Nitrogen-doped niobium carbide nanosheets and preparation method thereof
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A niobium carbide nanometer and nitrogen doping technology, applied in chemical instruments and methods, carbon compounds, nanotechnology, etc., can solve problems such as few reports
Active Publication Date: 2017-05-10
HUBEI ENG UNIV
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Although the synthesis of niobium carbide nanoparticles has been reported, they are all one-dimensional structure of niobium carb...
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Embodiment 1
[0020] First, 1.3292g of Nb 2 o 5 , 2.4748g NiCl 2 ·6H 2 O, 3.1573 g of C 3 h 6 N 6 Put it in a ball mill jar and mill it in a ball mill for 1 hour to make it fully mixed. After taking it out, put it in a mortar and grind until it becomes powder (grinding is for more convenient performance characterization, and no grinding will not affect the implementation of the present invention), and vacuum-dry at 60° C. for 20 minutes. Put the dried powder in a graphite box, cover it, and put it in a fixed tube atmosphere furnace (CVD tube furnace). After vacuuming, nitrogen gas is introduced, and the parameters are set, and the temperature is raised to 1100 at 5°C / min. ℃, and keep it warm for 2 hours, then cool down with the furnace to get the final product. (See figure 1 , figure 2 )
Embodiment 2
[0022] First, 1.3265g of Nb 2 o 5 , 4.7534g NiCl 2 ·6H 2 O, 3.1507g of C 3 h 6 N 6 Put it in a ball mill jar and mill it in a ball mill for 1 hour to make it fully mixed. After taking it out, grind it in a mortar until it becomes powder, and dry it under vacuum at 60°C for 20 minutes. Put the dried powder in a graphite box, cover it, put it in a CVD tube furnace, pump it into argon after vacuuming, set the parameters, raise the temperature to 1200°C at 7°C / min, and keep it warm for 3 hours , with furnace cooling to obtain the final product. (See image 3 )
Embodiment 3
[0024] First, 1.3292g of Nb 2 o 5 , 3.6754 g CoCl 2 ·6H 2 O, 3.1573 g of C 3 h 6 N 6 Put it in a ball mill jar and mill it in a ball mill for 1 hour to make it fully mixed. After taking it out, put it in a mortar and grind until it becomes powder, and dry it under vacuum at 60°C for 20 minutes. Put the dried powder in a graphite box, cover it, and put it in a CVD tube furnace. After vacuuming, nitrogen gas is introduced, and the parameters are set. The temperature is raised to 1100°C at a rate of 5°C / min, and the temperature is kept for 2 hours. Cool to obtain the final product.
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Abstract
The invention discloses a preparation method of nitrogen-doped niobium carbide nanosheets. The preparation method comprises the following steps: 1) putting Nb2O5, soluble metal chloride or hydrate thereof and C3H6N6 according to an amount ratio of 1: (2-5): (3-6) into a ball mill; 2) performing ball milling in the ball mill; 3) taking out, drying, putting into a fixed tubular atmosphere furnace, and in an inert atmosphere, heating to 900-1200 DEG C at a speed rate of 4-10 DEG C/min; 4) preserving heat for 1-3h, and cooling to room temperature to obtain the nitrogen-doped niobium carbide nanosheets. The invention further discloses the nitrogen-doped niobium carbide nanosheets prepared by the preparation method. According to the preparation method, with low-cost tripolycyanamide as a nitrogen source and a carbon source, the soluble metal chloride or the hydrate thereof as a catalyst and a flux, and the Nb2O5 as a niobium source, the temperature is raised to a specific temperature through temperature programming and a reaction is performed to prepare the nitrogen-doped niobium carbide with a two-dimensional structure; by the preparation method, the operating method is simple, the cost is low and industrialization is easy to implement.
Description
technical field [0001] The invention relates to the technical field of nanomaterials and their preparation, in particular to a nitrogen-doped niobium carbide nanosheet and a preparation method thereof. Background technique [0002] Niobium carbide is a gray-brown metallic powder with a melting point of 3490°C and a boiling point of 4300°C. It is a material with high melting point, high boiling point and high hardness. Molybdenum carbide is used for hot forging dies, cutting tools, jet engine turbine blades, valves, tail skirts and rocket nozzle coatings, etc. Niobium carbide has been widely used in wear-resistant tools, medical devices, semiconductors, engineering ceramics and chemical materials. At present, the methods for preparing niobium carbide mainly include: 1) a reduction method using niobium pentoxide as a raw material to prepare niobium carbide; 2) a direct method using metal niobium and carbon black as raw materials to prepare niobium carbide; 3) using niobium pe...
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