Method for preparing Ti2CTx from fuse salt

A technology of molten salt and potassium fluoride is applied in the field of preparation of new two-dimensional transition metal carbide Ti2CTx to achieve the effects of improving specific capacity and adsorption capacity, simple operation and high efficiency

Inactive Publication Date: 2018-11-23
HUBEI UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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  • Method for preparing Ti2CTx from fuse salt
  • Method for preparing Ti2CTx from fuse salt
  • Method for preparing Ti2CTx from fuse salt

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Embodiment 1

[0026] Ti 2 The mass ratio of the four raw materials of AlC powder, potassium fluoride, lithium fluoride and sodium fluoride is Ti 2 AlC:KF:LiF:NaF=1:0.59:0.29:0.12; mix evenly, put it into a tube furnace for calcination, and use argon protection. The heating rate is 10°C / min, the temperature is 550°C, and the temperature is kept for 50 minutes to obtain a molten salt product.

[0027] Take 1 gram of the molten salt product and add it to 10 milliliters of 4mol / L sulfuric acid solution and stir for 1 hour. After the reaction, add deionized water and repeatedly centrifuge and wash until the supernatant pH ≈ 7. Pour off the supernatant to obtain a precipitate; take 0.3 grams Mix the precipitate with 6 ml of ammonia water and stir for 1 hour, add deionized water and wash repeatedly by centrifugation for 4 to 5 times, after adding deionized water for the last time, sonicate for 60 minutes, and centrifuge at 6000rpm for 25 minutes, and collect the supernatant suspension with a filt...

Embodiment 2

[0029] Ti 2 The mass ratio of the four raw materials of AlC powder, potassium fluoride, lithium fluoride and sodium fluoride is Ti 2 AlC:KF:LiF:NaF=1:0.59:0.22:0.19; mix well, put into tube furnace for calcination. The heating rate is 10°C / min, the temperature is 650°C, and the temperature is kept for 40 minutes to obtain the molten salt product.

[0030] Take 1 gram of the molten salt product and add it to 10 milliliters of 4mol / L sulfuric acid solution and stir for 1 hour. After the reaction, add deionized water and repeatedly centrifuge and wash until the supernatant pH ≈ 7. Pour off the supernatant to obtain a precipitate; take 0.3 grams Mix the precipitate with 6 ml of ammonia water and stir for 1 hour, add deionized water to wash repeatedly by centrifugation for 4 to 5 times, add deionized water for the last time, and then sonicate for 60 minutes, and centrifuge at 6000rpm for 30 minutes, and collect the supernatant suspension with a filter membrane Particles in the la...

Embodiment 3

[0032] Ti 2 The mass ratio of the four raw materials of AlC powder, potassium fluoride, lithium fluoride and sodium fluoride is Ti 2 AlC:KF:NaF=1:0.675:0:0.325 (that is, there is no lithium fluoride, only Ti 2 AlC powder, potassium fluoride, sodium fluoride three raw materials); mix evenly, put into tube furnace for calcination. The heating rate is 10°C / min, the temperature is 850°C, and the temperature is kept for 30 minutes to obtain the molten salt product.

[0033] Take 1 gram of the molten salt product and add it to 10 milliliters of 4mol / L sulfuric acid solution and stir for 1 hour. After the reaction, add deionized water and repeatedly centrifuge and wash until the supernatant pH ≈ 7. Pour off the supernatant to obtain a precipitate; take 0.3 grams Mix the precipitate with 6 ml of ammonia water and stir for 1 hour, add deionized water and wash repeatedly by centrifugation for 4 to 5 times, after adding deionized water for the last time, sonicate for 60 minutes, and ce...

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Abstract

The invention provides a method for preparing Ti2CTx from fuse salt and performing positive ion intercalation. The method comprises the steps: weighing the raw materials of Ti2AlC powder, potassium fluoride, lithium fluoride and sodium fluoride according to a mass ratio of 1 to (0.58 to 0.675) to (0 to 0.3) to (0.12 to 0.325), evenly mixing, putting into a tubular furnace to be roasted and utilizing argon for protection; heating to 550 to 850 DEG C at a temperature rise rate of 10 DEG C/min and keeping warm for 30 to 50 min; finishing roasting, naturally cooling and obtaining a fuse salt product; adding the fuse salt product into 4 mol/L sulfuric acid, stirring for 1 h under the normal temperature, adding deionized water, centrifugally washing until a pH of liquid supernatant is about 7 and pouring out the liquid supernatant to obtain precipitate; adding the precipitate into ammonium hydroxide, stirring for 1 h under the normal temperature, then adding deionized water, centrifugally washing 4 to 5 times and pouring out the liquid supernatant to obtain precipitate; adding the precipitate into deionized water, performing ultrasonic treatment for 60 min, centrifuging for 25 to 45 minunder the rotation speed of 6000 rpm and filtering upper-layer suspension liquid to obtain a layered Ti2CTx material. The method breaks through a traditional chemical liquid phase etching method for preparing Ti2CTx, and a preparation method which has the advantages safety in operation, simpleness and high efficiency is provided.

Description

technical field [0001] The invention belongs to the field of advanced ceramic materials and relates to a novel two-dimensional transition metal carbide Ti 2 CT x method of preparation. Background technique [0002] Ti 2 CT x It belongs to one of the two-dimensional materials MXene, which is a new type of transition metal carbide or nitride, and its general formula is M n+1 x n T x (n=1-3), wherein M is an early transition metal, X is C or N, T x Refers to surface functional groups, generally hydroxyl, oxygen or fluorine [1] . MXene is usually prepared by selective etching of the A atomic layer in the MAX phase of the ternary layered compound with a strong acid, and has a two-dimensional structure similar to graphene. Preparation of Ti 2 CT x The precursor Ti 2 AlC is a MAX phase ceramic material, and A is mainly group III and IV main group elements. This type of compound has a hexagonal layered structure and belongs to P 63 / mmc space group. at Ti 2 In the str...

Claims

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Application Information

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IPC IPC(8): C04B35/56C04B35/622
CPCC04B35/5618C04B35/622C04B2235/445
Inventor 严明杨磊张晨邹云麒李超
Owner HUBEI UNIV OF TECH
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