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Method for preparing two-dimensional hafnium carbide nanosheets

A technology of hafnium carbide and nanosheets, which is applied in the field of preparation of two-dimensional hafnium carbide nanosheets, can solve the problems of unreported preparation process, increased energy consumption and cost, and high equipment requirements, and achieves simple and easy-to-operate process methods and reduced preparation costs. The effect of low cost and equipment requirements

Inactive Publication Date: 2018-01-12
CHONGQING JIAOTONG UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Two-dimensional HfC nanosheets are a kind of low-dimensional HfC nanomaterials, and their preparation process has hardly been reported.
This method has high requirements on raw materials, and ball milling is required for pretreatment of raw materials; the in-situ pulse current activation sintering process adopted is very complicated, and after sintering at 5MPa and 1900°C, vacuum heat treatment is carried out at 1600°C. The experimental conditions are harsh and the requirements for equipment are high. At the same time, the process is complicated, the preparation cycle is long, and the energy consumption and cost increase accordingly

Method used

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  • Method for preparing two-dimensional hafnium carbide nanosheets
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  • Method for preparing two-dimensional hafnium carbide nanosheets

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preparation example Construction

[0026] The preparation method of the two-dimensional hafnium carbide nanosheet provided in this embodiment comprises the following steps:

[0027] (1) Place the carbonaceous substrate on Ni(NO 3 ) 2 After soaking in the solution for 5h-10h, take it out and dry it to prepare Ni(NO 3 ) 2 carbonaceous substrate;

[0028] (2) The Ni(NO 3 ) 2 The carbonaceous substrate is placed in the high temperature zone of the dual temperature zone CVD tube furnace, and 2g-50g HfCl 4 The powder is placed in the low temperature zone of the dual temperature zone CVD tube furnace, and then the dual temperature zone CVD tube furnace is evacuated to 2kPa, wherein, Ni(NO 3 ) 2 carbonaceous substrate and HfCl 4 The powder is placed in the alumina crucible first, and then placed in the high temperature zone and the low temperature zone respectively;

[0029] (3) Feed H into the dual temperature zone CVD tube furnace at a flow rate of 15ml / min-100ml / min 2 At the same time, the temperature in the...

Embodiment 1

[0044] In this embodiment, the following steps are included:

[0045] (1) The cleaned 2D needle-punched carbon felt substrate with a size of 10mm×10mm×5mm was placed in a concentration of 0.20mol / L Ni(NO 3 ) 2 After soaking in ethanol solution for 5h, take it out and dry it in a drying oven at 50°C to prepare Ni(NO 3 ) 2 carbonaceous substrate;

[0046] (2) The Ni(NO 3 ) 2 The carbon substrate is placed in the alumina crucible A, and then the crucible A is placed in the high temperature zone of the double temperature zone CVD tube furnace, and 4g HfCl 4 The powder is placed in an alumina crucible B, and then the crucible B is placed in the low temperature zone of the dual temperature zone CVD tube furnace, and then the dual temperature zone CVD tube furnace is evacuated to 2kPa;

[0047] (3) Feed H into the double temperature zone CVD tube furnace at a flow rate of 50ml / min 2 At the same time, the temperature in the high temperature zone is raised to 1100°C at 8°C / min, ...

Embodiment 2

[0050] The preparation method of the two-dimensional hafnium carbide nanosheet provided in this embodiment comprises the following steps:

[0051] (1) Place the cleaned graphite paper substrate with a size of 10mm×10mm×10mm in 0.05mol / LNi(NO 3 ) 2 After soaking in ethanol solution for 5h, take it out and dry it in a drying oven at 45°C to prepare Ni(NO 3 ) 2 carbonaceous substrate;

[0052] (2) The Ni(NO 3 ) 2 The carbon substrate is placed in the alumina crucible A, and then the crucible A is placed in the high temperature zone of the double temperature zone CVD tube furnace, and 3g HfCl 4 The powder is placed in an alumina crucible B, and then the crucible B is placed in the low temperature zone of the dual temperature zone CVD tube furnace, and then the dual temperature zone CVD tube furnace is evacuated to 2kPa;

[0053] (3) Feed H into the double temperature zone CVD tube furnace at a flow rate of 15ml / min 2 At the same time, the temperature in the high temperature...

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Abstract

The invention provides a method for preparing two-dimensional hafnium carbide nanosheets. The method comprises the following steps: realizing large-scale preparation of rectangular two-dimensional HfCnanosheets with regular morphology in an H2+CH4+HfCl4+Ar gas system by adopting a low-pressure CVD (Chemical Vapor Deposition) method; by utilizing the characteristic that a double-temperature-area CVD tube furnace has two independent heating areas, heating a carbon substrate containing Ni(NO3)2 in the high temperature area, introducing H2 at a certain flow to provide a reducing atmosphere whileheating, enabling the Ni(NO3)2 on the carbon substrate in the high temperature area to carry out a reduction reaction, heating a low-temperature area, and controlling the HfCl4 sublimation ratio by controlling the heating rate and constant temperature in the low temperature area so as to control the flow of the HfCl4 gas introduced into the high-temperature area after realizing sublimation control; and controlling the flow of reaction gases H2, CH4 and Ar introduced into the double-temperature-area CVD tube furnace, controlling the pressure and reaction time in the furnace, and finally preparing the rectangular two-dimensional HfC nanosheets with regular morphology.

Description

technical field [0001] The invention relates to a nanomaterial preparation technology, in particular to a preparation method of a two-dimensional hafnium carbide nanosheet. Background technique [0002] Hafnium carbide (HfC) ceramics have ultra-high melting point, high hardness, high thermal stability, high chemical stability, low work function and good electrical conductivity, and have broad application prospects in vacuum microelectronics, nuclear energy, aerospace and other fields. Based on a series of excellent properties of bulk HfC materials, low-dimensional HfC materials can also show more excellent performance and new characteristics in mechanics, optics, and electricity due to their unique geometric characteristics at the nanoscale. At present, the reported transition metal carbide two-dimensional nanomaterials mainly include Mxene, α-Mo2C nanosheets, etc. These materials have high specific surface area, high elastic modulus, high thermal stability, high chemical st...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/914B82Y30/00B82Y40/00
Inventor 田松梁中天蔡子田周露
Owner CHONGQING JIAOTONG UNIVERSITY
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