JP2002146541A - Deposited film forming equipment, its forming method, and electrophotographic photosensitive body - Google Patents

Abstract

PROBLEM TO BE SOLVED: To improve the uniformity and reproducibility of deposited film characteristics under a superior production stability. SOLUTION: The deposited film forming equipment 100 is composed of a reaction container 102 that is capable of enclosing at least the base body 101 and reducing pressure, a supply system 104 for introducing a gaseous starting material into the reaction container 102, an evacuation system 105 for exhausting the reaction container 102, a power supply system 106 for introducing an electric power for dissolving the gas introduced, a motor 116 for rotating the base body 101 and a driving unit 118. The deposited film forming equipment 100 is provided with a base body rotation controller 120 for controlling the motor 116 and the driving unit 118 linked with a minimum of one control function among the gaseous starting material supply system 104, the evacuation system 105, and the power supply system.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a deposited film on a support, particularly a functional deposited film, particularly a semiconductor device, a light receiving member for electrophotography, a line sensor for image input, an imaging device, a photovoltaic element, and the like. TECHNICAL FIELD The present invention relates to a deposited film forming apparatus and a deposited film forming method for forming a deposited film used in a method.

[0002]

2. Description of the Related Art Conventionally, deposited films used in semiconductor devices, photoreceptors for electrophotography, image input line sensors, photographing devices, photovoltaic devices, etc. are formed by plasma CVD,
It is formed by a deposition film forming method using plasma generated by high frequency power such as an ion plating method and a plasma etching method, and therefore, many apparatuses have been put to practical use.

For example, a method of forming a deposited film using a plasma CVD method, that is, a method of forming a deposited film by generating plasma of a source gas by glow discharge of high-frequency power and depositing the decomposed species on a substrate. is there. When this method is used, for example, an amorphous silicon thin film can be formed by using silane gas as a source gas. Here, an outline of a method of forming an amorphous silicon thin film by a plasma CVD method will be described using an example of a method of manufacturing an electrophotographic photosensitive member using amorphous silicon as a base material.

FIG. 3 is a schematic configuration diagram showing an example of a manufacturing apparatus (deposited film forming apparatus) of an electrophotographic photosensitive member using amorphous silicon as a base material by using a plasma CVD method.

The apparatus comprises a reaction vessel 102 capable of containing a cylindrical substrate 101 and capable of reducing pressure, a source gas supply pipe 117 for supplying a source gas into the reaction vessel 102, and an electric power for decomposing the source gas. Film forming apparatus 100 including a cathode 114 for introducing
Source gas supply system 1 for supplying source gas into 2
04 and an exhaust system 10 for exhausting the inside of the reaction vessel 102
5 and a power supply system 106 that supplies power to the cathode 114. The right cylindrical body 101 of the two cylindrical bodies 101 shown in FIG. 3 shows a cross section broken in the longitudinal direction.

Further, in this apparatus, during the formation of the deposited film, the substrate 101 is rotated at a predetermined speed by the motor 116 via the drive unit 118, thereby improving the uniformity of the deposited film in the circumferential direction of the substrate 101. In addition, the deposited film forming apparatus provided with such a configuration (motor and drive unit)
It is disclosed in JP-A-11-92932.

FIG. 4 is a schematic sectional view showing a cross section of the deposited film forming apparatus in the apparatus shown in FIG.

As shown in FIG. 4, an exhaust port 119 is provided at the center of the bottom surface of the reaction vessel 102. In the reaction vessel 102, six cylindrical substrates 101 are arranged concentrically around the exhaust port 119, and further around a circular orbit formed by these cylindrical substrates 101.
The source gas supply pipe 117 is similarly arranged concentrically with the exhaust port 119. Further, the reaction vessel 10
Six cathodes 114 are arranged between 2 and the outer frame member of the deposited film forming apparatus 100.

Next, a process of forming a deposited film using the above-described apparatus will be described.

First, a cylindrical substrate 101 is placed on a substrate support 103 containing a heater (not shown) in a reaction vessel 102.
Is installed, and the inside of the reaction vessel 102 is evacuated by the exhaust pump 107 through the exhaust port 119. After the evacuation to a desired degree of vacuum is completed, for example, an inert gas such as Ar gas is supplied to the source gas supply system 104. It is supplied into the reaction vessel 102 at a predetermined flow rate using a mass flow controller. Then, the pressure inside the reaction vessel 102 is controlled to a desired pressure by adjusting the exhaust speed of the exhaust pump 107. After the internal pressure of the reaction vessel 102 is set to a desired pressure, the cylindrical substrate 1 is heated by a heater built in the substrate support 103.
Heat 01 to desired temperature. The cylindrical substrate 10
1 keeps maintaining the desired temperature required for forming the deposited film even during the formation of the deposited film.

After the heating step is completed by the above procedure,
Subsequently, a deposited film forming step is performed. Ar in the reaction vessel 102
After the gas is exhausted by the exhaust pump 107, the exhaust valve 108 and the main exhaust valve 109 are operated to fully open the throttle valve 110, and the inside of the reaction vessel 102 is opened by the main exhaust pump 112 via the oil diffusion pump 111. For example, the gas is evacuated to a degree of vacuum of 1 × 10 ⁻³ Pa. Subsequently, each raw material gas is supplied into the reaction vessel 102 at a predetermined flow rate by a raw material gas supply system 104 using a mass flow controller installed in each supply pipe. At this time, the internal pressure of the reaction vessel 102 is controlled to a desired pressure by adjusting the opening of the throttle valve 110 and adjusting the exhaust speed. When the internal pressure of the reaction vessel 102 becomes stable, power is supplied from the power source 113 to the cathode 114 via the matching box 115 to generate a glow discharge in the reaction vessel 102. The source gas introduced into the reaction vessel 102 is decomposed by the discharge energy, and a predetermined deposited film is simultaneously formed on each of the cylindrical substrates 101. When the deposited film reaches a desired film thickness, the supply of the electric power applied to the cathode 114 is stopped, and the supply of the source gas from the raw material gas supply system 104 is stopped, thereby completing the formation of the deposited film.

By repeating the same operation a plurality of times, a deposited film having a multilayer structure can be formed.

According to the above-described method for forming a deposited film, for example, as shown in FIG.
2. A photoconductor for electrophotography is formed by stacking deposited films in the order of photoconductive layer 203 and surface layer 204.

[0014]

It is possible to form a relatively good deposited film by the above-mentioned conventional deposited film forming method. However, the demand level in the market for products using these deposited films is increasing day by day, and higher quality deposited films are required to meet this demand.

For example, in the case of an electrophotographic apparatus, digitization is further advanced, and a document output by a digital multifunction peripheral or a color electrophotographic apparatus is not limited to a character document, but also to a high quality image such as a photograph or a digital image from a computer. The range has been widened to image originals that require. In particular,
The output frequency of such an image document is increasing, and there is an increasing demand for reducing the image density unevenness on the electrophotographic photosensitive member. Furthermore, there is a strong demand for downsizing and cost reduction of electrophotographic devices, and at the same time as improving the characteristics of the electrophotographic photoconductor as described above, a reduction in the production cost of the electrophotographic photoconductor is also strongly demanded. In order to satisfy these demands, there is a demand for an improved method of forming a deposited film.

Under these circumstances, there is still room for improvement in the above-described conventional method for forming a deposited film, with respect to the improvement of the deposited film characteristics and the reduction of the cost of forming the deposited film.

Specifically, for example, the uniformity and reproducibility of the characteristics of the deposited film to be formed can be improved. Insufficient uniformity and reproducibility of deposited film characteristics lead to variations in deposited film characteristics, lower product quality, and lower non-defective products. In particular, when a member having a stacked configuration of a plurality of deposited films is formed, if the film characteristics of a certain layer are deteriorated due to the variation in the characteristics, matching with other layers is also deteriorated, so that the entire member is greatly affected. Become.
Further, in a large-area member such as an electrophotographic photoreceptor, even if the film quality is locally deteriorated, only the portion cannot be removed, so that the influence is large. As described above, improving the uniformity and reproducibility of the deposited film characteristics and suppressing the variation in the deposited film characteristics greatly contribute to improving the characteristics of the deposited film as a whole and lowering the cost of forming the deposited film.

Further, by realizing a method for forming a deposited film capable of improving the uniformity and reproducibility of the deposited film characteristics with high production stability, it is possible to further reduce the production cost. It is indispensable in responding to the demands.

The present invention has been made to solve the above problems. That is, the object of the present invention is:
It is an object of the present invention to provide a deposited film forming apparatus and method capable of improving the uniformity and reproducibility of deposited film characteristics with excellent production stability in forming a deposited film.

[0020]

In order to achieve the above object, a deposition film forming apparatus of the present invention comprises a reaction vessel capable of containing at least a substrate and a decompressible reaction vessel, and a gas supply means for introducing a raw material gas into the reaction vessel. Exhaust means for exhausting the reaction vessel, power introducing means for introducing electric power for decomposing the introduced gas, and substrate rotating means for rotating the substrate, forming a deposited film on the substrate. The deposition film forming apparatus further includes a substrate rotation control unit that controls the substrate rotation unit in conjunction with control of at least one of the source gas introduction unit, the exhaust unit, and the power supply unit. .

According to the deposited film forming apparatus of the present invention, the substrate rotation control means allows the deposited film to be formed only when a region of the deposited film is formed under another forming condition different from the predetermined forming condition. Since the rotation speed of the base can be increased, deterioration of the characteristics of the vacuum seal of the base rotating shaft is prevented from being promoted. As a result, the uniformity and reproducibility of the deposited film can be improved without impairing the production stability.

Further, the reaction container may have a structure in which a plurality of the substrates are provided.

Further, the power supply means may have an oscillation frequency of 50 MHz to 450 MHz.

In the method of forming a deposited film according to the present invention, a rotatable substrate is installed in a reaction vessel capable of reducing pressure, and a raw material gas supplied into the reaction vessel is decomposed by electric power introduced from electric power introduction means. In the method for forming a deposited film on the substrate, the step of forming the deposited film on the substrate includes the steps of: forming the deposited film under predetermined forming conditions;
Forming the deposited film under another forming condition different from the predetermined forming condition, wherein the forming the deposited film under the other forming condition includes: Is made faster than the rotation speed of the substrate in the step of forming under the predetermined forming conditions.

According to the method of forming a deposited film of the present invention, the rotation speed of the substrate is increased only in the step of forming the deposited film under other forming conditions different from the predetermined forming conditions.
Acceleration of characteristic deterioration of the vacuum seal of the base rotating shaft is suppressed. As a result, without sacrificing production stability,
The uniformity and reproducibility of the deposited film can be improved.

[0026] Further, the formation conditions of the deposited film may be changed during the step of forming the deposited film under the other forming conditions.

The conditions for forming the deposited film include the type of the source gas supplied into the reaction vessel, the supply flow rate of the source gas, the pressure in the reaction vessel, and the power supplied to the reaction vessel. At least one configuration may be used.

Furthermore, a configuration may be adopted in which a plurality of the substrates are provided in the reaction vessel, and the deposited film is formed on the plurality of substrates simultaneously.

Furthermore, it is preferable to adopt a configuration in which electric power having an oscillation frequency of 50 MHz to 450 MHz is introduced into the reaction vessel.

Further, the electrophotographic photoreceptor of the present invention comprises a deposited film formed by the above-mentioned method of forming a deposited film of the present invention.

[0031]

Next, embodiments of the present invention will be described with reference to the drawings.

When a deposited film having a multi-layer structure is formed, the electric, optical, and optical characteristics of the region where each layer is in contact are improved for the purpose of improving the electrical, optical, or mechanical properties in the region where each layer is in contact. Alternatively, there may be a case where a change region in which the mechanical characteristics change continuously is provided.

For example, as shown in FIG. 2, a charge injection blocking layer 202, a photoconductive layer 203, and a surface layer 204 are formed on a substrate 201.
When the deposited films are stacked in this order, the charge injection blocking layer 202
On the side of the photoconductive layer 203 in order to improve the mobility of carriers between the charge injection blocking layer 202 and the photoconductive layer 203 and the mechanical adhesion, etc.
Or the mobility of carriers between the surface layer 204 and the photoconductive layer 203 on the photoconductive layer 203 side of the surface layer 204,
In some cases, a change region 206 of the surface layer is provided for the purpose of improving light transmittance, mechanical adhesion, and the like.

The present inventors have studied in detail that the uniformity and reproducibility of the deposited film are higher when such a change region exists than when no change region exists. It has been found that the properties may not always be fully satisfactory. This is because the change area of the deposited film is
Generally, it is formed under other forming conditions different from the predetermined forming conditions when forming the region other than the change region. At this time, the uniformity and stability of the plasma formed in the reaction vessel are reduced. It is supposed that this is because the characteristics may not be sufficiently satisfactory in the uniformity and reproducibility of the characteristics in the change region of the deposited film in such a case.

As an effective method for improving the uniformity of the deposited film, there is a method of rotating the substrate during the formation of the deposited film. The rotation speed of the substrate required for improvement is different between the case where the changed region of the deposited film is formed and the case where the other region is formed, and the uniformity of the deposited film is sufficient even in the changed region of the deposited film. We thought that it would be necessary to increase the rotation speed of the substrate to obtain reproducibility.

However, during the formation of the deposited film, the pressure in the reaction vessel is reduced. Therefore, if the rotation speed of the substrate is increased unnecessarily, the deterioration of the characteristics of the vacuum seal on the rotating shaft is promoted, and the inside of the reaction vessel is reduced. Leakage of raw material gas or atmospheric gas outside the reaction vessel occurs, resulting in deterioration of deposited film characteristics and failure of the deposited film forming apparatus, and frequent inspection or replacement of the vacuum seal is required. It is feared that the production stability will decrease.

As a result of studies conducted by the present inventors to solve such problems, when forming a deposited film, the rotation speed of the substrate is changed according to the conditions for forming the deposited film, and the change region of the deposited film is changed. When forming a region, the rotational speed of the substrate is increased compared to when forming the other region, and when forming the region other than the change region, the rotational speed of the substrate is set to a predetermined rotational speed similar to the conventional one. By doing so, it has been found that it is possible to suppress the deterioration of the characteristics of the vacuum seal of the rotating shaft from being promoted, and to improve the uniformity and reproducibility of the deposited film without impairing the production stability.

In the present invention, the object of the present invention can be effectively achieved by increasing the rotation speed of the base only when forming the change region of the deposited film. However, for example, when more importance is placed on preventing the deterioration of the characteristics of the vacuum seal of the rotating shaft, the rotation of the substrate is performed only when a region where the uniformity and stability of the plasma are most likely to be reduced is formed among the changed regions of the deposited film. A method of increasing speed is preferred. In the case where importance is placed on the reproducibility of the characteristics of the deposited film, it is preferable to increase the rotation speed of the substrate even when forming a wider region including the changed region of the deposited film. In any case, in forming the deposited film, the rotation speed of the substrate when forming the change region of the deposited film is set to be higher than the rotation speed when forming another region.

In the present invention, the rotation speed of the substrate is appropriately determined in consideration of the uniformity and stability of the plasma due to the change of the forming conditions, the method of vacuum sealing the rotating shaft of the substrate, the deposition speed of the deposited film, and the like. A preferable range of the rotation speed of the base when forming a region other than the change region of the deposited film is 0.1 rpm to 60 rpm. The rotation speed of the substrate when forming the changed region of the deposited film is about 1.5 to 2 times the rotation speed of the substrate when forming the region other than the changed region of the deposited film.
0 times is preferable, and about 2 times to about 10 times is more preferable. The upper limit of the increase in the rotation speed of the substrate when forming the change region of the deposited film is the degree of deterioration of the characteristics of the vacuum seal on the rotation axis of the substrate, that is, the characteristics of the deposited film are deteriorated due to gas leakage, It is desirable that the film formation apparatus be determined in consideration of not causing a trouble of the film forming apparatus, or reducing the production stability due to an increase in inspection frequency and replacement frequency of the vacuum seal. The lower limit of the increase in the rotation speed of the base when forming the change region of the deposited film is desirably determined in consideration of the uniformity and reproducibility of the deposited film being sufficiently improved.

As a means for vacuum-sealing the rotating shaft of the base, it is preferable to use an O-ring, a magnetic fluid, an omni-seal (trade name of Huron Co.) or the like.

The conditions for forming the deposited film to be changed when forming the changed region of the deposited film include the type of the source gas, the supply flow rate of the source gas, the pressure in the reaction vessel, and the electric power introduced into the reaction vessel. The formation conditions that easily affect the plasma in the reaction vessel are listed. By changing these conditions continuously or stepwise, a changed region of the deposited film is formed.

The method for forming a deposited film according to the present invention can provide uniformity and reproducibility of a deposited film even when a plurality of substrates are placed in a reaction vessel, that is, even when the plasma around the substrates in the reaction vessel has little symmetry. It is preferable to improve

As the power for decomposing the raw material gas, any oscillation frequency such as direct current, alternating current, and high frequency can be used, and it is appropriately selected according to the configuration in the reaction vessel, the type of the deposited film, and the like. In particular, from the viewpoint that stable plasma can be obtained even under a wider range of forming conditions, for example, higher vacuum, and more uniform plasma can be easily obtained without depending on the configuration of the reaction vessel, the oscillation frequency is 50 MHz to 450 MHz. It is mentioned as a preferable range to use the above power, and the effect of the present invention can be further obtained.
The deposited film forming apparatus for performing the deposited film forming method of the present invention may be any configuration as long as the source gas stays in the limited deposition space.
Basically, such a condition is satisfied by having a reaction vessel that can be depressurized. However, when actually forming a deposited film, the inside of the reaction space is in any of a depressurized state, an atmospheric pressure state, and a pressurized state. You may.

In the method of forming a deposited film of the present invention, a deposited film having uniform characteristics can be obtained on a substrate having a relatively large area, so that an electrophotographic photosensitive member having excellent uniformity in characteristics can be formed. In particular, when there is a change region of the deposited film on the light incident side where the optical characteristics are important, an electrophotographic photosensitive member having more excellent characteristics can be obtained.

An outline of the above-described method of forming a deposited film will be described below based on an example of manufacturing an electrophotographic photoreceptor and using one configuration example of a manufacturing apparatus shown in FIG. In FIG. 1, the members indicated by the same drawer numbers as those in FIG. 3 indicate the same members as those in FIG. Further, a schematic sectional view of the reaction vessel 102 is as shown in FIG.

First, a cylindrical substrate 101 is placed on a substrate support 103 containing a heater (not shown) in a reaction vessel 102.
Is installed, and the inside of the reaction vessel 102 is evacuated by the exhaust pump 107 through the exhaust port 119. After the evacuation to a desired degree of vacuum is completed, for example, an inert gas such as Ar gas is supplied to the source gas supply system 104. It is supplied into the reaction vessel 102 at a predetermined flow rate using a mass flow controller. Then, the pressure inside the reaction vessel 102 is controlled to a desired pressure by adjusting the exhaust speed of the exhaust pump 107. After the internal pressure of the reaction vessel 102 is set to a desired pressure, the cylindrical substrate 1 is heated by a heater built in the substrate support 103.
Heat 01 to desired temperature. The cylindrical substrate 10
1 keeps maintaining the desired temperature required for forming the deposited film even during the formation of the deposited film.

After the heating step is completed by the above procedure,
Subsequently, a deposited film forming step is performed. Ar in the reaction vessel 102
After the gas is exhausted by the exhaust pump 107, the exhaust valve 108 and the main exhaust valve 109 are operated to fully open the throttle valve 110, and the inside of the reaction vessel 102 is opened by the main exhaust pump 112 via the oil diffusion pump 111. For example, the gas is evacuated to a degree of vacuum of 1 × 10 ⁻³ Pa. Subsequently, each raw material gas is supplied into the reaction vessel 102 by the raw material gas supply system 104 at a predetermined flow rate (here, a flow rate condition for forming the charge injection blocking layer) using a mass flow controller installed in each supply pipe. ). Here, the deposited film forming apparatus according to the embodiment of the present invention includes at least a source gas supply system 104 as a source gas introduction unit, an exhaust system 105 as an exhaust unit, and a power supply system 106 as a power supply unit. A base rotation control device 120 that controls a motor 116 and a driving unit 118 as base rotation means in conjunction with one control is provided.
With 0, the number of rotations of the motor 116 is controlled, for example, so that the substrate rotation speed becomes 3 rpm. Then, the internal pressure of the reaction vessel 102 is controlled to a desired pressure by adjusting the opening of the throttle valve 110 and adjusting the exhaust speed. When the internal pressure of the reaction vessel 102 is stabilized, power is supplied from the power source 113 to the cathode 114 via the matching box 115, and the reaction vessel 102
A glow discharge is generated inside. The source gas introduced into the reaction vessel 102 is decomposed by this discharge energy, and a deposited film as a charge injection blocking layer is formed on each cylindrical substrate 101 at the same time. When the charge injection blocking layer reaches a desired film thickness, the substrate rotation control means 120 continuously changes the source gas type and its flow rate by a mass flow controller and a valve in the gas supply system 104 and / or supplies electric power. The output value of the power source 113 of the system 106 is continuously changed and / or the pressure in the reaction vessel is changed by the valves 108, 109, 1 in the exhaust system 105.
10 and the motor 11
The number of rotations of 6 is increased, for example, so that the substrate rotation speed becomes 6 rpm.

Thereafter, when certain conditions for forming the photoconductive layer are reached, that is, when the kind of source gas and its flow rate, the output value of the power source 113, and the pressure in the reaction vessel become constant,
The substrate rotation control means reduces the substrate rotation speed to, for example, 3 rpm.

Similarly, a deposited film is formed up to the surface layer. When the formation of the deposited film is completed, the supply of the power applied to the cathode 114 is stopped, and the supply of the source gas from the raw gas supply system 104 is stopped. By stopping, the formation of the deposited film is completed. Thus, the electrophotographic photosensitive member of the present invention is formed.

[0050]

EXAMPLES The present invention will be described in detail below with reference to examples, but the present invention is not limited to these examples.

(Example 1) Using the apparatus shown in FIG.
The amorphous silicon shown in FIG. 2 was formed on a cylindrical aluminum cylinder (substrate) 101 having a diameter of 80 mm and a length of 358 mm using a high-frequency power source 113 having an oscillation frequency of 105 MHz under the conditions for forming the deposited film shown in Table 1. An electrophotographic photoreceptor was prepared.

[0052]

[Table 1]

In the present embodiment, the rotation speed of the substrate in the change region 205 of the charge injection blocking layer and the change region 206 of the surface layer is set to the conditions shown in Table 2, and Example 1 (a) has 10 lots and Example 1 (a). In (b) to (d), electrophotographic photoconductors were manufactured in three lots.

[0054]

[Table 2]

Comparative Example 1 An electrophotographic photosensitive member was manufactured under the same conditions as in the first example except that the rotation speed of the substrate was kept constant during the formation of all the layers. In Comparative Example 1 (a), three lots of electrophotographic photoconductors were prepared with the rotation speed of the substrate being 3 rpm, and in Comparative Example 1 (b), ten lots of electrophotographic photoconductors were formed with the rotation speed of the substrate being 6 rpm. Was prepared.

Each of the electrophotographic photoreceptors manufactured in Example 1 and Comparative Example 1 was evaluated by the following specific evaluation method using a Canon copier NP-6750.
The copier used for the evaluation had an image exposure light source of wavelength 65.
A pre-exposure light source with a wavelength of 660n was applied to a 5nm semiconductor laser.
The LED has been changed to m.

-Uniformity and Reproducibility of Charging Ability-A dark portion potential at the developing device position when a constant current is applied to the main charging device of the copying machine is measured. As for the uniformity of the charging ability,
The variation width of the dark portion potential (unevenness of the dark portion potential) when the electrophotographic photoreceptor makes a round around the substrate was evaluated. The smaller the fluctuation width, the better the uniformity. Regarding the reproducibility of the charging ability, the standard deviation of the dark area potential in the electrophotographic photosensitive members of the first three lots was evaluated. The smaller the standard deviation, the better the reproducibility.

-Uniformity and Reproducibility of Sensitivity-The main charger current is adjusted so that the dark area potential at the developing device position of the copying machine becomes a constant value, and then a constant amount of image exposure is applied to the developing device. Measure the bright spot potential at the location. The uniformity of the sensitivity was evaluated by the fluctuation width of the light portion potential (unevenness of the light portion potential) when the electrophotographic photoreceptor circled around the substrate. The smaller the fluctuation width, the better the uniformity. As the reproducibility of the sensitivity, the standard deviation of the light portion potential in the electrophotographic photosensitive members of the first three lots was evaluated. The smaller the standard deviation, the better the reproducibility.

Further, Example 1 (a) and Comparative Example 1
The electrophotographic photosensitive member of (b) was evaluated for each item by the following specific evaluation method.

-Production stability- The average value of the sensitivity in the first to second lots and the average value of the sensitivity in the ninth to tenth lots are obtained by the same procedure as the above-described sensitivity evaluation method, and the average value of the sensitivity is calculated. The range of fluctuation was evaluated. The smaller the fluctuation width is, the smaller the leak which is a factor of deteriorating the deposited film characteristics is, and the more the production stability is improved. further,
Before manufacturing the electrophotographic photoconductor of the first lot and after manufacturing the electrophotographic photoconductor of the tenth lot, the amount of vacuum leak at the rotating shaft portion of the base of the reaction vessel was measured using a helium leak detector (PORTANTEST2 manufactured by Varian). ) To evaluate the fluctuation range of the amount of vacuum leak. The smaller the fluctuation width, the better the production stability.

Table 2 shows the above results. In Table 2, the uniformity and reproducibility were based on Comparative Example 1 (a), and the production stability was based on Comparative Example 1 (b).
The case of 0% improvement was A, the case of 20-30% improvement was B, the case of 30-40% improvement was C, and the case of 40% or more improvement was D. As can be seen from Table 2, it was found that increasing the rotation speed in the change region improved the uniformity and reproducibility of the deposited film, and showed that the base material was formed only when the change region was formed instead of the entire deposited film. It was confirmed that the production stability was improved by increasing the rotation speed of the above, and the excellent effect of the deposited film forming method of the present invention was confirmed.

Example 2 Three lots of electrophotographic photosensitive members were manufactured under the same conditions as in Example 1 except that the conditions for forming the deposited film shown in Table 3 were used.

[0063]

[Table 3]

Comparative Example 2 An electrophotographic photoreceptor was manufactured under the same conditions as in Example 2 except that the rotation speed of the substrate was kept constant at 3 rpm throughout the formation of all the layers.

The electrophotographic photosensitive members produced in Example 2 and Comparative Example 2 were evaluated for the above items by the same evaluation method as in Example 1. As a result, Example 2 was compared to Comparative Example 2.
It has been found that the electrophotographic photoreceptor has improved chargeability and sensitivity uniformity B, chargeability reproducibility A, and sensitivity reproducibility B, respectively. Excellent effect was confirmed.

(Example 3) In this example, an electrophotographic apparatus was used under the same conditions as in Example 1 except that the oscillation frequency was changed to a high-frequency electrode of 50 MHz and the deposition film forming conditions shown in Table 4 were used. Three lots of photoconductors were produced.

[0067]

[Table 4]

Comparative Example 3 Example 3 was repeated except that the rotation speed of the substrate was kept constant at 10 rpm throughout the formation of all the layers.
Under the same conditions as in the above, an electrophotographic photoconductor was prepared.

The electrophotographic photosensitive members produced in Example 3 and Comparative Example 3 were evaluated for the above items by the same evaluation method as in Example 1. As a result, as compared with Comparative Example 3, the electrophotographic photoreceptor of Example 3 had a chargeability and uniformity of B, a uniformity of sensitivity of C, a reproducibility of chargeability of B, and a reproducibility of sensitivity of C. Each of them was found to be improved, and the excellent effect of the deposited film forming method of the present invention was confirmed.

[0070]

As described above, according to the present invention, a deposited film is formed under a predetermined forming condition and other forming conditions different from the predetermined forming condition, and the deposited film is formed under another forming condition. In this case, the rotation speed of the substrate is set to be higher than the rotation speed of the substrate when the deposited film is formed under predetermined forming conditions, so that the uniformity and reproducibility of the deposited film can be improved. It can be realized under excellent production stability, and as a result, it becomes possible to stably produce semiconductor devices and electrophotographic photoreceptors with excellent characteristics at low cost.

[Brief description of the drawings]

FIG. 1 is a schematic configuration diagram illustrating an embodiment of a manufacturing apparatus (deposited film forming apparatus) for an electrophotographic photosensitive member of the present invention.

FIG. 2 is a diagram illustrating an example of an electrophotographic photoconductor.

FIG. 3 is a schematic configuration diagram illustrating an example of a conventional apparatus for manufacturing a photoconductor for electrophotography.

FIG. 4 is a cross-sectional view showing a cross section of a deposited film forming apparatus in the apparatus shown in FIG.

FIG. 5 is a diagram illustrating an example of an electrophotographic photoconductor.

[Explanation of symbols]

 REFERENCE SIGNS LIST 100 deposited film forming apparatus 101 cylindrical substrate 102 reaction vessel 103 substrate support 104 source gas supply system 105 exhaust system 106 power supply system 107 exhaust pump 108 exhaust valve 109 main exhaust valve 110 throttle valve 111 oil diffusion pump 112 main exhaust pump 113 Power source 114 Cathode 115 Matching box 116 Motor 117 Source gas supply pipe 118 Driving unit 119 Exhaust port 120 Substrate rotation control device 201 Base 202 Charge injection blocking layer 203 Photoconductive layer 204 Surface layer 205 Change area of charge injection blocking layer 206 Surface layer Area of change

 ──────────────────────────────────────────────────続 き Continuing on the front page (72) Inventor Jin Murayama 3-30-2 Shimomaruko, Ota-ku, Tokyo Within Canon Inc. (72) Inventor Tatsuyuki Aoike 3-30-2 Shimomaruko, Ota-ku, Tokyo Kia Non-corporation F term (reference) 2H068 EA25 EA30 FA11 FA30 4K030 AA06 AA09 AA17 BA30 CA02 CA16 FA03 GA09 JA18 KA05 LA17 5F045 AA08 AB04 AC01 AC16 AC19 AE15 CA16 EH15 EM10 GB15

Claims (9)

[Claims] 1. A reaction vessel capable of containing at least a substrate and capable of being decompressed, a gas supply means for introducing a raw material gas into the reaction vessel, an exhaust means for exhausting the reaction vessel, and decomposing the introduced gas. A deposition film forming apparatus for forming a deposition film on the substrate, comprising: a power introduction unit for introducing electric power; and a substrate rotation unit for rotating the substrate, wherein the source gas introduction unit, the exhaust unit, and the power supply An apparatus for forming a deposited film, comprising: substrate rotation control means for controlling said substrate rotation means in conjunction with control of at least one of the means. 2. The deposited film forming apparatus according to claim 1, wherein said reaction container has a configuration in which a plurality of said substrates are installed. 3. An oscillation frequency of said power introduction means is 50M.
The deposition film forming apparatus according to claim 1, wherein the frequency is in the range of Hz to 450 MHz. 4. A rotatable substrate is provided in a reaction vessel that can be decompressed, and a raw material gas supplied into the reaction container is decomposed by electric power introduced from a power introduction unit to form a deposited film on the substrate. In the method for forming a deposited film, the step of forming a deposited film on the substrate includes the step of forming the deposited film under predetermined forming conditions and the step of forming the deposited film under other forming conditions different from the predetermined forming conditions. Forming the deposited film under the other forming conditions, wherein the rotational speed of the substrate is set to be smaller than the rotational speed of the substrate in the step of forming the deposited film under the predetermined forming conditions. A method for forming a deposited film, wherein the method is also fast. 5. The deposited film forming method according to claim 4, wherein the forming conditions of the deposited film are changed during the step of forming the deposited film under the other forming conditions. 6. The conditions for forming the deposited film include the type of the source gas supplied into the reaction vessel, the supply flow rate of the source gas, the pressure in the reaction vessel, and the electric power introduced into the reaction vessel. The method for forming a deposited film according to claim 4, wherein the method is at least one. 7. The deposited film forming method according to claim 4, wherein a plurality of said substrates are provided in said reaction vessel, and said deposited film is formed simultaneously on said plurality of substrates. 8. An oscillation frequency of 50 MH in the reaction vessel.
The method for forming a deposited film according to claim 4, wherein power of z to 450 MHz is introduced. 9. An electrophotographic photoconductor comprising a deposited film formed by the deposited film forming method according to claim 4. Description: