KR101972350B1 - A ZrC Composites and A Manufacturing method of the same - Google Patents

Abstract

The present invention relates to a ZrC grain; And a SiC grain, wherein the grain boundary of the ZrC grain and the grain boundary of the SiC grain are in contact with each other, and a method of manufacturing the ZrC composite, and can provide a ZrC composite densified at a low temperature while being densified.

Description

A ZrC Composites and a Manufacturing Method of the Same

The present invention relates to a zirconium carbide composite and a method of manufacturing the same, and more particularly, to a zirconium carbide composite densified while sintering at a low temperature through zirconium carbide (ZrC) and silicon carbide (SiC) and a method for manufacturing the same.

Zirconium carbide (ZrC) is a chemically stable material with high melting point, high hardness, high electric conductivity and high heat shock resistance. Therefore, these characteristics are used for high temperature structural materials, hard metal tool materials, electron emission cathode materials and the like.

In addition, since it has a characteristic of converting far-infrared rays of sunlight efficiently into heat energy and reflecting far-infrared rays, it is a material having many possibilities such as being used in a high-temperature-resistant winter clothes.

On the other hand, zirconium carbide ceramic bodies are known in the art, and they are particularly useful as structural materials and coating materials for high-temperature regions in the nuclear power industry because of their high hardness, excellent abrasion resistance, and good nuclear nucleus properties.

An initial method for producing these ceramic bodies is a method of compressing zirconium carbide powder at a high temperature / high pressure at a temperature up to 2300 ° C. However, in the case of this conventional method, a high melting point (about 3600 ° C) of zirconium carbide Deg.] C, it is difficult to densify the zirconium carbide ceramic body.

On the other hand, silicon carbide (SiC) is a reinforcing material having a high tensile strength. If alumina (Al ₂ O ₃ ) is a representative of oxide ceramics, silicon carbide is a representative of non-oxide ceramics.

Silicon carbide is highly utilizable because it has excellent physical properties such as mechanical properties representative of abrasion resistance, thermal properties representing high temperature strength and creep resistance, chemical resistance typified by oxidation resistance and corrosion resistance, and silicon carbide Is widely used for 'mechanical seal', 'bearing', 'various nozzle', 'hot cutting tool', 'fireproof plate', 'abrasive material', 'steelmaking reducing material', 'arrester'.

However, since the process for producing the silicon carbide sintered body is not simple or easy, the manufacturing cost is very high, and therefore, there is a limitation that it can not be used more actively, and such manufacturing cost reduction is a great challenge in manufacturing the silicon carbide sintered body .

Therefore, it is required to develop a sintered composite which can be densified after a short time sintering at a lower temperature and pressure.

SUMMARY OF THE INVENTION The present invention has been made to solve the above-mentioned problems of the prior art, and it is an object of the present invention to provide a ZrC composite densified while sintering at a low temperature through zirconium carbide (ZrC) and silicon carbide (SiC) .

The objects of the present invention are not limited to the above-mentioned objects, and other objects not mentioned can be clearly understood by those skilled in the art from the following description.

In order to solve the above-mentioned problems, the present invention provides a ZrC grain; And SiC grains, wherein the grain boundary of the ZrC grain and the grain boundary of the SiC grain provide a ZrC composite in mutual contact.

Further, the present invention provides a ZrC composite wherein the size of each of the ZrC grain and the SiC grain is 50 nm to 1000 nm.

The present invention also provides a ZrC composite wherein there is no raw materials or intermediate phase between the grain boundary of the ZrC grain and the grain boundary of the SiC grain.

Further, the present invention provides the ZrC composite having a relative density of 95% or more.

The present invention also provides a ZrC composite, which is a ZrC-SiC composite.

The present invention also relates to a method of manufacturing a semiconductor device, comprising: mixing a zirconium silicide group (Zr _x Si _y , Zirconium silicide) and a carbon source; And sintering the mixture of the zirconium silicide group (Zr _x Si _y , Zirconium silicide) and the carbon source.

Further, the present invention provides a method for producing a ZrC composite in which the zirconium silicide group (Zr _x Si _y , Zirconium silicide) is ZrSi ₂ and the carbon source is carbon black.

In addition, the present invention is the in the mixing step further comprises a ZrC powder, and the ZrC powder, the zirconium silicide group (Zr _x Si _y, Zirconium silicide) and 100 mass% of the ZrC powder of the mixture of said carbon source 0 By mass and less than 60% by mass of the ZrC composite.

Further, the present invention further includes SiC powder in the mixing step, wherein the SiC powder has a composition of 0% by weight, based on 100% by weight of the SiC powder, the zirconium silicide group (Zr _x Si _y , Zirconium silicide) By mass and less than 30% by mass of the ZrC composite.

The present invention also provides a method for producing a ZrC composite having a sintering temperature in the range of 1700 to 2000 ° C.

In addition, the present invention provides a method of manufacturing a ZrC composite using the spark plasma sintering method and the spark plasma sintering method in the range of 30 MPa to 60 MPa.

The present invention also provides a method for producing a ZrC composite, which is a ZrC-SiC composite.

In the present invention as described above, it is possible to provide a ZrC composite which is densified while being sintered at a low temperature through zirconium carbide (ZrC) and silicon carbide (SiC).

In addition, the ZrC composite has a high fracture toughness value and high neutron irradiation damage resistance, and thus can provide a composite particularly useful as a structural material and a coating material of a high-temperature region in the nuclear power industry.

1 is a flowchart illustrating a method of manufacturing a ZrC composite according to a first embodiment of the present invention.
2 is a flowchart illustrating a method of manufacturing a ZrC composite according to a second embodiment of the present invention.
3 is a flowchart illustrating a method of manufacturing a ZrC composite according to a third embodiment of the present invention.
Figure 4 is a graph showing the Gibbs free energy of reactions during the sintering process.
5 is a graph showing XRD data according to temperature.
FIG. 6 is a microscope showing the microstructure of the mixture subjected to the heat treatment at 1400.degree.
FIG. 7A is a graph showing an XRD pattern of a ZrC-SiC composite according to a temperature condition, and FIG. 7B is an actual view showing a theoretical density and a relative density according to the condition of FIG. 7A.
FIG. 8A is a diagram showing the results of the EDS analysis of the ZrC-SiC composite according to the present invention, and FIG. 8B is a TEM image of the ZrC-SiC composite according to the present invention.
9 is a view showing the sintering state when ZrC is contained in an amount of 70% by mass, based on 100% by mass of the mixture.
Fig. 10 is a view showing the sintering condition according to the conditions of Table 4. Fig.
11 is XRD data according to the conditions of Tables 3 and 4.
12 is a view showing the sintering state in the case where ZrC is contained in an amount of 20 mass% with respect to 100 mass% of the mixture and sintering is carried out at a temperature of 1750 캜 for 30 minutes.
Fig. 13 is XRD data according to the conditions of Table 5. Fig.
14A is a view showing a sintering state when sintering is carried out at a temperature of 1750 DEG C for 30 minutes, wherein SiC is contained in an amount of 20% by mass based on 100% by mass of the mixture.
14B is a view showing a sintering state in which sintering is carried out for 30 minutes at a temperature of 1750 DEG C and 10% by mass of SiC based on 100% by mass of the mixture.
15 is XRD data according to the partial conditions of Table 6. < tb >< TABLE >

BRIEF DESCRIPTION OF THE DRAWINGS The advantages and features of the present invention and the manner of achieving them will become apparent with reference to the embodiments described in detail below with reference to the accompanying drawings. The present invention may, however, be embodied in many different forms and should not be construed as being limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art. Is provided to fully convey the scope of the invention to those skilled in the art, and the invention is only defined by the scope of the claims.

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Reference will now be made in detail to the preferred embodiments of the present invention, examples of which are illustrated in the accompanying drawings. &Quot; and / or " include each and every combination of one or more of the mentioned items. ≪ RTI ID = 0.0 >

Although the first, second, etc. are used to describe various components, it goes without saying that these components are not limited by these terms. These terms are used only to distinguish one component from another. Therefore, it goes without saying that the first component mentioned below may be the second component within the technical scope of the present invention.

The terminology used herein is for the purpose of illustrating embodiments and is not intended to be limiting of the present invention. In the present specification, the singular form includes plural forms unless otherwise specified in the specification. The terms " comprises " and / or " comprising " used in the specification do not exclude the presence or addition of one or more other elements in addition to the stated element.

Unless defined otherwise, all terms (including technical and scientific terms) used herein may be used in a sense commonly understood by one of ordinary skill in the art to which this invention belongs. Also, commonly used predefined terms are not ideally or excessively interpreted unless explicitly defined otherwise.

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

1 is a flowchart illustrating a method of manufacturing a ZrC composite according to a first embodiment of the present invention.

1, a method of manufacturing a ZrC composite according to a first embodiment of the present invention includes mixing a raw material powder and a carbon source (S110)

In this case, the raw material powder is zirconium silicide group, and characterized by using a (Zr _x Si _y, Zirconium silicide), zirconium silicide group (Zr _x Si _y, Zirconium silicide) is ZrSi ₂ according to the ratio of Zr and Si, _{ZrSi, Zr 5 Si 4, Zr} 5 Si 3, Zr 3 Si 2, may include at least one selected from the group consisting of Zr ₂ Si, and Zr ₃ Si, wherein the raw material powder in the present invention is that the ZrSi ₂ desirable.

The zirconium silicide group (Zr _x Si _y , Zirconium silicide) has a melting point ranging from 1620 to 2500 ° C. over a wide range, and since Zr and Si are uniformly mixed at the molecular level, ZrC and SiC can be simultaneously formed.

That is, in the present invention, by using a zirconium silicide group (Zr _x Si _y , Zirconium silicides) in which Zr and Si are uniformly mixed at a molecular unit level, local concentration of chemical composition is prevented, Uniformly distributed ZrC composite can be produced.

The carbon source may be at least one selected from solid carbon materials such as graphite, carbon black and activated carbon, and organic materials which are carbonized after pyrolysis such as phenol resin, pitch and sucrose. However, in the present invention, However, in the present invention, the carbon source is preferably carbon black.

The raw material powder and the carbon source may be mixed using a planetary mill, an attrition mill, a Spex mill, or a high energy ball mill operating on a similar principle. For example, Drying may be carried out for 0.1 to 3 hours. However, the mixing method of the raw material powder and the carbon source is not limited in the present invention.

On the other hand, when the raw material powder and the carbon source are mixed by using a Spex mill, the mixing of impurities caused in the production of the ZrC composite according to the present invention can be prevented as compared with other mixing methods.

That is, in the case of the attrition mill and the planetary mill, a large amount of contaminants may be introduced from the crushing ball and the crushing vessel upon crushing. However, in the case of the specs mill, such problems can be minimized.

Next, a method of manufacturing a ZrC composite according to a first embodiment of the present invention includes a step of sintering the raw material powder and a mixture containing the carbon source (S120).

Generally, the term "sintering" refers to a process of densifying a formed body made of a powder as a raw material at a high temperature. Densification and grain growth are typical sintering phenomena.

The sintering may be classified into normal sintering, pressure sintering, spark plasma sintering, and the like according to a technical method of densification.

Atmospheric pressure sintering is a method of densifying a compact by heat treatment at a high temperature of atmospheric pressure or an inert atmosphere in a normal sintering process. Pressure sintering is a method of densifying by applying pressure from the outside of the sintered body. Spark plasma sintering applies pressure to the sintered body And at the same time, a high current pulse is caused to flow to densify at a low temperature.

In the present invention, the sintering of the synthetic powder may be performed by a normal sintering method, a pressure sintering method, or a spark plasma sintering method. However, in the present invention, In sintering, it is preferable to use a spark plasma sintering method in which a pressure is applied to the sintered body while a pulse of a high current flows.

In the present invention, the sintering temperature may be in the range of 1750 to 2000 ° C, and the sintering atmosphere may be a vacuum, an argon (Ar) atmosphere, a nitrogen atmosphere, or a spark plasma sintering ) Method for 5 to 120 minutes.

If the sintering temperature is less than 1,700 캜, it is difficult to form a ZrC composite having a high relative density, and if the sintering temperature exceeds 2000 캜, densification can be performed, The sintering temperature in the sintering step of the present invention is in the range of 1700 to 2000 ° C since the composite material having a fine grain size for the purpose of the present invention can not be produced and the sintering in the low- It is more preferable that the sintering temperature of the sintering step in the present invention is 1750 to 2000 ° C.

Meanwhile, in the sintering step, typical reaction formulas of the raw material powder and the carbon source are as follows.

Zirconium silicides + C? ZrC + SiC (Scheme 1)

As shown in Reaction Scheme 1, in the sintering step, ZrC and SiC may be formed through reaction of the raw material powder and the carbon source.

That is, in the present invention, by mixing the zirconium silicide group as the source of Zr and Si with the source of carbon, it is possible to produce a high-purity ZrC composite having a fine grain size and a uniform microstructure despite heat treatment at a low temperature.

However, since the reaction in Reaction Scheme 1 described above is completed before the liquid phase formation temperature of ZrSi ₂ , which is 1620 ° C to 1680 ° C, ZrC can not be completely densified by the normal pressure sintering method.

That is, when only zirconium silicide is used, since the melting point of ZrSi ₂ is around 1650 ° C., a liquid phase is formed at 1650 ° C. In the present invention, the ZrSi ₂ contains the carbon source together with the zirconium suicide group. The ZrSi ₂ reacts with these carbon sources to form ZrC + SiC before reaching the point, so that a liquid phase due to ZrSi ₂ can not be formed and thus the problem of densification can not be obtained.

Therefore, in the present invention, it is preferable to use a spark plasma sintering method which applies a pressure to the sintered body while allowing a pulse of a high current to flow therethrough. In the spark plasma sintering method, There is an advantage that it can promote.

Generally, it is known that the material starts to deform due to the pressure at a temperature range of about 2/3 of the melting temperature.

In the case of the zirconium silicide group, for example, ZrSi ₂ , this temperature range corresponds to about 1100 ° C., and at 1400 ° C., it is reported that deformation due to the pressure of ZrSi ₂ occurs to a large extent.

Therefore, even in a relatively low temperature region where the reaction of ZrSi ₂ is not completed, deformation of ZrSi ₂ by pressurization can be induced, and thereby the densification of ZrC can be further accelerated. Thereafter, at a higher temperature, residual ZrSi ₂ It is possible to suppress the decrease in the physical properties of the produced ZrC composite at high temperature.

At this time, the range of the pressing in the spark plasma sintering method of the present invention can be performed in the range of the pressing force of 10 MPa to 120 MPa.

When the pressing force is less than 10 MPa, the effect of densification due to pressure deformation of zirconium silicides at low temperature is not apparent, and when the pressing force exceeds 120 MPa, it is difficult to industrially manufacture due to limitations of equipment. Is preferably in the range of a pressing force of 10 MPa to 120 MPa.

At this time, in the present invention, the spark plasma sintering method of the present invention preferably has a pressing range of 30 MPa to 60 MPa, and when the pressing force exceeds 60 MPa, sintering is achieved in a low pressure process Therefore, it is more preferable that the pressure condition in the sintering step in the present invention is 30 MPa to 60 MPa.

That is, in the present invention, the sintering step is carried out by using the spark plasma sintering method instead of the atmospheric pressure sintering method to prevent the coarsening phenomenon occurring at a high temperature and the sintering process using the low temperature deformation of the zirconium suicide group So that the ZrC composite can be completed at an extremely low temperature compared to the conventional results. Thus, a ZrC composite can be produced which minimizes grain growth and maximizes densification.

Thereby, a ZrC composite, that is, a ZrC-SiC composite can be produced (S130).

2 is a flowchart illustrating a method of manufacturing a ZrC composite according to a second embodiment of the present invention.

The method of manufacturing the ZrC composite according to the second embodiment of the present invention can be referred to the first embodiment described above, except as described below.

2, a method of manufacturing a ZrC composite according to a second embodiment of the present invention includes mixing ZrC, a sintering aid, and a carbon source (S210)

At this time, in the present invention, the sintering aid is characterized by using a zirconium silicide group (Zr _x Si _y ), and the zirconium silicide group (Zr _x Si _y , Zirconium silicide) It may contain at least one selected from the group consisting of ZrSi ₂ , ZrSi, Zr ₅ Si ₄ , Zr ₅ Si ₃ , Zr ₃ Si ₂ , Zr ₂ Si and Zr ₃ Si. In the present invention, ZrSi ₂ is preferable.

The zirconium silicide group (Zr _x Si _y , Zirconium silicide) has a melting point ranging from 1620 to 2500 ° C. over a wide range, and since Zr and Si are uniformly mixed at the molecular level, ZrC and SiC can be simultaneously formed.

That is, in the present invention, by using the zirconium silicide group (Zr _x Si _y , Zirconium silicides) in which Zr and Si are uniformly mixed at the molecular unit level as a sintering aid, local concentration of chemical composition is prevented, And ZrC composites having SiC uniformly distributed can be produced.

The carbon source may be at least one selected from solid carbon materials such as graphite, carbon black and activated carbon, and organic materials which are carbonized after pyrolysis such as phenol resin, pitch and sucrose. However, in the present invention, However, in the present invention, the carbon source is preferably carbon black.

The ZrC, the sintering assistant and the carbon source may be mixed with a high energy ball mill operating with a planetary mill, an attrition mill, a Spex mill, or the like. For example, , It may be mixed for 0.1 to 3 hours by a dry method. However, the present invention does not limit the mixing method of the ZrC, the sintering aid, and the carbon source.

On the other hand, when the ZrC, the sintering aid, and the carbon source are used as Spex mill, it is possible to prevent incorporation of impurities caused in the production of the ZrC composite according to the present invention, as compared with other mixing methods.

That is, in the case of the attrition mill and the planetary mill, a large amount of contaminants may be introduced from the crushing ball and the crushing vessel upon crushing. However, in the case of the specs mill, such problems can be minimized.

Next, a method of manufacturing a ZrC composite according to a second embodiment of the present invention includes a step of sintering the mixture containing ZrC, the sintering aid, and the carbon source (S220).

In the present invention, the sintering temperature in the sintering step may be in the range of 17500 to 2000 ° C, and the sintering atmosphere may be vacuum, argon (Ar), nitrogen atmosphere, or by spark plasma sintering For 5 to 120 minutes.

If the sintering temperature is less than 1,700 캜, it is difficult to form a ZrC composite having a high relative density, and if the sintering temperature exceeds 2000 캜, densification can be performed, The sintering temperature in the sintering step of the present invention is in the range of 1700 to 2000 ° C since the composite material having a fine grain size for the purpose of the present invention can not be produced and the sintering in the low- It is more preferable that the sintering temperature in the sintering step in the present invention is 1750 to 2000 ° C.

Meanwhile, in the sintering step, the chemical reaction formula of the sintering aid and the carbon source is as follows.

Zirconium silicides + C? ZrC + SiC (Reaction Scheme 2)

As shown in Reaction Scheme 2, in the sintering step, ZrC and SiC can be formed through the reaction of the sintering assistant and the carbon source.

That is, in the present invention, by mixing the zirconium silicide group as the Si source with the source of carbon, it is possible to produce a high purity ZrC composite having a fine grain size and a uniform microstructure despite heat treatment at a low temperature.

At this time, ZrC and SiC formed by the reaction of the above-described sintering assistant and the carbon source form a ZrC-SiC composite together with ZrC mixed separately from the sintering additive and the carbon source.

In other words, in the second embodiment of the present invention, a separate ZrC can be added to the mixture of the sintering aid and the carbon source, thereby improving the properties such as the control of the sintering amount, cost reduction and sintering promotion .

At this time, in the present invention, it is preferable that ZrC is contained in an amount of less than 60 mass% with respect to 100 mass% of the entire mixture including ZrC, the sintering assistant and the carbon source.

More specifically, the method of manufacturing the ZrC composite according to the first embodiment of the present invention includes mixing a raw material powder and a carbon source, wherein the raw material powder is a zirconium silicide group (Zr _x Si _y , Zirconium silicide ) Is used.

The method of manufacturing a ZrC composite according to the second embodiment of the present invention includes a step of mixing ZrC, a sintering aid, and a carbon source, wherein the sintering auxiliary is a zirconium silicide group (Zr _x Si _y , Zirconium silicide) is used.

That is, in the first embodiment, the zirconium silicide group (Zr _x Si _y , Zirconium silicide) is used as the raw material powder, while the zirconium silicide group (Zr _x Si _y , Zirconium silicide) is used as the sintering auxiliary agent in the second embodiment, These correspond to the same group of Zr _x Si _y , Zirconium silicide materials.

As a result, in the case of the second embodiment, a separate ZrC is added as compared with the first embodiment. In the case of the first embodiment, the ratio of the ZrC of the mixture of the raw material powders and the carbon source to 100 mass% It can be understood that the content is 0 mass%.

However, in the case of the second embodiment, ZrC is contained in an amount of less than 60% by mass based on 100% by mass of the entire mixture including ZrC, the sintering assistant and the carbon source. Therefore, ZrC is greater than 0 and less than 60 mass%.

As a result, according to the first and second embodiments of the present invention, the method of manufacturing a ZrC composite according to the present invention includes the steps of mixing a zirconium silicide group (Zr _x Si _y , Zirconium silicide) ; And sintering the mixture of the zirconium silicide group (Zr _x Si _y , Zirconium silicide) and the carbon source.

At this time, the method of manufacturing a ZrC composite according to the present invention may include ZrC in the mixing step, or may include ZrC in the mixing step, and when the mixing step includes ZrC, the zirconium suicide group exceeds a (Zr _x Si _y, Zirconium silicide) and 100 mass% of the ZrC is 0 a mixture of said carbon source, and preferably comprises less than 60% by mass, and the ZrC is more than 0 and 50 parts by mass % Or less.

In the second embodiment of the present invention, as in the first embodiment described above, the sintering is preferably performed using a spark plasma sintering method. At this time, the spark plasma sintering Spark Plasma Sintering) method can be performed in the range of the pressing force of 10 MPa to 120 MPa.

That is, when the pressing force is less than 10 MPa, the densification effect due to the pressing deformation of the zirconium silicides at low temperatures is not apparent, and when the pressing force exceeds 120 MPa, the manufacturing is difficult industrially due to the limitations of the equipment. Is preferably in the range of the pressing force of 10 MPa to 120 MPa.

At this time, in the present invention, the spark plasma sintering method is more preferably in the range of 30 MPa to 60 MPa, and when the pressing force exceeds 60 MPa, there is no meaning of achieving sintering in the low pressure process Therefore, in the present invention, the pressure condition in the sintering step is more preferably 30 MPa to 60 MPa.

That is, in the present invention, the sintering step is carried out by using the spark plasma sintering method instead of the atmospheric pressure sintering method to prevent the coarsening phenomenon occurring at a high temperature and the sintering process using the low temperature deformation of the zirconium suicide group So that the ZrC composite can be completed at an extremely low temperature compared to the conventional results. Thus, a ZrC composite can be produced which minimizes grain growth and maximizes densification.

Thus, a ZrC composite, that is, a ZrC-SiC composite can be produced (S230).

3 is a flowchart illustrating a method of manufacturing a ZrC composite according to a third embodiment of the present invention.

The method of manufacturing the ZrC composite according to the third embodiment of the present invention may refer to the first and second embodiments described above, except as described below.

Referring to FIG. 3, a method of manufacturing a ZrC composite according to a third embodiment of the present invention includes a step of mixing SiC, a sintering aid, and a carbon source (S310)

At this time, in the present invention, the sintering aid is characterized by using a zirconium silicide group (Zr _x Si _y ), and the zirconium silicide group (Zr _x Si _y , Zirconium silicide) It may contain at least one selected from the group consisting of ZrSi ₂ , ZrSi, Zr ₅ Si ₄ , Zr ₅ Si ₃ , Zr ₃ Si ₂ , Zr ₂ Si and Zr ₃ Si. In the present invention, ZrSi ₂ is preferable.

The zirconium silicide group (Zr _x Si _y , Zirconium silicide) has a melting point ranging from 1620 to 2500 ° C. over a wide range, and since Zr and Si are uniformly mixed at the molecular level, ZrC and SiC can be simultaneously formed.

That is, in the present invention, by using the zirconium silicide group (Zr _x Si _y , Zirconium silicides) in which Zr and Si are uniformly mixed at the molecular unit level as a sintering aid, local concentration of chemical composition is prevented, And ZrC composites having SiC uniformly distributed can be produced.

The carbon source may be at least one selected from among solid carbon species such as graphite, carbon black, and activated carbon. However, the present invention does not limit the kind of the carbon source, but the carbon source in the present invention is carbon black desirable.

The SiC, the sintering assistant and the carbon source may be mixed using a planetary mill, an attrition mill, a Spex mill, or a high energy ball mill operating on a similar principle. For example, , It may be mixed for 0.1 to 3 hours by a dry method. However, the present invention does not limit the mixing method of the SiC, the sintering aid, and the carbon source.

On the other hand, when the SiC, the sintering aid, and the carbon source are used as Spex mill, it is possible to prevent incorporation of impurities caused in the production of the ZrC composite according to the present invention, as compared with other mixing methods.

That is, in the case of the attrition mill and the planetary mill, a large amount of contaminants may be introduced from the crushing ball and the crushing vessel upon crushing. However, in the case of the specs mill, such problems can be minimized.

Next, a method of manufacturing a ZrC composite according to a third embodiment of the present invention includes a step of sintering the mixture containing SiC, the sintering aid, and the carbon source (S320).

In the present invention, the sintering temperature in the sintering step may be in the range of 1700 to 2000 ° C, and the sintering atmosphere may be vacuum, argon (Ar), nitrogen atmosphere, or spark plasma sintering For 5 to 120 minutes.

If the sintering temperature is less than 1,700 캜, it is difficult to form a ZrC composite having a high relative density, and if the sintering temperature exceeds 2000 캜, densification can be performed, The sintering temperature in the sintering step of the present invention is in the range of 1700 to 2000 ° C since the composite material having a fine grain size for the purpose of the present invention can not be produced and the sintering in the low- It is more preferable that the sintering temperature in the sintering step in the present invention is 1750 to 2000 ° C.

Meanwhile, in the sintering step, the chemical reaction formula of the sintering aid and the carbon source is as follows.

Zirconium silicides + C? ZrC + SiC (scheme 3)

As shown in Reaction Scheme 3, in the sintering step, ZrC and SiC can be formed through the reaction of the sintering assistant and the carbon source.

That is, in the present invention, by mixing the zirconium silicide group as the Si source with the source of carbon, it is possible to produce a high purity ZrC composite having a fine grain size and a uniform microstructure despite heat treatment at a low temperature.

At this time, the ZrC and SiC formed by the reaction of the sintering assistant and the carbon source form a ZrC-SiC composite together with the sintering additive and SiC mixed separately from the carbon source.

That is, in the third embodiment of the present invention, a separate SiC can be added to the mixture of the sintering auxiliary agent and the carbon source, thereby improving the characteristics such as the control of the sintering auxiliary amount, cost reduction, and sintering promotion .

At this time, in the present invention, it is preferable that the content of SiC is less than 30% by mass based on 100% by mass of the total mixture including the SiC, the sintering assistant and the carbon source.

More specifically, the method of manufacturing the ZrC composite according to the first embodiment of the present invention includes mixing a raw material powder and a carbon source, wherein the raw material powder is a zirconium silicide group (Zr _x Si _y , Zirconium silicide ) Is used.

The method of manufacturing a ZrC composite according to the third embodiment of the present invention includes a step of mixing SiC, a sintering aid, and a carbon source, wherein the sintering assistant is a zirconium silicide group (Zr _x Si _y , Zirconium silicide) is used.

That is, in the first embodiment, the zirconium silicide group (Zr _x Si _y , Zirconium silicide) is used as the raw material powder, and in the third embodiment, the zirconium silicide group (Zr _x Si _y , Zirconium silicide) These correspond to the same group of Zr _x Si _y , Zirconium silicide materials.

As a result, in the case of the third embodiment, a separate SiC is added as compared with the first embodiment. In the case of the first embodiment, compared to 100% by mass of the mixture containing the raw material powder and the carbon source, It can be understood that the content is 0 mass%.

However, in the case of the third embodiment, the content of SiC is less than 30% by mass based on 100% by mass of the entire mixture including the SiC, the sintering assistant and the carbon source. Therefore, SiC is more than 0 and less than 30 mass%.

In summary, the first and third embodiments of the present invention will be summarized as follows. The method for producing a ZrC composite according to the present invention comprises the steps of mixing a zirconium silicide group (Zr _x Si _y , Zirconium silicide) ; And sintering the mixture of the zirconium silicide group (Zr _x Si _y , Zirconium silicide) and the carbon source.

At this time, the method of producing a ZrC composite according to the present invention may include SiC in the mixing step, or may include SiC in the mixing step, and in the case where SiC is included in the mixing step, the zirconium suicide (Zr _x Si _y , Zirconium silicide) and the carbon source, the SiC is preferably more than 0 and less than 30 mass%, more preferably more than 0 and not more than 20 mass% % Or less.

In the third embodiment of the present invention, as in the first embodiment, the sintering is preferably performed using a spark plasma sintering method. At this time, the spark plasma sintering Spark Plasma Sintering) method can be performed in the range of the pressing force of 10 MPa to 120 MPa.

That is, when the pressing force is less than 10 MPa, the densification effect due to the pressing deformation of the zirconium silicides at low temperatures is not apparent, and when the pressing force exceeds 120 MPa, the manufacturing is difficult industrially due to the limitations of the equipment. Is preferably in the range of the pressing force of 10 MPa to 120 MPa.

At this time, in the present invention, the spark plasma sintering method is more preferably in the range of 30 MPa to 60 MPa, and when the pressing force exceeds 60 MPa, there is no meaning of achieving sintering in the low pressure process Therefore, in the present invention, the pressure condition in the sintering step is more preferably 30 MPa to 60 MPa.

That is, in the present invention, the sintering step is carried out by using the spark plasma sintering method instead of the atmospheric pressure sintering method to prevent the coarsening phenomenon occurring at a high temperature and the sintering process using the low temperature deformation of the zirconium suicide group So that the ZrC composite can be completed at an extremely low temperature compared to the conventional results. Thus, a ZrC composite can be produced which minimizes grain growth and maximizes densification.

Thereby, a ZrC composite, that is, a ZrC-SiC composite can be produced (S330).

The manufacturing method of the ZrC composite according to the present invention is summarized as follows.

That is, the method for producing a ZrC composite according to the present invention comprises: mixing a zirconium silicide group (Zr _x Si _y , Zirconium silicide) and a carbon source; And sintering the mixture of the zirconium silicide group (Zr _x Si _y , Zirconium silicide) and the carbon source.

At this time, the method of manufacturing a ZrC composite according to the present invention may include ZrC in the mixing step, or may include ZrC in the mixing step, and when the mixing step includes ZrC, the zirconium suicide group exceeds a (Zr _x Si _y, Zirconium silicide) and 100 mass% of the ZrC is 0 a mixture of said carbon source, and preferably comprises less than 60% by mass, and the ZrC is more than 0 and 50 parts by mass % Or less.

In addition, the method of producing a ZrC composite according to the present invention may include SiC in the mixing step, or may include SiC in the mixing step, and when the mixing step includes SiC, the zirconium suicide (Zr _x Si _y , Zirconium silicide) and the carbon source, the SiC is preferably more than 0 and less than 30 mass%, more preferably more than 0 and not more than 20 mass% % Or less.

Meanwhile, in the present invention, the sintering temperature in the sintering step is preferably 1700 to 2000 ° C, and more preferably, the sintering temperature in the sintering step is 1750 to 2000 ° C.

In the present invention, it is preferable to use the spark plasma sintering method. At this time, the spark plasma sintering method of the present invention may be applied in a range of the pressing force of 10 MPa to 120 MPa , And it is more preferable that the pressing force in the spark plasma sintering method is 30 MPa to 60 MPa.

Hereinafter, preferred experimental examples according to the present invention will be described, but the present invention is not limited thereto.

[Experimental Example 1]

First, a ZrSi ₂ powder (particle size 1 to 2 탆, purity of 99% or more) was prepared from a zirconium silicide group (Zr _x Si _y , Zirconium silicides), carbon black powder (SA: Purity: 99.5% or more).

Can be determined based on the following reaction formula (1) of the ZrSi ₂ powder and the carbon black.

ZrSi ₂ + 3C = ZrC + 2SiC (1)

The above powders were mixed and then the mixed powder was sintered.

More specifically, the powders were mixed by a HEBM (High Energy Ball Milling) method in a WC pot with an N ₂ atmosphere. Thereafter, the powder was mixed using a Spark Plasma Sintering method (heating rate: 100 ° C / min) And sintered at a constant temperature under a pressure of 40 MPa.

During the sintering process described above, various reactions may occur as follows.

ZrSi ₂ + C = ZrSi + SiC (2)

5 ZrSi ₂ + 7 C = Zr ₅ Si 3 + 7 SiC (3)

2 ZrSi ₂ + 3 C = Zr ₂ Si + 3 SiC (4)

Zr ₅ Si ₃ + 8 C = 5 ZrC + 3 SiC (5)

ZrSi ₂ + C = 2 Si + ZrC (6)

Si + C = SiC (7)

Various Zr-Si phases may exist as in the above reactions (2), (3) and (4), and this intermediate reaction can be represented by the following reaction (8).

ZrSi ₂ + x C? ZrSi _{2 - x} + x SiC (8)

Figure 4 is a graph showing the Gibbs free energy of reactions during the sintering process.

Referring to FIG. 4, the Gibbs free energy of reaction (1) corresponds to a negative region in the range of 20 to 1750 ° C, which means that the reaction of (1) occurs spontaneously.

5 is a graph showing XRD data according to temperature.

Referring to FIG. 5, the ZrC phase started to appear at a temperature of 600 ° C, and when heated to 1000 ° C, a Zr-Si phase such as ZrSi, Sr ₂ Si, Zr ₅ Si ₃ or the like was formed.

Further, as the temperature increased to 1250 占 폚, the formation of SiC and ZrC phases was promoted, and the formation of SiC and ZrC phases was completed as the temperature rises to 1300 占 폚.

Based on these results, the reaction path of the ZrC-SiC composite can be summarized as follows.

_{ZrSi 2 + 3 C → SiC +} ZrC + ZrSi phases + C + ZrSi 2 → SiC + ZrC + ZrSi phases + C → SiC + ZrC (9)

FIG. 6 is a microscope showing the microstructure of the mixture subjected to the heat treatment at 1400.degree.

As shown in FIG. 6, the mixture consists of SiC and ZrC, which corresponds to the green body of the final ZrC composite.

As described above, the formation of the SiC and ZrC phases was completed as the temperature rises to 1300 ° C through the spark plasma sintering method (temperature raising rate 100 ° C / min).

Thereafter, as the temperature gradually increased, the grains of SiC and ZrC began to grow and a ZrC-SiC composite was formed.

FIG. 7A is a graph showing an XRD pattern of a ZrC-SiC composite according to a temperature condition, and FIG. 7B is an actual view showing a theoretical density and a relative density according to the condition of FIG. 7A.

Referring to FIG. 7A, raw materials, intermediate phases, and the like are not detected when sintering is performed at temperatures of 1650 ° C., 1700 ° C., and 1750 ° C.

Referring to FIG. 7B, the relative density increases from 88.05% to 99.78% while the temperature rises from 1650 ° C to 1750 ° C.

In addition, when the sintering holding time at 1700 ℃ was increased from 1 hour to 5 hours, a dense body with a relative density of 99.2% was obtained.

At this time, in the present invention, it can be confirmed that when the sintering is carried out at 1700 ° C. or more by using the spark plasma sintering method, the ZrC-SiC composite having a high relative density can be formed by sintering densely.

Therefore, as described above, in the present invention, the sintering temperature in the sintering step is preferably 1700 to 2000 ° C, and when the sintering temperature is less than 1700, the ZrC composite is densely sintered to have a high relative density If the sintering temperature is higher than 2000 ° C., densification can be performed, but the formed grain boundary of the formed silicon carbide largely occurs, so that it is impossible to produce a composite material having a fine grain size for the purpose of the present invention. Further, Therefore, the sintering temperature in the sintering step in the present invention is preferably 1700 to 2000 ° C.

FIG. 8A is a diagram showing the results of the EDS analysis of the ZrC-SiC composite according to the present invention, and FIG. 8B is a TEM image of the ZrC-SiC composite according to the present invention.

Referring to FIG. 8A, it can be seen that the ZrC-SiC composite according to the present invention is very fine and uniformly distributed in the ZrC-SiC composite, wherein ZrC and SiC grains are homogeneously distributed. Each size of the grain of SiC corresponded to about 50 nm to 1000 nm.

At this time, the average size of the SiC grains corresponds to about 260 nm, the average size of the ZrC grains corresponds to 360 nm, and the grain of the ZrC grains are embedded between the grains of the SiC grains.

8B, the ZrC grain boundaries and the SiC grain boundaries are in mutual contact, and therefore, it is confirmed that there is no raw materials or intermediate phase between the ZrC grain boundary and the SiC grain boundary. .

At this time, the Young's modulus value of the ZrC-SiC composite according to the present invention was 319 GPa and the Vicker hardness value was 23.3 GPa (corresponding to about 25 GPa for each powder of ZrC and SiC).

The fracture toughness value of the ZrC-SiC composite according to the present invention was 2.87 MPa · m ^{1/2, which} was 69% higher than the fracture toughness value (1.7 MPa · m ^1/2 ) of the ZrC powder. And improved results.

Table 1 below shows the relative density at the time of sintering pure ZrC powder.

As shown in Table 1, pure ZrC powder requires a pressing force of 80 MPa at a temperature of 2100 ° C in order to obtain a relative density of 95% or higher. Therefore, in order to obtain a dense sintered body of pure ZrC powder, Is required.

Table 2 below shows the relative density of pure SiC powder during sintering.

Referring to Table 2, it can be seen that, in the case of pure SiC powder, it is very difficult to densify through sintering, and the relative density is only about 85% even at a temperature of 2400 캜 and a pressing force of 40 MPa.

However, in the present invention, it can be confirmed that when the sintering is carried out at 1700 ° C. or more by using the spark plasma sintering method, the ZrC-SiC composite having a high relative density can be formed by sintering densely .

That is, in the present invention, it is possible to provide a ZrC composite densified while sintering at a low temperature through zirconium carbide (ZrC) and silicon carbide (SiC).

At this time, the ZrC composite has a high fracture toughness value and high neutron irradiation damage resistance, so that it is possible to provide a composite particularly useful as a structural material and a coating material of a high-temperature region in the nuclear power industry.

[Experimental Example 2]

First, a ZrSi ₂ powder (particle size 1 to 2 탆, purity of 99% or more) was prepared from a zirconium silicide group (Zr _x Si _y , Zirconium silicides), carbon black powder (SA: Purity of 99.5% or more) was prepared. ZrC powder was separately prepared.

The above powders, i.e., ZrC powder, ZrSi ₂ powder and carbon black powder were mixed, and then the mixed powder was sintered.

More specifically, the powders were mixed by a HEBM (High Energy Ball Milling) method in a WC pot with an N ₂ atmosphere. Thereafter, the powder was mixed using a Spark Plasma Sintering method (heating rate: 100 ° C / min) And sintered at a constant temperature under a constant pressure.

The experiment shown in the following Table 3 is a case where ZrSi ₂ powder as a zirconium silicide group (Zr _x Si _y , Zirconium silicide), carbon black as a carbon source and the like are separately prepared as in the second embodiment Of ZrC, wherein ZrC is contained in an amount of 70 mass% (ZCZSC3 (30%)) based on 100 mass% of the mixture.

The relative density according to the theoretical density, sintering condition and sintering condition of each experiment is shown in Table 3 below.

Referring to Table 3, it can be seen that the relative density is only about 92.4% when ZrC is contained in an amount of 70% by mass relative to 100% by mass of the mixture, even when sintering is performed at a temperature of 1800 ° C.

9 is a view showing the sintering state when ZrC is contained in an amount of 70% by mass, based on 100% by mass of the mixture.

Referring to FIG. 9, when ZrC is contained in an amount of 70% by mass relative to 100% by mass of the mixture, the content of ZrC is excessive and the relative density is only about 92.4% even at a temperature of 1800 ° C, Can be confirmed.

The experiment shown in the following Table 4 shows the case where ZrSi ₂ powder (Zr _x Si _y , Zirconium silicide), carbon black as a carbon source, and ZrSi ₂ powder as a zirconium silicide group (ZCZSC4 (40%)) and 50% (ZCZSC5 (50%)) based on 100% by mass of the mixture.

The relative density according to the theoretical density, sintering condition and sintering condition of each experiment are shown in Table 4 below.

Referring to Table 4, even when ZrC is separately sintered at a temperature of 1750 ° C (ZCZSC4 (40%)), the relative density is about 94.63% when ZrC is contained in an amount of 60 mass% Can be confirmed.

However, when ZrC is separately contained in an amount of 50 mass% (ZCZSC5 (50%)) relative to 100 mass% of the mixture, when sintering is carried out at a temperature of 1750 ° C, the relative density corresponds to 95.15% Is 95% or more, indicating that densification is achieved.

Fig. 10 is a view showing the sintering condition according to the conditions of Table 4. Fig.

10, when ZrC is contained in an amount of 60% by mass with respect to 100% by mass of the mixture, the relative density is not more than 94.63% even at a temperature of 1750 ° C, %, It can be confirmed that the densification of the target value to be achieved does not occur.

However, when ZrC is contained in an amount of 40 mass% with respect to 100 mass% of the mixture and sintered at a temperature of 1750 ° C, the relative density corresponds to 95.15%, that is, the relative density corresponds to 95% Can be confirmed.

On the other hand, even when ZrC is contained in an amount of 40% by mass as compared with 100% by mass of the mixture, when sintering is carried out at a temperature of 1700 캜, the relative density corresponds to 94.22%, that is, the relative density is less than 95% It can be confirmed that the target value to be densified does not occur.

11 is XRD data according to the conditions of Tables 3 and 4.

11, irrespective of whether or not densification (relative density 95% or more) of the target value to be achieved has occurred, when ZrC is added in an amount of 50 to 70 mass%, residual ZrSi ₂ or the like, It can be seen that only the ZrC and SiC phases are formed without the ZrC phase, and that the size of the SiC phase increases with the decrease of the ZrC content.

The experiment shown in the following Table 5 is a case in which ZrSi ₂ powder (Zr _x Si _y , Zirconium silicide), carbon black as a carbon source, and ZrSi ₂ powder as a zirconium silicide group Of ZrC is mixed with 20 mass% (ZCZSC8 (80%)) based on 100 mass% of the mixture.

The relative density according to the theoretical density, sintering condition and sintering condition of each experiment is shown in Table 5 below.

Referring to Table 5, when ZrC was separately contained in an amount of 20 mass% (ZCZSC8 (80%)) relative to 100 mass% of the mixture, sintering at a temperature of 1750 ° C varied depending on the sintering time , The relative density corresponds to 96.58% (10 minutes) and 99.9% (30 minutes), that is, the relative density corresponds to 95% or more.

Particularly, when ZrC is separately contained in an amount of 20% by mass (ZCZSC8 (80%)) relative to 100% by mass of the above mixture, sintering at a temperature of 1800 ° C and a sintering time of 10 minutes also have a relative density of 99.5 %, That is, the relative density corresponds to 95% or more, so that the densification can be confirmed.

12 is a view showing the sintering state in the case where ZrC is contained in an amount of 20 mass% with respect to 100 mass% of the mixture and sintering is carried out at a temperature of 1750 캜 for 30 minutes.

Referring to FIG. 12, when the ZrC was contained in an amount of 20% by mass with respect to 100% by mass of the mixture, when the sintering was performed at a temperature of 1750 ° C. for 30 minutes, the relative density was 99.9% Can be confirmed.

Fig. 13 is XRD data according to the conditions of Table 5. Fig.

Referring to FIG. 13, it can be confirmed that when ZrC is added at 20 mass%, regardless of the degree of densification (relative density is 95% or more), only ZrC and SiC phases are formed without forming a residual phase such as ZrSi ₂ or a secondary phase , And that the size of the SiC phase increases with decreasing ZrC content.

In addition, at the same content (ZrC 20 mass%), the grain growth of SiC increases with increasing sintering temperature and sintering time, and the intensity of the peak increases.

According to the above results, the method of producing a ZrC composite according to the present invention is characterized in that, when the ZrC composite is included in the mixing step, 100 mass parts of the mixture of the zirconium silicide group (Zr _x Si _y , Zirconium silicide) %, The ZrC is preferably more than 0 and less than 60 mass%.

Also, in the present invention, the sintering temperature in the sintering step is preferably 1700 to 2000 ° C. In the present invention, the sintering is preferably a spark plasma sintering method, and the spark plasma sintering (Spark Plasma Sintering) method is more preferably 30 MPa to 60 MPa.

[Experimental Example 3]

First, a ZrSi ₂ powder (particle size 1 to 2 탆, purity of 99% or more) was prepared from a zirconium silicide group (Zr _x Si _y , Zirconium silicides), carbon black powder (SA: Purity of 99.5% or more) was prepared, and SiC powder was separately prepared.

The above powder, i.e., SiC powder, ZrSi ₂ powder and carbon black powder were mixed, and then the mixed powder was sintered.

More specifically, the powders were mixed by a HEBM (High Energy Ball Milling) method in a WC pot with an N ₂ atmosphere. Thereafter, the powder was mixed using a Spark Plasma Sintering method (heating rate: 100 ° C / min) And sintered at a constant temperature under a constant pressure.

The experiment shown in the following Table 6 is a case in which another ZrSi ₂ powder (Zr _x Si _y , Zirconium silicide), carbon black as a carbon source, and a zirconium silicide group SiC is mixed with 10 mass% (SCZSC9), 20 mass% (SCZSC8), 30 mass% (SCZSC7) and 40 mass% (SCZSC6) based on 100 mass% of the mixture.

The relative density according to the theoretical density, sintering condition and sintering condition of each experiment is shown in Table 6 below.

Referring to Table 6, it can be confirmed that the relative density is about 82.36% even when the SiC is separately sintered at a temperature of 1750 ° C in the case of containing 30% by mass (SCZSC7) relative to 100% by mass of the mixture.

Also, it can be confirmed that the relative density is about 76.6% even when the SiC is separately sintered at a temperature of 1750 DEG C (SCZSC6) when 40 mass% of the SiC is added to 100 mass% of the mixture.

However, when a separate SiC is contained in an amount of 20 mass% (SCZSC8) relative to 100 mass% of the mixture, when sintering is carried out at a temperature of 1750 ° C, the relative density corresponds to 99.6% , It can be confirmed that the densification is performed.

The relative density is 96.04% (10%) when sintering is carried out at a temperature of 1750 ° C, although the difference is dependent on the sintering time when separate SiC is contained at 10 mass% (SCZSC9) relative to 100 mass% Minute) and 98.81% (30 minutes), that is, the relative density corresponds to 95% or more, so that the densification can be confirmed.

On the other hand, it can be confirmed that the relative density is about 84.4% when the SiC is separately sintered at a temperature of 1700 ° C in the case of containing 20 mass% (SCZSC8) of the above mixture as 100 mass% (SCZSC9) relative to 100 mass% of the above mixture, the relative density is about 85.7% when sintering is carried out at a temperature of 1700 ° C.

14A is a view showing a sintering state when sintering is carried out at a temperature of 1750 DEG C for 30 minutes, wherein SiC is contained in an amount of 20% by mass based on 100% by mass of the mixture.

Referring to FIG. 14A, when 20% by mass of SiC is contained as compared with 100% by mass of the mixture, when the sintering is performed at a temperature of 1750 ° C for 30 minutes, the relative density is 99.6% Can be confirmed.

14B is a view showing a sintering state in which sintering is carried out for 30 minutes at a temperature of 1750 DEG C and 10% by mass of SiC based on 100% by mass of the mixture.

Referring to FIG. 14B, when the SiC was contained in an amount of 10% by mass based on 100% by mass of the mixture and sintered at a temperature of 1750 ° C for 30 minutes, the relative density was 98.81% Can be confirmed.

15 is XRD data according to the partial conditions of Table 6. < tb > < TABLE >

Referring to FIG. 15, when additional SiC is added at 10 mass% and 20 mass% regardless of the degree of densification (relative density is 95% or more), only ZrC and SiC phases are formed without residual phase such as ZrSi ₂ or secondary phase .

According to the above results, the method of producing a ZrC composite according to the present invention is characterized in that when the SiC is included in the mixing step, 100 mass% of the mixture of the zirconium silicide group (Zr _x Si _y , Zirconium silicide) %, The SiC is preferably more than 0 and less than 30 mass%.

Also, in the present invention, the sintering temperature in the sintering step is preferably 1700 to 2000 ° C. In the present invention, the sintering is preferably a spark plasma sintering method, and the spark plasma sintering (Spark Plasma Sintering) method is more preferably 30 MPa to 60 MPa.

While the present invention has been described in connection with what is presently considered to be practical exemplary embodiments, it is to be understood that the invention is not limited to the disclosed embodiments, but, on the contrary, It will be understood. It is therefore to be understood that the above-described embodiments are illustrative in all aspects and not restrictive.

Claims (12)

ZrC grain; And
SiC grain,
Characterized in that the grain boundary of the ZrC grain and the grain boundary of the SiC grain are in contact with each other and the grain of the ZrC is present between the grains of the SiC,
Wherein there is no raw materials or intermediate phase between the grain boundary of the ZrC grain and the grain boundary of the SiC grain. The method according to claim 1,
Wherein the ZrC grain and the SiC grain each have a size of 50 nm to 1000 nm. delete The method according to claim 1,
Wherein the ZrC composite has a relative density of 95% or more. The method according to claim 1,
Wherein the ZrC composite is a ZrC-SiC composite. In the method for producing a ZrC composite,
Mixing a zirconium silicide group (Zr _x Si _y , Zirconium silicide) and a carbon source; And
Sintering the mixture of the zirconium silicide group (Zr _x Si _y , Zirconium silicide) and the carbon source,
The ZrC composite may include ZrC grain; And a SiC grain, wherein the grain boundary of the ZrC grain and the grain boundary of the SiC grain are in mutual contact, and the grain of the ZrC is contained between the grains of the SiC,
Wherein no raw materials or intermediate phases are present between the grain boundary of the ZrC grain and the grain boundary of the SiC grain. The method according to claim 6,
Wherein the zirconium silicide group (Zr _x Si _y , Zirconium silicide) is ZrSi ₂ , and the carbon source is carbon black. The method according to claim 6,
Further comprising a ZrC powder in the mixing step,
Wherein the ZrC powder is contained in an amount of more than 0 and less than 60 mass% based on 100 mass% of the mixture of the ZrC powder, the zirconium silicide group (Zr _x Si _y ), and the carbon source. The method according to claim 6,
Further comprising a SiC powder in the mixing step,
Wherein the SiC powder is contained in an amount of more than 0 and less than 30% by mass based on 100% by mass of the SiC powder, the zirconium silicide group (Zr _x Si _y ), and the carbon source. The method according to claim 6,
Wherein the sintering temperature in the sintering step is 1700 to 2000 占 폚. The method according to claim 6,
Wherein the sintering is performed using a spark plasma sintering method and the sprue plasma sintering method is applied in a range of 30 MPa to 60 MPa. The method according to claim 6,
Wherein the ZrC composite is a ZrC-SiC composite.

Images