CN114031078B - Preparation method of fluorine-free MXene two-dimensional nanosheets - Google Patents
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Abstract
The invention discloses a preparation method of a fluorine-free MXene two-dimensional nano sheet, which is characterized in that MAX phase material and an initiator are heated and cleaned in vacuum or protective gas atmosphere, and then mixed with solid alkali, heated, cleaned and dried to prepare the fluorine-free MXene two-dimensional nano sheet. The invention replaces concentrated alkaline aqueous solution or fluorine-containing acid solution in the traditional preparation process with solid alkali, thereby improving the reactivity of the fluorine-free MXene two-dimensional nano-sheet while realizing environmental protection. The method is suitable for preparing the fluorine-free MXene nano-sheets, and the prepared fluorine-free MXene nano-sheets 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 in particular relates to a preparation method of a fluorine-free MXene two-dimensional nano sheet.
Background
MXene, an emerging two-dimensional (2D) transition metal carbide/nitride, has received much attention from researchers in various countries because of its advantages such as excellent conductivity, good hydrophilicity, and a large lamellar structure.
The current preparation method of MXene is mainly acid etching method, and the etchant comprises a mixture of hydrofluoric acid aqueous solution (HF), lithium fluoride and hydrochloric acidLif+hcl), ammonium bifluoride ((NH) 4 )HF 2 ) Etc. The method realizes the etching purpose by selectively etching the A atomic layer of the MAX phase by the fluorine-containing ion solution, and has the advantages of simple operation, relatively mild etching conditions, large interval between prepared MXene two-dimensional nano-sheets, few defects, large lamellar structure and the like; however, these fluorine-containing etchants have high corrosiveness, environmental pollution and potential safety hazards, and fluorine ion-terminated groups inhibit the reactivity of MXene, and reduce the service performance of the material, for example, in electrochemical energy storage, the presence of fluorine ions increases the diffusion energy barrier of lithium ions, and inhibits the reaction stability of the interface between electrolyte and MXene electrode. Thus, fluorine-free MXene production is particularly important.
Patent CN110371979B proposes a method for preparing an MXene quantum dot by alkali etching, but the quantum dot prepared by the method loses the characteristics of an MXene two-dimensional nano-sheet; gu Jiajun et al propose to synthesize fluorine-free high-purity MXene two-dimensional nanomaterial by alkali etching with a hydrothermal method, but the high-temperature high-concentration (270 ℃ and 27.5M) hydrothermal condition causes serious potential safety hazard in MXene production.
Therefore, finding 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 nano-sheet, which can protect the environment and ensure the reactivity of the fluorine-free MXene two-dimensional nano-sheet.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
the preparation method of the fluorine-free MXene two-dimensional nanosheets comprises the following steps of:
s1, uniformly mixing MAX phase material and initiator, heating in vacuum or protective gas atmosphere, cleaning,
obtaining solid alpha;
s2, uniformly mixing the solid alpha and alkali, heating in vacuum or protective gas atmosphere, cleaning and drying to obtain the fluorine-free MXene two-dimensional nano-sheet.
As a limitation, in step S1:
the element of the M layer of the MAX phase material 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 the step S1, the heating temperature is 100-600 ℃ and the heating time is 1-10h.
As a fourth limitation, the protective gas is argon, helium or nitrogen.
As a fifth limitation, the cleaning solution used for the cleaning is at least one of water, ethanol, dilute hydrochloric acid and nitric acid.
As a sixth limitation, in step S2, the alkali is at least one of LiOH, naOH and KOH, and the weight ratio of the alkali to the MAX phase material is 2-80:1.
as a seventh limitation, in step S2, the heating is performed at a temperature of 200 to 800 ℃ for a time of 2 to 24 hours.
As an eighth limitation, in the step S2, the drying is performed under vacuum at 60-100deg.C for 4-24 hours.
As a final definition, the fluorine-free MXene two-dimensional nano-sheet has a thickness of 1-200nm.
By adopting the technical scheme, compared with the prior art, the invention has the following technical progress:
(1) according to the preparation method of the fluorine-free MXene two-dimensional nano-sheet, the solid alkali is used for replacing the concentrated alkali solution, so that the hydrothermal reaction under the conditions of high temperature and high pressure is avoided, and the safety in the preparation process is improved;
(2) the preparation method of the fluorine-free MXene two-dimensional nano-sheet provided by the invention has the advantages of mild reaction conditions, simplicity in operation, environmental friendliness, no fluorine in the preparation process, no introduction of impurities and high yield;
(3) the preparation method of the fluorine-free MXene two-dimensional nano-sheet provided by the invention has the advantages that the sources of raw materials used in the whole preparation process are wide, the raw materials are easy to obtain and the cost is low, so that the preparation cost of the fluorine-free MXene nano-sheet is reduced;
(4) according to the preparation method of the fluorine-free MXene two-dimensional nano sheet, the edge of the MAX is etched through the initiator, the edge window is opened, the interference effect in the alkali etching process can be effectively avoided by the opened edge window, namely, the generated hydroxide is prevented from accumulating in the edge window of the MAX to prevent the reaction from further proceeding, and the molten alkali continuously etches the A layer element in the MAX through the edge window of the MAX, so that the continuous proceeding of the etching reaction is ensured;
(5) the fluorine-free MXene nano-sheet prepared by the method has high 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 nano-sheets, and the prepared fluorine-free MXene nano-sheets 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 below with reference to the attached drawings and specific examples:
FIG. 1 is a diagram of Ti in example 1 of the present invention 2 X-ray diffraction patterns of AlC raw materials and fluorine-free MXene two-dimensional nano-sheets beta 1;
FIG. 2 is an SEM image of fluorine-free MXene two-dimensional nanoplatelets 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 invention will now be described in further detail by way of specific examples, which are to be understood as illustrative only and not limiting.
Example 1 preparation method of fluorine-free MXene two-dimensional nanosheets
The embodiment comprises the following steps sequentially carried out:
s1, 300g of Ti 2 Uniformly mixing AlC material and 1kg of iodine simple substance, transferring into a circulating steam furnace, performing heat treatment for 1h at 500 ℃ in nitrogen atmosphere, alternately cleaning with ethanol and water to remove the iodine simple substance, and drying to constant weight at 60 ℃ under vacuum condition to obtain solid alpha 1;
s2, uniformly mixing the solid alpha 1 with 5kg of NaOH, transferring into a circulating steam furnace, performing heat treatment for 12 hours at 500 ℃ in an argon atmosphere, alternately cleaning with 1mol/l hydrochloric acid and water, repeating for 5 times, and drying to constant weight at 60 ℃ under a vacuum condition to obtain the fluorine-free MXene two-dimensional nanosheet beta 1;
s3, placing the fluorine-free MXene two-dimensional nano-sheet beta 1 prepared in the S2 under a scanning electron microscope for detection, wherein the thickness of the fluorine-free MXene two-dimensional nano-sheet beta 1 is 1-10nm;
FIG. 1 is Ti 2 As can be seen from FIG. 1, the fluorine-free MXene two-dimensional nanosheet beta 1 prepared by the method of the invention has no obvious Ti 2 Diffraction peaks for AlC, indicating Ti 2 The A layer element in AlC is fully etched;
FIG. 2 is an SEM image of a fluorine-free MXene two-dimensional nanosheet β1, as can be seen from FIG. 2, the fluorine-free MXene nanosheet exhibits a loose monolithic structure with a platelet thickness of about 1-10nm.
Examples 2 to 6 preparation method of fluorine-free MXene two-dimensional nanosheets
Examples 2 to 6 are a method for preparing fluorine-free MXene two-dimensional nanosheets, which are basically the same as example 1, and differ only in the parameters, and are specifically shown in Table 1:
table 1 list of parameters in examples 2 to 6
Other portions of examples 2 to 6 were the same as in example 1, and fluorine-free MXene two-dimensional nanoplatelets β2 to β6 were prepared in examples 2 to 6, respectively;
FIG. 3 is an SEM image of a two-dimensional fluorine-free MXene nanoplatelet β2 of example 2. As can be seen from FIG. 3, the fluorine-free MXene nanoplatelets exhibit a loose potato-chip-like structure.
Claims (8)
1. The preparation method of the fluorine-free MXene two-dimensional nanosheets is characterized by comprising the following steps of:
s1, uniformly mixing a MAX phase material and an initiator, heating in vacuum or protective gas atmosphere, and cleaning to obtain a solid alpha;
s2, uniformly mixing the solid alpha and the solid alkali, heating in vacuum or protective gas atmosphere, cleaning and drying to obtain the fluorine-free MXene two-dimensional nano-sheet;
in step S1:
the initiator is at least one of tin dichloride and silver nitrate;
the weight ratio of the initiator to the MAX phase material is 1-50:1, a step of;
in the step S2, the alkali is at least one of LiOH, naOH and KOH, and the weight ratio of the alkali to MAX phase material is 2-80:1.
2. the method for preparing fluorine-free MXene two-dimensional nanosheets according to claim 1, wherein in step S1:
the element of the M layer of the MAX phase material 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 according to claim 1, wherein in step S1: the heating temperature is 100-600deg.C, and the heating time is 1-10h.
4. The method for preparing fluorine-free MXene two-dimensional nano-sheets according to claim 1, wherein the protective gas is argon, helium or nitrogen.
5. The method for preparing fluorine-free MXene two-dimensional nano-sheets according to claim 1, wherein the cleaning solution is at least one of water, ethanol, dilute hydrochloric acid and nitric acid.
6. The method according to any one of claims 1 to 5, wherein in step S2, the heating is performed at a temperature of 200 to 800 ℃ for a time of 2 to 24 hours.
7. The method according to any one of claims 1 to 5, wherein in step S2, the drying is performed under vacuum at 60 to 100 ℃ for 4 to 24 hours.
8. The method for preparing fluorine-free MXene two-dimensional nano-sheets according to any one of claims 1 to 5, wherein the fluorine-free MXene two-dimensional nano-sheets have a thickness of 1 to 200nm.
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| KR102373455B1 (en) * | 2015-09-24 | 2022-03-11 | 삼성전자주식회사 | MXene nanosheet and Manufacturing method thereof |
| US12054428B2 (en) * | 2019-11-12 | 2024-08-06 | United States Of America As Represented By The Secretary Of The Air Force | Preparation of layered MXene via elemental halogen etching of MAX phase |
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