MAX AND MXene USING VANIUM CARBIDE, AND METHOD FOR PREPARING SAME
By using cheap vanadium carbides without expensive metal vanadium, MAX and MXene with low oxygen content, small particle size and excellent physical properties were prepared, which solved the problem of high preparation cost of vanadium MAX powder in the prior art, and realized economical and affordable preparation methods and wide application potential.
Patent Information
- Application Number
- CN202410844259.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Priority Date
- 2023-11-06
- Filing Date
- 2024-06-27
- Publication Date
- 2025-05-06
AI Technical Summary
In the prior art, the preparation cost of vanadium-based MAX powder is relatively high, mainly because the expensive metal vanadium is used, and the metal vanadium has a high affinity with the non-metal components, and carbides, nitrides or oxides are easily formed.
MAX and MXene were prepared by using inexpensive vanadium carbides without using metal vanadium. The specific method includes mixing the vanadium oxide and the carbon compound and performing high-energy grinding and vacuum heat treatment to form the vanadium carbide, and heat treatment with aluminum under an inactive gas to prepare MAX. MXene was then prepared by aluminum etching and interlayer peeling.
It has achieved MAX and MXene with low oxygen content, small particle size and excellent physical properties, reduced preparation costs, and expanded its application potential in the fields of MAX precursors, cemented carbides, catalysts or semiconductor materials.
Smart Images

Figure CN119929801A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to a MAX and MXene using cheap vanadium carbide instead of expensive metal vanadium and a preparation method thereof. Background Art
[0002] Generally, in the process of preparing vanadium-based MAX powder, vanadium-based MAX powder is prepared by reacting metal vanadium with aluminum and carbon. However, due to the high price of metal vanadium, the cost of preparing vanadium-based MAX powder is high, so it is difficult to apply in industry.
[0003] Furthermore, since metal vanadium has a high affinity with non-metallic components such as carbon, nitrogen, or oxygen, it is a substance that easily forms carbides, nitrides, or oxides.
[0004] Therefore, after a long period of hard work and various studies, the applicant has obtained MAX and MXene using inexpensive vanadium carbide instead of expensive metal vanadium and a preparation method thereof, thereby completing the present invention.
[0005] Prior art literature
[0006] Patent Literature
[0007] Korean Patent Publication No. 10-2017-0036507 (published on April 3, 2017) Summary of the invention
[0008] Technical issues
[0009] Therefore, an object of the present invention is to provide a MAX using inexpensive vanadium carbide instead of expensive metal vanadium.
[0010] Furthermore, an object of the present invention is to provide a MXene using inexpensive vanadium carbide instead of expensive metal vanadium.
[0011] Another object of the present invention is to provide a method for producing MAX using inexpensive vanadium carbide instead of expensive metallic vanadium.
[0012] Furthermore, an object of the present invention is to provide a method for preparing MXene using inexpensive vanadium carbide instead of expensive metallic vanadium.
[0013] The problems to be solved by the present invention are not limited to the above problems, and a person skilled in the art can clearly understand other problems not mentioned through the following description.
[0014] Technical Solution
[0015] In order to solve the above problems, according to one aspect of the present invention, there is provided a MAX using vanadium carbide, which is composed of vanadium, aluminum and carbon of vanadium carbide and is used as a raw material of a two-dimensional nanomaterial MXene, and is selected from at least one of the compounds shown in the following chemical formulas 1 to 3:
[0016] Chemical formula 1: V2AlC,
[0017] Chemical formula 2: V4AlC3,
[0018] Chemical formula 3: V 12 Al3C8.
[0019] According to an embodiment of the present invention, the MAX using vanadium carbide may be formed by heat treating a mixture of vanadium carbide and aluminum under an inert gas.
[0020] According to an embodiment of the present invention, the vanadium carbide may be formed by pulverizing vanadium oxide and carbon compound and then heat treating the mixture of vanadium oxide and carbon compound under vacuum and normal pressure.
[0021] According to an embodiment of the present invention, the molar ratio of vanadium to carbon in the vanadium carbide may be vanadium:carbon=2:1, 3:2 or 4:3.
[0022] According to an embodiment of the present invention, the MAX using vanadium carbide may exclude the use of metallic vanadium.
[0023] According to an embodiment of the present invention, the carbon content of the MAX using vanadium carbide may be 8-14 weight percent.
[0024] According to an embodiment of the present invention, the oxygen content of the MAX using vanadium carbide may be 1000-5000 ppm.
[0025] According to another aspect of the present invention, there is provided a MXene using vanadium carbide, which is a two-dimensional nanomaterial formed by performing aluminum etching and interlayer exfoliation on the above-mentioned MAX using vanadium carbide.
[0026] According to an embodiment of the present invention, the MXene using vanadium carbide may be selected from at least one of the compounds shown in the following Chemical Formulas 4 to 6.
[0027] Chemical formula 4: V2C
[0028] Chemical formula 5: V4C3
[0029] Chemical formula 6: V3C2
[0030] According to an embodiment of the present invention, the carbon content of the MXene using vanadium carbide may be 10.5-15 weight percent.
[0031] Furthermore, according to another aspect of the present invention, a method for preparing MAX is provided, the method comprising:
[0032] Step (a-1), mixing vanadium oxide and carbon compound to form mixed powder, then performing high-energy grinding using a high-energy grinding device to refine the particle size, and performing carbiding reduction reaction by vacuum heat treatment to prepare vanadium carbide; and
[0033] Step (a-2) is to mix the vanadium carbide and aluminum and perform heat treatment under an inert gas to prepare MAX using vanadium carbide.
[0034] According to an embodiment of the present invention, the particle size of the mixed powder of the vanadium oxide or the carbon compound may be 2 nm to 50 μm.
[0035] According to one embodiment of the present invention, the mixed powder of the vanadium oxide and the carbon compound can be placed together with steel balls in a rotating container in a high-energy grinding device, and then the high-energy grinding can be performed in an atmosphere of air, vacuum, nitrogen or argon. In the carbiding-reduction reaction, the vanadium oxide and the carbon compound can be micronized by the high-energy grinding to increase the contact area and increase the carbiding-reduction reaction rate.
[0036] Furthermore, according to another aspect of the present invention, a method for preparing MXene may be provided, the method comprising:
[0037] Step (b-1), mixing vanadium oxide and carbon compound to form a mixed powder, then performing high-energy grinding using a high-energy grinding device to refine the particle size, and performing a carburization reduction reaction by vacuum heat treatment to prepare vanadium carbide;
[0038] Step (b-2), mixing the vanadium carbide and aluminum, and heat treating the mixture under an inert gas to prepare MAX using vanadium carbide; and
[0039] Step (b-3), preparing MXene using vanadium carbide by performing aluminum etching and interlayer exfoliation on the above-mentioned MAX using vanadium carbide.
[0040] According to one embodiment of the present invention, in the above step (b-1) of mixing vanadium oxide and carbon compound to form a mixed powder, then using a high-energy grinding device to perform the above-mentioned high-energy grinding to refine the particle size, and performing a carburization reduction reaction through vacuum heat treatment to prepare vanadium carbide, the mixing ratio of the above-mentioned vanadium oxide and the above-mentioned carbon compound can be a weight ratio of 1:0.3 to 1:0.5.
[0041] According to one embodiment of the present invention, in the above step (b-1) of mixing vanadium oxide and carbon compound to form a mixed powder, then using a high-energy grinding device to perform the above-mentioned high-energy grinding to refine the particle size, and performing a carburization reduction reaction through vacuum heat treatment to prepare vanadium carbide, the steel ball of the above-mentioned high-energy grinding device can be at least one selected from ceramic balls, metal balls and cemented carbide balls.
[0042] According to one embodiment of the present invention, in the above step (b-1) of mixing vanadium oxide and carbon compound to form a mixed powder, then using a high-energy grinding device to perform the above-mentioned high-energy grinding to refine the particle size, and performing a carburization reduction reaction through vacuum heat treatment to prepare vanadium carbide, the heat treatment temperature of the above-mentioned vacuum heat treatment can be 1200°C to 1600°C, and the heat treatment time can be 1 hour to 5 hours.
[0043] According to one embodiment of the present invention, vanadium oxide and carbon compound are mixed to form a mixed powder, and then a high-energy grinding device is used to perform the above-mentioned high-energy grinding to refine the particle size, and a carburization reduction reaction is performed by vacuum heat treatment to prepare the above-mentioned step (b-1) of vanadium carbide. The rotating shaft of the above-mentioned high-energy grinding device rotates at 150-250rpm, and the above-mentioned rotating container rotates at 300-500rpm in a direction opposite to the rotation direction of the above-mentioned rotating shaft, and high-energy grinding can be performed for 1 to 20 hours.
[0044] According to one embodiment of the present invention, in the above step (b-2) of mixing vanadium carbide and aluminum and performing heat treatment under an inert gas to prepare MAX using vanadium carbide, the heat treatment temperature can be 1200° C. to 1600° C., and the heat treatment time can be 1 hour to 5 hours.
[0045] According to an embodiment of the present invention, the high energy grinding device may be a planetary ball mill, a spex ball mill or a grinding mill.
[0046] According to one embodiment of the present invention, in the above-mentioned step (b-3) of preparing MXene using vanadium carbide by performing aluminum etching and interlayer peeling on the above-mentioned MAX using vanadium carbide, the above-mentioned aluminum etching can be performed using one or more selected from hydrofluoric acid (HF), lithium fluoride (LiF), sodium fluoride (NaF), magnesium fluoride (MgF2), or a combination thereof, or a combination thereof with one or more of hydrochloric acid, sulfuric acid and nitric acid.
[0047] Effects of the Invention
[0048] According to the present invention, a MAX using inexpensive vanadium carbide instead of expensive metal vanadium is provided, so that the MAX using vanadium carbide has a low oxygen content, a small particle size, and excellent physical properties, and can be used for various purposes such as a MAX precursor, a raw material for a cemented carbide material, a catalyst, or a semiconductor material.
[0049] Furthermore, the present invention provides a MXene using inexpensive vanadium carbide instead of expensive metal vanadium, so that the MXene as a two-dimensional nanomaterial has excellent physical properties and can be used for various applications such as semiconductor materials, electronic materials, or catalysts.
[0050] Furthermore, the present invention provides a method for preparing MAX using inexpensive vanadium carbide instead of expensive metallic vanadium, thus having excellent process stability and being economical and affordable because it can be mass-produced.
[0051] Furthermore, the present invention provides a method for preparing MXene using inexpensive vanadium carbide instead of expensive metallic vanadium, thus having excellent process stability and being economical because it can be mass-produced.
[0052] The effects of the present invention are not limited to the above-mentioned effects, and should be understood to include all effects that can be inferred from the structure of the invention described in the detailed description of the present invention or the scope of claims of the invention. BRIEF DESCRIPTION OF THE DRAWINGS
[0053] Figure 1 FIG. 4 is a schematic diagram showing a process of using MAX and MXene of vanadium carbide according to an embodiment of the present invention.
[0054] Figure 2 FIG. 1 is a process flow chart showing a method for preparing MAX using vanadium carbide according to an embodiment of the present invention.
[0055] Figure 3 Schematic diagram showing a high energy grinding device in part (a), a rotating disk of the high energy grinding device in part (b), a vanadium carbide synthesis device in part (c), and a carburization reduction reaction in part (d) according to an embodiment of the present invention.
[0056] Figure 4 FIG. 4 is a process flow chart showing a method for preparing MXene using vanadium carbide according to an embodiment of the present invention.
[0057] Figure 5 FIG. 1 is a graph showing the carbon content in vanadium carbide according to an embodiment of the present invention as a function of carbon loading and heat treatment temperature.
[0058] Figure 6 FIG. 1 is a graph showing the oxygen content in vanadium carbide according to an embodiment of the present invention as a function of carbon loading and heat treatment temperature.
[0059] Figure 7 The V2AlC MAX powder (a) and the V2AlC MAX powder (b) are vanadium-based MAX powders according to an embodiment of the present invention. 12XRD pattern of Al3C8 MAX. DETAILED DESCRIPTION
[0060] Preferred embodiments of the present invention will be described in detail with reference to the following drawings.
[0061] By reference and attachment Figure 1 The advantages, features and methods of achieving the present invention will become clear from the embodiments described in detail below.
[0062] However, the present invention is not limited to the embodiments disclosed below and can be implemented in various forms that are different from each other. The present embodiments are only used to fully disclose the present invention and are provided in order to fully inform the scope of the invention to ordinary technicians in the field to which the present invention belongs. The present invention is only defined by the scope of the scope of protection claimed for the invention.
[0063] Furthermore, in the process of describing the present invention, when it is determined that related known technologies may obscure the gist of the present invention, the related detailed description will be omitted.
[0064] Hereinafter, the present invention will be described in detail.
[0065] MAX using vanadium carbide
[0066] The present invention provides a MAX that uses inexpensive vanadium carbide instead of expensive metallic vanadium.
[0067] The MAX using vanadium carbide of the present invention may be composed of vanadium, aluminum and carbon of vanadium carbide, and may be used as a raw material of a two-dimensional nanomaterial MXene, and may be selected from at least one of the compounds shown in the following chemical formulas 1 to 3:
[0068] Chemical formula 1: V2AlC,
[0069] Chemical formula 2: V4AlC3,
[0070] Chemical formula 3: V 12 Al3C8.
[0071] The present invention provides a MAX using inexpensive vanadium carbide instead of expensive metal vanadium. Therefore, the MAX using vanadium carbide has a low oxygen content, a small particle size, and excellent physical properties, and can be used for various purposes such as a MAX precursor, a raw material for a cemented carbide material, a catalyst, or a semiconductor material.
[0072] Generally, in the process of preparing vanadium-based MAX powder, vanadium-based MAX powder is prepared by reacting metal vanadium with aluminum and carbon. However, due to the high price of metal vanadium, the cost of preparing vanadium-based MAX powder is high, so it is difficult to apply in industry.
[0073] Furthermore, since metal vanadium has a high affinity with non-metallic components such as carbon, nitrogen, or oxygen, it is a substance that easily forms carbides, nitrides, or oxides.
[0074] Therefore, after a long period of hard work and various studies, the applicant has obtained MAX and MXene using inexpensive vanadium carbide instead of expensive metal vanadium and a preparation method thereof, thereby completing the present invention.
[0075] Among them, the present invention may be MAX using inexpensive vanadium carbide instead of expensive metal vanadium.
[0076] In this case, since metal vanadium has a high affinity with non-metallic components such as carbon, nitrogen, or oxygen, it is a substance that easily forms a carbide, a nitride, or an oxide.
[0077] The vanadium carbide of the present invention can be formed by mixing vanadium oxide and carbon compound, performing high energy grinding using a high energy grinding device to reduce the particle size, and performing a carburization reduction reaction by vacuum heat treatment.
[0078] That is, the MAX using vanadium carbide can be formed by heat-treating a mixture of vanadium carbide and aluminum under an inert gas.
[0079] In this case, the vanadium carbide can be formed by pulverizing vanadium oxide and carbon compound and then heat treating the mixture of vanadium oxide and carbon compound under vacuum and normal pressure.
[0080] Furthermore, the molar ratio of vanadium to carbon in the vanadium carbide may be vanadium:carbon=2:1, 3:2 or 4:3.
[0081] When the molar ratio of vanadium to carbon is the above ratio, the prepared MAX can have excellent physical properties because the vanadium carbide has excellent physical properties.
[0082] In particular, since the oxygen content of the MAX described above is low, the MAX can have excellent semiconductor characteristics.
[0083] In this case, the oxygen content may be 1000 to 5000 ppm.
[0084] When the oxygen content is within the above range, carbon oxides in the form of V(CxO1-x) having a large amount of oxygen may not be easily formed.
[0085] In this case, preferably, the oxygen content may be 1000 to 4980 ppm, and more preferably, may be 1000 to 4950 ppm.
[0086] Furthermore, the carbon content of the MAX using vanadium carbide may be 8 to 14 weight percent.
[0087] When the carbon content of the MAX using vanadium carbide is within the above range, the MAX using vanadium carbide may not easily form a MAX having a large amount of oxygen.
[0088] In this case, preferably, the carbon content of the MAX using vanadium carbide may be 8.2 to 13.8 weight percent, and more preferably, may be 8.5 to 13.5 weight percent.
[0089] Furthermore, the particle size of the mixed powder of the vanadium oxide or the carbon compound may be 2 nm to 50 μm.
[0090] When the particle size of the mixed powder of the vanadium oxide or the carbon compound is within the above range, the contact area between the vanadium oxide and the carbon compound increases, thereby increasing the carbonization reduction reaction rate.
[0091] In this case, preferably, the particle size of the mixed powder of the vanadium oxide or the carbon compound may be 2 nm to 48 μm, more preferably, may be 2 nm to 45 μm.
[0092] Furthermore, the MAX using vanadium carbide may be V2AlC, V 12 Al3C8 or V4AlC3.
[0093] The above V2AlC can be represented by the following reaction formula 1.
[0094] Reaction 1: 2VC 0.5 +Al→V2AlC
[0095] Furthermore, the above V 12 Al3C8 can be represented by the following reaction formula 2.
[0096] Reaction 2: 12VC 0.67 +3Al→V 12 Al3C8
[0097] Moreover, the above-mentioned V4AlC3 can be represented by the following reaction formula 3.
[0098] Reaction 3: 4VC 0.75 +Al→V4AlC3
[0099] The MAX using vanadium carbide mentioned above may exclude the use of metallic vanadium.
[0100] For example, when vanadium carbide having a molar ratio of vanadium to carbon of vanadium:carbon=2:1, 3:2, or 4:3 is used as a raw material, metallic vanadium can be excluded during the preparation of the vanadium-based MAX powder.
[0101] Furthermore, the vanadium oxide may be at least one selected from pentavanadium oxide (V2O5), sodium metavanadate (NaVO3), trivanadium oxide (V2VO3), chlorovanadium oxide (VOCl3) and ammonium metavanadate (H4NVO3).
[0102] Moreover, the above-mentioned carbon compound can be at least one selected from industrial carbon powder, coke, coal, coal tar, activated carbon, graphite, natural graphite, artificial graphite, carbon black, acetylene black, Ketjen black, channel black, furnace black, lamp black, pyrolytic black, industrial diamond and carbon fiber.
[0103] The carbon compound may also include at least one biomass selected from coffee grounds, fallen leaves and waste wood.
[0104] Furthermore, the carbon compound may further include at least one carbon-containing reducing gas selected from carbon monoxide, methane and hydrocarbons.
[0105] Moreover, the mixed powder of the above-mentioned vanadium oxide and carbon compound is placed together with steel balls in a rotating container in a high-energy grinding device, and then the above-mentioned high-energy grinding is carried out in an atmosphere of air, vacuum, nitrogen or argon. At this time, a high energy of 0.6J / g·s to 2.4J / g·s is input, the rotating shaft rotates at 150-250rpm, and the rotating container rotates at 300-500rpm in a direction opposite to the rotation direction of the above-mentioned rotating shaft, and high-energy grinding can be performed for 1 to 20 hours.
[0106] Furthermore, the high energy grinding device may be a planetary ball mill, a spex ball mill or a grinding mill.
[0107] The planetary ball mill can reduce the particle size of the mixed powder of the vanadium oxide and the carbon compound to the above range by placing steel balls together with the raw materials in a container and causing the container to rotate and revolve at high speed.
[0108] Furthermore, the SPEX ball mill can reduce the particle size of the mixed powder of the vanadium oxide and the carbon compound to the above range by placing steel balls together with the raw materials in a container and vibrating the container up and down and left and right at high speed.
[0109] Furthermore, the attritor may reduce the particle size of the mixed powder of the vanadium oxide and the carbon compound to the above range by placing steel balls and the raw materials in a container and transmitting energy through the rotational force of a rotor.
[0110] Furthermore, the high-energy grinding device can reduce the particle size of the mixed powder of the vanadium oxide and the carbon compound to the above-mentioned range by rotating the rotating container containing the mixed powder of the vanadium oxide and the carbon compound on the rotating disk in the opposite direction to the rotation direction of the rotating axis of the rotating disk.
[0111] Moreover, the heat treatment temperature of the above vacuum heat treatment can be 1200° C. to 1600° C., and the heat treatment time can be 1 hour to 5 hours.
[0112] Wherein, when the heat treatment temperature of the vacuum heat treatment is within the above range, the low-oxygen vanadium carbide can have excellent low-oxygen characteristics and preparation efficiency.
[0113] That is, the mixed powder of the vanadium oxide and the carbon compound produced by the high energy milling device can be subjected to vacuum heat treatment at the heat treatment temperature of the vacuum heat treatment to produce vanadium carbide having excellent low oxygen characteristics and production efficiency.
[0114] In this case, preferably, the heat treatment temperature of the vacuum heat treatment may be 1300°C to 1550°C, and more preferably, 1400°C to 1500°C.
[0115] Furthermore, when the heat treatment time of the vacuum heat treatment is within the above range, the vanadium carbide can have excellent low oxygen characteristics and preparation efficiency.
[0116] That is, the mixed powder of the vanadium oxide and the carbon compound produced by the high energy milling device may be subjected to vacuum heat treatment during the heat treatment time of the vacuum heat treatment to produce vanadium carbide having low oxygen characteristics and production efficiency.
[0117] In this case, preferably, the heat treatment time of the above vacuum heat treatment can be 2 hours to 4 hours, and more preferably, can be 2 hours to 3 hours.
[0118] Furthermore, the carburization reduction reaction can be performed by micronizing the vanadium oxide and the carbon compound through the high-energy milling to increase the contact area and the carburization reduction reaction rate.
[0119] Figure 1 FIG. 4 is a schematic diagram showing a process of using MAX and MXene of vanadium carbide according to an embodiment of the present invention.
[0120] refer to Figure 1 For example, vanadium oxide (V2O5) and graphite are mixed and ground in a high-energy grinding device to form a vanadium carbide (VC). x )powder.
[0121] Next, the above vanadium carbide (VC x ) powder and aluminum to prepare vanadium carbide-aluminum (VC x -Al) mixture.
[0122] Then, the vanadium carbide-aluminum (VC x The vanadium-aluminum-carbon carbide (V-Al-C) powder was prepared by heat treating a vanadium-aluminum-carbon carbide (V-Al-C) mixture.
[0123] Next, the vanadium-aluminum-carbon carbide (V-Al-C) powder was chemically etched to prepare MXene and its physical properties were evaluated.
[0124] Preparation method of MAX using vanadium carbide
[0125] The present invention provides a method for preparing MAX using inexpensive vanadium carbide instead of expensive metallic vanadium.
[0126] The method for preparing MAX using vanadium carbide of the present invention comprises:
[0127] Step (a-1), mixing vanadium oxide and carbon compound to form mixed powder, then performing high-energy grinding using a high-energy grinding device to refine the particle size, and performing carbiding reduction reaction by vacuum heat treatment to prepare vanadium carbide; and
[0128] Step (a-2) is to mix the vanadium carbide and aluminum and perform heat treatment under an inert gas to prepare MAX using vanadium carbide.
[0129] The present invention provides a method for preparing MAX using inexpensive vanadium carbide instead of expensive metallic vanadium, thus having excellent process stability and being economical and affordable because it can be produced on a large scale.
[0130] Furthermore, in the above step (a-1) of mixing vanadium oxide and carbon compound to form a mixed powder, then performing high-energy grinding using a high-energy grinding device to refine the particle size, and performing a carburization reduction reaction through vacuum heat treatment to prepare vanadium carbide, the mixing ratio of the above vanadium oxide and the above carbon compound can be 1:0.3 to 1:0.5 in terms of the weight ratio of vanadium oxide:carbon compound.
[0131] When the weight ratio of the vanadium oxide to the carbon compound is within the above range, it may not be easy to form V (C x O 1-x ) in the form of carbon oxides.
[0132] In this case, preferably, the mixing ratio of the above-mentioned vanadium oxide and the above-mentioned carbon compound can be 1:0.35 to 1:0.45 in terms of the weight ratio of vanadium oxide:carbon compound, and more preferably, the weight ratio of vanadium oxide:carbon compound can be 1:0.35 to 1:0.4.
[0133] Among them, the mixed powder of the above-mentioned vanadium oxide and carbon compound can be placed in a rotating container in a high-energy grinding device together with steel balls, and then the above-mentioned high-energy grinding is carried out in an atmosphere of air, vacuum, nitrogen or argon. In the above-mentioned carbide-reduction reaction, the above-mentioned vanadium oxide and carbon compound can be micronized by the above-mentioned high-energy grinding to increase the contact area and increase the carbide-reduction reaction rate.
[0134] Moreover, in the above step (a-1) of mixing vanadium oxide and carbon compound to form a mixed powder, then using a high-energy grinding device to perform high-energy grinding to refine the particle size, and performing a carburization reduction reaction through vacuum heat treatment to prepare vanadium carbide, the steel ball of the above high-energy grinding device can be at least one selected from ceramic balls, metal balls and cemented carbide balls.
[0135] Specifically, the material of the steel ball can be steel, tungsten or zirconium oxide.
[0136] The shape of the steel ball may be at least one selected from spherical, star-shaped, conical and cylindrical.
[0137] Furthermore, in the above step (a-1) of mixing vanadium oxide and carbon compound to form a mixed powder, then performing high-energy grinding using a high-energy grinding device to refine the particle size, and performing a carburization reduction reaction by vacuum heat treatment to prepare vanadium carbide, the rotating shaft of the above high-energy grinding device rotates at 150 to 250 rpm, and the above rotating container rotates at 300 to 500 rpm in a direction opposite to the rotation direction of the above rotating shaft, and high-energy grinding can be performed for 1 to 20 hours.
[0138] Among them, the above-mentioned high-energy grinding can be the following process: by making the rotation direction of the rotating axis and the rotating container opposite to each other, and rubbing the steel balls put into the above-mentioned rotating container with the mixed powder of the above-mentioned vanadium oxide and the above-mentioned carbon compound against each other for grinding, the particles of the mixed powder of the above-mentioned vanadium oxide and the above-mentioned carbon compound are crushed, so that the average particle size of the above-mentioned mixed powder is reduced to 2nm to 50μm.
[0139] Therefore, the particle size of the mixed powder of the vanadium oxide or the carbon compound may be 2 nm to 50 μm.
[0140] Furthermore, the high energy grinding device may be a planetary ball mill, a spex ball mill or a grinding mill.
[0141] The planetary ball mill may reduce the particle size of the mixed powder of the vanadium oxide and the carbon compound to the above range by placing steel balls together with the raw materials in a container and causing the container to rotate and revolve at high speed.
[0142] Furthermore, the SPEX ball mill can reduce the particle size of the mixed powder of the vanadium oxide and the carbon compound to the above range by placing steel balls together with the raw materials in a container and vibrating the container up and down and left and right at high speed.
[0143] Furthermore, the attritor may reduce the particle size of the mixed powder of the vanadium oxide and the carbon compound to the above range by placing steel balls and the raw materials in a container and transmitting energy through the rotational force of a rotor.
[0144] Furthermore, the high-energy grinding device can reduce the particle size of the mixed powder of the vanadium oxide and the carbon compound to the above-mentioned range by rotating the rotating container containing the mixed powder of the vanadium oxide and the carbon compound on the rotating disk in the opposite direction to the rotation direction of the rotating axis of the rotating disk.
[0145] Moreover, in the above step (a-1) of mixing vanadium oxide and carbon compound to form a mixed powder, then performing high-energy grinding using a high-energy grinding device to refine the particle size, and performing a carburization reduction reaction through vacuum heat treatment to prepare vanadium carbide, the heat treatment temperature of the above vacuum heat treatment can be 1200°C to 1600°C, and the heat treatment time can be 1 hour to 5 hours.
[0146] When the heat treatment temperature of the vacuum heat treatment is within the above range, the vanadium carbide can have excellent low oxygen characteristics and preparation efficiency.
[0147] That is, vanadium carbide having excellent low oxygen characteristics and production efficiency can be produced by vacuum heat treating the mixed powder of the vanadium oxide and the carbon compound produced by a high energy milling device at the heat treatment temperature of the vacuum heat treatment.
[0148] In this case, preferably, the heat treatment temperature of the vacuum heat treatment may be 1300°C to 1550°C, and more preferably, 1400°C to 1500°C.
[0149] Furthermore, when the heat treatment time of the vacuum heat treatment is within the above range, the vanadium carbide can have excellent low oxygen characteristics and preparation efficiency.
[0150] That is, the mixed powder of the vanadium oxide and the carbon compound produced by the high energy milling device may be subjected to vacuum heat treatment during the heat treatment time of the vacuum heat treatment to produce a product having low oxygen characteristics and production efficiency.
[0151] In this case, preferably, the heat treatment time of the above vacuum heat treatment can be 2 hours to 4 hours, and more preferably, can be 2 hours to 3 hours.
[0152] Furthermore, the carburization reduction reaction can be performed by micronizing the vanadium oxide and the carbon compound through the high-energy milling to increase the contact area and the carburization reduction reaction rate.
[0153] Furthermore, in the above step (a-2) of preparing MAX using vanadium carbide by mixing vanadium carbide and aluminum and performing heat treatment under an inert gas, the above inert gas may be argon, nitrogen or hydrogen.
[0154] Furthermore, the heat treatment temperature may be 1200° C. to 1600° C., and the heat treatment time may be 1 hour to 5 hours.
[0155] When the heat treatment temperature is within the above range, the MAX using vanadium carbide may have excellent low oxygen characteristics and preparation efficiency.
[0156] That is, MAX using vanadium carbide having excellent low oxygen characteristics and production efficiency can be produced by heat-treating the mixed powder of vanadium carbide and aluminum at the heat-treatment temperature.
[0157] In this case, preferably, the heat treatment temperature of the heat treatment may be 1300°C to 1550°C, and more preferably, may be 1400°C to 1500°C.
[0158] Also, when the heat treatment time is within the above range, the MAX using vanadium carbide may have excellent low oxygen characteristics and production efficiency.
[0159] That is, MAX using vanadium carbide having excellent low oxygen characteristics and production efficiency can be produced by heat-treating the mixed powder of the above-mentioned vanadium carbide and aluminum during the above-mentioned heat treatment time.
[0160] In this case, preferably, the heat treatment time of the heat treatment may be 2 hours to 4 hours, and more preferably, may be 2 hours to 3 hours.
[0161] Figure 2 FIG. 1 is a process flow chart showing a method for preparing MAX using vanadium carbide according to an embodiment of the present invention.
[0162] refer to Figure 2First, vanadium oxide and carbon compound are mixed to form a mixed powder, and then the high-energy grinding is performed using a high-energy grinding device to refine the particle size, and a carbonization reduction reaction is performed by vacuum heat treatment to prepare vanadium carbide (S110).
[0163] Then, the vanadium carbide and aluminum are mixed and heat-treated under an inert gas to prepare MAX using vanadium carbide ( S120 ).
[0164] Figure 3 Schematic diagram showing a high energy grinding device in part (a), a rotating disk of the high energy grinding device in part (b), a vanadium carbide synthesis device in part (c), and a carburization reduction reaction in part (d) according to an embodiment of the present invention.
[0165] Figure 3 Part a is an image of a high-energy grinding device for micronizing and mixing raw materials.
[0166] refer to Figure 3 In part b, the rotation direction of the main axis of the rotating disk of the above-mentioned high-energy grinding device is opposite to the rotation direction of the rotating container containing the mixed powder of the above-mentioned vanadium oxide and the above-mentioned carbon compound, and the particle size of the mixed powder of the above-mentioned vanadium oxide and the above-mentioned carbon compound can be reduced to 2nm to 50μm by this opposite direction rotational force.
[0167] refer to Figure 3 Part c is an image of a device for synthesizing vanadium carbide.
[0168] Figure 3 Part d is a schematic diagram of the carburization reduction reaction. The reaction formula of vanadium carbide prepared by the carburization reduction reaction of vanadium oxide and carbon compound is shown in the following reaction formula 4.
[0169] Reaction 4: VO a +(x+a)C→VC x +aCO
[0170] Furthermore, for example, when vanadium oxide (V2O5) is used as a raw material for synthesizing suboxygen vanadium carbide, vanadium carbide as shown in the following reaction formula 5 is formed by a reaction of the vanadium oxide with carbon, that is, by carbonization reduction.
[0171] Reaction 5: V2O5+(5+2x)C→2VC x +5CO
[0172] MXene using vanadium carbide
[0173] The present invention provides a MXene using inexpensive vanadium carbide instead of expensive metallic vanadium.
[0174] The present invention provides a MXene using vanadium carbide, which is a two-dimensional nanomaterial formed by aluminum etching and interlayer exfoliation of the above-mentioned MAX using vanadium carbide.
[0175] The present invention provides a MXene using inexpensive vanadium carbide instead of expensive metal vanadium, so that the MXene as a two-dimensional nanomaterial has excellent physical properties and can be used for various purposes such as semiconductor materials, electronic materials, or catalysts.
[0176] The MXene using vanadium carbide may be a two-dimensional nanomaterial formed by aluminum etching and interlayer exfoliation of the MAX using vanadium carbide.
[0177] Furthermore, the MXene using vanadium carbide may be a MXene using inexpensive vanadium carbide instead of expensive metal vanadium.
[0178] In this case, since metal vanadium has a high affinity with non-metallic components such as carbon, nitrogen, or oxygen, it is a substance that easily forms a carbide, a nitride, or an oxide.
[0179] The MXene using vanadium carbide of the present invention may be at least one selected from the compounds represented by the following Chemical Formulas 4 to 6.
[0180] Chemical formula 4: V2C
[0181] Chemical formula 5: V4C3
[0182] Chemical formula 6: V3C2
[0183] Furthermore, the carbon content of the MXene using vanadium carbide may be 10.5 to 15 weight percent.
[0184] When the carbon content of the MXene using vanadium carbide is within the above range, the MAX using vanadium carbide may not easily form a MXene having a large amount of oxygen.
[0185] In this case, preferably, the carbon content of the MXene using vanadium carbide may be 10.6 to 14.8 weight percent, and more preferably, may be 10.7 to 14.5 weight percent.
[0186] Furthermore, the oxygen content of the MXene using vanadium carbide may be 1000 to 5000 ppm.
[0187] When the oxygen content is within the above range, carbon oxides in the form of V(CxO1-x) having a large amount of oxygen may not be easily formed.
[0188] In this case, preferably, the oxygen content may be 1000 to 4980 ppm, and more preferably, may be 1000 to 4950 ppm.
[0189] Furthermore, the vanadium carbide can be formed by mixing vanadium oxide and a carbon compound, performing high-energy grinding using a high-energy grinding device to reduce the particle size, and performing a carburization reduction reaction by vacuum heat treatment.
[0190] Figure 1 FIG. 4 is a schematic diagram showing a process of using MAX and MXene of vanadium carbide according to an embodiment of the present invention.
[0191] Reference again Figure 1 For example, a vanadium oxide / graphite mixture (V2O5-C) in which vanadium oxide (V2O5) and graphite are mixed and ground in a high-energy grinding device is vacuum heat-treated to prepare vanadium carbide (VCx) powder.
[0192] Next, the vanadium carbide (VCx) powder and aluminum are mixed to prepare a vanadium carbide-aluminum (VCx-Al) mixture.
[0193] Then, vanadium-aluminum-carbon carbide (V-Al-C) powder was prepared by heat-treating the vanadium carbide-aluminum (VCx-Al) mixture under an argon atmosphere.
[0194] Next, MXene was prepared by chemically etching the above-mentioned vanadium-aluminum-carbon carbide (V-Al-C) powder and its physical properties were evaluated.
[0195] Preparation method of MXene using vanadium carbide
[0196] The present invention provides a method for preparing MXene using inexpensive vanadium carbide instead of expensive metallic vanadium.
[0197] The preparation method of MXene using vanadium carbide of the present invention comprises:
[0198] Step (b-1), mixing vanadium oxide and carbon compound to form a mixed powder, then performing high-energy grinding using a high-energy grinding device to refine the particle size, and performing a carburization reduction reaction by vacuum heat treatment to prepare vanadium carbide;
[0199] Step (b-2), mixing the vanadium carbide and aluminum, and heat treating the mixture under an inert gas to prepare MAX using vanadium carbide; and
[0200] Step (b-3), preparing MXene using vanadium carbide by performing aluminum etching and interlayer exfoliation on the above-mentioned MAX using vanadium carbide.
[0201] The present invention provides a method for preparing MXene using inexpensive vanadium carbide instead of expensive metallic vanadium, thus having excellent process stability and being economical because it can be mass-produced.
[0202] Furthermore, in the above step (b-1) of mixing vanadium oxide and carbon compound to form a mixed powder, then performing high-energy grinding using a high-energy grinding device to refine the particle size, and performing a carburization reduction reaction through vacuum heat treatment to prepare vanadium carbide, the mixing ratio of the above vanadium oxide and the above carbon compound can be 1:0.3 to 1:0.5 in terms of the weight ratio of vanadium oxide:carbon compound.
[0203] When the mixing ratio of the vanadium oxide to the carbon compound is within the above range in terms of weight ratio, carbon oxide in the form of V(CxO1-x) having a large amount of oxygen may not be easily formed.
[0204] In this case, preferably, the mixing ratio of the above-mentioned vanadium oxide and the above-mentioned carbon compound can be 1:0.35 to 1:0.45 in terms of the weight ratio of vanadium oxide:carbon compound, and more preferably, the weight ratio of vanadium oxide:carbon compound can be 1:0.35 to 1:0.4.
[0205] Moreover, in the above step (b-1) of mixing vanadium oxide and carbon compound to form a mixed powder, then using a high-energy grinding device to perform high-energy grinding to refine the particle size, and performing a carburization reduction reaction through vacuum heat treatment to prepare vanadium carbide, the steel ball of the above high-energy grinding device can be at least one selected from ceramic balls, metal balls and cemented carbide balls.
[0206] Specifically, the material of the steel ball can be steel, tungsten or zirconium oxide.
[0207] The shape of the steel ball may be at least one selected from spherical, star-shaped, conical and cylindrical.
[0208] Furthermore, in the above step (b-1) of mixing vanadium oxide and carbon compound to form a mixed powder, then performing high-energy grinding using a high-energy grinding device to refine the particle size, and performing a carburization reduction reaction by vacuum heat treatment to prepare vanadium carbide, the rotating shaft of the above high-energy grinding device rotates at 150 to 250 rpm, and the above rotating container rotates at 300 to 500 rpm in a direction opposite to the rotation direction of the above rotating shaft, and high-energy grinding can be performed for 1 to 20 hours.
[0209] Among them, the above-mentioned high-energy grinding can be the following process: by making the rotation direction of the rotating axis and the rotating container opposite to each other, and rubbing the steel balls put into the above-mentioned rotating container with the mixed powder of the above-mentioned vanadium oxide and the above-mentioned carbon compound against each other for grinding, the particles of the mixed powder of the above-mentioned vanadium oxide and the above-mentioned carbon compound are crushed, so that the average particle size of the above-mentioned mixed powder is reduced to 2nm to 50μm.
[0210] Therefore, the particle size of the mixed powder of the vanadium oxide or the carbon compound may be 2 nm to 50 μm.
[0211] Furthermore, the high energy grinding device may be a planetary ball mill, a spex ball mill or a grinding mill.
[0212] The planetary ball mill can reduce the particle size of the mixed powder of the vanadium oxide and the carbon compound to the above range by placing steel balls together with the raw materials in a container and causing the container to rotate and revolve at high speed.
[0213] Furthermore, the SPEX ball mill can reduce the particle size of the mixed powder of the vanadium oxide and the carbon compound to the above range by placing steel balls together with the raw materials in a container and vibrating the container up and down and left and right at high speed.
[0214] Furthermore, the attritor may reduce the particle size of the mixed powder of the vanadium oxide and the carbon compound to the above range by placing steel balls and the raw materials in a container and transmitting energy through the rotational force of a rotor.
[0215] Furthermore, the high-energy grinding device can reduce the particle size of the mixed powder of the vanadium oxide and the carbon compound to the above-mentioned range by rotating the rotating container containing the mixed powder of the vanadium oxide and the carbon compound on the rotating disk in the opposite direction to the rotation direction of the rotating axis of the rotating disk.
[0216] Moreover, in the above step (b-1) of mixing vanadium oxide and carbon compound to form a mixed powder, then performing high-energy grinding using a high-energy grinding device to refine the particle size, and performing a carburization reduction reaction through vacuum heat treatment to prepare vanadium carbide, the heat treatment temperature of the above vacuum heat treatment can be 1200°C to 1600°C, and the heat treatment time can be 1 hour to 5 hours.
[0217] When the heat treatment temperature of the vacuum heat treatment is within the above range, the vanadium carbide can have excellent low oxygen characteristics and preparation efficiency.
[0218] That is, vanadium carbide having excellent low oxygen characteristics and production efficiency can be produced by vacuum heat treating the mixed powder of the vanadium oxide and the carbon compound produced by a high energy milling device at the heat treatment temperature of the vacuum heat treatment.
[0219] In this case, preferably, the heat treatment temperature of the vacuum heat treatment may be 1300°C to 1550°C, and more preferably, 1400°C to 1500°C.
[0220] Furthermore, when the heat treatment time of the vacuum heat treatment is within the above range, the vanadium carbide can have excellent low oxygen characteristics and preparation efficiency.
[0221] That is, the mixed powder of the vanadium oxide and the carbon compound produced by the high energy milling device may be subjected to vacuum heat treatment during the heat treatment time of the vacuum heat treatment to produce a product having low oxygen characteristics and production efficiency.
[0222] In this case, preferably, the heat treatment time of the above vacuum heat treatment can be 2 hours to 4 hours, and more preferably, can be 2 hours to 3 hours.
[0223] Furthermore, in the above step (b-2) of mixing vanadium carbide and aluminum and heat-treating them under an inert gas to prepare MAX using vanadium carbide, the heat treatment temperature may be 1200° C. to 1600° C. and the heat treatment time may be 1 hour to 5 hours.
[0224] When the heat treatment temperature is within the above range, the MAX using vanadium carbide may have excellent low oxygen characteristics and preparation efficiency.
[0225] That is, the mixed powder of the vanadium carbide and aluminum may be heat-treated at the heat-treatment temperature to produce MAX using vanadium carbide having excellent low oxygen characteristics and production efficiency.
[0226] In this case, preferably, the heat treatment temperature of the vacuum heat treatment may be 1300°C to 1550°C, and more preferably, 1400°C to 1500°C.
[0227] Also, when the heat treatment time is within the above range, the MAX using vanadium carbide may have excellent low oxygen characteristics and production efficiency.
[0228] That is, MAX using vanadium carbide having excellent low oxygen characteristics and production efficiency can be produced by heat-treating the mixed powder of the above-mentioned vanadium carbide and aluminum during the above-mentioned heat treatment time.
[0229] In this case, preferably, the heat treatment time of the above vacuum heat treatment can be 2 hours to 4 hours, and more preferably, can be 2 hours to 3 hours.
[0230] Furthermore, the carburization reduction reaction can be performed by micronizing the vanadium oxide and the carbon compound through the high-energy milling to increase the contact area and the carburization reduction reaction rate.
[0231] Furthermore, in the above-mentioned step (b-3) of preparing the MXene using vanadium carbide by performing aluminum etching and interlayer peeling on the above-mentioned MAX using vanadium carbide, the above-mentioned aluminum etching can be performed using one or more selected from hydrofluoric acid (HF), lithium fluoride (LiF), sodium fluoride (NaF), magnesium fluoride (MgF2), or a combination thereof, or a combination thereof with one or more of hydrochloric acid, sulfuric acid and nitric acid.
[0232] Furthermore, the above-mentioned interlayer peeling can be performed using tetrabutylammonium hydroxide (TBAOH), tetrapropylammonium hydroxide (TPAOH), tetraethylammonium hydroxide (TEAOH), or tetramethylammonium hydroxide (TMAOH).
[0233] Figure 4 FIG. 4 is a process flow chart showing a method for preparing MXene using vanadium carbide according to an embodiment of the present invention.
[0234] refer to Figure 4 First, vanadium oxide and carbon compound are mixed to form a mixed powder, and then the high-energy grinding is performed using a high-energy grinding device to refine the particle size, and a carbonization reduction reaction is performed by vacuum heat treatment to prepare vanadium carbide (S210).
[0235] Then, the vanadium carbide and aluminum are mixed and heat-treated under an inert gas to prepare MAX using vanadium carbide ( S220 ).
[0236] Next, MXene using vanadium carbide is prepared by performing aluminum etching and interlayer peeling on the MAX using vanadium carbide ( S230 ).
[0237] Hereinafter, the present invention will be described in more detail by way of examples. However, the following examples are used to more specifically describe the present invention, and the scope of the present invention is not limited to the following examples. The following examples can be appropriately modified and changed within the scope of the present invention by those of ordinary skill in the art.
[0238] Example
[0239] Example 1 to Example 7: Preparation of vanadium carbide
[0240] Mixed powder of vanadium oxide and carbon compound was prepared using the components and contents shown in Table 1 below.
[0241] Then, the mixed powder was placed together with steel balls in a rotating container of a high energy milling device as shown in Table 1 below.
[0242] Next, in a high energy grinding device as shown in Table 1 below, high energy as shown in Table 1 below is introduced under an atmosphere of air, vacuum, nitrogen or argon as a gas condition when pulverizing particles, and the rotating shaft and the rotating container are rotated in opposite directions to perform high energy grinding to prepare fine powder.
[0243] Then, the above-mentioned subdivided matter was subjected to vacuum heat treatment under the conditions shown in the following Table 1 to perform a carburization reduction reaction to prepare vanadium carbide.
[0244] Comparative Example 1: Preparation of vanadium carbide
[0245] The vanadium carbide of the comparative example was prepared in the same manner as in Example 1 except that a high energy grinding device was used in Example 1.
[0246] Table 1
[0247]
[0248]
[0249] Figure 5 Graph showing the carbon content in vanadium carbide according to Examples 1 to 7 as a function of carbon loading and heat treatment temperature.
[0250] Figure 6 Graph showing the oxygen content in vanadium carbide according to Examples 1 to 7 as a function of carbon loading and heat treatment temperature.
[0251] Refer to Table 1 above and Figure 6 The oxygen content of the vanadium carbides of Examples 1 to 7 is 1440 ppm to 3870 ppm, which is significantly less than the oxygen content of the vanadium carbide of Comparative Example 1 of 12000 ppm.
[0252] Therefore, the vanadium carbides of the above-mentioned Examples 1 to 7 show a small amount of oxygen.
[0253] Furthermore, the average particle size of the vanadium carbide of Examples 1 to 7 is 20 nm, which is much smaller than the average particle size of the vanadium carbide of Comparative Example 1, which is 10 μm.
[0254] Example 8: Preparation of MAX using vanadium carbide
[0255] A mixed powder was prepared by mixing the vanadium carbide prepared in the above-mentioned Example 1 and Example 3 with aluminum.
[0256] Then, MAX using vanadium carbide was prepared by heat-treating the mixed powder at a temperature of 1500° C. for 3 hours under argon.
[0257] Comparative Example 2: Preparation of MAX
[0258] MAX was prepared in the same manner as in Example 8 except that the vanadium carbide of Comparative Example 1 was used.
[0259] Experimental example: Analysis of XRD patterns of MAX using vanadium carbide
[0260] The crystal structure (XRD) curves of the vanadium carbides prepared in the above-mentioned Examples 1 and 3 are shown in Figure 7 middle.
[0261] Figure 7 The V2AlC MAX powder of the vanadium-based MAX powder of Examples 1 and 3 is (a) V2AlC MAX, (b) V 12 XRD pattern of Al3C8 MAX.
[0262] refer to Figure 7 Part a does not show a metallic vanadium pattern in the XRD pattern of V2AlC MAX in Example 1 above.
[0263] refer to Figure 7 Part b, in the above Example 3, V 12 The XRD pattern of Al3C8 MAX does not show the metallic vanadium pattern.
[0264] Therefore, it can be confirmed that the V2AlCMAX in the (a) part and the V in the (b) part of the vanadium-based MAX powder in Examples 1 and 3 are 12 Al3C8 MAX uses vanadium carbide with controlled carbon content as raw material to successfully prepare vanadium-based MAX powder without using metallic vanadium.
[0265] Although specific embodiments related to MAX and MXene using vanadium carbide and the method for producing the same according to the present invention have been described so far, it is apparent that various modifications may be made without departing from the scope of the present invention.
[0266] Therefore, the scope of the present invention should not be limited to the described embodiments, but should be defined by the following claims and their equivalents.
[0267] That is, it should be understood that the above-mentioned embodiments are illustrative and not restrictive in all aspects, and the scope of the present invention is indicated by the scope of protection of the invention described later rather than a detailed description, and should be interpreted as all modifications or deformation forms derived from the meaning, scope and equivalent concepts of the scope of protection of the invention are included in the scope of the present invention.
Claims
1. A MAX using vanadium carbide, characterized in that: It is composed of vanadium, aluminum and carbon of vanadium carbide and is used as a raw material of a two-dimensional nanomaterial MXene, and is selected from at least one of the compounds shown in the following chemical formulas 1 to 3: Chemical formula 1: V2AlC, Chemical formula 2: V4AlC3, Chemical formula 3: V 12 Al3C8.
2. The MAX using vanadium carbide according to claim 1, characterized in that: The MAX using vanadium carbide is formed by heat-treating a mixture of vanadium carbide and aluminum under an inert gas.
3. The MAX using vanadium carbide according to claim 1, characterized in that: The vanadium carbide is formed by pulverizing vanadium oxide and a carbon compound and then heat treating the mixture of the vanadium oxide and the carbon compound under vacuum and normal pressure.
4. The MAX using vanadium carbide according to claim 1, characterized in that: The molar ratio of vanadium to carbon in the vanadium carbide is vanadium:carbon=2:1, 3:2 or 4:
3.
5. The MAX using vanadium carbide according to claim 1, characterized in that: The above-mentioned MAX using vanadium carbide excludes the use of metallic vanadium.
6. The MAX using vanadium carbide according to claim 1, characterized in that: The carbon content of the MAX using vanadium carbide is 8 to 14 weight percent.
7. The MAX using vanadium carbide according to claim 1, characterized in that: The oxygen content of the MAX using vanadium carbide is 1000 to 5000 ppm.
8. A MXene using vanadium carbide, characterized in that: This is a two-dimensional nanomaterial formed by performing aluminum etching and interlayer peeling on the MAX using vanadium carbide according to claim 1.
9. The MXene using vanadium carbide according to claim 8, characterized in that The MXene using vanadium carbide is selected from at least one of the compounds shown in the following chemical formulas 4 to 6: Chemical formula 4: V2C, Chemical formula 5: V4C3, Chemical formula 6: V3C2.
10. The MXene using vanadium carbide according to claim 8, characterized in that The carbon content of the MXene using vanadium carbide is 10.5 to 15 weight percent.
11. A method for preparing MAX, characterized in that: include: Step (a-1), mixing vanadium oxide and carbon compound to form a mixed powder, then performing high-energy grinding using a high-energy grinding device to refine the particle size, and performing a carburization reduction reaction by vacuum heat treatment to prepare vanadium carbide; as well as Step (a-2) is to mix the vanadium carbide and aluminum and perform heat treatment under an inert gas to prepare MAX using vanadium carbide.
12. The method for preparing MAX according to claim 11, characterized in that: The particle size of the mixed powder of the vanadium oxide or the carbon compound is 2 nm to 50 μm.
13. The method for preparing MAX according to claim 11, characterized in that: The mixed powder of the vanadium oxide and the carbon compound is placed together with steel balls in a rotating container in a high-energy grinding device, and then the high-energy grinding is performed in an atmosphere of air, vacuum, nitrogen or argon. In the carburization-reduction reaction, the vanadium oxide and the carbon compound are micronized by the high-energy grinding to increase the contact area and increase the carburization-reduction reaction rate.
14. A method for preparing MXene, characterized in that: include: Step (b-1), mixing vanadium oxide and carbon compound to form a mixed powder, then performing high-energy grinding using a high-energy grinding device to refine the particle size, and performing a carburization reduction reaction by vacuum heat treatment to prepare vanadium carbide; Step (b-2), mixing the vanadium carbide and aluminum, and heat treating them under an inert gas to prepare MAX using vanadium carbide; as well as Step (b-3), preparing MXene using vanadium carbide by performing aluminum etching and interlayer exfoliation on the above-mentioned MAX using vanadium carbide.
15. The method for preparing MXene according to claim 14, characterized in that: In the above-mentioned step (b-3) of preparing the MXene using vanadium carbide by performing aluminum etching and interlayer peeling on the above-mentioned MAX using vanadium carbide, the above-mentioned aluminum etching is performed using one or more selected from hydrofluoric acid, lithium fluoride, sodium fluoride, magnesium fluoride, or a combination thereof, or a combination thereof with one or more of hydrochloric acid, sulfuric acid and nitric acid.
Citation Information
Patent Citations
MXene nanosheet and Manufacturing method thereof
KR1020170036507A