JPH063834A - Method for manufacturing electrophotographic photoreceptor - Google Patents

Abstract

(57) [Summary] [Object] The present invention is a method for producing an electrophotographic photosensitive member, by which an electrophotographic photosensitive member having excellent image characteristics can be obtained. [Structure] In a method of manufacturing an electrophotographic photosensitive member in which a photosensitive layer is provided on a conductive support, at least the following steps are performed using an aluminum-based drum having an aqueous anodic oxide film formed on the surface as the conductive support. This is a method for manufacturing an electrophotographic photoreceptor. (1) Brush contact cleaning step with pure water at a temperature of 30 ° C to 90 ° C (2) Ultrasonic rinsing step with pure water at a temperature of 30 ° C to 90 ° C (3) Suction drying step with hot air

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for manufacturing an electrophotographic photosensitive member, and more particularly to a method for manufacturing an electrophotographic photosensitive member having excellent image characteristics.

[0002]

2. Description of the Related Art An electrophotographic photosensitive member has a structure in which a photosensitive layer is vacuum-deposited or coated on a conductive support and is used in copying machines, printers and the like. The support used for the electrophotographic photosensitive member may be any one as long as it has conductivity, but the most commonly used one is a metal drum (hereinafter referred to as a blank tube). The raw tube is a metal formed into a drum shape by impact molding, extrusion processing, drawing processing, or the like, and the surface may be further subjected to ironing processing or cutting processing. On the surface of such a raw pipe, metal powder generated in the process of raw pipe processing, dust and dust from the surrounding environment, oil used during processing, rust prevention of the surface when storing the raw pipe after processing The oil etc. applied to is adhered. Since these deposits adversely affect the image characteristics and electrophotographic properties of the electrophotographic photoreceptor after forming the photosensitive layer on the tube, it is necessary to remove these deposits in the manufacturing process of the electrophotographic photoreceptor. The tube is being cleaned. As the method for cleaning the raw tube, there are non-contact cleaning methods such as jet cleaning method, ultrasonic cleaning method, immersion cleaning method, steam cleaning method, etc., and contact cleaning method in which a brush, waste cloth, etc. are pressed against the surface of the raw tube. It is being appreciated. Methanol, ethanol, ethylene glycol, 1,3-butadiol, methylene chloride, Freon 113, Freon 225 and the like were used for these cleaning solutions. However, under the present circumstances, these organic solvents have drawbacks in hygiene, cost and environment.

[0003]

SUMMARY OF THE INVENTION The present invention provides a method for producing an electrophotographic photoreceptor having excellent image characteristics.

[0004]

The conductive support used in the present invention is an aluminum-based shell (hereinafter referred to as an alumite shell) having an aqueous anodic oxide film formed on its surface. To form an aqueous anodic oxide film on the surface of an aluminum tube, completely remove the dust, dust, oil, etc. adhering to the tube, and then conduct the conductivity in an aqueous solution of oxalic acid, sulfuric acid, etc. A method in which electrolysis is performed using a transparent support (aluminum-based tube) as an anode. As a result, an anodic oxide film is formed on the surface of the aluminum-based tube, and an alumite tube can be obtained. A water-soluble liquid is used to form the anodic oxide film, so no oily substance will adhere to the surface of the alumite tube, and the surface of the alumite tube does not rust unlike the aluminum tube. Therefore, it is not necessary to apply oil for rust prevention on the surface.
Therefore, after the alumite tube is processed, the substance that adheres to the surface of the alumite tube until the formation of the photosensitive layer is dust, dust, or a water-soluble substance. From the above and the fact that the surface of the alumite tube is an oxide film, the alumite tube can be washed with pure water.

In the present invention, the washing of the alumite tube is performed by at least the following three steps. (1) Brush contact cleaning step with pure water having a temperature of 30 ° C to 90 ° C (2) Ultrasonic rinsing step with pure water having a temperature of 30 ° C to 90 ° C (3) Suction drying step with hot air (1), (2) In the process, after forming the anodic oxide film on the raw tube, dust, dust, or water-soluble substances adhering to the surface of the raw tube are completely removed from the surface of the raw tube. Then (2)
After the process, when pulling up the drum, the pure temperature should be 80 ℃.
By keeping pure water at ˜90 ° C., the alumite tube is warmed, and the suction drying step (3) with hot air is quickly performed. Since the step (3) is completed in a short time, water-soluble impurities and the like adhere to the surface of the alumite tube during drying, and it is possible to prevent the occurrence of image noise called "water marks" in image characteristics.

In the present invention, pure water is sufficiently filtered and is kept at an electric conductivity of 3 μS / cm or less by passing through an ion-exchange resin type bath. Conductivity 3
By using pure water having a purity of μS / cm or less, it is possible to prevent image noise called "streak" in image characteristics.

After cleaning the alumite tube with pure water, the photosensitive layer is formed. As the charge generating agent used in the photosensitive layer, for example, the central metal is Cu, Co, Ni, Zn, M.
g, metal phthalocyanine such as TiO and α, β,
Examples thereof include metal-free phthalocyanine in a crystal form such as τ, τ ', η, η'. Examples of the charge transport agent used in the photosensitive layer include hydrazone compounds, styryl compounds, pyrazoline compounds, oxazole compounds, thiazole compounds, and particularly one or more hydrazone compounds and styryl compounds. It is preferable to use. The photosensitive layer according to the invention may contain a known sensitizer. In addition, if necessary, a surfactant, a plasticizer,
Antioxidants, ultraviolet absorbers, dispersion aids, antisettling agents and the like can also be used as appropriate. Further, the photoreceptor of the present invention has a structure in which a charge generating agent and a charge transporting agent are provided on the alumite tube in the same layer, which is usually referred to as a single-layer type photoreceptor, or mainly contains a charge generating agent. It is possible to have a structure generally called a laminated type photoreceptor, which is formed by laminating one layer and a second layer mainly containing a charge transfer agent on an alumite tube. In the case of a laminated type photoreceptor, which of the charge generation layer and the charge transport layer is to be the upper layer is determined by whether the chargeability is positive or negative. In general, when negatively charged, it is advantageous in terms of characteristics that the charge transport layer is an upper layer.

Examples of the present invention will be described below, but the present invention is not limited to the following examples. Less than,
In the examples, "parts" in the examples means parts by weight.

Example 1 Brush contact cleaning and ultrasonic rinsing cleaning were performed using pure water having a temperature of 55 ° C. and an electric conductivity of 1.5 μS / cm.
The τ-type metal-free phthalocyanine as a charge generating agent was added to an alumite tube that had been soaked in pure water with a conductivity of 1.5 μS / cm at 3 ° C and pulled up, and then dried by suction with hot air.
Parts, 3 parts of vinyl chloride-vinyl acetate copolymer resin (trade name VMCH manufactured by Union Carbide Co., Ltd.) together with 94 parts of tetrahydrofuran were coated with a coating solution dispersed for 2 hours in a ball mill, and 1
It was dried at 00 ° C. for 2 hours to form a 0.25 μm charge generation layer. Next, 1-benzyl-1, as a charge transport agent,
2,3,4-tetrahydroquinoline-6-carboxaldehyde-1 ', 1'-diphenylhydrazone 10 parts,
Polyester resin (product name Byron 20 manufactured by Toyobo)
A solution obtained by dissolving 0 part of 0) in 100 parts of methylene chloride was applied onto the charge generation layer and dried to form a 15 μm charge transport layer. When the electrophotographic photosensitive drum was visually observed, coating cissing did not occur. Next,
It was attached to an electrophotographic copying machine having a corona charger, an exposure part, a transfer charging part, a charge removal exposure part and a cleaner.
The dark area potential of this copier is -650 V and the light area potential is -15.
When the image obtained was set at 0 V and evaluated, it was an excellent image without black spots and streaks.

[0009]

[Example 2] Brush contact cleaning was performed using pure water having a temperature of 40 ° C and an electric conductivity of 1.7 µS / cm, and immersed in pure water having a temperature of 85 ° C and an electric conductivity of 1.7 µS / cm, and ultrasonic rinsing was performed. After pulling up, a photoreceptor similar to that of Example 1 was prepared in an alumite tube that was suction dried with hot air. Visual observation of this electrophotographic photosensitive drum revealed that coating cissing did not occur. Next, when the same image evaluation as in Example 1 was performed, it was an excellent image without black spots and streaks.

[0010]

[Comparative Example 1] An aluminum tube (no anodized film formed on the surface of the tube) was heated to 55 ° C and the electric conductivity was 1.5μ.
Brushed aluminum is cleaned with S / cm pure water and ultrasonically rinsed, immersed in pure water with a conductivity of 1.5 μS / cm at 83 ° C, pulled up, and suction dried with hot air. Then, a photoreceptor similar to that in Example 1 was manufactured. When this electrophotographic photosensitive drum was visually observed, coating cissing occurred. Next, when the same image evaluation as in Example 1 was performed, it was an image with black spots. A photoconductor similar to that of the example was manufactured on the tube.

[0011]

Comparative Example 2 Brush contact cleaning and ultrasonic rinsing cleaning were performed using pure water having a temperature of 15 ° C. and an electric conductivity of 5.5 μS / cm.
A photoreceptor similar to that of Example 1 was prepared in an alumite tube which was immersed in pure water having an electric conductivity of 1.5 μS / cm at 3 ° C., pulled up, and suction-dried with hot air. When this electrophotographic photosensitive drum was visually observed, coating cissing occurred. Next, when the same image evaluation as in the example was performed,
It was an image with a lot of black dots.

[0012]

COMPARATIVE EXAMPLE 3 Brush contact cleaning and ultrasonic rinsing cleaning were performed using pure water having a temperature of 15 ° C. and an electric conductivity of 5.5 μS / cm.
A photoreceptor similar to that of Example 1 was prepared in an alumite tube which was immersed in pure water having an electric conductivity of 1.5 μS / cm at 0 ° C., pulled up, and suction-dried with hot air. When this electrophotographic photosensitive drum was visually observed, coating cissing occurred. Next, when the same image evaluation as in the example was performed,
It was an image with black dots and streaks.

[0013]

INDUSTRIAL APPLICABILITY In a method of manufacturing an electrophotographic photosensitive member in which a photosensitive layer is provided on a conductive support, an aluminum-based drum having a water-based anodic oxide film formed on the surface thereof is used as the conductive support, and the drum is made of pure water. In the method of immersing and washing, the electrophotographic photoreceptor having excellent image characteristics can be obtained by performing at least the following steps. (1) Brush contact cleaning step with pure water at a temperature of 30 ° C to 90 ° C (2) Ultrasonic rinsing step with pure water at a temperature of 30 ° C to 90 ° C (3) Suction drying step with hot air

Front page continuation (72) Inventor Yasuhiro Fuse 2-33 Kyobashi, Chuo-ku, Tokyo Toyo Inki Manufacturing Co., Ltd. (72) Inventor Ryuichiro Kurata 2-3-3 Kyobashi, Chuo-ku, Tokyo Toyo Inki In Manufacturing Co., Ltd. (72) Inventor Toshio Nishimura 2-3-13 Kyobashi, Chuo-ku, Tokyo Toyo Inki Manufacturing Co., Ltd.

Claims (4)

[Claims] 1. A method of manufacturing an electrophotographic photosensitive member comprising a photosensitive layer provided on a conductive support, wherein an aluminum type drum having an aqueous anodic oxide film formed on the surface thereof is used as the conductive support, and the drum is made of pure water. A method for manufacturing an electrophotographic photosensitive member, which comprises performing at least the following step cleaning in the method of immersion cleaning. (1) Brush contact cleaning step with pure water at a temperature of 30 ° C to 90 ° C (2) Ultrasonic rinsing step with pure water at a temperature of 30 ° C to 90 ° C (3) Suction drying step with hot air 2. The method for producing an electrophotographic photosensitive member according to claim 1, wherein when the drum is pulled up from the step (2), the temperature of pure water is 80 ° C. to 90 ° C. 3. The method for producing an electrophotographic photosensitive member according to claim 1, wherein the pure water is pure water of 3 μs / cm or less. 4. The method for producing an electrophotographic photosensitive member according to claim 1, wherein the photosensitive layer contains at least a phthalocyanine derivative such as a metal phthalocyanine and a metal-free phthalocyanine.