JPH07268635A - Pressure control method and reaction treatment device - Google Patents

Abstract

PURPOSE:To prevent the failure of partition walls by receiving the influence of pressure with the device executing a chemical vapor deposition method by delineating a reaction chamber by these partition walls in a high-pressure vessel and maintaining a high pressure in this reaction chamber. CONSTITUTION:This reaction treatment device is provided with a pilot operated pressure control valve 43 between a gas supply pipeline 47 connected to a furnace chamber 14 between the high-pressure vessel 1 and the reaction chamber 12 and a gas conduit 40 connected to the reaction chamber 12. The internal pressures of the reaction chamber 12 and the furnace chamber 14 are compared at all times by the valve. The gas in a cylinder 48 is supplied into the furnace chamber 14 to increase the internal pressure of the furnace chamber 14 when the internal pressure of the reaction chamber 12 is higher. A release state is generated in the furnace chamber 14 to drop the internal pressure thereof when the internal pressure of the furnace chamber 14 is higher. As a result, the generation of the pressure difference between both chambers is obviated.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention mainly relates to a pressure control method and its reaction processing apparatus which are carried out in a reaction processing apparatus or the like in which a vapor phase chemical vapor deposition method or the like is performed under high temperature and high pressure.

[0002]

2. Description of the Related Art In the vapor phase chemical vapor deposition method, a hydrocarbon gas such as methane or propane is decomposed at a high temperature as a raw material gas to form a carbonized film (pyrolytic carbon film) on an object to be processed. Is. A hot wall type is often used as an apparatus for performing such a vapor deposition method. This device
A heat source is provided outside the reaction chamber in which the material to be processed is installed so as to be isolated from the source gas, and the material to be processed is indirectly heated. In this case, the object to be treated is generally treated under normal pressure.

On the other hand, recently, it has been attempted to carry out this kind of vapor deposition method under high pressure for the purpose of increasing the processing speed.

[0004]

With increasing the pressure in the reaction chamber, it is necessary to prevent the partition walls that define the reaction chamber from being damaged. Therefore, conventionally, the entire reaction chamber has been provided in a high-pressure container. It is considered that the pressure is balanced between the inside of the reaction chamber and the outside thereof (which becomes the furnace chamber).

In order to realize this structure, accuracy of control (complete prevention of breakage of partition walls) and simplification of structure are demanded. The present invention has been made in view of the above circumstances, and an object of the present invention is to provide a pressure control method and a reaction processing apparatus that enable the pressure balance inside and outside the reaction chamber to be structurally simplified and accurately controlled. .

[0006]

In order to achieve the above object, the present invention takes the following technical means. That is, in the pressure control method of the present invention according to claim 1, in the pressure control method of the pressure chamber connected to the pressurized fluid source and the auxiliary chamber attached to the pressure chamber, the internal pressures of the chambers are compared to each other and the auxiliary chamber is compared. When the internal pressure of the pressure chamber is high, the pressurized fluid source is communicated with the pressure chamber, while when the internal pressure of the pressure chamber is high, the internal pressure of the pressure chamber is released to the atmosphere to balance the pressure between the pressure chamber and the auxiliary chamber. It is characterized by that.

It is also possible to proportionally change the internal pressure of either the pressure chamber or the auxiliary chamber via the pressure increasing means or the pressure reducing means and then compare the internal pressures to generate a pressure difference between the two chambers. it can. In the reaction treatment apparatus of the present invention according to claim 3, an inverted cup-shaped heat insulating layer is provided in the high-pressure container, a partition is provided inside the heat insulating layer, and a heating element is provided between the heat insulating layer and the partition. And the inside of the partition wall as the reaction chamber of the object to be treated, the reactor chamber is provided with a non-reactive gas supply passage, and the reaction chamber is provided with a reaction pressure in the introduction passage and the passage of the raw material gas. A discharge passage provided with a regulating valve is provided, and a non-reactive gas source having a pressure higher than the upper limit pressure of the reaction chamber set by the reaction pressure regulating valve is provided at the primary end of the supply passage to supply the gas. A pilot type pressure control valve is provided in the path, and the pressure control valve connects the supply path only when the internal pressure of the reaction chamber is higher than the internal pressure of the furnace chamber. It is configured to release the furnace chamber to the atmosphere when it becomes lower It is characterized by a door.

It is preferable that the pilot type pressure control valve and the reaction chamber are connected to each other through a power gas conduit which is independent of the raw gas introducing passage and the discharge passage. Further, in the reaction treatment apparatus of the present invention according to claim 5, an inverted cup-shaped heat insulating layer is provided in the high-pressure container, a partition is provided inside the heat insulating layer, and a heating element is provided between the heat insulating layer and the partition. And the inside of the partition wall as a reaction chamber for the object to be treated, a furnace chamber is provided with a non-reactive gas supply path equipped with a pressure control valve, and a reaction chamber is provided with A discharge path provided with a reaction pressure adjusting valve is provided in the raw material gas introducing path and the path, the partition wall has gas permeability, and the pressure adjusting valve is set to a pressure higher than that of the reaction pressure adjusting valve. The state in which the non-reactive gas in the furnace chamber intrudes into the reaction chamber through the partition wall is always maintained, and the non-reactive gas flowing in the supply channel is introduced in the introduction channel via the flow rate controller. It is characterized in that it can be mixed with the raw material gas.

It is preferable that a flow rate detector for non-reactive gas is provided in the supply passage and the flow rate regulator is controlled by a signal from the flow rate detector. It is preferable that the supply passage and the introduction passage can be communicated with each other outside the high-pressure container via an on-off valve.

[0010]

According to the present invention of claims 1 to 4, when the internal pressure of the auxiliary chamber (for example, reaction chamber) is higher than the internal pressure of the pressure chamber (for example, furnace chamber), the pressurized fluid is used. The pressurized fluid is supplied from the source (for example, a cylinder of non-reactive gas) to the pressure chamber to increase the internal pressure of the pressure chamber. on the other hand,
When the internal pressure of the pressure chamber is higher than the internal pressure of the accessory chamber, the internal pressure is reduced by releasing the pressure chamber. In this way, the internal pressure of the pressure chamber is always balanced with the internal pressure of the accessory chamber.

When comparing the internal pressures of the auxiliary chamber and the pressure chamber, a pressure difference is generated between the two chambers by proportionally changing one of them by the pressure increasing means or the pressure reducing means before the comparison. Is possible. If the pilot type pressure control valve and the auxiliary chamber (reaction chamber) are connected to each other by an independent power gas conduit, disturbance is unlikely to affect the operation of the pressure control valve.

According to the present invention of claims 5 to 7,
By making the partition wall of the reaction chamber gas permeable or connecting the supply passage and the introduction passage, the raw material gas in the reaction chamber is mixed with the non-reactive gas, whereby the internal pressure of the furnace chamber and the reaction chamber The pressure can be balanced with the internal pressure of.

[0013]

Embodiments of the method and apparatus of the present invention will be described below in detail with reference to the drawings. In FIG. 1 showing a first embodiment of a reaction processing apparatus according to the present invention, a high pressure container 1 formed in a cylindrical shape.
The upper lid 2 and the lower lid 3 are fitted in the upper and lower openings of the high pressure chamber 6 by keeping airtightness by the seal members 4 and 5.
Is formed. Although not shown, the axial force acting on the upper and lower lids 2 and 3 is carried by a swivel type or traveling trolley type press frame which is detachably engaged with the upper and lower lids 2 and 3.

In the high-pressure chamber 6, an inverted cup-shaped heat insulating layer 7 is provided.
Is installed, and an inverted cup-shaped partition wall 8 is installed further inside the heat insulating layer 7. In the illustrated example, the partition wall 8 is the lower lid 3.
The inside of the partition wall 8 is defined as a reaction chamber 12 by being fixedly provided on the upper side with a seal member 9 and provided with a sample table 11 on which an object to be treated 10 is placed. Further, in the high pressure chamber 6, a heating body 13 is provided between the heat insulating layer 7 and the partition wall 8.
Is installed, and this part is the furnace chamber 14.

The lower lid 3 has a passage 18 communicating with the inside and outside of the reaction chamber 12, an inner pipe 19 connected to the inside of the passage 18 and an outer pipe 20 connected to the outside of the passage 18. Is provided. A pressurized fluid source 22 such as a cylinder filled with a raw material gas (such as methane gas) is connected to a primary end 21a of the introduction path 21, and an opening / closing valve 25, a pressure adjusting valve 26, and a flow rate adjusting are provided in the path. The container 27 is provided.

In addition to the introduction passage 21, the lower lid 3 has a passage 30 communicating with the inside and outside of the reaction chamber 12, and the passage 30.
Discharge path 3 consisting of an outer pipe 31 connected to the outdoor side of 0
Two are provided. An on-off valve 33 and a reaction pressure adjusting valve 34 are provided in the discharge passage 32, and the secondary end 32
a is released. Than the reaction pressure control valve 34
It goes without saying that the pressure adjustment valve 26 provided in the introduction passage 21 has a higher set pressure.

Further, the lower lid 3 has an introduction passage 21 and a discharge passage 32.
Separately and independently of the above, a passage 38 communicating with the inside and outside of the reaction chamber 12 and an external pipe 39 connected to the outside of the passage 38.
Is provided with a power gas conduit 40. This power gas conduit 40 is used for the pilot type pressure control valve 4 described later.
Connected to 3. It should be noted that the power gas conduit 40 may be configured to serve as the other passage 18 or 30, especially in the passage 38, but in this case, vapor deposition of pyrolytic carbon or the like generated by the raw material gas is performed. When the pipe path is blocked by an object, the operation of the pressure control valve 43 is disturbed, so that it is desirable that the power gas guide path 40 has an independent structure as described above.

The upper lid 2 is provided with a supply passage 47 consisting of a passage 45 communicating with the inside and outside of the high pressure chamber 6 (furnace chamber 14) and an external pipe 46 connected to the outside of the passage 45.
A pressurized fluid source 48 such as a cylinder filled with a non-reactive gas is connected to the primary end 47a of the supply path 47, and an opening / closing valve 49 and a pilot type pressure control valve 43 are interposed in the path. It is set up. As the non-reactive gas, a rare gas such as argon gas or a nitrogen gas can be used.

The pilot type pressure control valve 43 is shown in FIG.
As shown in, the valve section 50 and the comparison section 51 are connected to each other. The valve part 50 is provided with a primary port part 52 used for connection with the pressurized fluid source 48 side in the supply path 47 and a secondary port part 53 used for connection with the furnace chamber 14 side. 5
1 is provided with a pilot port 55 provided for connection to the reaction chamber 12 side by the power gas conduit 40 and a pilot port 57 provided for connection with the furnace chamber 14 side by the bypass pipe 56. Then, the internal pressure of the reaction chamber 12 and the furnace chamber 14
The internal pressure of the reaction chamber 1 is constantly compared with that of the reaction chamber 1
When the internal pressure of 2 is higher than the internal pressure of the furnace chamber 14, the pressurized fluid source 48 (on the side of the primary opening 52) and the furnace chamber 14 (the secondary opening 53).
Side) to increase the internal pressure of the furnace chamber 14, and conversely, when the internal pressure of the furnace chamber 14 is higher than the internal pressure of the reaction chamber 12, the reaction chamber 12 is opened via the release port 50a. When released, the internal pressure is reduced. Therefore, the internal pressure of the reaction chamber 12 is always balanced with the internal pressure of the furnace chamber 14.

The usage status of this reaction processing apparatus will be described.
First, the inside of the reaction chamber 12 is evacuated by a vacuum pump (not shown) through the discharge passage 32, and then the source gas is supplied from the pressurized fluid source 22 into the reaction chamber 12 through the introduction passage 21. At this time, the flow rate of the raw material gas is controlled to a predetermined value by the flow rate regulator 27, and the internal pressure of the reaction chamber 12 is kept constant by the reaction pressure regulating valve 34. Furthermore, the internal pressure of the reaction chamber 12 is the pressure control valve 43.
Is balanced with the internal pressure of the furnace chamber 14. In such a state, the object to be processed 10 is indirectly heated to a predetermined temperature through the partition wall 8 by the heating body 13 so that a vapor deposition film is formed or reacted on the object to be processed 10 by the vapor phase chemical vapor deposition reaction. Become. After the processing is finished, the heating of the heating element 13 is stopped, the on-off valve 25 is closed to stop the supply of the raw material gas, and the gas in the reaction chamber 12 is exhausted through the exhaust passage 32.

In such a series of processes, the gas expands or contracts in accordance with the temperature change in the reaction chamber 12, but since the pressure control valve 43 constantly carries out pressure balance as described above, The internal pressure of 12 and the internal pressure of the furnace chamber 14 are automatically made equal, and therefore the partition wall 8 is not damaged due to the pressure difference. The pressure control method according to the present invention is not limited to the implementation in the reaction processing apparatus, and is used for achieving the pressure balance between the two chambers of the pressure chamber A and the auxiliary chamber B as shown in the schematic view of FIG. It can be widely used as a technology. In the figure, if the pressure chamber A corresponds to the furnace chamber 14 of the above-described embodiment and the auxiliary chamber B corresponds to the reaction chamber 12, the pressurized fluid source C connected to the pressure chamber A is non-reactive. Although it corresponds to a gas cylinder (see reference numeral 48), it is also possible to correspond the pressure chamber A to the reaction chamber 12 and the auxiliary chamber B to the furnace chamber 14 on the contrary. The pressure fluid source C corresponds to a cylinder of the source gas (see reference numeral 22). With such a configuration change, the pipe connecting the pressure chamber A and the pressurized fluid source C is used as the supply passage 47 or the introduction passage 21, and the power gas conduit 4 is also used.
It goes without saying that the connection target of 0 will also be different.

FIG. 4 shows a boosting means 60 for the power gas conduit 40.
This is an example in which the booster means 60 is provided.
Is the pressure receiving area that receives the internal pressure of the auxiliary chamber B,
On the third side, that is, the piston structure is formed larger than the pressure receiving area for receiving the internal pressure of the pressure chamber A. for that reason,
The pressure control valve 43 inevitably becomes more affected by the internal pressure of the auxiliary chamber B than that of the pressure chamber A, and the pressure is balanced while the pressure difference between the two chambers is generated. The boosting means 60 may be provided on the supply path 47 (or the introduction path 21), and although not shown in the drawing, the boosting means 60 is connected in the opposite direction to reduce the pressure. Can also be used as

FIG. 5 shows a second embodiment of the reaction processing apparatus according to the present invention.
The embodiment shows an example of the pilot type pressure control valve 4
Instead of using No. 3, the following configuration is provided. That is, the partition wall 62 that defines the reaction chamber 12 is formed of a gas permeable structure, for example, a carbon material, and the supply passage 4
In the passage of No. 7, the pressure adjusting valve 63 whose set pressure is slightly higher than that of the reaction pressure adjusting valve 34 provided in the discharge passage 32
Is installed.

Therefore, the non-reactive gas supplied from the pressurized fluid source 48 into the furnace chamber 14 via the pressure regulating valve 63 is
At all times, the gas slightly invades into the reaction chamber 12 via the partition wall 62, and in the first place, no unreasonable pressure acts on the partition wall 62 from inside and outside the reaction chamber 12. Of course, the raw material gas in the reaction chamber 12 does not leak into the furnace chamber 14. Infiltration of such a non-reactive gas also promotes heat transfer from the heating body 13 to the object to be processed 10, and
It also has an advantage of suppressing unnecessary vapor deposition reaction generation on the inner surface of the partition wall 62.

The supply passage 47 is provided with a release valve 66 which is opened / closed by a controller 65 in response to a signal from the pressure gauge 64 so that the internal pressure of the furnace chamber 14 does not exceed a predetermined value. Has become. By using the same carbon material as the partition wall 62 for the heating body 13, heat resistance at high temperature against the synthesis of the carbonized film by the hydrocarbon-based gas and reaction resistance of the partition wall can also be obtained. Besides, it is also possible to use porous oxide ceramics for the partition wall 62, and in this case, oxidation resistance at high temperature can be obtained. Also, the partition wall 6
As the material 2, a material having a minute dispersion opening may be used (the forming material itself may be airtight (for example, a metal material)).

A first bypass passage 67 connects the primary side of the pressure regulating valve 63 in the supply passage 47 and the secondary side of the flow rate regulator 27 in the introduction passage 21.
An opening / closing valve 68 and a pressure regulator 6 are provided in the first bypass passage 67.
9. A flow rate regulator 70 is provided. Therefore, it is possible to positively mix the non-reactive gas with the raw material gas as necessary, and for example, it is possible to deal with the case where the amount of the non-reactive gas that enters the partition wall 62 is small. Become.

The flow rate regulator 70 is constructed so as to be remotely controllable, and the flow rate detector 71 is provided in the supply path 47.
The flow rate can be controlled by the indicator 72 which is operated by the signal from. Therefore, the total gas amount of the non-reactive gas can be maintained at a predetermined and constant value, which is useful for reaction control. In addition, the passage 18 in the introduction passage 21
On-off valves 75 and 76 are provided on the primary side of the supply path 47 and on the primary side of the passage 45, respectively, and an on-off valve 77 is provided between the secondary sides of these on-off valves 75 and 76. It is connected by the second bypass passage 78.

Therefore, at the start of the operation of this reaction processing apparatus, the on-off valves 49, 76 and 77 are opened and the on-off valve 2 is opened.
5, 68, 75 and 33 are closed and the pressurized fluid source 4
The reaction chamber 12 and the furnace chamber 14 can be filled with the non-reactive gas from the chamber 8 so as to have the same pressure. In this way, after the heating by the heating element 13 is started and the predetermined temperature is reached, the on-off valve 77 is closed and the on-off valves 75 and 33 are closed.
By switching to the open state, the introduction of the raw material gas can be started without causing a pressure difference. In this case, the internal pressure of the reaction chamber 12 is adjusted by the reaction pressure adjusting valve 34, and the internal pressure of the furnace chamber 14 is adjusted by the pressure adjusting valve 63.

When the reaction processing apparatus is stopped, the on-off valve 25 is first closed to wait for the inside of the reaction chamber 12 to be replaced with the non-reactive gas, and the on-off valves 33 and 49 are closed.
By opening the open / close valve 77, the reaction chamber 12 and the furnace chamber 14 are opened.
We will try to reach the final stop while maintaining a pressure balance with. Other configurations and operations are the same as those in the first embodiment, and the detailed description thereof will be omitted by giving the same reference numerals.

The present invention is not limited to high pressure, but can be carried out under reduced pressure.

[0031]

As described in detail above, according to the method and apparatus of the present invention, the pressure balance inside and outside the reaction chamber is simplified and the structure is simplified.
Moreover, it becomes possible to control accurately, and the partition wall that defines the reaction chamber is never damaged due to the pressure difference,
Therefore, it is possible to thoroughly prevent accidents and failures such as electric insulation breakdown due to leakage of the raw material gas.

[Brief description of drawings]

FIG. 1 is a sectional view of the overall configuration showing a first embodiment according to the present invention.

FIG. 2 is an operation explanatory view showing an enlarged pilot type pressure control valve.

FIG. 3 is a schematic diagram illustrating the principle of the method of the present invention.

FIG. 4 is a schematic diagram when a boosting means is used in the method of the present invention.

FIG. 5 is a sectional view showing the overall structure of a second embodiment according to the present invention.

[Explanation of symbols]

 DESCRIPTION OF SYMBOLS 1 High-pressure container 7 Thermal insulation layer 8 Partition wall 10 Processed object 12 Reaction chamber 13 Heating body 14 Furnace chamber 21 Introducing path 32 Discharging path 34 Reaction pressure adjusting valve 40 Power gas guiding path 43 Pilot type pressure control valve 47 Supply path 48 Pressurized fluid Source 60 Pressure rising means 62 Partition wall (having gas permeability) 70 Flow rate regulator 71 Flow rate detector 77 Open / close valve

Claims (7)

[Claims] 1. A pressure chamber (see furnace chamber 14) connected to a pressurized fluid source (48) and an auxiliary chamber (reaction chamber 12) attached thereto.
In the pressure control method of (1), the internal pressures of the chambers are compared with each other, and when the internal pressure of the auxiliary chamber (see the reaction chamber 12) is high, the pressurized fluid source (48) and the pressure chamber (see the furnace chamber 14) are used. And the internal pressure of the pressure chamber (see furnace chamber 14) is high, the pressure chamber (see furnace chamber 14) and the auxiliary chamber (see reaction chamber 12) are released by releasing the pressure chamber (see furnace chamber 14). A pressure control method comprising: 2. The internal pressure of any one of the pressure chamber (see the furnace chamber 14) and the auxiliary chamber (see the reaction chamber 12) is proportionally changed via the pressure increasing means or the pressure reducing means, and then the internal pressures are compared, The pressure control method according to claim 1, wherein a pressure difference is generated between both chambers. 3. An insulating cup-shaped heat insulating layer (7) is provided in the high-pressure vessel (1), and a partition (8) is provided inside the heat insulating layer (7), and the heat insulating layer (7) and the partition (8). A heating element (13) is provided between the heating chamber and the heating chamber to form a furnace chamber (14), and the inside of the partition wall (8) serves as a reaction chamber (12) for the object to be treated (10). Is a non-reactive gas supply path (4
7) is provided, and an inlet passage (21) for the raw material gas and an outlet passage (32) provided with a reaction pressure adjusting valve (34) in the passage are provided to the reaction chamber (12), and the supply passage ( 47)
The primary end (47a) is provided with a pressurized fluid source (48) of non-reactive gas having a pressure higher than the upper limit pressure of the reaction chamber (12) set by the reaction pressure control valve (34), A pilot type pressure control valve (43) is provided in the supply path (47), and the pressure control valve (43) is provided when the internal pressure of the reaction chamber (12) is higher than the internal pressure of the furnace chamber (14). Only the supply path (47) is communicated, and when the internal pressure of the reaction chamber (12) becomes lower than the internal pressure of the furnace chamber (14), the furnace chamber (14) is released. And a reaction processing device. 4. The pilot type pressure control valve (43) and the reaction chamber (12) are connected to each other through a power gas conduit (40) independent of a feed gas introduction passage (21) and a discharge passage (32). The reaction processing apparatus according to claim 3, wherein 5. A heat insulating layer (7) having an inverted cup shape is provided in the high pressure vessel (1), and a partition (8) is provided inside the heat insulating layer (7), and the heat insulating layer (7) and the partition (8). A heating element (13) is provided between the heating chamber and the heating chamber to form a furnace chamber (14), and the inside of the partition wall (8) serves as a reaction chamber (12) for the object to be treated (10). Is a pressure regulating valve (6
3) is provided with a non-reactive gas supply path (47),
The reaction chamber (12) is provided with an inlet passage (21) for the raw material gas and an outlet passage (32) provided with a reaction pressure adjusting valve (34) in the passage, and the partition wall (8) is gas permeable. And a reaction pressure adjusting valve (3)
The pressure is set higher than that of 4) so that the state in which the non-reactive gas in the furnace chamber (14) enters the reaction chamber (12) through the partition wall (8) is always maintained, and A reaction treatment device, characterized in that a non-reactive gas flowing through a supply passage (47) can be mixed with a raw material gas inside an introduction passage (21) through a flow rate regulator (70). 6. The flow path (47) is provided with a flow rate detector (71) for non-reactive gas, and the flow rate detector (71).
The reaction processing apparatus according to claim 5, wherein the flow rate regulator (70) is controlled by a signal from the. 7. The supply passage (47) and the introduction passage (21) can communicate with each other outside the high-pressure container (1) via an opening / closing valve (77). Item 6
The reaction processing apparatus described.