CN107128921B - A method of preparing niobium tungsten binary double carbide nano powder - Google Patents
A method of preparing niobium tungsten binary double carbide nano powder Download PDFInfo
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- CN107128921B CN107128921B CN201710270171.XA CN201710270171A CN107128921B CN 107128921 B CN107128921 B CN 107128921B CN 201710270171 A CN201710270171 A CN 201710270171A CN 107128921 B CN107128921 B CN 107128921B
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
Abstract
The invention discloses a kind of methods for preparing niobium tungsten binary double carbide nano powder, the steps include: S1, are added to wolframic acid salt powder in fluorine niobic acid solution, then plus surfactant, until pH value 9~12, it is still aging after filtering；S2, niobium tungsten presoma sediment is obtained, washed；S3, the sediment drying of washing, mill are sieved, obtains niobium tungsten presoma composite powder；S4, reduction treatment is carried out to niobium tungsten presoma composite powder, obtains niobium oxide-tungsten composite powder；S5, selection are practical with carbon ratio；S6, carbon is added, it is uniformly mixed with raw material powder；S7, uniformly mixed powder pine is mounted in graphite boat or ceramic boat, makees carbonization treatment, the cooling that is disposed is come out of the stove；S8, will come out of the stove after niobium tungsten double carbide mill sieve, obtain niobium tungsten binary complex carbide powder.This method realizes niobium tungsten binary double carbide in the mixing of molecular scale, and not only powder particle is tiny, but also chemical uniformity and purity are very high.
Description
Technical field
The present invention relates to powder metallurgical technologies, relate in particular to a kind of using chemical coprecipitation-hydrogen reduction-carbonization
The method for preparing ultra-fine/nanometer niobium tungsten binary complex carbide powder.
Background technique
Tungsten carbide is the most common hard phase of hard alloy, and WC-Co hard alloy is because having high intensity, hardness and excellent
Good wearability and inoxidizability is widely used in the fields such as machining, petroleum, mine, mold and structure wearing piece.
Ultra-fine cemented carbide efficiently solves the contradiction between conventional rigid alloy rigidity and intensity, with higher intensity, firmly
Degree and wearability meet the development of modern industry and extraordinary difficult-to-machine material, and it is miniature to be widely used in production integrated circuit board
Drill bit, dot-matrix printer drill bit, difficult-to-machine material cutter, medical dental drill etc..
However, the preparation of Ultra-fine Grained Talide always exists the technological difficulties of two aspects: preparing nanoscale
Crystal grain during powder and inhibition sintering is grown up.Mainly there are the method for 3 kinds of acquisition nanometer grade powders: mechanical ball mill, spray at present
Mist is dry, chemical synthesis.High-energy ball milling method be used to prepare nanometer grade powder, but need higher energy, and commercialization
Purity is low, and chemical uniformity is poor.Drying process with atomizing is that spray drying forms chemistry after mixing precursor compound solution
The mixture of uniform properties, then carburizing obtains nanometer grade powder.Although mechanical ball mill and drying process with atomizing are in industrial circle
Using relatively wide and achieve certain progress, but chemical synthesis route is always the prefered method of most researchers, this method
It is to mix metallic element on a molecular scale with chemical method, thus by the uniformity controlling in chemistry and microstructure in sub-micro
Metrical scale, the powder prepared in this way have very high chemical uniformity, degree of purity and nanoscale crystallite dimension.
Ultra-fine cemented carbide preparation another problem be how to inhibit sintering during crystal grain rapidly grow up.It grinds at present
Studying carefully at most most widely used method is addition transition metal carbide (such as VC, Cr3C2, NbC, TaC etc.) or rare earth addition come
Inhibit growing up for WC crystal.However the inhibitor due to addition always exists non-uniform ask with tungsten-carbide powder mixed process
Topic, inhibitor cannot be evenly distributed on around tungsten carbide powder, and there are localized clusters phenomenon, causing cannot be fine in sintering process
Inhibition tungsten carbide crystal grain grow up.
With science and technology and the fast development of processing manufacturing industry, to the performance of hard alloy, more stringent requirements are proposed,
The Ultra-fine Grained even research and development and production of Nanograin Cemented Carbide have obtained more and more concerns, and the preparation of nano powder and inhibition
Crystal grain both of these problems of growing up could not be solved effectively always, and the bottleneck of cemented carbide industry development is become.
Summary of the invention
It is an object of the invention to, provide a kind of to prepare niobium tungsten binary double carbide in view of the above-mentioned defects in the prior art
The method of nano powder prepares ultra-fine/nanometer niobium tungsten binary double carbide using chemical coprecipitation nanometer in situ complex technique
Powder.The technology has overturned the simple and mechanical hybrid technique of traditional raw material tungsten-carbide powder and inhibitor niobium carbide powder, real
Niobium tungsten binary double carbide is showed in the mixing of molecular scale, not only powder particle is tiny, but also chemical uniformity and purity
It is very high, solve the problems, such as that nano tungsten carbide preparation is difficult non-uniform with inhibitor mixed, the powder can be used for preparing it is ultra-fine/
Nanograin Cemented Carbide.
To achieve the goals above, the technical scheme is that
A method of niobium tungsten binary double carbide nano powder is prepared, steps of the method are:
S1, the wolframic acid salt powder of calculation amount is added in fluorine niobic acid solution, adds the surfactant of calculation amount, mixed
After closing uniformly, it is continuously added alkaline precipitating agent, until pH value 9~12, still aging 0.1~2h, are then filtered；
The niobium tungsten presoma sediment obtained after S2, filtering is washed with drum ammonia hot pure water, is reduced fluorine in sediment and is contained
It measures to 0.3% or less；
S3, the sediment after washing is dried in baking oven device, then the hardened shape sediment of drying is carried out
Mill sieve, obtains niobium tungsten presoma composite powder；
S4, reduction treatment is carried out to niobium tungsten presoma composite powder using hydrogen, obtains niobium oxide-tungsten composite powder；
S5, according to the proportion of niobium oxide and tungsten in niobium oxide-tungsten composite powder, be respectively carbonized by niobium oxide with tungsten
Reaction equation, calculate it is theoretical with carbon ratio, and according to the condition of practical carburizing reagent (reaction atmosphere, loading boat
Material, stove calandria etc.) select reality to match carbon ratio；
S6, according to niobium oxide-tungsten composite powder proportion and total amount, be added the carbon of calculation amount, carbon may be selected carbon black or
Then it is uniformly mixed by graphite with raw material powder；
S7, by uniformly mixed powder pine in graphite boat perhaps ceramic boat under vacuum or hydrogen atmosphere,
Carbonization treatment is carried out within the scope of 1000 DEG C~1800 DEG C, 0.5~5h of soaking time comes out of the stove after furnace cooling；
S8, will come out of the stove after niobium tungsten double carbide carry out mill sieve, obtain niobium tungsten binary complex carbide powder, and detect
Powder size, purity at being grouped as.
As improvement to above-mentioned technical proposal, tungstates selects ammonium paratungstate or ammonium metatungstate, more preferably secondary tungsten
Sour ammonium.
As improvement to above-mentioned technical proposal, fluorine niobic acid solution selects niobium anti-stripping agent, the more preferably niobium of high-purity
Anti-stripping agent, in terms of niobium oxide, content is 20~150g/L, 0.2~2mol/L of HF concentration.
As improvement to above-mentioned technical proposal, surfactant selects PEG-400, PEG-600, PEG-1000 and PEG-
One of 2000 or a variety of, more preferably PEG-600, dosage (volume) are the 0.1%-2% of fluorine niobic acid solution, more preferably
0.2-0.6%。
As improvement to above-mentioned technical proposal, alkaline precipitating agent select ammonium hydroxide and ammonium hydrogen carbonate one of or two
Kind, more preferably ammonium hydroxide.
As improvement to above-mentioned technical proposal, solution is stirred during addition alkaline precipitating agent or ultrasound is shaken
It swings, slowly at the uniform velocity adds, until solution ph 9~10.
As improvement to above-mentioned technical proposal, the still aging time is preferably 0.2~0.5h.
As improvement to above-mentioned technical proposal, filtering is selected suction filtration or filters pressing, is more preferably filtered.
As improvement to above-mentioned technical proposal, ammonia density is selected as 0.1~1mol/L in drum ammonia hot pure water, more preferably
0.3~0.5 mol/L；Drum ammonia hot pure water temperature is selected as 40~100 DEG C, more preferably 50~80 DEG C.
As improvement to above-mentioned technical proposal, the optional heated-air circulation oven of drying unit or vacuum oven, more preferably
For heated-air circulation oven；Baking temperature is selected as 80~200 DEG C, and drying time is selected as 2~12h.
As improvement to above-mentioned technical proposal, niobium tungsten presoma composite powder hydrogen reduction temperature selects 600~1000 DEG C,
More preferably 700~900 DEG C；0.3~3h of soaking time, more preferably 0.5~1.5h.
As improvement to above-mentioned technical proposal, niobium oxide-tungsten composite powder carbonisation can be in the carbon of hydrogen shield
Change in furnace or vacuum carbon tube furnace and carry out, more preferably vacuum carbon tube furnace；Carburizing temperature is preferably 1200~1600 DEG C.
Compared with prior art, the advantages and positive effects of the present invention are:
(1) niobium tungsten binary complex carbide powder prepared by the present invention realizes niobium tungsten molecule using chemical coprecipitation
The mixing of scale thoroughly solves the problems, such as that raw material tungsten-carbide powder and inhibitor mixed are uneven in conventional rigid alloy, and
The nanoscale niobium tungsten complex carbide powder purity is high of acquisition, crystallite dimension is tiny, and crystallite dimension is in 10~200nm；
(2) wolframic acid can be added by control in the ratio of niobium tungsten in niobium tungsten binary complex carbide powder prepared by the present invention
The content of salt changes, and the niobium tungsten binary complex carbide powder of different ratio needed for obtaining, the powder can be used alone as preparing
The hard phase powder of hard alloy, can also be with other hard phases (such as titanium carbide, tantalum carbide, titanium nitride, titanium boride, aluminium oxide)
It is used after powder mixing, is used to prepare polynary hard phase cemented carbide.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical scheme in the embodiment of the invention is clearly and completely described,
Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based in the present invention
Embodiment, every other embodiment obtained by those of ordinary skill in the art without making creative efforts, institute
Any modification, equivalent substitution, improvement and etc. of work, should all be included in the protection scope of the present invention.
The step of method of the invention, is:
(1) chemical coprecipitation.
First by the proportion of niobium and tungsten in final required niobium tungsten complex carbide powder, and according to the type of selected tungstates
The concentration of (ammonium metatungstate or ammonium paratungstate) and fluorine niobic acid solution calculates the weight of required tungstates Yu fluorine niobic acid solution；
The tungstates of calculation amount is added in the fluorine niobic acid solution of calculation amount, the PEG table of fluorine niobic acid liquor capacity 0.1~2% is added
Face activating agent, stirs evenly and is prepared into sol solution；Then ammonium hydroxide is slowly homogeneously added into solution ph 9~12, in ammonium hydroxide
Solution is stirred during the entire process of addition or ultrasonic vibration；Be then allowed to stand 0.1~2h of ageing, then carry out filter or
Person's filters pressing；Filtered sediment is washed small to fluorine content with the drum ammonia hot pure water that 50~80 DEG C of ammonia densities are 0.1~1mol/L
In 0.3%；Then sediment after washing carries out mill sieve in drying in oven, obtain niobium tungsten presoma composite powder.
(2) hydrogen reduction.
In a hydrogen atmosphere by the niobium tungsten presoma composite powder of acquisition, within the scope of 600~1000 DEG C, heat preservation 0.3~
3h then comes out and cools down, and obtains niobium oxide-tungsten composite powder.
(3) it is carbonized
It is calculated respectively according to the carbonation equation formula of niobium oxide and tungsten respective theoretical with carbon ratio, the wherein carbonization of niobium oxide
Reaction equation are as follows: Nb2O5The carburizing reagent equation of+7C=2NbC+5CO, W are as follows: W+C=WC；The theory of niobium oxide is calculated
With carbon ratio KIt manages (niobium oxide)The theory of=0.316, W match carbon ratio KIt manages (tungsten)=0.065；Then according to oxygen in niobium oxide-tungsten composite powder
Change niobium and tungsten respectively shared by mass fraction ω (Nb2O5) and ω (W), it is calculated needed for 1kg niobium oxide-tungsten composite powder
Theoretical mixed carbon comtent m (C)(reason)=0.316×ω(Nb2O5)+0.065×ω(W)；Then it (is put according to the difference of practical Carbonization Conditions
Expect boat, carburizing atmosphere etc.) mass fraction ω (C) with fixed carbon in addition carbon raw material (carbon black or graphite)Gu, determine
Practical mixed carbon comtent m (C) needed for 1kg niobium oxide-tungsten composite powder(reality)=K(0.316×ω(Nb2O5)+0.065×ω(W))/
ω(C)Gu, wherein K is selection with carbon ratio, between 0.90~1.10；Then the carbon and niobium oxide-added needed for calculating
Tungsten composite powder is uniformly mixed, and is carbonized under vacuum or hydrogen atmosphere, carburizing temperature 1000~1800, carbonization time
0.5~5h comes out of the stove after furnace cooling to room temperature, obtains niobium tungsten binary carbide composite powder.
(4) mill sieve and detection
Niobium tungsten binary carbide composite powder after coming out of the stove carries out mill sieve, then carries out granularity, purity, chemical component group
At the analysis of the powder physical and chemical performances such as, apparent density.
1 Nb-30wt%W of embodiment is ultra-fine/preparation of nanometer niobium tungsten binary complex carbide powder
(1) prepared by sol solution
Weigh the ammonium paratungstate (5 (NH of 5 crystallizations water of 1276g band4)2O-12WO3-5H2O), and it is dissolved into 30L fluorine
In niobic acid solution, Surfactant PEG -600 300ml are then added, sol solution is uniformly mixing to obtain；Wherein fluorine niobic acid concentration
100g/L, HF acid concentration 1.2mol/L are calculated as with niobium oxide.
(2) ammonia neutralization precipitation
The concentrated ammonia liquor that concentration is 9.6N is slowly added into sol solution, until solution ph=9~10, stops ammonification
Water, and still aging 30min；The stirring to solution is always maintained in ammonium hydroxide adition process.
(3) filtering and washing
Sediment after ammonia is neutralized is filtered with Suction filtration device, and is sufficiently washed with drum ammonia hot pure water to sediment
It washs, until the fluorine content in sediment is less than 0.3%.
(4) drying mill sieve
Sediment after washing is placed in heated-air circulation oven at 120 DEG C and is dried 5 hours, mistake after grinding is then taken out
100 meshes are obtained by Nb (OH)5, (NH4) (10H2W12O42)·4H2The niobium tungsten presoma composite powder of O phase composition.
(5) hydrogen reduction
The niobium tungsten presoma composite powder of acquisition is subjected to reduction treatment, reduction temperature in 14 pipe hydrogen reducing furnaces
800 DEG C, soaking time 1 hour, obtain niobium oxide-tungsten composite powder.
(6) it is carbonized
The carbon black 815g that fixed carbon content is 95% or more is weighed, after mixing with 3000g niobium oxide-tungsten composite powder,
It is fitted into graphite boat and is compacted, be then carbonized in vacuum carbon pipe, 1350 DEG C of carburizing temperature, keep the temperature furnace cooling after 1h
It comes out of the stove after to room temperature, obtains niobium tungsten binary double carbide powder.
(7) mill sieve and detection
Niobium tungsten binary double carbide powder after coming out of the stove sieves with 100 mesh sieve, and detects powder property, wherein powder grain size
50~200nm, 1.12 μm of Fisher particle size, total carbon content 9.83%, free carbon content 0.06%, oxygen content < 0.1%, nitrogen content <
0.01%, W content 26.9%, surplus is niobium.
2 Nb-50wt%W of embodiment is ultra-fine/preparation of nanometer niobium tungsten binary complex carbide powder
(1) prepared by sol solution
Weigh the ammonium paratungstate (5 (NH of 5 crystallizations water of 2332g band4)2O-12WO3-5H2O), and it is dissolved into 30L fluorine
In niobic acid solution, Surfactant PEG -600 300ml are then added, sol solution is uniformly mixing to obtain；Wherein fluorine niobic acid concentration
80g/L, HF acid concentration 1.0mol/L are calculated as with niobium oxide.
(2) ammonia neutralization precipitation
The concentrated ammonia liquor that concentration is 9.6N is slowly added into sol solution, until solution ph=9~10, stops ammonification
Water, and still aging 30min；The stirring to solution is always maintained in ammonium hydroxide adition process.
(3) filtering and washing
Sediment after ammonia is neutralized is filtered with Suction filtration device, and is sufficiently washed with drum ammonia hot pure water to sediment
It washs, until the fluorine content in sediment is less than 0.3%.
(4) drying mill sieve
Sediment after washing is placed in heated-air circulation oven at 120 DEG C and is dried 5 hours, mistake after grinding is then taken out
100 meshes are obtained by Nb (OH)5, (NH4) (10H2W12O42)·4H2The niobium tungsten presoma composite powder of O phase composition.
(5) hydrogen reduction
The niobium tungsten presoma composite powder of acquisition is subjected to reduction treatment, reduction temperature in 14 pipe hydrogen reducing furnaces
780 DEG C, soaking time 1 hour, obtain niobium oxide-tungsten composite powder.
(6) it is carbonized
The carbon black 900g that fixed carbon content is 95% or more is weighed, after mixing with 4078g niobium oxide-tungsten composite powder,
It is fitted into graphite boat and is compacted, be then carbonized in vacuum carbon pipe, 1320 DEG C of carburizing temperature, keep the temperature furnace cooling after 1h
It comes out of the stove after to room temperature, obtains niobium tungsten binary double carbide powder.
(7) mill sieve and detection
Niobium tungsten binary double carbide powder after coming out of the stove sieves with 100 mesh sieve, and detects powder property, wherein powder grain size
50~200nm, 1.07 μm of Fisher particle size, total carbon content 8.76%, free carbon content 0.07%, oxygen content < 0.1%, nitrogen content <
0.01%, W content 45.6%, surplus is niobium.
3 Nb-70wt%W of embodiment is ultra-fine/preparation of nanometer niobium tungsten binary complex carbide powder
(1) prepared by sol solution
Weigh the ammonium paratungstate (5 (NH of 5 crystallizations water of 1488g band4)2O-12WO3-5H2O), and it is dissolved into 30L fluorine
In niobic acid solution, Surfactant PEG -600 300ml are then added, sol solution is uniformly mixing to obtain；Wherein fluorine niobic acid concentration
50g/L, HF acid concentration 0.7mol/L are calculated as with niobium oxide.
(2) ammonia neutralization precipitation
The concentrated ammonia liquor that concentration is 9.6N is slowly added into sol solution, until solution ph=9~10, stops ammonification
Water, and still aging 30min；The stirring to solution is always maintained in ammonium hydroxide adition process.
(3) filtering and washing
Sediment after ammonia is neutralized is filtered with Suction filtration device, and is sufficiently washed with drum ammonia hot pure water to sediment
It washs, until the fluorine content in sediment is less than 0.3%.
(4) drying mill sieve
Sediment after washing is placed in heated-air circulation oven at 120 DEG C and is dried 5 hours, mistake after grinding is then taken out
100 meshes are obtained by Nb (OH)5, (NH4) (10H2W12O42)·4H2The niobium tungsten presoma composite powder of O phase composition.
(5) hydrogen reduction
The niobium tungsten presoma composite powder of acquisition is subjected to reduction treatment, reduction temperature in 14 pipe hydrogen reducing furnaces
760 DEG C, soaking time 1 hour, obtain niobium oxide-tungsten composite powder.
(6) it is carbonized
The carbon black 565g that fixed carbon content is 95% or more is weighed, after mixing with 2548g niobium oxide-tungsten composite powder,
It is fitted into graphite boat and is compacted, be then carbonized in vacuum carbon pipe, 1300 DEG C of carburizing temperature, keep the temperature furnace cooling after 1h
It comes out of the stove after to room temperature, obtains niobium tungsten binary double carbide powder.
(7) mill sieve and detection
Niobium tungsten binary double carbide powder after coming out of the stove sieves with 100 mesh sieve, and detects powder property, wherein powder grain size
50~200nm, 1.03 μm of Fisher particle size, total carbon content 7.72%, free carbon content 0.09%, oxygen content < 0.1%, nitrogen content <
0.01%, W content 64.6%, surplus is niobium.
Claims (10)
1. a kind of method for preparing niobium tungsten binary double carbide nano powder, it is characterised in that: steps of the method are:
S1, the wolframic acid salt powder of calculation amount is added in fluorine niobic acid solution, adds the surfactant of calculation amount, mixing is equal
After even, it is continuously added alkaline precipitating agent, until pH value 9~12, still aging 0.1~2h, are then filtered；
The niobium tungsten presoma sediment obtained after S2, filtering with drum ammonia hot pure water washed, reduce sediment in fluorine content extremely
0.3% or less；
S3, the sediment after washing is dried in baking oven device, mill sieve then is carried out to the hardened shape sediment of drying,
Obtain niobium tungsten presoma composite powder；
S4, reduction treatment is carried out to niobium tungsten presoma composite powder using hydrogen, obtains niobium oxide-tungsten composite powder；
S5, according to the proportion of niobium oxide and tungsten in niobium oxide-tungsten composite powder, be respectively carbonized by niobium oxide with tungsten anti-
Equation is answered, is calculated theoretical with carbon ratio and practical with carbon ratio according to the selection of the condition of practical carburizing reagent；
S6, according to niobium oxide-tungsten composite powder proportion and total amount, be added the carbon of calculation amount, carbon is carbon black or graphite, then
It is uniformly mixed with raw material powder；
S7, by uniformly mixed powder pine in graphite boat perhaps ceramic boat under vacuum or hydrogen atmosphere, 1000
DEG C~1800 DEG C within the scope of carry out carbonization treatment, 0.5~5h of soaking time comes out of the stove after furnace cooling；
S8, will come out of the stove after niobium tungsten double carbide carry out mill sieve, obtain niobium tungsten binary complex carbide powder, and detect powder
Granularity, purity at being grouped as.
2. the method for preparing niobium tungsten binary double carbide nano powder as described in claim 1, it is characterised in that: tungstates is selected
Ammonium paratungstate or ammonium metatungstate.
3. the method for preparing niobium tungsten binary double carbide nano powder as described in claim 1, it is characterised in that: fluorine niobic acid solution
Niobium anti-stripping agent is selected, in terms of niobium oxide, content is 20~150g/L, 0.2~2mol/L of HF concentration.
4. the method for preparing niobium tungsten binary double carbide nano powder as described in claim 1, it is characterised in that: surfactant
One of PEG-400, PEG-600, PEG-1000 and PEG-2000 or a variety of are selected, dosage is fluorine niobic acid liquor capacity
0.1%-2%。
5. the method for preparing niobium tungsten binary double carbide nano powder as described in claim 1, it is characterised in that: alkaline precipitating agent
Select one or both of ammonium hydroxide and ammonium hydrogen carbonate.
6. the method for preparing niobium tungsten binary double carbide nano powder as described in claim 1, it is characterised in that: it is heavy that alkalinity is added
Shallow lake agent is stirred in the process to solution or ultrasonic vibration, slowly at the uniform velocity adds, until solution ph 9~10.
7. the method for preparing niobium tungsten binary double carbide nano powder as described in claim 1, it is characterised in that: filtering, which is selected, takes out
Filter or filters pressing.
8. the method for preparing niobium tungsten binary double carbide nano powder as described in claim 1, it is characterised in that: drum ammonia hot pure water
Middle ammonia density is selected as 0.1~1mol/L, and drum ammonia hot pure water temperature is selected as 40~100 DEG C.
9. the method for preparing niobium tungsten binary double carbide nano powder as described in claim 1, it is characterised in that: drying unit choosing
Heated-air circulation oven or vacuum oven.
10. the method for preparing niobium tungsten binary double carbide nano powder as described in claim 1, it is characterised in that: niobium tungsten forerunner
Bluk recombination powder hydrogen reduction temperature selects 600~1000 DEG C, and soaking time is 0.3~3h.
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Address after: 341000 Yingbin Road, Ganzhou economic and Technological Development Zone, Jiangxi 62, China Patentee after: Ganzhou Nonferrous Metallurgy Research Institute Co.,Ltd. Address before: 341000 Yingbin Road, Ganzhou economic and Technological Development Zone, Jiangxi 62, China Patentee before: GANZHOU NONFERROUS METALLURGICAL Research Institute |