JPH0222664A - Production of electrophotographic sensitive body - Google Patents

Abstract

PURPOSE:To simplify a pretreatment process and to obtain a good washing effect by washing a substrate with water or an aqueous solution at a temperature of >=90 deg.C as the pretreatment process to form an oxide hydrate on the surface of the substrate and depositing a photosensitive film on this oxide hydrate. CONSTITUTION:The substrate is washed with water or an aqueous solution at a temperature of >=90 deg.C to form the oxide hydrate on the surface of the substrate as the pretreatment process before forming the photosensitive layer, and the photosensitive layer is formed on the oxide hydrate. The washing treatment is executed by dipping the substrate into the hot water, or blowing steam, or doing the like, thus permitting a good washing effect to be obtained in a short time, and adhesion between the substrate and the vapor deposited film of the photosensitive layer to be remarkably enhanced by the oxide hydrate layer formed at the time of the pretreatment, and an oxidation step to be omitted.

Description

DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a method for manufacturing an electrophotographic photoreceptor in which a photosensitive layer is coated on the surface of a substrate made of aluminum or an aluminum alloy.

[Conventional technology]

An electrophotographic photoreceptor used in an electrophotographic copying machine is usually manufactured by vacuum-depositing an inorganic material such as selenium or a selenium alloy onto the surface of a cylindrical base made of a conductive metal such as aluminum or an aluminum alloy. In this case, the oxide film formed on the surface of the substrate before vacuum deposition has a charge potential retention rate and residual potential.

Affects cyclic fatigue characteristics, etc. For example, if the thickness of this oxide film is as thin as the thickness of a natural oxide film (10 to 15 A0), it will not function sufficiently as a blocking layer against charge injection from the substrate, so the required charge potential will not be sufficient. Unable to obtain retention rate. On the other hand, if the oxide film is extremely thick, the residual potential becomes high, causing problems such as fogging of the copy image source and a decrease in AI contrast. Furthermore, if the cleanliness of the substrate surface before vapor deposition is not good, the adhesion of the oxide film may be poor in some areas, and variations may occur within the oxide film surface, resulting in black spots or white spots on the copied image, or in the worst case scenario. In some cases, pinholes occur due to film peeling.

[Problem to be solved by the invention]

For this reason, a pretreatment step is adopted before the step of applying a photoresist film to the substrate of the photoreceptor, and conventionally, the following pretreatment step has been carried out. That is, first, the substrate is cleaned with trichlene, nitrile, alkali, or pure water. Next, a thermal oxidation operation is started to provide an oxide film of sufficient thickness as a blocking layer for charge injection. Therefore, there was a problem in that it required a lot of work time and man-hours. Furthermore, the adhesion between the aluminum or aluminum alloy substrate and the deposited film after thermal oxidation is not necessarily high, and higher adhesion has been required.

This invention eliminates the above-mentioned drawbacks, simplifies the pretreatment process, provides good cleaning effects in a short time, and forms an oxide film as a protective and king layer for charge injection from the substrate. An object of the present invention is to provide a method for manufacturing an electrophotographic photoreceptor that provides high-quality images.

[Means for solving line waste]

In order to achieve the above-mentioned purpose, the following pretreatment process was carried out before the formation of the photosensitive layer. That is, in a method for producing an electrophotographic photoreceptor in which a photosensitive layer is formed by vacuum-depositing selenium or a selenium alloy on the surface of a substrate made of aluminum or an aluminum alloy, the substrate is heated to a temperature of ) A water-based treatment was performed to form a hydrated oxide on the surface of the substrate, and a photoresist film was applied via the hydrated oxide.

[Effect]

A hydrated oxide layer is formed on the surface of the substrate by immersing the substrate in hot water of 90"C or higher and spraying water vapor onto the surface of the substrate, and at the same time as cleaning (this process forms an oxide film as a king layer). .

〔Example〕

FIG. 1 is a longitudinal sectional view of a processing tank used in a first embodiment of the present invention, in which an electric heater 2 is embedded in a side wall surface 1 and water W is stored inside. The temperature of the electric heater 2 is adjusted by controlling the input current by a heater power supply 3 and a temperature control circuit 4 provided outside the tank. The control circuit 4 is regulated. Note that the water W is stirred by the stirring blade 6 so that the water temperature becomes uniform. The base body 7 is immersed in water W while being supported by a supporter 8.

The pretreatment process according to the first embodiment will be explained below. First, triclean cleaning is performed to remove fats and oils adhering to the cylindrical tubular substrate 7 made of aluminum or aluminum alloy. Next, the cleaned substrate 7 is immersed in a treatment bath shown in FIG. 1 while being supported by a supporter 8ζ. At this time, the temperature of water W in the treatment tank is 50℃, 70℃, 90℃.
Six types of experiments were conducted as shown in the table below by setting the temperature to C and changing the immersion time. A 0.12.5 wt % Te layer was vacuum deposited to a thickness of about 5 μm. The deposition conditions in this case were as follows.

(I) Shaft temperature: 60°C (II) Degree of vacuum: 10-0-5Torr (evaporation source temperature: 340°C As in the typical conventional process, after cleaning with trichlorethylene, cleaning with pure water is performed for 5 minutes, and then heat treatment at a temperature of 275°C is performed for 45 minutes.After this pretreatment process, vacuum evaporation is performed on the substrate under the same evaporation conditions as above. I did it.

Table 1 shows the results of copy image tests, electrical characteristics, and adhesion tests conducted by installing the photoreceptor according to the first example prepared as described above and the photoreceptor as a comparative example in a copying machine. .

After the immersion, the substrate 7 was taken out from the processing tank, and after the moisture had evaporated, it was attached to a support shaft of a vapor deposition device (not shown), and a Se-5wt% Te layer of about 55 Pm was vacuum-deposited as a first layer on the surface of the substrate 7. , and further Se as the second layer - Table 0...Extremely good O...Good Δ...Practically acceptable In Table 1, the electrical characteristics (sensitivity v2 z and residual potential v3 are These are the surface potential and blank paper exposure potential when exposure corresponding to halftone is performed with the band potential at 700 V-constant.Charging drop ΔVB3oo and residual potential after 300 times vR3oo are obtained by repeating the normal copying process 300 times. These are the amount of decrease in the charged potential after the initial value and the residual potential after repeating 300 times.

As is clear from Table 1, the photoreceptor according to the first example had good image uniformity similar to that of the comparative example (conventional pretreatment method). Under the substrate processing conditions of 90°C for 1 minute or more (Experiments 4, 5.6), superior adhesion can be obtained compared to the comparative example. No improvement in adhesion was observed in experiment 2). Although it had little effect on practical images, processing conditions (3) 5 minutes at ℃ (experiment 5), 90"C30
(Experiment 6), there is a slight tendency for sensitivity and residual potential to deteriorate, but this is due to the oxide film being too thick.
It is presumed that this was due to an accident. Therefore, the immersion conditions are 90℃ and 1
About 2 minutes is preferable.

FIG. 2 is a longitudinal cross-sectional view of a processing tank used in a second embodiment of the present invention. Inside the tank, which is sealed with a tank wall 11, there is a cylindrical support in the center with an electric heater 12 on the side wall. A container 13 is provided. The base body 14 is fitted into this supporter 13.

A plurality of water vapor introduction pipes 15 having a plurality of nozzles 15a on the pipe wall are installed on the outer periphery of the supporter 13 and the base body 14. 16 is a discharge port. In this treatment tank, the water vapor introduced from the water vapor introduction pipe 15 is transferred to the nozzle 1.
5a, this water vapor is sprayed onto the substrate 14 to form a hydrated oxide layer on the surface of the substrate, which can remove dust adhering to the surface of the substrate. A film can be formed, and the pretreatment time before photosensitive layer deposition can be shortened. Moreover, the adhesion between the substrate on which the hydrated oxide layer is formed and the photoresist film deposited by vacuum deposition is extremely good.

The pretreatment process according to the second embodiment will be explained below. First, triclean cleaning is performed to remove fats and oils adhering to the cylindrical tubular base 14 made of aluminum or aluminum alloy. The substrate that has been cleaned is placed in the treatment tank ζ shown in FIG.
Heat. This heating is performed to prevent water droplets from forming if water vapor is directly sprayed onto the base 14 at room temperature. Base temperature is 100”
When the temperature reaches C, the steam introduced from the steam introduction pipe 15 is jetted out from the nozzle 15a, and the steam is sprayed onto the surface of the base 14 for 3 minutes. When the water vapor spraying is finished, the substrate 14 is taken out of the processing tank and attached to a support shaft of a vapor deposition device (not shown).
Se-5w1%Te layer is applied as the first layer on the surface of the
8e-12,5 as the second layer.
A wt% Te9 layer was deposited to a thickness of approximately 5 μm. The vapor deposition conditions in this case are as follows.

(I) Shaft temperature: 60°C (II) Degree of vacuum: 1Q Torr (III) Evaporation source temperature: 340°C (IV) Evaporation rate: 1 pm/min As a comparative example for the second embodiment, the substrate was used as a conventional representative substrate. Similar to the process, after washing with Triclean, wash with pure water for 5 minutes, and then reduce the temperature to 27℃.
Heat treatment at 5°C is performed for 45 minutes. After this pretreatment step, vacuum deposition was performed on the substrate under the same deposition conditions as above.

Table 2 shows the results of copy image tests, electrical characteristics, and adhesion tests conducted by installing the photoreceptor according to the second example prepared as described above and the photoreceptor as a comparative example in a copying machine. .

Table 2 shows the surface potential and blank paper exposure potential when exposure corresponding to halftone is carried out with the sensitivity (2) in the electrical characteristics and the residual potential being constant at 700 V, respectively. The charge potential drop Δ■B3oo and the residual potential after 300 times vR300 are the initial values of the charge potential after repeating the normal copying cycle 300 times (the corresponding reduction amount and the residual potential after repeating 300 times), respectively. .

As shown in Table 2, the image density and image uniformity of the photoreceptor according to the second embodiment are comparative examples (conventional pretreatment method).
Similar good results were obtained.

Furthermore, the photoreceptor according to the second example had better adhesion than the comparative example. This is a hydrated oxide layer and Se
This is thought to be due to good adhesion with the vapor deposited layer. The sensitivity and residual potential of the second example were at the same level as the comparative example.

Further, the charge reduction amount and residual potential of the example after repeating the normal copying cycle 300 times are at a low level, and are at the same level as those of the comparative example.

〔Effect of the invention〕

According to this invention, in the process of manufacturing a photoreceptor, a substrate before vapor deposition is immersed in high-temperature water, and a cleaning treatment such as spraying water vapor is applied to the substrate surface to form a hydrated oxide layer on the substrate surface in a short period of time. A good cleaning effect can be obtained. Furthermore, the adhesion between the substrate and the deposited film was significantly improved due to the hydrated oxide layer obtained at the same time. Since the conventional thermal oxidation process can be omitted as a pretreatment process, the pretreatment process is shortened and the number of work steps is also reduced.

[Brief explanation of the drawing]

FIG. 1 is a longitudinal sectional view of a processing tank device used in a first embodiment of the invention, and FIG. 2 is a longitudinal sectional view of a processing tank device used in a second embodiment of the invention. 1.11: Side wall surface % 2,12: Electric heater, 3: Heater power supply, 4: Temperature control circuit, 6: Stirring blade, 7.14:
Base, 8.13: Supporter, 15: Steam introduction pipe, 1st
Ward

Claims (1)

[Claims] 1) In a method for manufacturing an electrophotographic photoreceptor in which a photosensitive layer is formed by vacuum-depositing selenium or a selenium alloy on the surface of a substrate made of aluminum or an aluminum alloy, the substrate is heated to a temperature of 90°C as a pretreatment step before forming the photosensitive layer. 1. A method for producing an electrophotographic photoreceptor, which comprises washing the substrate with an aqueous treatment at a temperature of at least .degree.