CN101863459A - Process for preparing titanium nitride with controllable shape by alcohol-heating method - Google Patents
Process for preparing titanium nitride with controllable shape by alcohol-heating method Download PDFInfo
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- CN101863459A CN101863459A CN 201010165316 CN201010165316A CN101863459A CN 101863459 A CN101863459 A CN 101863459A CN 201010165316 CN201010165316 CN 201010165316 CN 201010165316 A CN201010165316 A CN 201010165316A CN 101863459 A CN101863459 A CN 101863459A
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Abstract
The invention relates to a preparation method of a titanium nitride material, in particular to a process for preparing titanium nitride with controllable shape by an alcohol-heating method. The prior art has the defects of strict technological condition, difficult control of reaction process, low yield, impurities contained in a product, and irregular particle shape. The method comprises the steps of: slowly dripping 0.5mL to 2mL of titanium compound into 10mL to 60mL of alcohol solvent; stirring for 10 to 30 minutes at room temperature; putting into a water heating kettle; standing and aging at 373K to 443K for 0.5 to 72 hours; taking and naturally cooling products to room temperature; washing sediment by using anhydrous ethanol for 3 to 5 times; putting the washed substances into a vacuum oven at 373K, drying and transferring into a roasting furnace; roasting at 1573K under the nitrogen protection; and cooling the products to room temperature to obtain the titanium nitride material. The process has the advantages of simplicity, high product yield, high purity and regular titanium nitride particle shape, and can be used for preparing titanium nitride of different shape structures.
Description
Technical field
The present invention is the titanium nitride material preparation, and the hot legal system of particularly a kind of alcohol is equipped with the controlled titanium nitride technology of pattern.
Technical background
The microhardness of titanium nitride is 21GPa, 2950 ℃ of fusing points, be a kind ofly have hardness height, fusing point height, the type material of characteristics such as chemical stability is good, erosion resistance is strong, abrasion resistance and good in oxidation resistance.Can be used for improving the wear resistance of sintered carbide tools, make the molten metal crucible, be used for special environment such as heat-resisting, corrosion-resistant, wear-resisting.Titanium nitride has good electrical conductivity, as the superconducting material of electro-conductive material such as the electrode of fused salt electrolysis and electrical contact and higher superconduction critical temperature.Titanium nitride also has good catalytic performance and biocompatibility, as catalyzer or catalytic carrier and biomaterial.Owing to outstanding performance such as its catalytic property, electrical property and optical property, become the important materials in nanosecond science and technology field.
Existing preparation titanium nitride method has multiple: carbothermic method for example; Aluminothermy and magnesium reduction process; Chemical Vapor deposition process (CVD); Self propagating high temperature synthesis method (SHS); The microwave-assisted combustion method; Quick solid-phase synthesis (SSM); And spark-discharge method in the solid-liquid exchange process, plasma method, high light particle beam method of evaporation, fusion electrolysis method, high-energy ball milling method, liquefied ammonia; Metallic titanium powder or TiH
2Powder is at N
2Or NH
3Direct nitridation method or the like under the atmosphere.The processing requirement harshness that has in these methods; The reaction process that has is wayward; Contain impurity, the particle shape irregularity in the low and product of the product yield that has.Carbothermic method is most widely used owing to method is easy, easy to operate among the preparation method, is one of the most frequently used method of suitability for industrialized production metal nitride.Existing carbothermic method is utilized TiO
2Be raw material, under the situation that carbonaceous reducing agent exists, high-temperature roasting makes titanium nitride in the nitrogen atmosphere, 1380～1800 ℃ of synthesis temperatures, reaction times 5-20 hour.Because particle shape irregularity behind the sintering temperature height of synthetic nitride powder and the sintering influences and defines the widespread use of titanium nitride material.Therefore invent that a kind of synthesis temperature is low, processing ease, the preparation method is simple, titanium nitride pattern pure hot legal system controlled, good product quality is equipped with the controlled titanium nitride technology of pattern that important practical sense is arranged.
Summary of the invention
The purpose of this invention is to provide that a kind of synthesis temperature is low, processing ease, preparation method are simple, titanium nitride pattern pure hot legal system controlled, good product quality is equipped with the controlled titanium nitride technology of pattern.
Technical scheme of the present invention is as follows:
The hot legal system of a kind of alcohol is equipped with the controlled titanium nitride technology of pattern, and step is as follows:
(1) titanium compound with 0.5-2mL slowly splashes in the alcoholic solvent of 10-60mL, stirs 10-30min under the room temperature, adds the 10ml ether;
(2) step (1) product is put into water heating kettle, the still aging 0.5-72h of 373-443K;
(3) step (2) product is taken out, naturally cools to room temperature, throw out absolute ethanol washing 3-5 time;
(4) will wash the back material and put into vacuum drying oven 373K oven dry;
(5) step (4) product is moved in the stoving oven nitrogen protection, 1573K roasting;
(6) step (5) product is taken out, be cooled to room temperature.
Titanium compound in the step (1) is a kind of in titanium tetrachloride, tetra-n-butyl titanate, titanium sulfate, the titanyl sulfate.
Alcoholic solvent in the step (1) is ethanol, glycerol, or the mixed solvent of ethanol and glycerol.
Main points of the present invention are: by roasting under the gas shiled of the hot method combined nitrogen of alcohol, and the controlled titanium nitride of preparation pattern.By changing the kind in titanium source, the titanium nitride that the kind of alcohol and pure hot time can prepare the different-shape structure.
Technology of the present invention is divided into three sections and carries out: at first, at normal temperatures, the preparation precursor aqueous solution; Then precursor aqueous solution is transferred in the tetrafluoroethylene water heating kettle, the throw out that obtains washs drying treatment, control roasting time and temperature roasting under nitrogen protection; At last, be cooled to room temperature and can obtain titanium nitride.
Advantage of the present invention is:
1, technology is simple;
2, reaction process is controlled easily;
3, product yield height;
4, the product purity height is free from foreign meter;
5, the titanium nitride particles shape is regular;
The titanium nitride that 6, can prepare the different-shape structure.
Description of drawings
Fig. 1 is the SEM figure of TiN forerunner's sample of not roasting: (a) ball-like structure, (b) nucleocapsid structure, (c) flower-like structure, (d) sheet structure.
Under Fig. 2 nitrogen protection, the SEM of the TiN sample that roasting obtains figure.(a) ball-like structure, (b) nucleocapsid structure, (c) flower-like structure, (d) sheet structure.
The XRD figure of Fig. 3 titanium nitride sample.(a) ball-like structure, (b) nucleocapsid structure, (c) flower-like structure, (d) sheet structure.
Embodiment
Embodiment 1
Normal temperature slowly splashes into the glycerol (available from Shanghai chemical reagents corporation of Chinese Medicine group [experiment reagent CR]) of 10mL in the 20mL ethanol solution, and vigorous stirring obtains solution A.Get titanyl sulfate (available from the 15%H of Aldrich chemical reagents corporation [experiment reagent CR]
2SO
4Solution) 1ml splashes in the A solution and vigorous stirring, waits to drip off the back and continues to stir the TiO that 30min obtains homogeneous transparent
2Colloidal sol.The 10ml ether is joined in the resulting colloidal sol, continue to stir 10min, get sol B.Sol B is transferred in the 50mL water heating kettle, kept temperature 383K, place 1h, take out and naturally cool to room temperature.It is colourless to ethanol with washing with alcohol 3 times to take out throw out, puts into the 373K oven drying behind the suction filtration.With the TiO that obtains
2Precursor is transferred in the retort furnace, and under nitrogen protection, roasting 1573K keeps 8h.Be cooled to room temperature, so just obtained the titanium nitride of ball-like structure.
Embodiment 2
Normal temperature slowly splashes into the glycerol (available from Shanghai chemical reagents corporation of Chinese Medicine group [experiment reagent CR]) of 10mL in the 20mL ethanol solution, and vigorous stirring obtains solution A.Get titanyl sulfate (available from the 15%H of Aldrich chemical reagents corporation [experiment reagent CR]
2SO
4Solution) 1ml splashes in the A solution and vigorous stirring, waits to drip off the back and continues to stir the TiO that 30min obtains homogeneous transparent
2Colloidal sol.The 10ml ether is joined in the resulting colloidal sol, continue to stir 10min, get sol B.Sol B is transferred in the 50mL water heating kettle, kept temperature 383K, place 48h, take out and naturally cool to room temperature.It is colourless to ethanol with washing with alcohol 3 times to take out throw out, puts into the 373K oven drying behind the suction filtration.With the TiO that obtains
2Precursor is transferred in the retort furnace, and under nitrogen protection, roasting 1573K keeps 8h.Be cooled to room temperature, so just obtained the titanium nitride of nucleocapsid structure.
Normal temperature slowly splashes into the glycerol (available from Shanghai chemical reagents corporation of Chinese Medicine group [experiment reagent CR]) of 10mL in the 20mL ethanol solution, and vigorous stirring obtains solution A.Get titanium tetrachloride (Shanghai chemical reagents corporation of Chinese Medicine group [experiment reagent CR]) 1ml and splash in the A solution and vigorous stirring, wait to drip off the back and continue to stir the TiO that 30min obtains homogeneous transparent
2Colloidal sol.The 10ml ether is joined in the resulting colloidal sol, continue to stir 10min, get sol B.Sol B is transferred in the 50mL water heating kettle, kept temperature 383K, place 48h, take out and naturally cool to room temperature.It is colourless to ethanol with washing with alcohol 3 times to take out throw out, puts into the 373K oven drying behind the suction filtration.With the TiO that obtains
2Precursor is transferred in the retort furnace, and under nitrogen protection, roasting 1573K keeps 8h.Be cooled to room temperature, so just obtained the titanium nitride of flower-like structure.
Embodiment 4
Normal temperature with the glycerol (available from Shanghai chemical reagents corporation of Chinese Medicine group [experiment reagent CR]) of 10mL and titanyl sulfate (available from the 15%H of Aldrich chemical reagents corporation [experiment reagent CR]
2SO
4Solution) 1ml mix A solution, and vigorous stirring 30min obtains the TiO of homogeneous transparent
2Colloidal sol.The 10ml ether is joined in the resulting colloidal sol, continue to stir 10min, get sol B.Sol B is transferred in the 50mL water heating kettle, kept temperature 383K, place 48h, take out and naturally cool to room temperature.It is colourless to ethanol with washing with alcohol 3 times to take out throw out, puts into the 373K oven drying behind the suction filtration.With the TiO that obtains
2Precursor is transferred in the retort furnace, and under nitrogen protection, roasting 1573K keeps 8h.Be cooled to room temperature, so just obtained the titanium nitride of sheet structure.
The structural parameter of the titanium nitride of embodiment 1,2,3,4 preparations see Table 1:
Table 1: the structural parameter of different-shape structure titanium nitride
The above is the preferred embodiments of the present invention only, is not limited to the present invention, and for a person skilled in the art, the present invention can have various changes and variation.Within the spirit and principles in the present invention all, any modification of being done, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (3)
1. the hot legal system of alcohol is equipped with the controlled titanium nitride technology of pattern, and step is as follows:
(1) titanium compound with 0.5-2mL slowly splashes in the alcoholic solvent of 10-60mL, stirs 10-30min under the room temperature, adds the 10ml ether;
(2) step (1) product is put into water heating kettle, the still aging 0.5-72h of 373-443K;
(3) step (2) product is taken out, naturally cools to room temperature, throw out absolute ethanol washing 3-5 time;
(4) will wash the back material and put into vacuum drying oven 373K oven dry;
(5) step (4) product is moved in the stoving oven nitrogen protection, 1573K roasting;
(6) step (5) product is taken out, be cooled to room temperature.
2. the hot legal system of alcohol according to claim 1 is equipped with the controlled titanium nitride technology of pattern, it is characterized in that: the titanium compound in the step (1) is a kind of in titanium tetrachloride, tetra-n-butyl titanate, titanium sulfate, the titanyl sulfate.
3. the hot legal system of alcohol according to claim 1 is equipped with the controlled titanium nitride technology of pattern, it is characterized in that: the alcoholic solvent in the step (1) is ethanol, glycerol, or the mixed solvent of ethanol and glycerol.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102120567A (en) * | 2011-03-17 | 2011-07-13 | 上海师范大学 | Process for preparing vanadium nitride |
| CN102659087A (en) * | 2012-03-28 | 2012-09-12 | 上海师范大学 | A method for preparing titanium nitride by utilizing in-situ carbothermal reduction-nitridation |
| CN106744741A (en) * | 2016-12-07 | 2017-05-31 | 广东工业大学 | A kind of Fe2O3 doping titanium nitride nano pipe and its preparation method and application |
| CN107161963A (en) * | 2017-06-05 | 2017-09-15 | 陕西科技大学 | A kind of preparation method of particles self assemble titanium nitride material |
| CN109095445A (en) * | 2018-10-30 | 2018-12-28 | 合肥昂途纳米新材料有限公司 | A kind of preparation method of hollow out nanobelt, hollow out nanobelt and application |
| CN109179348A (en) * | 2018-08-17 | 2019-01-11 | 广东工业大学 | A kind of flower-shaped titanium nitride and its preparation method and application |
| CN110157937A (en) * | 2019-04-09 | 2019-08-23 | 中国科学院金属研究所 | A kind of titanium nitride block preparation method that ingredient is controllable |
| CN112897483A (en) * | 2021-01-22 | 2021-06-04 | 盐城工学院 | TiN(B)@TiO2Core-shell particle powder material and method of preparation |
Citations (3)
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|---|---|---|---|---|
| JPS6270208A (en) * | 1985-09-25 | 1987-03-31 | Toray Ind Inc | Production of titanium nitride composition |
| US5876682A (en) * | 1997-02-25 | 1999-03-02 | The United States Of America As Represented By The Secretary Of The Navy | Nanostructured ceramic nitride powders and a method of making the same |
| CN101318639A (en) * | 2008-07-15 | 2008-12-10 | 四川大学 | Method for preparing nano-titanium nitride with mesoporous organic-inorganic composite precursors |
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2010
- 2010-04-29 CN CN2010101653168A patent/CN101863459B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6270208A (en) * | 1985-09-25 | 1987-03-31 | Toray Ind Inc | Production of titanium nitride composition |
| US5876682A (en) * | 1997-02-25 | 1999-03-02 | The United States Of America As Represented By The Secretary Of The Navy | Nanostructured ceramic nitride powders and a method of making the same |
| CN101318639A (en) * | 2008-07-15 | 2008-12-10 | 四川大学 | Method for preparing nano-titanium nitride with mesoporous organic-inorganic composite precursors |
Non-Patent Citations (3)
| Title |
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| 《J. AM. CHEM. SOC.》 20070616 Hexing Li et al. Mesoporous Titania Spheres with Tunable Chamber Stucture and Enhanced Photocatalytic Activity 8406-8407 1-3 第129卷, 第27期 2 * |
| 《稀有金属材料与工程》 20070831 谈国强 等 溶剂热合成纳米氮化钛粉体的研究 247-249 1-3 第36卷, 2 * |
| 《陕西科技大学学报》 20041031 谈国强 等 合成氧化钛粉体的研究进展 157-162 1-3 第22卷, 第5期 2 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102120567A (en) * | 2011-03-17 | 2011-07-13 | 上海师范大学 | Process for preparing vanadium nitride |
| CN102659087A (en) * | 2012-03-28 | 2012-09-12 | 上海师范大学 | A method for preparing titanium nitride by utilizing in-situ carbothermal reduction-nitridation |
| CN106744741A (en) * | 2016-12-07 | 2017-05-31 | 广东工业大学 | A kind of Fe2O3 doping titanium nitride nano pipe and its preparation method and application |
| CN107161963A (en) * | 2017-06-05 | 2017-09-15 | 陕西科技大学 | A kind of preparation method of particles self assemble titanium nitride material |
| CN109179348A (en) * | 2018-08-17 | 2019-01-11 | 广东工业大学 | A kind of flower-shaped titanium nitride and its preparation method and application |
| CN109095445A (en) * | 2018-10-30 | 2018-12-28 | 合肥昂途纳米新材料有限公司 | A kind of preparation method of hollow out nanobelt, hollow out nanobelt and application |
| CN109095445B (en) * | 2018-10-30 | 2021-11-19 | 合肥昂途纳米新材料有限公司 | Preparation method of hollowed-out nanobelt, hollowed-out nanobelt and application |
| CN110157937A (en) * | 2019-04-09 | 2019-08-23 | 中国科学院金属研究所 | A kind of titanium nitride block preparation method that ingredient is controllable |
| CN112897483A (en) * | 2021-01-22 | 2021-06-04 | 盐城工学院 | TiN(B)@TiO2Core-shell particle powder material and method of preparation |
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| CN101863459B (en) | 2011-11-30 |
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