JP2009213946A - Surface treatment apparatus - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a surface treatment apparatus which can suppress impairs of members or the like constituting the apparatus, and a processing unevenness of an object to be treated. <P>SOLUTION: The surface treatment apparatus 100 includes a diluent gas supply unit 1 supplying a diluent gas, a fluorine gas supply unit 2 supplying a fluorine gas, a mixer 5 mixing the diluent gas and the fluorine gas to produce a mixed gas, and a reactor vessel 6 contacting the object to be treated with the mixed gas, and is characterized by comprising further a heating means 8 heating the diluent gas. <P>COPYRIGHT: (C)2009,JPO&INPIT

Description

  The present invention relates to a surface treatment apparatus that performs surface treatment, surface modification, etc. of a sample using fluorine gas.

  2. Description of the Related Art Conventionally, surface modification or surface treatment for treating an organic substance or the like with a fluorine gas has been performed. The surface treatment apparatus disclosed in Patent Document 1 is connected by a gas adjustment tank having a supply pipe communicating with a fluorine gas source and an inert gas source, and the gas adjustment tank and a gas conduit. The apparatus includes a treatment tank and an exhaust gas treatment apparatus, and is suitable for small-scale surface treatment and surface treatment performed using dilute fluorine gas.

JP 2000-319433 A

  Here, when surface treatment is performed using a treatment tank with a large capacity, processing unevenness may easily occur due to the influence of the filling position of the object to be treated, the gas flow path, gas stagnation, etc. in the treatment tank. It was. As a method for preventing this processing unevenness, for example, there is a method of performing a surface treatment under a heated condition, and there is a method in which a processing tank is provided with a heating means for heating an object to be processed to a predetermined temperature. However, even in such an apparatus, a temperature difference may occur between the object to be processed and the mixed gas supplied to process the object to be processed in the processing tank, resulting in processing unevenness. . Moreover, when the mixed gas is introduced into the treatment tank, the reaction is started immediately after the start of the mixed gas introduction by the highly reactive fluorine gas contained in the mixed gas, which may cause uneven processing. In particular, when the capacity of the treatment tank is large, the surface treatment is started from the vicinity of the gas introduction part before the mixed gas is uniformly diffused into the treatment tank and the conditions in the treatment tank become uniform, and uneven processing is caused. There was a risk of it occurring. In order to reduce such a problem, a preheated mixed gas is supplied to the treatment tank so that a temperature difference between the object to be treated and the mixed gas is less likely to occur, but in a short flow path to the reactor It is necessary to heat the mixed gas in a short time, and further, it is necessary to heat the mixed gas from the outside of the pipe through which the gas flows at a high temperature added to the desired heating (treatment) temperature by several tens of degrees. For this reason, the temperature of the fluorine gas contained in the mixed gas rises rapidly, and the reactivity of the fluorine gas is further increased to a high temperature, so that a metal member used for a gas conduit or a valve, Even if a resin material used as a packing or the like is formed using a material having high corrosion resistance, there is a risk of local damage such as corrosion due to its high reactivity.

  Then, an object of this invention is to provide the surface treatment apparatus which can suppress damage to the member etc. which comprise an apparatus, and the process nonuniformity of a to-be-processed object.

Means and effects for solving the problems

  A surface treatment apparatus according to the present invention includes a dilution gas supply device that supplies a dilution gas, a fluorine gas supply device that supplies a fluorine gas, and a mixer that generates a mixed gas by mixing the dilution gas and the fluorine gas. And a reactor for contacting the object to be treated with the mixed gas, further comprising a heating means for heating the dilution gas. In particular, it is preferable that the heating means heats the dilution gas before mixing the dilution gas and the fluorine gas.

  According to the above configuration, since the diluted gas can be heated by the heater and the heated diluted gas and the fluorine gas can be mixed, the fluorine gas is less likely to be heated to an unnecessarily high temperature, and the members constituting the apparatus. It is possible to prevent damage such as corrosion from occurring. Further, since the heated mixed gas can be supplied to the reactor, it is possible to provide a surface treatment apparatus that can suppress the occurrence of processing unevenness of the object to be processed.

  The surface treatment apparatus of the present invention preferably further includes an ejector that sucks in the fluorine gas using the dilution gas as a drive source. Here, the ejector is a device that can draw gas in a reduced pressure state by increasing the flow velocity.

  According to the above configuration, the ejector can draw the fluorine gas from the fluorine gas supply device using the dilution gas as the drive source. Thereby, since the supply pressure of fluorine gas can be reduced, high-pressure storage of fluorine gas can be suppressed, and fluorine gas can be stored and used more safely. In addition, it is possible to supply fluorine gas in a more accurate amount, which is less supplied than the dilution gas.

  In the surface treatment apparatus of the present invention, the first flow rate adjusting means connected to the dilution gas supply device and the mixer via a pipe, and upstream and downstream of the first flow rate adjusting means. A pressure control valve connected via a pipe to the pressure gauge provided and the pressure gauge provided upstream of the dilution gas supply device and the first flow rate adjustment means; Is preferred.

  According to the above configuration, since the first flow rate adjusting unit can be applied with a constant driving differential pressure by the pressure adjusting valve, the piping provided on the downstream side of the dilution gas supply device and the first flow rate adjusting unit, The dilution gas can be supplied at a constant flow rate regardless of the influence of pressure such as the reactor internal pressure. In addition, as a 1st flow volume adjustment means, a mass flow controller etc. can be used, for example. Here, the mass flow controller accurately controls the mass flow rate of gas with an electric signal. Therefore, since the mass flow rate of the dilution gas can be controlled, the flow rate of the dilution gas can be controlled more accurately and stably without being affected by the temperature and supply pressure.

  The surface treatment apparatus of the present invention further includes a pressure buffering tank provided between the pressure adjusting valve and the pressure gauge provided on the upstream side of the first flow rate adjusting means. Preferably it is.

  According to the above configuration, the pressure buffering tank can relieve the mutual influence between the pressure adjusting valve and the valve provided in the first flow rate adjusting means, thereby further improving the flow rate accuracy.

  Moreover, in the surface treatment apparatus of this invention, it is preferable to further provide the 2nd flow volume adjustment means connected to the said fluorine gas supply apparatus and the said mixer via piping.

  According to the above configuration, since the mass flow rate of the fluorine gas can be accurately controlled by the electric signal by the second flow rate adjusting means, more accurate and stable flow control of the fluorine gas without being affected by the temperature and supply pressure. Is possible. As the second flow rate adjusting means, for example, a mass flow controller or the like can be used in the same manner as the first flow rate adjusting means.

  Moreover, in the surface treatment apparatus of the present invention, the first communication pipe communicating with the mixer, the back pressure valve provided in the middle of the first communication pipe, and the middle between the first communication, A gas release valve provided on the downstream side of the back pressure valve, a second communication pipe connecting the mixer and the reactor, and a gas provided in the middle of the second communication pipe It is preferable to further include an introduction valve.

  According to the above configuration, the gas introduction valve is closed and the gas release valve is opened until the drive differential pressure for generating a sufficient vacuum in the ejector is generated and the flow rate of the dilution gas is stabilized, and dilution is performed through the first communication pipe. Gas, or diluent gas and fluorine gas can be released. Then, after the flow rate of the dilution gas is stabilized, the gas release valve is closed and the gas introduction valve is opened, so that the mixed gas can be guided to the reactor through the second communication pipe. Thus, when supplying the mixed gas to the reactor, it is possible to supply the mixed gas whose flow rate and concentration are adjusted to be constant immediately after the start of supply.

  Moreover, in the surface treatment apparatus of this invention, it is preferable to further provide the heating chamber which heats the said to-be-processed object.

  According to the above configuration, since the object to be processed can be heated in the heating chamber in advance before being brought into contact with the mixed gas, processing unevenness and inappropriate processing can be suppressed. In addition, by heating the object to be processed in advance, the heating time of the object to be processed in the reactor can be shortened, the cost can be suppressed, and the processing efficiency can be further improved.

  Moreover, in the surface treatment apparatus of this invention, it is preferable to further provide the movable member which has the corrosion resistance with respect to the said fluorine gas which can convey the said to-be-processed object to the said reactor.

  According to the said structure, a to-be-processed object can be easily conveyed and carried out to a reactor, and it can suppress that the influence of generation | occurrence | production of an impurity from a movable member, etc. arises with the fluorine gas contained in mixed gas.

  In the surface treatment apparatus of the present invention, the reactor further includes a plate-like member provided between the object to be treated and the mixed gas supplied to the reactor. It is preferable. As another viewpoint, the plate member may be provided on the movable member between the object to be processed and the mixed gas flowing into the reactor.

  According to the above configuration, the mixed gas is less likely to come into direct contact with the object to be processed in the vicinity of the mixed gas introduction unit in the reactor. Processing can be performed uniformly.

  Hereinafter, embodiments of the surface treatment apparatus according to the present invention will be described. FIG. 1 is a schematic configuration diagram of a main part of a surface treatment apparatus according to an embodiment of the present invention, and FIG. 2 is a schematic cross-sectional view of a reactor of the surface treatment apparatus according to an embodiment of the present invention.

  In FIG. 1, a surface treatment apparatus 100 includes a dilution gas supply device 1, a fluorine gas supply device 2, a mass flow controller (first flow rate adjusting means) 3a connected to the dilution gas generation device 1 via a pipe, A mass flow controller (second flow rate adjusting means) 3b connected to the fluorine gas supply device 2 via piping, an ejector 4 connected to the mass flow controllers 3a and 3b via piping, and the ejector 4 and piping Are connected to each other through a mixer 5 provided on the downstream side of the ejector 4, a reactor 6 that treats an object to be processed with a mixed gas supplied from the mixer 5, and a gas guided from the reactor 6. And a detoxifying device 7 for detoxifying the fluorine gas and hydrogen fluoride gas contained in the mass flow controller 3a Heaters (heating means) 8 is further provided between the ejector 4. In addition, pressure gauges 9 and 10 are provided on the upstream side and the downstream side of the mass flow controller 3a, respectively, and a pressure adjusting valve 11 and a pressure buffering tank 12 are provided further upstream of the pressure gauge 9. Yes. A second communication pipe 16 communicating with the mixer 5 and the reactor 6, a gas introduction valve 17 provided in the middle of the second communication pipe 16, and a branch from the middle of the second communication pipe 16 are branched. And a back pressure valve 14 and a gas release valve 15 provided in the middle of the first communication pipe 13 are further provided.

  The dilution gas supply device 1 is a device that supplies an inert gas for diluting the fluorine gas. Examples of the dilution gas include nitrogen gas, oxygen gas, and argon gas, but are not limited to these gases.

  The fluorine gas supply device 2 supplies fluorine gas. For example, a fluorine gas generation device that supplies hydrogen fluoride from a hydrogen fluoride supply device (not shown) or the like to electrolyze and generate fluorine gas, or fluorine Examples thereof include a gas cylinder filled with gas.

  The mass flow controllers (first flow rate adjusting means, second flow rate adjusting means) 3a, 3b are for accurately controlling the mass flow rate of the gas with an electric signal. As a result, the dilution gas and fluorine gas flow rates can be controlled more accurately and stably without being affected by temperature and supply pressure. The mass flow controllers 3a and 3b require a main body inlet / outlet gas pressure difference of 0.05 to 0.10 MPa in order to control the flow rate. Without this pressure difference, the flow rate cannot be accurately controlled due to the pressure loss inside the mass flow controllers 3a and 3b. For this purpose, the dilution gas and the fluorine gas supplied via the mass flow controllers 3a and 3b are used for the treatment pressure (for example, atmospheric pressure) of the reactor 6 provided downstream of the mass flow controllers 3a and 3b, and the mass flow. The pressure loss (for example, 0.05 to 0.10 MPa) of the controllers 3a and 3b and the difference necessary for extruding a necessary amount of dilution gas or fluorine gas from the dilution gas supply device 1 or fluorine gas supply device 2 as the supply source If the inlet pressure (for example, atmospheric pressure +0.10 to 0.20 MPa) equal to or higher than the total pressure (for example, 0.05 to 0.10 MPa) is not generated, normal dilution gas or fluorine gas is supplied. It will not be possible. Therefore, when the ejector 4 and the mass flow controllers 3a and 3b are combined, the outlet pressure of the mass flow controllers 3a and 3b can be lowered by the suction ability of the ejector 4, and the pressure of the reactor 6 does not affect at this time. As a result, the pressure required for driving the mass flow controllers 3a and 3b can be reduced. Therefore, the holding / supply pressure of fluorine gas can be reduced by the capacity of the ejector. Fluorine gas is a highly reactive gas, and if the holding pressure can be reduced, the risk of corrosion and gas leakage can be reduced accordingly.

  The ejector 4 is an instrument for drawing gas in a reduced pressure state by increasing the flow velocity. The ejector 4 can reliably draw fluorine gas using the dilution gas as a driving source, and the drawn gas is guided to the mixer 5. Here, instead of the ejector 4, for example, a vacuum generator or the like may be used. By providing the ejector 4, the fluorine gas supply device 2 can supply fluorine gas without any problem even when the pressure upper limit is 200 kPa or less, and the lower limit can be used up to -65 kPa (G).

  The mixer 5 mixes the dilution gas and the fluorine gas drawn by the ejector 4 and introduces them to the reactor 6. In the ejector 4, the mixed gas can also be generated by drawing in the fluorine gas using the diluent gas as a drive source.

  The reactor 6 receives a mixed gas of a dilution gas and a fluorine gas, and performs surface treatment and modification of the object to be processed. Here, the reactor 6 will be described in detail with reference to FIG. 2. The reactor 6 has a mixed gas supply port 18 and a mixed gas discharge port 19. A processed product 21 and a movable member 22 are disposed. A heating chamber 23 is provided in parallel with the reactor 6.

  The plate-like member 20 is erected in the reactor 6 between the mixed gas supply port 18 and the workpiece 21 so as to block the supplied gas. The plate-like member 20 may be provided on the movable member 22 or may be removable. The plate-like member 20 makes it difficult for the mixed gas to come into direct contact with the workpiece 21 in the vicinity of the mixed gas supply port 18 in the reactor 6, thereby preventing processing unevenness and inappropriate processing from occurring.

  The movable member 22 can move the workpiece 21 into or out of the reactor 6, and is made of a metal material having corrosion resistance against fluorine gas, for example, a mesh or punching metal using stainless steel or the like. Those used are preferred. Moreover, although the wheel is attached to the movable member 22, you may use the thing to which a wheel etc. are not attached as one modification. As another modification, the metal material may have a mesh or punching metal, a metal frame, and a wheel.

  The heating chamber 23 is provided for heating the workpiece 21 in advance before bringing the workpiece 21 into contact with the mixed gas. Here, since the workpiece 21 is preferably processed in contact with the mixed gas in a heated state, the workpiece 21 is preferably transferred from the heating chamber 23 to the reactor 6 quickly. Therefore, the heating chamber 23 is preferably provided in the vicinity of the reactor 6, and the heating chamber 23 and the reactor 6 may communicate with each other. Here, as a modified example, one in which the heating chamber 23 and the reactor 6 are provided adjacent to each other, or one in which the heating chamber 23 is provided in the reactor 6 may be used.

  The detoxification device 7 removes hydrogen fluoride gas, fluorine gas, and the like generated from the surface of the workpiece 21 in the surface treatment of the reactor 6 to render the gas harmless. The gas from which the fluorine gas and the hydrogen fluoride gas have been removed in the detoxifying apparatus 7 is discharged out of the surface treatment apparatus 100. In addition, in order to remove fluorine gas and hydrogen fluoride gas, for example, one filled with soda lime or the like may be used.

  The heater (heating means) 8 is provided in the middle of a pipe connecting the dilution gas supply device 1 and the ejector 4, and heats the dilution gas supplied from the dilution gas supply device 1. It is. The dilution gas is heated before the dilution gas and the fluorine gas are mixed. As the heater (heating means) 8, for example, a heater or the like can be used.

  The pressure gauge 9 measures the pressure on the upstream side of the mass flow controller 3a, and is provided on the upstream side of the mass flow controller 3a. The pressure gauge 10 measures the pressure on the downstream side of the mass flow controller 3a, and is provided on the downstream side of the mass flow controller 3a.

  The pressure adjusting valve 11 applies a constant driving differential pressure to the mass flow controller 3a in accordance with the difference between the pressure value of the pressure gauge 9 and the pressure value of the pressure gauge 10, and is connected to the dilution gas supply device 1 and the pressure. A pipe is provided between the buffer tank 12 and the buffer tank 12. As a result, the pressure adjusting valve 11 includes the maximum value of the pressure applied to the downstream side from the ejector 4, the drive differential pressure of the ejector 4, the drive differential pressure of the mass flow controller 3 a, and the elements constituting the surface treatment apparatus 100. The dilution gas can be supplied at a pressure equal to or higher than the sum of the pressure loss values. Further, when the dilution gas (flow rate) is supplied by being fixed by the mass flow controller 3a, no differential pressure is generated on the upstream side and the downstream side of the ejector 4, and pressure is generated only when the dilution gas is supplied. . For this reason, the differential pressure on the upstream side and downstream side of the mass flow controller 3a before the dilution gas supply often exceeds the drive differential pressure, and a valve (not shown) provided in the mass flow controller 3a is closed. Gas may not be supplied. In this case, the dilution gas flow rate can be adjusted by the pressure adjusting valve 11, and the dilution gas can be supplied by applying a constant driving differential pressure to the upstream side and the downstream side of the mass flow controller 3a.

  Here, the hunting phenomenon between the valve provided in the mass flow controller 3a and the pressure adjusting valve 11 will be described in detail. When the dilution gas flow rate is small, the valve provided in the mass flow controller 3a is opened, and the flow rate increases while the drive differential pressure decreases. As a result, the pressure adjusting valve 11 is opened to secure the pressure and the pressure increases, but the flow rate of the dilution gas exceeds the set value, and the valve (not shown) provided in the mass flow controller 3a is closed. Then, the drive differential pressure increases and the pressure adjusting valve 11 is closed. As a result, the drive differential pressure decreases, but the dilution gas flow rate also decreases.

  The pressure buffer tank 12 is provided between the pressure adjusting valve 11 and the pressure gauge 9 via a pipe, and can store the dilution gas supplied from the dilution gas supply device 1. For example, when a valve (not shown) provided in the mass flow controller 3a and the pressure adjusting valve 11 cause hunting due to a combination of a set flow rate, a piping system, a supply pressure, a response speed of a selected device, and the like, It is possible to suppress a decrease in flow rate accuracy. By this pressure buffering tank 12, the mutual influence between a valve (not shown) provided in the mass flow controller 3a and the pressure adjusting valve 11 is alleviated, and the flow rate accuracy of the dilution gas can be further improved.

  The first communication pipe 13 is a pipe through which the dilution gas drawn by the ejector 4 and passed through the mixer, or the dilution gas and the fluorine gas passes, and is branched from the second communication pipe 16. Further, in the middle of the first communication pipe 13, a back pressure valve 14 and a gas release valve 15 are provided further downstream of the back pressure valve 14. In the first communication pipe 13, the further downstream side of the gas release valve 15 is led to the abatement apparatus 7.

  The back pressure valve 14 is a valve for keeping the pressure of the fluid passing through the valve constant, and the gas whose pressure is adjusted by the back pressure valve 14 passes through the gas release valve 15 and is guided to the abatement device 7. The pressure of the dilution gas and / or fluorine gas drawn by the ejector 4 and passing through the mixer 5 is adjusted to be constant by the back pressure valve 14. Here, the set pressure value of the back pressure valve 14 is preferably measured in advance as a pressure stable value on the downstream side of the ejector 4 when the flow rate of the dilution gas set by the mass flow controller 3a is introduced into the reactor 6. Value. If this value is set, when supplying the mixed gas to the reactor 6, the mixed gas whose flow rate and concentration are controlled to be constant can be supplied to the reactor 6 immediately after the start of supply. More preferably, it is a value obtained by measuring in advance the pressure stable value on the downstream side of the ejector 4 when the set flow rate of the mixed gas is introduced into the reactor 6. If this value is set, the flow and concentration management accuracy can be further improved.

  The gas release valve 15 is opened until the flow rate of the dilution gas is stabilized, and is closed when the flow rate of the dilution gas is stabilized. This is because the drive differential pressure is required to generate a sufficient vacuum in the ejector 4, and immediately after the dilution gas is supplied, the pressure increase gradually occurs until the drive differential pressure is reached, so that the flow rate of the dilution gas is stabilized. This is because it takes time. Since the pressure fluctuation of the fluorine gas is small in the fluorine gas supply device 2, the flow rate is instantaneously stabilized when the supply is started. When the gas release valve 15 is opened, the dilution gas and / or the mixed gas are guided to the abatement apparatus 7. On the other hand, when the gas release valve 15 is closed, the dilution gas and / or the mixed gas are guided to the reactor 6 through the second communication pipe 16.

  The second communication pipe 16 is a pipe that guides the dilution gas and the fluorine gas to the reactor 6 after the flow rate of the dilution gas is stabilized.

  The gas introduction valve 17 is opened after the flow rate of the dilution gas is stabilized and a sufficient degree of vacuum is obtained, and is opened at the same time as the gas release valve 15 is closed. It is closed until the flow rate of the dilution gas is stabilized.

  The gas release valve 15 and the gas introduction valve 17 instantaneously close the gas release valve 15 and open the gas introduction valve 17 when the flow rate of the dilution gas is stabilized and a sufficient degree of vacuum is obtained in the ejector 4. Dilution gas and fluorine gas change the path from the first communication pipe 13 to the second communication pipe 16 and are led to the reactor 6. At this time, since the switching between the gas release valve 15 and the gas introduction valve 17 is performed instantaneously, the flow rate of the dilution gas and the fluorine gas and the disturbance in the degree of vacuum are extremely small. In the fluorine gas supply device 2, since the pressure fluctuation is small, when the supply is started, the flow rate of the fluorine gas is instantaneously stabilized. Therefore, it is preferable to start supplying fluorine gas simultaneously with switching between the gas release valve 15 and the gas introduction valve 17. In this case, what has been measured in advance for the pressure stable value downstream of the ejector 4 when the flow rate of the dilution gas set by the mass flow controller 3a is introduced into the reactor 6 is set in the back pressure valve 14. It is preferable. Further, only the dilution gas is supplied first, and the fluorine gas is supplied before switching between the gas release valve 15 and the gas introduction valve 17, and the mixed gas whose flow rate and concentration are controlled to be constant is supplied to the first communication pipe. Then, the gas release valve 15 may be closed and the gas introduction valve 17 may be opened. If it does in this way, the mixed gas by which the precision of the flow volume and the density | concentration was managed further can be supplied to the reactor 6. FIG. In this case, it is preferable to set in the back pressure valve 14 a pressure stable value measured in advance on the downstream side of the ejector 4 when the set flow rate of the mixed gas is introduced into the reactor 6.

  Next, the operation of the surface treatment apparatus 100 will be described. The dilution gas supplied from the dilution gas supply device 1 is guided to the pressure buffer tank 12 through the pressure adjustment valve 11 when the pressure adjustment valve 11 is opened. A part of the dilution gas is stored in the pressure buffer tank 12, and the other dilution gas is guided to the mass flow controller 3 a via the pressure gauge 9. In the mass flow controller 3 a, the mass flow rate is controlled, and the diluted gas whose flow rate is adjusted is led to the heater 8 via the pressure gauge 10.

  Here, when the pressure adjusting valve 11 is open, the difference in pressure value between the pressure gauge 9 on the upstream side of the mass flow controller 3a and the pressure gauge 10 on the downstream side is low, that is, the mass flow controller 3a. This is a case where no driving differential pressure is generated. On the other hand, when the pressure adjustment valve 11 is closed, the dilution gas supplied from the dilution gas supply device 1 is blocked by the pressure adjustment valve 11 and is not led to the pressure buffer tank 12. When the pressure adjusting valve 11 is closed, the pressure difference between the pressure gauge 9 on the upstream side of the mass flow controller 3a and the pressure gauge 10 on the downstream side is high, that is, the driving difference of the mass flow controller 3a. This is the case when pressure is generated. In this case, the dilution gas stored in the pressure buffer tank 12 is guided to the mass flow controller 3a.

  On the other hand, from the fluorine gas supply device 2, the fluorine gas is drawn by the ejector 4 through the mass flow controller 3 b using the dilution gas as a drive source. Similarly to the diluent gas, the mass flow controller 3b controls the mass flow rate of the fluorine gas, and the diluted gas whose flow rate is adjusted is drawn by the ejector 4. And the dilution gas and fluorine gas heated in the heater 8 are guide | induced to the mixer 5, and are mixed in the mixer 5, and the mixed gas of dilution gas and fluorine gas is produced | generated.

  Thereafter, the mixed gas is guided to the second communication pipe 16. Here, initially, the gas introduction valve 17 is closed and the gas release valve 15 is opened until the flow rate of the dilution gas is stabilized, and the dilution gas and / or the fluorine gas is guided to the first communication pipe 13. The pressure of the dilution gas and / or the fluorine gas guided to the first communication pipe 13 is adjusted by the back pressure valve 14, and then passes through the gas release valve 15 and is guided to the abatement apparatus 7.

  When the flow rate of the dilution gas is stabilized and a sufficient degree of vacuum is obtained in the ejector 4, the gas release valve 15 is instantaneously closed and the gas introduction valve 17 is opened. The flow path is changed from the communication pipe 13 to pass through the second communication pipe 16 and led to the reactor 6.

  In the reactor 6, an object to be processed 21 (see the dotted line diagram in FIG. 2) preliminarily heated in the heating chamber 23 is conveyed and arranged by the movable member 22. Then, the mixed gas supplied from the mixed gas supply port 18 collides with the plate-like member 20 in the reactor 6 and comes into contact with the object 21 to be subjected to surface treatment or surface modification. Thereafter, when a predetermined processing time elapses, the gas in the reactor 6 is discharged from the mixed gas discharge port 19 and guided to the detoxifying device 7, and the detoxifying device 7 detoxifies the fluorine gas and the hydrogen fluoride gas. And discharged to the outside of the surface treatment apparatus 100.

  According to the present embodiment, before the dilution gas and the fluorine gas are mixed, the dilution gas can be heated in advance by the heater 8, and the heated dilution gas and the fluorine gas can be mixed. Thereby, it becomes difficult for fluorine gas to become high temperature more than needed, and it can suppress that damage, such as corrosion of the member etc. which comprise the surface treatment apparatus 100 by fluorine gas, arises. Moreover, since the heated mixed gas can be supplied to the reactor 6, it can suppress that the process nonuniformity of the to-be-processed object 21 arises.

  Further, the ejector 4 can draw the fluorine gas from the fluorine gas supply device 2 using the dilution gas as a drive source. Thereby, since the supply pressure of fluorine gas can be reduced, high-pressure storage of fluorine gas can be suppressed, and fluorine gas can be stored and used more safely. In addition, it is possible to supply fluorine gas in a more accurate amount, which is less supplied than the dilution gas.

  In addition, since a constant driving differential pressure can be applied to the mass flow controller 3a by the pressure adjusting valve 11, piping provided on the downstream side of the dilution gas supply device 1 and the mass flow controller 3a, the internal pressure of the reactor 6, etc. Regardless of the influence of pressure, the dilution gas can be supplied at a constant flow rate. Furthermore, the pressure buffering tank 12 can further reduce the mutual influence between the pressure adjusting valve 11 and a valve (not shown) provided in the mass flow controller 3a, thereby further improving the flow rate accuracy. By using the mass flow controller 3a, accurate and stable gas flow rate control is possible without being affected by temperature and supply pressure.

  Further, since the mass flow rate of the fluorine gas can be accurately controlled by the electric signal by the mass flow controller 3b, the flow rate of the fluorine gas can be accurately and stably controlled without being influenced by the temperature and the supply pressure.

  Further, the gas introduction valve 17 is closed and the gas release valve 15 is opened until the drive differential pressure for generating a sufficient vacuum in the ejector 4 is generated and the flow rate of the dilution gas is stabilized. Gas and / or fluorine gas can be released to the abatement device 7 or the like. Then, after the flow rate of the dilution gas is stabilized, the gas release valve 15 is closed and the gas introduction valve 17 is opened so that the mixed gas can be guided to the reactor 6 through the second communication pipe 16. Thereby, when supplying mixed gas to the reactor 6, the mixed gas by which the flow volume and density | concentration were adjusted uniformly can be supplied immediately after supply start.

  Moreover, since the to-be-processed object 21 can be previously heated in the heating chamber 23 before making it contact with mixed gas, a process nonuniformity and improper process can be suppressed. Moreover, by heating the to-be-processed object 21 beforehand, the heating time of the to-be-processed object 21 in the reactor 6 can be shortened, cost can be held down, and processing efficiency can further be improved.

  Further, since the movable member 22 using a metal material having corrosion resistance for the fluorine gas is used, the workpiece 21 can be easily transported and carried out to the reactor 6, and the fluorine contained in the mixed gas can be used. It is possible to prevent the gas from causing an influence such as generation of impurities from the movable member 22.

  In addition, since the plate-like member 20 is provided between the workpiece 21 and the mixed gas supplied to the reactor 6, the mixed gas is treated in the vicinity of the mixed gas introduction part in the reactor 6. It becomes difficult to come into direct contact with the object 21, it is possible to suppress the processing unevenness of the object 21 to be processed, and the object 21 can be uniformly processed.

  Next, a modification of the reactor according to this embodiment will be described. FIG. 3 is a view showing a modification of the reactor of FIG.

  As shown in FIG. 3, a plate member 43 is further provided in the reactor 36, and the reaction chamber 36 a and the heating chamber 36 b are formed by the plate member 43. The mixed gas supply port 38, the mixed gas discharge port 39, the plate member 40, the workpiece 41, and the movable member 42 are the mixed gas supply port 18 and the mixed gas discharge port according to the above embodiment. 19, the plate-like member 20, the workpiece 21, and the movable member 22. The parts designated by reference numerals 18 to 22 in the above embodiment, and the reference numerals 38 to 42 in this modification example. Since each part touched is the same in order, description may be omitted.

  If the reactor 36 having the above-described configuration is used in place of the reactor 6 and the heating chamber 23 in the surface treatment apparatus 100, the same effect as that of the surface treatment apparatus 100 can be obtained, and the reaction chamber 36a and the heating chamber 36b can be obtained. Since they are provided adjacent to each other, the object to be processed can be moved to the reaction chamber 36a earlier after being heated in the heating chamber 36b. Here, if the plate-like member 43 can be removed, it can be moved to the reaction chamber 36a more easily. The plate-like member 43 may be removable or may not be removable. Further, for example, an openable / closable opening that communicates between the reaction chamber 36a and the heating chamber 36b may be provided. With such a configuration, the workpiece 41 can be moved from the heating chamber 36b to the reaction chamber 36a using the opening.

  The surface treatment apparatus according to the embodiment of the present invention has been described above. However, the present invention is not limited to the above-described embodiment, and various modifications are possible as long as they are described in the claims. For example, in this embodiment, the heat insulating material may be provided in the middle of the communication pipe between the ejector and the mixer or in the pipe on the downstream side of the mixer. By this heat insulating material, it becomes difficult to be affected by the outside air temperature, and the mixed gas can be supplied to the reactor at a high temperature. As a result, it is possible to suppress the occurrence of processing unevenness and the like, and to further improve the processing efficiency.

  In this embodiment, two or more reactors may be provided. In the surface treatment apparatus in this case, at least one reactor may be used as a reactor, and another reactor may be used as a heating chamber.

  Moreover, in this embodiment, the valve | bulb which can interrupt | block each apparatus which comprises a surface treatment apparatus may be further provided. An automatic valve, a manual valve, or the like may be used for part or all of this valve.

  In this embodiment, the plate member provided between the mixed gas and the object to be processed may be removable, or may be fixed to the reactor or the movable member.

  In the present embodiment, an exhaust device or the like may be further provided between the reactor and the abatement apparatus. The exhaust device facilitates exhaust of the mixed gas from the reactor.

  Moreover, in this embodiment, the piping which guide | induces the gas discharged | emitted from a reactor to a fluorine supply apparatus and a dilution gas supply apparatus may be further provided. Thereby, while being able to use again the fluorine gas and dilution gas which are contained in the gas discharged | emitted from the reactor, the quantity of the fluorine gas processed in an abatement apparatus can be reduced.

It is the schematic of the principal part of the surface treatment apparatus which concerns on embodiment of this invention. It is a cross-sectional schematic diagram of the reactor of the surface treatment apparatus which concerns on embodiment of this invention. It is the schematic of the reactor which concerns on the other modification of the surface treatment apparatus which concerns on embodiment of this invention.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 Dilution gas supply apparatus 2 Fluorine gas supply apparatus 3a, 3b Mass flow controller 4 Ejector 5 Mixer 6, 36 Reactor 7 Detoxification apparatus 8 Heater 9, 10 Pressure gauge 11 Pressure control valve 12 Pressure buffer tank 13 1st Communication pipe 14 Back pressure valve 15 Gas release valve 16 Second communication pipe 17 Gas introduction valve 18, 38 Mixed gas supply port 19, 39 Mixed gas discharge port 20, 40, 43 Plate member 21, 41 Workpiece 22, 42 Movable Member 23, 36b Heating chamber 36a Reaction chamber 100 Surface treatment apparatus

Claims (11)

A dilution gas supply device for supplying the dilution gas;
A fluorine gas supply device for supplying fluorine gas;
A mixer for mixing the dilution gas and the fluorine gas to generate a mixed gas;
A surface treatment apparatus comprising a reactor for contacting an object to be treated with the mixed gas,
The surface treatment apparatus further comprising heating means for heating the dilution gas.   The surface treatment apparatus, wherein the heating means heats the dilution gas before mixing the dilution gas and the fluorine gas.   The surface treatment apparatus according to claim 1, further comprising an ejector that sucks the fluorine gas using the dilution gas as a driving source. First flow rate adjusting means connected to the dilution gas supply device and the mixer;
Pressure gauges provided on the upstream side and the downstream side of the first flow rate adjusting means;
The pressure control valve further connected via the piping to the said dilution gas supply apparatus and the pressure gauge provided in the upstream of the said 1st flow volume adjustment means, The 1st characterized by the above-mentioned. 4. The surface treatment apparatus according to any one of 3 above.   5. A pressure buffering tank provided between the pressure adjusting valve and the pressure gauge provided upstream of the first flow rate adjusting means is further provided. The surface treatment apparatus according to any one of the above.   The surface treatment apparatus according to claim 1, further comprising a second flow rate adjusting unit connected to the fluorine gas supply device and the mixer. A first communication pipe communicating with the mixer;
A back pressure valve provided in the middle of the first communication pipe;
A gas release valve provided on the downstream side of the back pressure valve in the middle of the first communication;
A second communication pipe connecting the mixer and the reactor;
The surface treatment apparatus according to claim 1, further comprising a gas introduction valve provided in the middle of the second communication pipe.   The surface treatment apparatus according to claim 1, further comprising a heating chamber for heating the object to be processed.   The surface treatment apparatus according to claim 1, further comprising a movable member having corrosion resistance to the fluorine gas, which can transport the object to be treated to the reactor.   In the said reactor, it further has the plate-shaped member provided between the said to-be-processed object and the said mixed gas supplied to the said reactor, The any one of Claims 1-9 characterized by the above-mentioned. 2. The surface treatment apparatus according to item 1.   The surface treatment according to claim 9, further comprising a plate-like member provided between the object to be treated and the mixed gas flowing into the reactor on the movable member. apparatus.

Images