CN103274409A

CN103274409A - Method for preparing superfine TiC powder respectively by using TiOSO4 and phenolic resin as titanium source and carbon source

Info

Publication number: CN103274409A
Application number: CN2013102128185A
Authority: CN
Inventors: 吴一
Original assignee: Guilin University of Technology
Current assignee: Guilin University of Technology
Priority date: 2013-06-01
Filing date: 2013-06-01
Publication date: 2013-09-04

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

With TiOSO 4Be respectively the method that titanium source and carbon source prepare superfine Ti C powder with resol

Technical field

The invention belongs to superfine Ti C powder preparing technical field, particularly a kind of with TiOSO ₄Be respectively the method that titanium source and carbon source prepare superfine Ti C powder with 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 with TiOSO ₄Be respectively the method that titanium source and carbon source prepare superfine Ti C powder with resol.

Concrete steps are:

(1) with the TiOSO of 1 mass parts ₄The water-soluble saturated solution that makes is dissolved in dehydrated alcohol with the resol of 5 ~ 9 mass parts and makes saturated solution.

(2) two kinds of saturated solutions that step (1) is made evenly mix, and the gained mixed solution descended dry 24 ~ 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 superfine Ti C powder.

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

The composition of the prepared superfine Ti C 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) be carbon source with resol, with TiOSO ₄For the titanium source, through carbothermic reduction, 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 characteristics such as energy-conserving and environment-protective.

Embodiment

Embodiment:

(1) with 1 gram TiOSO ₄The water-soluble saturated solution that makes is dissolved in dehydrated alcohol with 7 gram resol and makes saturated solution.

(2) two kinds of saturated solutions that step (1) is made evenly mix, and the gained mixed solution descended dry 36 hours at 135 ℃, made presoma.

(3) presoma that step (2) is made is heated to 1800 ℃ under the nitrogen atmosphere protection, is incubated 2 hours and carries out carbothermic reduction, namely makes superfine Ti C powder.

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

Claims

1. one kind with TiOSO ₄Be respectively the method that titanium source and carbon source prepare superfine Ti C powder with resol, it is characterized in that concrete steps are:

(1) with the TiOSO of 1 mass parts ₄The water-soluble saturated solution that makes is dissolved in dehydrated alcohol with the resol of 5 ~ 9 mass parts and makes saturated solution;

(2) two kinds of saturated solutions that step (1) is made evenly mix, and the gained mixed solution descended dry 24 ~ 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 superfine Ti C powder;

2. the method for preparing superfine Ti C powder according to claim 1 is characterized in that: the composition of prepared superfine Ti C 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.