Method for preparing graphene-like two-dimensional laminar titanium carbide nanoplate

A two-dimensional titanium carbide and two-dimensional layered technology, which is applied in the field of synthesizing graphene-like two-dimensional layered titanium carbide nanosheets, can solve problems that affect the application of two-dimensional titanium carbide nanosheets, the layer is not smooth enough, and the layer conductance Reduced efficiency and other issues, to achieve the effect of low cost, controllable process and high efficiency

Inactive Publication Date: 2014-09-03
HOHAI UNIV
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  • Abstract
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Problems solved by technology

The preparation of two-dimensional layered structure materials by chemical liquid phase exfoliation has the characteristics of simple process, controllable process, high efficiency and low cost, but the three-dimensional layered Ti 3 AlC 2 After the Al atomic layer in the phase is stripped, the two-dimensional titanium carbide nanosheets prepared by the chemical liquid phase method inevitably have serious structural defects, as shown in the literature (Chang F., et al., Mater.Lett., 2013, 109, 295-297) prepared two-dimensional titanium carbide nanosheets with many lattice defects, and the layers are not smooth enough
Ti prepared by this method 3 C 2 The conductivity of the layer will decrease with the increase of defects
At the same time, Ti 3 AlC 2 After chemical reaction with HF in aqueous solution, Ti 3 C 2 A large number of OH functional groups will be adsorbed on the surface of the layer, and the increase of this functional group will further aggravate the deterioration of the electrical conductivity, which will affect the application of two-dimensional titanium carbide nanosheets in terms of electrical and electrochemical properties.

Method used

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  • Method for preparing graphene-like two-dimensional laminar titanium carbide nanoplate

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Embodiment 1

[0025] By Ti: Al: C = 3: 1: 2 molar ratio batching, its mixture and agate balls are dry-mixed in a ball mill tank for 10 hours at a ball-to-material ratio of 2: 1; put the uniformly mixed batching into a graphite mold Compact under a pressure of 5MPa, then place it in an argon-protected hot-press furnace, raise the temperature of the hot-press furnace to 1350°C at a rate of 15°C / min, then keep it at a pressure of 25MPa for 25 minutes, and cool to 60°C After getting loose bulk Ti 3 AlC 2 , after being crushed and ground through a 200-mesh sieve, Ti 3 AlC 2 powder. 8 g of Ti 3 AlC 2 Soak the powder in 100mL of 50wt% HF aqueous solution at room temperature, and react with magnetic stirring at a speed of 1500r / min for 20 hours to obtain a suspension; Wash with ethanol several times, then centrifuge at 5000r / min for 20 minutes to remove larger particles, then centrifuge at 8000r / min for 10 minutes and dry in a vacuum dryer at 40°C for 24 hours; place the vacuum-dried powder i...

Embodiment 2

[0027] According to the molar ratio of Ti: Al: C = 3: 1: 2, dry mix with agate balls in the ball mill tank for 8 hours according to the ball-to-material ratio of 2: 1; put the evenly mixed ingredients into the graphite mold under the pressure of 10MPa Compacted under the pressure, then placed in an argon-protected hot-press furnace, heated to 1300°C at a rate of 10°C / min, kept at a pressure of 30MPa for 20 minutes, and cooled to 60°C to obtain loose block Ti 3 AlC 2 , after being crushed and ground through a 200-mesh sieve; 6 grams of Ti 3 AlC 2 Soak the powder in 100ml of 50wt% HF aqueous solution at room temperature, and react with magnetic stirring at a speed of 2000r / min for 40 hours; the obtained suspension is filtered and washed repeatedly until the pH value is neutral, and then washed with absolute ethanol several times , and then centrifuged at 4000r / min for 30 minutes to remove larger particles, then centrifuged at 8000r / min for 10 minutes and then dried in a vacuum...

Embodiment 3

[0029] According to the molar ratio of Ti: Al: C = 3: 1: 2, dry mix with agate balls in a ball-to-material ratio of 2: 1 in a ball mill for 12 hours; put the uniformly mixed ingredients into a graphite mold under a pressure of 5 MPa Compacted under the pressure, then placed in an argon-protected hot-press furnace, heated to 1400°C at a rate of 20°C / min, kept at a pressure of 20MPa for 30 minutes, and cooled to 55°C to obtain loose block Ti 3 AlC 2 , after being crushed and ground through a 200-mesh sieve; 10 grams of Ti 3 AlC 2 The powder is soaked in 100 ml of 50wt% HF aqueous solution at 50°C, and reacted with magnetic stirring at a speed of 1000r / min for 6 hours; the obtained suspension is filtered and washed repeatedly until the pH value is neutral, and then washed with absolute ethanol several times , and then centrifuged at 5000r / min for 20 minutes to remove larger particles, then centrifuged at 10000r / min for 10 minutes and then dried in a vacuum dryer at 60°C for 24 ...

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Abstract

The invention discloses a method for preparing a graphene-like two-dimensional laminar titanium carbide nanoplate. The method comprises the following steps: preparing Ti3AlC2 powder by an in-situ hot-pressing solid-liquid reaction; preparing two-dimensional titanium carbide by a chemical liquid phase reaction; performing vacuum calcination post-treatment, and the like. The method can be used for preparing a Ti3AlC2 precursor with excellent crystallinity and high purity under simple process flow, stable process parameters, controllable process, high efficiency, low cost, short time and low pressure; the information that the transverse size of the two dimensional Ti3AlC2 nanoplate prepared by the method can be 5-10 microns, the average thickness of a single layer is about 10-20 nanometers can be found from an SEM picture, the inter-laminar spacing is remarkably enlarged after calcination treatment, and the laminar surface is regular and smooth.

Description

technical field [0001] The invention belongs to the technical field of preparation of nanomaterials, and in particular relates to a method for synthesizing graphene-like two-dimensional layered titanium carbide nanosheets. Background technique [0002] Since the discovery of graphene by Novoselov and Geim et al., the synthesis, performance and application of two-dimensional materials have become the most important research fields of material scientists, and a new wave of research on two-dimensional materials has been set off in the academic community. After the material structure is changed from three-dimensional to two-dimensional, it shows a unique surface structure and electronic properties, and has excellent mechanical, thermal, electrical and optical properties. For example, graphene, which can be obtained by exfoliating layered graphite with a simple micromechanical exfoliation method, has properties such as high light transmittance, high thermal conductivity, high ele...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/30B82Y30/00B82Y40/00C01B32/921
Inventor 张建峰王红兵吴玉萍
Owner HOHAI UNIV
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