JPS60166953A - Manufacture of vapor deposition source selenium material of photosensitive layer - Google Patents

Abstract

PURPOSE:To obtain a vapor deposition source Se material for forming a photosensitive layer good in repeating fatigue resisting characteristics by distilling the Se material specified in compsn. in vacuum, condensing it in an inert gas atm., remelting it, and dropping it into water to form granules. CONSTITUTION:An Se material having a specified compsn., such as Se-Te alloy, is distilled in vacuum, the obtained molten material is collected and condensed in an amt. of inert gas, such as N2, to form ingots. They are heated again in the inert gas atm. to melt them, and dropped into waer to form granules, thus manufacturing the intended vapor deposition source Se material. The electrophotographic sensitive body of Se obtained by vapor depositing this material on a conductive substrate is not deteriorated in copied image quality even by repeated uses, and it can form always sharp images.

Description

DETAILED DESCRIPTION OF THE INVENTION [Technical Field to which the Invention Pertains] The present invention relates to a method for producing a selenium material for use as a raw material for photosensitive layer vapor deposition, which is used to produce a selenium photoreceptor for electrophotography by vapor depositing it on a conductive support.

[Prior art and its problems]

A selenium photoreceptor widely used in electrophotography is manufactured by vacuum-depositing a selenium material such as selenium, a selenium alloy, or a selenium compound onto a conductive support made of aluminum or the like. Conventionally, this type of photoreceptor has had problems such as fatigue characteristics when repeatedly operated in an electrophotographic apparatus, such as a decrease in the contrast of a copied image due to a decrease in surface potential, or a decrease in image quality due to an increase in residual potential. In order to suppress the increase in residual potential, for example, impurities or oxides have been added to the selenium material, and some effects have been obtained. However, no significant measures have been taken to suppress the decrease in surface potential.

[Purpose of the invention]

In view of this, it is an object of the present invention to provide a method for producing a selenium material for use as a raw material for photosensitive layer deposition, which can suppress repeated fatigue properties, particularly reductions in surface potential.

[Key points of the invention]

According to the present invention, a selenium material for vapor deposition raw material that can achieve the above objective U] is obtained by vacuum distilling a selenium material having a predetermined composition and pulverizing the obtained selenium material liquid with nitrogen.

[Embodiments of the invention]

Conventionally, for example, in order to produce a vapor deposition raw material for a selenium-tellurium alloy, a commercially available Se alloy containing 5.5% by weight of Te was
It is heated to 0"C and distilled at I Torr, and the liquid that sticks to the vessel wall is collected in the atmosphere and made into an ingot. This ingot is heated to 380℃ in the atmosphere to melt it, and then dropped into water. In contrast, in the embodiment of the present invention, a liquid selenium-tellurium alloy obtained by vacuum distillation was collected into an ingot in a nitrogen gas atmosphere, and then heated with nitrogen at the same temperature as described above. Melting in the atmosphere,
Granular selenium-tellurium alloy was obtained by gamma potting in water.

5e02 in each 40 t of the pellets obtained by such conventional methods and Examples was analyzed by infrared spectroscopy. In infrared spectroscopy, the 760 cm-' peak (
'l'e02) and 250cTrL (Se 8 ring
) was calculated using the following formula.

Table 1 shows the oxidation degree of the materials measured by the conventional method and the examples of the present invention.

It can be seen from Table 1 that the degree of oxidation of the materials obtained by the examples of the present invention has less variation than that of the conventional method, and is a low value of 10 or less.

Next, these eight types of materials were vacuum-deposited onto an aluminum photoreceptor substrate using an evaporation source. The substrate temperature is approximately ω℃, the pressure is 1O-5Torr, and the evaporation source temperature is 340℃, approximately ωμ.
A charge transport layer of conventional thickness was obtained. Then on top of this 5e-5,
A charge generating layer having a thickness of 5 μm was laminated using a 5e-12 heavy f% Te alloy obtained by the conventional method and an example of the present invention as a vapor deposition raw material in the same manner as the 5 wt % Te alloy. In this way, four photoreceptors A-1, A-2, and
A-3, A-4, and four photoreceptors B-1, B-2, B-3, and B-4 were obtained using the raw materials of Examples of the present invention.

Next, the temperature characteristics and fatigue characteristics of this photoreceptor were evaluated.

+11 Evaluation of temperature characteristics Evaluation of temperature characteristics is based on two points on the temperature dependence curve of surface potential as shown in FIG. The temperature of each photoreceptor is 20”
As shown in Table 2, the photoreceptor using the raw material according to the example of the present invention has better temperature characteristics and is stable against temperature increases. I understand.

(2) Evaluation of Fatigue Characteristics Eight photoreceptors were subjected to the electrophotographic process 1,000 times in a copying machine, and the amount of charge reduction was calculated based on the difference between the first to fifth times and after 1,000 times. In addition, the half-attenuation exposure amount and residual potential after repetition were measured. Table 3 shows the results.

Table 3 Photoreceptors using the raw materials obtained in accordance with the examples of the present invention have better fatigue characteristics with respect to charge reduction, and other characteristics are similar to those obtained by conventional methods.

It is presumed that this improvement in properties is due to the low degree of oxidation of the vapor deposition raw material.

Similarly, for Se-based photosensitive layer materials other than the 5e-Te alloy, the vapor deposition raw materials prepared by the method according to the present invention showed improvement in the fatigue properties of the finished photoreceptors.

〔Effect of the invention〕

In the present invention, the process from distillation to granulation during the production of selenium material used as a vapor deposition raw material for electrophotographic selenium photoreceptors is carried out in an inert gas atmosphere such as nitrogen gas without contact with air. This provides a material with a low degree of oxidation. For example, by using such a selenium-tellurium alloy, the temperature characteristics of an electrophotographic photoreceptor are improved, and the amount of charge reduction in an actual copying process is less than half that when using a conventional material. Therefore, by using the selenium material according to the present invention, the quality of copied images does not deteriorate due to repeated copying, and extremely clear images can always be obtained.

[Brief explanation of drawings]

Claims (1)

[Claims] 1) A method for producing a vapor deposition raw material for manufacturing a selenium photoreceptor for electrophotography by vapor depositing it on a conductive support, the selenium material liquid obtained by vacuum distilling a selenium material having a predetermined composition. A method for producing a selenium material as a raw material for photosensitive layer deposition, comprising collecting and solidifying the selenium material in an inert gas atmosphere, melting it again in an inert gas atmosphere, and dropping it into water to form particles.