CN114031078A - Preparation method of fluorine-free MXene two-dimensional nanosheet - Google Patents
Preparation method of fluorine-free MXene two-dimensional nanosheet Download PDFInfo
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- CN114031078A CN114031078A CN202111390851.8A CN202111390851A CN114031078A CN 114031078 A CN114031078 A CN 114031078A CN 202111390851 A CN202111390851 A CN 202111390851A CN 114031078 A CN114031078 A CN 114031078A
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- 239000002135 nanosheet Substances 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 20
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 238000004140 cleaning Methods 0.000 claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 11
- 239000003513 alkali Substances 0.000 claims abstract description 10
- 239000007787 solid Substances 0.000 claims abstract description 9
- 239000003999 initiator Substances 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 7
- 230000001681 protective effect Effects 0.000 claims abstract description 7
- 239000012298 atmosphere Substances 0.000 claims abstract description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 6
- 239000002064 nanoplatelet Substances 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims description 4
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 4
- 239000002585 base Substances 0.000 claims description 4
- 229910052740 iodine Inorganic materials 0.000 claims description 4
- 239000011630 iodine Substances 0.000 claims description 4
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 229910052804 chromium Inorganic materials 0.000 claims description 2
- 239000006184 cosolvent Substances 0.000 claims description 2
- 229910052735 hafnium Inorganic materials 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- 239000001307 helium Substances 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
- 229910052758 niobium Inorganic materials 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 229910052706 scandium Inorganic materials 0.000 claims description 2
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 2
- 235000011150 stannous chloride Nutrition 0.000 claims description 2
- 229910052715 tantalum Inorganic materials 0.000 claims description 2
- AXZWODMDQAVCJE-UHFFFAOYSA-L tin(II) chloride (anhydrous) Chemical compound [Cl-].[Cl-].[Sn+2] AXZWODMDQAVCJE-UHFFFAOYSA-L 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 229910052720 vanadium Inorganic materials 0.000 claims description 2
- 229910052726 zirconium Inorganic materials 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 6
- 229910052731 fluorine Inorganic materials 0.000 abstract description 6
- 239000011737 fluorine Substances 0.000 abstract description 6
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 abstract description 4
- 238000006555 catalytic reaction Methods 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 3
- 238000004146 energy storage Methods 0.000 abstract description 3
- 238000000746 purification Methods 0.000 abstract description 3
- 238000001179 sorption measurement Methods 0.000 abstract description 3
- 239000002253 acid Substances 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract 1
- 238000005530 etching Methods 0.000 description 12
- 239000010410 layer Substances 0.000 description 8
- 239000000203 mixture Substances 0.000 description 7
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- -1 fluorine ions Chemical class 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000002096 quantum dot Substances 0.000 description 2
- 230000009257 reactivity Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- MIMUSZHMZBJBPO-UHFFFAOYSA-N 6-methoxy-8-nitroquinoline Chemical compound N1=CC=CC2=CC(OC)=CC([N+]([O-])=O)=C21 MIMUSZHMZBJBPO-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 235000002595 Solanum tuberosum Nutrition 0.000 description 1
- 244000061456 Solanum tuberosum Species 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000012983 electrochemical energy storage Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
- C01B32/921—Titanium carbide
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/076—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with titanium or zirconium or hafnium
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- C01B32/914—Carbides of single elements
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a preparation method of a fluorine-free MXene two-dimensional nanosheet, which comprises the steps of heating and cleaning MAX phase materials and an initiator in a vacuum or protective gas atmosphere, mixing with solid alkali, heating, cleaning and drying to prepare the fluorine-free MXene two-dimensional nanosheet. The method replaces concentrated alkali water solution or fluorine-containing acid solution in the traditional preparation process with solid alkali, realizes environmental friendliness and improves the reaction activity of the fluorine-free MXene two-dimensional nanosheets. The method is suitable for preparing the fluorine-free MXene nanosheets, and the prepared fluorine-free MXene nanosheets are further applied to the fields of energy storage, water purification, adsorption, catalysis and the like.
Description
Technical Field
The invention belongs to the technical field of nano materials, relates to MXene, and particularly relates to a preparation method of a fluorine-free MXene two-dimensional nanosheet.
Background
MXene, a new two-dimensional (2D) transition metal carbide/nitride, has received much attention from researchers in various countries because of its many advantages such as excellent conductivity, good hydrophilicity, and large sheet structure.
The existing MXene preparation method is mainly an acid etching method, and the etching agent comprises hydrofluoric acid aqueous solution (HF), a mixture of lithium fluoride and hydrochloric acid (LiF + HCl) and ammonium bifluoride ((NH)4)HF2) And the like. The method realizes the purpose of etching by selectively etching the MAX-phase A atomic layer through the fluorine-containing ion solution, and has the advantages of simple and convenient operation, relatively mild etching conditions, large interlayer spacing of the prepared MXene two-dimensional nanosheets, few defects, large lamellar structure and the like; however, these fluorine-containing etching agents not only have high corrosivity, but also have environmental pollution and potential safety hazards, and the group taking fluorine ions as the terminal can inhibit the reactivity of MXene and reduce the service performance of the material, for example, in electrochemical energy storage, the existence of fluorine ions can increase the diffusion energy barrier of lithium ions and inhibit the reaction stability of the interface of the electrolyte and the MXene electrode. Thus, the preparation of fluorine-free MXene is of great importance.
Patent CN110371979B proposes a method for preparing MXene quantum dots by adopting alkaline liquor etching, but quantum dots prepared by the method lose the characteristics of MXene two-dimensional nanosheets; gujun et al propose to synthesize fluoride-free high-purity MXene two-dimensional nanomaterial by hydrothermal method alkali etching, but serious potential safety hazard exists in MXene production under the hydrothermal condition of high temperature and high concentration (270 ℃, 27.5M).
Therefore, the finding of a green, safe and fluorine-free etching method has important significance for the practical application of MXene.
Disclosure of Invention
The invention aims to provide a green and safe preparation method of a fluorine-free MXene two-dimensional nanosheet, which can protect the environment and ensure the reactivity of the fluorine-free MXene two-dimensional nanosheet.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of fluorine-free MXene two-dimensional nanosheets comprises the following steps of:
s1, uniformly mixing MAX phase materials and an initiator, heating in vacuum or protective gas atmosphere, cleaning,
obtaining solid alpha;
s2, uniformly mixing the solid alpha and the alkali, heating in a vacuum or protective gas atmosphere, cleaning, and drying to obtain the fluorine-free MXene two-dimensional nanosheet.
As one limitation, in step S1:
the MAX phase material is characterized in that the element of the M layer is at least one of Ti, Zr, Hf, V, Nb, Ta, Cr and Sc;
the element of the A layer is Al or Si;
the element of the X layer is C or N.
As another limitation, in step S1:
the initiator is at least one of iodine cosolvent, tin dichloride and silver nitrate;
the weight ratio of the initiator to the MAX phase material is 1-50: 1.
as a third limitation, in step S1, the heating temperature is 100-600 ℃ and the heating time is 1-10 h.
As a fourth definition, the protective gas is argon, helium, or nitrogen.
As a fifth limitation, the cleaning is performed by using at least one of water, ethanol, diluted hydrochloric acid and nitric acid as a cleaning solution.
As a sixth limitation, in step S2, the base is at least one of LiOH, NaOH, and KOH, and the weight ratio of the base to the MAX phase material is 2-80: 1.
as a seventh limitation, in step S2, the heating temperature is 200-800 ℃ and the heating time is 2-24 h.
As an eighth limitation, in step S2, the drying is performed under vacuum at 60-100 deg.C for 4-24 h.
As a final definition, the thickness of the fluorine-free MXene two-dimensional nanosheets is from 1 to 200 nm.
Due to the adoption of the technical scheme, compared with the prior art, the invention has the technical progress that:
the preparation method of the fluorine-free MXene two-dimensional nanosheet provided by the invention has the advantages that solid alkali is used for replacing concentrated alkali solution, so that hydrothermal reaction under the conditions of high temperature and high pressure is avoided, and the safety in the preparation process is improved;
the preparation method of the fluorine-free MXene two-dimensional nanosheet provided by the invention is mild in reaction condition, simple to operate, environment-friendly, free of fluorine in the preparation process, free of impurity introduction and high in yield;
the preparation method of the fluorine-free MXene two-dimensional nanosheet provided by the invention has the advantages that the raw materials used in the whole preparation process are wide in source, easy to obtain and low in cost, so that the preparation cost of the fluorine-free MXene nanosheet is reduced;
the preparation method of the fluorine-free MXene two-dimensional nanosheet provided by the invention comprises the steps of etching the MAX edge through the initiator, opening the edge window, wherein the opened edge window can effectively avoid the interference effect in the alkali etching process, namely, the generated hydroxide is prevented from accumulating in the MAX edge window and blocking the further reaction, and the molten alkali continuously etches the A layer element in the MAX through the MAX edge window, so that the continuous etching reaction is ensured;
the fluorine-free MXene nanosheets prepared by the method are high in reaction activity and can be widely applied to the fields of energy storage, water purification, adsorption, catalysis and the like.
The method is suitable for preparing the fluorine-free MXene nanosheets, and the prepared fluorine-free MXene nanosheets are further applied to the fields of energy storage, water purification, adsorption, catalysis and the like.
Drawings
The invention will be described in more detail with reference to the following figures and embodiments:
FIG. 1 shows Ti in example 1 of the present invention2An X-ray diffraction spectrogram of an AlC raw material and fluorine-free MXene two-dimensional nanosheet beta 1;
FIG. 2 is an SEM image of fluorine-free MXene two-dimensional nanosheets prepared in example 1 of the present invention;
fig. 3 is an SEM image of fluorine-free MXene two-dimensional nanoplatelets prepared in example 2 of the present invention.
Detailed Description
The present invention is further illustrated by the following specific examples, which are to be construed as merely illustrative, and not limitative of the remainder of the disclosure.
Embodiment 1 preparation method of fluorine-free MXene two-dimensional nanosheet
The embodiment comprises the following steps which are carried out in sequence:
s1, mixing 300g of Ti2Uniformly mixing an AlC material and 1kg of iodine simple substance, transferring the mixture into a circulating steam furnace, carrying out heat treatment for 1h at 500 ℃ in the atmosphere of nitrogen, alternately cleaning the mixture with ethanol and water to remove the iodine simple substance, and drying the mixture to constant weight under the vacuum condition of 60 ℃ to obtain solid alpha 1;
s2, uniformly mixing the solid alpha 1 and 5kg of NaOH, transferring the mixture into a circulating steam furnace, carrying out heat treatment for 12 hours at 500 ℃ in an argon atmosphere, alternately cleaning the mixture by using hydrochloric acid with the concentration of 1mol/l and water, repeating the cleaning for 5 times, and drying the mixture to constant weight at 60 ℃ under a vacuum condition to obtain a fluorine-free MXene two-dimensional nanosheet beta 1;
s3, placing the fluorine-free MXene two-dimensional nanosheets beta 1 prepared in S2 under a scanning electron microscope for detection, wherein the thickness of the detected fluorine-free MXene two-dimensional nanosheets beta 1 is 1-10 nm;
FIG. 1 is Ti2As can be seen from FIG. 1, the X-ray diffraction spectrogram of AlC raw material and fluorine-free MXene two-dimensional nanosheet beta 1 does not have obvious Ti2Diffraction peak of AlC, indicating Ti2The A layer element in the AlC is fully etched;
FIG. 2 is an SEM image of a fluorine-free MXene two-dimensional nanosheet beta 1, and from FIG. 2, it can be seen that the fluorine-free MXene nanosheet exhibits a loose monolithic layer structure with a layer thickness of about 1-10 nm.
Example 2-6 preparation method of fluorine-free MXene two-dimensional nanosheet
TABLE 1 summary of the parameters of examples 2 to 6
The contents of other parts of the embodiments 2 to 6 are the same as the embodiment 1, and the embodiments 2 to 6 respectively prepare the fluoride-free MXene two-dimensional nanosheets beta 2 to beta 6;
fig. 3 is an SEM image of the fluorine-free MXene two-dimensional nanoplatelets β 2 of example 2, and it can be seen from fig. 3 that the fluorine-free MXene nanoplatelets exhibit a loose potato chip-like structure.
Claims (10)
1. The preparation method of the fluorine-free MXene two-dimensional nanosheet is characterized by comprising the following steps of:
s1, uniformly mixing MAX phase materials and an initiator, heating in vacuum or protective gas atmosphere, and cleaning to obtain solid alpha;
s2, uniformly mixing the solid alpha and the alkali, heating in a vacuum or protective gas atmosphere, cleaning, and drying to obtain the fluorine-free MXene two-dimensional nanosheet.
2. The method for preparing fluorine-free MXene two-dimensional nanosheets of claim 1, wherein in step S1:
the MAX phase material is characterized in that the element of the M layer is at least one of Ti, Zr, Hf, V, Nb, Ta, Cr and Sc;
the element of the A layer is Al or Si;
the element of the X layer is C or N.
3. The method for preparing fluorine-free MXene two-dimensional nanosheets of claim 1, wherein in step S1:
the initiator is at least one of iodine cosolvent, tin dichloride and silver nitrate;
the weight ratio of the initiator to the MAX phase material is 1-50: 1.
4. the method for preparing fluorine-free MXene two-dimensional nanosheets of claim 1, wherein in step S1: the heating temperature is 100-600 ℃, and the time is 1-10 h.
5. The method for preparing fluorine-free MXene two-dimensional nanosheets of claim 1, wherein the protective gas is argon, helium or nitrogen.
6. The method for preparing the fluorine-free MXene two-dimensional nanosheets of claim 1, wherein the cleaning solution used for the cleaning is at least one of water, ethanol, dilute hydrochloric acid and nitric acid.
7. The method for preparing fluorine-free MXene two-dimensional nanoplatelets according to any one of claims 1-6, wherein in step S2, the base is at least one of LiOH, NaOH and KOH, and the weight ratio of the base to MAX phase material is 2-80: 1.
8. the method for preparing fluorine-free MXene two-dimensional nanoplatelets as claimed in any one of claims 1-6, wherein the heating temperature is 200-800 ℃ and the heating time is 2-24h in step S2.
9. The method for preparing fluorine-free MXene two-dimensional nanoplatelets as claimed in any one of claims 1-6, wherein the drying is performed under vacuum condition of 60-100 ℃ for 4-24h in step S2.
10. The method for preparing the fluorine-free MXene two-dimensional nanosheets of any one of claims 1-6, wherein the fluorine-free MXene two-dimensional nanosheets are 1-200nm thick.
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102976295A (en) * | 2012-12-27 | 2013-03-20 | 山东大学 | Method for preparing two-dimensional hexagonal boron nitride nanosheet through molten caustic soda |
| US20170088429A1 (en) * | 2015-09-24 | 2017-03-30 | Samsung Electronics Co., Ltd. | Mxene nanosheet and manufacturing method thereof |
| CN106744733A (en) * | 2017-02-13 | 2017-05-31 | 华东理工大学 | A kind of preparation method of two-dimentional transition metal carbide or nitride |
| CN110371979A (en) * | 2019-07-31 | 2019-10-25 | 北京科技大学 | A kind of method that lye etching prepares MXene quantum dot |
| CN111591992A (en) * | 2020-06-10 | 2020-08-28 | 哈尔滨工业大学 | Single-layer MXene nanosheet and preparation method thereof |
| CN111943207A (en) * | 2020-07-17 | 2020-11-17 | 郑州骋憬材料科技有限公司 | Method for preparing fluorine-free two-dimensional material MXene simply and in pollution-free manner |
| US20210139379A1 (en) * | 2019-11-12 | 2021-05-13 | Government Of The United States, As Represented By The Secretary Of The Air Force | Preparation of Layered MXene via Elemental Halogen Etching of MAX Phase |
| CN112830459A (en) * | 2021-01-21 | 2021-05-25 | 华中科技大学 | Method for preparing two-dimensional transition metal nitride with assistance of decomposable alkali metal compound |
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Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102976295A (en) * | 2012-12-27 | 2013-03-20 | 山东大学 | Method for preparing two-dimensional hexagonal boron nitride nanosheet through molten caustic soda |
| US20170088429A1 (en) * | 2015-09-24 | 2017-03-30 | Samsung Electronics Co., Ltd. | Mxene nanosheet and manufacturing method thereof |
| CN106744733A (en) * | 2017-02-13 | 2017-05-31 | 华东理工大学 | A kind of preparation method of two-dimentional transition metal carbide or nitride |
| CN110371979A (en) * | 2019-07-31 | 2019-10-25 | 北京科技大学 | A kind of method that lye etching prepares MXene quantum dot |
| US20210139379A1 (en) * | 2019-11-12 | 2021-05-13 | Government Of The United States, As Represented By The Secretary Of The Air Force | Preparation of Layered MXene via Elemental Halogen Etching of MAX Phase |
| CN111591992A (en) * | 2020-06-10 | 2020-08-28 | 哈尔滨工业大学 | Single-layer MXene nanosheet and preparation method thereof |
| CN111943207A (en) * | 2020-07-17 | 2020-11-17 | 郑州骋憬材料科技有限公司 | Method for preparing fluorine-free two-dimensional material MXene simply and in pollution-free manner |
| CN112830459A (en) * | 2021-01-21 | 2021-05-25 | 华中科技大学 | Method for preparing two-dimensional transition metal nitride with assistance of decomposable alkali metal compound |
Non-Patent Citations (2)
| Title |
|---|
| 党阿磊 等: "新型二维纳米材料MXene的制备及在储能领域的应用进展", 材料工程, vol. 48, no. 04, pages 1 - 14 * |
| 吕康乐;李开宁;李志鹏;黄蔚欣;李覃;沈群: "新型二维材料MXene在光催化领域应用的研究进展", 徐州工程学院学报(自然科学版), vol. 34, no. 04, pages 18 - 23 * |
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