CN101053906B - Method for manufacturing nickel nanoparticles - Google Patents
Method for manufacturing nickel nanoparticles Download PDFInfo
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- CN101053906B CN101053906B CN2007100872556A CN200710087255A CN101053906B CN 101053906 B CN101053906 B CN 101053906B CN 2007100872556 A CN2007100872556 A CN 2007100872556A CN 200710087255 A CN200710087255 A CN 200710087255A CN 101053906 B CN101053906 B CN 101053906B
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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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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- 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
- B22F2301/00—Metallic composition of the powder or its coating
- B22F2301/15—Nickel or cobalt
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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
- B22F2304/00—Physical aspects of the powder
- B22F2304/05—Submicron size particles
- B22F2304/054—Particle size between 1 and 100 nm
Abstract
The invention provides a method for preparing nickel nano-particles and the nickel nano-particles produced by reduction after forming a nickel-hydrazine complex in a reverse micro emulsion by the method. The nickel nano-particles have excellent dispersion stability and smooth surface. The invention also provides a method for preparing nickel nano-particles with narrow particle size distribution less than 100 nm especially between 10 nm and 50 nm and the nickel nano-particles prepared by the method. According to one side of the invention, the method comprises the steps of: (a) forming a solution containing nickel precursor, a surfactant and a hydrophobic solvent; (b) forming the nickel-hydrazine complex by adding hydrazine containing compound into the mixture; (c) adding a reducing agent into the mixture containing the nickel-hydrazine complex to prepare the nickel nano-particles.
Description
The cross reference of related application
The application requires korean patent application 10-2006-0032632 number from April 11st, 2006 to Korea S Department of Intellectual Property that submit to and the priority of the korean patent application submitted on August 21st, 2006 10-2006-0078618 number, and its full content is hereby expressly incorporated by reference.
Technical field
The present invention relates to make the method for nano nickel particles, relate in particular to the manufacture method of even nano nickel particles with good dispersion stabilization.
Background technology
Recently, because the microminiaturization of electricapparatus and instrument, requirement for height is with the electric component microminiaturization.Therefore, require to have the multilayer ceramic capacitor (MLCC) of high power capacity microminiaturization,, require multi-layer sheet with high density and high integration equally for circuit board.
For these MLCC and circuit board, use noble metal for example silver, platinum or palladium as inner conductive material or electrode material.But in order to reduce manufacturing cost, they are substituted by the nickel particle.Among the MLCC in these, the nickel electrode layer have with powder metallurgy in the packing density of layered product compare lower density, and it is higher than conductive layer by shrinkage degree that the sintering in solidifying produces, and this causes the high fraction defective that causes because of opening circuit of the short circuit of nickel electrode layer or wiring.In order to prevent these problems, nickel by powder should be bigger particle, has the size distribution of uniform close limit, shows good size distribution and does not lump.Therefore, need to make the method for nano nickel particles with good dispersion stabilization and uniform-dimension.But, the existing method of making nano nickel particles can not provide be lower than the 100nm size have fine dispersion stability and an inhomogeneity nano particle.
According to the existing specific embodiment, though provide a kind of under about 1000 ℃ high temperature the method by the hydrogen reduction particle, but, this method is not enough to be applied to internal electrode or internal wiring, make particle simultaneously nucleation and growth because reaction at high temperature has thermal cycle, so that the particle of producing like this have the size distribution of wide region and 1 micron bulky grain wherein.And according to another existing specific embodiment, though can have the attritive powder of submicron order according to wet reducing process manufacturing, the nano particle of making may be inhomogeneous because of many response variables like this.In addition, attritive powder rough though can manufacture the size of 200nm～1 μ m, is difficult to the single-size of manufacturing dimension less than 100nm.
Summary of the invention
The invention provides a kind of nano nickel particles of making the method for nano nickel particles and making thus, it forms by reduction form nickel-hydrazine complex compound in reverse micro emulsion after, has uniform-dimension, good dispersion stabilization and smooth surface.
And, the invention provides the method for making nano nickel particles and the nano nickel particles of making thus, this particle is less than 100nm, and preferred 10～50nm has narrow size distribution.
According to an aspect of the present invention, the present invention can provide the manufacture method of nano nickel particles, and it comprises: (a) form the aqueous solution that contains nickel precursor, surfactant and hydrophobic solvent; (b) form nickel-hydrazine complex compound by in mixture, adding the compound that contains hydrazine; And (c) by in the mixture that contains nickel-hydrazine complex compound, adding reducing agent manufacturing nano nickel particles.
The nickel precursor can be selected from by NiCl for one or more herein
2, Ni (NO
3)
2, NiSO
4, and (CH
3COO)
2The compound of the group that Ni forms.Herein, surfactant can be that one or more are selected from the compound in the group of being made up of cetrimonium bromide, lauryl sodium sulfate, sodium carboxymethylcellulose and polyvinylpyrrolidone.Surfactant can comprise one or more and be selected from cosurfactant in the group of being made up of ethanol, propyl alcohol and butanols.Herein, hydrophobic solvent can be that one or more are selected from the compound in the group of being made up of hexane, cyclohexane, heptane, octane, isooctane, decane, the tetradecane, hexadecane, toluene, dimethylbenzene, 1-octadecylene and 1-hexadecylene.
Herein, the aqueous solution of relative 100 weight portions can contain the nickel precursor of 0.1～10 weight portion.
Can contain 0.1～20 mole surfactant with respect to 1 mole of distilled water that joins in the aqueous solution herein.
The cosurfactant that further, can contain 20～40 weight portions with respect to the distilled water of 100 weight portions.
The hydrophobic solvent that can contain 30～60 weight portions herein, with respect to the aqueous solution of 100 weight portions.
And the compound that contains hydrazine can be one or more compounds that are selected from the group of being made up of hydrazine, hydrazine hydrate and hydrazine hydrochloride.According to good good embodiment, the relative 1 mole nickel ion that is provided by the nickel precursor can contain 1～10 mole the compound that contains hydrazine.
Herein, reducing agent can be a sodium borohydride.According to good good embodiment, the relative 1 mole nickel ion that is provided by the nickel precursor can contain 0.1～1 mole sodium borohydride.
And this step (a) and step (c) can be carried out under 25～60 ℃, and step (c) can be carried out 0.5～2 hour.
Can generate the single-size of 10～50nm with smooth surface and good dispersion stabilization herein.
According to a further aspect in the invention, in passing through the method for reverse micro emulsion manufactured nano nickel particles, the method that the present invention can provide a kind of manufacturing to have the nano nickel particles of uniform-dimension, fine dispersion stability and smooth surface, this method comprises: form nickel hydrazine complex compound with the compound that contains hydrazine; And reduce this nickel hydrazine complex compound.
According to a further aspect in the invention, the present invention can provide a kind of and have the method for the nano nickel particles of uniform-dimension, fine dispersion stability and smooth surface by the reverse micro emulsion manufactured, and described method comprises: form nickel hydrazine complex compound with the compound that contains hydrazine; And reduce described nickel hydrazine complex compound.
According to a further aspect in the invention, the present invention can provide the nano nickel particles that described method is made.
Herein, the present invention can provide the even nano nickel particles of 10～50nm, and it has smooth surface and good dispersion stabilization and has 90%～97% nickel content by weight.
According to a further aspect in the invention, the present invention can provide the electrically conductive ink that contains foregoing nano nickel particles.
According to a further aspect in the invention, the present invention can provide multilayer ceramic capacitor, and it comprises that foregoing nano nickel particles is as electrode material.
Description of drawings
Fig. 1 is the figure that the XRD analysis result of the nano nickel particles of making according to embodiments of the invention 1 is shown.
Fig. 2 is the figure that the TGA analysis result of the nano nickel particles of making according to embodiments of the invention 1 is shown.
Fig. 3 is the figure that the size distribution result of the metal nanoparticle of making according to embodiments of the invention 1 is shown.
Fig. 4 is the photo that the sem analysis result of the metal nanoparticle of making according to embodiments of the invention 1 is shown.
Fig. 5 is the photo that the sem analysis result of the metal nanoparticle of making according to embodiments of the invention 2 is shown.
Fig. 6 is the photo that the sem analysis result of the metal nanoparticle of making according to embodiments of the invention 3 is shown.
The specific embodiment
Below, will describe the method for nano nickel particles constructed in accordance and the nano nickel particles of making thus in detail.Before the specific embodiment of the present invention is described, at first reverse micro emulsion is described.
When by adding surfactant when making insoluble compound be dissolved in water or the hydroaropic substance, along with the insoluble compound dissolving that becomes, intermicellar swelling (expand).Herein, the micella system of expanding by dissolving is known as microemulsion.This microemulsion is thermodynamically stable system, and it has (two kinds of forms): oil-in-water (oil-in-water) form, and micella expands in water or in the hydrophily system; Water-In-Oil (water-in-oil) form, water that the reversed phase micelle dissolving is a large amount of or hydroaropic substance are so that expand in oil or hydrophobicity system.Use the method for this water in oil form to be called reverse microemulsion process.
The present invention relates to form the method for the symmetrical liquid drop of the nano-scale that generates by the surfactant of introducing by this reverse microemulsion process.
Because nano nickel particles is made by the following method, can make nano nickel particles: at first add the compound that contains hydrazine so that form complex compound in the drop slightly at this with smooth surface and fine dispersion stability, then these complex compound reduction are generated uniform nickel particle, prevent simultaneously and other nanoparticle agglomerates.For this reason, can add cosurfactant according to the specific embodiment of the present invention.
The method according to this invention comprises: (a) form the aqueous solution that contains nickel precursor, surfactant, hydrophobic solvent; (b) form nickel-hydrazine complex compound by in mixture, adding the compound that contains hydrazine; And (c) by in the mixture that contains nickel-hydrazine complex compound, adding reducing agent manufacturing nano nickel particles.
Method of the present invention is different from the existing method of making nano particle by reverse micro emulsion because at first form nickel complex, then with its reduction so that stably make the single-size of nano-scale.And by this method, the nano nickel particles that can obtain to have good dispersion stabilization is an advantage.
Below each step is described in detail.
At first, carry out the preparation of reverse micro emulsion with the nickel precursor that contains nickel ion and surfactant.Herein, any compound that contains nickel ion can be suitably as the nickel precursor and unrestricted, preferred nickel salt.The example of nickel salt can comprise NiCl
2, Ni (NO
3)
2, NiSO
4, (CH
3COO)
2Ni and composition thereof.The nickel precursor that can add 0.1～10 weight portion with respect to the whole aqueous solution of 100 weight portions.If add the nickel precursor less than 0.1 weight portion, then the amount of the nickel ion of Xing Chenging is too low so that do not have an effect; If add the nickel precursor greater than 10 weight portions, then the particle of Xing Chenging is reunited mutually, is not suitable for forming nano particle like this.Herein, it is low more that the content of nickel precursor becomes, and the nano nickel particles that can form is just more little.
As surfactant, can use cetrimonium bromide (CTAB), lauryl sodium sulfate (SDS), sodium carboxymethylcellulose (Na-CMC), polyvinylpyrrolidone (PVP) or its mixture.Except that these surfactants, cosurfactant can also be added so that stably form little micella.Cosurfactant can be that alcohol is as ethanol, propyl alcohol or butanols., can add 0.1～20 mole surfactant herein, because surfactant can wrap up water droplet fully, so this ratio is preferred with respect to 1 mole of distilled water that joins in the aqueous solution.Herein, it is high more that the content of surfactant becomes, and the nano nickel particles that can form is more little.And, can add the cosurfactant of 20～40 weight portions with respect to the distilled water of 100 weight portions.When the amount that adds during, then can not influence the stability of microemulsion less than 20 weight portions; And when the amount that adds during greater than 40 weight portions, the effect that then may the interference table surface-active agent and the stable formation of microemulsion.
Nickel precursor and surfactant are mixed with hydrophobic solvent and distilled water, wherein can be separately or mix ground and use based on the compound of hydrocarbon for example hexane, cyclohexane, heptane, octane, isooctane, decane, the tetradecane, hexadecane, toluene, dimethylbenzene, 1-octadecylene or 1-hexadecylene for hydrophobic solvent.Can add the hydrophobic solvent of 30～60 weight portions with respect to the aqueous solution of 100 weight portions, because when in this scope, adding hydrophobic solvent, can form the stable microemulsion that contains nickel ion.
What next step carried out is to form nickel complex in reverse micro emulsion.For this reason, add the compound that contains hydrazine, for example can individually or mix ground and use hydrazine, hydrazine hydrate and hydrazine hydrochloride.Herein, the structural formula of hydrazine is NH
2NH
2, the structural formula of hydrazine hydrate is NH
2NH
2NH
2O, the structural formula of hydrazine hydrochloride are NH
2NH
3Cl.Relative 1 mole of nickel ion that is provided by the nickel precursor can add 1～10 mole the compound that contains hydrazine.When the amount that adds was less than 1 mole, nickel complex can not form fully; And when the amount that adds during greater than 10 moles, aspect efficient, be unsuitable.
Then, form the nickel particle by in reverse micro emulsion, adding reducing agent.Reducing agent can be sodium borohydride (NaBH
4).The sodium borohydride that can add 0.1～1 mole herein, with respect to 1 mole of nickel ion.When the amount that adds during less than 0.1 mole, nickel-hydrazine complex compound can not fully be reduced; And, can cause extra side reaction when the amount that adds during greater than 1 mole.Because amount is inappropriate aspect efficient greater than the needed reducing agent of reduction 100% nickel.Add reducing agent afterwards through 0.5～2 hour, form nano particle less than the narrow size distribution of 100nm.When reacting less than 0.5 hour, nickel ion can not fully be reduced; And when reaction greater than 2 hours, the nickel particle is undue growth and become inhomogeneous inadequately.Be reflected under 25～60 ℃ according to the bright good good embodiment of this law and carry out, when being higher than 60 ℃, reaction takes place too fast so that not only be difficult to obtain uniform nano particle, and is difficult to control the growth of particle.
This method also comprises separates the nano nickel particles of making by these methods from reverse micro emulsion, and washing and the dry nano particle that separates like this.Separate, wash and dry can being undertaken by the conventional method that adopts in the association area, for example, centrifugal process is used for separating, and acetone and distilled water are used for washing, and vacuum drying chamber is used for drying.
The manufacture method of nano nickel particles and nano nickel particles is described in the above, more specifically is described in detail with reference to specific embodiment below.
Embodiment 1
18g nickel chloride, 18g PVP, 150g ethanol and 150g toluene are joined in the 300g distilled water, stir aqueous mixture down to make reverse micro emulsion at 40 ℃.The 40g hydrazine hydrate is joined in the reverse micro emulsion aqueous solution, it was stirred 30 minutes so that form nickel-hydrazine complex compound.NaBH with 0.04 mole
4Join in the reverse micro emulsion that contains nickel-hydrazine complex compound, it is stirred 1 hour so that make the nickel particle by reduction.By centrifugal nano nickel particles is separated from reverse micro emulsion.The nano particle that separates is being washed after 3 times with distilled water with acetone, by in vacuum drying chamber, obtaining nano nickel particles in 3 hours 50 ℃ of dryings.
Expression is tested illustrating in Fig. 1 of (XRD) result by the X-ray diffraction of the nano nickel particles that embodiment 1 makes.With reference to Fig. 1, it shows and has formed the pure nickel crystal and free from foreign meter and oxidation material.
And thermogravimetric analysis (TGA) result's of the nano nickel particles that expression is made by embodiment 1 diagram is among Fig. 2.With reference to Fig. 2, it shows that the content of organic substance is 3～10wt% of formed nano nickel particles.That is, show that nickel accounts for 90～97wt% of formed nano nickel particles.
And the size distribution of the nano nickel particles of making by embodiment 1 the results are shown among Fig. 3.With reference to Fig. 3, it shows and has generated the uniform nanoparticles with narrow size distribution.
And SEM (SEM) photo of the nano nickel particles of making by embodiment 1 is shown among Fig. 4.With reference to Fig. 4, it shows the circular single-size that has formed 30～40nm size.
Embodiment 2
18g nickel chloride, 20g CTAB, 150g ethanol and 150g toluene are joined in the 300g distilled water, stir this aqueous mixture down to make reverse micro emulsion at 40 ℃.The 30g hydrazine hydrate is joined in the reverse micro emulsion, stirred 30 minutes, so that form nickel-hydrazine complex compound.NaBH with 0.03 mole
4Join in the reverse micro emulsion that contains nickel-hydrazine complex compound, stirred 1 hour so that generate nano nickel particles by reduction.By centrifugal nano nickel particles is separated from reverse micro emulsion.The nano particle that separates is being washed after 3 times with distilled water with acetone, by in vacuum drying chamber, obtaining nano nickel particles in 3 hours 50 ℃ of dryings.
In addition, the photo of the SEM (SEM) of the nano nickel particles of making by embodiment 2 is shown among Fig. 5.With reference to Fig. 5, it shows the circular uniform nanoparticles that has formed 15～20nm size.
Embodiment 3
18g nickel chloride, 12g Na-CMC, 150g ethanol and 150g toluene are joined in the 300g distilled water, stir this aqueous mixture down to make reverse micro emulsion at 40 ℃.The 30g hydrazine hydrate is joined in the reverse micro emulsion, stirred 30 minutes, so that form nickel-hydrazine complex compound.NaBH with 0.03 mole
4Join in the reverse micro emulsion that contains nickel-hydrazine complex compound, stirred 1 hour so that generate the nickel particle by reduction.By centrifugal nano nickel particles is separated from reverse micro emulsion.The nano particle that separates is being washed after 3 times with distilled water with acetone, by in vacuum drying chamber, obtaining nano nickel particles in 3 hours 50 ℃ of dryings.
In addition, expression is shown among Fig. 6 by the photo of the SEM (SEM) of the nano nickel particles of embodiment 3 manufacturings.With reference to Fig. 6, it shows the circular uniform nanoparticles that has formed 30～40nm size.
Comparing embodiment 1
18g nickel chloride, 60g PVP, 150g ethanol and 150g toluene are joined in the 300g distilled water, stir this moisture mixture down to make reverse micro emulsion at 40 ℃.NaBH with 0.03 mole
4Join in the reverse micro emulsion that contains nickel-hydrazine complex compound, stirred 1 hour so that generate the nickel particle by reduction.By centrifugal nano nickel particles is separated from reverse micro emulsion.The nano particle that separates is being washed after 3 times with distilled water with acetone, by in vacuum drying chamber, obtaining nano nickel particles in 3 hours 50 ℃ of dryings.
Though the nano nickel particles of making by comparing embodiment 1 is 15～20nm, its shape is inhomogeneous, and highly reunites so that can not form the nano particle with suitable (granularity) distribution.
In embodiment 1, obtain the 4g nano nickel particles from the 18g nickel chloride.Be distributed to nano nickel particles in the ethanol again and centrifugation 5 minutes under 3000rpm, obtaining the nano nickel particles that 3.5g has dispersion stabilization by shifting out sediment.Obtained similar result in embodiment 2 and embodiment 3, this result determines by same analytical method.
On the contrary, in comparing embodiment 1,, find highly to reunite so that can not obtain to have the nano nickel particles of dispersion stabilization in 5 minutes by centrifugation under the 3000rpm when nano particle disperses as embodiment 1 again.
Embodiment 4～10
Except adding nickel chloride as shown in table 1 and various surfactant, other makes nano nickel particles as embodiment 1.This is for the relation between the content of the size of confirming nano nickel particles and nickel precursor and surfactant.Record manufacturing nano nickel particles size and be summarised in the table 1.
Table 1
| Nickel chloride | Surfactant | Average grain diameter (nm) | |
| Embodiment 4 | 7g | PVP 14g | 34 |
| Embodiment 5 | 7g | PVP 35g | 18 |
| Embodiment 6 | 40g | PVP 14g | 55 |
| Embodiment 7 | 2g | Na-CMC 6g | 35 |
| Embodiment 8 | 7g | Na-CMC 6g | 52 |
| Embodiment 9 | 2g | CTAB 22g | 8 |
| | 7g | CTAB 22g | 17 |
As shown in table 1, the content of nickel precursor content low more and surfactant is high more, and the size of prepared nano nickel particles is more little.
The manufacturing of electrically conductive ink
In the aqueous solution of butyl carbitol acetate and ethanol, add nano nickel particles, and it is disperseed to make the electrically conductive ink of 20cps with supersonic generator.The electrically conductive ink of making like this can be printed on the circuit board to form conducting wiring by ink-jet technology.
Multilayer ceramic capacitor
To be dispersed on the binding agent according to the nickel by powder that embodiment 1～3 makes and have full-bodied nickel slurry so that make.By serigraphy with the ceramic conductive layer of this slurry coating at barium titanate on and after the drying, in the above a plurality of layer is piled up, suppress, and under reducing condition, calcine so that make MLCC down at 1300 ℃.
In addition, on the ceramic conductive layer of above-mentioned electrically conductive ink ink jet printing and after the drying, can form internal electrode by the calcining under reducing condition at barium titanate.
Although enumerated and described specific embodiment more of the present invention, but it will be appreciated by those skilled in the art that, can change these specific embodiment under the condition that does not deviate from principle of the present invention and spirit, scope of the present invention is limited in appended claims and the equivalent thereof.
Claims (21)
1. method by reverse micro emulsion manufactured nano nickel particles, described method comprises:
(a) form the aqueous solution that contains nickel precursor, surfactant and hydrophobic solvent;
(b) form nickel-hydrazine complex compound by in the described aqueous solution, adding the compound that contains hydrazine; And
(c) by in the described aqueous solution that contains described nickel-hydrazine complex compound, adding the nano nickel particles that the reducing agent manufacturing has uniform-dimension, fine dispersion stability and smooth surface.
2. method according to claim 1, wherein, described nickel precursor is that one or more are selected from by NiCl
2, Ni (NO
3)
2, NiSO
4, and (CH
3COO)
2Compound in the group that Ni forms.
3. method according to claim 1, wherein, described surfactant is that one or more are selected from the compound in the group of being made up of cetrimonium bromide, lauryl sodium sulfate, sodium carboxymethylcellulose and polyvinylpyrrolidone.
4. method according to claim 1, wherein, described surfactant further comprises one or more and is selected from cosurfactant in the group of being made up of ethanol, propyl alcohol and butanols.
5. method according to claim 1, wherein, described hydrophobic solvent is that one or more are selected from the compound in the group of being made up of hexane, cyclohexane, heptane, octane, isooctane, decane, the tetradecane, hexadecane, toluene, dimethylbenzene, 1-octadecylene and 1-hexadecylene.
6. method according to claim 2, wherein, the described aqueous solution of relative 100 weight portions adds the described nickel precursor of 0.1～10 weight portion.
7. method according to claim 3 wherein, adds 0.1～20 mole described surfactant with respect to 1 mole of distilled water that joins in the described aqueous solution.
8. method according to claim 4 wherein, adds the described cosurfactant of 20～40 weight portions with respect to the distilled water of 100 weight portions.
9. method according to claim 5 wherein, adds the described hydrophobic solvent of 30～60 weight portions with respect to the described aqueous solution of 100 weight portions.
10. method according to claim 1, wherein, the described compound that contains hydrazine is that one or more are selected from the compound in the group of being made up of hydrazine, hydrazine hydrate and hydrazine hydrochloride.
11. method according to claim 10 wherein, adds 1～10 mole the described compound that contains hydrazine with respect to 1 mole the nickel ion that is provided by described nickel precursor.
12. method according to claim 1, wherein, described reducing agent is a sodium borohydride.
13. method according to claim 12, wherein, the relative 1 mole nickel ion that is provided by described nickel precursor adds 0.1～1 mole described sodium borohydride.
14. method according to claim 1, wherein, described step (a) and step (c) are carried out under 25～60 ℃.
15. method according to claim 1, wherein, described step (c) was carried out 0.5～2 hour.
16. method according to claim 1, wherein, described nano nickel particles has the uniform-dimension of 10～50nm, smooth surface and good dispersion stabilization.
17. nano nickel particles by the described method manufacturing of claim 1.
18. nano nickel particles according to claim 17, wherein, described nano nickel particles has the uniform-dimension of 10～50nm, smooth surface and good dispersion stabilization.
19. nano nickel particles according to claim 17, wherein, described nano nickel particles comprises 90%～97% nickel content.
20. contain the electrically conductive ink of the described nano nickel particles of claim 17.
21. comprise the multilayer ceramic capacitor of the described nano particle of claim 17, described nano particle is as electrode material.
Applications Claiming Priority (6)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR1020060032632 | 2006-04-11 | ||
| KR20060032632 | 2006-04-11 | ||
| KR10-2006-0032632 | 2006-04-11 | ||
| KR20060078618A KR100795987B1 (en) | 2006-04-11 | 2006-08-21 | Method for Manufacturing Nickel Nano Particle |
| KR10-2006-0078618 | 2006-08-21 | ||
| KR1020060078618 | 2006-08-21 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101053906A CN101053906A (en) | 2007-10-17 |
| CN101053906B true CN101053906B (en) | 2011-02-02 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2007100872556A Expired - Fee Related CN101053906B (en) | 2006-04-11 | 2007-03-21 | Method for manufacturing nickel nanoparticles |
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|---|---|
| JP (1) | JP2011122248A (en) |
| KR (1) | KR100795987B1 (en) |
| CN (1) | CN101053906B (en) |
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| CN101538692B (en) * | 2009-04-24 | 2011-01-19 | 同济大学 | Method for preparing two-dimensional Ni-based amorphous alloy nanophase material by soft and hard composite template method |
| CN102240816B (en) * | 2011-06-17 | 2013-05-22 | 华东理工大学 | Method for preparing nano nickel by taking nano spherical polyelectrolyte brush as reactor and application of nano nickel |
| CN102389983B (en) * | 2011-11-09 | 2014-04-23 | 西北大学 | Synthesis method of noble metal nano particles |
| KR20130136639A (en) | 2012-06-05 | 2013-12-13 | 삼성전기주식회사 | Nickel nano particle, manufacturing method thereof and multi-layered ceramic capacitor using the same |
| KR101445375B1 (en) | 2013-01-28 | 2014-10-07 | 순천대학교 산학협력단 | manufacturing method of nickel nano fluid using liquid phase plasma reaction |
| JP6100563B2 (en) * | 2013-03-05 | 2017-03-22 | Ｄｏｗａエレクトロニクス株式会社 | Method for producing nickel nanoparticles |
| CN103570480B (en) * | 2013-11-01 | 2015-09-30 | 南京理工大学 | The super-refinement dispersing method of a kind of water-soluble oxidizers in composite material containing energy |
| JP6338419B2 (en) * | 2014-03-28 | 2018-06-06 | 新日鉄住金化学株式会社 | Metal particle composition, bonding material, and bonding method using the same |
| JP6718687B2 (en) * | 2015-01-19 | 2020-07-08 | ユニチカ株式会社 | Ferromagnetic metal nanowire |
| US10508360B2 (en) | 2015-01-20 | 2019-12-17 | United Technologies Corporation | Multifunctional nanocellular single crystal nickel for turbine applications |
| JP6986360B2 (en) * | 2017-04-05 | 2021-12-22 | 太陽誘電株式会社 | Multilayer ceramic capacitors and their manufacturing methods |
| JP6986361B2 (en) | 2017-04-05 | 2021-12-22 | 太陽誘電株式会社 | Multilayer ceramic capacitors and their manufacturing methods |
| CN108597834A (en) * | 2018-05-02 | 2018-09-28 | 徐靖才 | A kind of preparation method of induced by magnetic field overlength one-dimentional structure magnetic material |
| CN114433864A (en) * | 2022-01-17 | 2022-05-06 | 淮安中顺环保科技有限公司 | Preparation method of nano nickel powder |
| CN115041698B (en) * | 2022-07-01 | 2023-10-13 | 武汉船用电力推进装置研究所（中国船舶重工集团公司第七一二研究所） | Preparation method of silver-palladium alloy powder |
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| KR100598082B1 (en) * | 2004-07-08 | 2006-07-07 | 한국화학연구원 | Preparation method of highly concentrated aqueous metal nano sol printable on hydrophobic substrate by inkjet method |
| KR100658492B1 (en) * | 2005-03-21 | 2006-12-15 | 주식회사 잉크테크 | Conductive inks and their methods for forming thin layers |
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| CN1127177A (en) * | 1995-01-16 | 1996-07-24 | 中国科学技术大学 | Ionization radiation chemistry redox preparation method for nm metal powder |
| CN1197708A (en) * | 1998-03-03 | 1998-11-04 | 浙江大学 | Preparation of nanometer silver-copper alloy powder |
| CN1404424A (en) * | 2000-02-18 | 2003-03-19 | 加拿大电子学粉末公司 | Nickel powder for use as electrodes in base metal electrode multilayered ceramic capacitors |
| CN1709618A (en) * | 2005-07-08 | 2005-12-21 | 昆明理工大学 | Method for preparing nano or submicron silver powder |
Also Published As
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| JP2011122248A (en) | 2011-06-23 |
| CN101053906A (en) | 2007-10-17 |
| KR20070101091A (en) | 2007-10-16 |
| KR100795987B1 (en) | 2008-01-21 |
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