CN1206070C - Process for preparing fibrous nickel powder - Google Patents

Process for preparing fibrous nickel powder Download PDF

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Publication number
CN1206070C
CN1206070C CN 02147655 CN02147655A CN1206070C CN 1206070 C CN1206070 C CN 1206070C CN 02147655 CN02147655 CN 02147655 CN 02147655 A CN02147655 A CN 02147655A CN 1206070 C CN1206070 C CN 1206070C
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CN
China
Prior art keywords
nickel powder
nickel
present
thermal decomposition
fibrous
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Expired - Fee Related
Application number
CN 02147655
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Chinese (zh)
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CN1491762A (en
Inventor
张传福
邬建辉
黎昌俊
戴曦
湛菁
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Shenzhen Nonfemet Technology Co., Ltd.
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Central South University
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Priority to CN 02147655 priority Critical patent/CN1206070C/en
Publication of CN1491762A publication Critical patent/CN1491762A/en
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Publication of CN1206070C publication Critical patent/CN1206070C/en
Anticipated expiration legal-status Critical
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  • Powder Metallurgy (AREA)
  • Fuel Cell (AREA)

Abstract

The present invention relates to a process for preparing powder metallurgy material. The utility model is characterized in that a precipitation transition heat decomposing method is adopted, a precursor synthesizing process of preparing nickel powder in a Ni2+-NH3-NH4+-Cl-C2O42-H2O system under the conditions of normal temperature and normal pressure, and a subsequent thermal decomposition process; the present invention has the advantages of safety, reliability, no toxin and no pollution. The nickel powder produced by the present invention has the advantages of fibriform shape, nanometer-stage granularity, a plurality of holes, large specific surface area and strong oxidization preventing ability; the present invention satisfies the requirements of all kinds of use performance.

Description

A kind of preparation method of fibrous nickel powder
Technical field
The present invention is a kind of preparation technology of powdered metallurgical material.
Background technology
At present the fibrous Special Nickel Powder of using all is to adopt carbonyl process to produce, and this method is to carry out under HTHP, and carbonyl nickel is inflammable and explosive in process of production, poisonous, contaminated environment, and the product particle degree can only reach micron order, and range of application is limited.And novel Ni-Cd battery, Ni-MH battery, Li-Ion battery, particularly MCFC type fuel cell all need be with a large amount of nickel powders:
Summary of the invention
The objective of the invention is to overcome the weak point of said method, and a kind of preparation method of nickel powder is provided.This method is safe and reliable, nontoxic pollution-free; The fibrous nickel powder purity height of preparing, granularity is little, specific area is big, satisfies the demand of domestic battery performance to nickel powder, with performance and the development fuel cell technology that improves existing Ni-MH battery.
Technical scheme of the present invention is: control sedimentary pattern and granularity in solution, and under the atmosphere regulation and control, dried sediment carried out thermal decomposition subsequently and make the metal dust of required pattern and granularity.
It is characterized in that: at first the soluble nickel salting liquid is also flowed in the adding reactor, at Ni from different containers respectively through the spraying feeding device with the composite precipitation agent solution 2+-NH 3-NH 4 +-Cl --C 2O 4 2--H 2The O system is carried out the composite precipitation conversion, and 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 powdered nickel precursor body through washing, filtration and drying; And then powdered nickel precursor body is inserted in the electric furnace of PID adjusting, the control temperature is 350~600 ℃, and at (H 2+ N 2) atmosphere regulation and control under carry out thermal decomposition; Nickel powder after again thermal decomposition being finished cools off immediately with surface anti-oxidation to be handled to room temperature, is fibrous nano level Special Nickel Powder.
Advantage of the present invention and good effect compared with prior art mainly show as:
1. adopted precipitation critical heat decomposition method, Ni at normal temperatures and pressures 2+-NH 3-NH 4 +-Cl --C 2O 4 2--H 2The nickel powder that carries out in the O system prepares the presoma building-up process, and follow-up safe and reliable, the nontoxic pollution-free of presoma thermal decomposition process.
2. the surface treatment of fibrous nickel powder is that thermal decomposition and surface treatment two processes are finished in the lump: cool off immediately after thermal decomposition is finished and the atmosphere regulation and control, carry out the anti-oxidation processing of powder surface, thermal decomposition and surface treatment process are finished in same device.
3. to be fibrous, granularity be nanoscale, porous to the nickel powder produced of the present invention, specific area is big, anti-aging capability is strong, satisfies multiple serviceability requirement, as:
1. as the conductive additive of battery electrode, improve the electric conductivity of conductive frame in the electrode, replace the Co powder, do not influence electrode performance;
2. improve the structure of sintered electrode substrate, comprising the adhesion strength that increases between substrate and the sintrered nickel bisque;
3. as the binding agent of carbide alloy, can reduce its sintering temperature, shorten sintering time;
4. be applied to the surface of Cd electrode or MH negative pole, improve the recombination rate of oxygen, reduce inner pressure of battery, improve battery life, increase battery capacity in the process of overcharging:
5. directly be used as the anode of MCFC fuel cell;
6. be used for electronic shield material and catalyst etc.
Description of drawings
Be described further below in conjunction with accompanying drawing:
Fig. 1: preparation technology's flow chart of the fibrous nickel powder of the present invention
Fig. 2: presoma SEM photo
Fig. 3: Special Nickel Powder SEM photo
The specific embodiment
Fig. 1 has described the preparation process of fibrous nickel powder:
1. the soluble nickel salting liquid is also flowed from different containers respectively through the spraying feeding device with the composite precipitation agent solution and add in the reactor at Ni 2+-NH 3-NH 4 +-Cl --C 2O 4 2-H 2The O system is carried out the composite precipitation conversion, and 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;
2. the composite precipitation thing that obtains after reaction being finished is powdered nickel precursor body through washing, filtration and drying;
3. powdered nickel precursor body is inserted in the electric furnace of PID adjusting, the control temperature is 350~600 ℃, and at (H 2+ N 2) atmosphere regulation and control under carry out thermal decomposition;
4. the nickel powder after thermal decomposition being finished cools off immediately with surface anti-oxidation to be handled to room temperature, is fibrous nano level Special Nickel Powder.
After testing, its physicochemical property is as follows:
Granularity :≤50nm; Fiber major diameter: 〉=10 μ m; Specific area: 〉=13m 2/ g; Carbon :≤0.01wt%;
Sulphur :≤0.001wt%; Oxygen :≤0.15wt%; Iron :≤0.01wt%.
Its SEM photo is as shown below:
Fig. 3 compares with Fig. 2, knows and finds out that the microstructure of material nickel powder is fibrous, and the characteristic of nanoscale Special Nickel Powder and purposes are by its microstructure decision.

Claims (1)

1. the preparation method of a fibrous nickel powder is characterized in that: at first the soluble nickel salting liquid is also flowed in the adding reactor, at Ni from different containers respectively through the spraying feeding device with the composite precipitation agent solution 2+-NH 3-NH 4 +-Cl --C 2O 4 2--H 2The O system is carried out the composite precipitation conversion, and 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 powdered nickel precursor body through washing, filtration and drying; And then powdered nickel precursor body is inserted in the electric furnace of PID adjusting, the control temperature is 350~600C, and at (H 2+ N 2) atmosphere regulation and control under carry out thermal decomposition; Nickel powder after again thermal decomposition being finished cools off immediately with surface anti-oxidation to be handled to room temperature, is fibrous nano level Special Nickel Powder.
CN 02147655 2002-10-22 2002-10-22 Process for preparing fibrous nickel powder Expired - Fee Related CN1206070C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN 02147655 CN1206070C (en) 2002-10-22 2002-10-22 Process for preparing fibrous nickel powder

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN 02147655 CN1206070C (en) 2002-10-22 2002-10-22 Process for preparing fibrous nickel powder

Publications (2)

Publication Number Publication Date
CN1491762A CN1491762A (en) 2004-04-28
CN1206070C true CN1206070C (en) 2005-06-15

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Family Applications (1)

Application Number Title Priority Date Filing Date
CN 02147655 Expired - Fee Related CN1206070C (en) 2002-10-22 2002-10-22 Process for preparing fibrous nickel powder

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CN (1) CN1206070C (en)

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100387383C (en) * 2005-11-17 2008-05-14 广州有色金属研究院 Preparation method of ultra-fine nickel powder
CN101708558B (en) * 2009-11-16 2011-04-06 吉林吉恩镍业股份有限公司 Liquid phase preparation method of superfine nickel metal powder
CN103498071B (en) * 2013-09-18 2015-06-17 中南大学 Preparation method of porous copper-nickel alloy fiber
CN107093743B (en) * 2017-05-31 2019-07-12 淄博君行电源技术有限公司 The preparation method of water system power battery combined conductive agent

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Address after: No. 2, Jinxiu West Road, great industry zone, Shenzhen, Longgang

Patentee after: Shenzhen Nonfemet Technology Co., Ltd.

Address before: 24 floor, China Nonferrous building, No. 6013 Shennan Road, Futian District, Shenzhen, Che Kung Temple

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