes non-uniform (completely dissolved and homogenized, and the wood powder does not harden). Solubility is not a problem, even if a portion of the resin is dissolved.
【0024】アルコール類又はそれ以外があまり多くな
ると混合溶媒としても効果が薄くなるのでアルコール類
が5%〜95%特には20〜80%が好ましい。溶媒を
用いる処理例えば、洗浄においては溶媒温度を混合溶媒
系の共沸点以下に設定して不純物の抽出効率を高めるこ
とも可能である。例えば、メタノールにメチルエチルケ
トンの組み合わせについては、メタノール5〜50%、
好ましくは20〜40%(v/v)である。[0024] If alcohol or other substances are too large, the effect as a mixed solvent will be weakened, so alcohol is preferably 5% to 95%, particularly 20 to 80%. In processing using a solvent, for example, in cleaning, it is also possible to increase the efficiency of extracting impurities by setting the solvent temperature below the azeotropic point of the mixed solvent system. For example, for a combination of methanol and methyl ethyl ketone, methanol 5-50%,
Preferably it is 20-40% (v/v).
【0025】また、樹脂に対する溶媒の使用料は重量比
で前者/後者=1/3以上、好ましくは1/5以上に選
ぶ。[0025] The amount of solvent to be used relative to the resin is selected so that the weight ratio of the former/latter is 1/3 or more, preferably 1/5 or more.
【0026】また、樹脂が固着しないためおよび不純物
の抽出効率を高めるため洗浄中に溶媒を攪拌してもよい
。洗浄は1回でも良いが、2回、3回行なうことにより
より高い純度が得られる。[0026] Furthermore, the solvent may be stirred during washing to prevent the resin from sticking and to improve the efficiency of extracting impurities. Although washing may be carried out once, higher purity can be obtained by washing twice or three times.
【0027】本発明の中間層はアルコール可溶性ナイロ
ン樹脂、好ましくは共重合ナイロン樹脂又はアルコキシ
メチル化ナイロン樹脂のみで構成されていても良く、必
要に応じて二種類以上のアルコール可溶性ナイロン樹脂
、好ましくは共重合ナイロン樹脂又はアルコキシメチル
化ナイロン樹脂の混合系、他の樹脂、添加剤を加えた系
で構成されていてもよい。ここで加える他の樹脂の例と
しては、ポリエステル、ポリウレタン、ポリウレア、フ
エノール樹脂などが挙げられる。添加剤の例としては、
シリコーン樹脂などの粉体類、界面活性剤、シリコーン
レーベリング剤、シランカップリング剤、チタネートカ
ップリング剤などが挙げられる。The intermediate layer of the present invention may be composed only of an alcohol-soluble nylon resin, preferably a copolymerized nylon resin or an alkoxymethylated nylon resin, or, if necessary, two or more alcohol-soluble nylon resins, preferably It may be composed of a mixed system of copolymerized nylon resin or alkoxymethylated nylon resin, or a system to which other resins and additives are added. Examples of other resins added here include polyester, polyurethane, polyurea, phenolic resin, and the like. Examples of additives include:
Examples include powders such as silicone resins, surfactants, silicone labeling agents, silane coupling agents, and titanate coupling agents.
【0028】このような中間層を有する電子写真感光体
の層構成を第1図に示す。中間層2は感光層1と導電性
支持体3の間に設けられている。The layer structure of an electrophotographic photoreceptor having such an intermediate layer is shown in FIG. The intermediate layer 2 is provided between the photosensitive layer 1 and the conductive support 3.
【0029】本発明の中間層の膜厚は、電子写真特性お
よび支持体上の欠陥を考慮して設定されるものであり、
0.1〜50μm、特に0.5〜5μmの範囲が好まし
い。中間層の塗工は浸漬コーティング、スプレーコーテ
ィング、ロールコーティングなどの方法で行うことがで
きる。The thickness of the intermediate layer of the present invention is determined by taking into consideration the electrophotographic properties and defects on the support.
A range of 0.1 to 50 μm, particularly 0.5 to 5 μm is preferred. The intermediate layer can be applied by dip coating, spray coating, roll coating, or the like.
【0030】本発明においては、感光層は単一層型でも
、電荷発生層と電荷輸送層に機能分離した積層構造型で
も良い。In the present invention, the photosensitive layer may be of a single layer type or of a laminated structure type in which the functions are separated into a charge generation layer and a charge transport layer.
【0031】積層構造型感光層の電荷発生層はスーダン
レッド、ダイアンブルーなどのアゾ顔料。ピレンキノン
、アントアントロンなどのキノン顔料、キノシアニン顔
料、ペリレン顔料、インジゴ、チオインシゴなどのイン
ジゴ顔料、アズレニウム塩顔料、銅フタロシアニン、ア
ルミクロルフタロシアニンなどのフタロシアニン顔料な
どの電荷発生物質をポリビニルブチラール、ポリスチレ
ン、ポリ酢酸ビニル、アクリル樹脂、ポリビニルピロリ
ドン、エチルセルロース、酢酸酪酸セルロースなどの結
着剤樹脂に分散させて、この分散液を前述の中間層の上
に塗工することによって形成できる。このような、電荷
発生層の膜厚は、5μm以下、好ましくは0.05〜2
μmである。The charge generating layer of the laminated photosensitive layer is an azo pigment such as Sudan Red or Diane Blue. Charge-generating substances such as quinone pigments such as pyrenequinone and anthanthrone, quinocyanine pigments, perylene pigments, indigo pigments such as indigo and thioinsigo, phthalocyanine pigments such as azulenium salt pigments, copper phthalocyanine, and aluminophthalocyanine, polyvinyl butyral, polystyrene, and polyacetic acid. It can be formed by dispersing it in a binder resin such as vinyl, acrylic resin, polyvinylpyrrolidone, ethyl cellulose, cellulose acetate butyrate, and coating this dispersion on the above-mentioned intermediate layer. The thickness of such a charge generation layer is 5 μm or less, preferably 0.05 to 2 μm.
It is μm.
【0032】電荷発生層の上に設ける電荷輸送層は、主
鎖または側鎖にビフェニレン、アントラセン、ピレン、
フェナントレンなどの構造を有する多環芳香族化合物、
インドール、カルバゾール、オキサジアゾール、ピラゾ
リンなどの含窒素環式化合物、ヒドラゾン化合物、スチ
リル化合物などの電荷輸送物質を成膜性を有する樹脂に
溶解させた塗工液を用いて形成される。このようにして
形成する理由は、電荷輸送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 transport layer provided on the charge generation layer has biphenylene, anthracene, pyrene,
Polycyclic aromatic compounds with structures such as phenanthrene,
It is formed using a coating liquid in which a charge transport substance such as a nitrogen-containing cyclic compound such as indole, carbazole, oxadiazole, or pyrazoline, a hydrazone compound, or a styryl compound is dissolved in a resin that has film-forming properties. The reason why it is formed in this way is that the charge transport material generally has a low molecular weight and has poor film-forming properties by itself.
【0033】このような成膜性を有する樹脂としてはポ
リエステル、ポリカーボネート、ポリメタクリル酸エス
テル、ポリスチレンなどが挙げられる。Examples of resins having such film-forming properties include polyester, polycarbonate, polymethacrylate, and polystyrene.
【0034】電荷輸送層の膜厚は5〜40μm、特には
10〜30μmの範囲が好ましい。The thickness of the charge transport layer is preferably in the range of 5 to 40 μm, particularly 10 to 30 μm.
【0035】なお、電荷輸送層は電荷発生層の下に設け
てもよい。Note that the charge transport layer may be provided below the charge generation layer.
【0036】また、単一層型感光層は、前述の電荷発生
物質と電荷輸送物質を前述のような適当なバインダー樹
脂に同時に含有させて形成することができる。この場合
の膜厚は8〜50μm、特には10〜40μmの範囲が
好ましい。Further, a single layer type photosensitive layer can be formed by simultaneously containing the above-mentioned charge generating substance and charge transporting substance in the above-mentioned suitable binder resin. In this case, the film thickness is preferably in the range of 8 to 50 μm, particularly 10 to 40 μm.
【0037】さらに、本発明では、ポリビニルカルバゾ
ール、ポリビニルアントラセンなどの有機光導電性ポリ
マー層:セレン蒸着層、セレン−テルル蒸着層、アルモ
ルファスシリコン層なども感光層に用いることができる
。Furthermore, in the present invention, an organic photoconductive polymer layer such as polyvinylcarbazole or polyvinylanthracene, such as a selenium vapor deposited layer, a selenium-tellurium vapor deposited layer, or an amorphous silicon layer, can also be used as the photosensitive layer.
【0038】なお、感光層の上には耐久性向上のための
保護層を設けてもよい。Note that a protective layer may be provided on the photosensitive layer to improve durability.
【0039】一方、本発明で用いる支持体は導電性を有
するものであれば、何れのものでもよく、例えばアルミ
ニウム、銅、クロム、ニッケル、亜鉛、ステンレスなど
の金属をドラムまたはシート状に成型したもの、アルミ
ニウムや銅などの金属箔をプラスチックフィルムにラミ
ネートしたもの、アルミニウム、酸化インジウム、酸化
スズなどをプラスチックフィルムに蒸着したもの、ある
いは、導電性物質を単独または適当なバインダー樹脂と
ともに塗布して導電層を設けた金属、プラスチックフィ
ルム、紙などが挙げられる。On the other hand, the support used in the present invention may be any material as long as it has electrical conductivity, such as a drum or sheet made of metal such as aluminum, copper, chromium, nickel, zinc, or stainless steel. conductive materials, laminated metal foils such as aluminum or copper on plastic films, vapor-deposited materials such as aluminum, indium oxide, tin oxide, etc. on plastic films, or conductive materials coated alone or with a suitable binder resin. Examples include layered metal, plastic film, and paper.
【0040】この導電層に用いられる導電性物質として
は、アルミニウム、銅、ニッケル、銀などの金属粉体、
金属箔および、金属短繊維;酸化アンチモン、酸化イン
ジウム、酸化スズなどの導電性金属酸化物;ポリピロー
ル、ポリアニリン、高分子電解質などの高分子導電材;
カーボンファイバー、カーボンブラック、グラファイト
粉体;有機および無機の電解質;またはこれらの導電性
物質で表面を被覆した導電性粉体などが挙げられる。[0040] As the conductive substance used for this conductive layer, metal powder such as aluminum, copper, nickel, silver, etc.
Metal foils and short metal fibers; conductive metal oxides such as antimony oxide, indium oxide, and tin oxide; polymer conductive materials such as polypyrrole, polyaniline, and polymer electrolytes;
Examples include carbon fiber, carbon black, graphite powder; organic and inorganic electrolytes; and conductive powder whose surface is coated with these conductive substances.
【0041】また、導電層に用いられるバインダー樹脂
としては、ポリアミド、ポリエステル、アクリル樹脂、
ポリアミノ酸エステル、ポリ酢酸ビニル、ポリカーボネ
ート、ポリビニルホルマール、ポリビニルブチラール、
ポリビニルアルキルエーテル、ポリアルキレンエーテル
、ポリウレタンエラストマーなどの熱可塑性樹脂や、熱
硬化性ポリウレタン、フェノール樹脂、エポキシ樹脂な
どの熱硬化性樹脂が挙げられる。Binder resins used for the conductive layer include polyamide, polyester, acrylic resin,
Polyamino acid ester, polyvinyl acetate, polycarbonate, polyvinyl formal, polyvinyl butyral,
Examples include thermoplastic resins such as polyvinyl alkyl ether, polyalkylene ether, and polyurethane elastomer, and thermosetting resins such as thermosetting polyurethane, phenol resin, and epoxy resin.
【0042】導電性物質とバインダー樹脂の重量混合比
は、10:1〜1:10、特には5:1〜1:5の範囲
が好ましい。この混合比は導電層の抵抗値、表面性、塗
布適性などを考慮して決められる。The weight mixing ratio of the conductive substance and the binder resin is preferably in the range of 10:1 to 1:10, particularly 5:1 to 1:5. This mixing ratio is determined in consideration of the resistance value, surface properties, coating suitability, etc. of the conductive layer.
【0043】導電性物質が粉体の場合にはボールミル、
ロールミル、サンドミルなどを用いて常法により混合物
を調製して用いる。When the conductive substance is a powder, a ball mill,
A mixture is prepared and used in a conventional manner using a roll mill, sand mill, etc.
【0044】また、他の添加剤として界面活性剤、シラ
ンカップリング剤、チタネートカップリング剤、シリコ
ーンオイル、シリコーンレベリング剤などを添加しても
よい。[0044] Other additives such as surfactants, silane coupling agents, titanate coupling agents, silicone oil, and silicone leveling agents may also be added.
【0045】また、本発明におけるアルコール可溶性ナ
イロン樹脂、好ましくは共重合ナイロン樹脂又はアルコ
キシメチル化ナイロン樹脂を含有する中間層は、導電性
物質を含有することにより導電性の中間層として用いて
もよい。この場合の導電性物質例、導電性物質と樹脂の
混合比、調製法、加えてもよい他の添加剤例は前記の導
電層の場合と同様である。Furthermore, the intermediate layer containing an alcohol-soluble nylon resin, preferably a copolymerized nylon resin or an alkoxymethylated nylon resin in the present invention may be used as a conductive intermediate layer by containing a conductive substance. . Examples of the conductive substance in this case, the mixing ratio of the conductive substance and the resin, the preparation method, and examples of other additives that may be added are the same as in the case of the conductive layer described above.
【0046】なお、この導電性の中間層を設ける支持体
は、支持体自体が導電性でなくてもよい。Note that the support provided with this conductive intermediate layer does not need to be conductive itself.
【0047】さらに、バリヤー性のコントロールなどの
ために、この導電性の中間層上には樹脂を主成分とする
第二の中間層を設けてもよい。Furthermore, in order to control barrier properties, a second intermediate layer containing resin as a main component may be provided on this conductive intermediate layer.
【0048】この第二の中間層に用いられる樹脂材料と
しては、ポリアミド、ポリエステル、ポリウレタン、ポ
リウレア、フェノール樹脂などが挙げられる。[0048] Examples of the resin material used for the second intermediate layer include polyamide, polyester, polyurethane, polyurea, and phenol resin.
【0049】この第二の中間層の厚さは、0.1〜5μ
mが好適である。[0049] The thickness of this second intermediate layer is 0.1 to 5μ.
m is preferred.
【0050】本発明の電子写真感光体は、複写機、レー
ザープリンター、LEDプリンター、液晶シャッター式
プリンターなどの電子写真装置一般に適用し得るが、さ
らに電子写真技術を応用したディスプレー、記録、軽印
刷、製版、ファクシミリなどの装置にも幅広く適用し得
るものである。The electrophotographic photoreceptor of the present invention can be applied to general electrophotographic devices such as copying machines, laser printers, LED printers, and liquid crystal shutter printers, but it can also be applied to displays, recording, light printing, etc. that apply electrophotographic technology. It can also be widely applied to devices such as plate making and facsimile machines.
【0051】以下に、具体的実施例を挙げて、本発明を
さらに詳しく説明する。The present invention will be explained in more detail below with reference to specific examples.
【0052】[0052]
【実施例】実施例1
10%の酸化アンチモンを含有する酸化スズで被覆した
導電性酸化チタン粉体50部、フェノール樹脂25部、
メチルセロソルブ20部、メタノール5部およびシリコ
ーンオイル(ポリジメチルシロキサンポリオキシアルキ
レン共重合体、平均分子量3000)0.002部をφ
1mmガラスビーズを用いたサンドミル装置で2時間分
散して導電層用塗料を調製した。[Example] Example 1 50 parts of conductive titanium oxide powder coated with tin oxide containing 10% antimony oxide, 25 parts of phenolic resin,
20 parts of methyl cellosolve, 5 parts of methanol and 0.002 part of silicone oil (polydimethylsiloxane polyoxyalkylene copolymer, average molecular weight 3000) were added to φ
A conductive layer paint was prepared by dispersing for 2 hours in a sand mill using 1 mm glass beads.
【0053】アルミニウムシリンダー(外径30mm×
長さ260mm)上に、上記塗料を浸漬塗布し、140
℃で30分間乾燥させ、膜厚20μmの導電層を形成し
た。[0053] Aluminum cylinder (outer diameter 30mm x
The above paint was applied by dip coating on the 140 mm length).
It was dried at ℃ for 30 minutes to form a conductive layer with a thickness of 20 μm.
【0054】次にN−メトキシメチル化ナイロン6の洗
浄工程として、
N−メトキシメチル化ナイロン6
100重量部(商品名:トレシンEF
30T帝国化学産業製)をメチルエチルケトン(MEK
) 1000重量部
メタノール
400重量部の混
合溶媒中に投入した。Next, as a cleaning step for N-methoxymethylated nylon 6, N-methoxymethylated nylon 6
100 parts by weight (Product name: Toreshin EF
30T (manufactured by Teikoku Kagaku Sangyo) to methyl ethyl ketone (MEK)
) 1000 parts by weight
methanol
The mixture was poured into 400 parts by weight of a mixed solvent.
【0055】3時間撹拌しながら洗浄した後ヌッチェ上
で溶媒と樹脂を分離する。After washing with stirring for 3 hours, the solvent and resin are separated on a Nutsche.
【0056】再度樹脂を
メチルエチルケトン(MEK)
1000重量部 メタノール
400重量部の混合溶媒中に投入し3時
間撹拌しながら洗浄した後ヌッチェで溶媒を分離した。
樹脂は5時間風乾した後80℃で4時間熱乾燥した。[0056] Re-resin methyl ethyl ketone (MEK)
1000 parts by weight methanol
The mixture was poured into 400 parts by weight of a mixed solvent and washed with stirring for 3 hours, after which the solvent was separated using a Nutsche filter. The resin was air-dried for 5 hours and then heat-dried at 80° C. for 4 hours.
【0057】次に中間層の塗料の作成として上記洗浄ず
みN−メトキシメチル化ナイロン6、10重量部をメタ
ノール45重量部とn−ブタノール、45重量部に溶解
し中間層塗料を調製した。Next, to prepare an intermediate layer paint, 10 parts by weight of the washed N-methoxymethylated nylon 6.1 was dissolved in 45 parts by weight of methanol and 45 parts by weight of n-butanol to prepare an intermediate layer paint.
【0058】この塗料を、上記導電層上に浸漬塗布し、
100℃で20分間乾燥させ、膜厚0.6μmの中間層
を形成した。[0058] This paint is dip-coated on the conductive layer, and
It was dried at 100° C. for 20 minutes to form an intermediate layer with a thickness of 0.6 μm.
【0059】次に下記構造式Next, the following structural formula
【0060】[0060]
【化1】
のジスアゾ顔料3部、ポリビニルベンザール(ベンザー
ル化率80%、重量平均分子量11000)2部および
シクロヘキサノン35部をφ1mmガラスビーズを用い
たサンドミル装置で12時間分散した後、メチルエチル
ケトン(MEK)60部を加えて電荷発生層用分散液を
調製した。この分散液を上記の中間層上に浸漬塗布し、
80℃で20分間乾燥させ、膜厚0.2μmの電荷発生
層を形成した。After dispersing 3 parts of the disazo pigment of [Chemical 1], 2 parts of polyvinyl benzal (benzalization rate 80%, weight average molecular weight 11000) and 35 parts of cyclohexanone for 12 hours in a sand mill apparatus using φ1 mm glass beads, methyl ethyl ketone (MEK) was dispersed for 12 hours. ) to prepare a dispersion for a charge generation layer. This dispersion is dip coated onto the above intermediate layer,
It was dried at 80° C. for 20 minutes to form a charge generation layer with a thickness of 0.2 μm.
【0061】次に下記構造式Next, the following structural formula
【0062】[0062]
【化2】
のスチリル化合物10部およびポリカーボネート(重量
平均分子量46000)10部をジクロルメタン20部
、モノクロルベンゼン40部の混合溶媒中に溶解し、こ
の溶液を上記の電荷発生層上に浸漬塗布し、120℃で
60分間乾燥させ、膜厚18μmの電荷輸送層を形成し
た。10 parts of the styryl compound of formula 2 and 10 parts of polycarbonate (weight average molecular weight 46,000) are dissolved in a mixed solvent of 20 parts of dichloromethane and 40 parts of monochlorobenzene, and this solution is dip coated on the above charge generation layer, It was dried at 120° C. for 60 minutes to form a charge transport layer with a thickness of 18 μm.
【0063】このようにして製造した電子写真感光体を
、帯電−露光−現像−転写−クリーニングのプロセスを
1.5秒サイクルで繰り返す反転現像方式のレーザープ
リンターに取り付け、露光量を1.7μJ/cm2 に
調整し、常温常湿下(23℃、50%RH)および高温
高湿下(30℃、85%RH)の環境で電子写真特性の
評価を行った。The electrophotographic photoreceptor thus produced was attached to a reversal development type laser printer in which the process of charging, exposure, development, transfer and cleaning was repeated in a 1.5 second cycle, and the exposure amount was set at 1.7 μJ/. cm2, and the electrophotographic properties were evaluated under normal temperature and normal humidity (23°C, 50% RH) and high temperature and high humidity (30°C, 85% RH) environments.
【0064】この結果、表1に示すように実施例1の感
光体では、暗部電位(VD )と明部電位(VL )の
差が大きく、十分な電位コントラストが得られたととも
に、高温高湿下でも暗部電位(VD )は安定し、黒点
上の欠陥(黒ポチ)、カブリのない良好な画像が得られ
た。
実施例2〜5
中間層に用いるN−メトキシメチル化6−ナイロンの洗
浄に用いる混合溶媒を表1に示したものをそれぞれ用い
たほかは、実施例1と同様にして電子写真感光体を製造
し、それぞれ実施例2〜5とした。As a result, as shown in Table 1, in the photoreceptor of Example 1, the difference between the dark area potential (VD) and the light area potential (VL) was large, and sufficient potential contrast was obtained. The dark potential (VD) was stable even under low conditions, and good images without black dot defects (black spots) or fog were obtained. Examples 2 to 5 Electrophotographic photoreceptors were produced in the same manner as in Example 1, except that the mixed solvents shown in Table 1 were used to wash the N-methoxymethylated 6-nylon used in the intermediate layer. and Examples 2 to 5, respectively.
【0065】これらの感光体を実施例1と同様にして評
価したところ、いずれも高温高湿下でも暗部電位(VD
)は安定し、黒点上の欠陥(黒ポチ)、かぶりのない
良好な画像が得られた。When these photoreceptors were evaluated in the same manner as in Example 1, all of them showed low dark potential (VD) even under high temperature and high humidity.
) was stable, and a good image was obtained without defects on black spots (black spots) or fog.
【0066】この結果を表2に示す。The results are shown in Table 2.
【0067】[0067]
【表2】
比較例1
中間層用塗料として未精製のN−メトキシメチル化6−
ナイロンを用いたほかには、実施例1と同様にして電子
写真感光体を製造し、比較例1とした。[Table 2] Comparative Example 1 Unrefined N-methoxymethylated 6- as intermediate layer paint
An electrophotographic photoreceptor was produced as Comparative Example 1 in the same manner as in Example 1 except that nylon was used.
【0068】この感光体を実施例1と同様にして評価し
たところ、常温常湿下(23℃、50%RH)下で明部
電位(VL )が高く感度低下が見られ電位コントラス
トも低下している。さらに高温高湿下になると帯電能が
悪化し、暗部電位(VD )の低下が見られ、画像上に
は黒点上の欠陥(黒ポチ)が発生するようになった。こ
の結果を表2に示す。
比較例2
中間層用塗料としてN−メトキシメチル化ナイロン6を
100重量部用いて400重量部のメタノールに溶解し
、1000重量部のメチルエチルケトン中に滴下して樹
脂分を再沈精製し、ヌッチェ上にて溶媒を分離した後に
、80℃で1晩真空乾燥したものを比較品として用いた
ほかには、実施例1と同様にして電子写真感光体を製造
し、比較例2とした。When this photoreceptor was evaluated in the same manner as in Example 1, the bright area potential (VL) was high at room temperature and humidity (23° C., 50% RH), and a decrease in sensitivity was observed, as well as a decrease in potential contrast. ing. Furthermore, under high temperature and high humidity conditions, the charging ability deteriorated, a decrease in dark area potential (VD) was observed, and defects on black spots (black spots) began to appear on the image. The results are shown in Table 2. Comparative Example 2 100 parts by weight of N-methoxymethylated nylon 6 was used as an intermediate layer paint, dissolved in 400 parts by weight of methanol, and dropped into 1000 parts by weight of methyl ethyl ketone to purify the resin by reprecipitation. An electrophotographic photoreceptor was produced in the same manner as in Example 1, and was used as Comparative Example 2, except that after the solvent was separated at 100° C., the product was vacuum-dried at 80° C. overnight and used as a comparison product.
【0069】この感光体を実施例1と同様にして評価し
たところ、高温高湿下になると帯電能が悪化し、暗部電
位(VD )の低下が見られ、画像上には黒点上の欠陥
(黒ポチ)が発生するようになった。この結果を表3に
示す。
比較例3
中間層用塗料として、N−メトキシメチル化6−ナイロ
ン10重量部をメチルエチルケトン100重量部により
70℃で5時間還流加熱して熱洗浄したものを比較精製
品として用いたほかには、実施例1と同様にして電子写
真感光体を製造し、比較例3とした。When this photoreceptor was evaluated in the same manner as in Example 1, it was found that under high temperature and high humidity conditions, the charging ability deteriorated, the dark area potential (VD) decreased, and defects (black spots) appeared on the image. Black spots) now occur. The results are shown in Table 3. Comparative Example 3 As a paint for the intermediate layer, 10 parts by weight of N-methoxymethylated 6-nylon was heated under reflux at 70°C for 5 hours with 100 parts by weight of methyl ethyl ketone and then heat-washed, which was used as a comparative purified product. An electrophotographic photoreceptor was produced in the same manner as in Example 1, and Comparative Example 3 was prepared.
【0070】この感光体を実施例1と同様に評価したと
ころ、高温高湿下になると帯電能が悪化し、暗部電位(
VD )の低下が見られ、画像上には全面にかぶりが発
生するようになった。この結果を表3に示す。When this photoreceptor was evaluated in the same manner as in Example 1, it was found that the charging ability deteriorated under high temperature and high humidity conditions, and the dark area potential (
A decrease in VD was observed, and fog appeared over the entire image. The results are shown in Table 3.
【0071】[0071]
【表3】 実施例6 実施例1と同様の中間層用塗料を調製した。[Table 3] Example 6 A paint for an intermediate layer similar to that in Example 1 was prepared.
【0072】この塗料をマルミニウムシリンダー(外径
30mm×長さ360mm)上に浸漬塗布し、100℃
で15分間乾燥させ、膜厚1.2μmの中間層を形成し
た。[0072] This paint was dip-coated onto a marminium cylinder (outer diameter 30 mm x length 360 mm) and heated at 100°C.
It was dried for 15 minutes to form an intermediate layer with a thickness of 1.2 μm.
【0073】次に、下記構造式Next, the following structural formula
【0074】[0074]
【化3】
のジスアゾ顔料4部、ポリビニルブチラール(ブチラー
ル化率68%、重量平均分子量24000)2部および
シクロヘキサノン34部をφ1mmガラスビーズを用い
たサンドミル装置で42時間分散した後、メチルエチル
ケトン(MEK)60部を加えて電荷発生層用分散液を
調製した。この分散液を上記それぞれの中間層上に浸漬
塗布し、80℃で15分間乾燥させ、膜厚0.15μm
の電荷発生層を形成した。After dispersing 4 parts of the disazo pigment of [Chemical 3], 2 parts of polyvinyl butyral (butyralization rate: 68%, weight average molecular weight: 24,000) and 34 parts of cyclohexanone for 42 hours in a sand mill device using φ1 mm glass beads, methyl ethyl ketone (MEK) was dispersed. A dispersion liquid for a charge generation layer was prepared by adding 60 parts. This dispersion was dip coated onto each of the above intermediate layers and dried at 80°C for 15 minutes to give a film thickness of 0.15 μm.
A charge generation layer was formed.
【0075】次に、実施例1で用いたスチリル化合物1
0部およびポリカーボネート(重量平均分子量6300
0)10部をジクロルメタン15部、モノクロルベンゼ
ン45部の混合溶媒中に溶解し、この溶液を上記の電荷
発生層上に浸漬塗布し、120℃で60分間乾燥させ、
膜厚25μmの電荷輸送層を形成した。Next, styryl compound 1 used in Example 1
0 parts and polycarbonate (weight average molecular weight 6300
0) Dissolve 10 parts in a mixed solvent of 15 parts of dichloromethane and 45 parts of monochlorobenzene, apply this solution by dip coating onto the above charge generation layer, and dry at 120°C for 60 minutes.
A charge transport layer having a thickness of 25 μm was formed.
【0076】このようにして製造した電子写真感光体を
、帯電−露光(露光量2.2lux・sec)−現像−
転写−クリーニングのプロセスを0.6秒サイクルで繰
り返す複写機に取り付けた。The electrophotographic photoreceptor thus produced was charged, exposed (exposure amount: 2.2 lux·sec), developed, and
It was installed in a copying machine that repeated the transfer-cleaning process in 0.6 second cycles.
【0077】この感光体に対して低温低湿下(15℃、
15%RH)の環境で電子写真特性の評価を行ったとこ
ろ、表2に示すように、この感光体は暗部電位(VD
)と明部電位(VL )との差が大きく、十分な電位コ
ントラストが得られた。さらに、連続1000枚の画像
を出したところ、明部電位(VL )の上昇もなく非常
に安定した画像が得られた。
実施例7〜10
中間層用塗料として実施例2〜5のものをそれぞれ用い
たほかには、実施例6と同様にして電子写真感光体を製
造し、それぞれ実施例7〜10とした。[0077] This photoreceptor was exposed to low temperature and low humidity (15°C,
When the electrophotographic characteristics were evaluated in an environment of 15% RH), as shown in Table 2, this photoreceptor had a
) and the bright area potential (VL), and sufficient potential contrast was obtained. Furthermore, when 1000 images were continuously produced, very stable images were obtained without any rise in bright area potential (VL). Examples 7 to 10 Electrophotographic photoreceptors were produced in the same manner as in Example 6, except that Examples 2 to 5 were used as intermediate layer coatings, respectively, to give Examples 7 to 10, respectively.
【0078】これらの感光体を実施例6と同様にして評
価したところ、いずれの感光体も暗部電位(VD )と
明部電位(VL )との差が大きく、十分な電位コント
ラストが得られるとともに連続1000枚の画像を出し
ても、明部電位(VL )の上昇がほとんどなく非常に
安定した画像が得られた。この結果を表4に示す。
比較例4
中間層用塗料として比較例2、3を用いたほかには、実
施例6と同様にして電子写真感光体を製造し、比較例4
及び5とした。When these photoreceptors were evaluated in the same manner as in Example 6, the difference between the dark area potential (VD) and the light area potential (VL) was large for each photoreceptor, and sufficient potential contrast was obtained. Even when 1000 images were continuously produced, very stable images were obtained with almost no increase in bright area potential (VL). The results are shown in Table 4. Comparative Example 4 An electrophotographic photoreceptor was produced in the same manner as in Example 6, except that Comparative Examples 2 and 3 were used as the intermediate layer paint, and Comparative Example 4
and 5.
【0079】この感光体を実施例6と同様にして評価し
たところ、連続1000枚の繰り返しで明部電位(VL
)が上昇し、画像上にはカブリを生じるようになった
。この結果を表4に示す。When this photoreceptor was evaluated in the same manner as in Example 6, the bright area potential (VL
) increased, causing fog to appear on the image. The results are shown in Table 4.
【0080】[0080]
【表4】
実施例11
6,12,66,610−四元共重合ナイロン(樹
脂) 100重量部 〔商品名:CM−8000(
東レ社製)〕を
n−ブタノール
200
重量部 メタノール
200重量部 メチルエチルケトン
1000重量部からなる混合溶媒中に投入して2時間
撹拌しながら洗浄した後に、ヌッチェで溶媒を分離した
。得られた洗浄済樹脂は5時間風乾した後に80℃で4
時間熱乾燥した。
次にこの共重合ナイロン10重量部をn−ブタノール5
0重量部、メタノール40重量部に溶解し中間層塗料を
調製した。この塗布液を実施例1で用いた導電層上に浸
漬塗布して1.2μm厚の中間層を形成させた。[Table 4] Example 11 6,12,66,610-quaternary copolymerized nylon (resin) 100 parts by weight [Product name: CM-8000 (
(manufactured by Toray Industries, Inc.)] n-butanol
200
Part by weight Methanol
200 parts by weight methyl ethyl ketone
After pouring into a mixed solvent of 1000 parts by weight and washing with stirring for 2 hours, the solvent was separated using a Nutsche. The obtained washed resin was air-dried for 5 hours and then heated at 80°C for 4 hours.
Heat dried for an hour. Next, 10 parts by weight of this copolymerized nylon was mixed with 5 parts by weight of n-butanol.
0 parts by weight and 40 parts by weight of methanol to prepare an intermediate layer paint. This coating solution was applied by dip coating onto the conductive layer used in Example 1 to form an intermediate layer with a thickness of 1.2 μm.
【0081】次に、下記構造式Next, the following structural formula
【0082】[0082]
【化4】
のジスアゾ顔料2部、ポリビニルブチラール(ブチラー
ル化率72%、重量平均分子量18000)1部および
シクロヘキサノン30部をφ1mmガラスビーズを用い
たサンドミル装置で20時間分散した後、メチルエチル
ケトン(MEK)65部を加えて電荷発生層用分散液を
調製した。この分散液を第二の中間層上に浸漬塗布し、
80℃で20分間乾燥させ、膜厚0.2μmの電荷発生
層を形成した。After dispersing 2 parts of the disazo pigment of [Chemical 4], 1 part of polyvinyl butyral (butyralization rate 72%, weight average molecular weight 18,000) and 30 parts of cyclohexanone in a sand mill device using φ1 mm glass beads for 20 hours, methyl ethyl ketone (MEK) was dispersed. A dispersion liquid for a charge generation layer was prepared by adding 65 parts. This dispersion is dip coated onto the second intermediate layer,
It was dried at 80° C. for 20 minutes to form a charge generation layer with a thickness of 0.2 μm.
【0083】次に下記構造式Next, the following structural formula
【0084】[0084]
【化5】
のヒドラゾン化合物10部およびポリカーボネート(重
量平均分子量46000)10部をジクロルメタン20
部、モノクロルベンゼン40部の混合溶媒中に溶解し、
この溶液を上記の電荷発生層上に浸漬塗布し、120℃
で60分間乾燥させ、膜厚23μmの電荷輸送層を形成
した。10 parts of the hydrazone compound of formula 5 and 10 parts of polycarbonate (weight average molecular weight 46,000) were mixed with 20 parts of dichloromethane.
part, dissolved in a mixed solvent of 40 parts of monochlorobenzene,
This solution was dip coated onto the above charge generation layer and heated to 120°C.
This was dried for 60 minutes to form a charge transport layer with a thickness of 23 μm.
【0085】このようにして製造した電子写真感光体を
、帯電−露光(露光量2.8lux・sec)−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
り返す複写機に取り付けた。The electrophotographic photoreceptor thus produced was charged, exposed (exposure amount: 2.8 lux·sec), developed, and
It was installed in a copying machine that repeated the transfer-cleaning process in a 0.8 second cycle.
【0086】この感光体に対して低温低湿下(10℃、
10%RH)の環境で電子写真特性の評価を行ったとこ
ろ、表3に示すように、この感光体は暗部電位(VD
)と明部電位(VL )の差が大きく、十分な電位コン
トラストが得られた。さらに、連続1000枚の画像を
出したところ、明部電位(VL )の上昇もなく非常に
安定した画像が得られた。
実施例12
6,66,610−四元共重合ナイロン〔商品名:アミ
ラン4000(東レ社製)〕100重量部をn−ブタノ
ール200重量部、エタノール200重量部及びメチル
エチルケトン1000重量部からなる混合溶媒で洗浄す
る他には実施例11と同様にして導電性の中間層、電荷
発生層および電荷輸送層を形成し、実施例12の電子写
真感光体を製造した。[0086] This photoreceptor was exposed to low temperature and low humidity (10°C,
When the electrophotographic characteristics were evaluated in an environment of 10%RH), as shown in Table 3, this photoreceptor had a
) and the bright area potential (VL), and sufficient potential contrast was obtained. Furthermore, when 1000 images were continuously produced, very stable images were obtained without any rise in bright area potential (VL). Example 12 100 parts by weight of 6,66,610-quaternary copolymerized nylon [trade name: Amilan 4000 (manufactured by Toray Industries, Inc.)] was mixed with a mixed solvent consisting of 200 parts by weight of n-butanol, 200 parts by weight of ethanol, and 1000 parts by weight of methyl ethyl ketone. A conductive intermediate layer, a charge generation layer, and a charge transport layer were formed in the same manner as in Example 11 except for washing with water, and an electrophotographic photoreceptor of Example 12 was manufactured.
【0087】この感光体を実施例11と同様にして評価
したところ、暗部電位(VD )と明部電位(VL )
との差が大きく、十分な電位コントラストが得られると
ともに連続1000枚の画像を出しても、明部電位(V
L )の上昇がほとんどなく非常に安定した画像が得ら
れた。
この結果を表5に示す。
比較例6及び7
6,12,66,610−四元共重合ナイロン、6,6
6,610−三元共重合ナイロン樹脂からなる未洗浄の
ものを用いたほかには、実施例11および12と同様に
して電子写真感光体を製造し、それぞれ比較例6及び7
とした。When this photoreceptor was evaluated in the same manner as in Example 11, the dark area potential (VD) and the light area potential (VL)
The bright area potential (V
A very stable image was obtained with almost no increase in L). The results are shown in Table 5. Comparative Examples 6 and 7 6,12,66,610-quaternary copolymerized nylon, 6,6
Electrophotographic photoreceptors were produced in the same manner as in Examples 11 and 12, except that an unwashed one made of 6,610-terpolymerized nylon resin was used, and Comparative Examples 6 and 7 were produced, respectively.
And so.
【0088】この各感光体を実施例11と同様にして評
価したところ、比較例4では連続1000枚の繰り返し
で明部電位(VL )が上昇し、画像上にはカブリを生
じるようになった。この結果を表4に示す。[0088] When each of these photoreceptors was evaluated in the same manner as in Example 11, it was found that in Comparative Example 4, the bright area potential (VL) increased after 1000 continuous sheets were printed, and fog appeared on the image. . The results are shown in Table 4.
【0089】[0089]
【表5】[Table 5]
【0090】[0090]
【発明の効果】本発明の電子写真感光体は支持体と感光
層との間の中間層としてアルコール類とケトン類とを含
む混合溶媒中において実質的には溶解せずに不均一な状
態で洗浄されたアルコール可溶性のナイロン樹脂を含有
する樹脂層を設けることにより、低温低湿下から高温高
湿下に至る全環境において安定した電位特性を保ち、良
好な画像を形成させ得る。Effects of the Invention The electrophotographic photoreceptor of the present invention does not substantially dissolve in a mixed solvent containing alcohols and ketones as an intermediate layer between the support and the photosensitive layer, but remains in a non-uniform state. By providing a resin layer containing a washed alcohol-soluble nylon resin, stable potential characteristics can be maintained in all environments from low temperature and low humidity to high temperature and high humidity, and good images can be formed.
【図1】図1は電子写真感光体の層構成の概略断面図を
示す。FIG. 1 shows a schematic cross-sectional view of the layer structure of an electrophotographic photoreceptor.
1 感光層 2 本発明の中間層 3 支持体 1 Photosensitive layer 2 Intermediate layer of the present invention 3 Support
Claims (2)
する電子写真感光体において、該中間層がアルコール類
とケトン類とを含む混合溶媒中において完全には溶解せ
ずに該溶媒と接解処理されたアルコール可溶性ナイロン
樹脂を含有することを特徴とする電子写真感光体。Claim 1: In an electrophotographic photoreceptor having a photosensitive layer on a support via an intermediate layer, the intermediate layer does not completely dissolve in a mixed solvent containing alcohols and ketones, and is mixed with the solvent. An electrophotographic photoreceptor characterized by containing an alcohol-soluble nylon resin that has been subjected to a melting process.
合ナイロン樹脂又はアルコキシメチル化ナイロンである
ことを特徴とする請求項1に記載の電子写真感光体。2. The electrophotographic photoreceptor according to claim 1, wherein the alcohol-soluble nylon resin is a copolymerized nylon resin or an alkoxymethylated nylon.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2384991A JP2887209B2 (en) | 1991-01-25 | 1991-01-25 | Electrophotographic photoreceptor |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2384991A JP2887209B2 (en) | 1991-01-25 | 1991-01-25 | Electrophotographic photoreceptor |
Publications (2)
Publication Number | Publication Date |
---|---|
JPH04240862A true JPH04240862A (en) | 1992-08-28 |
JP2887209B2 JP2887209B2 (en) | 1999-04-26 |
Family
ID=12121860
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP2384991A Expired - Fee Related JP2887209B2 (en) | 1991-01-25 | 1991-01-25 | Electrophotographic photoreceptor |
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JP (1) | JP2887209B2 (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2001312078A (en) * | 2000-04-28 | 2001-11-09 | Sharp Corp | Electrophotographic photoreceptor and method for manufacturing the same |
JP2007052255A (en) * | 2005-08-18 | 2007-03-01 | Ricoh Co Ltd | Electrophotographic photoreceptor, electrophotographic apparatus, and process cartridge for same |
-
1991
- 1991-01-25 JP JP2384991A patent/JP2887209B2/en not_active Expired - Fee Related
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2001312078A (en) * | 2000-04-28 | 2001-11-09 | Sharp Corp | Electrophotographic photoreceptor and method for manufacturing the same |
JP2007052255A (en) * | 2005-08-18 | 2007-03-01 | Ricoh Co Ltd | Electrophotographic photoreceptor, electrophotographic apparatus, and process cartridge for same |
US7960081B2 (en) | 2005-08-18 | 2011-06-14 | Ricoh Company, Ltd. | Electrophotographic photoreceptor having N-alkoxymethylated nylon intermediate layer, and image forming apparatus having the electrophotographic photoreceptor |
Also Published As
Publication number | Publication date |
---|---|
JP2887209B2 (en) | 1999-04-26 |
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