TWI419206B - The opening method and the memory medium of the container - Google Patents

Description

Open atmosphere method and memory medium for processing containers

The present invention relates to an atmosphere opening method of a processing container when a fluorine-based by-product is added to a processing container in a gas processing apparatus such as a film forming apparatus, and is useful for performing such a method. Method of program memory media.

In the manufacturing process of a semiconductor device, in order to form a metal film such as a W film, a CVD film forming apparatus is used. In the CVD film formation of the W film, WF ₆ gas as a film forming gas and H ₂ gas as a reducing gas are used, and on the heated semiconductor wafer (hereinafter, simply referred to as a wafer), These react to form a film W film.

In such a CVD film forming apparatus, by-products are applied to the wall portion of the processing container during the film forming process, and if the reaction by-products are placed, they are peeled off and become particles. Therefore, after a film formation process of a specific number of wafers is performed, ClF3 gas as a clean gas is introduced into the processing container, and then cleaned, and then N ₂ gas is used to treat the inside of the processing container. Wash in a number of wash cycles and then open to the atmosphere.

However, when the wafer to be processed is a film in which a Ti film or a TiN film is formed, F (fluorine) in the processing container reacts with Ti, and a large amount of by-products such as TiFx are paid. The wall of the container is treated and remains after the ClF ₃ is cleaned.

When the processing container is opened to the atmosphere in such a state in which a by-product such as TiFx is applied, TiFx reacts with moisture in the air, and there is a possibility of generating toxic HF gas.

In order to open a treatment container in which a fluorine-based reaction product or a residual gas is present, in a manner that does not generate toxic HF gas, Patent Document 1 proposes opening of a processing container. Before that, a gas which reacts with a by-product or a residual gas in the processing chamber, for example, a gas containing moisture or air, hydrogen, or the like is introduced.

However, the technique of Patent Document 1 is to remove a reaction product generated during dry etching, and when it is produced as a by-product in the processing chamber at the time of CVD film formation, it is like In Patent Document 1, generally, only air or the like is introduced, and the by-products are not necessarily sufficiently removed, which is not sufficient.

[Patent Document 1] Japanese Patent Laid-Open Publication No. 2004-111811

The present invention has been made in view of such a situation, and an object thereof is to provide a case where even if a by-product formed of a metal fluoride is formed in a processing container, it is hardly produced. An atmosphere opening method of a processing container capable of opening a processing container to the atmosphere, such as a toxic gas such as HF.

Further, it is an object of the present invention to provide a memory medium for carrying out the program of such a method.

In order to solve the above problems, a first aspect of the present invention provides a method for opening an atmosphere of a processing container, which is a processing container in which a processing container to which a metal fluoride is applied and which is opened to the atmosphere is subjected to a specific treatment. An atmosphere opening method characterized by repeatedly introducing a plurality of times into the atmosphere in the processing vessel and maintaining a sufficient time for the metal fluoride to react with moisture in the atmosphere, and then performing the first operation of exhausting Then, the second operation of discharging the reaction product generated mainly by the first operation is performed by repeatedly introducing the atmosphere into the processing container and exhausting it.

In the above first aspect, the first operation is preferably 5 minutes or longer, and more preferably 5 to 20 minutes. Further, it is preferable that the first operation is performed 2 to 10 times in a repeated manner.

In the second operation, it is preferable that the holding time in the state in which the atmosphere is introduced is 1 to 5 minutes. Further, it is preferable that the second operation is performed 20 times or more in a repeated manner.

In the above-described first aspect, the atmosphere opening method is preferably a case where the treatment is a CVD film formation treatment and the metal fluoride is TiFx.

According to a second aspect of the present invention, there is provided a method for opening an atmosphere of a processing container, which is an atmosphere opening method in which a processing container in which a CVD treatment is performed and a processing container having TiFx is opened in the atmosphere is provided. : introducing the atmosphere into the treatment vessel repeatedly over 5 times, and maintaining enough to cause TiFx to react with moisture in the atmosphere to produce HF. After the first operation of sufficient time, the second operation of discharging the HF mainly by the first operation is performed by introducing the atmosphere into the processing container 25 times or more and discharging it.

In the second aspect, the first operation is performed by setting the holding time to 5 minutes or longer, and the second operation is preferably 1 to 5 minutes in a state in which the atmosphere is introduced. .

In the first and second aspects described above, it is preferable that the processing container is washed with an inert gas before the first operation.

According to a third aspect of the present invention, a memory medium is provided as a memory medium in which a program for controlling a processing device is stored, wherein the control program is executed to perform the first viewpoint as described above. And the method of any one of the second aspects, wherein the processing device is controlled by a computer.

According to the present invention, after the specific treatment is performed, the treatment container having the metal fluoride as the by-product is repeatedly introduced into the atmosphere repeatedly, and is kept sufficiently high in the metal fluoride to be in the atmosphere. The first operation of the water for a sufficient period of time for the reaction to sufficiently react the metal fluoride with the water, and then the reaction product is discharged by repeatedly introducing the atmosphere and the exhaust gas over a plurality of times. In the second operation, the reaction between the metal fluoride in the processing container and the water can be almost completely performed, and then, when the atmosphere is opened, a toxic gas such as HF is hardly generated.

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

Fig. 1 is a schematic cross-sectional view showing a CVD film forming apparatus used in the practice of the atmosphere opening method of one embodiment of the present invention. In the CVD film forming apparatus 100, a tungsten (W) film is formed on a semiconductor wafer W (hereinafter simply referred to as a wafer W) which is a substrate to be processed by using H2 gas and WF ₆ gas.

The CVD film forming apparatus includes a main body 1 and a bulb unit 85 is provided below the main body 1. A cover 3 for supporting the shower head 22, which will be described later, is provided on the upper portion of the main body 1.

The main body 1 is provided with a processing container 2 which is formed into a bottomed cylindrical shape by, for example, aluminum or the like. In the processing container 2, a cylindrical shielding substrate 8 is erected from the bottom of the processing container 2. At the opening of the upper portion of the shielding substrate 8, an annular base ring 7 is disposed, and on the inner peripheral side of the base ring 7, an annular ATTACHMENT 6 is supported and is provided to be protruded from the attachment. The mounting table 5 on which the wafer W is placed is supported by a protruding portion (not shown) of the inner peripheral edge portion of the inner portion. On the outer side of the shielding substrate 8, a baffle 9 is provided. Further, the cover 3 is provided in an opening portion of the upper portion of the processing container 2, and the shower head 3 is provided with a shower head 22 at a position facing the wafer W placed on the mounting table 5. . The cover 3 and the processing container 2 are connected by a hinge portion 25, whereby the cover portion 3 is opened and closed by the hinge portion 25. However, when the processing container is opened to the atmosphere, the cover The cover 3 is in a state of being opened.

In a space surrounded by the mounting table 5, the attachment 6, the base ring 7, and the shielding base 8, a cylindrical reflector 4 is erected from the bottom of the processing container 2, at which, for example, the reflector 4 A slit portion (in one of the places shown in FIG. 1) is provided at three places to lift the wafer W from the mounting table 5 at a position corresponding to the slit portion. The lift pins 12 are respectively configured to be lifted and lowered. The lift pin 12 is supported by the push rod 15 via the annular holding member 13 and the street 14 provided on the outer side of the reflector 4, and the rod 15 is pushed up and attached to the attachment 16. The lift pin 12 is constructed by passing through a material of a hot wire, such as quartz. Moreover, the support member 11 integrated with the lift pin 12 is provided, and this support member 11 penetrates the attachment 6, and supports the ring-shaped clamp ring 10 provided above it. The clamp ring 10 is made of amorphous carbon which easily absorbs heat rays, a carbon-based member such as SiC, or a ceramic such as Al ₂ O ₃ , AlN or black AlN.

According to this configuration, the lifter 12 is lifted and lowered by the attachment member 16, and the lift pin 12 and the clamp ring 10 are integrally raised and lowered. When the wafer 12 is lifted by the lift pin 12 and the clamp ring 10, the lift pin 12 is raised until it protrudes from the mounting table 5 by a specific length, and is supported on the wafer W supported by the lift pin 12. When placed on the mounting table 5, as shown in Fig. 1, the lift pin 12 is retracted into the mounting table 5, and the clamp ring 10 is lowered to a position where it is brought into contact with the wafer W and held.

Further, at the bottom of the processing container 2, a cleaning gas flow path 19 is provided, and is connected to the cleaning gas flow path 19, and faces the mounting table 5, the attachment 6, the base ring 7, and the shielding. In the manner of the space S surrounded by the substrate 8, the flow path 19a is disposed at eight places on the lower inner side of the reflector 4, and the N ₂ gas is connected to the clean gas flow path 19 via the pipe 20. The cleaning gas supply mechanism 18 of the cleaning gas. At the piping 20, an opening and closing valve 21 is installed. The purge gas such as N ₂ gas from the purge gas supply unit 18 is supplied into the space S through the pipe 20, the purge gas flow path 19, and the flow path 19a. By supplying the cleaning gas supplied in this manner from the gap between the mounting table 5 and the attachment 6 outward in the radial direction, it is possible to prevent the processing gas from the shower head 22 from entering the mounting table 5 . The back side.

Further, at the pipe 20, an atmosphere introduction pipe 41 for taking in the atmosphere into the processing container 2 is connected. The atmosphere introduction pipe 41 is provided with a gasket filter 42, a second opening and closing valve 43, a restriction orifice gasket 44, and a first opening and closing valve 45 from the upstream side. The first and second opening and closing valves 45 and 43 are opened, and the inside of the processing container 2 can be air-washed through the piping 20, the cleaning gas flow path 19, and the flow path 19a from the atmosphere introduction pipe 41. In this way, two opening and closing valves are provided in order to reliably prevent the atmosphere from intruding into the processing container 2 during actual processing.

Further, in a plurality of places where the base 8 is shielded, a plurality of pressure adjusting mechanisms (not shown) that operate when the pressure difference between the inside and the outside of the shielding base 8 is equal to or greater than a certain amount, and that open and close the inside and outside of the shielding base 8 are provided.

The bottom of the processing container 2 directly below the mounting table 5 is provided with an opening 2a that surrounds the periphery of the reflector 4, and the opening 2a is airtightly attached to a heat transmitting member such as quartz. Through the window 17. through The through window 17 is held by a holder (not shown). The lamp unit 85 is disposed below the transmission window 17. The lamp unit 85 is provided with a heating chamber 90, a rotating table 87 provided in the heating chamber, a lamp tube 86 installed at the rotating table 87, and a bottom portion of the heating chamber 90, and A rotary motor 89 that rotates the rotary table 87 via the rotary shaft 88. Further, the lamp tube 86 is provided with a reflecting portion for reflecting the hot line, and the heat rays radiated from the respective lamps 86 are directly or reflected in the inner circumference of the reflector 4 to be equally Arranged to reach the lower side of the mounting table 5. By the lamp unit 85, the rotating table 87 is rotated by the rotating motor 89, and the hot wire is radiated from the lamp tube 86, and the heat wire radiated from the lamp tube 86 is irradiated to the mounting table 5 via the transmission window 17. Below this, the mounting table 5 is uniformly heated by the hot line.

The shower head 22 is provided with a cylindrical showerhead base 39 formed such that its outer edge is fitted to the upper portion of the cover 3, and an inner peripheral side upper portion of the showerhead base 39, and further A disk-shaped ceiling 29 having a gas introduction port 23 at its center and a lower portion of the shower head base 39 are formed, and a plurality of gas discharge holes 46 are formed in the shower head plate 35. On the outer circumference of the shower head plate 35, a spacer ring 40 is disposed.

The processing gas introduction pipe 31 is connected to the upper surface of the ceiling 29 so as to be continuous with the gas introduction port 23. At this processing gas introduction pipe 31, a pipe from a gas cartridge 50 for supplying various processing gases is connected.

In the space inside the shower head 22, a rectifying plate 33 having a plurality of gas passage holes 34 is horizontally disposed, whereby the rectifying plate 33, the shower head 22 The internal space is separated into an upper space 22a and a lower space 22b.

In the outer edge portion of the upper portion of the shower head plate 35, a ring-shaped refrigerant flow path 36 is provided, and in the refrigerant flow path 36, cooling water is supplied as a refrigerant through the refrigerant supply path 37a, and the refrigerant is discharged through the refrigerant. At 37b, the cooling water is discharged to circulate the cooling water as the refrigerant, and the showerhead 35 is cooled during the film formation process to suppress the undesired reaction.

The gas cartridge 50 is provided with ClF ₃ gas which is a clean gas, WF ₆ gas which is a film forming gas, Ar gas and N 2 gas which are used as a diluent gas, and H which is a reducing gas. ₂ gas and SiH ₄ gas are respectively supplied as a plurality of gas sources, and these gas sources are supplied to the process gas introduction pipe 31, and further supplied to the shower head 22, for example, through the pipes 51 to 56. . Further, at the time of the film formation treatment, film formation can be performed by general CVD in which a film formation gas and a reducing gas are simultaneously supplied, and SSF (sequential flow deposition) in which a film formation gas is intermittently supplied can be used. To form a film.

On the side wall of the processing container 2, two pressure measuring lines 61 and 62 are connected, and at these pressure measuring lines 61, 62, respectively, a capacitance manometer 63 as a pressure gauge is provided. 64. One of these is used to measure the pressure when the degree of vacuum is low, and the other is to measure the pressure at a high degree of vacuum with high accuracy. Further, on the pressure measurement lines 61 and 62, on/off valves 65 and 66 are provided, respectively.

At the bottom of the processing container 2, an exhaust port 67 is formed, and an exhaust pipe 68 is connected to the exhaust port 67. At the exhaust pipe 68, from the upper stream The exhaust mechanism 70 formed by the pressure control valve 69, the vacuum pump, and the like is provided on the side. Further, although not shown, a side wall of the processing container 2 is provided with a gate valve for loading and unloading the wafer, and a gate valve for opening and closing the loading and unloading port.

The CVD film forming apparatus 100 includes a process controller 71 formed of a microprocessor (computer) for controlling each component, and each component is connected to and controlled by the process controller 71. Composition. For example, the supply of the gas in the processing container 2, the pressure in the processing container 2, the exhaust mechanism 70, the lift pin 12, and the like are controlled by the process controller 71.

Further, the process controller 71 is connected to a keyboard for inputting an instruction or the like for the operator to manage the CVD film forming apparatus 100, or to visualize the operation state of the CVD film forming apparatus. A user interface 72 formed by a display or the like.

Further, the process controller 71 is connected to a memory unit 73 for storing various processes executed in the CVD film forming apparatus 100 under the control of the process controller 71. The implemented control program or the program for performing processing in each component of the plasma processing apparatus 10 in response to the processing conditions, that is, a recipe. The recipe is stored in the memory medium in the memory unit 73. The memory medium can be a hard disk or a semiconductor memory, and can also be a removable person such as a CDROM, a DVD, or a flash memory. Further, the recipe can be appropriately transferred from other devices, for example, via a dedicated line.

Then, any recipe is taken out from the memory unit 73 by an instruction from the user interface 72, etc., as needed, and is in the process control unit 71. In the middle, the desired processing in the CVD film forming apparatus 100 can be performed under the control of the process control unit 71.

Next, an operation of forming a W film on the surface of the wafer W by the above-described CVD film forming apparatus which is generally configured will be described. Further, this processing operation is performed under the control of the process controller 71 based on the program (recipe) stored in the memory medium of the storage unit 73.

First, a gate valve (not shown) provided on the side wall of the processing container 2 is opened, and the wafer W is carried into the processing container 2 by the transfer arm, and the lift pin 12 is raised until it protrudes from the mounting table 5. After receiving the wafer W for a certain length, the transfer arm is withdrawn from the processing container 2, and the gate valve is closed. Next, the lift pin 12 and the clamp ring 10 are lowered, and the lift pin 12 is immersed in the mounting table 5, and the wafer W is placed on the mounting table 5, and at the same time, the clamp ring 10 is lowered. To the position where the wafer is abutted and held. Further, the exhaust mechanism 70 is operated to exhaust the inside of the processing container 2, and the inside of the processing container 2 is brought to a specific pressure, and the lamp tube 86 in the heating chamber 90 is turned on, and the motor 86 is rotated by the motor 89. The rotating table 87 is rotated to radiate a hot wire to heat the wafer W to a specific temperature. The pressure control in the processing container 2 at this time is performed by controlling the opening degree of the pressure control valve 69 based on the measurement results of the capacitance pressure gauges 63, 64.

Next, Ar gas, N ₂ gas, SiH ₄ gas, and H ₂ gas are supplied at a specific flow rate, and introduced into the processing container 2 from the shower head 22, whereby the reaction is performed in the middle. The SiHx (x<4) of the body is attracted to the initiation process on the wafer W.

After the initial treatment, the flow rate of each of the processing gases is maintained as it is, and the WF ₆ gas is supplied at a specific flow rate which is less than a formal film forming process. In this state, the following formula (1) is used. The general SiH ₄ reduction reaction is carried out for a specific period of time, and a nucleation film is formed on the surface of the wafer W.

2WF ₆ +3SiH ₄ →2W+3SiF ₄ +6H ₂ (1)

Then, the supply of WF ₆ gas and SiH ₄ gas is stopped, and Ar gas, N ₂ gas, and H ₂ gas are supplied, and the exhaust amount of the exhaust mechanism 70 is lowered to increase the processing container for the purpose of the formal film forming process. The pressure inside 2, at the same time, makes the temperature of the wafer W stable.

Then, the supply of the WF ₆ gas is started again, and the supply amount of the other gas is controlled, and the W is formed into a film by a general reduction reaction represented by the following formula (2) at a specific time. A film forming process in which a W film is formed on the surface of the wafer W.

WF ₆ +3H ₂ →W+6HF (2)

After the completion of the film formation, the supply of the WF ₆ gas is stopped, and the supply of the Ar gas, the H ₂ gas, and the N ₂ gas is maintained, and the inside of the processing container 2 is rapidly depressurized by the exhaust mechanism 70. The processing gas remaining after the film formation is officially swept away from the processing container 2. Next, in a state where the supply of all the gases is stopped, the pressure reduction is continued, and the inside of the processing container 2 is brought into a high vacuum state, and thereafter, the lift pins 12 and the clamp ring 10 are raised, and the lift pins are lifted. 12 protrudes from the mounting table 5, raises the wafer W to a position that can be received by the transfer arm, opens the gate valve, and causes the transfer arm to enter the processing container 2, and receives the lift pin 12 by the transfer arm. The wafer W is taken out from the processing container 2 by the transfer arm, and the wafer W is taken out, and the film forming operation is completed.

When the film formation process is repeated a plurality of times, the by-product is added to the processing container 2, so that the ClF3 gas is supplied to the processing container 2 at the time when the film formation process of the specific number is completed. After that, the inside of the processing container 2 is cleaned, and after that, the cleaning process is performed, and then, in order to perform wet cleaning or maintenance, the cover 3 is opened, and the processing container 2 is opened to the atmosphere.

In this case, when the fluorine-based by-product is not formed in the processing container 2, after the cleaning by the ClF3 gas is performed, the supply of the N ₂ gas is discharged as a cleaning process. The cycle cleaning is performed a plurality of times, whereby the gas system in the processing container 2 is discharged, and the atmosphere can be safely opened. However, in the case of forming a W film, a wafer in which a Ti film or a TiN film is formed on a substrate is often used. In this case, TiFx is used as a by-product by a film formation process. It is formed, and this is applied to the wall portion of the processing container 2, and even if it is cleaned by ClF ₃ gas, it remains. When the atmosphere of the processing container 2 is opened in the state in which TiFx remains, TiFx reacts with moisture in the air to generate toxic HF gas.

In the present embodiment, in order to open the processing container to the atmosphere without generating such a toxic gas, the atmosphere is opened by the following procedure. Take The following procedure is performed under the control of the process controller 71 based on the program (recipe) stored in the memory medium of the memory unit 73. Figure 2 is a flow chart showing the procedure at this time.

After the cleaning by the ClF3 gas, first, a cycle cleaning by an inert gas such as N ₂ gas is carried out (Project 1). At this time, the N ₂ gas is supplied from both the gas and the cleaning gas supply mechanism 18 . At this time, the cycle is washed, for example, in 30 minutes, the introduction of the exhaust gas and the N ₂ gas in the processing container 2 is repeated 5 to 6 times. Thereby, the gas component in the processing container 2 is discharged.

Next, the first stage of atmospheric cleaning (Project 2) is performed. This process is carried out in order to react TiFx, which is a by-product generated during the film formation process, with moisture in the atmosphere to generate HF. In the first stage of the air-cleaning process, the air is introduced into the processing container 2 through the atmosphere introduction pipe 41, the pipe 20, and the like, and is sufficiently maintained. Time to react TiFx with moisture in the atmosphere and then vent. This is because it takes a certain amount of time until the start of the reaction, and if the period in which the atmosphere is held in the processing container 2 is too short, it is difficult to generate the above reaction, and if the first reaction is performed only once, In operation, the reaction between TiFx and moisture in the air does not proceed sufficiently.

In order to effectively carry out the reaction of TiFx with moisture in the atmosphere, it is preferable to keep the atmosphere in the processing container 2 for 5 minutes or more. However, if it is too long, the productivity will be lowered and the effect will be saturated. Therefore, the holding time is preferably 5 to 20 minutes. More ideal, the system is 10~15 Minutes, for example, 13 minutes. Moreover, it is preferable that the first operation is performed twice or more in a repeated manner, and more preferably five times or more. However, if the number of times of repetition is too large, the effect is saturated and the productivity is lowered only. Therefore, the number of times of repetition is preferably 10 or less.

In the first stage of the above-described atmospheric cleaning, the water is impregnated into the TiFx applied to the wall portion of the processing container 2, and the reaction between TiFx and water is performed. However, TiFx still remains somewhat and reacts. The generated HF gas system is not discharged and remains. In order to discharge this quickly, the second stage of atmospheric cleaning is performed (Project 3). This is a general second operation in which a plurality of times are carried out, in which the atmosphere is introduced into the processing container 2 and exhausted, and the reaction product mainly produced by the second project is discharged.

In this case, from the viewpoint of rapidly discharging HF, the second operation is performed by introducing the atmosphere into the processing container 2 and discharging it in a short time, and it is preferable to repeat the number of times. In this project, it is necessary to generate a reaction between TiFx and moisture remaining due to the introduction of the atmosphere, but the TiFx applied to the treatment container 2 is sufficiently saturated by the above-mentioned work 2. Moisture, therefore, a sufficient reaction can be produced by holding in a short time atmosphere compared to the first operation.

In the second operation of the above-described operation 3, as described above, the holding time in which the atmosphere is introduced into the processing container 2 is only required to be short, and it is preferably 1 to 5 minutes. More preferably, it is 1 to 3 minutes, for example, for 1 minute. Moreover, it is preferable that the number of such second operations is repeated over the course of 20 times or more, and more preferably, it is repeated 25 times or more. However, if the number of repetitions is too large, the effect will be saturated and only the productivity will be lowered. Therefore, it is desirable to repeat the number of times of 50 times or less.

In the air cleaning of the first stage and the second stage of the work 2 and the third stage, it is preferable to control the pressure in the processing container 2 to be equal to or lower than atmospheric pressure, for example, to be controlled at about 600 Torr. If the inside of the processing container 2 is raised to about atmospheric pressure, the HF generated in the processing container 2 may leak to the outside of the processing container 2. However, by controlling the temperature below atmospheric pressure as described above, it is possible to prevent HF. Leaked.

After the atmospheric washing is completed as described above, the inert gas, for example, the N ₂ gas is washed in an arbitrary period of time (engineering 4). This process is carried out in order to lower the temperature of the processing container 2 to about room temperature.

Then, the cover 3 is opened, and the atmosphere of the processing container 2 is opened (Engineering 5). At this time, the HF generation reaction system in the processing container 2 is almost completed by the atmospheric cleaning of the first stage and the second stage of the work 2 and the third stage, and the generation of HF from the processing container 2 can be suppressed. The limit below the limit value (TLV).

Next, an experiment for confirming the effects of the present invention will be described.

Here, after forming 5,000 or more films of the W film on which the film of Ti is formed by normal CVD or SFD, the No. 1 to 7 shown in Table 1 are used. The program was washed. In Table 1, the N2 cycle cleaning 1 is an operation in which the N ₂ gas is introduced into the processing container and exhausted, and the N ₂ gas introduction time + N ₂ gas holding time is set to 1 minute, and includes The time for leaving the N ₂ gas to be exhausted was 1 minute, and 1 cycle was set to 2 minutes, and this was repeated for 15 cycles, and the total was carried out for 0.5 hour. In addition, in the first stage, the atmosphere is washed, and the time for keeping the atmosphere in the processing container is set to 13 minutes, and the time for introducing the atmosphere for one minute and the time for exhausting for one minute are included, and the total time is 15 minutes. And repeat this for a specific number of times. The second stage of the atmosphere cleaning is set to 1 minute in the processing vessel to maintain the atmosphere, and includes 1 minute of introduction of the atmosphere and 1 minute of exhaust time, and becomes a total of 3 minutes, and This is repeated a specific number of times, and is carried out. Further, in the N2 cycle cleaning 2, the N ₂ gas introduction time + N2 gas holding time is set to 1 minute, and the time for holding the N ₂ gas for exhausting is 1 minute, and 1 cycle is set to 2 minutes, and This was done for a specific time.

The procedure of No. 1 in Table 1 is that only N ₂ cycle cleaning is performed, and the procedure of No. 2 is that after the N ₂ cycle cleaning 1 is performed, the first stage of atmospheric cleaning is not performed. In the second stage of the five-stage atmospheric cleaner, the No. 3 procedure was performed after the N ₂ cycle cleaning 1 and the first stage of the atmospheric cleaning was not performed, and 35 cycles were performed. The second stage atmospheric cleaner, No. 4, was subjected to the N ₂ cycle cleaning 1 and then the first stage of the atmosphere was washed for 5 cycles, and then the 25th cycle of the second stage atmosphere was performed. In the procedure of No. 5, after the N ₂ cycle cleaning 1 is performed, the first stage of the first stage is washed in the air, and then the second stage of the 35 cycles is washed, and further The procedure of No. 6 was carried out for 2 hours of N ₂ cycle cleaning, and after the procedure of No. 4, the N ₂ cycle was washed for 30 minutes. The procedure of No. 7 is to replace the air washing in the first stage and the second stage, and after performing the operation of holding the atmosphere in the processing container for 150 minutes once, the N ₂ cycle is washed for 45 minutes. 2 people.

After washing with these procedures, as shown in Fig. 3, generally, at a position A of 30 cm above the processing container and at a position of 50 cm (IH test position) B, by a portable gas detector (Research) The concentration of HF was measured by the meter SC-90) and the gas detecting tube. The results are shown in Table 1. Further, at a position C above the crystal holder in the processing container, the concentration of HF was also measured by a portable gas detector.

As shown in Table 1, in general, No. 1 which was not subjected to atmospheric washing was detected to have an extremely high amount of HF. Further, as is apparent from Nos. 2 and 3, even if the number of cycles of cleaning the atmosphere in the second stage is increased, the HF concentration is not sufficient when the first stage of atmospheric cleaning is not performed. The reduction. Further, as shown in No. 5, it was confirmed that when the number of cycles of atmospheric cleaning in the first stage was once, the HF concentration was not sufficiently lowered. Further, as shown in Fig. 7, in general, even if the atmospheric holding time of the atmospheric cleaning is simply increased, there is almost no effect, and the concentration level of HF immediately before the liberation of the processing container is too high, and is NG.

On the other hand, in No. 4 and 6 in which the atmosphere of the first stage was washed five times and the atmosphere of the second stage was washed 25 times, the concentration of HF after atmospheric liberation was within the allowable range. Moreover, the HF concentrations of these were in the same level, and it was confirmed that the presence or absence of the N ₂ cycle cleaning 2 did not affect the concentration of the HF gas.

Next, the change in the HF concentration in the processing container when the process of No. 4 was carried out was confirmed. The results are shown in Figure 4. As shown in the figure, in general, in the first stage of atmospheric cleaning, since the reaction between TiFx and moisture in the air is performed, the HF concentration is high, and the second stage is atmospheric washing. At the time of net, since the HF is discharged, the concentration of HF is drastically lowered.

Next, after the treatment was carried out in the procedure of No. 0034, the IH test was performed. The sampling position is the above position A. The analysis target, the analysis target collection method, the analysis device, the analysis target component, and the detection lower limit at this time are shown in Table 2. Further, the results of the IH test are shown in Table 3. Specifically, the analysis target, the allowable concentration of these, the concentration between 5 minutes after opening, and the concentration within 10 minutes after opening were displayed.

As shown in Table 3, it was confirmed that the atmosphere was washed by the present invention, and any component was able to be a detection amount equal to or lower than the allowable concentration.

Further, the present invention is not limited to the above embodiment, and various modifications can be made. For example, in the above-described embodiment, the apparatus for forming a film of CVD by CVD is described as an example in which the processing container to which TiFx is applied is opened to the atmosphere by treatment. Any treatment can be applied as long as it is treated with metal fluoride in the processing container.

[Industry use possibility]

The present invention can be applied to all applications in which a treatment container for metal fluoride is safely opened to the atmosphere.

1‧‧‧ Ontology

2‧‧‧Processing container

3‧‧‧ Cover

18‧‧‧Clean gas supply mechanism

41‧‧‧Atmospheric introduction piping

50‧‧‧ gas box

70‧‧‧Exhaust mechanism

71‧‧‧Process Controller

73‧‧‧Memory Department

100‧‧‧CVD film forming device

Fig. 1 is a schematic cross section of a CVD film forming apparatus used in an atmosphere opening method according to an embodiment of the present invention.

Fig. 2 is a flow chart for explaining the atmospheric opening procedure of the processing container in the apparatus of Fig. 1.

[Fig. 3] for explaining the position of gas concentration measurement inside and outside the processing container Stereo picture.

Fig. 4 is a graph showing changes in the concentration of HF gas in a processing vessel at the time of atmospheric cleaning in the range of the present invention.

Claims (8)

An atmosphere opening method for processing a container is an atmosphere opening method of a processing container in which a treatment container having a metal fluoride is opened in the atmosphere, which is subjected to a specific treatment therein, characterized in that the plurality of times are repeated in the foregoing Introducing the atmosphere into the processing vessel, and maintaining a sufficient time for the metal fluoride to react with the moisture in the atmosphere, and then performing the first operation of exhausting, and then repeatedly introducing the atmosphere into the processing container repeatedly, and a second operation for discharging the reaction product mainly generated by the first operation, and the first operation is to set the holding time to 5 minutes or longer, and the second operation is performed. The hold time in the state where the atmosphere is introduced is set to 1 to 3 minutes. The atmosphere opening method of the processing container according to the first aspect of the invention, wherein the first operation is performed by setting the holding time to 5 to 20 minutes. The method for opening an atmosphere of a processing container according to the first or second aspect of the invention, wherein the first operation is repeated 2 to 10 times. The method for opening an atmosphere of a processing container according to the first or second aspect of the invention, wherein the second operation is repeated 20 times or more. The method for opening an atmosphere of a processing container according to the first or second aspect of the invention, wherein the processing is a CVD film forming process, The metal fluoride is TiFx. An atmosphere opening method for processing a container is an atmosphere opening method in which a processing container in which a CVD treatment is performed and a treatment container having TiFx is opened in the atmosphere is used, and is characterized in that the processing container is repeatedly performed five times or more. Introducing the atmosphere, maintaining a sufficient time for the TiFx to react with the moisture in the atmosphere to generate HF, and then performing the first operation of the exhaust gas, and then repeatedly introducing the atmosphere into the processing container 25 times or more. The second operation of discharging the HF generated mainly by the first operation, and the first operation is to set the holding time to 5 minutes or longer, and the second operation is introduced. The holding time in the atmospheric state is set to 1 to 3 minutes. The method for opening an atmosphere of a processing container according to any one of claims 1 to 2, wherein the processing container is washed with an inert gas before the first operation. net. A memory medium is a memory medium for storing a program for controlling a processing device operating on a computer, wherein the control program is executed to perform the first and second aspects of the patent application range as described above. The method of the method according to any one of the preceding claims, wherein the processing device is controlled by a computer.