KR20160129458A - Composition used for preparing electrically conductive SiC-BN composite ceramic and method for preparing electrically conductive SiC-BN composite ceramic using the same - Google Patents
Composition used for preparing electrically conductive SiC-BN composite ceramic and method for preparing electrically conductive SiC-BN composite ceramic using the same Download PDFInfo
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- KR20160129458A KR20160129458A KR1020150061655A KR20150061655A KR20160129458A KR 20160129458 A KR20160129458 A KR 20160129458A KR 1020150061655 A KR1020150061655 A KR 1020150061655A KR 20150061655 A KR20150061655 A KR 20150061655A KR 20160129458 A KR20160129458 A KR 20160129458A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/06—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/06—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances
- H01B1/08—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances oxides
Abstract
Description
The present invention relates to a composition for preparing a ceramic composite material, a method for manufacturing a ceramic composite material using the same, and a ceramic composite material produced thereby.
Ceramics are used to manufacture products in various industrial fields due to excellent physical and mechanical properties, which is a general term for non-metallic inorganic materials made by applying heat.
In recent years, there has been a great deal of research on structural ceramics having high strength as the demands of industry for lightweight, high strength, or high heat resistant materials are increasing. Materials for such structural ceramics include silicon carbide (SiC) Alumina (Al 2 O 3 ), zirconia (MgO stabilized ZrO 2 / Y 2 O 3 stabilized ZrO 2 ), boron nitride (BN) or silicon nitride (Si 3 N 4 ) are widely used.
Among them, silicon carbide (SiC) is used for manufacturing semiconductor process parts and chemical resistant machine parts because it has various advantages such as high strength and hardness, excellent high temperature property, radiation resistance characteristic and plasma plasma corrosion characteristic.
Hexagonal boron nitride (h-BN) has a low coefficient of thermal expansion, and has excellent thermal shock resistance. It has excellent lubrication, thermal conductivity, electrical insulation, and excellent processability. Thus, semiconductor process parts, melting crucible, And the like.
A silicon carbide-boron nitride composite material is known as a material having the advantages of silicon carbide and hexagonal boron nitride having different advantages as described above. Such a composite material is superior in thermal shock resistance And machinability.
However, the silicon carbide-boron nitride composite material in which silicon carbide and hexagonal boron nitride are combined as well as the silicon carbide-boron nitride composite material is also low in electrical conductivity and can be used for electric power, electro-chemical, gas appliance ), Which are used in various industrial fields.
SUMMARY OF THE INVENTION The present invention has been made in order to solve the problems of the prior art as described above, and it is an object of the present invention to provide an electrically conductive silicon carbide-boron nitride composite material which exhibits high electrical conductivity while retaining the advantages of the known silicon carbide- And to provide a method for producing a silicon carbide-boron nitride composite material using the same.
(Β-SiC) of not less than 93 and not more than 97.5% by weight, hexagonal boron nitride (h-BN) of not less than 1.0 and not more than 4.0% (Y 2 O 3 ) in an amount of less than 3.0% by weight based on the total weight of the silicon carbide-boron nitride composite material.
The average particle size of the beta-phase silicon carbide is 0.1 to 1 mu m.
(A) a powder of beta-SiC (beta-SiC) in an amount of 93 to 97.5% by weight, a powder of hexagonal boron nitride (h-BN) in an amount of 1.0 to 4.0% Of yttrium oxide (Y 2 O 3 ) powder; And (b) fabricating a sintered body of a silicon carbide-boron nitride composite material under a nitrogen (N 2 ) atmosphere using the mixed powder obtained in the step (a). ≪ / RTI >
Further, in the step (b), pressure sintering is performed for 1 to 12 hours at a temperature of 1900 to 2050 캜 and a pressure of 20 to 40 MPa.
Also, the Y-B-Si-O-C-N-based liquid phase is formed in the step (b) and densified through a liquid phase sintering mechanism.
In addition, in step (b), silicon carbide doped with nitrogen atoms (N) is precipitated and grown from the Y-B-Si-O-C-N based liquid phase through a dissolution-reprecipitation mechanism.
The present invention also provides an electrically conductive silicon carbide-boron nitride ceramic composite material produced by the above-described method.
Also, the electrically conductive silicon carbide-boron nitride ceramic composite material has an electrical resistivity of 7.2 x 10 < -2 & gt ; OMEGA .cm or less.
Also, the electrically conductive silicon carbide-boron nitride ceramic composite material has a flexural strength of 536 MPa or more and a thermal shock resistance of ΔT = 500 ° C. or more.
The present invention also provides an electrically conductive part manufactured by electrical discharge machining (EDM) of the above-described ceramic composite material.
According to the method for producing the electrically conductive silicon carbide-boron nitride composite material according to the present invention, yttria (Y 2 O 3 ) powder is added as a sintering additive to silicon carbide and boron nitride powder and sintered in a nitrogen (N 2 ) atmosphere , A YB-Si-OCN-based liquid phase is formed, densification is promoted by a liquid phase sintering mechanism, and nitrogen-doped silicon carbide particles are grown by a dissolution-reprecipitation mechanism, A ceramic composite material having a significantly improved electrical conductivity as compared with that of the present invention and having excellent mechanical strength and thermal shock resistance can be produced.
In addition, the ceramic composite material produced by the process for producing the electrically conductive silicon carbide-boron nitride composite material according to the present invention has high electrical conductivity and can be processed by discharge, so that IT, which is required to be highly precise, It can be used for manufacturing parts of electronic products.
BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a process diagram showing each step of the method for producing an electrically conductive boron carbide-silicon nitride composite material according to the present invention.
2 is an image of a part manufactured by electrodeposition of an electrically conductive silicon carbide-boron nitride composite material according to the present invention.
3 is a scanning electron microscope (SEM) image of a silicon carbide-boron nitride composite material specimen prepared according to Example 1 of the present application.
Hereinafter, the present invention will be described in detail.
The composition for preparing an electrically conductive silicon carbide-boron nitride composite material according to the present invention is characterized by containing beta-SiC (beta-SiC) in the range of 93 to 97.5% by weight, hexagonal boron nitride (h- And yttria (Y 2 O 3 ) of 1.0 to less than 3.0% by weight.
The beta-phase silicon carbide exhibits excellent properties such as abrasion resistance, corrosion resistance, high thermal conductivity and chemical stability. The beta-phase silicon carbide is a main component of the ceramic composite material and is contained in a mixed powder for producing a ceramic composite material in an amount of 93 to 97.5% .
On the other hand, the particle size of the beta-phase silicon carbide is not particularly limited, but it is preferable that the average particle size is 0.1 to 1 탆 in order to reduce the content of the sintering additive which causes the sintering property and the volume resistivity to increase depending on the high specific surface area .
The hexagonal boron nitride (h-BN) exhibits a high electrical resistivity and a low thermal expansion coefficient. The composition according to the present invention contains 1.0 to 4.0% by weight of a mixed powder for the production of a ceramic composite material. .
When the hexagonal boron nitride is contained in an amount of less than 1.0% by weight, the hardness of the ceramic composite material tends to increase during sintering and brittleness tends to increase. When the hexagonal boron nitride is contained in an amount exceeding 4.0% by weight, The average particle size of the material tends to decrease so that the fracture toughness increases and the flexural strength decreases. It is preferable to adjust the content of the boron nitride to the above range Do.
The yttria (Y 2 O 3 ) is included in the composition for preparing the electrically conductive silicon carbide-boron nitride composite material according to the present invention as a sintering additive.
Since the yttrium oxide is included in the composition according to the present invention, the YB-Si-OCN-based liquid phase is formed during the sintering process, and the densification of the sintered body is promoted by the liquid phase sintering mechanism. The silicon carbide particles doped with nitrogen atoms are grown by the mechanism to improve the electrical conductivity of the composite material and further to improve the strength and thermal shock resistance of the composite material.
In order to achieve the above-described effects, the yttria is preferably contained in an amount of 1.0 to 3.0% by weight in the composition for preparing an electrically conductive silicon carbide-boron nitride composite material according to the present invention. If the content of yttria (Y 2 O 3 ) is less than 1.0% by weight, sintering is insufficient due to insufficient sinterability and the sintered density is decreased, so that a dense ceramic composite material can not be produced. As a result, pores are formed in the ceramic composite material So that electrical conductivity and mechanical properties may be deteriorated. When the content of the sintering additive is more than 3.0% by weight, the excess sintering additive remains in the silicon carbide grain boundary state without a significant increase in the sintering density, so that the specific resistivity increases and the electric conductivity decreases. So that it is preferable to adjust the content of the sintering additive to the above-mentioned range.
Next, a method for manufacturing the electrically conductive silicon carbide-boron nitride composite material according to the present invention will be described below.
A method for producing an electrically conductive boron carbide-silicon carbide composite material according to the present invention comprises the steps of: (a) providing a powder of beta-SiC powder in an amount of 93 to 97.5% by weight, 1.0 to 4.0% (hexagonal BN) powder and 1.0 to 3.0 weight percent and less than of yttrium oxide (Y 2 O 3) to prepare a mixed powder containing a powder and (b) nitrogen a mixed powder prepared in step (a) (N 2 ) ≪ / RTI > atmosphere.
Said step (a) the beta silicon carbide (β-SiC) powder, the hexagonal boron nitride (hexagonal BN) powder and yttrium oxide (Y 2 O 3) and mix the powder, the above-mentioned silicon carbide-boron nitride composite material for manufacture of Thereby preparing a mixed powder composition.
Further, in this step, the step of grinding the mixed powder may be further carried out as necessary to form a mixed powder having a uniform particle size and a high specific surface area. In order to crush the mixed powder, various well-known powder crushing methods may be used. For example, an oil-based ball milling method in which a mixed powder is mixed and dispersed in an organic solvent such as ethanol and pulverized using zirconia balls or the like is used But can be configured to crush the powder using various methods without being limited to these methods.
Next, the step (b) is a step of producing a sintered body composed of a silicon carbide-boron nitride composite material in a nitrogen (N 2 ) atmosphere using the mixed powder obtained in the step (a).
Generally, a silicon carbide-boron nitride composite material obtained by sintering using silicon carbide and boron nitride as a starting material exhibits high electrical resistance. Depending on the boron nitride to be added, the additive and the manufacturing process, the silicon carbide-boron nitride composite material has a range of 10 10 to 10 12 ? Lt; / RTI >
However, in the present invention, the mixed powder of the above-mentioned composition is sintered in a nitrogen (N 2 ) atmosphere to grow silicon carbide particles doped with nitrogen to form a ceramic composite material having high electrical conductivity and excellent mechanical strength and thermal shock resistance Can be manufactured.
To be more specific, when the sintering in a nitrogen (N 2) atmosphere by using the above mixed powder, silicon carbide, silicon carbide, silicon dioxide on the surface (SiO 2), boron nitride (BN), antimony trioxide, boron of the boron nitride surface (B 2 O 3 ) and yttria (Y 2 O 3 ) react with each other to form a YB-Si-OCN-based liquid phase. The liquid phase is formed by densifying the silicon carbide-boron nitride composite material by a liquid phase sintering mechanism, The silicon carbide-boron nitride composite material having high electrical conductivity can be obtained by inducing grain growth of the electroconductive silicon carbide doped with nitrogen atoms (N) by a particle-re-precipitation mechanism.
For reference, if yttrium oxide (Y 2 O 3 ) is not contained in the mixed raw material powder for producing a sintered body, no liquid phase is formed during sintering, and nitrogen-doped silicon carbide particles are not produced by the dissolution- The nitrogen atoms contained in the boron nitride must be introduced into the silicon carbide particles through diffusion from the outside of the silicon carbide particles. However, since the diffusion of nitrogen atoms in the silicon carbide crystal lattice is very slow, there is a problem that it is virtually impossible to obtain silicon carbide particles having a sufficient nitrogen content to have a satisfactory electric conductivity.
The step (b) is preferably, but not necessarily, performed by pressure sintering under a nitrogen atmosphere at a pressure of 20 to 40 MPa at a temperature of 1900 to 2050 ° C for 1 to 12 hours.
(Y 2 O 3 ) powder as a sintering additive is added to silicon carbide and boron nitride powders, and a nitrogen (N 2 ) atmosphere is added to the silicon carbide and boron nitride powders , A YB-Si-OCN-based liquid phase is formed, densification is promoted by a liquid phase sintering mechanism, and furthermore, nitrogen-doped silicon carbide particles are dispersed by a dissolution-reprecipitation mechanism A ceramic composite material having improved electrical conductivity and superior mechanical strength and thermal shock resistance can be produced.
In addition, the ceramic composite material produced by the method of manufacturing the electrically conductive silicon carbide-boron nitride composite material according to the present invention has high electrical conductivity and can be subjected to electrical discharge machining (EDM) Various types of electronic parts and IT-related parts requiring miniaturization can be manufactured. For example, as shown in Fig. 2, they can be usefully used for manufacturing various parts through electric discharge machining.
Hereinafter, the present invention will be described in more detail with reference to examples.
The embodiments presented are only a concrete example of the present invention and are not intended to limit the scope of the present invention.
≪ Examples 1 to 4 >
Step 1: In order to produce the ceramic composite materials according to Examples 1 to 4 of the present invention, a mixture of a mixture of a mixture of a mixture of a mixture of a mixture of a mixture of a mixture of a mixture of a mixture of a mixture of ) And yttria (average particle diameter: 2 mu m) were prepared in the same manner as in Example 1, and 100 wt% of ethanol was added to the resulting mixture in an amount of 100 wt% based on the weight% of the mixture. Using a polypropylene container and a silicon carbide ball Milled for 6 hours to produce a uniform mixture powder.
Step 2: The prepared mixture powder was pressed and sintered under the sintering conditions shown in Table 1 below to prepare ceramic composite materials according to Examples 1 to 4 of the present invention.
[Table 1]
The surface of the specimen of the ceramic composite material according to Example 1 manufactured as described above was polished, plasma-etched, and the surface was photographed with a scanning electron microscope (SEM).
As shown in Fig. 3, the black elongated portion is a portion where boron nitride is plasma-etched and indicates that boron nitride is in a plate-like shape. In addition, the white part represents the Y 2 O 3 phase added by the sintering aid, and it can be confirmed that the Y 2 O 3 phase is mainly distributed at the ternary junction between the silicon carbide particles.
≪ Comparative Example 1 &
Step 1: A mixture of the same Beta-phase silicon carbide powder, hexagonal boron nitride powder, and yttrium oxide as in Example 1 in the ratio shown in Table 1 was prepared. To the mixture thus prepared, , 100% by weight of ethanol was further added, and a uniform mixture powder was prepared by using a polypropylene container and a silicon carbide ball for 6 hours.
Step 2: The prepared mixture powder was pressure-sintered under the conditions shown in Table 1 to prepare a ceramic composite material according to Comparative Example 1. [
≪ Comparative Example 2 &
Step 1: A mixture of the same silicon carbide powder and hexagonal boron nitride powder as in Example 1 in the ratio shown in Table 1 was prepared. To the mixture thus prepared was added 100% by weight of ethanol as a solvent, And a uniform mixture powder was prepared by using a polypropylene container and a silicon carbide ball for 6 hours by an oil-based ball mill.
Step 2: The prepared mixture powder was pressed and sintered under the conditions shown in Table 1 to prepare a ceramic composite material according to Comparative Example 2. [
<Experimental Example> Analysis of physical properties of ceramic composite materials
In order to analyze the physical properties of the ceramic composite materials according to the above-described Examples 1 to 4 and Comparative Examples 1 and 2, the density was measured using the Archimedes method and is shown in Table 2 below.
Also, electrical resistivity (resistivity) of the ceramic composite material was measured by applying a magnetic field of 1 Tesla (T) using Hall measurement method, and the measured electrical resistivity is shown in Table 2 below.
In order to analyze the mechanical properties of the ceramic composite materials according to Examples 1 to 4 and Comparative Examples 1 and 2, a bending test (Standard Test Method for Flexural Strength of Advanced Ceramics at Ambient Temperature, ASTM C-1161-02c ), And the bending strength was analyzed. The bending strengths analyzed are shown in Table 2 below.
In addition, a thermal shock test was conducted by applying a thermal shock to a temperature of ΔT = 500 ° C. in accordance with KS L 2424 (heat-resistant glass standard) through a thermal shock test, The thermal shock resistance of the ceramic composite material was analyzed. The results of the analysis are shown in Table 2 below. At this time, when the thermal shock was applied to? T = 500 占 폚, it was judged to be normal without cracking and no cracking.
[Table 2]
As shown in Table 2, in the case of the ceramic composite materials according to Examples 1 to 4, the specimens prepared by mixing Y 2 O 3 with sintering additive and beta-phase silicon carbide with hexagonal boron nitride powder had a sintered density of 99.0 %, And the electrical resistivity of the prepared ceramic composite material showed a very high electrical conductivity in the range of 3.0 x 10 -2 to 7.2 x 10 -2 Ω · cm and exhibited a bending strength as high as the bending strength in the range of 536 to 622 MPa, It can be confirmed that the thermal shock resistance exhibits very good physical properties as? T = 500 占 폚 or more.
On the other hand, the electrical resistivities of Comparative Examples 1 and 2 were 4.2 x 10 3 ? Cm and 7.5 x 10 6 ? Cm, respectively, which were significantly higher than those of the ceramic composite materials of Examples 1 to 4 This is because, in the case of Comparative Example 1 and Comparative Example 2, nitrogen is volatilized in the YB-Si-OCN-based liquid phase formed during sintering by sintering in an argon (Ar) atmosphere to grow nitrogen-doped silicon carbide particles On the other hand, the bending strengths of the specimens prepared in Comparative Examples 1 and 2 were less than 400 MPa, and the thermal shock resistance was less than 500 캜, indicating that the mechanical properties of the specimens prepared in Examples 1 to 4 Respectively.
Claims (10)
Wherein the beta-phase silicon carbide has an average particle size of 0.1 to 1 [mu] m.
(b) a step of producing a sintered body of a silicon carbide-boron nitride composite material under a nitrogen (N 2 ) atmosphere using the mixed powder obtained in the step (a) .
Wherein the step (b) comprises pressing and sintering at a temperature of 1900 to 2050 ° C and a pressure of 20 to 40 MPa for 1 to 12 hours.
Wherein the YB-Si-OCN-based liquid phase is formed in the step (b) and the densification is performed through a liquid phase sintering mechanism.
Wherein the silicon carbide doped with nitrogen atoms (N) is precipitated and grown from the YB-Si-OCN-based liquid phase through a dissolution-reprecipitation mechanism in the step (b) - A method for producing a boron nitride composite material.
Wherein the electrical resistivity of the silicon carbide-boron nitride ceramic composite material is 7.2 x 10 < -2 & gt ; OMEGA .cm or less.
Wherein the flexural strength of the electrically conductive silicon carbide-boron nitride composite material is 536 MPa or more and the thermal shock resistance is at least 500 캜.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| KR20200019070A (en) | 2018-08-13 | 2020-02-21 | 에스케이씨솔믹스 주식회사 | Manufacturing method of boroncarbide sintered body and shaping die |
| CN111004036A (en) * | 2019-12-25 | 2020-04-14 | 中国科学院兰州化学物理研究所 | High-density hexagonal boron nitride-based solid lubricating composite material and preparation method thereof |
| EP3594968A4 (en) * | 2017-03-07 | 2021-01-20 | Sung Bok Wee | Conductive ceramic composition having excellent electrical conductivity |
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| JPH11147768A (en) * | 1997-11-17 | 1999-06-02 | Mitsubishi Materials Corp | Nitrogen-containing ceramic composite material and its production |
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| JPH11147768A (en) * | 1997-11-17 | 1999-06-02 | Mitsubishi Materials Corp | Nitrogen-containing ceramic composite material and its production |
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| EP3594968A4 (en) * | 2017-03-07 | 2021-01-20 | Sung Bok Wee | Conductive ceramic composition having excellent electrical conductivity |
| KR20200019070A (en) | 2018-08-13 | 2020-02-21 | 에스케이씨솔믹스 주식회사 | Manufacturing method of boroncarbide sintered body and shaping die |
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| CN111004036A (en) * | 2019-12-25 | 2020-04-14 | 中国科学院兰州化学物理研究所 | High-density hexagonal boron nitride-based solid lubricating composite material and preparation method thereof |
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