JP2717235B2 - Gas phase reaction processing method - Google Patents

Description

Description: BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an apparatus and a method for producing a vapor phase reactive coating. According to the present invention, when producing a coating using a reactive gas, a non-oxide coating is produced by performing a gas phase reaction (hereinafter referred to as CVD) using a turbo molecular pump in an exhaust system. The present invention relates to a gas phase reaction apparatus for controlling the concentration of oxygen to a concentration of 5 × 10 ¹⁸ cm ⁻³ or less, and a method for producing a coating film using the apparatus. 2. Description of the Related Art Conventionally, in a CVD apparatus such as a PCVD apparatus, the pressure of a reaction system is as high as 0.01 to 10 torr. It has been considered impossible to provide a TP or the like for generating the above. However, the inventor of the present invention has found that in such a PCVD apparatus, when the exhaust system is only RP, the RP makes a discontinuous rotational movement, so that the atmosphere (particularly oxygen) from the atmospheric exhaust system in contact with air is exhausted. It was found that the gas flowed back, and a part of the air was mixed into the oil, and from there, was re-vaporized and flowed back into the reaction vessel. Further, for this reason, oxygen is mixed into the film formed by the backflow, and for example, when a silicon film is formed, oxygen is contained in the film at 3 × 10 3.
^It was mixed at a concentration of ^{19 to} 2.5 × 10 ²⁰ cm ⁻³ . [0004] For this reason, hydrogen or fluorine is added to such a film, so that what should be a silicon semiconductor can be called lower silicon oxide. The object of the present invention is to prevent such disadvantages. Further, the present invention provides a T
In addition to providing P, a pressure adjusting valve is provided between TP and RP. That is, if a pressure regulating valve is provided between the reaction vessel and the TP, the inner diameter of the valve is generally 1 to 2 inches. Therefore, even when this valve is fully opened, the conductance at this valve portion is low, and it takes a long time even if the inside of the reaction vessel is kept at a background level (3 × 10 ⁻⁸ torr or less). Further, when this valve has a large diameter of 5 to 10 inches, there is a disadvantage that the pressure cannot be adjusted with sufficient accuracy. The present invention eliminates these drawbacks,
A complex molecular pump capable of evacuating even at 0.01 to 10 torr is used as the TP, and in addition, the pressure regulating valve is
And RP, and pressure control is performed for both the inside of the TP and the reaction vessel. [0008] The gas phase reaction processing method of the present invention uses a variable-rotation speed turbo-molecular pump capable of exhausting from atmospheric pressure by lowering the rotation speed. According to the present invention, in the production of a non-oxygen or non-oxide type coating film, in order to prevent the backflow of the atmosphere from the exhaust system, a discontinuous rotation type such as an oil rotary type rotary pump or a mechanical booster pump is used. Rough quoted vacuum pump (hereinafter simply referred to as “rotary pump” or “RP”) is used instead of continuous pumping type molecular pump or turbo-molecular pump (hereinafter simply referred to as “turbo-molecular pump” or “TP”).
Is interposed between the reaction vessel and the vacuum pump to prevent backflow of the atmosphere from the exhaust system. The non-oxide film of the present invention, for example, non-single-crystal silicon is replaced with a reactive gas of silane (Si _n H _{2n + 2} n ≧ 1).
When forming using, the amount of oxygen in the film is 5 ×
In order to reduce the flow to 10 ¹⁸ cm ⁻³ or less, preferably 1 × 10 ¹⁸ cm ⁻³ or less, an object is to prevent backflow of the atmosphere from the exhaust system. According to the present invention, the exhaust system is provided with a TP in a reaction chamber and a V.
By interposing a pressure control valve between P and P through a pressure regulating valve during the reaction, a plasma gas phase reaction (referred to as PCVD) and a photo CVD (referred to as Photo CVD) can be performed within a pressure range of 0.05 to 10 torr in the reaction chamber. Alternatively, a film is formed by a method using these together (hereinafter, simply referred to as a CVD method) and controlled by a pressure adjusting valve (also called a control valve or a butterfly valve). Therefore, the reverse flow of the oil component from the RP and the RP
The purpose of the present invention is to form a high quality non-oxide film by preventing a backflow of the atmosphere mixed in oil during rotation. Further, according to the present invention, when the reaction vessel is evacuated before performing the gas phase reaction, the TP and the reaction vessel can be connected by a large-diameter pipe, and the TP can be further connected to the reaction vessel. it can. Therefore, the inside of the reaction vessel is 3 × 10 ⁻⁸ t.
orr or lower pressure (3 × 10 ^-8 to 1 × 10
^-10 torr) can be performed using the same TP. That is, the inside of the reaction vessel is 10 ⁻⁸ by the apparatus of the present invention.
The vacuum evacuation of not more than torr and the pressure of 0.01 to 10 torr required for film formation by the CVD method can be controlled by using the same TP in addition to preventing the backflow of oxygen. Further, the present invention relates to a plasma CVD apparatus in which a plurality of reaction chambers are connected to each other to form a film as a semiconductor, and a P-type non-single-crystal semiconductor, an I-type non-single-crystal semiconductor, and an N-type The present invention relates to an apparatus and a method for manufacturing a semiconductor device in which a single crystal semiconductor is stacked over a substrate to form a PIN junction. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS A gas phase reactor according to the present invention will be described below with reference to a plasma CV.
The case where a PIN junction is provided by the D apparatus is shown and described. FIG. 1 shows an outline of the apparatus according to the present invention.
That is, it has a doving system (50) for introducing a reactive gas, a reaction vessel (51), and an exhaust system (52). The reaction vessel has a semiconductor layer formed as a double reaction vessel type having a reaction space in which an inner surface is formed by an insulator, and additionally has a P-type semiconductor (system I in the drawing) and an I-type semiconductor (system II in the drawing).
In forming the junction on the substrate by laminating with the N-type semiconductor and the N-type semiconductor, the respective reaction vessels are separated from each other by a separation unit (system I in the drawing).
Multi-chamber CVD linked via I)
An apparatus, particularly a PCVD apparatus, is proposed as shown in FIG. According to the present invention, by forming a non-single-crystal semiconductor layer to which hydrogen or a halogen element is added, a semiconductor layer having a P, I, and N-type conductivity type having a low recombination center density is formed, and a lamination boundary is formed. To form a PIN junction, to prevent each semiconductor layer from being mixed with impurities from another adjacent semiconductor layer to thereby degrade the junction characteristics. And to a plasma gas phase reaction for performing continuous production without forming an interlayer insulator by oxidizing a part of a semiconductor. Further, the present invention relates to a so-called mass production system in which a large number of substrates are simultaneously increased at the same time in a multi-chamber plasma reaction method in which a large number of such reaction vessels are independently connected in each reaction. . According to the present invention, the distance is 10 to 50 c in the direction of the electrode.
m having a width of 15 to 120 c
For example, a substrate of 30 cm in size (10 batches of 15 cm × 30 cm were arranged in one batch) was used. In FIG. 1, the reactive gas introduction means (5
0), exhaust means (52),
An exhaust nozzle is provided, and a pair of electrodes (61), (51) or (62)
(52) and reactive gas supply nozzles (17), (1)
8) and exhaust nozzles (17 ') (18'). That is, a structure in which the outside of the electrode is wrapped with a hood insulator (3)
8), (39 '). Further, in order to confine the reaction space between the hoods, the outer periphery is made of insulators (38), (3).
8 '). Although not shown, flat doors were provided before and after the reaction vessel, and a means for heating the substrate by a halogen lamp or the like was provided on the inner surface of the door. This drawing shows a PIN junction, a PIP junction, N
An IN junction or PINPEN ... PIN junction or the like is formed on a semiconductor on a substrate by using a semiconductor layer having a different main component or a different stoichiometric ratio of a semiconductor to be formed while being of a different conductivity type or a different material. This is an apparatus for automatically and continuously forming a multilayer to be laminated without being affected (mixed) by a semiconductor layer formed in a previous step. In the drawings, a part of a plurality of reaction systems constituting a PIN junction is shown. That is, a multi-chamber system having two (I, II) of three reaction systems formed by laminating P, I, and N type semiconductor layers, and further having a first preliminary chamber and a buffer chamber (II) for transfer. 1 shows an example of a plasma gas phase reaction apparatus. The systems I, II and III in the drawing have two reaction vessels (101) and (103) and a buffer chamber (102), and a separation section (4) is provided between the respective reaction vessels.
4), (45), (46), and (47). This apparatus has a first spare room (1) at the entrance side.
00), first, two substrates (1) each having two surfaces to be formed were attached to two surfaces of the substrate holder (2) from the door (42). Further, the holder (3) was disposed at a predetermined equal distance from each other by an outer frame jig (only the outer periphery is shown as (38) and (38 ')). That is, the substrate having the surface to be formed is in contact with the substrate holder (2) on the back surface on which no film is formed, and has a gap of 6 cm ± 0.5 cm using two substrates and the substrate holder as one holder (3). The trees were erected in the outer frame jig of the insulator. As a result, 15c
As a result, 10 substrates of mx 30 cm could be simultaneously coated. Thus, height 55cm, depth 40cm, width 4
The 0 cm reaction spaces (6) and (8) are surrounded by insulators (39) and (39 ') on the upper and lower sides, and the periphery of the sides is electrically connected by insulating outer jigs (38) and (38'). Enclosed in an insulator. The first preliminary chamber (100) was evacuated by the RP (35) through the TP (86) and the stop valve (71). This TP used a compound molecular pump TG550 manufactured by Osaka Vacuum. This compound molecular pump has a constant speed of 4
00 rps (revolutions per second), and N ₂ and SiH ₄ have a pumping speed of 500 l / s. Further 0.01 to 1
Exhaust at 0 torr is possible, and 1 at 10 torr
Evacuation of 0 l / sec is possible. In particular, at 0.1 to 1 torr generally used for a gas phase reaction, 450 l / s
Evacuation of ec to 440 l / sec is possible. The present invention makes the rotation of the TP variable. Therefore, even if the reaction vessel is at atmospheric pressure, the rotation speed of the TP is set to 100 to 200 rps.
And lower than the quantitative value, and the rotation was continued. And TP was not damaged. Therefore, the reaction vessel was evacuated at atmospheric pressure while the RP was opened by opening the valve (71) and the evacuation was driven by the TP. As a result, the TP prevents the oil component from flowing backward from the RP, and the substrate surface is not contaminated with the oil component. Thereafter, the pressure adjusting valve (72) and the gate valve (85) have inner diameters of TP (VG15
0, that is, the same as JIS B2290 vacuum flange), the gate valve (85) is fully opened, and the reaction vessel (which is previously evacuated to 3 × 10 ^-8 torr or less by TP (also using TG550)). 101) and a gate valve (44) for separation (opening 35 cm × 30 cm)
Was opened, and the substrate held by the outer frame jig (38) was transferred. For example, the first reaction vessel (1
01), and the substrate was moved to the first reaction vessel (101) by closing the gate valve (44). At this time, the substrate (1) and the like held in the first reaction vessel (101) are preliminarily or simultaneously placed in the buffer chamber (102), the jig and the jig held in the buffer chamber (102). The substrate (2) is placed in the second reaction vessel (10
3), the substrate held in the second reaction vessel (103) is stored in the second buffer chamber (104), and the substrate and jig of the third reaction chamber are not shown in the drawing. Gate valves (45), (46) in the second spare chamber on the exit side,
(47) is opened and moved. After this, the gate valve (4
4), (45), (46), and (47) were closed. The case where the P-type semiconductor layer is formed by the PCVD method in the first reaction vessel (101) in the system I will be described below. The reaction system I (including the reaction vessel (101)) is 0.01 to 10 torr, preferably 0.01 to 1 torr.
r, for example, 0.1 torr. That is, the pressure in the reaction vessel and the TP (87) (101) is reduced from 0.01 to 10 torr, particularly from 0.05 to 1 torr by closing the pressure regulating valve (72).
The degree of vacuum is controlled by controlling the opening and closing of the pressure regulating valve (72) below the TP (87), and the rotational speed of the TP is controlled by 10
It is achieved as 0 rps. The reason why the rotational speed of the TP was reduced was that the pressure control of the pressure regulating valve was easily performed by reducing the compression ratio of the TP from a constant of 10 ⁷ to 10 ⁸ to 10 ² to 10 ³ . In the present invention, since the continuous exhaust type TP is operated, it is possible to prevent, for the first time, the reverse diffusion of the polymerized oil of the RP (36) and the backflow of the exhaust air impregnated in the oil, particularly oxygen. did it. The reactive gas is a doping system of system I (50).
Supplied more. That is, silane (Si) purified as a silicide gas (24) and further filled in a stainless steel cylinder is used.
_n H _{2n + 2 n} ≧ 1 in particular SiH ₄ or Si ₂ H _6), using silicon fluoride (SiF ₄ or SiF _2). Here, ultra-high-purity silane (purity 99.99) which is easy to handle
%, But water and oxygenates are 0.1 PPM or less). In order to form Si _x C _{1 -x} (0 <x <1) in this embodiment, Si—C is used as a carbide gas (25) in advance.
Methylsilane (56) having a bond, ie, MMS (HSi
(CH ₃ ) ₃ ) or DMS (dimethylsilane (SiH
₂ (CH ₃ ) ₂ purity 99.99%). For silicon carbide (Si _x C _{1 -x} 0 <x <1), a cylinder (24) in which boron as a P-type impurity is mixed at a concentration of 0.5% in the above-mentioned monosilane is used. Supplied with silane. If necessary, hydrogen (purity of 7 N or more) or nitrogen (purity of 7 N or more) is applied to the reaction chamber at atmospheric pressure (2
3). These reactive gases have diameters of respective flow meters (33) and valves (32), and are supplied from a reactive gas supply nozzle (17) to a reaction space (6) via a negative electrode (61) of a high frequency power supply (14). Supplied. The reactive gas was supplied into the cylindrical space (6) surrounded by the holder (38), and a film was formed on the substrate (1) constituting this space. Further, electric energy, for example, 13.56 MHz, is applied between the negative electrode (61) and the positive electrode (51).
Was applied to cause a plasma reaction to form a film of the reaction product on the substrate. The substrate was heated to 100 to 400.degree. C., for example, 200.degree. C. by the same means as the infrared heater disposed before and after the reaction vessel (103) shown in FIG. This infrared heater uses a near-infrared halogen lamp (constant emission wavelength 1 to 3 μm) heater or far-infrared ceramic heater (emission wavelength 8 to 25 μm), and has a cylindrical shape surrounded by a holder in the reaction vessel. The space was set within 210 ± 10 ° C., preferably within ± 5 ° C. Thereafter, as described above, the above-mentioned reactive gas is introduced into this container, and further 5 to 100 w, for example, 20 w
Was supplied with high-frequency energy (14) to cause a plasma reaction. Thus, the P-type semiconductor layer is made of B ₂ H ₆ / SiH
_{Under the conditions of 4} = 0.5% and MS / (SiH ₄ + MS) = 20%, this reaction system I was formed as a thin film having an average film thickness of 30 to 300 A, for example, about 200 A. Eg
= 2.15 eVσ = 1 × 10 ^{−6 to} 3 × 10 ⁻⁵ (Ωcm)
It was ^-1 . The substrate may be a conductor substrate (stainless steel, titanium, aluminum, or another metal), a semiconductor (silicon, germanium), an insulator (glass, organic thin film) or a composite substrate (glass or translucent organic resin). (A single layer of a conductive film such as tin oxide to which fluorine is added, ITO, or the like, or a two-layer film in which SnO ₂ is formed on ITO) is used. In this example, a composite substrate was used. Thus, a plasma gas phase reaction was performed for 1 to 5 minutes to produce a silicon carbide film to which boron as a P-type impurity was added to a thickness of about 200A. Further, the substrate on which the first semiconductor layer was formed was opened to the gate (45), moved to the buffer chamber (102) according to the operation sequence described above, and the gate (45) was closed. The buffer chamber (102) is previously evacuated to 10 ⁻⁸ torr or less, for example, 4 × 10 ⁻¹⁰ torr by a cryopump (88). This substrate is similar to the system III in that the TP (8
According to 9), it was transferred to the reaction vessel maintained at 3 × 10 ⁻⁸ torr or less through opening and closing of the gate (46). That is, in the reaction system III in FIG.
Ultra-high-purity monosilane or disilane (water or silicon oxide, the concentration of oxide gas is 0.
(1 PPM or less) From (28), and to add boron of 10 ¹⁷ cm ^-3 or less, hydrogen or silane or the like is used.
From the B ₂ H ₆ diluted to 5~30PPM (27), was also supplied from in accordance with the carrier gas necessary (26). After reacting in the reaction vessel, the reactive gas reaches the TP (89) via the gate valve (84), further reaches the control valve (74) and the RP (34). For a thickness of 7000A, 60 cc of SiH ₄ /
Min, film formation rate 2.5 A / sec, substrate (20 cm × 60
20 cm, a total area of 24000 cm ² ) and a pressure of 0.
1 torr. When Si ₂ H ₆ was used, the film formation rate was 28 A / sec. Thus, the P-type semiconductor layer is formed in the first reaction chamber by the plasma vapor phase method, and then the P-type semiconductor layer is formed by the PCVD method.
A PI junction was formed by forming a mold semiconductor layer. After being formed to a thickness of about 7000 A in the system III, the substrate is transferred to the next buffer chamber (102) according to the above-mentioned operation, and further transferred to the next reaction chamber to perform the same PCVD. An N-type semiconductor layer was formed by the process. This N-type semiconductor layer is supplied by supplying silane with a phosphine of PH ₃ / SiH ₄ = 1.0% and hydrogen of a carrier gas as SiH ₄ / H ₂ = 20% by PCVD.
A polycrystalline semiconductor layer having an N-type microcrystalline or fibrous structure is formed at a thickness of about 500 A in the same manner as in system I, and silicon carbide is further formed on its upper surface by MS / (SiH ₄ + MS) =
As 0.2 Si _x C _1-x N represented by (D <x <1)
It is formed by laminating the mold semiconductor layers to a thickness of 10 to 200 A, for example, a thickness of 50 A. Other reactors are the same as in system I. After such a step, P
100-1500 on the substrate which is formed by forming the IN junction
Further, a reflective or sublimable metal electrode such as an aluminum electrode having a thickness of about 1 μm is formed on the glass substrate to a thickness of about 1 μm by a vacuum evaporation method, and (ITO + SnO) is formed on a glass substrate.
₂ ) A front electrode- (PIN semiconductor)-(back electrode) was formed. The characteristics of the photoelectric conversion device are 8 to 10
% Average 8.5% with 10cm x 10cm substrate
(100 mw / cm ² ) 40cm × 6 which has intrinsic efficiency characteristics and is integrated into a hybrid type under the condition of (100 mw / cm ² )
4. Even in a NEDO panel with a 0 cm glass substrate,
7% was obtained with an effective efficiency. As a result, the open circuit voltage of one element is 0.8
5 to 0.9 V (0.87 ± 0.02 V), but the short-circuit current was as large as 18 ± ² mA / cm ² , the FF was also as large as 0.60 to 0.70, and the variation was within the panel. Small in a batch, the method of the present invention has been found to be very effective industrially. FIG. 2 shows the concentration distribution of oxygen and carbon impurities in a semiconductor in a PIN photoelectric conversion device manufactured by the present invention and the conventional method by SIMS (Cameca 3).
F)). Drawing Aluminum-ITO-Back electrode (94), N-type semiconductor (93), I-type semiconductor (92),
A P-type semiconductor (91) and a tin oxide translucent conductive film (90) on a substrate are shown, respectively. In the conventional exhaust method using only the RP pump, the exhaust system using the RP pump alone does not use the TP of the continuous exhaust system. Therefore, carbon contains high-concentration impurities shown by the curve (95) and oxygen by the curve (96). I was In particular, oxygen is 5 × 10 ¹⁹ to 2 × 10 ²⁰ cm
^-3 in the I-type semiconductor (92). The drawing is 5
This is a case where oxygen of × 10 ¹⁹ cm ⁻³ is contained. In addition, carbon is reduced by 5 × 10 ¹⁹ ~ due to the backflow of the oil component from the oil rotary pump.
It had a size of 4 × 10 ²⁰ cm ⁻³ . The drawing is 1 × 10 ²⁰ cm
^-3 . On the other hand, the exhaust system as shown in the present invention has a carbon concentration of 1 × 10 ^{17 to} 5 × 10 ¹⁸ cm ^-3 , and generally contains only 1 × 10 ¹⁸ cm ^-3 or less. In addition, oxygen is also 5 × 10 ¹⁸ cm ⁻³ or less, generally 1 × 10 ¹⁸ cm ⁻³ or less, and FIG. 2 shows the case of 2 × 10 ¹⁸ cm ⁻³ . In FIG. 3, the aluminum of the back electrode (94) has oxygen of ^{3 to} 6 × 10 ²⁰ cm ^-3 .
For this reason, this oxygen is used for SIMS (secondary ion analysis).
In the measurement (using a 3F type by Kameka), the oxygen became background oxygen, and the oxygen in the N-type semiconductor (93) was 1%.
It is probable that it was 0 ¹⁸ to 10 ²⁰ cm ^-3 . Oxygen in the P-type semiconductor and oxide impurities such as water in MS are contained in the P-type semiconductor. The starting material is purified in the same manner as silane to obtain oxygen or oxide of 0.1 PPM or less. The possibility of further lowering the oxygen concentration can be estimated. Regarding the type of semiconductor to be formed,
Not only other group IV _{Ge, Si x C 1-x} (0 <x <
_{1), Si x Ge 1-} x (0 <x <1), Si x Sn 1-x
(0 <x <1) It goes without saying that it may be a single layer or a multi-layer, or may be a non-oxide such as a compound semiconductor such as GaAs, GaAs, BP, and CdS. The present invention has shown the PCVD method in a multi-chamber system using three reaction vessels. However, this was used as one reaction vessel, and silicon nitride was converted to silane (SiH ₄ or Si ₂ H ₆ ) and ammonia (NH
It is effective to form them by the PCVD reaction with ₃ ). Further, one reaction of the present invention, for example, the reaction of the system I is carried out by mixing MS and Si ₂ H ₆ with B ₂ H ₆ by the photo CVD method, and at the same time, the TP of the present invention and the pressure adjusting valve are connected to the exhaust system. It is effective to use. Further, according to the present invention, a single reaction vessel
PCVD reaction between Cl ₄ and SiH ₄ , MoCl ₅ , WF
₅ or Ti, TiSi by reaction of these with silicide
₂ , Mo, MoSi ₂ , W, WSi _2, etc. are similarly effective for producing a non-oxygenated film. In the present invention, the separating section may be constituted by omitting the system II and using only the gate valve. It goes without saying that the plasma CVD apparatus of the present invention can be applied to a single-chamber or multi-chamber system having another structure. The embodiment of the present invention is a multi-chamber system shown in FIG.
Act supplied. However, if necessary, a part or the whole of the photo-CVD method using no plasma, the LTCVD method (HO method)
The composite coating may be formed by employing a low pressure CVD method (also referred to as MO CVD method). According to the present invention, a variable-rotation-speed turbo-molecular pump capable of evacuating from the atmospheric pressure by lowering the rotation speed can be used in the gas-phase reaction processing method of the present invention.

BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 shows an outline of an apparatus for producing a coating for a plasma vapor phase reaction for carrying out the present invention. FIG. 2 shows the distribution of impurities in a semiconductor device manufactured according to the present invention and a conventional method. [Description of Signs] 1 Substrate 2, 3 Holder 50 Doving system 51 Reaction vessel 52 Exhaust system

   ────────────────────────────────────────────────── ─── Continuation of front page    (72) Inventor Minoru Miyazaki               7-21-21 Kitakarasuyama, Setagaya-ku, Tokyo               Semiconductor Energy Laboratory Co., Ltd.                (56) References JP-A-57-44786 (JP, A)                 JP-A-59-16328 (JP, A)                 JP-A-57-49082 (JP, A)                 JP-A-56-151287 (JP, A)

Claims (1)

(57) [Claims] A reaction vessel for forming a film under reduced pressure , a means for supplying a reactive gas to the reaction vessel,
Gi, light energy, electric energy or using these
Means for supplying energy to a reactive gas in the reaction vessel
And a composite molecular pump for evacuating the reaction vessel to a relatively high vacuum.
And the compound molecular pump connected in series via a valve
Exhaust means for evacuating the reaction vessel to a relatively low vacuum.
And a compression ratio of 10 ⁷ to 10 ⁸ by the composite molecular pump using a gas phase reactor having
After evacuating the reaction vessel to a high vacuum, the composite molecular pump
And the number of rotations of the composite molecular pump is reduced to 10 ² to 1
0 while continuously evacuated ³ compression ratio, the reaction vessel 0.
The reaction is performed while maintaining the pressure in the range of 01 to 10 Torr.
A method for forming a coating film, comprising: 2. A reaction vessel for forming a film under reduced pressure , a means for supplying a reactive gas to the reaction vessel,
Gi, light energy, electric energy or using these
Means for supplying energy to a reactive gas in the reaction vessel
And a composite molecular pump for evacuating the reaction vessel to a relatively high vacuum.
And the compound molecular pump connected in series via a valve
Exhaust means for evacuating the reaction vessel to a relatively low vacuum.
And a compression ratio of 10 ⁷ to 10 ⁸ by the composite molecular pump using a gas phase reactor having
After evacuating the reaction vessel to a high vacuum, the valve was operated.
And reducing the rotation speed of the composite molecular pump to
The molecular pump Do is continuously evacuated compression ratio of ¹⁰ 2 to 10 ³
Meanwhile, the pressure in the reaction vessel is in a pressure range of 0.01 to 10 Torr.
Film formation method characterized by carrying out reaction treatment while holding at
Law.