CN1872460A - Method for preparing round nickel powder in submicro - Google Patents
Method for preparing round nickel powder in submicro Download PDFInfo
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- CN1872460A CN1872460A CN 200610065021 CN200610065021A CN1872460A CN 1872460 A CN1872460 A CN 1872460A CN 200610065021 CN200610065021 CN 200610065021 CN 200610065021 A CN200610065021 A CN 200610065021A CN 1872460 A CN1872460 A CN 1872460A
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Abstract
A process for preparing submicron spherical Ni particles by liquid-phase reducing method includes such steps as reduction reaction between nickel sulfate (or nitrate or chloride) and ammonia-alcohol or citric acid in the aqueous solution of sodium hydroxide containing hydrazine hydrate, water washing, alcohol washing, separating, drying and sintering in N2+H2 atmosphere.
Description
Technical field
A kind of method for preparing the submicron order globular powdered nickel relates to the method that a kind of liquid phase reduction prepares the submicron order globular powdered nickel.
Background technology
Extra-fine nickel powder is opened up it gradually and is used in fields such as the energy, electronics, chemical industry, conductive materials, the research of nickel powder is become heat subject always.All in the requirement of constantly bringing forth new ideas and producing extra-fine nickel powder to adapt to, the method for preparing extra-fine nickel powder at present has following several at aspects such as preparation technology, equipment:
(1) carbonyl nickel thermal decomposition method, this method is covered moral by Britain and is proposed, and it mainly carries out in two steps: the first step makes CO and nickel reactant generate carbonyl nickel (CO)
4Second step made carbonyl nickel decompose in the thermal decomposition tower and obtains nickel powder.The nickel powder particle diameter that this method is produced is generally about 1 μ m.All there are production in order Canada, Britain, the U.S., Russia.There are two shortcomings in this method: the one, and decomposition temperature height in the pyrolysis tower, nickel powder easy-sintering event particle diameter pattern bigger than normal is rounding not; The 2nd, carbonyl nickel is a kind of extremely toxic substance, hinders health, and environment is caused very big pollution.
(2) it has been the classical way of implementing aborning for many years that electrochemical process, electrolysis prepare the micron order nickel powder, and shortcoming is that the nickel powder that makes is thicker, and pattern is rounding not.
(3) evaporation-condensation method is heated to 1425 ℃ with metallic nickel among the EP62112711, promptly the gasification, steam by cold-trap rapidly condensation can make nickel powder.Adopt the vacuum environment evaporation can reduce evaporating temperature, the cooling mode difference, the nickel powder of generation differs from one another.This method shortcoming is that production efficiency is low, the easy oxidation of particle, and the equipment complexity, the specification requirement height, therefore the cost height is difficult to realize suitability for industrialized production.
(4) pressurization liquid phase reduction, the analogy gram is peaceful to be waited at Ni (OH)
2The hydro-thermal hydrogen reduction prepares in extra-fine nickel powder one literary composition have been reported in alkaline medium, with PdCl
2Be catalyst, at autoclave pressure inner control uniform temperature H
2Reduction nickel hydroxide slip makes the nickel powder of average grain diameter tens nanometers.In order to substitute expensive PdCl
2Liang Huanzhen is at Ni (OH)
2Reported with anthraquinone in water slurry anthraquinone catalysis hydro-thermal method reduction preparation extra-fine nickel powder one literary composition and made catalyst, made 0.1～2.0 micron nickel powder with hydrogen reducing basic nickel carbonate slip.The hydrogen reduction of pressurization liquid phase needs high-tension apparatus and expensive catalysts, is unfavorable for suitability for industrialized production.
(5) normal pressure liquid phase reduction, the normal pressure liquid phase reduction is in nickel salt aqueous solution or Ni (OH)
2Use sodium borohydride in the suspension, hydrazine etc. for reducing agent under alkali condition, carry out reduction reaction, Xie Kenan etc. in extra-fine nickel powder preparation system research hydrazine reduction Ni (OH)
2Slip is produced in the process of extra-fine nickel powder, and reaction condition is to product yield, the influence of granularity and pattern.Liao stands in the research that liquid phase reduction prepares nano-nickel powder and then adopts hydrazine+inferior sodium phosphate to make reducing agent, makes the globular powdered nickel that particle mean size is 60nm under optimal conditions.Kwang Ho Kim etc. are solvent with normal propyl alcohol-water in Preparation of fine nickel powders in aqueous solutionunder wet chemical process one literary composition, add carboxymethyl cellulose and make dispersant, making particle diameter is 0.27～0.85 micron, and specific area is 8.98m
2The globular powdered nickel of/g.Normal pressure liquid phase reduction raw material is easy to get that equipment is simple, easy and simple to handle, efficient is high, particle size is little, even particle size distribution, arranged development prospect preferably.But sodium borohydride costs an arm and a leg in the reducing agent, and inferior sodium phosphate generates the Ni-P alloy easily again and influences properties of product, and hydrazine just becomes first-selected reducing agent.But the reducing agent consumption is more in these methods, is a problem that need solve.
(6) gas phase reduction process, gas phase reduction process are based on that high temperature makes metal chloride vaporization more than 1000 ℃ and feed hydrogen in reduction reactor carries out vapour phase reduction, and the metal dust of production is taken out of, cools off, collected by inert gas.Nickel chloride partial vapour pressure among US6500227, the US6203768 in the reactor remains between 0.2～0.7, hydrogen volume flow 0.02～0.07L/sec, can obtain average grain diameter less than 1 micron extra-fine nickel powder 1000 ℃ of following reduction, the nickel powder good sphericity, the degree of crystallinity height, distribution of particles is narrow, and is most between 0.1～0.4 micron.Change the nickel powder that nickel chloride partial vapour pressure and hydrogen volume flow just can get the different-grain diameter scope.Then the chlorination process of metallic nickel is combined with nickel chloride gas phase reduction process among the US6168752, the reactor of two processes is linked as integral body, by the intake velocity of chlorine just can control nickel chloride formation speed and and then stable control produce the nickel powder particle diameter between 0.1～1.0 micron.Above method has production process carries out continuously, the automaticity height, advantage such as product granularity is controlled, but since chlorination reaction and reduction reaction at high temperature more than 1000 ℃ and highly corrosive medium Cl
2, carry out among the HCl, very high to the equipment material requirement, equipment investment is huge, in addition equipment precision and control system is also had high requirements, and the at present domestic ability that does not still possess this kind equipment of processing is not so have the industrialization possibility at present.
Summary of the invention
The objective of the invention is to deficiency at above-mentioned prior art existence, provide a kind of can produce have completely spherical structure, the smooth rounding of particle surface, particle diameter is controlled and narrow diameter distribution, and the brief easily control of production technology, production cost is low, process units is simple, be easy to realize the industrialized method for preparing the submicron order globular powdered nickel.
The objective of the invention is to be achieved through the following technical solutions.
A kind of method for preparing the submicron order globular powdered nickel is characterized in that preparation process may further comprise the steps:
A. soluble nickel salt is dissolved in the deionized water, is mixed with the nickel salt complex solution with low mass molecule alcohol, ammonia, natrium citricum:
B. under heating condition, the nickel salt complex solution joined and contain hydrazine hydrate N
2H
4H
2Carry out reduction reaction in the sodium hydrate aqueous solution of O;
C. product obtains the nickel powder filter cake through liquid-solid separation, the impurity of slurry in washing removal filter cake;
D. the nickel powder filter cake after the washing is removed moisture with absolute ethanol washing;
E. the filter cake drying under reduced pressure of the nickel powder behind the absolute ethanol washing is removed ethanol and micro-moisture obtains dry nickel powder powder;
F. the nickel powder powder leads to nitrogen N in tube furnace
2With hydrogen H
2Gaseous mixture makes the submicron order globular powdered nickel of purity 〉=99%, surface finishing at 200～350 ℃ of following sintering.
Method of the present invention is characterized in that described soluble nickel salt is selected from NiSO
4, NiCl
2, Ni (NO
3)
2In a kind of or its hydrate, the concentration that is mixed with behind the aqueous solution is nickeliferous 30～60g/L,
Method of the present invention is characterized in that being mixed with that the nickel salt complex solution adopts is that the nickel sulfate solution of nickeliferous 40～50g/L of producing of nickel production process is a raw material.
Method of the present invention is characterized in that described nickel salt complex solution is made up of the component that is selected from water soluble nickel salt, low mass molecule alcohol, ammonia, citric acid and water, and comprise low mass molecule alcohol at least, two kinds of components in the ammonia, citric acid.
Method of the present invention,, it is characterized in that described low mass molecule alcohol is C
1～C
3Low mass molecule alcohol, preferred alcohol.
Method of the present invention is characterized in that described ammonia is liquefied ammonia or ammoniacal liquor, preferred liquefied ammonia.
Method of the present invention,, in the nickel salt complex solution that it is characterized in that preparing, ammonia/nickel=6～10mol/mol, preferred 8～9mol/mol.
Method of the present invention, in the nickel salt complex solution that it is characterized in that preparing, low mass molecule alcohol/nickel=3～6mol/mol, preferred 4～5mol/mol.
Method of the present invention, in the nickel salt complex solution that it is characterized in that preparing, natrium citricum/nickel=0.05～0.07mol/mol.
Method of the present invention is characterized in that the nickel salt complex solution joins and contains hydrazine hydrate N
2H
4H
2When carrying out reduction reaction in the sodium hydrate aqueous solution of O, N
2H
4H
2O/Ni=1～2mol/mol, preferred 1.3～1.6mol/mol.
Method of the present invention is characterized in that employed sodium hydrate aqueous solution concentration is 1～5mol/L, preferred 2～3mol/L, 50～100 ℃ of sodium hydrate aqueous solution temperature, preferred 70～90 ℃.
Method of the present invention is characterized in that sintering carries out in tube furnace, gases used is N
2-H
2Gaseous mixture, sintering temperature are 200～500 ℃, preferred 250～350 ℃.
Basic thought of the present invention is to use NH
3, at least two kinds of polynary complex systems that component is formed among the ROH, citric acid, use N
2H
4H
2O is a reducing agent, at the controlled synthesizing submicron globular powdered nickel of normal pressure liquid phase, through tube furnace N
2+ H
2Sintering obtains meeting the commodity submicron order globular powdered nickel of instructions for use.
Method of the present invention, the shortcoming that overcome prior art effectively reduces reducing agent hydrazine hydrate consumption, and the submicron order nickel powder of production has spherical structure completely, the smooth rounding of particle surface, the controlled and narrow diameter distribution of particle diameter; The brief easily control of production technology, production cost is low, and process units is simple, is easy to realize advantages such as industrialization.
Description of drawings
Fig. 1 is the process chart of method of the present invention.
Fig. 2 is product pattern SEM (SEM) the test picture among the embodiment 1.
Fig. 3 is product thing phase X-ray diffraction (XRD) spectrogram among the embodiment 1.
Fig. 4 is the SEM picture among the embodiment 2.
Fig. 5 is the X ray diffracting spectrum among the embodiment 2.
Fig. 6 is the product pattern among the embodiment 3.
Fig. 7 is the product material phase analysis figure among the embodiment 3.
Fig. 8 is the SEM test picture of embodiment 4.
Fig. 9 is the XRD figure spectrum of embodiment 4.
The specific embodiment
The method that the present invention prepares the submicron order globular powdered nickel is to be selected from its nickel content of the aqueous solution of a kind of nickel salt in nickelous sulfate, nickel chloride, nickel nitrate or their hydrate or their aqueous solution at 30～60g/L and NH
3, at least two kinds of component reaction form among the ROH, citric acid polynary complex system with contain N
2H
4H
2The sodium hydrate aqueous solution of 1～5mol/L of O is at 50～80 ℃ of normal pressures reaction, 1～2h, and product is through liquid-solid separation, and washing is used absolute ethanol washing after removing impurity in the nickel powder filter cake, negative pressure drying again in tube furnace or other forms of reactor at 200～300 ℃ of N
2+ H
2Sintering obtains commodity submicron order globular powdered nickel.
If used nickel salt raw material uses the nickel salt aqueous solution in the nickel production process then more has superiority economically, especially the nickel sulfate solution of nickel content 40～50g/L.Each raw material use amount is as follows: low mass molecule alcohol/ammonia (mol/mol)=0.4～0.6, preferred 0.5; Low mass molecule alcohol/nickel (mol/mol)=3～6; Reducing agent N
2H
4H
2O/Ni (mol/mol)=1～2, preferred 1.3～1.5.Wherein alcohol is C
1～C
3One or more of low mass molecule alcohol, preferred alcohol.
The liquid-solid separation of product can be vacuum filtration or centrifugation, can select for use continuous sedimentation formula centrifuge to be beneficial to the serialization production of factory when use is centrifugal.The washing of product is carried out in ultrasonic cleaner, uses ultrasonic wave to help to make product particle fully to disperse to be beneficial to washing.
A spot of nickel hydroxide is arranged in the dried product, is unallowed as the commodity nickel powder, therefore the nickel hydroxide in the product need be removed, and the inventor herein uses N in the tube furnace
2+ H
2The method success of sintering nickel hydroxide in the product is removed fully, and more rounding, product apparent density and the tap density increase of nickel particle surface.N
2+ H
2Sintering carries out in tube furnace, to push away the charging of boat mode, N
2+ H
2Airintake direction is in reverse to boat direct of travel, N
2+ H
2In hydrogen volume concentration be about 10%, reduction temperature is between 200～350 ℃, too high temperature can make the nickel powder particle bond influence the product decentralization, low excessively temperature deficiency so that nickel hydroxide be reduced.
The present invention produces the method for submicron order globular powdered nickel, and its advantage is that (1) technological process is simple, and production process is easy to control; (2) adopt standard device, invest lowly, the cycle of founding the factory lacks; (3) raw material hydrazine hydrate consumption is low, improves the product price competitiveness; (4) product submicron order nickel powder have completely that spherical structure, the smooth rounding of particle surface, particle diameter are controlled, narrow diameter distribution, constant product quality.
Following illustrating implemented method of the present invention, but implementation method is not limited to embodiment.
Embodiment 1
Ammonia-citric acid complex-hydrazine reduction system test operation is as follows:
The material liquid configuration: 1620g nickel sulfate hexahydrate and 120g trisodium citrate have been made into 3 liters of solution, add 4.8 liters of ammoniacal liquor again and become material liquid.
The configuration of reaction end liquid: 3.6 liters of 2N NaOH add 5.4 premium on currency and make end liquid.
To react end liquid adding reactor and be heated to 80～95 ℃, and add the 840ml hydrazine hydrate and add material liquid simultaneously, keep the pH value in the process about pH11～13, finish until reaction.The sedimentation separation mother liquor is precipitated into ultrasound reactor and handled 5 minutes, is washed to no SO then
4 2-, transfer with absolute ethyl alcohol again and wash filtration, 50～70 ℃ of following vacuum drying, take out grind product.The product chemical composition analysis sees Table 1.The product pattern is by SEM (SEM) test, and the test picture is seen Fig. 2, and picture shows that the nickel powder granularity is main between 0.8～0.9 μ m, be the more smooth spheric granules in surface.The product thing determines that by X-ray diffraction (XRD) XRD spectra is seen Fig. 3, and the diffraction maximum of sample and conformance to standard are a cube phase crystal structure, does not have other impurity peaks and occurs.
The instrumental analysis of table 1 product
| Chemical composition %) | Ca | Mg | Na | Fe | Co | Cu | Zn |
| 0.001 | 0.011 | 0.005 | 0.03 | ＜0.001 | ＜0.002 | ||
| Al | Mn | Si | Pb | Sn | C | S | O |
| ＜0.0014 | ＜0.001 | 0.0047 | ＜0.0005 | ＜0.0006 | 0.12 | 0.011 | 1.27 |
Embodiment 2
The raw material configuration: the 48g nickel sulfate hexahydrate is dissolved in 100ml distilled water, the mixed liquor of 100ml ammoniacal liquor and 40ml absolute ethyl alcohol.
Reaction end liquid configuration: 2N Na (OH)
2200ml.
To react end liquid earlier and add reactor, be warming up to 80～90 ℃, and under agitation add the 15ml hydrazine hydrate, and add whole material liquids simultaneously.Reaction finishes, discharging, and from mother liquor, precipitation is washed, vacuum drying, is pulverized and obtain nickel powder through ultrasonic processing, washing, ethanol.Yield 98.4%, product granularity 0.3～0.5 μ m, pattern is a smooth, spherical, and its SEM picture is seen Fig. 4, and X ray diffracting spectrum is seen Fig. 5.
Embodiment 3
Ammonia-ethanol complexing-hydrazine reduction system operation sequence is as follows:
The raw material configuration: the 1440g nickel sulfate hexahydrate is dissolved in 3000ml distilled water, the mixed liquor of 3000ml ammoniacal liquor and 1200ml absolute ethyl alcohol.
Reaction end liquid configuration: 2N Na (OH)
26000ml.
To react end liquid earlier and add reactor, be warming up to 80～90 ℃, and under agitation add the 450ml hydrazine hydrate, and add whole material liquids simultaneously.Reaction finishes, discharging.Separate mother liquor, precipitation is washed, vacuum drying, is pulverized and obtain nickel powder through ultrasonic processing, washing, ethanol.Yield 97.91%.The product pattern is seen Fig. 6, and the product material phase analysis is seen Fig. 7, through the XRD data computation, and Ni in the nickel powder (OH)
2Account for 3.64%, this shows, need carry out H product
2Reduction is to remove Ni (OH) wherein
2
Embodiment 4
In the most literature of preparation extra-fine nickel powder, relate to nickel powder and contain Ni (OH)
2Document seldom, but the research work in inventor herein's past finds usually to have in the nickel powder Ni (OH) more or less
2, weak Ni (OH) can appear on the XRD spectra of sample
2Diffraction maximum.
The reason that this phenomenon occurs has: the one, and reduction reaction is incomplete, the Ni of remnants in alkaline medium
2+Can be with Ni (OH)
2Precipitation is wrapped in the nickel powder surface; The 2nd, because of extra-fine nickel powder active high, in water-washing process the surface very easily oxidation generate Ni (OH)
2The thin more oxidation of film, particle is remarkable more.Therefore, the post processing of nickel powder is to eliminate Ni (OH)
2It is necessary to improve nickel powder purity.
Studied at N with embodiment 3 gained nickel powders
2+ H
2Sintering temperature is to the influence of nickel powder in the atmosphere.Test is carried out in tube furnace, and nickel powder is packed in stainless steel (1Crl8Ni9Ti) bateau, earlier at N
2Be warming up to required reduction temperature under the stream protection, be incubated 10min behind the arrival reduction temperature, begin logical N
2+ H
2Gaseous mixture, control also temperature stop heating after being respectively 250～350 ℃ of 60min, at N
2Stream protection cooling back is down taken out, and carries out SEM and XRD test.Test result is shown in table 2, and SEM test picture is seen Fig. 8, and the XRD figure spectrum is seen Fig. 9, and with embodiment 3 in Fig. 6, Fig. 7 contrast.
Table 2 embodiment 4 result of the tests
| The experiment number | Ni(OH) 2Content % | Particle diameter um | Crystallite dimension nm | Shape | Smoothness | Tap density g/cm 3 | S ％ | O ％ | C ％ | N ％ |
| Sintering not | 3.64 | 0.2～0.3 | 35.29968 | Spherical | Better | 1.315 | 0.08 | 4.4 | - | - |
| Sintering | 0 | 0.2～0.3 | 49.25283 | Spherical | Smooth | 1.527 | 0.018 | 0.85 | 0.038 | 0.05 |
By the result of the test of embodiment 4 as can be known, under 250～350 ℃, carry out Ni in the sintering nickel powder (OH)
2Complete obiteration oxygen content reduces, and crystallite dimension behind the sintering and tap density increase, and sphericity and smoothness improve.
Claims (12)
1. method for preparing the submicron order globular powdered nickel is characterized in that preparation process may further comprise the steps:
A. soluble nickel salt is dissolved in the deionized water, is mixed with the nickel salt complex solution with low mass molecule alcohol, ammonia, natrium citricum;
B. under heating condition, the nickel salt complex solution joined and contain hydrazine hydrate N
2H
4H
2Carry out reduction reaction in the sodium hydrate aqueous solution of O;
C. product obtains the nickel powder filter cake through liquid-solid separation, the impurity of slurry in washing removal filter cake;
D. the nickel powder filter cake after the washing is removed moisture with absolute ethanol washing;
E. the filter cake drying under reduced pressure of the nickel powder behind the absolute ethanol washing is removed ethanol and micro-moisture obtains dry nickel powder powder;
F. the nickel powder powder leads to nitrogen N in tube furnace
2With hydrogen H
2Gaseous mixture makes the submicron order globular powdered nickel of purity 〉=99%, surface finishing at 200～350 ℃ of following sintering.
2. method according to claim 1 is characterized in that described soluble nickel salt is selected from NiSO
4, NiCl
2, Ni (NO
3)
2In a kind of or its hydrate, the concentration that is mixed with behind the aqueous solution is nickeliferous 30～60g/L,
3. method according to claim 1 is characterized in that being mixed with that the nickel salt complex solution adopts is that the nickel sulfate solution of nickeliferous 40～50g/L of producing of nickel production process is a raw material.
4. method according to claim 1 is characterized in that described nickel salt complex solution is made up of the component that is selected from water soluble nickel salt, low mass molecule alcohol, ammonia, citric acid and water, and comprise low mass molecule alcohol at least, two kinds of components in the ammonia, citric acid.
5. method according to claim 1 is characterized in that described low mass molecule alcohol is C
1～C
3Low mass molecule alcohol, preferred alcohol.
6. method according to claim 1 is characterized in that described ammonia is liquefied ammonia or ammoniacal liquor, preferred liquefied ammonia.
7. method according to claim 1, in the nickel salt complex solution that it is characterized in that preparing, ammonia/nickel=6～10mol/mol, preferred 8～9mol/mol.
8. method according to claim 1, in the nickel salt complex solution that it is characterized in that preparing, low mass molecule alcohol/nickel=3～6mol/mol, preferred 4～5mol/mol.
9. method according to claim 1, in the nickel salt complex solution that it is characterized in that preparing, natrium citricum/nickel=0.05～0.07mol/mol.
10. method according to claim 1 is characterized in that the nickel salt complex solution joins and contains hydrazine hydrate N
2H
4H
2When carrying out reduction reaction in the sodium hydrate aqueous solution of O, N
2H
4H
2O/Ni=1～2mol/mol, preferred 1.3～1.6mol/mol.
11. method according to claim 1 is characterized in that employed sodium hydrate aqueous solution concentration is 1～5mol/L, preferred 2～3mol/L, 50～100 ℃ of sodium hydrate aqueous solution temperature, preferred 70～90 ℃.
12. method according to claim 1 is characterized in that sintering carries out in tube furnace, gases used is N
2-H
2Gaseous mixture, sintering temperature are 200～500 ℃, preferred 250～350 ℃.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102120257A (en) * | 2011-01-26 | 2011-07-13 | 宁波广博纳米材料有限公司 | Method for removing impurities on surface of ultrafine nickel powder and lubricating and modifying surface of ultrafine nickel powder |
| CN102528073A (en) * | 2012-02-16 | 2012-07-04 | 四川大学 | Non-ferromagnetic nickel powder and preparation method for same |
| CN103894621A (en) * | 2014-03-10 | 2014-07-02 | 上海交通大学 | Method for preparing Cu through reducing CuO by carbohydrate biomass |
| CN105081347A (en) * | 2015-09-07 | 2015-11-25 | 赣州市华新金属材料有限公司 | Normal-pressure production method for low-apparent-density high-purity spherical ultrafine nickel powder |
| CN105624405A (en) * | 2016-01-08 | 2016-06-01 | 湖北鄂信钻石科技股份有限公司 | Recovery method for accelerant metal ions in synthetic diamond wastewater |
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| CN1302709A (en) * | 2001-01-09 | 2001-07-11 | 山东大学 | Process for preparing nm-class Ni powder |
| CN1219617C (en) * | 2001-12-19 | 2005-09-21 | 北京有色金属研究总院 | Method of preparing nano metal nickel powder |
| CN1208163C (en) * | 2002-11-15 | 2005-06-29 | 北京科技大学 | Method for preapaing nano nickel and its alloy powder in water solution by chemical reduction method |
| CN1225336C (en) * | 2003-12-19 | 2005-11-02 | 北京科技大学 | Preparation of nano nickle powder by micro-wave activated aqueous solution reduction process |
| CN1299862C (en) * | 2004-02-19 | 2007-02-14 | 西北师范大学 | Technological method for preparating ultrafine nickel powder |
| CN1305617C (en) * | 2005-02-06 | 2007-03-21 | 金川集团有限公司 | Production method of dentritic morphology nickel powder |
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| CN102120257A (en) * | 2011-01-26 | 2011-07-13 | 宁波广博纳米材料有限公司 | Method for removing impurities on surface of ultrafine nickel powder and lubricating and modifying surface of ultrafine nickel powder |
| CN102120257B (en) * | 2011-01-26 | 2013-07-24 | 江苏博迁新材料有限公司 | Method for removing impurities on surface of ultrafine nickel powder and lubricating and modifying surface of ultrafine nickel powder |
| CN102528073A (en) * | 2012-02-16 | 2012-07-04 | 四川大学 | Non-ferromagnetic nickel powder and preparation method for same |
| CN103894621A (en) * | 2014-03-10 | 2014-07-02 | 上海交通大学 | Method for preparing Cu through reducing CuO by carbohydrate biomass |
| CN105081347A (en) * | 2015-09-07 | 2015-11-25 | 赣州市华新金属材料有限公司 | Normal-pressure production method for low-apparent-density high-purity spherical ultrafine nickel powder |
| CN105624405A (en) * | 2016-01-08 | 2016-06-01 | 湖北鄂信钻石科技股份有限公司 | Recovery method for accelerant metal ions in synthetic diamond wastewater |
| CN109575707A (en) * | 2018-11-26 | 2019-04-05 | 深圳市广田环保涂料有限公司 | Aqueous dual-component fluorine carbonaceous conductive anti-decaying paint and preparation method thereof and application method |
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| CN100509220C (en) | 2009-07-08 |
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