JP2002016011A - Cleaning method for dry film forming apparatus, dry etching method, and article manufacturing method including a step of performing any one of these methods - Google Patents

Abstract

(57) Abstract: A deposition capable of efficiently removing by-products in a reaction vessel and stably obtaining a high-quality deposited film, particularly a high-quality electrophotographic photosensitive member. Provided is a method for manufacturing an article including a cleaning method for a film forming apparatus, a dry etching method, and a step of performing any one of these methods. Kind Code: A1 A method of cleaning a deposited film forming apparatus for cleaning a deposited film forming apparatus for forming a deposited film on a substrate disposed in a reaction vessel capable of being decompressed using a cleaning gas and high frequency power. In the cleaning process, the supply of the high-frequency power is temporarily stopped during the cleaning process, and then the cleaning process is restarted to perform the cleaning process.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method of cleaning a deposited film forming apparatus, a method of dry etching, and a method of manufacturing an article including a step of performing any one of the methods. Receiving member, solar cell, image input line sensor, imaging device, TFT
Cleaning treatment method of a deposited film forming apparatus and a vacuum processing apparatus for producing a deposited film suitable as a semiconductor element such as,
The present invention relates to a dry etching method and a method for manufacturing an article including a step of performing any one of the methods.

[0002]

2. Description of the Related Art Conventionally, light receiving members for electrophotography, solar cells, line sensors for image input, image pickup devices, TFTs
As a deposited film used as a semiconductor element such as, for example, amorphous silicon, for example, amorphous silicon compensated with hydrogen and / or halogen (for example, fluorine, chlorine, etc.) (hereinafter referred to as “a-Si (H, X)”) ) Films and the like have been proposed, some of which have already been put to practical use. Various devices have been proposed for forming a deposited film such as an a-Si (H, X) film. In these apparatuses, for example, a vacuum deposition method, an ion plating method, a sputtering method, a thermal CVD method, a plasma CVD method, a photo CVD method, or the like can be performed. Among these methods, plasma C
The film is formed by a film forming method of forming a film under reduced pressure such as a VD method.

When a deposited film is formed on a desired substrate by these film forming methods, the deposited film or a powdery polymer (hereinafter abbreviated as polysilane) is deposited on a film forming chamber constituent member or the like. . For example, plasma C by glow discharge decomposition
When a film is formed by the VD method, a deposited film or polysilane is formed on a susceptor, a counter electrode, or an inner wall of a reaction film in a deposition film forming apparatus (hereinafter abbreviated as a reaction container) other than a substrate. You. These deposited films or polysilanes deteriorate the properties of the resulting film by being incorporated as impurities into the film formed at the next film formation, or the polysilane adheres to the substrate, causing defects in the formed deposited film. To form If the deposition is repeated several times,
The yield of the target deposited film is greatly reduced.

[0004] For this reason, it is necessary to clean the film forming chamber after several film forming cycles or at every film forming cycle to remove the film or polysilane deposited on the portion other than the target film forming position. Will be As a cleaning method at that time, there is a method in which an element forming a deposited film or polysilane is reduced by a gas phase molecule by a gas phase chemical reaction, and cleaning is performed. The gas used for cleaning is C
F ₄ gas, a NF ₃ gas, a gas such as SF _6, which flowed in the reaction vessel, plasma, heat, and an excited state by the energy of light or the like, to form a deposited film or powder which element the reaction In this method, these elements are converted into gas phase molecules, eliminated by an exhaust means, and cleaned.

In recent years, ClF ₃ gas has attracted attention as a gas having an etching action. ClF ₃ gas is decomposed with low energy and is highly reactive, and has an extremely high etching rate as compared with a conventional etching gas. Various dry etching cleaning methods using this ClF ₃ have been proposed. For example, the 27th
Japanese Patent Publication No. 20966 describes a cleaning method containing at least one of ClF, ClF ₃ and ClF ₅ . By such a cleaning process, cleaning can be efficiently performed.

On the other hand, in recent years, higher image quality of an electrophotographic apparatus has been required, and accordingly, the resolution of an electrophotographic light-receiving member for developing a latent image has been increasingly improved. In addition, as the speed of the copier advances and the charging conditions become severe such as the time required for charging decreases, the portion where the potential is not applied on the surface substantially affects the potential around the surface, As a result, it has been pointed out that image defects occur due to such portions. Further, in the conventional electrophotographic apparatus, the main purpose of the apparatus is to copy characters, so that the original document (so-called line copy) was mainly used, so that the image defect did not become a serious problem in practical use. On the other hand, in recent years, as the image quality of a copying machine has been improved, many originals including halftones such as photographs have been copied, and image defects that were not noticed by line copying have been recognized. as a result,
At present, there is a need for an electrophotographic photosensitive member (light receiving member) having less abnormally grown portions than ever before. In particular, in a copying machine, which is one of the electrophotographic apparatuses that have become widespread in recent years, the copier becomes more visually evident, and therefore, an electrophotographic photoreceptor having less abnormally grown portions is required. Under the circumstances described above, it has become necessary to more efficiently produce products with higher yields than ever before.

[0007]

However, in the prior art described above, when cleaning the deposited film or polysilane remaining in the reaction vessel after the formation of the deposited film, articles such as a light receiving member are required. In view of the performance required especially for the photoreceptor, there are still the following problems to be solved. That is, conventionally, polysilane and C
By reacting with 1F ₃ gas to remove polysilane,
In order to achieve satisfactory removal, a long time is required for the cleaning process, and as a result, the supply amount of ClF ₃ gas and the supply amount of electric power increase. Also, since the exhaust means, especially the rotary pump, continuously sucks the ClF ₃ gas for a long time,
The load on the exhaust means increases. If the removal is not satisfactory, the fine powder will remain mainly on the inner wall of the reaction vessel. When such fine powder remains,
It has been confirmed that when a deposited film is formed next, it may scatter and form a defect on the deposited film.

[0008] This is delicate in products such as electrophotographic photoreceptors having a large area that is long in the longitudinal direction, due to the formation of deposited films or unevenness in the formation of polysilane remaining in the reaction vessel furnace. This is considered to be caused by unevenness in the cleaning process. as a result,
As a result, minute image defects occur in the electrophotographic photoreceptor produced. Although this is a level that has not been a problem in the past, as described above, it cannot be ignored especially in recent years where high resolution and higher image quality are required.

Accordingly, the present invention solves the above-mentioned problems in the conventional art, and can efficiently remove by-products in a reaction vessel, and can deposit a high-quality deposited film, particularly a high-quality electrophotographic photosensitive material. It is an object of the present invention to provide a method of cleaning a deposited film forming apparatus and a method of dry etching capable of stably obtaining a body.

[0010] The present invention also provides a deposition film forming apparatus for cleaning a deposition film forming apparatus for forming a deposited film on a substrate disposed in a reaction vessel capable of reducing pressure using a cleaning gas and high frequency power. In the cleaning method, there is provided a cleaning method for a deposited film forming apparatus for performing a cleaning process by temporarily stopping supply of the high-frequency power during the cleaning process and then restarting the cleaning process again. The purpose is to do.

Further, the present invention provides a dry etching method for a vacuum processing apparatus, wherein a high-frequency power and a gas for dry etching are supplied under reduced pressure to dry-etch unnecessary solid matter present in the vacuum processing apparatus. The first dry etching step is stopped by stopping the processing step and the supply of the high-frequency power and the dry etching gas, and the solid unnecessary matter is dry-etched while the first dry etching step is stopped. A second dry etching process to be performed, and a third dry process for stopping the second dry etching process by supplying high frequency power and a dry etching gas to dry etch the unnecessary solid matter present in the vacuum processing apparatus. To provide a dry etching method having an etching step To.

Further, the present invention provides a deposition film forming step of arranging a substrate in a reaction vessel and forming a deposition film on the substrate, and forming a deposition film by the deposition film forming step, and then forming the deposition film in the reaction vessel. A first cleaning process for supplying the cleaning gas and the high-frequency power into the reaction vessel, a second cleaning process for stopping the supply of the high-frequency power, and a third cleaning process for supplying the cleaning gas and the high-frequency power to the reaction vessel. A cleaning treatment step of performing each treatment of the cleaning treatment in the order described above, and after the cleaning treatment step, forming a deposited film on another substrate by the deposited film forming step. The purpose is to provide.

Further, the present invention provides a deposited film forming apparatus for cleaning a deposited film forming apparatus for forming a deposited film on a substrate disposed in a reaction vessel which can be decompressed, using a cleaning gas and high frequency power. In the cleaning method, the cleaning processing includes at least a first processing step and a second cleaning processing step, and the concentration of the cleaning gas in the first step is the cleaning gas in the second step. It is an object of the present invention to provide a cleaning method for a deposited film forming apparatus in which the internal pressure of the first step is lower than the internal pressure of the first step, which is higher than the concentration of the second step.

[0014]

In order to achieve the above object, the present invention provides a cleaning method, a dry etching method, and a cleaning method for a deposited film forming apparatus having the following constitutions (1) to (24). An object of the present invention is to provide a method for manufacturing an article including a step of performing any one of the methods. (1) A cleaning method of a deposition film forming apparatus for cleaning a deposition film forming apparatus that forms a deposited film on a substrate disposed in a reaction vessel that can be depressurized using a cleaning gas and high-frequency power, In the cleaning process, the supply of the high-frequency power is temporarily stopped during the cleaning process, and then the supply of the high-frequency power is restarted. Cleaning treatment method. (2) The deposition film formation according to (1), wherein the cleaning process includes a cleaning process by a gentle reaction of a cleaning gas in the deposition film forming apparatus by stopping the supply of the high-frequency power. Cleaning method for the device. (3) The cleaning gas according to (1) or (2), wherein the concentration of the cleaning gas used in restarting the cleaning process is different from the concentration of the cleaning gas used in the cleaning process before restarting. Cleaning method for a deposited film forming apparatus. (4) the cleaning gas is the characterized in that it is a mixed gas of inert gas and ClF ₃ (1) ~
The cleaning method of the deposited film forming apparatus according to any one of (3). (5) The cleaning method according to the above (4), wherein the inert gas is Ar. (6) In the cleaning process, the timing at which the supply of the high-frequency power is stopped is determined based on a result of the detection of the temperature or pressure in the deposition film forming apparatus. 1) to (5)
The cleaning method for a deposited film forming apparatus according to any one of the above. (7) The cleaning process includes a period during which the supply of the cleaning gas is temporarily stopped during the cleaning process.
The cleaning method for a deposited film forming apparatus according to any one of the above. (8) The deposited film according to (7), wherein the period in which the supply of the cleaning gas is temporarily stopped is included in the period in which the supply of the high-frequency power is temporarily stopped. A cleaning method for a forming apparatus. (9) The deposition film forming apparatus according to (7), wherein the period in which the supply of the cleaning gas is temporarily stopped is a period in which the supply of the high-frequency power is temporarily stopped. Cleaning treatment method. (10) The temporary stop and restart of the supply of the cleaning gas are performed in accordance with the temporary stop and restart of the supply of the high-frequency power.
3. The cleaning method for a deposited film forming apparatus according to item 1. (11) The period in which the supply of the cleaning gas is temporarily stopped is determined based on the temperature or the pressure in the deposited film forming apparatus. Cleaning treatment method. (12) In the course of the cleaning process, after temporarily stopping the supply of the cleaning gas and the high-frequency power, the reaction container unit constituting a part of the deposited film forming apparatus is moved to the deposited film forming apparatus. The deposition according to the above (7), which includes relocating the reactor to a different location, restarting the cleaning process for the reaction vessel unit at the same time or with a time lag with the deposition film forming apparatus, and cleaning these components. A cleaning method for a film forming apparatus. (13) In the cleaning process, the timing at which the supply of the high-frequency power is stopped is determined based on the detected result by detecting the temperature or pressure in the deposition film forming apparatus, and based on these results. The deposition film forming apparatus according to any one of (1) to (11), wherein a processing time until the temporary stop is set in advance, and a cleaning process is performed based on the set time. Cleaning treatment method. (14) In any one of the above (1) to (12), wherein the cleaning process is performed by supplying the cleaning gas into the reaction vessel, setting the internal pressure to a predetermined value, and then supplying the high-frequency power. A cleaning method for a deposited film forming apparatus according to any one of the above. (15) The cleaning process of the deposited film forming apparatus according to any one of (1) to (13), wherein the cleaning process is performed while reducing a load of an exhaust device that exhausts the inside of the reaction vessel. Method. (16) A cleaning method of a deposition film forming apparatus for cleaning a deposition film forming apparatus that forms a deposited film on a substrate disposed in a reaction vessel capable of reducing pressure using a cleaning gas and high frequency power. In the cleaning process, the cleaning process includes at least a first process and a second process, and the concentration of the cleaning gas in the first process is higher than the concentration of the cleaning gas in the second process. Wherein the internal pressure in the first step is lower than the internal pressure in the second step. (17) The cleaning process temporarily stops supply of the cleaning gas and the high-frequency power between the first step and the second step, and changes the concentration of the cleaning gas in each of the steps. The cleaning process of the deposited film forming apparatus according to the above (16), wherein the cleaning process is started. (18) In a dry etching method for a vacuum processing apparatus, a first dry etching processing step of supplying high-frequency power and a dry etching gas under reduced pressure to dry-etch solid unnecessary substances present in the vacuum processing apparatus; Stopping the supply of high-frequency power to stop the first dry etching step, and dry-etching the solid undesired matter with the first dry etching step stopped; Supplying a dry etching gas to stop the second dry etching step, and dry-etching the unnecessary solid matter present in the vacuum processing apparatus. Dry etching method. (19) The dry etching method according to (18), wherein the supply of the second dry etching gas is stopped in the second dry etching process. (20) The method for cleaning a deposited film forming apparatus according to any one of (1) to (17), or (1)
8) A method of manufacturing an article, comprising a step of performing any one of the dry etching methods according to any one of the items 19) to 19). (21) The method for producing an article according to (20), wherein the article includes a light receiving member for electrophotography. (22) disposing a substrate in a reaction vessel, forming a deposited film on the substrate, forming a deposited film in the deposited film forming step, and taking out the substrate from the reaction vessel A first cleaning process for supplying a cleaning gas and high-frequency power to the reaction vessel, a second cleaning process for stopping the supply of high-frequency power, and a third cleaning process for supplying a cleaning gas and high-frequency power to the reaction vessel. And a cleaning process step of performing the above steps in the above order, and after the cleaning process step, forming a deposited film on another substrate by the deposited film forming step. (23) The method for manufacturing an article according to (22), wherein the supply of the cleaning gas is stopped in the second cleaning process. (24) The method for producing an article according to the above (22) or (23), wherein the article includes a light receiving member for electrophotography.

[0015]

DESCRIPTION OF THE PREFERRED EMBODIMENTS In an embodiment of the present invention,
When the cleaning process is performed by applying the above-described configuration, after the supply of the high-frequency power or the cleaning gas and the high-frequency power is temporarily stopped during the cleaning process, the cleaning remaining in the deposited film forming apparatus is performed. During the mild reaction by the reactive gas, that is, the reaction between the cleaning gas and the solid unnecessary substances such as the deposited film and polysilane, the pressure is reduced in a state in which the factor that actively promotes the reaction is stopped. The cleaning process is restarted again while accelerating the reaction to remove solid unwanted substances underneath, and by performing the cleaning process, the efficiency of the cleaning process is reduced, the variation of the deposited film is suppressed, and the deposited film of high quality, especially high quality (Photoreceptive member for electrophotography) can be stably obtained. When performing the cleaning process, at least the first step and the second step are performed.
A cleaning process step, wherein the concentration of the cleaning gas in the first step is higher than the concentration of the cleaning gas in the second step, and the internal pressure of the first step is the second pressure.
It can be configured to perform a cleaning process set lower than the internal pressure of the process.

In the present invention, the cleaning process includes a process of supplying a cleaning gas to the inside of the reaction container of the deposition film forming apparatus and a process of supplying electric power to the inside of the reaction container to which the cleaning gas has been supplied. That is. In the present invention, it may be configured to include a step of stopping the supply of high-frequency power, preferably the supply of cleaning gas and the supply of high-frequency power, during the cleaning process. Of course, even when the supply of the high-frequency power is not completely stopped, the case where the power is supplied in a state in which substantially no discharge occurs is considered to be stopped.

The cleaning process of the present invention can also be viewed as follows. That is, the cleaning gas is supplied into the reaction container of the deposition film forming apparatus in a period before and after a period in which the supply of the high-frequency power or the supply of the cleaning gas and the supply of the high-frequency power are stopped halfway, and the cleaning gas is supplied. It can be considered that the cleaning process is performed in a period during which power is supplied to the inside of the supplied reaction container.

In the present invention, a reaction performed at least between a certain cleaning process and the next cleaning process, that is, at least between the two cleaning processes, is referred to as a "mild reaction". Even in this mild reaction, the cleaning process is performed, that is, the dry etching of the unnecessary material is performed.

During the cleaning process sandwiching the mild reaction (that is, before and after the mild reaction), an etching gas, that is, a cleaning gas is supplied into the reaction vessel, and power is supplied to the reaction space. It enables active removal of solid waste. On the other hand, in this mild reaction, high-frequency power or high-frequency power and a cleaning gas are not supplied into the reaction vessel, so that the solid waste is removed under reduced pressure in a state where the reaction is not actively performed. Is performed.

In the present invention, the power frequencies of the two cleaning processes sandwiching the mild reaction may be the same or different. However,
It is preferable that the cleaning conditions are the same because the cleaning process can be performed in a short time even under the same conditions.

In addition, the gas type of the cleaning gas (dry etching gas) and the supply flow rate thereof may be the same or different in both cleaning processes sandwiching the mild reaction. However, it is preferable to use the same cleaning method because the cleaning process can be performed in a short time under the same conditions.

This is based on the following findings of the present inventors. That is, the deposited film or polysilane remaining in the reaction vessel after the deposited film is formed is
Initially, it was predicted that solid unwanted substances could be removed by reacting with the cleaning gas activated by the discharge energy.However, in that case, cleaning unevenness occurs in the reaction vessel, causing The fine powder after the reaction remains. Then, it takes time to remove such remaining fine powder, which results in an increase in gas consumption and power consumption. To solve this problem, we attempted to increase the concentration of the cleaning gas to make the cleaning uniform. However, simply increasing the concentration caused the deposited film or powder to react with the cleaning gas. The amount of the fine powder remaining in the container increased, which was an adverse effect. On the other hand, on the contrary, an attempt was made to lower the concentration of the cleaning gas. However, if only the concentration of the cleaning gas was lowered, although a gentle reaction was performed, the cleaning speed was reduced and the tact was increased, so that practical use was not possible. These were unsuitable, and none of them could be a means for solving the occurrence of uneven cleaning.

Accordingly, the present inventors have made intensive studies on an efficient and more stable treatment method. When supplying a cleaning gas and high-frequency power into the reaction vessel and performing the cleaning process, the cleaning gas and the cleaning gas are mixed during the cleaning process. It was confirmed that it is best to temporarily stop supplying the high-frequency power and restart the cleaning process again. This is because the cleaning process can proceed from the start of the cleaning process to the area of the exhaust pipe by lowering the internal pressure in a state where the concentration of the cleaning gas is high, so that the cleaning process time can be reduced and the reaction vessel can be reduced. Within, a gentle reaction can be promoted without lowering the concentration of the cleaning gas to reduce uneven cleaning and to remove fine powder, that is, fine powder remaining in a place that could not be easily removed due to uneven cleaning in a short time. It is considered that it can be removed. It was also confirmed that it is best to temporarily stop the supply of the cleaning gas and the high-frequency power during the cleaning process and restart the cleaning process again. This is because, by temporarily stopping the cleaning process in the middle, a gentle reaction can be promoted by the cleaning gas remaining in the reaction container before restarting the cleaning process again, thereby reducing cleaning unevenness. Further, it is considered that the fine powder, that is, the fine powder remaining at a place where it was not easily removed due to uneven cleaning can be removed in a short time. Also,
At that time, it was found that a quick reaction was promoted by restarting the cleaning process having a different concentration, thereby shortening the cleaning process time.

Further, according to the method for manufacturing an article of the present invention,
Since the reaction container can be efficiently cleaned between the deposited film forming steps, the performance of the article can be stabilized and the cost can be reduced.

Hereinafter, the present invention will be described in more detail with reference to the drawings. FIG. 1 is a schematic cross-sectional view showing one configuration example of a deposition film forming apparatus for an electrophotographic photosensitive member according to the present embodiment. In FIG. 1, the deposited film forming apparatus has a reaction container unit 1001 and an exhaust unit 1002. A substrate holder 108 is provided in a reaction vessel 101 which is a vacuum vessel.
A supporting portion of the cylindrical base 102 held by the heater, a heater 103 for heating the base, and a raw material gas introduction pipe 104 are installed, and a high-frequency power supply 105 is connected to the reaction vessel 101 via a matching BOX (not shown).

The substrate heating heater 103 is located within the inner wall of the cylindrical substrate 102 when the cylindrical substrate 102 is accommodated in the reaction vessel, and the heater 103 is controlled by the cylindrical substrate 102 during discharge. Because it is covered, direct contact with the discharge can be prevented.

The high-frequency power supply 105 has a power in a frequency band arbitrarily set in an RF frequency band, a VHF frequency band, a UHF frequency band, or a frequency band including at least two frequency bands. Can be supplied.

The reaction vessel unit 1001 and the exhaust unit 1002 are connected by a base plate 106 on the reaction vessel unit side and an exhaust pipe 111 on the exhaust unit side. These may be configured to be separable and separable.

When the cleaning gas is supplied into the reaction vessel from the gas introduction pipe 104, the cleaning gas flows from the reaction vessel to the lower side of the reaction vessel provided with the exhaust pipe by the exhaust means. Then, the cleaning gas enters the exhaust pipe from the reaction container unit, and the exhaust pipe, that is, the exhaust unit is cleaned next.

Of course, it does not mean that the cleaning process is not performed at all in the exhaust unit while the cleaning process is performed in the reaction container unit.
Also, while the exhaust unit is being cleaned, it does not mean that the reaction unit has not been cleaned at all. In other words, the fact that the deposited film forming apparatus is cleaned means that the reaction container unit is mainly cleaned first, and then the exhaust unit is mainly cleaned.

The raw material gas for the electrophotographic photosensitive member is supplied from the mass flow controller 109 to the raw material gas inflow valve 11.
0 is connected to a gas introduction pipe 104 in the reaction vessel 101. Further, ClF ₃ for cleaning, an inert gas, and the like are also connected to the gas introduction pipe 104 in the reaction vessel 101 through the mass flow controller 109 and the source gas inflow valve 110.

The formation and cleaning of the deposited film using this apparatus can be performed, for example, as follows. First, the cylindrical substrate 102 held by the substrate holder 108 is installed in the reaction vessel 101 via the gate valve 107, and an exhaust device (mechanical booster pump 115-1, Rotary pump 115-2, oil cleaner 115-
The inside of the reaction vessel 101 is evacuated according to 3). Subsequently, the temperature of the cylindrical base 102 is controlled to a predetermined temperature of 20 ° C. to 400 ° C. by the base heater 103, the temperature monitor 116 of the base heater, and a temperature controller (not shown). When the temperature of the cylindrical substrate 102 reaches a desired temperature, a predetermined raw material gas is introduced into the reaction vessel 101 through the gas introduction pipe 104.

Next, the mass flow controller 109 adjusts each raw material gas so as to have a predetermined flow rate. At that time, the exhaust device is adjusted so that the internal pressure of the reaction vessel 101 becomes a predetermined pressure of 133 Pa or less. When the internal pressure becomes stable, electric power is introduced into the reaction vessel 101 from the high-frequency power supply 105 through a matching box (not shown),
Generates glow discharge. The source gas introduced into the reaction vessel is decomposed by the discharge energy, and a deposited film mainly containing predetermined silicon is formed on the cylindrical substrate 102. To achieve uniform film formation,
During the film formation, the cylindrical substrate 102 is rotated at a predetermined speed by a driving device (not shown).

The cleaning process of the apparatus is performed as follows. First, after the deposited film is formed, the formed electrophotographic photoreceptor is taken out of the reaction container 101, and then a cleaning substrate for protecting the substrate heating heater 103 is put in place of the cylindrical substrate (not shown). Then, the gas introduction pipe 10 is exhausted by the exhaust devices 115-1 to 115-3.
The inside of the reaction vessel 101 including the chamber 2 is evacuated to a predetermined pressure. Subsequently, the cleaning gas is adjusted by the mass flow controller 109 so that the cleaning gas has a desired flow rate, and is introduced into the reaction vessel 101 through the raw material gas introduction pipe 104. When the internal pressure is stabilized or reaches a predetermined internal pressure, electric power is introduced into the reaction vessel 101 from the high-frequency power supply 105 through a matching box (not shown) to generate glow discharge. The cleaning energy introduced into the reaction vessel is decomposed by the discharge energy, and the by-products in the reaction vessel 101 including the gas introduction pipe 102 and the exhaust pipe 111 are cleaned.

In the present invention, for example, in this cleaning process, the supply of the high-frequency power 105 and the cleaning gas is temporarily stopped during the cleaning process, and a stepwise cleaning process in which the concentration of the cleaning gas is changed is performed. You can do so. that time,
The timing of stopping the supply of the high-frequency power 105 and the cleaning gas is determined by the temperature monitor 1 installed at each point of the apparatus.
17-1 to 117-2 and / or the internal pressure detecting means 113. The temperature monitor is provided at a location where information for determining the timing of stopping or starting the cleaning process is easily obtained, and the location and number of the temperature monitor may be determined as appropriate. For example, the temperature monitor 117-1 can be provided in the middle of the path of the exhaust pipe 111. Further, by providing the temperature monitor 117-1 at a position close to the reaction vessel unit, it is possible to grasp not only the etching state of the exhaust pipe but also the etching state of the reaction vessel unit by observing the temperature change from the temperature monitor. .

The temperature monitor 117-2 can be provided in an exhaust device 115-2 which is a rotary pump. Temperature monitor 117-
By providing 1, it is possible to directly or indirectly observe a change in temperature in the exhaust path, and also to observe directly or indirectly the temperature of the exhaust device.

When the cleaning gas removes unnecessary substances by etching, the temperature rises. If a temperature monitor 117-1 is provided in the path of the exhaust pipe and the manner in which the temperature in the exhaust pipe changes is observed, when the temperature rises, it is said that unnecessary substances have been removed by etching in the exhaust pipe. From this, it can be determined that the cleaning process in the reaction vessel unit is almost completed while the temperature in the exhaust pipe is changing, for example.

Further, by providing the exhaust device 115-2 on the rotary pump 111, it is possible to observe a rise in the temperature inside the rotary pump. Since the temperature rise in the rotary pump can be observed, it is possible to prevent the temperature of the rotary pump from rising more than necessary.

The rise in the temperature inside the rotary pump means that solid undesired substances existing in the exhaust pipe on the upstream side are removed, and solid unnecessary matters near the rotary pump on the downstream side are removed by etching. It suggests that.

Therefore, both temperature monitors 117-1 and 117 are used.
By observing the temperature change of each of -2, it becomes easy to grasp the etching removal state of the solid unnecessary matter in the reaction vessel unit and the etching removal state of the solid unnecessary matter in the exhaust pipe.
As a result, unnecessary gas introduction and processing time can be reduced, so that the total cleaning processing time can be reduced and processing cost can be reduced. Also, in the stepwise cleaning process, the oil of the exhaust device 115-2 is removed via the oil cleaner 115-3.
It is preferable to reduce the load on the exhaust pump by showering to the exhaust pipe on the upstream side for protection of the exhaust gas.

In the present invention, examples of the cleaning gas used include CF ₄ , CF ₄ / O ₂ , SF ₆ , and ClF ₃ (chlorine trifluoride).
ClF ₃ is effective. Further, in the present invention, the concentration can be adjusted by using an inert gas for dilution in order to adjust the concentration of the cleaning gas. Examples of the inert gas to be introduced include He, Ne, and Ar, and it is preferable to use Ar. In the present invention, if the concentration of the cleaning gas is too low, the cleaning effect is weakened. Conversely, if the concentration is too high, the reaction is abrupt and the load on a device such as a pump is increased. Is preferably 10% or more and 70% or less. In the present invention, it is preferable to perform the cleaning process by changing the concentration of the cleaning gas.

In the present invention, the effect of the pressure in the discharge space during the cleaning process was observed in any region, but the discharge stability and the discharge pressure were particularly increased at 20 Pa or more and 200 Pa or less, preferably 50 Pa or more and 120 Pa or less. Particularly good results in terms of cleaning properties can be obtained with good reproducibility.

In the present invention, when performing a cleaning process in the exhaust pipe and the exhaust device for reducing the pressure inside the reaction vessel, the oil of the exhaust device is also used to reduce the load on the exhaust device. It is preferable to blow it to the intake port of the exhaust pipe.

In the present invention, the timing for temporarily stopping the cleaning gas and the high frequency power is preferably determined by a temperature monitor installed in the deposited film forming apparatus and / or a pressure in the deposited film forming apparatus. . In the present invention, the processing time in each step may be set in advance based on the determination result, and the cleaning processing may be performed based on the set time. Further, when using the cleaning method according to the present invention, after performing a certain amount of cleaning processing in the deposited film forming apparatus, the cleaning gas and the high-frequency power as described above are stopped, and then the reaction container unit is set to the above-described state. The cleaning processing may be performed again by installing the apparatus in a place different from the deposited film forming apparatus. As described above, the cleaning process may be performed at different places with a time difference.

That is, in the present invention, both the reaction container unit and the exhaust unit can be cleaned at one time. However, the cleaning process can be performed by separating the reaction container unit from the exhaust unit. It can be done individually.

For example, when only one of the reaction container unit and the exhaust unit requires cleaning, only the one to be cleaned is cleaned, and the other is cleaned to the side that does not need cleaning. Since the deposited film forming process can be performed using the deposited film forming apparatus in which the substitute is integrated, the operation efficiency of forming the deposited film on the substrate can be improved. In particular, when cleaning only inside the reaction container, only the reaction container can be separately removed from the production apparatus for processing. In this case, since the exhaust for cleaning performed separately does not directly affect production, the control system can be simplified.

In the cleaning process of the present invention, the power supply and the supply of the etching gas are stopped during the cleaning process. However, after the power supply and the supply of the etching gas are stopped, the reaction vessel unit and the exhaust device are stopped. The units can be separated from each other, and at least one of the units can be cleaned again. An example of the method is shown below.

First, after the cleaning process has been performed to remove almost completely the solid undesired substances, or after the solid undesired substances have been removed to a level at which there is no problem with safety, the reaction vessel unit is removed from the exhaust unit. At least one of them is further subjected to dry etching (cleaning).

The second is a method in which the reaction vessel unit is almost completely dry-etched by a cleaning process, then the two units are separated, and only the exhaust unit is continuously dry-etched by a cleaning process.

As described above, at the time when the cleaning of either the reaction vessel unit or the exhaust unit is completed, the reaction vessel is moved to a different place from the deposition film forming apparatus or to the same place. It is effective to restart one of the cleaning processes. Further, in the present invention, the shape of the substrate may have any shape, but a cylindrical shape is particularly optimal. The size of the substrate is not particularly limited, but practically, the diameter is preferably 20 mm or more and 500 mm or less, and the length is 10 mm or more and 1000 mm or less.

According to the present invention, it is used when forming a deposited film.
The source gas used is silane (SiH_Four), Disilane
(Si_TwoH₆), Silicon tetrafluoride (SiF_Four), Disilicon hexafluoride
(Si _TwoF₆) And other amorphous silicon forming gas
Is also effective using a mixed gas thereof. With dilution gas
Hydrogen (H_Two), Argon (Ar), helium (H
It is also effective to use e). Also, the band gap of the deposited film
Nitrogen (N
_Two), Ammonia (NH_Three) And other elements containing nitrogen atoms, acids
Element (O_Two), Nitric oxide (NO), nitrogen dioxide (N
O_Two), Nitrous oxide (N _TwoO), carbon monoxide (CO),
Carbon oxide (CO_Two) Such as methane (C)
H_Four), Ethane (C_TwoH₆), Ethylene (C_TwoH_Four), Ase
Cylene (C_TwoH_Two), Propane (C_ThreeH₈) And other hydrocarbons,
Germanium tetrafluoride (GeF_Four), Nitrogen fluoride (NF_Three)etc
It is effective to use together fluorine compounds or their mixed gas
It is. For the purpose of doping, diborane (B_Two
H₆), Boron fluoride (BF_Three), Phosphine (PH_Three)
May be introduced into the discharge space at the same time.
No.

In the electrophotographic photosensitive member produced according to the present invention, the total thickness of the deposited film deposited on the substrate is appropriately determined depending on the required characteristics and the like. However, the film has a thickness of 5 μm or more and 100 μm or less, more preferably 10 μm or more and 7 μm or more.
It is preferably at most 0 μm, more preferably at least 15 μm and at most 50 μm, whereby a particularly good image as an electrophotographic photosensitive member can be obtained at low cost.

The electrophotographic photoreceptor of the present invention is produced by appropriately setting the pressure in the discharge space during the deposition of the deposited film, but is preferably 0.06 Pa or more and 13.3 Pa or less, more preferably 0.1 Pa or less. By setting the pressure to 133 Pa or more and 6.65 Pa or less, particularly good results can be obtained with good reproducibility in terms of discharge stability and uniformity of the deposited film. The substrate temperature during the deposition of the deposited film is preferably 100 ° C. or more and 500 ° C. or less, more preferably 150 ° C. or more and 450 ° C. or less, further preferably 200 ° C. or more and 400 ° C. or less, and most preferably 250 ° C. As described above, the temperature is desirably 350 ° C. or lower.

As the means for heating the substrate, most heating means can be used as long as they are heating elements of a vacuum specification. More specifically, an electric resistance heating element such as a winding heater of a sheath-shaped heater, a plate-shaped heater, or a ceramic heater, a heat radiation lamp heating element such as a halogen lamp or an infrared lamp, a liquid, or a gas is used as a heating medium by a heat exchange means. A heating element; As the surface material of the heating means, metals such as stainless steel, nickel, aluminum, and copper, ceramics, heat-resistant polymer resins, and the like can be used. In addition, other methods such as providing a dedicated heating vessel separately from the reaction vessel, heating, and then transporting the substrate into the reaction vessel in a vacuum can be used. It is possible in the present invention to use the above means alone or in combination.

In the cleaning process of the present invention, in addition to cleaning the deposited film forming apparatus on which the deposited film forming step has been performed, for example, a so-called first deposited film forming apparatus in which the deposited film forming step has never been performed. It may be performed during driving.

The step of forming a deposited film in the present invention means that a substrate to be processed is accommodated in a deposited film forming apparatus, a deposited film is formed on the substrate, and the substrate on which the deposited film is formed is deposited. One-step process of taking out of the device (film formation cycle)
Or a step of repeating the first step (film forming cycle) a plurality of times, that is, storing a substrate in a deposition film forming apparatus and forming a deposition film on the substrate,
Then, the substrate on which the deposited film is formed is taken out of the deposited film forming apparatus, then another substrate is accommodated in the deposited film forming apparatus, and after the deposited film is formed on the substrate, the substrate is taken out of the deposited film forming apparatus. The process may be such that a plurality of cycles of film formation are performed.

[0057]

EXAMPLES Examples of the present invention will be described below, but the present invention is not limited to these examples. [Embodiment 1] In Embodiment 1, a diameter 108 m of aluminum was used by using the deposition film forming apparatus shown in FIG.
An amorphous silicon deposited film was formed on a cylindrical substrate having a length of 358 mm, a length of 358 mm, and a thickness of 5 mm under the conditions shown in Table 1 to repeatedly form a blocking type electrophotographic photosensitive member having a layer configuration shown in FIG. The cleaning process in the reaction vessel was performed under the cleaning conditions shown in Table 2. In FIG. 2, 205 is a conductive substrate, 204 is a charge injection blocking layer (first layer), 203 (second layer), 202 (third layer) are photoconductive layers having different compositions, and 201 is surface protection. Each layer (fourth layer) is shown.

In the cleaning process, (ClF ₃ + A
r) The timing for stopping the gas and the high frequency power was changed at each point shown in FIG. When restarting the cleaning process, (ClF ₃ + Ar) gas was introduced into the reaction vessel, and after confirming that the internal pressure was stabilized, high-frequency power was supplied to start the cleaning process. At the same time, the rotary pump, which is a part of the exhaust device, was showered.

In this embodiment, (ClF ₃
+ Ar) The timing of stopping the gas and the high frequency power will be described with reference to FIG. The graph of FIG. 3 is a graph showing the timing at which the cleaning gas and the high frequency power are stopped, and the horizontal axis (X axis) represents time. The internal pressure of the apparatus rises on the way as shown. Although the reason is not clear, the cleaning gas reacts with the solid undesired substances, and the internal pressure rises as a result of generating gaseous products.When the solid undesired substances can be removed, the internal pressure returns to the original internal pressure value and becomes constant again. Conceivable.

The temperature sensor represents a temperature change of the temperature sensor 117-1 in FIG. 1, and the graph of the temperature sensor also rises on the way. Although this phenomenon is speculation, it is considered that this is due to strong reaction with unnecessary solid matter in the vicinity of the reaction vessel unit in the cleaning gas reaction vessel unit or the exhaust device unit, and etching and removal. Then, it is considered that the temperature decreases after the solid unnecessary substances can be removed. The temperature sensor indicates a temperature change of the temperature sensor 117-2 in FIG. 1, and the graph of the temperature sensor also rises on the way. Although this phenomenon is speculation, the reaction of the cleaning gas in the reaction vessel is completed or almost completed, and the cleaning gas strongly reacts with the solid unnecessary matter near the exhaust device 115-2, and the unnecessary matter is removed by etching. It is thought that it is. Then, it is considered that the temperature decreases after the solid unnecessary substances can be removed.

The points provide information for determining the timing at which the supply of power and the supply of cleaning gas are stopped. That is,
These points provide information for deciding the timing when the above-described mild reaction is started by stopping the reaction for strongly removing unnecessary substances by performing the plasma discharge. More specifically, the step of stopping the discharge during the time indicated by the X axis in FIG. 3 is performed twice. That is, a step of performing a cleaning process by first supplying power and a cleaning gas (step a), and then performing a cleaning process by a gentle reaction by stopping power supply or power supply and supply of the cleaning gas. (B step),
Next, a step of performing a cleaning process by supplying power and a cleaning gas again (step c), and a step of performing a cleaning process by a gentle reaction by stopping power supply or power supply and supply of the cleaning gas again (step d) ) Is performed.

The timing used as a reference when determining the timing for starting the step b is a point or a period between the points. The timing that is used as reference when determining the timing to start the d step is a point or a period between the points. Of course, the starting point of each step can be adjusted according to the situation, without being limited to the period between the points. The point does not need to be the exact timing of starting the step b or the step d. A preferable point for each step may be appropriately selected from the respective points, and the timing for starting the step b or the step d may be specifically determined based on the timing of the selected point. Of course, select the preferred points as appropriate from each point,
The timing itself may be used as the start timing of the step b or the step d.

FIG. 3 shows the timing at which the step a starts, and FIG.
The timing at which the process ends and the process c starts, or a point which is used as a reference when determining the timing, is not shown. The timing of starting the step c may be, for example, after a predetermined time arbitrarily set from the start of the step b, or after an arbitrarily set constant temperature change. It is convenient and convenient to set the time (period) of the step b in advance so that the timing of starting the step c is after a desired time has elapsed from the start of the step b.

The point is a point in time when the internal pressure of the apparatus is at a peak or in the vicinity thereof. It is presumed that at this peak, the solid undesired substance and the cleaning gas are most frequently reacted.

The point is a point in time or near the point when the internal pressure value of the apparatus has substantially stopped decreasing rapidly, and a point in time or near the point in time when the temperature value indicated by the temperature sensor 117-1 is almost at the peak. It is.

The point is the temperature sensor 117
-1 is a time point when the temperature value indicated by the temperature sensor decreases or is maintained substantially constant after the decrease.
This is the time point when the temperature value indicated by the temperature sensor 17-2 is almost at or near the peak value.

The point is the temperature sensor 117
The temperature value indicated by the temperature sensor of -1 is maintained at a substantially constant value, and the temperature value indicated by the temperature sensor of the temperature sensor 117-2 decreases or is maintained at a substantially constant value after the reduction. Nevertheless, the timing for starting the step d does not need to be determined so severely.

The evaluation of the electrophotographic characteristics of the electrophotographic photosensitive member produced as described above was performed as follows. The process speed of the prepared electrophotographic photoreceptor was set to 20 in advance for experiments.
A Canon copier, NP6060, modified so that it can be changed arbitrarily in the range of 0 to 800 mm / sec, performs corona charging by applying a voltage of 6 to 7 kV to the charger, and performs a normal copying process. An image was formed on a transfer paper, and the electrophotographic properties and image quality were evaluated according to the following procedure. The electrophotographic photoreceptors thus manufactured under the same manufacturing conditions were evaluated, and the results of evaluation of each evaluation item are shown in Table 3. In Table 3, the total cleaning processing time is shown as a relative value when Comparative Example 1 is 100%.

<Evaluation of Appearance> The appearance of the produced electrophotographic photosensitive member was observed, and the presence of defects in the deposited film in which the abnormally grown deposited films were collected was visually confirmed. ◎… “Very good” ○… “Slight and no problem at the point where clear confirmation is difficult” △… “Confirmation is possible but the degree is light” ×… “Clear confirmation and quite large” <Evaluation of scratched flower image> An image sample having the most image defects was selected from among image samples obtained when the entire halftone original and the character original were copied on a platen by changing the process speed, and evaluated. As an evaluation method, the image sample was observed with a magnifying glass, and evaluation was performed based on the state of white spots within the same area. (Image defects spread in the form of streaks (fine spherical projections))…: “Very good” ○: “Some small white spots are present but very small and no problem” △: “Small white spots are present on the entire surface There is no problem in character recognition. × × “Some characters are difficult to read due to many white spots.” <Evaluation of image deletion> Canon test chart consisting of all characters on a white background (part number FY9-9058) ) Is placed on a platen and irradiated with light at twice the normal exposure to make a copy. The image thus obtained was observed, and it was evaluated whether the thin lines on the image were connected without interruption by the following four steps. In addition, when there was unevenness on the image, evaluation was made at the worst part in the entire image area. …: “Very good” ○: “Good” △: “There are many interruptions, but they can be read as characters, and there is no practical problem.” ×: “There are many interruptions, it is difficult to read as characters, and there may be practical problems.”

[0070]

[Table 1]

[0071]

[Table 2]

[0072]

[Table 3] From the above results, good results were obtained by temporarily stopping the supply of the source gas and the high-frequency power during the cleaning process after the sudden change in the internal pressure at the point disappeared.

(Comparative Example 1) C during the cleaning process
An electrophotographic photosensitive member was prepared in the same manner as in Example 1 except that the 1F ₃ gas and the high-frequency power were not stopped, and the results of evaluation by the same method are shown in Table 3 as Comparative Example 1.

[Embodiment 2] In the embodiment 2, the cleaning process and the preparation of the electrophotographic photosensitive member were performed in the same manner as in the embodiment 1 except that the initial stop point was set as the cleaning completion point. And the same evaluation was performed. Table 3 also shows the results.

Example 3 Example 3 is similar to Example 1 except that the concentration of the source gas was changed before and after the stop of the source gas and the high-frequency power during the cleaning process as shown in Table 4. An electrophotographic photosensitive member was prepared and cleaned by the same method, and evaluated by the same method. At the same time, the result of relative comparison when the cost required for cleaning is set to 100% in the comparative example is also shown. Table 5 shows the above results. However, the timing for stopping the source gas and the high-frequency power was the same as in Example 1.

[0076]

[Table 4]

[0077]

[Table 5] As is clear from Table 5, it was confirmed that the effect was obtained by changing the concentration. Example 4 In Example 4, an electrophotographic photosensitive member was prepared and cleaned by the same method as in Example 1 except that the internal pressure was changed as shown in Table 6, and the same method was used. The evaluation and the abnormally grown deposited film on the photoreceptor shown below, that is, the film defect were evaluated. At this time, the comparative example is 100% in cost required for cleaning at the same time.
The results of the relative comparison when “” are also shown. Table 7 shows the above results. However, the timing of stopping the source gas and the high frequency power was performed at points. <Evaluation of Film Defects> The number and size of the deposited films that abnormally grew on the surface of the prepared electrophotographic photosensitive member were observed using an optical microscope, and comparison was made based on the following criteria. ◎ “Very small and good” ○… “There are some but the number is not good and there is no problem” △… “There are a lot of numbers but the size is small and the degree is light” ×… “A lot of numbers and a lot of sizes” large"

[0078]

[Table 6]

[0079]

[Table 7] As is clear from Table 7, it was confirmed that by balancing the internal pressure and the concentration of the cleaning gas, the substantial cleaning processing time could be shortened, and the effect on the gas usage was accordingly brought about. Further, the amount of film defects of the produced electrophotographic photosensitive member could be significantly reduced.

[Embodiment 5] In Embodiment 5, Embodiment 3
When the time required for the temperature of the temperature sensor shown in FIG. 3 to reach a peak when the cleaning process was performed in the same manner as in Example 1 was set to 100% in Comparative Example 1, a comparison was made between Example 3 and Comparative Example 1.

[0081]

[Table 8] As is clear from Table 8, by balancing the internal pressure and the concentration of the cleaning gas, the cleaning process could be efficiently performed up to the exhaust pipe.

[Embodiment 6] In Embodiment 6, (Cl
F ₃ + Ar) except that the timing of stopping the gas and the high frequency power was determined by the processing time required up to the point.
A cleaning process was performed in the same manner as in Example 1. When the deposited film thus produced was evaluated in the same manner as in Example 1, similar good results were obtained.

[Embodiment 7] In Embodiment 7, (Cl
F ₃ + Ar) except that the timing of stopping the gas and the high frequency power was determined by the processing time required up to the point.
A cleaning process was performed in the same manner as in Example 1. When the deposited film thus produced was evaluated in the same manner as in Example 1, similar good results were obtained.

Example 8 In Example 8, the cleaning process was performed in the same manner as in Example 1 except that the electrophotographic photosensitive member was repeatedly produced under the conditions shown in Table 9 using the VHFPCVD apparatus shown in FIG. Was carried out. 4 in FIG.
01 is a reaction vessel, 402 is a conductive substrate, 403 is a heater, 404 is a VHF electrode / gas introduction tube, 405 is a mass flow controller, 406 is a discharge space, and 408 is a driving device. When the deposited film thus produced was evaluated in the same manner as in Example 1, very good results were obtained.

[0085]

[Table 9]

[0086]

As described above, according to the present invention, during the cleaning process, the supply of high frequency power, preferably the supply of the cleaning gas, is temporarily stopped during the cleaning process, and then the cleaning process is performed again. By restarting the cleaning process, by-products in the reaction vessel can be efficiently removed, and a high-quality deposited film, particularly a high-quality electrophotographic photoreceptor, can be stably obtained. Becomes When restarting the cleaning process,
By restarting the cleaning process while changing the concentration, it is possible to promote a quick reaction and perform a more efficient cleaning process.

[Brief description of the drawings]

FIG. 1 is a schematic sectional view showing an example of a deposited film forming apparatus to which the present invention can be applied.

FIG. 2 is a schematic cross-sectional view illustrating a configuration example of a light receiving member for electrophotography.

FIG. 3 is a diagram illustrating an example of a stop point of a cleaning gas and high-frequency power.

FIG. 4 is a schematic configuration diagram for explaining a reaction vessel of a deposition film manufacturing apparatus using a VHF wave band for high-frequency power.

[Explanation of symbols]

 101, 401: reaction vessels 102, 201, 402: conductive substrate 103, 403: heater 104: source gas introduction tube 404: VHF electrode / source gas introduction tube 105: high frequency power supply 405, 109: mass flow controller 106: base plate 406 : Discharge space 107: Gate valve 108: Conductive substrate holder 408: Driving device 110: Source gas inflow valve 111: Exhaust pipe 112: Leak valve 113: Baratron 114: Exhaust valve 115-1 to 115-3: Exhaust device 116: Substrate heating temperature sensor 117-1 to 117-2: temperature sensor, 1001: reaction vessel unit 1002: exhaust unit

 ──────────────────────────────────────────────────続 き Continuing on the front page (72) Tetsuya Karaki, Inventor 3-30-2 Shimomaruko, Ota-ku, Tokyo Inside Canon Inc. (72) Inventor Hideaki Matsuoka 3-30-2 Shimomaruko, Ota-ku, Tokyo Canon (72) Inventor Koji Hitsuishi 3-30-2 Shimomaruko, Ota-ku, Tokyo F-term in Canon Inc. (reference) 2H068 EA21 EA24 EA26 EA27 4K030 AA06 AA10 AA17 AA24 BA30 CA02 CA16 DA06 KA30 LA17 5F004 AA15 AA16 BB13 CA08 CA09 DA00 DA01 DA18 DA23 DA26 DB02 EA28 5F045 AA08 AB04 AC01 AC02 AC16 AC17 AD05 AD06 AD07 AD08 AD09 AE13 AE15 AE17 AE19 AF10 BB08 BB14 CA16 DP25 EB06 EE11 EE14 EH12 EH19

Claims (24)

[Claims] 1. A cleaning method for a deposition film forming apparatus for cleaning a deposition film forming apparatus for forming a deposition film on a substrate disposed in a reaction vessel capable of reducing pressure using a cleaning gas and high frequency power. In the cleaning process, after temporarily stopping the supply of the high-frequency power during the cleaning process,
A cleaning method for a deposited film forming apparatus, comprising a cleaning process for restarting the supply of high frequency power. 2. The deposited film according to claim 1, wherein the cleaning process includes a cleaning process by a gentle reaction of a cleaning gas in the deposition film forming apparatus when the supply of the high-frequency power is stopped. A cleaning method for a forming apparatus. 3. The cleaning gas according to claim 1, wherein the concentration of the cleaning gas used in restarting the cleaning process is different from the concentration of the cleaning gas used in the cleaning process before restarting. Cleaning method for a deposited film forming apparatus. 4. The cleaning method according to claim 1, wherein the cleaning gas is a mixture of ClF ₃ and an inert gas. 5. The cleaning method according to claim 4, wherein the inert gas is Ar. 6. The cleaning process, wherein the timing for stopping the supply of the high-frequency power is determined based on a result of detecting a temperature or a pressure in the deposition film forming apparatus. Claims 1-5
The cleaning method of the deposited film forming apparatus according to any one of the above. 7. The cleaning process according to claim 1, further comprising a period during which the supply of the cleaning gas is temporarily stopped during the cleaning process.
The cleaning method of the deposited film forming apparatus according to any one of the above. 8. A period in which the supply of the cleaning gas is temporarily stopped is included in a period in which the supply of the high-frequency power is temporarily stopped.
3. The cleaning method for a deposited film forming apparatus according to item 1. 9. The deposited film forming apparatus according to claim 7, wherein the period during which the supply of the cleaning gas is temporarily stopped is a period during which the supply of the high-frequency power is temporarily stopped. Cleaning treatment method. 10. The deposition according to claim 7, wherein the temporary stop and restart of the supply of the cleaning gas are performed in accordance with the temporary stop and restart of the supply of the high-frequency power. A cleaning method for a film forming apparatus. 11. The deposited film forming apparatus according to claim 7, wherein a period during which the supply of the cleaning gas is temporarily stopped is determined based on a temperature or a pressure in the deposited film forming apparatus. Cleaning treatment method. 12. In the course of the cleaning process,
After temporarily stopping the supply of the cleaning gas and the high-frequency power, the reaction vessel unit constituting a part of the deposited film forming apparatus is moved to a different place from the deposited film forming apparatus, and the reaction is stopped. 8. The method according to claim 7, further comprising restarting the cleaning process on the container unit at the same time as or with a time difference from the deposited film forming apparatus, and cleaning the container units. 13. In the cleaning process, the timing for stopping the supply of the high-frequency power is determined based on the detected result by detecting the temperature or pressure in the deposition film forming apparatus, and based on the detected result. In advance, the processing time until the temporary stop is set in advance,
12. The cleaning method according to claim 1, wherein the cleaning process is performed based on the set time. 14. The cleaning process according to claim 1, wherein the cleaning process is performed by supplying the cleaning gas into the reaction vessel, setting the internal pressure to a predetermined value, and then supplying the high-frequency power. 2. The method for cleaning a deposited film forming apparatus according to claim 1. 15. The cleaning of the deposited film forming apparatus according to claim 1, wherein the cleaning process is performed while reducing a load on an exhaust device for exhausting the inside of the reaction vessel. Processing method. 16. A cleaning method for a deposition film forming apparatus for cleaning the interior of a deposition film forming apparatus for forming a deposited film on a substrate disposed in a reaction vessel capable of reducing pressure using a cleaning gas and high frequency power. In the cleaning process, the cleaning process includes at least a first process and a second process, and the concentration of the cleaning gas in the first process is equal to the concentration of the cleaning gas in the second process. Higher than the first
A cleaning method for a deposited film forming apparatus, wherein the internal pressure in the step is lower than the internal pressure in the second step. 17. The cleaning process includes temporarily stopping the supply of the cleaning gas and the high-frequency power between the first step and the second step, and changing the concentration of the cleaning gas in each step. 17. The cleaning method according to claim 16, wherein the cleaning process is started later. 18. A dry etching method for a vacuum processing apparatus, comprising: a first dry etching processing step of supplying high-frequency power and a gas for dry etching under reduced pressure to dry-etch unnecessary solid substances present in the vacuum processing apparatus; A second dry etching step of stopping the supply of the high-frequency power to stop the first dry etching step, and dry-etching the unnecessary solid matter with the first dry etching step stopped; A third dry etching step of stopping the second dry etching step by supplying electric power and a gas for dry etching to dry-etch the solid unnecessary matter present in the vacuum processing apparatus. Dry etching method. 19. The dry etching method according to claim 18, wherein in the second dry etching process, the supply of the second dry etching gas is stopped. 20. A method for cleaning a deposited film forming apparatus according to any one of claims 1 to 17, and a dry etching method according to any one of claims 18 to 19. A method for producing an article, comprising the steps of: 21. The method according to claim 20, wherein the article includes a light receiving member for electrophotography. 22. A step of disposing a substrate in a reaction vessel, forming a deposited film on the substrate, forming a deposited film by the deposited film forming step, and then removing the substrate from the reaction vessel. First, a cleaning process for supplying the cleaning gas and the high-frequency power to the reaction container, a second cleaning process for stopping the supply of the high-frequency power, and a third cleaning process for supplying the cleaning gas and the high-frequency power to the reaction vessel.
A cleaning treatment step of performing each treatment of the cleaning treatment in the order described above, and after the cleaning treatment step, forming a deposited film on another substrate by the deposited film forming step. . 23. In the second cleaning process,
The method for manufacturing an article according to claim 22, wherein the supply of the cleaning gas is stopped. 24. The method according to claim 22, wherein the article includes a light receiving member for electrophotography.