JP2008037674A - Method of manufacturing vitreous carbon-made core tube - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a method of manufacturing a vitreous carbon-made core tube by which the vitreous carbon-made core tube is manufactured without causing dimensional distortion even in a joined body comprising a cylindrical body and a half-cylindrical body. <P>SOLUTION: The method of manufacturing the vitreous carbon-made core tube includes a step for making the joined body by joining both parallel edges of the half-cylindrical body having a shape formed by halving a cylinder having nearly the same length as that of the cylindrical body and smaller diameter than that of the cylindrical body and formed from the thermosetting resin to the outer surface of the cylindrical body formed from a thermosetting resin so that the axial direction of the cylindrical body is parallel to the axial direction of the half-cylindrical body, a step for carbonizing the joined body and a step for processing to remove a removing part of the cylindrical body which is surrounded by both edges of the half-cylindrical body. <P>COPYRIGHT: (C)2008,JPO&INPIT

Description

  The present invention relates to a wafer heat treatment apparatus for heat-treating a silicon wafer or forming a film on a silicon wafer surface by chemical vapor deposition, in a reaction vessel (quartz outer tube) for maintaining airtightness. The present invention relates to a method for manufacturing a glassy carbon core tube (inner tube) that is housed and used.

  Conventionally, quartz, silicon carbide, or glassy carbon has been used as a material for a core tube (inner tube) having a circular cross section. Recently, however, as a result of emphasizing the uniformity of wafer processing and the ease of use for distributing reaction gas and cooling gas, reactor core tubes having a non-circular cross section have been commercialized. However, this type of non-circular cross-section core tube is currently limited to quartz or silicon carbide, and even glassy carbon that has the advantages of being chemically stable and less likely to generate contaminants. There has been a long-awaited development of a technology capable of manufacturing a core tube having a non-circular cross section.

As shown in Patent Document 1, a glassy carbon core tube is conventionally circular only in cross section, and a glassy carbon core tube having a non-circular cross section has not been realized. This is thought to be due to the glassy carbon production method. That is, glassy carbon is generally obtained by carbonizing a molded body made of a thermosetting resin such as a phenol resin in an inert atmosphere at a high temperature of 1000 ° C. or higher. This is because the size of the molded body shrinks by about 20% and dimensional distortion is likely to occur. If the cross section is circular, various devices for improving the dimensional accuracy can be applied as shown in Patent Document 1, but if the cross section is non-circular, in order to avoid a dimensional deviation. It was the actual situation that there was no way.
JP 2000-313666 A

  The present invention was invented in view of the above-mentioned conventional situation, and even a joined body composed of a cylinder and a semi-cylinder can produce a core tube made of glassy carbon without causing dimensional deviation, It is an object of the present invention to provide a method for producing a glassy carbon core tube that can produce a glassy carbon core tube having a non-circular cross section that is chemically stable and hardly generates contaminants.

  According to the first aspect of the present invention, a cylinder formed of a thermosetting resin having the same length as that of the cylinder and a small diameter is substantially divided into two on the outer surface of the cylinder formed of the thermosetting resin. Joining both parallel edges of the shape semi-cylindrical body so that the axial directions of the cylindrical body and the semi-cylindrical body are parallel, and a step of carbonizing the joined body; It is a manufacturing method of the glass-like carbon core tube characterized by including the process of removing the removal part enclosed by the both ends of the said semi-cylindrical body among the said cylindrical bodies.

  According to a second aspect of the present invention, the thermosetting resin forming the cylindrical body and the semi-cylindrical body is a liquid phenol resin, and in the step of joining the cylindrical body and the semi-cylindrical body, the same liquid phenol as described above 2. A method for producing a glassy carbon furnace core tube according to claim 1, wherein the resin is bonded as an adhesive.

  The invention according to claim 3 is a pre-removal part, leaving at least a plurality of connecting parts connecting the two end edges among the removal parts surrounded by the both end edges of the semi-cylindrical body of the cylindrical body, 3. The method for producing a glassy carbon furnace core tube according to claim 1, wherein the pre-removal part is pre-removed before the step of performing the chemical conversion treatment.

  According to the method for manufacturing a glassy carbon core tube of the present invention, a glassy carbon core tube can be manufactured without any dimensional deviation even in a joined body composed of a cylinder and a semi-cylinder. It is possible to produce a glassy carbon core tube having a non-circular cross section that is stable and hardly generates pollutants.

  Hereinafter, the present invention will be described in more detail based on embodiments shown in the accompanying drawings.

  The glassy carbon shown in the present invention can be generally obtained by carbonizing a cured product of a thermosetting resin. Examples of thermosetting resins include phenolic resins, epoxy resins, unsaturated polyester resins, furan resins, melamine resins, alkit resins, xylene resins, and mixtures thereof, among which glass with good characteristics It is desirable to use a phenol resin from which carbon-like carbon is obtained. Furthermore, it is desirable to use a liquid phenol resin. This is because, since it is liquid, the large-diameter cylindrical body 1 can be manufactured relatively easily by the centrifugal molding method shown in the embodiment.

  FIG. 1 is a drawing showing a method for manufacturing a glassy carbon core tube of the present invention in the order of manufacturing steps. Reference numeral 1 denotes a cylindrical body made of a thermosetting resin such as the liquid phenol resin described above, and 2 denotes a semi-cylindrical body made of the same thermosetting resin. The cylindrical body 1 and the semi-cylindrical body 2 have substantially the same length, and the radius of the semi-cylindrical body 2 is smaller than the radius of the cylindrical body 1. In the embodiment shown in FIG. 1, the radius is one tenth or less.

  First, before the cylindrical body 1 and the semi-cylindrical body 2 are joined, the semi-cylindrical body 2 is formed by cutting and dividing the cylinder 4 formed of a thermosetting resin into approximately half. The completed semi-cylindrical body 2 is arranged on the outer surface of the cylindrical body 1 so that the axial directions thereof are parallel to each other, and both parallel edges 2a and 2a are connected to the outer surface of the cylindrical body 1 with an adhesive. It joins with the cylindrical body 1 by press-contacting.

  Next, the joined body 3 composed of the joined cylindrical body 1 and semi-cylindrical body 2 is carbonized to become glassy carbon. (Detailed carbonization treatment methods are shown in the examples.)

  Finally, the glass tube core A is completed by cutting and removing the portion of the cylindrical body 1 surrounded by the two end edges 2a, 2a of the semi-cylindrical body 2, that is, the removing portion 1a. The space surrounded by the semi-cylindrical body 2 is used as a space for storing a specially shaped board, injector nozzle, and the like.

  The cylindrical body 1 and the semi-cylindrical body 2 may be joined and integrated by high-temperature heat treatment, but it is desirable to join them with an adhesive as described above from the viewpoint of joining strength and the like. The type of the adhesive is not particularly limited, but it is optimal to use the same liquid phenol resin as that of the cylindrical body 1 and the semi-cylindrical body 2. This is because if the adhesive is the same resin as the cylindrical body 1 and the semi-cylindrical body 2, the dimensional distortion of the joint portion is reduced because the same dimensional shrinkage rate is exhibited in the carbonization process.

  FIG. 2 shows another embodiment of the present invention. In this embodiment, before the carbonization treatment step, a part of the removal portion 1a surrounded by the both end edges of the semi-cylindrical body 2 of the cylindrical body 1 is used as the preliminary removal portion 1b, and before the carbonization treatment step. To remove. That is, since glassy carbon is not a material with good workability, by removing the pre-removal portion 1b first, the dimensional distortion of the joint portion in the carbonization process is minimized, and after the carbonization treatment The productivity of machining can be improved. Note that if all of the removal portion 1a is removed before the carbonization step, both the cylindrical body 1 and the semi-cylindrical body 2 are relatively undesirably strained.

  FIG. 2 shows a plurality of pre-removal portions 1b made of rectangular holes with rounded ends arranged at regular intervals with a constant interval between them, but at least between both end edges 2a, 2a of the semi-cylindrical body 2. The pre-removal unit 1b may have any shape as long as the pre-removal unit 1b is formed while leaving a plurality of connected portions. For example, it may be a circular hole, a window shape in which the pre-removal portion 1b itself reaches the both end edges 2a and 2a, a plurality of holes having different shapes, or the like.

(Example 1)
In Example 1, a commercially available liquid phenol resin (PL-4804 manufactured by Gunei Chemical Industry Co., Ltd.) was used as a raw material for a glass core carbon core tube. The characteristic values of this raw material are as follows: density (at 25 ° C.): 1198 kg / m ³ , viscosity (at 25 ° C.): 690 cP, gelation time (at 150 ° C.): 7 minutes 50 seconds, nonvolatile component: 72.5% by mass It is. This liquid phenol resin was heat-treated at 100 ° C. for 5 hours to obtain a molding raw material.

  First, 12 kg of resin was loaded into a cylindrical mold (not shown) having an inner diameter of 450 mm and a length of 1500 mm, and the mold was kept at 100 ° C. and centrifuged at 300 rpm for 20 hours to obtain an outer diameter of 445 mm. A cylindrical body 1 having a length of 1460 mm was obtained.

  At the same time, 0.9 kg of resin was loaded into a cylindrical mold (not shown) with an inner diameter of 35 mm and a length of 1500 mm, and the mold was kept at 100 ° C. and centrifuged at 300 rpm for 20 hours. A cylinder 4 having an outer diameter of 34 mm and a length of 1460 mm was formed. This cylinder 4 was divided into two parallel to the axis to obtain a semi-cylindrical body 2.

  Next, both end edges 2a and 2a of the semi-cylindrical body 2 are pressed against the outer surface of the cylindrical body 1 using a liquid phenol resin as an adhesive, and held at 100 ° C. for 10 hours, so that the cylindrical body 1 and the semi-cylindrical body 2 are The bonded body 3 was obtained by bonding.

  Next, this bonded body 3 was subjected to a curing process in which it was heated in air at 200 ° C. for 50 hours, and then heated in a nitrogen atmosphere at 2 ° C./h to 1000 ° C., and further to 2000 ° C. The temperature was raised at 10 ° C./h to carbonize. The glassy carbon furnace core tube A in the middle of production obtained by the above production method had a length of 1180 mm, the outer diameter of the cylindrical body 1 part was 360 mm, and the outer diameter of the semi-cylindrical body 2 part was 30 mm.

  Finally, the final shape glassy carbon core tube A from which the removal portion 1a of the cylindrical body 1 has been removed has a cross-sectional dimensional distortion within ± 1 mm, and is suitable as a core tube.

(Example 2)
In Example 2, the same commercially available liquid phenolic resin as that in Example 1 (PL-4804 manufactured by Gunei Chemical Industry Co., Ltd.) was used as a forming raw material.

  First, 12 kg of resin was loaded into a cylindrical mold (not shown) having an inner diameter of 450 mm and a length of 1500 mm, and the mold was kept at 100 ° C. and centrifuged at 300 rpm for 20 hours to obtain an outer diameter of 445 mm. A cylindrical body 1 having a length of 1460 mm was obtained. In the axial direction of the outer surface of the cylindrical body 1, twelve pre-removal portions 1b made of rectangular holes having a width of 30 mm and a length of 100 mm were formed at regular intervals with a pitch of 20 mm.

  Separately, 0.9 kg of resin is loaded into a cylindrical mold (not shown) with an inner diameter of 35 mm and a length of 1500 mm, the mold is kept at 100 ° C., and is centrifuged at 300 rpm for 20 hours. A cylinder 4 having an outer diameter of 34 mm and a length of 1460 mm was formed. This cylinder 4 was divided into two parallel to the axis to obtain a semi-cylindrical body 2.

  Next, both end edges 2a and 2a of the semi-cylindrical body 2 are pressed against the outer surface of the cylindrical body 1 using a liquid phenol resin as an adhesive so as to straddle the arrangement of the pre-removing portions 1b, and are performed at 100 ° C. for 10 hours. The cylindrical body 1 and the semi-cylindrical body 2 were bonded to obtain a joined body 3.

  Next, this bonded body 3 was subjected to a curing process in which it was heated in air at 200 ° C. for 50 hours, and then heated in a nitrogen atmosphere at 2 ° C./h to 1000 ° C., and further to 2000 ° C. The temperature was raised at 10 ° C./h to carbonize. The glassy carbon furnace core tube A in the middle of production obtained by the above production method had a length of 1180 mm, the outer diameter of the cylindrical body 1 part was 360 mm, and the outer diameter of the semi-cylindrical body 2 part was 30 mm.

  Finally, the final shape glassy carbon furnace core tube A from which the removal portion 1a including the pre-removal portion 1b of the cylindrical body 1 has been removed has a cross-sectional dimensional distortion within ± 1 mm, and is suitable as a furnace core tube.

(Comparative example)
Also in the comparative example, the same commercially available liquid phenolic resin as that of Example 1 (PL-4804 manufactured by Gunei Chemical Industry Co., Ltd.) was used as a forming raw material.

  First, 12 kg of resin was loaded into a cylindrical mold (not shown) having an inner diameter of 450 mm and a length of 1500 mm, and the mold was kept at 100 ° C. and centrifuged at 300 rpm for 20 hours to obtain an outer diameter of 445 mm. A cylindrical body 1 having a length of 1460 mm was obtained. A slit having a width of 35 mm parallel to the axial direction was formed on the outer surface of the cylindrical body 1 by cutting and removing, so that the cylindrical body 1 had a C-shaped cross section. (Although it has a C-shaped cross section, the following is also referred to as the cylindrical body 1)

  Separately, 0.9 kg of resin is loaded into a cylindrical mold (not shown) with an inner diameter of 35 mm and a length of 1500 mm, the mold is kept at 100 ° C., and is centrifuged at 300 rpm for 20 hours. A cylinder 4 having an outer diameter of 34 mm and a length of 1460 mm was formed. This cylinder 4 was divided into two parallel to the axis to obtain a semi-cylindrical body 2.

  Next, both end edges 2a and 2a of the semi-cylindrical body 2 are pressed against the outer surface of the cylindrical body 1 using a liquid phenol resin as an adhesive so as to straddle the slit of the cylindrical body 1, and held at 100 ° C. for 10 hours. The cylindrical body 1 and the semi-cylindrical body 2 were bonded to obtain a joined body 3.

  Next, this bonded body 3 was subjected to a curing process in which it was heated in air at 200 ° C. for 50 hours, and then heated in a nitrogen atmosphere at 2 ° C./h to 1000 ° C., and further to 2000 ° C. The temperature was raised at 10 ° C./h to carbonize. The glassy carbon furnace core tube A obtained by the above manufacturing method has a length of 1180 mm, the outer diameter of the cylindrical body 1 part is 360 mm, and the outer diameter of the semi-cylindrical body 2 part is 30 mm. The dimensional distortion of the cross section was ± 5 mm or more, and it could not be practically used as a core tube.

It is the longitudinal cross-sectional view which showed one Embodiment of this invention in order of the manufacturing process. It is a perspective view which shows the manufacture middle stage of another embodiment of this invention.

Explanation of symbols

A ... Glass-like carbon furnace core tube 1 ... Cylindrical body 1a ... Removal part 1b ... Pre-removal part 2 ... Semi-cylindrical body 2a ... Both ends edge 3 ... Joined body 4 ... Cylinder

Claims (3)

The outer surface of the cylinder formed of the thermosetting resin is parallel to a semi-cylindrical body having a substantially the same length as the cylinder and a half cylinder formed by dividing the cylinder formed of the small-diameter thermosetting resin. Joining both end edges so that the axial directions of the cylindrical body and the semi-cylindrical body are parallel;
A step of carbonizing the joined body;
A method of manufacturing a glassy carbon core tube, comprising a step of removing a removal portion surrounded by both end edges of the semi-cylindrical body of the cylindrical body.   The thermosetting resin that forms the cylindrical body and the semi-cylindrical body is a liquid phenol resin, and in the step of joining the cylindrical body and the semi-cylindrical body, the same liquid phenol resin as described above is joined as an adhesive. The method for producing a glassy carbon core tube according to claim 1.   Among the removal parts surrounded by the both end edges of the semi-cylindrical body of the cylindrical body, at least a plurality of connecting parts connecting between the both end edges are left as pre-removal parts, and prior to the step of carbonization treatment 3. The method for producing a glassy carbon furnace core tube according to claim 1, wherein the removing portion is removed in advance.

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