CN1631589A - Wet manufacturing method for high vibrancy solid ultra micro sphere metal nickel powder - Google Patents

Wet manufacturing method for high vibrancy solid ultra micro sphere metal nickel powder Download PDF

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CN1631589A
CN1631589A CNA200410081611XA CN200410081611A CN1631589A CN 1631589 A CN1631589 A CN 1631589A CN A200410081611X A CNA200410081611X A CN A200410081611XA CN 200410081611 A CN200410081611 A CN 200410081611A CN 1631589 A CN1631589 A CN 1631589A
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nickel
nickel powder
yttrium
tap
density
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CN1265921C (en
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何国端
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KAIFEI HIGH ENERGY CHEM INDUCTRY CO Ltd CHENGDU CITY
Chengdu Chemphys Chemical Industry Co Ltd
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KAIFEI HIGH ENERGY CHEM INDUCTRY CO Ltd CHENGDU CITY
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Priority to CNB200410081611XA priority Critical patent/CN1265921C/en
Publication of CN1631589A publication Critical patent/CN1631589A/en
Priority to PCT/CN2005/001861 priority patent/WO2006069513A1/en
Priority to JP2007548671A priority patent/JP4837675B2/en
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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
    • 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
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/054—Nanosized particles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • 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
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Composite Materials (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Materials Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Powder Metallurgy (AREA)
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Abstract

The invention discloses a highly vibrated intensity super-micro sphere particle nickel powder wet production technique. The technique is adding polyhydric alcohol as shape controlling agent and lanthanon yttrium salt as core forming agent, into nickel hydroxide or nickel basic salt obtained in the reaction between bivalent nickel sulfate solution and the mixed solution of sodium hydroxide and sodium carbonic acid, and then deoxidating with hydrazine hydrate to produce high quality sphere particle nickel powder with highly vibrated intensity, narrow particle size distribution, strong oxidating resistance, fine dispersibility and particle size controllable between 0.2 to 1 mu-meter. The invention greatly increases the nickel powder vibrated intensity produced in wet method, reduces the environment pollution, and lowers the production cost. The obtained nickel powder is applicable on MLCC, powder metallurgy and magnetic material and other fields.

Description

Wet process for preparing superfine spherical metallic nickel powder with high tap density
The technical field is as follows:
the invention belongs to the technical field of powder material manufacturing, and particularly relates to a wet manufacturing method of high-tap-density ultrafine spherical metallic nickel powder.
Background art:
there are many methods for preparing metallic nickel powders. Such as: electrolytic method, carbonyl thermal decomposition method, vacuum distillation condensation method, mechanical pulverization method, slurry high pressure hydrogen reduction method, solution reduction method, and the like. These methods produce nickel powders that are either irregular in shape, too low in density, too costly to manufacture, or have a broad particle size distribution.
The preparation of nickel powder by the liquid phase reduction method is generally completed by two steps. Firstly, preparing nickel hydroxide colloid, nickel carbonate colloid or basic salt of nickel at normal temperature, belonging to liquid phase nucleation reaction; the second step is to reduce nickel hydroxide, or nickel carbonate, or basic salt of nickel by hydrazine hydrate under certain temperature condition to generate metal nickel powder, which belongs to oxidation-reduction reaction, and the basic chemical reaction of the two steps is as follows:
japanese Hei 4-74810, which is a nickel powder prepared by reducing nickel salt with hydrazine hydrate and hypophosphorous acid (or sodium borohydride) mixed reducing agent, has small density, large particle size, irregular shape and serious agglomeration.
Japanese translation of 5-51610, direct reduction of Ni (OH) with hydrazine or hydrazine compounds2The obtained nickel powder has small density, large granularity, wide powder distribution and poor process stability.
The Shanghai east China university uses hydrazine hydrate as a reducing agent, silver nitrate as a nucleating agent and PVP as a protective agent to prepare nickel powder. Mixing NiSO4The solution is directly added dropwise to a solution containing Na2CO3Adding AgNO into the mixed solution of hydrazine hydrate and PVP3The nickel powder prepared by the method has large granularity, large PVP consumption and high cost, and flaky nickel is generated in the reduction process.
Japanese Hei 8-246001 using NiCl2The nickel powder prepared by the steam gas phase reduction method has wide particle size distribution range, high production cost and great equipment investment, although the nickel powder is high-tap-density nickel powderIs easy to be produced on a large scale.
The invention content is as follows:
the invention aims to overcome the defects and provide a method which can greatly reduce the production cost and has the density similar to NiCl2The steam gas phase reduction method is comparable, and the particle size distribution range is narrow, so that the method can be easily carried outA method for preparing high-tap density ultra-micro spherical metallic nickel powder by a solution reduction method in large-scale production.
The purpose of the invention is realized by the following steps:
the invention relates to a wet method manufacturing method of high-tap-density ultrafine spherical metallic nickel powder, which comprises the steps of reacting a divalent nickel sulfate solution with a mixed solution of sodium hydroxide and sodium carbonate to generate nickel hydroxide and basic salt of nickel, adding polyalcohol serving as a morphology control agent and rare earth yttrium salt) serving as a nucleating agent, adding hydrazine or hydrazine hydrate at the pH of 8.5-12.5 and the temperature of 40-95 ℃, and reducing the basic salt of the nickel hydroxide and the basic salt of the nickel to prepare the ultrafine spherical metallic nickel powder with high tap density.
The above polyol is at least one of glycerol, butanetriol, butanetetraol and diethylene glycol, and other polyols can also be adopted, and the rare earth yttrium salt is at least one of yttrium sulfate, yttrium nitrate, yttrium chloride, yttrium acetate and yttrium formate, and other rare earth yttrium salts can also be adopted.
The addition amount of the polyhydric alcohol is 10-500% of the weight of nickel in the reaction system.
The molar concentration of the nickel sulfate solution is 0.1-2.5 mol/L.
Sodium hydroxide (NaOH) and sodium carbonate (Na) as described above2CO3) Sodium hydroxide (NaOH) and sodium carbonate (Na) in the mixed solution2CO3) The weight ratio of (0.2-10) to 1.
The amount of yttrium salt is 0.0002-0.2% of the weight of nickel in the reaction system.
The concentration of hydrazine or hydrazine hydrate is 10-80% (weight percentage concentration).
The method of the invention uses divalent nickel sulfate solution and NaOH and Na2CO3Reacting the mixed solution of (1) to produce Ni (OH)2And NiCO3·Ni(OH)2Precipitating, adding polyalcohol and rare earth yttrium salt, adding hydrazine or hydrazine hydrate under the conditions that the pH is 8.5-12.5 and the temperature is 40-95 ℃, and reducing Ni (OH)2And NiCO3·Ni(OH)2And preparing the high-tap-density ultrafine spherical metallic nickel powder with the controllable average particle size of 0.2-1.0 mu m.
The invention is characterized in that the polyol is added into a reduction system, and the agglomeration of nickel powder generated during reduction is effectively prevented by utilizing the good dispersion effect and the special adsorption property of the polyol. Meanwhile, the growth of the nickel powder particles in all directions tends to be consistent, so that the prepared nickel powder has good uniformity, smooth surface and good sphericity. Moreover, the addition of the yttrium salt nucleating agent ensures that the oxidation-reduction reaction is smoothly and stably carried out, and simultaneously weakens the magnetism of the nickel, so that the nickel powder is generated more compactly during reduction, and the high-density nickel powder is obtained.
The invention can prepare the metal nickel powder with the average particle size of 0.2-1 mu m, controllable particle size, high tap density and regular sphere, has high tap density, smooth surface, low oxidation rate (oxygen content is less than 0.5 percent), strong oxidation resistance (the oxygen content can not be increased after the metal nickel powder is placed in the air for 2 hours at the temperature of 120-140 ℃), and narrow particle size distribution range, and is shown in the following table:
average particle diameter (μm) Range of particle size distribution (μm) Tap density (g/cm3) Specific surface area (m2/g)
0.25 0.1-0.4 ≥4.0 ＜2.2
0.45 0.3-0.7 ≥4.5 ＜1.6
0.7 0.4-0.9 ≥4.6 ＜1.5
0.9 0.5-1.2 ≥4.8 ＜1.3
The invention can greatly reduce environmental pollution, has less equipment investment and low production cost, is suitable for large-scale industrial production, and the prepared nickel powder can be widely applied to industries of MLCC (multilayer ceramic chip capacitor), powder metallurgy, magnetic materials and the like.
Description of the drawings:
FIG. 1 is a diagram showing the morphology, particle size and distribution of metallic nickel powder with a diameter of 0.45 μm produced by the method of the present invention.
FIG. 2 is a diagram showing the morphology, particle size and distribution of metallic nickel powder with a diameter of 0.7 μm produced by the method of the present invention.
The specific implementation mode is as follows:
example 1:
1500L of deionized water, 19.6 kg of NaOH and 3.8 kg of Na are added into an enamel reaction kettle with the volume of 2000L2CO3Stirring to dissolve completely, adding about 19L of 1.3mol/L nickel sulfate solution while stirring to a pH value of 12, adding 15 kg of glycerol, stirring for 30 minutes, heating to 70 ℃, adding 44L of 40% (weight percentage concentration) hydrazine hydrate solution and 0.03 g of nucleating agent yttrium sulfate to perform reduction reaction for 30 minutes, and filtering, washing and vacuum dryingafter the reaction is finished to obtain the metallic nickel powder.
The nickel powder prepared by the method is observed to be regular spherical under an electron microscope 20000 times, the surface is smooth, the average particle size is 0.9 mu m, the particle size distribution range is 0.5-1.2 mu m, and the tap density is4.85g/cm3Specific surface area of 1.13m2/g。
Example 2:
1500L of deionized water, 20.8 kg of NaOH and 12 kg of Na are added into a reaction kettle with the volume of 2000L2CO3Stirring to dissolve fully, adding about 200L of 1.4mol/L nickel sulfate solution while stirring to pH value of 11.8, adding 17 kg of butanetriol, stirring for 20 min, heating to 80 ℃, adding 34L of 60% (weight percentage concentration) hydrazine hydrate and 0.05 g of nucleating agent yttrium chloride for reduction, reacting for 30 min, filtering, washing, filtering, and drying,Vacuum drying to obtain the metallic nickel powder.
The nickel powder prepared by the method is observed to be regular spherical under an electron microscope 20000 times, the surface is smooth, the average particle size is 0.8 mu m, the particle size distribution range is 0.5-1.2 mu m, and the tap density is 4.7g/cm3Specific surface area of 1.21m2/g。
Example 3:
1500L of deionized water, 24.5 kg of NaOH and 25.2 kg of Na are added into a reaction kettle with the volume of 2000L2CO3After being sufficiently dissolved by stirring, 0.05 g of yttrium sulfate is added into about 200L1.7mol/L of nickel sulfate solution, and then the nickel sulfate solution is added into NaOH and Na while stirring2CO3Adding 10 kg of diglycol into the mixed solution until the pH value is 11.7, continuing stirring for 20 minutes, then heating to 90 ℃, adding 60L of 40% (weight percentage concentration) hydrazine hydrate for reduction, reacting for 30 minutes, filtering, washing and drying in vacuum to obtain the metallic nickel powder (see figure 2) with the average particle size of 0.7 mu m, good sphericity, smooth surface, narrow particle size distribution and tap density of 4.65g/cm3。
Example 4:
1500L of deionized water, 25 kg of NaOH and 33.1 kg of Na are added into a reaction kettle with the volume of 2000L2CO3Stirring to dissolve the mixture fully, adding 1.8mol/L nickel sulfate solution with stirring, adding about 200L of nickel sulfate solution with pH value of 11.5, adding 15 kg of erythritol, stirring for 20 minutes, heating to 90 ℃, adding 32L of 80% (weight percentage concentration) hydrazine hydrate and 0.07 g of yttrium sulfate, reducing, and finishing the reaction for 20 minutes. Filtering, washing, and vacuum drying to obtain smooth spherical metallic nickel powder with average particle diameter of 0.45 μm (see figure 1) and tap density of 4.6g/cm3The particle size distribution range is 0.3-0.7 μm, the specific surface area is 1.48m2/g。
Example 5:
1500L of deionized water, 28 kg of NaOH and 17.4 kg of Na are added into a reaction kettle with the volume of 2000L2CO3After fully dissolving, 2.0mol/L nickel sulfate solution is added while stirringAbout 200L to pH 11.4, and then 30 kgAnd (3) continuously stirring the glycerol for 20 minutes, then heating to 80 ℃, adding 40 percent (weight percentage concentration) of hydrazine hydrate 65L and 0.08 yttrium sulfate for reduction, and finishing the reaction after 20 minutes. Filtering, washing and vacuum drying to obtain the metal nickel powder with the average particle size of 0.45 mu m, good sphericity, smooth surface and tap density of 4.5g/cm3The particle size distribution range is 0.3-0.9 μm, the specific surface area is 1.45m2/g。
Example 6:
1400L of deionized water, 42 kg of glycerol, 32.4 kg of NaOH and 84.4 kg of Na are added into a reaction kettle with the volume of 2000L2CO3After the nickel sulfate is fully dissolved, 2.3mol/L nickel sulfate solution of about 206L is added while stirring to the pH value of 11, the temperature is raised to 90 ℃ after stirring for 20 minutes, 60 percent (weight percentage concentration) of hydrazine hydrate 56L and 0.1 g of yttrium sulfate are added for reduction, and the reaction is finished after 20 minutes. Filtering, washing, and vacuum drying to obtain metal nickel powder with average particle diameter of 0.25 μm, which has good sphericity, smooth surface, and tap density of 4.1g/cm under observation of 20000 times electron microscope3The particle size distribution range is 0.1-0.4 μm, the specific surface area is 1.84m2/g。
The above embodiments are further illustrative of the present invention, but it should not be construed that the scope of the above subject matter is limited to the above embodiments. All the technologies realized based on the above contents belong to the scope of the present invention.

Claims (7)

1. The wet method for preparing the high-tap-density ultrafine spherical metallic nickel powder is characterized in that a divalent nickel sulfate solution reacts with a mixed solution of sodium hydroxide and sodium carbonate to generate nickel hydroxide and basic salt of nickel, polyhydric alcohol is added to serve as a morphology control agent, rare earth yttrium salt is added to serve as a nucleating agent, hydrazine or hydrazine hydrate is added under the conditions that the pH value is 8.5-12.5 and the temperature is 40-95 ℃, and the basic salt of the nickel hydroxide and the nickel is reduced to prepare the high-tap-density ultrafine spherical metallic nickel powder.
2. The wet process for preparing nickel powder with high tap density and ultra-fine spherical shape according to claim 1, wherein the polyol is at least one of glycerol, butanetriol, butanetetraol and diethylene glycol, and the yttrium salt is at least one of yttrium sulfate, yttrium nitrate, yttrium chloride, yttrium acetate and yttrium formate.
3. The wet process for producing nickel powder having a high tap density and ultrafine spherical shape according to claim 1 or 2, wherein the amount of the polyol added is 10 to 500% by weight based on the weight of nickel in the reaction system.
4. The wet process for producing high-tap-density ultrafine spherical metallic nickel powder according to claim 1 or 2, wherein the molar concentration of the nickel sulfate solution is 0.1 to 2.5.
5. The wet process for producing high-tap-density ultrafine spherical metallic nickel powder according to claim 1 or 2, wherein the weight ratio of sodium hydroxide to sodium carbonate in the mixed solution of sodium hydroxide and sodium carbonate is (0.2 to 10) to 1.
6. The wet process for preparing nickel powder having high tap density and ultrafine spherical shape according to claim 1 or 2, wherein the amount of yttrium salt is 0.0002 to 0.2% by weight based on the weight of nickel in the reaction system.
7. The wet process for producing high-tap-density ultrafine spherical metallic nickel powder according to claim 1 or 2, wherein the hydrazine or the hydrazine hydrate is contained in an amount of 10 to 80% by weight.
CNB200410081611XA 2004-12-28 2004-12-28 Wet manufacturing method for high vibrancy solid ultra micro sphere metal nickel powder Active CN1265921C (en)

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CNB200410081611XA CN1265921C (en) 2004-12-28 2004-12-28 Wet manufacturing method for high vibrancy solid ultra micro sphere metal nickel powder
PCT/CN2005/001861 WO2006069513A1 (en) 2004-12-28 2005-11-07 Spherical ultrafine nickel powder with high tap density and its wet processes preparing mothod
JP2007548671A JP4837675B2 (en) 2004-12-28 2005-11-07 High tap density ultrafine spherical metallic nickel powder and wet manufacturing method thereof

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CN100436008C (en) * 2007-04-10 2008-11-26 北京科技大学 Chemical production of metal nickel nano-line
CN100444433C (en) * 2006-12-27 2008-12-17 河南师范大学 Method of nickel hydroxide surface metallization
US7601199B2 (en) * 2006-01-19 2009-10-13 Gm Global Technology Operations, Inc. Ni and Ni/NiO core-shell nanoparticles
CN102423808A (en) * 2011-12-14 2012-04-25 天津工业大学 Quick high concentration synthesizing method of silver nanometer line
CN106270545A (en) * 2015-06-12 2017-01-04 中国振华集团云科电子有限公司 A kind of high-tap density noble metal raw powder's production technology

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JP6834235B2 (en) * 2016-08-10 2021-02-24 住友金属鉱山株式会社 Manufacturing method of nickel hydroxide particles
JP6772646B2 (en) * 2016-08-10 2020-10-21 住友金属鉱山株式会社 Nickel oxide fine powder and its manufacturing method
CN112481501B (en) * 2020-11-12 2022-09-27 阳谷祥光铜业有限公司 Method for preparing nickel powder by using decoppering final solution
CN114203326B (en) * 2021-12-13 2024-04-30 中国核动力研究设计院 Graphene-encapsulated ultrathin nickel-63 radiation source film and preparation method and application thereof
CN114433864B (en) * 2022-01-17 2024-06-18 淮安中顺环保科技有限公司 Preparation method of nano nickel powder

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JPH0474810A (en) * 1990-07-18 1992-03-10 Agency Of Ind Science & Technol Manufacture of nickel base metal fine powder
JP3197454B2 (en) * 1995-03-10 2001-08-13 川崎製鉄株式会社 Ultra fine nickel powder for multilayer ceramic capacitors
JP2991700B2 (en) * 1997-09-11 1999-12-20 三井金属鉱業株式会社 Method for producing nickel fine powder
JP3635451B2 (en) * 1998-09-11 2005-04-06 株式会社村田製作所 Metal powder, method for producing the same, and conductive paste
JP4081987B2 (en) * 2000-05-30 2008-04-30 株式会社村田製作所 Metal powder manufacturing method, metal powder, conductive paste using the same, and multilayer ceramic electronic component using the same
JP4244583B2 (en) * 2002-07-29 2009-03-25 株式会社村田製作所 Conductive paste, method for producing conductive paste, and multilayer ceramic electronic component
JP4059035B2 (en) * 2002-08-20 2008-03-12 株式会社村田製作所 Nickel powder manufacturing method, nickel powder, conductive paste, and multilayer ceramic electronic component

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7601199B2 (en) * 2006-01-19 2009-10-13 Gm Global Technology Operations, Inc. Ni and Ni/NiO core-shell nanoparticles
CN101104206B (en) * 2006-01-19 2012-03-21 通用汽车环球科技运作公司 Ni and Ni/NiO core-shell nanoparticles
CN100444433C (en) * 2006-12-27 2008-12-17 河南师范大学 Method of nickel hydroxide surface metallization
CN100436008C (en) * 2007-04-10 2008-11-26 北京科技大学 Chemical production of metal nickel nano-line
CN102423808A (en) * 2011-12-14 2012-04-25 天津工业大学 Quick high concentration synthesizing method of silver nanometer line
CN106270545A (en) * 2015-06-12 2017-01-04 中国振华集团云科电子有限公司 A kind of high-tap density noble metal raw powder's production technology

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CN1265921C (en) 2006-07-26

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