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Method for preparing high-activity titanium boride ceramic powder through low-temperature microwave carbon thermal reduction

A ceramic powder, high activity technology, used in boron/boride, metal boride, chemical industry and other directions, can solve the problems of polluted environment, poor product activity and high reaction temperature

Active Publication Date: 2021-09-07
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In summary, the existing TiB 2 There are deficiencies in the preparation methods of ceramic powder: such as high reaction temperature, long reaction time, and poor product activity; Washing and purification process pollutes the environment, etc.

Method used

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  • Method for preparing high-activity titanium boride ceramic powder through low-temperature microwave carbon thermal reduction
  • Method for preparing high-activity titanium boride ceramic powder through low-temperature microwave carbon thermal reduction
  • Method for preparing high-activity titanium boride ceramic powder through low-temperature microwave carbon thermal reduction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Take 36g of boric acid with a purity of 99.2% and a particle size range of 50 to 80 μm, 24 g of metatitanic acid with a purity of 99.4%, and a particle size range of 10 to 20 μm, 37 g of sucrose, and 3.88 g of Na 2 O for batching, placed in a kneader with a stirring speed of 20r / min, a heating rate of 10°C / min, and a temperature of 100°C for 2.4 hours. React in a microwave atmosphere furnace at 1300°C for 40 minutes to obtain highly active TiB with a purity of 99.2% and an average particle size of 1.8 μm 2 Ceramic powder.

[0038] figure 2 Prepare TiB for the present invention 2 The XRD pattern of the ceramic powder shows that only TiB appears 2 Sharp diffraction peaks without other miscellaneous peaks (such as TiC, Ti 2 o 3 etc.), indicating that the TiB prepared by the present invention 2 The purity of the ceramic powder is high, which can meet the requirements of high-purity raw materials for subsequent sintering.

Embodiment 2

[0040] Take 33g of boric acid with a purity of 99.5% and a particle size range of 240 to 300 μm, 24 g of metatitanic acid with a purity of 99.2%, and a particle size range of 20 to 30 μm, 38 g of dextrin, and 8 g of Na 2 CO 3 For batching, place the kneader with a stirring speed of 100r / min, a heating rate of 20°C / min, and a temperature of 300°C for 0.3h, then place the dried raw materials in a kneader with a heating rate of 100°C / min and a temperature of React in a microwave atmosphere furnace at 1550°C for 10 minutes to obtain highly active TiB with a purity of 99.5% and an average particle size of 1.6 μm 2 Ceramic powder.

[0041] image 3 Gained TiB for the present invention 2 Microscopic morphology of ceramic powder. It can be seen from the figure that the particle size of the powder is relatively uniform, the grain size is small (2 Ceramic powder has high sintering activity.

Embodiment 3

[0043] Take 39g of boric acid with a purity of 99% and a particle size range of 100-160 μm, 24 g of metatitanic acid with a purity of 99.6% and a particle size range of 10-15 μm, 22 g of citric acid + 22 g of dextrin, 6.5 g K 2 CO 3 For batching, place the kneader with a stirring speed of 80r / min, a heating rate of 15°C / min, and a temperature of 200°C for 1.2h, then place the dried raw materials in a kneader with a heating rate of 60°C / min and a temperature of React in a microwave atmosphere furnace at 1400°C for 30 minutes to obtain highly active TiB with a purity of 99.3% and an average particle size of 1.4 μm 2 Ceramic powder.

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Abstract

The invention belongs to the field of ceramic material preparation, and discloses a method for preparing high-activity titanium boride ceramic powder through low-temperature microwave carbon thermal reduction. The process comprises the following steps: uniformly mixing boric acid, metatitanic acid, an organic carbon source and a reaction accelerator with deionized water, drying, and carrying out low-temperature carbon thermal reduction in a microwave atmosphere furnace to prepare the high-activity titanium boride ceramic powder. According to the invention, deionized water is used as a solvent, and a complex and lengthy sol-gel process is not needed; the raw materials directly react after being heated and decomposed, and the reaction activity is high; a reaction accelerator is introduced to improve the reaction rate and promote the reaction to be carried out at low temperature; and the high-activity TiB2 ceramic powder with fine crystal grains and uniform size is prepared by using microwaves at 1200-1550 DEG C within 5-50 minutes . Compared with an existing TiB2 powder preparation method with high energy consumption (1800-2100 DEG C) and high cost, the method has the advantages of being low in reaction temperature, short in reaction time, short in process, low in cost, environmentally friendly, capable of saving energy, reducing consumption and the like, simple and easy to control in process and suitable for industrial large-scale application.

Description

technical field [0001] The invention belongs to the field of preparation of ceramic materials, and relates to a low-temperature preparation method of high-activity titanium boride ceramic powder. Background technique [0002] Titanium boride (TiB 2 ) is an important ceramic material with high melting point (3253°C), high hardness (33.5GPa), low density (4.52g / cm 3 ), high temperature resistance and excellent acid and alkali corrosion resistance, it is widely used in conductive ceramic materials, abrasive materials and alloy additives. At the same time, TiB 2 Excellent electrical conductivity and good wettability with aluminum liquid are widely used in wettable cathodes for carbon-free aluminum electrolysis. But the current high-purity TiB 2 The preparation cost of powder is high and the activity is poor, which greatly limits the TiB 2 Large-scale application of powder. [0003] TiB 2 The preparation methods of powder mainly include carbothermal reduction method, self-...

Claims

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Application Information

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IPC IPC(8): C01B35/04
CPCC01B35/04C01P2002/72C01P2004/03C01P2006/80C01P2004/61C01P2004/51Y02P20/10
Inventor 李欣乔佳杨建红牛群
Owner JIANGSU UNIV
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