CN103387215B - The method that titanium source and carbon source prepare TiCN powder is respectively with tetrabutyl titanate and starch - Google Patents
The method that titanium source and carbon source prepare TiCN powder is respectively with tetrabutyl titanate and starch Download PDFInfo
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- CN103387215B CN103387215B CN201310319549.2A CN201310319549A CN103387215B CN 103387215 B CN103387215 B CN 103387215B CN 201310319549 A CN201310319549 A CN 201310319549A CN 103387215 B CN103387215 B CN 103387215B
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Abstract
The invention discloses and be a kind ofly respectively with tetrabutyl titanate and starch the method that titanium source and carbon source prepare TiCN powder.Tetrabutyl titanate and dehydrated alcohol are mixed obtained solution in 1:0.01 ~ 4 in mass ratio, starch and deionized water are mixed obtained mixed solution in 1:5 ~ 8 in mass ratio; Solution and mixed solution are pressed tetrabutyl titanate and starch quality than 1:4 ~ 10 Homogeneous phase mixing, at 100 ~ 150 DEG C dry 24 ~ 48 hours, obtained presoma; Under nitrogen atmosphere or ammonia dissolving atmosphere protection, be heated to 1300 ~ 2000 DEG C, be incubated and carry out carbothermic reduction and nitrogenize in 1 ~ 2 hour, obtained TiCN powder; The purity of described chemical reagent and raw material is analytical pure and above purity; The composition of obtained powder controls by adding proportioning raw materials, and purity and granularity are determined jointly by order of addition(of ingredients) and preparation technology.The present invention has that raw material mixes, technique is simple, synthesis temperature is low, generated time is short and the feature such as energy-conserving and environment-protective.
Description
Technical field
The invention belongs to TiCN Preparation Technique of Powders field, be particularly a kind ofly respectively with tetrabutyl titanate and starch the method that titanium source and carbon source prepare TiCN powder.
Background technology
TiCN has high-melting-point, high rigidity, high-wearing feature and the special feature such as functional, not only be widely used in the reinforcement etc. of grinding tool, cutting tool and matrix material, also be used widely as energy and material, and have a wide range of applications in new function material.
Superfine Ti CN powder is badly in need of in modern energy industrial development.Tradition TiO
2synthesize TiCN powder with high temperature reduction after carbon solid phase mixing, with low cost but preparation powder thicker; Current superfine Ti CN powder mainly with pure titanium, titanium organism or gaseous titanium compound for raw material, with the technique such as vapour deposition, plasma heating preparation, raw material and process costs high, make superfine Ti CN powder expensive.Investigation and application low cost prepares superfine Ti CN new technology highly significant.
The TiCN powder of current industrialization scale operation is mostly 2 ~ 5 μm, and along with modernization industrial expansion, the especially development of energy industry, increasing to the demand of ultrafine powder TiCN, superfine Ti CN has higher using value, has a extensive future.But existing market supply superfine Ti CN powder because raw materials cost and preparation technology's cost high and expensive.Therefore carry out the research that low cost prepares ultrafine powder TiCN and there is very large realistic meaning.
The preparation of superfine Ti CN powder is the focus of material supply section scholar research, the existing raw material aspect, aspect of research, also has process aspect.But diverse ways has 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 nitrogen-based atmosphere, the direct contact reacts of reactant generates TiCN, product purity is high, carbon metering than large, technological process is simple.But titanium valve is expensive, the preparation of purification ultrafine titanium powder is more difficult; Reaction process difficulty controls, and the TiCN synthesized needs further grinding broken, causes the purity drop of product, also will purify further, make this legal system obtain large-scale promotion for superfine Ti CN powder.
Carbothermic method is the traditional method of TiCN powder suitability for industrialized production.This technique is with TiO
2for titanium source, be C source with graphite, carbon black, activated carbon etc., under high temperature, nitrogen group protecting atmosphere, TiO
2tiCN powder is generated by C reduction.Advantage is: raw materials cost is low; Technique is simple, and production efficiency is higher; The granularity of TiCN is micron order.But raw material is poor by mechanically mixing homogeneity; TiCN is also easily oxidized.With regard to current production technology, the powder synthesized can not meet the requirement of fine ceramics completely in granularity and purity.
Also have some other method to prepare superfine Ti CN, but generally there is the high organic compound etc. as high pure metal titanium valve, titanium of ingredient requirement; Synthesis technique is complicated, and as needed heating plasma, microwave heating, vapour deposition etc., appointed condition requires the problems such as high, preparation method or complex process or output limited, cause cost high.The TiCN ultrafine powder technology of exploitation high-level efficiency, low cost, remains the emphasis of countries nowadays scientist and business circles research.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, provide a kind of and be respectively with tetrabutyl titanate and starch the method that titanium source and carbon source prepare TiCN powder.
Concrete steps are:
(1) tetrabutyl titanate and dehydrated alcohol are mixed obtained solution in 1:0.01 ~ 4 in mass ratio, starch and deionized water are mixed obtained mixed solution in 1:5 ~ 8 in mass ratio.
(2) solution obtained for step (1) and mixed solution press tetrabutyl titanate and starch quality than 1:4 ~ 10 Homogeneous phase mixing, gained mixed solution at 100 ~ 150 DEG C dry 24 ~ 48 hours, obtains 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.
The composition of the TiCN powder obtained by the present invention 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.
The advantage of the inventive method:
(1) be carbon source with starch, be titanium source with tetrabutyl titanate, through carbothermic reduction, low cost prepares high-purity, superfine Ti CN.
(2), compared with the method preparing TiCN with tradition, have that raw material mixes, technique is simple, synthesis temperature is low, generated time is short and the feature such as energy-conserving and environment-protective.
Embodiment
embodiment:
(1) by tetrabutyl titanate and dehydrated alcohol 1:3 mixing obtained solution in mass ratio, by starch and the deionized water obtained mixed solution of 1:7 mixing in mass ratio.
(2) solution obtained for step (1) and mixed solution press tetrabutyl titanate and starch quality than 1:7 Homogeneous phase mixing, gained mixed solution at 125 DEG C dry 40 hours, obtains presoma.
(3) presoma obtained for step (2) is heated to 1700 DEG C under ammonia dissolving atmosphere protection; be incubated and carry out carbothermic reduction and nitrogenize in 1.5 hours; i.e. obtained TiCN powder, gained TiCN powder is through the superfine Ti CN powder of testing graininess analysis to be particle diameter be 150 ~ 300 nanometers.
The purity of described chemical reagent and raw material is analytical pure.
Claims (2)
1. prepare a method for TiCN powder, it is characterized in that concrete steps are:
(1) tetrabutyl titanate and dehydrated alcohol are mixed obtained solution in 1:0.01 ~ 4 in mass ratio, starch and deionized water are mixed obtained mixed solution in 1:5 ~ 8 in mass ratio;
(2) solution obtained for step (1) and mixed solution press tetrabutyl titanate and starch quality than 1:4 ~ 10 Homogeneous phase mixing, gained mixed solution at 100 ~ 150 DEG C dry 24 ~ 48 hours, obtains 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;
Use the purity of raw material to be 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.
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| CN103387215B true CN103387215B (en) | 2016-03-02 |
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| CN106241756B (en) * | 2016-08-08 | 2018-10-23 | 厦门理工学院 | A kind of preparation method of nano-carbon titanium nitride powder |
| CN113307630B (en) * | 2021-04-28 | 2023-03-24 | 中国有色桂林矿产地质研究院有限公司 | Superfine composite powder and preparation method thereof |
Citations (2)
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|---|---|---|---|---|
| CN101462722A (en) * | 2009-01-09 | 2009-06-24 | 北京科技大学 | Method for preparing titanium carbide ceramic powder |
| CN101863663A (en) * | 2010-07-15 | 2010-10-20 | 武汉工程大学 | Combustion method for preparing submicron grade titanium carbide polycrystal powder |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103130506B (en) * | 2013-03-15 | 2014-07-09 | 长沙伟徽高科技新材料股份有限公司 | Method for preparing superfine titanium carbonitride |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101462722A (en) * | 2009-01-09 | 2009-06-24 | 北京科技大学 | Method for preparing titanium carbide ceramic powder |
| CN101863663A (en) * | 2010-07-15 | 2010-10-20 | 武汉工程大学 | Combustion method for preparing submicron grade titanium carbide polycrystal powder |
Non-Patent Citations (5)
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| Carbothermal Reduction Synthesis of Superfined TiC Powders From TiOSO4;Jie Li;《Advanced Materials Research》;20111218;第415-417卷;510-513 * |
| NaBr-KCl和不同炭源对合成Ti(C,N)粉末的影响;陈希来等;《耐火材料》;20070630;第41卷(第6期);413-416 * |
| 以酚醛树脂为碳源碳热还原制备TiC的研究;李鹏飞等;《硅酸盐通报》;20121031;第31卷(第5期);1312-1316 * |
| 溶胶-凝胶工艺合成Ti(C,N)超细粉末;向军辉等;《无机材料学报》;19981031;第740页1-4行 * |
| 高钛渣提取碳氮化钛的研究;李慈颖等;《钢铁钒钛》;20060930;第7页右栏第2段以及第2.2节 * |
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