JP2013006258A - Surface treatment method and method for manufacturing electrophotographic photoreceptor - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a surface treatment method that prevents residue of abrasives and suppresses embedment and rubbing of fine powder and burrs generated from a workpiece while maintaining the ability of removing such an adhered matter as a deposited film, by honing processing at a high level, to obtain a clean surface of the workpiece.SOLUTION: The honing processing uses at least two injection guns for honing processing at one time with respect to one workpiece in one processing container, injects one or more sorts of abrasives having a Mohs hardness higher than that of the workpiece and one or more sorts of abrasives having a Mohs hardness lower than that of the workpiece from respective injection guns, and processes the surface by blasting a part to be processed with the abrasives in the order of one having a higher Mohs hardness.

Description

The present invention relates to a surface treatment method for obtaining a clean surface by spraying a large number of abrasives on the surface of a material to be treated to remove a film adhered to the surface of the material to be treated.
The present invention also relates to a method for producing an electrophotographic photosensitive member using a substrate holder treated according to the present invention.

Conventionally, when removing an adhesion film such as rust and metal, a deposition film, an oxide film, and dirt attached to a surface of a material to be processed such as a deposited film manufacturing apparatus component, it is processed by a peening treatment method such as honing and blasting.
In this type of processing method, for example, fine glass particles are used as an abrasive, and this is sprayed onto the surface of the material to be processed with compressed air together with water to polish the surface of the material to be processed. As the abrasive, ceramic, glass, metal, resin, fine particles such as ice and dry ice are used depending on the application.

  The shape, size, hardness, specific gravity, spraying pressure, spraying speed, spraying amount, suspension concentration, etc. of the abrasive are appropriately controlled according to the required surface finish. However, if the ability to remove the adhesion film is increased, the following problems occur. That is, the occurrence of re-adhesion increases in that the abrasive residue remains on the surface of the material to be processed, or the attached film is embedded or slid into the material to be processed (hereinafter also referred to as “fine powder adhesion”). In order to suppress this, Patent Document 1 discloses a method of cleaning by performing fine powder removal and deposit removal after the honing process. Patent Document 2 discloses a method in which alum that dissolves in water is used as an abrasive in order to prevent grinding waste such as abrasives and fine powder from remaining in the honing process. Patent Document 3 discloses a method for obtaining surface uniformity by honing a material to be processed in a plurality of injection directions. In Patent Document 4, in order to obtain a uniform and smooth surface with a minute average roughness, two impact guns are used and the impact force on the first stage is made larger than that on the second stage for a plurality of times. A method of processing is disclosed.

JP 2007-108395 A JP 2004-314273 A JP 2002-361557 A JP-A-6-67441

  However, the following problems remain in the above prior art. In the method of Patent Document 1, although the effect of fine powder removal and adhering matter removal can be obtained, an increase in the process sometimes becomes a problem. In the method of Patent Document 2, although the effect of preventing the remaining of the abrasive is obtained, the ability to remove the attached film of the material to be processed may be insufficient. In the method of Patent Document 3, although the effect of obtaining surface uniformity is recognized, fine powder adhesion sometimes becomes a problem. In the method of Patent Document 4, although the effect of obtaining a surface having a uniform average roughness can be obtained, adhesion of fine powder sometimes becomes a problem.

An object of the present invention is to solve the above problems, and to provide a surface treatment method for efficiently removing an adhesion film and obtaining a clean surface.
That is, the present invention aims to provide a surface treatment method for obtaining a clean surface to be treated while suppressing adhesion of fine powders while maintaining a high level of deposit removal ability such as a deposited film by honing treatment. And

In addition, the present invention can efficiently remove the adhesion film adhering to the parts used in the deposited film manufacturing apparatus by the plasma CVD method and obtain a clean surface of the material to be processed. An object of the present invention is to provide a surface treatment method capable of suppressing the occurrence of film defects.
The film defect referred to here is an abnormal growth of the film based on the dust adhering to the substrate.

  In order to solve the above problems, the surface treatment method according to the present invention performs surface peeling or deposit removal on a material to be treated by a honing treatment using an abrasive. At least two honing treatment spray guns are simultaneously used for one material to be treated in one processing container, and at least one kind of abrasive having a Mohs hardness greater than the material to be treated and Mohs hardness to be processed It is characterized in that at least one kind of abrasive material smaller than the material is sprayed from individual spray guns, and sprayed onto the processing target in order from the abrasive material having the largest Mohs hardness.

According to the surface treatment method of the present invention, a very good clean surface can be obtained very efficiently. It can be suitably used for removing attached films such as components used in the plasma CVD apparatus, deposition preventing plate, substrate stage, and substrate holder.
Furthermore, in the method for producing an amorphous silicon electrophotographic photoreceptor using the plasma CVD method, the surface treatment of the substrate holder is performed by the surface treatment method of the present invention, whereby an electrophotographic photoreceptor capable of high image quality with very few image defects is obtained. Obtainable.

Schematic diagram for explaining an apparatus configuration for carrying out the processing method of the present invention. Schematic diagram illustrating the trace processing that can be used in the processing method of the present invention. Schematic diagram showing an example of an electrophotographic photoreceptor manufacturing apparatus Schematic diagram for explaining the arrangement of spray guns when surface-treating the substrate holder Schematic diagram showing an example of the layer structure of an electrophotographic photosensitive member The schematic diagram which showed an example of the honing processing apparatus which can be used for the processing method of this invention Schematic diagram illustrating an example of a magnetic abrasive separation and recovery device Schematic diagram explaining the configuration of the substrate holder Schematic of an abrasive collection container that can be used when measuring abrasive collision mass Schematic diagram of impeller-type flow velocity measuring device for measuring jet velocity

  The present inventors have studied by paying attention to the hardness of the material to be treated and the abrasive used for the honing treatment. Hardness includes Rockwell hardness, Vickers hardness, Mohs hardness, Martens hardness, Bianel hardness and the like. Rockwell hardness and Vickers hardness are indentation hardness, and Mohs hardness, Martens hardness and Bianel hardness are scratch hardness. The present inventors considered that the scratch hardness should be noted from the viewpoint of suppressing fine powder adhesion. The Martens hardness and the Bianel hardness are determined by the size of the scratches of the diamond indenter. In this study, in order to pay attention to the fact that fine-grained abrasives generate fine powder and burrs of the material to be treated, the examination was conducted focusing on Mohs hardness which is qualitative but can directly compare materials. As a result, it has been found that when the honing process is performed with an abrasive having a smaller Mohs hardness than the material to be treated, adhesion of fine powder is reduced.

However, when an abrasive having a low Mohs hardness is used, the ability to remove the attached film is small, and even if the processing time is extended, it may not be sufficiently removed. On the other hand, it was found that when an abrasive having a Mohs hardness greater than that of the material to be treated was used, the attached film removal ability was sufficient, but there was much fine powder adhesion. Further, it was found that if the honing process is continued even after the adhered film is removed, the fine powder adhesion further increases.
The present inventors further confirmed that when the material to which the fine particles adhere was subjected to a honing process with an abrasive having a smaller Mohs hardness than the material to be treated, the fine powder adhesion after the treatment decreased. This is considered to be due to the following actions. First, since the Mohs hardness of the abrasive is smaller than that of the material to be treated, it is considered that the occurrence of burrs and fines in the material to be treated is very small. In the state where fine dust and burrs of the material to be treated are embedded or rubbed into the material to be treated, if an abrasive having a low Mohs hardness is sprayed, the fine powder or burrs that have been buried or rubbed in will be scraped off. It seems that it can be removed. Furthermore, since it is difficult to damage the surface of the material to be treated when scraping, it is considered that new burrs and fine particles are hardly generated.

Therefore, the present inventors have further intensively studied a surface treatment method in which the adhesion film is efficiently removed, fine powder adhesion is suppressed, and a clean surface can be obtained.
As a result, at least two injection guns for honing treatment are used simultaneously, and at least two abrasives are injected from individual injection guns, and the Mohs hardness of each abrasive and the Mohs hardness of the material to be processed are in a predetermined relationship. As a result, it has been found that a great effect can be obtained with respect to the aforementioned problems.

  That is, the present invention simultaneously uses at least two injection guns for honing treatment for one material to be processed in one processing container, and has at least one kind of abrasive having a Mohs hardness higher than that of the material to be processed. The surface treatment is performed by spraying at least one type of abrasive having a smaller Mohs hardness than that of the material to be treated from individual spray guns and spraying the surface of the material to be treated in descending order of the Mohs hardness.

Here, the surface treatment is performed by spraying the treated material in order from the polishing material having the larger Mohs hardness. After the polishing is performed, the polishing material having the larger Mohs hardness is sprayed on the entire surface of the treated material. It does not indicate only that the next abrasive is sprayed for processing. In the treated portion of the material to be treated, a process using an abrasive having a Mohs hardness greater than that of the material to be treated is performed, followed by a process using an abrasive having a Mohs hardness of less than the previous abrasive. It should be. When two kinds of abrasives are used, the Mohs hardness of the abrasives to be sprayed later is smaller than the Mohs hardness of the agent to be treated.
Even when three or more spray guns are used, it suffices that the surface treatment is performed by spraying the parts to be treated in order from the abrasive having the largest Mohs hardness.

  FIG. 1A shows an example of a processing apparatus that can be used in the present invention. In the surface treatment apparatus, the material 101 to which the adhesion film 104 adheres, the first injection gun 102, and the second injection gun 103 are arranged as shown in the figure. Here, it is assumed that the first injection gun 102 injects an abrasive having a Mohs hardness greater than that of the material to be processed, and the second injection gun 103 injects an abrasive having a Mohs hardness of less than that of the material to be processed.

  Specifically, the Z axis is taken in the normal direction of the material 101 to be processed, and the XY plane is taken as a plane orthogonal to the Z axis. The workpiece 101 is installed with the adhesion film 104 side as the Z-axis plus side, and the spray gun is installed on the Z-axis plus side. In addition, when the material to be processed is moved in the negative direction of the Y axis (the direction opposite to the Y axis arrow), the first injection gun 102 and the second injection gun 103 are arranged in this order from the Y axis positive side. . At that time, the processing target part is arranged in consideration of the center line of the injection gun so that the processing is first performed by spraying from the first injection gun 102 and then processed by spraying from the second injection gun 103. To do. Specifically, before the jet flow blown from the first injection gun 102 and the jet flow blown from the second injection gun 103 hit the surface to be processed, that is, so as not to collide with each other in the positive side space of the Z axis. Place the spray gun.

  Further, as shown in FIG. 1 (a), the central axis of the jet flow blown from the first injection gun 102 and the central axis of the jet flow blown from the second injection gun 103 are spaced at a certain distance 105 on the workpiece. It is preferable to have. As a result, the jet flow blown from the first injection gun 102 and the jet flow blown from the second injection gun 103 collide with each other before reaching the material to be processed 101, resulting in turbulence of the jet flow or mixing of abrasives. Is prevented.

  The region on the material to be treated where the jet flow of the first injection gun 102 collides (collision region 108) and the region on the material to be treated where the jet flow of the second injection gun 103 collide (collision region 109) do not overlap. It is preferable to set the interval 105 as described above. The interval 105 is from the point where the central axis of the jet sprayed from the first injection gun 102 intersects the material 101 to the point where the central axis of the jet sprayed from the second injection gun 103 intersects the material 101. Distance. The specific interval is not uniquely determined because the size of the collision area varies depending on conditions such as the distance between the spray gun and the material to be processed and the discharge amount per unit time from the nozzle. Adjust as appropriate.

Thus, the surface treatment method of the present invention uses at least two spray guns simultaneously for one material to be treated. Then, it is necessary to inject at least one type of abrasive having a Mohs hardness greater than that of the material to be processed and at least one type of abrasive having a Mohs hardness smaller than that of the material to be processed from individual injection guns.
The abrasive preferably has a particle size equivalent to 100-1000 mesh or in the range of 10-100 μm. A fine powder having a specific gravity of 0.5 to 10 and having a spherical shape is preferably used. Examples of the material of the abrasive preferably used include iron, stainless steel, glass, alumina, ferrite, zirconia, chromium oxide, silicon carbide, boron carbide, boron nitride, epoxy resin, nylon, ice particles, and dry ice pellets.

  In the surface treatment of the present invention, the continuous surface treatment of spraying the polishing portion in order from the polishing material having the larger Mohs hardness followed by the spraying of the polishing material having the Mohs hardness larger than the processing material is divided into a plurality of times. Preferably it is done. The removal of the adhered film by spraying an abrasive having a Mohs hardness higher than that of the material to be treated tends to increase fine powder and burrs and increase fine powder adhesion as the spray time becomes longer. Furthermore, a plurality of fine powders and burrs may overlap and be embedded or rubbed. In such a situation, when these fine powders and burrs are removed by spraying an abrasive whose Mohs hardness is lower than that of the material to be treated, the removal is due to the large amount of fine powders and burrs and their overlapping. Hard to do. In particular, the overlapped fine powder and burrs often reduce the removal effect by spraying an abrasive having a Mohs hardness smaller than that of the material to be treated.

  On the other hand, when performing a series of surface treatments in which the surface to be treated is sprayed in order from the abrasive material having the largest Mohs hardness in a plurality of times, the time of one spraying is shortened and the amount of fine dust and burrs generated is suppressed. Can do. In addition, fine powder and burrs overlap and are less likely to be embedded or rubbed. That is, fine powder adhesion is reduced. Therefore, it is possible to remove almost all fine particles and burrs embedded or slid even if the treatment by spraying an abrasive having a smaller Mohs hardness than the material to be treated is performed in a short time.

As described above, a plurality of continuous surface treatments in which one spraying time is shortened, followed by spraying an abrasive having a Mohs hardness greater than that of the material to be treated, followed by spraying the material to be treated in order from an abrasive having a large Mohs hardness. It is preferable to divide the treatment into times to obtain a clean surface state.
Such processing can be performed using a separate processing apparatus for each abrasive, but the processing cost increases because the apparatus cost increases, the apparatus installation area increases, and a process for moving the processing object is required. Will increase. For this reason, in the same container, the surface treatment is carried out by simultaneously using individual spray guns for each abrasive.

  The abrasive used in the present invention is preferably a combination of abrasives that can be separated and recovered and reused to reduce abrasive costs. For example, an abrasive with a Mohs hardness greater than the material to be treated is solid, and an abrasive with a Mohs hardness less than the material to be treated is used by cooling and solidifying an abrasive that becomes liquid or gas at room temperature. An abrasive larger than the material to be treated can be recovered and reused. An abrasive having a smaller Mohs hardness than a material to be treated becomes a liquid or a gas at room temperature. Therefore, mixing with an abrasive having a larger Mohs hardness than the material to be treated is suppressed, and it is suitable for maintaining the effect. In addition, normal temperature shall mean the range of 20 degreeC +/- 15 degreeC (namely, 5 degreeC or more and 35 degrees C or less).

  As an abrasive that becomes liquid at room temperature, or an abrasive that becomes gas at room temperature, ice or dry ice can be used because of its strength, required Mohs hardness, ease of handling and availability, and cost. Is preferred. When ice is used as an abrasive, the ice lump is crushed to form fine ice particles and sprayed with water for surface treatment. When dry ice is used as an abrasive, surface treatment is performed by spraying dry ice pellets with an air stream.

Also, an abrasive formed of a magnetic material (hereinafter simply referred to as “magnetic abrasive”) and an abrasive formed of a non-magnetic material (hereinafter also simply referred to as “non-magnetic abrasive”) are used. This is also preferable because it can be separated and recovered and reused.
In addition to the selection of the abrasive material, the degree of the effect of the present invention varies depending on the mass of the abrasive material sprayed on the portion to be processed. Therefore, the present inventors have examined the relationship between the abrasive collision energy per unit area per unit time sprayed on the processing target (hereinafter also simply referred to as “abrasive collision energy”) and the effect of the present invention.

  First, the abrasive mass per unit area (hereinafter, also referred to as “abrasive collision mass”) per unit time sprayed on the portion to be treated was calculated as follows. A point where the central axis of the spray gun intersects with the material to be processed was obtained and designated as point 110. Next, the plane in contact with the material to be processed at the point 110 was taken as the XY plane. Then, a circle S having a diameter of 1 cm centered on the point 110 on the XY plane was determined, and the mass A (g) of the abrasive per unit time reaching the circle S was measured to obtain the abrasive collision mass. . More specifically, the mass A of the abrasive that reaches the circle S for 60 seconds as described above was measured, and the abrasive collision mass was calculated from the following formula.

Abrasive collision mass (D) [g / cm ² · sec] that collides in 1 ^second per square cm ² = A / (0.5 × 0.5 × π × 60)
For the measurement of the mass of the abrasive, an abrasive collection container 901 as shown in FIG. 9 can be used, for example. In FIG. 9, the opening 902 is circular with a diameter of 1 cm. Then, the abrasive collection container 901 is installed so that the center of the opening 902 of the abrasive collection container 901 overlaps with the point 110 and the circular edge of the opening 902 is on the XY plane. In this state, the abrasive is sprayed from the spray gun for a predetermined time, and after a predetermined time, the abrasive in the abrasive recovery container 901 is recovered and the mass of the abrasive is obtained.

Next, the jet velocity incident on the material to be treated was measured with an impeller type speedometer as shown in FIGS. 10 (a) and 10 (b). The central axis 1002 of the jet flow from the spray gun 1001 was applied horizontally to the impeller 1003, the rotational speed of the impeller was measured, and the jet velocity was calculated. Using an impeller 1003 having eight rectangular blades having a blade length of 10 cm and a blade width of 2 cm, the central axis of the jet is at the center of the blade width of 2 cm and 1 cm from the blade tip (position 1005 in FIG. 10B). It installed so that 1002 may inject. The first gear 1009 is installed coaxially with the central shaft 1008 of the impeller 1003, the second gear 1006 is installed so as to mesh with the first gear 1009, and the rotational speed of the second gear 1006 is detected by the magnetoelectric rotation detection. Counting was performed using a measuring instrument 1007 (Ono Sokki AP-981). The central axis 1008 and the central axis 1010 of the second gear 1006 are parallel.
When the number of rotations per second was B, the jet velocity was calculated by the following equation.
18 × π × B [cm / sec]

The abrasive collision energy (E) per 1 cm ² per second was calculated from the following formula by calculating the Z-axis component with the jet velocity as the velocity in the central axial direction of the jet.
(Abrasive collision mass per second) × (Z-axis component of jet velocity) × (Z-axis component of jet velocity) / 2 [g / sec ² ]

  Since the contribution of the velocity in the Z-axis direction that collides with the material to be treated is larger than the contribution of the velocity for rubbing the material to be treated in the Y-axis direction, the polishing energy is calculated by calculating the jet velocity Z-axis. Ingredients were used. The abrasive collision energy depends not only on the speed and amount of the abrasive to be sprayed, but also on the inclination, distance, and spread angle of the spray gun. Therefore, it is preferable to optimally adjust the abrasive collision energy in consideration of these factors. .

  When the abrasive collision energy E1 of the abrasive whose Mohs hardness is larger than that of the material to be treated is smaller than the abrasive collision energy E2 of the abrasive whose Mohs hardness is smaller than that of the material to be treated (E1 <E2), It becomes like this. When E1 is set to a value that can provide sufficient adhesion film removal ability, E2 is too large, and although embedding and rubbing due to spraying of an abrasive whose Mohs hardness is smaller than that of the material to be treated are generated at the same time, There is. Therefore, fine powder adhesion after the surface treatment may be larger than in the case of E1> E2. Further, when E2 is set to a value at which fine powder adhesion does not occur, E1 may be small and the attached film removing ability may be reduced. Here, the abrasive collision energy is obtained from the mass of the abrasive in the mixed liquid when the mixed liquid of water and abrasive is jetted. Further, when only the abrasive is sprayed by air, it is determined from the mass of the abrasive.

The degree of the effect of the present invention varies depending on the angle of spraying of the abrasive with respect to the material to be processed. Specifically, as shown in FIG. 1A, the injection angle 106 (θ1) formed by the Z axis taken in the normal line direction of the workpiece 101 and the central axis of the first injection gun is 0 ° < It is preferable that θ1 ≦ 45 °.
When the injection gun is on the Y axis (−) side with respect to the XZ plane, the angle θ is expressed as a positive value. When the injection gun is on the Y axis (+) side, the angle θ is expressed as a negative value. It was supposed to be indicated. Furthermore, the injection angle 107 (θ2) formed by the Z axis and the central axis of the second injection gun is preferably θ1 ≦ θ2 <90 °. When the injection angle θ1 exceeds 45 °, the component in the vertical direction of the material to be processed of the jet velocity decreases, so that the processing time required for removing the adhered film may be long. In addition, at an injection angle of 0 ° perpendicular to the material to be processed, the abrasive material that once collided with the material to be processed tends to stay in the processing region, and it takes time to be discharged from there. Therefore, there is a case where the abrasive once collided with the material to be treated repeatedly collides with the surface of the material to be treated, resulting in an increase in fine powder adhesion. When the injection angle θ1 is less than 0 °, the central axis direction of the first injection gun and the central axis direction of the second injection gun are reversed, and the abrasive sprayed from each gun is discharged out of the collision area. Facing each other. For this reason, the abrasives collide with each other, and there is a tendency that the residual abrasives, fine powder, burrs are embedded and rubbed. Note that due to the expansion of the jet, there may be a portion where the jet direction faces even if the injection angle θ1 is not less than 0 °. However, since the density of the abrasive and the jet velocity become smaller toward the outside of the jet spread, the above phenomenon hardly poses a problem if it is installed so that the directions of the central axes do not face each other.

  When the injection gun is installed so that θ2 <θ1 as shown in FIG. 1B, the interval 105 is increased due to the apparatus configuration. When the interval 105 is increased, the movement distance of the material to be processed or the spray gun is increased in order to process the entire surface of the material to be processed, resulting in an increase in processing time and an increase in the size of the apparatus. From this point of view, θ1 ≦ θ2 is preferable. Further, when the central axis of the first injection gun and the central axis of the second injection gun are arranged so as to overlap at a certain point between the material to be processed and the injection gun, the spraying is disturbed and stabilized. It becomes difficult to obtain an adhesion film removing ability and a fine powder adhesion suppressing effect. For this reason, the surface condition of the material to be treated after the surface treatment may be uneven.

  As the abrasive, it is particularly preferable to use an approximately spherical abrasive made of iron or stainless steel. Iron or stainless steel has moderate ductility and is less likely to be embedded or rubbed into the material to be processed. Further, the generation of fine powder and burrs in the material to be processed tends to be smaller than when a ceramic abrasive such as SiC or alumina is used. Further, by selecting a substantially spherical abrasive, it is possible to further reduce the generation of fine powder and burrs on the material to be processed.

  The present invention as described above is suitable for obtaining a clean surface by removing an adhesion film on a deposition furnace or a substrate holder made of aluminum or an aluminum alloy, for example, a deposition apparatus for a plasma CVD apparatus. Can be used. Further, the present invention can provide a clean surface by plasma CVD method in removing the adhesion film (surface peeling or deposit removal) of an aluminum alloy substrate holder used for producing an amorphous silicon-based electrophotographic photosensitive member. A surface treatment method is suitable.

The production of an amorphous silicon-based electrophotographic photosensitive member will be described below.
FIG. 3 is a diagram schematically showing an example of an apparatus for depositing a photoreceptor by RF plasma CVD using a high frequency power source. This apparatus is roughly composed of a deposition apparatus 3100 having a reaction vessel 3122, a raw material gas supply apparatus 3200, and an exhaust device (not shown) for depressurizing the reaction container 3122. In the reaction vessel 3122, a conductive substrate 3112 attached to a substrate holder 3121 connected to the ground, a conductive substrate heating heater 3113, and a source gas introduction pipe 3114 are installed. Further, a high frequency power source (not shown) is connected to the cathode electrode 3111 via a high frequency matching box 3115.

The source gas supply device 3200 includes source gas cylinders 3221 to 3225 such as SiH ₄ , H ₂ , CH ₄ , NO, B ₂ H ₆ , CF ₄ , valves 3231 to 3235, pressure regulators 3261 to 3265, and inflow valves 3241 to 3245. And outflow valves 3251 to 3255 and mass flow controllers 3211 to 3215. The source gas cylinders 3221 to 3225 in which each source gas is sealed are connected to a source gas introduction pipe 3114 in the reaction vessel 3122 via an auxiliary valve 3260.

  Next, a method for forming a deposited film using this apparatus will be described. A conductive substrate 3112 that has been degreased and washed in advance is mounted on the substrate holder 3121 that has been treated by the surface treatment method of the present invention, and then placed in the reaction vessel 3122. Next, an exhaust device (not shown) is operated to exhaust the reaction vessel 3122. While viewing the display of the vacuum gauge 3119, when the pressure in the reaction vessel 3122 reaches a predetermined pressure of, for example, 1 Pa or less, power is supplied to the heater 3113 for heating the substrate, and the conductive substrate 3112 is moved from 50 ° C. to 350 ° C., for example. To the desired temperature. At this time, an inert gas such as Ar or He can be supplied from the gas supply device 3200 into the reaction vessel 3122 and heated in an inert gas atmosphere. Next, a gas used to form a deposited film is supplied from the gas supply device 3200 into the reaction vessel 3122. That is, if necessary, the valves 3231 to 3235, the inflow valves 3241 to 3245, and the outflow valves 3251 to 3255 are opened, and the flow rate is set in the mass flow controllers 3211 to 3215. When the flow rate of each mass flow controller is stabilized, the main valve 3118 is operated while viewing the display of the vacuum gauge 3119 to adjust the pressure in the reaction vessel 3122 to a desired pressure. When a desired pressure is obtained, high-frequency power is applied from a high-frequency power source (not shown) and simultaneously the high-frequency matching box 3115 is operated to generate plasma discharge in the reaction space 3110. Thereafter, the high frequency power is quickly adjusted to a desired power, and a deposited film is formed. By performing such an operation a plurality of times, an electrophotographic photosensitive member composed of a plurality of deposited layers can be formed.

  FIG. 5 is a schematic view showing an example of the layer structure of the electrophotographic photosensitive member produced. An electrophotographic photoreceptor 500 shown in FIG. 5 has a structure in which an amorphous silicon-based light receiving layer 502 is deposited on a conductive substrate 501, and the light receiving layer 502 includes a lower injection blocking layer 505, a photoconductive layer 503, An intermediate layer 506 and a surface layer 504 are included. The lower injection blocking layer 505 is preferably provided to block charge injection from the conductive substrate side. In addition, the intermediate layer 506 is preferably provided in order to reduce charge injection from the top and improve the chargeability.

EXAMPLES Hereinafter, although an Example and a comparative example demonstrate this invention further in detail, this invention is not restrict | limited at all by these.
<Example 1>
Eight aluminum alloy plates (5052), two stainless steel plates (SUS304), and two titanium alloy plates (SSAT-64) were prepared as materials to be processed. The material to be treated is a flat plate having a length of 127 mm, a width of 50 mm, and a thickness of 3 mm. A hydrogenated amorphous silicon (hereinafter also referred to as “a-Si: H”) film is deposited by about 5 μm on the prepared metal flat plate under the conditions shown in Table 1 using a deposition apparatus by RF plasma CVD shown in FIG. Thus, a material to be treated with an attached film was prepared. At that time, a metal plate was attached using a substrate processed so that the metal plate could be attached to the cylindrical substrate, and the substrate was placed instead of the conductive substrate 3112 in FIG. One aluminum alloy plate (5052), one stainless steel plate (SUS304), and one titanium alloy plate (SSAT-64) were stored without depositing films.

  Next, the material to be processed on which the a-Si: H film was deposited was subjected to surface treatment under the conditions shown in Table 2. The processing conditions in Table 2 show the abrasive material injected from the first injection gun as abrasive material-1 and the abrasive material injected from the second injection gun as abrasive material-2. In FIG. 1A, the injection angle 106 (θ1) of the first injection gun is 30 °, and the injection angle 107 (θ2) of the second injection gun is 45 °. Further, the nozzle of the spray gun used was an expansion angle of 15 ° and a spray port diameter of 20 mm, and the distance from the spray port of the spray gun to the point where the central axis of the spray gun intersected the workpiece was set to 100 mm. The interval 105 was set to be 120 mm.

In Table 2, the abrasive collision energy per cm ² sprayed from the first spray gun is E1 [g / sec ² ], and the abrasive collision energy per cm ² sprayed from the second spray gun is E2. It is shown as [g / sec ² ]. Mm represents the Mohs hardness of the material to be treated, M1 represents the Mohs hardness of the abrasive 1, and M2 represents the Mohs hardness of the abrasive 2.

For the surface treatment, a treatment apparatus having the configuration shown in FIG. 1 was used. In Example 1, the surface treatment was performed while changing the relationship between the Mohs hardness of the material to be treated and the abrasive. The water sprayed at the same time as the abrasive was 2 L / min, and E1 and E2 were adjusted by adjusting the amount of abrasive to be mixed. In addition, when the abrasive was dry ice, it was sprayed with air without using water.
The particle size of the abrasive used for the first spray gun was equivalent to 120 mesh. Also, the shape of each of them was substantially spherical. As the particle size of the abrasive used for the second spray gun, ice or dry ice having a substantially elliptical shape and passing through a 30th mesh was used. The iron used was approximately spherical with a mesh equivalent to 150 mesh, and the nylon was approximately cylindrical with a mesh equivalent to 30 mesh. As the acrylic, particles obtained by pulverizing a resin having a size corresponding to a 60th mesh were used.

  The treatment material was sprayed as follows. FIG. 2A shows the internal structure of the surface treatment apparatus showing the arrangement of the spray gun and the moving direction of the material to be treated. Processing is performed by the first spray gun 202 in a longitudinal direction of 127 mm of the flat plate, and then the processed material 201 is moved in one direction (direction indicated by an arrow 207) so as to be processed by the second spray gun 203. Surface treatment of the entire surface of the treatment material on which the film was adhered was performed. The moving speed of the material to be treated was 5 mm / second.

  FIG. 2B shows the processing progress direction on the surface of the material to be processed as the moving order of the abrasive collision area 205. The processed material 201 was moved in the negative direction of the Y axis (the direction indicated by the arrow 207) so that the collision area 205 moved from the right end of the processed material 201 in the positive direction of the Y axis. When the processing reaches the left end of the material 201 to be processed, the material 201 to be processed is moved so that the collision area 205 is translated by 15 mm in the X-axis plus direction (X-axis arrow direction). Furthermore, after moving so that a collision area | region may come to the right end of the to-be-processed material 201 (collision area | region 205 '), it processed from the right end of the to-be-processed material 201 toward the left end similarly. Although not shown in FIG. 2B, the collision region 206 is the same. A solid arrow 208 indicates the direction of movement of the collision area during which the abrasive is being injected from the injection gun, and a broken line arrow 209 indicates the direction of movement of the collision area during which the abrasive is not being injected from the injection gun.

Such processing was performed from the end portion in the X-axis direction (the negative side end portion of the X axis) to the other end portion (the positive side end portion of the X axis), and this was performed as a single process. In this way, the processing for tracing with the second injection gun was performed 15 times following the processing for the first injection gun, and the processing was terminated.
In Example 1-7, the moving speed of the material to be processed is set to 0.3 mm / second, and the tracing process for tracing with the second injection gun is performed once after the first injection gun process. Then, the entire surface of the material to be treated was treated (one time treatment). That is, the trace process was performed once and the process was terminated.

実施例１で表面処理した被処理材を以下の方法で評価した。評価結果を表４に示す。

The material to be treated which was surface-treated in Example 1 was evaluated by the following method. The evaluation results are shown in Table 4.

(Adhesion film removal ability evaluation)
The material to be treated after the surface treatment is placed in an ultra-high resolution field emission scanning electron microscope S4800 manufactured by Hitachi High-Technologies Corporation, and Si element is obtained by EPMA (Electron Probe Micro Analyzer) using Genesis manufactured by EDAX. A qualitative analysis was performed. And the mapping analysis of Si element was performed with Genesis software, and the area of the part where Si element was detected was obtained.
The signal peak was confirmed and evaluated under the following measurement conditions.
Acceleration voltage: 20 kV
Irradiation current: 20 nA

Analyze a total of 20 mm ² by arbitrarily selecting five 2 mm × 2 mm fields of view and evaluating by the ratio of the total area where the Si element was detected to the total evaluation area (total area where the Si element was detected ÷ 20 mm ² ). did. The smaller the area where Si element is detected, the better the state of removal of the adhered film, and the following evaluation was made.
A: 1% or less, B: greater than 1% and 3% or less, C: greater than 3% and 8% or less, D: greater than 8% and 15% or less, E: greater than 15%. In the E evaluation, a clear film residue was observed, and it was judged that the film was insufficient for cleaning the components in the film forming furnace for the plasma CVD apparatus.

(Fine powder adhesion evaluation)
The treated material after the surface treatment and the untreated treated material that was not subjected to film deposition and not subjected to surface treatment were both dried after shower cleaning with pure water. The shower cleaning was performed with pure water at a flow rate of 10 L / min for 2 minutes. Thereafter, a carbon double-sided tape (7314) of Nissin EM Co., Ltd. is adhered to the entire surface of the surface-treated material and the untreated material, and the surface of the material to be treated is adhered to the carbon double-sided tape. Was transcribed. The evaluation tape obtained by transferring the deposit on the surface of the treated material after the surface treatment onto the carbon double-sided tape was designated as T-1. Moreover, T-2 was set as the evaluation tape which transferred the deposit | attachment on the to-be-processed material surface which has not surface-treated to the carbon double-sided tape. Each evaluation tape was installed in an ultra-high resolution field emission scanning electron microscope S4800 and analyzed by EPMA in the same manner as in the evaluation of the attached film removal state. Mapping analysis of the base elements (Al, Fe, Ni, Cr, Ti) of the material to be treated was performed. For each of the evaluation tapes, 5 fields of 2 mm × 2 mm were arbitrarily selected and a total of 20 mm ² was subjected to mapping analysis to obtain a total area (hereinafter also referred to as “detected total area”) of the portion where the host element was detected.

The evaluation was performed using the value calculated from the following formula as an index.
((Total detection area of T-1)-(Total detection area of T-2)) / (Total evaluation area (20 mm ² ))
The smaller the index, the better. A: 2% or less, B: greater than 2% and 4% or less, C: greater than 4% and 7% or less, D: greater than 7% and less than 10%, E: greater than 10%. It was. In the E evaluation, for example, adhesion to a glove may be recognized when handling the cleaning component. Although it thinks because of such a situation, if the member of E evaluation is used, the occurrence frequency of a film defect will increase. Since it is thought to be due to scattering of deposits in the vacuum apparatus, it was determined that the cleaning was not sufficient for cleaning the components in the film forming furnace for the plasma CVD apparatus.

<Comparative Example 1>
Using five aluminum alloy plates (5052) having a length of 127 mm, a width of 50 mm, and a thickness of 3 mm as the material to be treated, a material to be treated with an adhesion film was prepared in the same manner as in Example 1. Next, under the surface treatment conditions shown in Table 3, the surface of the adhesion film of the material to be treated was surface treated in the same manner as in Example 1. The particle size and shape of the abrasive were also the same as in Example 1. However, the walnut is non-spherical with the abrasive of the first spray gun.
The material to be treated thus subjected to the surface treatment was evaluated by the same evaluation method as in Example 1. The evaluation results are shown in Table 4.

<Comparative example 2>
Using a single aluminum alloy plate (5052) having a length of 127 mm, a width of 50 mm, and a thickness of 3 mm as the material to be treated, a material to be treated with an adhesion film was prepared in the same manner as in Example 1. Next, under the surface treatment conditions shown in Table 3, the surface of the adhesion film of the material to be treated was surface treated in the same manner as in Example 1. However, in this comparative example, the surface treatment was performed only by spraying the first spray gun. The particle size and shape of the abrasive were also the same as in Example 1.
The material to be treated thus subjected to the surface treatment was evaluated by the same evaluation method as in Example 1. The evaluation results are shown in Table 4.

From the evaluation results in Table 4, M1>Mm> M2, and the surface treatment is performed by spraying the treated parts in order from the abrasive material having the largest Mohs hardness, thereby maintaining the adhesion film removing capability at a high level and adhering fine particles. It turns out that effective suppression is compatible and a clean surface is obtained.
In Example 1-7, when the surface treatment was performed once, Example 1 in which a trace process was performed in which the spraying by the second spray gun was divided into a plurality of times following the spraying by the first spray gun. There was a slight increase in fine powder adhesion over -1. In Example 1-8, the result was that the fine powder adhesion slightly increased because the alumina as the first abrasive had a corner shape.

In Comparative Examples 1-1, 1-4, 1-5, 1-6, 1-7, 1-8, and 1-9, since the treatment is performed with an abrasive that satisfies M2> Mm, the effect of suppressing the adhesion of fine powder is obtained. It was hardly obtained. In Comparative Examples 1-2 and 1-3, since the treatment was performed with the abrasive that satisfies Mm> M1, the film removal ability was insufficient and the film residue was generated. In Comparative Examples 1-1 and 1-4, since Mm> M1 and M2> Mm are used for the treatment, Mm> M1 and Mm> M2 in Comparative Examples 1-2 and 1-3 are set. Although the ability to remove the adhered film was improved, the state of fine powder adhesion deteriorated.
In Comparative Example 2, since the surface treatment was performed only by spraying the first spray gun, the adhesion film removing ability was good, but the generation of fine powder and burrs was large, and the fine powder was adhered.

From the above, it was found that a clean surface can be obtained by both the removal of the adhered film and the suppression of fine powder adhesion by the following method.
1) At least two spray guns for honing treatment are simultaneously used for one workpiece.
2) At least one type of abrasive having a Mohs hardness greater than that of the material to be treated and at least one type of abrasive having a Mohs hardness of less than that of the material to be treated are sprayed from individual spray guns, and the abrasive having a large Mohs hardness. The surface treatment is performed by spraying the parts to be treated in order.
Furthermore, it has been found that the following trace treatment can achieve a clean surface with both adhesion film removal ability and fine powder adhesion suppression, compared to a single treatment.
1) Following the spraying of an abrasive having a Mohs hardness greater than that of the material to be treated, a continuous surface treatment of spraying the material to be treated in order from the abrasive having a large Mohs hardness is performed in a plurality of times.

<Example 2> Reuse of abrasive material As the material to be treated, two aluminum alloy plates (5052) having a length of 127 mm, a width of 50 mm, and a thickness of 3 mm were used. Two sheets were made. Next, the adhesion film surface of the material to be treated was treated under the surface treatment conditions shown in Table 5. Conditions other than those shown in Table 5 were the same as in Example 1.

In Example 2, a honing apparatus having the configuration shown in FIG. The workpiece 601 was placed in the processing container 610 and surface treatment was performed using the first spray gun 602 and the second spray gun 603. A mixture of the two types of abrasives after spraying and water was collected in a recovery tank 611 and recovered by precipitation separation of the abrasives. Then, the set abrasive is sent together with the mixed solution from the bottom of the recovery tank 611 to the adjustment tank 608 from the first spray gun 602. Next, replenishment adjustment of water and a new abrasive is performed in the adjustment tank 608 so as to obtain a predetermined abrasive collision energy E1 per 1 cm ² . Thereafter, the spray pump 604 of the first injection gun 602 sends a mixture of water and abrasives to the first injection gun 602 for reuse.

The surface-treated material was evaluated by the same evaluation method as in Example 1. The evaluation results are shown in Table 6.
The separation / recovery ability collects a mixture of abrasive and water sprayed from the first spray gun immediately after the surface treatment is completed, and the ice particles or dry ice particles that are abrasives of the second spray gun are mixed and floated. It was confirmed visually whether or not. As a result, neither ice particles nor dry ice particles could be confirmed. Ice is turned into liquid water in the recovery tank 611, dry ice is turned into gas, and the only abrasive that returns from the recovery tank 611 to the first spray gun 602 is SUS430, and the separation and recovery capability is good. Was confirmed.
In addition, it can be seen from the results in Table 6 that even when a recycled abrasive is used, a good surface treatment can be performed as in Examples 1-1 and 1-3.

<Example 3> Recovery and separation of abrasives As the materials to be treated, two aluminum alloy plates (5052) having a length of 127 mm, a width of 50 mm, and a thickness of 3 mm, two stainless steel plates (SUS304), and a titanium alloy plate (SSAT-64). ) One sheet was used. Then, five processed materials with an adhesion film were prepared in the same manner as in Example 1.
Next, the adhesion film surface of the material to be treated was treated under the surface treatment conditions shown in Table 7. In Example 3, iron, SUS430, which is a substantially spherical and magnetic abrasive, walnut, which is a non-spherical, non-magnetic abrasive, SiC, nylon, glass, zircon, which is a substantially spherical, non-magnetic abrasive, are used. It was. SUS430 used was a substantially spherical shape corresponding to a 120th mesh, and the glass was a substantially spherical shape corresponding to a 150th mesh. The size and shape of other abrasives were the same as in Example 1.
Conditions other than those shown in Table 7 were the same as in Example 1.

In Example 3, a honing apparatus having a configuration as shown in FIG. 6B was used. In Example 3, the mixture of the two types of abrasives after spraying and water was collected in the recovery tank 611, and the abrasives were separated and recovered.
FIG. 6B shows a configuration example in the case where a magnetic abrasive is used for the first spray gun 602. The abrasive used in the processing container 610 is collected in a collection tank 611. Here, the magnetic abrasive is separated by a separation and recovery device 612 installed in the recovery tank 611. The separated magnetic abrasive is sent to the precipitation tank 613 and then sent to the adjustment tank 608, where water and a new abrasive are replenished and adjusted to a predetermined E1. Thereafter, the spray pump 604 of the first injection gun 602 sends a mixture of water and abrasives to the first injection gun 602 for reuse. The nonmagnetic abrasive is sent from the bottom of the recovery tank 611 to the precipitation tank 614. And it is sent to the adjustment tank 609, and replenishment adjustment of water and a new abrasive is performed so that it may become predetermined E2 there. After that, the spray pump 605 of the second injection gun 603 sends the mixed liquid of water and abrasives to the second injection gun 603 for reuse.

  Briefly described, the separation and recovery device 612 collects magnetic abrasives with a magnetic roller and captures them with a magnetic stirring rod, thereby separating and recovering magnetic and nonmagnetic abrasives. For example, a configuration as shown in FIG. 7A can be used. FIG. 7B is a schematic diagram for explaining the magnetic roller 702 and the stripping blade 703 portion in FIG. A magnetic abrasive and a non-magnetic abrasive can be separated by a magnetic roller 702 and a peeling blade 703 provided in the recovery tank 701. The stripped magnetic abrasive was again settled in the tank 708, and adjusted to be a predetermined E1 as an abrasive for the spray gun from the bottom of the tank and reused. The non-magnetic abrasive remaining in the recovery tank 701 was again introduced into another tank 614 and stirred with a magnetic stirring rod (not shown) to capture the magnetic abrasive. Further, the settled non-magnetic abrasive was adjusted from the bottom of the tank to a predetermined E2 as an abrasive for the spray gun and reused.

In Example 3-2, since the abrasive used for the second spray gun 603 is a magnetic abrasive, the spray pump 604 of FIG. 6B is connected to the second spray gun 603, and the spray pump 605 is connected to the first spray gun 605. It changed to the structure connected to the injection gun 602.
The surface-treated material was evaluated by the same evaluation method as in Example 1. The evaluation results are shown in Table 8.

  Separation and recovery capability is evaluated by collecting a mixture of abrasive and water sprayed from the first spray gun and a mixture of abrasive and water sprayed from the second spray gun immediately after completion of the surface treatment. did. Specifically, the abrasive liquid mixture is filtered through a filter paper and dried to obtain 10 g of the abrasive. The abrasive was sprinkled on a magnet rod, and the mass of the magnetic abrasive adhered to the magnet and the mass of the non-magnetic abrasive not attached to the magnet were determined.

For example, in Example 3-1, the separation / recovery capacity is evaluated. In the abrasive collected from the first spray gun that injects the magnetic abrasive, the mass ratio of the non-magnetic abrasive to the magnetic abrasive is calculated. Asked. Specifically, the abrasives sprayed from the spray gun are collected using the abrasive recovery container shown in FIG. 9, and 10 g of them is transferred to a plastic container. Next, the magnetic abrasive was removed from the abrasive in the plastic container using a neodymium magnet. Repeated about 20 times, the mass of the abrasive remaining when the mass of the plastic container almost did not decrease was determined. (Mass of remaining abrasive) = (Mass of non-magnetic abrasive not attached to magnet) and (10 g−Mass of non-magnetic abrasive not attached to magnet) = (Mass of magnetic abrasive attached to magnet) ). The mass ratio was (mass of nonmagnetic abrasive not attached to magnet) / (mass of magnetic abrasive attached to magnet).
Further, in the abrasive collected from the second spray gun that injects the non-magnetic abrasive, the mass ratio was determined as the ratio of the magnetic abrasive attached to the magnet to the non-magnetic abrasive that was not attached to the magnet. The evaluation results are shown in Table 8. The smaller the mass ratio, the better the separation and recovery capability.

  In all of Examples 3-1, 3-2, 3-3, 3-4, and 3-5, the adhesion film removing ability and the fine powder adhesion evaluation were good. The reason why the fine powder adhesion evaluation of Example 3-2 is B is because SiC, which is the abrasive material of the first injection gun, is non-spherical and slightly more fine particles are generated. In addition, the fine powder adhesion evaluation of Example 3-5 is B because there is a glass that is the abrasive material of the first injection gun that is crushed in the surface treatment process, and as a result of the crushing, an abrasive material having a sharp shape can be obtained. End up. For this reason, the generation of fine powder, the sticking of the abrasive, etc. increased. The separation / recovery ability was good, less than 5% by mass. In particular, the nonmagnetic abrasive mixed in the magnetic abrasive had a mass ratio of less than 1%, and the separation and recovery ability was very good.

<Embodiment 4> Influence of abrasive material collision energy As an object to be treated, an aluminum alloy plate (5052) having a length of 127 mm, a width of 50 mm, and a thickness of 3 mm was used. Created.
Next, the surface treatment conditions shown in Table 9 were used, and the surface of the adhesion film of the material with the adhesion film was treated in the same manner as in Example 1. The particle size and shape of the abrasive were also the same as in Example 1.
The surface-treated material was evaluated in the same manner as in Example 1. Table 10 shows the evaluation results.

From Table 10, it can be seen that, in any of the examples, the evaluation of adhesion film removal ability and the evaluation of fine powder adhesion are evaluation results of C or more, and the effect of the present invention is obtained. In more detail, the following can be understood.
In Examples 4-1 to 4-23, E1 is changed by changing the jet velocity V1 of the abrasive injected from the first injection gun. Further, the magnitude relationship between E1 and E2 is changed by changing the jet velocity V2 of the abrasive injected from the second injection gun. It can be seen that as E1 is reduced, the ability to remove the adhered film decreases.

In Examples 4-1 to 4-5, since E1 is small, the same trace processing results in a slightly lower adhesion film removing ability than in Examples 4-6 and later. In Example 4-5, the evaluation of the adhesion film removing ability is higher than in Examples 4-1 to 4-4 in which E1 is the same. This is probably because E2 is large and the attached film removing ability is slightly improved.
Moreover, from the comparison under the same condition of E1, it can be seen that the effect of suppressing fine powder adhesion is improved by setting E2 to E1> E2.

In Examples 4-6 to 4-23, since E1 is sufficiently large, the adhesion film removing ability is highly evaluated.
As in Examples 4-2, 4-9, 4-15, and 4-22, when E1 = E2, the effect of suppressing the adhesion of fine powder is slightly reduced.
From the above, it can be seen that it is preferable to satisfy E1> E2 in order to obtain a clean surface in which the maintenance of the adhesion film removing ability at a high level and the effective suppression of the adhesion of fine powder are compatible.

<Example 5> Influence of injection angle of injection gun. When E1> E2.
Using the aluminum alloy plate (5052) having a length of 127 mm, a width of 50 mm, and a thickness of 3 mm as the material to be treated, 26 materials to be treated with an adhesion film were prepared in the same manner as in Example 1.
Next, the surface of the adhesion film of the material to be treated was treated in the same manner as in Example 1 except that the surface treatment conditions shown in Table 11 were used. In this embodiment, the influence of the injection angle on the surface treatment is confirmed. The injection angle (θ1) of the first injection gun refers to an angle 106 formed by the Z axis shown in FIG. 1 and the central axis of the first injection gun. The injection angle (θ2) of the second injection gun refers to an angle 107 formed by the Z axis shown in FIG. 1 and the central axis of the second injection gun.
The treated material thus surface-treated was evaluated in the same manner as in Example 1. The evaluation results are shown in Table 12.

From Table 12, it can be seen that in any of the examples, the evaluation of the adhesion film removing ability and the evaluation of fine powder adhesion are evaluation results of C or more, and the effect of the present invention is obtained. In more detail, the following can be understood.
In Example 5, a comparison was made by changing the injection angle (θ1) of the first injection gun and the injection angle (θ2) of the second injection gun. E1 and E2 were adjusted to be constant. In Examples 5-11 and 5-19, θ2 was set to the upper limit of 83 degrees on the configuration of the apparatus, so that the vertical component of the jet velocity was reduced and the abrasive collision energy was reduced. The film removal ability and effective suppression of fine powder adhesion were compatible.

In Examples 5-25 and 5-26, the injection angle (θ1) of the first injection gun is over 45 degrees, the vertical component of the jet velocity is reduced, and the same abrasive collision energy as in 5-24 Even so, the abrasive tends to slide slightly on the surface. As a result, the ability to remove the adhered film was slightly reduced.
In Examples 5-1, 5-2, and 5-3, since the injection angle (θ1) of the first injection gun is 0 degree, the polishing material remains on the surface of the material to be processed, fine powder, burrs are embedded, The amount of rubbing increases, and therefore, the effect of suppressing fine powder adhesion is reduced.

In Examples 5-5 and 5-13, since the injection angle (θ2) of the second injection gun is smaller than the injection angle (θ1) of the first injection gun, the fine powder adhesion suppressing effect is reduced.
From the above, in the condition of E1> E2, by setting 0 ° <θ1 ≦ 45 ° and θ1 ≦ θ2 <90 °, it is possible to maintain a high level of adhesion film removing ability and more effectively suppress fine particle adhesion. It can be seen that a clean and compatible surface can be obtained.

<Example 6> Effect of injection angle of injection gun. When E1 <E2.
Using the aluminum alloy plate (5052) having a length of 127 mm, a width of 50 mm, and a thickness of 3 mm as the material to be treated, 23 materials to be treated with an adhesion film were prepared in the same manner as in Example 1.
Next, as shown in Table 13, the surface treatment conditions are such that the relationship between E1 and E2 is E1 <E2, and the injection angle (θ1) of the first injection gun and the injection angle (θ2) of the second injection gun are changed. Except that, the surface of the adhesion film of the material to be treated was treated in the same manner as in Example 1.
The treated material thus surface-treated was evaluated in the same manner as in Example 1. The evaluation results are shown in Table 14.

From Table 14, it can be seen that, in any of the examples, the evaluation of adhesion film removal ability and the evaluation of fine powder adhesion are evaluation results of D or more, and the effect of the present invention is obtained. In more detail, the following can be understood.
In Examples 6-1, 6-2, and 6-3, since the injection angle (θ1) of the first injection gun is 0 degree, the abrasive remains on the surface of the material to be processed, or fine particles and burrs are embedded. As a result, the amount of rubbing increases, and as a result, the effect of suppressing fine powder adhesion is reduced. In Examples 6-5 and 6-13, since the injection angle (θ2) of the second injection gun is smaller than the injection angle (θ1) of the first injection gun, the fine powder adhesion suppressing effect is reduced. In Examples 6-22 and 6-23, since θ1 exceeds 45 °, it can be seen that the ability to remove the attached film is slightly lowered.
Compared with Example 5 where E1> E2, the effect of suppressing the adhesion of fine powder is small, but a clean surface that achieves both a high level of adhesion film removal ability and effective suppression of adhesion of fine powder is obtained under any conditions. You can see that It can be seen that, even under the condition of E1 <E2, it is more preferable that 0 ° <θ1 ≦ 45 ° and θ1 ≦ θ2 <90 °.

<Example 7> Influence of injection angle of injection gun. When E1 = E2.
Sixteen processed materials with an adhesion film were prepared in the same manner as in Example 1 using an aluminum alloy plate (5052) having a length of 127 mm, a width of 50 mm, and a thickness of 3 mm as the processed material.
Next, the surface of the adhesion film of the material to be treated was treated in the same manner as in Example 1 except that the surface treatment conditions shown in Table 15 were used. In this example, the surface of the adhesion film of the material to be processed was processed under the condition of E1 = E2. The particle size and shape of the abrasive were also the same as in Example 1.
The treated material thus surface-treated was evaluated in the same manner as in Example 1. The evaluation results are shown in Table 16.

From Table 16, it can be seen that in any of the examples, the evaluation of the attached film removal ability and the evaluation of fine powder adhesion are evaluation results of D or more, and the effect of the present invention is obtained. In more detail, the following can be understood.
In Examples 7-1 and 7-2, since the injection angle (θ1) of the first injection gun is 0 degree, the polishing material remains on the surface of the material to be processed, fine particles, burrs are embedded, or rubbed in. As a result, the effect of suppressing the adhesion of fine powder is reduced. In Examples 7-3 and 7-8, since the injection angle (θ2) of the second injection gun is smaller than the injection angle (θ1) of the first injection gun, the fine powder adhesion suppressing effect is reduced. In Examples 7-15 and 7-16, since θ1 exceeds 45 °, it can be seen that the attached film removing ability is slightly lowered.
Compared with Example 5 where E1> E2, the effect of suppressing the adhesion of fine powder is small, but a clean surface that achieves both a high level of adhesion film removal ability and effective suppression of adhesion of fine powder is obtained under any conditions. I understand that Further, it is understood that it is more preferable that 0 ° <θ1 ≦ 45 ° and θ1 ≦ θ2 <90 ° even under the condition of E1 = E2.

<Example 8> Abrasive material-1: iron ball, abrasive material-2: ice particles, E2 is changed with respect to E1.
Sixteen processed materials with an adhesion film were prepared in the same manner as in Example 1 using an aluminum alloy plate (5052) having a length of 127 mm, a width of 50 mm, and a thickness of 3 mm as the processed material.
Next, the surface of the adhesion film of the material to be treated was treated in the same manner as in Example 1 except that the surface treatment conditions shown in Table 17 were used. In this example, the abrasive material-1 was changed to an iron ball, the abrasive material-2 was changed to an ice particle, and E2 was changed with respect to E1, and the adhesion film surface of the material to be treated was obtained in the same manner as in Example 1. Was processed. The treated material thus surface-treated was evaluated in the same manner as in Example 1. The evaluation results are shown in Table 18.

From Table 18, it can be seen that in any of the examples, both the evaluation of the attached film removal ability and the evaluation of fine powder adhesion are evaluation results of C or more, and the effect of the present invention is obtained. Further details are as follows.
In Examples 8-1 to 8-6, E2 was changed while keeping all the conditions of the injection gun 1 constant. Compared with Examples 8-1, 8-2, and 8-3 under the condition of E1> E2, Example 8-4 under the condition of E1 = E2 has a slightly reduced fine powder adhesion suppressing effect. In Examples 8-5 and 8-6 where E1 <E2 is satisfied, it can be seen that the effect of suppressing fine powder adhesion is further reduced.

In Examples 8-7 to 8-11, E2 was changed while keeping all the conditions of the injection gun 1 constant. It can be seen that in Example 8-10 under the condition of E1 = E2, the fine powder adhesion suppressing effect is slightly reduced, and in Example 8-11 where E1 <E2, the fine powder adhesion suppressing effect is further reduced.
In Examples 8-12 to 8-16, E2 was changed with all the conditions of the injection gun 1 being constant. It can be seen that in Example 8-16 under the condition of E1 = E2, the effect of suppressing the adhesion of fine powder is slightly lowered.
From the above, even when the abrasive 1 is an iron ball and the abrasive 2 is an ice particle, it is more possible to maintain E1> E2 at a high level of adhesion film removal ability and to prevent fine powder adhesion. It turns out to be effective.

<Example 9> Abrasive material-1: iron ball, abrasive material-2: ice particles, θ2 is changed with respect to θ1.
Using the aluminum alloy plate (5052) having a length of 127 mm, a width of 50 mm, and a thickness of 3 mm as the material to be treated, 14 materials to be treated with an adhesion film were prepared in the same manner as in Example 1.
Next, the surface of the adhesion film of the material to be treated was treated in the same manner as in Example 1 except that the surface treatment conditions shown in Table 19 were used. In this example, the surface of the adhesion film of the material to be treated is processed in the same manner as in Example 1 by changing the θ2 to θ1 with the abrasive 1 as an iron ball and the abrasive 2 as an ice particle. It was. Table 20 shows the evaluation results.

From Table 20, it can be seen that in any of the examples, the evaluation of the adhering film removal ability and the evaluation of fine powder adhesion are evaluation results of C or more, and the effect of the present invention is obtained. In more detail, the following can be understood.
In Example 9-1, since the injection angle (θ1) of the first injection gun is 0 °, the polishing material remains on the surface of the material to be processed, or fine particles, burrs are embedded, and the slid in increases. Therefore, the fine powder adhesion inhibitory effect is small. In Example 9-5, since the injection angle (θ2) of the second injection gun is smaller than the injection angle (θ1) of the first injection gun, the effect of suppressing fine powder adhesion is reduced. In Example 9-14, since the injection angle (θ1) of the first injection gun exceeds 45 °, the component in the vertical direction of the material to be processed of the jet velocity becomes small, and the adhesion film removing ability is slightly reduced. .
From the above, even when the abrasive 1 is an iron ball and the abrasive 2 is an ice grain, the adhesion film removing ability can be improved by satisfying 0 ° <θ1 ≦ 45 ° and θ1 ≦ θ2 <90 °. It can be seen that a clean surface that achieves both high level maintenance and more effective suppression of fine powder adhesion can be obtained.

<Example 10> Abrasive material-1: iron ball, abrasive material-2: ice particles, E2 <θ2 was changed with respect to θ1 under the condition of E2.
An aluminum alloy plate (5052) having a length of 127 mm, a width of 50 mm, and a thickness of 3 mm was used as the material to be treated, and 18 materials to be treated with an adhesion film were prepared in the same manner as in Example 1.
Next, the surface of the adhesion film of the material to be treated was treated in the same manner as in Example 1 except that the surface treatment conditions shown in Table 21 were used. In this example, the abrasive material-1 is an iron ball, the abrasive material-2 is an ice particle, and θ2 is changed with respect to θ1 under the condition of E1 <E2. The surface of the adhesion film was processed. The evaluation results are shown in Table 22.

From Table 22, it can be understood that in any of the examples, the evaluation of the attached film removal ability and the evaluation of fine powder adhesion are evaluation results of D or more, and the effect of the present invention is obtained. In more detail, the following can be understood.
In Example 10-1, since the injection angle (θ1) of the first injection gun is 0 °, the abrasive remains on the surface of the material to be processed, and fine powder, burrs are embedded and slid. Therefore, the effect of suppressing the adhesion of fine powder is small. In Examples 10-3 and 10-10, since the injection angle (θ2) of the second injection gun is smaller than the injection angle (θ1) of the first injection gun, the fine powder adhesion suppressing effect is reduced. In Example 10-18, since θ1 exceeds 45 °, it can be seen that the ability to remove the attached film is slightly lowered.

Compared with Example 9 where E1> E2, the embedding squeezing suppression effect is small, but a clean surface that achieves both a high level of adhesion film removal ability and an effective suppression of fine powder adhesion under any conditions. You can see that Further, it is understood that it is more preferable that 0 ° <θ1 ≦ 45 ° and θ1 ≦ θ2 <90 ° even under the condition of E1 <E2.
From the above, by setting the abrasive material-1 as an iron ball and the abrasive material-2 as an ice particle, and even under the condition of E1 <E2, by setting 0 ° <θ1 ≦ 45 ° and θ1 ≦ θ2 <90 °, It can be seen that a clean surface can be obtained in which both the maintenance of the adhesion film removing ability at a high level and the more effective suppression of the adhesion of fine powder are achieved.

<Example 11> Abrasive material-1: Iron ball, Abrasive material-2: Ice particles, E2 = θ2 was changed with respect to θ1 under the condition of E2.
Using the aluminum alloy plate (5052) having a length of 127 mm, a width of 50 mm, and a thickness of 3 mm as the material to be treated, 14 materials to be treated with an adhesion film were prepared in the same manner as in Example 1.
Next, the surface of the adhesion film of the material to be treated was treated in the same manner as in Example 1 except that the surface treatment conditions shown in Table 23 were used. In this embodiment, the abrasive 1 is an iron ball, the abrasive 2 is an ice particle, and θ2 is changed with respect to θ1 under the condition of E1 = E2. The membrane surface was treated. The evaluation results are shown in Table 24.

From Table 24, it can be seen that in any of the examples, the evaluation of the adhesion film removing ability and the evaluation of fine powder adhesion are evaluation results of D or more, and the effect of the present invention is obtained. In more detail, the following can be understood.
In Example 11-1, since the injection angle (θ1) of the first injection gun is 0 °, the polishing material remains on the surface of the material to be processed, or fine powder, burrs are embedded and rubbed in. For this reason, the effect of suppressing the adhesion of fine powder is small. In Examples 11-2 and 11-8, since the injection angle (θ2) of the second injection gun is smaller than the injection angle (θ1) of the first injection gun, the fine powder adhesion suppressing effect is reduced. In Examples 11-14, since θ1 exceeds 45 °, it can be seen that the ability to remove the attached film is slightly lowered.

  Compared with Example 9 where E1> E2, the embedding squeezing suppression effect is small, but a clean surface that achieves both a high level of adhesion film removal ability and an effective suppression of fine powder adhesion under any conditions. You can see that It can be seen that, even under the condition of E1 <E2, it is more preferable that 0 ° <θ1 ≦ 45 ° and θ1 ≦ θ2 <90 °.

<Example 12> Abrasive material-1: iron ball, abrasive material-2: ice particles, relationship between E1 and E2.
Using a titanium alloy plate (SSAT-64) having a length of 127 mm, a width of 50 mm, and a thickness of 3 mm as the material to be treated, 16 materials to be treated with an adhesion film were prepared in the same manner as in Example 1.
Next, the surface of the adhesion film of the material to be treated was treated in the same manner as in Example 1 except that the surface treatment conditions shown in Table 25 were used. The material to be treated thus subjected to the surface treatment was evaluated by the same evaluation method as in Example 1. The evaluation results are shown in Table 26.

From Table 26, it can be seen that in any of the examples, the evaluation of the adhesion film removing ability and the evaluation of fine powder adhesion are evaluation results of D or more, and the effect of the present invention is obtained. In more detail, the following can be understood.
In Examples 12-1 to 12-5, E2 was changed while keeping all the conditions of the injection gun 1 constant. Compared to Examples 12-1 and 12-2 under the condition of E1> E2, Example 12-3 under the condition of E1 = E2 has a slightly reduced fine powder adhesion suppressing effect, and further, Example 12 under the condition of E1 <E2. In -4 and 12-5, it turns out that the fine powder adhesion inhibitory effect is falling further.

In Examples 12-6 to 12-10, all the conditions of the injection gun 1 were made constant and E2 was changed. It can be seen that in Example 12-9 under the condition of E1 = E2, the fine powder adhesion suppressing effect is slightly reduced, and in Example 12-10 where E1 <E2, the fine powder adhesion suppressing effect is further reduced.
In Examples 12-11 to 12-16, E2 was changed with all the conditions of the injection gun 1 being constant. It can be seen that in Examples 8-15 under the condition of E1 = E2, the effect of suppressing the adhesion of fine powder is slightly lowered. Furthermore, in Examples 12-16 in which E1 <E2, it can be seen that the fine powder adhesion suppressing effect is further reduced.
From the above, even when the abrasive 1 is an iron ball and the abrasive 2 is an ice particle, it is more possible to maintain E1> E2 at a high level of adhesion film removal ability and to prevent fine powder adhesion. It turns out to be effective.

<Example 13> Material to be treated: Titanium alloy plate (SSAT-64), relationship between θ1 and θ2 in the case of E1> E2.
Titanium alloy plate (SSAT-64) having a length of 127 mm, a width of 50 mm, and a thickness of 3 mm was used as the material to be treated, and 24 materials to be treated with an adhesion film were prepared in the same manner as in Example 1.
Next, the surface of the adhesion film of the material to be treated was treated in the same manner as in Example 1 except that the surface treatment conditions shown in Table 27 were used. The material to be treated thus subjected to the surface treatment was evaluated by the same evaluation method as in Example 1. The evaluation results are shown in Table 28.

From Table 28, it can be seen that in any of the examples, the evaluation of the adhesion film removing ability and the evaluation of fine powder adhesion are evaluation results of C or more, and the effect of the present invention is obtained. In more detail, the following can be understood.
In Examples 13-1 and 13-2, since the injection angle (θ1) of the first injection gun is 0 °, the abrasive remains on the surface of the material to be processed, or fine particles and burrs are embedded and rubbed in. As a result, the effect of suppressing the adhesion of fine powder is reduced. In Examples 13-14, 13-15, 13-16, and 13-23, since the injection angle (θ2) of the second injection gun is smaller than the injection angle (θ1) of the first injection gun, fine powder adhesion The inhibitory effect is reduced. Further, in Examples 13-23 and 13-24, the injection angle (θ1) of the first injection gun is over 45 degrees, the component of the jet velocity in the vertical direction is small, and the abrasive slightly covers the surface. It tends to slip. As a result, the ability to remove the adhered film was slightly reduced.
From the above, even when a titanium alloy plate (SSAT-64) is used as the material to be treated, a high level of adhesion film removing ability can be obtained by satisfying 0 ° <θ1 ≦ 45 ° and θ1 ≦ θ2 <90 °. It can be seen that a clean surface can be obtained in which both maintenance at low temperatures and more effective suppression of fine powder adhesion are achieved.

<Example 14> Material to be treated: Titanium alloy plate (SSAT-64), relationship between θ1 and θ2 when E1 <E2.
Titanium alloy plate (SSAT-64) having a length of 127 mm, a width of 50 mm, and a thickness of 3 mm was used as the material to be treated, and 23 materials to be treated with an adhesion film were prepared in the same manner as in Example 1.
Next, the surface of the adhesion film of the material to be treated was treated in the same manner as in Example 1 except that the surface treatment conditions shown in Table 29 were used. The material to be treated thus subjected to the surface treatment was evaluated by the same evaluation method as in Example 1. The evaluation results are shown in Table 30.

From Table 30, it can be seen that in any of the examples, the evaluation of the attached film removal ability and the evaluation of fine powder adhesion are evaluation results of D or more, and the effect of the present invention is obtained. In more detail, the following can be understood.
In Examples 14-1, 14-2, and 14-3, since the injection angle (θ1) of the first injection gun is 0 degree, the polishing material remains on the surface of the material to be processed, or fine particles and burrs are not generated. The embedding and rubbing increase, and for that reason, the effect of suppressing the adhesion of fine powder is reduced. In Examples 14-5 and 14-13, since the injection angle (θ2) of the second injection gun is smaller than the injection angle (θ1) of the first injection gun, the effect of suppressing fine powder adhesion is reduced. It can also be seen that in Examples 14-22 and 14-23, when θ1 is 50 °, the ability to remove the attached film is slightly lowered.

Compared with Example 13 where E1> E2, the effect of suppressing the adhesion of fine powder is small, but a clean surface that achieves both a high level of adhesion film removal ability and effective suppression of adhesion of fine powder is obtained under any conditions. I understand that Further, it is understood that it is more preferable that 0 ° <θ1 ≦ 45 ° and θ1 ≦ θ2 <90 ° even under the condition of E1 <E2.
As described above, a titanium alloy plate (SSAT-64) is used as the material to be treated, and even if the conditions of E1 <E2 are satisfied, 0 ° <θ1 ≦ 45 ° and θ1 ≦ θ2 <90 ° are satisfied. It can be seen that a clean surface that achieves both a high level of maintenance and more effective suppression of fine powder adhesion can be obtained.

<Example 15> Material to be treated: Titanium alloy plate (SSAT-64), relationship between θ1 and θ2 when E1 = E2.
Using a titanium alloy plate (SSAT-64) having a length of 127 mm, a width of 50 mm, and a thickness of 3 mm as the material to be treated, 16 materials to be treated with an adhesion film were prepared in the same manner as in Example 1.
Next, the surface of the adhesion film of the material to be treated was treated in the same manner as in Example 1 except that the surface treatment conditions shown in Table 31 were used. The material to be treated thus subjected to the surface treatment was evaluated by the same evaluation method as in Example 1. The evaluation results are shown in Table 32.

From Table 32, it can be seen that in any of the Examples, both the evaluation of adhesion film removal ability and the evaluation of fine powder adhesion are evaluation results of D or more, and the effect of the present invention is obtained. In more detail, the following can be understood.
In Examples 15-1 and 15-2, since the injection angle (θ1) of the first injection gun is 0 °, the polishing material remains on the surface of the material to be processed, or fine particles and burrs are embedded and rubbed in. As a result, the effect of suppressing the adhesion of fine powder is reduced. In Examples 15-3, 15-4, and 15-8, since the injection angle (θ2) of the second injection gun is smaller than the injection angle (θ1) of the first injection gun, the effect of suppressing the adhesion of fine powder is reduced. is doing. In Examples 15-15 and 15-16, since θ1 exceeds 45 °, it can be seen that the ability to remove the attached film is slightly lowered.

Compared with Example 13 where E1> E2, the effect of suppressing the adhesion of fine powder is small, but a clean surface that achieves both a high level of adhesion film removal ability and effective suppression of adhesion of fine powder is obtained under any conditions. I understand that
From the above, it is more preferable that a titanium alloy plate (SSAT-64) is used as the material to be treated, and that 0 ° <θ1 ≦ 45 ° and θ1 ≦ θ2 <90 ° even under the condition of E1 = E2. I understand.

<Example 16> Material to be treated: Relationship between E1 and E2 in the case of stainless steel plate (SUS304).
Using a stainless steel plate (SUS304) having a length of 127 mm, a width of 50 mm, and a thickness of 3 mm as a material to be treated, 19 materials to be treated with an adhesion film were prepared in the same manner as in Example 1.
Next, the surface of the adhesion film of the material to be treated was treated in the same manner as in Example 1 except that the surface treatment conditions shown in Table 33 were used. The material to be treated thus subjected to the surface treatment was evaluated by the same evaluation method as in Example 1. The evaluation results are shown in Table 34.

  From Table 34, it can be seen that in any of the examples, the evaluation of the attached film removal ability and the evaluation of fine powder adhesion are evaluation results of C or more, and the effect of the present invention is obtained. In addition, when a stainless steel plate (SUS304) is used as the material to be treated, a clean surface can be obtained by satisfying E1> E2, and both the maintenance of the adhesion film removing ability at a high level and the fine powder adhesion suppressing effect can be achieved. It turns out that it becomes effective.

<Example 17> Three or more spray guns are used.
An aluminum alloy plate (5052) having a length of 127 mm, a width of 50 mm, and a thickness of 3 mm was used as the material to be treated, and three materials to be treated with an adhesion film were prepared in the same manner as in Example 1.
Next, the surface of the adhesion film of the material to be treated was treated in the same manner as in Example 1 except that the surface treatment conditions shown in Table 35 were used. In this embodiment, the surface treatment was performed by arranging three or more guns. The Mohs hardness of the abrasive of the first spray gun is M1, the Mohs hardness of the abrasive of the second spray gun is M2, and similarly, the Mohs hardness of the abrasive is M1, M2, M3, M4 in the order of spraying. It was. The Mohs hardness of the material to be treated was Mm.

In Example 17-1, the Mohs hardness of the abrasive was M1 = M2>Mm> M3 using three spray guns. In Example 17-2, three injection guns were used so that the Mohs hardness of the abrasive became M1>Mm>M2> M3. In Example 17-3, the Mohs hardness of the abrasive was set to satisfy M1 = M2>Mm>M3> M4 using four spray guns.
In addition, in each case, the spray gun that sprays the abrasive having a small Mohs hardness is arranged so that the spray angle becomes large.
The treated material thus surface-treated was evaluated in the same manner as in Example 1. The evaluation results are shown in Table 36.

  From the evaluation results shown in Table 36, Example 17-1 has a slightly larger amount of fine powder adhesion than Examples 17-2 and 17-3. This uses two spray guns that spray abrasives with a Mohs hardness greater than Mm, whereas there is one spray gun that sprays abrasives with a Mohs hardness less than Mm, so it can remove fines and burrs. Is considered to be smaller than Example 17-2 and Example 17-3. In Example 17-2, by using one spray gun for spraying an abrasive larger than Mm and two spray guns for spraying an abrasive smaller than Mm, the fine powder adhesion suppressing effect is remarkably obtained. Yes.

Furthermore, in Example 17-3, even if there are two spray guns that spray an abrasive larger than Mm, the number of spray guns that spray an abrasive smaller than Mm is also two, so that the effect of suppressing the adhesion of fine powder is remarkable. Has been obtained.
From the above, it is possible to increase the number of spray guns for injecting abrasives with a Mohs hardness less than Mm to be the same as or greater than the number of spray guns for injecting abrasives with a Mohs hardness greater than Mm. It has been confirmed that it is particularly effective for maintaining both the maintenance of the powder and the suppression of fine powder adhesion.

<Example 18> Material to be treated: Aluminum alloy As the material to be treated, three types of aluminum alloy plates shown in Table 37 having a length of 127 mm, a width of 50 mm, and a thickness of 3 mm were used. Three treatment materials were prepared.
Next, the surface of the adhesion film of the material to be treated was treated in the same manner as in Example 1 except that the surface treatment conditions shown in Table 37 were used. The material to be treated thus subjected to the surface treatment was evaluated by the same evaluation method as in Example 1. The evaluation results are shown in Table 38.

  From the evaluation results shown in Table 38, by performing the surface treatment of the present invention, a clean surface can be obtained in any aluminum alloy-based material, and the adhesion film removal ability can be maintained at a high level and fine powder adhesion can be suppressed It turned out to be effective in terms of coexistence of effects.

<Example 19>
In this embodiment, two substrate holders 801 for producing an amorphous silicon electrophotographic photosensitive member made of an aluminum alloy plate (5052) shown in FIG. Specifically, an electrophotographic photosensitive member having an outer diameter of 84 mm and a length of 381 mm was prepared twice by the plasma CVD method under the conditions shown in Table 39, and the two substrate holders 801 used for the preparation were the same as in Example 1-1. The surface treatment was performed.

  The substrate holder 801 includes a cylindrical body 803, a holder body 806 including a cylindrical skirt portion 802 having a larger outer diameter than the body 803, and a cap portion 804. A conductive base 805 is installed on the body 803, and the cap 804 is installed on the body 803 so that the conductive base 805 is sandwiched between the skirt 802 and the cap 804. The skirt portion 802 and the cap portion 804 have the same outer diameter as that of the conductive base, and in this example, the outer diameter is 84 mm. The outer diameter of the body 803 is 76 mm, and the length of the base holder 801 is 1000 mm.

  An amorphous silicon film is adhered to the skirt portion 802 and the cap portion 804 on the surface of the substrate holder after the electrophotographic photosensitive member is formed. FIG. 4 shows the arrangement of the base holder and the spray gun, which are materials to be processed. The body holder 803 surface of the base holder has a Y axis in the tangent line in the generatrix direction, the body part 803 surface has an X axis perpendicular to the Y axis, passes through the central axis of the body part 803, and is perpendicular to the XY plane. Take the Z axis. In the first injection gun 402, the central axis of the jet blown from the injection gun 402 is on the YZ plane, and the central axis is set at a predetermined angle 406 with respect to the Z axis. In the second injection gun 403, the central axis of the jet sprayed from the injection gun 103 is on the YZ plane, and the central axis is installed at a predetermined angle 407 with respect to the Z axis.

  During the surface treatment, the substrate holder 401 was moved in the Y-axis direction and rotated in the circumferential direction with the central axis of the substrate holder as the rotation axis. Further, the portions where the amorphous silicon film adhered on the substrate holder are the skirt portion and the cap portion, but the other portions were also subjected to surface treatment for cleaning. The distance from the injection port of the injection gun to the body part of the base holder was set to 100 mm.

  In order to evaluate the cleanliness of the substrate holder subjected to the surface treatment in this way, an evaluation sample was cut out from one of the two substrate holders subjected to the surface treatment. The cut-out portion was a skirt portion and cut out with a size of 100 mm in the axial direction and 20 mm in the circumferential direction. The evaluation sample cut out in this manner was evaluated in the same manner as in Example 1. As a result, both the ability to remove the attached film and the evaluation of embedded slidability were evaluated as A.

Next, the surface-treated substrate holder that was not cut was reused, and an amorphous silicon electrophotographic photosensitive member was formed again under the conditions shown in Table 39. The surface of the electrophotographic photosensitive member thus prepared was polished with a wrapping tape having a width of 360 mm (manufactured by Reflight Co., Ltd., model number: GC4000). The wrapping tape is pressed against the drum surface with a pressure roller having a JIS rubber hardness of 30 at a pressure of about 0.8 kgf / cm ² . The pressure roller axis and the electrophotographic photosensitive member axis were pressed so as to be parallel. In this state, the surface was polished by rotating the electrophotographic photosensitive member at a rotational speed of 40 rpm while moving the wrapping tape at a speed of 50 mm / min in the tangential direction of the electrophotographic photosensitive member.

Next, the produced electrophotographic photosensitive member was installed in the color imageRUNNER iR C6880N electrophotographic apparatus manufactured by Canon Inc., and A3 image output was performed. The output image was a cyan single-color image and a black single-color image each having a halftone density of 64 gradations, assuming that the maximum density of 256 gradations was 256 and white was 0. The presence or absence of image defects appearing as high-density point images in the output image was evaluated using a loupe. As a result, an image defect of 0.05 mm or more could not be detected.
As described above, an amorphous silicon electrophotographic photoreceptor capable of obtaining a good image in which image defects were suppressed was obtained by using the clean substrate holder subjected to the surface treatment of the present invention.

101 Material 102 First injection gun 103 Second injection gun 104 Adhering film 105 Distance 106 Injection angle (θ1) of first injection gun
107 Injection angle (θ2) of second injection gun
108 Collision area 109 by first injection gun 109 Collision area 201 by second injection gun 201 Material 202 First injection gun 203 Second injection gun 401 Base holder 402 First injection gun 403 Second injection gun 601 Material 602 First injection gun 603 Second injection gun 604, 605 Spray gun spray pumps 606, 607 Abrasive supply pipes 608, 609 Adjustment tank 610 Processing container 611 Recovery tank 701 Recovery tank 702 Magnetic roller 703 Stripping Blade 704 Conveying roller 705 Stirring blade 706 Processed liquid mixture introduction pipe 707 Discharge pipe 708 Tank 709 Discharge pipe adjustment tank 801 Base holder 802 Skirt part 803 Body 804 Cap part 805 Conductive base body 806 Holder body 901 Recovery container 902 Opening 1001 Injection Ga 1002 Central shaft 1003 Impeller 1004 Length of central shaft from spray gun to workpiece 1005 Spray point 1006, 1009 Gear 1007 Magnetoelectric rotation detector

Claims (12)

  In a surface treatment method for performing surface peeling or deposit removal on a material to be treated by a honing treatment using an abrasive, at least two honing treatments for one material to be treated in one treatment container Using a spray gun at the same time, at least one type of abrasive having a Mohs hardness greater than that of the material to be treated and at least one type of abrasive having a Mohs hardness of less than that of the material to be treated are sprayed from individual guns, and the Mohs hardness The surface treatment method is characterized by spraying the object to be treated in order from an abrasive having a large diameter.   The abrasive having a larger Mohs hardness than the material to be treated is a solid abrasive, and the abrasive having a smaller Mohs hardness than the material to be treated cools and solidifies a material that becomes liquid at room temperature or a gas that becomes gas at room temperature. The surface treatment method according to claim 1, wherein the surface treatment method is performed.   The surface treatment method according to claim 1, wherein the magnetic abrasive and the nonmagnetic abrasive are each sprayed from individual spray guns.   The magnetic abrasive is at least one selected from the group consisting of iron and SUS430, and the nonmagnetic abrasive is at least one selected from the group consisting of zircon, walnut, nylon and glass. The surface treatment method according to claim 3.   The abrasive collision energy per unit area per unit time sprayed from the spray gun to the material to be processed is sprayed to the processing portion in order from the largest. Surface treatment method.   When an angle formed between the normal line of the processing target part and the central axis of the injection gun is an injection angle, and an injection angle of an injection gun for injecting an abrasive whose Mohs hardness is larger than the processing object is θ1, 0 ° < The angle θ1 ≦ 45 °, and θ1 ≦ θ2 <90 °, where θ2 is an injection angle of an injection gun for injecting an abrasive having a Mohs hardness smaller than that of the material to be processed. The surface treatment method according to any one of the above.   The surface treatment method according to any one of claims 1 to 6, wherein a spray gun that sprays an abrasive having a small Mohs hardness has a large spray angle.   The surface treatment method according to any one of claims 1 to 6, wherein the abrasive having a Mohs hardness greater than that of the material to be treated is an iron or stainless steel substantially spherical abrasive.   The surface treatment according to claim 2, wherein the polishing material obtained by cooling and solidifying the material that becomes liquid at normal temperature or the material that becomes gas at normal temperature is ice or dry ice. Method.   The surface treatment method according to any one of claims 1 to 9, wherein the material to be treated is formed of aluminum and / or an aluminum alloy.   The surface treatment method according to claim 1, wherein the material to be treated is a film-forming furnace part for a plasma CVD apparatus. A method for producing an electrophotographic photosensitive member, wherein the electrophotographic photosensitive member is produced by a plasma CVD apparatus using the substrate holder surface-treated by the surface treatment method according to claim 11.

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