CN103274409A - Method for preparing ultrafine TiC powder with TiOSO4 and phenolic resin as titanium source and carbon source respectively - Google Patents

Abstract

The invention discloses a method for preparing superfine TiC powder respectively by using TiOSO4 and phenolic resin as a titanium source and a carbon source, which comprises the following steps: dissolving 1 part by mass of TiOSO4 in water to obtain a saturated solution, and dissolving 5-9 parts by mass of phenolic resin in anhydrous ethanol to obtain a saturated solution; evenly mixing the two saturated solutions, and drying the mixed solution at 100-150 DEG C for 24-48 hours to obtain a precursor; heating the precursor to 1500-2000 DEG C in a hydrogen protective atmosphere, and keeping the temperature for 1-2 hours to carry out carbon thermal reduction, thereby obtaining the superfine TiC powder. The chemical reagents and raw materials are analytically pure or above; the composition of the prepared superfine TiC powder is controlled by the proportion of the added raw materials; and the purity and particle size of the powder are codetermined by the charging sequence and preparation technique. The method disclosed by the invention has the advantages of uniformly mixed raw materials, simple technique, low synthesis temperature, short synthesis time, energy saving, environmental protection and the like.

Description

Method for preparing ultrafine TiC powder with TiOSO4 and phenolic resin as titanium source and carbon source respectively

technical field

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

Background technique

TiC 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 widely used as energy materials, such as nuclear energy materials. Utilization, TiC coating materials can resist H ⁺ ion radiation and resist large temperature gradients and thermal cycles. The anti-tritium permeation layer of these coating materials has stable performance for a long time. In terms of infrared radiation ceramic materials, the cordierite structure TiC is not only introduced as a conductive phase, but also has excellent near-infrared radiation characteristics, and has broad application prospects in new composite electrical contact materials.

The development of modern energy industry urgently needs ultra-fine TiC powder. Traditionally, TiC powder is synthesized by mixing TiO ₂ and carbon solid phase at high temperature. Titanium compounds are used as raw materials and prepared by vapor deposition, plasma heating and other processes. The cost of raw materials and processes is high, which makes ultrafine TiC powder expensive. It is very meaningful to research and apply new technologies for preparing ultrafine TiC at low cost.

At present, most of the TiC 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 TiC powder is increasing, and ultra-fine TiC has higher application value. The prospect is broad, but the ultra-fine TiC powder currently available in the market is expensive because of the high cost of raw materials and preparation process. Therefore, the research on low-cost preparation of ultra-fine TiC powder has great practical significance.

The preparation of ultrafine TiC powder is a hotspot of research by material scientists. 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. Under high temperature, inert atmosphere or vacuum, the reactants directly contact and react to form TiC. The product has high purity, large carbon metering ratio, and the process is simple. However, the price of titanium powder is expensive, and the preparation of ultra-fine titanium powder is difficult; the reaction process is difficult to control, and the synthesized TiC needs to be further pulverized and broken, resulting in a decrease in the purity of the product, and further purification is required, so that this method can prepare ultra-fine TiC powder It has not been widely promoted.

The carbothermal reduction method is a traditional method for the industrial production of TiC powder. In this process, TiO ₂ is used as the titanium source, and graphite, carbon black, activated carbon, etc. are used as the C source. Under high temperature and protective atmosphere, TiO ₂ is reduced by C to form TiC powder. , the advantages are: low cost of raw materials; simple process, high production efficiency; the particle size of TiC is micron level, but the uniformity of raw materials is poor through mechanical mixing; the remaining carbon black is processed by combustion method, and TiC is also easily oxidized; as far as the current From the perspective of production technology, the synthesized powder cannot fully meet the requirements of fine ceramics in terms of particle size and purity.

There are other methods to prepare ultra-fine TiC, 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 Problems such as demanding conditions, complex preparation methods or processes, or limited output lead to high costs. The development of high-efficiency, low-cost TiC 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 of the prior art and provide a method for preparing ultrafine TiC powder with TiOSO ₄ and phenolic resin as titanium source and carbon source respectively.

The specific steps are:

(1) Dissolve 1 mass part of TiOSO ₄ in water to obtain a saturated solution, and dissolve 5 to 9 mass parts of phenolic resin in absolute ethanol to obtain a saturated solution.

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

(3) Heat the precursor prepared in step (2) to 1500-2000°C under the protection of a hydrogen atmosphere, and keep it warm for 1-2 hours for carbothermal reduction to obtain ultrafine TiC powder.

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

The composition of the superfine TiC powder prepared by the 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 addition and the preparation process.

The advantage of the inventive method:

(1) Using phenolic resin as a carbon source and TiOSO ₄ as a titanium source, high-purity, ultrafine TiC was prepared at low cost by carbothermal reduction.

(2) Compared with the traditional method of preparing TiC, 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) 1 gram of TiOSO ₄ was dissolved in water to obtain a saturated solution, and 7 grams of phenolic resin was dissolved in absolute ethanol to obtain a saturated solution.

(2) The two saturated solutions prepared in step (1) were evenly mixed together, and the obtained mixed solution was dried at 135° C. for 36 hours to obtain a precursor.

(3) Heating the precursor prepared in step (2) to 1800° C. under the protection of a hydrogen atmosphere, and keeping it warm for 2 hours to carry out carbothermal reduction to obtain ultrafine TiC powder.

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

Claims (2)

1. a method for preparing ultra-fine TiC powder with _TiOSO4 and phenolic resin as titanium source and carbon source respectively, is characterized in that concrete steps are: (1) the _TiOSO4 of 1 mass part is dissolved in water and makes saturated solution, and the phenolic resin of 5～9 mass parts is dissolved in dehydrated alcohol and makes saturated solution; (2) uniformly mix the two saturated solutions prepared in step (1), and dry the obtained mixed solution at 100-150° C. for 24-48 hours to obtain a precursor; (3) Heating the precursor prepared in step (2) to 1500-2000°C under the protection of a hydrogen atmosphere, keeping it warm for 1-2 hours for carbothermal reduction, and then obtaining ultra-fine TiC powder; The purity of the chemical reagents and raw materials is above analytical purity. 2. The method for preparing ultrafine TiC powder according to claim 1, characterized in that: the composition of the prepared ultrafine TiC powder is controlled by the proportioning of adding raw materials, and the purity and particle size of the powder are determined by the order of addition. It is determined jointly with the preparation process.