Low-oxygen vanadium aluminum carbide max and method for producing the same

Abstract

This invention provides low-oxygen vanadium aluminum carbide (V2AlC) max for producing high-purity vanadium maxine, and a method for producing the same.

Description

[Technical Field]

[0001] The present invention relates to low-oxygen vanadium aluminum carbide (V2AlC) max for producing high-purity vanadium max, and to a method for producing the same. [Background technology]

[0002] Vanadium metal is a substance that readily forms carbides, nitrides, or oxides due to its high affinity for nonmetallic components such as carbon, nitrogen, or oxygen.

[0003] Therefore, although vanadium carbides, produced by the bonding of vanadium and carbon, are easily synthesized compounds, due to vanadium's strong affinity for oxygen, it is not easy to synthesize pure (low-oxygen) carbides.

[0004] That is, V(C x O 1-x Because x<1 form oxycarbides are readily formed, the production of vanadium carbides with low oxygen content is not easily carried out.

[0005] Therefore, through many years of painstaking effort and various research, the applicant has obtained low-oxygen vanadium aluminum carbide max, which is formed by using both an inert gas and hydrogen gas in the carbide reaction of vanadium and aluminum in a state in which the oxygen content is reduced, and a method for producing the same, thereby completing the present invention. [Overview of the Initiative] [Problems that the invention aims to solve]

[0006] Therefore, the object of the present invention is to provide low-oxygen vanadium aluminum carbide max, which is formed in a state where the oxygen content is reduced by using both an inert gas and hydrogen gas in the carbide reaction of vanadium and aluminum.

[0007] Furthermore, an object of the present invention is to provide a method for producing low-oxygen vanadium aluminum carbide max, which is formed in a state where the oxygen content is reduced by using both an inert gas and hydrogen gas in the carbide reaction of vanadium and aluminum.

[0008] Furthermore, an object of the present invention is to provide applications for low-oxygen vanadium aluminum carbide max, which is formed in a state where the oxygen content is reduced by using both an inert gas and hydrogen gas in the carbide reaction of vanadium and aluminum.

[0009] Furthermore, an object of the present invention is to provide low-oxygen vanadium aluminum carbide max produced by the method for producing low-oxygen vanadium aluminum carbide max described above, having an oxygen content of 10 ppm to 8,000 ppm.

[0010] The problems that this invention aims to solve are not limited to those mentioned above, and other problems not mentioned can be clearly understood by those skilled in the art from the following description. [Means for solving the problem]

[0011] In order to solve the aforementioned problems, according to one aspect of the present invention, Low-oxygen vanadium aluminum carbide max, vanadium; Aluminum; and, Composed of carbon, The low-oxygen vanadium aluminum carbide max is characterized by being formed using both an inert gas and hydrogen gas in the carbide reaction of vanadium and aluminum. We offer low-oxygen vanadium aluminum carbide max.

[0012] According to one embodiment of the present invention, the low-oxygen vanadium aluminum carbide max is After mixing vanadium oxide, aluminum compounds and carbon compounds, After the mixed powder is manufactured into BulkMax with larger particle sizes by sintering heat treatment, After the aforementioned bulkmax is crushed and pulverized to produce fine powder max, The fine powder Max may be used together with the inert gas and hydrogen gas, and subjected to a carbonization-reduction heat treatment to form a product with reduced oxygen content.

[0013] According to one embodiment of the present invention, the oxygen content may be 10 ppm to 8,000 ppm.

[0014] According to one embodiment of the present invention, the low-oxygen vanadium aluminum carbide max may have the chemical formula V2AlC.

[0015] According to one embodiment of the present invention, the molar ratio (B / A) of the aluminum compound (B) to the vanadium oxide (A) may be 0.2 to 10. The molar ratio (C / A) of the carbon compound (C) to the vanadium oxide (A) may be 0.2 to 10.

[0016] According to one embodiment of the present invention, the particle size of the mixed powder of vanadium oxide, aluminum oxide, and carbon compound may be 2 nm to 50 μm.

[0017] According to one embodiment of the present invention, the vanadium oxide may be at least one selected from vanadium pentoxide (V2O5), sodium metavanadate (NaVO3), vanadium trioxide (V2O3), vanadium oxychloride (VOCl3), and ammonium metavanadate (H4NVO3).

[0018] According to one embodiment of the present invention, the aluminum compound may be at least one selected from alumina (Al2O3), aluminum hydroxide (Al(OH)3), aluminum chloride (AlCl3), aluminum fluoride (AlF3), and aluminum sulfate (Al2(SO4)3).

[0019] According to an embodiment of the present invention, the carbon compound may be at least any one selected from industrial carbon powder, coke, coal, coal tar, activated carbon, natural graphite, artificial graphite, carbon black, acetylene black, ketjen black, channel black, furnace black, lamp black, summer black, industrial diamond, and carbon fiber.

[0020] According to an embodiment of the present invention, the content of the inert gas and hydrogen gas may be 10:1 to 1:10 in volume ratio.

[0021] According to an embodiment of the present invention, the sintering heat treatment temperature is 800°C to 1600°C, and the sintering heat treatment time may be 10 minutes to 24 hours.

[0022] According to an embodiment of the present invention, the particle size of the bulk max is 50 nm to 100 μm, and the particle size of the fine powder may be 2 nm to 20 μm.

[0023] Also, according to another aspect of the present invention, a method for producing low-oxygen vanadium aluminum carbide max, comprising: (a-1) mixing vanadium oxide, an aluminum compound, and a carbon compound to produce a mixed powder; (a-2) subjecting the mixed powder to sintering heat treatment to produce bulk max; (a-3) crushing and pulverizing the bulk max to produce a fine powder max; and (a-4) subjecting the fine powder max to a carbothermal reduction heat treatment using both an inert gas and hydrogen gas in an atmosphere of air, vacuum, nitrogen, or argon in a high-temperature synthesis furnace or a supercantor furnace to reduce the oxygen content and produce low-oxygen vanadium aluminum carbide max. A method for producing low-oxygen vanadium aluminum carbide max is provided.

[0024] According to one embodiment of the present invention, in the step of producing a mixed powder by mixing (a-1) vanadium oxide, an aluminum compound and a carbon compound, The mixing ratio of the vanadium oxide, the aluminum compound, and the carbon compound may be 1:0.2 to 0.7:0.1 to 0.5 by weight.

[0025] According to one embodiment of the present invention, in the step of manufacturing Bulkmax by heat-treating the (a-2) mixed powder, The sintering heat treatment temperature is 800°C to 1600°C. The sintering heat treatment time may be between 10 minutes and 24 hours.

[0026] According to one embodiment of the present invention, in the step of crushing and pulverizing the Bulkmax (a-3) to produce a fine powder, The particle size of the aforementioned Bulkmax is 50 nm to 100 μm. The particle size of the fine powder may be 2 nm to 20 μm.

[0027] According to one embodiment of the present invention, in the step of producing low-oxygen vanadium aluminum carbide max by subjecting the (a-4) fine powder max to a carbonization reduction heat treatment in a high-temperature synthesis furnace or superkanthal furnace under an atmosphere of air, vacuum, nitrogen or argon, using both an inert gas and hydrogen gas, the oxygen content is reduced. The heat treatment temperature for the carbonization reduction reaction using both the inert gas and hydrogen gas is 500°C to 1100°C. The heat treatment time for the carbonization reduction reaction may be between 10 minutes and 24 hours.

[0028] Furthermore, according to another aspect of the present invention, The present invention provides low-oxygen vanadium aluminum carbide max, which has applications as a maxine precursor, a raw material for cemented carbide materials, a catalyst, or a semiconductor material.

[0029] Furthermore, according to another aspect of the present invention, The present invention provides low-oxygen vanadium aluminum carbide max produced by the method for producing low-oxygen vanadium aluminum carbide max, having an oxygen content of 10 ppm to 8,000 ppm.

[0030] Furthermore, according to another aspect of the present invention, The low-oxygen vanadium aluminum carbide max produced by the above-mentioned method for producing low-oxygen vanadium aluminum carbide max has applications as a maxine precursor, a raw material for cemented carbide materials, a catalyst, or a semiconductor material. [Effects of the Invention]

[0031] According to the present invention, low-oxygen vanadium aluminum carbide max is formed by using both an inert gas and hydrogen gas in the carbide reaction of vanadium and aluminum, resulting in a reduced oxygen content. Therefore, low-oxygen vanadium aluminum carbide max has a low oxygen content, small particle size, and excellent physical properties, making it suitable for various applications such as maxine precursors, raw materials for cemented carbide materials, catalysts, or semiconductor materials.

[0032] Furthermore, the present invention provides a method for producing low-oxygen vanadium aluminum carbide max, which is formed by using both an inert gas and hydrogen gas in the carbonization reaction of vanadium and aluminum, thereby reducing the oxygen content. This method offers excellent process stability, enables mass production, and is economical.

[0033] Furthermore, the present invention provides low-oxygen vanadium aluminum carbide max produced by the method for producing low-oxygen vanadium aluminum carbide max, having an oxygen content of 10 ppm to 8,000 ppm. As a result, low-oxygen vanadium aluminum carbide max has a low oxygen content, small particle size, and excellent physical properties, and can be used in various applications such as maxine precursors, raw materials for cemented carbide materials, catalysts, or semiconductor materials.

[0034] The effects of the present invention are not limited to those described above, but should be understood to include all effects that can be inferred from the detailed description of the present invention or the configuration of the invention as described in the claims. [Brief explanation of the drawing]

[0035] [Figure 1] This is a schematic diagram of a method for producing low-oxygen vanadium aluminum carbide max, which is formed by using both an inert gas and hydrogen gas in the carbide reaction of vanadium and aluminum according to one embodiment of the present invention, thereby reducing the oxygen content. [Figure 2] This is a flowchart illustrating a process for producing low-oxygen vanadium aluminum carbide max according to one embodiment of the present invention. [Figure 3] This graph shows the DSC analysis results and gas charging interval of a 2V+Al+C mixture according to one embodiment of the present invention. [Figure 4] This graph shows the oxygen content of low-oxygen vanadium aluminum carbide max according to one embodiment of the present invention. [Modes for carrying out the invention]

[0036] In the following, preferred embodiments of the present invention will be described in detail with reference to the attached drawings.

[0037] The advantages and features of the present invention, and the methods for achieving them, will become clear when you refer to the embodiments described in detail below, along with the accompanying drawings.

[0038] However, the present invention is not limited to the embodiments disclosed below, but can be embodied in a variety of different forms. These embodiments are provided to complete the disclosure of the present invention and to fully inform those who are ordinary skill in the art to which the invention pertains, and the present invention is defined only by the scope of the claims.

[0039] Furthermore, in describing the present invention, if it is determined that related known technologies or other elements would obscure the gist of the present invention, a detailed explanation thereof will be omitted.

[0040] The present invention will be described in detail below.

[0041] Low-oxygen vanadium aluminum carbide max The present invention provides low-oxygen vanadium aluminum carbide max, which is formed by using both an inert gas and hydrogen gas in the carbide reaction of vanadium and aluminum, thereby reducing the oxygen content.

[0042] The present invention relates to low-oxygen vanadium aluminum carbide max, vanadium; Aluminum; and, Composed of carbon, The low-oxygen vanadium aluminum carbide max is formed by using both an inert gas and hydrogen gas in the charring reaction of vanadium and aluminum.

[0043] This invention provides low-oxygen vanadium aluminum carbide max, which is formed by using both an inert gas and hydrogen gas in the carbide reaction of vanadium and aluminum to reduce the oxygen content. As a result, low-oxygen vanadium aluminum carbide max has a low oxygen content, small particle size, and excellent physical properties, and can be used in various applications such as maxine precursors, raw materials for cemented carbide materials, catalysts, or semiconductor materials.

[0044] Vanadium metal is a substance that readily forms carbides, nitrides, or oxides due to its high affinity for nonmetallic components such as carbon, nitrogen, or oxygen.

[0045] Therefore, although vanadium carbides, produced by the bonding of vanadium and carbon, are easily synthesized compounds, due to vanadium's strong affinity for oxygen, it is not easy to synthesize pure (low-oxygen) carbides.

[0046] That is, V(C x O 1-x Because x<1 form oxycarbides are readily formed, the production of vanadium carbides with low oxygen content is not easily carried out.

[0047] Therefore, through many years of painstaking effort and various research, the applicant has obtained low-oxygen vanadium aluminum carbide max and a method for producing the same, which are formed in a state where the oxygen content is reduced by using both an inert gas and hydrogen gas in the carbide reaction of vanadium and aluminum, thus completing the present invention.

[0048] Furthermore, the low-oxygen vanadium aluminum carbide max of the present invention is After mixing vanadium oxide, aluminum compounds and carbon compounds, After the mixed powder is manufactured into BulkMax with larger particle sizes by sintering heat treatment, After the aforementioned bulkmax is crushed and pulverized to produce fine powder max, The fine powder Max may be used together with the inert gas and hydrogen gas, and subjected to a carbonization-reduction heat treatment to form a product with reduced oxygen content.

[0049] In this case, the oxygen content may be between 10 ppm and 8,000 ppm.

[0050] Here, if the oxygen content is within the above range, V(C) has a high oxygen content. x O 1-x ) Acid carbides of this form may not be easily formed.

[0051] In this case, the oxygen content may preferably be 30 ppm to 8,000 ppm, and more preferably 100 ppm to 7,000 ppm.

[0052] Furthermore, the low-oxygen vanadium aluminum carbide max may have the chemical formula V2AlC.

[0053] Further, the molar ratio (B / A) of the aluminum compound (B) to the vanadium oxide (A) may be 0.2 to 10, and the molar ratio (C / A) of the carbon compound (C) to the vanadium oxide (A) may be 0.2 to 10.

[0054] Here, when the molar ratio (B / A) of the aluminum compound (B) to the vanadium oxide (A) is within the above range, the low-oxygen vanadium aluminum carbide MAX may not easily form oxycarbides in the form of V(C x O 1-x ).

[0055] At this time, the molar ratio (B / A) of the aluminum compound (B) to the vanadium oxide (A) may preferably be 0.5 to 9, and more preferably 1 to 8.

[0056] Also, when the molar ratio (B / A) of the carbon compound (C) to the vanadium oxide (A) is within the above range, the low-oxygen vanadium aluminum carbide MAX may not easily form oxycarbides in the form of V(C x O 1-x ).

[0057] At this time, the molar ratio (C / A) of the carbon compound (C) to the vanadium oxide (A) may preferably be 0.5 to 9, and more preferably 1 to 8.

[0058] And the particle size of the mixed powder of the vanadium oxide, the aluminum oxide and the carbon compound may be 2 nm to 50 μm.

[0059] Here, when the particle size of the mixed powder of the vanadium oxide, the aluminum oxide and the carbon compound is within the above range, the contact area of the vanadium oxide, the aluminum oxide and the carbon compound increases, and the carboreduction reaction rate may increase.

[0060] In this case, the particle size of the mixed powder of the vanadium oxide, aluminum oxide, and carbon compound may preferably be 2 nm to 48 μm, and more preferably 2 nm to 45 μm.

[0061] Furthermore, the vanadium oxide may be at least one selected from vanadium pentoxide (V2O5), sodium metavanadate (NaVO3), vanadium trioxide (V2O3), vanadium oxychloride (VOCl3), and ammonium metavanadate (H4NVO3).

[0062] Furthermore, the aluminum compound may be at least one selected from alumina (Al2O3), aluminum hydroxide (Al(OH)3), aluminum chloride (AlCl3), aluminum fluoride (AlF3), and aluminum sulfate (Al2(SO4)3).

[0063] Furthermore, the carbon compound may be at least one selected from industrial carbon powder, coke, coal, coal tar, activated carbon, natural graphite, artificial graphite, carbon black, acetylene black, Ketjen black, channel black, furnace black, lamp black, summer black, industrial diamond, and carbon fiber.

[0064] Here, the carbon compound may further include biomass, which is at least one selected from coffee grounds, fallen leaves, and waste wood.

[0065] In this case, the carbon compound may further include a carbon-containing reducing gas, which is at least one selected from carbon monoxide, methane, and hydrocarbons.

[0066] Here, when vanadium (V) and aluminum (Al) are used as raw materials for synthesizing vanadium carbide, the vanadium carbide is formed by the reaction of vanadium and aluminum with carbon, i.e., by carbonization reduction, as shown in Chemical Formula 1 below.

[0067] 2V(s)+ Al(l)+ C(s)→V2AlC(s) -----(Chemical 1)

[0068] In this process, theoretically, by adjusting the amount of carbon to less than 1 mole for every 2 moles of vanadium, a hypoxic vanadium aluminum carbide max in the V2AlC form may be synthesized.

[0069] However, in actual processes, reducing the amount of carbon that acts as a reducing agent decreases the reaction rate for reduction, and V(C) with a high oxygen content x O 1-x Acid carbides of the ) form can be easily formed.

[0070] Furthermore, in order to form vanadium carbides, it is necessary not only to adjust the amount of carbon, but also to perform treatments to increase the rate of the carbonization reduction reaction.

[0071] In this invention, the particle size of the raw material, a mixed powder of vanadium oxide, alumina, and carbon, is reduced to the above range by a crushing and grinding process to increase the reaction rate. After introducing an inert gas and hydrogen gas, the mixture is subjected to a carbonization reduction heat treatment to reduce the oxygen content and synthesize low-oxygen vanadium aluminum carbide max.

[0072] Furthermore, the volume ratio of the inert gas to the hydrogen gas may be 10:1 to 1:10.

[0073] Here, if the content of the inert gas and hydrogen gas is within the above range, a low-oxygen vanadium aluminum carbide max can be synthesized with reduced oxygen content.

[0074] In this case, the content of the inert gas and hydrogen gas may preferably be 10:2 to 2:10 by volume, and more preferably 10:3 to 3:10 by volume.

[0075] Furthermore, the sintering heat treatment temperature is 800°C to 1600°C. The sintering heat treatment time may be between 10 minutes and 24 hours.

[0076] Furthermore, the particle size of the Bulkmax is 50 nm to 100 μm. The particle size of the fine powder Max may be 2 nm to 20 μm.

[0077] Here, if the sintering heat treatment temperature is within the above range, the particle size of the bulkmax may be 50 nm to 100 μm.

[0078] In this case, the sintering heat treatment temperature may preferably be 850°C to 1600°C, and more preferably 900°C to 1600°C.

[0079] Furthermore, if the sintering heat treatment time is within the above range, the particle size of the bulkmax may be 50 nm to 100 μm.

[0080] In this case, the sintering heat treatment time may preferably be 20 minutes to 24 hours, and more preferably 30 minutes to 24 hours.

[0081] Furthermore, the aforementioned carbonization-reduction reaction can produce low-oxygen vanadium aluminum carbide max using both an inert gas and a hydrogen gas.

[0082] Manufacturing method for low-oxygen vanadium aluminum carbide max The present invention provides a method for producing low-oxygen vanadium aluminum carbide max, which is formed by using both an inert gas and hydrogen gas in the carbide reaction of vanadium and aluminum, thereby reducing the oxygen content.

[0083] The present invention is a method for producing low-oxygen vanadium aluminum carbide max, (a-1) A step of mixing vanadium oxide, aluminum compounds and carbon compounds to produce a mixed powder; (a-2) The step of manufacturing Bulkmax by heat-treating the mixed powder with sintering heat; (a-3) The step of crushing and grinding the bulk max to produce fine powder max; and, (a-4) The process includes the step of producing low-oxygen vanadium aluminum carbide max by subjecting the fine powder max to a carbonization reduction heat treatment in a high-temperature synthesis furnace or superkanthal furnace under an atmosphere of air, vacuum, nitrogen, or argon, using both an inert gas and hydrogen gas to reduce the oxygen content.

[0084] This invention provides a method for producing low-oxygen vanadium aluminum carbide max, which is formed by using both an inert gas and hydrogen gas in the carbonization reaction of vanadium and aluminum, thereby reducing the oxygen content. As such, the method offers excellent process stability, enables mass production, and is economical.

[0085] Furthermore, in the step of (a-1) mixing vanadium oxide, aluminum compound and carbon compound to produce a mixed powder, The mixing ratio of the vanadium oxide, the aluminum compound, and the carbon compound may be 1:0.2 to 0.7:0.1 to 0.5 by weight.

[0086] Here, if the mixing ratio of the vanadium oxide, the aluminum compound, and the carbon compound is within the above range in terms of weight ratio, then V(C) has a high oxygen content. x O 1-x ) Acid carbides of this form may not be easily formed.

[0087] In this case, the mixing ratio of the vanadium oxide, the aluminum compound, and the carbon compound may preferably be 1:0.3 to 0.7:0.2 to 0.5 by weight, and more preferably 1:0.3 to 0.6:0.2 to 0.4 by weight.

[0088] Then, in the step of manufacturing Bulkmax by heat-treating the (a-2) mixed powder, The sintering heat treatment temperature is 800°C to 1600°C. The sintering heat treatment time may be between 10 minutes and 24 hours.

[0089] Furthermore, in the step of crushing and pulverizing the Bulkmax (a-3) to produce a fine powder, The particle size of the aforementioned Bulkmax is 50 nm to 100 μm. The particle size of the fine powder may be 2 nm to 20 μm.

[0090] Here, if the sintering heat treatment temperature is within the above range, the particle size of the bulkmax may be 50 nm to 100 μm.

[0091] In this case, the sintering heat treatment temperature may preferably be 850°C to 1600°C, and more preferably 900°C to 1600°C.

[0092] Furthermore, if the sintering heat treatment time is within the above range, the particle size of the bulkmax may be 50 nm to 100 μm.

[0093] In this case, the sintering heat treatment time may preferably be 20 minutes to 24 hours, and more preferably 30 minutes to 24 hours.

[0094] Furthermore, in the step of producing low-oxygen vanadium aluminum carbide max by subjecting the fine powder max described above (a-4) to a carbonization reduction heat treatment in a high-temperature synthesis furnace or super Kanthal furnace under an atmosphere of air, vacuum, nitrogen, or argon, using both an inert gas and hydrogen gas, thereby reducing the oxygen content, The heat treatment temperature for the carbonization reduction reaction using both the inert gas and hydrogen gas is 500°C to 1100°C. The heat treatment time for the carbonization reduction reaction may be between 10 minutes and 24 hours.

[0095] Here, the carbonization reduction reaction heat treatment may be a process in which the fine powder Max is heat-treated in a high-temperature synthesis furnace or a super Kanthal furnace under an atmosphere of air, vacuum, nitrogen, or argon, using both an inert gas and hydrogen gas.

[0096] Here, if the heat treatment temperature for the carbonization-reduction reaction using both the inert gas and hydrogen gas is within the above range, the low-oxygen vanadium aluminum carbide max may exhibit excellent low-oxygen properties and manufacturing efficiency.

[0097] In this case, the heat treatment temperature for the carbonization reduction reaction using both the inert gas and hydrogen gas is preferably 550°C to 1050°C, and more preferably 600°C to 1000°C.

[0098] Furthermore, if the heat treatment time for the carbonization-reduction reaction using both the inert gas and hydrogen gas is within the above range, the low-oxygen vanadium aluminum carbide max may exhibit excellent low-oxygen properties and manufacturing efficiency.

[0099] In this case, the heat treatment time for the carbonization reduction reaction using both the inert gas and hydrogen gas is preferably 20 minutes to 24 hours, and more preferably 30 minutes to 24 hours.

[0100] Figure 1 is a schematic diagram of a method for producing low-oxygen vanadium aluminum carbide max, which is formed by using both an inert gas and hydrogen gas in the carbide reaction of vanadium and aluminum according to one embodiment of the present invention, thereby reducing the oxygen content.

[0101] Referring to Figure 1, a mixed powder is produced by mixing (blending) vanadium oxide, aluminum compounds, and carbon compounds.

[0102] Subsequently, the mixed powder is subjected to sintering heat treatment to produce Bulkmax.

[0103] Subsequently, the bulk max is crushed and pulverized to produce fine powder max.

[0104] Subsequently, the fine powder Max is subjected to a carbonization reduction heat treatment in a high-temperature synthesis furnace or super Kanthal furnace under an atmosphere of air, vacuum, nitrogen, or argon, using both inert gas and hydrogen gas to produce low-oxygen vanadium aluminum carbide Max with reduced oxygen content.

[0105] Subsequently, when the oxygen content of the low-oxygen vanadium aluminum carbide max is analyzed to be 0.8 wt% or less, maxine is produced.

[0106] If the oxygen content of the low-oxygen vanadium aluminum carbide max, as determined by analysis, exceeds 0.8 wt%, the vanadium aluminum carbide max is returned to the mixed powder manufacturing process, and then the low-oxygen vanadium aluminum carbide max is manufactured again.

[0107] Figure 2 is a flowchart of the process for producing low-oxygen vanadium aluminum carbide max according to one embodiment of the present invention.

[0108] Referring to Figure 2, first, a mixed powder is produced by mixing vanadium oxide, an aluminum compound, and a carbon compound (S110).

[0109] Subsequently, the mixed powder is subjected to sintering heat treatment to produce Bulkmax (S120).

[0110] Subsequently, the bulk max is crushed and pulverized to produce fine powder max (S130).

[0111] Subsequently, the fine powder Max is subjected to a carbonization reduction heat treatment in a high-temperature synthesis furnace or a super Kanthal furnace under an atmosphere of air, vacuum, nitrogen, or argon, using both an inert gas and hydrogen gas to produce low-oxygen vanadium aluminum carbide Max with reduced oxygen content (S140).

[0112] Figure 3 shows the DSC analysis results and gas charging interval graph of a 2V+Al+C mixture according to one embodiment of the present invention.

[0113] Referring to Figure 3, the 600-1000°C range, where the reaction is most active, is selected as the hydrogen reduction gas injection range. By injecting hydrogen, which can rapidly reduce oxygen, into this reaction range, the oxygen content of the final V2AlCmax can be reduced.

[0114] Applications of low-oxygen vanadium aluminum carbide max This invention provides applications for low-oxygen vanadium aluminum carbide max, which is formed by using both an inert gas and hydrogen gas in the carbide reaction of vanadium and aluminum, thereby reducing the oxygen content.

[0115] The present invention provides low-oxygen vanadium aluminum carbide max, which can be used as a maxine precursor, a raw material for cemented carbide materials, a catalyst, or a semiconductor material.

[0116] Low-oxygen vanadium aluminum carbide MAX with an oxygen content of 10 ppm to 8,000 ppm. The present invention provides low-oxygen vanadium aluminum carbide max, which is produced by the method for producing low-oxygen vanadium aluminum carbide max described above, and has an oxygen content of 10 ppm to 8,000 ppm.

[0117] The present invention provides low-oxygen vanadium aluminum carbide max, which is produced by a method for producing low-oxygen vanadium aluminum carbide max and has an oxygen content of 10 ppm to 8,000 ppm.

[0118] The present invention provides low-oxygen vanadium aluminum carbide max, which is produced by the method described above for producing low-oxygen vanadium aluminum carbide max, and has an oxygen content of 10 ppm to 8,000 ppm. As a result, the low-oxygen vanadium aluminum carbide max has a low oxygen content, small particle size, and excellent physical properties, and can be used in various applications such as maxine precursors, raw materials for cemented carbide materials, catalysts, or semiconductor materials.

[0119] The present invention provides low-oxygen vanadium aluminum carbide max, manufactured by a method for producing low-oxygen vanadium aluminum carbide max, which has applications as a maxine precursor, a raw material for cemented carbide materials, a catalyst, or a semiconductor material.

[0120] The present invention will be described in more detail below with reference to examples. However, the following examples are provided to illustrate the present invention more concretely, and the scope of the present invention is not limited by these examples. The following examples may be modified or changed as appropriate by those skilled in the art within the scope of the present invention.

[0121] <Examples> <Examples 1-8> Production of Low-Oxygen Vanadium Aluminum Carbide Max A mixed powder was prepared by mixing vanadium oxide, aluminum compounds, and carbon compounds according to the components and content shown in Table 1 below.

[0122] Subsequently, the mixed powder was placed in a heat treatment apparatus, and Bulkmax was manufactured according to the sintering heat treatment conditions shown in Table 1 below.

[0123] Subsequently, the bulk max was crushed and pulverized using a crushing and pulverizing device to produce fine powder max with the particle sizes shown in Table 1 below.

[0124] Subsequently, the fine powder Max was subjected to a carbonization-reduction reaction heat treatment in a high-temperature synthesis furnace or a super Kanthal furnace, according to the carbonization-reduction reaction heat treatment conditions shown in Table 1 below, under an atmosphere of air, vacuum, nitrogen, or argon, using both an inert gas and hydrogen gas, to produce low-oxygen vanadium aluminum carbide Max with reduced oxygen content.

[0125] <Comparative Example> Production of Vanadium Carbide The comparative example vanadium carbide was produced in the same manner as in Example 1, except that the carbonization reduction reaction heat treatment was performed using both the inert gas and hydrogen gas as in Example 1.

[0126] [Table 1] JPEG2026509564000003.jpg102162

[0127] Referring to Table 1 above, the low-oxygen vanadium aluminum carbide max of Examples 1 to 4 had an oxygen content of 3400 ppm to 4200 ppm, which was significantly lower than the 12,000 ppm oxygen content of the vanadium carbide in the comparative example.

[0128] Here, it was shown that the low-oxygen vanadium aluminum carbide max of Examples 1 to 4 contains little oxygen.

[0129] Figure 4 is a graph showing the oxygen content of low-oxygen vanadium aluminum carbide max according to Examples 1 to 4 of the present invention.

[0130] Referring to Figure 4, it was confirmed that the low-oxygen vanadium aluminum carbide max of Examples 1 to 4 had an oxygen content of 3400 ppm to 4200 ppm.

[0131] While specific examples of the low-oxygen vanadium aluminum carbide max and the method for producing the same according to the present invention have been described so far, it is clear that various modifications are possible within the limits that do not deviate from the scope of the present invention.

[0132] Therefore, the scope of the present invention should not be limited to the embodiments described, but should be defined not only by the claims described later, but also by equivalent claims, etc.

[0133] In other words, the embodiments described above should be understood to be illustrative and not limiting, and the scope of the present invention is indicated by the claims described below rather than by the detailed description, and all modifications or variations conceived from the meaning and scope of those claims and their equivalent concepts should be interpreted as being included within the scope of the present invention. [Industrial applicability]

[0134] The present invention can be used in a method for producing vanadium aluminum carbide max.

Claims

1. Low-oxygen vanadium aluminum carbide max, vanadium; Aluminum; and, Composed of carbon, The low-oxygen vanadium aluminum carbide max is characterized by being formed using both an inert gas and hydrogen gas in the carbide reaction of vanadium and aluminum. Low-oxygen vanadium aluminum carbide max.

2. The aforementioned low-oxygen vanadium aluminum carbide max is After mixing vanadium oxide, aluminum compounds and carbon compounds, After the mixed powder is manufactured into BulkMax with larger particle sizes by sintering heat treatment, After the aforementioned bulkmax is crushed and pulverized to produce fine powder max, The fine powder Max is used together with the inert gas and hydrogen gas, and subjected to a carbonization-reduction heat treatment to form a product with reduced oxygen content. Low-oxygen vanadium aluminum carbide max as described in claim 1.

3. The oxygen content is characterized by being between 10 ppm and 8,000 ppm. Low-oxygen vanadium aluminum carbide max as described in claim 1.

4. The aforementioned low-oxygen vanadium aluminum carbide max is V ２ Characterized by having the chemical formula AlC, Low-oxygen vanadium aluminum carbide max as described in claim 1.

5. The molar ratio (B / A) of the aluminum compound (B) to the vanadium oxide (A) is 0.2 to 10. The molar ratio (C / A) of the carbon compound (C) to the vanadium oxide (A) is characterized by being 0.2 to 10. The low-oxygen vanadium aluminum carbide max according to claim 2.

6. The particle size of the mixed powder of the vanadium oxide, the aluminum compound, and the carbon compound is characterized by being 2 nm to 50 μm. The low-oxygen vanadium aluminum carbide max according to claim 2.

7. The vanadium oxide is at least one selected from vanadium pentoxide (V ２ O ５ ), sodium metavanadate (NaVO ３ ), vanadium trioxide (V ２ O ３ ), vanadium oxychloride (VOCl ３ ), and ammonium metavanadate (H ４ NVO ３ ). The low-oxygen vanadium aluminum carbide max according to claim 2.

8. The aforementioned aluminum compound is alumina (Al ２ O ３ ), aluminum hydroxide (Al(OH) ３ ), aluminum chloride (AlCl ３ ), aluminum fluoride (AlF ３ ), and aluminum sulfate (Al ２ (SO4) ３ It is characterized by being at least one of the following selected from: The low-oxygen vanadium aluminum carbide max according to claim 2.

9. The carbon compound is characterized by being at least one selected from industrial carbon powder, coke, coal, coal tar, activated carbon, natural graphite, artificial graphite, carbon black, acetylene black, Ketjen black, channel black, furnace black, lamp black, summer black, industrial diamond, and carbon fiber. The low-oxygen vanadium aluminum carbide max according to claim 2.

10. The inert gas and hydrogen gas are characterized in that their volume ratio is 10:1 to 1:

10. Low-oxygen vanadium aluminum carbide max as described in claim 1.

11. The sintering heat treatment temperature is 800°C to 1600°C. The sintering heat treatment time is characterized by being 10 minutes to 24 hours. The low-oxygen vanadium aluminum carbide max according to claim 2.

12. The particle size of the aforementioned Bulkmax is 50 nm to 100 μm. The particle size of the aforementioned fine powder Max is characterized by being 2 nm to 20 μm. The low-oxygen vanadium aluminum carbide max according to claim 2.

13. A method for producing low-oxygen vanadium aluminum carbide max, (a-1) A step of mixing vanadium oxide, aluminum compounds and carbon compounds to produce a mixed powder; (a-2) The step of manufacturing Bulkmax by heat-treating the mixed powder with sintering heat treatment; (a-3) The step of crushing and grinding the bulk max to produce fine powder max; and, (a-4) A step to produce low-oxygen vanadium aluminum carbide max by subjecting the fine powder max to a carbonization reduction heat treatment in a high-temperature synthesis furnace or superkanthal furnace under an atmosphere of air, vacuum, nitrogen, or argon, using both an inert gas and hydrogen gas to reduce the oxygen content. including, A method for producing low-oxygen vanadium aluminum carbide max.

14. In the step of (a-1) mixing vanadium oxide, an aluminum compound, and a carbon compound to produce a mixed powder, The mixing ratio of the vanadium oxide, the aluminum compound, and the carbon compound is characterized by being 1:0.2 to 0.7:0.1 to 0.5 by weight. A method for producing low-oxygen vanadium aluminum carbide max according to claim 13.

15. In the step of manufacturing Bulkmax by heat-treating the (a-2) mixed powder, The sintering heat treatment temperature is 800°C to 1600°C. The sintering heat treatment time is characterized by being 10 minutes to 24 hours. A method for producing low-oxygen vanadium aluminum carbide max according to claim 13.

16. In the step of crushing and pulverizing the Bulkmax (a-3) to produce a fine powder, The particle size of the aforementioned Bulkmax is 50 nm to 100 μm. The fine powder is characterized by having a particle size of 2 nm to 20 μm. A method for producing low-oxygen vanadium aluminum carbide max according to claim 13.

17. In the step of producing low-oxygen vanadium aluminum carbide max by subjecting the fine powder max described above (a-4) to a carbonization reduction heat treatment in a high-temperature synthesis furnace or superkanthal furnace under an atmosphere of air, vacuum, nitrogen, or argon, using both an inert gas and hydrogen gas, thereby reducing the oxygen content, The heat treatment temperature for the carbonization reduction reaction using both the inert gas and hydrogen gas is 500°C to 1100°C. The heat treatment time for the carbonization reduction reaction is characterized by being 10 minutes to 24 hours. A method for producing low-oxygen vanadium aluminum carbide max according to claim 13.

18. The uses of the low-oxygen vanadium aluminum carbide max described in any one of claims 1 to 12 are as a maxine precursor, a raw material for cemented carbide materials, a catalyst, or a semiconductor material. Low-oxygen vanadium aluminum carbide max.

19. The oxygen content of the oxygen produced by the method for producing low-oxygen vanadium aluminum carbide max according to any one of claims 13 to 17 is 10 ppm to 8,000 ppm. Low-oxygen vanadium aluminum carbide max.

20. The uses of the low-oxygen vanadium aluminum carbide max produced by the method for producing low-oxygen vanadium aluminum carbide max according to any one of claims 13 to 17 are as a maxine precursor, a raw material for cemented carbide materials, a catalyst, or a semiconductor material. Low-oxygen vanadium aluminum carbide max.

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