JP2016169422A - Manufacturing method of ceramic member - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a manufacturing method of a ceramic member capable of preventing burrs or tiny cracks from generating around a support point in manufacturing the ceramic member.SOLUTION: A ceramic film 21 is formed on the surface of a substrate 20 by a CVD method after the substrate 20 is supported by a support member 30. The support member 30 has a top face enclosed by a contour line 332 and a support part 32 higher than the contour line 332 inside the top face. The outside region of the top face enclosed by the contour line 332 prevents a CVD raw gas from entering the support part 32 and thus prevents adhesion of the support part 32 to the substrate 20 caused by the formed ceramic film 21.SELECTED DRAWING: Figure 1

Description

  The present invention relates to a method for manufacturing a ceramic member in which a ceramic coating is formed on a substrate.

Ceramic members in which a ceramic film is formed on a substrate by a CVD method are used in various fields because the substrate can be protected with the ceramic film. Ceramic parts that use graphite with excellent workability as the base material and whose surface is protected by a ceramic coating are used for semiconductor manufacturing equipment, single crystal pulling, etc., for the purpose of preventing reaction of the base material due to the ceramic coating and improving wear resistance. It is used in various fields such as equipment and structural ceramic parts.
However, in the CVD method, it is necessary to support the base material, and a ceramic coating cannot be formed at the support point, so that a portion where the base material is exposed is formed. When the substrate is exposed and used in a reactive environment, there is a problem that the support point portion is consumed and deteriorated. Various solutions have been made to solve such problems.

In Patent Document 1, a ceramic member is manufactured by supporting a ceramic substrate at the tip and forming a ceramic member coating on the ceramic substrate in a reaction furnace so as not to form an exposed support point of the substrate. At this time, it is described that a ceramic base material support having a core material made of graphite and a support film having a pyrolytic carbon layer interposed on a surface including at least a tip portion is used. Yes.
According to this ceramic substrate support, the ceramic substrate support has a graphite core, the surface of the graphite is coated with pyrolytic carbon, and the surface is further coated with the support coating. . Since pyrolytic carbon has no pores, when the support coating is coated, the support coating is not formed by penetrating into the pyrolytic carbon layer, thereby reducing the adhesive force between the support coating and the pyrolytic carbon layer. be able to.

  Therefore, when the ceramic substrate support is removed from the ceramic member and the ceramic substrate support having the ceramic member coating formed on the ceramic substrate, there is a gap between the pyrolytic carbon layer of the ceramic substrate support and the support coating (that is, determined). It is easily separated at Therefore, the ceramic substrate is exposed from the ceramic member, or the remaining amount of the support member coating of the ceramic substrate support on the surface of the ceramic member coating formed on the ceramic substrate is excessively large. It is described that it becomes difficult to do.

JP 2012-184152 A

  However, in the invention described in Patent Document 1, burrs of the ceramic coating are generated when the support is separated from the base material, and it tends to remain as harmful protrusions that cause scratches and particles. Further, a minute crack is generated when the support and the substrate are separated. The minute crack rarely reaches the base material of the ceramic member and causes the life of the ceramic member to be shortened. For this reason, a ceramic member free from burrs or minute cracks around the support point is desired.

  An object of this invention is to provide the manufacturing method of the ceramic member which can prevent that a burr | flash or a micro crack generate | occur | produces around the support point at the time of ceramic member manufacture in view of the said subject.

  The method for producing a ceramic member of the present invention for solving the above-mentioned problem is the method for producing a ceramic member in which a ceramic film is formed on the surface of the base material by a CVD method after supporting the base material using a support. The support has a top surface surrounded by a contour line, and has a support portion higher than the contour line inside the top surface.

  According to the method for producing a ceramic member of the present invention, the base material is supported using the support tool, and in this state, the ceramic film is formed on the surface of the base material by the CVD method. At this time, the support has a top surface surrounded by the outline, and has a support portion higher than the outline on the inside of the top surface.

Since the top surface of the support tool faces the base material and has a support portion higher than the outline on the inside of the top surface, the inside of the top surface is in contact with the base material and the outside is separated from the base material. For this reason, since the outline of the top surface is lower than the support portion, the outer portion of the top surface can prevent the entry of the CVD source gas into the support portion, and the support portion and the base material are formed. It is possible to prevent sticking by the formed ceramic coating.
For this reason, since the base material placed on the support is not fixed by the ceramic film after CVD, it is possible to prevent the generation of harmful burrs and micro cracks around the support point when removing the base material. it can.

Furthermore, it is desirable that the method for producing a ceramic member of the present invention is as follows.
(1) The support portion is at the center of the top surface.
When the support portion is at the center of the top surface, the substrate is supported at the center of the thin support region of the ceramic coating that the top surface of the support device faces. For this reason, the area of the non-film forming region can be reduced.

(2) The top surface is a convex surface rising from the outline.
If the shape of the top surface is a convex surface that rises from the outline, the distance between the top surface and the base material is rapidly narrowed from the outer portion toward the support portion, so that the source gas wraps around the support region. It can suppress efficiently and can further reduce the area of the non-film-forming area | region formed in the support area | region of a base material.

(3) The support has a protrusion inside.
If the support has a protrusion, it is possible to secure a sufficient distance between the base and the top surface, so that the base and the support are fixed even if a thick ceramic film is formed. Can be prevented.

(4) The ceramic coating is SiC.
When the ceramic coating is SiC, there are the following merits. That is, since SiC is chemically stable, consumption of the base material can be prevented. Further, since SiC is a hard and wear-resistant ceramic material, it is possible to prevent the substrate from being worn or damaged.

(5) The base material has a core material made of graphite.
Since graphite has a cleavage plane in the crystal, if the core material is made of graphite, it can be easily processed, and various shapes of ceramic members can be obtained. The base material having a graphite core material includes a base material itself made of graphite or having a ceramic film formed on graphite.

(6) The step of forming the ceramic coating is repeated a plurality of times by changing the position of the support relative to the substrate.
In the method for producing a ceramic member of the present invention, the core material of the substrate can be completely covered with the ceramic coating by repeating the step of forming the ceramic coating by changing the position of the support relative to the substrate multiple times. For example, when the base material is graphite, in the first formation of the ceramic coating, the base material made of graphite is exposed in the vicinity where the support portion abuts. However, by changing the position of the support and using the ceramic member, which is the base material on which the ceramic coating is formed, as a new base material, a second ceramic coating is formed, so that two layers of exposed graphite base material are formed. Can be covered with a ceramic coating on the eyes.

  According to the method for producing a ceramic member of the present invention, the base material is supported using the support tool, and in this state, the ceramic film is formed on the surface of the base material by the CVD method. At this time, the support tool has a top surface surrounded by the outer shape line and a support portion higher than the outer shape line inside the top surface.

Since the top surface of the support tool faces the base material and has a support portion higher than the outline on the inside of the top surface, the inside of the top surface is in contact with the base material and the outside is separated from the base material. For this reason, since the outline of the top surface is lower than the support portion, the outer portion of the top surface can prevent the entry of the CVD source gas into the support portion, and the support portion and the base material are formed. It is possible to prevent sticking by the formed ceramic coating.
For this reason, since the base material placed on the support is not fixed by the ceramic film after CVD, it is possible to prevent the generation of harmful burrs and micro cracks around the support point when removing the base material. it can.

(A) thru | or (C) is process drawing which shows the manufacturing method of the ceramic member which concerns on embodiment of this invention. (A) is a perspective view of a support tool, (B) is sectional drawing of the BB position in (A). (A)-(D) are the perspective view and sectional drawing which show the modification of a support tool. (A), (B) is sectional drawing and the bottom view of the site | part supported with the support tool, when forming a 2nd ceramic film.

  The manufacturing method of the ceramic member of this invention is demonstrated.

  The method for producing a ceramic member according to the present invention is a method for producing a ceramic member in which a ceramic film is formed on a surface of the base material by a CVD method after the base material is supported using a support tool. And a support portion that is higher than the contour line inside the top surface.

Since the top surface of the support tool faces the base material and has a support portion higher than the outline on the inside of the top surface, the inside of the top surface is in contact with the base material and the outside is separated from the base material. For this reason, since the outline of the top surface is lower than the support portion, the outer portion of the top surface can prevent the entry of the CVD source gas into the support portion, and the support portion and the base material are formed. It is possible to prevent sticking by the formed ceramic coating.
For this reason, since the base material placed on the support is not fixed by the ceramic film after CVD, it is possible to prevent the generation of harmful burrs and micro cracks around the support point when removing the base material. it can.

Furthermore, it is desirable that the method for producing a ceramic member of the present invention is as follows.
(1) The support portion is at the center of the top surface.
When the support portion is at the center of the top surface, the substrate is supported at the center of the thin support region of the ceramic coating that the top surface of the support device faces. For this reason, the area of the non-film forming region can be reduced.

(2) The top surface is a convex surface rising from the outline.
If the shape of the top surface is a convex surface that rises from the outline, the distance between the top surface and the base material rapidly narrows from the outer part toward the support part, so it is efficient to circulate the source gas into the support area. It can suppress well and can reduce a non-film forming area | region more.

(3) The support has a protrusion inside.
If the support has protrusions, the space between the base and the top surface can be secured sufficiently, preventing the base and the support from sticking even when a thick ceramic film is formed. can do.

(4) The ceramic coating is SiC.
When the ceramic coating is SiC, there are the following merits. That is, since SiC is chemically stable, consumption of the base material can be prevented. Further, since SiC is a hard and wear-resistant ceramic material, it is possible to prevent the substrate from being worn or damaged.

(5) The base material has a graphite core material.
Since graphite has a cleavage plane in the crystal, if the core material of the base material is made of graphite, it can be easily processed, and ceramic members having various shapes can be obtained. The base material having a graphite core material includes a base material itself made of graphite or having a ceramic film formed on graphite.

(6) The step of forming the ceramic coating is repeated a plurality of times by changing the position of the support relative to the substrate.
In the method for producing a ceramic member of the present invention, the core material of the substrate can be completely covered with the ceramic coating by repeating the step of forming the ceramic coating by changing the position of the support relative to the substrate multiple times. For example, when the base material is graphite, in the first formation of the ceramic coating, the base material made of graphite is exposed in the vicinity where the support portion abuts. However, by changing the position of the support and using the ceramic member, which is the base material on which the ceramic coating is formed, as a new base material, a second ceramic coating is formed, so that two layers of exposed graphite base material are formed. Can be covered with a ceramic coating on the eyes.

(Embodiment)
The manufacturing method of the ceramic member of embodiment of this invention is demonstrated. In the method for manufacturing a ceramic member according to the embodiment of the present invention, the ceramic member 10 </ b> A is manufactured by forming the ceramic coating 21 on the base material 20 using the support 30.
First, as shown in FIG. 1A, the base material 20 is supported by a support tool 30. The number of the support tools 30 is not particularly limited. If the center of gravity of the substrate 20 can be lower than the support surface 322 at the tip of the support portion 32, even one support 30 can be stably formed by the CVD method using the ceramic coating 21 (the first ceramic coating 22 and the second ceramic coating 23). ) Can be formed. Further, the ceramic coating 21 can be formed by the CVD method by arranging the support portion 32 described later so that the area of the support portion 32 is sufficiently large and the center of gravity of the substrate 20 enters the support surface 322 of the support portion 32. .
Here, the case where the base material 20 is mounted substantially horizontally on a plurality of (three or more) support tools 30 will be described.

The substrate 20 is not particularly limited. For example, anything such as metal or ceramic can be used. Ceramic is suitable because it has heat resistance. Among them, ALN, Al ₂ O ₃ , graphite, BN, SiO ₂ , Si ₃ N _{4 and the} like can be used as the ceramic, and among them, graphite can be preferably used because it has excellent workability.
The shape of the base material 20 is not particularly limited. Since the ceramic member 10A is manufactured by forming the ceramic coating 21 on the base material 20, the base material 20 is processed into the shape of the target ceramic member 10A. The ceramic member 10A is manufactured in various shapes according to the application. For example, any disk, ring, cylinder, plate, box, etc. may be used and there is no particular limitation.

As shown in FIG. 2A and FIG. 2B, the support tool 30 has, for example, a columnar support tool body 31, a top surface on the main body upper surface 311, and the base material 20. The support portion 32 is in contact with the surface 201 and is higher than the outline 312 on the top surface. The support portion 32 has an overall truncated cone shape, and has a side surface 321 and a support surface 322. The support surface 322 has a planar shape with a certain area, but may have a shape with a sharp tip (conical shape).
The top surface of the main body upper surface 311 has a flat area excluding the support portion 32.

That is, as shown in FIG. 2B, the support portion 32 protrudes upward from a plane constituting most of the top surface of the main body upper surface 311, and the support surface 322 of the support portion 32 supports the base material 20. In doing so, a gap S is formed between the base material 20 and the top surface of the main body upper surface 311.
The distance L between the outermost edge 323 on the support surface 322 of the support portion 32 and the outer shape line 312 on the top surface is 4 to 20 times the gap S.

As for the support tool 30, the support tool main body 31 and the support part 32 are integrally formed. For example, the support tool main body 31 and the support part 32 can be formed by shaving or molding integrally with a mold. Moreover, the support tool main body 31 and the support part 32 can also be integrated by bonding with an adhesive or the like.
In addition, as the support tool 30, the following shapes are also employable.
The support tool 30A shown in FIG. 3A has a convex surface that rises in a curved shape from the outer shape line 312 toward the center on the top surface of the support tool main body 31, and the uppermost portion of the convex surface corresponds to the support portion.
A support tool 30 </ b> B shown in FIG. 3B has a hemispherical convex support part 32 partially formed at the center of the top surface, which is a flat surface of the support tool main body 31.
A support tool 30 </ b> C shown in FIG. 3C has a support part 32 that is partially conical at the center of the top surface that is the plane of the support tool main body 31.
A support tool 30D shown in FIG. 3D has a support tool body 31 formed in a quadrangular prism shape, and has a support part 32 having a generally truncated cone shape on the top surface of a quadrangle.
As described above, in any case, the support tools 30 </ b> A to 30 </ b> D are the same in that the shape of the support portion 32 and the support portion 32 protrude above the outline of the support tool main body 31.

As shown in FIG. 1B, a first ceramic film 22 (ceramic film 21) is formed on the surface of the base material 20 supported by the support 30 by a CVD method. At this time, the outer region of the top surface of the support 30 restricts the flow of the raw material gas of the coating into the inner region, and only a small amount of the raw material gas flows from the gap S between the outline 312 and the substrate 20. .
As a result, the first ceramic coating 22 is formed with an inclined portion 221 that is inclined toward the base member 20 toward the support portion 32 in the support region where the top surface of the support 30 is opposed. An opening 222 that is a non-film-forming region where the first ceramic coating 22 is not formed is formed inside the inclined portion 221.
In addition, a support part can be arrange | positioned in the center part of a top surface by making the outline of the top surface of a support tool, and the support part 32 concentric shape in planar view. In this way, the deviation in the distance that the source gas reaches can be made small, and the fixation with the base material 20 can be prevented equally regardless of the direction, and the area of the non-film forming region can be reduced.

  The ceramic coating 21 (the first ceramic coating 22 and the second ceramic coating 23 described later) is not particularly limited. For example, SiC, TaC, TiN, etc. can be used. Since SiC has the same thermal expansion coefficient as graphite having excellent workability, it is difficult to peel off, is harder than graphite, and has corrosion resistance. Therefore, it is desirable to use SiC in combination with a graphite base material.

  Subsequently, as shown in FIG. 1C, the portion of the base material 20 supported by the support tool 30 is changed and placed on the support tool 30 again, and the second ceramic coating 23 (ceramic) is formed by the CVD method. A coating 21) is formed. Here, for example, the case where the upper and lower surfaces of the base material 20 are reversed and placed on the support 30 is shown. In addition, the base 20 can be rotated while the upper and lower surfaces are left as they are, and the support portion by the support 30 on the lower surface can be changed.

Next, the ceramic member 10A manufactured as described above will be described. The ceramic member 10A is subjected to CVD twice, and has two ceramic coatings 21 (first ceramic coating 22 and second ceramic coating 23).
In the ceramic member 10 </ b> A manufactured in FIG. 1C, the base material 20 is covered with the first ceramic film 22 and the second ceramic film 23.
Here, in the first CVD, the base material 20 corresponds to the “base material” of the present invention, and the first ceramic coating 22 corresponds to the “ceramic coating” of the present invention. In the second (last) CVD, the substrate 20 and the first ceramic coating 22 correspond to the “substrate” of the present invention, and the second ceramic coating 23 corresponds to the “ceramic coating” of the present invention. To do. In the first CVD, the position of the support relative to the substrate is changed, and the substrate 20 is covered with the first ceramic film and / or the second ceramic film. In any CVD, the base material has a graphite core material.

In the first ceramic coating 22, a support region 220 including an inclined portion 221 and an opening 222 is formed by the support tool 30 that is supported when the first ceramic coating 22 is formed (FIG. 1B). reference). The support region is formed to face the top surface of the support tool.
The opening 222 and the inclined portion 221 generated when the first ceramic coating 22 is formed are covered with the second ceramic coating 23 by the second (last) CVD as shown in FIG. That is, the opening 222 and the inclined portion 221 formed by the first CVD become the portion 222 ′ and the inclined portion 221 ′ which are the opening portions by the second (last) CVD, and the support region 220 is A portion 220 ′ that was covered with the second ceramic coating 23 and was a support region is formed.

Further, as shown in FIGS. 4A and 4B, the second ceramic film is formed on the portion supported by the support tool 30 when the second ceramic film 23 is formed in the second CVD. There is an opening 222 through which the first ceramic coating 22 is exposed without the coating 23 being formed. Around the opening 222, an inclined portion 221 is formed in which the film thickness gradually decreases from the surface of the second ceramic coating 23 to the interface 232 with the first ceramic coating 22. Note that the opening 222 and the inclined portion 221 constitute a support region 220.
The area of the opening 222 is 10% to 60% of the area of the support region 220.

Next, the operation and effect of the method for manufacturing a ceramic member according to the embodiment of the present invention will be described.
According to the method for manufacturing a ceramic member of the embodiment of the present invention, the base material 20 is supported using the support tool 30, and the ceramic coating 21 is formed on the surface of the base material 20 by the CVD method in this state. At this time, the support 30 is surrounded by the outline 312 on the top surface so that the support 30 has a gap S with respect to the support 201 and the surface 201 of the base 20 and the surface 201 of the base 20. .

For this reason, it is possible to prevent the CVD source gas from entering the support portion 32 by the outer region of the top surface surrounded by the outline, and the ceramic coating 21 formed with the support portion 32 and the base material 20 is fixed. Can be prevented.
For this reason, the base material 20 placed on the support tool 30 is not fixed by the ceramic coating 21 after the CVD, and when it is removed, harmful burrs and micro cracks are prevented from occurring around the support point. can do.

According to the method for manufacturing a ceramic member of the embodiment of the present invention, since the support 30 is integrally formed with the support portion 32, the base material 20 is placed when the base material 20 is placed on the support tool 30. If the substrate 20 is to be placed at an angle, the base material 20 comes into contact first from the end, which is the outline 312 on the top surface. For example, when the base material 20 is a flat surface, the support portion 32 comes into contact with the base material 20 only when the mounting surface formed by the tips of the plurality of (for example, three points) support portions 32 and the base material 20 become parallel. become able to.
For this reason, it is difficult to damage the tip of the support portion 32. Moreover, the space | interval of the clearance gap S of the base material 20 and a top surface is securable.

According to the method for manufacturing a ceramic member of the embodiment of the present invention, the distance L between the outermost edge 323 of the support portion 32 and the outer shape line 312 which is the end portion of the top surface of the support 30 is 4 of the gap S. When it is twice or more, the raw material gas that has entered from the gap S can hardly reach the contact point between the support portion 32 and the base material 20. For this reason, sticking of the support tool 30 and the base material 20 can be made difficult to occur.
In addition, when the distance L between the outermost edge 323 of the support portion 32 and the outer shape line 312 which is the end portion of the top surface in the support tool 30 is 20 times or less of the gap S, the ceramic film 21 is applied to the base material 20. Since the opening 222 that is not formed can be reduced, that is, the area covered with the ceramic coating 21 can be increased, the substrate 20 can be easily protected.

  According to the method for manufacturing a ceramic member of the embodiment of the present invention, when the ceramic coating 21 is SiC, there are the following merits. That is, since SiC is chemically stable, consumption of the base material 20 can be prevented. Further, since SiC is a hard and wear-resistant ceramic material, it is possible to prevent the substrate 20 from being worn or damaged.

  According to the method for manufacturing a ceramic member of the embodiment of the present invention, the substrate 20 is made of graphite in the first CVD. Since graphite has a cleavage plane in the crystal, if the central portion of the substrate 20 is made of graphite, it can be easily processed, and ceramic members 10A having various shapes can be obtained. In the second CVD, a base material made of graphite covered with the ceramic coating 21 (first ceramic coating 22) is used. Since graphite is a core material, it can be easily processed in the same manner, and various shapes of ceramic members 10A can be obtained.

  According to the method for manufacturing a ceramic member of the embodiment of the present invention, the core material of the base material 20 can be completely covered with the ceramic coating by changing the position of the support 30 with respect to the base material 20 and repeating a plurality of times. it can. For example, when the base material 20 is graphite, in the first formation of the ceramic coating 21 (first ceramic coating 22), the base material 20 made of graphite is exposed in the vicinity where the support portion 32 abuts. However, by changing the position of the support 30, the ceramic member 10 </ b> A that is the base material 20 on which the ceramic coating 21 is formed is used as a new base material 20 to form the second ceramic coating 21 (second ceramic coating 23). I do. As a result, the exposed graphite substrate 20 can be covered with the second ceramic coating 21 (second ceramic coating 23).

  The method for producing a ceramic member of the present invention can be used to produce a ceramic member having a ceramic film formed on a substrate.

10A, 10B Ceramic member 20 Base material 201 Surface 21 Ceramic coating 30, 30A, 30B, 40 Support tool 312 Outline line 32, 42 Support part 323 Outermost edge S Clearance

Claims (7)

In a method for producing a ceramic member, in which a ceramic film is formed on the surface of the base material by a CVD method after the base material is supported using a support tool,
The said support tool has a top surface surrounded by the outline, and has a support part higher than the said outline on the inner side of the said top surface, The manufacturing method of the ceramic member characterized by the above-mentioned.   The method for manufacturing a ceramic member according to claim 1, wherein the support portion is in the center of the top surface.   The method for manufacturing a ceramic member according to claim 2, wherein the top surface is a convex surface rising from the outline.   The method for manufacturing a ceramic member according to claim 1, wherein the support has a protrusion inside.   The method of manufacturing a ceramic member according to claim 1, wherein the ceramic coating is SiC.   The method for producing a ceramic member according to any one of claims 1 to 5, wherein the base material has a graphite core material.   7. The ceramic member according to claim 1, wherein the step of forming the ceramic coating is repeated a plurality of times by changing the position of the support relative to the base material. 8. Production method.

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