CN106927436A - A kind of preparation method of chromium nitride nano powder - Google Patents
A kind of preparation method of chromium nitride nano powder Download PDFInfo
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- CN106927436A CN106927436A CN201511010963.0A CN201511010963A CN106927436A CN 106927436 A CN106927436 A CN 106927436A CN 201511010963 A CN201511010963 A CN 201511010963A CN 106927436 A CN106927436 A CN 106927436A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/0615—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with transition metals other than titanium, zirconium or hafnium
- C01B21/062—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with transition metals other than titanium, zirconium or hafnium with chromium, molybdenum or tungsten
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- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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Abstract
A kind of preparation method of chromium nitride nano powder of the present invention, the method using catalytic behavior of materials high temperature and plasma etching effect, realize that chemical gaseous phase synthesis obtains chromium nitride superfines.The method is the collection of chromium nitride nano powder, the packaging and other steps realization for integrally being vacuumized by equipment, producing high-temperature plasma, regulation ammonia flow, solid nano powder to condense, solidify, the inventive method can obtain the nanoscale chromium nitride nano powder of average grain diameter 40nm or so, its narrower particle size distribution, powder has the advantages that simple processing step, burn rate, reaction temperature, course of reaction be easy to control, no pollutant is produced for spherical.
Description
Technical field
The present invention relates to nano powder manufacture field, more particularly to a kind of preparation method of chromium nitride nano powder, the party
Method using catalytic behavior of materials high temperature and plasma etching effect, realize chemical gaseous phase synthesis obtain chromium nitride it is ultra-fine
Powder.
Background technology
Nano-powder has the physical and chemical performance different from common material, shows in machinery, electromagnetism, light, heat, chemical field
Its property is shown, is the important component of current new material.
Chromium nitride（CrN）With good physical and mechanical properties, its hardness is high, acid-alkali-corrosive-resisting is good, chemically stable
Property the good, high-melting-point of high, wearability etc., meanwhile, uniquely there are antiferromagnetic materials in chromium nitride or nitride.Make it in magnetic
The aspects such as, electronics industry, high-temperature-resistant structure ceramics are used widely, and used as a kind of new material, chromium nitride has wide
Application prospect.
At present, ultra-fine chromium nitride produces that there are as below methods：
1st, high-energy ball milling method：By chromium powder 180 ~ 300h of high-energy ball milling under nitrogen atmosphere, the CrN of 100 nanometers of average grain diameter can be obtained
Powder, but have that equipment is complicated, the deficiency that long, product of producing the time is easily polluted by ball-milling medium.
2nd, the hot method of benzene：By appropriate CrCl3And Li3N is placed in stainless steel cauldron, adds benzene as solvent, is then heated
350~420 DEG C of insulation 6h of reactor, naturally cool to room temperature.The LiCl and excess Li in product are washed away with absolute ethyl alcohol3After N,
Product is vacuum dried 2h under the conditions of 80 DEG C, the CrN powders of 25 rans can be obtained.
3rd, self-propagating high-temperature method：2 microns of pine dress chromium powder of average grain diameter is loaded into graphite crucible, the closed appearance of stainless steel is placed in
In device, nitrogen is passed through after vacuumizing and certain pressure is kept, then by current heating resistor silk and the chromium powder that ignites, by resistance wire
What is heated is a bit of chromium powder, can continue to spread under the support of self-heat generation once being chemically reacted after burning, until entirely earthenware
Crucible, the product of acquisition is Cr2N and CrN, the method technique, equipment are simple, but there is also that manufactured goods particle is excessive, need two
It is secondary broken, and the uppity deficiency of burn rate, reaction temperature, course of reaction.
4th, ammonolysis process：With ammonia（NH3）It is catalyst, ammonia and reactant direct reaction are generating nitride at high temperature
Method.In recent years, ammonolysis process has been widely used in the preparation of nitride powder, successfully prepared CrN, TiN,
Various nitride such as NbN.Such as will be equipped with Cr2S3Quartz ampoule be placed on Muffle furnace, be passed through flowing and ammonia and be heated to 800 DEG C and protect
Warm 48 hours, then natural cooling can obtain CrN powders, and its accessory substance is H2S, it has the disadvantage that the reaction time is long, finished particle
Greatly, H2S causes environmental pollution.Also ammonolysis CrCl3, ammonolysis Cr2O3, ammonolysis urea chromic salts etc., be required for reaction temperature higher
Reaction time more long, and produced with pollutant.
The content of the invention
The invention aims to provide a kind of method that use catalytic behavior of materials produces chromium nitride nano powder, can
To obtain the nanoscale chromium nitride nano powder of average grain diameter 40nm or so, its narrower particle size distribution, powder is spherical, with work
Skill step is simple, burn rate, reaction temperature, the advantages of course of reaction is easy to control, no pollutant is produced.
The object of the present invention is achieved like this, and the method is comprised the following steps：1st, a kind of preparation method of chromium nitride nano powder,
It is characterized in that：The method is comprised the following steps：
1., start vacuum pump set first integrally to vacuumize " High-frequency plasma multifunctional powder production equipment ", make equipment
Vacuum reaches 6.0 × 10-2Pa, is then injected into high-purity argon gas, and equipment makes energy storage tank gas pressure reach 0.6MPa before starting, if
Standby internal pressure reaches 0MPa；
2., starting device, it is ion-gas and interior cooling gas to use argon gas, and plasma is formed in high-frequency and high-voltage electric excitation down-firing
Body, adjustment gas flow makes ion-gas flow reach 40~60L/min, interior more than the L/min of cooling gas flow 140, adjustment sun
Stabilization, the plasma flame stream of rule are formed in 7~8.5KV of pole tension, 5.5~8A of anode current, light fixture 20, is flowed from top to bottom
Enter main frame tank；
3. ammonia flow, is adjusted by flowmeter, adjustment powder feeder conveys the powder sending quantity of chromium powder, two are determined according to reaction equation
Person's molal weight ratio, the ratio of ammonia can be bigger, and the raw material chromium powder conveyed by ammonia enters plasma flame flow through powder feeding rifle, passes through
Visor observes plasma flame flow wake flame, should then reduce powder sending quantity if any the shinny particle of Meteor-shape or increase plant capacity, should be first
Consider that selection reduces powder sending quantity；
4., argon plasma temperature about 10000K, 2672 DEG C of 1857 DEG C of the fusing point of chromium, boiling point, controls technological parameter, flows through
The raw material chromium powder of ion flame stream will all be gasificated into metallic vapour and possess great work under the corrasion of plasma
Property, ammonia is Nitrogen ion and hydrogen ion through plasma high-temperature heat resolve, and the chromium metallic vapour and Nitrogen ion for possessing activity exist
There is combination reaction in plasma flame flow, generate chromium nitride and driven into main frame tank by plasma flame flow, supplied through quenching gas circuit
The argon gas given is cooled down, and chromium nitride steam condensation is solid nano powder；To reduce production cost, quenching air-flow can also use nitrogen
Gas；
5., the chromium nitride nano powder and argon gas, undecomposed ammonia and hydrogen of solidification are mixed in aerosol form disperse
In main frame tank interior, collection device is entered under mixed gas drive, powder is filtered by filter core forced quarantine, filter core Yin Neibiao
Flour body is piled up and will excessively influence filter efficiency, can reach setting value by the pressure differential of differential pressure pickup detection filter core both sides
Start blowback magnetic valve, the powder that filter core inner surface is piled up is removed in the blowback air back flush provided by blowback gas circuit, also may be used
After differential pressure pickup sends alarm, to take artificial impact method vibration filter core, make the powder that its inner surface is piled up because of vibration
Drop, blowback air can be argon gas or nitrogen, and whether using gas back-flushing or using impact mode of vibration, its purpose is all
It is the bottom for making the powder for being deposited in filter core inner surface drop to collection device, the vacuum packet of finished product powder is realized by packing case
Dress.
A kind of High-frequency plasma multifunctional powder production equipment includes gas flow switch board, energy storage tank, ammonia bottle, stream
Gauge, powder feeding air pipe, ion-gas gas circuit, interior cooling gas circuit, quenching gas circuit, outer cold air, powder feeder, powder feeding rifle, blowback gas circuit,
Collection device, filter core, exhaust gas processing device, packing case, argon bottle, main frame tank, visor, light fixture and induction coil.
The present invention is synthesized by chemical gaseous phase and is obtained using the corrasion of the high temperature and plasma of catalytic behavior of materials
Chromium nitride nano powder is obtained, device therefor is High-frequency plasma multifunctional powder production equipment, and raw materials used is 10 microns
Hafnium metal powfer and ammonia（NH3）, its chemical equation is：
Argon gas can produce temperature up to the argon plasma of 10000K, this etc. under the excitation of induction coil in quartzy light fixture
Gas ions are produced by electromagnetic induction, do not have electrode fouling, are a kind of pure plasma heat sources.
Plasma is sent into chromium powder end through powder feeding rifle by powder feeder, chromium powder can moment gas when plasma flame stream is flowed through
Turn to nano-liquid droplet and active through plasma etching.
Together enter plasma using ammonia as the powder feeding carrier gas at conveying chromium powder end, ammonia and chromium powder end, in plasma
Under body high temperature action, ammonia molecule is decomposed into Nitrogen ion, hydrogen ion, and wherein Nitrogen ion chemically reacts with chromium nano-liquid droplet,
Generation chromium nitride, chromium nitride nanometer powder is solidified as through quenching gas cooling.
The chromium nitride nanometer powder disperse of solidification in argon gas, hydrogen ion, remaining Nitrogen ion and ammonia, in a kind of aerosol
State enters powder collection device after entering machine hall through pipeline liquid injecting device, by porous filter core forced collection, filters out nano-powder,
Tail gas includes that a small amount of ammonia of argon gas, hydrogen, residue, nitrogen are outer after can processing and arranges that such as reaction controlling must get well, and efflux gas only have
Argon gas and hydrogen, hydrogen can be consumed by ignition way.
The present invention has the advantages that：
1st, argon plasma flame stream temperature of the present invention reaches as high as 10000K, and wake flame temperature, can be according to required reaction up to 3000K
Temperature selects suitable powder feeding position.
2nd, of the invention because the generation of catalytic behavior of materials is independent of electrode, argon gas is inert gas, will not and be made
For the chromium of raw material, ammonia and Nitrogen ion, hydrogen ion chemically react, it is ensured that the purity of product.
3rd, the present invention control raw material diameter of particle and equipment power output, can be readily available Unusually narrow particle size distribution
Spherical super fine powder finished product.
4th, production process of the present invention is continuous, it is easy to accomplish automatic industrial is produced.
Brief description of the drawings
Fig. 1 is present device structural representation.
Fig. 2 is technological process of production schematic diagram of the present invention.
Specific embodiment
As shown in figure 1, a kind of High-frequency plasma multifunctional powder production equipment, including gas flow switch board 1, accumulation of energy
Tank 2, ammonia bottle 3, flowmeter 4, powder feeding air pipe 5, ion-gas gas circuit 6, interior cooling gas circuit 7, quenching gas circuit 8, outer cold air 9, send
Powder device 10, powder feeding rifle 11, blowback gas circuit 12, collection device 13, filter core 14, exhaust gas processing device 15, packing case 16, argon bottle
17th, main frame tank 18, visor 19, light fixture 20 and induction coil 21.
The gas flow switch board 1 is for detecting, gas flow needed for each road of control device, and energy storage tank 2 is placed in gas
Inside flow switch board 1, the one end of the energy storage tank 2 is connected with argon bottle 17, other end gas outlet respectively with ion-gas gas circuit 6,
Interior cooling gas circuit 7, quenching gas circuit 8 and blowback gas circuit 12 are connected, wherein the ion-gas gas circuit 6 and interior cooling gas circuit 7 and light fixture
20 connections, quenching gas circuit 8 is connected with the top of main frame tank 18, and the outer cooling gas circuit 9 connects through pressure with other air compressor
Contracting air is cooled down to light fixture, and the ammonia bottle is connected through flowmeter 4 and powder feeding air pipe 5 with powder feeder 10.
The induction coil 21 is sleeved on outside light fixture 20, in the electromagnetic field of high frequency of induction coil 21 and moment external high-frequency high pressure
Under electric joint incentive, high-temperature plasma is produced in light fixture 20, external high-frequency high-tension electricity, light fixture are removed after plasma ignition
There is no electrode in 20.The powder feeding rifle 11 is located at the inside of light fixture 20 simultaneously coaxially, and powder feeder 10 is connected with powder feeding rifle 11.
The light fixture 20 is placed in the top of main frame tank 18, and the side of main frame tank 18 is provided with visor 19.
The powder collection device 13 is connected by pipeline with main frame tank 18, the top of powder collection device 13 and blowback
Gas circuit 12 is connected, and it is internally provided with filter core 14, and the filter core 14 is rigid hollow cylinder, can use ceramic material, powder
Metallurgical material or fibrous material make.
The exhaust gas processing device 15 is connected by pipeline with powder collection device 13.
The bottom of main frame tank 18, the bottom of powder collection device 13 are all connected with packing case 16, true to powder for realizing
Empty package.
As shown in Figure 2：A kind of preparation method of chromium nitride nano powder, comprises the following steps：
1. start vacuum pump set first integrally to vacuumize " High-frequency plasma multifunctional powder production equipment ", make the true of equipment
Reciprocal of duty cycle reaches 6.0 × 10-2Pa, is then injected into high-purity argon gas, and equipment makes the gas pressure of energy storage tank 2 reach 0.6MPa before starting（Table
Pressure）, device interior pressure reaches 0MPa（Gauge pressure）；
2. it is ion-gas and interior cooling gas to use argon gas, and starting device, induction coil produces electromagnetic field of high frequency in light fixture,
Moment high-frequency and high-voltage electric excitation down-firing forms plasma, removes high-frequency high-voltage, and adjustment gas flow makes ion-gas flow
Reach 40~60L/min, interior more than the L/min of cooling gas flow 140,7~8.5KV of adjustment anode voltage, anode current 5.5
Stabilization, the plasma flame stream of rule are formed in~8A, light fixture 20, main frame tank 18 is flowed into from top to bottom；
3. ammonia flow is adjusted by flowmeter 4, adjustment powder feeder 10 conveys the powder sending quantity of chromium powder, determines according to reaction equation
The two molal weight ratio, the ratio of ammonia can be bigger, and the raw material chromium powder conveyed by ammonia enters plasma flame flow through powder feeding rifle 11,
Plasma flame flow wake flame is observed by visor 19, powder sending quantity should be then reduced if any the shinny particle of Meteor-shape or be increased plant capacity,
Should first consider that selection reduces powder sending quantity；
4. argon plasma temperature about 10000K, 2672 DEG C of 1857 DEG C of the fusing point of chromium, boiling point, control technological parameter, flow through
The raw material chromium powder of ion flame stream will all be gasificated into metallic vapour and possess great work under the corrasion of plasma
Property, ammonia is Nitrogen ion and hydrogen ion through plasma high-temperature heat resolve, and the chromium metallic vapour and Nitrogen ion for possessing activity exist
There is combination reaction in plasma flame flow, generate chromium nitride and driven into main frame tank by plasma flame flow, supplied through quenching gas circuit 8
The argon gas given is cooled down, and chromium nitride steam condensation is solid nano powder；To reduce production cost, quenching air-flow can also use nitrogen
Gas；
5. the chromium nitride nano powder for solidifying is mixed with argon gas, undecomposed ammonia and hydrogen and existed in aerosol form disperse
Main frame tank interior, enters collection device 13 under mixed gas drive, and powder is filtered by the forced quarantine of filter core 14, and filter core is because of table
Flour body is piled up and will excessively influence filter efficiency, can reach setting value by the pressure differential of differential pressure pickup detection filter core both sides
Start blowback magnetic valve, the powder that cartridge surface is piled up is removed by the back flush of blowback gas circuit 11, it is also possible in pressure difference sensing
After device sends alarm, artificial impact method vibration filter core is taken, make the powder of its surface sediment because vibration is dropped, blowback air can be with
It is argon gas or nitrogen, whether using gas back-flushing or using impact mode of vibration, its purpose is all to make to be deposited in filter core
Powder drop to the bottom of collection device 13, the vacuum packaging of finished product powder is realized by packing case 16.
It should be noted that such as controlling bad technological parameter, the product of acquisition is probably the nanometer powder mixture of CrN+Cr,
Process above can be repeated, the mixture to CrN+Cr carries out after-treatment.
Claims (2)
1. a kind of preparation method of chromium nitride nano powder, it is characterised in that：The method is comprised the following steps：
1., start vacuum pump set first integrally to vacuumize " High-frequency plasma multifunctional powder production equipment ", make equipment
Vacuum reaches 6.0 × 10-2Pa, is then injected into high-purity argon gas, and equipment makes energy storage tank gas pressure reach 0.6MPa before starting, if
Standby internal pressure reaches 0MPa；
2. it is ion-gas and interior cooling gas, starting device, to use argon gas, makes induction coil that the higher-order of oscillation to occur, in the line of induction
Under the electromagnetic field of high frequency and moment external high-frequency high-tension electricity joint incentive of circle 21, high-temperature plasma is produced in light fixture 20, etc.
Gas ions remove external high-frequency high-tension electricity after lighting, adjustment gas flow makes ion-gas flow reach 40~60L/min, interior cooling
More than the L/min of gas flow 140,7~8.5KV of adjustment anode voltage, 5.5~8A of anode current, the interior formation stabilization of light fixture 20,
The plasma flame stream of rule, flows into main frame tank from top to bottom；
3. ammonia flow, is adjusted by flowmeter, adjustment powder feeder conveys the powder sending quantity of chromium powder, two are determined according to reaction equation
Person's molal weight ratio, the ratio of ammonia can be bigger, and the raw material chromium powder conveyed by ammonia enters plasma flame flow through powder feeding rifle, passes through
Visor observes plasma flame flow wake flame, should then reduce powder sending quantity if any the shinny particle of Meteor-shape or increase plant capacity, should be first
Consider that selection reduces powder sending quantity；
4., argon plasma temperature about 10000K, 2672 DEG C of 1857 DEG C of the fusing point of chromium, boiling point, controls technological parameter, flows through
The raw material chromium powder of ion flame stream will all be gasificated into metallic vapour and possess great work under the corrasion of plasma
Property, ammonia is Nitrogen ion and hydrogen ion through plasma high-temperature heat resolve, and the chromium metallic vapour and Nitrogen ion for possessing activity exist
There is combination reaction in plasma flame flow, generate chromium nitride and driven into main frame tank by plasma flame flow, supplied through quenching gas circuit
The argon gas given is cooled down, and chromium nitride steam condensation is solid nano powder；To reduce production cost, quenching air-flow can also use nitrogen
Gas；
5., the chromium nitride nano powder and argon gas, undecomposed ammonia and hydrogen of solidification are mixed in aerosol form disperse
In main frame tank interior, collection device is entered under mixed gas drive, powder is filtered by filter core forced quarantine, filter core Yin Neibiao
Flour body is piled up and will excessively influence filter efficiency, can reach setting value by the pressure differential of differential pressure pickup detection filter core both sides
Start blowback magnetic valve, the powder that filter core inner surface is piled up is removed in the blowback air back flush provided by blowback gas circuit, also may be used
After differential pressure pickup sends alarm, to take artificial impact method vibration filter core, make the powder that its inner surface is piled up because of vibration
Drop, blowback air can be argon gas or nitrogen, and whether using gas back-flushing or using impact mode of vibration, its purpose is all
It is the bottom for making the powder for being deposited in filter core inner surface drop to collection device, the vacuum packet of finished product powder is realized by packing case
Dress.
2. the preparation method of a kind of chromium nitride nano powder according to claim 1, it is characterised in that：The 1. described height of step
The multi-functional power production equipment of frequency plasma includes gas flow switch board（1）, energy storage tank（2）, ammonia bottle（3）, flowmeter
（4）, powder feeding air pipe（5）, ion-gas gas circuit（6）, interior cooling gas circuit（7）, quenching gas circuit（8）, outer cold air（9）, powder feeder
（10）, powder feeding rifle（11）, blowback gas circuit（12）, collection device（13）, filter core (14), exhaust gas processing device (15), packing case
(16), argon bottle (17), main frame tank (18), visor (19), light fixture (20) and induction coil (21)；The gas flow switch board
(1) for detecting, needed for each road of control device gas flow, it is internal that energy storage tank (2) is placed in gas flow switch board (1), described
Energy storage tank (2) one end is connected with argon bottle (17), other end gas outlet respectively with ion-gas gas circuit (6), it is interior cooling gas circuit (7),
Quenching gas circuit (8) and blowback gas circuit (12) are connected, wherein the ion-gas gas circuit (6) and interior cooling gas circuit (7) and light fixture (20)
Connection, quenching gas circuit (8) is connected with main frame tank (18) top, and outer cooling gas circuit (9) is connected logical with other air compressor
Overcompression air is cooled down to light fixture, and the ammonia bottle is connected through flowmeter (4) and powder feeding air pipe (5) with powder feeder (10)；Institute
Induction coil (21) is stated to be sleeved on light fixture (20) outside, activate working gas in light fixture by the electromagnetic viscosimeter of electromagnetic field of high frequency
(20) it is internal to produce high-temperature plasma；The powder feeding rifle (11) is internal and coaxial positioned at light fixture (20), powder feeder (10) with give
Powder rifle (11) is connected；The light fixture (20) is placed in main frame tank (18) top, main frame tank（18）Side is provided with visor（19）；It is described
Powder collection device（13）It is connected with main frame tank (18) by pipeline, powder collection device (13) top and blowback gas circuit
(12) connect, it is internally provided with filter core (14), and the filter core (14) is forced to be isolated in it for rigid hollow cylinder, powder
Surface, can be made using ceramic material, powdered metallurgical material or fibrous material；The exhaust gas processing device (15) is by pipeline
It is connected with powder collection device (13)；Main frame tank (18) bottom, powder collection device (13) bottom are all connected with packing case
(16), for realizing packing vacuum powder.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107812956A (en) * | 2017-09-19 | 2018-03-20 | 南京航空航天大学 | A kind of composite powder preparation method and equipment for directly generating FeN enhancing phases |
| CN108163821A (en) * | 2018-01-30 | 2018-06-15 | 攀枝花学院 | The preparation method of spherical titanium nitride |
| CN108746652A (en) * | 2018-06-22 | 2018-11-06 | 上海硕余精密机械设备有限公司 | A kind of preparation facilities of metal powder and preparation method thereof |
| CN110128148A (en) * | 2019-04-26 | 2019-08-16 | 山东科技大学 | A kind of preparation method of chromium nitride ceramic membrane |
| CN111620312A (en) * | 2020-06-09 | 2020-09-04 | 合肥中航纳米技术发展有限公司 | Preparation method of nano chromium nitride powder |
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| CN103641082A (en) * | 2013-12-12 | 2014-03-19 | 河南工业大学 | Method of synthesizing nano chromium nitride powder by carbon-thermal-reduction nitriding process |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107812956A (en) * | 2017-09-19 | 2018-03-20 | 南京航空航天大学 | A kind of composite powder preparation method and equipment for directly generating FeN enhancing phases |
| CN107812956B (en) * | 2017-09-19 | 2019-07-30 | 南京航空航天大学 | A kind of composite powder preparation method and equipment directly generating FeN reinforced phase |
| CN108163821A (en) * | 2018-01-30 | 2018-06-15 | 攀枝花学院 | The preparation method of spherical titanium nitride |
| CN108746652A (en) * | 2018-06-22 | 2018-11-06 | 上海硕余精密机械设备有限公司 | A kind of preparation facilities of metal powder and preparation method thereof |
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| CN110128148A (en) * | 2019-04-26 | 2019-08-16 | 山东科技大学 | A kind of preparation method of chromium nitride ceramic membrane |
| CN111620312A (en) * | 2020-06-09 | 2020-09-04 | 合肥中航纳米技术发展有限公司 | Preparation method of nano chromium nitride powder |
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