KR20110012902A - Method of preparing rbsc assembly and rbsc assembly prepared thereby - Google Patents

Abstract

PURPOSE: A method for preparing a silicon carbide sintered body assembly is provided to enable defect processing per one piece and to perform silicon impregnation, thereby improving productivity. CONSTITUTION: A method for preparing a silicon carbide sintered body assembly comprises the steps of: manufacturing a pre-sintered body for a reactive sintering process; impregnating the pre-sintered body in molten silicon; processing a silicon carbide sintered body which is impregnated in silicon; and adding an Six-Ge(1-x) (0.65<x<0.95) solid solution from a bonding agent to the processed silicon carbide sintered body, and heating it at 1300-1400°C to complete the assembly.

Description

Method for manufacturing silicon carbide sintered body bonded body and silicon carbide sintered body body manufactured thereby {METHOD OF PREPARING RBSC ASSEMBLY AND RBSC ASSEMBLY PREPARED THEREBY}

The present invention relates to a method for producing a silicon carbide sintered body assembly and a silicon carbide sintered body manufactured thereby. More specifically, a silicon body is not impregnated after bonding the body, for example, a jig and the whole, but the silicon impregnated by collecting the individual parts. Since it is possible to impregnate more items in the same impregnation tank, it is possible to increase the productivity, and if the defect occurs in the processing process after impregnation, it is possible to process the defects in single unit, so that the product manufacturing productivity can be improved. A method for producing a silicon sintered compact and a silicon carbide sintered compact manufactured thereby.

Silicon carbide (silicon carbide, SiC) has good thermal conductivity, corrosion resistance, chemical resistance and low thermal expansion rate compared to conventional silicon or quartz materials used in LP-CVD process. It is attracting attention as a material to become.

In particular, high-purity silicon carbide conjugates (particularly jigs) are stable even at high temperatures of more than 1,200 ° C, which greatly contributes to quality and efficiency improvement in semiconductor diffusion processes, atmospheric CVD, and LP-CVD processes. Specific examples thereof include wafer boats for semiconductor processes, and in particular, diffusion boats.

The manufacture of such silicon carbide conjugates is usually made by a reaction sintering method, and the silicon carbide sintered body thus prepared is called a reaction bonded silicon carbide (RBSC). A method for producing a silicon carbide sintered body according to a reaction sintering method for manufacturing a conventional RBSC is as disclosed in Korean Patent Laid-Open Publication No. 10-2004-111393, and the silicon carbide sintered body thus prepared always maintains uncarburized residual Si. It is sometimes referred to as Si-SiC because it has a degree.

By the way, when manufacturing a bonded body (wafer boat) as shown in the drawing of the Republic of Korea Patent Application Publication No. 10-2004-111393 by the method of manufacturing a silicon carbide sintered body assembly, a single part (parts) constituting the entire bonded body (jig) These products were calcined at 1500 to 2000 ° C., respectively, to form a single-piece plasticized body, and then processed into the required shape. It forms a binder and immerses it in molten silicon at 1450 ~ 1700 ℃, the molten silicon penetrates into the pores of the plasticized body, and then reacts with the free carbon in the plasticized body to form silicon carbide to fill the pores with silicon carbide and unreacted silicon (Impregnation process), and in order to form a SiC rich layer on the surface of the sintered body is coated with Si and heated to 1450 ~ 1700 ℃ again Going through.

In actual production, however, when the wafer boat is manufactured in the above-described process, the precision of the bonded body (jig) decreases after being immersed in the molten silicon, and thus a separate processing step is further required after the impregnation process. Processing after the process has a lot of problems of damage or damage during processing due to the high strength of the sintered body, there is a problem that the entire assembly (jig) should be discarded in the case of such defects, immersed by impregnating the assembly plasticity There is a problem that the size of the impregnating tank must be large, the use efficiency of the impregnating tank falls, and there is a problem that Si is eluted in the heating process due to the high heating temperature in the heating process for forming the SiC rich layer.

Therefore, there is an urgent need to develop a manufacturing method that can solve such a problem and reduce the defects of a complicated shape joined body (jig) with high productivity without causing problems such as Si elution.

In order to solve the problems of the prior art as described above, the present invention is not to proceed with silicon impregnation after joining the entire assembly, but can be impregnated with a single product so that the impregnation of more articles in the same impregnation tank to increase the productivity It is possible to provide a method for producing a silicon carbide sintered body assembly and a silicon carbide sintered body manufactured thereby, which can be treated in a single unit when a defect occurs in the processing process after the impregnation, thereby increasing the product manufacturing productivity. For the purpose of

In addition, an object of the present invention is to provide a method for producing a silicon carbide sintered compact and a silicon carbide sintered compact manufactured thereby, which can solve the problems of Si dissolution and binder dissolution while achieving the above object.

In order to achieve the above object, the present invention

In the method of manufacturing a RBSC (Reaction bonded silicon carbide) conjugate,

Manufacturing each component constituting the joined body into a single silicon carbide calcined body for reaction sintering;

Impregnating the obtained single-piece plastic sintered body into molten silicon;

Processing the single silicon carbide sintered body made of silicon impregnation; And,

And a step of adding the single-component silicon carbide sintered body to which Si _x -Ge _(1-x) (0.65 <x <0.95) solid solution is processed as a binder and heat-processing at 1300 to 1400 ° C. to complete the assembly of the assembly. Provided is a method for producing a silicon carbide sintered body joined body.

Also,

It is produced by the method for producing the silicon carbide sintered compact,

A silicon carbide sintered body joined body is provided, wherein each of the parts forming the joined body and the joined body having a joining portion at a bonding surface between the single parts are provided.

According to the manufacturing method of the silicon carbide sintered body assembly of the present invention and the silicon carbide sintered body manufactured thereby, the silicon impregnation is carried out after the bonding of the whole body rather than the silicon impregnation, so that the silicon impregnation can proceed to the same impregnation tank. Impregnation can be performed to increase productivity, and when impairment occurs in the processing process after impregnation, defects can be treated in a single unit, thereby increasing the product manufacturing productivity.

In addition, the present invention obtains the effects described above, and does not cause problems of Si elution and binder elution, so that the effect of excellent strength and a stable bonded body can be obtained.

Hereinafter, the present invention will be described in detail with reference to the accompanying drawings.

The present invention relates to a method for producing a silicon carbide sintered body assembly, the method of manufacturing a reaction bonded silicon carbide (RBSC) assembly, comprising: manufacturing each component constituting the body into a single silicon carbide plastic body for reaction sintering; Impregnating the obtained single-piece plastic sintered body into molten silicon; Processing the single silicon carbide sintered body made of silicon impregnation; And an assembling step of adding the single silicon carbide sintered body processed to Si _x -Ge _(1-x) (0.65 <x <0.95) solid solution as a binder and performing heat treatment at 1300 to 1400 ° C. to complete assembly of the bonded body. It is composed.

That is, an example of a conventional reaction sintering method is as shown in the Republic of Korea Patent Publication No. 10-2004-111393, each individual process of the present invention shares the same principle as the reaction sintering method. However, in the present invention, in order to improve the problems of the conventional manufacturing process described above in the case of a bonded body (for example, a jig) having a complicated structure, to assemble the assembly first in the conventional manufacturing process and then impregnated it, After the impregnation, the process of assembly was developed.

However, as described above, if only the process sequence is changed, the assembly step is performed by the bonding slurry conventionally used in the assembling step, and the sintering process is required for the sintering of the bonded slurry, and the temperature for sintering the normal bonding slurry is 1500. Si-eluting from the sintered body during heat treatment for bonding due to higher than the silicon melting temperature (about 1410 ℃) to 2000 ℃ to occur, the strength of the sintered body, deformation of the shape occurs, the process can not be carried out to develop the process of the present invention will be.

To this end, the present invention, in the manufacturing method of the reaction bonded silicon carbide (RBSC) bonded body, the step of manufacturing each component constituting the bonded body as a single piece silicon carbide plastic sinter for the reaction sintering method is first performed. This is the same as the step of preparing the plasticized body in a conventional reaction sintering method, in which an organic material as a carbon source, preferably a solvent (for example, phenol, PVA, PVB, etc.) is mixed with a conventional silicon carbide powder. It may include all processes such as sintering after drying and immersion in an organic solvent or resin as a carbon source for additional carbon supply. Here, the plasticized body is produced in each unit of the bonded body forming the whole bonded body. Preferably, the one-piece silicon carbide sintered body may be manufactured by mixing and molding the silicon carbide powder and the carbon source, followed by molding and plasticizing at 1500 to 2000 ° C.

Next, the step of impregnating the obtained single-piece plastic sintered body into the molten silicon is carried out. Conventionally, this is done for the assembly, so if only one assembly could be immersed in the same impregnating bath containing molten silicon, when immersing in a single piece, the single parts can be immersed in the impregnation tank at a time to produce more assemblies. It can increase the utilization of the impregnation tank and increase the productivity of the process. The impregnation process is the same as the impregnation step in a conventional reaction sintering method.

Next, the step of processing to the required shape for the manufacture of the bonded body to the specimen subjected to the impregnation process is performed. That is, the step of processing the single silicon carbide sintered body made of silicon impregnation is performed. For example, in the case of a wafer boat, this may be the machining of a slot for wafer mounting. Therefore, in this process, the faulty or damaged unit may be disposed of as a unit, so that the yield can be improved as compared with the case of discarding a conventional assembly.

Finally, the assembly step of adding the single silicon carbide sintered compact thus processed to Si _x -Ge _(1-x) (0.65 <x <0.95) solid solution is added as a binder and heat-treated at 1300 to 1400 ° C. to complete the assembly of the assembly. Perform. That is, since the conventional bonding slurry is a slurry composed of an organic solvent of SiC and a carbon source, in order to form the bonding between the components, the bonding slurry needs to be subjected to a heat treatment of at least 1500 ° C. after applying the bonding slurry, and then applied after the Si-impregnation. Since Si elution occurs, it is possible to bond parts at a temperature lower than the melting point of Si to prevent Si elution, but also has a high melting point of the adhesive itself. 1200 ° C.) is developed, and there is little problem in the coefficient of thermal expansion after solidification, the sintered body is easily impregnated, and a binder which does not affect the semiconductor manufacturing process is developed and applied. That is, as shown in the Ge-Si state diagram in FIG. 1, the Si-Ge solid solution having a concentration in the range of Si _x -Ge _(1-x) (0.65 <x <0.95, x: atomic percent of silicon) is Si It has a higher melting point (more than 1200 ° C.) but lower than the melting point, and thus does not melt in the coating process as a later process, which will be described later.

Preferably x is from 0.75 to 0.85 may reduce the high temperature stability and Si dissolution, the heat treatment time may vary depending on the size of the bonding surface and the bonding (jig), and sufficient melting and bonding of the bonding agent is made It is preferable that it is a time which can be used, for example, it is good to proceed for 30 minutes-2 hours.

One embodiment of the manufacturing method of the binder is as shown in Figure 2, according to this, by mixing the Si and Ge powder in the above range by pressing and then sintered for about 3 hours at 1000 to 1200 ℃ The sintered compact is obtained and pulverized into a desired form to be used as a binder. Thus, the binder may be prepared in the form of a slurry in which the binder is bulk or powder or a mixture of the powder and the solvent (preferably an organic solvent that can act as a carbon source).

As shown in FIG. 1, since Ge-Si is a completely solid solution in the entire mixing ratio region, the sintered compact is a Si-Ge solid solution.

Further preferably, as shown in the specific example of Figure 3, in the assembling step, the processed single silicon carbide sintered body is bonded (for example, oven dried by bonding after bonding) to the bonding slurry, the bonding The bonding process is performed by adding the Si _x -Ge _(1-x) (0.65 <x <0.95) solid solution as a bonding agent on the bonding surface bonded by slurry or on the bonding surface on which the carbon fiber or the carbon fiber nonwoven fabric is attached. Since it is easy to inject | pour into a bonding surface of a binder, it is good.

Here, the bonding slurry is a bonding slurry used for ordinary RBSC bonding, a mixture of a solvent mixed with a silicon carbide powder or a mixture further containing a carbon source material containing a carbon block as a carbon source (for example, , SiC: carbon black: phenol = 100: 1 to 10: 1 to 30 (weight ratio)) (in the case of Fig. 3) i) a mixture of SiC powder + carbon black + phenol having a size of # 1000 mesh (100: 1 to 10: 1 to 30 (weight ratio) bonding slurry is applied and the bonding agent is attached thereto, followed by heat treatment to impregnate the bonding agent, followed by polishing to complete the bonding.

In this case, the bonding slurry has a low temperature during the bonding process so that no sintering occurs, a partially melted binder is impregnated between the silicon carbide powder, and the silicon melt reacts with the carbon source to be converted into SiC to bond the bonding surface. .

To this end, as shown in FIG. 3, a bulk or powder binder is attached onto the bonding slurry to be fixed to the bonding surface bonded by the bonding slurry, or the carbon fiber is formed on the bonding slurry forming the bonding surface. B, a carbon fiber nonwoven fabric may be attached, and a bulk or powder binder may be attached thereon to allow the melt of the binder to be guided and flow along the carbon fiber to the bonding surface.

In addition, when the binder is composed of a slurry type, in the granulation step, the processed single silicon carbide sintered body in the form of a slurry containing the Si _x -Ge _(1-x) (0.65 <x <0.95) solid solution powder A method of adding the Si _x -Ge _(1-x) (0.65 <x <0.95) solid solution as a binder by bonding to a mixture (for example, solid solution powder: phenol = 30 to 80: 1 to 30 (weight ratio)) You can also take In this case, the slurry mixture containing the solid solution powder may further include silicon carbide powder, a carbon source material, and the like (for example, solid solution powder: SiC powder: carbon black: phenol = 30 to 80: 100:). 1 to 10: 1 to 30 (weight ratio))

Through the bonding step, the RBSC unit may be composed of an assembly. As a specific example of this, in the bonding process by the method shown in FIG. 3, the bonding slurry is made of SiC powder of +1000 mesh size + carbon black + phenol. After bonding in the case of application in a mixture, the microphotograph is shown in FIG. That is, it was confirmed that the bonding surface having a continuous microstructure was formed through this. In addition, as a result of performing a three-point bending strength test, in the case of Figure 4 was obtained a strength of about 250 MPa was able to confirm the excellent adhesion.

In addition, after such assembling process, it may further include a further processing or surface treatment process for the joint as necessary. That is, after the assembling step, the surface treatment step of forming a silicon carbide rich layer on the surface of the assembled assembly can be further included, thereby ensuring stability and strength. Preferably, the surface treatment step may be treated by chemical vapor deposition (CVD) of silicon carbide at 1200 to 1300 ℃, in this process, the elution of the binder or the elution in the sintered body does not occur. Since the CVD process is a conventional surface treatment process, a detailed description thereof will be omitted.

In another aspect, the present invention provides a silicon carbide sintered body assembly manufactured by the above-described manufacturing method, which is manufactured by the above-described method of manufacturing a silicon carbide sintered body assembly, each of the components forming the assembly and the coupling between the individual components It is made of a bonded body having a junction on the surface, and specific examples thereof may include various jigs used as heat treatment jigs in a semiconductor process and the like, and examples thereof may include wafer boats for semiconductor processes.

The present invention described above is not limited to the above-described embodiment and the accompanying drawings, and various modifications and changes made by those skilled in the art without departing from the spirit and scope of the present invention described in the claims below. Changes are also included within the scope of the invention.

1 shows a two-component state diagram of Ge-Si.

2 is a view schematically showing an embodiment of a manufacturing method of a bonding agent applied to the manufacturing method of the silicon carbide sintered compact of the present invention.

Figure 3 is a schematic step-by-step view of the bonding process applied to the method for producing a silicon carbide sintered compact of the present invention.

4 is a photomicrograph of the microstructure of the junction of the bonded body produced by the method for producing a silicon carbide sintered body bonded body of the present invention.

Claims (10)

In the method of manufacturing a RBSC (Reaction bonded silicon carbide) conjugate, Manufacturing each component constituting the joined body into a single silicon carbide calcined body for reaction sintering; Impregnating the obtained single-piece plastic sintered body into molten silicon; Processing the single silicon carbide sintered body made of silicon impregnation; And, And the assembling step of adding the Si _x -Ge _(1-x) (0.65 <x <0.95) solid solution to the processed silicon carbide sintered body as a binder and performing heat treatment at 1300 to 1400 ° C. to complete the assembly of the joined body. The manufacturing method of the silicon carbide sintered compact joined. The method of claim 1, In the production of the single-piece silicon carbide sintered body, the silicon carbide powder and the carbon source are mixed and then molded and plasticized at 1500 to 2000 ° C. The method of claim 1, In the assembling step, the processed single silicon carbide sintered body is bonded with a bonding slurry, and the Si _x -Ge is bonded on the bonding surface bonded to the bonding slurry or on a bonding surface where a carbon fiber or a carbon fiber nonwoven fabric is attached to the bonding surface. _{(1-x) A} method for producing a silicon carbide sintered compact, comprising adding a solid solution (0.65 <x <0.95) as a binder. The method of claim 1, In the assembling step, the processed single silicon carbide sintered body is bonded to a mixture in the form of a slurry containing the Si _x -Ge _(1-x) (0.65 <x <0.95) solid solution powder to form the Si _x -Ge _{(1 -x) A} method for producing a silicon carbide sintered compact, characterized by adding a (0.65 <x <0.95) solid solution as a binder. The method according to claim 1 or 3, The binder is a bulk or powder or a method of producing a silicon carbide sintered compact, characterized in that the slurry is a mixture of the powder and the solvent. The method of claim 3, Said bonding slurry is a mixture of a silicon carbide powder mixed with a solvent or a mixture containing a carbon source material containing carbon black in the mixture further comprising a silicon carbide sintered body manufacturing method. The method of claim 1, After the assembling step Method for producing a silicon carbide sintered body assembly further comprising a surface treatment step of forming a silicon carbide rich layer on the surface of the assembled assembly. The method of claim 7, wherein The surface treatment step is a method of producing a silicon carbide sintered compact, characterized in that the chemical vapor deposition of silicon carbide made at 1200 to 1300 ℃. It is manufactured by the manufacturing method of the silicon carbide sintered compact of any one of Claims 1-8, A silicon carbide sintered body joined body, comprising: a single body comprising each joined part that forms the joined body, and a joined part that has a joining surface at a bonding surface between the single parts. 10. The method of claim 9, And the bonded body is a wafer boat for a semiconductor process.

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