JP2010145478A - Method for manufacturing electrophotographic photoreceptor - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a method for manufacturing an electrophotographic photoreceptor that does not have peel off of films in a cooling step, by which an electrophotographic photoreceptor can be inexpensively manufactured with stable qualities, by reducing the tact time and raise the capacity utilization rate, as well as, to suppress the amount of capital investment. <P>SOLUTION: The method for manufacturing an electrophotographic photoreceptor includes the steps, wherein the photoreceptor having at least a photoconductive layer formed of an amorphous material containing silicon on the surface of a cylindrical substrate having conductivity. The steps include: a film forming step of depositing at least a photoconductive layer formed of an amorphous material containing silicon on the surface of a cylindrical substrate which is held by a substrate holding member and heated, in a process container; a discharge step of removing the electrophotographic photoreceptor into air, after the film forming step; an outer surface cooling step of cooling the electrophotographic photoreceptor through the outer surface with a cooling gas after the discharge step; and an inner surface cooling step of cooling the electrophotographic photoreceptor through the inner surface with a cooling gas, after the outer surface cooling step. <P>COPYRIGHT: (C)2010,JPO&INPIT

Description

  The present invention relates to a method for producing an amorphous silicon (hereinafter also referred to as “a-Si”) electrophotographic photosensitive member, and more particularly to a cooling step of the electrophotographic photosensitive member.

  Conventionally, a plasma CVD (Chemical Vapor Deposition) method and an ion plating method are known as methods for forming an electrophotographic photosensitive member, a semiconductor device, an image input line sensor, a photographing device, and a photovoltaic device. These methods are film forming methods using plasma generated by high frequency power. Many devices for this purpose have been put into practical use.

  For example, there is a film forming method using a plasma CVD method, that is, a method of forming a deposited film by generating plasma of a source gas by glow discharge with high frequency power and depositing the decomposition species on a substrate. When this method is used, for example, it is known that an a-Si thin film can be easily formed by using a silane gas as a raw material gas, and various production apparatuses have been proposed.

  Further, when an a-Si thin film is formed on a heated substrate, the product after the formation of the a-Si thin film must be cooled, but the a-Si thin film is peeled off during cooling. There is a case where a phenomenon called peeling occurs. For this reason, a method of gradually cooling over time is generally taken. Various proposals have also been made regarding methods and apparatuses relating to cooling of products after formation of such an a-Si thin film.

  In a manufacturing device equipped with a depressurized charging chamber, heating chamber, reaction chamber, and cooling chamber, the heating and cooling chambers are always kept at a constant temperature, and the base is heated and cooled efficiently, thereby operating the equipment. An apparatus for manufacturing a photoelectric conversion member that increases the rate is disclosed (Patent Document 1).

In addition, after the film formation is completed, a cooling gas is filled in the reaction vessel at a pressure of 100 to 100,000 Pa, and a plasma processing method and apparatus for increasing the facility operation rate by performing the cooling process on the substrate after the film formation process is completed. Is disclosed (Patent Document 2).
JP 60-010681 A JP 2002-080972 A

By using the plasma processing method or apparatus as described above, the tact time can be shortened without causing film peeling. However, there is still room for improvement in order to manufacture products at a lower cost by further reducing the amount of capital investment and improving the equipment utilization rate.
For example, when the electrophotographic photosensitive member cooling process is performed using a container that can be decompressed, it is necessary to make the container strong enough to withstand the decompression environment, and a pump or piping for reducing the pressure. Such a gas exhaust facility must also be provided, and the amount of capital investment becomes high.
For this reason, although the tact time is improved by the manufacturing apparatus described above, the capital investment is high because the cooling process of the electrophotographic photosensitive member is performed in a container that can be depressurized. Therefore, in order to realize further cost reduction, it is desirable to reduce the number of containers that can be decompressed as much as possible.

In addition, when the electrophotographic photosensitive member is cooled in the reaction vessel, the film formation process cannot be performed in the reaction vessel until the cooling step is completed, and the tact time becomes longer. End up. For this reason, although the takt time is improved by the above-described plasma processing method, it is desired to perform the cooling step outside the reaction vessel in order to further reduce the takt time.
That is, a cooling method that can be carried out without using a depressurizable container such as a reaction container and does not cause film peeling is desired.

Accordingly, the present invention solves the above-mentioned problems, increases the equipment operation rate by shortening the tact time, and suppresses the capital investment, thereby producing an electrophotographic photosensitive member with stable quality at a lower cost. An object of the present invention is to provide a method for producing an electrophotographic photosensitive member. Another object of the present invention is to provide a method for producing an electrophotographic photosensitive member that does not cause film peeling in the cooling step.
The method for producing an electrophotographic photosensitive member of the present invention has the following configuration. That is, a method for producing an electrophotographic photosensitive member having at least a photoconductive layer formed of an amorphous material containing silicon on the surface of a cylindrical substrate having conductivity, which is held by a substrate holding member and heated. A film forming step of depositing at least a photoconductive layer formed of an amorphous material containing silicon in a processing container on the surface of the cylindrical substrate, and taking out the electrophotographic photoreceptor into the atmosphere after the film forming step A discharge step, an outer surface cooling step for cooling the electrophotographic photosensitive member from the outer surface of the electrophotographic photosensitive member with a cooling gas after the discharging step, an electrophotographic photosensitive member after the outer surface cooling step, and an electrophotographic photosensitive member with a cooling gas. It has the internal surface cooling process cooled from an internal surface, It is characterized by the above-mentioned.
Moreover, it is preferable to perform an outer surface cooling process until the temperature of an electrophotographic photoreceptor becomes the range of 50 degreeC or more and 150 degrees C or less, and then performs an inner surface cooling process.
Moreover, it is preferable that either one or both of an outer surface cooling process and an inner surface cooling process is performed in the space enclosed.
Moreover, it is preferable that either one or both of the outer surface cooling step and the inner surface cooling step is performed while sucking the cooling gas.
The inner surface cooling step is preferably performed by spraying a cooling gas on the inner surface of the electrophotographic photosensitive member with the electrophotographic photosensitive member removed from the substrate holding member.
The cooling gas is preferably nitrogen gas or air.

According to the method for producing an electrophotographic photosensitive member of the present invention, the product after the a-Si thin film is formed can be cooled without causing film peeling even in a container other than a depressurizable container. For this reason, the container which can be pressure-reduced for cooling required until now becomes unnecessary, and the amount of capital investment can be suppressed. Moreover, since it is not necessary to cool in the reaction vessel, the tact time of the production equipment can be shortened and the equipment operation rate can be increased.
In the outer surface cooling step in the method for producing an electrophotographic photosensitive member of the present invention, cooling is performed until an electrophotographic photosensitive member having a temperature before cooling of 200 ° C. or higher is in a temperature range of 50 ° C. or higher and 150 ° C. or lower. preferable. By doing in this way, the cooling gas cost can be suppressed and workability can be improved.

In the cooling step in the method for producing an electrophotographic photosensitive member of the present invention, a place where the cooling step is performed may be enclosed. By performing the cooling step in the enclosed place, it is possible to prevent the by-products and dust attached to the electrophotographic photosensitive member and the support member from scattering.
Further, the cooling step may be performed while sucking the cooling gas after being sprayed on the electrophotographic photosensitive member. By doing so, it is possible to further prevent the by-products and dust attached to the electrophotographic photosensitive member and the support member from being scattered.

In the inner surface cooling step in the method for producing an electrophotographic photosensitive member of the present invention, it is preferable to remove the electrophotographic photosensitive member from the substrate holding member and blow a cooling gas on the inner surface of the electrophotographic photosensitive member. By doing in this way, a cooling efficiency improves and a tact time can further be shortened.
The cooling gas in the method for producing an electrophotographic photosensitive member of the present invention is preferably nitrogen gas or air (about 80% is nitrogen and about 20% is oxygen). By using these, the cost of the cooling gas can be further suppressed.

Hereinafter, the present invention will be described in detail with reference to the drawings as necessary.
FIG. 1 is a schematic diagram illustrating an example of a manufacturing apparatus used in the method for manufacturing an electrophotographic photosensitive member according to the present invention. FIG. 2 is a schematic diagram illustrating an example of a cooling stage used in the method for manufacturing an electrophotographic photosensitive member according to the present invention. FIG.

In FIG. 1, in a clean atmosphere such as a clean room, a cylindrical base 151 having conductivity is mounted on a base holding member 152 made of metal, and the cylindrical base 151 held by the base holding member 152 is mounted. Install on the input stage 101.
The heating processing container 102 heats and holds the cylindrical substrate 151 at a predetermined temperature. The film formation processing container 103 forms an a-Si thin film on the cylindrical substrate 151. The electrophotographic photosensitive member after the formation of the a-Si thin film is placed on the cooling stage 104 and cooled. Gate valves 111 and 112 are provided in each processing container.

The first transfer container 105 a is in charge of moving the cylindrical substrate 151 from the input stage 101 to the heating processing container 102 and from the heating processing container 102 to the film forming processing container 103. The second transfer container 105b is in charge of movement from the film forming process container 103 to the cooling stage 104.
The exhaust device 131 depressurizes the heating processing container 102, and the exhaust device 132 depressurizes the film forming processing container 103.
The exhaust device 141 decompresses the space between the transfer container gate valve 121 and the gate valve 111 when the first transfer container 105 a is connected to the heating processing container 102. The exhaust device 142 depressurizes the space between the transfer container gate valve 121 or 122 and the gate valve 112 when the first transfer container 105 a or the second transfer container 105 b is connected to the film formation processing container 103.

Next, the cooling stage 104 of FIG. 1 will be described in more detail.
FIG. 2 shows an example of the cooling stage. The cooling stage 201 includes an outer surface cooling area 202 for cooling from the outer surface of the electrophotographic photosensitive member and an inner surface cooling area 203 for cooling from the inner surface of the electrophotographic photosensitive member.
The outer surface cooling area 202 is provided with a cradle 204 on which the substrate holding member 205 is installed, and a cooling gas blowing plate 207 provided with a cooling gas blowing port 206 through which cooling gas is blown out.
The cooling gas blowing plate 207 is not particularly limited as long as the cooling gas can be blown onto the outer surface of the electrophotographic photosensitive member. The cooling gas blowing plate 207 may have a plate shape as shown in FIG. 2 or a gas pipe (not shown). Such a tube may be used.
The cooling gas outlet 206 is not particularly limited as long as the cooling gas can be blown onto the outer surface of the electrophotographic photosensitive member, and may have a hole shape as shown in FIG. 2 or a slit shape (not shown). )

The inner surface cooling area 203 is provided with a cradle 204 for installing the electrophotographic photosensitive member 210 and a cooling gas blowing pipe 209 provided with a cooling gas blowing port 208 through which cooling gas is blown.
The cooling gas blowing pipe 209 is not particularly limited as long as the cooling gas blowing pipe 209 has a shape capable of blowing the cooling gas to the substrate holding member 205 on which the electrophotographic photosensitive member 210 is mounted or the inner surface of the electrophotographic photosensitive member 210, and is shown in FIG. It may be tubular or plate-shaped (not shown).
The cooling gas outlet 208 is not particularly limited as long as it has a shape capable of blowing the cooling gas to the substrate holding member 205 on which the electrophotographic photosensitive member 210 is mounted or the inner surface of the electrophotographic photosensitive member 210, and is shown in FIG. Thus, a hole shape or a slit shape (not shown) may be used.

In the method of manufacturing the electrophotographic photosensitive member of the present invention, first, the cylindrical substrate 151 is mounted on the substrate holding member 152 in the clean room, installed on the input stage 101, and accommodated in the first transfer container 105a. Then, the transfer container gate valve 121 of the first transfer container 105a is closed. Next, the first transfer container 105 a is moved onto the heating processing container 102, and the space between the transfer container gate valve 121 and the gate valve 111 is reduced by the exhaust device 141.
Next, the transfer container gate valve 121 is opened, and the inside of the first transfer container 105 a is decompressed by the exhaust device 141. Next, the gate valve 111 is opened, and the cylindrical substrate 151 is placed in the heating processing container 102 by a vertical movement mechanism (not shown) provided in the first transfer container 105a, and the cylindrical substrate is brought to a predetermined temperature. 151 is heated.

When the heat treatment of the cylindrical substrate 151 is completed, the transfer container gate valve 121 and the gate valve 111 are opened, and the heated cylindrical substrate 151 is accommodated in the first transfer container 105a. Next, the first transfer container 105 a is moved onto the film formation processing container 103, and the space between the transfer container gate valve 121 and the gate valve 112 is reduced by the exhaust device 142. Next, the transfer container gate valve 121 and the gate valve 112 are opened, and the cylindrical substrate 151 is moved from the first transfer container 105 a into the film forming process container 103.
Thereafter, an a-Si thin film is formed on the cylindrical substrate 151 in the film-forming treatment container 103, and a film forming process for forming an electrophotographic photosensitive member is performed. The temperature of the electrophotographic photosensitive member after the film forming step is preferably 200 ° C. or higher in view of the characteristics of the electrophotographic photosensitive member. This is because the surface reaction on the surface of the cylindrical substrate during film formation is promoted and the structure is sufficiently relaxed.

After completion of the film formation step, the second transfer container 105b is moved onto the film formation processing container 103, and the space between the transfer container gate valve 122 and the gate valve 112 is reduced by the exhaust device 142. Next, the transfer container gate valve 122 and the gate valve 112 are opened, and the electrophotographic photosensitive member is moved from the film formation processing container 103 to the second transfer container 105b. Next, the transfer container gate valve 122 is closed, and the inside of the second transfer container 105b is vented with nitrogen (N ₂ ) gas.
Then, the second transfer container 105b is moved onto the cooling stage 104, the transfer container gate valve 122 is opened, and the electrophotographic photosensitive member is taken out (discharged) from the second transfer container 105b to the cooling stage 104 into the atmosphere. I do.

Next, a cooling process is performed on the cooling stage 201. In the cooling process of the present invention, an outer surface cooling process is first performed, and then an inner surface cooling process is performed. By adopting such a method, the electrophotographic photosensitive member can be cooled without causing film peeling even in containers other than those capable of decompression.
It is considered that film peeling occurs because the balance of thermal stress of the film is lost during the cooling process. In the cooling method of the present invention, by cooling from the outer surface and then from the inner surface, the film can be cooled while maintaining the balance of the thermal stress of the film, and the occurrence of film peeling can be suppressed. It is guessed that there is not.

In the outer surface cooling step, the electrophotographic photosensitive member 210 is cooled by spraying the cooling gas blown from the cooling gas outlet 206 onto the outer surface of the electrophotographic photosensitive member 210. At this time, the electrophotographic photosensitive member 210 may be removed from the substrate holding member 205. However, since the electrophotographic photosensitive member 210 and the substrate holding member 205 after film formation are at a high temperature, the substrate is considered in consideration of workability. It is preferable to carry out it while it is mounted on the holding member 205.
In the outer surface cooling process, the electrophotographic photosensitive member having a temperature before cooling of 200 ° C. or higher is cooled until it reaches a temperature range of 50 ° C. or higher and 150 ° C. or lower. It is more preferable in terms of prevention. Further, the cooling rate of the electrophotographic photosensitive member is more preferably in the range of 5 ° C./min to 30 ° C./min in terms of suppressing film peeling and shortening tact time.

In the inner surface cooling process, the cooling gas blown out from the cooling gas outlet 208 is blown onto the substrate holding member 205 on which the electrophotographic photosensitive member 210 is mounted or the inner surface of the electrophotographic photosensitive member 210 to thereby remove the electrophotographic photosensitive member 210. Cooling.
At this time, the electrophotographic photosensitive member 210 may be mounted while being attached to the substrate holding member 205, but it is more preferable that the operation is performed with the electrophotographic photosensitive member 210 removed from the substrate holding member 205 in consideration of cooling efficiency. This is because the electrophotographic photosensitive member 210 after the outer surface cooling process is in a temperature range of 50 ° C. or higher and 150 ° C. or lower, so that a certain degree of work safety is ensured.
In the inner surface cooling step, it is preferable to cool the electrophotographic photosensitive member until the temperature of the electrophotographic photosensitive member becomes 10 ° C. or higher and lower than 50 ° C. in order to suppress film peeling. Further, the cooling rate of the electrophotographic photosensitive member is more preferably in the range of 5 ° C./min to 30 ° C./min in terms of suppressing film peeling and shortening tact time.

Moreover, it is preferable that either one or both of an outer surface cooling process and an inner surface cooling process is performed in the space enclosed. For example, as shown in FIG. 3, it is preferable to perform the process on a cooling stage 301 surrounded by a partition plate 311. However, in FIG. 3, the front partition plate is illustrated as being transparent so that the inside can be seen.
Surrounding the periphery of the cooling stage 301 with the partition plate 311 is that film-forming by-products attached to the electrophotographic photosensitive member and the substrate holding member and dust on the cooling stage are wound up by the cooling gas and scattered around. It is preferable to prevent this. There are no particular restrictions on the members of the partition plate surrounding the periphery, but metals such as aluminum and SUS (Stainless Used Steel) are preferred because they generate relatively little dust. Further, a part or all of the partition plate may be freely opened and closed like a roll curtain.
The cooling gas blowing plate 307 is provided with a slit-shaped cooling gas blowing port 306. The cooling gas blowing pipe 309 is also provided with a slit-shaped cooling gas blowing port 308.

Moreover, it is preferable to perform either one or both of the outer surface cooling step and the inner surface cooling step while sucking the cooling gas. For example, as shown in FIG. 4, the cooling gas after being blown onto the electrophotographic photosensitive member may be sucked from a cooling gas suction port 412 by a cooling gas suction device (not shown). Also in FIG. 4, the front partition plate is illustrated as being transparent so that the inside can be seen.
Surrounding the cooling stage 401 with a partition plate 411 and sucking the cooling gas after sprayed onto the electrophotographic photosensitive member from the cooling gas suction port 412 is a film deposited on the electrophotographic photosensitive member or the substrate holding member. By-products and dust on the cooling stage are more preferable for preventing the dust from being wound up by the cooling gas and scattered around. The cooling gas suction port 412 is not particularly specified as long as it can suck the cooling gas, and may have a slit shape or a hole shape (not shown) as shown in FIG.
The gas used for the cooling gas is not particularly limited as long as it is a gas that does not cause safety problems, but nitrogen gas or air is preferable in terms of handling and cost. The temperature of the cooling gas is such that the cooling gas used in the outer surface cooling step is in a temperature range of 50 ° C. or higher and 150 ° C. or lower, and the cooling gas used in the inner surface cooling step is in a temperature range of 10 ° C. or higher and lower than 50 ° C. This is preferable in terms of preventing overcooling and shortening the tact time.

  Hereinafter, the present invention will be described in detail with reference to Examples and Comparative Examples. The present invention is not limited to these examples.

Example 1
Using the electrophotographic photoreceptor manufacturing apparatus shown in FIG. 1 and the cooling stage shown in FIG. 2, a photoconductive film formed of an amorphous material containing at least silicon on an aluminum cylindrical substrate having a diameter of 84 mm and a length of 381 mm. An electrophotographic photoreceptor having a layer was produced under the conditions shown in Table 1.
The following items were verified for each item of the amount of capital investment, tact time, film peeling evaluation, cooling gas cost, and comprehensive evaluation. The results are shown in Table 10.

《Capital investment》
The capital investment required for configuring the electrophotographic photosensitive member manufacturing apparatus was ranked by relative evaluation when the capital investment in Example 1 was set to 100% as a reference.
A: 90% or more and less than 110% compared to the reference, and level equivalent to the reference B: 110% or more and less than 150% compared to the reference

"Tact time"
An average required for one cycle calculated from the time required to complete the five cycles is defined as one cycle from the mounting of the cylindrical substrate to the substrate holding member and the setting of the input stage to the sending of the electrophotographic photosensitive member to the inspection process. Time was taken as takt time. And ranking was performed by relative evaluation when the average required time in Example 1 was set to 100%.
AA: 80% or more and less than 90% level A compared to the reference A: 90% or more and less than 110% compared to the reference level B: 110% or more and less than 150% level C compared to the reference C: Reference 150% or more and less than 190% level

<Evaluation of film peeling>
Whether the produced electrophotographic photosensitive member caused film peeling was evaluated based on the following criteria as film peeling evaluation.
A: No film peeling occurs
B: Minor film peeling occurs at the edge of the electrophotographic photosensitive member

《Cooling gas cost》
The cooling gas used for cooling the electrophotographic photosensitive member was ranked as the cooling gas cost, and the ranking was performed based on the relative evaluation when the cooling gas cost in Example 1 was set to 100%.
AAA: Level less than 70% compared to reference AA: Level 70% or more and less than 90% compared to reference A: Level equal to or greater than 90% or less than 110% compared to reference, equivalent to reference

"Comprehensive evaluation"
The results obtained in the items of capital investment, tact time, film peeling evaluation, cooling gas cost, AAA rank 4 points, AA rank 3 points, A rank 2 points, B rank 1 point, C rank Based on the total score of 0 points, ranking was performed as follows.
AA: 10 points or more A: 8 points or more and 9 points or less B: 6 points or more and 7 points or less

(Example 2)
In the procedure of Example 1, the point where the electrophotographic photosensitive member was removed from the substrate holding member and the inner surface cooling step was performed and the point where air was used as the cooling gas were changed, and the electrophotographic photosensitive member was subjected to the conditions shown in Table 2. Produced.
Then, the items of capital investment, tact time, film peeling evaluation, cooling gas cost, and comprehensive evaluation were verified by the same method as in Example 1. The results are shown in Table 10.

(Example 3)
In the procedure of Example 2, the point that the cooling stage shown in FIG. 3 was used as the cooling stage was changed, and an electrophotographic photosensitive member was produced under the conditions shown in Table 3.
Then, the items of capital investment, tact time, film peeling evaluation, cooling gas cost, and comprehensive evaluation were verified by the same method as in Example 1. The results are shown in Table 10.

Example 4
In the procedure of Example 2, the point using the cooling stage shown in FIG. 4 as the cooling stage and the point using nitrogen gas as the cooling gas were changed, and an electrophotographic photosensitive member was produced under the conditions shown in Table 4.
Then, the items of capital investment, tact time, film peeling evaluation, cooling gas cost, and comprehensive evaluation were verified by the same method as in Example 1. The results are shown in Table 10.

(Comparative Example 1)
In the procedure of Example 1, the conventional manufacturing apparatus shown in FIG. 5 was used as an apparatus for manufacturing an electrophotographic photosensitive member, and the electrophotographic photosensitive member was cooled in a cooling processing container. An electrophotographic photoreceptor was produced under the conditions shown.
The cooling processing container 504 of the conventional manufacturing apparatus shown in FIG. 5 does not have a function of cooling the electrophotographic photosensitive member from the inner surface.
Then, the items of capital investment, tact time, film peeling evaluation, cooling gas cost, and comprehensive evaluation were verified by the same method as in Example 1. The results are shown in Table 10.

(Comparative Example 2)
In the procedure of Example 1, the point that the electrophotographic photosensitive member was cooled in the film-forming processing container was changed, and an electrophotographic photosensitive member was produced under the conditions shown in Table 6.
Then, the items of capital investment, tact time, film peeling evaluation, cooling gas cost, and comprehensive evaluation were verified by the same method as in Example 1. The results are shown in Table 10.

(Comparative Example 3)
In the procedure of Example 1, the point where the electrophotographic photosensitive member was cooled on the cooling stage was changed, and an electrophotographic photosensitive member was produced under the conditions shown in Table 7.
Then, the items of capital investment, tact time, film peeling evaluation, cooling gas cost, and comprehensive evaluation were verified by the same method as in Example 1. The results are shown in Table 10.

(Comparative Example 4)
In the procedure of Example 1, the electrophotographic photoconductor was cooled in the order of the inner surface cooling step and the outer surface cooling step, and an electrophotographic photoconductor was produced under the conditions shown in Table 8.
Then, the items of capital investment, tact time, film peeling evaluation, cooling gas cost, and comprehensive evaluation were verified by the same method as in Example 1. The results are shown in Table 10.

(Comparative Example 5)
The electrophotographic photosensitive member was manufactured under the conditions shown in Table 9 by changing the point that the outer surface cooling step and the inner surface cooling step were simultaneously performed in the procedure of Example 1.
Then, the items of capital investment, tact time, film peeling evaluation, cooling gas cost, and comprehensive evaluation were verified by the same method as in Example 1. The results are shown in Table 10.

From Table 10, in Example 1 using the method for producing an electrophotographic photosensitive member of the present invention that does not use a cooling processing container, capital investment was compared with Comparative Example 1 using a conventional cooling processing container. The amount can be reduced.
Further, in Example 1 using the method for producing an electrophotographic photosensitive member of the present invention in which the cooling process is not performed in the film formation processing container, as compared with Comparative Example 2 in which the cooling process is performed in the film formation processing container. The tact time can be shortened.
Further, in Example 1 using the method for producing an electrophotographic photosensitive member of the present invention in which an outer surface cooling process and an inner surface cooling process using a cooling gas are performed, the tact time is shortened and film peeling is suppressed as compared with Comparative Example 3. Became possible.
Further, in Example 1 using the method of manufacturing the electrophotographic photosensitive member of the present invention in which the outer surface cooling process is performed and then the inner surface cooling process is performed, tact time is shortened and film peeling is suppressed as compared with Comparative Example 4. It has become possible.
Further, in Example 1 using the electrophotographic photosensitive member manufacturing method of the present invention in which the outer surface cooling step and then the inner surface cooling step are performed, film peeling can be suppressed as compared with Comparative Example 5.
In addition, it is possible to reduce the cost of the cooling gas by using nitrogen gas as the cooling gas, and it is possible to further reduce the cost of the cooling gas by using air as the cooling gas.
Further, in Examples 2, 3 and 4 in which the electrophotographic photosensitive member was removed from the substrate holding member and the inner surface cooling step was performed, it was possible to further shorten the tact time as compared with Example 1.
And it was confirmed that the Example using the manufacturing method of the electrophotographic photoreceptor of the present invention is comprehensively superior to the comparative example.

Next, with respect to Example 1 to Example 4, the items of the film formation by-product and the dust scattering area were verified by the following method. The results are shown in Table 11.
<< Film formation by-products and dust scattering area >>
In the cooling step, the area where the film formation by-product attached to the electrophotographic photosensitive member and the substrate holding member and the dust on the cooling stage were scattered by the cooling gas was defined as the film formation by-product and the dust scattering area. And it ranked by the relative evaluation at the time of setting the cooling gas cost in Example 1 to 100% of a reference. As for the scattering area, an adhesive sheet was placed on the floor around the cooling stage, and the area where the deposition by-products and dust adhered was measured.
AAA: Level of less than 30% compared to reference AA: Level of 30% or more and less than 90% compared to reference A: 90% or more and less than 110% compared to reference, level B equivalent to reference B: 110 compared to reference % Or more and less than 170%

From Table 11, in Example 3 which performs a cooling process using the cooling stage with which the circumference | surroundings were enclosed, compared with Example 1, 2, it became a result by which scattering of the film-forming by-product and dust was suppressed. .
Further, in Example 4 in which the cooling process was performed while sucking the cooling gas, as compared with Example 3, the film formation by-product and dust scattering were further suppressed.

(Example 5)
In the procedure of Example 1, electrophotographic photosensitive members in which the temperature of the electrophotographic photosensitive member at the end of the outer surface cooling step was changed to the temperatures shown in Table 12 were produced as Examples 5-1 to 5-6. .
And about the item of a film formation by-product and a dust scattering area, it verified by the method similar to the method which verified Example 1- Example 4, and verified the item of workability | operativity with the following method. The results are also shown in Table 13.

"Workability"
In the cooling process, the workability when removing the electrophotographic photosensitive member from the substrate holding member was ranked according to the following criteria.
A: One person can work while wearing heat-resistant protective equipment. B: Two persons must work while wearing heat-resistant protective equipment.

From Table 13, in Example 5-1 to Example 5-5 in which the inner surface cooling process is performed after the temperature of the electrophotographic photosensitive member at the end of the outer surface cooling process reaches a temperature of 150 ° C. or less, the workability is good. As a result. Further, in Examples 5-2 to 5-6 in which the inner surface cooling process is performed at a temperature of the electrophotographic photosensitive member at the end of the outer surface cooling process of 50 ° C. or higher, it is possible to suppress scattering of film formation byproducts and dust. It became.
In addition, each item of the amount of capital investment, tact time, film peeling evaluation, cooling gas cost, and comprehensive evaluation was equivalent to Example 1.

It is a schematic diagram showing an example of the manufacturing apparatus used for the manufacturing method of the electrophotographic photoreceptor by this invention. It is a schematic diagram showing an example of the cooling stage used for the manufacturing method of the electrophotographic photosensitive member by this invention. It is a schematic diagram showing an example of the cooling stage used for the manufacturing method of the electrophotographic photosensitive member by this invention. It is a schematic diagram showing an example of the cooling stage used for the manufacturing method of the electrophotographic photosensitive member by this invention. It is a schematic diagram showing an example of the manufacturing apparatus used for the manufacturing method of the conventional electrophotographic photoreceptor.

Explanation of symbols

101 Input stage 102 Processing container for heating 103 Processing container for film formation 104 Cooling stage 105a First transport container 105b Second transport container 111, 112 Gate valve 121, 122 Transport container gate valve 131, 132 Exhaust device 141, 142 Exhaust device 151 Cylindrical substrate 152 Substrate holding member 201, 301, 401 Cooling stage 202 Outer surface cooling area 203 Inner surface cooling area 204 Receiving base 205 Substrate holding member 206, 306 Cooling gas blowing port 207, 307 Cooling gas blowing plate 208, 308 Cooling gas blowing port 209, 309 Cooling gas blowing tube 210 Electrophotographic photosensitive member 311 Partition plate 412 Cooling gas suction port 504 Cooling processing vessel

Claims (6)

A method for producing an electrophotographic photosensitive member having at least a photoconductive layer formed of an amorphous material containing silicon on a surface of a cylindrical substrate having conductivity,
A film forming step of forming a photoconductive layer formed of an amorphous material containing silicon in a processing container on the surface of the cylindrical substrate held and heated by the substrate holding member;
A discharging step of taking out the electrophotographic photosensitive member into the atmosphere after the film forming step;
An outer surface cooling step for cooling the electrophotographic photosensitive member from the outer surface of the electrophotographic photosensitive member with a cooling gas after the discharging step;
A method for producing an electrophotographic photosensitive member, comprising: an inner surface cooling step of cooling the electrophotographic photosensitive member from an inner surface of the electrophotographic photosensitive member with a cooling gas after the outer surface cooling step. The temperature of the electrophotographic photosensitive member at the end of the film forming step is 200 ° C. or higher, and the outer surface cooling step is performed until the temperature of the electrophotographic photosensitive member is in a range of 50 ° C. or higher and 150 ° C. or lower.
The method for producing an electrophotographic photosensitive member according to claim 1, wherein the inner surface cooling step is then performed.   3. The method of manufacturing an electrophotographic photosensitive member according to claim 1, wherein one or both of the outer surface cooling step and the inner surface cooling step is performed in a space surrounded by the periphery.   4. The method for producing an electrophotographic photosensitive member according to claim 1, wherein one or both of the outer surface cooling step and the inner surface cooling step is performed while sucking the cooling gas.   5. The inner surface cooling step is performed by spraying a cooling gas on the inner surface of the electrophotographic photosensitive member in a state where the electrophotographic photosensitive member is removed from the substrate holding member. A process for producing an electrophotographic photoreceptor according to 1. The method for producing an electrophotographic photosensitive member according to claim 1, wherein the cooling gas is nitrogen gas or air.

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