JP2015146369A - Lid opening method of reactor of vapor phase growth apparatus and vapor phase growth apparatus - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a lid opening method of a reactor of a vapor phase growth apparatus and a vapor phase growth apparatus, which can inhibit adherence of a particle on a substrate when the lid is opened.SOLUTION: A lid opening method comprises the steps of: introducing only an inert gas from an introduction path 15 to a reactor 11 while discharging a gas in the reactor from an exhaust path 16 after forming a thin film; decreasing a temperature in the reactor; gradually increasing an aperture of an exhaust valve when the temperature inside the reactor decreases to a preset temperature and decreasing pressure in the reactor; gradually decreasing the aperture of the exhaust valve when the pressure in the reactor decreases to a first preset pressure and increasing pressure in the reactor; gradually increasing the aperture of the exhaust valve when the pressure in the reactor increases to a second preset pressure and decreasing the pressure in the reactor; gradually decreasing the aperture of the exhaust valve when the pressure in the reactor decreases to the first preset pressure and increasing the pressure in the reactor; and closing an introduction valve and the exhaust valve when the pressure in the reactor increases to the second preset pressure and opening a lid of the reactor after the valve closing, in which increase and decrease of the pressure in the reactor is repeated at least twice.

Description

  TECHNICAL FIELD The present invention relates to a method for opening a reactor in a vapor phase growth apparatus and a vapor phase growth apparatus, and more particularly, to perform a method for opening a reaction furnace in a vapor phase growth apparatus that reduces the generation of particles and the method for opening the lid. This invention relates to a vapor phase growth apparatus.

  In recent years, as the demand for light emitting devices such as light emitting diodes (LEDs) and laser diodes (LD) and electronic devices such as high electron mobility transistors (HEMT) increases, a vapor phase growth apparatus is used as a method for manufacturing these devices. A method is generally used in which a compound semiconductor film is formed on a growth substrate. In a vapor phase growth apparatus, a thin film is formed by heating a substrate and supplying a raw material gas. However, not all of the raw material gas contributes to the formation of the thin film. It adheres as a by-product to walls, members around the installed substrate, and the like. Part of this by-product adheres with very weak force, and when it is peeled off by pressure fluctuation or gas flow force or vibration, it becomes fine particles and floats in the reactor, and it is attached to the substrate after forming the thin film. Adhere to. The area where the particles are attached becomes a defective part, which leads to a decrease in yield and productivity.

  The timing at which the particles adhere varies, but the risk is high when the reactor lid is opened to remove the substrate after the thin film is formed. To reduce this effect as much as possible, the reaction chamber and the load lock chamber should be separated. By connecting and equalizing pressure, a method of suppressing particles when the substrate is taken out (see Patent Document 1) and a shock wave and convection generated when the gate valve is opened to prevent the particles from rolling up are suppressed. A method (see Patent Document 2) is known.

  Furthermore, as a method of improving the methods of Patent Documents 1 and 2, while exhausting gas from the reaction chamber, the pressure in the reaction chamber and the working chamber is equalized, and when the reaction chamber is opened, the gas is introduced into the reaction chamber from the introduction path. There is known a method of introducing (see Patent Document 3).

JP-A-6-177060 JP 2006-128341 A Japanese Patent No. 5079902

  However, as in the method described in Patent Document 3, it is not easy to actually equalize the pressure in the reaction chamber and the working chamber while exhausting from the exhaust valve. When controlling the reaction chamber near atmospheric pressure, if the amount of gas introduced is small relative to the size of the reaction chamber, the opening of the exhaust valve must be very close to 0%, and particles are discharged. The effect will fade. On the other hand, if a large amount of gas is introduced, the opening of the exhaust valve will also increase, and the effect of discharging particles will increase, but the pressure fluctuation in the reaction chamber will increase even with slight fluctuations in the flow rate, so the pressure will remain constant. In order to keep it, the opening degree of the discharge valve must be adjusted by a control method such as PID control. In addition, when the reaction chamber and the work chamber are in communication, part of the atmospheric gas in the work chamber is exhausted from the exhaust valve together, and particles in the work chamber enter the reaction chamber and particles on the substrate. There is a risk of increasing Also, since the introduction valve for introducing the inert gas into the reaction chamber is opened after sufficiently reducing the pressure in the reaction chamber, the pressure in the reaction chamber is very low compared to the pressure of the inert gas. A high-pressure shock at the moment of introduction is unavoidable, and there is a risk that particles in the reaction chamber roll up and adhere to the substrate.

  In view of the above, the present invention aims to solve the above problems and provide a method for opening a reactor and a vapor phase growth apparatus for a vapor phase growth apparatus that can reliably suppress adhesion of particles onto a substrate when the lid is opened. Yes.

In order to achieve the above object, the method of opening a reactor of a vapor phase growth apparatus according to the present invention contains a susceptor on which a substrate can be placed, introduces a source gas, and forms a thin film on the substrate surface by vapor phase reaction. A reaction furnace, an introduction path for introducing gas into the reaction furnace, an introduction valve provided in the introduction path,
A gas phase comprising an exhaust passage for exhausting the gas in the reactor, an exhaust valve provided in the exhaust passage, a pump for decompressing the reactor, and a glove box for opening and closing the lid of the reactor A method of opening a reaction furnace of a growth apparatus, wherein after a thin film is formed, only the inert gas is introduced into the reaction furnace from the introduction path while the gas in the reaction furnace is exhausted from the exhaust path by the pump. A temperature lowering step for lowering the temperature in the reaction furnace, and an initial pressure-lowering step for gradually increasing the opening of the exhaust valve and lowering the pressure in the reaction furnace when the temperature in the reaction furnace decreases to a set temperature by the temperature lowering step And when the pressure in the reactor is reduced to the first set pressure by the initial pressure reducing step, the opening degree of the exhaust valve is gradually reduced to increase the pressure in the reactor, and the reaction by the pressure increasing step The pressure in the furnace is the second setting When the pressure increases, the opening degree of the exhaust valve is gradually increased to lower the pressure in the reaction furnace, and when the pressure in the reaction furnace is lowered to the first set pressure by the pressure reduction process, The final pressurization step in which the opening degree is gradually reduced and the pressure in the reactor is increased, and when the pressure in the reactor rises to the second set pressure by the final pressurization step, the introduction valve and the exhaust valve are closed And a step of opening the lid of the reactor after the valve closing step, wherein the step of increasing pressure and the step of decreasing pressure are repeated at least twice.

  Moreover, it is preferable to perform the pressure equalization process which makes the pressure in the reaction furnace and the pressure in the glove box uniform before the opening process.

  Furthermore, the vapor phase growth apparatus of the present invention accommodates a susceptor on which a substrate can be placed, introduces a source gas, and forms a thin film on the substrate surface by a vapor phase reaction, and introduces the gas into the reaction furnace. A first introduction passage, a first introduction valve provided in the first introduction passage, a first exhaust passage for exhausting gas in the reaction furnace, a first exhaust valve provided in the first exhaust passage, and a reaction In a vapor phase growth apparatus comprising a pump for depressurizing the inside of the furnace and a glove box for opening and closing the lid of the reaction furnace, a pressure equalizing path communicating between the inside of the glove box and the inside of the reaction furnace, A pressure equalizing valve provided in the pressure passage, a second introduction passage for introducing an inert gas into the glove box, a second introduction valve provided in the second introduction passage, and exhausting the gas in the glove box Second exhaust path and second exhaust valve provided in the second exhaust path A first pressure gauge for measuring the pressure in the reactor, a second pressure gauge for measuring the pressure in the glove box, and a differential pressure gauge for measuring a pressure difference inside and outside the glove box, , And either or both of a fan filter unit and a downflow system are provided in the glove box.

  According to the method for opening the reactor of the vapor phase growth apparatus of the present invention, the number of particles adhering to the substrate is obtained by repeating the pressure increasing step and the pressure decreasing step a plurality of times while introducing an inert gas into the reaction furnace. The gas in the reaction furnace can be replaced with an inert gas and the lid of the reaction furnace can be safely opened while reliably suppressing the above.

  Further, by making the pressure in the reaction furnace and the pressure in the glove box uniform before the lid opening step, it is possible to reliably prevent particles from adhering to the substrate when the lid is opened.

  In addition, according to the vapor phase growth apparatus of the present invention, by providing either or both of the fan filter unit and the downflow system in the glove box, particles entering the glove box from inside the reaction furnace Returning to the reactor again can be reliably prevented.

It is explanatory drawing which shows the 1st form example of the vapor phase growth apparatus which can implement the lid opening method of the reactor of the vapor phase growth apparatus of this invention. It is explanatory drawing which shows the 2nd form example of the vapor phase growth apparatus which can implement the lid opening method of the reactor of the vapor phase growth apparatus of this invention. It is a figure which shows the number of the particles on the board | substrate after the thin film growth by the lid opening method of the reactor of the vapor phase growth apparatus of this invention, and the conventional lid opening method.

  FIG. 1 shows a first embodiment of a vapor phase growth apparatus capable of carrying out a method for opening a reactor of a vapor phase growth apparatus according to the present invention. The vapor phase growth apparatus 10 includes a reaction furnace 11 formed from a reaction furnace main body 11a having an opening at the top and a lid 11b that closes the opening, and a glove box 12 that opens and closes the lid 11b. . The entire reaction furnace 11 need not be accommodated in the glove box 12, and the lid 11 b and the opening of the reaction furnace main body 11 a may be accommodated in the glove box 12.

  A susceptor 14 on which a substrate 13 can be placed is accommodated inside the reaction furnace main body 11a. In addition, a first introduction path 15 for introducing a gas such as a raw material gas and an inert gas into the reaction furnace 11 and a first exhaust path 16 for exhausting the gas in the reaction furnace 11 are respectively provided in the reaction furnace 11. Communicate.

  The first introduction path 15 is provided with a first introduction valve 17 for introducing, stopping, or controlling the flow of various gases. A plurality of first introduction valves 17 may be provided according to various gases.

  The first exhaust passage 16 is provided with a first exhaust valve 18 capable of PID control, a pump 19 for depressurizing the inside of the reactor 11, and a filter 20 for collecting particles contained in the exhausted gas. ing.

  Further, the vapor phase growth apparatus 10 has a pressure equalizing path 21 that communicates the inside of the reaction furnace 11 and the inside of the glove box 12, and the pressure equalizing path 21 is provided with a pressure equalizing valve 22. The piping that forms the pressure equalizing path 21 has a diameter of ¼ inch or less, and is sufficiently thinner than the size inside the reactor 11.

  The vapor phase growth apparatus 10 includes a first pressure gauge 23 that is an absolute pressure gauge for measuring the pressure in the reaction furnace 11 and a second pressure gauge that is used for measuring the pressure in the glove box 12. A pressure gauge 24 and a differential pressure gauge 25 for measuring a pressure difference between the pressure in the glove box 12 and the external atmospheric pressure are provided.

  The glove box 11 has a second introduction path 26 for introducing an inert gas into the glove box 11 and a second exhaust for exhausting the gas in the glove box 11 to a scrubber (not shown) or a detoxifying device (not shown). The road 27 is in communication. The second introduction passage 26 has a second introduction valve 28 for introducing, stopping or controlling the flow rate of the inert gas, and the second exhaust passage 27 has a second exhaust valve 29 whose opening degree can be adjusted by PID control. Is provided.

  The pressure difference inside and outside the glove box 12 is monitored by the differential pressure gauge 25 so that the pressure inside the glove box 12 is adjusted within a predetermined range that is slightly higher than the outside air pressure. When it falls below the lower limit value of the predetermined range, the second introduction valve 28 is opened, the inert gas is introduced from the second introduction passage 26, and when it rises above the upper limit value of the predetermined range, (2) An automatic control system that performs an operation of exhausting by increasing the opening of the exhaust valve 29 is used.

  In addition, a fan filter unit 30 that collects floating particles is provided in the glove box 12 in order to prevent particles that have entered the glove box 12 from the reaction furnace 11 from returning to the reaction furnace 11 again. Yes.

In order to form a thin film on the substrate 13 using the vapor phase growth apparatus 10 described above, a raw material gas is supplied from the first introduction path 15 while the substrate 13 is heated via the susceptor 14 to grow the thin film. The substrate temperature during thin film growth is changed from 400 ° C. to 1400 ° C. depending on the film type. The pressure in the reaction furnace 11 at the time of thin film growth can be controlled to be equal to or lower than the atmospheric pressure, and can be changed depending on the film type. The source gas is composed of organic metal gas such as TMG, TEG, TMA, TMI, Cp ₂ Mg corresponding to the film type to be grown, carrier gas such as hydrogen or nitrogen accompanying these, ammonia as N source, SiH ₄ and a dopant such as Si ₂ H ₆ or B ₂ H ₆ .

  Next, a method of opening the lid 11b of the reaction furnace 11 in order to take out the substrate 13 after forming the thin film will be described.

  After the thin film is formed, first, the supply of the raw material gas from the first introduction path 15 is stopped, and the inert gas is supplied from the first introduction path 15 to lower the temperature of the substrate 13 (the temperature lowering step of the present invention). During this time, the first exhaust valve 18 continues to exhaust with the air opened to some extent.

  After that, when the temperature drops to a preset substrate extraction temperature (the substrate temperature is 100 ° C. or lower if manually extracted, and the substrate temperature is 500 ° C. or lower if automatically extracted), the inert gas is introduced from the first introduction path 15. While the above is continued, the opening degree of the first exhaust valve 18 is gradually increased, and the pressure in the reaction furnace 11 is lowered (initial pressure reducing step of the present invention).

  Then, when the pressure in the reaction furnace 11 is reduced to a preset pressure (first set pressure of the present invention), for example, 5 kPa, the opening degree of the first exhaust valve 18 is gradually decreased, The pressure is increased (pressure increase process of the present invention).

  At this time, the first exhaust valve 18 is PID-controlled so as to linearly increase the pressure in the reactor 11 during the set time, and the opening degree of the first exhaust valve 18 is 0 during this process. % (Completely closed state) is set.

  When the pressure in the reaction furnace 11 rises to a preset pressure (second set pressure of the present invention), for example, 100 kPa, the opening of the first exhaust valve 18 is gradually increased, and the pressure in the reaction furnace 11 is increased. It is lowered (step-down step of the present invention).

  This boosting step and the step-down step are repeated a plurality of times, for example, twice. During these steps, the inert gas that is always introduced from the first introduction passage 15 is exhausted from the second exhaust passage 16, so that particles floating in the reaction furnace 11 are collected by the filter 20.

  When the pressure in the reaction furnace 11 is reduced to the first set pressure by the second step-down process, the opening of the first exhaust valve 18 is gradually reduced to increase the pressure in the reaction furnace 11 (this The final pressurization step of the invention).

  Next, when the pressure in the reaction furnace 11 rises to the second set pressure, the first introduction valve 17 and the first exhaust valve 18 are closed (the valve closing process of the present invention).

  After the first introduction valve 17 and the first exhaust valve 18 are closed, the pressure in the reaction furnace 11 and the pressure in the glove box 12 are made uniform (equalization step of the present invention). When the pressure in the reaction furnace 11 is lower than the pressure in the glove box 12, the first introduction valve 17 is opened, a small amount of inert gas is supplied, and the same pressure as the pressure in the glove box 12 at a moderate speed. Raise to. Thereafter, when the pressure becomes the same, the first introduction valve 17 is closed, the pressure equalizing valve 22 is opened, and the reaction furnace 11 and the glove box 12 are communicated with each other through the pressure equalizing path 21. When the pressure in the reaction furnace 11 is higher than the pressure in the glove box 12, the pressure equalization valve 22 is opened, and the gas in the reaction furnace 11 flows out to the glove box 12 side via the pressure equalization path 21. And make the pressure uniform. Here, the particles flowing out from the reactor 11 to the glove box 12 through the pressure equalizing path 21 are collected by the fan filter unit 30.

  After equalizing the pressure in the reaction furnace 11 and the pressure in the glove box 12, the lid 11b of the reaction furnace 11 is gently opened by the work from the glove box 12 (the opening process of the present invention).

  Through such a series of steps, the raw material gas can be removed from the reactor 11 and replaced with an inert gas, and particles in the reactor 11 can be prevented from adhering to the substrate 13 when the lid is opened. .

  FIG. 2 shows a second embodiment of the vapor phase growth apparatus capable of carrying out the lid opening method of the present invention. Components that are the same as those in the first embodiment are denoted by the same reference numerals. Detailed description thereof will be omitted.

  In the second embodiment, instead of the fan filter unit of the first embodiment, the downflow system 31 that collects particles by flowing an inert gas from the ceiling of the glove box 12 to the dust collecting portion on the floor surface is provided in the glove box 12. Provided. The downflow system 31 can prevent particles that have flowed out of the reactor 11 into the glove box 12 from returning to the reactor again.

<Example>
Using the vapor phase growth apparatus 10 shown in the first embodiment, the lid opening method of the present invention was performed, and the number of particles adhering to the substrate was measured. No maintenance is performed, and the thin film growth is continuously performed 20 times. In the state where a lot of dirt is adhered in the reaction furnace 11, the lid opening method of the present invention is performed 4 times, and particles having a size of 0.3 μm or more are obtained. Counted and compared. The result is shown in FIG.

  In addition, as a comparative example, the result of the conventional lid opening method is also shown in FIG. In the conventional lid opening method, first, after the temperature in the reaction furnace 11 is lowered to the substrate take-out temperature after the thin film is formed, the pressure in the reaction furnace 11 is set to atmospheric pressure, and the first introduction valve 17 and the first exhaust valve 18 is closed. At this time, when the pressure in the reaction furnace 11 is lower than the atmospheric pressure, the first exhaust valve 18 is closed, and an inert gas is introduced into the reaction furnace 11 from the first introduction path 15 to reach the atmospheric pressure. Then, the first introduction valve 17 is closed. Thereafter, the pump 19 is started with the first introduction valve 17 and the first exhaust valve 18 closed, and the first exhaust valve 18 is opened to sufficiently reduce the pressure in the reaction furnace 11. When the pressure is sufficiently reduced, the first exhaust valve 18 is closed, the first introduction valve 17 is opened, an inert gas is introduced into the reaction furnace 11 from the first introduction passage 15, and when the atmospheric pressure is again reached, 1 Close the introduction valve 17. Thereafter, the pressure equalizing valve 22 was opened, and the lid 11b was opened after 10 seconds had elapsed.

  As shown in FIG. 3, in the comparative example, a little less than 1000 particles are attached, whereas according to the opening method of the present invention, the number of attached particles is 200 to 300, and the number of attached particles is as follows. It turns out that there exists an effect which can suppress.

  Note that the vapor phase growth apparatus used in the present invention is not limited to each embodiment, and can be similarly applied to various vapor phase growth apparatuses such as a self-revolving vapor phase growth apparatus. Moreover, you may provide both the fan filter unit and the downflow system in the glove box. Furthermore, the number of repetitions of the step-up step and the step-down step may be two or more, and it is possible to automatically control by providing a predetermined number of times in advance.

  DESCRIPTION OF SYMBOLS 10 ... Vapor growth apparatus, 11 ... Reaction furnace, 11a ... Reaction furnace main body, 11b ... Cover, 12 ... Glove box, 13 ... Substrate, 14 ... Susceptor, 15 ... First introduction path, 16 ... First exhaust path, 17 DESCRIPTION OF SYMBOLS 1st introduction valve, 18 ... 1st exhaust valve, 19 ... Pump, 20 ... Filter, 21 ... Pressure equalization path, 22 ... Pressure equalization valve, 23 ... 1st pressure gauge, 24 ... 2nd pressure gauge, 25 ... Differential pressure gauge , 26 ... second introduction path, 27 ... second exhaust path, 28 ... second introduction valve, 29 ... second exhaust valve, 30 ... fan filter unit

Claims (3)

A reactor that houses a susceptor on which a substrate can be placed, introduces a source gas, and forms a thin film on the substrate surface by a gas phase reaction;
An introduction path for introducing gas into the reactor;
An introduction valve provided in the introduction path;
An exhaust passage for exhausting the gas in the reactor;
An exhaust valve provided in the exhaust passage and a pump for depressurizing the inside of the reaction furnace;
A glove box that opens and closes the lid of the reactor;
A method for opening a reactor of a vapor phase growth apparatus comprising:
After the thin film is formed, while the gas in the reaction furnace is exhausted from the exhaust passage by the pump, only a inert gas is introduced into the reaction furnace from the introduction passage, and the temperature lowering step to lower the temperature in the reaction furnace;
When the temperature in the reaction furnace is lowered to a set temperature by the temperature lowering step, an initial pressure reducing step for gradually increasing the opening degree of the exhaust valve and lowering the pressure in the reaction furnace;
When the pressure in the reaction furnace is reduced to the first set pressure by the initial pressure reduction process, the pressure increase process to gradually reduce the opening of the exhaust valve and increase the pressure in the reaction furnace;
When the pressure in the reaction furnace rises to a second set pressure by the pressure increasing step, the pressure reducing step to gradually increase the opening of the exhaust valve and reduce the pressure in the reaction furnace;
When the pressure in the reaction furnace is reduced to the first set pressure by the pressure reduction process, the final pressure increase process for gradually decreasing the opening of the exhaust valve and increasing the pressure in the reaction furnace;
A valve closing step of closing the introduction valve and the exhaust valve when the pressure in the reactor rises to a second set pressure by the final pressure raising step;
A lid opening step of opening the lid of the reactor after the valve closing step;
Including
A method for opening a reactor of a vapor phase growth apparatus, wherein the step of increasing pressure and the step of decreasing pressure are repeated at least twice.
The method for opening a reactor of a vapor phase growth apparatus according to claim 1, wherein a pressure equalizing step for making the pressure in the reactor and the pressure in the glove box uniform is performed before the opening step.
A reactor that houses a susceptor on which a substrate can be placed, introduces a source gas, and forms a thin film on the substrate surface by a gas phase reaction;
A first introduction path for introducing gas into the reactor;
A first introduction valve provided in the first introduction path;
A first exhaust path for exhausting the gas in the reaction furnace;
A first exhaust valve provided in the first exhaust passage and a pump for reducing the pressure in the reaction furnace;
A glove box that opens and closes the lid of the reactor;
In a vapor phase growth apparatus comprising:
A pressure equalization path communicating between the inside of the glove box and the inside of the reactor;
A pressure equalizing valve provided in the pressure equalizing path;
A second introduction path for introducing an inert gas into the glove box;
A second introduction valve provided in the second introduction path;
A second exhaust path for exhausting the gas in the glove box;
A second exhaust valve provided in the second exhaust path;
A first pressure gauge for measuring the pressure in the reactor;
A second pressure gauge for measuring the pressure in the glove box;
A differential pressure gauge for measuring the pressure difference inside and outside the glove box;
With
One or both of a fan filter unit and a downflow system are provided in the glove box.

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