KR101199088B1 - Method for manufacturing silicon carbide sintered body and susceptor including silicon carbide sintered body - Google Patents

Method for manufacturing silicon carbide sintered body and susceptor including silicon carbide sintered body Download PDF

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KR101199088B1
KR101199088B1 KR20100074434A KR20100074434A KR101199088B1 KR 101199088 B1 KR101199088 B1 KR 101199088B1 KR 20100074434 A KR20100074434 A KR 20100074434A KR 20100074434 A KR20100074434 A KR 20100074434A KR 101199088 B1 KR101199088 B1 KR 101199088B1
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silicon carbide
sintered body
method
carbide sintered
raw material
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KR20100074434A
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Korean (ko)
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KR20120012344A (en
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김명정
김민성
김영남
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엘지이노텍 주식회사
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Abstract

The method for producing a silicon carbide sintered compact according to an embodiment includes: mixing a first silicon carbide powder having a first central particle diameter and a second silicon carbide powder having a second central particle diameter smaller than the first central particle diameter; And a heating step of heat treating the mixed raw material to form a silicon carbide sintered body.

Description

METHOD FOR MANUFACTURING SILICON CARBIDE SINTERED BODY AND SUSCEPTOR INCLUDING SILICON CARBIDE SINTERED BODY}

The present substrate relates to a method for producing a silicon carbide sintered body and a susceptor including the silicon carbide sintered body.

In a semiconductor process or the like, a substrate or a wafer is placed on a susceptor for deposition, etching, and the like. Such a susceptor may be made using silicon carbide having high heat resistance to withstand conditions such as high temperature. A general susceptor is formed by depositing a high purity silicon carbide layer on a body containing graphite.

When a sintering aid of metal is added to form a sintered body formed of silicon carbide, the substrate or wafer may be contaminated by the sintering aid which is an impurity. If the sintering aid of the metal is not added, the sintered density may be lowered and the durability of the sintered compact may be lowered.

An embodiment is to provide a method for producing a silicon carbide sintered body capable of producing a silicon carbide sintered body having high purity and excellent characteristics, and a susceptor including the silicon carbide sintered body produced thereby.

The method for producing a silicon carbide sintered compact according to an embodiment includes: mixing a first silicon carbide powder having a first central particle diameter and a second silicon carbide powder having a second central particle diameter smaller than the first central particle diameter; And a heating step of heat treating the mixed raw material to form a silicon carbide sintered body.

The first central particle diameter may be 1 to 100 μm, and the second central particle diameter may be 30 nm to 10 μm. For example, the first central particle size may be 1 to 5 μm, and the second central particle size may be 30 nm or more and less than 1 μm.

Pressing in the heating step may be performed together with the molding step. In the raw material mixing step, the second silicon carbide powder may be the same as the first silicon carbide powder or more than the first silicon carbide powder. In the raw material mixing step, the first silicon carbide powder may be mixed 10 to 50 wt%, the second silicon carbide powder 50 to 90 wt%, the resin 1 to 20 wt%.

And a molding step of molding the mixed raw material between the raw material mixing step and the heating step, and may be heated by adding silicon to the molded mixed raw material in the heating step. In the raw material mixing step, the second silicon carbide powder may be the same as the first silicon carbide powder or less than the first silicon carbide powder. In the raw material mixing step, 50 to 90 wt% of the first silicon carbide powder, 10 to 50 wt% of the second silicon carbide powder, and 1 to 20 wt% of the resin may be mixed. A processing step may be further included between the forming step and the heat treatment step.

The susceptor according to the embodiment includes a silicon carbide sintered body manufactured by the above-described method for producing a silicon carbide sintered body.

The silicon carbide sintered body manufactured by the method for producing the silicon carbide sintered body according to the embodiment may be manufactured with high purity since it does not contain a sintering aid. As a result, since the silicon carbide layer does not have to be formed by a separate deposition process, a bulk silicon carbide sintered body may be used as the susceptor.

The silicon carbide sintered body may have a high density since the first silicon carbide powder and the second silicon carbide powder having different center particle diameters are mixed and sintered. Thereby, the strength, electrical conductivity, and thermal conductivity of the silicon carbide sintered body can be improved.

1 is a process flowchart showing a method for producing a silicon carbide sintered body according to the first embodiment.
2 is a schematic view of a hot press sintering apparatus that can be used in the method for producing a silicon carbide sintered body according to the first embodiment.
3 is a perspective view illustrating a mold member of the hot pressure sintering apparatus of FIG. 2.
4 is a process flowchart showing a method of manufacturing the silicon carbide sintered body according to the second embodiment.

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

1 is a process flowchart showing a method for producing a silicon carbide sintered body according to the first embodiment.

Referring to FIG. 1, the method of manufacturing the silicon carbide sintered body according to the present embodiment may include a raw material mixing step ST10, a granulation step ST20, and a heating and molding step ST30. In the present embodiment, the method for producing a silicon carbide sintered body forms a silicon carbide sintered body by a hot pressure sintering method. This will be described in more detail as follows.

In the raw material mixing step ST10, the first silicon carbide powder having the first central particle diameter and the second silicon carbide powder having the second central particle diameter smaller than this are mixed. At this time, the first and second silicon carbide powder may be mixed with the solvent in a solvent. As such a resin, a phenol resin may be used, and the solvent may include an alcohol or an aqueous substance. Examples of the alcohol-based substance include methanol, ethanol, and isopropyl alcohol (IPA), and water may be used as the aqueous substance. However, the embodiment is not limited thereto.

In this embodiment, since the first silicon carbide powder and the second silicon carbide powder having different center particle diameters are mixed, the mixed raw material may have a high density. Thereby, the density of the silicon carbide sintered compact manufactured using this mixed raw material can be improved, and the durability of a silicon carbide sintered compact can be improved.

For example, the first central particle size may be 1 to 100 μm, the second central particle size may be 30 nm to 10 μm, and the first central particle size may be larger than the second central particle size. In this case, when the first center particle size exceeds 100 μm, the particle size of the silicon carbide may be increased, and it may be difficult to form a sintered body of high purity silicon carbide. When the first center particle size is less than 1 μm, the difference from the second center particle size may be small. The degree of improvement may be small. When the second central particle diameter exceeds 10 μm, the difference with the first central particle diameter may be small, and the degree of density improvement may be small. When the second central particle diameter is less than 30 nm, problems such as explosion due to fine powder may occur.

In this case, the first central particle diameter may be 1 to 5 μm, and the second central particle diameter may be 30 nm or more and less than 1 μm. This omits the step of pulverizing the silicon carbide powder in order to form a sintered body of high-purity silicon carbide, it is considered that the sinterability may be reduced when the center particle size exceeds a certain level. That is, the above-mentioned 1st and 2nd center particle diameters are determined in the range which can improve sinterability.

In this case, the first silicon carbide powder and the second silicon carbide powder may be included in the same amount, or more second silicon carbide powder may be included than the first silicon carbide powder. This is to improve the sinterability in consideration of the smoother material movement to break the covalent bond than the first silicon carbide powders having a small particle diameter than the second silicon carbide powders having a large particle size.

For example, 10 to 50 wt% of the first silicon carbide powder, 50 to 90 wt% of the second silicon carbide powder, and 1 to 20 wt% of the resin may be mixed in the solvent.

In order to form a high purity silicon carbide sintered body in the present embodiment, the first and second silicon carbide powder may contain impurities of 10 ppm (parts per million) or less. This was determined to form a sintered body of high purity silicon carbide.

Subsequently, in the granulation step ST20, the mixed raw materials are granulated. In one example, a spray dryer may be used to granulate the mixed raw materials.

Subsequently, in the heating and molding step ST30, the granulated mixed raw material may be put into a hot pressurizing sintering apparatus and hot pressed to form a silicon carbide sintered body having a desired shape. That is, in the hot pressure sintering apparatus, the molding can be performed together in the heating step.

In the heating and molding step ST30, for example, the mixed raw material granulated at a pressure of 20 MPa or more at a temperature of 2100 ° C. or more may be hot pressed. However, the embodiment is not limited thereto.

An example of a hot press sintering apparatus 100 that can be used in the heating and forming step ST30 is shown in FIGS. 2 and 3.

Referring to FIG. 2, the hot pressurizing and sintering apparatus 100 according to the present embodiment includes a chamber 10 in which a vacuum is maintained, a mold member 20, a pressurizing member 30, and heating located in the chamber 10. The member 40 and the heat insulation member 50 are included. This will be described in more detail as follows.

Chamber 10 may be closed to maintain a vacuum. Thereby, oxidation of the heating member 40 etc. which are located in the chamber 10 can be prevented, and it can prevent that a contaminant mixes in a raw material during a sintering process.

A vacuum jump 102 for the vacuum is positioned outside the chamber 10 to maintain the vacuum, and the vacuum pump 102 and the chamber 10 may be connected through the opening / closing valve 104 and the exhaust port 106. . As a result, the air may be selectively discharged to maintain the interior of the chamber 10 at a predetermined level of vacuum. In addition, a separate gas supply source (not shown), an open / close valve (not shown), and an injection hole (not shown) may be positioned to inject an inert gas into the chamber 10.

The raw material is filled in the mold member 20 located in the chamber 10. Such a mold member 20 will be described in more detail later with reference to FIG. 3.

The pressurizing member 30 for press-molding the raw material in the mold member 20 may include a lower pressurizing member 31 positioned below and an upper pressurizing member 32 positioned above. The pressing member 30 may be made of a material that can withstand high temperatures, for example, may include graphite.

In this case, a graphite plate or / and graphite sheet 31a including graphite having high purity, for example, 99.99 to 99999%, may be disposed on the upper surface of the lower pressing member 31. Similarly, a graphite plate or / and graphite sheet 32a including graphite of high purity, for example, 99.99 to 99.9% of the graphite, may be disposed on the lower surface of the upper pressing member 32.

Outside the mold member 20, a heating member 40 for heating the inside of the chamber 10 (in particular, a raw material located in the mold member 20) is located. As the heating member 40, various methods for heating the mold member 20 may be applied. For example, the heating member 40 may include graphite and generate heat by power supplied from the outside to heat the mold member 20.

The insulating member 50 positioned between the heating member 40 and the chamber 10 serves to maintain the mold member 20 at a temperature suitable for the reaction. The heat insulating member 20 may include graphite to withstand high temperatures.

In the hot pressurizing and sintering apparatus 100, the raw material is filled into the mold member 20 while the lower pressing member 31 is located in the mold member 20, and the high temperature is maintained by the heating member 40. The raw material is pressurized using the upper press member 32 in the state. Then, the raw material is sintered to a desired shape by high temperature and high pressure.

Hereinafter, the mold member 20 of this embodiment will be described in more detail with reference to FIG. 3. 3 is a perspective view illustrating a mold member of the hot pressurizing and sintering apparatus according to the embodiment.

Referring to FIG. 3, the mold member 20 is inserted into the first mold portion 22 constituting the outer shape and the opening 22a of the first mold portion 22 and includes a mold space portion 24a. The second mold part 24 is included. The raw material is filled into the mold space 24a, and the raw material is pressurized by the pressing member (30, the same as below in Fig. 2) to sinter the raw material into a desired shape.

In this case, the second mold part 24 may be formed with a narrower area than the upper part. For example, the second mold part 24 may have a shape in which the area gradually decreases from the top to the bottom. The opening 22a of the first mold part 22 may have a shape corresponding to the outer shape of the second mold part 24. That is, the opening 22a may have a shape in which the area gradually decreases from the top to the bottom.

As a result, the second mold part 24 can be easily inserted into the first mold part 22 by inserting the second mold part 24 into the opening 22a of the first mold part 22.

At this time, a value obtained by subtracting the radius R2 of the mold space portion 24a from the radius R1 of the second mold portion 24 measured at the upper portion of the second mold portion 24 is a and the second mold portion 24 is obtained. When b is the value obtained by subtracting the radius R4 of the mold space portion 24a from the radius R3 of the second mold portion 24 measured at the lower portion of b), the ratio of b to a is 0.1 to 0.9 days. Can be. This is to prevent the second mold part 24 from being separated from the first mold part 22 by inserting the second mold part 24 in close contact with the opening 22a of the first mold part 22.

If the value obtained by subtracting the radius R4 of the mold space portion 24a from the radius R3 of the second mold portion 24 measured at the lower portion of the second mold portion 24 is 0, the second mold portion 24 There is a high risk of breakage at the bottom. Therefore, the lower portion of the second mold portion 24 may have a larger area than the mold space portion 24a.

Such mold member 24 may comprise a material that can withstand high temperatures, such as graphite.

In the present embodiment, the second mold portion 24 constituting the mold space portion 24a filled with the raw material contains graphite of high purity (for example, 99.99 to 99999%), and the second mold portion 24 is The first mold part 22 to be inserted may include graphite of general purity (eg, 90% or more and less than 99.99%).

As such, the second mold part 24 directly contacting the raw material may be formed of high purity graphite to prevent the mold member 20 from being damaged at high temperature and high pressure. For example, the conventional mold member made of graphite of general purity has a breaking strength of 30 MPa, whereas the mold member 20 according to the present embodiment may have a breaking strength of 60 MPa. As such, it can be seen that in the present embodiment, the fracture strength can be approximately twice that, and the damage can be effectively prevented. Thereby, the cost of component replacement of a hot pressure sintering apparatus (reference numeral 100 of FIG. 2, below same) can be reduced.

At the same time, the first mold part 22 may be formed of graphite of general purity, thereby reducing the manufacturing cost of the mold member 20.

In this case, in order to further prevent damage to the mold member 20, a release sheet 26 including graphite of high purity may be attached to an inner wall of the second mold part 24 forming the mold space part 24a.

In addition, as described above, when the high purity graphite plate and / or the graphite sheet (reference numerals 31a and 32a of FIG. 2) are positioned on the pressing member 30 in contact with the raw material, the mold member 20 in contact with the raw material. And graphite of high purity is located on all surfaces of the pressing member 30. As a result, damage to the mold member 20 and the pressing member 30 can be effectively prevented, thereby further reducing component replacement costs of the hot pressure sintering apparatus 100.

Since the silicon carbide sintered body manufactured by the method for producing the silicon carbide sintered body according to the present embodiment does not include a sintering aid, it can be produced with high purity. As a result, since the silicon carbide layer is not required to be formed by a separate deposition process, the silicon carbide layer may be used as a susceptor in the form of a bulk.

The silicon carbide sintered body may have a high density since the first silicon carbide powder and the second silicon carbide powder having different center particle diameters are mixed and sintered. Thereby, the strength, electrical conductivity, and thermal conductivity of the silicon carbide sintered body can be improved.

Hereinafter, with reference to FIG. 4, the manufacturing method of the silicon carbide sintered compact which concerns on 2nd Example is demonstrated. 4 is a process flowchart showing a method of manufacturing the silicon carbide sintered body according to the second embodiment.

Referring to FIG. 4, in the method for manufacturing the silicon carbide sintered body according to the present embodiment, the raw material mixing step (ST12), granulation step (ST22), forming step (ST32), processing step (ST42), and heating step (ST52) It may include. In this embodiment, the silicon carbide sintered body is formed by a reaction bonded silicon carbide method (hereinafter referred to as “RBSB method”). This will be described in more detail as follows.

In the raw material mixing step ST12, the first silicon carbide powder having the first central particle diameter and the second silicon carbide powder having the second central particle diameter smaller than this are mixed. At this time, the first and second silicon carbide powder may be mixed with the solvent in a solvent. As such a resin, a phenol resin may be used, and the solvent may include an alcohol or an aqueous substance. Examples of the alcohol-based substance include methanol, ethanol, and isopropyl alcohol (IPA), and water may be used as the aqueous substance. However, the embodiment is not limited thereto.

In this embodiment, since the first silicon carbide powder and the second silicon carbide powder having different center particle diameters are mixed, the mixed raw materials may be mixed to have a high density. Thereby, the density of the manufactured silicon carbide sintered compact can be improved, and the durability of a silicon carbide sintered compact can be improved.

In the present embodiment, the second silicon carbide powder may be included in the same manner as the first silicon carbide powder, or less second silicon carbide powder may be included than the first silicon carbide powder. In the present embodiment, the molten silicon is charged together in the heating step, because the amount of the second silicon carbide powder having a large particle diameter is relatively large so that the molten silicon easily penetrates into the mixed raw material.

For example, 50 to 90 wt% of the first silicon carbide powder, 10 to 50 wt% of the second silicon carbide powder, and 1 to 10 wt% of the resin may be mixed in the solvent.

In order to form a high purity silicon carbide sintered body in the present embodiment, the first and second silicon carbide powder may contain impurities of 10 ppm (parts per million) or less.

Next, in the granulation step ST22, the mixed raw materials are granulated. In one example, a spray dryer may be used to granulate the mixed raw materials.

Subsequently, in the molding step ST32, the granulated mixed raw material may be molded into a desired shape by slip casting in a cold isostatic press (CIP). At this time, the pressure of the cold isostatic molding apparatus may be 300 MPa or less. However, the embodiment is not limited thereto.

Subsequently, the mixed raw material molded in the processing step ST42 may be processed. In such a processing step (ST42), an embossed or intaglio is formed on the molded mixed raw material, or the molded mixed raw material is processed into a ring or slab shape. In this processing step (ST42) may be performed by the machining center (MCT).

Subsequently, in the heating step ST52, silicon is put together with the mixed raw material formed in a vacuum heat treatment apparatus or the like and then subjected to heat treatment to form a silicon carbide sintered body. At this time, the heat treatment temperature may be 1600 ° C or less. However, the embodiment is not limited thereto.

Since the silicon carbide sintered body manufactured by the method for producing the silicon carbide sintered body according to the present embodiment does not include a sintering aid, it can be produced with high purity. As a result, it is not necessary to form the silicon carbide layer by a separate deposition process, so that it may be used as a susceptor in bulk form.

The silicon carbide sintered body may have a high density since the first silicon carbide powder and the second silicon carbide powder having different center particle diameters are mixed and sintered. Thereby, the strength, electrical conductivity, and thermal conductivity of the silicon carbide sintered body can be improved.

Hereinafter, the examples will be described in more detail with reference to Preparation Examples and Comparative Examples. Preparation examples are only presented to more clearly describe the embodiments, and the embodiments are not limited to the preparation examples.

Manufacturing example  One

To the solvent of IPA, 10 weight% of phenolic resins, 30 weight% of silicon carbide powders with a center particle diameter of 4um, and 60 weight% of silicon carbide powders with a center particle diameter of 400 nm were added and mixed.

The mixed raw materials were then granulated using a spray dryer.

Subsequently, the raw material mixed in the hot pressure sintering apparatus was charged, and then hot pressed at a pressure of 40 MPa at a temperature of 2200 ° C to form a silicon carbide sintered compact.

Manufacturing example  2

To the solvent of IPA, 10 weight% of phenolic resins, 60 weight% of silicon carbide powders with a 4 micrometers center diameter, and 30 weight% of silicon carbide powders with a 400 micrometers center diameter were added and mixed.

The mixed raw materials were then granulated using a spray dryer.

Subsequently, after charging the mixed raw material into the crucible of the cold isostatic pressure forming apparatus which consists of urethane materials, the mixed raw material was shape | molded at 300 Mpa.

Subsequently, silicon was charged together with the mixed raw material molded into the vacuum heat treatment apparatus, and then heat treated at a temperature of 1600 ° C. to form a silicon carbide sintered body.

Comparative example  One

Silicon carbide powder having the same central particle diameter was sintered by hot pressure sintering to form a silicon carbide sintered body.

Comparative example  2

Silicon carbide powder having the same central particle diameter was sintered by the RBSC method to form a silicon carbide sintered body.

The impurity concentration, density, bending strength and thermal conductivity of the silicon carbide sintered body formed in Preparation Examples 1 and 2 and the susceptor according to Comparative Examples 1 and 2 were measured and shown in Table 1 below.

Production Example 1 Production Example 2 Comparative Example 1 Comparative Example 2 Impurity Concentration [ppm] 5 or less 5 or less 100 or less 100 or less Density [g / cm 3 ] 3.15 3.05 3.08 2.8 Bending Strength [MPa] 600 330 450 250 Thermal Conductivity [W / mK] 217 245 170 175

Referring to Table 1, it can be seen that the impurity concentrations in Preparation Examples 1 and 2 were much lower than in Comparative Examples 1 and 2. That is, according to the embodiment, it can be seen that a high purity silicon carbide sintered body can be formed.

In addition, it can be seen that the density, the bending strength and the thermal conductivity in Preparation Examples 1 and 2 were also much better than those in Comparative Examples 1 and 2. That is, according to the embodiment, it can be seen that the silicon carbide sintered body having high density and excellent properties such as strength and thermal conductivity can be formed.

The features, structures, effects and the like described in the foregoing embodiments are included in at least one embodiment of the present invention and are not necessarily limited to one embodiment. In addition, the features, structures, effects, and the like illustrated in the embodiments may be combined or modified with respect to other embodiments by those skilled in the art to which the embodiments belong. Therefore, it should be understood that the present invention is not limited to these combinations and modifications.

While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it is clearly understood that the same is by way of illustration and example only and is not to be construed as limiting the scope of the present invention. It can be seen that various modifications and applications are possible. For example, each component specifically shown in the embodiments may be modified. It is to be understood that the present invention may be embodied in many other specific forms without departing from the spirit or essential characteristics thereof.

Claims (11)

  1. A raw material mixing step of mixing the first silicon carbide powder having a first central particle diameter and the second silicon carbide powder having a second central particle diameter smaller than the first central particle diameter; And
    A heating step of forming a silicon carbide sintered body by heat treating the mixed raw materials,
    The said 1st central particle diameter is 1 micrometer-5 micrometers, The said 2nd center particle diameter is 30 nm or more, and the manufacturing method of the silicon carbide sintered compact less than 1 micrometer.
  2. delete
  3. delete
  4. The method of claim 1,
    A method for producing a silicon carbide sintered body which is carried out together with the step of pressing under pressure in the heating step.
  5. 5. The method of claim 4,
    In the raw material mixing step, the second silicon carbide powder is the same as the first silicon carbide powder or more than the first silicon carbide powder manufacturing method of the silicon carbide sintered body.
  6. delete
  7. The method of claim 1,
    Between the raw material mixing step and the heating step,
    It includes a molding step of molding the mixed raw material,
    In the heating step, a method for producing a silicon carbide sintered body is heated by adding silicon to the molded mixed raw material.
  8. The method of claim 7, wherein
    In the raw material mixing step, the second silicon carbide powder is the same as the first silicon carbide powder or less than the first silicon carbide powder manufacturing method of the silicon carbide sintered body.
  9. delete
  10. The method of claim 7, wherein
    Method for producing a silicon carbide sintered body further comprising a processing step between the forming step and the heat treatment step.
  11. A susceptor comprising a silicon carbide sintered body manufactured by the method for producing a silicon carbide sintered body according to any one of claims 1, 4, 5, 7, 8, and 10.
KR20100074434A 2010-07-30 2010-07-30 Method for manufacturing silicon carbide sintered body and susceptor including silicon carbide sintered body KR101199088B1 (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101496330B1 (en) * 2013-08-29 2015-03-02 (주) 이노쎄라 Method of fabricating silicon carbide sintered body having single-heterojunction structure and silicon carbide sintered body fabricated by the same

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20040141880A1 (en) 2002-07-24 2004-07-22 Erich Handler System and cartridge for processing a biological sample
EP1693884A2 (en) 2005-02-16 2006-08-23 Bridgestone Corporation Susceptor

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20040141880A1 (en) 2002-07-24 2004-07-22 Erich Handler System and cartridge for processing a biological sample
EP1693884A2 (en) 2005-02-16 2006-08-23 Bridgestone Corporation Susceptor

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101496330B1 (en) * 2013-08-29 2015-03-02 (주) 이노쎄라 Method of fabricating silicon carbide sintered body having single-heterojunction structure and silicon carbide sintered body fabricated by the same

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