CN100579898C - Preparation of titanium nitride nanopower - Google Patents
Preparation of titanium nitride nanopower Download PDFInfo
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- CN100579898C CN100579898C CN200810049914A CN200810049914A CN100579898C CN 100579898 C CN100579898 C CN 100579898C CN 200810049914 A CN200810049914 A CN 200810049914A CN 200810049914 A CN200810049914 A CN 200810049914A CN 100579898 C CN100579898 C CN 100579898C
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Abstract
The invention relates to a method for producing the nanometer-level powdery titanium nitride. The method adopts the nanometer tube titanic acid as the titanium source, and feeds ammonia gas into a pipe heater, then the temperature is raised from the room temperature to 800-1000 DEG C to make nitridation reaction for 0.5 to 24 hours, then the nanometer-level powdery titanium nitride can be obtained after the cooling step. The method adopts the nanometer tube titanic acid as one of the raw materials, which is simple in technology, convenient to operate and is suitable for large-scale production. The nanometer-level powdery titanium nitride produced by the method is small in particle size and uniform in distribution; nearly complete absorption is realized in the visible area and the near infrared area; meanwhile, the product has no fluorescence emission property and can be used as heat-absorbing material.
Description
(1) technical field
The present invention relates to a kind of preparation method of titanium nitride nano powder.
(2) background technology
Titanium nitride is a kind of type material, has hardness height, fusing point height, characteristics that chemical stability is good.Because it has good abrasion resistance, in mechanical cutting processing industry, extensively adopts chemical Vapor deposition process depositing titanium nitride coating on cutting tool,, prolong the work-ing life of cutting tool to improve the wear resisting property of cutter.
At present, the method for preparing titanium nitride powder has multiple, as spark discharge in chemical gas phase (CVD) method, fusion electrolysis method, high-energy ball milling method, the liquefied ammonia, metallic titanium powder or TiH
2Powder is at N
2Or NH
3Direct nitridation method etc. under the atmosphere, as people such as Li Jingguo is raw material with titanium dioxide, adopt the ammonia ammoniation process to prepare Nano titanium nitride particulate (Li Jingguo, high Lian, Zhang Qinghong etc., the preparation of Nano titanium nitride powder and influence factor thereof [J]. Journal of Inorganic Materials, 2003,18 (4): 765～771).
The nanotube metatitanic acid is a kind of novel monodimension nanometer material, has nano tubular structure, bigger specific surface area, and people are synthetic to it, big quantity research has been carried out in structure, character and application.Its application mainly is as catalyzer or support of the catalyst, sensing or optics; Be used for the additive of pottery, coating, plastics, the recovery catalyst of silver ions and the chromatogram carrier of analyzing lower paraffin hydrocarbons.But do not find the nanotube metatitanic acid is used for the report of titanium nitride nano powder preparing as yet.
(3) summary of the invention
The object of the present invention is to provide a kind of preparation method of titanium nitride nano powder, is one of raw material with the nanotube metatitanic acid, and method is simple, and the titanium nitride nano powder characteristic that makes is good.
The technical solution used in the present invention is as follows:
A kind of preparation method of titanium nitride nano powder is the titanium source with the nanotube metatitanic acid, feeds ammonia in tube furnace, is warming up to 800-1000 ℃ from room temperature and carries out nitrogenizing reaction 0.5-24h, can obtain the titanium nitride nano powder after the cooling.
The present invention is the titanium source with the nanotube metatitanic acid, guarantees the transformation efficiency of nanotube metatitanic acid and the operability of reaction when producing in enormous quantities by strict control reaction temperature, simultaneously by also can obtain the nano-powder of different-grain diameter to the control of temperature and time; By adopting the nanotube metatitanic acid is the titanium source, and other parameter control, and the titanium nitride nano diameter of particle that present method makes is smaller, and it is more even to distribute, substantially at 10-50nm; And the titanium nitride nano powder that makes is a black, is close to absorption fully at visible light and near-infrared region, and does not have fluorescent emission character.
Preferably, before nitrogenizing reaction is carried out in heating, preferably feed ammonia for some time the ammonia environment during with the assurance reaction in advance.The flow rate of ammonia is good with 20-200mL/min during reaction.
Further, heat up to adopt temperature programming, be raised to 800-1000 ℃ with the speed of 10 ℃/min from room temperature.
Aforesaid raw material nano pipe metatitanic acid can adopt laxative remedy to make: with titanium dioxide and mass concentration is that the strong base solution of 20-60% mixes, 80-150 ℃ of reflux 5-30h in oil bath, leave standstill after the cooling, getting precipitation, to be washed with distilled water to pH be 6-8, in the strong acid of 0.01-0.1mol/L, soak 5-10h again after the filtration, filter after scouring once more and be drying to obtain described nanotube metatitanic acid.
The present invention has following advantage with respect to prior art:
Present method is one of raw material with the nanotube metatitanic acid, and method is simple, is convenient to operation, is fit to produce in enormous quantities.The titanium nitride nano diameter of particle that makes is little, distribution is more even; Be close to absorption fully at visible light and near-infrared region, and do not have fluorescent emission character, can be used as heat-sink material.
(4) description of drawings
Fig. 1 is the transmission electron microscope picture of the titanium nitride nano powder of preparation among the embodiment 2.
Fig. 2 is the X-ray diffractogram of the titanium nitride nano powder of preparation among the embodiment 2.
Fig. 3 is the ultraviolet-visible-near-infrared spectrum figure of the titanium nitride nano powder of preparation among the embodiment 2.
Fig. 4 is the fluorescence spectrum figure of the titanium nitride nano powder of preparation among the embodiment 2.
Fig. 5 is the transmission electron microscope picture of the ammonification nano-ti powder body of preparation among the embodiment 3.
Fig. 6 is the X-ray diffractogram of the titanium nitride nano powder of preparation among the embodiment 3.
(5) embodiment:
Below with specific embodiment technical scheme of the present invention is described, but protection scope of the present invention is not limited thereto:
Embodiment 1: the preparation of nanotube metatitanic acid
3g titanium dioxide (anatase octahedrite) powder slowly joined fill in the polytetrafluoroethylcontainer container that the 300ml mass concentration is a 40%NaOH solution, place oil bath to be warming up to 118 ℃, constant temperature backflow 24h, cooling-sedimentation, inclining supernatant liquor, and being precipitated to PH with distilled water wash is 8.0, filters, use the salt acid soak 5 hours of 0.1mol/L then, filter, wash, be drying to obtain presoma nanotube metatitanic acid.
Embodiment 2-3 is the preparation of titanium nitride nano powder
Embodiment 2
The nanotube metatitanic acid presoma of 1.5g embodiment 1 preparation is placed in the tube furnace, pre-logical ammonia was warming up to 900 ℃ from room temperature with the temperature rise rate of 10 ℃/min after 30 minutes, and constant temperature keeps 4h, and this process keeps logical ammonia, and then naturally cool to room temperature, promptly prepare the Nano titanium nitride powder.Its transmission electron microscope (TEM) is schemed as shown in Figure 1, and visible particle diameter of nanometer powder is about 20nm; Fig. 2 is its X-ray diffractogram, as seen is the titanium nitride structure of cube phase; The ultraviolet-visible-near-infrared spectrum of Fig. 3 and the fluorescence spectrum of Fig. 4 show that this titanium nitride nano powder is close to all absorptions at visible light and near-infrared region, and do not have fluorescent emission character.
Embodiment 3
The nanotube metatitanic acid presoma of 1.5g embodiment 1 preparation is placed in the tube furnace, pre-logical ammonia was warming up to 1000 ℃ from room temperature with the temperature rise rate of 10 ℃/min after 30 minutes, and constant temperature keeps 4h, and this process keeps logical ammonia, and then naturally cool to room temperature, promptly prepare the Nano titanium nitride powder.Its transmission electron microscope picture is seen Fig. 5, and the particle diameter of nanometer powder that makes is about 40nm; X-ray diffractogram is seen Fig. 6.
Claims (4)
1. the preparation method of a titanium nitride nano powder is characterized in that described method for being the titanium source with the nanotube metatitanic acid, feeds ammonia in tube furnace, and being warming up to 800-1000 ℃ from room temperature carries out nitrogenizing reaction 0.5-24h, promptly gets the titanium nitride nano powder after the cooling; Described nanotube metatitanic acid is made by laxative remedy: with titanium dioxide and mass concentration is that the strong base solution of 20-60% mixes, 80-150 ℃ of reflux 5-30h in oil bath, leave standstill after the cooling, getting precipitation, to be washed with distilled water to pH be 6-8, in the strong acid of 0.01-0.1mol/L, soak 5-10h again after the filtration, filter after scouring once more and be drying to obtain described nanotube metatitanic acid.
2. the preparation method of titanium nitride nano powder as claimed in claim 1 is characterized in that in the tube furnace being warmed up to 800-1000 ℃ from room temperature with the speed of 10 ℃/min.
3. the preparation method of titanium nitride nano powder as claimed in claim 1, the flow rate that it is characterized in that ammonia is 20-200mL/min.
4. the preparation method of titanium nitride nano powder as claimed in claim 1 is characterized in that the titanium nitride nano diameter of particle that makes is 10-50nm.
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| Application Number | Priority Date | Filing Date | Title |
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| CN200810049914A CN100579898C (en) | 2008-05-30 | 2008-05-30 | Preparation of titanium nitride nanopower |
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| CN200810049914A CN100579898C (en) | 2008-05-30 | 2008-05-30 | Preparation of titanium nitride nanopower |
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| CN100579898C true CN100579898C (en) | 2010-01-13 |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102351157A (en) * | 2011-08-10 | 2012-02-15 | 河南大学 | Iron-doped novel titanium nitride nano particle |
| CN105355883B (en) * | 2015-11-18 | 2017-09-29 | 海南大学 | A kind of TiN/TiO2Core-shell nano linear array and preparation method thereof |
| CN107215851A (en) * | 2016-03-22 | 2017-09-29 | 纳琳威纳米科技（上海）有限公司 | A kind of high heat insulation nano ceramic powder and its production and use |
| CN107161963B (en) * | 2017-06-05 | 2019-03-26 | 陕西科技大学 | A kind of preparation method of particles self assemble titanium nitride material |
| CN108325553B (en) * | 2018-02-02 | 2020-12-22 | 河南科技大学 | Preparation method of titanium nitride microsphere catalyst with coated magnetic core structure |
| CN108557783B (en) * | 2018-06-26 | 2022-02-11 | 重庆大学 | Preparation method of high-purity nano titanium nitride powder |
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Inventor after: Zhang Jiwei Inventor after: Wang Haiyan Inventor after: Chen Weiping Inventor after: Wu Zhishen Inventor after: Zhang Zhijun Inventor after: Jin Zhensheng Inventor before: Zhang Jiwei Inventor before: Chen Weiping Inventor before: Wu Zhishen Inventor before: Zhang Zhijun Inventor before: Jin Zhensheng |
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Free format text: CORRECT: INVENTOR; FROM: ZHANG JIWEI CHEN WEIPING WU ZHISHEN ZHANG ZHIJUN JIN ZHENSHENG TO: ZHANG JIWEI WANG HAIYAN CHEN WEIPING WU ZHISHEN ZHANG ZHIJUN JIN ZHENSHENG |
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Granted publication date: 20100113 Termination date: 20140530 |