WO2012157370A1

WO2012157370A1 - Method of opening reaction chamber and vapor phase growth device

Info

Publication number: WO2012157370A1
Application number: PCT/JP2012/059644
Authority: WO
Inventors: 正明児玉; 俊範岡田
Original assignee: シャープ株式会社
Priority date: 2011-05-13
Filing date: 2012-04-09
Publication date: 2012-11-22
Also published as: JP5079902B1; JP2012238772A; TW201303972A

Abstract

The purpose of the present invention is to provide a method of opening a reaction chamber and a vapor phase growth device such that the reaction chamber is opened while the occurrence and the spread of particles are suppressed. A reaction chamber (101) is pressurized by gas introduced thereinto, a discharge valve (112b) and an equalizing valve (107b) are opened when the pressure difference between the reaction chamber (101) and a working chamber (102) is reduced to a given value or less, then the reaction chamber (101) communicates with the working chamber (102) through the equalizing path (107a) while discharging the gas from the reaction chamber (101), and after the pressures in the reaction chamber (101) and the working chamber (102) are equalized, the reaction chamber (101) is opened.

Description

Method of opening reaction chamber and vapor phase growth apparatus

The present invention relates to a method of opening a reaction chamber, which suppresses generation and diffusion of particles to open a reaction chamber, and a vapor phase growth apparatus.

Semiconductor light-emitting devices such as light-emitting diode devices and laser diode devices are considered to be widely applied to high-density optical disks, full-color displays, and further to the environment and medical fields. Chemical vapor deposition (CVD) is generally used as a method of manufacturing a semiconductor light emitting device. Using this chemical vapor deposition method, the vapor phase growth apparatus introduces a reaction gas into the reaction chamber, and vapor-phase grows the heated substrate on the inside of the reaction chamber to form a thin film of a compound semiconductor crystal. In such a vapor phase growth apparatus, while improving the quality of a thin film of a compound semiconductor crystal, it is always highly demanded how to secure the maximum yield and production capacity while suppressing the production cost. .

When forming a thin film, the reaction gas also adheres as a by-product to the inner wall of the reaction chamber, piping, members inside the reaction chamber, etc., and among the adhered by-products, the separated by-product or fine particle by-product Are the particles. When the particles adhere to the surface of the substrate, the characteristics of the compound semiconductor are degraded, and measures have been taken to prevent the generation and diffusion of the particles.

For example, in Japanese Patent Application Laid-Open No. 6-177060 (Patent Document 1), a reaction chamber into which a substrate (a wafer in Japanese Patent Application Laid-Open No. 6-177060 (Patent Document 1) is inserted), and insertion of the substrate into the reaction chamber An exhaust path (Japanese Patent Application Laid-Open No. 6-177060) including a work chamber (load lock room in Japanese Patent Application Laid-Open No. 6-177060) for taking out and connected to the reaction chamber A gas phase growth apparatus is disclosed in which a gas exhaust line) and an exhaust path connected to the working chamber are short-circuited by a pressure equalizing path (a connecting pipe in JP-A-6-177060 (Patent Document 1)). The vapor phase growth apparatus of Japanese Patent Application Laid-Open No. 6-177060 (Patent Document 1) opens a pressure equalizing valve (inter-contact valve in Japanese Patent Application Laid-open No. 6-177060 (Patent Document 1)) provided in the pressure equalizing passage, By opening the reaction chamber to the working chamber after eliminating the pressure difference between the reaction chamber and the working chamber, the rapid flow of gas caused by the pressure difference between the reaction chamber and the working chamber when the reaction chamber is opened To reduce the generation of particles.

Japanese Patent Application Laid-Open No. 6-177060

In JP-A-6-177060 (Patent Document 1), the pressure difference between the reaction chamber and the working chamber is eliminated and then the reaction chamber is opened to suppress the generation of particles when the reaction chamber is opened. However, when the pressure equalizing valve is opened, there is a pressure difference between the reaction chamber and the working chamber, and this pressure difference causes a problem that particles are generated and are diffused to the reaction chamber or the working chamber. Further, in Japanese Patent Application Laid-Open No. 6-177060 (Patent Document 1), it is necessary to take out a port loaded with a substrate from the reaction chamber in order to take out the substrate after film formation processing from the reaction chamber after opening the reaction chamber. However, there is a problem that particles are generated due to the vibration caused by the operation of the device for moving the port to take out the substrate.

The present invention has been made to solve the above-mentioned problems, and an object of the present invention is to provide a reaction chamber opening method and a vapor phase growth apparatus which suppress generation and diffusion of particles.

In order to solve the above problems, the reaction chamber opening method according to the present invention is a reaction chamber opening method for opening a reaction chamber accommodated in a working chamber, wherein a gas is introduced into the reaction chamber to increase the pressure in the reaction chamber. A process of communicating the reaction chamber with the working chamber while exhausting the gas from the reaction chamber after raising the pressure in the reaction chamber until the pressure difference between the reaction chamber and the working chamber becomes equal to or less than a predetermined value; And the step of opening the reaction chamber after communicating the operation chamber with the working chamber.

The step of communicating the reaction chamber with the working chamber while exhausting the gas from the reaction chamber is provided in an exhaust path for exhausting the gas from the reaction chamber when the pressure difference between the reaction chamber and the working chamber becomes equal to or less than a predetermined value. Preferably, the discharge valve is opened, and the pressure equalizing valve provided in the pressure equalizing passage for communicating the reaction chamber with the working chamber is opened.

It is preferable to further include the steps of closing the discharge valve before opening the reaction chamber after opening the pressure equalization valve, and opening the discharge valve after opening the reaction chamber.

It is preferable to adjust the amount of gas exhausted from the reaction chamber based on the amount of gas introduced into the working chamber.

It is preferable to introduce a gas into the reaction chamber when the reaction chamber is opened.
It is preferable to adjust the amount of gas exhausted from the reaction chamber based on the amount of gas introduced into the reaction chamber and the amount of gas introduced into the working chamber.

In the reaction chamber opening method of the present invention, the pressure in the reaction chamber is increased until the pressure difference between the reaction chamber and the reaction chamber falls below a predetermined value. The method further comprises the steps of: communicating the reaction chamber with the reaction chamber while exhausting the gas from the reaction chamber; and opening the reaction chamber after connecting the reaction chamber with the reaction chamber.

The step of communicating the reaction chamber with the reaction chamber while exhausting the gas from the reaction chamber is provided in an exhaust path for exhausting the gas from the reaction chamber when the pressure difference between the reaction chamber and the reaction chamber is less than a predetermined value. Preferably, the discharge valve is opened, and the pressure equalizing valve provided in the pressure equalizing passage for communicating the reaction chamber with the reaction chamber is opened.

It is preferable to introduce a gas into the reaction chamber when the reaction chamber is opened.
It is preferable to adjust the amount of gas exhausted from the reaction chamber based on the amount of gas introduced into the reaction chamber.

A vapor phase growth apparatus according to the present invention is a vapor phase growth apparatus including a reaction chamber accommodated in a working chamber, and the pressure adjusting unit adjusts the pressure of the working chamber from a first pressure to a second pressure. The pressure equalization unit for connecting the reaction chamber and the working chamber to equalize the pressure of the reaction chamber with the pressure of the working chamber, the gas is exhausted when the reaction chamber and the working chamber are communicated, and particles are discharged from the reaction chamber It is characterized by comprising an exhaust part for discharging and an opening part for opening the reaction chamber.

The exhaust unit preferably has an exhaust valve that is opened when the difference between the pressure in the reaction chamber and the first pressure is less than or equal to a predetermined value.

Preferably, the exhaust unit further includes a flow control valve for adjusting the amount of gas exhausted from the reaction chamber based on the amount of gas introduced into the working chamber.

The exhaust unit preferably further includes a flow control valve for adjusting the amount of gas exhausted from the reaction chamber based on the amount of gas introduced into the reaction chamber and the amount of gas introduced into the working chamber.

According to the present invention, it is possible to provide a reaction chamber opening method and a vapor phase growth apparatus in which the reaction chamber is opened by suppressing generation and diffusion of particles.

It is a block diagram which shows the vapor phase growth apparatus of Example 1 of this invention. It is explanatory drawing for demonstrating the structure of the vapor phase growth apparatus of Example 1 of this invention. It is explanatory drawing for demonstrating the air flow at the time of open | release of the vapor phase growth apparatus of Example 1 of this invention. It is a flowchart which shows the reaction chamber open method of Example 1 of this invention. It is a flowchart which shows the reaction chamber open method of Example 2 of this invention. It is explanatory drawing for demonstrating the airflow at the time of open | release of the vapor phase growth apparatus of Example 3 of this invention. It is a block diagram which shows the vapor phase growth apparatus of Example 4 of this invention. It is a flowchart which shows the reaction chamber open method of Example 4 of this invention.

Example 1
Hereinafter, Example 1 of the present invention will be described based on FIGS. 1 to 4. FIG. 1 is a block diagram showing an outline of a vapor phase growth apparatus 100 according to a first embodiment. The vapor deposition apparatus 100 accommodates the reaction chamber 101 in the working chamber 102, introduces a gas into the reaction chamber 101 by the first introduction unit 103, and generates a thin film of a compound semiconductor crystal on a substrate in the reaction chamber 101. The gas and particles in the reaction chamber 101 are exhausted from the exhaust unit 104. In the vapor phase growth apparatus 100, a gas is introduced into the working chamber 102 by the second introduction unit 105 to isolate the reaction chamber 101 from the atmosphere, and the pressure of the working chamber 102 is adjusted by the pressure adjusting unit 106. After the pressure of the reaction chamber 101 and the working chamber 102 is equalized by the pressure equalizing unit 107, the substrate on which the thin film is formed is taken out by opening the reaction chamber 101. In the vapor phase growth apparatus 100, the pressure detection unit 108 monitors the pressure of the reaction chamber 101, the pressure detection unit 109 monitors the pressure of the working chamber 102, and the control unit 110 controls each unit.

The reaction chamber 101 is a space for growing a compound semiconductor composed of the reaction chamber opening portion 101a and the reaction chamber main body 101b. The substrate is disposed in the reaction chamber main body 101b, and the opening of the reaction chamber main body 101b is covered with the reaction chamber opening 101a. After thin film formation, the reaction chamber 101 is opened by operating the reaction chamber opening portion 101a by the opening portion (not shown), and the processed substrate is taken out. In a state where the working chamber 102 is isolated from the atmosphere so that impurities do not enter the reaction chamber 101, the substrate insertion into the reaction chamber 101, the removal of the substrate from the reaction chamber 101, the maintenance of the reaction chamber 101, etc. It is a space for It is not necessary for the entire reaction chamber 101 to be accommodated in the working chamber 102, and it is sufficient that the opening portions of the reaction chamber opening part 101a and the reaction chamber main body 101b be accommodated in the working chamber 102.

The first introducing unit 103 has an introducing path 103 a connected to the reaction chamber 101 and a first gas supply unit 103 b, and is an introducing unit for introducing a gas into the reaction chamber 101. The first gas supply unit 103 b has a reactive gas source, an inert gas source, and a valve for performing introduction, stop, or control of the flow rate of various gases, and the first introduction unit 103 reacts via the introduction path 103 a. Introduce a gas, an inert gas, or a mixture of these. The second introducing unit 105 includes an introducing path 105 a connected to the working chamber 102 and a second gas supply unit 105 b, and is an introducing unit for introducing a gas into the working chamber 102. The second gas supply unit 105b has an inert gas source and a valve for introducing, stopping or controlling the flow rate of the inert gas, and the second introduction unit 105 is not connected to the working chamber 102 through the introduction passage 105a. Introduce the active gas. The reaction gas is a mixture of an organometallic gas such as trimethylgallium (TMG) or trimethylaluminum (TMA) and a hydrogen compound gas such as ammonia (NH ₃ ), phosphine (PH ₃ ), or arsine (AsH ₃ ). These reaction gases are introduced into the reaction chamber 101 together with a carrier gas such as nitrogen (N ₂ ). The inert gas is nitrogen (N ₂ ), hydrogen (H ₂ ), argon (Ar) or the like.

The exhaust unit 104 includes an exhaust passage 111 connected to the reaction chamber 101, an exhaust valve 112 provided in the exhaust passage 111, and an exclusion unit 113, and exhausts gas from the reaction chamber 101. The exclusion unit 113 sucks the gas from the reaction chamber 101 through the exhaust passage 111 and exhausts the gas to the atmosphere. At this time, particles are also discharged from the reaction chamber 101 together with the gas.

The pressure adjusting unit 106 is provided in the working chamber 102 and exhausts gas from the working chamber 102 to adjust the pressure in the working chamber 102 to a predetermined range. When the pressure in the working chamber 102 reaches the upper limit value By starting the exhaust of inert gas in the working chamber 102 and stopping the exhaust when the lower limit value is reached, the pressure of the working chamber 102 is adjusted to a predetermined range. Assuming that the lower limit value of the pressure adjustment unit 106 is a first pressure and the upper limit value is a second pressure, the pressure in the working chamber 102 is adjusted in the range from the first pressure to the second pressure.

The pressure equalizing unit 107 includes a pressure equalizing passage 107a for communicating the reaction chamber 101 with the working chamber 102, and a pressure equalizing valve 107b provided in the pressure equalizing passage 107a. The pressure equalizing portion 107 communicates the reaction chamber 101 with the working chamber 102 to equalize pressure. It is a pressure equalization part.

The pressure detection unit 108 and the pressure detection unit 109 are pressure detection units that detect the pressure in the reaction chamber 101 and the work chamber 102, respectively. The control unit 110 receives detection signals from the pressure detection unit 108 and the pressure detection unit 109, and controls the first gas supply unit 103b, the pressure equalizing valve 107b, and the exhaust valve 112 based on the pressure in the reaction chamber 101 and the working chamber 102. . The second introducing unit 105 always introduces the gas into the working chamber 102 at a constant introducing amount, but the controlling unit 110 may control the introducing amount based on the pressure of the reaction chamber 101 or the working chamber 102. Similarly, although the exclusion unit 113 always exhausts the gas, the control unit 110 may control the exhaust amount. Further, although the pressure adjustment unit 106 automatically adjusts the pressure in the working chamber 102, the control unit 110 may control the start and stop of the exhaust to adjust the pressure. The vapor deposition apparatus 100 may be provided with a differential pressure detection unit that detects the pressure difference between the reaction chamber 101 and the working chamber 102, and the control unit 110 receives a detection signal from the differential pressure detection unit and sends control signals to each unit. You may send it.

FIG. 2 is an explanatory view for explaining the structure of the vapor phase growth apparatus of the first embodiment. However, the control unit 110 is not shown. The reaction chamber 101 is formed of a reaction chamber opening portion 101a and a reaction chamber main body 101b opened at the upper side, and the reaction chamber opening portion 101a is attached to the opening of the reaction chamber main body 101b through an O ring 114. Is sealed. The reaction chamber opening portion 101a and the reaction chamber main body 101b are made of a material excellent in corrosion resistance, and are made of, for example, stainless steel. The lifting device 115 is an opening part which raises and lowers the reaction chamber opening part 101a and raises the reaction chamber opening part 101a to open the reaction chamber 101. The reaction chamber opening part 101a is connected to the introduction path 103a, and the reaction gas and the inert gas are introduced from the first gas supply part 103b. One or more introduction paths 103a may be connected. In addition, the reaction chamber opening portion 101a includes a shower plate 116, and the introduced gas is uniformly diffused by the shower plate 116 and supplied. The pressure in the reaction chamber 101 is measured by the pressure detection unit 108.

The reaction chamber main body 101 b accommodates a disk-shaped susceptor 117, and the susceptor 117 includes a substrate holder 118. The susceptor 117 may have a plurality of substrate holders 118, but may have one substrate holder 118 concentric with the susceptor 117. A rotation drive shaft 119 for rotating the susceptor 117 is provided at the center of the bottom of the susceptor 117. Further, a heater 120 is provided concentrically with the susceptor 117 below the susceptor 117. The substrate on which the thin film is to be produced is placed on the substrate holder 118.

The work chamber 102 is a space for working the reaction chamber 101 isolated from the atmosphere, and is, for example, a glove box or a clean room. The work chamber 102 is connected to the introduction path 105a, and an inert gas is introduced from the second gas supply unit 105b to isolate the reaction chamber 101 from the atmosphere. The pressure in the working chamber 102 is adjusted to a predetermined range by the pressure adjusting unit 106. The pressure adjustment unit 106 is, for example, an oil bubbler, and exhausts the inert gas through the exhaust passage 121 connected to the working chamber 102 when the pressure in the working chamber 102 rises from the set value (first pressure). Start. The pressure in the working chamber 102 decreases due to the exhaust of the inert gas, and when the pressure returns to the set value, the pressure adjustment unit 106 stops the exhaust of the inert gas. In the working chamber 102, the inert gas is always introduced from the second gas supply unit 105b, so when the exhaust is stopped, the pressure in the working chamber 102 rises again. Assuming that the pressure at which the pressure adjusting unit 106 starts exhausting is the second pressure, the pressure adjusting unit 106 repeats the start and stop of the exhaust, so that the pressure of the working chamber 102 ranges from the first pressure to the second pressure. And, for example, in the range of 101.3 [kPa] to 101.6 [kPa]. The pressure adjustment unit 106 may be a solenoid valve that starts exhausting when the pressure in the working chamber 102 reaches the upper limit of the setting and stops exhausting when the pressure in the working chamber 102 reaches the lower limit. The pressure in the working chamber 102 is measured by the pressure detection unit 109.

The exhaust unit 104 includes an exhaust passage 111 connected to the reaction chamber 101, an exhaust valve 112 provided in the exhaust passage 111, a filter 122, and an exclusion unit 113. The exclusion unit 113 sucks the gas from the reaction chamber 101 through the exhaust passage 111 and exhausts the gas to the atmosphere. The reaction chamber 101 has a plurality of exhaust ports, and the reaction gas and the inert gas are exhausted from the exhaust port via the exhaust passage 111. In addition, the particles are exhausted together with the exhaust gas and trapped by the filter 122. Although the exhaust passage 111 may be connected to a plurality of exhaust ports of the reaction chamber 101 and the plurality of exhaust passages 111 may join into one, the reaction chamber 101 has one exhaust port, and one exhaust passage 111 May be connected to the reaction chamber 101.

The exhaust passage 111 is made of, for example, stainless steel, and includes a main exhaust passage 111a, an auxiliary exhaust passage 111b, and an overpressurization preventing passage 111c. In addition, the exhaust valve 112 includes a main exhaust valve 112a, an exhaust valve 112b, an overpressurization prevention valve 112c, and a flow rate adjustment valve 112d. The main exhaust passage 111a is provided with a main exhaust valve 112a and a vacuum pump 123, and the vacuum pump 123 performs roughing to reduce the pressure of the reaction chamber 101 via the main exhaust passage 111a. The sub-exhaust passage 111b is provided with a discharge valve 112b and a flow control valve 112d, and the flow control valve 112d adjusts the flow rate of the gas. The flow rate of the auxiliary exhaust passage 111b may be set in advance, but may be arbitrarily changed. The overpressure protection path 111c is provided with an overpressure protection valve 112c, and is used when the pressure in the reaction chamber 101 becomes abnormally high. That is, the overpressurization prevention valve 112 c is opened when the pressure in the reaction chamber 101 becomes an abnormally high pressure, and the gas is forcibly exhausted from the reaction chamber 101 to return the pressure in the reaction chamber 101 to the normal state.

The pressure equalizing path 107a is made of, for example, stainless steel, one end is connected to the reaction chamber main body 101b, the other end is connected to the working chamber 102, and the pressure equalizing valve 107b is opened to communicate the reaction chamber 101 with the working chamber 102. The reaction chamber 101 and the working chamber 102 may be in communication with each other via the pressure equalizing path 107 a. For example, one end of the pressure equalizing path 107 a may be connected to the exhaust path 111 and the other end may be connected to the exhaust path 121. . Further, the pressure equalizing path 107 a may be a vent provided on the wall surface of the reaction chamber main body 101 b in the working chamber 102. When the pressure equalizing valve 107 b is opened, the discharge valve 112 b is opened and the gas is sucked from the excluding portion 113, so the inert gas introduced into the working chamber 102 by the second introducing portion 105 is the pressure equalizing path 107 a from the working chamber 102. Into the reaction chamber 101 and exhausted through the auxiliary exhaust passage 111b. That is, the inert gas is exhausted by the air flow from the working chamber 102 → the pressure equalizing path 107 a → the reaction chamber 101 → the exhaust path 111 (sub exhaust path 111 b). At this time, if the displacement of the sub-exhaust passage 111b is larger than the introduction amount of the second introduction part 105, the pressure of the working chamber 102 becomes smaller than the first pressure. The valve 112 d is adjusted to be equal to or less than the introduction amount of the second introduction unit 105.

FIG. 3 is an explanatory view for explaining the air flow when the reaction chamber 101 is opened. The reaction chamber 101 is released by releasing the seal by the O-ring 114 and the lifting device 115 raising the reaction chamber opening portion 101a. The movement of the reaction chamber opening portion 101 a for opening the reaction chamber 101 generates particles. In order to suppress the generation of particles, it is preferable that the reaction chamber open part 101a ascend at an equal velocity for vibration suppression, and after an acceleration of 0.25 [mm / s ² ], an equal velocity of 5 [mm / s] To rise. Immediately after the sealing is released, the rising of the reaction chamber opening 101a may be once stopped and the rising may be started again. The air flow 124 represents the flow of gas in the reaction chamber 101 and the working chamber 102 when the reaction chamber 101 is opened. That is, the inert gas introduced into the working chamber 102 from the introduction path 105a is exhausted by the air flow of the working chamber 102 → the opening of the reaction chamber main body 101 b → the reaction chamber main body 101 b → the exhaust path 111 (sub exhaust path 111b) Ru. Since the cross sectional area of the pressure equalizing path 107 a is sufficiently smaller than the opening area of the reaction chamber 101, the flow of inert gas from the working chamber 102 to the reaction chamber 101 passes through the pressure equalizing path 107 a before the reaction chamber 101 is opened. The air flow is naturally switched to the air flow passing through the opening of the reaction chamber main body 101b. Therefore, particles generated by vibration due to the movement of the reaction chamber open portion 101 a are carried to the exhaust portion 104 by the air flow 124 and discharged, and the diffusion of the particles is suppressed.

Next, a method of forming a thin film using the vapor deposition apparatus 100 will be described. When producing a thin film, the reaction chamber 101 is evacuated of gas and the pressure is maintained in a reduced pressure environment (about 10 to 60 [kPa]). Therefore, first, the main exhaust valve 112a is opened, and the vacuum pump 123 exhausts gas of 450 [L / min]. When the reaction chamber 101 is in a reduced pressure environment, the first introduction unit 103 introduces a reaction gas. At this time, the substrate disposed in the substrate holder 118 is heated to a predetermined temperature by the heater 120, and is rotated together with the susceptor 117 by the rotational drive shaft 119. The introduced reaction gas causes a gas phase reaction on the heated substrate to form a thin film. As the substrate, a semiconductor substrate, a wafer, a glass substrate, a sapphire substrate or the like is used. For example, when trimethylgallium (TMG) and ammonia (NH ₃ ) are introduced as reaction gases and vapor-phase grown, gallium nitride (GaN) is formed on the substrate. After the thin film is formed, the introduction of the reaction gas is stopped. However, since the reaction gas remains in the reaction chamber 101, the vacuum pump 123 exhausts the reaction gas in the reaction chamber 101 via the main exhaust path 111a. The exhaust of the reaction gas is performed until the pressure in the reaction chamber 101 becomes sufficiently small, and the pressure in the reaction chamber 101 at this time is, for example, 1.0 × 10 ⁻² [kPa].

Next, based on FIG. 4, a reaction chamber opening method until the reaction chamber 101 is opened in order to take out the processed substrate from the reaction chamber 101 whose pressure is reduced by evacuating the reaction gas will be described. First, the first introducing unit 103 starts introducing an inert gas into the reaction chamber 101 to pressurize the pressure of the reaction chamber 101 (step S101). At this time, the exhaust unit 104 may not exhaust the gas from the reaction chamber 101, but may exhaust the exhaust gas with an exhaust amount smaller than the introduction amount of the inert gas. By introducing an inert gas while exhausting, the pressure of the air flow can be minimized and the pressure can be increased while suppressing the diffusion of particles. Here, the opening degree of the main exhaust valve 112a is adjusted to The exhaust gas is exhausted at a displacement smaller than the introduction amount of the inert gas through the exhaust passage 111a. The introduction of the inert gas is performed until the pressure in the reaction chamber 101 becomes substantially equal to the pressure in the working chamber 102. Set the pressure differential _{P 1} of the reaction chamber 101 and the working chamber 102 at this time in advance, the pressure difference between the reaction chamber 101 and the working chamber 102 continues to introduction of the inert gas until the _{P 1} or less (NO in step S102) . The control unit 110 determines the pressure difference from the detection values of the pressure detection unit 108 and the pressure detection unit 109. Further, the control unit 110 may monitor the pressure difference between the detection value of the pressure detection unit 108 and the first pressure or the second pressure. Here, the pressure of the working chamber 102 is adjusted by the pressure adjustment unit 106 to a range of 101.3 [kPa] (atmospheric pressure) to 101.6 [kPa], and the pressure detection unit 108 detects 100 [kPa]. Introduce inert gas.

When the pressure difference between the reaction chamber 101 and the working chamber 102 is _{P 1} or less (YES at step S102), and stopping the introduction of inert gas (step S103). When the inert gas is exhausted through the main exhaust passage 111a simultaneously with the introduction of the inert gas in step S101, the main exhaust valve 112a is closed simultaneously with the stop of the inert gas introduction, and the exhaust of the inert gas is also stopped. . Here, if setting the P ₁ to 0 [kPa], even if stopping the introduction of inert gas when the detected value of the pressure detection unit 108 and the pressure detection unit 109 is equal, the pressure detecting unit 108 and the pressure detecting portion The variation of the characteristic value of 109 causes a pressure difference. Further, the control unit 110 receives detection signals from the pressure detection unit 108 and the pressure detection unit 109, and when the pressure difference between the reaction chamber 101 and the working chamber 102 becomes zero, the first gas supply unit 103b and the main exhaust Even when the control signal for performing introduction stop and exhaust stop is transmitted to the valve 112a, the timing at which the first gas supply unit 103b receives the control signal and stops the introduction of the inert gas, and the main exhaust valve 112a performs the control The timing at which the signal is received and the inert gas exhaust is stopped is shifted due to the difference in response or the like, resulting in a pressure difference. Therefore, when the reaction chamber 101 is opened at this stage, the pressure difference between the reaction chamber 101 and the working chamber 102 generates an impact or vibration, and this impact or vibration generates particles. Furthermore, while the pressure in the reaction chamber 101 is constant when the introduction and exhaust of the inert gas is stopped, the pressure in the working chamber 102 fluctuates in the range from the first pressure to the second pressure. The pressure difference also occurs between the reaction chamber 101 and the working chamber 102 depending on the timing of opening the chamber.

Therefore, in a state where the pressure difference between the reaction chamber 101 and the working chamber 102 and the _{P 1} or less, open the exhaust valve 112b opens the pressure equalizing valve 107 b, communicating the working chamber 102 and reaction chamber 101 (step S104). At this time, the discharge valve 112b and the pressure equalization valve 107b may be simultaneously opened, but the discharge valve 112b may be opened earlier than the pressure equalization valve 107b. By opening the pressure equalizing valve 107b and connecting the reaction chamber 101 and the working chamber 102 via the pressure equalizing path 107a, the pressures in the reaction chamber 101 and the working chamber 102 become equal. Further, particles are generated due to impact or vibration due to a pressure difference between the reaction chamber 101 and the working chamber 102 when the pressure equalizing valve 107 b is opened. Therefore, it occurs when the pressure equalization valve 107b is opened by simultaneously opening the pressure equalization valve 107b or opening the discharge valve 112b before opening the pressure equalization valve 107b and opening the pressure equalization valve 107b while exhausting the inert gas from the reaction chamber 101. It is possible to suppress the diffusion of the particles into the reaction chamber 101 and the working chamber 102 in order to discharge the particles.

The pressure equalizing valve 107b is opened, and after a predetermined time has elapsed, the reaction chamber 101 is opened (step S105). Since the pressure in the reaction chamber 101 is equal to the pressure in the working chamber 102 by communicating the reaction chamber 101 with the working chamber 102 for a predetermined time, vibration, impact, and the like at the moment of opening the reaction chamber 101 due to the pressure difference. Turbulence generation can be minimized and particle generation can be suppressed. However, since particles are also generated by the operation of the reaction chamber opening portion 101a for opening the reaction chamber 101, the reaction chamber 101 is opened in a state where gas exhaust is continued after step S104, and the generated particles are discharged.

Thus, the process for opening the reaction chamber 101 is completed. In addition, since particles are generated also when taking out a substrate from which thin film has been generated from the reaction chamber 101 or at the time of maintenance of the vapor deposition apparatus 100, gas exhaust is continued even after the reaction chamber 101 is opened. It is preferable to discharge the

Since the inner diameter of the pressure equalizing path 107a in this embodiment is sufficiently smaller than the opening area of the reaction chamber main body 101b, when the reaction chamber 101 is opened, the air flow passing through the pressure equalizing path 107a flows to the air flow passing through the opening of the reaction chamber 101. However, the air pressure may be switched by closing the pressure equalizing valve 107b at the same time as opening the reaction chamber 101 in step S105.

The exhaust passage 111 of this embodiment is branched into a plurality of paths having different flow rates, and a plurality of exhaust valves 112 are provided. However, fine flow control can be performed with one exhaust valve 112, and the flow rate in each process If it is possible to reliably switch, the exhaust passage 111 may not be branched into a plurality of paths, and one exhaust valve 112 may be provided. In addition, if the opening and closing of the sub exhaust path 111b and the flow control can be simultaneously performed by the discharge valve 112b, the flow control valve 112d may be omitted. Furthermore, various valves provided in the vapor deposition apparatus 100 may be mass flow controllers.

As described above, this embodiment suppresses the diffusion of particles generated when the reaction chamber 101 and the working chamber 102 communicate with each other by exhausting through the sub exhaust path 111 b when the pressure equalizing valve 107 b is opened. be able to. In addition, by connecting the reaction chamber 101 and the working chamber 102 and equalizing the pressure, the reaction chamber 101 is opened to suppress generation of particles, and when the reaction chamber 101 is opened, the sub exhaust path 111b is used. By exhausting through the space, it is possible to suppress the diffusion of particles generated by the movement of the reaction chamber opening portion 101a.

(Example 2)
Next, a second embodiment of the present invention will be described based on FIG. Here, since the structure of the vapor phase growth apparatus is the same as that of the first embodiment, the description will be omitted.

FIG. 5 is a flow chart for explaining the reaction chamber opening method of the vapor phase growth apparatus of the second embodiment. Here, since the steps up to step S104 are the same as in the first embodiment, the description will be omitted. By opening the discharge valve 112b in step S104 and then opening the pressure equalization valve 107b, it is possible to discharge particles generated when the pressure equalization valve 107b is opened. Here, by reducing the flow rate of the pressure equalizing path 107a, the generation of turbulent flow can be suppressed, and the generation of particles due to the turbulent flow can be suppressed to connect the reaction chamber 101 and the working chamber 102. When the flow rate of the sub exhaust path 111b is set larger than the flow rate of the pressure equalizing path 107a by the valve 112d, when the discharge valve 112b is opened in step S104 and the exhaust from the sub exhaust path 111b is continued, the pressure of the reaction chamber 101 is It becomes smaller than the pressure of the work room 102. Therefore, after the pressure equalization valve 107b is opened and a predetermined time has elapsed, particles generated when the pressure equalization valve 107b is opened are sufficiently discharged and then the discharge valve 112b is closed (S205). After the discharge valve 112 b is closed and a predetermined time has elapsed, the pressure in the reaction chamber 101 and the pressure in the working chamber 102 become equal, and then the reaction chamber 101 is opened (S 206). Immediately after the reaction chamber 101 is opened, the discharge valve 112b is opened again (S207). Further, as in the first embodiment, at the same time as opening the reaction chamber 101 in step S206, the pressure equalizing valve 107b may be closed to switch the air flow.

In this embodiment, the pressure equalizing valve 107b is opened and then the discharge valve 112b is closed, and the reaction chamber 101 is opened after a predetermined time elapses, so that generation of particles when the pressure equalizing valve 107b is opened is suppressed. Even when the gas flow rate of 107 a is reduced, the pressures in the reaction chamber 101 and the working chamber 102 can be equalized when the reaction chamber 101 is opened. Further, by opening the discharge valve 112b again immediately after opening the reaction chamber 101, it is possible to discharge particles generated by the movement of the reaction chamber opening part 101a when the reaction chamber 101 is opened.

(Example 3)
Next, a third embodiment of the present invention will be described based on FIG. Here, since the structure of the vapor phase growth apparatus is the same as that of the first embodiment, the description will be omitted, and only the portions different from the first and second embodiments will be described.

FIG. 6 is an explanatory view for explaining the flow of the inert gas when the reaction chamber 101 is opened. In the present embodiment, when the reaction chamber 101 is opened, an inert gas is introduced from the introduction path 103a. That is, in step S105 of the first embodiment or step S206 of the second embodiment, at the same time as the reaction chamber 101 is opened, the first introduction portion 103 introduces an inert gas into the reaction chamber opening portion 101a. The introduced inert gas is uniformly supplied from the shower plate 116 to the opening of the reaction chamber main body 101 b, and a down air stream 301 is generated to the exhaust unit 104. The inert gas introduced by the first introduction unit 103 is exhausted from the exhaust unit 104 together with the inert gas introduced by the second introduction unit 105. The particles generated by the movement of the reaction chamber opening portion 101 a for opening the reaction chamber 101 can be carried to the exhaust portion 104 by the down air flow 301 and effectively discharged.

At this time, if the amount of the inert gas exhausted from the reaction chamber 101, that is, the exhaust amount of the sub exhaust passage 111b, is smaller than the introduction amount of the inert gas introduced into the reaction chamber 101 by the first introduction part 103, The inert gas introduced by the introducing unit 103 flows from the reaction chamber opening unit 101 a to the working chamber 102, and the particles flow out to the working chamber 102, which is not preferable. Further, the sum of the amount of inert gas introduced into the reaction chamber 101 by the first introducing unit 103 and the amount of inert gas introduced into the working chamber 102 by the first introducing unit 103 is larger than the sum of the amount of inert gas Then, the pressure in the working chamber 102 is less than the first pressure, which is not preferable. Therefore, the exhaust amount of the sub-exhaust passage 111 b is equal to or more than the introduction amount of the first introduction part 103 and not more than the sum of the introduction amount of the first introduction part 103 and the introduction amount of the second introduction part 105.

The flow rate of the auxiliary exhaust passage 111b may be preset by the flow rate adjustment valve 112d, but the flow rate of the auxiliary exhaust passage 111b may be adjusted by the flow rate adjustment valve 112d at the same time as the first introduction part 103 introduces inert gas. Good. For example, the flow rate of the secondary exhaust passage 111b is adjusted to be equal to or less than the introduction amount of the second introduction unit 105 before the first introduction unit 103 starts the introduction of the inert gas into the reaction chamber 101, and the first introduction unit 103 is inactive. When gas introduction is started, it may be adjusted to be equal to or less than the sum of the introduction amount of the first introduction unit 103 and the introduction amount of the second introduction unit 105.

(Example 4)
Next, a fourth embodiment of the present invention will be described based on FIGS. FIG. 7 is a view for explaining a vapor phase growth apparatus according to a fourth embodiment. Here, the same reference numerals are given to the same components as in the first to third embodiments, and the description will be omitted. The vapor deposition apparatus 400 includes the second introducing unit 105 connected to the working chamber 102 and the working chamber 102 from the vapor deposition apparatus 100 of the first embodiment, the pressure adjusting unit 106, the pressure equalizing unit 107, and the pressure detecting unit 109. The reaction chamber 101 is not accommodated in the working chamber, but is disposed in the atmosphere. The pressure equalizing portion 401 includes a pressure equalizing passage 401 a connected at one end to the reaction chamber 101 and open to the atmosphere at the other end, and a pressure equalizing valve 401 b provided in the pressure equalizing passage 401 a. The control unit 402 receives a detection signal from the pressure detection unit 108, and controls the first gas supply unit 103b, the exhaust valve 112, and the pressure equalization valve 401b based on the pressure of the reaction chamber 101.

FIG. 8 is a flow chart for explaining the reaction chamber opening method of the vapor phase growth apparatus of the fourth embodiment. Here, as in the first to third embodiments, after film formation, the reaction gas is exhausted and introduction of an inert gas into the reaction chamber 101 in a reduced pressure state is started (step S401). At this time, the exhaust may be performed with an exhaust amount smaller than the introduction amount of the inert gas. The introduction of the inert gas into the reaction chamber 101 is performed until the pressure in the reaction chamber 101 becomes substantially equal to the pressure outside the reaction chamber 101, that is, the atmospheric pressure. Set the reaction chamber 101 and out of the pressure difference between _{P 2} at this time in advance, the pressure difference between the reaction chamber 101 and out continues to introduction of the inert gas until the _{P 2} less (NO at step S402). The control unit 110 determines the pressure difference from the detection value of the pressure detection unit 108 and the atmospheric pressure (101.3 [kPa]). Here, as in the first embodiment, the inert gas is introduced until the pressure detection unit 108 detects 100 [kPa].

When the pressure difference between the inside and the outside of the reaction chamber 101 becomes P ₂ or less (YES in step S 402), the introduction of the inert gas is stopped (step S 403). When the inert gas is exhausted simultaneously with the introduction of the inert gas in step S101, the inert gas introduction is stopped and the inert gas exhaust is also stopped simultaneously. Then, the pressure difference inside and outside the reaction chamber 101 while the _{P 2} below opens the exhaust valve 112b opens the pressure equalizing valve 401b, communicating inside and outside of the reaction chamber 101 (step S404). At this time, the discharge valve 112b and the pressure equalization valve 401b may be simultaneously opened, but the discharge valve 112b may be opened earlier than the pressure equalization valve 401b. By opening the pressure equalizing valve 401 b and opening the reaction chamber 101 to the atmosphere via the pressure equalizing path 401 a, the pressure inside and outside the reaction chamber 101 becomes equal. At the same time as opening pressure equalizing valve 401b or before opening pressure equalizing valve 401a, exhaust valve 112b is exhausted to exhaust the gas, so that particles generated when pressure equalizing valve 401b is opened can be discharged from the inside of reaction chamber 101. Alternatively, the particles can be prevented from diffusing to the outside. The pressure equalizing valve 401b is opened, and after a predetermined time has elapsed, the reaction chamber 101 is opened (step S405). Since the pressure inside and outside the reaction chamber 101 is equal, it is possible to minimize the occurrence of vibration, impact and turbulence at the moment of opening the reaction chamber 101, and to suppress the generation of particles. However, since particles are also generated by the operation of the reaction chamber opening portion 101a for opening the reaction chamber 101, the discharge valve 112b opened in step S404 is opened and the reaction chamber 101 is opened, and the generated particles are generated. Drain.

As in the second embodiment, after the pressure equalizing valve 401b is opened in step S404, the discharge valve 112 is closed before the reaction chamber 101 is opened in step S405, and after the reaction chamber 101 is opened in step S405, the discharge valve 112 is reopened. You may open it. Further, as in the third embodiment, the first introducing unit 103 may introduce an inert gas into the reaction chamber 101 when the reaction chamber 101 is opened in step S405. At this time, in order to prevent the inert gas introduced by the first introduction unit 103 from flowing out of the reaction chamber 101 to the outside of the reaction chamber 101, the exhaust amount of the inert gas in the exhaust unit 104 is made equal to or more than the introduction amount of the first introduction unit 103. You may adjust.

As described above, in the present embodiment, the diffusion of particles generated when the inside and the outside of the reaction chamber 101 are communicated can be suppressed. In addition, by connecting the inside and outside of the reaction chamber 101 and equalizing the pressure and then opening the reaction chamber 101, generation of particles is suppressed, and when the reaction chamber 101 is opened, movement of the reaction chamber opening portion 101a is performed. Diffusion of generated particles can be suppressed.

The reaction chamber opening method and the vapor phase growth apparatus according to the present invention are not limited to the above-described embodiments, and various modifications can be made within the scope of the claims, which are disclosed in different embodiments. Embodiments obtained by appropriately combining technical means are also included in the technical scope of the present invention. For example, although the above embodiment has described the shower type vapor phase growth apparatus for supplying the reaction gas to the reaction chamber 101 via the shower plate 116, the introduction path 103a is disposed along the central axis of the reaction chamber 101. The present invention can be similarly applied to a central radiation type vapor phase growth apparatus in which a reaction gas is introduced radially from the central portion to the outer peripheral portion of 101. Further, although the low pressure CVD apparatus has been described in the above embodiment, the same can be applied to a normal pressure or pressurized CVD apparatus, and can also be applied to a plasma CVD apparatus or the like.

According to the present invention, since the reaction chamber can be opened by suppressing generation and diffusion of particles, deterioration of the characteristics of the compound semiconductor crystal due to the adhesion of particles can be prevented, and the reaction chamber and the working chamber can be By keeping it clean, the maintenance process can be shortened.

DESCRIPTION OF SYMBOLS 100 vapor phase growth apparatus, 101 reaction chamber, 101a reaction chamber opening part, 101b reaction chamber main body, 102 working chamber, 103 1st introduction part, 103a introduction path, 103b 1st gas supply part, 104 exhaust part, 105 2nd introduction Section, 105a introduction path, 105b second gas supply section, 106 pressure adjusting section, 107 pressure equalizing section, 107a pressure equalizing path, 107b pressure equalizing valve, 108, 109 pressure detecting section, 110 control section, 111 exhaust path, 111a main exhaust Path, 111b auxiliary exhaust path, 111c overpressure protection path, 112 exhaust valve, 112a main exhaust valve, 112b exhaust valve, 112c overpressure protection valve, 112d flow control valve, 113 exclusion portion.

Claims

A reaction chamber opening method for opening a reaction chamber (101) accommodated in a working chamber (102), comprising:
Introducing a gas into the reaction chamber (101) to increase the pressure in the reaction chamber (101) (S101);
The pressure in the reaction chamber (101) is increased until the pressure difference between the reaction chamber (101) and the working chamber (102) becomes equal to or less than a predetermined value (P 1 ), and then the gas is exhausted from the reaction chamber (101). Connecting the reaction chamber (101) and the working chamber (102) with each other (S104);
And a step (S105) of opening the reaction chamber (101) after the reaction chamber (101) and the working chamber (102) are communicated with each other.
The step (S104) of communicating the reaction chamber (101) with the working chamber (102) while exhausting the gas from the reaction chamber (101) is performed by the reaction chamber (101) and the working chamber (102). The exhaust valve (112b) provided in the exhaust passage (111b) for exhausting the gas from the reaction chamber (101) when the pressure difference becomes equal to or less than the predetermined value (P 1 ) is opened, and the reaction chamber (101) The reaction chamber opening method according to claim 1, wherein a pressure equalization valve (107b) provided in a pressure equalization path (107a) for communicating with the working chamber (102) and equalizing pressure is opened.
After the pressure equalizing valve (107b) is opened, the discharge valve (112b) is closed before the reaction chamber (101) is opened (S205), and after the reaction chamber (101) is opened, the discharge valve (112b) 3. The method for opening a reaction chamber according to claim 2, further comprising the step of:) (S207).
The reaction chamber opening method according to claim 1, wherein the amount of gas exhausted from the reaction chamber (101) is adjusted based on the amount of gas introduced into the working chamber (102).
The method for opening a reaction chamber according to claim 1, wherein a gas is introduced to the reaction chamber (101) when the reaction chamber (101) is opened.
The amount of gas exhausted from the reaction chamber (101) is adjusted based on the amount of gas introduced into the reaction chamber (101) and the amount of gas introduced into the working chamber (102). The reaction chamber opening method as described in 5.
A method for opening a reaction chamber (101), comprising:
Introducing a gas into the reaction chamber (101) to increase the pressure in the reaction chamber (101) (S401);
After raising the pressure in the reaction chamber (101) until the pressure difference between the inside of the reaction chamber (101) and the outside of the reaction chamber (101) becomes equal to or less than a predetermined value (P 2 ), the inside of the reaction chamber (101) Communicating the inside of the reaction chamber (101) with the outside of the reaction chamber (101) while exhausting the gas from the chamber (S404);
A step (S405) of opening the reaction chamber (101) after the inside of the reaction chamber (101) is communicated with the outside of the reaction chamber (101) (S405).
The step (S404) of communicating the inside of the reaction chamber (101) with the outside of the reaction chamber (101) while exhausting the gas from the inside of the reaction chamber (101) comprises the inside of the reaction chamber (101) and the reaction chamber (101). 101) Open a discharge valve (112) provided in an exhaust passage (111) for exhausting the gas from inside the reaction chamber (101) when the pressure difference with the outside becomes equal to or less than a predetermined value (P 2 ) The pressure equalizing valve (401b) provided in the pressure equalizing path (401a) for bringing the inside of the reaction chamber (101) and the outside of the reaction chamber (101) into communication and equalizing the pressure is opened. How to open the reaction chamber.
A step of closing the discharge valve (112) after opening the pressure equalization valve (401b) and before opening the reaction chamber (101), and opening the discharge valve (112) after opening the reaction chamber (101) The method according to claim 8, further comprising the steps of:
The reaction chamber opening method according to claim 7, wherein a gas is introduced into the reaction chamber (101) when the reaction chamber (101) is opened.
The reaction chamber opening method according to claim 10, wherein the amount of gas exhausted from the reaction chamber (101) is adjusted based on the amount of gas introduced into the reaction chamber (101).
A vapor phase growth apparatus (100) comprising a reaction chamber (101) accommodated in a work chamber (102), wherein
A pressure adjusting unit (106) for adjusting the pressure in the working chamber (102) from a first pressure to a second pressure;
A pressure equalizing portion (107) for communicating the reaction chamber (101) with the working chamber (102) to make the pressure in the reaction chamber (101) equal to the pressure in the working chamber (102);
An exhaust unit (104) for evacuating gas and discharging particles from the reaction chamber (101) when the reaction chamber (101) and the working chamber (102) are communicated with each other;
And an opening (115) for opening the reaction chamber (104).
Wherein the exhaust unit (104) is characterized by having a discharge valve the difference between the pressure and the first pressure of the reaction chamber (101) is opened when a predetermined value (P 1) below (112b) The vapor phase growth apparatus (100) according to Item 12.
The exhaust unit (104) further comprises a flow control valve (112d) for adjusting the amount of gas exhausted from the reaction chamber (101) based on the amount of gas introduced into the working chamber (102). The vapor deposition apparatus (100) according to claim 12, characterized in that:
The exhaust unit (104) adjusts the amount of gas exhausted from the reaction chamber (101) based on the amount of gas introduced into the reaction chamber (101) and the amount of gas introduced into the working chamber (102). The vapor deposition apparatus (100) according to claim 12, further comprising a flow control valve (112d).