CN106927436B - 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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- CN106927436B CN106927436B CN201511010963.0A CN201511010963A CN106927436B CN 106927436 B CN106927436 B CN 106927436B CN 201511010963 A CN201511010963 A CN 201511010963A CN 106927436 B CN106927436 B CN 106927436B
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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, this method obtain chromium nitride superfines using the high temperature and the etching effect of plasma, realization chemical gaseous phase synthesis of catalytic behavior of materials.This method be integrally vacuumized by equipment, generate high-temperature plasma, adjust ammonia flow, the condensation of solid nano powder, solidification chromium nitride nano powder collect, packaging and other steps realize, the method of the present invention can obtain the nanoscale chromium nitride nano powder of average grain diameter 40nm or so, its narrower particle size distribution, powder is spherical shape, has many advantages, such as that simple processing step, burn rate, reaction temperature, reaction process are easy to control, generate without pollutant.
Description
Technical field
The present invention relates to nano powder manufacturing fields, more particularly to a kind of preparation method of chromium nitride nano powder, the party
Method is ultra-fine using the high temperature of catalytic behavior of materials and etching effect, the realization chemical gaseous phase synthesis acquisition chromium nitride of plasma
Powder.
Background technique
Nano-powder has the physical and chemical performance different from common material, aobvious in machinery, electromagnetism, light, heat, chemical field
Its property is shown, is the important component of current new material.
Chromium nitride (CrN) has good physical and mechanical properties, and hardness is high, acid-alkali-corrosive-resisting is good, chemical stabilization
Property height, the good, high-melting-point of wearability etc., meanwhile, uniquely there are antiferromagnetic materials in chromium nitride or nitride.Make it in magnetic
, electronics industry, high-temperature-resistant structure ceramics etc. are used widely, and as a kind of new material, chromium nitride has wide
Application prospect.
Currently, ultra-fine chromium nitride produces that there are as below methods:
1, high-energy ball milling method: by chromium powder 180 ~ 300h of high-energy ball milling under nitrogen atmosphere, it can get 100 nanometers of average grain diameter
CrN powder, but in the presence of the device is complicated, produces time length, the deficiency that product is easily polluted by ball-milling medium.
2, benzene thermal method: by suitable CrCl3And Li3N is placed in stainless steel cauldron, and benzene is added as solvent, then heats
350~420 DEG C of heat preservation 6h of reaction kettle, naturally cool to room temperature.The LiCl and excess Li in product are washed away with dehydrated alcohol3After N,
Product is dried in vacuo 2h under the conditions of 80 DEG C, can get the CrN powder of 25 rans.
3, self-propagating high-temperature method: 2 microns of average grain diameter of pine dress chromium powder is packed into graphite crucible, is placed in the closed appearance of stainless steel
In device, it is passed through nitrogen after vacuumizing and keeps certain pressure, then by current heating resistor silk and the chromium powder that ignites, passes through resistance wire
What is heated is a bit of chromium powder, and chemical reaction can continue to spread under the support of self-heat generation after burning, until entire earthenware
Crucible, the product of acquisition are Cr2N and CrN, this method technique, equipment are simple, but that there is also manufactured goods particles is excessive, needs two
The secondary broken and uppity deficiency of burn rate, reaction temperature, reaction process.
4, ammonolysis process: with ammonia (NH3) it is catalyst, ammonia is directly reacted with reactant to generate nitride at high temperature
Method.In recent years, ammonolysis process has been widely used in the preparation of nitride powder, successfully prepared CrN, TiN,
A variety of nitride such as NbN.Cr will be such as housed2S3Quartz ampoule be placed on Muffle furnace, be passed through flowing and ammonia and be heated to 800 DEG C and protect
Temperature 48 hours, then natural cooling can get CrN powder, by-product H2S, the disadvantage is that the reaction time is long, finished particle
Greatly, H2S leads to environmental pollution.There are also ammonolysis CrCl3, ammonolysis Cr2O3, ammonolysis urea chromic salts etc., require higher reaction temperature
With the longer reaction time, and generated with pollutant.
Summary of the invention
It, can the invention aims to provide a kind of method for producing chromium nitride nano powder using catalytic behavior of materials
To obtain the nanoscale chromium nitride nano powder of average grain diameter 40nm or so, narrower particle size distribution, powder is spherical shape, has work
Skill step is simple, burn rate, reaction temperature, reaction process is easy to control, does not have the advantages that pollutant generates.
The object of the present invention is achieved like this, method includes the following steps: a kind of 1, preparation of chromium nitride nano powder
Method, it is characterised in that: method includes the following steps:
1., first starting vacuum pump set to " High-frequency plasma multifunctional powder production equipment " integrally vacuumize, make to set
Standby vacuum degree reaches 6.0 × 10-2Pa is then injected into high-purity argon gas, reaches energy storage tank gas pressure before equipment starting
0.6MPa, equipment internal pressure reach 0MPa；
2., starting device, use argon gas for ion-gas and interior cooling gas, formed in high-frequency and high-voltage electric excitation down-firing
Gas ions, adjustment gas flow make ion-gas flow reach 40~60L/min, interior 140 L/min or more of cooling gas flow, adjust
Whole 7~8.5KV of anode voltage, 5.5~8A of anode current, formed in lamps and lanterns 20 stablize, the plasma flame stream of rule, from upper
It flows down into host tank；
3., by flowmeter adjust ammonia flow, adjustment powder feeder conveying chromium powder powder sending quantity, it is true according to reaction equation
Both fixed molal weight ratio, the ratio of ammonia can be bigger, enters plasma flame flow through powder feeding rifle by the raw material chromium powder that ammonia conveys,
Plasma flame flow wake flame is observed by visor, should then reduce powder sending quantity if any the shinny particle of Meteor-shape or increases plant capacity, is answered
Consider that selection reduces powder sending quantity first；
4., argon plasma temperature about 10000K, 2672 DEG C of 1857 DEG C of fusing point, the boiling point of chromium control technological parameter, flows
Raw material chromium powder through plasma flame flow will all be gasificated into metallic vapour and have under the corrasion of plasma greatly
Activity, ammonia through plasma high-temperature heat resolve be Nitrogen ion and hydrogen ion, have active chromium metallic vapour and nitrogen from
Combination reaction occurs in plasma flame flow for son, generates chromium nitride and is driven by plasma flame flow into host tank, through quenching gas
The argon gas of road supply is cooling, and chromium nitride steam condensation is solid nano powder；To reduce production cost, quenching air-flow can also be used
Nitrogen；
5., solidification chromium nitride nano powder and argon gas, undecomposed ammonia and hydrogen mix in aerosol form
Disperse enters collection device under mixed gas drive in host tank interior, and powder is filtered by filter core forced quarantine, filter core because
The accumulation of inner surface powder will excessively will affect filter efficiency, and the pressure difference of filter core two sides can be detected by differential pressure pickup, reaches and sets
Definite value starts blowback solenoid valve, and the powder of filter core inner surface accumulation is removed by the blowback air back flush that blowback gas circuit provides,
Artificial impact method vibration filter core can also be taken after differential pressure pickup issues alarm, the powder for accumulating its inner surface because
Vibration is fallen, and blowback air can be argon gas or nitrogen, whether using gas back-flushing or using impact mode of vibration, mesh
Be all the bottom for making the powder for being deposited in filter core inner surface fall to collection device, pass through packing case realize finished product powder it is true
Empty package.
A kind of High-frequency plasma multifunctional powder production equipment includes gas flow control cabinet, energy storage tank, ammonia bottle, stream
Meter, 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, host tank, visor, lamps and lanterns and induction coil.
The present invention is obtained using the corrasion of the high temperature and plasma of catalytic behavior of materials by chemical gaseous phase synthesis
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), chemical equation are as follows:
Argon gas can generate the argon plasma that temperature reaches 10000K under the excitation of induction coil in quartzy lamps and lanterns,
The plasma is generated by electromagnetic induction, is a kind of pure plasma heat source without electrode fouling.
Plasma is sent into through powder feeding rifle in chromium powder end by powder feeder, chromium powder can moment gas when flowing through plasma flame stream
Turn to nano-liquid droplet and active through plasma etching.
Using ammonia as the powder feeding carrier gas at conveying chromium powder end, ammonia and chromium powder end enter plasma together, in plasma
Under body high temperature action, ammonia molecule is decomposed into Nitrogen ion, hydrogen ion, and wherein Nitrogen ion is chemically reacted with chromium nano-liquid droplet,
Chromium nitride is generated, is solidified as chromium nitride nanometer powder through quenching gas cooling.
The chromium nitride nanometer powder disperse of solidification is in a kind of aerosol in argon gas, hydrogen ion, remaining Nitrogen ion and ammonia
State enters behind machine hall and enters powder collection device through pipeline liquid injecting device, by porous filter core forced collection, filters out nano-powder,
Tail gas includes that ammonia, nitrogen can handle rear outlet on a small quantity for argon gas, hydrogen, residue, and if reaction controlling must be got well, efflux gas only has
Argon gas and hydrogen, hydrogen can be consumed by ignition way.
The present invention has the advantages that:
1, argon plasma flame stream temperature of the present invention reaches as high as 10000K, and wake flame temperature, can be according to required up to 3000K
Reaction temperature selects suitable powder feeding position.
2, of the invention since the generation of catalytic behavior of materials does not depend on electrode, argon gas is inert gas, will not and be made
It is chemically reacted for the chromium of raw material, ammonia and Nitrogen ion, hydrogen ion, it is ensured that the purity of product.
3, present invention control raw material diameter of particle and equipment output power, can be readily available Unusually narrow particle size distribution
Spherical super fine powder finished product.
4, production process of the present invention is continuous, it is easy to accomplish automatic industrial production.
Detailed description of the invention
Fig. 1 is present device structural schematic diagram.
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 control cabinet 1, accumulation of energy
Tank 2, 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, is sent ammonia bottle 3
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
17, host tank 18, visor 19, lamps and lanterns 20 and induction coil 21.
The gas flow control cabinet 1 is placed in gas for gas flow needed for detecting, controlling each road of equipment, energy storage tank 2
Inside flow control cabinet 1, described 2 one end of energy storage tank connect 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 connect, wherein the ion-gas gas circuit 6 and interior cooling gas circuit 7 and lamps and lanterns
20 connections, quenching gas circuit 8 are connect with 18 top of host tank, and the outer cooling gas circuit 9 is connect with other air compressor passes through pressure
Contracting air is cooling to lamps and lanterns, and the ammonia bottle is connect through flowmeter 4 and powder feeding air pipe 5 with powder feeder 10.
The induction coil 21 is sleeved on outside lamps and lanterns 20, electromagnetic field of high frequency and moment external high-frequency in induction coil 21
Under high-voltage electricity joint incentive, high-temperature plasma is generated in lamps and lanterns 20, external high-frequency high-voltage electricity is removed after plasma ignition,
Without electrode in lamps and lanterns 20.The powder feeding rifle 11 is located at the inside of lamps and lanterns 20 and coaxial, and powder feeder 10 is connect with powder feeding rifle 11.
The lamps and lanterns 20 are placed in 18 top of host tank, and 18 side of host tank is provided with visor 19.
The powder collection device 13 is connect by pipeline with host tank 18,13 top of powder collection device and blowback
Gas circuit 12 connects, and 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 production.
The exhaust gas processing device 15 is connect by pipeline with powder collection device 13.
18 bottom of host tank, 13 bottom of powder collection device are connected with packing case 16, all for realizing true to powder
Empty package.
It is as shown in Figure 2: a kind of preparation method of chromium nitride nano powder, comprising the following steps:
1. starting vacuum pump set integrally vacuumizes " High-frequency plasma multifunctional powder production equipment " first, make equipment
Vacuum degree reach 6.0 × 10-2Pa is then injected into high-purity argon gas, so that 2 gas pressure of energy storage tank is reached 0.6MPa before equipment starting
(gauge pressure), equipment internal pressure reach 0MPa(gauge pressure)；
2. using argon gas for ion-gas and interior cooling gas, starting device, induction coil generates high-frequency electromagnetic in lamps and lanterns
, plasma is formed in moment high-frequency and high-voltage electric excitation down-firing, removes high-frequency high-voltage, adjustment gas flow makes ion-gas
Flow reaches 40~60L/min, interior 140 L/min or more of cooling gas flow, adjusts 7~8.5KV of anode voltage, anode current
5.5~8A, the interior plasma flame stream for forming stable rule of lamps and lanterns 20, flows into host tank 18 from top to bottom；
3. adjusting ammonia flow by flowmeter 4, adjustment powder feeder 10 conveys the powder sending quantity of chromium powder, according to reaction equation
Determine the two molal weight ratio, the ratio of ammonia can be bigger, enters plasma through powder feeding rifle 11 by the raw material chromium powder of ammonia conveying
Flame stream observes plasma flame flow wake flame by visor 19, should then reduce powder sending quantity if any the shinny particle of Meteor-shape or increase equipment
Power should consider that selection reduces powder sending quantity first；
4. argon plasma temperature about 10000K, 2672 DEG C of 1857 DEG C of fusing point, the boiling point of chromium, control technological parameter, stream
Raw material chromium powder through plasma flame flow will all be gasificated into metallic vapour and have under the corrasion of plasma greatly
Activity, ammonia through plasma high-temperature heat resolve be Nitrogen ion and hydrogen ion, have active chromium metallic vapour and nitrogen from
Combination reaction occurs in plasma flame flow for son, generates chromium nitride and is driven by plasma flame flow into host tank, through quenching gas
The argon gas that road 8 supplies is cooling, and chromium nitride steam condensation is solid nano powder；To reduce production cost, quenching air-flow can also be adopted
Use nitrogen；
5. the chromium nitride nano powder solidified and argon gas, undecomposed ammonia and hydrogen are mixed in aerosol form more
It is dispersed in host tank interior, collection device 13 is entered under mixed gas drive, powder is filtered by 14 forced quarantine of filter core, filter core
Because powder accumulation in surface will excessively will affect filter efficiency, the pressure difference of filter core two sides can be detected by differential pressure pickup, reaches and sets
Definite value starts blowback solenoid valve, and the powder of cartridge surface accumulation is removed by 11 back flush of blowback gas circuit, can also be in pressure difference
After sensor issues alarm, artificial impact method vibration filter core is taken, the powder for accumulating its surface is because vibration is fallen, blowback air
It can be argon gas or nitrogen, whether using gas back-flushing or using impact mode of vibration, purpose is all to make to be deposited in
The powder of filter core falls to the bottom of collection device 13, and 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 may be the nanometer powder mixture of CrN+Cr,
Process above can be repeated, secondary treatment is carried out to the mixture of CrN+Cr.
Claims (2)
1. a kind of preparation method of chromium nitride nano powder, it is characterised in that: method includes the following steps:
1., first starting vacuum pump set to " High-frequency plasma multifunctional powder production equipment " integrally vacuumize, make equipment
Vacuum degree reaches 6.0 × 10-2Pa is then injected into high-purity argon gas, so that energy storage tank gas pressure is reached 0.6MPa before equipment starting, if
Standby internal pressure reaches 0MPa；
2., use argon gas for ion-gas and interior cooling gas, starting device, make induction coil occur the higher-order of oscillation, in the line of induction
It encloses under the electromagnetic field of high frequency and moment external high-frequency high-voltage electricity joint incentive of (21), high-temperature plasma is generated in lamps and lanterns (20)
Body removes external high-frequency high-voltage electricity after plasma ignition, and adjustment gas flow makes ion-gas flow reach 40~60L/min,
Interior 140 L/min or more of cooling gas flow adjusts 7~8.5KV of anode voltage, 5.5~8A of anode current, lamps and lanterns (20) interior shape
At the plasma flame stream of stabilization, rule, host tank is flowed into from top to bottom；
3., by flowmeter adjust ammonia flow, adjustment powder feeder conveying chromium powder powder sending quantity, determine two according to reaction equation
Person's molal weight ratio, the ratio of ammonia can be bigger, enters plasma flame flow through powder feeding rifle by the raw material chromium powder that ammonia conveys, 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, Ying Shouxian
Consider that selection reduces powder sending quantity；
4., argon plasma temperature 10000K, 2672 DEG C of 1857 DEG C of fusing point, the boiling point of chromium control technological parameter, flow through etc. from
The raw material chromium powder of sub- flame stream will all be gasificated into metallic vapour and have great activity under the corrasion of plasma,
Ammonia through plasma high-temperature heat resolve be Nitrogen ion and hydrogen ion, have active chromium metallic vapour and Nitrogen ion wait from
Combination reaction occurs in sub- flame stream, generate chromium nitride and is driven by plasma flame flow into host tank, is supplied through quenching gas circuit
Argon gas is cooling, and chromium nitride steam condensation is solid nano powder；To reduce production cost, quenching air-flow uses nitrogen；
5., solidification chromium nitride nano powder and argon gas, undecomposed ammonia and hydrogen mix in aerosol form disperse
In host tank interior, enter collection device under mixed gas drive, powder is filtered by filter core forced quarantine, filter core Yin Neibiao
The accumulation of flour body will excessively will affect filter efficiency, and the pressure difference of filter core two sides can be detected by differential pressure pickup, reaches setting value
Start blowback solenoid valve, the powder of filter core inner surface accumulation is removed by the blowback air back flush that blowback gas circuit provides, is being pressed
After gap sensor issues alarm, artificial impact method vibration filter core is taken, the powder for accumulating its inner surface is because vibration is fallen, instead
Air blowing is argon gas or nitrogen, and whether using gas back-flushing or using impact mode of vibration, purpose is all to make to be deposited in
The powder of filter core inner surface falls to the bottom of collection device, and the vacuum packaging of finished product powder is realized by packing case.
2. a kind of preparation method of chromium nitride nano powder according to claim 1, it is characterised in that: the step 1. height
The multi-functional power production equipment of frequency plasma includes gas flow control cabinet (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 cooling gas circuit (9), powder feeding
Device (10), powder feeding rifle (11), blowback gas circuit (12), powder collection device (13), filter core (14), exhaust gas processing device (15), packet
Vanning (16), argon bottle (17), host tank (18), visor (19), lamps and lanterns (20) and induction coil (21)；The gas flow control
For cabinet (1) processed for gas flow needed for detecting, controlling each road of equipment, energy storage tank (2) is placed in gas flow control cabinet (1) inside,
Described energy storage tank (2) one end connect 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) connection, wherein the ion-gas gas circuit (6) and interior cooling gas circuit (7) and lamps and lanterns
(20) it connects, quenching gas circuit (8) is connect with host tank (18) top, and the outer cooling gas circuit (9) and other air compressor connect
It is cooling to lamps and lanterns to connect overcompression air, the ammonia bottle connects through flowmeter (4) and powder feeding air pipe (5) and powder feeder (10)
It connects；The induction coil (21) is sleeved on lamps and lanterns (20) outside, activates working gas to exist by the electromagnetic viscosimeter of electromagnetic field of high frequency
High-temperature plasma is generated inside lamps and lanterns (20)；The powder feeding rifle (11) is located at lamps and lanterns (20) inside and coaxial, powder feeder (10)
It is connect with powder feeding rifle (11)；The lamps and lanterns (20) are placed at the top of host tank (18), and host tank (18) side is provided with visor (19)；
The powder collection device (13) is connect by pipeline with host tank (18), powder collection device (13) top and blowback air
Road (12) connection, is internally provided with filter core (14), and the filter core (14) is rigid hollow cylinder, powder is forced to be isolated in it
Inner surface is made of ceramic material, powdered metallurgical material or fibrous material；The exhaust gas processing device (15) by pipeline with
Powder collection device (13) connection；Host tank (18) bottom, powder collection device (13) bottom are all connected with packing case
(16), it is packed for realizing to vacuum powder.
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| 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 |
| CN108163821B (en) * | 2018-01-30 | 2019-12-13 | 攀枝花学院 | Preparation method of spherical titanium nitride |
| CN108746652B (en) * | 2018-06-22 | 2021-08-31 | 上海硕余精密机械设备有限公司 | Preparation device and preparation method of metal powder |
| CN110128148B (en) * | 2019-04-26 | 2021-11-02 | 山东科技大学 | 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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| CN102847950A (en) * | 2011-06-29 | 2013-01-02 | 王志平 | High-frequency plasma multifunctional powder production equipment |
| CN103318855A (en) * | 2013-06-09 | 2013-09-25 | 上海大学 | Preparation method of chromium nitride |
| 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 |
| CN104261837A (en) * | 2014-09-22 | 2015-01-07 | 辽宁科技大学 | Method for preparing high-nitrogen chromium powder |
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| US6090223A (en) * | 1997-06-25 | 2000-07-18 | Showa Denko K.K. | Chromium nitride film and method for forming the same |
| CN102847950A (en) * | 2011-06-29 | 2013-01-02 | 王志平 | High-frequency plasma multifunctional powder production equipment |
| CN103318855A (en) * | 2013-06-09 | 2013-09-25 | 上海大学 | Preparation method of chromium nitride |
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Effective date of registration: 20190712 Address after: 725000 No. 37 Innovation Road, Hanbin District, Ankang City, Shaanxi Province Patentee after: Shaanxi Ankang San hang nano Polytron Technologies Inc Address before: 136001, Siping East Road, Siping City, Jilin Province, No. 309 Patentee before: SIPING GAOSIDA NANO MATERIAL & EQUIPMENT CO., LTD. |
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Denomination of invention: Preparation method of chromium nitride nanometer powder Effective date of registration: 20190814 Granted publication date: 20190416 Pledgee: Ankang Hi-tech Industry Development Co., Ltd. Pledgor: Shaanxi Ankang San hang nano Polytron Technologies Inc Registration number: Y2019610000012 |
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