JP2002080972A - Plasma treatment process and plasma treatment system - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a plasma treatment process and a plasma treatment system by which plasma treatment extremely excellent in productivity can be realized with small equipment investment by increasing the working ratio of equipment and further improving operability. SOLUTION: In this plasma treatment process in which plasma treatment is performed to a substrate arranged in a reaction vessel, after the completion of the plasma treatment to the substrate, the inside of the reaction vessel is charged with a cooling gas under the pressure of 100-100,000 Pa, and the substrate is subjected to cooling treatment.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a plasma processing method and a plasma processing apparatus, and more particularly to a plasma processing method, such as a photoreceptive member for electrophotography, a solar cell, a line sensor for image input, an imaging device, a TFT, etc. The present invention relates to an apparatus and a method for forming a deposited film particularly suitable for forming a deposited film as a semiconductor element, or a plasma processing apparatus and a processing method such as an etching apparatus and a method for a semiconductor device.

[0002]

2. Description of the Related Art There are various methods for plasma processing used in semiconductors and the like according to their respective applications. For example, various devices and methods utilizing characteristics of plasma, such as formation of an oxide film, a nitride film, and an amorphous silicon-based semiconductor film using a plasma CVD method, or fine processing technology by etching, are used. Further, in recent years, demands for improving film quality and processing capacity have become stronger, and various devices have been studied. In particular, a plasma process using high-frequency power is widely used because of its advantages such as discharge stability and application to dielectric materials such as oxide films and nitride films.

An amorphous silicon film formed by this method using silane gas (SiH ₄ ) as a film forming source gas has relatively few localized levels in the forbidden band of amorphous silicon, and valence electrons can be controlled by doping impurities. It has been studied that an amorphous silicon electrophotographic photoreceptor is possible and has excellent characteristics. Japanese Patent Publication No. 60-35059 discloses a light receiving member for electrophotography in which hydrogenated amorphous silicon is applied to a photoconductive portion.

Further, there is a demand for shortening the dead time and improving the equipment operation rate while coping with multi-kind production. Japanese Patent Application Laid-Open No. H10-168576 discloses a plasma processing apparatus and method capable of coping with multi-product production and reducing the dead time by adopting a structure in which a vacuum device can be freely moved. .

[0005]

However, by using the plasma processing apparatus or the processing method as described above, that is, by using a freely movable vacuum apparatus, multi-product production can be easily achieved, Although the time can be shortened, there is still room for improvement in order to further increase production efficiency and obtain higher quality deposited films and semiconductor devices.

For example, in a plasma processing apparatus, gas facilities such as a gas supply unit and a gas exhaust unit, power supply facilities, and the like are expensive, so it is necessary to reduce the investment amount of these facilities and increase the operation rate. It is required to realize a certain cost reduction, and although the plasma processing method or the processing apparatus described above is considerably improved, the reaction vessel used for the plasma processing is also generally a vacuum apparatus,
The capital investment is similarly high, and it is desired to minimize the number of required reaction vessels in order to realize cost reduction. In addition, in order to obtain stable quality, the easiness of work when handling the reaction vessel is an important factor that leads to improvement in workability and, consequently, improvement in productivity. Therefore, further improvement of these is desired. .

Therefore, the present invention solves the above-mentioned problems, improves the operation rate of the equipment, and improves the workability, thereby providing a high-quality plasma treatment with extremely excellent productivity.
It is another object of the present invention to provide a plasma processing method and a plasma processing apparatus that can be realized with a small capital investment.

[0008]

SUMMARY OF THE INVENTION The present invention provides a plasma processing method and a plasma processing apparatus configured as described in the following (1) to (16) in order to achieve the above object. (1) a reaction vessel for forming a plasma, a reaction gas supply unit for supplying a reaction gas into the reaction vessel, and a gas exhaust unit for exhausting the inside of the reaction vessel; And a plasma processing method for decomposing the reaction gas by the discharge power introduced into the reaction vessel and performing plasma processing on the substrate disposed in the reaction vessel, after the plasma processing on the substrate is completed. And 100 to 100,000 Pa of cooling gas in the reaction vessel.
A plasma treatment method, wherein the substrate is filled with the above pressure and the substrate is cooled. (2) The plasma processing method according to (1), wherein the cooling gas filled in the reaction vessel is hydrogen and / or helium. (3) The plasma processing method according to the above (1) or (2), wherein the processing is performed by separating the reaction container from the reaction gas supply unit and the gas exhaust unit. (4) The method according to (3), wherein the reaction vessel is cut off from the reaction gas supply section and the gas exhaust section, and then the reaction vessel is filled with a cooling gas and the substrate is cooled. The plasma processing method as described above. (5) The plasma processing method according to any one of (1) to (4), wherein the outer peripheral surface of the reaction vessel filled with the cooling gas is cooled by a gas and / or a liquid. (6) Any of the above (1) to (5), wherein the cooling gas filled in the reaction vessel is filled in the reaction vessel from a supply section different from the reaction gas supply section. A plasma processing method according to any one of the above. (7) The plasma processing method according to any one of (1) to (6), wherein a cylindrical substrate is used as the substrate, and a plurality of the cylindrical substrates are arranged in the reaction vessel. (8) The plasma processing method according to any one of (1) to (7) above, wherein the plasma processing method is a method for forming an electrophotographic photosensitive member. (9) A reaction vessel for forming plasma, a reaction gas supply unit for supplying a reaction gas into the reaction vessel, an electrode for introducing discharge power into the reaction vessel, and an exhaust for the inside of the reaction vessel. In a plasma processing apparatus comprising: a gas exhaust unit; a substrate disposed in the reaction vessel; and a plasma treatment performed on the substrate by decomposing the reaction gas by the discharge power. A cooling gas supply unit for introducing a cooling gas after completion of the process. (10) The plasma processing apparatus according to (9), wherein the cooling gas supply unit is configured by a supply unit different from the reaction gas supply unit. (11) The plasma processing apparatus according to (9) or (10), wherein the cooling gas supply unit is a supply unit of hydrogen and / or helium. (12) The plasma processing apparatus according to any one of (9) to (11), wherein the reaction container is configured to be detachable from the reaction gas supply unit and the gas exhaust unit. (13) The plasma processing apparatus according to any one of (9) to (12), wherein the reaction vessel is provided with a cooling mechanism for cooling an outer peripheral surface of the reaction vessel. (14) The plasma processing apparatus according to the above (13), wherein the cooling mechanism is a cooling mechanism using air cooling and / or water cooling. (15) The plasma processing apparatus according to any one of (9) to (14), wherein the substrate is a cylindrical substrate, and a plurality of the cylindrical substrates are arranged in the reaction vessel. (16) The plasma processing apparatus according to any one of the above (9) to (15), wherein the plasma processing apparatus is an electrophotographic photoreceptor forming apparatus.

[0009]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS With the above-described structure, the facility operation rate is improved, and the workability is also improved, thereby realizing high quality plasma processing with excellent productivity and with a small capital investment. This is based on the following findings of the present inventors.
That is, although there is essentially no involvement in the plasma treatment, there is a process in which the base is cooled in a process that requires time in the plasma treatment process. By performing this cooling process under certain conditions, it is possible to greatly reduce the time required for the cooling process, not only to increase production efficiency, but also to contribute to production stability. It was found that it was a practical solution.

Hereinafter, this will be described in more detail. As described above, in order to increase the production efficiency, that is, to increase the number of production units per unit time, a method of increasing the number of production systems using a plasma processing apparatus can be considered. In general, a plasma processing apparatus which is also a vacuum apparatus is used. Production systems are expensive to invest, so increasing the number of production systems may not always be the optimal method. It is also conceivable to increase the number of substrates that can be processed at one time by increasing the size of the plasma processing apparatus. However, in the case of a plasma processing apparatus that performs plasma processing in a vacuum, the size of the plasma processing apparatus is limited by the structural strength. Or the re-use of the plasma processing apparatus becomes complicated and the work efficiency is reduced.In particular, the size of the plasma processing apparatus is limited by the exhaust capacity of the gas exhaust unit, or the volume of the reaction space is excessive. There is a case where the problem that the loss increases, which is a big obstacle, may not always be the optimal method.

As a result of the present inventors' detailed studies on the steps of the plasma treatment in order to solve these problems, as a result of the general plasma processing, the substrate is subjected to the plasma treatment after the plasma treatment. After cooling, the substrate is taken out of the plasma processing apparatus, maintenance of the plasma processing apparatus is performed, and then the substrate is installed in the plasma processing apparatus again, and plasma processing is performed on the substrate. In this step, although not essentially involved in the plasma processing, a step in which a certain amount of time is required in the plasma processing step is a step of cooling the substrate.

The inventors of the present invention have studied a method and an apparatus for performing a cooling process in a short time as far as possible without affecting the plasma processing. As a result, as described above, by performing cooling under constant conditions, It has been found that the time required for the cooling process can be greatly reduced, which not only increases the production efficiency but also contributes to the production stability.

Generally, in the cooling step of the substrate, the heat radiated from the substrate is transmitted to the wall surface of the reaction vessel of the plasma processing apparatus, and the substrate is cooled by radiating heat from the wall surface of the reaction vessel into the atmosphere. In the cooling step, since the plasma processing is generally performed in a vacuum state, the cooling of the substrate is also performed in a vacuum state, so that the process of transferring the heat of the substrate to the wall surface of the reaction vessel is performed. Improving the heat transfer process from the substrate to the reaction vessel, which is rate-limiting in the process, is the best way to reduce the cooling time of the substrate. Japanese Patent Application Laid-Open No. 58-88030 discloses a method of introducing hydrogen gas into a reaction vessel as a method for promoting cooling of a substrate.

As a result of the investigations by the present inventors, although the effect of introducing hydrogen gas is certainly obtained, the best effect cannot be obtained under the conditions described in the above-mentioned publication, and the improvement is still far from being achieved. It turned out there was room for it. First, the pressure of hydrogen gas described in the above-mentioned publication is set to 0.
In the range of 013 to 1.3 Pa, a sufficient cooling effect was not obtained, and it was found that the pressure range of 100 to 100,000 Pa was more effective. Further, it has been found that not only hydrogen gas but also helium gas is effective as a cooling gas. Furthermore, it has been found that the productivity can be further improved by improving the plasma processing method and the plasma processing apparatus incorporating these cooling methods.

As described above, by shortening the cooling time of the substrate, the cycle time required for the plasma processing is shortened, so that the number of units produced per unit time can be increased. Furthermore, it is already possible to improve the productivity by, for example, replacing the reaction vessel portion from the plasma processing apparatus after the plasma processing is completed, and subsequently continuing the plasma processing in the plasma processing apparatus with a new reaction vessel. As described above, the time for cooling the substrate in the reaction container removed at the same time as the plasma treatment is significantly reduced by the method of the present invention, so that the removed reaction container is prepared for performing the next plasma treatment. Since the required time is greatly reduced, the number of reaction vessels required for performing the plasma treatment can be reduced, and the capital investment can be reduced.

Also, unlike the case where the cooling is left to natural cooling, the cooling process, that is, the timing of taking out the substrate from the reaction vessel after the cooling can be controlled, so that the whole process control can be performed more accurately and more than necessary. It is possible to eliminate the waste of taking a long cooling time, and to avoid the trouble of taking out the substrate before the substrate is not sufficiently cooled because the cooling time is too short, thereby improving the production stability. It becomes possible. Further, by filling the inside of the reaction vessel with a cooling gas after removing the reaction vessel from the plasma processing apparatus, the time required for filling the reaction vessel with the cooling gas has little effect on the process. Even if the filling pressure of is set high, it is possible to prevent the effect on productivity.

In addition, since the heat conductivity from the substrate to the wall surface of the reaction vessel is improved, the heat radiation from the wall surface of the reaction vessel to the atmosphere becomes a nonnegligible factor. Therefore, the wall surface of the reaction vessel is actively cooled. Thereby, the cooling rate of the whole reaction vessel is improved, and the cooling time of the substrate can be further shortened, which is more effective.

Hereinafter, a plasma processing apparatus and a processing method according to an embodiment of the present invention will be described in more detail with reference to the drawings. FIG. 1 is a schematic cross-sectional view schematically showing one example of a plasma processing apparatus for an electrophotographic light-receiving member used in the plasma processing method of the present embodiment. In FIG.
The plasma processing apparatus 100 includes a reaction vessel 101, a gas supply unit 102, a gas exhaust unit 103, and a power supply unit 104.

The gas for plasma processing is supplied to the gas supply unit 10.
2 through a gas supply valve 106, a gas supply connection 107 and a gas supply valve 108,
The gas is supplied into the plasma processing space 110 from a gas supply pipe 109 in the reaction vessel 101. The discharge power for the plasma processing is supplied from the power supply 111 of the power supply unit 104 to the matching box 112 and the power supply line connection unit 1 provided as necessary.
13, a plasma processing space 110 from an electrode 114 for introducing discharge power also serving as a wall surface of the reaction vessel 101.
Supplied within.

The exhaust gas after the plasma processing is exhausted from the plasma processing space 110 by an exhaust device 119 through an exhaust pipe 115, an exhaust valve 116, a gas exhaust connection 117 and an exhaust valve 118. Plasma processing space 110
Inside, a cylindrical substrate 120 on which a deposited film is formed is arranged. The cylindrical substrate 120 is held by a shaft 121 and is heated by a heating element 122 as needed. A mechanism for rotating the shaft 121 by driving the motor 123 and rotating the cylindrical body 120 around the center axis in the generatrix direction is provided as necessary.

Further, as shown in FIG. 2, which schematically shows another example of a plasma processing apparatus for a light receiving member for electrophotography using the plasma processing method of the present embodiment, at least a part thereof is made of a dielectric material. By using a method in which discharge power is supplied from the electrode 226 to the plasma processing space 210 through the wall surface 225 of the reaction container formed of the members, the degree of freedom in designing the electrode 226 can be improved.

In this embodiment, the cylindrical substrate 120
The number is not particularly limited, but the production efficiency is better when a plurality of cylindrical substrates 120 are provided. However, in general, as the number of cylindrical substrates 120 increases, the size of the reaction vessel 101 increases, the required capacity of the power supply 111 and the exhaust device 119 increase.
Therefore, the number of cylindrical substrates 120 is appropriately determined in consideration of these points.

In this embodiment, the effect of the present invention can be obtained regardless of the shape of the reaction vessel 101 forming the plasma processing space 110, but the variation in the characteristics of the plasma processing is reduced. From the viewpoint of the shape of the cylindrical substrate 120 itself and the shape of the cylindrical substrate 120
It is preferable to make the shape similar to the disposition shape of. The content of the plasma processing is not particularly limited, and productivity is improved in any plasma processing such as deposition of a semiconductor element such as a light receiving member for electrophotography, a solar cell, and a TFT, and etching of a semiconductor device. It can be mentioned as a preferred method.

The plasma processing using such an apparatus is as follows.
For example, the deposition of an electrophotographic light-receiving member is generally performed by the following method. First, the cylindrical substrate 120 is placed in the reaction vessel 101, and the inside of the plasma processing space 110 is exhausted by the exhaust device 119 through the exhaust pipe 115. continue,
The cylindrical body 120 is heated and controlled to a predetermined temperature by the heating element 122.

When the temperature of the cylindrical substrate 120 reaches a predetermined temperature, a gas used for plasma processing is supplied from the gas supply unit 102 through the gas supply pipe 109 to the plasma processing space 1.
Introduce into 10. After confirming with the pressure gauge 124 that the flow rate of the plasma processing gas has reached the set flow rate and that the pressure in the plasma processing space 110 has reached the set pressure, the power supply 1
11 through the matching box 112 to the electrode 114
A predetermined discharge power is supplied to. A glow discharge is generated in the plasma processing space 110 by the supplied discharge power, and the plasma processing gas is excited and dissociated to generate a cylindrical substrate 120.
A deposited film is formed thereon.

After the desired film thickness is formed, the supply of the discharge power is stopped, and then the supply of the plasma processing gas is stopped to complete the formation of the deposited film. When forming a multi-layered deposited film, the same operation is repeated a plurality of times. in this case,
As described above, once the formation of one layer is completed, the discharge is completely stopped between the layers, and after the setting of the gas flow rate and the pressure of the next layer is changed, the discharge is caused again to generate the next layer. May be formed, or a plurality of layers may be formed continuously by gradually changing the gas flow rate, pressure, and discharge power to the set values of the next layer within a certain period of time after the formation of one layer. Is also good.

During the formation of the deposited film, the rotating shaft 12
The cylindrical base 120 may be rotated at a predetermined speed by the motor 123 via the first motor. After the deposition film is formed, a cooling gas is introduced into the reaction vessel 101 from the gas supply unit 102, and when the pressure in the reaction vessel 101 reaches a desired value by the pressure gauge 124, the supply of the cooling gas is stopped. Thereafter, when a desired time has elapsed, or by monitoring the temperature of the cylindrical substrate 120 (not shown),
When the temperature reaches a desired temperature, the inside of the reaction vessel 101 is returned to the atmospheric pressure, and the cylindrical substrate 120 is taken out.

Further, in order to improve the operation rate of the plasma processing apparatus, a preferred method is to separate the reaction vessel 101 after the plasma processing is completed, and to newly attach the reaction vessel 101 to perform the plasma processing. Even in this case, by filling the inside of the reaction vessel 101 after the plasma processing with the cooling gas, the cylindrical substrate 120 is quickly cooled and can be taken out in a short time, so that the preparation of the reaction vessel 101 for the next plasma processing is short. Since the time is set, the production efficiency can be improved.

At this time, as shown in FIG. 3, by separately providing the cooling gas supply device 327, the filling time of the cooling gas in the plasma processing device 300 can be reduced, and the operation rate of the plasma processing device can be reduced. Is further improved. Further, by providing the common cooling gas supply device 327, it is not necessary to provide a dedicated supply pipe for the cooling gas in the gas supply unit 302 of the plasma processing device 300, so that capital investment can be reduced depending on the contents of the plasma processing. Becomes possible.

Further, as shown in FIG.
By providing a water-cooling jacket 432 so as to actively cool the water of the cylinder 14, or by providing an air-cooling device 533 so as to actively cool the wall surface 525 of the reaction vessel as shown in FIG. The cooling time can be further reduced. There is no particular limitation on the cooling method of the wall surface. However, as a method that can be easily realized, direct cooling with the above-described refrigerant such as gas or liquid is preferable.

The pressure range for filling the cooling gas is 100 to 1
00,000 Pa is preferred, and more preferably 500-10,000 Pa.
00Pa is more preferable. If the cooling gas filling pressure is low, the heat transfer from the substrate to the reaction vessel wall surface is insufficient, and the cooling effect cannot be sufficiently obtained.If the cooling gas filling pressure is high, it takes time to fill the cooling gas, Therefore, an optimum filling pressure can be obtained within the above range according to the configuration of the plasma processing method and the processing apparatus. The type of the cooling gas is not particularly limited, but hydrogen, helium, and the like are useful because they are easily available and have excellent heat conductivity. Further, since it is inert, helium gas which can be vented to the atmospheric pressure as it is after the completion of cooling is mentioned as a preferable cooling gas.

[0032]

EXAMPLES Examples of the present invention will be described below, but the present invention is not limited thereto. Example 1 In the plasma processing apparatus 100 shown in FIG. 1, an aluminum cylindrical substrate 12 having a diameter of 80 mm was used.
6, an a-Si film was formed on the cylindrical substrate 120 using a high frequency power supply 111 of 13.56 MHz according to the film forming conditions shown in Table 1 to form an electrophotographic light-receiving member having a layer structure shown in FIG. Filmed. Thereafter, the reaction vessel 101 was filled with hydrogen gas to the pressure shown in Table 2, and an optical fiber thermometer (790 manufactured by LUXTRON) attached to the surface of the cylindrical substrate 120 was used.
The temperature of the surface of the cylindrical substrate 120 was measured with a Fluorooptic Thermometer, and the temperature of the cylindrical substrate 1 was measured.
The time for cooling until the temperature of No. 20 could be taken out of the reaction vessel 101 was evaluated. The results are shown in Table 2 as relative values of Comparative Example 1 where the pressure was 1 Pa as a reference value. Table 2
As can be seen from the above, it has been found that the cooling time can be reduced by using the plasma processing method of the present invention, and the productivity is extremely excellent.

[0033]

[Table 1]

[0034]

[Table 2] A: The cooling time is reduced to 1/2 of the reference value. B: The cooling time is reduced to 1/2 to 1/3 of the reference value. C: The cooling time is reduced to 1/3 to 1 / of the reference value. D: The cooling time was reduced to 1/4 to 1/5 of the reference value. [Example 2] A light receiving member for electrophotography was produced in the same manner as in Example 1 except that helium gas was used as a cooling gas. Plasma treatment was performed, and the same evaluation as in Example 1 was performed. The results are shown in Table 3 as relative values of Comparative Example 2 where the pressure was 1 Pa as a reference value. As can be seen from Table 3, the use of the plasma processing method of the present invention made it possible to shorten the cooling time, and it was found that the productivity was extremely excellent.

[0035]

[Table 3] A: The cooling time is reduced to 1/2 of the reference value. B: The cooling time is reduced to 1/2 to 1/3 of the reference value. C: The cooling time is reduced to 1/3 to 1 / of the reference value. 4 D: Cooling time reduced to 1/4 to 1/5 of the reference value [Example 3] In the plasma processing apparatus 200 shown in FIG.
An a-Si film having a layer structure shown in FIG. 4 was formed on the cylindrical substrate 220 by using a 100 MHz high frequency power source 211 under the conditions shown in FIG. . Thereafter, the reaction vessel 201 was filled with helium gas to a pressure shown in Table 5. After that, the reaction container 201 is connected to the gas supply unit 202, the gas exhaust unit 203, and the power supply unit 2.
04, and after cooling the temperature of the cylindrical substrate 220 to a point where it can be taken out, take out the cylindrical substrate 220, perform maintenance on the reaction vessel, and evaluate the time until preparation for the next plasma treatment is completed. did. The results are shown in Table 5 as relative values of Comparative Example 3 where the pressure was 1 Pa as a reference value.
It was shown to. As can be seen from Table 5, by using the plasma processing method of the present invention, it is possible to reduce the time required until the preparation for the next plasma processing is completed, and it is not necessary to prepare extra reaction vessels. Therefore, it was found that the cost reduction effect by reducing the amount of capital investment was excellent, and the productivity was extremely excellent.

[0036]

[Table 4]

[0037]

[Table 5] A: Preparation completion time for reference value is reduced to 10% B: Preparation completion time for reference value is 10% to 20%
%: Preparation completion time for reference value is 20% to 30%
%: D: Time to complete preparation against the reference value is 30% to 40%
Example 4 During the cooling of the cylindrical substrate by the cooling gas, the same as in Example 1 except that the wall surface 414 of the reaction vessel 401 shown in FIG. 4 was water-cooled by the cooling water supply device 431 and the water cooling jacket 432. The light receiving member for electrophotography was subjected to plasma treatment, and the same evaluation as in Example 1 was performed. The results are shown in Table 6 as relative values of Comparative Example 4 where the pressure was 1 Pa as a reference value. As can be seen from Table 6, the use of the plasma processing method of the present invention made it possible to reduce the cooling time, and it was found that the productivity was extremely excellent.

[0038]

[Table 6] A: Cooling time is reduced to 1/2 for reference value B: Cooling time is reduced to 1/2 to 1/3 for reference plant C: Cooling time is reduced to 1/3 to 1 / for reference value D: Cooling time is reduced to 1/4 to 1/5 with respect to the reference value E: Cooling time is reduced to 1/5 to 1/6 with respect to the reference value [Example 5] Cylinder with cooling gas During cooling of the substrate, the wall 525 of the reaction vessel 501 shown in FIG.
The plasma treatment of the electrophotographic light-receiving member was performed in the same manner as in Example 3 except that the air-cooling member was air-cooled, and the same evaluation as in Example 3 was performed. The results are shown in Table 7 as relative values of Comparative Example 5 where the pressure was 1 Pa as a reference value. As can be seen from Table 7,
By using the plasma processing method of the present invention, it is possible to reduce the time required until the preparation for the next plasma processing is completed, and it is not necessary to prepare extra reaction vessels, thereby reducing the capital investment. It has been found that the cost reduction effect obtained by doing so is excellent, and the productivity is also extremely excellent.

[0039]

[Table 7] A: Preparation completion time for reference value is reduced to 10% B: Preparation completion time for reference value is 10% to 20%
%: Preparation completion time for reference value is 20% to 30%
%: D: Time to complete preparation against the reference value is 30% to 40%
% E: Time to complete preparation for reference value is 40% to 50%
Example 6 In the plasma processing apparatus 300 shown in FIG. 3, after forming a light receiving member for electrophotography in the same manner as in Example 3, the reaction container 301 was replaced with a gas supply unit 302 and a gas exhaust unit 303. After disconnecting from the power supply unit 304 and connecting the cooling gas supply unit 328 to the reaction vessel 301, the reaction vessel 301 was filled with helium gas to 1000 Pa. In this embodiment, the plasma processing apparatus 300 is
The cooling time of the cylindrical substrate is the same as that of the third embodiment, and a helium gas supply line for a cooling gas is installed in the gas supply unit 302 of each plasma processing apparatus 300. It is not necessary to use the plasma processing method of the present invention, so that it is possible to reduce the capital investment by using the plasma processing method, thereby achieving an excellent cost reduction effect, shortening the cooling time, and achieving extremely excellent productivity. found.

Example 7 A plasma treatment was performed in the same manner as in Example 6, except that the wall 525 of the reaction vessel was air-cooled by an air-cooling device 533 shown in FIG. The cooling time of the cylindrical substrate 520 was further reduced by about 20% from that of Example 6, and the cooling time could be reduced by using the plasma processing method of the present invention, and it was found that the productivity was extremely excellent. did.

[0041]

As described above, according to the present invention, by improving the equipment operation rate and improving the workability, high-quality plasma processing with extremely excellent productivity can be performed. It can be realized with the capital investment amount.

[Brief description of the drawings]

FIG. 1 shows an embodiment of the present invention, Example 1, and Example 2.
FIG. 4 is a schematic view showing an example of a plasma processing apparatus for an electrophotographic light-receiving member used in the plasma processing method of FIG.

FIG. 2 is a schematic view showing an example of a plasma processing apparatus for an electrophotographic light-receiving member used in the plasma processing method according to the embodiment of the present invention and the plasma processing method of Example 3.

FIG. 3 is a schematic view showing an example of a plasma processing apparatus for an electrophotographic light-receiving member used in the plasma processing method according to the embodiment of the present invention and Example 6.

FIG. 4 is a schematic view illustrating an example of a plasma processing apparatus for an electrophotographic light-receiving member used in the plasma processing method according to the embodiment of the present invention and the plasma processing method according to Example 4.

FIG. 5 shows an embodiment of the present invention, Example 5, and Example 7;
FIG. 4 is a schematic view showing an example of a plasma processing apparatus for an electrophotographic light-receiving member used in the plasma processing method of FIG.

FIG. 6 is a schematic diagram illustrating an example of a layer configuration of an electrophotographic light-receiving member formed by a plasma processing method or apparatus according to an embodiment of the present invention.

[Explanation of symbols]

100, 200, 300, 400, 500: plasma processing apparatus 101, 201, 301, 401, 501: reaction vessel 102, 202, 302: gas supply unit 103, 203, 303: gas exhaust unit 104, 204, 304: power supply Units 105, 205: Gas supply devices 106, 206: Gas supply valves 107, 207: Gas supply connection units 108, 208, 408, 508: Gas supply valves 109, 209, 409, 509: Gas supply pipes 110, 210, 410 , 510: Plasma processing space 111, 211: Power supply 112, 212: Matching box 113, 213: Power supply line connection part 114, 414: Reaction vessel wall surface 115, 215, 415, 515: Exhaust pipe 116, 216, 416, 516 : Exhaust valve 117, 217: gas exhaust connection part 11 , 218: Exhaust valve 119, 219: Exhaust device 120, 220, 420, 520: Cylindrical base 121, 221, 421, 521: Shaft 122, 222, 422, 522: Heating element 123, 223, 423, 523: Motor 124, 224, 424, 524: pressure gauge 225, 525: wall surface 226, 526: electrode 327: cooling processing unit 328: cooling gas supply unit 431: cooling water supply unit 432: cooling jacket 533: air cooling unit 600: for electrophotography Light receiving member 601: base 602: charge injection blocking layer 603: photoconductive layer 604: surface layer

 ──────────────────────────────────────────────────続 き Continued on the front page (72) Inventor Daisuke Tazawa 3-30-2 Shimomaruko, Ota-ku, Tokyo Canon Inc. (72) Inventor Hitoshi Murayama 3-30-2 Shimomaruko, Ota-ku, Tokyo Canon (72) Inventor Kazutaka Akiyama 3-30-2 Shimomaruko, Ota-ku, Tokyo Canon Inc. (72) Inventor Toshiyasu Shirasuna 3-30-2, Shimomaruko 3-chome, Ota-ku, Tokyo Canon Inc. ( 72) Inventor Takashi Otsuka 3-30-2 Shimomaruko, Ota-ku, Tokyo F-term within Canon Inc. (reference) 2H068 DA03 DA23 DA53 EA24 EA30 EA43 4K030 AA06 AA17 BA30 CA02 CA14 DA08 FA03 KA05 KA26 LA17 5F045 AB04 AC01 AC17 AE19 AE21 AE23 AE25 AF10 BB08 CA16

Claims (16)

[Claims] 1. A reaction vessel for forming a plasma, a reaction gas supply unit for supplying a reaction gas into the reaction vessel, and a gas exhaust unit for exhausting the inside of the reaction vessel. A plasma processing method of supplying the reaction gas to the reaction vessel, decomposing the reaction gas by discharge power introduced into the reaction vessel, and performing plasma processing on a substrate disposed in the reaction vessel. After the treatment is completed, a cooling gas is charged into the reaction vessel at a pressure of 100 to 100,000 Pa to perform a cooling treatment of the substrate. 2. The plasma processing method according to claim 1, wherein the cooling gas filled in the reaction vessel is hydrogen and / or helium. 3. The plasma processing method according to claim 1, wherein the reaction vessel is processed separately from the reaction gas supply section and the gas exhaust section. 4. The method according to claim 3, wherein the reaction vessel is separated from the reaction gas supply section and the gas exhaust section, and then the reaction vessel is filled with a cooling gas to cool the substrate. 4. The plasma processing method according to 1. 5. The plasma processing method according to claim 1, wherein an outer peripheral surface of the reaction vessel filled with the cooling gas is cooled by a gas and / or a liquid. 6. The reaction vessel according to claim 1, wherein the cooling gas filled in the reaction vessel is filled in the reaction vessel from a supply section different from the reaction gas supply section. 2. The plasma processing method according to claim 1. 7. The plasma processing method according to claim 1, wherein a cylindrical substrate is used as the substrate, and a plurality of the cylindrical substrates are arranged in the reaction vessel. 8. The plasma processing method according to claim 1, wherein the plasma processing method is a method for forming a photoconductor for electrophotography. 9. A reaction vessel for forming plasma, a reaction gas supply section for supplying a reaction gas into the reaction vessel, an electrode for introducing discharge power into the reaction vessel, and exhausting the inside of the reaction vessel. A plasma processing apparatus that includes a gas exhaust unit for performing a plasma treatment on the substrate by disposing the substrate in the reaction container and decomposing the reaction gas by the discharge power. A plasma processing apparatus comprising a cooling gas supply unit for introducing a cooling gas after the plasma processing is completed. 10. The plasma processing apparatus according to claim 9, wherein said cooling gas supply unit is constituted by a supply unit different from said reaction gas supply unit. 11. The cooling gas supply unit is a supply unit for supplying hydrogen and / or helium.
Alternatively, the plasma processing apparatus according to claim 10. 12. The plasma processing apparatus according to claim 9, wherein the reaction vessel is configured to be separated from the reaction gas supply unit and the gas exhaust unit. 13. The plasma processing apparatus according to claim 9, wherein the reaction vessel is provided with a cooling mechanism for cooling an outer peripheral surface of the reaction vessel. . 14. The plasma processing apparatus according to claim 13, wherein said cooling mechanism is a cooling mechanism using air cooling and / or water cooling. 15. The plasma processing apparatus according to claim 9, wherein said substrate is a cylindrical substrate, and a plurality of said cylindrical substrates are arranged in said reaction vessel. . 16. The plasma processing apparatus according to claim 9, wherein the plasma processing apparatus is an electrophotographic photoreceptor forming apparatus.