JP2907404B2 - Deposition film forming equipment - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION A vacuum charging container which can be evacuated and evacuated to almost a vacuum after a substrate is charged, and a vacuum container which carries the substrate from the vacuum charging container and which can heat the substrate to a constant temperature. A vacuum heating vessel capable of being evacuated, the substrate heated by the vacuum heating vessel being carried in, forming a thin film on the substrate, a vacuum reaction vessel capable of being evacuated to substantially vacuum, and a film formed from the vacuum reaction vessel. A substrate is loaded, the substrate can be cooled to a constant temperature, a vacuum cooling container that can be evacuated to substantially a vacuum, and the substrate is the vacuum charging container,
The present invention relates to a deposition film forming apparatus including: a vacuum heating container, a vacuum reaction container, and a vacuum transfer container that can be evacuated to substantially a vacuum, which are sequentially transferred to the vacuum cooling container.

[0002]

2. Description of the Related Art Conventionally, amorphous silicon, such as hydrogen, has been used as an element member for a semiconductor device, an electrophotographic photoreceptor device, an image input line sensor, an imaging device, a photovoltaic device, and other various electronic elements and optical elements. Also, amorphous deposited films such as amorphous silicon (hereinafter simply referred to as a-Si) compensated with halogen (for example, fluorine, chlorine, etc.) have been proposed, and some of them have been put to practical use.

Conventionally, as a method of forming such a deposited film, a sputtering method, a method of decomposing a source gas by heat (thermal CVD method), and a method of decomposing a source gas by light (optical CV)
Many methods are known, such as a method D) for decomposing a source gas by plasma (plasma CVD method). Among them, the plasma CVD method, that is, the raw material gas is decomposed by direct current or high frequency, microwave glow discharge or the like, and glass, quartz,
The method of forming a thin film deposition film on a substrate made of a heat-resistant synthetic resin film, stainless steel, aluminum or the like has been very practically used at present, such as a method of forming an amorphous silicon deposition film for electrophotography. Various proposals have been made.

FIG. 5 is a schematic view of a typical so-called batch type plasma CVD apparatus. The vacuum reaction vessel 301
A cathode electrode 302 also serving as a side wall, an upper wall 303, and a bottom wall 304 are formed.
3 and the bottom wall 304 are insulated by insulators 305, respectively. The substrate 30 installed in the vacuum reactor 301
6 is grounded and becomes an anode electrode. Some of the substrates 306 are used to heat the substrate to a predetermined temperature before film formation, maintain the substrate at a predetermined temperature during film formation, or anneal the substrate after film formation. A substrate heating heater 307 is provided. The deposition film forming source gas introduction pipe 308 is provided with a large number of gas discharge holes 309 for discharging the source gas into the vacuum reaction vessel 301, and the other end is connected to the deposition film forming source gas through a gas valve 310. It is in communication with the gas supply device 320. An exhaust pipe 311 for evacuating the vacuum reaction vessel 301 is provided with an exhaust valve 31.
2 and communicates with an evacuation device (not shown)
A power supply 313 is connected to the cathode electrode 302.

Next, the operation of the deposited film forming apparatus using the plasma CVD method will be described. The gas in the vacuum reaction vessel 301 is evacuated through the exhaust pipe 311, and the substrate 306 is heated and maintained at a predetermined temperature by the heater 307. Next, via the source gas introduction pipe 308,
For example, in the case of forming an a-SiH deposited film, a source gas such as silane is introduced into the vacuum reaction vessel 301 and the vacuum reaction vessel
Release into. At the same time, for example, a high frequency is supplied from the power source 313 to the cathode electrode 302 and the base (anode electrode) 3.
06 to generate a plasma discharge. The raw material gas in the vacuum reactor 301 is excited and becomes an excited species, and Si ^* ,
Radical particles such as SiH ^{* and the} like (“*” represents an excited state), electrons, ionic particles, etc. are generated, and a chemical interaction between these particles or between these particles and the surface of the substrate is caused on the surface of the substrate. To form a deposited film. However,
In the above-mentioned plasma CVD apparatus, the reaction furnace is exposed to the atmosphere each time a film-forming product is taken out, so that it adsorbs moisture and gas in the atmosphere, thereby deteriorating the quality of the film or becoming unstable. Had the disadvantage of doing so.

In order to eliminate these disadvantages, Japanese Patent Application Laid-Open No.
No. 84678 discloses an improved manufacturing apparatus for a photoelectric conversion member. In other words, a dedicated vacuum vessel is provided for each processing step, and a transfer-only vacuum vessel movable between these vacuum vessels is provided, so that the substrate can be taken in and out and moved between the processing-only vacuum vessel and the transfer-only vacuum vessel. Is disclosed.

[0007] These conventional techniques have made it possible to mass-produce photoconductive materials with a certain quality.
FIG. 6 shows an example of a conventional deposited film forming apparatus improved in this way. FIG. 6 is a layout view of the entire deposited film forming apparatus, which shows a vacuum charging vessel 410 for assembling a substrate in a holding member (not shown) in a clean atmosphere and applying a vacuum, and heating and holding the substrate at a predetermined temperature. Vacuum heating container 4
11 and a vacuum reactor 412 for forming a deposited film
A vacuum cooling container 413 for cooling and taking out the holding member after forming the deposited film, and a vacuum charging container 41
0, vacuum transfer container 4 for sequentially transferring to vacuum heating container 411, vacuum reaction container 412, and vacuum cooling container 413
34. Vacuum charging container 410, vacuum heating container 4
11, the vacuum reaction vessel 412, and the vacuum cooling vessel 413 have exhaust devices 414, 415, 416, 417 and exhaust valves 430, 431, 432, 433, respectively. Are connected to the gate 435 and the gates 422 and 42
3, 424, 425 have vacuum evacuation devices 418, 419, 420, 421 and vacuum valves 426, 427, 428, 429 for evacuating the respective spaces.

For example, when the holding member is put in and out of the vacuum heating container 411, the gate 435 of the vacuum transfer container 434 is brought into close contact with the gate 423 of the vacuum heating container 411,
The space between 35 and the gate 423 is evacuated by the vacuum exhaust device 419. Next, the gates 435 and 423 are opened, and the inside of the vacuum heating container 411 and the vacuum transfer container 434 are moved by a vertical movement mechanism (not shown) provided in the vacuum transfer container 434.
Of the holding member in the inside. FIG. 7 shows the holding member 443.
Is a schematic diagram showing a state in which is carried into a vacuum reaction vessel 412. In the figure, the vacuum reaction vessel 412 includes a cathode electrode 442 also serving as a side wall, a gate 424 also serving as an upper wall, a cathode electrode 442 and a bottom wall 444, and the cathode electrode 442, the gate 424, and the bottom wall 444 Each is insulated by glass 445. The holding member 443 installed in the vacuum reaction vessel 412 holds the base 446, and
46 is grounded and becomes an anode electrode. In the base 446, a heater 447 for heating the base is provided.
It is used for heating the substrate to a predetermined temperature before film formation, maintaining the substrate at a predetermined temperature during film formation, or annealing the substrate after film formation. The deposition film forming source gas introduction pipe 448 is provided with a large number of gas discharge holes 449 for discharging the source gas into the vacuum reactor 412, and the other end is connected to the deposition film forming source gas via a valve 450. It communicates with the gas supply device 451. Vacuum reactor 41
An exhaust pipe 452 for evacuating the inside of the pump 2 is provided with an exhaust valve 4.
The cathode electrode 442 is connected to a power supply 453.

The procedure for forming a deposited film will be described below.

First, the base is placed on the holding member 443, and
The holding member 44 is placed in the vacuum charging container 410 placed in the state of FIG.
3 through the exhaust valve 430 by the exhaust device 414
Vacuum container 410 is evacuated. Then vacuum transfer volume
The container 434 is moved, and the gate 43 of the vacuum transfer container 434 is moved.
5 and the gate 422 of the vacuum charging container 410 are connected to each other.
Then, the connection between these gates 435 and 422 is evacuated.
Vacuum device 418 provides vacuum through vacuum valve 426
I do. After that, open gates 435 and 422 and carry vacuum
By an elevating mechanism (not shown) provided in the feeding container 434
The holding member 443 is moved from the vacuum charging container 410 to the vacuum transfer container.
Transfer to 434, close gates 435 and 422 and apply vacuum
The container 410 and the vacuum transfer container 434 are separated from each other. Security
The vacuum transfer container 434 containing the holding member 443 is vacuum-applied.
Moved over the heat vessel 411 while the vacuum input vessel 410
Prepares for the next insertion of the substrate after introducing the atmosphere. Vacuum heating capacity
Vacuum transfer container 434 moved to
The same as when removing the holding member 443 from the container 410
Operation is performed, and the vacuum heating container
The holding member 443 is carried into the vacuum heating container 411.
The substrate is heated to a predetermined temperature by a heating heater (not shown) inside.
Heat and hold each time. Once the substrate has reached the specified temperature,
The same gate operation and transfer can be performed by the empty transfer container 434.
Then, the holding member 443 is carried into the vacuum reaction vessel 412.
You. On the other hand, the vacuum heating vessel 411 continues to be evacuated.
Ready for the insertion of the next substrate. In the vacuum reactor 412
Is heated at a predetermined temperature by the heater 447 for heating.
Heat and hold each time. Next, from the gas supply device 451,
For example, an a-SiH deposition film is formed through the gas introduction pipe 448.
In the case of forming, raw material gas such as silane is reacted in vacuum
The raw material gas introduced into the container 412 is supplied to the gas introduction pipe 448.
From the gas discharge hole 449 into the vacuum reaction vessel 412.
It is. At the same time, for example, a high frequency
Vacuum reactor 412 (cathode electrode) and substrate 446 (A
(A node electrode) to generate a plasma discharge. true
The gas in the empty reaction vessel 412 is excited and becomes an excited species,
^* , SiH ^* ("*" Indicates an excited state)
Cal particles, electrons, ionic particles, etc. are generated and these particles
Chemical interaction between particles or between these particles and the substrate surface
A deposited film is formed on the surface of the substrate 446 by use.

When the film forming process is completed, the vacuum transfer container 43
4 is moved onto the vacuum reaction vessel 412 and the gate 435 of the vacuum transfer vessel 434 and the gate 4 of the vacuum reaction vessel 412 are moved.
24 are connected to each other, and the connection between the gates 424 and 435 is evacuated by the vacuum exhaust device 420 via the vacuum valve 428. Thereafter, the gates 435 and 424 are opened, and the holding member 443 is moved from the vacuum reaction container 412 to the vacuum transfer container 434 by an elevating mechanism (not shown) provided in the vacuum transfer container 434, and the gates 435 and 424 are closed and the vacuum is removed. The reaction container 412 and the vacuum transfer container 434 are separated from each other.

The vacuum transfer container 434 in which the holding member 443 is transferred is moved above the vacuum cooling container 413, while the vacuum reaction container 412 is evacuated to prepare for the next insertion of the base. The same operation as when the holding member 445 is taken out from the vacuum reaction container 412 is performed on the vacuum transfer container 434 moved onto the vacuum cooling container 413, and the holding member is loaded from the vacuum transfer container 434 to the vacuum cooling container 413, and the vacuum After cooling the substrate in the cooling container 413, the inside of the vacuum cooling container 413 is set to the atmospheric pressure, and the substrate 446 is taken out.

[0013]

It is possible to manufacture a deposited film with a certain device efficiency (high yield and high operation rate) from such a conventional deposited film forming apparatus. In addition, if the inside of the vacuum vessel is strictly cleaned, it is possible to obtain a deposited film with few defects. However, in these conventional deposited film forming apparatuses, for example, when manufacturing a product requiring a relatively large deposited film having a large area, such as an electrophotographic photoreceptor, the efficiency of the apparatus is high and the image forming process is performed by an electrophotographic process. It is difficult to obtain a deposited film with few image defects.

Further, at present, the electrophotographic apparatus is required to have higher image quality, higher speed, and higher durability. As a result, in the electrophotographic photoreceptor, it is required to further improve the optical characteristics and the electric characteristics and to extend the durability in all environments while maintaining high charging ability and high sensitivity.

In recent years, optical exposure systems, developing devices, transfer devices, and the like in electrophotographic apparatuses have been improved in order to improve the image characteristics of electrophotographic apparatuses. Improvements in characteristics have been required. In particular, as a result of the improvement in the resolution of images, it is necessary to reduce the number of white or black spot image defects, commonly called "pots", and in particular, to reduce the small-sized "potches" that were not often considered in the past. It has come to be. In particular, with regard to “pochi”, most of the cause is abnormal growth of a film called a spherical projection, and it is very important to reduce the number of occurrences. It has been confirmed that dust, such as dust and dirt, adhering to the substrate triggers the growth of the spherical projections. For this reason, the substrate before film formation is precisely cleaned, and set in a vacuum charging container in a dust-controlled environment such as a clean room, so that dust adheres to the substrate as much as possible. Furthermore, by strictly cleaning the processing containers such as the vacuum charging container, the vacuum heating container, the vacuum reaction container, and the vacuum transfer container, dust adheres to the substrate before film formation during transfer and each process as much as possible. I try to avoid it.

Certainly, by cleaning each processing container as described above, it is possible to form a film to some extent continuously thereafter while reducing the number of spherical projections. However, when the film is formed more continuously, the number of spherical projections increases, and the image characteristics are greatly reduced. On the other hand, frequent cleaning makes it possible to avoid an increase in spherical projections. However, in that case, it is necessary to stop the apparatus, so that the operation rate of the apparatus decreases.

The reason why the number of spherical projections increases is that the dust in each processing container such as a vacuum charging container, a vacuum heating container, a vacuum reaction container, and a vacuum transfer container increases as film formation is repeated,
This is because the probability that dust adheres to the substrate before film formation increases. When an amorphous silicon deposition film is formed in a vacuum reactor by a plasma CVD method, a by-product called polysilane is generated. This is in the form of fine powder, and is deposited on the wall surface of the vacuum reactor after film formation. In addition, the deposited film is formed not only on the substrate, but also on a part of a wall surface of the vacuum reaction vessel and a source gas introduction part, for example. In particular, when a relatively thick deposited film is formed as in an electrophotographic photoreceptor, these films are easily peeled. When film peeling occurs, the strips scatter into the vacuum reactor. When unloading the substrate from the vacuum reaction vessel after the film formation in such a situation, the vacuum transfer vessel is in communication with the vacuum reaction vessel, so the inside of the vacuum transfer vessel is contaminated by the polysilane and film fragments. I will. In addition, if the film peels off from the substrate or the substrate holding member while the substrate after the film formation is being transferred to the vacuum cooling container, the vacuum transfer container is further contaminated. If the substrate is transported for the next film formation in a situation where the vacuum transport container is contaminated with dust, the probability that dust adheres to the substrate increases. Furthermore, since the vacuum transfer container communicates with the vacuum charging container and the vacuum heating container for transferring the substrate, if the vacuum transfer container is contaminated with dust at that time, the vacuum charging container and the vacuum heating container are also contaminated. When performing continuous film formation,
Since the above is repeated, after each processing container is cleaned, the number of spherical projections increases each time film formation is repeated, despite the small number of spherical projections.

On the other hand, when forming a deposited film, stabilizing the optical and electrical characteristics of the deposited film is an important factor for increasing the yield. for that reason,
Various deposition parameters (for example, source gas flow rate, internal pressure, high-frequency power, etc.) during the formation of the deposited film are managed so as to be always constant, so that variations in characteristics are minimized. However, even though the film formation parameters are strictly controlled, the characteristics are degraded. The reason for this is
When unloading the substrate from the vacuum reaction vessel after the film formation, the vacuum transfer vessel communicates with the vacuum reaction vessel. However, since there is residual gas of the source gas used for film formation in the vacuum reaction vessel, the residual gas Is mixed into the vacuum transfer container and is adsorbed on the inner wall of the vacuum transfer container. Alternatively, the raw material gas adsorbed on the substrate and the holding member is desorbed while the substrate is being transferred to the vacuum cooling container, and is adsorbed on the inner wall of the vacuum transfer container. It is considered that during transport of the next substrate for forming a deposited film, the substrate is detached from the inner wall of the vacuum transport container and exerts some influence on the surface of the substrate before film formation. Alternatively, the impurities desorbed from the inner wall of the vacuum transfer container are adsorbed on the base and the holding member, and the impurities are separated from the base and the holding member during the formation of the deposited film and are mixed into the deposited film. It is thought to occur.

Further, in the conventional deposited film forming apparatus, there is a waiting time of each processing vessel due to the transport of the substrate, and this waiting time is one factor which hinders a reduction in manufacturing tact. The waiting time means, for example, that the film formation is completed in the vacuum reaction vessel, the substrate after the film formation is carried out, and the film formation can be started immediately when the next substrate is carried in.
However, the vacuum transfer container cannot move to a series of operations for transferring the substrate to the vacuum reaction container until the substrate on which the film has been formed is carried into the vacuum cooling container. Therefore, the vacuum reaction container is in a “waiting” state until the vacuum transport container carries the film-formed substrate into the vacuum cooling container. This “waiting” time is called a waiting time. An increase in the waiting time is one of the causes of lowering the utilization efficiency of the apparatus, which is contrary to a reduction in manufacturing tact. The microwave CVD method can form a film at a higher deposition film speed than other deposition film formation methods. Certainly, the film formation time can be reduced by forming the deposited film by the microwave CVD method, but in this case, the ratio of the waiting time to the manufacturing tact becomes large, and the advantage of the high-speed film formation by the microwave CVD method is obtained. Has not been fully utilized in shortening the manufacturing tact time.

The above-described conventional deposited film forming apparatus has a drawback that it is difficult to produce a deposited film of high quality with a small number of spherical projections on a large-area substrate with high apparatus efficiency.

An object of the present invention is to provide a plasma C as described above.
By overcoming the problems of the conventional deposited film forming apparatus by the VD method, a deposited film having good characteristics to be used as an element member of a semiconductor device, other various electronic elements, and optical elements can be formed by a plasma CVD method with high apparatus efficiency. An object of the present invention is to provide a deposited film forming apparatus capable of forming a high quality deposited film with reduced defects when forming an amorphous silicon deposited film having a relatively thick film thickness by a plasma CVD method with high apparatus efficiency. It is to provide a device.

[0022]

A first vacuum transfer container for sequentially transferring a substrate before film formation from a vacuum charging container to a vacuum heating container, a vacuum heating container to a vacuum reaction container, and a film formation device. And a second vacuum transfer container for transferring the used substrate from the vacuum reaction container to the vacuum cooling container.

[0023]

A first vacuum transfer container in which the vacuum transfer container transfers only the substrate before film formation, and a second vacuum transfer container in which only the substrate after film formation is transferred.
Since the first vacuum transfer container does not communicate with the vacuum reaction container immediately after the completion of the film formation and does not transfer the substrate after the film formation, Is not contaminated by dust sources such as Further, the first vacuum transfer container remains in the vacuum reaction container,
Since there is no contamination by the residual gas of the source gas used for the film formation, the substrate before the film formation is not affected at all, and the deposited film is not affected at all. Since the second vacuum transfer container does not communicate with the vacuum charging container and the vacuum heating container, the vacuum charging container and the vacuum heating container are not contaminated by the dust source as described above. Further, the first vacuum transport container transports only the substrate before film formation.
And a second vacuum transfer container for transferring only the substrate after film formation, so that the process of transferring the substrate before film formation and the process of transferring the substrate after film formation can be performed simultaneously. The substrate can be efficiently transported, the waiting time occupying the manufacturing tact is reduced, and the advantage of high-speed film formation by the microwave CVD method can be directly reflected on the manufacturing tact.

In the present invention, the combination of the numbers of the vacuum charging vessel, the vacuum heating vessel, the vacuum reaction vessel, and the vacuum cooling vessel is selected so as to minimize the waste in each processing time. In addition, a high-frequency or microwave power supply used for a group of vacuum reaction vessels, an exhaust pump, a reaction gas introduction system,
Valves, vacuum gauges, etc. are commonly or individually installed as most suitable depending on the application.

Further, the method for heating the substrate in the present invention is as follows.
Any heating element having a vacuum specification may be used. More specifically, a sheet-shaped winding heater, a plate-shaped heater,
An electric resistance heating element such as a ceramic heater, a heat radiation lamp heating element such as a halogen lamp or an infrared lamp, a heating element using a liquid or a gas as a heating medium, or the like by a heat exchange means may be appropriately selected and used. The surface material of the heating element is metals such as stainless steel, nickel, aluminum, copper, ceramics,
A heat-resistant polymer resin or the like can be used. In the present invention, for example, silane (SiH
₄ ), source gas for forming amorphous silicon such as disilane (Si ₂ H ₆ ), germane (GeH ₄ ), methane (C
H ₄ ) or another functional deposition film forming raw material gas or a mixed gas thereof. Hydrogen (H ₂ ), argon (Ar), helium (H
e), neon (Ne) and the like. Further, as a characteristic improving gas for changing the band gap width of the deposited film, an element containing a nitrogen atom such as ammonia (NH ₃ ) and nitrogen (N ₂ ), oxygen (O ₂ ), nitrogen oxide (NO), An element containing an oxygen atom such as nitrous oxide (N ₂ O), methane (CH
_4), ethane (C ₂ H _6), ethylene (C ₂ H _4), acetylene (C ₂ H _2). Hydrocarbons such as propane (C ₃ H ₈ ), silicon tetrafluoride (SiF ₄ ), and silicon hexafluoride (S
Fluorine compounds such as i ₂ F ₆ ) and germanium tetrafluoride (GeF ₄ ) or a mixed gas thereof can also be used. Furthermore, the present invention is similarly effective when dopant gases such as diborane (B ₂ H ₆ ), boron fluoride (BF ₃ ), and phosphine (PH ₃ ) are simultaneously introduced into the discharge space for the purpose of doping impurities. is there.

As the base material used in the present invention, a conductive material or a material whose surface is subjected to a conductive treatment is used. For example, stainless steel, Al, Cr, Mo, Au, In, N
Metals such as b, Te, V, Ti, Pt, Pd, and Fe, alloys thereof, and synthetic resin glasses such as polycarbonates whose surfaces are conductively treated, ceramics, and paper are usually used. When the substrate has a cylindrical shape, the diameter of the substrate is not particularly limited, but is practically about 20 mm or more and 500 mm or less, and the length is preferably about 10 mm or more and 1000 mm or less.

In the present invention, any substrate temperature is effective at the time of forming a deposited film. However, in the case of depositing amorphous silicon, the substrate temperature is preferably from 20 ° C. to 500 ° C., and more preferably from 50 ° C. to 450 ° C. Preferred for showing results.

[0028]

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

FIG. 1 shows an embodiment of the present invention. FIG. 2 is an arrangement view of the entire deposited film forming apparatus. FIG.
43 is a schematic diagram of the inside of a vacuum reaction vessel 112 when a deposition film 43 is loaded and a deposited film is formed by a high-frequency plasma CVD method.

The deposition film forming apparatus of this embodiment includes a vacuum charging container 110 into which a holding member 143 with a substrate 146 incorporated therein is charged in a clean atmosphere, and a vacuum charging container 110 which can be evacuated to a substantially vacuum, and a substrate 146 at a predetermined temperature. A vacuum heating vessel 111 for heating and holding, and a vacuum reaction vessel 11 for forming a deposited film
2, a vacuum cooling container 113 for cooling and taking out the holding member 143 after forming the deposited film, and a holding member 14 before forming the film.
3 and the substrate 146 are sequentially transferred from the vacuum charging container 110 to the vacuum heating container 111, and from the vacuum heating container 111 to the vacuum reaction container 112, and the holding member 143 and the substrate 146 after film formation are evacuated. Second vacuum transfer container 1 for transferring from reaction container 112 to vacuum cooler 113
02. The vacuum charging container 110, the vacuum heating container 111, the vacuum reaction container 112, and the vacuum cooling container 113 include exhaust devices 114, 115, 116, 117 for exhausting the inside of each container to a vacuum, and exhaust valves 130, 131, 132, 133, when the first vacuum transfer container 101 is connected to each of the containers 110, 111, 112, the first gate 134 and the gates 122, 12
Evacuation devices 118, 119, 120 for evacuating the respective spaces 3, 124, and vacuum valves 126, 1
27, 128, and the second gate 135 when the second vacuum transfer container 102 is connected to each of the containers 112, 113.
And vacuum evacuation devices 120 and 121 for evacuating the respective spaces of the gates 124 and 125 and the vacuum valve 12
8,129. The vacuum reaction vessel 112 has a cathode electrode 142 also serving as a side wall and a gate 1 serving also as an upper wall.
24 and the bottom wall 144, and the cathode electrode 142
And the gate 124, and the cathode electrode 142 and the bottom wall 144 are insulated by an insulator 145, respectively. Vacuum reactor 1
The holding member 143 installed in the inside 12 holds the base 146, and the base 146 is grounded and becomes an anode electrode. A heater 147 for heating the substrate is provided in the substrate 146, and the substrate 146 is heated to a predetermined temperature before film formation, the substrate 146 is maintained at a predetermined temperature during film formation, or formed. It is used for annealing the substrate 146 after the film. The source gas introduction pipe 148 for forming a deposited film includes:
A large number of gas discharge holes 149 for discharging the source gas are provided in the vacuum reaction vessel 112, and the other end is provided with a valve 1
It communicates with the source gas supply device 151 for depositing film formation through 50. An exhaust pipe 152 for evacuating the inside of the vacuum reaction vessel 112 is connected to an exhaust device 1 through an exhaust valve 132.
16 and the cathode electrode 142 is connected to the power supply 15.
3 are connected.

Next, the operation of this embodiment will be described.

First, the base 146 is placed on the holding member 143, and the holding member 143 is placed in the vacuum charging container 110 placed in the atmosphere, and the vacuum charging container 110 is evacuated to the exhaust device 11.
4 to make a vacuum through the exhaust valve 130. next,
The first vacuum transfer container 101 is moved, and the first gate 134 and the vacuum input container 1 of the first vacuum transfer container 101 are moved.
10 gates 122 are connected to each other, and these gates 1
The connection between 34 and 122 is evacuated by the vacuum exhaust device 118 via the vacuum valve 126. Thereafter, the first gate 134 and the gate 122 are opened, and the holding member 143 is moved from the vacuum charging container 110 to the first vacuum transfer container 101 by an elevating mechanism (not shown) provided in the first vacuum transfer container 101. Then, the first gate 134 and the gate 122 are closed, and the vacuum charging container 110 and the first vacuum transfer container 101 are closed.
Are separated from each other. The first vacuum transfer container 101 containing the holding member is moved to a position above the vacuum heating container 111, while the vacuum charging container 110 is ready for the next insertion of the base after introducing the atmosphere. The same operation as when the holding member 143 is removed from the vacuum charging container 110 is performed on the first vacuum transfer container 101 moved onto the vacuum heating container 111, and the first vacuum transfer container 101 is moved from the first vacuum transfer container 101 to the vacuum heating container 111. Holding member 1
The substrate 43 is carried in, and the base 146 is heated and held at a predetermined temperature by a heater (not shown) for heating in the vacuum heating container 111. When the temperature of the base 146 reaches a predetermined temperature, a similar gate operation and transfer are performed by the first vacuum transfer container 101, and the holding member 143 is loaded into the vacuum reaction container 112. On the other hand, the vacuum heating container 111 is continuously evacuated to prepare for the next insertion of the base. In the vacuum reaction vessel 112, the loaded substrate is heated and held at a predetermined temperature by a heater 147 for heating. Next, from the gas supply device 151,
In the case of forming an a-SiH deposition film, for example, via the gas introduction pipe 148, a source gas such as silane is introduced into the vacuum reaction vessel 112, and the source gas is supplied to the gas introduction pipe 148.
Are discharged into the vacuum reaction vessel 112 from the gas discharge holes 149 of the first and second portions. At the same time, a high frequency is applied from the power supply 153 between the vacuum reaction vessel 112 (cathode electrode) and the base 146 (anode electrode) to generate plasma discharge. The gas in the vacuum reaction vessel 112 is excited and becomes an excited species, and Si ^* , S
Radical particles such as iH ^{* and the} like (“*” represents an excited state), electron, ionic particles, and the like are generated, and the chemical interaction between these particles or between these particles and the substrate surface causes the surface of the substrate 146 to enter. A deposited film is formed thereon.

At the stage where the film forming process is completed, the second vacuum transfer container 102 is moved above the vacuum reaction container 112, and the second gate 135 of the second vacuum transfer container 102 and the gate 124 of the vacuum reaction container 112 are moved. Are connected to each other, and the connection between these two gates 135 and 124 is evacuated by the vacuum exhaust device 120 via the vacuum valve 128. Second gate 1
35, opening the gate 124 to open the second vacuum transfer container 102
The holding member 14 is moved by an elevating mechanism (not shown)
3 from the vacuum reaction vessel 112 to the second vacuum transfer vessel 102
Then, the second gate 135 and the gate 124 are closed to separate the vacuum reaction vessel 112 and the second vacuum transfer vessel 102 from each other. The second vacuum transfer container 102 in which the holding member 143 has been transferred is moved onto the vacuum cooling container 113, while the vacuum reaction container 112 is evacuated continuously,
Prepare for the insertion of the next substrate. The second vacuum transfer container 102 moved onto the vacuum cooling container 113 is provided with a vacuum reaction container 112.
The holding member 143 is carried into the vacuum cooling container 113 from the second vacuum transfer container 102 by performing the same operation as when the holding member is taken out from the second container. Substrate 1 in vacuum cooling container 113
After the 46 is cooled, the inside of the vacuum cooling container 113 is set to the atmospheric pressure, and the base 146 is taken out.

Next, the present invention is applied to microwave plasma CVD.
An example in which the present invention is applied to formation of a deposited film by a method will be described.

FIG. 3 is a schematic view showing a state in which the holding member 276 holding the dielectric window 277 and the base 278 has been carried into the vacuum reaction vessel 212, and FIG. 4 is a perspective view before carrying the holding member 276. It is.

An exhaust device 216 for evacuating the vacuum reactor 212 is connected to the vacuum reactor 212 via an exhaust valve 232. The holding member 276 carried into the vacuum reaction vessel 212 has a dielectric window 277 and a base 27.
8 is held, and the holding member 276 is
It also serves as the 12 opening / closing parts. That is, the holding member 276
Is in close contact with the inside of the side wall of the vacuum reaction vessel 212 via a vacuum seal member 279.
12 and the holding member 276 form a deposited film formation space sealed. A rotation shaft 280 for supporting and rotating the base 278 is connected to the motor 281. A heater 282 for heating the substrate 278 is provided in the substrate 278, and a source gas introduction pipe 283 for supplying the source gas into the vacuum reaction vessel 212 is connected to a source gas supply source (not shown) through a gas valve 284. )It is connected to the.
A gate 224, a vacuum valve 228, and a vacuum evacuation device 220 are provided similarly to the vacuum reaction vessel 112 shown in FIG.

Next, the operation of this embodiment will be described.
After carrying the holding member 276 together with the base 278 into the vacuum reaction container 212 by the vacuum transfer container, the space formed by the gate 224 and the holding member 276 is brought into the atmospheric pressure state, the gate 224 is opened, and the microwave is applied to the dielectric window 277. A waveguide (not shown) connected from a power supply is connected.
At this time, as described above, the holding member 276 doubles as the opening / closing part of the vacuum reaction vessel 212, and the vacuum sealing member 279.
As a result, the deposition film forming space is kept in a vacuum.

After connecting the microwave waveguide, the substrate 2
While rotating 78, it is heated and maintained at a predetermined temperature. Next, a source gas is introduced through a gas introduction pipe 283, and while maintaining a predetermined degree of vacuum, a frequency of 2.45 GHz is used.
The microwave of z is introduced through the dielectric window 277 to decompose the source gas and form a deposited film on the base 278.

After the formation of the deposited film, the introduction of the microwave and the source gas, the heating and the rotation of the substrate are stopped, and the waveguide is removed from the dielectric window 277. Next, after the gate 224 is closed and the space formed by the gate 224 and the holding member 276 is evacuated, the holding member 276 is moved to the vacuum transfer container 212 in the same manner as in the previous embodiment, and thereafter, the same applies. The operation is performed. In this embodiment, the number of the bases 278 is not particularly limited.

Hereinafter, test examples performed by the present inventors will be described. Test Example 1 Using a deposition film forming apparatus shown in FIG.
According to the procedure described above, 30 cycles of an amorphous silicon electrophotographic photosensitive member were formed on the aluminum cylindrical substrate according to the procedure described above. The produced electrophotographic photosensitive member was installed in an electrophotographic apparatus in which a copying machine NP-9330 manufactured by Canon Inc. was modified for an experiment, and the electrophotographic characteristics such as sensitivity, residual potential, ghost, and white spots, and the electrophotographic photosensitive member were set. Was evaluated for the number of spherical projections generated on the surface and the time required for film formation for 30 cycles.

Each item was evaluated by the following methods. (1) Number of spherical projections The number of spherical projections generated on the surface of the produced electrophotographic photosensitive member was measured. The number of spherical protrusions is a unit area (1 cm × 1 cm × 3) of three locations in the circumferential direction above and below the cylindrical substrate.
The number of spherical projections having a diameter of 20 μm or more per 1 cm) was counted using an optical microscope. (2) Sensitivity The electrophotographic photosensitive member is charged to a dark surface potential of 400 V. Then, the light image is immediately emitted. The light image was irradiated with light excluding light in the wavelength range of 550 nm or less using a filter using a xenon lamp light source. At this time, the surface potential of the light portion of the electrophotographic photosensitive member is measured by a surface potentiometer. The exposure amount is adjusted so that the bright portion surface potential becomes a predetermined potential, and the exposure amount at this time is used as the sensitivity. (3) Residual potential After the electrophotographic photosensitive member was charged to a surface potential of a dark portion of 400 V, a photo image was immediately irradiated. The light image was obtained by using a xenon lamp light source and using a filter to remove light in a wavelength range of 550 nm or less excluding 1.5 nm.
1xs. Irradiated for sec. At this time, the surface potential of the light portion of the electrophotographic photosensitive member is measured by a surface voltmeter, and the surface potential at this time is defined as a residual potential. (4) Ghost Ghost test chart (part number:
FY9-9040) with a black circle having a reflection density of 1.1 and a diameter of 5 mm attached to the leading edge of the image on the platen, and a halftone chart manufactured by Canon Inc. superimposed thereon. The difference between the reflection density of φ5 mm of the ghost test chart and the reflection density of the halftone portion observed on the half-length copy was measured.

In each case, ◎ means “particularly good”, and ○
Indicates “good”, Δ indicates “no practical problem”, and “x” indicates “practical problem”. (5) White Pochi Canon Inc. full black chart (product number: FY9-
9073) was placed on a platen and a copy image obtained when copying was evaluated for white spots having a diameter of 0.2 mm or less within the same area, and the following judgment was made.

◎ indicates “especially good”, は indicates “good”, Δ indicates “no problem in practical use”, and X indicates “problem in practical use”. (6) Time required for film formation in 30 cycles The time from when the substrate in the first cycle was charged into the vacuum charging container to when the substrate after film formation in the 30th cyclone was loaded into the vacuum cooling container was 30 cycles. The time required for film formation.

Table 2 shows the evaluation results.

In Table 2, the number of spherical projections, the sensitivity and the residual potential were respectively 30 when the number of spherical projections, the sensitivity and the residual potential of the electrophotographic photosensitive member prepared in the first cycle were 100. The numbers, sensitivities and residual potentials of the spherical projections of the electrophotographic photosensitive member produced at the cycle are shown relatively. Further, as for the time required for film formation for 30 cycles, when the time required for using the deposited film forming apparatus of the present invention was set to 100, the result of Comparative Example 1 using the conventional apparatus was relatively calculated. It is expressed in a way. Comparative Example 1 An electrophotographic photosensitive member was manufactured in the same manner as in Test Example 1 using the deposited film forming apparatus shown in FIG. 6, and the same evaluation as in Test Example 1 was performed. Table 2 shows the obtained results. In Table 2, the number of spherical projections, the sensitivity, and the residual potential are shown assuming that the number of spherical projections, the sensitivity, and the residual potential of the electrophotographic photosensitive member manufactured in the first cycle in Test Example 1 are 100. The relative number, sensitivity, and residual potential of the spherical projections of the electrophotographic photosensitive member produced at the first cycle and the 30th cycle are shown relatively.

As is evident from Table 2, it was found that the use of the deposited film forming apparatus of the present invention makes it possible to produce an electrophotographic photosensitive member having few spherical projections and excellent characteristics such as image characteristics and sensitivity. Further, the tact time of the deposited film of the present invention can be further reduced. Test Example 2 Using the deposited film forming apparatus of the present invention shown in FIG. 1 and under the conditions shown in Table 3, a micro-process was performed on a mirror-finished aluminum cylindrical substrate having a diameter of 108 mm according to the procedure described above. An amorphous silicon electrophotographic photosensitive member was prepared for 30 cycles by a wave glow discharge method. The prepared electrophotographic photosensitive member was installed in an electrophotographic apparatus in which a copying machine NP-8550 manufactured by Canon Inc. was modified for experiments, and the same evaluation as in Test Example 1 was performed. Table 4 shows the results of the above evaluations.

In Table 4, the number of spherical projections, the sensitivity and the residual potential were respectively 30 when the number of spherical projections, the sensitivity and the residual potential of the electrophotographic photosensitive member produced in the first cycle were 100. The numbers, sensitivities and residual potentials of the spherical projections of the electrophotographic photosensitive member produced at the cycle are shown relatively. Further, as for the time required for film formation for 30 cycles, when the time required for using the deposited film forming apparatus of the present invention was set to 100, the result of Comparative Example 1 using the conventional apparatus was relatively calculated. It is expressed in a way. Comparative Example 2 An electrophotographic photosensitive member was manufactured in the same manner as in Test Example 2 using the deposited film forming apparatus shown in FIG. 6, and the same evaluation as in Test Example 2 was performed. Table 2 shows the obtained results. In Table 2, each of the number of spherical projections, sensitivity, and residual potential was 1 in Test Example 1.
The number of spherical projections of the electrophotographic photosensitive member manufactured in the cycle,
When the sensitivity and the residual potential are set to 100, the number, the sensitivity, and the residual potential of the spherical projections of the electrophotographic photosensitive member manufactured in the first cycle and the 30th cycle are relatively expressed.

As is clear from Table 2, it was found that the use of the deposited film forming apparatus of the present invention can produce an electrophotographic photosensitive member having few spherical projections and further excellent characteristics such as image characteristics and sensitivity. Further, by using the deposited film forming apparatus of the present invention, it has become possible to shorten the manufacturing tact. Test Example 3 Using the deposition film forming apparatus of the present invention shown in FIG. 1, the film forming conditions were changed to the conditions shown in Table 5, and the other conditions were the same as in Test Example 2 to produce 60 electrophotographic photosensitive members. did. Then, the same evaluation as in Test Example 2 was performed, and it was found that an electrophotographic photoreceptor having few spherical protrusions and excellent characteristics such as image characteristics and sensitivity was produced as in Test Example 2.

Table 1 Table 2 Table 3 Table 4 Table 5

[0050]

As described above, the present invention provides a first vacuum transfer container for transferring only a substrate before film formation and a second vacuum transfer container for transferring only a substrate after film formation. Due to this, the number of spherical protrusions can be significantly reduced because dust adhering to the substrate before film formation is reduced, and
Since the substrate before film formation is not contaminated by the residual material gas, the deposited film can be formed stably without deteriorating the characteristics of the deposited film, and the transfer of the substrate before film formation and the transfer of the substrate after film formation. At the same time, the ratio of the waiting time to the manufacturing cost can be reduced, and the deposition film can be formed at a high productivity and at a low cost by fully utilizing the advantage of the high-speed film formation by the microwave CVD method. .

[Brief description of the drawings]

FIG. 1 is a layout view of an entire deposited film forming apparatus showing an embodiment of the present invention.

FIG. 2 is a schematic view of the inside of a vacuum reaction vessel into which a substrate and a holding member have been loaded when the present invention is applied to a high-frequency plasma CVD method.

FIG. 3 is a schematic view of the inside of a vacuum reaction vessel into which a substrate and a holding member have been loaded when the present invention is applied to a microwave plasma CVD method.

FIG. 4 is a perspective view showing a dielectric window, a base, and a holding member in the apparatus of FIG. 3;

FIG. 5 is a schematic sectional view of a conventional batch type plasma CVD apparatus.

FIG. 6 is an overall layout view of a conventional deposited film forming apparatus.

FIG. 7 is a schematic view of a conventional deposited film forming apparatus, showing a state in which a base and a holding member are carried into a vacuum reaction vessel.

DESCRIPTION OF SYMBOLS 101 First vacuum transfer container 102 Second vacuum transfer container 110 Vacuum charging container 111 Vacuum heating container 112 Vacuum reaction container 113 Vacuum cooling container 114-117 Exhaust device 118-121 Vacuum exhaust device 122-125 Gate 126 to 129 Vacuum valve 130 to 133 Exhaust valve 134 First gate 135 Second gate 142 Cathode electrode 143 Holding member 144 Bottom wall 145 Insulator 146 Base 147 Heater 148 Gas introduction pipe 149 Gas emission hole 150 Gas valve 151 Gas supply device 152 Exhaust pipe 153 Power supply 212 Vacuum reaction vessel 216 Exhaust device 220 Vacuum exhaust device 224 Gate 228 Vacuum valve 232 Exhaust valve 276 Holding member 277 Dielectric window 278 Base 279 Vacuum seal member 280 Rotating shaft 28 DESCRIPTION OF SYMBOLS 1 Motor 282 Heater 283 Gas introduction pipe 284 Gas valve 301 Vacuum reaction vessel 302 Cathode electrode 303 Top wall 304 Bottom wall 305 Insulator 306 Base 307 Heating heater 308 Gas introduction pipe 309 Gas discharge hole 310 Gas valve 311 Exhaust pipe 312 Exhaust valve 313 Power supply 320 Gas supply device 410 Vacuum charging container 411 Vacuum heating container 412 Vacuum reaction container 413 Vacuum cooling container 414-417 Exhaust device 418-421 Vacuum exhaust device 422-425 Gate 426-429 Vacuum valve 430-433 Exhaust valve 434 Vacuum transfer container 435 Gate 442 Cathode electrode 443 Holding member 444 Bottom wall 445 Insulator 446 Base 447 Heater 448 Gas introduction pipe 449 Gas discharge hole 450 Gas valve 451 Gas supply device 452 exhaust pipe 453 power supply

Claims (2)

(57) [Claims] 1. A vacuum charging container that can be evacuated and evacuated to a substantially vacuum after a substrate is charged, and a substrate that is loaded from the vacuum charging container and can be heated to a constant temperature and can be evacuated to a substantially vacuum. A vacuum heating container, the substrate heated by the vacuum heating container is loaded, a thin film is formed on the substrate, a vacuum reaction container that can be almost evacuated, and the substrate that has been formed from the vacuum reaction container is A vacuum cooling container that is carried in and can cool the substrate to a constant temperature and can be evacuated to substantially a vacuum, and the substrate is sequentially transferred to the vacuum charging container, the vacuum heating container, the vacuum reaction container, and the vacuum cooling container. A vacuum transport container that can be evacuated to substantially a vacuum, wherein the vacuum transport container is
A first vacuum transfer container for sequentially transferring the substrate before film formation from the vacuum charging container to the vacuum heating container, the vacuum heating container to the vacuum reaction container, and the vacuum reaction container And a second vacuum transfer container that transfers the vacuum film to the vacuum cooling container. 2. The apparatus according to claim 1, wherein a deposited film is formed on the substrate by microwave plasma CVD in said vacuum reactor.