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Preparation method of M-site doped vanadium MXene

A vanadium-based, powder-based technology, applied in the field of preparation of two-dimensional layered materials, can solve the problems of limited material performance control, V-layer doping, simultaneous doping, etc., to achieve improved liquid phase stripping ability, process controllable, promote the lifting effect

Active Publication Date: 2020-09-08
SHAANXI UNIV OF SCI & TECH
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Problems solved by technology

[0004] The Chinese patent "An MXene material and its preparation method and application" with the application number CN201910847191.8 mixed MAX phase materials, transition metal bromides and / or transition metal iodides, and performed high-temperature reactions to obtain Br or I The MXene material, which is a surface group, has unique electrochemical properties, but it does not realize the doping of the V layer, and the performance control of the material is limited; the Chinese patent application number CN201510164821.3 "A porous two-dimensional transition Metal carbide and preparation method thereof " have set forth (V 1-x Cr x ) 2 The preparation process of AlC ceramic powder was obtained by liquid phase etching (V 1-x Cr x ) 2 CT x , to achieve V-doped Cr two-phase solid solution, but obviously, it can not achieve simultaneous doping of two elements in the V phase to prepare M-site doped V 2 CT x

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  • Preparation method of M-site doped vanadium MXene

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preparation example Construction

[0022] A preparation method of M-site doped vanadium-based MXene, comprising the following steps:

[0023] Step 1: Mix metal powder, aluminum powder, carbon powder and molten salt in a certain proportion to make powder. The mixing ratio of metal powder, aluminum powder, carbon powder and mixed molten salt is the molar ratio (2-2.3): (1.05~1.2): (1~1.1): (5~25), wherein the metal powder is a three-mixed powder formed by V powder and any two of Ti, Cr, Mo, Zr, and Nb powders, and V powder is required to be in The molar proportion of the three-phase mixed powder is greater than 50%. The mixed molten salt is a mixture of sodium chloride and potassium chloride in any proportion, and it needs to be mixed and recrystallized before use, that is, the weighed mixed molten salt is dissolved in A small amount of water, then heat and evaporate the water to obtain crystalline salt, and finally grind and refine to obtain the final usable mixed molten salt. The carbon powder is any one of gra...

Embodiment 1

[0027] Metal powder (containing 80% V powder, 5% Ti powder and 15% Cr powder), aluminum powder, graphite powder and molten salt (sodium chloride: potassium chloride = 2:1) according to 2:1.05:1.1:5 Mix the ratio of powder 1 to make powder 1; then put powder 1 in a mortar, add 10ml of deionized water and grind it under air condition for 5 minutes to make it preliminarily mix, and then transfer it to a ball mill tank for ball milling for 6 hours to get powder 2 , and then put the powder 2 in a magnetic boat and sinter at 960°C for 3 hours under the atmosphere (95% argon, 5% carbon dioxide) to obtain the M-site doped MAX phase, which is recorded as MAX phase powder 1; take 5g of the MAX phase Powder 1 was added to 30ml of lithium fluoride hydrochloride solution, followed by magnetic stirring at 30°C for 12 hours. After completion, it was cleaned, centrifuged, and dried to obtain the M-site solid-solution doped MXene material. We doped the synthesized M-site Ti and Cr dual element...

Embodiment 2

[0029] Metal powder (containing 90% V powder, 5% Zr powder and 5% Ti powder), aluminum powder, conductive carbon black and molten salt (sodium chloride: potassium chloride = 1:1) according to 2.3:1.2:1.05: The ratio of 25 was mixed to make powder 1; then powder 1 was placed in a mortar, 18ml of ethanol was added, and it was ground for 8 minutes under air conditions for preliminary mixing, and then transferred to a ball mill jar for ball milling for 3 hours to obtain powder 2. Finally, put the powder 2 in a magnetic boat and sinter at a high temperature of 1430°C for 4 hours under the atmosphere (argon 95%, hydrogen 5%) to obtain the M-site doped MAX phase, which is designated as MAX phase powder 1; take 8g of MAX phase powder Body 1 was added to 32ml of hydrofluoric acid solution, followed by magnetic stirring at 20°C for 24 hours, after completion, it was cleaned, centrifuged, and dried to obtain the M-site solid-solution doped MXene material. The XRD analysis of the synthesi...

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Abstract

The invention discloses a preparation method of M-site doped vanadium MXene. The preparation method comprises the following steps: mixing metal powder, aluminum powder, carbon powder and fused salt according to a certain proportion to prepare powder; then putting the powder into a mortar, adding a grinding fluid, and grinding for 3-8 minutes under an air condition so that the powder is primarily mixed; transferring into a ball milling tank and carrying out ball milling for 3-6 hours to obtain powder; then putting the powder into a magnetic boat for high-temperature atmosphere sintering to obtain M-site doped MAX-phase powder; and mixing the M-site doped MAX-phase powder with an etching agent according to a certain ratio, then magnetically stirring at 20-35 DEG C for 12-36 hours, cleaning,centrifugally separating and drying to obtain M-site doped V2CTxMXene. The MXene powder material prepared by the method has the characteristics of high purity, multiple hybrid sites and the like, canbe subjected to structure fine adjustment according to working condition requirements, and has a wide application prospect in the field of electrochemistry.

Description

technical field [0001] The invention relates to a method for preparing a two-dimensional layered material, in particular to a method for preparing an M-site ternary doped vanadium-based MXene. Background technique [0002] A series of two-dimensional nanomaterials with similar structures (collectively referred to as MXene materials) can be prepared based on the selective corrosion of layer A atoms in MAX phase powders combined with liquid phase exfoliation. This kind of material has a variety of electrical, magnetic, thermoelectric properties and excellent electrochemical, heavy metal ion adsorption, gas adsorption and other characteristics, and has very broad application prospects in the fields of ion batteries, supercapacitors, sewage treatment, hydrogen storage, etc. Therefore, the preparation of MXene materials by corrosion exfoliation of MAX phase powders has become one of the hotspots in the field of two-dimensional nanomaterials research in recent years. [0003] V ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/907
CPCC01P2004/20C01B32/907
Inventor 刘毅罗威郭守武朱建锋张利锋霍京浩王晓飞
Owner SHAANXI UNIV OF SCI & TECH
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