CN102491289B - Method for preparing nanoscale magnesium nitride powder - Google Patents
Method for preparing nanoscale magnesium nitride powder Download PDFInfo
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- CN102491289B CN102491289B CN201110409990.0A CN201110409990A CN102491289B CN 102491289 B CN102491289 B CN 102491289B CN 201110409990 A CN201110409990 A CN 201110409990A CN 102491289 B CN102491289 B CN 102491289B
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Abstract
The invention discloses a method for preparing magnesium nitride powder. The method comprises the following steps of: adding nano magnesium powder into a quartz tube; and fully reacting the nano magnesium powder with high-purity nitrogen at the temperature of between 600 and 900 DEG C to prepare the nanoscale magnesium nitride powder. The preparation method is simple, the problem that magnesium is easily oxidized by air in the conventional preparation method is solved, and high-purity magnesium nitride powder is prepared.
Description
Technical field
The present invention relates to a kind of method of preparing magnesium nitride powder, particularly a kind of method of preparing nanoscale magnesium nitride powder.
Background technology
Magnesium nitride (Mg
3n
2) mineral compound that formed by nitrogen and magnesium.It is at room temperature yellowish green powder.Density is 2712kg/m
3, fusing point is 800 ℃, boiling point is 700 ℃, belongs to isometric system.
Magnesium nitride very easily reacts with water and generates magnesium hydroxide and emit ammonia, can absorb airborne water vapour rotten in air, therefore magnesium nitride generally adopts vacuum to preserve; Magnesium nitride almost all can react with all acid; Magnesium nitride Heat stability is good, in air 800 ℃ above just with the oxygen generation magnesium oxide that reacts.
Magnesium nitride is of wide application: in the solid state reaction of preparation high rigidity, high thermal conductance, wear-resisting, corrosion-resistant, resistant to elevated temperatures type material boron nitride, silicon nitride, magnesium nitride is indispensable sintering aid.In addition, magnesium nitride also can be used for reclaiming nuclear fuel, prepares special stupalith, manufactures the fields such as special glass; Magnesium nitride can effectively take off alum as additive, thereby improves density, intensity, pulling force and the holding capacity of steel.Meanwhile, it was still one of storage hydrogen series material by the M-N-H of extensive concern (M refers to I ，IV family and some magnesium-yttrium-transition metals) in recent years.In addition, generally believe that at present magnesium nitride powder is direct band-gap semicondictor material, bandwidth is 2.8eV left and right, so aspect photodiode and laser diode, magnesium nitride also has potential using value.And nano silicon nitride magnesium dust has larger potential using value because of features such as nano material specific surface area are large.
At present the main preparation methods of magnesium nitride have magnesium powder and nitrogen direct reaction method, magnesium in nitrogen plasma with nitrogen reaction method, nitrogen atmosphere under magnesium coil explosion method, self propagating high temperature synthesis method and Low Pressure Chemical Vapor Deposition.Although wherein direct the reaction with nitrogen of magnesium powder is to have the method that industrial production is worth, but the temperature of reaction that the need of production of magnesium nitride powder is higher (high temperature of 800 ℃ to 900 ℃) and longer reaction times, and the shape of particle is imperfect easily lumps and is difficult to reach comparatively desirable purity again, does not reach industrial quality requirement.Additive method because of or the shortcoming such as cost is high or technical process is long or operation of equipment is complicated or productivity ratio magnesium nitride is lower, and limited its industrialized production.
In recent years, how Chinese scholars is prepared aspect magnesium nitride powder and has been done a large amount of research.2004, the people such as G.Soto adopted the method for pulsed laser deposition, prepared the unformed magnesium nitride film of the different proportionings of Mg: N in the environment of dinitrogen on Si substrate.At home, the Zhang Yuan of Chinese Academy of Sciences Dalian Chemistry and Physics Institute chief waits people to utilize the synthetic MgH of catalysis method under mild conditions
2the activated carbon powder that thermolysis makes, the at a lower temperature magnesium nitride of synthesis of nano size.People's use magnesium powder such as the Ai Yujie of Shandong Normal University and ammonia direct reaction legal system are for the higher magnesium nitride powder of purity, but ammonia is very easily water-soluble, need experiment to keep good dry environment, and ammonia also has the nature of dangers such as corrodibility and toxicity, price is also higher than nitrogen, and these are all unfavorable for scale operation.
Summary of the invention
The object of the invention is to overcome above-mentioned the deficiencies in the prior art, a kind of preparation method of magnesium nitride powder is provided, and preparation technology of the present invention is simple, has overcome the problem of the easy oxidation by air of magnesium in existing preparation method, and make highly purified magnesium nitride powder, and gained magnesium nitride powder is nano level.
For achieving the above object, the present invention is by the following technical solutions:
A preparation method for nano level magnesium nitride powder, comprises the following steps:
Nanometer Mg powder is put into ceramic boat and pack silica tube into, after being put into tube furnace, silica tube first silica tube one end valve is tightened to sealing, then the other end be evacuated down to-0.1MPa that connects vacuum pump, pass into again purity and be 99.99% high pure nitrogen to 1atm, complete once " gas washing " process, gas washing need to carry out five times totally; After completing, gas washing connects respectively anti-gas-leak and dehumidification system at described silica tube two ends; Then the circulation status that keeps high pure nitrogen, and to keep air pressure in described silica tube be 1atm, heated Tube-furnace to 600～900 ℃, and after being incubated 2h described nanometer Mg powder fully being reacted with described high pure nitrogen, make tube furnace cool to room temperature in the described high pure nitrogen atmosphere flowing, prepared powder is described nano level magnesium nitride powder, takes out to be placed in glove box and preserves.
Dehumidification system of the present invention comprises a flask that silica gel is housed, and is equipped with described in preferably on the flask of silica gel with gas pressure reducer.
Air leakage prevention system of the present invention comprises the surge flask of a fluid-tight, in described surge flask, liquid oils is housed, and preferably described air leakage prevention system also comprises the flask of an anti-suck.
The flow direction of nitrogen of the present invention is followed successively by: described in the flask of silica gel, described silica tube, the flask of described anti-suck, the surge flask of described fluid-tight are housed.
Nanometer Mg powder of the present invention adopts DC arc plasma preparation, comprise following concrete steps: using pure MAG block as anode, tungsten bar is negative electrode, is placed in DC arc plasma equipment, when described DC arc plasma equipment is evacuated to vacuum tightness, is 5 * 10
-2during Pa, be filled with the argon gas of 0.7atm and the hydrogen of 0.1atm; The starting the arc after unlatching cooling water system, described system hydraulic pressure is 2Mpa, and adjusting electric current is 80-120A, and it is 0.8-1atm that the logical hydrogen of continuation keeps described equipment air pressure, reaction 10-20min, extinguish arcs, is cooled to room temperature; DC arc plasma equipment is evacuated to 0.01MPa, is then filled with argon gas 0.6-0.7atm and air 0.3-0.4atm carries out passivation operation; After passivation, collect inwall powder, be the nanometer Mg powder making;
Advantage of the present invention is:
1, the present invention connects respectively anti-gas-leak and dehumidification system by the two ends at silica tube, well avoided entering of in reaction process outside air, while entering to have air in silica tube, magnesium can generate magnesium oxide by preferential and airborne oxygen reaction, so that reaction products therefrom purity is very low, generate magnesium oxide even completely, and the present invention has well avoided this shortcoming, make magnesium can be completely, react the highly purified magnesium nitride of generation fully with nitrogen.
2. the magnesium nitride powder making is nano level, compares existing magnesium nitride reactive behavior high.
Accompanying drawing explanation
The XRD figure spectrum that Fig. 1 is the magnesium nitride powder that makes 750 ℃ of reactions.
The TEM figure that Fig. 2 is the magnesium nitride powder that makes 750 ℃ of reactions, image is obtained by JEOL-2100 transmission electron microscope.
The XRD figure spectrum that Fig. 3 is the magnesium nitride powder that makes 800 ℃ of reactions.
Embodiment
Embodiment 1
1. by the pure MAG block of any surface finish (long 60mm, wide 30mm, high 10mm left and right), as anode, tungsten bar is negative electrode, is placed in DC arc plasma equipment; When device is evacuated to vacuum tightness, be 5 * 10
-2during Pa, be filled with the argon gas of 0.7atm and the hydrogen of 0.1atm; Open the starting the arc after cooling water system (hydraulic pressure 2Mpa), regulate electric current to 120A, continuing logical hydrogen, to keep equipment air pressure be 0.8-1atm, reacts 10min, and extinguish arcs is closed cooling water system after being cooled to room temperature; DC arc plasma equipment is evacuated to 0.01Mpa; Then be first filled with 60KPa argon gas, then every half an hour, be filled with 5KPa air and be filled with altogether 40Kpa air, carry out the passivation of powder,, passivation time is 12 hours; Collect inwall powder, be the nanometer Mg powder making;
2. take the above-mentioned nanometer Mg powder of 2g, be evenly spread out in ceramic boat bottom; The ceramic boat that nanometer Mg powder is housed is put into silica tube, put into again tube furnace, first silica tube one end valve is tightened to sealing, then the other end be evacuated down to-0.1MPa that connects vacuum pump, nitrogengas cylinder in changing-over again, pass into purity and be 99.99% high pure nitrogen to 1atm, complete once " gas washing " process, gas washing need to carry out five times totally; After completing, gas washing connects respectively the flask that silica gel is housed with gas pressure reducer at silica tube two ends, and the surge flask of anti-suck flask and oil sealing, prevent suck-back and gas leakage, keeping air pressure in silica tube is 1atm, and keeps the circulation status of high pure nitrogen;
3. set diamond heating program, idiographic flow is: within one hour, be heated to 600 ℃, be then incubated half hour, reheat 750 ℃ and be incubated 2 hours; Finally in mobile high pure nitrogen, naturally cool to room temperature; Prepared powder is Mg
3n
2, take out to be placed in glove box and preserve.
By the Mg making
3n
2powder characterizes, and the XRD figure spectrum of accompanying drawing 1 can be found out Mg
3n
2purity very high; The TEM picture of accompanying drawing 2 can be found out the Mg making
3n
2the particle of powder is all in nanometer scale.
Embodiment 2:
1. by the pure MAG block of any surface finish (long 60mm, wide 30mm, high 10mm left and right), as anode, tungsten bar is negative electrode, is placed in DC arc plasma equipment; When device is evacuated to vacuum tightness and is 5 * 10-2Pa, be filled with the argon gas of 0.7atm and the hydrogen of 0.1atm; Open the rear starting the arc of cooling water system (hydraulic pressure 2Mpa), regulate electric current to 120A, continuing logical hydrogen and keeping equipment air pressure is 0.8-1atm reaction 20min, and extinguish arcs, is cooled to room temperature; DC arc plasma equipment is evacuated to 0.01MPa, is then filled with argon gas 0.7atm and air 0.3atm carries out passivation operation; After passivation, collect inwall powder, be the nanometer Mg powder making;
2. weigh the above-mentioned nanometer Mg powder of 2g, be evenly spread out in ceramic boat bottom; The ceramic boat that magnesium powder is housed is put into silica tube, put into again tube furnace, first silica tube one end valve is tightened to sealing, then the other end be evacuated down to-0.1MPa that connects vacuum pump, nitrogengas cylinder in changing-over again, pass into purity and be 99.99% high pure nitrogen to 1atm, complete once " gas washing " process, gas washing need to carry out five times totally; After completing, gas washing connects respectively the flask that silica gel is housed with gas pressure reducer at silica tube two ends, and the surge flask of anti-suck flask and oil sealing, to prevent suck-back and gas leakage, keeping air pressure in silica tube is 1atm, and keeps the circulation status of high pure nitrogen;
3. set diamond heating program, idiographic flow is: within one hour, be heated to 600 ℃, be then incubated half hour, reheat 800 ℃ and be incubated 2 hours; Finally in mobile high pure nitrogen, naturally cool to room temperature; Prepared powder is Mg
3n
2, take out to be placed in glove box and preserve.
By the Mg making
3n
2powder characterizes, and the XRD figure spectrum of accompanying drawing 3 can be seen Mg
3n
2purity very high.
Claims (1)
1. a preparation method for nano level magnesium nitride powder, comprises the following steps: using pure MAG block as anode, tungsten bar is negative electrode, is placed in DC arc plasma equipment, when described DC arc plasma equipment is evacuated to vacuum tightness, is 5 * 10
-2during Pa, be filled with the argon gas of 0.7atm and the hydrogen of 0.1atm, the starting the arc after unlatching cooling water system, described system hydraulic pressure is 2MPa, and adjusting electric current is 80-120A, and it is 0.8-1atm that the logical hydrogen of continuation keeps described equipment air pressure, reaction 10-20min, extinguish arcs, is cooled to room temperature, DC arc plasma equipment is evacuated to 0.01MPa, is then filled with argon gas 0.6-0.7atm and air 0.3-0.4atm carries out passivation operation, after passivation, collect inwall powder, be nanometer Mg powder, described nanometer Mg powder is put into ceramic boat and pack silica tube into, then after silica tube being put into tube furnace, seal, pass into purity and be 99.99% high pure nitrogen gas washing five times, silica tube two ends are connected respectively to anti-gas-leak and dehumidification system, then passing into mobile described high pure nitrogen to air pressure in described silica tube is 1atm, heated Tube-furnace is to 600-900 ℃, and after being incubated 2h described nanometer Mg powder fully being reacted with described high pure nitrogen, make tube furnace cool to room temperature in the described high pure nitrogen atmosphere flowing, prepared powder is described nano level magnesium nitride powder.
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| CN105692571A (en) * | 2014-11-28 | 2016-06-22 | 鞍钢股份有限公司 | Equipment for preparing magnesium nitride through laser radiation and a method therefor |
| CN105271138A (en) * | 2015-10-16 | 2016-01-27 | 甘肃稀土新材料股份有限公司 | Preparation method of alkaline earth metal nitride |
| CN105845895A (en) * | 2016-05-09 | 2016-08-10 | 上海交通大学 | Preparation method for negative electrode material of lithium ion battery |
| CN106995208A (en) * | 2017-05-11 | 2017-08-01 | 吉林大学 | A kind of preparation method of amorphous vanadium nitride nano particle |
| CN108817379A (en) * | 2018-05-23 | 2018-11-16 | 航天材料及工艺研究所 | A kind of powder metallurgy superalloy properties of product stability of improving fills out powder device |
| CN110329998B (en) * | 2019-07-23 | 2021-02-02 | 英特美光电（苏州）有限公司 | Method for preparing strontium nitride powder in high-pressure nitriding furnace |
| CN110817813B (en) * | 2019-12-19 | 2022-11-04 | 湖南众鑫新材料科技股份有限公司 | Preparation method of nanocrystalline vanadium nitride powder |
| CN112872348B (en) * | 2020-12-31 | 2021-11-30 | 广东省科学院稀有金属研究所 | Method for improving nitriding efficiency of rare earth-iron alloy |
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| CN1109022A (en) * | 1994-03-21 | 1995-09-27 | 中国科学院大连化学物理研究所 | Synthesis of nm-sized magnesium nitride |
| CN101269978A (en) * | 2007-03-21 | 2008-09-24 | 中国科学院理化技术研究所 | Method for synthesizing ultra-fine azotized magnesium powder with combustion |
| CN102241393A (en) * | 2010-09-28 | 2011-11-16 | 南昌大学 | Process for preparing magnesium nitride through airflow method |
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| CN100554142C (en) * | 2006-08-04 | 2009-10-28 | 北京大学 | Magnesium hydride nano particle and its production and application |
| US20080131350A1 (en) * | 2006-08-31 | 2008-06-05 | Burkes Douglas E | Method for Production of Metal Nitride and Oxide Powders Using an Auto-Ignition Combustion Synthesis Reaction |
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| CN1109022A (en) * | 1994-03-21 | 1995-09-27 | 中国科学院大连化学物理研究所 | Synthesis of nm-sized magnesium nitride |
| CN101269978A (en) * | 2007-03-21 | 2008-09-24 | 中国科学院理化技术研究所 | Method for synthesizing ultra-fine azotized magnesium powder with combustion |
| CN102241393A (en) * | 2010-09-28 | 2011-11-16 | 南昌大学 | Process for preparing magnesium nitride through airflow method |
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