CN1124977C - Microwave synthesis process for nanometer level titaniuym carbide - Google Patents
Microwave synthesis process for nanometer level titaniuym carbide Download PDFInfo
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- CN1124977C CN1124977C CN 01129991 CN01129991A CN1124977C CN 1124977 C CN1124977 C CN 1124977C CN 01129991 CN01129991 CN 01129991 CN 01129991 A CN01129991 A CN 01129991A CN 1124977 C CN1124977 C CN 1124977C
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Abstract
The present invention relates to a method of synthesizing nano-grade titanium carbide by using microwaves. The method comprises the steps: drying titanium dioxide and acetylene carbon black, uniformly mixing the material in the mass ratio of material to zirconium pellet to anhydrous ethyl alcohol of 1:1 to 5:3 to 6 in a ball milling mode, drying, and heating with microwaves for synthesis. The method mainly utilizes the principle of a carbothermic process, and adopts microwave heating synthesis, thereby having the advantages of low reaction temperature, simple technological process and easy control. The obtained TiC powder is not easy to agglomerate, does not need processing, and has no impurity.
Description
(1) technical field
The present invention relates to technical field of inorganic material, specifically be meant a kind of method of microwave synthetizing nano level titanium carbide.
(2) background technology
At present, the method for general synthesizing titanium carbide (TiC) can be divided into three classes: (1) synthesizes TiC with metal titanium or the direct carbonization of halogenated titanium; (2) use the gas halogenated titanium (as TiCl
4) the synthetic TiC of pyrolysis in carbonaceous atmosphere; (3) in the atmosphere of being controlled, high temperature is down with carbon carbothermic reduction TiO
2Synthetic TiC.Synthetic TiC comparatively inexpensive method is to adopt TiO
2Make 1700～2100 ℃ of reactions with carbon black.Reaction formula is:
With metal Ti powder and the synthetic TiC of C powder, adopt self propagating high temperature synthesis method (SHS) more, with the synthetic TiC of SHS method, its purity can be subjected to the influence of contained gas in the reactant, as aqueous vapor, hydrogen, carbonic acid gas and hydrocarbon polymer etc.Therefore before reaction is carried out, reactant vacuum baking under suitable temperature is handled.In addition; can also adopt the chemical coprecipitation in-situ synthesis; this method pre-reaction material is liquid (as titanium sulfate or metatitanic acid fourth fat); mix with sucrose by reaction ratio and to be made into certain buffered soln; then at a certain temperature; the thickening carbonization is warming up to 1750 ℃ then under protective atmosphere, TiC is synthesized in carburizing reagent.At present, the somebody explores with the reaction ball milling technology and prepares TiC.
Take a broad view of the prior art of these preparations TiC, part all comes with some shortcomings: the temperature of reaction height, all more than 1400 ℃; The difficult control of complicated process of preparation, technological process; The TiC of SHS method preparation is a block, also needs ball milling processing, can only reach micron order after the processing, also may mix various impurity in the course of processing.
(3) summary of the invention
The present invention is exactly the defective that exists in the prior art in order to overcome, provide a kind of technological process simple, easy to control, need not reprocessing, inclusion-free, can be under lower temperature (1200 ℃) method of synthetic microwave synthetizing nano level titanium carbide fast.
A kind of method of microwave synthetizing nano level titanium carbide is characterized in that, it comprises the steps and processing condition:
The first step dries Nano titanium dioxide and Shawinigan black to constant weight, and according to titanium dioxide: the quality of Shawinigan black=80: 36 compares weighing;
Second goes on foot according to material: zirconium ball: the mass ratio of dehydrated alcohol=1: 1～5: 3～6 carries out ball milling to be mixed 12～24 hours, to even;
The 3rd step dried slip to constant weight;
Behind the 4th step microwave heating to 1200～1400 ℃, constant temperature got final product in 10～30 minutes.
When microwave heating, can feed argon gas and do shielding gas.
The present invention has utilized the carbothermic method principle, and its reaction formula is:
The present invention compared with prior art has following advantage and beneficial effect:
1. the present invention has gas CO to produce in reaction, so the pressure of CO can exert an influence to the reacting initial temperature of this reaction formula, according to reference, works as P
CODuring=0.1atm, the starting temperature of above-mentioned reaction is 1200 ℃.Since with the synthetic TiC of microwave heating, so reaction reaches 1200～1400 ℃ very soon, and can be at the synthetic fast TiC of this temperature range, synthetic ratio reaches more than 97%.The grain size of product TiC is 45.63～87.57nm.
2. technological process of the present invention is simple, easy to control, and gained TiC powder is difficult for reuniting, and need not reprocess inclusion-free.
(4) embodiment
Embodiment one
The first step is with titanium dioxide (15nm, rutile-type, content＞91%) and Shawinigan black (specific surface area 58.866m
2/ g) in baking oven 105 ℃ dry to constant weight, take by weighing titanium dioxide 87.7 gram, Shawinigan black 36 grams;
Second step was got sub 450 grams of zirconia ball, and 95% ethanol 500ml is reinforced, carries out ball milling and mixed 12 hours in aluminum oxide ball milling jar (or vulcanizer), to even;
The 3rd step dried slip to constant weight under 100 ℃;
The 4th step claimed the 75 gram MFM-863 type microwave agglomerating furnaces of packing into compound, vacuumized then 20 minutes, fed argon gas and made protection gas, and pressure is 1atm, microwave heating to 1200 ℃, and constant temperature got final product in 30 minutes.
Embodiment two
The first step is with titanium dioxide (15nm, rutile-type, content＞91%) and Shawinigan black (specific surface area 58.866m
2/ g) in baking oven 80 ℃ dry to constant weight, take by weighing titanium dioxide 87.7 gram, Shawinigan black 36 grams;
Second step was got sub 125 grams of zirconia ball, and 95% ethanol 300ml is reinforced, carries out ball milling and mixed 24 hours in aluminum oxide ball milling jar (or vulcanizer), to even;
The 3rd step dried slip to constant weight under 80 ℃;
The 4th step claimed the 75 gram MFM-863 type microwave agglomerating furnaces of packing into compound, vacuumized then 20 minutes, fed argon gas and made protection gas, and pressure is 1atm, microwave heating to 1300 ℃, and constant temperature got final product in 20 minutes.
Embodiment three
The first step is with titanium dioxide (15nm, rutile-type, content＞91%) and Shawinigan black (specific surface area 58.866m
2/ g) in baking oven 90 ℃ dry to constant weight, take by weighing titanium dioxide 87.7 gram, Shawinigan black 36 grams;
Second step was got sub 620 grams of zirconia ball, and 95% ethanol 600ml is reinforced, carries out ball milling and mixed 18 hours in aluminum oxide ball milling jar (or vulcanizer), to even;
The 3rd step dried slip to constant weight under 90 ℃;
The 4th step claimed the 75 gram MFM-863 type microwave agglomerating furnaces of packing into compound, vacuumized then 20 minutes, fed argon gas and made protection gas, and pressure is 1atm, microwave heating to 1400 ℃, and constant temperature got final product in 10 minutes.
Above-mentioned three embodiment are cooled to discharging and weighing after the room temperature, to calculate synthetic ratio, get a certain amount of TiC then and carry out material phase analysis with X-ray diffraction method, carry out sreen analysis with transmission electron microscope).Analytical results sees the following form:
| Synthetic ratio % | Material phase analysis | Grain size (nm) | |
| Embodiment one | 97 | Product 97% is TiC, and all the other are TiO 2 | 45.63 |
| Embodiment two | 100 | Product is TiC entirely | 87.57 |
| Embodiment three | 100 | Product is TiC entirely | 59.04 |
Claims (2)
1. the method for a microwave synthetizing nano level titanium carbide is characterized in that, it comprises the steps and processing condition:
The first step dries Nano titanium dioxide and Shawinigan black to constant weight, and according to titanium dioxide: the quality of Shawinigan black=80: 36 compares weighing;
Second goes on foot according to material: zirconium ball: the mass ratio of dehydrated alcohol=1: 1～5: 3～6 carries out ball milling to be mixed 12～24 hours, to even;
The 3rd step dried slip to constant weight;
Behind the 4th step microwave heating to 1200～1400 ℃, constant temperature got final product in 10～30 minutes;
Described nano level carbonization titanium is 45.63～87.57 nano titanium carbides.
2. the method for a kind of microwave synthetizing nano level titanium carbide according to claim 1 is characterized in that, feeds argon gas and do shielding gas when microwave heating.
Priority Applications (1)
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| CN 01129991 CN1124977C (en) | 2001-11-29 | 2001-11-29 | Microwave synthesis process for nanometer level titaniuym carbide |
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| CN 01129991 CN1124977C (en) | 2001-11-29 | 2001-11-29 | Microwave synthesis process for nanometer level titaniuym carbide |
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| CN1348919A CN1348919A (en) | 2002-05-15 |
| CN1124977C true CN1124977C (en) | 2003-10-22 |
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Families Citing this family (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1299982C (en) * | 2004-07-08 | 2007-02-14 | 武汉科技大学 | Method of preparing titanium carbide material using fused salt method |
| CN1323949C (en) * | 2004-09-27 | 2007-07-04 | 南京大学 | Preparation method of titanium carbide and titanium nitride one dimension nanometer construction material |
| CN100429176C (en) * | 2005-12-02 | 2008-10-29 | 中国科学院上海硅酸盐研究所 | Process for preparing nano complex phase ceramic material by in-situ reaction |
| CN100484872C (en) * | 2006-03-31 | 2009-05-06 | 华南理工大学 | Method of continuous microwave synthesis of nano-class titanium carbide and microwave synthetizer |
| DE102008025582A1 (en) * | 2008-01-11 | 2009-07-16 | Tesa Ag | Process for the production of titanium carbide |
| CN101792140B (en) * | 2010-03-13 | 2012-02-01 | 浙江大学 | Titanium carbide micropowder and preparation method thereof |
| CN102050449B (en) * | 2010-05-31 | 2012-07-04 | 东阳市沃诺斯硬质合金有限公司 | Production method of nano TiC powdered material |
| CN101920958A (en) * | 2010-08-06 | 2010-12-22 | 刘昭晖 | Method for preparing nano zirconium carbide |
| CN102373358B (en) * | 2010-08-12 | 2013-09-04 | 苏州艾默特材料技术有限公司 | Preparation method of TiC dispersion-strengthened molybdenum alloy |
| CN103332691A (en) * | 2013-06-25 | 2013-10-02 | 桂林理工大学 | Method for preparing TiC powder by respectively using tetrabutyl titanate and sucrose as titanium source and carbon source |
| CN104961130A (en) * | 2015-06-09 | 2015-10-07 | 四川大学 | Rotary dynamic continuous preparation method of metal carbide powder, and rotary dynamic continuous preparation apparatus thereof |
| CN104961129A (en) * | 2015-06-09 | 2015-10-07 | 四川大学 | Push type dynamic continuous preparation method of metal carbide powder, and push type dynamic continuous preparation apparatus thereof |
| CN105014090A (en) * | 2015-07-08 | 2015-11-04 | 上海大学 | Method for preparing TiFe alloy by reducing ferrotitanium oxide under microwave field |
| CN105314635A (en) * | 2015-12-07 | 2016-02-10 | 武汉科技大学 | High-purity titanium carbide powder and preparation method thereof |
| CN106587063A (en) * | 2016-12-19 | 2017-04-26 | 北方民族大学 | Method for synthesizing titanium carbide through soft mechanical force chemical auxiliary microwaves |
| CN108637268B (en) * | 2018-04-24 | 2021-12-28 | 海南大学 | Method for preparing composite Ti (C, N) metal ceramic powder by microwave carbothermic reduction |
| CN112850688A (en) * | 2021-02-03 | 2021-05-28 | 成都市丽睿科技有限公司 | Preparation method of nanoscale carbon material |
| CN112777597A (en) * | 2021-03-23 | 2021-05-11 | 上海简巨医学生物工程有限公司 | Niobium carbide nano material and preparation method thereof |
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