JP2003049278A - Vacuum treatment method and vacuum treatment device - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a vacuum treatment method and a vacuum treatment device in which decrease in yield is minimized even when any abnormality occurs in the vacuum treatment, and a large number of high quality works are formed at a low cost. SOLUTION: In the vacuum treatment in which each reaction vessel is connected to a pipe branched from one and the same exhaust means and a gas feed and flow rate control means, and evacuated, gas required for treating each reaction vessel is introduced, the high frequency power is simultaneously applied to each reaction vessel to form plasma, and a plurality of works are simultaneously treated, the vacuum treatment of the reaction vessel in which an abnormality occurs is stopped when any abnormality in the vacuum treatment occurs in at least one reaction vessel, the vacuum treatment control set value is changed from the normal set value.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a vacuum processing method used for forming a semiconductor film, an electrophotographic photosensitive member, an image input line sensor, a photographing device, a photovoltaic device, etc., such as deposition film formation and etching. The present invention relates to a vacuum processing device.

[0002]

2. Description of the Related Art Conventionally, as a vacuum processing method used for producing semiconductor devices, electrophotographic photoconductors, image input line sensors, photographing devices, photovoltaic devices, other various electronic elements, optical elements, etc. Many are known, such as a vacuum vapor deposition method, a sputtering method, an ion plating method, a thermal CVD method, a photo CVD method, and a plasma CVD method, and an apparatus therefor is put into practical use. Among them, the plasma process using high frequency power is used because of its various advantages such as being able to be used for deposition film formation and etching using various materials and also for forming insulating materials such as oxide films and nitride films. There is. Preferable examples of use of the plasma process include, for example, hydrogenated amorphous silicon for electrophotography (hereinafter referred to as a-Si: H).
Practical applications such as formation of a deposited film have been very advanced at present, and various apparatuses for that purpose have been proposed.

Further, various measures have been taken in order to manufacture a high quality deposited film at low cost.

For example, Japanese Unexamined Patent Publication No. 10-168574 discloses a technique for shortening the total time required for manufacturing by devising a cleaning method for a deposited film forming apparatus. An example of a deposited film forming apparatus that exhausts by a single exhaust means is disclosed.
In addition, Japanese Patent Publication No. 7-13947 discloses a technique of forming a plurality of thin film transistor arrays by using a plurality of reaction vessels in which a source gas supply means and an exhaust means are made common. By connecting a plurality of reaction vessels to a single exhaust means or a single gas supply means in this way, capital investment in the gas supply means or exhaust means can be reduced.

Further, Japanese Unexamined Patent Publication No. 10-168576 discloses the details of a deposition film forming apparatus in which a vacuum container is connected to an evacuation unit and a source gas supply unit via a connection mechanism that can be attached and detached, and an attachment and detachment mechanism. There is. By making it detachable in this way, for example, when manufacturing different kinds of deposited films, only the reaction container needs to be changed, which is advantageous in terms of equipment investment, equipment downtime, and the like.

Further, as another device related to the exhaust mechanism, Japanese Patent Laid-Open No. 8-121345 discloses that a plurality of vacuum containers are connected to each other and even if one exhaust device is stopped, another exhaust device can be used for exhausting. An exhaust method is disclosed.
By providing such an emergency backup function, it is possible to avoid a plurality of vacuum vessels from trouble.

Further, as a coping method when a trouble occurs,
Japanese Unexamined Patent Publication No. 2000-133596 discloses an apparatus and a processing method capable of quickly suppressing abnormal discharge and maintaining discharge by introducing a predetermined amount of raw material gas in a pulse form when abnormal discharge occurs. . By avoiding such troubles, it becomes possible to continue vacuum processing.

On the other hand, in recent years, a plasma CVD method using a high frequency high frequency power source has been reported (Plasma Chemist
ry and Plasma Processing, Vol.7, No.3, (1987), p26
7-273), the discharge frequency is 13.56MHz of the conventional
It has been noted that the possibility of increasing the deposition rate without deteriorating the performance of the deposited film can be achieved by making the value higher than the above value, and has been drawing attention. For example, Japanese Unexamined Patent Publication No. 6-287760 discloses an apparatus and method for PCVD using a frequency in the VHF band which can be used for forming a light receiving member for a-Si electrophotography. By improving the deposition rate without deteriorating the performance of the deposited film, the total time required for manufacturing can be shortened and the cost can be reduced. Further, Japanese Patent Laid-Open No. 7-288233 discloses a technique of simultaneously forming a plurality of deposited films on a plurality of cylindrical substrates arranged on the same circumference by using a high frequency wave in the VHF band.

[0009]

With the above-mentioned conventional method and apparatus, a large number of deposited films can be simultaneously produced, and there is an advantage that auxiliary equipment such as gas flow rate control means and gas exhaust means can be made common, resulting in cost reduction. It is advantageous to down.

However, as described above, in the case of the constitution in which the auxiliary equipment such as the gas flow rate control means and the gas exhaust means are shared and a large number of deposited films are simultaneously formed in a plurality of reaction vessels, among a plurality of reaction vessels When an abnormality occurs in a certain one reaction vessel, other reaction vessels that are normally performing processing may be adversely affected due to the shared auxiliary equipment. In particular, in the case of an abnormality that could not have been assumed in the prior art, that is, in the case of an abnormality other than that solved by switching the pump or introducing a gas pulse, the vacuum treatment of the reaction container in which the abnormality occurred must be stopped. In such a case, it has a considerable influence on other reaction vessels.

As a specific example, there is a reaction container capable of producing 10 electrophotographic photoconductors with one reaction container, and it is assumed that an apparatus in which three reaction containers are connected and ancillary equipment is shared. . Consider a case where an abnormal discharge is generated in a certain reaction container during formation of an a-Si photosensitive member using silane gas using this apparatus, and the discharge of the reaction container has to be stopped.

When the discharge is stopped, a large amount of unreacted silane gas is exhausted by the exhaust device through the reaction container. After reacting by the normal discharge, the exhaust gas has a different composition and amount from the unreacted gas, so that the exhaust balance may be disturbed. That is, if the composition or amount of gas to be exhausted changes with respect to the constant exhaust speed of the pump, the pressure inside the reaction container may change, and the pressure inside the remaining reaction container during normal operation may change. It may change and the deposition film forming condition may change. In particular, JP-A-6-2877
When using a high frequency wave in the VHF band or microwave as described in Japanese Patent No. 60, the gas decomposition efficiency is higher than the high frequency wave in the RF band, and good deposition film forming conditions are higher vacuum than the RF band. Since it is on the side, there is a high possibility that the change in the exhaust balance has a large influence on the film deposition.

Further, in such a case, it is advantageous in terms of cost to prevent the raw material gas from being wasted because the raw material gas is not wasted into the reaction vessel in which the discharge has been stopped. It is more preferable because the load can be reduced.

Therefore, it is considered to stop the gas flow into the reaction vessel where the discharge is stopped. Then, in the above example, the gas that has been branched into three after leaving the gas flow rate control means is branched into two, and 3/2 times as much raw material gas is supplied to each of the two normally operating reaction vessels. As a result, the conditions for deposit film formation in the reaction vessel, which was operating normally, change significantly.

In the mass production type apparatus capable of processing a large amount of deposited film at one time as in the above-described specific examples, it is very advantageous in terms of cost, but once a trouble occurs, in the worst case, ancillary equipment is attached. There is a problem in that all the deposited films prepared in all the reaction vessels sharing the same may become defective products.

In order to solve the above problems, the present invention is a vacuum processing method and a vacuum processing apparatus capable of simultaneously depositing a large number of deposited films by using a plurality of reaction vessels, and shares auxiliary equipment such as gas supply means and exhaust means. By doing so, the cost of the equipment can be significantly reduced, and when an abnormality occurs in one reaction container, it does not adversely affect other reaction containers that are operating normally and minimizes the decrease in yield. It is an object of the present invention to provide a vacuum processing method and a vacuum processing apparatus capable of performing the same.

[0017]

In order to solve the above-mentioned problems, the vacuum processing method of the present invention is to install an object to be processed in a plurality of depressurizable reaction vessels, and to use the same exhaust means for each reaction vessel. Connected to the branched pipes and evacuated, connected to each reaction vessel, after passing through the same gas supply means and gas flow rate control means, branched pipes to introduce the gas necessary for the treatment, and to each reaction vessel In the vacuum processing method of simultaneously applying high-frequency power to form plasma and simultaneously processing a plurality of the objects to be processed, when an abnormality occurs in the vacuum processing in at least one reaction container of the plurality of reaction containers In addition, the vacuum processing of the reaction container in which the abnormality occurs is stopped, and at the same time, the control setting value of the vacuum processing is changed from the normal setting value and the remaining vacuum processing is continued.

The control set value to be changed may be a gas flow rate set value.

In this case, when the total number of reaction vessels connected to the same gas supply means and gas flow rate control means is n and the number of reaction vessels in which an abnormality occurs is i, the total amount supplied from the gas flow rate control means It is preferable to change the set value of the gas amount of (n-i) / n times.

Further, when an abnormality occurs, the gas introduction into the reaction vessel in which the vacuum processing is stopped is gradually reduced, and in conjunction with this, the gas flow rate supplied from the gas supply means and the gas flow rate control means is gradually decreased. It is preferable to change so that the total gas flow rate to the other reaction vessels becomes (n−i) / n times at the same time when the gas introduction to the reaction vessel where the abnormality occurs is stopped.

The control set value to be changed may be the pressure inside each of the reaction vessels.

Further, it is preferable that the high frequency power for generating plasma is a high frequency wave in the VHF band or a microwave.

The plurality of reaction vessels may be covered with a common shield, and the control set value for changing may be an electric power value supplied to each of the reaction vessels.

The reaction vessel is connected to each of the exhaust means, the gas supply means, the gas flow rate control means, and the high frequency power applying means through a detachable connection mechanism, and when an abnormality occurs, the abnormality is detected. It is preferable that the generated reaction container is separated from the exhaust means, the gas supply means, the gas flow rate control means, and the high frequency power application means.

In order to solve the above-mentioned problems, the vacuum processing apparatus of the present invention has a plurality of depressurizable reaction vessels in which objects to be treated are installed, and the respective reaction vessels are connected to a pipe branched from the same exhaust means. A gas supply unit and a gas flow rate control unit for connecting and exhausting the gas, and connecting each reaction container to the branched pipe after passing through the same gas supply unit and the same gas flow rate control unit to supply the gas required for processing. In a vacuum processing apparatus having a high frequency power applying means and capable of simultaneously processing a plurality of objects to be processed, when an abnormality occurs in vacuum processing in at least one reaction container among the plurality of reaction containers, A means for detecting an abnormality, a means for stopping the vacuum processing of the reaction vessel in which the abnormality has occurred, and a means for changing the control set value of the vacuum processing from the normal set value are provided. .

As another structure of the vacuum processing apparatus of the present invention, a plurality of reaction vessels in which objects to be treated are installed and which can be decompressed, and each reaction vessel is connected to a pipe branched from the same exhaust means. A gas supply means and a gas flow rate control means for connecting the reaction means and the exhaust means for exhausting the gas to a pipe branched after passing through the same gas supply means and gas flow rate control means. In a vacuum processing apparatus having a high-frequency power applying means and capable of simultaneously processing a plurality of objects to be processed, among the plurality of reaction vessels, when an abnormality occurs in vacuum processing in at least one reaction vessel, A means for detecting an abnormality, a means for stopping the vacuum processing of the reaction vessel in which an abnormality has occurred, a valve for stopping the gas introduction to the reaction vessel in which an abnormality has occurred, and a gas flow rate set value for another reaction vessel Total When the total number of reaction vessels connected to the same gas supply means and gas flow rate control means is n, and the number of reaction vessels in which an abnormality has occurred is i, a means for changing to (n-i) / n times It is characterized by having.

Furthermore, the valve for stopping the introduction of gas into the reaction vessel in which an abnormality has occurred has a function of gradually reducing the flow rate, and in conjunction with this, the gas supplied from the gas supply means and the gas flow rate control means. A mechanism that gradually reduces the flow rate and changes so that the total gas flow rate to other reaction vessels becomes (n-i) / n times at the same time when gas introduction to the reaction vessel where an abnormality has occurred is stopped. Is preferred.

Further, it is preferable that the evacuation means has an evacuation conductance control means for controlling the pressure inside the reaction container, which is normally vacuum-processed when an abnormality occurs, to be constant.

Further, the exhaust conductance control means is
It is preferable that each reaction vessel can be independently controlled.

Further, it is preferable that the reaction container is attachable / detachable to / from each of the exhaust means, the gas supply means, the gas flow rate control means, and the high frequency power applying means via a detachable connection mechanism.

(Function) As a result of intensive investigations by the present inventors to achieve the above object, a large amount of vacuum treatment is simultaneously performed by connecting a plurality of reaction vessels to the same exhaust means and the same gas supply means. In the vacuum processing method and apparatus capable of performing, when an abnormality occurs in a certain reaction container, by using the configuration as described above, a defective product can be generated only in the reaction container in which the abnormality has occurred. It has made it possible to prevent the yield rate from decreasing as much as possible. In addition, it is possible to prevent a large amount of unreacted gas from flowing into the exhaust pipe when an abnormality occurs, which makes it possible to reduce gas costs and prevent an increase in the load on the detoxification equipment. In addition, it is possible to quickly disconnect the reaction vessel in which an abnormality has occurred, and it is possible to repair the abnormal point and prepare for the next vacuum processing sequence while minimizing the time loss.
The downtime of the device can be reduced.

Regarding the embodiment of the present invention as described above,
The details will be described below. In the vacuum treatment of the present invention, first, a plurality of reaction vessels are connected to the same exhaust means, the same gas supply and flow rate control means, and at least one reaction vessel among the plurality of reaction vessels is subjected to vacuum treatment. When an abnormality occurs in the reaction vessel, the vacuum processing of the reaction vessel in which the abnormality has occurred is stopped, and at the same time, the control setting value related to the vacuum processing is changed from the normal setting value, so that the vacuum processing of the reaction vessel in which no abnormality has occurred Characterized by keeping normal.

The abnormality of the vacuum processing here is defined as an abnormality which can be detected in some way in any process of the vacuum processing. For example, damage to the vacuum holding member, vacuum seal, etc.,
Abnormality due to leakage due to deterioration, sequence abnormality due to malfunction of valve, etc., internal pressure control abnormality due to failure of exhaust conductance control means, pressure detection means and their feedback, abnormal discharge, discharge abnormality such as spark, high frequency matching circuit and high frequency power supply Discharge interruption or abnormality due to damage to capacitors, vacuum tubes, semiconductors, etc. may be considered. Among these abnormalities, especially with regard to discharge abnormalities such as sparks, even if there is no accident such as breakage of members, it may easily occur depending on the type of vacuum processing and processing conditions, so special attention is required. is there. For example,
When performing vacuum processing with high power, when using a device configuration in which self-bias is easily applied, or when it is necessary to positively apply a bias, etc., when an abnormality occurs in discharge, Effective measures must be taken so as not to interfere with other normal vacuum processing. In addition to this, for example, when starting the vacuum processing, it may be difficult for discharge to occur in the first place. That is, there is a case where the gas pressure for processing must be made extremely low. Alternatively, even when high-frequency waves having different frequencies are used by being superimposed on the same electrode, the discharge conditions are rarely generated because the degree of freedom of discharge conditions is relatively narrow. In this way, when vacuum processing is started in a plurality of reaction vessels at the same time under conditions where discharge is relatively difficult to occur, some of the reaction vessels rarely fail to start discharge, that is, within a predetermined time. May not be able to start discharge. As described above, it is necessary to pay special attention to the discharge abnormality, as compared with other abnormality.

The control set value related to vacuum processing is
Specifically, it is defined as a controllable numerical value such as gas flow rate, exhaust speed or exhaust conductance, pressure, heater control temperature, substrate or substrate rotation speed, and high-frequency power value. On the other hand, these determine vacuum processing conditions in the reaction vessel. Here, the vacuum processing conditions include the amount of gas in the reaction container, the gas residence time, the surface temperature of the substrate or the substrate,
It refers to the conditions during vacuum processing that are determined in the reaction container, such as high-frequency energy density. In the present invention, since it is configured as described above, even if a certain reaction vessel is stopped due to an abnormality, the vacuum control conditions in other normal reaction vessels do not change as much as possible, the control set value from the normal set value. By making the change, it is possible to substantially eliminate the influence on the normal vacuum processing.

Specifically, the set value of the pressure in the reaction vessel may be changed. The pressure is a detected value, but based on the detected value, the set value of the exhaust speed of the exhaust means is changed, and the conductance control means is provided at the connection between the reaction vessel and the exhaust means to set the exhaust conductance value. Can be controlled by changing For example, when the discharge of the reaction container in which an abnormality has occurred is stopped, the exhaust balance changes. At that time, if the detected pressure is the true pressure in the reaction container, the exhaust speed and the exhaust conductance may be controlled so that the pressure becomes a normal set value. However, it is usually difficult to detect the true pressure. For example, the pressure detecting means is installed outside the discharge space, especially outside the discharge space on the exhaust side, because a film is deposited by vacuum processing, damaged by plasma, or the pressure detecting means itself becomes a dust source. Sometimes
In that case, the true pressure in the reaction vessel, the pressure gauge is installed in the discharge space, the correlation with the pressure gauge outside the discharge space,
It can be obtained experimentally in advance by a pressure gauge outside the discharge space. In that case, in order to set the true pressure in the reaction vessel to a desired set value, it may be preferable to change the value of the pressure gauge installed outside the discharge space from the normal set value. That is, the change in the exhaust balance may change the correlation between the pressure detected outside the discharge space and the true internal pressure. In this case, if control is performed by the detected pressure outside the discharge space so that the normal set value is obtained, the true pressure in the reaction container may deviate from a preferable value. Correspondingly, it is possible to keep the true pressure in the reaction container constant by changing from the normal set value to the set value when a trouble occurs which is experimentally determined in advance.

In order to control the pressure, it is more preferable to use the exhaust conductance control means. The exhaust conductance control means is preferably located closer to the exhaust means than the pressure detection means described above, and most preferably arranged so that the exhaust conductance of each reaction vessel can be controlled independently. By doing this,
The pressure can be controlled more accurately when an abnormality occurs, and the influence on normal vacuum processing can be minimized.

By the way, it is preferable that the gas flow rate control means for mixing and supplying the raw material gas at an accurate ratio is shared by a plurality of reaction vessels in order to reduce equipment cost. For example, when forming a deposited film of a-Si or the like, monosilane gas or the like is used as a raw material gas, but in addition, diborane gas for controlling valence electrons, phosphine gas, hydrogen as a diluting gas, helium, argon, etc. In many cases, an extremely large amount of raw material gas such as a halogen-containing gas is mixed. Further, the desired film cannot be obtained unless the mixing ratio and the flow rate are accurately controlled. Therefore, it is necessary to provide a mass flow controller for each gas so as to accurately mix them. Further, a complicated pipe for mixing and purging these gases and a gas flow rate control / mixing facility equipped with many valves are required. Such equipment is generally expensive, and when there are a large number of reaction vessels, preparing each of these reaction vessels individually will result in an enormous amount of equipment investment. Therefore, by connecting a plurality of reaction vessels to pipes branched from the same gas flow rate control means and supplying gas at the same time, it is possible to significantly reduce the apparatus cost related to the gas supply facility.

However, as described above, in the apparatus sharing the gas flow rate control means, if an abnormality occurs in a certain reaction vessel and the discharge is stopped, if the raw material gas is kept flowing, unreacted gas will flow into the exhaust system. Therefore, it is not preferable in terms of maintenance of the exhaust pipe, increase of load on the detoxification equipment, and increase of gas cost. On the other hand, when the flow of gas into the reaction vessel is blocked, the number of reaction vessels connected to the gas flow rate control means changes, and the flow rate of gas per reaction vessel changes from a desired value. Therefore, it is desirable to stop the gas flow into the abnormal reaction container and change the control parameter of the gas flow rate in other normal reaction containers. That is, when the total number of reaction vessels connected to the same gas flow rate control means is n and the number of reaction vessels having an abnormality is i, when an abnormality occurs, gas is introduced into the reaction vessel having an abnormality. And the total gas flow rate to the remaining reaction vessels that are normally vacuumed is (n-i) / n
By doubling it, it becomes possible to keep the flow rate of gas consumed in the reaction container that is normally vacuum-treated constant.

At this time, a rapid change in the gas flow rate occurs, but the discharge may be disturbed depending on the degree of change, and in some cases, the vacuum treatment process may be affected. In such a case, the temporal change rate of the gas flow rate to be changed may be made gentle, that is, the flow rate may be slowly changed to a desired value. Specifically, the flow of gas into the i reaction vessels whose discharge has stopped is gradually reduced, and in conjunction with this, the total value of the gas flow rates is also gradually reduced. Then, at the same time as stopping the inflow of gas into the reaction vessel where the discharge has stopped, the total flow rate flowing into the other reaction vessel may be (n−i) / n times. As a means for realizing such a method, for example, a valve whose flow rate is variable is provided in the middle of the gas pipe to each reaction vessel, and when the discharge is stopped, the flow rate at the inlet of the reaction vessel where the discharge is stopped Gradually close the variable valve.
At the same time, the gas flow rate control means may gradually reduce the total flow rate while keeping the gas mixture ratio constant so that the total flow rate becomes (n−i) / n times. In this way, the amount of gas flowing into each reaction vessel that is normally vacuum-processed is kept almost constant, no sudden changes in gas amount occur, and the effect on normal vacuum processing is minimized. Be stopped by.

Depending on the device configuration, it may be desirable to change the set value of the high frequency power. For example, in the case of sharing a shield that prevents high-frequency waves from leaking to the outside, there is no ground potential shield between the electrodes into which high-frequency power is introduced, and therefore, the electrodes influence each other. It is in. In the case of such a device configuration, it is considered that when the electric power supplied to the electrode around the reaction container where the trouble occurs is lost, the electrode around the normal reaction container is also greatly affected.
Therefore, in order to make the electric powers actually supplied to the discharge space uniform, it may be better to change the set value of the electric power from the normal set value to the set value obtained experimentally in advance.

Further, the reaction vessel is connected to each means of the exhaust means, the gas supply means and the high frequency power applying means through a detachable connection mechanism, and when an abnormality occurs, the reaction vessel in which the abnormality has occurred is separated. Is more preferable. In particular,
With regard to the gas supply / exhaust means, a detachable connection mechanism means that a valve capable of holding a vacuum is provided on at least the supply / exhaust means side of the separating member so long as it has a shape that does not cause gas inflow / emission. Any mechanism may be used. For example, in the exhaust pipe, there is a connection form in which the exhaust means and the reaction vessel are vacuum-sealed with a flange-shaped member,
It is not particularly limited to this. More preferably, the method of fixing the flange by means of a clamp or the like is preferable because the attachment / detachment is easier. Further, in the gas supply pipe, in addition to requiring a valve at least on the supply side of the member to be disconnected, it is desirable to have a mechanism capable of exhausting the material gas in advance so that the raw material gas is not held therebetween. Any type of connection mechanism may be used as long as it has such a mechanism. For example, the cut-off portion may have a joint structure, and more preferably, the shape integrated with the flange connecting member of the exhaust pipe is more preferable. Further, it is more preferable that the purge gas pipe for purging and the exhaust pipe are connected to each other so that the purging gas can surely purge the connecting portion.

By adopting such a configuration, the reaction vessel in which an abnormality has occurred can be immediately separated without affecting other reaction vessels that are normally vacuum-processed, and the cause of the abnormality is generated. It is possible to immediately investigate and eliminate abnormalities, prepare for the next vacuum processing, etc., and reduce downtime of the apparatus.

[0043]

DESCRIPTION OF THE PREFERRED EMBODIMENTS Next, embodiments of the present invention will be described with reference to the drawings.

FIG. 1A is a schematic side view showing an example of the vacuum processing apparatus of the present invention, FIG. 1B is a partially enlarged detailed side view of FIG. 2A, and FIG. A schematic cross-sectional view of an electrophotographic photoconductor manufacturing apparatus using a plasma CVD method capable of suitably using electric power, (b) is a top view of (a), and FIG. 3 (a) is high frequency power of RF band. Can be suitably used,
Plasma C capable of simultaneously processing a plurality of objects to be processed
FIG. 4A is a top view of FIG. 4A, and FIG. 4A is a schematic side view of an electrophotographic photoconductor manufacturing apparatus using the VD method.
(B) is a schematic side view of an apparatus for manufacturing an electrophotographic photosensitive member using a plasma CVD method capable of suitably using high frequency power of a band and capable of simultaneously processing a plurality of objects to be processed.
5A is a cross-sectional view taken along the line AA ′ in FIG. 5A, and FIG. 5A uses the plasma CVD method in which three devices shown in FIG. 4 are integrated and the high frequency power in the VHF band sharing the shield can be suitably used. FIG. 2B is a schematic side view of the manufacturing apparatus for the electrophotographic photoconductor,
It is a top view of (a).

In FIG. 1A, four reactors 10 are provided.
1 is connected to one exhaust means 106 and is connected to one gas supply and flow rate control means 111. Figure 1
Although the exhaust means 106 is not described in detail in (a), a rotary pump, a mechanical booster pump,
Any pump or any combination thereof may be used as long as it is an exhaust means such as an oil diffusion pump, a turbo molecular pump, etc. that can obtain a desired exhaust speed. Further, although the gas supply and flow rate control means 111 is not described in detail in the same manner, it is desirable that the gas supply and flow rate control means 111 include a plurality of gas cylinders, regulators, valves, mass flow controllers and the like necessary for vacuum processing, and a desired gas is desired. Any configuration may be used as long as it can be supplied at the flow rate and the mixing ratio of. Further, it is desirable to further include a gas cylinder for purging and a purging line. In addition, although there are four reactors 101 in FIG. 1A, the number may be arbitrarily determined in consideration of the exhaust capacity of the pump.

A gate valve 103 is connected to the reaction apparatus 101, and is connected to an exhaust means 106 via a collective exhaust pipe 105. At this time, it is desirable to provide a connection mechanism 102 between the reaction device 101 and the gate valve 103 for connection. The connection mechanism 102 preferably has a flange structure for maintaining a vacuum, and the vacuum seal may be any of an O-ring seal and a metal seal, and the fixing method may be any method using a bolt, a coupler, a clamp, or the like. More preferably, it can be easily attached and detached. Further, it is more preferable to provide the exhaust conductance control means 104 in order to adjust the pressure inside the reaction device 101. Regarding gas supply, it is connected to a gas supply pipe 110 through a flow rate variable valve 109 and is connected to a gas supply and flow rate control means 111. When an abnormality occurs in the reaction container and the discharge is stopped, by gradually closing the flow rate variable valve 109, it is possible to gradually reduce the gas introduction into the reaction container where the abnormality has occurred. At that time, the gas supply and flow rate control means 111 gradually reduces the total flow rate of the gas while keeping the gas mixture ratio constant, and the flow rate variable valve 109 is fully closed, and at the same time, the gas supply and flow rate control means 111. The desired gas flow rate from (1) (if n and i described above are used, (ni))
/ N times the value). Also,
It is desirable to provide a gas connection mechanism 107 between the reaction device 101 and the variable flow valve 109. Further, when it is necessary to exhaust the gas remaining in the connection portion, it is possible to exhaust the gas through the exhaust path connected to the collective exhaust pipe 105 via the valve 108. This connection mechanism 10
7. Reactor 1 having an exhaust mechanism for the connecting portion
It is possible to quickly disconnect 01 from the gas supply system. Regarding high frequency introduction, it is connected to a high frequency power source 113 via a connector 112. Further, it is desirable to provide a shield (not shown) on the outside of the reaction container for preventing high frequency from leaking to the outside. This shield may be installed for every reaction container, or may be shared if it is desired to be shared for the purpose of space efficiency and cost reduction.

FIG. 1B is a schematic view showing an example of a connection mechanism in which an exhaust connection mechanism and a gas supply connection mechanism are integrated. FIG. 1B shows only the periphery of one reactor, and a plurality of such configurations are connected to each other and connected to a common exhaust means and a common gas supply means, and the whole vacuum processing apparatus is connected. Is forming.

In FIG. 1B, the reaction device 101 is connected to the integrated connection mechanism 114 via a gate valve 116. The gas supply system is also connected to the integrated connection mechanism 114 via the valve 115. The integrated connection mechanism 114 has a structure in which the gas connection mechanism is included inside the vacuum holding structure of the exhaust pipe. The structure of the shared exhaust means and the path to the gas supply means is the same as in FIG. With the structure as shown in FIG. 1B, even if gas leaks in the gas connection mechanism, the gas connection mechanism is enclosed in the vacuum holding region in the exhaust pipe, so that the gas is released into the atmosphere. Never be done.

FIG. 2 shows a schematic cross-sectional view of a reaction apparatus for forming a deposited film, particularly a reaction apparatus capable of favorably producing an electrophotographic photoreceptor on a cylindrical substrate. The reaction apparatus is provided with a cylindrical substrate 201, substrate supports 204a and 204b containing a substrate heater 202, and a source gas introduction pipe 203, and a high frequency matching box 217 is connected to a cathode electrode 207 which constitutes a part of the reaction container. Has been done. The cathode electrode 207 is insulated from the ground potential by the insulators 208 and 209, is maintained at the ground potential through the substrate support 204b, and a high frequency voltage can be applied between the cathode electrode 207 and the cylindrical substrate 201 which also serves as the anode electrode. The raw material gas is connected to the gas supply and flow rate control means as shown in FIG.
As shown in FIG. 1, it is connected to a common exhaust means via a flange 216.

FIG. 3 shows a reaction apparatus for forming a deposited film of FIG.
An example of a reactor unit in which individual units are integrated and made into one module is shown. Such a unit is shown in FIG.
By further connecting and using as shown in (b), a large amount of deposited film can be formed at one time. In this case, stopping the film deposition due to a defect is performed in units of this unit. The reaction container 301 has the same configuration as that of FIG. 2, and has a form in which a portion corresponding to the cathode electrode 207 in FIG. 2 is electrically connected, and is further connected to a connector 309 via a matching box 308. . This connector 309 will be connected to the high frequency power supply 113 via the connector 112 in FIG. In addition, the gas introduction part and the exhaust part are the collective pipes 302 and 3.
03, and they are connected to the connection mechanisms 306 and 307 via valves 304 and 305, respectively. These are Figure 1
Gas connection mechanism 107 and exhaust connection mechanism 10 in (a)
2 will be connected respectively.

Next, an example of a procedure for producing an electrophotographic photosensitive member as a vacuum process using the apparatus shown in FIGS. 1 and 2 will be described. First, the exhaust unit 106 exhausts the inside of the reaction container. At this time, the exhaust conductance control unit 104 sets the conductance to be maximum. When the inside of the reaction vessel reaches a desired pressure, an inert gas such as He or Ar is supplied from the gas supply means 111, and the conductance control means 104 adjusts the pressure inside the reaction vessel to be constant. Next, the substrate is heated by the substrate heater 202 to 200 ° C. to 350 ° C.
Control to a predetermined temperature of ° C. Next, after the inert gas for heating is stopped and exhausted, the gases necessary for forming the deposited film are mixed, the flow rate is controlled, and the source gas is supplied into the reaction vessel.
Also in this case, the conductance control means 104 is used to adjust the pressure inside the reaction vessel to a constant value. When the internal pressure is stable, the high frequency power is set to a desired value from the high frequency power supply 113, supplied to the cathode 207 through the connector 218, the matching box 217 and the matching box 217. On this occasion,
The cylindrical substrate 201 acts as an anode to cause glow discharge in the reaction vessel. The source gas is decomposed by this discharge energy, and a predetermined deposited film is formed on the cylindrical substrate 201. After the formation of the predetermined film thickness, the supply of the high frequency power is stopped, the inflow of the gas into the reaction container is stopped, and the formation of the deposited film is completed. By repeating the same operation a plurality of times, a desired multi-layered electrophotographic photoreceptor is formed. Note that the deposited film can be formed by the same procedure by using the unit of the reaction device shown in FIG. 3 instead of the reaction device shown in FIG.

By performing such a series of operations,
A procedure will be described in the case where a desired deposited film is obtained, but an abnormality occurs in the discharge in the initial stage or during the vacuum process.

First, the supply of high frequency power from the high frequency power supply 113 is stopped in order to stop the discharge in the reaction device 101 in which a defect has occurred. Next, assuming that the exhaust balance will be lost, the pressure in another reaction container that is normally performing vacuum processing is monitored, and the exhaust speed of the exhaust means 106 is adjusted. Specifically, for example, when the exhaust means 106 is composed of a combination of a rotary pump and a mechanical booster pump, the control frequency of the mechanical booster pump is adjusted and the pressure in the reaction container which is normally vacuum-processed. May be set to a set pressure value experimentally obtained in advance. Further, when the exhaust conductance control means is provided, the conductance may be adjusted in the same manner, and it is more preferable that the conductance control means be individually installed for each reaction device. It is all right if the system has a mechanism for automatically adjusting the conductance in conjunction with each other.

Further, as described above, if the gas is left flowing in the reactor where the discharge is stopped, various adverse effects occur. Therefore, the flow of the gas into the reactor where the discharge is stopped is stopped and the other reactors are stopped. It is desirable to change the flow rate of the above gas to an appropriate value. First, the flow rate variable valve 109 on the gas supply pipe of the reactor in which the malfunction has occurred is closed. At this time, it is desirable to gradually reduce the gas introduction amount. As the flow rate variable valve, a needle valve or the like can be preferably used, and it is desirable that it can be electrically controlled by a motor or the like. When the gas is supplied by branching to four reactors as shown in FIG. 1 (a), the amount of gas must be 3/4 times. The flow rate of each gas used is gradually reduced to 3/4 times using the gas flow rate control means (included in 111). Then, the output value from the gas flow rate control means may be 3/4 times at the same time when the flow rate variable valve 109 is fully closed. These interlocked changes may be linear or stepwise, and any change pattern may be used as long as the rapid change is moderated.

Further, for example, when the shield connected to the ground is arranged so as to include all the reaction vessels, among the high frequency power supplied from the high frequency power source, the power input into the reaction vessel is delicate. It may shift to
At this time, the set value is changed to the power value that is experimentally determined in advance.

Regarding the change of the control set value upon occurrence of trouble as described above, the means for detecting an abnormality, the pressure control means, the gas flow rate control means, the high frequency power control means, etc. are interlocked to automatically set the set value. Most desirable to change. Specifically, using a sequencer, computer, etc., various detection means (pressure, reflected power, temperature, plasma emission, etc.)
To monitor for abnormalities. For example, pressure gauge, high frequency power supply,
Some thermometers, photodiode sensors, and the like have an analog output (function of converting a detected value into a voltage of about 0 to 5 V and outputting the voltage). Using this, using a sequencer, computer, etc., if the detected value deviates from the normal value within a certain limit range and does not recover even after a certain period of time (for example, several seconds to several tens of seconds), it is abnormal A method such as determining that Then, upon detecting an abnormality, the flow rate variable valve 109 is used by using a sequencer or the like.
The electric control, the flow rate control of the gas flow rate control means (included in 111), the output control of the high frequency power, etc. may be automatically changed to the preset set value at the time of abnormality.

Further, it is more preferable to disconnect the reaction device in which the defect has occurred, investigate the cause of the defect, take countermeasures, make adjustments, and prepare for the next discharge. For example, in FIG. 2, the valve 213 and the valve 214 are closed, only the piping portion is evacuated through the valve 108, a purge gas is caused to flow by a purge means (not shown) to sufficiently purge the gas, and a venting means (not shown) is used to disconnect the valve, thereby performing normal operation. It is possible to separate only the reaction device in which the malfunction has occurred, with almost no effect on the other reaction devices that are performing. After the separation, it is possible to connect to another evacuation means having a purging means to carry out purging and vent to open a defective reaction apparatus for investigation. Alternatively, it is also possible to carry out purging before separation by the following procedure. For example, after confirming that the gate valve 103 and the valve 109 of the gas introduction unit are closed, a purging unit (preferably including an independent purging gas supply unit and exhaust unit) (not shown) is used to form a reaction vessel, piping, etc. Should be sufficiently purged. After confirming that the remaining material gas has been sufficiently replaced, if necessary, nitrogen for venting is introduced, and the connecting means 107, 102, 112 in FIG. 1 (a) and the connecting means 107, 102, 112 in FIG. By removing the connecting portions 114 and 112, respectively, the reaction device 101 having a defect can be separated.

Further, the reaction apparatus for forming a deposited film shown in FIG. 4 may be used in combination. FIG. 4 shows a deposited film forming apparatus that can suitably use a high frequency called a VHF band, which has a relatively higher frequency than the RF band of 13.56 MHz.
FIG. 3 is a schematic view of an apparatus capable of suitably depositing an electrophotographic photoreceptor on a cylindrical substrate 401. Figure 4 (a)
This is an amorphous silicon photoconductor manufacturing apparatus having a configuration in which a cathode electrode 404 is installed outside the reaction container 402 and a plurality of cylindrical substrates 401 are installed in the reaction container 402. In addition, FIG.4 (b) has shown the AA 'cross section figure of FIG.4 (a).

In the apparatus shown in FIG. 4, the high frequency power oscillated from the high frequency power supply 408 is applied to the power feeding point of the power branch 413 via the matching box 409, and the reaction container 40
2 is configured so that electric power is supplied to the reaction container 402 from a plurality of cathode electrodes 404 provided outside the device and plasma is generated in the reaction container 402 to form a deposited film.

In order to efficiently introduce the high frequency power emitted from the cathode electrode 404 into the reaction vessel 402, a ceramic material which is a dielectric is used on the side wall of the cylindrical reaction vessel 402. Specific examples of ceramic materials include alumina, titanium dioxide, aluminum nitride, boron nitride, zircon, cordierite, zircon-cordierite, silicon oxide, and beryllium oxide mica ceramics. Of these, alumina, aluminum nitride, and boron nitride are preferable from the viewpoints of suppressing contamination of impurities during vacuum processing, heat resistance, and the like.

Furthermore, the reaction apparatus shown in FIG.
In the structure 02, six cylindrical substrates 401 are installed at equal intervals on the same circumference. Although the number of the cylindrical substrates 401 is six in FIG. 4, it can be arbitrarily changed according to the diameters of the reaction container and the cylindrical substrates. Also,
Six gas introduction pipes 403 for introducing gas are installed at equal intervals on the same circumference outside the arrangement circle of the cylindrical substrate. Also for this gas introduction pipe, any number can be used as long as the gas can be uniformly supplied.

Further, the power branch 413 and each cathode electrode 4
The connection of 04 may be connected via a capacitor.

The outline of the deposited film formation using the apparatus of FIG. 4 will be described below.

First, the cylindrical substrate 40 is placed in the reaction vessel 402.
1 is installed and the inside of the reaction vessel 402 is exhausted through an exhaust pipe by an exhaust device (not shown). Then, while the inert gas is flowing, the cylindrical substrate 401 is moved to 2 by a heater (not shown).
It is heated and controlled to a predetermined temperature of about 00 ° C to 300 ° C.

When the cylindrical substrate 401 reaches a predetermined temperature, the gas supply / adjustment means 111 and the valve 1
09, the raw material gas is supplied to the reaction vessel 4 via the connection mechanism 107.
Introduced in 02. Thereafter, the pressure inside the reaction vessel 402 is adjusted to 0.05 by using the exhaust conductance control means 104.
It is set to a predetermined pressure of 0.1 to 10 Pa, preferably ˜20 Pa. After confirming that the pressure in the reaction container 402 has been stabilized, high frequency power is supplied from the high frequency power source 408 to the cathode electrode 404 via the matching box 409. As a result, high-frequency power of two different frequencies is introduced into the reaction container 402, glow discharge occurs in the reaction container 402, the source gas is excited and dissociated, and a deposited film is formed on the cylindrical substrate. During formation of the deposited film, the cylindrical substrate 401 is rotated at a predetermined speed by the motor 411 via the rotating shaft 410, so that the deposited film is formed over the entire circumference of the surface of the cylindrical substrate 401.

After the desired film thickness is formed, the high frequency power supply is stopped, and then the source gas supply is stopped to complete the formation of the deposited film. By repeating the same operation a plurality of times, a desired light-receiving layer having a multilayer structure is formed.

Here, the apparatus shown in FIG. 4 uses a high frequency in the VHF band, and as described above, both high speed deposition and high quality can be achieved and it can be suitably used as a deposited film forming apparatus.
On the other hand, the pressure inside the reaction vessel during discharge is often lower than that in an apparatus using a high frequency in the RF band, and the exhaust balance may be greatly disturbed. This is because when high frequency waves in the VHF band are used, it may be preferable to lower the pressure in order to improve the characteristics. In the apparatus having such a low pressure and being connected to one exhaust means 106 by using the collecting pipe 105, when a problem occurs in one reaction vessel and the discharge is interrupted, the exhaust balance may be disturbed. Get higher In that case, it is desirable to provide the exhaust conductance control means 104 for each reaction container.

Further, in the apparatus shown in FIG. 4, two high frequency powers having different frequencies may be simultaneously supplied to the same electrode for vacuum processing. In this case, it is necessary to perform matching at two high frequencies at the same time, the latitude of the optimum matching point may be narrowed, and in rare cases, the discharge may not be successfully started at the start of vacuum processing. At this time, if there is a reaction device in which discharge cannot be started within a predetermined time, the characteristics may not be uniform. In that case, in the same procedure, the vacuum treatment of the reactor in which the discharge could not be started within the predetermined time is stopped, and the control set value of the other reactor which is normally performing the vacuum treatment may be changed.

Further, in FIG. 5, three devices of FIG. 4 are integrated and surrounded by one shield 415, and the common exhaust pipe 10 is provided.
5 and the common gas supply pipe 110 are connected to each other to show an integrated reactor. With such a configuration, space efficiency can be improved. In FIG. 5, the devices of FIG. 4 are not detachable,
It may be detachable. Even in the apparatus shown in FIG. 5, vacuum processing can be performed in the same manner as in the apparatus shown in FIG.

(Examples) The present invention will be described in more detail with reference to the following examples, but the present invention is not limited thereto.

Example 1 Four units of the reaction apparatus shown in FIG. 3 were connected on a cylindrical support by using a vacuum processing apparatus connected by the connection method shown in FIG. 1B. a-S
An i-type electrophotographic photosensitive member was prepared. An aluminum cylinder having a diameter of 30 mmφ and a length of 358 mm was used as the cylindrical support, and four cylinders were used for one reactor unit.
A total of 16 pieces were vacuum-processed at the same time. These four reactor units were connected to one exhaust means and one gas supply / flow rate control means. The pressure detecting means is installed outside the discharge space as in the case of the first embodiment, and the correlation with the true pressure is experimentally obtained in advance. As a high frequency power supply, the frequency is 13.56 MH
Four zs were used and were connected to each reactor unit independently. Then, Ar gas was added to each reaction vessel at 500
ml / min (normal), 200 per unit
0 ml / min (normal), total 8000 ml
/ Min (normal), and the internal pressure of each reaction vessel was controlled to 80 Pa using the exhaust conductance control means. In this state, the aluminum cylinder was heated using a heater, and the heater was controlled at a control temperature that had been measured in advance so that the surface temperature was around 260 ° C. After heating until the surface temperature was sufficiently stabilized, the aluminum cylinder was rotated at a speed of 2 rpm using a motor. From the gas supply / flow rate control means, a gas in which the amount of gas per reaction vessel shown in Table 1 was increased by 16 times was supplied, and a high frequency of 13.56 MHz was introduced from a high frequency power source to start discharge.

[0072]

[Table 1]

Next, during the deposition of the charge injection blocking layer, of the input terminals of the sequencer, the terminal for detecting the reflected power of the high frequency power source of one reactor unit was removed, and a high reflected power was obtained by using the DC power source. By deliberately inputting the corresponding voltage, the reflected power increased sharply. In response to this, the sequencer immediately stopped the discharge of one reactor unit. Upon detection of an abnormality, the variable flow valve (using a needle valve) is driven by a motor, and the gas supply is stopped only for the reactor by gradually closing it over 2 minutes. 3 /
It was changed to 4 times. Such setting value change is performed in all layers by changing the control program,
The film was continuously deposited to the end.

After a total of 12 electrophotographic photoconductors were taken out from the three reaction device units, three items of charging ability, sensitivity and optical memory were evaluated by the following method, and all reaction device units were normal. Comparison was made with the average value of the evaluation results of the electrophotographic photosensitive member when the film was deposited on.

<Evaluation of Charging Ability> The obtained photoconductor is installed in a modified Canon copying machine GP-55 modified for experiment, a constant current is applied to the main charging device, and the developing device is removed to develop. An electrometer was inserted in the container position, the photoreceptor was rotated in the same manner as in a normal copying operation, and the surface potential (dark area potential) was measured with the light source for exposure removed. The value at the center of the axis is
The representative value of chargeability was used. Further, such measurement was carried out at 7 points in the axial direction to examine the distribution of values. Further, the difference between the maximum value and the minimum value was defined as the value of the unevenness.

<Evaluation of Sensitivity> After returning the halogen lamp to the original state and adjusting the main charger current so that the dark part potential at the developing device position is constant, a predetermined blank paper having a reflection density of 0.1 or less is used as the original. The sensitivity is evaluated by the image exposure light amount when the image exposure light amount is adjusted so that the bright portion potential at the developing device position becomes a predetermined value. The value at the center in the axial direction was used as the representative value of sensitivity. Further, such measurement was carried out at 7 points in the axial direction to examine the distribution of values. Further, the difference between the maximum value and the minimum value was defined as the value of the unevenness.

<Optical Memory Evaluation> After the current value of the main charger is adjusted so that the dark portion potential at the developing device position becomes a predetermined value, the light portion potential when a predetermined blank sheet is used as an original becomes a predetermined value. The image exposure light amount is adjusted so that In this state, return the developing device and put on a Canon ghost chart (part number FY
9-9040) on which a black circle having a reflection density of 1.1 and a diameter of 5 mm is attached is placed on a document table, and a Canon halftone chart is overlaid on the original image.
Ghost Chart Diameter 5 Appears on Halftone Copy
The optical memory was evaluated by measuring the difference between the reflection density of the black circle of mm and the reflection density of the halftone portion. The value of the part where the optical memory was the worst on the image was used as the representative value of the optical memory.

As a result of the above evaluation, the charging ability, the sensitivity, and the optical memory all fell within a distribution of 5% or less from the average value of the photoreceptor characteristics when vacuum processing was performed as usual. It was found that the value of was almost unchanged from the normal value, and that there was almost no deterioration in characteristics.

(Comparative Example 1) An electrophotographic photosensitive member was prepared by using the same apparatus, conditions and procedures as in Example 1.

Similar to Example 1, during the deposition of the charge injection blocking layer, the discharge of one reactor unit was intentionally stopped by inputting the status of the increase in reflected power to the sequencer. At this time, the gas supply to the reactor where the discharge was stopped was not stopped, and the set value was not changed. That is, the overall setting value remains unchanged (as usual), the unreacted gas continues to flow, the pressure setting value is not changed, and the film is continuously deposited to the end to complete the electrophotographic photoreceptor. It was

As a result, it was confirmed that the charging performance was deteriorated by about 7% at the maximum, the sensitivity was deteriorated by about 5% at the maximum, and the optical memory was deteriorated by 8% at the maximum. Further, the distribution shape of the values in the axial direction was slightly changed, the unevenness value was worse than in the usual case, and both the charging ability and the sensitivity were deteriorated by about 10%.

Further, waste of gas cost has occurred. In addition, since a large amount of unreacted gas was exhausted, it was found that the load on the exhaust gas abatement device (not shown in FIG. 1) was increased.

(Example 2) The three reactors shown in FIGS. 4 (a) and 4 (b) were connected to each other by using the vacuum treatment equipment in which the exhaust system was shared by the connecting method shown in FIG. 1 (b). An a-Si-based electrophotographic photosensitive member was prepared on a cylindrical support. Further, the gas supply / flow rate control means is similarly shared. An aluminum cylinder having a diameter of 80 mmφ and a length of 358 mm is used as the cylindrical support, and six cylinders are used in one reactor, and they are arranged on the circumference for vacuum treatment. As the high-frequency power source, three power sources each having a frequency of 100 MHz were used, and each reactor was individually connected. Although the pressure detection means was installed outside the discharge space on the exhaust means side, the true pressure in the discharge space can be set by experimentally obtaining the correlation with the value of the pressure gauge in the discharge space in advance. .

First, He gas was added to each reaction vessel at 700 ml /
After flowing for min (normal), the internal pressure of each reaction vessel was controlled to 80 Pa using the exhaust conductance control means. In this state, the aluminum cylinder is heated by a heater (not shown) in FIG.
The heater was controlled at a control temperature that was measured in advance so as to be around 0 ° C. After heating until the surface temperature was sufficiently stabilized, the aluminum cylinder was rotated at a speed of 10 rpm using a motor. From the gas supply / flow rate control means, the amount of gas per reaction vessel shown in Table 2 was flown from each gas supply / flow rate control means, and a high frequency of 100 MHz was introduced from a high frequency power source to start discharge.

[0085]

[Table 2]

Next, during the formation of the charge injection blocking layer, the breaker of the high frequency power source of one of the three reactors was intentionally turned off to stop the discharge of the one reactor. . The termination of discharge was detected by monitoring the emission of plasma. Upon receipt of this abnormality detection by the sequencer, the flow rate variable valve (using a needle valve) provided in the gas introduction path of the reactor in which the discharge was stopped was driven by a motor to gradually reduce the flow rate over 2 minutes. In conjunction with this, the total gas flow rate is also gradually reduced by the gas flow rate control means, and at the same time when the introduction of gas into the reaction vessel (furnace) in which the discharge has stopped is stopped, the total flow rate is equal to the flow rate per furnace. It was controlled so as to be 2/3 times. Further, the pressure setting value of the other reactor was changed from 0.7 Pa to 1 Pa. This change of the pressure set value is based on a value experimentally obtained in advance, and it is known that the change causes the pressure in the discharge space to become a desired pressure. Such changes in the conditions (changes in the flow rate and pressure) were made in all layers by changing the control program, and the film was continuously deposited under the optimum conditions to the end.

After taking out a total of 12 electrophotographic photoconductors from the two reactors, a copier NP-6750 manufactured by Canon Inc.
Using the modified one, the three items of chargeability, sensitivity, and optical memory were evaluated in the same manner as in Example 1, and the results of evaluation of the electrophotographic photosensitive member when the film was normally deposited in all reactors were shown. Compared to the average value.

As a result, it was found that the charging ability, the sensitivity, and the optical memory were within the distribution of 3% or less from the average value of the characteristics of the photoconductor when vacuum processing was performed as usual, and there was almost no deterioration in the characteristics. . Moreover, the distribution shape of the values in the axial direction and the value of the unevenness were almost the same.

(Comparative Example 2) An electrophotographic photosensitive member was prepared in the same manner as in Example 2, and the discharge of one reactor was intentionally stopped in the middle of the charge injection blocking layer as in Example 2. The gas supply to the reactor where the discharge was stopped was not stopped, and the set value was not changed. In other words, the setting value of the whole is left as it is (as usual), the unreacted gas is kept flowing,
The electrophotographic photosensitive member was completed by continuously depositing a film without changing the pressure setting value.

The obtained photosensitive member was evaluated in the same manner as in Example 2 and compared with the average value of the evaluation results of the electrophotographic photosensitive member when the film was normally deposited in all the reaction devices.

As a result, the charging ability is 10 at maximum.
%, The sensitivity was up to 12%, and the optical memory was up to 25%. Especially, the distribution shape in the axial direction is considerably changed, which suggests that the gas balance in the reaction vessel is changed. In terms of unevenness, the charging ability was deteriorated by up to 18% and the sensitivity was deteriorated by 22%.

Further, waste of gas cost occurs. Furthermore, since a large amount of unreacted gas was exhausted, it was found that the load on the exhaust gas abatement device (not shown in FIG. 1) increases.

Example 3 Using the reaction apparatus shown in FIG. 5, an a-Si electrophotographic photosensitive member was prepared on a cylindrical support. The cylindrical support has a diameter of 30 mm and a length of 3
Using a 58mm aluminum cylinder,
A total of 30 reactors were vacuum-treated with 10 reactors at the same time. These three reactors are connected to one exhaust means and one gas supply / flow rate control means. A high-frequency power source having a frequency of 105 MHz was used, and each reactor was individually connected. As shown in FIG. 5, the shield is common to the three reaction vessels. Subsequently, He gas was caused to flow into each reactor at 700 ml / min (normal), a total of 2100 ml / min (normal), and the internal pressure of each reaction vessel was controlled to 80 Pa by using an exhaust conductance control means. In this condition, the heater is used to heat the aluminum cylinder, and the surface temperature is about 2
The heater was controlled at a control temperature which was measured in advance and set to 30 ° C. After heating until the surface temperature was sufficiently stabilized, the aluminum cylinder was rotated at a speed of 10 rpm using a motor. From the gas supply / flow rate control means, set the gas amount per reaction vessel shown in Table 3 to 3
A doubled gas was flowed and a high frequency of 105 MHz was introduced from a high frequency power source to start discharge.

[0094]

[Table 3]

Next, at the initial stage of the deposition of the photoconductive layer, the exhaust pressure conductance control means of one of the three reactors was intentionally fully opened to extremely lower the internal pressure, and abnormal discharge was generated. Let In response to this, the sequencer automatically stopped the discharge of one reactor.
In addition, the gas supply is stopped only by gradually closing the flow rate variable valve, and the total gas flow rate is 2
It was gradually changed to 3 times. At this time, the pressure set value of the other reactor is adjusted from the normal 0.8 Pa to 1.2 Pa which is a set value experimentally obtained in advance so that the true internal pressure becomes a desired value. I was able to maintain it.
Further, in this apparatus configuration, when the electric power supplied to one reaction container is stopped, the value of the power supplied to the two reaction containers which are normally vacuum-processed is reduced by 7%. It has been experimentally obtained in advance that the values are appropriate. Therefore, the value of electric power was reduced by 7% from the result of the preliminary experiment. Such a change in the set value was performed in all the subsequent layers, and the film was continuously deposited to the end.

After taking out a total of 20 electrophotographic photoconductors from two reaction vessels (reaction furnaces), the three items of charging ability, sensitivity and optical memory were evaluated in the same manner as in Example 1, and all were evaluated. This was compared with the average value of the evaluation results of the electrophotographic photosensitive member when the film was normally deposited by the reactor.

As a result, the charging ability, the sensitivity, and the optical memory were all within the distribution of 3% or less from the average value of the characteristics of the photoconductor when vacuum processing was performed as usual, and the characteristics were hardly deteriorated. Further, the distribution shape in the axial direction and the value of unevenness were almost the same as the normal values.

(Embodiment 4) Using a vacuum processing apparatus in which four reactors shown in FIG. 4 were connected by the connecting method shown in FIG. 1 (b), a- was formed on the cylindrical support. A Si-based electrophotographic photosensitive member was prepared. 80 for a cylindrical support
An aluminum cylinder having a diameter of mmφ and a length of 358 mm was used, and a total of 24 cylinders, 6 cylinders in one reactor, were simultaneously vacuum-treated. These four reactors were connected to one exhaust means and one gas supply / flow rate control means. A high frequency power source having a frequency of 100 MHz and a high frequency power source having a frequency of 60 MHz were used, and two types of high frequencies were combined in a matching box and applied simultaneously to the same electrode. These two types of high frequency power supplies and matching boxes are individually connected to each reaction device. Then, He gas is supplied to each reactor 7 times.
00 ml / min (normal), total 2800 m
1 / min (normal) was flown, and the internal pressure of each reaction furnace was controlled to 80 Pa using the exhaust conductance control means. In this state, the aluminum cylinder was heated using a heater, and the heater was controlled at a control temperature that was measured in advance so that the surface temperature was about 230 ° C. After heating until the surface temperature was sufficiently stabilized, the aluminum cylinder was rotated at a speed of 10 rpm using a motor. From the gas supply / flow rate control means, a gas having four times the amount of gas per reaction device shown in Table 4 was flowed,
High-frequency waves of 100 MHz and 60 MHz were introduced from two types of high-frequency power sources to start discharge.

[0099]

[Table 4]

Next, at the initial stage of the deposition of the photoconductive layer, one of the input terminals of the sequencer was disconnected from the pressure detection input terminal of one reactor, and a voltage corresponding to the case where the internal pressure became abnormally high by using the DC power supply. Was intentionally input to create an abnormal pressure situation. Upon receiving this abnormality, the sequencer immediately stopped the discharge of one reactor. The gas supply was also stopped only by gradually closing the flow rate variable valve. At this time, in the stopped reactor, the gas supply valve and the exhaust valve on the side of the reaction container are closed from the connection part, the connection part is purged in a state where the inside of the reaction container is vacuum-sealed, the connection means is removed, and the reaction device is removed. Removed. In parallel with this, the exhaust conductance control means of the other reactor was adjusted so that the internal pressure was from 1 Pa to 1.2 Pa, and the gas flow rate was gradually changed to 3/4 times. In this state, the film was continuously deposited until the end.

The removed reactor is opened after being sufficiently purged by an independent purging means, and while the film of another reactor is being deposited, the internal parts are replaced and the aluminum cylinder is replaced, and the film is immediately removed. It was possible to prepare for deposition. This means that it is possible to immediately elucidate the cause of the failure and take measures against it.

After taking out a total of 18 electrophotographic photoconductors from the three reactors on which the film was normally deposited, the charging ability, sensitivity, and optical memory were measured in the same manner as in Example 1. The evaluation was performed, and the result was compared with the average value of the evaluation results of the electrophotographic photosensitive member when the film was normally deposited in all the reaction devices.

As a result, the charging ability, the sensitivity, and the optical memory were all within the distribution of 3% or less from the average value of the characteristics of the photoconductor when vacuum processing was performed as usual, and the characteristics were hardly deteriorated. Further, the distribution shape in the axial direction and the value of unevenness were almost the same as the normal values.

As described above, it was confirmed that the film deposition can be performed more efficiently by connecting the reactor with the detachable connecting means.

[0105]

As described above, according to the present invention, when a plurality of objects to be processed are vacuum-processed simultaneously by using a plurality of reaction vessels sharing an exhaust means and a gas supply means, an abnormality occurs in a certain reaction vessel. When the above occurs, it is possible to minimize the effect on the object to be processed in the reaction vessel that is normally vacuum processing, minimize the decrease in product yield, and gas supply. By sharing the system, it is not necessary to provide a gas supply / flow rate control means, which is a very complicated and expensive incidental equipment, for each reaction vessel, and the equipment cost can be reduced, and the gas supply system is shared. At this time, even if the gas flow to the reaction vessel where the vacuum processing is stopped due to an abnormality is stopped, the balance of the gas amount into the reaction vessel that is normally vacuum processing is not disturbed, and the reduction in product yield is minimized. By doing In addition, the reaction vessel in which the abnormality has occurred can be immediately separated to quickly investigate the cause, respond, adjust, prepare for the next film deposition, and minimize the dead time of the production equipment. There is an effect that a high quality device can be supplied at a lower cost.

[Brief description of drawings]

1A is a schematic side view showing an example of a vacuum processing apparatus of the present invention, and FIG. 1B is a partially enlarged detailed side view of FIG. 1A.

FIG. 2A is a schematic cross-sectional view of an electrophotographic photoconductor manufacturing apparatus using a plasma CVD method that can suitably use high frequency power in an RF band, and FIG. 2B is a top view of FIG. Is.

FIG. 3A is a schematic diagram of an apparatus for manufacturing an electrophotographic photosensitive member using a plasma CVD method, which can suitably use high-frequency power in an RF band and can simultaneously process a plurality of objects to be processed. A side view and (b) are top views of (a).

FIG. 4A is a schematic diagram of an apparatus for manufacturing an electrophotographic photosensitive member using a plasma CVD method, which can suitably use high-frequency power in the VHF band and can simultaneously process a plurality of objects to be processed. A side view and (b) are sectional views taken along the line AA ′ of (a).

FIG. 5A is a diagram illustrating an apparatus for manufacturing an electrophotographic photosensitive member using a plasma CVD method, in which three devices shown in FIG. 4 are integrated and VHF band high-frequency power sharing a shield is preferably used. The schematic side view and (b) are the top views of (a).

[Explanation of symbols]

101 reactor 102 exhaust connection mechanism 103,116,214,305 Gate valve 104 Exhaust conductance control means 105 Collecting exhaust pipe 106 Exhaust means 107 gas connection mechanism 108, 115, 213, 304 valves 109 Flow rate variable valve 110, 211, 302 Gas supply piping 111 Gas supply / flow rate control means 112,218,309 connectors 113,408 High frequency power supply 114 Exhaust / gas supply integrated connection mechanism 201, 401 cylindrical substrate 202 Substrate heating heater 203 Raw material gas introduction pipe 204a, 204b, 406 Base support 205 exhaust port 207,404 Cathode electrode 208,209 Insulator 210 stand 212, 303, 407 Exhaust pipe 215,306 Coupler 216,307 Flange 217,308,409 Matching Box 301,402 Reaction container (reactor) 403 Gas introduction pipe 405 High-frequency power supply device 410 rotation axis 411 motor 412 gear 413 High-frequency power branch unit 415 shield

Front page continuation (51) Int.Cl. ⁷ Identification code FI theme code (reference) H01L 21/205 H01L 21/205 H05H 1/46 H05H 1/46 M (72) Inventor Hitoshi Murayama 3 Shimomaruko Ota-ku, Tokyo Canon No. 30-2 Canon Inc. (72) Inventor Toshiyasu Shirasuna 3-30-2 Shimomaruko, Ota-ku, Tokyo Canon Inc. F-term (reference) 2H068 DA23 EA25 EA30 4G075 AA24 AA30 BC01 BC02 BC03 BC04 BC06 CA25 CA26 CA47 CA65 DA02 4K030 AA06 AA10 AA17 BA30 CA02 FA01 FA03 JA05 KA01 KA08 KA28 KA30 KA39 KA41 LA17 5F045 AA03 AB04 AC01 AC07 AC16 AD06 AE19 BB20 CA16 DP25 EE17 EG02 EH15 EK07 EM10

Claims (14)

[Claims] 1. An object to be treated is installed in a plurality of depressurizable reaction vessels, each reaction vessel is connected to a pipe branched from the same exhaust means, and exhausted, and the same gas supply means is supplied to each reaction vessel. Further, after passing through the gas flow rate control means, a branched pipe is connected to introduce a gas required for processing, high-frequency power is simultaneously applied to each reaction vessel to form plasma, and a plurality of objects to be processed are processed simultaneously. In the vacuum processing method, when an abnormality occurs in the vacuum processing in at least one of the plurality of reaction vessels, the vacuum processing of the reaction vessel in which the abnormality occurs is stopped, and at the same time, the vacuum processing control setting is performed. A vacuum processing method, wherein the value is changed from a normal set value and the remaining vacuum processing is continued. 2. The vacuum processing method according to claim 1, wherein the changed control set value is a set value of a gas flow rate. 3. The set value of the gas flow rate is changed when the total number of reaction vessels connected to the same gas supply means and the same gas flow rate control means is n and the number of reaction vessels in which an abnormality occurs is i, The vacuum processing method according to claim 2, wherein the vacuum processing method is performed so that the set value of the total gas amount supplied from the gas flow rate control means is (n-i) / n times. 4. When an abnormality occurs, the amount of gas introduced into the reaction vessel whose vacuum processing has been stopped is gradually reduced, and in conjunction therewith, the gas flow rate supplied from the gas supply means and the gas flow rate control means is gradually decreased. 4. The vacuum processing method according to claim 3, wherein at the same time when the gas introduction into the reaction container where the abnormality occurs is stopped, the total gas flow rate to the other reaction container is changed to be (n−i) / n times. 5. The vacuum processing method according to claim 1, wherein the changed control set value is a pressure inside each of the reaction vessels. 6. The high frequency power for generating plasma is V
The vacuum processing method according to claim 5, wherein the high frequency or microwave of the HF band is used. 7. The plurality of reaction vessels are covered with a common shield, and the control set value to be changed is a power value supplied to each of the reaction vessels. The vacuum processing method according to claim 1. 8. The reaction container is provided with an exhaust means, a gas supply means, and a gas flow rate control means via a detachable connection mechanism,
8. The high-frequency power applying means is connected to each means, and when an abnormality occurs, the reaction container having the abnormality is disconnected from the exhaust means, the gas supply means, the gas flow rate control means, and the high-frequency power applying means. The vacuum processing method according to claim 1. 9. A plurality of reaction vessels capable of depressurization in which an object to be treated is installed, exhaust means for connecting each reaction vessel to a pipe branched from the same exhaust means, and exhausting the same gas for each reaction vessel. A gas supply means and a gas flow rate control means for supplying a gas required for processing by connecting to a branched pipe after passing through the supply means and the gas flow rate control means, and a high frequency power application means, and a plurality of objects to be processed are provided. In a vacuum processing apparatus capable of performing simultaneous processing, a means for detecting an abnormality when a vacuum processing abnormality occurs in at least one of the plurality of reaction vessels, and a vacuum processing for the reaction vessel in which the abnormality occurs A vacuum processing apparatus comprising: a means for stopping and a means for changing a control set value for vacuum processing from a normal set value. 10. A plurality of depressurizable reaction vessels in which an object to be treated is installed, exhaust means for connecting each reaction vessel to a pipe branched from the same exhaust means, and exhausting the reaction vessels, and each reaction vessel,
A plurality of gas supply means and a gas flow rate control means, which are connected to a branched pipe after passing through the same gas supply means and a gas flow rate control means to supply a gas required for processing, and a high frequency power application means, In a vacuum processing apparatus capable of simultaneously processing an object to be processed, a means for detecting an abnormality when an abnormality occurs in vacuum processing in at least one of the plurality of reaction vessels, and a reaction vessel in which the abnormality occurs Means for stopping the vacuum treatment of the reactor, a valve for stopping the introduction of gas into the reaction container where an abnormality has occurred, and the sum of the gas flow rate set values for other reaction vessels are the same gas supply means and gas flow rate control means. And n is the total number of reaction vessels connected to each other and i is the number of reaction vessels in which an abnormality has occurred, and a means for changing the number to (n-i) / n times. . 11. A valve for stopping the introduction of gas into a reaction vessel in which an abnormality has occurred has a function of gradually reducing the flow rate, and in conjunction therewith, the gas flow rate supplied from the gas supply means and the gas flow rate control means. And a mechanism for changing the total gas flow rate to another reaction container to (n−i) / n times at the same time when the gas introduction to the reaction container where the abnormality occurs is stopped. Item 10. The vacuum processing apparatus according to item 10. 12. The exhaust means comprises exhaust conductance control means for controlling the pressure in the reaction container, which is normally vacuum-processed when an abnormality occurs, to be constant. The vacuum processing apparatus described. 13. The exhaust conductance control means comprises:
13. The vacuum processing apparatus according to claim 12, which can be independently controlled in each reaction container. 14. The reactor according to claim 9, wherein the reaction container is attachable / detachable to / from each of the exhaust means, the gas supply means, the gas flow rate control means, and the high-frequency power applying means via a detachable connection mechanism. The vacuum processing apparatus according to item 1.