JP4827608B2 - Deposited film forming apparatus, deposited film forming method, and electrophotographic photoreceptor manufacturing method - Google Patents

Description

  The present invention relates to a deposited film forming apparatus for forming a photoreceptive member using a deposited film, particularly an amorphous or polycrystalline deposited film on a substrate to be processed. The present invention particularly relates to a deposited film forming apparatus for forming a deposited film by a plasma CVD (Chemical Vapor Deposition) method.

  Conventionally, a deposited film for a semiconductor or the like composed of an amorphous material (hereinafter referred to as “amorphous” refers to a non-single crystal) has been proposed, some of which have been put to practical use. Yes. For example, amorphous silicon (hereinafter abbreviated as “a-Si”) compensated for at least one of hydrogen and halogen (for example, fluorine, chlorine, etc.) is used as the light receiving member. Such a light receiving member can be used as an element member in, for example, a semiconductor device, an electrophotographic photoreceptor device, an image input line sensor, an imaging device, a photovoltaic device, other various electronic elements, optical elements, and the like. .

  In forming this kind of deposited film, it is often required to make the deposited film uniform in film thickness and film characteristics. Therefore, it is effective to devise a method for supplying a source gas or to use a plasma CVD method to take a uniform plasma or to rotate a substrate to be processed on which a deposited film is formed. It is shown.

  Also, an apparatus has been proposed in which the arrangement of the source gas supply means and the deposited film forming substrate and the exhaust direction are appropriately defined to improve the utilization efficiency of the source gas and make the deposited film uniform (patent). Reference 1).

  There has also been proposed an electrophotographic photoreceptor manufacturing apparatus in which the electrode is configured to blow out source gas, the direction of the source gas outlet and the outlet is appropriately defined, and the film thickness distribution is made uniform (patent) Reference 2).

We also propose a device that achieves uniform plasma processing by appropriately defining the raw material gas supply means, the material of the electrode components that blow out the raw material gas, and the conductance of the suction port near the periphery of the workpiece. (See Patent Document 3).
Japanese Patent Publication No. 5-32472 Japanese Patent No. 027776087 JP-A-8-153679

  Conventionally, the deposited film has been made uniform by the above-described measures. However, in recent years, the uniformity of the deposited film has been demanded more than ever with the enhancement of the function of the apparatus using such a deposited film, for example, the digitization and colorization of the electrophotographic apparatus. That is, for example, in recent high-quality color apparatuses using an electrophotographic process, the gradation is improved, so that even a non-uniformity of the deposited film, which has not been a practical problem in the past, can be displayed in the formed image. There is a possibility of causing visible unevenness.

  At this time, for example, when a cylindrical deposited film is formed as seen in an electrophotographic photosensitive member, further improvement in uniformity of the film quality in the longitudinal direction is required. In this regard, in the related art as described above, the exhaust gas in the deposited film forming apparatus is not sufficiently considered. That is, it is expected that the uniformity of the plasma processing, particularly the uniformity of the gas flow, can be further improved by making the gas exhaust speed uniform in the longitudinal direction of the deposited film forming apparatus.

  In the deposited film forming apparatus, a powdery by-product is generated when the deposited film is formed. In particular, when a product such as an electrophotographic photoreceptor that requires a relatively large area and a thick deposited film is produced, the by-product may be considerably large. Therefore, the exhaust mechanism of the deposited film forming apparatus is less likely to be clogged by such by-products or to partially affect the exhaust velocity distribution and internal pressure distribution during the deposition film formation. It is required to do.

  In recent years, for example, in an electrophotographic apparatus, a deposited film capable of further improving the electrophotographic characteristics has been required, and as a result, the layer configuration of the deposited film has been diversified. Therefore, the deposited film forming conditions are also complicated. Therefore, when multi-product production is performed, the deposition film forming conditions differ for each product, so it is necessary to optimize the deposited film forming apparatus according to each product. Regarding the uniform gas exhaust rate as described above, it may be necessary to make adjustments according to each product type. Therefore, in order to suppress a decrease in productivity, it is required to easily perform such adjustment.

  The present invention has been made in view of the prior art as described above, and an object of the present invention is to provide a deposited film forming apparatus capable of forming a deposited film having excellent uniformity in film thickness and film characteristics. . Another object of the present invention is to provide a deposited film forming apparatus capable of maintaining stable production quality for a long time even when a thick deposited film is formed.

  In order to achieve the above-described object, a deposited film forming apparatus according to the present invention includes a reaction vessel that can be depressurized, an evacuation unit that can depressurize the reaction vessel, and a substrate holder that holds a substrate installed in the reaction vessel. Means, a source gas introduction means for introducing a source gas for forming a deposited film into the reaction vessel, and an application means for applying discharge energy to excite the source gas to generate excited species. In the deposited film forming apparatus for forming the deposited film, the exhaust means is attached so as to cover an opening formed in at least one direction of the side wall of the reaction vessel, and an exhaust tube mounting plate in which a plurality of holes are formed, A plurality of exhaust pipes detachably fitted in the holes, and is connected via an exhaust part, wherein at least one of the plurality of exhaust pipes has a conductance different from that of the other exhaust pipes. To do.

  According to the present invention, the uniformity of the gas flow in the deposited film forming apparatus is improved, and a deposited film having excellent uniformity of film thickness and film characteristics in the deposited film forming surface of the substrate is obtained over a long period of time. It can be formed stably.

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

  FIG. 1 is a diagram schematically showing an example of a deposited film forming apparatus 110 for manufacturing an electrophotographic photoreceptor by an RF (Radio Frequency) -CVD (Chemical Vapor Deposition) method. 1A is a longitudinal sectional view, and FIG. 1B is a transverse sectional view.

Deposited film forming apparatus 110 is an apparatus for forming a deposited film on the cylindrical substrate 112 by plasma treatment, that form a pressure can be reduced reaction space anti reaction container 111 (cylindrical reaction vessel 111), into the reaction vessel A substrate holder (substrate holding means) 117 that holds the cylindrical substrate 112 is provided.

  The cylindrical substrate 112 only needs to have a material according to the purpose of use. As the material of the cylindrical substrate 112, for example, copper, aluminum, gold, silver, platinum, lead, nickel, cobalt, iron, chromium, molybdenum, titanium, stainless steel, and the like are preferable because of their good electrical conductivity. is there. Among these, aluminum is optimal in consideration of workability and manufacturing cost. In this case, as the aluminum forming the cylindrical substrate 112, it is preferable to use, for example, either an Al—Mg alloy or an Al—Mn alloy.

  A heater 113 is provided inside the base holder 117. Any heater 113 may be used as long as it can be used in vacuum. Specifically, electrical resistance heating elements such as sheath heaters, plate heaters, ceramic heaters and carbon heaters, heat radiation lamps such as halogen lamps and infrared lamps, and heat exchange means using liquid, gas, etc. as a heat medium Is the target. As the surface material of the heater 113, metals such as stainless steel, nickel, aluminum, and copper, ceramics, heat resistant polymer resins, and the like can be used.

  Further, in the cylindrical reaction vessel 111, a raw material gas introduction pipe (raw material gas introduction means) 114 for introducing the raw material gas into the cylindrical reaction vessel 111 is provided. The source gas introduction pipe 114 extends parallel to the longitudinal direction of the cylindrical base body 112 to be held. The source gas introduction pipe 114 is connected to a gas supply system (not shown). The connection pipe includes a mixing 123 with a mass flow controller (not shown) for adjusting the flow rate of the source gas, and a source gas inflow valve for adjusting the flow rate of the source gas supplied to the source gas introduction pipe 114. 130 is provided.

  A high frequency power source (applying means) 116 is electrically connected to the cylindrical side wall of the cylindrical reaction vessel 111 via a matching box 115 having a matching circuit. This side wall is insulated from the lower plate 118 and the upper lid 119 of the cylindrical reaction vessel 111 by the insulator 131 made of ceramics.

  Further, a rotation support mechanism 105 that rotatably supports a substrate holder 117 that holds the cylindrical substrate 112 is provided below the cylindrical reaction vessel 111. The rotation support mechanism 105 includes a turntable 121 on which the base holder 117 is placed, a support shaft 122 that supports the turntable 121, and a motor 120 that is connected to the support shaft 122 and rotates the turntable 121. Have. Accordingly, the cylindrical base body 112 can be rotated around the support shaft 122 together with the turntable 121 while being mounted on the base body holder 117.

  The exhaust system included in the deposited film forming apparatus 110 includes an exhaust part 124 connected to the cylindrical reaction vessel 111 and an exhaust pipe 128 communicating with the exhaust part 124. A vacuum pump unit (exhaust means) 132 is connected to the exhaust pipe 128 and an exhaust main valve 129 is provided. The cylindrical reaction vessel 111 is attached with a vacuum gauge 133 for measuring the internal pressure. By using these, the inside of the cylindrical reaction vessel 111 can be maintained at a predetermined pressure suitable for each step. As the vacuum pump unit 132, for example, a rotary pump, a mechanical booster pump, or the like can be used.

  The exhaust part 124 is connected to an approximately rectangular opening 125 on the side wall of the cylindrical reaction vessel 111 via an insulator 131. The exhaust portion 124 has a hollow structure, and an exhaust tube mounting plate 126 shown in FIG. 3A is attached to the insulator 131 side so as to cover the opening 125. A plurality of holes 126 </ b> A to 126 </ b> I arranged in a substantially straight line in the longitudinal direction of the held cylindrical substrate 112, and thus in the longitudinal direction of the cylindrical reaction vessel 111, are formed in the exhaust tube mounting plate 126 as through holes. Yes.

  An exhaust tube 127 shown in FIG. 3C is fitted in these holes 126A to 126I. The exhaust tube 127 has a collar structure and can be inserted and attached to the holes 126A to 126I from the cylindrical reaction vessel 111 side, and can be easily replaced without removing the exhaust part 124 or the exhaust pipe 128. Is possible. As the exhaust cylinder 127, those having the same outer diameter and different at least one of the length and the inner diameter (opening area) of the cylinder are prepared. The exhaust cylinder 127 selected according to the deposition film formation conditions is prepared before the deposition film formation. Install. Further, some of the holes 126A to 126I can be closed by the plug 301 shown in FIG. 3D, and the number of the exhaust pipes 127 can be changed.

  In the present embodiment, as shown in FIG. 1A, the exhaust pipe 128 is connected to the center of the exhaust portion 124 in the longitudinal direction of the cylindrical base body 112. In this case, the exhaust pipe 127 having the smallest conductance is disposed at the center of the holes 126A to 126I that is closest to the exhaust pipe 128, and the exhaust pipe 127 having the larger conductance is provided as the distance from the center increases. As a result, the exhaust speed is suppressed from becoming too high at a position close to the exhaust pipe 128, and the exhaust speed at a distant position is suppressed from slowing down. By utilizing this, by using an appropriate exhaust cylinder 127 according to the deposition film forming conditions such as the pressure in the cylindrical reaction vessel 111 and the flow rate of the supply gas, the longitudinal direction of the cylindrical substrate 112 can be increased. Can improve the uniformity.

  In the example shown in FIG. 1 (a), an exhaust pipe 127 having the same inner diameter and different lengths is used, and the center one is the longest and the one farther from the center is shorter. In FIG. 1A, only a small number of exhaust pipes 127 are shown for the sake of brevity. As the exhaust tube 127, ones having the same length and different inner diameters may be used. In this case, the exhaust tube 127 having the smallest inner diameter is attached to the center, and the exhaust tube 127 having the larger inner diameter is attached to the center. Moreover, you may use the exhaust pipe 127 which changed both length and an internal diameter.

  The exhaust tube mounting plate 126 only needs to have a plurality of holes arranged in the longitudinal direction of the cylindrical reaction vessel 111. For example, as shown in FIG. 3B, the holes may be arranged in a staggered manner. Good. Further, the exhaust tube 127 may be fixed with a screw or the like.

  An example of a procedure for forming a deposited film using the deposited film forming apparatus 110 configured as described above will be described below.

  First, a substrate holder 117 on which a cylindrical substrate 112 is mounted is installed in the cylindrical reaction vessel 111, and the inside of the cylindrical reaction vessel 111 is evacuated by the vacuum pump unit 132. Subsequently, a gas such as Ar or He necessary for heating the cylindrical substrate 112 is introduced into the cylindrical reaction vessel 111 through the mixing 123, the source gas inflow valve 130, and the source gas introduction pipe 114. Then, using the vacuum pump unit 132 and the exhaust main valve 129, adjustment is performed while looking at the vacuum gauge 133 so that the inside of the cylindrical reaction vessel 111 becomes a predetermined pressure. Next, after the predetermined pressure is reached, the temperature of the cylindrical substrate 112 is about 200 [° C.] to 450 [° C.], more preferably about 250 [° C.] to 350 [° C.] by the heater 113 for heating. Control to temperature.

  After the preparation for forming the deposited film is completed by the above procedure, a photoconductive layer is formed on the cylindrical substrate 112.

  For this purpose, first, a heating gas and a raw material gas for forming a deposited film are mixed and introduced through a mixing 123, and the introduced gas is adjusted to have a desired flow rate. At that time, the vacuum pump unit 132 and the exhaust main valve 129 are adjusted while checking the vacuum gauge 133 so that the inside of the cylindrical reaction vessel 111 has a desired pressure of about 13.3 [mPa] to 1330 [Pa]. . This adjustment can be performed, for example, by adjusting the rotation frequency of the mechanical booster pump of the vacuum pump unit 132.

As a source gas used for forming a deposited film, amorphous silicon such as silane (SiH ₄ ), disilane (Si ₂ H ₆ ), silicon tetrafluoride (SiF ₄ ), and disilicon hexafluoride (Si ₂ F ₆ ) is formed. Raw material gas or a mixed gas thereof can be used. As the dilution gas, hydrogen (H ₂ ), argon (Ar), helium (He), or the like can be used. Further, as a characteristic improving gas for changing the band gap width of the deposited film, an element containing a nitrogen atom, an element containing an oxygen atom, a hydrocarbon, a fluorine compound, or a mixed gas thereof may be used in combination. Examples of the element containing a nitrogen atom used at this time include nitrogen (N ₂ ) and ammonia (NH ₃ ). As an element containing an oxygen atom, oxygen (O ₂ ), nitric oxide (NO), nitrogen dioxide (NO ₂ ), dinitrogen oxide (N ₂ O), carbon monoxide (CO), carbon dioxide (CO ₂ ) Etc. Examples of the hydrocarbon include methane (CH ₄ ), ethane (C ₂ H ₆ ), ethylene (C ₂ H ₄ ), acetylene (C ₂ H ₂ ), propane (C ₃ H ₈ ) and the like. Examples of the fluorine compound include germanium tetrafluoride (GeF ₄ ) and nitrogen fluoride (NF ₃ ). Further, for the purpose of doping treatment, a dopant gas such as diborane (B ₂ H ₆ ), boron fluoride (BF ₃ ), or phosphine (PH ₃ ) may be simultaneously introduced into the discharge space.

  Next, after the pressure in the cylindrical reaction vessel 111 is stabilized, the high-frequency power source 116 is set to a desired power, and the high-frequency power is supplied to the cylindrical reaction vessel 111 via the high-frequency matching box 115, thereby Causes a glow discharge. The supplied power can be, for example, an RF band of about 13.56 [MHz] to 45 [MHz], particularly a frequency of 13.56 [MHz]. By this discharge energy, the source gas introduced into the cylindrical reaction vessel 111 is excited to generate excited species, that is, decomposed to form a deposited film mainly containing desired silicon atoms on the cylindrical substrate 112. It is formed.

  In order to form a uniform deposited film, the cylindrical substrate 112 is rotated at the same time as the deposited film is formed or from the stage where the cylindrical substrate 112 is heated. This rotation is about 1 [rpm] to 10 [rpm], for example, 1 [rpm]. By doing so, a uniform deposited film is formed in the circumferential direction of the cylindrical substrate 112.

  As described above, a deposited film is formed on the outer peripheral surface of the cylindrical substrate 112.

After the deposited film is formed, the supply of the source gas and the high frequency power is stopped and the inside of the cylindrical reaction vessel 111 is exhausted. Thereafter, the inside of the cylindrical reaction vessel 111 and the raw material gas introduction pipe 114 is purged using a purge gas, for example, at least one of an inert gas such as Ar and N ₂ . After the purge process is completed, the inside of the cylindrical reaction vessel 111 is returned to atmospheric pressure using at least one of an inert gas such as Ar and N ₂ gas, and the cylindrical substrate 112 is taken out from the cylindrical reaction vessel 111.

  Thereafter, the deposited powdery by-product is cleaned as necessary. As a procedure at that time, first, a dummy dummy substrate for cleaning (not shown) having the same shape is installed in the cylindrical reaction vessel 111 instead of the cylindrical substrate 112, and the cylindrical reaction vessel 111 is formed by the vacuum pump unit 132. Exhaust inside. Subsequently, a cleaning gas necessary for the cleaning process is introduced into the cylindrical reaction vessel 111 via the mixing 123 and the source gas introduction pipe 114. Then, using the vacuum pump unit 132 and the exhaust main valve 129, adjustment is performed while looking at the vacuum gauge 133 so that the inside of the cylindrical reaction vessel 111 becomes a predetermined pressure.

Examples of the cleaning gas used during the cleaning process include CF ₄ , CF ₄ / O ₂ , SF ₆ , and ClF ₃ (chlorine trifluoride). In this embodiment, the cleaning time is shortened. Use ClF ₃ which is effective. In the present embodiment, it is effective to use an inert gas for dilution in order to adjust the concentration of the cleaning gas. Examples of the inert gas include He, Ne, and Ar. Among them, it is preferable to use Ar.

  After the pressure in the cylindrical reaction vessel 111 is stabilized, the high-frequency power supply 116 is set to a desired power, and the high-frequency power is supplied to the cylindrical reaction vessel 111 via the high-frequency matching box 115, whereby high-frequency glow discharge is generated. Raise it. The supplied power can be, for example, an RF band of about 13.56 [MHz] to 45 [MHz], particularly a frequency of 13.56 [MHz]. With this discharge energy, the cleaning source gas introduced into the cylindrical reaction vessel 111 is decomposed, and the inside of the cylindrical reaction vessel 111 is cleaned.

Next, the supply of high frequency power is stopped after the cleaning process, and the inside of the cylindrical reaction vessel 111 is evacuated. Thereafter, the inside of the cylindrical reaction vessel 111 and the raw material gas introduction pipe 114 is purged using a purge gas, for example, at least one of an inert gas such as Ar and N ₂ . After the purge process is completed, the inside of the cylindrical reaction vessel 111 is returned to atmospheric pressure by using at least one of an inert gas such as Ar and N ₂ gas, and a dummy substrate for cleaning (not shown) is removed from the inside of the cylindrical reaction vessel 111. Take out.

  In the deposited film forming apparatus 110 of the present embodiment configured as described above, the exhaust unit 124 is provided in the opening 125 of the side wall of the cylindrical reaction vessel 111 that extends in parallel with the longitudinal direction of the cylindrical substrate 112. A plurality of exhaust pipes 127 are installed at 124. And as the exhaust pipe 127, at least one having a conductance different from the others is used. As a result, the gas flow rate in the cylindrical reaction vessel 111 is reduced by slowing the exhaust speed of the part where the gas flow is faster than the other parts by exhausting, or increasing the exhaust speed of the part where the gas flow is slow. Can improve the uniformity.

  At this time, in particular, as in the example illustrated in FIG. 1, it is preferable to change the conductance of the exhaust cylinder 127 to be installed according to the distance from the exhaust pipe 128 according to the position of the cylindrical base body 112 in the longitudinal direction. . According to this configuration, the uniformity of the longitudinal distribution of the cylindrical substrate 112 in the exhaust velocity can be improved by using the appropriate exhaust cylinder 127 according to the deposition film forming conditions. Thereby, the uniformity of the gas flow in the cylindrical reaction vessel 111 in the longitudinal direction of the cylindrical substrate 112 can be improved. As a result, even when a thick deposited film is formed, the uniformity of the deposited film in the longitudinal direction of the cylindrical substrate 112 can be improved.

  In addition, when performing multi-product production, the same thing can be done by simply exchanging with the exhaust tube 127 selected in advance according to each deposited film forming condition in accordance with the deposited film forming conditions that differ for each type of deposited film to be formed. Good production is possible using the deposited film forming apparatus 110. Therefore, it is not necessary to change the apparatus significantly or use a plurality of apparatuses in accordance with the deposited film forming conditions, and the production cost can be suppressed. Moreover, since the exhaust pipe 127 has a relatively simple configuration, the apparatus cost can be reduced. Further, since the exhaust tube 127 can be easily replaced, it is advantageous in terms of productivity.

  Further, in the configuration in which the exhaust cylinder 127 is used for conductance adjustment, as described above, the conductance can be reduced by lengthening the exhaust cylinder 127 in addition to reducing the inner diameter of the exhaust cylinder 127. Therefore, the inner diameter of the exhaust tube 127 can be set to be relatively large as compared with the case where the conductance is adjusted only by the size of the opening and the slit. Furthermore, since the exhaust velocity distribution can be adjusted by the exhaust cylinder 127, the exhaust part 124 and the exhaust pipe 128 do not need to have a complicated configuration, and can have a simple configuration. Therefore, according to the present embodiment, powdery by-products generated during the formation of the deposited film are deposited on the exhaust pipe 127, the exhaust part 124, and the exhaust pipe 128, and the exhaust conductance changes, Occurrence of blockage can be suppressed. Therefore, even when a thick deposited film with a relatively large area is formed over a long period of time, such as an electrophotographic photoreceptor, it is possible to maintain a gas flow at the initial stage of deposited film formation and form a deposited film stably. It becomes.

  In the present embodiment, the exhaust portion 124 is disposed in the circumferential direction on the opposite side of the raw material gas introduction pipe 114 with the cylindrical base body 112 in view of gas utilization efficiency and simplification of the apparatus. It is desirable to do. Further, as described above, a plurality of exhaust cylinders 127 may be disposed in the longitudinal direction of the cylindrical base body 112 in the exhaust part 124. However, in terms of uniformity in the longitudinal direction, the exhaust cylinders 127 are substantially linear in the longitudinal direction. It is preferable to arrange in.

In the present embodiment, the distance (exhaust region, L1 in FIG. 1) from one end to the other end of the cylindrical base body 112 in the longitudinal direction of the exhaust portion 124 is the longitudinal direction of the cylindrical base body 112 to be installed. It is preferable from the surface of the uniformity of a longitudinal direction that it is 1 time or more of length (L2 in FIG. 1). However, since it is preferable that the deposited film forming apparatus 110 is smaller in terms of apparatus cost and gas utilization efficiency, it is preferable that “L1” is 2.5 times or less of “L2”.

  Further, in the present embodiment, the feeding point of the discharge energy for exciting the source gas to generate the excited species is provided on the opposite side of the exhaust part 124 with the cylindrical base 112 interposed therebetween, so that the source gas can be efficiently used. Since discharge energy can be given, it is preferable. As a result, the uniformity of plasma in the discharge space is improved.

  Next, another specific embodiment of the present invention will be described with reference to FIG.

  FIG. 2 is a diagram schematically showing an example of a deposited film forming apparatus 210 for manufacturing an electrophotographic photosensitive member by RF (Radio Frequency) -CVD (Chemical Vapor Deposition), as in FIG. is there. 2A is a longitudinal sectional view, and FIG. 2B is a transverse sectional view. 2, the same parts as those in FIG. 1 are denoted by the same reference numerals, and detailed description thereof is omitted.

  2 is different from FIG. 1 in that the connection position of the exhaust pipe 128 to the exhaust part 124 is different. That is, in this embodiment, the exhaust pipe 128 is connected to one end surface of the exhaust portion 124 in the longitudinal direction of the cylindrical base body 112, and in the example shown in FIG. In this case, as the exhaust pipe 127, the one having a conductance that is smaller toward the lower side of the figure and that becomes larger toward the upper side is used.

  As in the present embodiment, by connecting the exhaust pipe 128 to one end surface of the exhaust base 124 in the longitudinal direction of the cylindrical substrate 112, in the longitudinal direction of the cylindrical substrate 112, and thus in the longitudinal direction of the cylindrical reaction vessel 111. It is possible to prevent the device from becoming large in the intersecting direction. As a result, the floor area occupied by the deposited film forming apparatus 210 can be reduced, and the apparatus cost can be reduced. Even in this configuration, it is possible to improve the uniformity of the deposited film in the longitudinal direction by selecting the number of exhaust cylinders 127 and at least one of the length and inner diameter of each exhaust cylinder 127 according to the deposition film forming conditions.

  EXAMPLES Hereinafter, although an Example demonstrates this invention further in detail, this invention is not limited at all by these. In the following description, the same reference numerals are used for the same portions as those shown in the above-described embodiments.

Example 1
The deposited film forming apparatus 110 shown in FIG. 1 is used to form an amorphous layer structure shown in FIG. 4 on a cylindrical substrate 112 made of aluminum having a diameter of 80 mm, a length of 358 mm, and a thickness of 3 mm under the conditions shown in the table of FIG. A silicon deposited film (hereinafter abbreviated as an electrophotographic photosensitive member) was formed. In FIG. 4, reference numeral 401 denotes a component of the cylindrical substrate 112, reference numeral 402 denotes a lower blocking layer (first layer), reference numeral 403 denotes a photoconductive layer (second layer), and reference numeral 404 denotes a surface layer (third layer). Layer).

  In this embodiment, as shown in FIG. 3A, the exhaust tube 127 and the plug 301 are attached to the exhaust tube mounting plate 126 having exhaust tube mounting holes at nine locations. The inner diameters of the exhaust cylinders 127 used were all equal to 20 mm, and the exhaust conductance was adjusted by changing the length of the exhaust cylinder 127. The arrangement of the exhaust tube 127 is shown in the table of FIG. The exhaust region in the table of FIG. 9 indicates the distance “L1” in the longitudinal direction between the attached exhaust cylinders 127 at both ends in the longitudinal direction. In this embodiment, the cylindrical base 112 is used. Is the same as the length “L2”.

  With respect to the produced electrophotographic photosensitive member, evaluation of “thickness bus bar unevenness”, “Vd bus bar unevenness”, “Vh bus bar unevenness”, and “white spot” was performed as follows. In addition, “apparatus cost” was also evaluated.

Evaluation of “thickness bus line unevenness” Using a film thickness meter (Fisher Instruments, FISCO SCOPE MMS), the film thickness was measured at 35 points at 10 mm intervals in the longitudinal direction of the electrophotographic photosensitive member, and the measured values at the 35 points. The difference between the maximum value and the minimum value was evaluated as film thickness bus unevenness. At this time, the value of the film thickness at each point in the longitudinal direction was the average value of the measured values at four points at intervals of 90 degrees in the circumferential direction. Evaluation was carried out by relative evaluation when the result obtained in Comparative Example 1 described later was taken as 100. In other words, the smaller the number, the better the evaluation result.

Evaluation of “Vd bus line unevenness” and “Vh bus line unevenness” A copy machine (iR5000 manufactured by Canon Inc.) was used for evaluating these electrophotographic photosensitive member characteristics. FIG. 7 shows a schematic diagram of the copying machine. In FIG. 7, an electrophotographic photosensitive member 701 is supported so as to be rotatable in the clockwise direction in the figure. Around the electrophotographic photoreceptor 701, a pre-exposure device 708 for forming an electrostatic latent image, a main charger 702, a potential sensor 703, and a latent image forming exposure device 709 are sequentially arranged in the clockwise direction. ing. Next, a developing unit 704 for performing development by attaching toner on the electrostatic latent image, a transfer charging unit 705a for transferring the toner image to a recording medium, and a separation charging unit 705b are arranged. Thereafter, a cleaner 710 having a cleaning roller 706 and a cleaning blade 707 for removing residual toner is disposed.

  When measuring the characteristics of the electrophotographic photosensitive member, the developing device 704 and the cleaner 710 are removed. Then, a potential probe (Model 344 manufactured by TREK, not shown) capable of measuring the electrophotographic characteristics at a predetermined position in the axial direction of the electrophotographic photosensitive member is attached instead of the developing unit 704 to measure the electrophotographic characteristics of the electrophotographic photosensitive member. To do. The electrophotographic characteristics thus measured were evaluated according to the following criteria.

"Vd bus line unevenness"
The process speed is 265 mm / sec, the amount of pre-exposure (LED with a wavelength of 680 nm) is 4 lx · s, and the surface potential at the middle position in the longitudinal direction of the electrophotographic photosensitive member is 450 V (dark potential) as measured by the potential probe. The current value of the main charger 702 is adjusted. Thereafter, the potential probe is moved in the axial direction from the end of the electrophotographic photosensitive member, and measurement is performed at nine points at intervals of 40 mm in the longitudinal direction. The difference between the maximum value and the minimum value at the nine points is calculated as Vd. It was evaluated as busbar unevenness. Evaluation was carried out by relative evaluation with the result obtained in Comparative Example 1 as 100. In other words, the smaller the number, the better the evaluation result.

"Vh bus unevenness"
The current value of the main charger 702 was adjusted so that the surface potential at the middle position in the longitudinal direction of the electrophotographic photosensitive member was 450 V (dark potential) by the same procedure as the Vd bus line unevenness. Thereafter, image exposure (laser with a wavelength of 660 nm) was irradiated to adjust the light quantity of the image exposure light source so that the surface potential at the middle position measured with the potential probe was 200 V (bright potential). Thereafter, the potential probe is moved in the axial direction from the end of the electrophotographic photosensitive member, and measurement is performed at nine points at intervals of 40 mm in the longitudinal direction. The difference between the maximum value and the minimum value at the nine points is expressed as Vh. It was evaluated as busbar unevenness. Evaluation was carried out by relative evaluation with the result obtained in Comparative Example 1 as 100. In other words, the smaller the number, the better the evaluation result.

Evaluation of “White Pochi” Using a Canon iR5000 copying machine, an image obtained by copying an A3-sized original was observed, and the diameter per electrophotographic photosensitive member was 0.10 mm or more. The number of white spots (portions where no image was formed) was counted. Evaluation was carried out by relative evaluation with the result obtained in Comparative Example 1 as 100. In other words, the smaller the number, the better the evaluation result.

Evaluation of “Device Cost” Relative evaluation was performed with the result obtained in Comparative Example 4 as 100. In other words, the smaller the number, the better the evaluation result.

Ranking of each evaluation result Each evaluation result was ranked according to the following criteria.
☆ ... less than 60 ◎ ... 60 or more and less than 80 ○ ... 80 or more and less than 100 △ ... 100 (same as Comparative Example 1)
× ... Over 100 Overall evaluation For the evaluation results of the above five items ("Thickness bus unevenness", "Vd bus unevenness", "Vh bus unevenness", "White potty", "Equipment cost") went.
☆ ・ ・ ・ Each item is 4 or more levels ◎ ・ ・ ・ Each item is ◎ 4 or more levels ○ ・ ・ ・ Each item is more than 4 levels △ ・ ・ ・ Each item is △ level 4 or more in the above × △ Level 3 or more in each item However, if there is at least one in each item, the overall evaluation is △, if there is at least one in each item, the overall evaluation is × And

  The results of each evaluation and comprehensive evaluation are shown in the table of FIG.

(Example 2)
The exhaust tube 127 and the plug 301 are changed to the arrangement shown in the table of FIG. 9 with respect to Example 1, and the electrophotographic photosensitive member is manufactured by setting the exhaust region to 1.5 times the base length. Similar evaluations were made. The results are shown in the table of FIG.

(Example 3)
The exhaust tube 127 and the plug 301 are changed to the arrangement shown in the table of FIG. 9 with respect to Example 1, and the electrophotographic photosensitive member is manufactured by setting the exhaust region to twice the base length. Evaluation was performed. The results are shown in the table of FIG.

Example 4
Compared to Example 1, the same exhaust cylinder 127 having a length of 20 mm was used, the exhaust conductance was adjusted with the inner diameter of the exhaust cylinder 127, and the arrangement shown in the table of FIG. Evaluation similar to Example 1 was performed. The results are shown in the table of FIG.

(Example 5)
Compared to Example 1, the same exhaust cylinder 127 having a length of 80 mm was used, the exhaust conductance was adjusted by the inner diameter of the exhaust cylinder 127, and the arrangement shown in the table of FIG. Evaluation similar to Example 1 was performed. The results are shown in the table of FIG.

(Example 6)
Compared to Example 1, the same exhaust cylinder 127 having a length of 150 mm was used, the exhaust conductance was adjusted by the inner diameter of the exhaust cylinder 127, and the arrangement shown in the table of FIG. Evaluation similar to Example 1 was performed. The results are shown in the table of FIG.

(Comparative Example 1)
Using the deposited film forming apparatus 510 shown in FIG. 5, an electrophotographic photosensitive member was produced on a cylindrical substrate 512 made of aluminum having a diameter of 80 mm, a length of 358 mm, and a thickness of 3 mm, and the same evaluation as in Example 1 was performed. went. The results are shown in the table of FIG.

  The deposited film forming apparatus 510 used in this comparative example is different from the deposited film forming apparatus 110 of the embodiment corresponding to the present invention shown in FIG. 1 in that the exhaust tube mounting plate 126 and the plate 526 having slit-shaped openings are used. It is different in that it is replaced with. In this comparative example, the slit of the plate 526 has a width of 20 mm, and the slit length, that is, the exhaust region, is the same as the base length.

(Comparative Example 2)
Compared to the first embodiment, the exhaust tube 127 is 40 mm in length and the same, and therefore the inner diameter is the same, so the same conductance is used to produce an electrophotographic photosensitive member. Similar evaluations were made. The results are shown in the table of FIG.

(Comparative Example 3)
Compared to Example 1, the same exhaust cylinder 127 having a length of 10 mm was used, the exhaust conductance was adjusted by the inner diameter of the exhaust cylinder 127, and the arrangement shown in the table of FIG. Evaluation similar to Example 1 was performed. The results are shown in the table of FIG.

(Comparative Example 4)
Using the deposited film forming apparatus 610 shown in FIG. 6, an electrophotographic photosensitive member was produced on a cylindrical substrate 512 made of aluminum having a diameter of 80 mm, a length of 358 mm, and a thickness of 3 mm, and the same evaluation as in Example 1 was performed. went. The results are shown in the table of FIG.

  The exhaust system of the deposited film forming apparatus 610 shown in FIG. 6 includes three exhaust pipes 601A to 601C connected to the side wall of the cylindrical reaction vessel 111 at positions separated in the longitudinal direction of the cylindrical substrate 112. Yes. Each of the exhaust pipes 601A to 601C is provided with conductance valves 602A to 602C and pressure gauges 604A to 604C for measuring the pressure on the cylindrical reaction vessel 511 side. The exhaust pipes 601 </ b> A to 601 </ b> C join the common collective pipe 628 and are connected to the vacuum pump unit 132 via the exhaust main valve 129.

  In this comparative example, the exhaust pipe 601B is disposed at a position corresponding to the center in the longitudinal direction of the cylindrical base body 112, and the exhaust pipes 601A and C are disposed at positions corresponding to both ends. That is, the exhaust region is the same as the base length.

  In this comparative example, the conductance valve was controlled so that the pressures of the pressure gauges 604A to 604C were the same during the formation of the deposited film.

  As apparent from the table of FIG. 11, the uniformity of the deposited film in the longitudinal direction of the cylindrical substrate is greatly improved by adjusting the exhaust conductance in the longitudinal direction of the reaction vessel according to the present invention with respect to each bus unevenness. (Comparative Examples 1 and 2 versus Examples 1, 4, 5, and 6). Furthermore, the uniformity was improved by increasing the number of exhaust pipes to be installed and expanding the exhaust region (Example 2). However, in Example 2 and Example 3, the results were the same with respect to the bus line unevenness, and it was found that the effect was small even if the exhaust region was made larger than 1.5 times the base length.

  When the exhaust tube was used in the same manner as in the present invention and the exhaust tube had an inner diameter of 12 mm (Comparative Example 3), the bus-line unevenness deteriorated. This is a result of a change in the exhaust conductance because the inner diameter of the exhaust tube is too small and by-products are deposited on the exhaust tube during the formation of the deposited film. Since this phenomenon does not occur when the inner diameter is 14 mm or more, it can be seen that the exhaust tube needs to have an inner diameter of 14 mm or more. Therefore, it is necessary to adjust the conductance by the length of the exhaust tube so that the inner diameter of the exhaust tube becomes 14 mm or more.

  Even if the inner diameter is increased as in Examples 5 and 6, the bus bar unevenness is good and can be further increased. However, the outer diameter of the exhaust pipe is limited by the interval between the exhaust pipes, and thus the inner diameter is also limited. The length of the exhaust pipe is limited by the depth of the exhaust section, etc. There are practical limitations on the size and length. In the present embodiment, the inner diameter can be set up to a maximum of 80 mm, but the inner diameter is preferably 50 mm or less because of the limitation of the length and the ease of adjusting the exhaust conductance.

  About the length of an exhaust pipe, since it is set as the fitting structure in the Example of this invention, it is preferable to set it as 10 mm or more so that it may become stable at the time of fitting, and it is preferable to set it as 300 mm or less from the ease at the time of replacement | exchange.

  In Comparative Example 4, the same effects as those of Examples 1, 4, 5 and 6 of the present invention are obtained. However, since the by-product accumulates on the conductance valve during the formation of the deposited film, the opening degree is gradually increased. There is a need to increase the size and control is difficult.

  Regarding the white spot, it was reduced by the present invention (Examples 1, 4, 5, and 6). Further reduction was achieved by increasing the number of exhaust tubes and expanding the exhaust region (Example 2, Example 3). About this reason, it estimates as follows. First, as described above, according to the present invention, it is speculated that the uniformity of the deposited film on the substrate is improved, while the uniformity of the deposited film deposited on the substrate other than the substrate is also improved. As a result, the strain such as internal stress in the deposited film, which had been generated in the past, has been reduced, so the adhesion of the deposited film has been improved, and the film peeling of the deposited film deposited on the substrate other than the substrate during the formation of the deposited film has been reduced. Guessed. Secondly, if the exhaust region is widened, the regions where the gas flow rate is slow in the upper and lower portions of the cylindrical reaction vessel 111 decrease. In the cylindrical reaction vessel 111, the upper and lower regions where the gas flow rate is slow accumulates a large amount of powdery by-products, but since this region decreases, the amount of powdery by-products deposited decreases, and the cylinder during deposition film formation is reduced. It is presumed that the adhesion to the substrate is reduced.

  Regarding the apparatus cost, the comparative example 4 has a complicated apparatus configuration, whereas each example that can reduce the bus line unevenness to the same level or more is composed of a relatively simple apparatus structure. It can be seen that this is also effective in reducing the device cost.

It is sectional drawing which shows typically an example of the deposited film formation apparatus which concerns on this invention. It is sectional drawing which shows typically an example of the deposited film formation apparatus which concerns on this invention. It is a schematic diagram which shows an exhaust pipe mounting plate, an exhaust pipe, and a stopper based on this invention. It is a schematic diagram showing an example of a layer structure of an amorphous silicon electrophotographic photoreceptor. It is sectional drawing which shows typically the deposited film forming apparatus of a comparative example. It is sectional drawing which shows typically the deposited film formation apparatus of another comparative example. FIG. 2 is a schematic view of a copying machine used for evaluating electrophotographic photosensitive member characteristics. It is a table | surface which shows the deposited film formation conditions in an Example and a comparative example. It is a table | surface which shows arrangement | positioning of the exhaust pipe in each Example and a comparative example. It is a table | surface which shows arrangement | positioning of the exhaust pipe in each Example and a comparative example. It is a table | surface which shows the evaluation result of each Example and a comparative example.

Explanation of symbols

111 reaction vessel 114 source gas introduction pipe (source gas introduction means)
116 High frequency power supply (applying means)
117 Substrate holder (Substrate holding means)
125 Opening portion 126 Exhaust tube mounting plate 127 Exhaust tube 126A to I hole 132 Exhaust pump unit (exhaust means)

Claims (7)

A reaction vessel capable of depressurization, an evacuation unit capable of depressurizing the inside of the reaction vessel, a substrate holding unit for holding a substrate installed in the reaction vessel, and a raw material gas for forming a deposited film in the reaction vessel In a deposited film forming apparatus for forming a deposited film on the substrate, comprising source gas introducing means for introducing and applying means for applying discharge energy for generating excited species by exciting the source gas,
The exhaust means is attached so as to cover an opening formed in at least one direction on the side wall of the reaction vessel, and is attached to an exhaust tube mounting plate in which a plurality of holes are formed, and is detachably fitted in the holes. A plurality of exhaust pipes, and connected via an exhaust part having
At least one of the plurality of exhaust cylinders has a conductance different from that of the other exhaust cylinders.   2. The deposited film forming apparatus according to claim 1, wherein the plurality of exhaust cylinders can be replaced with another exhaust cylinder having at least one of an opening area and a length or a plug closing a hole of the exhaust cylinder mounting plate. 3. The deposited film according to claim 1, wherein a distance between the exhaust pipes located at both ends when viewed in the longitudinal direction of the substrate is not less than 1 and not more than 2.5 times the length in the longitudinal direction of the substrate. Forming equipment. The deposited film forming apparatus has an exhaust pipe connecting the said exhaust means and the exhaust unit, the exhaust pipe is longer the distance from the exhaust pipe, or of the conductance is greater claim 1-3 2. The deposited film forming apparatus according to item 1 . The chimney is cylindrical, inner diameter of 14mm or more 50mm or less, and is 10mm or more 300mm or less long according to claim 1 deposited film forming apparatus according to any one of 4. In the deposited film forming method for forming a deposited film on a body, and forming the deposited film on the substrate using the deposited film forming apparatus according to any one of claims 1 to 5 Deposited film forming method. In the manufacturing method of the electrophotographic photosensitive body which forms a deposited film on a base | substrate and manufactures an electrophotographic photosensitive body, the said film | membrane is formed on the said base | substrate using the deposited film forming apparatus of any one of Claims 1-5. A method for producing an electrophotographic photoreceptor, comprising forming a deposited film.

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