CN102491289A - Method for preparing nanoscale magnesium nitride powder - Google Patents
Method for preparing nanoscale magnesium nitride powder Download PDFInfo
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- CN102491289A CN102491289A CN2011104099900A CN201110409990A CN102491289A CN 102491289 A CN102491289 A CN 102491289A CN 2011104099900 A CN2011104099900 A CN 2011104099900A CN 201110409990 A CN201110409990 A CN 201110409990A CN 102491289 A CN102491289 A CN 102491289A
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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 for preparing the magnesium nitride powder, particularly a kind of method for preparing nano level magnesium nitride powder.
Background technology
Magnesium nitride (Mg
3N
2) mineral compound formed by nitrogen and magnesium.It at room temperature is yellowish green powder.Density is 2712kg/m
3, fusing point is 800 ℃, boiling point is 700 ℃, belongs to isometric system.
Magnesium nitride very easily generates Marinco H and emits ammonia with the water reaction, and it is rotten in air, can to absorb airborne water vapour, so magnesium nitride generally adopts vacuum to preserve; Magnesium nitride almost all can react with all acid; The magnesium nitride Heat stability is good, in air more than 800 ℃ just with the oxygen generation Natural manganese dioxide that reacts.
Magnesium nitride is of wide application: in the solid state reaction of preparation high firmness, high thermal conductance, wear-resisting, corrosion-resistant, resistant to elevated temperatures type material SP 1, silicon nitride, magnesium nitride is indispensable sintering aid.In addition, magnesium nitride also can be used for reclaiming nuclear fuel, prepares special stupalith, makes 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.Simultaneously, it was one of storage hydrogen series material by the M-N-H of extensive concern (M is meant I, IV family and some magnesium-yttrium-transition metals) in recent years still.In addition, generally believe that at present the magnesium nitride powder is the direct band-gap semicondictor material, bandwidth is about 2.8eV, so aspect photodiode and laser diode, magnesium nitride also has potential using value.And the nano silicon nitride magnesium dust has bigger potential using value because of characteristics such as the nano material specific surface area are big.
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.Though wherein the magnesium powder is the method with industrial production value with the nitrogen reaction directly; But the production of magnesium nitride powder needs higher temperature of reaction (800 ℃ to 900 ℃ high temperature) and long reaction times; And imperfect the caking easily again of coating of particles is difficult to reach comparatively ideal purity, do not reach the industrial quality requirement.Additive method because of or shortcoming such as cost is high or technical process is long or operation of equipment productivity ratio complicated or magnesium nitride is lower, and limited its industrialized production.
In recent years, how Chinese scholars prepares and has done a large amount of research aspect the magnesium nitride powder.2004, people such as G.Soto adopted the method for pulsed laser deposition, in the environment of dinitrogen, on the Si substrate, prepared the unformed magnesium nitride film of the different proportionings of Mg: N.At home, the people such as Zhang Yuan chief of the Chinese Academy of Sciences Dalian Chemistry and Physics Institute utilize catalysis method synthetic MgH under the mild conditions
2The activated carbon powder that thermolysis makes, the magnesium nitride of synthesis of nano size at a lower temperature.Human magnesium powder such as the Ai Yujie of Shandong Normal University and ammonia direct reaction method have prepared 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 nature of dangers such as corrodibility and toxicity, and price also is higher than nitrogen, and these all are unfavorable for scale operation.
Summary of the invention
The objective of the invention is to overcome the deficiency of above-mentioned 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 among the existing preparation method; And make highly purified magnesium nitride powder, and gained magnesium nitride powder is a nano level.
For realizing above-mentioned purpose, the present invention adopts following technical scheme:
A kind of preparation method of nano level magnesium nitride powder may further comprise the steps:
Nanometer Mg powder is put into the ceramic boat silica tube of packing into; Silica tube put into behind the tube furnace earlier silica tube one end valve door is tightened sealing; The other end connects vacuum pump and is evacuated down to-0.1MPa then; Feed purity again and be 99.99% high pure nitrogen to 1atm, accomplish once " gas washing " process, gas washing need carry out five times totally; Gas washing connects anti-gas-leak and dehumidification system respectively at said silica tube two ends after accomplishing; The circulation status that keeps high pure nitrogen then; And keep that air pressure is 1atm in the said silica tube; Heating tube furnace to 600～900 ℃, and after insulation 2h fully reacts said nanometer Mg powder and said high pure nitrogen, make tube furnace cool to room temperature in the said high pure nitrogen atmosphere of mobile; Prepared powder is said nano level magnesium nitride powder, takes out to be placed in the glove box and preserves.
Dehumidification system according to the invention comprises a flask that silica gel is housed, and has gas pressure reducer on the preferable said flask that silica gel is housed.
Anti-gas-leak according to the invention system comprises the surge flask of a fluid-tight, in the said surge flask liquid oil is housed, and preferable said anti-gas-leak system also comprises the flask of an anti-suck.
The flow direction of nitrogen according to the invention is followed successively by: the said flask of the flask of silica gel, said silica tube, said anti-suck, the surge flask of said fluid-tight of being equipped with.
Nanometer Mg powder according to the invention adopts the preparation of DC arc plasma method; Comprise following concrete steps: with pure MAG block as anode; Tungsten bar is a negative electrode, places DC arc plasma equipment, is 5 * 10 when said DC arc plasma equipment is evacuated to vacuum tightness
-2During Pa, charge into the argon gas of 0.7atm and the hydrogen of 0.1atm; The starting the arc behind the unlatching cooling water system, said system hydraulic pressure is 2Mpa, and the adjusting electric current is 80-120A, and it is 0.8-1atm that the logical hydrogen of continuation keeps said equipment air pressure, reaction 10-20min, extinguish arcs is cooled to room temperature; DC arc plasma equipment is evacuated to 0.01MPa, charges into argon gas 0.6-0.7atm then and air 0.3-0.4atm carries out passivation operation; After the passivation, collect the inwall powder, be the nanometer Mg powder that makes;
Advantage of the present invention is:
1, the present invention connects anti-gas-leak and dehumidification system respectively through the two ends at silica tube; Well avoided the entering of outside air in reaction process, when advancing air is arranged in the silica tube, magnesium can generate Natural manganese dioxide by preferential and airborne oxygen reaction; So that reaction products therefrom purity is very low; Even generate Natural manganese dioxide fully, and the present invention has well avoided this shortcoming, make magnesium can be fully, fully with the highly purified magnesium nitride of nitrogen reaction generation.
2. the magnesium nitride powder that makes is nano level, and it is high to compare existing magnesium nitride reactive behavior.
Description of drawings
Fig. 1 is the XRD figure spectrum of the magnesium nitride powder that makes 750 ℃ of reactions.
Fig. 2 is the TEM figure of the magnesium nitride powder that makes 750 ℃ of reactions, and image is obtained by the JEOL-2100 transmission electron microscope.
Fig. 3 is the XRD figure spectrum of the magnesium nitride powder that makes 800 ℃ of reactions.
Embodiment
Embodiment 1
1. as anode, tungsten bar is a negative electrode, places DC arc plasma equipment with the pure MAG block (long 60mm, wide 30mm is about high 10mm) of any surface finish; When device is evacuated to vacuum tightness is 5 * 10
-2During Pa, charge into the argon gas of 0.7atm and the hydrogen of 0.1atm; Open cooling water system (hydraulic pressure 2Mpa) the back starting the arc, 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; Charge into the 60KPa argon gas then earlier, charge into the 5KPa air and charge into the 40Kpa air altogether every then separated half a hour, carries out the passivation of powder,, passivation time is 12 hours; Collect the inwall powder, be the nanometer Mg powder that makes;
2. take by weighing the above-mentioned nanometer Mg powder of 2g, evenly be spread out in the ceramic boat bottom; The ceramic boat that nanometer Mg powder is housed is put into silica tube; Put into tube furnace again, earlier silica tube one end valve door is tightened sealing, the other end connects vacuum pump and is evacuated down to-0.1MPa then; Nitrogengas cylinder in the changing-over again; Feed purity and be 99.99% high pure nitrogen to 1atm, completion is " gas washing " process once, and gas washing need carry out five times totally; Gas washing is accomplished the back and is connected the flask that silica gel is housed that has gas pressure reducer at the silica tube two ends respectively, and anti-suck flask and squalid surge flask, prevents suck-back and gas leakage, and air pressure is 1atm in the maintenance silica tube, and the circulation status of maintenance high pure nitrogen;
3. set the tube furnace heating schedule, idiographic flow is: be heated to 600 ℃ in one hour, and be incubated half hour then, reheat to 750 ℃ also is incubated 2 hours; In the mobile high pure nitrogen, naturally cool to room temperature at last; Prepared powder is Mg
3N
2, take out to be placed in the glove box and preserve.
With the Mg that makes
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 that makes
3N
2Particles of powder is all in nanometer scale.
Embodiment 2:
1. as anode, tungsten bar is a negative electrode, places DC arc plasma equipment with the pure MAG block (long 60mm, wide 30mm is about high 10mm) of any surface finish; When device is evacuated to vacuum tightness and is 5 * 10-2Pa, charge into the argon gas of 0.7atm and the hydrogen of 0.1atm; Open cooling water system (hydraulic pressure 2Mpa) the back starting the arc, 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, charges into argon gas 0.7atm then and air 0.3atm carries out passivation operation; After the passivation, collect the inwall powder, be the nanometer Mg powder that makes;
2. the above-mentioned nanometer Mg powder of weighing 2g evenly is spread out in the ceramic boat bottom; The ceramic boat that the magnesium powder is housed is put into silica tube; Put into tube furnace again, earlier silica tube one end valve door is tightened sealing, the other end connects vacuum pump and is evacuated down to-0.1MPa then; Nitrogengas cylinder in the changing-over again; Feed purity and be 99.99% high pure nitrogen to 1atm, completion is " gas washing " process once, and gas washing need carry out five times totally; Gas washing is accomplished the back and is connected the flask that silica gel is housed that has gas pressure reducer at the silica tube two ends respectively, and anti-suck flask and squalid surge flask, and to prevent suck-back and gas leakage, air pressure is 1atm in the maintenance silica tube, and the circulation status of maintenance high pure nitrogen;
3. set the tube furnace heating schedule, idiographic flow is: be heated to 600 ℃ in one hour, and be incubated half hour then, reheat to 800 ℃ also is incubated 2 hours; In the mobile high pure nitrogen, naturally cool to room temperature at last; Prepared powder is Mg
3N
2, take out to be placed in the glove box and preserve.
With the Mg that makes
3N
2Powder characterizes, and the XRD figure spectrum of accompanying drawing 3 can be seen Mg
3N
2Purity very high.
Claims (10)
1. the preparation method of a nano level magnesium nitride powder may further comprise the steps:
Nanometer Mg powder is put into the ceramic boat silica tube of packing into; Seal after then silica tube being put into tube furnace; Feed purity and be 99.99% high pure nitrogen gas washing five times, the silica tube two ends are connected anti-gas-leak and dehumidification system respectively, feed then that air pressure is 1atm in the said high pure nitrogen of mobile to the said silica tube; Heating tube furnace to 600～900 ℃; And insulation makes tube furnace cool to room temperature in the said high pure nitrogen atmosphere of mobile after 2h fully reacts said nanometer Mg powder and said high pure nitrogen, and prepared powder is said nano level magnesium nitride powder.
2. preparation method according to claim 1 is characterized in that: said dehumidification system comprises a flask that silica gel is housed.
3. preparation method according to claim 2 is characterized in that: have gas pressure reducer on the said flask that silica gel is housed.
4. according to any described preparation method of claim 1～3, it is characterized in that: said anti-gas-leak system comprises the surge flask of a fluid-tight.
5. preparation method according to claim 4 is characterized in that: in the said surge flask liquid oil is housed.
6. preparation method according to claim 4 is characterized in that: said anti-gas-leak system also comprises the flask of an anti-suck.
7. preparation method according to claim 1; It is characterized in that; The concrete operations step of said gas washing is: earlier silica tube one end valve door is tightened sealing; The other end connects vacuum pump and is evacuated down to-0.1MPa then, feeds purity again and be 99.99% high pure nitrogen to 1atm, accomplishes once " gas washing " process.
8. preparation method according to claim 1 is characterized in that: the flow direction of said nitrogen is followed successively by said dehumidification system, said silica tube, said anti-gas-leak system.
9. preparation method according to claim 1 is characterized in that: said tube furnace type of heating is for being heated to 600 ℃ and be incubated half a hour earlier, and then continues heating.
10. preparation method according to claim 1; It is characterized in that the preparation method of said nanometer Mg powder is: as anode, tungsten bar is a negative electrode with pure MAG block; Placing DC arc plasma equipment, is 5 * 10 when said DC arc plasma equipment is evacuated to vacuum tightness
-2During Pa, charge into the argon gas of 0.7atm and the hydrogen of 0.1atm; The starting the arc behind the unlatching cooling water system, said system hydraulic pressure is 2Mpa, and the adjusting electric current is 80-120A, and it is 0.8-1atm that the logical hydrogen of continuation keeps said equipment air pressure, reaction 10-20min, extinguish arcs is cooled to room temperature; DC arc plasma equipment is evacuated to 0.01MPa, charges into argon gas 0.6-0.7atm then and air 0.3-0.4atm carries out passivation operation; After the passivation, collect the inwall powder, be the nanometer Mg powder that makes.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| 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 |
| CN110329998A (en) * | 2019-07-23 | 2019-10-15 | 英特美光电（苏州）有限公司 | A method of preparing strontium nitride powder in high pressure nitriding furnace |
| CN110817813A (en) * | 2019-12-19 | 2020-02-21 | 湖南众鑫新材料科技股份有限公司 | Preparation method of nanocrystalline vanadium nitride powder |
| CN112872348A (en) * | 2020-12-31 | 2021-06-01 | 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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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| CN110329998A (en) * | 2019-07-23 | 2019-10-15 | 英特美光电（苏州）有限公司 | A method of preparing strontium nitride powder in high pressure nitriding furnace |
| CN110817813A (en) * | 2019-12-19 | 2020-02-21 | 湖南众鑫新材料科技股份有限公司 | Preparation method of nanocrystalline vanadium nitride powder |
| 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 |
| CN112872348A (en) * | 2020-12-31 | 2021-06-01 | 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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