CN103391824A - Nickel powder production method - Google Patents
Nickel powder production method Download PDFInfo
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- CN103391824A CN103391824A CN2011800683012A CN201180068301A CN103391824A CN 103391824 A CN103391824 A CN 103391824A CN 2011800683012 A CN2011800683012 A CN 2011800683012A CN 201180068301 A CN201180068301 A CN 201180068301A CN 103391824 A CN103391824 A CN 103391824A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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Abstract
Provided is a nickel powder production method capable of efficiently producing, by a wet process, a high-quality nickel powder with a low magnesium content ratio. The nickel compound containing magnesium impurities is reduced to a metallic nickel in an alkaline solution with pH exceeding 10.5 to precipitate a nickel powder. Then, a pH adjuster containing at least one type of organic or inorganic acid is added to adjust the pH to 10.5 or less, and after allowing the magnesium impurities present on the surface of the nickel powder to migrate from the surface of the nickel powder to the solution, the nickel powder is washed with pure water. When the pH adjuster is added to reduce the pH to 10.5 or less, the pH is adjusted to 3.0-10.5.
Description
Technical field
The present invention relates to a kind of manufacture method of nickel by powder, specifically, relate to a kind of material of internal electrode as monolithic ceramic electronic components such as laminated ceramic capacitors and the manufacture method of useful nickel by powder.
Background technology
Electroconductive powder as forming conductive paste, be widely used nickel by powder, and wherein said conductive paste is used to form internal electrode of laminated ceramic capacitor.
And,, as the manufacture method of the nickel by powder that can be used for this purposes, knownly roughly can be divided into vapor phase method and liquid phase method.
The manufacture method of the nickel by powder of employing liquid phase method related to the present invention, to add the reducing agents such as hydrazine, sodium borohydride, sodium hypophosphite in the nickel compound solution that has dissolved the water-soluble nickel compounds such as nickelous sulfate, nickel chloride, nickel acetate, nickel compound is reduced, thereby obtain the method (for example, with reference to patent documentation 1) of nickel by powder.
And, in liquid phase method,, in order to promote the reduction of nickel compound to nickel by powder, usually implement the reduction operation in highly basic.
Yet, in the nickel compound of the nickel raw material as can be used for making nickel by powder, contain impurity.Particularly because magnesium is that impurity is difficult to carry out solvent extraction from nickel compound, therefore under the susceptible condition of majority, comparing magnesium with other composition is that impurity remains in nickel compound in a large number.
And to contain in a large number this magnesium be the nickel compound of impurity while making nickel by powder by damp process, reducing, and actual conditions are, the nickel by powder that namely uses the pure water washing to be restored, and also being difficult to fully remove magnesium contained in nickel by powder is impurity.
Using this nickel by powder that more magnesium is impurity that contains, form in the situation of the internal electrode of laminated ceramic capacitor for example, magnesium in internal electrode diffuses to the dielectric layer (ceramic layer) with the internal electrode adjacency, thereby have the reduced dielectric constant of dielectric layer, and as the problem of the deterioration in characteristics of the laminated ceramic capacitor of product.
Therefore, for fear of this problem, the magnesium that needs to implement for reducing nickel compound is the special processing of impurity, perhaps when the nickel by powder that the washing reduction is separated out, therefore use the methods such as a large amount of pure water wash to tackle, needing a kind of can high efficiency manufacture magnesium be the manufacture method of the nickel by powder of the low nickel by powder of the containing ratio of impurity.
Technical literature formerly
Patent documentation
Patent documentation 1: Japanese kokai publication hei 7-278619 communique
Summary of the invention
Invent problem to be solved
The invention solves the problems referred to above, its purpose is, provides a kind of and can make efficiently magnesium containing ratio low high-quality nickel by powder, manufacture method nickel by powder by damp process.
Be used for solving the method for problem
In order to address the above problem, the manufacture method of nickel by powder of the present invention, is characterized in that, possesses:
The reduction operation, the nickel compound that will comprise magnesium and be impurity surpasses in 10.5 alkaline solution and is reduced to metallic nickel and nickel by powder is separated out at pH;
PH regulates operation, in described alkaline solution after described nickel by powder being separated out to reduction in operation, add at least a pH adjusting agent that comprises in inorganic acid and organic acid, making pH is below 10.5, and to be present in the lip-deep magnesium of described nickel by powder be that impurity is transferred to solution side from the surface of described nickel by powder thereby make; And
Washing procedure, using the pure water washing to make described magnesium is that impurity is transferred to solution side described nickel by powder afterwards.
In addition, the manufacture method of nickel by powder of the present invention, is characterized in that, at described pH, regulates in operation, and to make pH be 10.5 when following when adding described pH adjusting agent, and preferably making pH is more than 3.0 and below 10.5.
In addition, can be preferably to be selected from least a in sulfuric acid, hydrochloric acid, nitric acid, phosphoric acid as the described inorganic acid of described pH adjusting agent, in addition, can be preferably and be selected from least a in formic acid, acetic acid, citric acid, oxalic acid as the described organic acid of described pH adjusting agent.
In addition, particularly preferably use the aqueous solution of hydrochloric acid or sulfuric acid as described pH adjusting agent.
The invention effect
In the manufacture method of nickel by powder of the present invention, in the alkaline solution after nickel by powder being separated out in the reduction operation that surpasses at pH under 10.5 condition, add at least a pH adjusting agent that comprises in inorganic acid and organic acid, making pH is below 10.5, to be present in the lip-deep magnesium of nickel by powder be that impurity (being mainly magnesium hydroxide) is transferred to solution side from the surface of nickel by powder thereby make, then, use pure water washing nickel by powder, therefore can remove efficiently magnesium by damp process is impurity, makes high-quality nickel by powder.
Need to prove, in the reduction operation of the manufacture method of nickel by powder of the present invention, the reducing agent as being used for the reduced nickel compound, can use the known various reducing agents such as hydrazine, sodium borohydride, sodium hypophosphite.
In addition, in the manufacture method of nickel by powder of the present invention, be more than 3.0 and below 10.5 by make pH in pH adjusting operation, thereby can avoid nickel by powder to dissolve again, making efficiently magnesium is low, the high-quality nickel by powder of containing ratio of impurity.
Need to prove, although be near 3.0 at pH, if exist through the regular hour the tendency that nickel by powder dissolves, due to the meltage of nickel by powder at short notice seldom, it is hereby ensured its practicality.
In addition, in the present invention, be selected from least a inorganic acid in sulfuric acid, hydrochloric acid, nitric acid, phosphoric acid by use, or be selected from least a organic acid in formic acid, acetic acid, citric acid, oxalic acid as pH adjusting agent, regulate thereby can carry out pH accurately, and make efficiently high-quality nickel by powder.Need to prove, according to circumstances, above-mentioned inorganic acid and organic acid can also be used in combination.
In addition, the aqueous solution by using hydrochloric acid or sulfuric acid is as above-mentioned pH adjusting agent, can be efficiently and make economically low, the high-quality nickel by powder of containing ratio that magnesium is impurity.
Description of drawings
Fig. 1 means to use uses the profile of structure of the laminated ceramic capacitor that nickel by powder produces as the conductive paste of conductive compositions, and wherein said nickel by powder is by method manufacturing of the present invention.
The specific embodiment
Below, embodiments of the invention are shown, feature of the present invention is described in detail.
Embodiment 1
[1] preparation of the nickel compound aqueous solution
As nickel compound, as shown in table 1, use and comprise in the scope of 120～250ppm the nickelous sulfate that magnesium is impurity in Mg, it is dissolved in water, prepare the nickel compound aqueous solution (in this embodiment 1, being for example the 1.5mol% aqueous solution of nickelous sulfate).
[2] preparation of the reducing agent aqueous solution
Prepare hydrazine as reducing agent, it is dissolved in water, regulate pH, prepare thus pH and be 14 the reducing agent aqueous solution (for example, the 5mol% aqueous solution of hydrazine).
, as reducing agent, except hydrazine, can also use the various reducing agents such as sodium borohydride, sodium hypophosphite.
[3] reduction operation
After the nickel compound aqueous solution that as above operates and prepare and the reducing agent aqueous solution are heated to respectively 55 ℃, both are mixed, the reduced nickel compound, the pH that obtains thus having separated out nickel by powder is about 14 slurries (synthetic liquid).
[4] pH regulates operation
The pH that obtains in the operation by above-mentioned [1], separated out nickel by powder is about in 14 synthetic liquid, adds pH adjusting agent, pH is adjusted to the value (pH=10.5) shown in the specimen coding 4～6 of table 1.
Need to prove, in this embodiment 1, use the 1mol% aqueous solution of sulfuric acid as pH adjusting agent.
In the present invention, use and give the acid of proton as pH adjusting agent.With regard to inorganic acid, can suitably use sulfuric acid, hydrochloric acid, nitric acid, phosphoric acid, with regard in organic acid, can suitably use the carboxylic acids such as formic acid, acetic acid, citric acid, oxalic acid.Wherein, more preferably use hydrochloric acid or sulfuric acid.
Need to prove, pH adjusting agent can be used separately any in them, also multiple combination can be used in addition.
The pH value of table 1, be the stability number of measuring after pH adjusting agent dropping into.
In addition, in order to compare, for with the nickel compound aqueous solution and reducing agent aqueous solution, nickel compound is reduced and nickel by powder is separated out after pH be about 14 mixed liquor (synthetic liquid) (specimen coding 1～3 of table 1), do not carry out especially pH and regulate, and in following washing procedure.
[5] washing procedure
PH is adjusted to the related nickel by powder suspension of 10.5 embodiments of the invention (synthetic liquid) (specimen coding 4～6) and does not carry out the nickel by powder suspension (synthetic liquid) (specimen coding 1～3) that pH that pH regulates is about 14 comparative example and filter, then with pure water, wash as above operating.
Wash following carrying out: supply with pure water on the nickel cake that obtains to filtering nickel by powder suspension (synthetic liquid), it is filtered by the nickel cake.And, carry out this and wash to the conductance of filtrate and reach below 10 μ S/cm.
[6] estimate
(1) amount of the Mg in nickel by powder
Nickel cake after as above operation use pure water washs is carried out drying, and by ICP(inductively coupled plasma apparatus for analyzing luminosity) to measure contained magnesium in dried nickel by powder be the amount of impurity, to be impurity count situation more than 50ppm with Mg that to be judged as the magnesium that do not eliminate be impurity with magnesium, and be evaluated as bad (*).In addition, it is that impurity is removed that Mg is judged as magnesium less than the situation of 50ppm, and is evaluated as good (zero).
It is the results are shown in table 1.
(2) the required pure water amount of washing
As mentioned above, use pure water to wash, until the conductance of filtrate reaches below 10 μ S/cm.Then,, in order to estimate the required pure water amount of washing, obtain conductance and reach the pure water amount (the washing pure water amount of every 1g nickel) that 10 μ S/cm use when following.
It is the results are shown in table 1.
[table 1]
As shown in table 1, confirmation in the situation that will not carry out that pH regulates, pH is about 14 nickel by powder suspension (synthetic liquid) directly in the specimen coding 1～3(of washing procedure comparative example), although reaching the pure water amount that 10 μ S/cm use when following, the conductance of filtrate reaches 0.15～0.30 liter of every 1g nickel by powder, but the amount of the Mg in nickel by powder still all reaches 50ppm above (in the evaluation of table 1 being *), and can't fully remove magnesium contained in nickel by powder is impurity.
On the other hand, confirmation is after the pH with nickel by powder suspension (synthetic liquid) is adjusted to 10.5, filter, wash, and meet specimen coding 4～6(embodiment of necessary condition of the present invention) situation under, can be low to moderate the washing pure water amount of 0.03 liter with every 1g nickel by powder the conductance of filtrate is reached below 10 μ S/cm, and can make magnesium in nickel by powder be impurity be reduced to take Mg less than 50ppm(in the evaluation of table 1 as zero).
Embodiment 2
As nickel compound, use the nickel chloride shown in table 2 and nickel acetate to replace the nickelous sulfate that uses in above-described embodiment 1, in addition, under the identical condition of the situation of the specimen coding 6 with above-described embodiment 1, each operation that the preparation of the enforcement nickel compound aqueous solution, the preparation of the reducing agent aqueous solution, reduction operation, pH regulate operation, washing procedure, make nickel by powder.
Need to prove,, as the nickel compound aqueous solution, respectively nickel chloride and nickel acetate are made the 1.5mol% aqueous solution and use.
And, use the method identical with the situation of above-described embodiment 1, the amount of the Mg in nickel by powder, the needed pure water amount of washing are estimated.
To the results are shown in table 2.
[table 2]
As shown in table 2, confirmation is being used nickel chloride (specimen coding 7) and is being used in nickel acetate (specimen coding 8) any one situation as nickel compound, pH by the suspension after nickel by powder is separated out (synthetic liquid) is adjusted to 10.5, and filter, wash, thereby can the conductance of filtrate be reduced to below 10 μ S/cm, and can make magnesium in nickel by powder be impurity level be reduced to take Mg less than 50ppm(in the evaluation of table 2 as zero).
Embodiment 3
As pH adjusting agent, as shown in table 3, use the aqueous solution of the sulfuric acid that uses in aqueous solution replacement above-described embodiment of hydrochloric acid, nitric acid, phosphoric acid, formic acid, acetic acid, citric acid and oxalic acid, in addition, (use nickelous sulfate as nickel compound) under the identical condition of the situation of the specimen coding 6 with above-described embodiment 1, each operation that the preparation of the enforcement nickel compound aqueous solution, the preparation of the reducing agent aqueous solution, reduction operation, pH regulate operation, washing procedure, make nickel by powder.
Need to prove,, as pH adjusting agent, use respectively the 1mol% aqueous solution of hydrochloric acid, nitric acid, phosphoric acid, formic acid, acetic acid, citric acid and oxalic acid.
And, use the method identical with the situation of above-described embodiment 1, the Mg amount in the investigation nickel by powder.
In addition, in this embodiment 3, in pH regulates operation, pH is adjusted to 10.5, and after pH is stable, at the time point through 10 seconds with through the time point of 5 minutes, to nickel by powder filter, wash, drying, obtain the nickel yield.
Need to prove, the nickel yield is the ratio of the nickel by powder that obtains with respect to the nickel 100 in the nickel compound as raw material, when the nickel yield is 95% when following, judge that the nickel yield is insufficient and be evaluated as bad (*), in addition, when yield surpasses 95%, judge yield fully and be evaluated as good (zero).
To be shown in the lump table 3 about the evaluation result of the amount of the Mg in nickel by powder and nickel yield.
[table 3]
As shown in table 3, confirmation is in the situation that use the aqueous solution of hydrochloric acid, nitric acid, phosphoric acid, formic acid, acetic acid, citric acid and oxalic acid to replace sulfuric acid to be used as pH adjusting agent, pH by the suspension after nickel by powder is separated out (synthetic liquid) is adjusted to 10.5, then filter, wash, thus can to obtain magnesium in nickel by powder be impurity take Mg less than 50ppm(in the evaluation of table 3 as zero) the few nickel by powder of impurity.
In addition, in the situation that the aqueous solution of use hydrochloric acid, phosphoric acid, formic acid, acetic acid, citric acid and oxalic acid is as pH adjusting agent (specimen coding 9,11～15), after the pH that regulates in pH regulates operation is stable, through the time point in 10 seconds and all good through the nickel yield of the time point of 5 minutes.
In addition, confirm in the situation that use the specimen coding 10 of the aqueous solution of nitric acid as pH adjusting agent, pH regulate the pH that regulates in operation stable after, good through the nickel yield of the time point in 10 seconds, but through the nickel yield of the time point of 5 minutes, decline is arranged slightly.
By this result as can be known,, in the situation that use nitric acid as pH adjusting agent, after pH regulates, need in time separate, reclaim nickel by powder,, although therefore can actually use, need to carry out process management etc. with high accuracy.
Therefore,, as the sour kind that is used for the pH adjusting,, although also can use nitric acid, more preferably use nitric acid sour kind in addition.
Embodiment 4
In this embodiment 4, change the pH setting value in pH adjusting operation, in addition, (use nickelous sulfate as nickel compound under the identical condition of the situation of the specimen coding 6 with above-described embodiment 1, and use aqueous sulfuric acid as pH adjusting agent), each operation that the preparation of the enforcement nickel compound aqueous solution, the preparation of the reducing agent aqueous solution, reduction operation, pH regulate operation, washing procedure, make nickel by powder.
And, using the method identical with the situation of above-described embodiment 1, the Mg in the investigation nickel by powder measures and washs required pure water amount.
In addition, with above-described embodiment 3 similarly, obtain pH stable after, through the time point in 10 seconds with through the nickel yield of the time point of 5 minutes.
Will to nickel by powder in the required pure water amount of Mg amount, the washing evaluation result relevant with the nickel yield be shown in the lump table 4.
[table 4]
As shown in table 4, confirm to be that pH regulates in operation pH is adjusted to specimen coding 16(comparative example 11, discontented foot necessary condition of the present invention) situation under, although the nickel yield is good, following required washing pure water quantitative change is many but the conductance of filtrate reaches 10 μ S/cm, not only the requirement of the pure water of every 1g nickel increases, and the magnesium in nickel by powder is (in the evaluation of table 4 as *) more than impurity is counted 50ppm take Mg, and can't fully remove magnesium contained in nickel by powder is impurity.
On the other hand, confirm to be that pH regulates in operation that pH is adjusted to specimen coding 17 2,7 and 3, that meet necessary condition of the present invention, 18,19(embodiment) situation under, can obtain magnesium in nickel by powder and be impurity take Mg less than 50ppm(in the evaluation of table 3 as zero) the few nickel by powder of impurity.
But, confirm to be that pH regulates in operation in the situation that pH is adjusted to 2 specimen coding 17, although pH regulate the pH that regulates in operation stable after, good through the nickel yield of the time point in 10 seconds, not enough through the nickel yield of the time points of 5 minutes.
On the other hand, be that pH regulates in operation in the situation that pH is adjusted to 7 and 3 specimen coding 18 and 19, pH regulate the pH that regulates in operation stable after, through the time point in 10 seconds and all good through the nickel yield of the time point of 5 minutes.
Can be confirmed by this result, regulate in operation at pH, can make pH according to the condition situation is 2, but from stably guaranteeing the viewpoint of nickel yield, the pH scope in pH adjusting operation is preferably the scope of pH3～10.5.
[making of laminated ceramic capacitor]
, with the nickel by powder (nickel by powder of the specimen coding 6 of table 1) of employing said method manufacturing, mixing with the organic carrier that has mixed adhesive resin and solvent (organic vehicle), make conductive paste.
Then, the stacked ceramic green sheet that has formed internal electrode pattern by being coated with this conductive paste, form duplexer.then, after duplexer is divided into single element, burn till, and via the operation that forms outer electrode, produce laminated ceramic capacitor shown in Figure 1, it is laminated ceramic capacitor 20, described laminated ceramic capacitor has following structure: in laminated ceramic element 11, across the stacked a plurality of internal electrode 13a of ceramic layer (dielectric layer) 12, 13b, and with mutual internal electrode 13a in opposite directions, 13b alternately leads to the end face 14a of the not homonymy of laminated ceramic element 11, 14b, with at this end face 14a, the outer electrode 15a of the upper formation of 14b, the structure that 15b connects.
Then, study its characteristic for the laminated ceramic capacitor of gained, results verification: with used to contain more magnesium in the past, be that the nickel of impurity is compared as the laminated ceramic capacitor that the conductive paste of conductive compositions forms internal electrode, magnesium component in internal electrode is few, fully suppressed to spread the reduced dielectric constant of the dielectric layer that causes to the ceramic layer with the internal electrode adjacency (dielectric layer) because of magnesium, can obtain the laminated ceramic capacitor of stability of characteristics.
Need to prove, nickel by powder of the present invention is not limited to the internal electrode of laminated ceramic capacitor, when it can be widely used as and make stacked rheostat, stacked LC composite component, ceramic multi-layer baseplate etc. and have the various laminated ceramic capacitor of internal electrode, form internal electrode and form electroconductive powder with conductive paste.
The present invention also is not limited to the various embodiments described above in other side, and regulate the actual conditions of operation, the washing methods of nickel by powder while implementing washing procedure and condition etc. about the kind of nickel compound and reducing agent, reduction operation and pH, can carry out various application, distortion in scope of invention.
Symbol description
11 laminated ceramic elements
12 ceramic layers (dielectric layer)
13a, 13b internal electrode
The end face of 14a, 14b laminated ceramic element
15a, 15b outer electrode
20 laminated ceramic capacitors
Claims (4)
1. the manufacture method of a nickel by powder, is characterized in that, possesses:
The reduction operation, the nickel compound that will comprise magnesium and be impurity surpasses in 10.5 alkaline solution and is reduced to metallic nickel and nickel by powder is separated out at pH;
PH regulates operation, in described alkaline solution after described nickel by powder being separated out to reduction in operation, add at least a pH adjusting agent that comprises in inorganic acid and organic acid, making pH is below 10.5, and to be present in the lip-deep magnesium of described nickel by powder be that impurity is transferred to solution side from the surface of described nickel by powder thereby make; And
Washing procedure, using the pure water washing to make described magnesium is that impurity is transferred to solution side described nickel by powder afterwards.
2. the manufacture method of nickel by powder according to claim 1, is characterized in that, at described pH, regulates in operation, and to make pH be 10.5 when following when adding described pH adjusting agent, and making pH is more than 3.0 and below 10.5.
3. the manufacture method of nickel by powder according to claim 1 and 2, it is characterized in that, can be to be selected from least a in sulfuric acid, hydrochloric acid, nitric acid, phosphoric acid as the described inorganic acid of described pH adjusting agent, in addition, can be to be selected from least a in formic acid, acetic acid, citric acid, oxalic acid as the described organic acid of described pH adjusting agent.
4. the manufacture method of the described nickel by powder of any one according to claim 1～3, is characterized in that, uses the aqueous solution of hydrochloric acid or sulfuric acid as described pH adjusting agent.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2011039553 | 2011-02-25 | ||
| JP2011-039553 | 2011-02-25 | ||
| PCT/JP2011/079780 WO2012114637A1 (en) | 2011-02-25 | 2011-12-22 | Nickel powder production method |
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| CN103391824A true CN103391824A (en) | 2013-11-13 |
| CN103391824B CN103391824B (en) | 2015-11-25 |
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| CN201180068301.2A Active CN103391824B (en) | 2011-02-25 | 2011-12-22 | The manufacture method of nickel by powder |
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| JP (1) | JP5590212B2 (en) |
| KR (1) | KR101486229B1 (en) |
| CN (1) | CN103391824B (en) |
| TW (1) | TWI449582B (en) |
| WO (1) | WO2012114637A1 (en) |
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| CN105992662A (en) * | 2014-02-17 | 2016-10-05 | 住友金属矿山株式会社 | Production method for seed crystal used in production of hydrogen-reduced nickel powder |
| CN106029269A (en) * | 2014-02-17 | 2016-10-12 | 住友金属矿山株式会社 | Nickel powder production method |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP6056532B2 (en) * | 2013-02-18 | 2017-01-11 | 株式会社村田製作所 | Method for producing nickel powder |
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- 2011-12-22 KR KR1020137022211A patent/KR101486229B1/en active IP Right Grant
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| CN106029269A (en) * | 2014-02-17 | 2016-10-12 | 住友金属矿山株式会社 | Nickel powder production method |
| CN106029269B (en) * | 2014-02-17 | 2017-12-12 | 住友金属矿山株式会社 | The manufacture method of nickel powder |
| CN105992662B (en) * | 2014-02-17 | 2018-03-02 | 住友金属矿山株式会社 | The manufacture method of crystal seed used in the manufacture of hydrogen reduction nickel powder |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103391824B (en) | 2015-11-25 |
| KR101486229B1 (en) | 2015-01-26 |
| JPWO2012114637A1 (en) | 2014-07-07 |
| TW201235132A (en) | 2012-09-01 |
| JP5590212B2 (en) | 2014-09-17 |
| TWI449582B (en) | 2014-08-21 |
| KR20130101589A (en) | 2013-09-13 |
| WO2012114637A1 (en) | 2012-08-30 |
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