CN103387217B - With TiOSO 4the method that titanium source and carbon source prepare TiCN powder is respectively with tetramethylolmethane - Google Patents

Abstract

The invention discloses a method for preparing TiCN powder by using _TiOSO4 and pentaerythritol as titanium source and carbon source respectively. Weigh TiOSO ₄ and pentaerythritol according to the mass ratio of 1:3~7, and dissolve them in deionized water to obtain a saturated solution; the two saturated solutions are evenly mixed together, and then the obtained mixed solution is dried at 100~150°C for 24 After ~48 hours, the precursor is prepared; the precursor is heated to 1300~2000°C under the protection of nitrogen atmosphere or ammonia decomposition atmosphere, and kept for 1~2 hours for carbothermal reduction and nitriding to obtain TiCN powder; the chemical The purity of the reagents and raw materials are analytically pure and above; the composition of the prepared powder is controlled by the proportion of raw materials added, and the purity and particle size are determined by the order of addition and the preparation process. The invention has the characteristics of uniform mixing of raw materials, simple process, low synthesis temperature, short synthesis time, energy saving and environmental protection, and the like.

Description

The method for preparing TiCN powder with TiOSO4 and pentaerythritol as titanium source and carbon source respectively

technical field

The invention belongs to the technical field of TiCN powder preparation, in particular to a method for preparing TiCN powder by using _TiOSO4 and pentaerythritol as titanium source and carbon source respectively.

Background technique

TiCN has the characteristics of high melting point, high hardness, high wear resistance and special functionality. It is not only widely used in abrasive tools, cutting tools and reinforcements of composite materials, but also as an energy material. The material has broad application prospects.

The development of modern energy industry urgently needs ultra-fine TiCN powder. Traditionally, TiCN powder is synthesized by mixing TiO ₂ and carbon solid phase at high temperature after high-temperature reduction. The cost is low, but the prepared powder is relatively coarse. At present, ultra-fine TiCN powder is mainly made of pure titanium, titanium organic matter or gaseous titanium compound. It is prepared by processes such as body heating, and the cost of raw materials and processes is high, making ultrafine TiCN powder expensive. It is very meaningful to study and apply the new technology of preparing ultrafine TiCN at low cost.

At present, most of the TiCN powder produced in large-scale industrialization is 2~5μm. With the development of modern industry, especially the development of energy industry, the demand for ultra-fine TiCN powder is increasing, and ultra-fine TiCN has higher application value. Broad prospects. However, the ultra-fine TiCN powder currently available in the market is expensive because of the extremely high cost of raw materials and preparation process. Therefore, it is of great practical significance to study the preparation of ultrafine powder TiCN at low cost.

The preparation of ultrafine TiCN powder is a research hotspot for material scientists, and the research aspects include both raw materials and processes. But different methods have their advantages and disadvantages for industrial production.

The direct carbonization method uses elemental carbon and metal titanium powder (or TiH ₂ ) as raw materials. At high temperature and in a nitrogen-based atmosphere, the reactants directly contact and react to form TiCN. The product has high purity, large carbon stoichiometric ratio, and the process is simple. However, the price of titanium powder is expensive, and the preparation of ultrafine titanium powder is relatively difficult; the reaction process is difficult to control, and the synthesized TiCN needs to be further pulverized and broken, resulting in a reduction in the purity of the product, and further purification is required, so that this method can prepare ultrafine TiCN powder It has not been widely promoted.

Carbothermal reduction is a traditional method for the industrial production of TiCN powder. The process uses _TiO2 as the titanium source, graphite, carbon black, activated carbon, etc. as the C source, and under high temperature and nitrogen-based protective atmosphere, _TiO2 is reduced by C to generate TiCN powder. The advantages are: low cost of raw materials; simple process and high production efficiency; the particle size of TiCN is micron level. However, the uniformity of raw materials is poor through mechanical mixing; TiCN is also easily oxidized. As far as the current production technology is concerned, the synthesized powder cannot fully meet the requirements of fine ceramics in terms of particle size and purity.

There are other methods to prepare ultrafine TiCN, but generally speaking, there are high raw material requirements such as high-purity metal titanium powder, organic compounds of titanium, etc.; the synthesis process is complicated, such as plasma heating, microwave heating, vapor deposition, etc., equipment The conditions require high problems, the preparation method or process is complex or the output is limited, resulting in high cost. The development of high-efficiency, low-cost TiCN ultrafine powder preparation technology is still the focus of research by scientists and business circles in various countries.

Contents of the invention

The purpose of the present invention is to overcome the deficiencies in the prior art and provide a method for preparing TiCN powder with TiOSO ₄ and pentaerythritol as titanium source and carbon source respectively.

The specific steps are:

(1) Weigh TiOSO ₄ and pentaerythritol according to the mass ratio of 1:3~7, and dissolve them in deionized water respectively to obtain a saturated solution.

(2) Evenly mix the two saturated solutions prepared in step (1), and then dry the obtained mixed solution at 100-150° C. for 24-48 hours to prepare the precursor.

(3) Heat the precursor prepared in step (2) to 1300-2000°C under the protection of nitrogen atmosphere or ammonia decomposition atmosphere, and keep it warm for 1-2 hours for carbothermal reduction and nitriding to obtain TiCN powder.

The purity of the chemical reagents and raw materials are analytical purity and above.

The composition of the TiCN powder prepared by the present invention is controlled by the ratio of the added raw materials, and the purity and particle size of the powder are jointly determined by the order of feeding and the preparation process.

The advantage of the inventive method:

(1) Using pentaerythritol as the carbon source and TiOSO ₄ as the titanium source, high-purity, ultrafine TiCN was prepared at low cost through carbothermal reduction and nitriding.

(2) Compared with the traditional method of preparing TiCN, it has the characteristics of uniform raw material mixing, simple process, low synthesis temperature, short synthesis time, energy saving and environmental protection.

Detailed ways

Example:

(1) Weigh 1 gram of TiOSO ₄ and 5.5 grams of pentaerythritol, and dissolve them in deionized water to obtain a saturated solution.

(2) The two saturated solutions prepared in step (1) were evenly mixed together, and then the obtained mixed solution was dried at 125° C. for 35 hours to prepare a precursor.

(3) Heat the precursor prepared in step (2) to 1750°C under the protection of ammonia decomposition atmosphere, and keep it warm for 1.5 hours for carbothermal reduction and nitriding to obtain TiCN powder, which is analyzed by particle size test It is an ultrafine TiCN powder with a particle size of 150-300 nanometers.

The purity of the chemical reagents and raw materials are analytically pure.

Claims (2)

1. prepare a method for TiCN powder, it is characterized in that concrete steps are:

(1) TiOSO is taken according to mass ratio 1:3 ~ 7 ₄with tetramethylolmethane, be dissolved in obtained saturated solution in deionized water respectively;

(2) by two kinds of obtained for step (1) saturated solution Homogeneous phase mixing together, and then by the mixing solutions that obtains at 100 ~ 150 DEG C dry 24 ~ 48 hours, obtained presoma;

(3) presoma obtained for step (2) is heated to 1300 ~ 2000 DEG C under nitrogen atmosphere or ammonia dissolving atmosphere protection, is incubated and carries out carbothermic reduction and nitrogenize in 1 ~ 2 hour, be i.e. obtained TiCN powder;

The purity of described chemical reagent and raw material is analytical pure and above purity.

2. the method preparing TiCN powder according to claim 1, is characterized in that: the composition of obtained TiCN powder controls by adding proportioning raw materials, and the purity of powder and granularity are determined jointly by order of addition(of ingredients) and preparation technology.