CN1299866C - Method for preparing powder of fibroid nickel powder and powder of nickelous oxide - Google Patents
Method for preparing powder of fibroid nickel powder and powder of nickelous oxide Download PDFInfo
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- CN1299866C CN1299866C CNB031595774A CN03159577A CN1299866C CN 1299866 C CN1299866 C CN 1299866C CN B031595774 A CNB031595774 A CN B031595774A CN 03159577 A CN03159577 A CN 03159577A CN 1299866 C CN1299866 C CN 1299866C
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Abstract
The present invention relates to a preparing technology for special powder functional material, particularly to a method for preparing fibroid nickel powder and nickelous oxide powder. The utility model is characterized in that a sediment transition and thermal decomposition method is adopted, the precursor sediment of nickel powder or nickelous oxide powder is synthesized in a Ni-NH3-NH4-SG-C2O4-H2O system under the conditions of normal temperature and normal pressure; the precursor is thermally decomposed under the condition of an oxidizing atmosphere to obtain the fibroid nickelous oxide powder; the precursor is thermally decomposed under the condition of a non-oxidizing atmosphere to obtain the fibroid nickel powder. The oxidation preventing treatment of the surface of the fibroid nickel powder is carried out in the same suit of devices by regulating temperature and atmospheres. The whole preparing process has the advantages of safety, reliability, no poison and no pollution. The nickel powder and the nickelous oxide powder produced by the present invention are fibroid and have granularity in a nanometer level, a plurality of holes and large specific surface areas. The oxidation preventing ability of nickel powder is strong; the nickelous oxide powder can also obtain spherical nickelous oxide powder after fine ground; the powder can satisfy the multipurpose requirements.
Description
Technical field:
The present invention relates to a kind of preparation technology of extraordinary powder functional material, the preparation method of especially fibrous nickel powder and nickel protoxide powder.
Background technology:
Special Nickel Powder is owing to have great bulk effect, skin effect and shape characteristic, demonstrate many exceptional functions in fields such as catalyst, battery material, electrocondution slurry, electromagnetic wave absorbent material, micro porous filtration modulator material, powder metallurgy, as a kind of new material, more and more receive publicity, its purposes is wide, and demand is big.The Special Nickel Powder of using mainly adopts carbonyl process production at present.This method is to carry out under HTHP, and carbonyl nickel is inflammable, explosive, poisonous, contaminated environment, and the process control complexity, and product granularity can only reach micron order, and range of application is limited.Though disclose a kind of method for preparing needle-like or fibrous nickel powder among the Japan Patent JP64-28309, the presoma of this method is synthetic to be to carry out in autoclave, and its treating capacity is limited, and requires HTHP, cost height, complicated operation.
Nickel protoxide is a kind of up-and-coming important inorganic material, and it is widely used in aspects such as catalyst material, battery material, magnetic material, electronic material, glass, enamel, ceramic material.At present both at home and abroad the preparation method of nickel protoxide powder generally is that carbonate, nitrate or hydroxide with nickel are raw material, get through calcining, and also having with the nickel chloride is raw material, adds ammonium oxalate and generates nickel oxalate and precipitate, and calcines in air and gets; Impurity content is higher in the product that these methods obtain, and coarse size does not have fibrous shape characteristic again.In addition, preparation nickel protoxide powder also has some additive methods, but the overwhelming majority focuses on spherical nickel protoxide of preparation or nanometer film in these methods, and the report of fibrous nickel protoxide powder is seldom arranged.
Summary of the invention:
The objective of the invention is to overcome the weak point of said method, the preparation method of a kind of fibrous nickel powder and nickel protoxide powder is provided.This method is safe and reliable, and nontoxic pollution-free is environmentally friendly; Adopt flow process one covering device, just can obtain two kinds of superfine powdery materials as long as change the atmosphere of thermal decomposition, and be easy to realize industrialization; The nickel powder purity height of wherein preparing, granularity is little, specific area is big, non-oxidizability is strong, can satisfy the requirement of domestic and international many fields to nickel powder.
Technical scheme of the present invention: control sedimentary pattern and granularity in solution, under certain temperature and atmosphere regulation and control, the sediment of drying is carried out thermal decomposition subsequently, obtain the metal and the oxide powder thereof of required pattern and granularity.
The preparation method of fibrous nickel powder is characterized in that: at first adds in the reactor through feeding device with the soluble nickel salting liquid with by the composite precipitation agent solution of stoichiometry with oxalic acid or ammonium oxalate or sodium oxalate and ammonia and dispersant PVP formation,
Ni
2+-NH
3-NH
4 +-SG
n--C
2O
4 2--H
2O
Carry out composite precipitation in the system and transform, the control temperature is 55～85 ℃, and the pH value is 7.0～9.0, initial Ni in the feed liquid
2+Concentration is 0.4～1.2mol/L; The composite precipitation thing that obtains after then reaction being finished is through washing, filtration and the dry presoma that is nickel powder; The electric furnace that subsequently powdered nickel precursor body is placed PID to regulate, the control temperature is 350～650 ℃, and carries out thermal decomposition under the non-oxidizing atmosphere regulation and control; Nickel powder after thermal decomposition finished cools off immediately and surface anti-oxidation is handled, and obtains fibrous nickel powder, wherein the SG in the composite precipitation transformation system
N-Represent acid group Cl-, SO
4 2-, CH
3COO
-Perhaps NO
3 -
Said non-oxidizing atmosphere comprises that hydrogen, hydrogen add nitrogen, hydrogen adds inert gas or pure inert gas atmosphere among the preparation method of above-mentioned fibrous nickel powder.
Said surface anti-oxidation processing method is the carbon dioxide absorption method under the temperature adjusting among the preparation method of above-mentioned fibrous nickel powder.
The preparation method of fibrous nickel protoxide powder is characterized in that: at first adds in the reactor through feeding device with the soluble nickel salting liquid and by the composite precipitation agent solution of stoichiometry with oxalic acid or ammonium oxalate or sodium oxalate and ammonia and dispersant PVP formation,
Ni
2+-NH
3-NH
4 --SG
n--C
2O
4 2--H
2O
Carry out composite precipitation in the system and transform, the control temperature is 55～85 ℃, and pH is 7.0～9.0, initial Ni in the feed liquid
2+Concentration is 0.4～1.2mol/l; The composite precipitation thing that obtains after then reaction being finished is through washing, filtration and the dry presoma that is the nickel protoxide powder; And then the presoma of nickel protoxide is placed the electric furnace of PID adjusting, the control temperature is 350～800 ℃, and carries out thermal decomposition under the oxidizing atmosphere regulation and control; Nickel protoxide powder after thermal decomposition finished cools off naturally and promptly obtains fibrous nickel protoxide powder, the SG in the composite precipitation transformation system
N-Represent acid group Cl
-, SO
4 2-, CH
3COO
-Perhaps NO
3 -
Said oxidizing atmosphere comprises oxygen or air atmosphere among the preparation method of above-mentioned fibrous nickel protoxide powder.
Said soluble nickel salt comprises six water nickel chlorides among the preparation method of above-mentioned fibrous nickel powder and nickel protoxide powder, nickel sulfate hexahydrate, four water acetic acid nickel, six water nickel nitrate or nickel chloride solutions, nickel sulfate solution, nickel acetate solution, nickel nitrate solution.
Said compound precipitants comprises that oxalic acid, ammonium oxalate or sodium oxalate and ammonia, dispersant PVP constitute among the preparation method of above-mentioned fibrous nickel powder and nickel protoxide powder.
Said among the preparation method of above-mentioned fibrous nickel powder and nickel protoxide powder is the mol ratio 1.0～20 of nickel and compound precipitants mesoxalic acid or ammonium oxalate by stoichiometric stoichiometric coefficient.
Among the preparation method of above-mentioned fibrous nickel powder and nickel protoxide powder, the pH value is regulated with ammoniacal liquor, and control ammonia nickel mol ratio is 2.0～10.0.
The present invention has the following advantages:
1. adopt precipitation critical heat decomposition method, Ni at normal temperatures and pressures
2+-NH
3-NH
4 +-SG
N--C
2O
4 2--H
2Carry out nickel powder or nickel protoxide powder presoma building-up process in the O system, and follow-up safe and reliable, the nontoxic pollution-free of presoma thermal decomposition process, environmentally friendly.
2. it is to carry out in the same set of device under temperature and atmosphere regulation and control that the fibrous nickel powder surface anti-oxidation after thermal decomposition is finished is handled.
3. nickel powder and the nickel protoxide powder of producing according to the present invention is fibrous, granularity be nanoscale, porous, specific area greatly, wherein the nickel powder anti-aging capability is strong; And fibrous nickel protoxide powder can also obtain spherical nickel protoxide powder through after the fine grinding; These powders all can satisfy multi-purpose requirement.
Description of drawings:
Fig. 1: preparation technology's flow chart of fibrous nickel powder and nickel protoxide powder among the present invention
Fig. 2: the presoma XRD figure of fibrous nickel powder or nickel protoxide powder among the present invention
Fig. 3: the XRD figure of fibrous nickel powder among the present invention
Fig. 4: the XRD figure of fibrous nickel protoxide powder among the present invention
Fig. 5: the presoma SEM of fibrous nickel powder or nickel protoxide powder figure among the present invention
Fig. 6: the SEM of fibrous nickel powder figure among the present invention
Fig. 7: the SEM of fibrous nickel protoxide powder figure among the present invention
Fig. 8: the SEM figure after fibrous nickel protoxide powder grinds among the present invention
Fig. 1 has described the preparation process of fibrous nickel powder and nickel protoxide powder:
1. soluble nickel salting liquid and composite precipitation agent solution are added reactor respectively through feeding device, at Ni
2+-NH
3-NH
4 +-SG
N--C
2O
4 2--H
2O (SG
N-Represent acid group Cl
-, SO
4 2-, NO
3 -Or CH
3COO
-) carry out the composite precipitation conversion reaction in the system, the control temperature is 55～85 ℃, pH value is 7.0～9.0, initial Ni in the feed liquid
2+Concentration is 0.4～1.2mol/l;
2. the composite precipitation thing that obtains after reaction being finished is nickel powder or nickel protoxide powder presoma through washing, filtration and drying;
3. presoma is inserted in the electric furnace of PID adjusting, the control temperature is 350～650 ℃, carries out thermal decomposition under the non-oxidizing atmosphere regulation and control; In same set of device, cool off with surface anti-oxidation immediately and handle, obtain fibrous nickel powder to room temperature;
4. presoma is inserted in the electric furnace of PID adjusting, the control temperature is 350～800 ℃, carries out thermal decomposition under the oxidizing atmosphere regulation and control, obtains fibrous nickel protoxide powder.
After testing, its physicochemical property is as follows:
Fibrous nickel powder:
Granularity: minor axis≤100nm; Major diameter: 〉=10 μ m; Specific area: 〉=13m
2/ g;
Carbon :≤0.01wt%; Sulphur :≤0.001wt%; Iron :≤0.01wt%; Oxygen :≤0.15wt%
Fibrous nickel protoxide powder:
Granularity: minor axis≤150nm; Major diameter: 〉=10 μ m; Specific area: 〉=10m
2/ g;
Carbon :≤0.01wt%; Sulphur :≤0.001wt%; Iron :≤0.01wt%;
The specific embodiment:
Embodiment 1:
Nickel chloride solution and the composite precipitation agent solution be made up of ammonia, ammonium oxalate and dispersant PVP are added reactor through feeding device, at Ni
2+-NH
3-NH
4 +-Cl
--C
2O
4 2--H
2Carry out composite precipitation in the O system and transform, the control temperature is about 60 ℃, is about 8.5 with ammoniacal liquor regulator solution pH value, initial Ni in the feed liquid
2+Concentration is 0.8mol/l, C
2O
4 2-Concentration is 0.88mol/L.
After reaction is finished the composite precipitation thing that obtains is powdered nickel precursor body through after washing, filtration and the drying, thereafter presoma is put into and burnt boat and insert the electric furnace that PID regulates, the control temperature is about 450 ℃, and at (H
2+ N
2) atmosphere regulation and control under carry out thermal decomposition.Cool off under carbon dioxide atmosphere with surface anti-oxidation immediately after thermal decomposition is finished and handle to room temperature, the dark gray powder that take out from burn boat the back of coming out of the stove is fibrous nano level Special Nickel Powder.
Embodiment 2:
Nickel nitrate solution and the composite precipitation agent solution be made up of ammonia, ammonium oxalate and dispersant PVP are added reactor through feeding device, at Ni
2+-NH
3-NH
4 +-NO
3 --C
2O
4 2--H
2Carry out composite precipitation in the O system and transform, the control temperature is about 65 ℃, and the pH value is about 8.6, initial Ni in the feed liquid
2+Concentration is 0.6mol/L, C
2O
4 2-Concentration is 0.72mol/L.
After reaction is finished the composite precipitation thing that obtains is powdered nickel precursor body through after washing, filtration and the drying, thereafter presoma is put into and burnt boat and insert the electric furnace that PID regulates, the control temperature is about 400 ℃, and at N
2Atmosphere regulation and control carry out thermal decomposition down, under carbon dioxide atmosphere, cool off with surface anti-oxidation immediately after thermal decomposition is finished and handle to room temperature, the dark gray powder that take out from the burning boat back of coming out of the stove is fibrous nano level Special Nickel Powder.
Embodiment 3:
Nickel sulfate solution and the composite precipitation agent solution be made up of ammonia, ammonium oxalate and dispersant PVP are added reactor through feeding device, at Ni
2+-NH
3-NH
4 +--NO
3 --C
2O
4 2--H
2Carry out composite precipitation in the O system and transform, the control temperature is 70 ℃, and the pH value is 8.8, initial Ni in the feed liquid
2+Concentration is 0.5mol/l, C
2O
4 2-Concentration is 0.65mol/l.
After reaction is finished the composite precipitation thing that obtains is powdered nickel precursor body through after washing, filtration and the drying, thereafter presoma is put into and burnt boat and insert the electric furnace that PID regulates, the control temperature is 360 ℃, and at (H
2+ N
2) atmosphere regulation and control carry out thermal decomposition down, under carbon dioxide atmosphere, cool off with surface anti-oxidation immediately after thermal decomposition is finished and handle to room temperature, the dark gray powder that take out from the burning boat back of coming out of the stove is fibrous nano level Special Nickel Powder.
Embodiment 4:
Nickel acetate solution and the composite precipitation agent solution be made up of ammonia, oxalic acid and dispersant PVP are added reactor through feeding device, at Ni
2+-NH
3-NH
4 +--NO
3 --C
2O
4 2--H
2Carry out composite precipitation in the O system and transform, the control temperature is 65 ℃, and the pH value is 8.7, initial Ni in the feed liquid
2+Concentration is 0.7mol/l, C
2O
4 2-Concentration is 0.85mol/l.
After reaction is finished the composite precipitation thing that obtains is powdered nickel precursor body through after washing, filtration and the drying, thereafter presoma is put into and burnt boat and insert the electric furnace that PID regulates, the control temperature is 420 ℃, and at N
2Atmosphere regulation and control carry out thermal decomposition down, under carbon dioxide atmosphere, cool off with surface anti-oxidation immediately after thermal decomposition is finished and handle to room temperature, the dark gray powder that take out from the burning boat back of coming out of the stove is fibrous nano level Special Nickel Powder.
Embodiment 5:
Nickel chloride solution and the composite precipitation agent solution be made up of ammonia, ammonium oxalate and dispersant PVP are added reactor through feeding device, at Ni
2+-NH
3-NH
4 +--NO
3 --C
2O
4 2--H
2Carry out composite precipitation in the O system and transform, the control temperature is about 60 ℃, is about 8.5 with ammoniacal liquor regulator solution pH value, initial Ni in the feed liquid
2+Concentration is 0.8mol/l, C
2O
4 2-Concentration is 0.88mol/l.
The composite precipitation thing that obtains after reaction is finished is nickel protoxide powder presoma through after washing, filtration and the drying, presoma put into and burn boat and insert the electric furnace that PID regulates thereafter, the control temperature is 400 ℃, and under air atmosphere, carry out thermal decomposition, be cooled to room temperature after thermal decomposition is finished immediately, black or the shallow green powder that take out from burn boat the back of coming out of the stove are fibrous nickel protoxide powder.
Embodiment 6:
Nickel nitrate solution and the composite precipitation agent solution be made up of ammonia, sodium oxalate and dispersant PVP are added reactor through feeding device, at Ni
2+-NH
3-NH
4 +-NO
3 --C
2O
4 2--H
2Carry out composite precipitation in the O system and transform, the control temperature is about 65 ℃, and the pH value is about 8.6, initial Ni in the feed liquid
2+Concentration is 0.6mol/l, C
2O
4 2-Concentration is 0.72mol/l.
After reaction is finished the composite precipitation thing that obtains is nickel protoxide powder presoma through after washing, filtration and the drying, presoma put into and burn boat and insert the electric furnace that PID regulates thereafter, the control temperature is 450 ℃, under oxygen atmosphere, carry out thermal decomposition, be cooled to room temperature after thermal decomposition is finished immediately, black or the shallow green powder that take out from burn boat the back of coming out of the stove are fibrous nickel protoxide powder.
Embodiment 7:
Nickel sulfate solution and the composite precipitation agent solution be made up of ammonia, ammonium oxalate and dispersant PVP are added reactor through feeding device, at Ni
2+-NH
3-NH
4 +-NO
3 --C
2O
4 2--H
2Carry out composite precipitation in the O system and transform, the control temperature is 70 ℃, and the pH value is 8.8, initial Ni in the feed liquid
2+Concentration is 0.5mol/l, C
2O
4 2-Concentration is 0.65mol/l.
After reaction is finished the composite precipitation thing that obtains is nickel protoxide powder presoma through after washing, filtration and the drying, presoma put into and burn boat and insert the electric furnace that PID regulates thereafter, the control temperature is 500 ℃, under air atmosphere, carry out thermal decomposition, be cooled to room temperature after thermal decomposition is finished immediately, black or the shallow green powder that take out from burn boat the back of coming out of the stove are fibrous nickel protoxide powder.
Embodiment 8:
Nickel acetate solution and the composite precipitation agent solution be made up of ammonia, oxalic acid and dispersant PVP are added reactor through feeding device, at Ni
2+-NH
3-NH
4 +--NO
3 --C
2O
4 2--H
2Carry out composite precipitation in the O system and transform, the control temperature is 65 ℃, and the pH value is 8.7, initial Ni in the feed liquid
2+Concentration is 0.7mol/l, C
2O
4 2-Concentration is 0.85mol/l.
After reaction is finished the composite precipitation thing that obtains is nickel protoxide powder presoma through after washing, filtration and the drying, presoma put into and burn boat and insert the electric furnace that PID regulates thereafter, the control temperature is 650 ℃, under oxygen atmosphere, carry out thermal decomposition, be cooled to room temperature after thermal decomposition is finished immediately, black or the shallow green powder that take out from burn boat the back of coming out of the stove are fibrous nickel protoxide powder.
Claims (8)
1. the preparation method of fibrous nickel powder is characterized in that: at first the composite precipitation agent solution that soluble nickel salting liquid and oxalic acid or ammonium oxalate or sodium oxalate and ammonia and dispersant PVP are constituted adds in the reactor through feeding device by stoichiometry,
Ni
2+-NH
3-NH
4 +-SG
n--C
2O
4 2--H
2O
Carry out composite precipitation in the system and transform, the control temperature is 55～85 ℃, and the pH value is 7.0～9.0, initial Ni in the feed liquid
2+Concentration is 0.4～1.2mol/l; The composite precipitation thing that obtains after then reaction being finished is through washing, filtration and the dry presoma that is nickel powder; The electric furnace that subsequently powdered nickel precursor body is placed PID to regulate, the control temperature is 350～650 ℃, carries out thermal decomposition under the non-oxidizing atmosphere regulation and control; Nickel powder after thermal decomposition finished cools off immediately and surface anti-oxidation is handled, and obtains fibrous nickel powder, the SG in the composite precipitation transformation system
N-Represent acid group Cl
-, SO
4 2-, CH
3COO
-Perhaps NO
3 -
2. method according to claim 1 is characterized in that described non-oxidizing atmosphere is that hydrogen, hydrogen add nitrogen, hydrogen adds inert gas or pure inert gas.
3. method according to claim 1 is characterized in that described surface anti-oxidation processing method is meant the carbon dioxide absorption method under the temperature adjusting.
4. method according to claim 1 is characterized in that described is the mol ratio 1.0～2.0 of nickel and compound precipitants mesoxalic acid or ammonium oxalate by stoichiometric stoichiometric coefficient.
5. the preparation method of fibrous nickel protoxide powder is characterized in that: at first the composite precipitation agent solution with soluble nickel salting liquid and oxalic acid or ammonium oxalate or sodium oxalate and ammonia and dispersant PVP formation adds in the reactor through feeding device by stoichiometry,
Ni
2+-NH
3-NH
4 +-SG
n--C
2O
4 2--H
2O
Carry out composite precipitation in the system and transform, the control temperature is 55～85 ℃, and pH is 7.0～9.0, initial Ni in the feed liquid
2+Concentration is 0.4～1.2mol/l; The composite precipitation thing that obtains after then reaction being finished is through washing, filtration and the dry presoma that is nickel oxide powder; And then the presoma of nickel protoxide is placed the electric furnace of PID adjusting, the control temperature is 350～800 ℃, and carries out thermal decomposition under the oxidizing atmosphere regulation and control; Nickel protoxide powder after thermal decomposition finished cools off naturally and promptly obtains fibrous nickel protoxide powder, the SG in the composite precipitation transformation system
N-Represent acid group Cl
-, SO
4 2-, CH
3COO
-Perhaps NO
3 -
6. method according to claim 5 is characterized in that described oxidizing atmosphere is air atmosphere or oxygen atmosphere.
7. method according to claim 5 is characterized in that described soluble nickel salt comprises six water nickel chlorides, nickel sulfate hexahydrate, four water acetic acid nickel, six water nickel nitrate or nickel chloride solutions, nickel sulfate solution, nickel acetate solution, nickel nitrate solution.
8. method according to claim 5 is characterized in that described is the mol ratio 1.0～2.0 of nickel and compound precipitants mesoxalic acid or ammonium oxalate by stoichiometric stoichiometric coefficient.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031595774A CN1299866C (en) | 2003-09-24 | 2003-09-24 | Method for preparing powder of fibroid nickel powder and powder of nickelous oxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031595774A CN1299866C (en) | 2003-09-24 | 2003-09-24 | Method for preparing powder of fibroid nickel powder and powder of nickelous oxide |
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| Publication Number | Publication Date |
|---|---|
| CN1600480A CN1600480A (en) | 2005-03-30 |
| CN1299866C true CN1299866C (en) | 2007-02-14 |
Family
ID=34660690
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|---|---|---|---|
| CNB031595774A Expired - Fee Related CN1299866C (en) | 2003-09-24 | 2003-09-24 | Method for preparing powder of fibroid nickel powder and powder of nickelous oxide |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103498071B (en) * | 2013-09-18 | 2015-06-17 | 中南大学 | Preparation method of porous copper-nickel alloy fiber |
| CN103464784B (en) * | 2013-09-27 | 2016-01-20 | 南开大学 | A kind of preparation method of carbon loaded with nano nickel |
| CN109134235A (en) * | 2018-09-17 | 2019-01-04 | 郑州工程技术学院 | A kind of preparation method of the complicated oxalic acid nickel salt of threadiness |
| CN109369380A (en) * | 2018-11-23 | 2019-02-22 | 中南大学 | A method of fine shape is prepared by recrystallization and ties up oxalic acid nickel powder, fibrous nickel powder and fibrous nickel protoxide powder |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1423285A1 (en) * | 1987-01-09 | 1988-09-15 | Научно-исследовательский институт физико-химических проблем Белорусского государственного университета им.В.И.Ленина | Method of producing nickel powder |
| JPS6428309A (en) * | 1987-07-23 | 1989-01-30 | Sumitomo Metal Mining Co | Production of fine nickel powder |
| US5130204A (en) * | 1988-02-11 | 1992-07-14 | Jenkin William C | Randomly dispersed metal fiber mat |
| CN1074946A (en) * | 1992-01-31 | 1993-08-04 | 孟宇 | Refine the processing method of nickel oxide from the aluminium scrap nickel alloy powder |
| US5665324A (en) * | 1994-07-27 | 1997-09-09 | Taihei Chemical Industrial Co., Ltd. | Recovery of valuable substances |
-
2003
- 2003-09-24 CN CNB031595774A patent/CN1299866C/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1423285A1 (en) * | 1987-01-09 | 1988-09-15 | Научно-исследовательский институт физико-химических проблем Белорусского государственного университета им.В.И.Ленина | Method of producing nickel powder |
| JPS6428309A (en) * | 1987-07-23 | 1989-01-30 | Sumitomo Metal Mining Co | Production of fine nickel powder |
| US5130204A (en) * | 1988-02-11 | 1992-07-14 | Jenkin William C | Randomly dispersed metal fiber mat |
| CN1074946A (en) * | 1992-01-31 | 1993-08-04 | 孟宇 | Refine the processing method of nickel oxide from the aluminium scrap nickel alloy powder |
| US5665324A (en) * | 1994-07-27 | 1997-09-09 | Taihei Chemical Industrial Co., Ltd. | Recovery of valuable substances |
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