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Preparation method for titanium carbide nanoparticles

A nanoparticle, titanium carbide technology, applied in the field of inorganic materials, can solve the problems of reduced purity of titanium carbide, complicated synthesis process, etc., and achieve the effect of easy large-scale production, simple process and equipment

Active Publication Date: 2012-09-19
NANJING TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In addition, titanium carbide can also be prepared by magnestic reduction reaction. The preparation temperature of this method is lower, at 900-1100°C, but the introduction of magnesium makes the synthesis process more complicated, and the purity of the obtained titanium carbide is reduced to a certain extent.
Moreover, the titanium carbide nanoparticles reported in the literature are relatively large, around 100nm

Method used

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  • Preparation method for titanium carbide nanoparticles

Examples

Experimental program
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Effect test

example 1

[0022] (1) Mix resorcinol, formaldehyde, anhydrous sodium carbonate, and ethanol at a molar ratio of 1:2:0.002:3.5 and pre-react at 40°C for 90 minutes to obtain carbon sol;

[0023] (2) Mix tetrabutyl titanate, nitric acid, deionized water, and ethanol at a molar ratio of 1:0.2:4:27 to form a solution; among them, tetrabutyl titanate, nitric acid and a total of 25% of Mix ethanol evenly, then add deionized water and remaining ethanol to form a solution; react at 5°C for 10 minutes to obtain titanium sol;

[0024] (3) Mix the carbon sol obtained in step (1) with the titanium sol obtained in step (2) and perform a sol-gel reaction at 20°C for 40 minutes to obtain a wet gel, in which resorcinol and titanium The mol ratio of acid tetrabutyl ester is 1: 1;

[0025] (4) Aging the gel obtained in step (3) at 60°C for 5 days, and then drying at 50°C for 48 hours to obtain a titanium carbide precursor;

[0026] (5) heat-treating the titanium carbide precursor obtained in step (4) at...

example 2

[0030] (1) Mix resorcinol, formaldehyde, anhydrous sodium carbonate, and ethanol at a molar ratio of 1:2:0.01:10 and pre-react at 50°C for 60 minutes to obtain carbon sol;

[0031] (2) Mix tetraethyl titanate, nitric acid, deionized water, and ethanol at a molar ratio of 1:0.4:8:35 to form a solution, in which tetraethyl titanate, nitric acid, and a total of 50% of The ethanol was first mixed evenly, then deionized water and remaining ethanol were added, and reacted at 5°C for 15 minutes to obtain titanium sol;

[0032] (3) Mix the carbon sol obtained in step (1) with the titanium sol obtained in step (2), and then perform a sol-gel reaction at 50°C for 25 minutes to obtain a wet gel, in which resorcinol and titanium The mol ratio of acid tetraethyl ester is 1: 2;

[0033] (4) Aging the gel obtained in step (3) at 75°C for 1 day, and then drying at 60°C for 48 hours to obtain a titanium carbide precursor;

[0034] (5) heat treating the titanium carbide precursor obtained in ...

example 3

[0039] (1) Mix resorcinol, formaldehyde, anhydrous sodium carbonate, and ethanol at a molar ratio of 1:2:0.005:7 and pre-react at 40°C for 120 minutes to obtain carbon sol;

[0040] (2) Mix tetrabutyl titanate, nitric acid, deionized water, and ethanol at a molar ratio of 1:0.3:2:15 to form a solution, in which tetrabutyl titanate, nitric acid and a total of 75% of The ethanol was mixed evenly first, then deionized water and remaining ethanol were added, and reacted at 25°C for 5 minutes to obtain titanium sol;

[0041] (3) Mix the carbon sol obtained in step (1) with the titanium sol obtained in step (2), and then perform a sol-gel reaction at 30°C for 30 minutes to obtain a wet gel, in which resorcinol and titanium The mol ratio of acid tetrabutyl ester is 1: 0.5;

[0042] (4) Aging the gel obtained in step (3) at 70°C for 2 days, and then drying at 90°C for 24 hours to obtain a titanium carbide precursor;

[0043] (5) Heat treating the titanium carbide precursor obtained ...

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Abstract

The invention belongs to the field of inorganic materials and material synthesis process, and relates to a preparation method for titanium carbide nanoparticles. Titanium carbide nanoparticles are prepared by adopting a sol-gel method and a carbon thermal reduction processThe method comprises the following steps of: preparing carbon sol by using resorcinol, methanal and anhydrous sodium carbonate as raw materials; preparing titanium sol by using tetrabutyl titanate or tetraethyl titanate as reactants and using nitric acid and deionized water as raw materials; mixing the carbon sol with the titanium sol, and performing a sol-gel reaction to obtain wet gel; aging the wet gel, and drying the wet gel under normal pressure to obtain titanium carbide precursors; performing a carbon thermal reduction reaction on the titanium carbide precursors in inert gas; and calcining in air, soaking in hydrochloric acid, washing, filtering and drying to obtain the titanium carbide nanoparticles. The preparation method has the advantages of readily available raw materials, simple equipment, and easy large-scale production; the prepared titanium carbide nanoparticles have small particle sizes and larger specific surface areas, can be used in the fields of high-temperature insulation materials, ceramic composite materials, cutting materials, abrasion-proof materials, photocatalytic materials, aerospace materials and the like.

Description

technical field [0001] The invention belongs to the technical field of inorganic materials, and relates to a method for preparing titanium carbide nanoparticles by using a sol-gel method and a carbothermal reduction process. Background technique [0002] Titanium carbide (TiC) has many excellent physical and chemical properties, such as high melting point, high hardness, low density, corrosion and oxidation resistance, high Young's modulus, wear resistance, good thermal conductivity and thermal shock resistance, so It has broad application space in cutting materials, grinding and wear-resistant materials, aerospace materials and other fields. In industry, titanium dioxide and carbon black are generally used as raw materials, and titanium carbide is prepared by carbothermal reduction reaction at about 2200°C for 24 hours. In addition, titanium carbide can also be prepared by magnestic reduction reaction. The preparation temperature of this method is lower, at 900-1100°C, but...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/30B82Y40/00C01B32/921
Inventor 沈晓冬孔勇崔升仲亚
Owner NANJING TECH UNIV