CN103274412A - TiC powder preparation method taking tetrabutyl titanate and phenolic resin serving as titanium source and carbon source respectively - Google Patents

Abstract

The invention discloses a TiC powder preparation method taking tetrabutyl titanate and a phenolic resin serving as a titanium source and a carbon source respectively. The method comprises the steps that tetrabutyl titanate and phenolic resin are weighted in a mass ratio of 1: (5-9), and respectively dissolved in absolute ethyl alcohol to prepare saturated solutions; the two saturated solutions are mixed together uniformly, then deionized water with equal volume is dropwise added in the mixed solution to prepare mixed gel, the mixed gel is dried for 36-48 hours at the temperature ranging from 100 DEG C to 150 DEG C, and precursor is prepared; the precursor is heated to 1,500 DEG C-2,000 DEG C under the protection of hydrogen atmosphere, the heat preservation is performed for 1-2 hours, carbon thermal reduction is performed, and then TiC powder is prepared; purity of chemical reagents and raw materials are analytically pure and above; and components of the prepared TiC powder are controlled by an added raw material ratio, and purity and granularity are commonly determined by charging sequences and preparation technics. The method disclosed by the invention has the advantages of uniform mixing of the raw materials, simple processing, low synthetic temperature, short synthetic time, energy conservation, environment protection and the like.

Description

Be respectively the method that titanium source and carbon source prepare the TiC powder with tetrabutyl titanate and resol

Technical field

The invention belongs to TiC powder preparing technical field, particularly a kind ofly be respectively the method that titanium source and carbon source prepare the TiC powder with tetrabutyl titanate and resol.

Background technology

TiC has high-melting-point, high rigidity, high-wearing feature and special characteristics such as functional, not only be widely used in the enhancing body of grinding tool, cutting tool and matrix material etc., also be used widely as energy and material, as the nuclear energy material use, the coated material of TiC can anti-H ⁺Ion irradiation and anti-very big thermograde and thermal cycling, the long-time use properties of anti-tritium-permeation layer of these coated materials is stable, aspect the infrared radiation ceramic material, add TiC in the cordierite structure, not only be used as conductive phase and introduce, and itself be again good near-infrared radiation characteristic material, and in the NEW TYPE OF COMPOSITE contact material, have a wide range of applications.

Superfine Ti C powder, tradition TiO are badly in need of in modern energy industry development ₂With the synthetic TiC powder of high temperature reduction after the carbon solid phase mixing, with low cost but powder preparation is thicker; Superfine Ti C powder is raw material with pure titanium, titanium organism or gaseous state titaniferous compound mainly at present, with prepared such as vapour deposition, plasma heating, raw material and technology cost height make superfine Ti C powder expensive, and research and the low-cost preparation of application superfine Ti C new technology are highly significant.

The TiC powder of large-scale industrialization production at present mostly is 2 ~ 5 μ m greatly, development along with modernization industry, especially the development of energy industry, demand to ultrafine powder TiC is increasing, superfine Ti C has higher using value, have a extensive future, but therefore the superfine Ti C powder of existing market supply carries out the low-cost research for preparing ultrafine powder TiC and has very big realistic meaning because raw materials cost and preparation technology's cost are high and expensive.

The preparation of superfine Ti C powder is the focus of material supply section scholar research, existing raw material aspect, the aspect of research, process aspect is also arranged, but diverse ways there are its relative merits for suitability for industrialized production.

Direct carborization is with simple substance carbon, metallic titanium powder (or TiH ₂) be raw material, at high temperature, in inert atmosphere or the vacuum, the direct contact reacts of reactant generates TiC, and product purity height, carbon metering are than big, and technological process is simple, but titanium valve is expensive, and the preparation of purification ultrafine titanium powder is difficulty relatively; The difficult control of reaction process, the TiC that synthesizes needs further grinding fragmentation, causes degree of purity of production to reduce, and also will further purify, and makes this legal system be equipped with superfine Ti C powder and obtains large-scale promotion.

Carbothermic method is the traditional method of TiC powder suitability for industrialized production, and this technology is with TiO ₂Being the titanium source, is the C source with graphite, carbon black, activated carbon etc., under high temperature, protective atmosphere, and TiO ₂Generated the TiC powder by the C reduction, advantage is: raw materials cost is low; Technology is simple, and production efficiency is higher; The granularity of TiC is micron order, but raw material is relatively poor by the mechanically mixing homogeneity; Utilize combustion method to handle the residue carbon black, TiC is also easily oxidized; With regard to present production technology, the powder that synthesizes can not satisfy the requirement of fine ceramics fully on granularity and purity.

Also have some other method to prepare superfine Ti C, but generally have the high organic compound as high pure metal titanium valve, titanium of ingredient requirement etc.; The synthesis technique complexity, as the heating of need plasma, microwave heating, vapour deposition etc., appointed condition requires problems such as height, preparation method or complex process or output are limited, cause the cost height, exploitation high-level efficiency, TiC ultrafine powder technology of preparing cheaply remain the emphasis of countries nowadays scientist and business circles research.

Summary of the invention

The objective of the invention is to overcome the deficiencies in the prior art, provide a kind of and be respectively the method that titanium source and carbon source prepare the TiC powder with tetrabutyl titanate and resol.

Concrete steps are:

(1) takes by weighing tetrabutyl titanate and resol according to mass ratio 1:5 ~ 9, be dissolved in respectively and make saturated solution in the dehydrated alcohol.

(2) two kinds of saturated solutions that step (1) is made evenly mix, and then to mixed solution and dripping and the isopyknic deionized water of mixing solutions, make mixed gel, and the gained mixed gel descended dry 36 ~ 48 hours at 100 ~ 150 ℃, made presoma.

(3) presoma that step (2) is made is heated to 1500 ~ 2000 ℃ under the nitrogen atmosphere protection, is incubated 1 ~ 2 hour and carries out carbothermic reduction, namely makes the TiC powder.

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

The composition of the prepared TiC powder of the present invention is by adding proportion of raw materials control, and the purity of powder and granularity are determined jointly by order of addition(of ingredients) and preparation technology.

The advantage of the inventive method:

(1) being carbon source with resol, is the titanium source with the tetrabutyl titanate, through carbothermic reduction, and high-purity, the superfine Ti C of low-cost preparation.

(2) compare with the method for traditional preparation process TiC, have that raw material mixes, technology is simple, synthesis temperature is low, generated time is short and advantage such as energy-conserving and environment-protective.

Embodiment

Embodiment:

(1) takes by weighing 1 gram tetrabutyl titanate and 8 gram resol, be dissolved in respectively and make saturated solution in the dehydrated alcohol.

(2) two kinds of saturated solutions that step (1) is made evenly mix, and then to mixed solution and dripping and the isopyknic deionized water of mixing solutions, make mixed gel, and the gained mixed gel descended dry 36 hours at 150 ℃, made presoma.

(3) presoma that step (2) is made is heated to 2000 ℃ under the nitrogen atmosphere protection, is incubated 1 hour and carries out carbothermic reduction, namely makes the TiC powder, and gained TiC powder is that particle diameter is the superfine Ti C powder of 150 ~ 300 nanometers through the testing graininess analysis.

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

Claims (2)

1. method for preparing the TiC powder is characterized in that concrete steps are:

(1) takes by weighing tetrabutyl titanate and resol according to mass ratio 1:5 ~ 9, be dissolved in respectively and make saturated solution in the dehydrated alcohol;

(2) two kinds of saturated solutions that step (1) is made evenly mix, and then to mixed solution and dripping and the isopyknic deionized water of mixing solutions, make mixed gel, and the gained mixed gel descended dry 36 ~ 48 hours at 100 ~ 150 ℃, made presoma;

(3) presoma that step (2) is made is heated to 1500 ~ 2000 ℃ under the nitrogen atmosphere protection, is incubated 1 ~ 2 hour and carries out carbothermic reduction, namely makes the TiC powder;

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

2. the method for preparing the TiC powder according to claim 1 is characterized in that: the composition of prepared TiC powder is by adding proportion of raw materials control, and the purity of powder and granularity are determined jointly by order of addition(of ingredients) and preparation technology.