JP2010094572A - Method and apparatus for obtaining functional gas continuously - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a method for producing a functional gas continuously by a thermal reaction of a plurality of gaseous raw materials even when a compound such as a fluorine compound having high reactivity is used as the gaseous raw material. <P>SOLUTION: The method for producing the functional gas continuously by reacting the plurality of gaseous raw materials with one another comprises the steps of: introducing the plurality of gaseous raw materials into a cylinder the outer wall of which is heated; moving the gaseous raw materials introduced into the cylinder and a gaseous reaction product from the upstream side thereof to the downstream side; and withdrawing the gaseous raw materials and the gaseous reaction product from the cylinder. At the step of moving the gaseous raw materials and the gaseous reaction product, they are moved from the upstream side thereof to the downstream side while turning them from the inner wall surface thereof to the opposite inner wall surface. <P>COPYRIGHT: (C)2010,JPO&INPIT

Description

  The present invention relates to a technique for continuously obtaining a functional gas such as an etching gas, a cleaning gas, and a raw material gas for forming a thin film by reacting multiple types of raw material gases.

  A functional material such as a functional gas is manufactured by reacting a raw material gas by a thermal reaction through a raw material gas through a heated internal space. In order to increase the efficiency of functional material production, the raw material gas is continuously passed through the internal space, the raw material gas undergoes a thermal reaction in the internal space, the reaction product moves from upstream to downstream, and the reaction product is transferred to the internal space. Need to be taken out of.

One point of increasing the efficiency of the process is to uniformly heat the raw material gas introduced into the internal space. For example, in Patent Document 1, in a coal direct liquefaction continuous reaction apparatus into which hydrogen is introduced, a system in which a heat coil is installed on the central axis in a cylinder constituting the reaction apparatus in order to improve thermal efficiency when the apparatus scale is expanded. Is disclosed.
JP-A-10-53772

  When the raw material gas is a highly reactive material such as a fluorine compound, for example, in the method of providing a heating mechanism in a cylinder as in Patent Document 1, there is a problem that the heating mechanism is severely deteriorated. This is particularly noticeable in a process in which multiple types of raw material gases are reacted by thermal reaction.

  The present invention provides a method capable of continuously producing a functional gas by thermally reacting multiple types of source gases even when a highly reactive material such as a fluorine compound is used as the source gas. The task is to do. In the present invention, “continuous” means that the raw material is introduced without interruption during the operation of the technical means to cause a reaction to generate a functional gas.

The method for continuously obtaining the functional gas of the present invention is a method for continuously obtaining a functional gas by reacting multiple kinds of raw material gases.
The step of introducing multiple types of source gases into the cylinder whose outer wall is heated The step of the source gas and reaction product gas introduced into the cylinder moving from upstream to downstream in the cylinder The source gas and reaction product gas from the cylinder A source gas and a reaction product gas from the inner wall surface of the cylindrical body to the inner wall surface in the opposite direction while moving from the upstream side to the downstream side of the cylindrical body. . And the reaction product gas, ie, functional gas, is obtained continuously by continuing the above-mentioned three processes without interruption.

  Since the outer wall of the cylinder into which multiple kinds of source gases are introduced is heated, even if the inside of the cylinder is lower than the desired temperature, the outer wall of the cylinder is heated, so Since it is in a heated state, when the source gas is in contact with the inner wall surface or in the vicinity of the inner wall surface, multiple types of source gases react by a thermal reaction to generate a reaction product gas.

Further, in the present invention, in order to make it easy for the source gas to contact the inner wall surface or to pass through the vicinity of the inner wall surface, the rib is formed substantially vertically from both the inner wall surface and the inner wall surface in the direction opposite to the inner wall surface. Formed,
A plurality of the ribs are formed from upstream to downstream in the cylinder,
The rib formed from the inner wall surface and the rib formed from the inner wall surface in the opposite direction are arranged alternately so that the moving step (the raw material gas and the reaction product gas introduced into the cylinder are in the cylinder) In the step of moving the gas from upstream to downstream, the source gas and the reaction product gas move from the upstream side to the downstream side of the cylindrical body while moving from the inner wall surface of the cylindrical body to the inner wall surface in the opposite direction.

  The ribs installed in the cylinder as described above easily cause the source gas and the reaction product gas to move from the upstream side to the downstream side of the cylindrical body while moving from the inner wall surface of the cylindrical body to the inner wall surface in the opposite direction. . Further, since the rib is heated as the outer wall of the cylindrical body is heated, the thermal reaction efficiently occurs when the raw material gas flows along the rib, and the effect of generating the reaction product gas is also preferable.

Furthermore, the apparatus for continuously obtaining the functional gas of the present invention is for continuously obtaining a functional gas by reacting multiple kinds of raw material gases,
Part where multiple types of source gas are introduced into the cylinder whose outer wall is heated. Part where source gas and reaction product gas introduced into the cylinder are moved from upstream to downstream in the cylinder. Source gas and reaction product gas are introduced from the cylinder. Has a part to be removed,
Since the source gas and the reaction product gas move from the inner wall surface of the cylinder to the inner wall surface in the opposite direction while moving from the upstream side to the downstream side in the opposite direction, Ribs are formed in a substantially vertical direction from both wall surfaces,
A plurality of the ribs are formed from upstream to downstream in the cylinder,
The ribs formed from the inner wall surface and the ribs formed from the inner wall surface in the opposite direction are alternately adjacent to each other.

  In a preferred embodiment of the present invention, it is possible to introduce a raw material gas into the reaction system without interruption and to cause a reaction to produce a functional gas. And since the inner wall in the cylinder is in a heated state through the heating of the outer wall, the source gas is reliably heated when the source gas contacts the inner wall surface or passes through the vicinity of the inner wall surface. It can be easily accommodated to increase the size of the reactor. In addition, since it is not necessary to provide a heater for heating in the system in which the thermal reaction of the raw material gas occurs, the maintenance of the apparatus is easy, and the raw material gas has a highly reactive material such as a fluorine compound. Even when it is used, it is also easy to produce a functional gas continuously for a long time by thermally reacting multiple kinds of raw material gases.

  An apparatus suitably used in the method for continuously obtaining the functional gas of the present invention will be described with reference to the drawings. FIG. 1 is a perspective view of a main part of a device 1 preferably used in the present invention, FIG. 2 is a cross-sectional view of ab-a′b ′ shown in the perspective view of the device 1 shown in FIG. FIG. 3 is a cross-sectional view taken along the line cc ′ shown in the cross-sectional view of the device 1 shown in FIG. 2.

  The raw material gas introduced from the gas inlet 2 flows from the upstream side to the downstream side while generating a reaction product through the cylindrical body 9 of the cylindrical device 1. Then, the reaction product is taken out from the gas outlet 3. The unreacted raw material gas may also be taken out from the gas outlet 3.

  In the apparatus 1, due to the presence of the rib 4, the gas moves from the upstream side to the downstream side of the cylindrical body while facing the inner wall surface 6 c in the opposite direction from the inner wall surface 6 b of the cylindrical body as illustrated in FIG. 2. In the embodiment of FIG. 2, a plate material 8 that seals the cylinder body 9 is provided in the downstream region of the cylinder body 9, gas flows along the plate material 8, and reaction products and the like are taken out from the gas outlet 3. However, it is good also as an aspect which takes out a reaction product etc. from the most downstream area in a cylinder.

  As shown in FIG. 2, a plurality of ribs 4 are formed from the upstream side to the downstream side of the cylindrical body 9, and are formed substantially vertically from the inner wall surface 6c in the opposite direction. The ribs 4 are preferably arranged alternately. By arranging the ribs 4 in this manner, the gas flowing through the cylindrical body 9 can easily flow from the upstream side to the downstream side in the cylindrical body from the inner wall surface 6b toward the inner wall surface 6c. Further, the number of ribs arranged in the cylindrical body 9 is appropriately set depending on the size of the device 1 and the type of raw material gas.

  Since the inner wall surfaces 6a to 6c are heated through the outer wall 5 by the heater 7, the raw material gas is surely heated when passing or contacting the inner wall surfaces 6a to 6c. The raw material gas reacts to produce a reaction product, that is, a functional gas.

  Further, the embodiment in which the ribs 4 are provided as shown in FIG. 2 is preferable because the ribs 4 are also heated by heat transfer, so that the thermal reaction of the raw material gas is efficient.

  When the cross section of the device 1 is viewed as in cc ′, the area occupied by the rib 4 in the cylindrical body 9 (the total area of the gap 10 formed by the rib 4 and the rib 4 in FIG. 3) is preferably 50% or more. More preferably, it is 50 to 95%, and further preferably 75 to 85%. If it is less than 50%, the rib 4 tends to reduce the amount of gas flowing from the upstream side to the downstream side in the cylinder from the inner wall surface 6b toward the inner wall surface 6c. On the other hand, if it exceeds 95%, the pressure loss tends to increase, and the gas tends not to flow smoothly from the upstream side to the downstream side.

  The distance between the rib and the adjacent rib is preferably set to 1/5 or more of the inner diameter of the cylindrical body because the gas flow may not be smooth if the distance is short. Further, if the distance is too long, the effect of the rib becomes small, and therefore it is preferably set to be equal to or smaller than the inner diameter of the cylinder.

  As the material used for the rib 4 and the inner wall surfaces 6a to 6c, when a highly reactive material such as a fluorine compound is used for the raw material gas, a nickel-based metal material such as nickel or inconel is generally used. There is no particular limitation as long as it is chemically and chemically resistant. The material used for the outer wall 5 may be the same material as the inner wall surfaces 6a to 6c, but is not particularly limited as long as it has heat resistance.

In the present invention, examples of the functional gas obtained as a reaction product include chlorine trifluoride (ClF ₃ ) obtained by reacting fluorine (F ₂ ) and chlorine (Cl ₂ ) at a temperature of about 300 ° C., Seven obtained by reacting F ₂ and bromine (Br ₂ ) at a temperature of around 200 ° C., bromide pentafluoride (BrF ₅ ), F ₂ and iodine (I ₂ ) at a temperature of around 250 ° C. Examples thereof include iodine fluoride (IF ₇ ). The present invention is not limited to the production of the functional gas described above.

Example 1. Preparation of apparatus for continuously obtaining functional gas An apparatus 1 having a main structure shown in FIGS. 1 to 3 was prepared as the general structure. The inner diameter of the cylinder was 300 mm, and the distance from the gas inlet 2 to the gas outlet 3 was 1 m. Further, the distance between the rib 4 formed substantially vertically from the inner wall surface 6b and the adjacent rib 4 formed substantially vertically from the inner wall surface 6c was set to 75 mm, and 13 ribs 4 were arranged from the upstream side to the downstream side. Furthermore, the size of each rib was such that the occupied area of the rib 4 when viewed in FIG. 3 was 80%. And the heating of the heater 7 was started and it kept keeping so that the temperature of the inner wall surfaces 6a thru | or c might be 290-310 degreeC.

2. Continuous synthesis of functional gas Continue to introduce F ₂ and Cl ₂ as raw gases from the gas inlet 2 and N ₂ as diluent gases at a rate of 4.5 SLM, 1.5 SLM and 8.5 SLM, respectively. The reaction product ClF ₃ was continuously taken out as a functional gas at a rate of 2.25 SLM.

Comparative Example The reaction was continuously performed in the same procedure as in Example 1 except that no rib 4 was provided. ClF ₃ as a functional gas could be continuously taken out only at a rate of 1.6 SLM.

It is a figure which shows the perspective view of the principal part of the apparatus suitably used by this invention. It is a figure which shows the cross section of ab-a'b 'shown with the apparatus 1 shown in FIG. It is a figure which shows the cross section of c-c 'shown in sectional drawing of the apparatus 1 shown by FIG.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 Apparatus which has a cylindrical body for obtaining functional gas continuously 2 Gas inlet 3 Gas outlet 4 Rib 5 Outer wall 6 Inner wall 7 Heater 8 Plate 9 to seal

Claims (6)

It is a method of continuously obtaining a functional gas by reacting multiple kinds of source gases,
The step of introducing multiple types of source gases into the cylinder whose outer wall is heated The step of the source gas and reaction product gas introduced into the cylinder moving from upstream to downstream in the cylinder The source gas and reaction product gas from the cylinder And the step of moving is characterized in that the source gas and the reaction product gas move from the inner wall of the cylinder to the inner wall in the opposite direction while moving from the upstream to the downstream in the cylinder. A method for continuously obtaining a functional gas. Ribs are formed substantially vertically from both the inner wall surface and the inner wall surface in the opposite direction,
A plurality of the ribs are formed from upstream to downstream in the cylinder,
The ribs formed from the inner wall surface and the ribs formed from the inner wall surface in the opposite direction are alternately arranged, and in the moving step, the source gas and the reaction product gas are discharged from the inner wall surface of the cylinder. The method for continuously obtaining a functional gas according to claim 1, wherein the functional gas continuously moves from the upstream side to the downstream side while facing the inner wall surface in the opposite direction. The method for continuously obtaining a functional gas according to claim 1 or 2, wherein the area of each rib is 50% or more of the area of the inner diameter portion of the cylinder. The functional gas according to any one of claims 1 to 3, wherein a distance between the rib and a rib disposed adjacent thereto is 1/5 or more of the inner diameter of the cylinder and not more than the inner diameter of the cylinder. How to get continuously. The method for continuously obtaining a functional gas according to any one of claims 1 to 4, wherein an end of the cylindrical body is sealed. An apparatus for continuously obtaining a functional gas by reacting multiple kinds of source gases,
Part where multiple types of source gas are introduced into the cylinder whose outer wall is heated. Part where source gas and reaction product gas introduced into the cylinder are moved from upstream to downstream in the cylinder. Source gas and reaction product gas are introduced from the cylinder. Has a part to be removed,
Since the source gas and the reaction product gas move from the inner wall surface of the cylinder to the inner wall surface in the opposite direction while moving from the upstream side to the downstream side in the opposite direction, Ribs are formed in a substantially vertical direction from both wall surfaces,
A plurality of the ribs are formed from upstream to downstream in the cylinder,
An apparatus characterized in that a rib formed from an inner wall surface and a rib formed from an inner wall surface in the opposite direction are alternately adjacent to each other.