Low-oxygen vanadium aluminum carbide max and manufacturing method therefor

Abstract

The present invention provides low-oxygen vanadium aluminum carbide (V2AlC) MAX for producing high-purity vanadium MXene, and a manufacturing method therefor.

Description

Low-oxygen vanadium aluminum carbide max and its manufacturing method

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

[0002] Vanadium metal is a material that readily forms carbides, nitrides, or oxides due to its high affinity for non-metallic elements such as carbon, nitrogen, or oxygen.

[0003] Therefore, vanadium carbide, which is manufactured through the combination of vanadium and carbon, can be said to be a compound that can be easily manufactured, but due to the characteristic of vanadium having a high affinity for oxygen, it is not easy to synthesize pure carbide (with a low amount of oxygen).

[0004] That is, V(C x O 1-x ), it is not easy to manufacture vanadium carbide with a low oxygen content because the formation of oxycarbide in the form of x < 1 is easy.

[0005] Accordingly, the present applicant, through long-term, arduous efforts and various studies, has obtained a low-oxygen vanadium aluminum carbide max and a method for producing the same, which are formed with a reduced oxygen content by using an inert gas and hydrogen gas together in the carbonization reaction of vanadium and aluminum, thereby completing the present invention.

[0006] Accordingly, the purpose of the present invention is to provide a low-oxygen vanadium aluminum carbide max formed with a reduced oxygen content by using an inert gas and hydrogen gas together in the carbonization reaction of vanadium and aluminum.

[0007] In addition, an object of the present invention is to provide a method for producing low-oxygen vanadium aluminum carbide max formed with a reduced oxygen content by using an inert gas and hydrogen gas together in a carbonization reaction of vanadium and aluminum.

[0008] In addition, it is an object of the present invention to provide a use of low-oxygen vanadium aluminum carbide max formed with a reduced oxygen content by using an inert gas and hydrogen gas together in the carbonization reaction of vanadium and aluminum.

[0009] In addition, an object of the present invention is to provide a low-oxygen vanadium aluminum carbide max having an oxygen content of 10 ppm to 8,000 ppm, manufactured by the method for manufacturing the low-oxygen vanadium aluminum carbide max.

[0010] The problems to be solved by the present invention are not limited to the problems mentioned above, and other problems not mentioned will be clearly understood by those skilled in the art from the description below.

[0011] In order to solve the above problem, according to one aspect of the present invention,

[0012] As low-oxygen vanadium aluminum carbide max,

[0013] vanadium;

[0014] aluminum; and

[0015] It is composed of carbon,

[0016] The above low-oxygen vanadium aluminum carbide max is characterized in that it is formed by using an inert gas and hydrogen gas together in the carbonization reaction of the vanadium and the aluminum.

[0017] We offer low-oxygen vanadium aluminum carbide max.

[0018] According to one embodiment of the present invention, the low-oxygen vanadium aluminum carbide max

[0019] After mixing vanadium oxide, aluminum compound and carbon compound,

[0020] The mixed powder is then manufactured into a bulk max with large particle size through sintering heat treatment,

[0021] After the above bulk max is crushed and manufactured into fine powder max,

[0022] The fine powder Max can be formed by heat-treating the carbonization reduction reaction with the above inert gas and hydrogen gas to reduce the oxygen content.

[0023] According to one embodiment of the present invention, the oxygen content may be from 10 ppm to 8,000 ppm.

[0024] According to one embodiment of the present invention, the low-oxygen vanadium aluminum carbide max may have a chemical formula of V2AlC.

[0025] 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,

[0026] The molar ratio (C / A) of the carbon compound (C) to the vanadium oxide (A) may be 0.2 to 10.

[0027] According to one embodiment of the present invention, 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.

[0028] 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 (V2VO3), vanadium oxychloride (VOCl3), and ammonium metavanadate (H4NVO3).

[0029] 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).

[0030] According to one embodiment of the present invention, 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.

[0031] According to one embodiment of the present invention, the content of the inert gas and hydrogen gas may be 10:1 to 1:10 in volume ratio.

[0032] According to one embodiment of the present invention, the sintering heat treatment temperature is 800°C to 1600°C,

[0033] The sintering heat treatment time can be from 10 minutes to 24 hours.

[0034] According to one embodiment of the present invention, the particle size of the bulk max is 50 nm to 100 μm,

[0035] The particle size of the above fine powder may be 2 nm to 20 μm.

[0036]

[0037] In addition, according to another aspect of the present invention,

[0038] A method for manufacturing low-oxygen vanadium aluminum carbide max,

[0039] (a-1) A step of preparing a mixed powder by mixing vanadium oxide, aluminum compound and carbon compound;

[0040] (a-2) A step of manufacturing bulk max by sintering heat treatment of the above mixed powder;

[0041] (a-3) a step of crushing the bulk max to produce fine powder max; and

[0042] (a-4) A step of manufacturing low-oxygen vanadium aluminum carbide max by subjecting the above fine powder max to a carbonization reduction heat treatment using an inert gas and hydrogen gas together under an atmosphere of air, vacuum, nitrogen or argon in a high-temperature synthesis furnace or supercandal furnace, thereby reducing the oxygen content.

[0043] A method for manufacturing low-oxygen vanadium aluminum carbide max is provided.

[0044] According to one embodiment of the present invention, in the step of preparing a mixed powder by mixing vanadium oxide, aluminum compound and carbon compound (a-1),

[0045] The mixing ratio of the above vanadium oxide, the above aluminum compound and the above carbon compound may be 1:0.2 to 0.7:0.1 to 0.5 by weight.

[0046] According to one embodiment of the present invention, in the step of manufacturing bulk max by sintering heat treatment of the above (a-2) mixed powder,

[0047] The sintering heat treatment temperature is 800 ℃ to 1600 ℃,

[0048] The sintering heat treatment time can be from 10 minutes to 24 hours.

[0049] According to one embodiment of the present invention, in the step of crushing and finely powdering the bulk max (a-3),

[0050] The particle size of the above bulk max is 50 nm to 100 ㎛,

[0051] The particle size of the above fine powder may be 2 nm to 20 μm.

[0052] According to one embodiment of the present invention, in the step of manufacturing low-oxygen vanadium aluminum carbide max by performing a carbonization-reduction heat treatment on the (a-4) fine powder max in a high-temperature synthesis furnace or supercandal furnace using an inert gas and hydrogen gas together under an atmosphere of air, vacuum, nitrogen or argon,

[0053] The temperature of the heat treatment for the carbonization reduction reaction using the above inert gas and hydrogen gas together is 500°C to 1100°C,

[0054] The carbonization reduction reaction heat treatment time can be from 10 minutes to 24 hours.

[0055]

[0056] In addition, according to another aspect of the present invention,

[0057] The present invention provides low-oxygen vanadium aluminum carbide max, which is used as a maxene precursor, a raw material for superalloy materials, a catalyst, or a semiconductor material.

[0058]

[0059] In addition, according to another aspect of the present invention,

[0060] A low-oxygen vanadium aluminum carbide max having an oxygen content of 10 ppm to 8,000 ppm is provided, manufactured by the above method for manufacturing low-oxygen vanadium aluminum carbide max.

[0061]

[0062] In addition, according to another aspect of the present invention,

[0063] The use of the low-oxygen vanadium aluminum carbide max manufactured by the above method for manufacturing the low-oxygen vanadium aluminum carbide max provides the low-oxygen vanadium aluminum carbide max as a maxene precursor, a raw material for a superalloy material, a catalyst, or a semiconductor material.

[0064] According to the present invention, a low-oxygen vanadium aluminum carbide max is provided in which an inert gas and hydrogen gas are used together in a carbonization reaction of vanadium and aluminum to form a low-oxygen vanadium aluminum carbide max with a reduced oxygen content, so that the low-oxygen vanadium aluminum carbide max has a low oxygen content, a small particle size, excellent physical properties, and can be used for various purposes such as a MXene precursor, a raw material for a superalloy material, a catalyst, or a semiconductor material.

[0065] In addition, the present invention provides a method for producing low-oxygen vanadium aluminum carbide max formed with a reduced oxygen content by using an inert gas and hydrogen gas together in a carbonization reaction of vanadium and aluminum, so that the process stability is excellent and mass production is possible, making it economical.

[0066] In addition, the present invention provides low-oxygen vanadium aluminum carbide max having an oxygen content of 10 ppm to 8,000 ppm, manufactured by the method for manufacturing the low-oxygen vanadium aluminum carbide max, so that the low-oxygen vanadium aluminum carbide max has a low oxygen content, a small particle size, excellent physical properties, and can be used for various purposes such as a MXene precursor, a raw material for a superalloy material, a catalyst, or a semiconductor material.

[0067] The effects of the present invention are not limited to the effects described above, and should be understood to include all effects that can be inferred from the detailed description of the present invention or the composition of the invention described in the claims.

[0068] FIG. 1 is a schematic diagram of a method for manufacturing low-oxygen vanadium aluminum carbide max formed with a reduced oxygen content by using an inert gas and hydrogen gas together in a carbonization reaction of vanadium and aluminum according to one embodiment of the present invention.

[0069] Figure 2 is a process flow diagram of a method for manufacturing low-oxygen vanadium aluminum carbide max according to one embodiment of the present invention.

[0070] Figure 3 is a graph of the DSC analysis results and gas charging section of a 2V + Al + C mixture according to one embodiment of the present invention.

[0071] FIG. 4 is a graph showing the oxygen content of low-oxygen vanadium aluminum carbide max according to one embodiment of the present invention.

[0072] Hereinafter, a preferred embodiment according to the present invention will be described in detail with reference to the attached drawings.

[0073] The advantages and features of the present invention and the method for achieving them will become clear with reference to the embodiments described in detail below together with the attached drawings.

[0074] However, the present invention is not limited to the embodiments disclosed below, but may be implemented in various different forms, and these embodiments are provided only to make the disclosure of the present invention complete and to fully inform a person having ordinary skill in the art to which the present invention pertains of the scope of the invention, and the present invention is defined only by the scope of the claims.

[0075] In addition, when describing the present invention, if it is determined that related known technologies or the like may obscure the gist of the present invention, a detailed description thereof will be omitted.

[0076] Hereinafter, the present invention will be described in detail.

[0077]

[0078] Low-oxygen vanadium aluminum carbide max

[0079] The present invention provides a low-oxygen vanadium aluminum carbide max formed with a reduced oxygen content by using an inert gas and hydrogen gas together in a carbonization reaction of vanadium and aluminum.

[0080] The present invention is a low-oxygen vanadium aluminum carbide max,

[0081] vanadium;

[0082] aluminum; and

[0083] It is composed of carbon,

[0084] The above low-oxygen vanadium aluminum carbide max is formed by using an inert gas and hydrogen gas together in a carbonization reaction of the vanadium and the aluminum.

[0085] The present invention provides a low-oxygen vanadium aluminum carbide max formed with a reduced oxygen content by using an inert gas and hydrogen gas together in a carbonization reaction of vanadium and aluminum, so that the low-oxygen vanadium aluminum carbide max has a low oxygen content, a small particle size, excellent physical properties, and can be used for various purposes such as a MXene precursor, a raw material for a superalloy material, a catalyst, or a semiconductor material.

[0086]

[0087] Vanadium metal is a material that readily forms carbides, nitrides, or oxides due to its high affinity for non-metallic elements such as carbon, nitrogen, or oxygen.

[0088] Therefore, vanadium carbide, which is manufactured through the combination of vanadium and carbon, can be said to be a compound that can be easily manufactured, but due to the characteristic of vanadium having a high affinity for oxygen, it is not easy to synthesize pure carbide (with a low amount of oxygen).

[0089] That is, V(C x O 1-x ), it is not easy to manufacture vanadium carbide with a low oxygen content because the formation of oxycarbide in the form of x < 1 is easy.

[0090] Accordingly, the present applicant, through long-term, arduous efforts and various studies, has obtained a low-oxygen vanadium aluminum carbide max and a method for producing the same, which are formed with a reduced oxygen content by using an inert gas and hydrogen gas together in the carbonization reaction of vanadium and aluminum, thereby completing the present invention.

[0091]

[0092] In addition, the low-oxygen vanadium aluminum carbide max of the present invention

[0093] After mixing vanadium oxide, aluminum compound and carbon compound,

[0094] The mixed powder is then manufactured into a bulk max with large particle size through sintering heat treatment,

[0095] After the above bulk max is crushed and manufactured into fine powder max,

[0096] The fine powder Max can be formed by heat-treating the carbonization reduction reaction with the above inert gas and hydrogen gas to reduce the oxygen content.

[0097] At this time, the oxygen content may be 10 ppm to 8,000 ppm.

[0098] Here, if the content of oxygen is within the above range, V(C) with a high oxygen content x O 1-x ) may not be easily formed in the form of carbonates.

[0099] At this time, the oxygen content may preferably be 30 ppm to 8,000 ppm, and more preferably 100 ppm to 7,000 ppm.

[0100] And, the above low-oxygen vanadium aluminum carbide max may have a chemical formula of V2AlC.

[0101] In addition, the molar ratio (B / A) of the aluminum compound (B) to the vanadium oxide (A) may be 0.2 to 10,

[0102] The molar ratio (C / A) of the carbon compound (C) to the vanadium oxide (A) may be 0.2 to 10.

[0103] 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 is V(C) with a high oxygen content. x O 1-x ) may not be easily formed in the form of carbonates.

[0104] 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.

[0105] In addition, 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 is V(C) with a high oxygen content. x O 1-x ) may not be easily formed in the form of carbonates.

[0106] 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.

[0107] 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.

[0108] 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, so that the carbon reduction reaction rate can increase.

[0109] At this time, the particle size of the mixed powder of the vanadium oxide, the aluminum oxide, and the carbon compound may preferably be 2 nm to 48 μm, and more preferably 2 nm to 45 μm.

[0110] Additionally, the vanadium oxide may be at least one selected from vanadium pentoxide (V2O5), sodium metavanadate (NaVO3), vanadium trioxide (V2VO3), vanadium oxychloride (VOCl3), and ammonium metavanadate (H4NVO3).

[0111] And, 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).

[0112] Additionally, 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.

[0113] Here, the carbon compound may further include biomass selected from at least one of coffee grounds, fallen leaves, and waste wood.

[0114] At this time, the carbon compound may further include a reducing gas containing carbon, at least one selected from carbon monoxide, methane, and hydrocarbons.

[0115] Here, when vanadium (V) and aluminum (Al) are used as raw materials for synthesizing vanadium carbide, vanadium carbide is formed as shown in the following chemical formula 1 through the reaction of vanadium and aluminum with carbon, i.e., carbon reduction.

[0116]

[0117] 2V(s) + Al(l) + C(s) → V2AlC(s) ----- (Chemical Formula 1)

[0118]

[0119] In this process, theoretically, if the amount of carbon is adjusted to less than 1 mole for 2 moles of vanadium, low-oxygen vanadium aluminum carbide Max in the form of V2AlC can be synthesized.

[0120] However, in the actual process, if the amount of carbon that acts as a reducing agent is lowered, the reaction rate for reduction decreases, and V(C) with a high amount of oxygen x O1-x ) form of carbonates are easily formed.

[0121] In addition, in order to form vanadium carbide, treatment is required to increase the speed of the carbon reduction reaction as well as adjust the carbon amount.

[0122] In the present invention, the particle size of the mixed powder of vanadium oxide, alumina and carbon as raw materials was reduced to the above range through a pulverization process to increase the reaction rate, and then an inert gas and hydrogen gas were added thereto and heat-treated to perform a carbonization reduction reaction, thereby synthesizing low-oxygen vanadium aluminum carbide max with a reduced oxygen content.

[0123]

[0124] Additionally, the content of the above inert gas and hydrogen gas may be 10:1 to 1:10 in volume ratio.

[0125] Here, when the contents of the above inert gas and hydrogen gas are within the above range, a low-oxygen vanadium aluminum carbide max with a reduced oxygen content can be synthesized.

[0126] At this time, the content of the inert gas and hydrogen gas may preferably be 10:2 to 2:10 by volume ratio, and more preferably 10:3 to 3:10 by volume ratio.

[0127] And, the sintering heat treatment temperature is 800 ℃ to 1600 ℃,

[0128] The sintering heat treatment time can be from 10 minutes to 24 hours.

[0129] In addition, the particle size of the bulk max is 50 nm to 100 ㎛,

[0130] The particle size of the above fine powder max can be 2 nm to 20 μm.

[0131] Here, when the sintering heat treatment temperature is within the above range, the particle size of the bulk max may be 50 nm to 100 μm.

[0132] At this time, the sintering heat treatment temperature may preferably be 850°C to 1600°C, and more preferably 900°C to 1600°C.

[0133] And, when the sintering heat treatment time is within the above range, the particle size of the bulk max can be 50 nm to 100 μm.

[0134] At this time, the sintering heat treatment time may preferably be 20 minutes to 24 hours, and more preferably 30 minutes to 24 hours.

[0135] In addition, the above carbon reduction reaction can be used together with an inert gas and hydrogen gas to produce low-oxygen vanadium aluminum carbide max.

[0136]

[0137] Method for manufacturing low-oxygen vanadium aluminum carbide max

[0138] The present invention provides a method for producing low-oxygen vanadium aluminum carbide max formed with a reduced oxygen content by using an inert gas and hydrogen gas together in a carbonization reaction of vanadium and aluminum.

[0139] The present invention relates to a method for manufacturing low-oxygen vanadium aluminum carbide max,

[0140] (a-1) A step of preparing a mixed powder by mixing vanadium oxide, aluminum compound and carbon compound;

[0141] (a-2) A step of manufacturing bulk max by sintering heat treatment of the above mixed powder;

[0142] (a-3) a step of crushing the bulk max to produce fine powder max; and

[0143] (a-4) A step of manufacturing low-oxygen vanadium aluminum carbide max by subjecting the above fine powder max to a carbonization reduction heat treatment using an inert gas and hydrogen gas together under an atmosphere of air, vacuum, nitrogen or argon in a high-temperature synthesis furnace or super-candal furnace to reduce the oxygen content.

[0144] The present invention provides a method for manufacturing low-oxygen vanadium aluminum carbide max formed with a reduced oxygen content by using an inert gas and hydrogen gas together in a carbonization reaction of vanadium and aluminum, so that the process stability is excellent and mass production is possible, making it economical.

[0145]

[0146] In addition, in the step of manufacturing a mixed powder by mixing the above (a-1) vanadium oxide, aluminum compound and carbon compound,

[0147] The mixing ratio of the above vanadium oxide, the above aluminum compound and the above carbon compound may be 1:0.2 to 0.7:0.1 to 0.5 by weight.

[0148] Here, when the mixing ratio of the vanadium oxide, the aluminum compound and the carbon compound is within the above range by weight ratio, V(C) with a large amount of oxygen x O 1-x ) may not be easily formed in the form of carbonates.

[0149] At this time, 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.

[0150] And, in the step of manufacturing bulk max by sintering heat treatment of the above (a-2) mixed powder,

[0151] The sintering heat treatment temperature is 800 ℃ to 1600 ℃,

[0152] The sintering heat treatment time can be from 10 minutes to 24 hours.

[0153] In addition, in the step of crushing and finely powdering the above (a-3) bulk max,

[0154] The particle size of the above bulk max is 50 nm to 100 ㎛,

[0155] The particle size of the above fine powder may be 2 nm to 20 μm.

[0156] Here, when the sintering heat treatment temperature is within the above range, the particle size of the bulk max may be 50 nm to 100 μm.

[0157] At this time, the sintering heat treatment temperature may preferably be 850°C to 1600°C, and more preferably 900°C to 1600°C.

[0158] And, when the sintering heat treatment time is within the above range, the particle size of the bulk max can be 50 nm to 100 μm.

[0159] At this time, the sintering heat treatment time may preferably be 20 minutes to 24 hours, and more preferably 30 minutes to 24 hours.

[0160] In addition, in the step of manufacturing low-oxygen vanadium aluminum carbide max by reducing the oxygen content by heat-treating the above (a-4) fine powder max by carbonization reduction reaction using inert gas and hydrogen gas together under an atmosphere of air, vacuum, nitrogen or argon in a high-temperature synthesis furnace or supercandal furnace,

[0161] The temperature of the heat treatment for the carbonization reduction reaction using the above inert gas and hydrogen gas together is 500°C to 1100°C,

[0162] The carbonization reduction reaction heat treatment time can be from 10 minutes to 24 hours.

[0163] Here, the above carbonization reduction heat treatment may be a process of heat treating the fine powder max using an inert gas and hydrogen gas together in an atmosphere of air, vacuum, nitrogen or argon in a high-temperature synthesis furnace or supercandal furnace.

[0164] Here, when the temperature of the carbonization reduction reaction heat treatment using the above inert gas and hydrogen gas together is within the above range, the low-oxygen characteristics and manufacturing efficiency of the low-oxygen vanadium aluminum carbide max can be excellent.

[0165] At this time, the temperature of the carbonization reduction reaction heat treatment using the inert gas and hydrogen gas together may be preferably 550°C to 1050°C, and more preferably 600°C to 1000°C.

[0166] In addition, when the heat treatment time for the carbonization reduction reaction using the above-mentioned inert gas and hydrogen gas together is within the above range, the low-oxygen characteristics and manufacturing efficiency of the low-oxygen vanadium aluminum carbide max can be excellent.

[0167] At this time, the heat treatment time for the carbonization reduction reaction using the inert gas and hydrogen gas together may be preferably 20 minutes to 24 hours, and more preferably 30 minutes to 24 hours.

[0168]

[0169] FIG. 1 is a schematic diagram of a method for manufacturing low-oxygen vanadium aluminum carbide max formed with a reduced oxygen content by using an inert gas and hydrogen gas together in a carbonization reaction of vanadium and aluminum according to one embodiment of the present invention.

[0170] Referring to Figure 1, a mixed powder is prepared by mixing (blending) vanadium oxide, aluminum compound, and carbon compound.

[0171] Afterwards, the above mixed powder is sintered and heat treated to manufacture bulk max.

[0172] Then, the bulk max is pulverized to produce fine powder max.

[0173] Afterwards, the fine powder Max is subjected to a carbonization reduction heat treatment using an inert gas and hydrogen gas together in an atmosphere of air, vacuum, nitrogen or argon in a high-temperature synthesis furnace or supercandal furnace to produce low-oxygen vanadium aluminum carbide Max with reduced oxygen content.

[0174] Then, when the oxygen content analyzed in the above low-oxygen vanadium aluminum carbide max becomes 0.8 wt% or less, maxine is manufactured.

[0175] Here, if the oxygen content analyzed in the low-oxygen vanadium aluminum carbide max exceeds 0.8 wt%, the vanadium aluminum carbide max is returned to the mixed powder manufacturing process, and then low-oxygen vanadium aluminum carbide max is manufactured again.

[0176]

[0177] Figure 2 is a process flow diagram of a method for manufacturing low-oxygen vanadium aluminum carbide max according to one embodiment of the present invention.

[0178] Referring to Fig. 2, first, a mixed powder is prepared by mixing vanadium oxide, aluminum compound, and carbon compound (S110).

[0179] After that, the above mixed powder is sintered and heat treated to manufacture bulk max (S120).

[0180] Then, the bulk max is pulverized to produce fine powder max (S130).

[0181] Afterwards, the fine powder Max is subjected to a carbonization reduction heat treatment using an inert gas and hydrogen gas together in an atmosphere of air, vacuum, nitrogen or argon in a high-temperature synthesis furnace or supercandal furnace to produce low-oxygen vanadium aluminum carbide Max with reduced oxygen content (S140).

[0182]

[0183] Figure 3 is a graph of the DSC analysis results and gas charging section of a 2V + Al + C mixture according to one embodiment of the present invention.

[0184] Referring to Figure 3, the 600-1000°C region, where the most reaction occurs, is selected as the hydrogen reduction gas injection region. By injecting hydrogen, which can rapidly reduce oxygen, into this reaction region, the oxygen content of the final V2AlC Max can be reduced.

[0185]

[0186] Applications of Low-Oxygen Vanadium Aluminum Carbide Max

[0187] The present invention provides a use of low-oxygen vanadium aluminum carbide max formed with a reduced oxygen content by using an inert gas and hydrogen gas together in a carbonization reaction of vanadium and aluminum.

[0188] The present invention can provide a low-oxygen vanadium aluminum carbide max, the use of which is a maxene precursor, a raw material for a superalloy material, a catalyst, or a semiconductor material.

[0189]

[0190] Low-oxygen vanadium aluminum carbide max with an oxygen content of 10 ppm to 8,000 ppm

[0191] The present invention provides a low-oxygen vanadium aluminum carbide max having an oxygen content of 10 ppm to 8,000 ppm, manufactured by the above method for manufacturing low-oxygen vanadium aluminum carbide max.

[0192] The present invention provides a low-oxygen vanadium aluminum carbide max having an oxygen content of 10 ppm to 8,000 ppm, manufactured by a method for manufacturing low-oxygen vanadium aluminum carbide max.

[0193] The present invention provides low-oxygen vanadium aluminum carbide max having an oxygen content of 10 ppm to 8,000 ppm, manufactured by the method for manufacturing the low-oxygen vanadium aluminum carbide max, so that the low-oxygen vanadium aluminum carbide max has a low oxygen content, a small particle size, excellent physical properties, and can be used for various purposes such as a MXene precursor, a raw material for a superalloy material, a catalyst, or a semiconductor material.

[0194] The present invention provides a low-oxygen vanadium aluminum carbide max manufactured by a method for manufacturing low-oxygen vanadium aluminum carbide max, and uses the low-oxygen vanadium aluminum carbide max as a maxene precursor, a raw material for a superalloy material, a catalyst, or a semiconductor material.

[0195]

[0196] Hereinafter, the present invention will be described in more detail through examples. However, the following examples are intended to further illustrate the present invention, and the scope of the present invention is not limited by these examples. Those skilled in the art may appropriately modify or alter the following examples within the scope of the present invention.

[0197]

[0198] <Example>

[0199] <Examples 1 to 8> Manufacturing of low-oxygen vanadium aluminum carbide max

[0200] A mixed powder was prepared by mixing vanadium oxide, aluminum compound, and carbon compound with the ingredients and contents shown in Table 1 below.

[0201] Afterwards, the above mixed powder was put into a heat treatment device and bulk max was manufactured through the sintering heat treatment conditions shown in Table 1 below.

[0202] Then, the bulk max was pulverized in a pulverizer to produce fine powder max having particle sizes shown in Table 1 below.

[0203] Afterwards, the above fine powder Max was subjected to a carbonization-reduction heat treatment using an inert gas and hydrogen gas together under an atmosphere of air, vacuum, nitrogen or argon in a high-temperature synthesis furnace or super-Kanda furnace under the carbonization-reduction heat treatment conditions shown in Table 1 below, thereby producing a low-oxygen vanadium aluminum carbide Max with a reduced oxygen content.

[0204]

[0205] <Comparative Example> Manufacture of vanadium carbide

[0206] Vanadium carbide of the comparative example was manufactured in the same manner as in Example 1, except that the carbonization-reduction heat treatment was performed using an inert gas and hydrogen gas together in Example 1.

[0207]

[0208] Example 1 Example 2 Example 3 Example 4 Example 5 Example 6 Example 7 Example 8 Comparative Example Vanadium oxide (A) Vanadium pentoxide (V2O5) Vanadium pentoxide (V2O5) Sodium metavanadate (NaVO3) Vanadium trioxide (V2VO3) Vanadium oxychloride (VOCl3) Ammonium metavanadate (H4NVO3) Vanadium pentoxide (V2O5) Vanadium pentoxide (V2O5) Vanadium pentoxide (V2O5) Aluminum Compound (B) Aluminum hydroxide (Al(OH)3) Aluminum hydroxide (Al(OH)3) Aluminum hydroxide (Al(OH)3) Aluminum fluoride (AlF3) Aluminum sulfate (Al2(SO4)3) Alumina (Al2O3) Aluminum chloride (AlCl3) Aluminum hydroxide (Al(OH)3) Carbon compound (C) Industrial carbon powder Industrial carbon powder Industrial carbon powder Industrial carbon powder Natural graphite Artificial Graphite coke coal industrial carbon powder A:B:C (weight ratio) 1:0.5:0.3 1:0.5:0.3 1:0.5:0.3 1:0.5:0.3 1:0.2:0.5 1:0.7:0.5 1:0.4:0.4 1:0.5:0.5 1:0.5:0.3 Average particle size of mixed powder 10 ㎛ 10 ㎛ 10 ㎛ 10 ㎛ 0.2 ㎛ 0.05 ㎛ 20 nm 30 ㎛ 10 ㎛ Bulk Max average particle size 35 ㎛ 35 ㎛ 35 ㎛ 3 ㎛ 0.1 ㎛ 50 nm 100 ㎛ 35 ㎛ Fine powder Maxine average particle size 5 ㎛ 5 ㎛ 5 ㎛ 5 ㎛ 0.1㎛50 nm10 nm20 ㎛5 ㎛Sintering heat treatment temperature (℃)10001000100010001100900140016001000Sintering heat treatment time1 hour1 hour1 hour1 hour3 hours6 hours10 minutes12 hours1 hourCarbonization reduction heat treatment reactor gas conditionVacuumVacuumVacuumVacuumAtmosphereNitrogenArgonVacuumCarbonization reduction reactorHigh temperature synthesis furnaceHigh temperature synthesis furnaceHigh temperature synthesis furnaceHigh temperature synthesis furnaceHigh temperature synthesis furnaceSuper candal furnaceSuper candal furnaceSuper candal furnaceHigh temperature synthesis furnaceInert gas TypeArgonArgonArgonArgonNitrogenNitrogenNitrogenArgon-Inert gas:Hydrogen(cc)500:0400:100300:200200:300400:100300:200200:300250:250-Carbon reduction heat treatment temperature(℃)600~1000600~1000600~1000600~1000500~1100500~1100500~1100500~1100600~1000Carbon reduction heat treatment time3 hours3 hours3 hours3 hours10 minutes9 hours12 hours24 hours3 hoursOxygen content(ppm) of low-oxygen vanadium aluminum carbide max4200410038003400----12000.

[0209]

[0210] 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 oxygen content of 12,000 ppm of the vanadium carbide of the comparative example.

[0211] Here, the low-oxygen vanadium aluminum carbide max of Examples 1 to 4 was found to contain less oxygen.

[0212] FIG. 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.

[0213] Referring to FIG. 4, the low-oxygen vanadium aluminum carbide max of Examples 1 to 4 was confirmed to have an oxygen content of 3400 ppm to 4200 ppm.

[0214]

[0215] Although specific embodiments of the low-oxygen vanadium aluminum carbide max and the method for manufacturing the same according to the present invention have been described so far, it is obvious that various modifications are possible within the scope of the present invention.

[0216] Therefore, the scope of the present invention should not be limited to the described embodiments, but should be defined not only by the claims described below but also by equivalents of the claims.

[0217] That is, it should be understood that the above-described embodiments are exemplary in all respects and not restrictive, and the scope of the present invention is indicated by the claims to be described later rather than the detailed description, and all changes or modified forms derived from the meaning and scope of the claims and their equivalent concepts should be interpreted as being included in the scope of the present invention.

[0218] The present invention can be used in a method for manufacturing vanadium aluminum carbide max.

Claims

1. As low-oxygen vanadium aluminum carbide max, vanadium; aluminum; and It is composed of carbon, The above low-oxygen vanadium aluminum carbide max is characterized in that it is formed by using an inert gas and hydrogen gas together in the carbonization reaction of the vanadium and the aluminum. Low-oxygen vanadium aluminum carbide max.

2. In paragraph 1, The above low-oxygen vanadium aluminum carbide max is After mixing vanadium oxide, aluminum compound and carbon compound, The mixed powder is then manufactured into a bulk max with large particle size through sintering heat treatment, After the above bulk max is crushed and manufactured into fine powder max, The fine powder Max is characterized in that it is formed in a state in which the oxygen content is reduced by heat treatment through carbonization reduction reaction using the above inert gas and hydrogen gas. Low-oxygen vanadium aluminum carbide max.

3. In paragraph 1, The oxygen content is characterized by being 10 ppm to 8,000 ppm. Low-oxygen vanadium aluminum carbide max.

4. In paragraph 1, The above low-oxygen vanadium aluminum carbide max is characterized by having a chemical formula of V2AlC. Low-oxygen vanadium aluminum carbide max.

5. In paragraph 2, 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 in that it is 0.2 to 10. Low-oxygen vanadium aluminum carbide max.

6. In paragraph 2, The particle size of the mixed powder of the vanadium oxide, the aluminum oxide and the carbon compound is characterized in that it is 2 nm to 50 ㎛. Low-oxygen vanadium aluminum carbide max.

7. In paragraph 2, The above vanadium oxide is characterized in that at least one selected from vanadium pentoxide (V2O5), sodium metavanadate (NaVO3), vanadium trioxide (V2VO3), vanadium oxychloride (VOCl3), and ammonium metavanadate (H4NVO3). Low-oxygen vanadium aluminum carbide max.

8. In paragraph 2, The above aluminum compound is characterized in that it is at least one selected from alumina (Al2O3), aluminum hydroxide (Al(OH)3), aluminum chloride (AlCl3), aluminum fluoride (AlF3), and aluminum sulfate (Al2(SO4)3). Low-oxygen vanadium aluminum carbide max.

9. In paragraph 2, The carbon compound is characterized in that it is 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. Low-oxygen vanadium aluminum carbide max.

10. In paragraph 1 or 2, The content of the above inert gas and hydrogen gas is characterized by a volume ratio of 10:1 to 1:

10. Low-oxygen vanadium aluminum carbide max.

11. In paragraph 2, The above sintering heat treatment temperature is 800 ℃ to 1600 ℃, The sintering heat treatment time is characterized by being 10 minutes to 24 hours. Low-oxygen vanadium aluminum carbide max.

12. In paragraph 2, The particle size of the above bulk max is 50 nm to 100 ㎛, The particle size of the above fine powder Max is characterized by being 2 nm to 20 ㎛. Low-oxygen vanadium aluminum carbide max.

13. A method for manufacturing low-oxygen vanadium aluminum carbide max, (a-1) A step of preparing a mixed powder by mixing vanadium oxide, aluminum compound and carbon compound; (a-2) A step of manufacturing bulk max by sintering heat treatment of the above mixed powder; (a-3) a step of crushing the bulk max to produce fine powder max; and (a-4) A step of manufacturing low-oxygen vanadium aluminum carbide max by subjecting the above fine powder max to a carbonization reduction heat treatment using an inert gas and hydrogen gas together under an atmosphere of air, vacuum, nitrogen or argon in a high-temperature synthesis furnace or supercandal furnace, thereby reducing the oxygen content. Method for manufacturing low-oxygen vanadium aluminum carbide max.

14. In paragraph 13, In the step of manufacturing a mixed powder by mixing vanadium oxide, aluminum compound and carbon compound (a-1), The mixing ratio of the vanadium oxide, the aluminum compound and the carbon compound is characterized in that it is 1:0.2 to 0.7:0.1 to 0.5 by weight. Method for manufacturing low-oxygen vanadium aluminum carbide max.

15. In paragraph 13, In the step of manufacturing bulk max by sintering heat treatment of the above (a-2) mixed powder, The sintering heat treatment temperature is 800 ℃ to 1600 ℃, The sintering heat treatment time is characterized by being 10 minutes to 24 hours. Method for manufacturing low-oxygen vanadium aluminum carbide max.

16. In paragraph 13, In the step of crushing and finely powdering the above (a-3) bulk max, The particle size of the above bulk max is 50 nm to 100 ㎛, The particle size of the above fine powder is characterized by being 2 nm to 20 ㎛. Method for manufacturing low-oxygen vanadium aluminum carbide max.

17. In paragraph 13, In the step of manufacturing low-oxygen vanadium aluminum carbide max by reducing the oxygen content by heat-treating the above (a-4) fine powder max by carbonization reduction reaction using inert gas and hydrogen gas together under an atmosphere of air, vacuum, nitrogen or argon in a high-temperature synthesis furnace or supercandal furnace, The temperature of the heat treatment for the carbonization reduction reaction using the above inert gas and hydrogen gas together is 500°C to 1100°C, The carbonization reduction reaction heat treatment time is characterized by being 10 minutes to 24 hours. Method for manufacturing low-oxygen vanadium aluminum carbide max.

18. Low-oxygen vanadium aluminum carbide max according to any one of claims 1 to 12, wherein the use of the low-oxygen vanadium aluminum carbide max is as a maxene precursor, a raw material for superalloy materials, a catalyst, or a semiconductor material.

19. Low-oxygen vanadium aluminum carbide max having an oxygen content of 10 ppm to 8,000 ppm, manufactured by a method for manufacturing low-oxygen vanadium aluminum carbide max according to any one of claims 13 to 17.

20. The use of the low-oxygen vanadium aluminum carbide max manufactured by the method for manufacturing low-oxygen vanadium aluminum carbide max according to any one of claims 13 to 17 is as a low-oxygen vanadium aluminum carbide max as a MAXEN precursor, a raw material for a superalloy material, a catalyst, or a semiconductor material.

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