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A method for prepare a nitrogen doped carbon nanotube three-dimensional composite material by in-situ growth of a small lay of titanium carbide

A nitrogen-doped carbon, in-situ growth technology, used in electrical components, battery electrodes, circuits, etc., can solve the problems of high price and lack of firmness of CNTs, and achieve the effect of improving transmission capacity, improving conductivity and low cost.

Inactive Publication Date: 2019-01-08
UNIV OF JINAN
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Problems solved by technology

[0005] The document "Peng Yu, Yanwei Ma; Nanoscale, 2018, 10: 5906-5913" reported that the dispersion of few-layer titanium carbide and the dispersion of CNTs were thoroughly mixed by ultrasonic treatment, and then the mixture was filtered and dried to obtain d-Ti 3 C 2 / CNT composite film; but the price of commercial CNTs is relatively high, and the combination of the two is not as firm as the in situ growth

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  • A method for prepare a nitrogen doped carbon nanotube three-dimensional composite material by in-situ growth of a small lay of titanium carbide
  • A method for prepare a nitrogen doped carbon nanotube three-dimensional composite material by in-situ growth of a small lay of titanium carbide
  • A method for prepare a nitrogen doped carbon nanotube three-dimensional composite material by in-situ growth of a small lay of titanium carbide

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Effect test

Embodiment 1

[0038] First, the 3 g ternary layered Ti 3 AlC 2 The ceramic powder is slowly immersed in 50 mL of hydrofluoric acid solution (40 wt.%) and magnetically stirred at 50°C for 72 h at a speed of 500 r / min, and then the corrosion products are centrifuged, 8000 r / min with absolute ethanol After centrifugation and cleaning until the pH of the supernatant is 6, the resulting precipitate is dried in a vacuum drying oven at 60°C for 24 hours to obtain a two-dimensional layered titanium carbide nanopowder. Then, 0.2 g of titanium carbide nanopowder was added to 10 mL of tetramethylammonium hydroxide solution (25wt.%), heated and stirred at 30 ℃ for 24 h, then centrifuged, and then centrifuged with deionized water to obtain a few layers of titanium carbide Nanosheet dispersion, the dispersion concentration is about 1 mg / mL. Take 125 mL of small-layer titanium carbide nanosheet dispersion, add 0.25 g of cobalt acetate tetrahydrate, and ultrasonically disperse for 30 min with an ultrasonic ...

Embodiment 2

[0041] First, the 3 g ternary layered Ti 3 AlC 2 The ceramic powder is slowly immersed in 50 mL of hydrofluoric acid solution (40 wt.%), magnetically stirred at 50°C for 72 h at a speed of 500 r / min, and then the corrosion products are centrifuged, 8000 r / min with ultrapure The supernatant was washed by centrifugation with water until the pH of the supernatant was 6, and then washed with absolute ethanol for 5 times. The resulting precipitate was dried in a vacuum drying oven at 60°C for 24 h to obtain a two-dimensional layered titanium carbide nanopowder. Then, 0.2 g of titanium carbide nanopowder was added to 10 mL of tetramethylammonium hydroxide solution (25 wt.%), heated and stirred at 30 ℃ for 24 h, and then centrifuged, and then centrifuged with deionized water to obtain less layer carbonization Titanium nanosheet dispersion, the dispersion concentration is about 1 mg / mL. Take 100 mL of the dispersion of titanium carbide nanosheets with few layers and add 0.2 g C 4 H 6 C...

Embodiment 3

[0043] First, add 3 g of ternary layered Ti 3 AlC 2 The ceramic powder is slowly immersed in 50 mL of hydrofluoric acid solution (40 wt.%), magnetically stirred at 50°C for 72 h at a speed of 500 r / min, and then the corrosion products are centrifuged, 8000 r / min with ultrapure The supernatant was washed by centrifugation with water until the pH of the supernatant was 6, and then washed with absolute ethanol for 5 times. The resulting precipitate was dried in a vacuum drying oven at 60°C for 24 h to obtain a two-dimensional layered titanium carbide nanopowder. Then, 0.2 g of titanium carbide nanopowder was added to 5 mL of tetramethylammonium hydroxide solution (25 wt.%), heated and stirred at 30 ℃ for 24 h, and then centrifuged, and then centrifuged with deionized water to obtain less layer carbonization Titanium nanosheet dispersion, the dispersion concentration is about 1 mg / mL. Take 200 mL of small-layer titanium carbide nanosheet dispersion, add 0.4 g of cobalt chloride he...

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Abstract

The invention belongs to the technical field of preparation of nano-functional materials, in particular to a method for preparing a nitrogen doped carbon nanotube three-dimensional composite materialby in-situ growth of a few layers of titanium carbide, immersing ternary layered Ti3AlC2 ceramic powder in hydrofluoric acid solution, heating and stirring, centrifugally cleaning with ultrapure waterand absolute ethanol, drying to obtain two-dimensional layered titanium carbide nano-powder, adding it into tetramethylammonium hydroxide solution, heating and stirring, centrifuging with deionized water to obtain a few layers of titanium carbide nano-sheet dispersion; Adding cobalt salt into a dispersion of a few layers of titanium carbide nano-sheets for reaction, adding dicyandiamide, heatingand stirring until dicyandiamide is completely dissolved, freezing, and freeze-drying to obtain precursor powder; Nitrogen-doped carbon nanotubes (CNTs) three-dimensional composites were prepared by in-situ growth of a few layers of titanium carbide after grinding the precursor powder and heat treatment. A three-dimensional composite material is prepared by a simple pyrolysis method using a few layers of titanium carbide as a carrier, cobalt as a catalyst, dicyandiamide as a carbon and nitrogen source, and the electrochemical performance of the few layers of titanium carbide can be improved.

Description

Technical field [0001] The invention belongs to the technical field of preparation of nano-functional materials, and particularly relates to a preparation method of a three-dimensional composite material of nitrogen-doped carbon nanotubes grown in situ with a few layers of titanium carbide. Background technique [0002] Transition metal carbide or carbon / nitride MXenes is a new member of the two-dimensional material world, and its structure is similar to graphene. MXene is prepared by selective etching-assisted liquid phase stripping method, which removes the A layer elements in the MAX phase by etching, and can keep the original MX structure unchanged, and has excellent electrical, optical and mechanical properties. Compared with traditional two-dimensional materials, MXenes has metal-like conductivity, and the abundant -F, -OH and other functional groups on the surface also endow it with excellent chemical reactivity and hydrophilicity. It is expected to be an ideal for constru...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/62
CPCH01M4/62Y02E60/10
Inventor 原长洲谭可刘洋侯林瑞
Owner UNIV OF JINAN
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