JP2011146704A - Hydrogen annealing treatment method and hydrogen annealing treatment device - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To allow pressure-reduced hydrogen annealing treatment to be safely performed. <P>SOLUTION: A hydrogen annealing treatment device includes: a reaction chamber 2; a hydrogen gas introduction line 18 for introducing hydrogen gas into the reaction chamber; a pressure reducing exhaust line 5 connected to the reaction chamber; an exhauster which is provided in the pressure reducing exhaust line and reduces pressure in the reaction chamber; and an exhaust dilution line 48 which provides an inert gas to the downstream side of the exhauster to dilute a hydrogen concentration in exhaust gas to a predetermined value or lower. Safe pressure-reduced hydrogen anneal treatment is achieved by a hydrogen annealing treatment method including steps of: subjecting a target substrate to be treated, to pressure-reduced annealing treatment while introducing hydrogen gas from the hydrogen gas introduction line into the reaction chamber wherein pressure is reduced, and sucking and exhausting residual gas in the reaction chamber after the pressure-reduced annealing treatment, to the downstream side of the exhauster via the pressure reducing exhaust line by the exhauster; and supplying the inert gas from the exhaust dilution line 48 to the downstream side of the exhauster to dilute the hydrogen concentration in the residual gas to a predetermined value or lower. <P>COPYRIGHT: (C)2011,JPO&INPIT

Description

  The present invention relates to a hydrogen annealing method and apparatus for performing hydrogen annealing, which is one of the manufacturing steps of a semiconductor manufacturing apparatus.

  Device wiring is formed of an Al film and a Cu film. If oxygen remains in the Al film and the Cu film, the fine wiring may cause a change with time, which may cause disconnection. For this reason, Al film and Cu film reduction treatment is performed on the substrate to be treated by hydrogen annealing treatment.

Al wiring is frequently used for the wiring of the above devices because it is inexpensive and has good workability.
However, since Al itself has a large conductor resistance, Cu or Cu alloy wiring is advantageous for manufacturing a device capable of higher-speed processing. However, since Cu easily oxidizes, hydrogen annealing is more important when Cu or Cu alloy is used for the wiring.

  As a conventional hydrogen annealing treatment apparatus, there is a hydrogen annealing treatment at normal pressure as seen in Japanese Patent Laid-Open No. 5-291268. The outline of an annealing apparatus shown in Japanese Patent Laid-Open No. 5-291268 will be described below with reference to FIG.

  A reaction chamber 2 is defined inside the reaction furnace 1, and a boat 3 is inserted into and removed from the reaction chamber 2. A hydrogen gas introduction pipe 4 and a vacuum exhaust pipe 5 communicate with the reaction chamber 2, and a vacuum exhaust apparatus 7 is connected to the vacuum exhaust pipe 5 through a valve 6. A hydrogen combustion pipe 9 communicates with the upstream side of the vacuum exhaust pipe 5 via a valve 8, the hydrogen combustion pipe 9 communicates with a combustion box 10, and a tip of the hydrogen combustion pipe 9 serves as a combustion nozzle 11. . A hydrogen flame line 12 communicates with the combustion box 10, and the tip of the hydrogen flame line 12 is led to the vicinity of the combustion nozzle 11 to light the flame. An exhaust duct 13 communicates with the combustion box 10 and is connected to an exhaust device (not shown). In the figure, 14 is a damper that opens the inside of the combustion box 10 to the atmosphere.

  In the hydrogen annealing apparatus, when hydrogen annealing is performed, the valve 6 is opened, the air in the reaction chamber 2 is exhausted by the vacuum exhaust device 7, and then the valve 6 is closed. The valve 8 is opened. Hydrogen is introduced into the reaction chamber 2 from the hydrogen gas introduction pipe 4 at normal pressure, and a hydrogen annealing process is performed.

  Further, surplus hydrogen gas after the treatment is exhausted to the combustion box 10. Hydrogen discharged from the combustion nozzle 11 through the hydrogen combustion pipe 9 is ignited by the seed fire and burned in the combustion box 10. As the exhaust hydrogen burns in the combustion box 10, the exhaust duct 13 is discharged with exhaust gas from which hydrogen has been removed or whose concentration has been reduced to a predetermined concentration or less.

  The purpose of performing the hydrogen annealing treatment is to remove oxygen (reduction) in the metal conductor film as described above and to remove impurities in the metal conductor film, particularly the Cu film, thereby improving the electrical characteristics. It may be performed for the purpose and to improve the adhesion between the base and the Cu film.

For the purpose of reduction, it is more effective to perform the treatment under normal pressure, which is the case where the reduction treatment is performed on the multilayer wiring.

  In order to improve electrical characteristics and adhesion to the substrate, it is effective to perform the treatment under reduced pressure (for example, about 50 Torr).

This is because etching or the like, which is a pre-process of the hydrogen annealing process, may have residual impurities and additives attached thereto, which are considered to have an adverse effect on device characteristics. These substances are substances that have a low vapor pressure and are difficult to vaporize, and the conditions for removal are preferably reduced pressure. After the residual impurities are removed by supplying hydrogen, they are replaced with hydrogen atoms. Therefore, it is considered that the molecular bond becomes stronger, and as a result, the adhesion is improved. That is, when hydrogen annealing treatment is performed under reduced pressure, reduction treatment can be performed, electrical characteristics can be improved, and adhesion to the substrate can be improved. Accordingly, when higher quality is required, a reduced pressure hydrogen annealing process is performed.

  As described above, when performing the hydrogen annealing treatment, there are cases where it is better to perform the atmospheric pressure treatment depending on the purpose, and cases where it is better to perform the pressure reduction treatment.

  However, the hydrogen annealing apparatus described above performs hydrogen annealing only at normal pressure and cannot perform reduced pressure hydrogen annealing. Accordingly, a hydrogen annealing apparatus for performing the reduced pressure hydrogen annealing process must be provided separately.

  Further, in the above hydrogen annealing apparatus, when the reaction chamber is used at a reduced pressure in order to perform a decompression process, the combustion box 10 is a system in which hydrogen gas is burned at normal pressure. There is a possibility that the atmosphere will flow backward, and if it flows backward, it is possible that unreacted hydrogen gas reacts with oxygen in the atmosphere and explodes, and the fire for burning hydrogen gas in the combustion box flows backward. However, it is considered that it is difficult to treat unreacted hydrogen gas, and no vacuum hydrogen annealing treatment apparatus has been put to practical use.

  In view of such circumstances, the present invention realizes a reduced pressure hydrogen annealing apparatus and enables both the reduced pressure hydrogen annealing process and the atmospheric hydrogen annealing process to be performed by the same hydrogen annealing apparatus, thereby reducing the equipment cost. Is.

The present invention is provided in a reaction chamber, a hydrogen gas introduction line for supplying hydrogen gas to the reaction chamber, a vacuum exhaust line connected to the reaction chamber, and the vacuum exhaust line for decompressing the reaction chamber. A gas exhaust line, an exhaust gas dilution line for supplying an inert gas downstream of the gas exhaust apparatus to dilute a hydrogen concentration in the exhaust gas to a predetermined value or less, a normal pressure exhaust line connected to the reaction chamber, A hydrogen gas combustion section connected to a normal pressure exhaust line; and a communication line connecting the reaction chamber and the downstream side of the exhaust device, the reduced pressure exhaust line, the normal pressure exhaust line, and the communication line; The exhaust dilution is performed while supplying the hydrogen gas from the hydrogen gas introduction line to the reaction chamber in a state where the reaction chamber is decompressed by driving the exhaust device and exhausting from the decompression exhaust line. Rye The inert gas is supplied to the downstream side of the exhaust device from the above, and the reduced pressure hydrogen annealing treatment for diluting the hydrogen concentration in the exhaust gas to a predetermined value or less and the normal pressure hydrogen annealing treatment for exhausting from the normal pressure exhaust line and the communication The present invention relates to a hydrogen annealing treatment method that is performed by selecting a dormant state that is exhausted from a line.
The present invention also includes a reaction chamber, a hydrogen gas introduction line for supplying hydrogen gas to the reaction chamber, a reduced pressure exhaust line connected to the reaction chamber, and the reduced pressure exhaust line to depressurize the reaction chamber. An exhaust system for supplying the inert gas downstream of the exhaust system, diluting the hydrogen concentration in the exhaust gas below a predetermined value, and a normal pressure exhaust line connected to the reaction chamber, The hydrogen gas combustion unit connected to the normal pressure exhaust line, the communication line connecting the reaction chamber and the downstream side of the exhaust device, the normal pressure exhaust line, the vacuum exhaust line, the communication line, and the The present invention relates to a hydrogen annealing apparatus comprising a valve for switching a connection state with a reaction chamber.
The present invention also includes a reaction chamber, a hydrogen gas introduction line for supplying hydrogen gas to the reaction chamber, a reduced pressure exhaust line connected to the reaction chamber, and the reduced pressure exhaust line to depressurize the reaction chamber. An exhaust system for supplying the inert gas downstream of the exhaust system, diluting the hydrogen concentration in the exhaust gas below a predetermined value, and a normal pressure exhaust line connected to the reaction chamber, The hydrogen gas combustion unit connected to the normal pressure exhaust line, the communication line connecting the reaction chamber and the downstream side of the exhaust device, the normal pressure exhaust line, the vacuum exhaust line, the communication line, and the It comprises a valve for switching the connection state with the reaction chamber, a gas concentration detector provided downstream of the exhaust device, and a flow rate controller provided in the exhaust dilution line, and the hydrogen concentration released is 4%. Inactive gas so that Those related to the hydrogen annealing device for controlling the supply flow rate.

According to the present invention, it is possible to perform a low-pressure hydrogen annealing process, effectively degassing and detaching impurities from the substrate to be processed, and the electrical characteristics of the device are improved.

  The apparatus further comprises a reaction chamber, a hydrogen gas introduction line for introducing hydrogen gas into the reaction chamber, and a normal pressure exhaust line and a vacuum exhaust line connected to the reaction chamber. Since the annealing treatment and the atmospheric hydrogen annealing treatment can be selected and performed, a treatment method according to the object to be treated such as a device that requires reduction or a device that requires removal of impurities can be selected, thereby improving product quality.

  A reaction chamber, a hydrogen gas introduction line for introducing hydrogen gas into the reaction chamber, a normal pressure exhaust line and a vacuum exhaust line connected to the reaction chamber, the normal pressure exhaust line, the vacuum exhaust line, and the reaction chamber And a valve for switching the connection state between the hydrogen annealing process and the low pressure hydrogen annealing process and the normal pressure hydrogen annealing process can be performed with one hydrogen annealing apparatus. Exhibits excellent effects such as reduction of

  Hereinafter, embodiments of the present invention will be described with reference to the drawings.

  In FIG. 1, the same components as those shown in FIG.

  The reaction furnace 1 has a configuration in which a reaction tube 15, a soaking tube 16, and a heater 17 are provided concentrically. A reaction chamber 2 is defined inside the reaction tube 15.

  A gas introduction pipe 18 and an exhaust gas pipe 19 are connected to the reaction pipe 15 so as to communicate with the reaction chamber 2.

  The gas introduction pipe 18 is branched upstream, one of the branches is connected to a hydrogen gas supply source (not shown) as a hydrogen gas introduction pipe 21, and the other branch is connected to a nitrogen gas supply source (not shown) as a nitrogen gas introduction pipe 22. Has been.

  The hydrogen gas introduction pipe 21 is further branched and led to the combustion box 10 as a hydrogen fire type line 12. A hydrogen gas supply / stop valve 23 and a flow rate controller 24 are sequentially provided in the hydrogen gas introduction pipe 21 at a position downstream of the branch point of the hydrogen fire type line 12. An on-off valve 25 and a flow rate controller 26 are provided.

The nitrogen gas introduction pipe 22 is further branched into two nitrogen gas dilution lines 27 and 28. One nitrogen gas dilution line 27 is led to a space between the reaction pipe 15 and the soaking pipe 16, and the other nitrogen gas is supplied. The dilution line 28 is led to a space between the soaking tube 16 and the heater 17. A nitrogen gas supply / stop valve 29 and a flow rate controller 31 are sequentially provided at a position downstream of the branch point of the nitrogen gas dilution lines 27 and 28, and a first dilution line opening / closing valve 32 is provided in the nitrogen gas dilution line 27. The nitrogen gas dilution line 28 is provided with a second dilution line opening / closing valve 33. A position upstream of the nitrogen gas supply / stop valve 29 of the nitrogen gas introduction pipe 22 and a position between the fire line open / close valve 25 of the hydrogen fire type line 12 and the flow rate controller 26 are connected by a nitrogen gas bypass line 34, and the nitrogen gas A bypass opening / closing valve 35 is provided in the bypass line 34.

  The exhaust gas pipe 19 is provided with a pressure sensor 36 for detecting the pressure in the reaction chamber 2, and the exhaust gas pipe 19 branches downstream of the pressure sensor 36, and one of them serves as a vacuum exhaust pipe 5 as a vacuum exhaust line. The other is led to the combustion box 10 as a hydrogen combustion pipe 9, and the tip opens as a combustion nozzle 11 near the tip of the hydrogen fire line 12.

  An exhaust opening / closing valve 37, a flow rate adjusting valve 38, and an exhaust pump 40 are sequentially provided in the vacuum exhaust pipe 5 from the upstream side, and an exhaust duct 50 is connected to the downstream side of the exhaust pump 40. A first nitrogen gas ballast line 39 and a second nitrogen gas ballast line 41 are connected between the flow rate adjusting valve 38 of the vacuum exhaust pipe 5 and the exhaust pump 40, and the first nitrogen gas ballast line 39, The 2 nitrogen gas ballast line 41 is connected to a nitrogen gas supply source (not shown).

  The first nitrogen gas ballast line 39 is provided with a first on-off valve 42, a first backflow prevention valve 43, and a first flow control valve 44 in that order upstream, and the second nitrogen gas ballast line 41 is upstream. A second on-off valve 45, a second backflow prevention valve 46, and a second flow rate control valve 47 are sequentially provided toward the side.

  An exhaust dilution line 48 communicates with the exhaust duct 50, and an L-shaped nozzle 49 opening toward the downstream side is provided at the tip of the exhaust dilution line 48. The exhaust dilution line 48 is connected to a nitrogen gas supply source (not shown). It is connected. The exhaust dilution line 48 is provided with a flow rate controller 66, an on-off valve 67, and a backflow prevention valve 68 from the nitrogen gas supply source side toward the downstream.

  A pressure switch 51 and an opening / closing valve 52 are provided downstream from the branch point of the hydrogen combustion pipe 9, and a position between the pressure switch 51 and the opening / closing valve 52 of the hydrogen combustion pipe 9 and an exhaust pump of the vacuum exhaust pipe 5 are provided. The downstream position of 40 is connected by a connecting line 53, and an open / close valve 54 and a backflow prevention valve 55 are provided from the hydrogen combustion pipe 9 side to the connecting line 53.

  The combustion box 10 is connected to an exhaust device (not shown) through an exhaust duct 56, an exhaust dilution line 57 is connected to the exhaust duct 56, and the exhaust dilution line 57 is connected to a nitrogen gas supply source (not shown). A flow rate controller 58, a backflow prevention valve 59, and an on-off valve 60 are sequentially provided from the nitrogen gas supply source side. Further, the combustion box 10 is provided with a temperature sensor 62 and a flame detection sensor 63, which detect whether or not hydrogen gas is being burned in the combustion box 10, and the exhaust duct 56. Is provided with a gas concentration detector 69 for detecting the hydrogen concentration in the exhaust gas discharged from the exhaust duct 56.

  The operation will be described below.

  First, referring to FIG. 1, the reduced-pressure hydrogen annealing process will be described.

  The second dilution line opening / closing valve 33, the first dilution line opening / closing valve 32, the nitrogen gas supply / closing valve 29, the fire type line opening / closing valve 25, the bypass opening / closing valve 35, the second opening / closing valve 45, the opening / closing valve 54, the opening / closing valve 52, opening / closing. The valves 60 are closed, and the hydrogen gas supply / stop valve 23, the exhaust on / off valve 37, the first on / off valve 42, and the on / off valve 67 are opened.

  The exhaust pump 40 is driven, and the reaction chamber 2 is in a reduced pressure state. Here, the reduced pressure state means not a high vacuum state but a state where the pressure during the reduced pressure is lower than the atmospheric pressure, and the reduced pressure state is determined by the state of the hydrogen annealing treatment.

The hydrogen gas supply / stop valve 23 is opened, and hydrogen gas is introduced into the reaction chamber 2 while the flow rate is controlled by the flow rate controller 24. The residual gas after the reaction is sucked and exhausted by the exhaust pump 40 through the vacuum exhaust pipe 5. The pressure of the evacuation pipe 5 is detected by the pressure sensor 36, the opening / closing degree of the flow rate adjusting valve 38 is adjusted, and the inflow amount of nitrogen gas from the first nitrogen gas ballast line 39 is controlled. By controlling the back pressure in the reaction chamber 2, the pressure in the reaction chamber 2 is controlled. Here, the pressure in the reaction chamber during the low-pressure hydrogen annealing treatment is preferably in the range of 1 to 750 Torr in order to improve the electrical characteristics of the wiring formed on the substrate and improve the adhesion to the substrate. About 50 Torr is more preferable.
Moreover, the nitrogen gas flowing in from the first nitrogen gas ballast line 39 dilutes the exhaust gas and lowers the hydrogen gas concentration.

The natural explosion condition of hydrogen gas is a hydrogen gas concentration of 4% to 70%. The exhaust dilution line 48 dilutes the exhaust gas while adjusting the nitrogen gas supply amount by the flow rate controller 66 so that the hydrogen gas concentration in the gas exhausted from the exhaust pump 40 is 4% or less.
Note that the L-shaped nozzle 49 is opened on the downstream side so that the flow of the exhaust gas in the exhaust duct 50 is not disturbed.

  Thus, the exhaust gas diluted so as not to interfere with the release to the atmosphere is discharged through the exhaust duct 50.

  As described above, the reaction chamber 2 is maintained in a predetermined reduced pressure state by adjusting the exhaust resistance by the flow rate adjusting valve 38 and by controlling the back pressure by supplying nitrogen gas from the first nitrogen gas ballast line 39. By supplying nitrogen gas from the first nitrogen gas ballast line 39 and further supplying nitrogen gas from the exhaust dilution line 48, the hydrogen gas concentration in the released gas can be controlled to 4% or less, so the pressure can be safely reduced. The hydrogen annealing process is realized.

  FIG. 2 shows a dormant state.

  In the resting state, the exhaust pump 40 is stopped, the second dilution line opening / closing valve 33, the first dilution line opening / closing valve 32, the hydrogen gas supply / stop valve 23, the fire type line opening / closing valve 25, the exhaust opening / closing valve 37, the first opening / closing valve 42. The on-off valve 52 is closed, and the nitrogen gas supply / stop valve 29, the bypass on-off valve 35, the second on-off valve 45, the on-off valve 54, the on-off valve 67, and the on-off valve 60 are opened.

  Nitrogen gas flows through the gas introduction pipe 18 through the nitrogen gas introduction pipe 22 and is supplied to the reaction chamber 2. Hydrogen gas in the reaction chamber 2 is extruded, and the reaction chamber 2 is replaced with nitrogen gas. The nitrogen gas discharged from the reaction chamber 2 is further discharged to the exhaust duct 50 on the downstream side of the exhaust pump 40 through the hydrogen combustion pipe 9 and the connection line 53, and the residual hydrogen gas in the hydrogen combustion pipe 9 is discharged. To do.

  Further, nitrogen gas is supplied from the second nitrogen gas ballast line 41 to the upstream side of the exhaust pump 40 of the vacuum exhaust pipe 5, the vacuum exhaust pipe 5 is replaced with nitrogen gas, and excess nitrogen gas passes through the exhaust pump 40. It is discharged to the exhaust duct 50. In the resting state, the exhaust pump 40 is stopped, and the flow rate of the nitrogen gas discharged from the second nitrogen gas ballast line 41 through the exhaust pump 40 is small.

  At the beginning of supply of nitrogen gas, hydrogen gas is contained in the exhaust gas, and nitrogen gas is supplied from the exhaust dilution line 48 so that the concentration of hydrogen gas in the exhaust gas becomes 4% or less. .

  Further, the nitrogen gas is circulated to the hydrogen flame line 12 through the nitrogen gas bypass line 34, and the hydrogen gas in the hydrogen flame line 12 is discharged. Nitrogen gas is discharged to the combustion box 10 through the hydrogen flame line 12 and further discharged through the exhaust duct 56. If the nitrogen gas discharged from the hydrogen fire line 12 contains hydrogen gas, the nitrogen gas is supplied from the exhaust dilution line 57 at the time of discharge from the exhaust duct 56, and the concentration of the hydrogen gas is reduced. It is certainly 4% or less.

  The nitrogen gas dilution line 27 and the nitrogen gas dilution line 28 leak hydrogen gas, and hydrogen gas is accumulated in the space between the reaction tube 15 and the soaking tube 16 and in the space between the soaking tube 16 and the heater 17. In this case, the second dilution line opening / closing valve 33 and the first dilution line opening / closing valve 32 are opened and nitrogen gas is supplied to reduce the hydrogen concentration to a safe value. Nitrogen gas supply to the space may flow periodically or a small amount may flow constantly.

  The hydrogen annealing process at normal pressure will be described with reference to FIG.

  The second dilution line opening / closing valve 33, the first dilution line opening / closing valve 32, the nitrogen gas supply / closing valve 29, the bypass opening / closing valve 35, the second opening / closing valve 45, the first opening / closing valve 42, the exhaust opening / closing valve 37, the opening / closing valve 67, The on-off valve 54 is closed, and the on-off valve 52 and the on-off valve 60 are opened.

  The hydrogen gas supply / stop valve 23 is opened. Hydrogen gas is introduced into the reaction chamber 2 at normal pressure while the flow rate is controlled by the flow rate controller 24. The fire line open / close valve 25 is opened, hydrogen gas is introduced into the combustion box 10 via the hydrogen fire line 12, and ignited and burned as a fire.

  The residual gas introduced into the reaction chamber 2 and subjected to the hydrogen annealing treatment passes through the hydrogen combustion pipe 9 and is exhausted from the combustion nozzle 11. Unreacted hydrogen gas is ignited and burned by the above-mentioned seed fire.

The exhaust gas after combustion is discharged through the exhaust duct 56. Nitrogen gas for reducing the hydrogen gas concentration is supplied to the exhaust duct 56 through the exhaust dilution line 57, and the hydrogen gas concentration in the exhaust gas flowing through the exhaust duct 56 is the gas concentration detector 69. The supply flow rate is controlled so that the detected hydrogen gas concentration is 4% or less, and if the hydrogen gas concentration detected by the gas concentration detector 69 exceeds 4%, the exhaust dilution line While the nitrogen gas is supplied from 57, the hydrogen annealing process sequence of the apparatus is stopped, for example, the hydrogen gas supply / stop valve 23 and the fire type open / close valve 25 are closed. When the hydrogen gas concentration is 4% or more, for example, the seed fire 70 may be extinguished and the combustion of the hydrogen gas flowing out from the combustion nozzle 11 may be stopped.

  Thus, hydrogen annealing at normal pressure is performed.

  When the hydrogen annealing process at normal pressure is completed, the second dilution line opening / closing valve 33, the first dilution line opening / closing valve 32, the hydrogen gas supply / closing valve 23, the fire type line opening / closing valve 25, and the exhaust opening / closing valve 37 as shown in FIG. The first opening / closing valve 42 and the opening / closing valve 52 are closed.

  The nitrogen gas supply / stop valve 29, the bypass on / off valve 35, the second on / off valve 45, the on / off valve 67, the on / off valve 54, and the on / off valve 60 are opened.

When the nitrogen gas supply stop valve 29 is opened, nitrogen gas is supplied into the reaction chamber 2 through the nitrogen gas introduction pipe 22, and the hydrogen gas in the reaction chamber 2 is replaced with nitrogen gas. In the process until the hydrogen gas in the reaction chamber 2 is replaced with nitrogen gas, the hydrogen gas is discharged from the hydrogen combustion pipe 9. Since the on-off valve 52 is closed, the gas is discharged to the exhaust duct 50 through the communication line 53. Nitrogen gas is supplied to the exhaust duct 50 from an L-type nozzle 49 from an exhaust dilution line 48. The hydrogen concentration in the exhaust gas discharged from the exhaust duct 50 is detected by a gas concentration detector 71, and the nitrogen gas supply flow rate from the L-type nozzle 49 is set to the flow controller 66 so that the hydrogen concentration is diluted to 4% or less. Controlled by

  When the bypass opening / closing valve 35 is opened, nitrogen gas is supplied to the hydrogen flame line 12 through the nitrogen gas bypass line 34, and the hydrogen gas in the hydrogen flame line 12 is pushed out by nitrogen gas. The seed fire 70 is maintained until the hydrogen gas in the hydrogen fire line 12 runs out. Further, the hydrogen concentration in the gas discharged from the exhaust duct 56 is detected by the gas concentration detector 69, and from the exhaust dilution line 57 so that the hydrogen concentration in the discharged gas becomes 4% or less. The flow rate of the supplied nitrogen gas is controlled by the flow rate controller 58.

  Thus, the exhaust gas diluted so as not to interfere with the release to the atmosphere is discharged through the exhaust duct 50 and the exhaust duct 56.

  When the hydrogen gas in the reactor 1, the hydrogen combustion pipe 9, and the hydrogen flame line 12 is completely discharged, the rest state after the decompression process shown in FIG. 2 and the rest state after the normal pressure process shown in FIG. The state is the same.

  In any of the above-described reduced pressure hydrogen annealing treatment and normal pressure hydrogen annealing treatment, the pressure in the reaction chamber 2 by the pressure sensor 36, or in the exhaust gas discharged by the gas concentration detector 69 and the gas concentration detector 71 is used. The hydrogen concentration, the combustion state of the exhaust gas by the temperature sensor 62 and the flame detection sensor 63, etc. are constantly monitored, and if the detection results from the various sensors indicate an abnormality, an error is displayed on the display device of the operation unit. Further, when the hydrogen concentration of the released gas exceeds a predetermined value, or when the temperature sensor 62 and the flame detection sensor 63 do not detect the combustion of hydrogen gas, the hydrogen gas supply / stop valve 23 is closed, and the device Is controlled to be in a dormant state.

  As described above, the degree of decompression in the decompression process is 1 to 750 Torr, and a high degree of vacuum is not required. Therefore, instead of the exhaust pump 40, an orifice is provided in the exhaust line, and the orifice is decompressed. It may be a Convum type exhaust device that communicates the space (reaction chamber 2) and uses the static pressure of the fluid. The convert system can reduce the pressure up to several tens of Torr, and is sufficient for the decompression process of the present invention. Also, in the case of an exhaust pump, when the pump stops due to mechanical trouble or the like, the atmosphere flows backward and there is a danger of explosion. However, in the case of this comb system, it can be used safely. Furthermore, the inert gas may be any gas that suppresses the combustion of hydrogen gas, and is not limited to nitrogen gas.

FIG. 2 is a structural outline diagram showing an embodiment of the present invention. It is explanatory drawing explaining the effect | action of the pressure reduction process of embodiment of this invention same as the above. It is explanatory drawing explaining the effect | action of the normal pressure process of embodiment of this invention same as the above. It is explanatory drawing explaining the effect | action of the normal pressure process of embodiment of this invention same as the above. It is explanatory drawing which shows the conventional hydrogen annealing treatment apparatus.

DESCRIPTION OF SYMBOLS 1 Reaction furnace 2 Reaction chamber 5 Vacuum exhaust pipe 9 Hydrogen combustion pipe 10 Combustion box 12 Hydrogen fire type line 18 Gas introduction pipe 19 Exhaust pipe 22 Nitrogen gas introduction pipe 24 Flow controller 34 Nitrogen gas bypass line 36 Pressure sensor 38 Flow control valve 39 1st 1 Nitrogen gas ballast line 40 Exhaust pump 41 Second nitrogen gas ballast line 48 Exhaust dilution line 49 L-type nozzle 50 Exhaust duct 59 Backflow prevention valve 66 Flow controller 69 Gas concentration detector 71 Gas concentration detector

Claims (3)

A reaction chamber, a hydrogen gas introduction line for supplying hydrogen gas to the reaction chamber, a vacuum exhaust line connected to the reaction chamber, an exhaust device provided in the vacuum exhaust line for decompressing the reaction chamber, An exhaust dilution line for supplying an inert gas downstream of the exhaust device to dilute a hydrogen concentration in the exhaust gas to a predetermined value or less; a normal pressure exhaust line connected to the reaction chamber; and the normal pressure exhaust line And a communication line that connects the reaction chamber and the downstream side of the exhaust device, and switching between the reduced pressure exhaust line, the normal pressure exhaust line, and the communication line. The exhaust device is driven, and the reaction chamber is decompressed by exhausting from the decompression exhaust line, while supplying hydrogen gas from the hydrogen gas introduction line to the reaction chamber, From the communication line, the reduced pressure hydrogen annealing process for supplying the inert gas downstream of the gas apparatus and diluting the hydrogen concentration in the exhaust gas below a predetermined value, the atmospheric hydrogen annealing process for exhausting from the atmospheric pressure exhaust line, and the communication line A hydrogen annealing treatment method characterized by selecting a dormant state to be exhausted. A reaction chamber, a hydrogen gas introduction line for supplying hydrogen gas to the reaction chamber, a vacuum exhaust line connected to the reaction chamber, an exhaust device provided in the vacuum exhaust line for decompressing the reaction chamber, An exhaust gas dilution line for supplying an inert gas downstream of the exhaust device to dilute a hydrogen concentration in the exhaust gas to a predetermined value or less; a normal pressure exhaust line connected to the reaction chamber; and the normal pressure exhaust gas A hydrogen gas combustion section connected to a line, a communication line connecting the reaction chamber and the downstream side of the exhaust device, a connection between the normal pressure exhaust line, the vacuum exhaust line, the communication line, and the reaction chamber A hydrogen annealing apparatus comprising: a valve for switching a state. A reaction chamber, a hydrogen gas introduction line for supplying hydrogen gas to the reaction chamber, a vacuum exhaust line connected to the reaction chamber, an exhaust device provided in the vacuum exhaust line for decompressing the reaction chamber, An exhaust gas dilution line for supplying an inert gas downstream of the exhaust device to dilute a hydrogen concentration in the exhaust gas to a predetermined value or less; a normal pressure exhaust line connected to the reaction chamber; and the normal pressure exhaust gas A hydrogen gas combustion section connected to a line, a communication line connecting the reaction chamber and the downstream side of the exhaust device, a connection between the normal pressure exhaust line, the vacuum exhaust line, the communication line, and the reaction chamber A valve for switching the state, a gas concentration detector provided on the downstream side of the exhaust device, and a flow rate controller provided in the exhaust dilution line, so that the concentration of released hydrogen is 4% or less. Active gas supply flow rate Hydrogen annealing apparatus Gosuru.