JP2925291B2 - Deposition film forming equipment - Google Patents

Description

Description: TECHNICAL FIELD The present invention relates to a deposited film on a substrate, especially a functional film, especially a semiconductor device, a photosensitive device for electrophotography, a line sensor for image input, an imaging device, and a photovoltaic device. The present invention relates to an apparatus for forming a functional deposition film such as an amorphous semiconductor used for a power element or the like.

[Description of Prior Art]

2. Description of the Related Art Conventionally, amorphous silicon, such as hydrogen or / and halogen, has been used as an element member used for a semiconductor device, a photosensitive device for electrophotography, a line sensor for image input, an imaging device, a photovoltaic element, other various electronic elements, an optical element, and the like. For example, fluorine, chlorine, etc.)
Amorphous silicon compensated by (hereinafter, "a-Si
(H, X). " And the like, and deposited films such as amorphous semiconductors have been proposed, and some of them have been put to practical use.

And such a deposited film is a plasma CVD method, that is,
It is known that the raw material gas is directly or high-frequency, microwave, decomposed by glow discharge, and formed by a method of forming a thin film deposition film on a substrate such as glass, quartz, stainless steel, and aluminum. Various devices have been proposed.

Especially, plasma using microwave glow discharge decomposition in recent years
The CVD method, that is, the microwave plasma CVD method has attracted industrial attention.

The microwave plasma CVD method has the advantages of a higher deposition rate and higher source gas utilization efficiency than other methods.

One example of a microwave plasma CVD apparatus utilizing such advantages is described in Japanese Patent Application Laid-Open No. Sho 60-186849. In the device described in the publication, the substrate is arranged so as to surround the means for introducing microwave energy, so that an internal chamber (ie, a discharge space) is formed, thereby greatly improving the gas use efficiency. Things.

Japanese Patent Application Laid-Open No. 61-283116 discloses an improved microwave system for manufacturing semiconductor members. That is, the publication discloses that an electrode is provided in a plasma space as a plasma potential control, and a desired voltage is applied to the electrode to perform film deposition while controlling ion bombardment of deposition species, thereby improving the characteristics of the deposited film. It discloses a method for causing this to occur.

Thus, in recent years, the plasma CVD method using microwaves (hereinafter, referred to as “μW, PCVD method”) has attracted attention,
Several apparatuses for this purpose have been proposed, and production of the above-mentioned deposited film by the μW, PCVD method on an industrial scale has been attempted. Such a conventionally proposed apparatus using the μW, PCVD method typically has an apparatus configuration as schematically shown in FIG.

In FIG. 4, reference numeral 401 denotes a reaction vessel, which has a vacuum tight structure. 402, 402 'are materials that can efficiently transmit microwave power into the reaction vessel and maintain vacuum tightness (eg, quartz glass, alumina ceramics, etc.).
This is a dielectric window formed by: Reference numeral 403 denotes a microwave power transmission unit formed of a metal waveguide and connected to a microwave power supply (not shown) via a stub tuner (not shown) and an isolator (not shown). An exhaust pipe 404 has one end opened into the vacuum vessel 401 and the other end connected to the exhaust device 406 via the exhaust valve 405. 407 is a cylindrical substrate on which a deposited film is to be formed, and 408 is a cylindrical substrate 4
The discharge space surrounded by 07 is shown.

Deposition film formation by such a conventional deposition film formation method is as follows.
This is performed as follows.

First, with the exhaust valve 405 closed in the reaction vessel 401
A gas such as N ₂ or _Ar is introduced to make the state of atmospheric pressure, a door (not shown) is opened, the inside of the reaction vessel 401 is cleaned, and then a gas discharge pipe is set. At this time, the gas discharge tube and the reaction vessel must be electrically insulated. Next, the cylindrical substrate 407 is set on the rotating shaft 419 and the heater 413. Further, after installing the dielectric window 402, the door (not shown) is closed, and the exhaust pipe 404 is opened by a vacuum pump (not shown).
The reaction vessel 401 is degassed via
Adjust to ^10-7 Torr or less. Next, the temperature of the substrate 407 is heated and maintained by the heater 413 at a temperature suitable for film deposition.

Therefore, the raw material gas is adjusted to a desired flow rate by the mass flow controller 409, and the discharge space 4 is controlled by the gas discharge tube 410.
Introduced to 08. For example, in the case of forming an amorphous silicon deposition film, a source gas such as a silane gas and a hydrogen gas is introduced into the discharge space 408. Simultaneously therewith, a microwave power source (not shown) generates a microwave having a frequency of 500 MHz or more, preferably 2.45 GHz,
Introduced into the reaction vessel 401 through the dielectric windows 402, 402 'through 03.

Further, the raw material gas discharge tube 410 is connected to a DC power supply 411, and applies a predetermined DC voltage at the same time as introducing a microwave to generate a plasma and simultaneously generate the plasma.
An electric field is applied between the substrate and the cylindrical substrate 407. At this time, the cylindrical substrate 407 was electrically grounded (earthed). In this way, the source gas is excited by microwave energy and dissociated, forming a deposited film on the surface of the cylindrical substrate 407. At this time, by rotating the cylindrical base body 407 around the base line direction center axis by the rotation mechanism 421,
A deposited film is formed over the entire circumference of the cylindrical substrate 407.

However, such a conventional apparatus configuration is still inadequate in terms of characteristics and economics when manufacturing a member requiring a large area, a thick film and uniform characteristics such as an electrophotographic photosensitive member. Was.

That is, in the above-described apparatus configuration, since the dielectric window and the gas emission tube are stationary facing the discharge space, a film about 4 to 5 times as thick as the surface of the cylindrical substrate adheres at the end of deposition film formation. Therefore, it is necessary to replace these parts every time. In the above-described conventional apparatus, the inside of the vacuum vessel needs to be once set to the atmospheric pressure in order to replace the dielectric window, the gas discharge tube, and the cylindrical substrate for forming the next deposited film. For this reason, moisture and the like may be adsorbed in the vacuum vessel, which adversely affects the deposited film. For this reason, a method of removing the adsorbed material in the vacuum container by performing sufficient evacuation or sometimes baking the vacuum container has been performed.

In addition, since the installation of the cylindrical substrate for forming the deposited film and the installation of the gas discharge tube must be performed by humans, improvement in quality and yield due to dust generation cannot be expected. Further, in the conventional apparatus configuration, evacuation, heating, film formation, cooling, air leak, substrate and the like are set,
It took time per cycle and was very disadvantageous in terms of cost. Therefore, in order to improve these, industrially, the cylindrical substrate is generally taken in and out in a vacuum atmosphere. However, there are a plurality of cylindrical substrates for forming a deposited film, and further, the gas release tube and the dielectric window are provided. For the replacement, the transfer device becomes complicated, and there are many difficulties in automation.

[Object of the invention]

SUMMARY OF THE INVENTION The present invention overcomes the above-described problems in a conventional deposited film forming apparatus using a μM-PCVD method as described above, and provides a semiconductor device, an electrophotographic photoreceptor device, an image input line sensor, an imaging device, and a photovoltaic device. It is another object of the present invention to provide an apparatus capable of mass-producing a deposited film having good performance as an element member used for various other electronic elements and optical elements by a μW-PCVD method.

[Structure and effect of the invention]

The inventors of the present invention have conducted devoted research to overcome the above-described problems in the conventional deposition film forming apparatus using the μW-PCVD method, and as a result, in order to obtain a stable and high-quality deposition film at high speed,
A plurality of cylindrical substrates and a gas discharge tube that releases a source gas into the discharge space and applies an electric field to the cylindrical substrate tube and a dielectric window for introducing microwaves into the discharge space are transported to the reaction vessel in a vacuum atmosphere. It has been found that the problem can be solved by forming a deposited film.

The present invention has been completed on the basis of the above knowledge, and the gist of the invention is that a means for supplying a raw material gas into a reaction vessel capable of being vacuum-tight, a means for exhausting the reaction vessel, Means for generating microwave discharge plasma, and a plurality of cylindrical substrates held in the reaction vessel, and a deposition film forming apparatus by means of a microwave plasma CVD method having means for rotating, the inside of the reaction vessel A circular dielectric window for introducing microwaves, a plurality of cylindrical substrates arranged so as to surround the dielectric window, and a source gas discharged into a space surrounded by the cylindrical substrates; A dielectric member, a cylindrical substrate, and a holding member having a function of simultaneously holding a source gas discharge tube having a mechanism for applying an electric field between the base and the means for discharging the source gas;
Means for holding the source gas discharge tube, transferring the holding member into the reaction vessel in a vacuum atmosphere, and holding the reaction vessel in a vacuum again after the transfer.
M, in a deposited film forming apparatus by the PCVD method.

According to such an apparatus of the present invention, each time a deposited film is formed,
The cylindrical substrate, gas discharge tube, and microwave introduction derivative, which must be renewed each time, can be simultaneously and easily transported in a vacuum state, increasing the efficiency as a mass production device and causing defective products due to dust generation. Can be further reduced. Further, by providing the gas discharge tube with a mechanism having an electric field between the gas discharge tube and the cylindrical substrate, not only the device is simplified, but also the introduced source gas is excited by microwave power until reaching the substrate, Decomposition and the like are performed, and electrons having a large energy accelerated by the electric field are present around the entire discharge space around the gas introducing means, so that excitation, decomposition and the like are performed smoothly and sufficiently. For this reason, the utilization efficiency of the source gas is greatly improved.

On the other hand, when the source gas reaches the substrate, it is a sufficiently decomposed precursor, has high energy, and has high surface mobility on the substrate, so that a deposited film with low internal stress is formed.

Furthermore, after the source gas is introduced by applying a voltage to the source gas introducing means itself, the ions ionized by the plasma are sufficiently accelerated by the electric field, and bombard the substrate with a large kinetic energy. Therefore, it is possible to sufficiently perform local annealing on the deposited film even at a relatively low voltage on the source gas introducing means, and to form a deposited film having excellent characteristics in order to reduce stress in the film and reduce defects. be able to.

Further, since the gas discharge tube is located surrounded by the cylindrical substrate, the gas discharge tube is more efficiently warmed by preheating in which the cylindrical substrate is heated.

In addition, since the cylindrical substrate, the gas discharge tube, and the dielectric window are already heated before being loaded into the reaction vessel 101, the deposition film is formed on the inner surface of the reaction vessel 101 at room temperature. For this reason, the adverse effect on the deposited film due to impurities (contamination) adhering to the inner surface of the reaction vessel or the like is reduced as compared with the conventional apparatus.

Hereinafter, an apparatus for forming a deposited film by the μW-PCVD method of the present invention will be described with reference to the drawings.

FIGS. 1, 2 and 3 are schematic views schematically showing a typical example of a deposited film forming apparatus by the μW-PCVD method of the present invention.

FIG. 1 is a layout view of the entire mass production apparatus. Numeral 120 is a vacuum vessel for applying a vacuum in a clean atmosphere by incorporating a substrate for forming a deposited film, a dielectric window, and a gas discharge tube into a holding member.
FIG. 3 shows a schematic diagram of a holding member 314 in which a deposition film forming base 307 and a dielectric window 302 are incorporated. 101 is a vacuum container for forming a deposited film, and 140 is a vacuum container for taking out a holding member after forming the deposited film. 130 is the holding member for the vacuum vessel 10
This is a transfer vacuum vessel for moving to positions 1, 120, and 140. 106, 122, 142 are exhaust devices for evacuating each vacuum vessel, 118, 125, 146 are gate valves 131 when the transfer vacuum vessel 130 is connected to the vacuum vessels 101, 120, 140.
And an exhaust device for evacuating the spaces of the gate valves 116, 125 and 143. That is, for example, when the holding member is taken in and out of the vacuum vessel 101, the gate valve 131 of the vacuum vessel 130 is brought into close contact with the gate valve 116 of the vacuum vessel 101, and the space between the gate valve 131 and the gate valve 116 is evacuated by the exhaust device 118. I do. Next, the gate valves 116 and 131 are opened, and the holding member is moved in the vacuum vessel 101 and the vacuum vessel 130 by a vertical movement mechanism (not shown) provided in the vacuum vessel 130.

FIG. 2 is a schematic diagram showing a state in which a holding member holding a dielectric window and a substrate for forming a deposited film is carried into a vacuum vessel 201.

In the figure, reference numeral 206 denotes an exhaust device for evacuating the vacuum container 201, which is connected to the vacuum container 201 via an exhaust valve 205. 214 is a holding member. The holding member 214 carried into the vacuum chamber 201 for forming a deposited film includes a dielectric window 20.
2 and a substrate 207 for forming a deposited film are held, and the holding member 214 also serves as an opening / closing part of the vacuum vessel 201. That is,
The holding member 214 is connected to the vacuum container via the vacuum seal member 215.
A deposition film forming space that can be in close contact with the inside of the sidewall of 201 and is sealed by the vacuum vessel 201 and the holding member 214.
208 can be formed. Reference numeral 219 denotes a rotation shaft for supporting and rotating the base 207 for forming a deposited film, and is connected to the rotation motor 212. Reference numeral 210 denotes a source gas discharge tube for supplying a source gas into the vacuum vessel. The source gas discharge tube 210 is connected to a source gas supply source (not shown) via a mass flow controller (not shown). . twenty one
Reference numeral 1 denotes a power supply connected to the gas discharge tube 210. An electric field is applied between the cylindrical substrate 207 and the gas discharge tube 210 when a deposited film is formed by applying a voltage.

The procedure of forming a deposited film using the apparatus of the embodiment of the present invention shown in FIGS. 1, 2 and 3 will be described below.

First, as shown in FIG.
3. Attach the gas discharge tube fixing member 321 and the dielectric window 302. Next, the gas discharge pipe 310 is connected to, for example, a metal gasket type face joint (VCR (registered trademark; Vacuum Coupling gas manufactured by CAJON)).
Attach it to the gas discharge tube fixing member 321 by ket ring)) or the like. Next, the cylindrical base 307 is set on the auxiliary base 324 processed so as to be hung on the hanger 323 and placed on the holding member 314. Note that these operations are preferably performed in a clean room or the like. The set assembled in the holding member 314 as shown in FIG.
The vacuum chamber 120 is evacuated from the exhaust device 122 by closing the gate valve 123 and opening the valve 121. Thereafter, if necessary, they are heated to a desired temperature, and then the transfer vacuum vessel 130 is moved onto the vacuum vessel 120, and the gate valve 131 of the transfer vacuum vessel 130 is brought into close contact with the gate valve 123 of the vacuum vessel 120. Then, the space between the gate valve 131 and the gate valve 123 is evacuated by the exhaust device 125. Next, the gate valve 131 and the gate valve 123 are opened, and the holding member is moved into the moving vacuum container 130 by a vertical moving mechanism (not shown) provided in the moving vacuum container 130. After that, the gate valve 131 and the gate valve 123 are closed, and the gate valve 13 is closed.
After returning the space between 1 and the gate valve 123 to atmospheric pressure, the transfer vacuum container 130 is brought into close contact with the gate valve 131 of the transfer vacuum container 130 and the gate valve 116 of the vacuum container 101 on the vacuum container 101. Thereafter, the holding member is moved into the reaction vessel 101 by the same procedure as described above. The holding member 314 has a waveguide 313 and a dielectric window 302 provided at the tip of the waveguide,
By the vacuum seal member 215, the deposited film forming space 208 can be kept in a vacuum. After the holding member has been moved to the reaction vessel 101, the waveguide from the microwave power supply is connected to the waveguide on the vacuum vessel 101 side.

After the microwave waveguide is connected, the raw material gas supply pipe is rotated while rotating the base 207 (307) for forming the deposited film.
The source gas is introduced through 33, and while maintaining a predetermined degree of vacuum by adjusting the valve 15, a microwave having a frequency of 2.45 GHz is introduced through the dielectric windows 202 and 202 'to decompose the source gas. , A deposited film is formed on the deposited film forming substrate 207 (307).

After the formation of the deposited film, the introduction of the microwave and the source gas and the rotation of the cylindrical substrate for forming the deposited film are stopped, and the waveguide is removed from the dielectric window. Next, after closing the gate valve 116 and evacuating the space B formed by the gate valve 116 and the holding member 314, the moving vacuum vessel 130 is moved to deposit the space B with the gate valve 131 of the moving vacuum vessel 130. The gate valve 116 of the film forming vacuum container 102 is brought into close contact with the vacuum chamber 102, and the space between the gate valve 131 and the gate valve 116 is evacuated by the exhaust device 118. After this, the vacuum chamber 10 for forming a deposited film
The holding member 314 in 1 is carried into the transfer vacuum container 130, and the gate valves 116 and 131 are closed.

The transfer vacuum container 130 having the holding member 314 built-in is then transferred to the cooling vacuum container 140 held in a vacuum, and the same procedure as described above, that is, the gate valve 131 and the gate valve 143 are moved. After being brought into close contact with each other, the space between the two gate valves is evacuated by the exhaust device 146, the two gate valves 131 and 143 are opened, and the holding member 314 is carried into the cooling vacuum container 140 from the moving vacuum container 130 and the gate valve. 131, 14
Close 3. After the substrates 207 (307), on which the deposited films are formed, are cooled to about room temperature in the vacuum vessel 140, the inside of the vacuum vessel 140 is set to atmospheric pressure, the gate valve 143 is opened, and the dielectric window is opened. Substrates 307, 307 with 302 and deposited film formed
..., the holding member 314 holding the gas discharge tube 310 is taken out.

In the present invention, the cylindrical members 20 are attached to the holding members 214 and 314.
Various arrangements are required to simultaneously dispose the gas discharge tubes 210, 310 and the dielectric windows 202, 302. For example, the cylindrical substrates 207 and 307 can be
The cylindrical members may be disposed on the holding members 214 and 314, but may be set in advance on auxiliary members 224 and 324 processed so as to be hung by hangers 223 and 323 or the like. , 314 are also preferable in terms of workability and cleanliness. With respect to the gas discharge tubes 210 and 310, after being conveyed to the reaction vessel (vacuum vessel) 201, the raw material gas must be introduced into the discharge space 208 without leaving anything. Therefore, as shown in FIG. 2, it is necessary to ensure that the source gas is not leaked while being accurately joined to the gas discharge nozzle 220.
Therefore, the O-ring 225 is attached to the gas discharge tube fixing members 221 and 321.
It is desirable to have a mechanism for setting and holding down. However, in this state, the O-ring 215
Since it leaks more, the gas discharge pipe fixing member 221
Or a spring-like mechanism 2 that absorbs the force to the gas discharge nozzle 220
It is necessary to devise 22 mags.

In the present invention, the material of the holding member is not particularly limited, but any material may be used as long as it can serve as a part of the vacuum vessel and has little distortion or the like. Generally, stainless steel, Al or the like is used.

The number of the cylindrical substrates in the present invention may be any number as long as the discharge space is formed. Generally, 3 or more, 10
The following is preferred.

As the cylindrical base material, for example, stainless steel, Al,
In the present invention, metals such as Cr, Mo, Au, In, Nb, Te, V, Ti, Pt, Pd, and Fe, synthetic resins such as alloys or polycarbonates whose surfaces are conductively treated, glass, ceramics, paper, and the like are used in the present invention. Usually used.

Although the substrate temperature at the time of forming a deposited film in the present invention is effective at any temperature, it is particularly 20 ° C. or more and 500 ° C. or less, preferably 50 ° C.
A temperature of 450 ° C. or lower is desirable because a good effect is exhibited.

As a method of introducing microwaves into the reactor in the present invention, a method using a waveguide is mentioned.
One way is to introduce from one or more dielectric windows.

At this time, the material of the window for introducing the microwave into the furnace is alumina (Al ₂ O ₃ ), aluminum nitride (AlN), boron nitride (BN), silicon nitride (SiN), silicon carbide (Si
C), silicon oxide (SiO ₂ ), beryllium oxide (BeO), Teflon, polystyrene, and other materials with low microwave loss are usually used.

The size and shape of the gas discharge tube may be any as long as they do not disturb the discharge, but in practice, a cylindrical shape having a diameter of 1 mm or more and 5 cm or less is preferable. At this time, the length of the electrode can be arbitrarily set as long as the electric field is uniformly applied to the base.

As the material of the gas release tube, any material may be used as long as the surface thereof becomes conductive, for example, stainless steel, A
l, Cr, Mo, Au, In, Nb, Ni, Cu, Ag, Te, V, Ti, P
In the present invention, metals such as t, Pd, Fe, Zn, etc., their alloys or glass, ceramics, and plastics whose surfaces are subjected to conductive treatment are generally used in the present invention.

In the present invention, the electric field generated between the electrode and the substrate is preferably a DC electric field, and the direction of the electric field is more preferably directed from the electrode to the substrate.

The average magnitude of the DC voltage applied to the electrodes to generate the electric field is 15 V or more and 300 V or less, preferably 30 V or more and 200 V or less.
The following are suitable:

The DC voltage waveform is not particularly limited, and the present invention is effective. In other words, it may be any case as long as the direction of the voltage does not change with time.For example, a constant voltage whose magnitude does not change with time, as well as a pulse-like voltage and a time that is rectified by a rectifier, change in magnitude. The present invention is effective even with a pulsating voltage.

The present invention is also effective to apply an AC voltage. There is no problem with the frequency of the alternating current, and practically, 50 Hz or 60 Hz for a low frequency and 13.56 MHz for a high frequency are suitable. The AC waveform may be a sine wave, a short wave, or any other waveform, but a sine wave is suitable for practical use. However, at this time, the voltage refers to an effective value in any case.

The source gas of the deposited film used in the apparatus of the present invention includes, for example, an amorphous silicon forming source gas such as silane (SiH ₄ ) and disilane (Si ₂ H ₆ ), and other functional deposited films such as germane (GeH ₄ ). A forming raw material gas or a mixed gas thereof may be used.

Examples of the dilution gas include hydrogen (H ₂ ), argon (Ar), helium (He), and the like.

In addition, as a characteristic improving gas for changing the band gap width of the deposited film, an element containing a nitrogen atom such as nitrogen (N ₂ ) and ammonia (NH ₃ ), oxygen (O ₂ ), nitrogen oxide (NO),
An element containing an oxygen atom such as nitrous oxide (N ₂ O), methane (C
H _4), ethane (C ₂ H _6), ethylene (C ₂ H _4), acetylene (C ₂ H _2), hydrocarbons such as propane (C ₃ H _8), four Hutu of silicon (SiF _4), six Fluorinated compounds such as silicon fluoride (Si ₂ F ₆ ) and germanium tetrafluoride (GeF ₄ ), and a mixed gas thereof are exemplified.

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 doping.

Further, the present invention provides a photoreceptor for a copying machine or a printer, such as a blocking type amorphous silicon photoreceptor, a high resistance type amorphous silicon photoreceptor, and any other type which requires a functional deposited film having good electrical characteristics. It can also be applied to device fabrication.

The present invention can be applied to any device using microwaves, but is particularly applicable to a device in which a base is provided so as to surround a discharge space and microwaves are introduced from at least one end of the base by a waveguide. It has a great effect.

As described above, the deposited film is formed on the cylindrical substrate. The effect of the present invention is further enhanced by repeating this series of flows, and further enhanced by further contrivance.

[Experimental Examples and Examples]

Hereinafter, the effects of the present invention will be described in more detail with reference to experimental examples and examples.

However, the present invention is not limited by the examples.

Test Example 1 and Comparative Test Example 1 The procedures described in detail above using the deposited film forming apparatus according to the present invention as shown in FIGS. 1, 2 and 3 and the conventional apparatus shown in FIG. 4, respectively. According to cylindrical substrate, dielectric window,
The gas discharge tubes were arranged in vacuum (reaction) vessels 201 and 401.
At this time, a vacuum dust counter was set at the same time, and after the arrangement was completed, the amount of dust in each of the containers 201 and 401 was measured. The measurement method is every 5 minutes for 30 minutes from the end of placement
Or more in diameter 0.3μm in 1000 cm ³ of the number of dust respectively 10
Measured times. The results are shown in FIG.

As shown in FIG. 5, the difference in the amount of dust is clearly reduced by the present invention as compared with the prior art. Furthermore, the variation width by 10 measurements is small, and the average value of 10 measurements is 5 minutes after the placement is completed.
25 / 1000cm ^{3 and} stable. In the conventional apparatus, the average value of 10 times even after 30 minutes was 200/1000 cm ³ . Also, the variation during the 10 runs was large.

Test Example 2 and Comparative Test Example 2 Using the deposited film forming apparatus according to the present invention as shown in FIGS. 1, 2 and 3, and the conventional apparatus shown in FIG. In the apparatus of the present invention, the cylindrical substrate, the gas release tube, and the dielectric window are conveyed to the reaction vessel 101 after heating in the vacuum vessel 120. The gas was exhausted by the exhaust devices 106 (206) and 406, and the ultimate pressure after 10 minutes was measured. As a result, the reaction vessel 10 of the present invention
6 (206) was 1.0 × 10 ⁻⁸ torr. Conventional reaction vessel 4
In 06 it was 9.0 × 10 ^-8 torr.

Example 1 and Comparative Example 1 Example 1 The second example was performed by the deposition film forming apparatus used in the present invention as shown in FIG. 1, FIG. 2 and FIG.
Under the conditions shown in the table, a deposited film was formed on an aluminum cylinder having a length of 358 mm, an outer diameter of 108 mm, and a thickness of 5 mm, thereby producing an a-Si: H photosensitive drum having a blocking structure.

The photosensitive drum produced in this manner was installed in a copier NP7550 (trade name) manufactured by Canon Inc., and images on all photosensitive drums (of six drums) in the same lot were evaluated. At this time, charging was performed by applying a voltage of 6 KV to the charger. The image thus produced was evaluated as follows.

Fine line reproducibility: An image sample obtained when a normal original consisting of characters on the entire surface was placed on a platen and copied on a white background was observed, and it was evaluated whether the fine lines on the image were connected without interruption.

…: Good.

○… There are some interruptions.

Δ: There are many interruptions, but they can be recognized as characters.

×: Some characters cannot be recognized as characters.

Fog on white background: An image sample obtained when a normal original consisting of whole characters was placed on a platen and copied on a white background was observed, and the fog on the white background was evaluated.

…: Good.

…: There is some fog.

Δ: Fogging over the entire surface, but no problem in character recognition.

×: There is fog so that the characters are difficult to read.

Image unevenness: An image sample obtained when the original half-tone document was placed on a platen and copied was observed, and the shading was evaluated.

…: Good.

…: There is a slight difference in density.

Δ: There is a difference in shading over the entire surface, but there is no problem in character recognition.

×: There are irregularities so that the characters are difficult to read.

Image Defects: Evaluation was made by the number of white spots within the same area of an image sample obtained when a black original was placed on a platen and copied.

…: Good.

○: Some small white spots.

Δ: There is a white spot on the entire surface, but there is no problem in character recognition.

×: There are many white spots as the characters are hard to read.

Comparative Example 1 Using the deposition film forming apparatus shown in FIG. Similarly, an a-Si: H photosensitive drum having a blocking type structure was manufactured. The produced a-Si: H photosensitive drum was evaluated in the same manner as in Example 1.

Table 2 also shows the results of Example 1 and Comparative Example 1.
As shown in Table 2, in all of the items, the photosensitive drum manufactured by the deposited film forming apparatus of the present invention showed very good results.

Example 2 Using the deposited film forming apparatus shown in FIG. 1, FIG. 2 and FIG.
Example 1 except that the deposition rate was higher than in Example 1.
An amorphous silicon photosensitive drum was prepared in the same manner as described above. The amorphous silicon photosensitive drum thus produced was evaluated in the same manner as in Example 1. As a result, as in Example 1, in the present invention, very good results were obtained for the image quality of the photosensitive drum.

Example 3 Using the deposited film forming apparatus shown in FIGS. 1, 2 and 3, Under the conditions shown in the table, formation of a function-separated type photosensitive drum using amorphous silicon and amorphous silicon carbide was performed in the same manner as in Example 1. The photosensitive drum thus produced was evaluated in the same manner as in Example 1. As a result, as in Examples 1 and 2, in the present invention, very good results were obtained for the image quality of the photosensitive drum.

Example 4 The eddy current meter was used to measure the thickness of the photosensitive drum manufactured in Example 1 and Comparative Example 1, and the thickness of the photosensitive drum manufactured by the conventional apparatus shown in FIG. 4 under the same conditions as in Example 2 and Example 3. Was measured and compared. As a result, the photosensitive drum manufactured according to the present invention was about 5% less than the photosensitive drum manufactured using the conventional apparatus.
The result was that the film was thicker and the gas use efficiency was improved.

[Brief description of the drawings]

FIG. 1 is a cross-sectional view of the overall arrangement of a deposited film mass-production apparatus by the μW-PCVD method of the present invention, FIG. 2 is a schematic cross-sectional view of a volume film forming apparatus by the μW-PCVD method of the present invention, and FIG. FIG. 4 is a schematic view showing a state in which a cylindrical member, a gas discharge tube, and a dielectric window are set on a holding member. FIG. 4 is a schematic view of a conventional deposited film forming apparatus. FIG. 5 is a view showing the effect of the present invention. 101, 201, 401: Reaction vessel (vacuum vessel) 120: Vacuum vessel (heating chamber) 130: Transport vessel 140: Cooling vessel 116, 123, 131, 143 Gate valve 105, 117, 124, 121 , 141, 145, 205, 217, 405 exhaust valve 106, 118, 122, 125, 142, 146, 206, 218, 406 exhaust device 202, 202 ', 302, 402 dielectric window 203, 313, 403: Waveguides 204, 404: Exhaust pipes 207, 307, 407: Cylindrical substrates 208, 408: Discharge space 209, 409: Mass flow controllers 210, 310, 410: Gas emission pipe 211 , 411 DC power supply 212, 412 Rotating mechanism 219, 419 Rotating shaft 214, 314 Holding member 215, 225 Vacuum holding material (O-ring) 220 Gas discharge nozzle 221, 321 Gas discharge tube fixing member 222: spring-like mechanism 223, 323: hanger 224, 324, 424: auxiliary base

────────────────────────────────────────────────── ─── Continuing on the front page (72) Inventor Hirokazu Ohri 3-30-2 Shimomaruko, Ota-ku, Tokyo Inside Canon Inc. (58) Field surveyed (Int.Cl. ⁶ , DB name) C23C 16 / 50 H01L 21/205

Claims (2)

(57) [Claims] 1. A means for supplying a raw material gas into a reaction vessel capable of vacuum sealing, a means for discharging the reaction vessel, a means for generating microwave discharge plasma in the reaction vessel, and a plurality of means in the reaction vessel. In a deposition film forming apparatus using a microwave plasma CVD method having means for holding and rotating a cylindrical substrate, a circular dielectric window for introducing microwaves into the reaction vessel and a circular dielectric window surrounding the dielectric window are provided. Having a mechanism for discharging a source gas into a space surrounded by a plurality of cylindrical substrates disposed in the cylindrical substrate and applying an electric field between the cylindrical substrate and the means for discharging the source gas Means for holding the dielectric window, the cylindrical substrate, and the raw material gas discharge tube on a holding member having a function of simultaneously holding the gas discharge tube and transferring the holding member into the reaction vessel in a vacuum atmosphere. A and deposited film forming apparatus, wherein the reaction container transfer after again can be vacuum retention. 2. The method according to claim 2, wherein said holding member holding said cylindrical substrate, dielectric window, and gas discharge tube is heated in advance in a vacuum vessel separate from said reaction vessel and then vacuum-transferred into said reaction vessel. The deposited film forming apparatus according to claim 1, wherein: