CN1431146A - Method for preparing powder of nano vanadium nitride in cubic phase - Google Patents
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- CN1431146A CN1431146A CN 03115491 CN03115491A CN1431146A CN 1431146 A CN1431146 A CN 1431146A CN 03115491 CN03115491 CN 03115491 CN 03115491 A CN03115491 A CN 03115491A CN 1431146 A CN1431146 A CN 1431146A
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Abstract
A process for preparing cubic-phase nano vanadium nitride powder features that the V2O5.H2O powder is nitrified in tubular reactor at 500-800 deg.c for 3-5 hr in ammonia atmosphere. Its advantages are low reaction temp and short reaction time.
Description
Technical Field
The invention relates to a preparation method of cubic phase nano vanadium nitride powder, which can be used for preparing high-performance ceramics, wear-resistant materials, catalysts and superconducting materials. Belongs to the field of nanometer material.
Background
Metal nitrides (particularly transition metal nitrides) have unique physical and chemical properties, and have recently received increasing attention from material researchers and business persons. Due to its potential application prospect, the preparation technology of the ultrafine particles of the metal nitride is widely regarded. Vanadium nitride has high relative density (6.04), high melting point (2030 ℃), high hardness (Mohs hardness of 9), and catalytic activity and superconductivity. As a novel material, vanadium nitride has wide application prospect.
The nano vanadium nitride refers to nitrogen with the grain size within 100nmThe vanadium nitride product can be used for replacing micron-sized vanadium nitride, so that the sintering temperature can be reduced, and the sintering performance can be improved; the reinforcing phase can effectively improve the strength and the wear resistance of metal and ceramic matrixes; as a catalyst, has higher activity; it can also be used as a superconducting material. Therefore, the nano vanadium nitride has great practical value. Industrially, vanadium nitride is generally produced by a reduction method. The reduction method is to fully mix stoichiometric carbon and vanadium pentoxide and carry out reduction nitridation reaction at 1250 ℃ in a nitrogen atmosphere to obtain vanadium nitride. The biggest defects of the reaction are high reaction temperature, difficult preparation of the superfine powder, secondary carbon removal required by a reduction method, complex process and certain amount of impurities contained in the product. Can also be prepared by reacting the mixed gas of hydrogen and nitrogen with vanadium tetrachloride at 1400-1600 ℃; or reacting ammonia gas with ammonium metavanadate at the temperature of 1000-1100 ℃. At present, the research on vanadium nitride Films is more, and the preparation of the vanadium nitride Films by adopting a pulse laser deposition method is reported by Z.N.Dail et al in ThinSolid Films Vol.347(1999) PP.117-120. C.H.Ma et al, Surface and coatings Technology, Vol.133-134(2000) pp.289-294, reported the use of ion assisted deposition for the preparation of vanadium nitride coatings. Relatively few reports are made on the preparation of vanadium nitride ultrafine powder. Choi, J.G.In Applied Catalysis A: gemeral Vol.168(1998) pp.47-56 reports that V2O5 is used as a raw material, ammonia gas is used as a nitriding agent, and a temperature-programmed reaction method is adopted to prepare vanadium nitride powder, but the reaction temperature is high, and the prepared product has large granularity. In recent years, researchers at home and abroad have researched new methods for preparing nitride ultrafine powder. The method for preparing the corresponding nano nitride powder by directly nitriding the nano oxide powder by ammonia gas is a new method for synthesizing the nano metal nitride powder. Recently we have reported in the Journal of American ceramic Society Vol.84(2001) No.11 pp.2710-2712 and Vol.85(2002) No.5 pp.1294-1296, respectively, as nano TiO2And Cr2O3Synthesizing nano TiN and CrN powder by using the raw materials. However, they generally use nano-oxide as a premise, i.e. to prepare nano-nitride, the nano-oxide is prepared first, obviously, the process is complicated and the cost is high.
Disclosure of Invention
The invention aims to provide a method for preparing cubic phase nano vanadium nitride powder. More precisely, the method for preparing the cubic nanometer VN powder is not to prepare nanometer V firstly2O5A method for the precondition
The object of the invention is thus achieved: dissolving ammonium metavanadate as a starting material into distilled water at a certain temperature, adjusting the pH value by using a nitric acid solution, dropwise adding an ammonia water solution to generate a precipitate, and washing and drying to prepare vanadium pentoxide monohydrate powder; then, the monohydrate vanadium pentoxide powder is nitrified in a tubular reaction furnace at high temperature under the condition of flowing ammonia gas to synthesize cubic phase nano vanadium nitride powder.
It can be seen that the implementation can be divided into two major steps:
firstly, preparing monohydrate vanadium pentoxide powder; and secondly, nitriding the monohydrate vanadium pentoxide powder to prepare cubic phase nano vanadium nitride powder. Now, the following are detailed respectively:
preparation of monohydrate vanadium pentoxide powder
The invention takes ammonium metavanadate as a starting material. Firstly, adding ammonium metavanadate into distilled water, heating to dissolve the ammonium metavanadate, adjusting the pH value to 2.5-3 by using 30-60% nitric acid solution, and dropwise adding the ammonium metavanadate into 1-2M ammonia water solution under the stirring of 400-fold sand at the rotating speed of 800 rpm to generate precipitation. Filtering the precipitate, washing with anhydrous ethanol for 2-5 times, removing water in the precipitate to obtain amorphous vanadium pentoxide monohydrate powder with good dispersibility, drying the product, and sieving to obtain vanadium pentoxide monohydrate powder. The precipitation temperature is 50-70 ℃, the precipitation time is 1-12 hours, the drying condition of the precipitation product is 80 ℃ and 12 hours, and the precipitation product is ground and sieved by a 200-mesh sieve.
Preparation of cubic phase nano vanadium nitride powder
Putting the obtained vanadium pentoxide monohydrate powder into a quartz boat, putting the quartz boat into a tubular atmosphere furnace, introducingammonia gas, heating to 500-800 ℃ at a heating rate of 5-10 ℃/min at a flow rate of 0.5-5L/min, keeping the temperature for 3-5 hours, and naturally cooling to room temperature under flowing ammonia gas to obtain the nano vanadium nitride powder. The particle size and the nitriding speed of the nano vanadium nitride powder can be controlled by the reaction temperature; controlling the grain diameter of the nano vanadium nitride powder by controlling the nitriding heat preservation time; the reaction time is shortened by controlling the flow rate of ammonia gas. Therefore, the selection of the three parameters has a crucial influence on the particle size and yield after reaction, and the reasonable selection of the three parameters is important for organic matching.
The reaction process is as follows:
the preparation method of the nano vanadium nitride powder provided by the invention is characterized by comprising the following steps:
1. the reaction temperature is low and the reaction time is short.
2. The prepared nano vanadium nitride powder has the particle size of less than or equal to 50nm, good dispersibility and purity of more than 95 percent.
3. The production process is simple, the required production equipment is simple, and the industrial production is easy to realize.
4. The ammonia gas is used as the nitriding agent in the production process, and the reaction is more facilitated and the safety is higher than that of using nitrogen gas and hydrogen gas as the nitriding agent.
Drawings
FIG. 1X-ray diffraction Patternof vanadium nitride powder obtained by nitriding at 550 ℃ for 5 hours
FIG. 2.600 ℃ scanning electron micrograph of vanadium nitride powder obtained by nitriding at 5 hours
FIG. 3.700 ℃ X-ray diffraction pattern of vanadium nitride powder obtained by nitriding at 3 hours
FIG. 4.650 deg.C, scanning electron micrograph of vanadium nitride powder obtained by nitriding for 3 hours
FIG. 5.650 ℃ X-ray diffraction pattern of vanadium nitride powder obtained by nitriding at 5 hours
Detailed Description
Example 1:
11.7g of ammonium metavanadate was added to 1000ml of distilled water, and the mixture was heated to dissolve it. A50% nitric acid solution was added dropwise to adjust the pH to 3. 1M aqueous ammonia was added dropwise with stirring at 600 rpm, resulting in precipitation. And filtering the precipitate, washing the precipitate for 2 times by using absolute ethyl alcohol, drying a filter cake for 12 hours at the temperature of 80 ℃, grinding the filter cake, and sieving the filter cake by using a 200-mesh sieve to obtain the vanadium pentoxide monohydrate powder. Putting the prepared vanadium pentoxide monohydrate powder into a quartz boat, putting the quartz boat into a tubular atmosphere furnace, introducing ammonia gas, heating the quartz boat to 550 ℃ at a heating rate of 10 ℃/min with the flow of the ammonia gas being 1 liter/min, keeping the temperature for 5 hours, and naturally cooling the quartz boat to room temperature under flowing ammonia gas to obtain the nano vanadium nitride powder. FIG. 1 is an X-ray diffraction diagram of the nano vanadium nitride powder prepared in this example, which shows, in comparison with JCPDS card 35-0768: the powder is cubic phase vanadium nitride, which shows that the vanadium nitride powder with the purity of more than 95 percent can be obtained by nitriding the monohydrate vanadium pentoxide powder for 5 hours at 550 ℃ in ammonia gas flow, and five diffraction peaks in the figure are diffraction peaks of a 111 crystal face, a 200 crystal face, a 220 crystal face, a 311 crystal face and a 222 crystal face of the cubic phase vanadium nitride respectively. FIG. 2 is a field emission scanning electron micrograph showing that the particle size is 25-35 nm.
Example 2:
vanadium pentoxide monohydrate powder was prepared as described in example 1. Putting the monohydrate amorphous vanadium pentoxide powder into a quartz boat, putting the quartz boat into a tubular atmosphere furnace, introducing ammonia gas, heating the quartz boat to 600 ℃ at the temperature of 10 ℃/min with the flow rate of the ammonia gas being 1 liter/min, keeping the temperature for 5 hours, and naturally cooling the quartz boat to room temperature under flowing ammonia gas to obtain the nano vanadium nitride powder. FIG. 3 is an X-ray diffraction diagram of the nano vanadium nitride powder prepared in this example, which shows, in comparison with JCPDS card 35-0768: the powder is cubic phase vanadium nitride, which shows that the vanadium nitride powder with the purity of more than 95 percent can be obtained by nitriding the monohydrate vanadium pentoxide powder for 5 hours in ammonia gas flow at the temperature of 600 ℃, and five diffraction peaks in the figure are diffraction peaks of a 111 crystal face, a 200 crystal face, a 220 crystal face, a 311 crystal face and a 222 crystal face of the cubic phase vanadium nitride respectively. FIG. 4 is a field emission scanning electron micrograph showing that the particle size is 30-40 nm.
Example 3:
vanadium pentoxide monohydrate powder was prepared as described in example 1. Putting the monohydrate amorphous vanadium pentoxide powder into a quartz boat, putting the quartz boat into a tubular atmosphere furnace, introducing ammonia gas, heating the quartz boat to 700 ℃ at the flow rate of 1 liter/minute at the temperature of 10 ℃/minute for 3 hours, and naturally cooling the quartz boat to room temperature under flowing ammonia gas to obtain the nano vanadium nitride powder. FIG. 5 is an X-ray diffraction diagram of the nano vanadium nitride powder prepared in this example, which shows, in comparison with JCPDS card 35-0768: the powder is cubic phase vanadium nitride, which shows that the amorphous hydrated vanadium pentoxide powder can be nitrided in ammonia gas flow at 700 ℃ for 3 hours to obtain vanadium nitride powder with the purity of more than 95 percent, and five diffraction peaks in figure 5 are diffraction peaks of a 111 crystal face, a 200 crystal face, a 220 crystal face, a 311 crystal face and a 222 crystal face of the cubic phase vanadium nitride respectively. The field emission scanning electron microscope test shows that the particle size is 40-50 nm.
Example 4:
vanadium pentoxide monohydrate powder was prepared as described in example 1. Putting the prepared vanadium pentoxide monohydrate powder into a quartz boat, putting the quartz boat into a tubular atmosphere furnace, introducing ammonia gas, heating the quartz boat to 650 ℃, keeping the temperature for 3 hours at the temperature with the ammonia gas flow rate of 1 liter/minute and the heating rate of 10 ℃/minute, and naturally cooling the quartz boat to room temperature under flowing ammonia gas to obtain the nano vanadium nitride powder. X-ray diffraction studies showed that: the powder is cubic phase vanadium nitride. The vanadium pentoxide powder monohydrate is nitridized for 3 hours in ammonia gas flow at 650 ℃, and the vanadium nitride powder with the purity of more than 95 percent can be obtained. The field emission scanning electron microscope test shows that the particle size is 35-45 nm.
Example 5:
vanadium pentoxide monohydrate powder was prepared as described in example 1. Putting the prepared vanadium pentoxide monohydrate powder into a quartz boat, putting the quartz boat into a tubular atmosphere furnace, introducing ammonia gas, heating the quartz boat to 650 ℃, keeping the temperature for 5 hours at the temperature with the ammonia gas flow rate of 1 liter/minute and the heating rate of 10 ℃/minute, and naturally cooling the quartz boat to room temperature under flowing ammonia gas to obtain the nano vanadium nitride powder. X-ray diffraction studies showed that: the powder is cubic phase vanadium nitride. The vanadium pentoxide powder monohydrate is nitridized for 5 hours in ammonia gas flow at 650 ℃, and the vanadium nitride powder with the purity of more than 95 percent can be obtained. The field emission scanning electron microscope test shows that the particle size is 40-50 nm.
Claims (5)
1. A method for preparing cubic phase nano vanadium nitride powder is characterized by comprising the following steps: taking ammonium metavanadate as a starting material, firstly synthesizing vanadium pentoxide powder monohydrate, and then synthesizing cubic phase nano vanadium nitride powder in a tubular reaction furnace in a flowing ammonia atmosphere; the temperature of the nitridation reaction is controlled at 500-800 ℃, and the nitridation heat preservation time is 3-5 hours.
2. The method for preparing cubic phase nano vanadium nitride powder as claimed in claim 1, wherein the synthesis of the vanadium pentoxide monohydrate comprises dissolving ammonium metavanadate in hot distilled water under normal pressure, adjusting pH to 2.5-3with 30-60% nitric acid solution, adding 1-2M ammonia water solution dropwise into the ammonium metavanadate solution under stirring at a speed of 400-800 rpm to precipitate, washing, and drying.
3. The method for preparing vanadium pentoxide monohydrate powder according to claim 2, wherein: the precipitation temperature is 50-70 ℃, the pH value is 5-6, and the precipitation time is 1-12 hours.
4. The method for preparing vanadium pentoxide monohydrate powder according to claim 2, wherein the washing is carried out with an absolute ethyl alcohol solution for 2 to 5 times. The drying condition of the precipitate is 80 ℃ and 12 hours.
5. The method for preparing cubic phase nano vanadium nitride powder according to claim 1, wherein the flow rate of ammonia gas is 0.5 to 5 liters per minute during the nitriding reaction, and the temperature rise rate of the nitriding is 5 to 10 ℃/minute.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100436328C (en) * | 2004-02-17 | 2008-11-26 | 攀枝花钢铁(集团)公司 | Drying method of raw material blank in continuous production of vanadium nitride and its device |
| CN103626140A (en) * | 2013-12-12 | 2014-03-12 | 河南工业大学 | Method for synthesizing nanometer vanadium nitride/chromium nitride composite powder by carbon-thermal reduction and nitridation process |
| CN104505509A (en) * | 2014-12-09 | 2015-04-08 | 武汉科技大学 | Carbon-coated porous vanadium nitride nanowire film and preparation method thereof |
| CN104528667A (en) * | 2014-12-18 | 2015-04-22 | 长春理工大学 | Vanadium nitride (VN) porous nano-belt and preparation method thereof |
| CN105742633A (en) * | 2016-04-08 | 2016-07-06 | 武汉理工大学 | Porous oxygen-rich vanadium nitride nanosheet and preparation method and application therefor |
| CN106809808A (en) * | 2015-11-27 | 2017-06-09 | 中国科学院大连化学物理研究所 | A kind of preparation method of uniform hollow ball-shape VN nano particles |
| CN108569680A (en) * | 2018-04-23 | 2018-09-25 | 武汉科技大学 | A kind of vanadium nitride powder-body and preparation method thereof based on low temperature nitride |
| CN109437126A (en) * | 2018-10-29 | 2019-03-08 | 福州大学 | A kind of method and application of simple synthesis VN hollow sphere |
| CN109980205A (en) * | 2019-04-01 | 2019-07-05 | 北京航空航天大学 | A kind of vanadic anhydride/graphene composite material and its preparation method and application |
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2003
- 2003-02-21 CN CNB031154913A patent/CN1187261C/en not_active Expired - Fee Related
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100436328C (en) * | 2004-02-17 | 2008-11-26 | 攀枝花钢铁(集团)公司 | Drying method of raw material blank in continuous production of vanadium nitride and its device |
| CN103626140A (en) * | 2013-12-12 | 2014-03-12 | 河南工业大学 | Method for synthesizing nanometer vanadium nitride/chromium nitride composite powder by carbon-thermal reduction and nitridation process |
| CN103626140B (en) * | 2013-12-12 | 2015-06-10 | 河南工业大学 | Method for synthesizing nanometer vanadium nitride/chromium nitride composite powder by carbon-thermal reduction and nitridation process |
| CN104505509A (en) * | 2014-12-09 | 2015-04-08 | 武汉科技大学 | Carbon-coated porous vanadium nitride nanowire film and preparation method thereof |
| CN104505509B (en) * | 2014-12-09 | 2017-01-04 | 武汉科技大学 | A kind of carbon coated porous vanadium nitride nano wire film and preparation method thereof |
| CN104528667A (en) * | 2014-12-18 | 2015-04-22 | 长春理工大学 | Vanadium nitride (VN) porous nano-belt and preparation method thereof |
| CN106809808A (en) * | 2015-11-27 | 2017-06-09 | 中国科学院大连化学物理研究所 | A kind of preparation method of uniform hollow ball-shape VN nano particles |
| CN105742633A (en) * | 2016-04-08 | 2016-07-06 | 武汉理工大学 | Porous oxygen-rich vanadium nitride nanosheet and preparation method and application therefor |
| CN105742633B (en) * | 2016-04-08 | 2018-03-20 | 武汉理工大学 | Porous oxygen-enriched vanadium nitride nanometer sheet and its preparation method and application |
| CN108569680A (en) * | 2018-04-23 | 2018-09-25 | 武汉科技大学 | A kind of vanadium nitride powder-body and preparation method thereof based on low temperature nitride |
| CN109437126A (en) * | 2018-10-29 | 2019-03-08 | 福州大学 | A kind of method and application of simple synthesis VN hollow sphere |
| CN109980205A (en) * | 2019-04-01 | 2019-07-05 | 北京航空航天大学 | A kind of vanadic anhydride/graphene composite material and its preparation method and application |
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