CN108793167B - Method for preparing layered MXenes material by utilizing ternary MAX material - Google Patents
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Abstract
A method for preparing a layered MXenes material by using a ternary MAX material comprises the steps of using strong acid or strong base as corrosive liquid and placing the corrosive liquid in a reaction container, placing MAX powder into the corrosive liquid, adding soluble mixed salt while stirring, continuously corroding for 0.5-48 hours, then carrying out centrifugal separation, cleaning and drying to obtain the layered MXenes material. According to the invention, by utilizing the principle of a galvanic cell, soluble mixed salt of metal with metal activity weaker than that of the metal on the layer A is added into corrosive liquid, so that the soluble metal salt is reduced by the metal on the layer A to obtain the metal with metal activity weaker than that of the metal on the layer A, the metal and the metal on the layer A are combined to form a corrosive couple, the reaction is promoted to be carried out rightwards, the corrosion of the metal on the layer A is accelerated, and thus the single-layer two-dimensional nanomaterial with complete denudation is obtained. The method disclosed by the invention is simple, strong in operability and good in realization result, and can be used for obtaining the Mxenes material with higher stripping degree and better micro-morphology.
Description
Technical Field
The invention relates to a preparation process of a special layered material, in particular to a method for preparing a layered MXenes material by utilizing a ternary MAX material.
Background
MAX material is a three-dimensional lamellar crystal with novel lamellar structure and chemical general formula of MAX material is Mn+1AXn(n is 1 to 6) and is abbreviated as MAX. Wherein M is transition metal element, A is III and IV main group element, X is C or N element, each kind of atom is combined by covalent bond in plane to form sheet layer with atomic-scale thickness, and the sheet layers are combined by Van der Waals force. Peeling of the materialThe separation is to utilize the difference of bond energy between M-A and M-C, and to destroy the chemical bond between M-A while maintaining the structure of M-C, so as to separate the A layer from the MAX matrix, thereby obtaining the two-dimensional layered nano material, which is also called MXenes material. The material has various electromagnetic and thermoelectric properties and excellent characteristics of electrochemistry, heavy metal ion adsorption, gas adsorption and the like, and has very wide application prospects in the fields of ion batteries, supercapacitors, sewage treatment, hydrogen storage and the like. Therefore, the preparation of MXene materials by the corrosion exfoliation of MAX phase powders has become one of the hot spots in the two-dimensional nanomaterial research field in recent years.
At present, the layer A is usually etched by hydrofluoric acid to obtain MXenes material, such as Ti used by Michael Naguib et al3AlC2Material preparation to obtain Ti3C. The specific corrosion process of the material in HF is as follows:
Mn+1AXn+3HF＝AF3+Mn+1Xn+1.5H2
Mn+1AXn+2H2O＝Mn+1Xn(OH)2+H2
Mn+1Xn+2HF＝Mn+1XnF2+H2
in order to obtain the layered MXenes material with good appearance, the method has strict requirements on corrosion temperature, corrosion time and the like. However, the small distance between the original MAX sheets can prevent the reactant of the A layer and HF from contacting each other poorly, and the slow speed of MAX corrosion stripping can cause the problems of low corrosion yield, uneven corrosion, incomplete stripping and the like in the process. However, if the corrosion time is prolonged, the M-C structure is destroyed, and M-C fragments are formed, so that the layered MXenes material with good appearance cannot be obtained.
Disclosure of Invention
In order to overcome the problems in the prior art, the invention aims to provide a method for preparing a layered MXenes material by using a ternary MAX material.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for preparing a layered MXenes material by using a ternary MAX material comprises the steps of using strong acid or strong base as corrosive liquid and placing the corrosive liquid in a reaction container, placing MAX powder into the corrosive liquid, adding soluble mixed salt while stirring, continuously corroding for 0.5-48 hours, then carrying out centrifugal separation, cleaning and drying to obtain the layered MXenes material.
The invention is further improved in that the temperature of the corrosive liquid is 4-60 ℃.
The invention is further improved in that the stirring speed is 200-1600 r/min.
The invention is further improved in that the strong base is NaOH aqueous solution; the strong acid is hydrofluoric acid and HNO3And one or more of hydrochloric acid.
The invention is further improved in that the mass fraction of the hydrofluoric acid is 40 percent, and the HNO is3The mass fraction of (3) is 40%, the mass fraction of hydrochloric acid is 40%, and the concentration of NaOH aqueous solution is 6 mol/L.
The invention has the further improvement that the adding amount of the soluble metal mixed salt is 2 to 15 percent of the total mass of the corrosive liquid.
The further improvement of the invention is that the soluble metal mixed salt is one, two or three of titanium, zirconium, vanadium, manganese, zinc, gallium, cobalt, nickel, molybdenum, tin, lead, copper and silver salt.
A further improvement of the invention is that when the soluble metal mixed salt is two salts, the molar ratio of the two salts is 1: 1.
The invention is further improved in that when the soluble metal mixed salt is three salts, the molar ratio of the three salts is 1:1: 1.
Compared with the prior art, the invention has the beneficial effects that: according to the method, by utilizing the principle of a galvanic cell, when the MAX material is corroded, soluble mixed salt of metal with metal activity weaker than that of the layer A metal is added into a corrosive liquid, so that the soluble metal salt is reduced by the layer A metal to obtain metal with metal activity weaker than that of the layer A metal, the metal and the layer A metal are combined to form a corrosion couple, the reaction is promoted to be carried out rightwards, the corrosion of the layer A metal is accelerated, and the completely degraded single-layer two-dimensional nanomaterial is obtained. The method disclosed by the invention is simple, strong in operability and good in realization result, and can be used for obtaining the Mxenes material with higher stripping degree and better micro-morphology.
Drawings
FIG. 1 is an X-ray diffraction pattern of the MAX starting material used in example 1 of the present invention.
FIG. 2 shows the X-ray diffraction pattern of the MXenes layered material obtained in example 1 of the present invention.
FIG. 3 is an SEM scanning electron microscope picture of the MXenes layered material prepared in example 1 of the present invention. Wherein, the product appearance after 1h of corrosion is shown in (a), the product appearance after 3h of corrosion is shown in (b), the product appearance after 6h of corrosion is shown in (c), the product appearance after 12h of corrosion is shown in (d), and the product appearance after 24h of corrosion is shown in (e).
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The method for preparing the layered MXenes material by utilizing the ternary MAX material comprises two main processes of preparation of the ternary MAX material and corrosion stripping of the MAX material, and specifically comprises the following steps:
(1) synthesis preparation of MAX Material: weighing raw materials M, A and X which accord with the stoichiometric ratio of the ternary MAX material, and a small amount of rare earth oxide (lanthanum oxide, cerium oxide, neodymium oxide, samarium oxide or europium oxide), wherein the using amount of M is 55-76 mol%, the using amount of A is 17-32 mol%, and the using amount of X is 4-13 mol%; putting the high-temperature flux and absolute ethyl alcohol into an alumina ball milling tank for ball milling, and uniformly mixing to obtain slurry; and (3) sieving the slurry subjected to ball milling, drying, and carrying out high-temperature reaction on the dried powder in a vacuum furnace under a protective atmosphere to obtain the ternary MAX material.
(2) Etching and stripping of MAX material: corroding the A phase in the ternary MAX material to obtain the Mxenes material, which specifically comprises the following steps: and (2) taking strong acid or strong base as corrosive liquid and placing the corrosive liquid into a reaction container, weighing MAX powder and placing the MAX powder into the corrosive liquid, keeping the temperature of the corrosive liquid at 4-60 ℃, adding strong stirring, stirring at the rotating speed of 200-1600 r/min, adding soluble mixed salt into the corrosive liquid in the process, and continuously corroding for 0.5-48 h to obtain a corroded mixture.
Wherein the strong base is NaOH aqueous solution; the strong acid is hydrofluoric acid and HNO3And one or more of hydrochloric acid.
The mass fraction of hydrofluoric acid is 40 percent, and HNO3The mass fraction of (3) is 40%, the mass fraction of hydrochloric acid is 40%, and the concentration of NaOH aqueous solution is 6 mol/L.
(3) Drying and collecting layered MXenes material: and (4) carrying out centrifugal separation on the corrosive mixture, repeatedly washing the obtained solid substance with deionized water for 8-10 times, and removing components of the corrosive liquid. And (4) putting the cleaned solid into an oven for drying to obtain the layered MXenes material.
In the step (1), the raw material M is one or more of Ti, Cr, Nb, V, Mo, Zr and Hf elements; the raw material A is one or more of Cd oxide, Al, Sn, In, Pb and Ga; the raw material X is a carbon simple substance or a compound containing N.
In the step (3), the added soluble metal mixed salt contains one to three salts, which are respectively one of titanium, zirconium, vanadium, manganese, zinc, gallium, cobalt, nickel, molybdenum, tin, lead, copper, mercury and silver salts, and the adding amount of the soluble metal mixed salt is 2 wt.% to 15 wt.% of the total amount of the corrosive liquid. When the soluble metal mixed salt is two salts, the molar ratio of the two salts is 1: 1. When the soluble metal mixed salt is three salts, the molar ratio of the three salts is 1:1: 1.
The invention is described only with reference to the starting materials used in example 1, example 9, but the MAX materials can be prepared from any of the starting materials M, a starting material a, and a starting material X listed in the present invention, and any of the other soluble salts listed can achieve the effect of promoting corrosion of the galvanic cell.
The following is a detailed description of specific examples.
Example 1
1) Mixing Ti, Al, C and Nb2O5And the composite K salt is ball-milled and mixed evenly by a wet method to obtain a mixture; specific raw material ratios are shown in table 1 below, and KCl in the complex potassium salt: k2SO4In a molar ratio of 2: 1, the dosage of the composite potassium salt is 2 times of the total weight of all other raw materials.
Table 1 example 1 weight percent of each raw material
And (3) preparing the mixture into slurry by using absolute ethyl alcohol, wherein the absolute ethyl alcohol: the mixture (mass ratio) is 2.2: 1; the slurry was ball milled for 2.5h and mixed well. Putting the mixed raw materials into a drying box, drying at 40 deg.C to prevent oxidation of the raw materials at excessive temperature, grinding and pulverizing the raw materials after ethanol is completely volatilized, putting into a corundum crucible, keeping the temperature at 1180 deg.C for 3h in a vacuum furnace, protecting with Ar gas, and cooling with the furnace to obtain Ti3AlC2Of the ternary MAX material.
2) Mixing Ti3AlC2After grinding and crushing the ternary MAX material (1 g) of the ternary MAX material powder, 1g of the ternary MAX material powder was added to 40mL of hydrofluoric acid with a mass fraction of 40% (mass fraction of commercially available hydrofluoric acid solute, corresponding to 22.5 mol/L. commercially available hydrofluoric acid was used here), and vigorous stirring was performed at a stirring speed of 800 r/min. Adding MnCl2And CuSO4，MnCl2And CuSO4The molar ratio of the two is 1:1, MnCl2And CuSO4Adding 7 wt.% of the total weight of the corrosive liquid, keeping the temperature at 45 ℃, and reacting for 24 hours to obtain a corroded mixture.
3) And (3) performing centrifugal separation on the corroded mixture, repeatedly cleaning the obtained solid with deionized water, removing corrosive liquid components, and drying the cleaned solid in an oven at 60 ℃ to obtain the layered MXenes material.
The crystalline phase composition and the micro-morphology of the layered MXenes material prepared in this example are shown in FIGS. 1-3.
Referring to fig. 1, it can be seen from fig. 1 that after the reaction, a TiAlC ternary MAX material is obtained.
Referring to fig. 2, it can be seen from fig. 2 that after etching a TiC binary MXenes material is obtained.
Referring to fig. 3, it can be seen from fig. 3 that the obtained binary MXenes material has a better layered structure.
Example 2
1) Mixing Cr, Al, C, Nb2O5And uniformly mixing the compound K salt by wet ball milling to obtain a mixture, wherein the specific raw material ratio is shown in the following table 2, and KCl in the compound potassium salt is as follows: k2SO4In a molar ratio of 1.8: 1, the dosage of the composite potassium salt is 2 times of the total weight of other raw materials.
Table 2 weight percent of each of the raw materials of example 2
And (3) preparing the mixture into slurry by using absolute ethyl alcohol, wherein the absolute ethyl alcohol: the mixture (mass ratio) is 2.2: 1; the slurry was ball milled for 2.5h and mixed well. Putting the mixed raw materials into a drying box, drying at 40 deg.C to prevent oxidation of the raw materials at excessive temperature, grinding and pulverizing the raw materials after ethanol is completely volatilized, putting into a corundum crucible, keeping the temperature of 1220 deg.C for 2.5h in a vacuum furnace, protecting with Ar gas, and cooling with the furnace to obtain Cr3AlC2Of the ternary MAX material.
2) Mixing Ti3AlC2The ternary MAX material is ground and crushed, 1g of ternary MAX material powder is added into 40mL of mixed acid liquid of hydrofluoric acid and hydrochloric acid with the mass fraction of 40%, strong stirring is carried out, and the stirring speed is 1000 r/min. Adding Ga2(SO4)3And Ti (OC)4H9)4Ga in a molar ratio of 1:12(SO4)3And Ti (OC 4H)9)4Adding 11 wt.% of the total mass of the corrosive liquid, keeping the temperature at 45 ℃, and reacting for 36 hours to obtain a corroded mixture.
3) And (4) performing centrifugal separation on the corroded mixture, repeatedly washing the obtained solid with deionized water, and removing corrosive liquid components. And (3) drying the cleaned solid in an oven at 60 ℃ to obtain the layered MXenes material.
Example 3
1) Mixing Ti, Mo, Al, C and Al2O3And uniformly mixing the compound K salt by wet ball milling to obtain a mixture, wherein the specific raw material ratio is shown in the following table 3, and KCl in the compound potassium salt is as follows: k2SO4In a molar ratio of 4: 1, the dosage of the composite potassium salt is 2 times of the total weight of other raw materials.
Table 3 weight percent of each of the raw materials of example 3
| Ti | Mo | Al | C | Al2O3 | Total of | |
| wt.％ | 24 | 32.5 | 27 | 12 | 4.5 | 100 |
And (3) preparing the mixture into slurry by using absolute ethyl alcohol, wherein the absolute ethyl alcohol: the mixture (mass ratio) is 2.2: 1; the slurry was ball milled for 2.5h and mixed well. Placing the mixed raw materials into a drying oven, drying at 40 deg.C to prevent oxidation of the raw materials, grinding and pulverizing the raw materials after ethanol completely volatilizes, placing into a corundum crucible, maintaining at 1250 deg.C for 2 hr in a vacuum furnace under protection of Ar gas, and furnace cooling to obtain (Ti, Mo)3AlC2Of the ternary MAX material.
2) Mixing Ti3AlC2Grinding and crushing the ternary MAX material, then adding 1g of ternary MAX material powder into 35mL of mixed acid liquid of hydrofluoric acid and hydrochloric acid with the mass fraction of 40%, and performing strong stirring at the stirring speed of 1200 r/min. Adding Zn (NO)3)2And Zr (SO)4)2Zn (NO) with the molar ratio of 1:13)2And Zr (SO)4)2Adding 2 wt.% of the total mass of the corrosive liquid, keeping the temperature at 45 ℃, and reacting for 36 hours to obtain a corroded mixture.
3) And (4) performing centrifugal separation on the corroded mixture, repeatedly washing the obtained solid with deionized water, and removing corrosive liquid components. And (3) drying the cleaned solid in an oven at 60 ℃ to obtain the layered MXenes material.
Example 4
1) Mixing Ti, Sn, C and V2O3、Nb2O5And uniformly mixing the compound K salt by wet ball milling to obtain a mixture, wherein the specific raw material ratio is shown in the following table 3, and KCl in the compound potassium salt is as follows: k2SO4In a molar ratio of 5:1, the dosage of the composite potassium salt is 2.4 times of the total weight of other raw materials.
Table 4 weight percent of each of the raw materials of example 4
| Ti | Sn | C | V2O5 | Nb2O5 | Total of | |
| wt.％ | 58 | 26.5 | 12 | 2 | 1.5 | 100 |
And (3) preparing the mixture into slurry by using absolute ethyl alcohol, wherein the absolute ethyl alcohol: the mixture (mass ratio) is 2.2: 1; the slurry was ball milled for 2.5h and mixed well. Putting the mixed raw materials into a drying box, drying at 40 deg.C to prevent oxidation of the raw materials at excessive temperature, grinding and pulverizing the raw materials after ethanol is completely volatilized, putting into a corundum crucible, keeping the temperature of 1150 deg.C for 3h in a vacuum furnace, protecting with Ar gas, and cooling with the furnace to obtain Ti3SnC2Of the ternary MAX material.
2) Mixing Ti3SnC2Grinding and crushing the ternary MAX material, then adding 1g of ternary MAX material powder into 55mL of mixed acid liquid of hydrofluoric acid with the mass fraction of 40% and nitric acid, and carrying out strong stirring at the stirring speed of 1400 r/min. Adding Pb (NO)3)2And AgNO3Molar ratio of 1:1, Pb (NO)3)2And AgNO3Adding 15 wt.% of the total mass of the corrosive liquid, keeping the temperature at 55 ℃, and reacting for 32 hours to obtain a corroded mixture.
3) And (4) carrying out centrifugal separation on the corrosion mixture, repeatedly washing the obtained solid with deionized water, and removing the components of the corrosion solution. And (3) drying the cleaned solid in an oven at 60 ℃ to obtain the layered MXenes material.
Example 5
1) The ternary MAX material was prepared by the following procedure: putting the raw material M, the raw material A, the raw material X, the high-temperature flux and absolute ethyl alcohol into an alumina ball milling tank for ball milling, and uniformly mixing to obtain slurry; sieving the slurry subjected to ball milling, drying, and carrying out high-temperature reaction on the dried powder in a vacuum furnace under a protective atmosphere to obtain a ternary MAX material;
wherein the raw material M is Ti; the raw material A is Pb; the raw material X is a carbon simple substance. The protective atmosphere is hydrogen. The high temperature solvent is KCl and K2SO4And KCl with K2SO4In a molar ratio of 0.5: 1; the high-temperature reaction is carried out at the temperature of 800 ℃ for 4 h.
2) Adding corrosive liquid into a plastic container, adding ternary MAX material powder into the corrosive liquid, corroding for 48 hours at 4 ℃ under the stirring of 200r/min, and adding Cu (NO)3)2And AgNO3The molar ratio of the two is 1:1, Cu (NO)3)2And AgNO3Adding 15 wt% of the total weight of the corrosive liquid, washing and drying to obtain the layered MXenes material. The raw material A is an oxide of Al and Sn.
Wherein the corrosive liquid is hydrofluoric acid.
Example 6
1) The ternary MAX material was prepared by the following procedure: putting the raw material M, the raw material A, the raw material X, the high-temperature flux and absolute ethyl alcohol into an alumina ball milling tank for ball milling, and uniformly mixing to obtain slurry; sieving the slurry subjected to ball milling, drying, and carrying out high-temperature reaction on the dried powder in a vacuum furnace under a protective atmosphere to obtain a ternary MAX material;
wherein the raw material M is Cr; the raw material A is Ga; the raw material X isSimple substance of carbon. The protective atmosphere was nitrogen. The high temperature solvent is KCl and K2SO4And KCl with K2SO4In a molar ratio of 8: 1; the high temperature reaction temperature is 1350 ℃ and the time is 0.5 h.
2) Adding corrosive liquid into a plastic container, adding ternary MAX material powder into the corrosive liquid, corroding for 2h at the temperature of 20 ℃ under the stirring of 200r/min, and adding Ni (NO)3)2、Co(NO3)2And CuSO4The molar ratio of the three is 1:1:1, Ni (NO3)2、Co(NO3)2And CuSO4Adding 15 wt% of the total weight of the corrosive liquid, washing and drying to obtain the layered MXenes material.
Wherein the corrosive liquid is HNO3。
Example 7
1) The ternary MAX material was prepared by the following procedure: putting the raw material M, the raw material A, the raw material X, the high-temperature flux and absolute ethyl alcohol into an alumina ball milling tank for ball milling, and uniformly mixing to obtain slurry; sieving the slurry subjected to ball milling, drying, and carrying out high-temperature reaction on the dried powder in a vacuum furnace under a protective atmosphere to obtain a ternary MAX material;
wherein the raw material M is a mixture of Nb and V; the raw material A is a mixture of Sn and In; the raw material X is a carbon simple substance. The protective atmosphere was argon. The high temperature solvent is KCl and K2SO4And KCl with K2SO4The molar ratio of (A) to (B) is 0.5-8: 1; the high-temperature reaction is carried out at 1000 ℃ for 2 h.
2) Adding corrosive liquid into a plastic container, adding ternary MAX material powder into the corrosive liquid, corroding for 25h at the temperature of 60 ℃ under the stirring of 500r/min, and adding Pb (NO)3)2、Cu(NO3)2And AgNO3The molar ratio of the three is 1:1:1, Pb (NO)3)2、Cu(NO3)2And AgNO3And (3) adding 11.5 wt% of the total weight of the corrosive liquid, washing and drying to obtain the layered MXenes material.
Wherein, the corrosive liquid is NaOH aqueous solution.
Example 8
1) The ternary MAX material was prepared by the following procedure: putting the raw material M, the raw material A, the raw material X, the high-temperature flux and absolute ethyl alcohol into an alumina ball milling tank for ball milling, and uniformly mixing to obtain slurry; sieving the slurry subjected to ball milling, drying, and carrying out high-temperature reaction on the dried powder in a vacuum furnace under a protective atmosphere to obtain a ternary MAX material;
wherein the raw material M is a mixture of Mo, Zr and Hf; the raw material A is Cd oxide; the raw material X is NH4HCO3(ii) a The protective atmosphere was argon. The high temperature solvent is KCl and K2SO4And KCl with K2SO4In a molar ratio of 5: 1; the high-temperature reaction temperature is 1250 ℃ and the time is 1 h.
2) Adding corrosive liquid into a plastic container, adding ternary MAX material powder into the corrosive liquid, corroding for 15h at 10 ℃ under stirring at 1600r/min, and adding Pb (NO)3)2、Cu(NO3)2And AgNO3The molar ratio of the three is 1:1:1, Pb (NO)3)2、Cu(NO3)2And AgNO3And (3) adding 8.5 wt% of the total weight of the corrosive liquid, washing and drying to obtain the layered MXenes material.
Wherein the corrosive liquid is hydrofluoric acid.
Example 9
1) The ternary MAX material was prepared by the following procedure: putting the raw material M, the raw material A, the raw material X, the high-temperature flux and absolute ethyl alcohol into an alumina ball milling tank for ball milling, and uniformly mixing to obtain slurry; sieving the slurry subjected to ball milling, drying, and carrying out high-temperature reaction on the dried powder in a vacuum furnace under a protective atmosphere to obtain a ternary MAX material;
wherein the raw material M is a mixture of Zr and Hf; the raw material A is Zn and Ga; the starting material X is (NH)4)2CO3(ii) a The protective atmosphere is hydrogen, nitrogen or argon. The high temperature solvent is KCl and K2SO4And KCl with K2SO4The molar ratio of (A) to (B) is 0.5-8: 1; the high-temperature reaction is carried out at the temperature of 11000 ℃ for time of1h。
2) Adding corrosive liquid into a plastic container, adding ternary MAX material powder into the corrosive liquid, corroding for 0.5h at 30 ℃ under the stirring of 700r/min, and adding Pb (NO)3)2、Ni(NO3)2And CuSO4The molar ratio of the three is 1:1:1, Pb (NO)3)2、Ni(NO3)2And CuSO4And (3) adding 4.5 wt% of the total weight of the corrosive liquid, washing and drying to obtain the layered MXenes material.
Wherein the corrosive liquid is hydrofluoric acid.
Claims (3)
1. A method for preparing a layered MXenes material by using a ternary MAX material is characterized by comprising the steps of placing strong acid or strong base serving as corrosive liquid into a reaction container, placing MAX powder into the corrosive liquid, adding soluble mixed salt while stirring, continuously corroding for 0.5-48 hours, then carrying out centrifugal separation, cleaning and drying to obtain the layered MXenes material;
the temperature of the corrosive liquid is 4-60 ℃; stirring at a rotation speed of 200-1600 r/min;
the strong base is NaOH aqueous solution, and the concentration of the NaOH aqueous solution is 6 mol/L; the strong acid is hydrofluoric acid and HNO3One or more of hydrochloric acid; the mass fraction of hydrofluoric acid is 40%; HNO3The mass fraction of the hydrochloric acid is 40 percent, and the mass fraction of the hydrochloric acid is 40 percent;
the adding amount of the soluble metal mixed salt is 2-15% of the total mass of the corrosion liquid;
the soluble metal mixed salt is one, two or three of titanium, zirconium, vanadium, manganese, zinc, gallium, cobalt, nickel, molybdenum, tin, lead, copper and silver salt;
the metal activity of the metal in the soluble metal mixed salt is weaker than that of the metal in the layer A in MAX;
HNO3the mass fraction of (3) is 40%, the mass fraction of hydrochloric acid is 40%, and the concentration of NaOH aqueous solution is 6 mol/L.
2. The method of claim 1, wherein the soluble metal mixed salt is two salts, and the molar ratio of the two salts is 1: 1.
3. The method of claim 1, wherein the soluble metal mixed salt is three salts, and the molar ratio of the three salts is 1:1: 1.
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| CN111634914B (en) * | 2020-06-12 | 2021-10-22 | 陕西科技大学 | Preparation method of M-site vanadium-doped MXene |
| CN112226644B (en) * | 2020-09-25 | 2021-12-28 | 河海大学 | MXene reinforced copper-based composite material and preparation method thereof |
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