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Nickel nanoparticles / Samsung Electro-mechanics Co., Ltd.




Title: Nickel nanoparticles.
Abstract: Nickel nanoparticles including an aqueous solution including a nickel precursor, a surfactant, a hydrophobic solvent, and distilled water, the hydrophobic solvent being one or more compounds selected from the group consisting of hexane, cyclohexane, heptane, octane, isooctane, decane, tetradecane, hexadecane, toluene, xylene, 1-octadecene, and 1-hexadecene; a compound including hydrazine which is added to the aqueous solution to form a nickel-hydrazine complex; and a reducing agent added to the compound including the nickel-hydrazine complex. ...


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USPTO Applicaton #: #20100078604
Inventors: Young-il Lee, Jae-woo Joung, Kwi-jong Lee


The Patent Description & Claims data below is from USPTO Patent Application 20100078604, Nickel nanoparticles.

CROSS-REFERENCE TO RELATED APPLICATIONS

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This application is a divisional and claims priority to U.S. application Ser. No. 11/708,508, filed Feb. 21, 2007, which in turn claims the benefit of Korean Patent Applications No. 10-2006-0032632 filed on Apr. 11, 2006 and No. 10-2006-0078618 filed on Aug. 21, 2006, with the Korea Intellectual Property Office, the contents of which are incorporated here by reference in their entirety.

BACKGROUND

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1. Field

The present invention relates to a nickel nanoparticles, and in particular, to uniform nickel nanoparticles having superior dispersion stability.

2. Description of the Related Art

Recently, according to the miniaturization of electrical machines and apparatus, it is highly required for electrical parts to be miniaturized. Accordingly, in case of Multi-Layer Ceramic Condenser (MLCC), the miniaturized that have high capacity are required, also in case of circuit boards, multilayer boards with high density and high-integration are required.

As to these MLCC and circuit board, precious metals such as silver, platinum or palladium have been used for inside conducting material or the electrode material. However, they are substituted with nickel particles for reducing production cost. In MLCC among these, a nickel electrode layer has lower density in comparison with the packing density of the molding product in the powder metallurgy and has higher degree of contraction according to sintering in curing than conducting layer, which cause high defective rate due to short of the nickel electrode layer or disconnection of wiring. To prevent these problems, the nickel powder should be fine particles, have a uniform narrow range of particle distribution, and exhibit superior particle distribution without agglomeration. For this, a method of manufacturing nickel nanoparticles having superior dispersion stability and uniform size is needed. However, the existing methods for manufacturing nickel nanoparticles could not provide nanoparticles having superior dispersion stability and uniformity of below 100 nm size.

According to an existing embodiment, though a method where particles are reduced by hydrogen under at a high temperature of about 1000° C. is provided, this method is not enough to be applied to internal electrode or internal wiring since its thermal history under a high temperature forces simultaneous generation and growth of particle so that the particles thus produced have a wide range of particle distribution and large particles of 1 micron among them. Further, according to another existing embodiment, though manufacturing of the micropowder having sub-micron level according to the wet reduction method is possible, the nanoparticles thus produced may be unequal due to plentiful variables of the reaction. Also the surface of the micropowder is not smooth, and though they may be produced in 200 nm-1 μm size, it is difficult to produce uniform particles of below 100 nm size.

SUMMARY

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As a solution to the foregoing problems, an aspect of the invention provides a method of manufacturing nickel nanoparticles and nickel nanoparticles thus produced, having uniform size, superior dispersion stability and smooth surface, by reducing after forming a nickel-hydrazine complex in a reverse microemulsion.

Further, another aspect of the invention provides a method of manufacturing nickel nanoparticles and nickel nanoparticles thus produced, having a narrow dispersion stability of below 100 nm, preferably 10-50 nm.

Additional aspects and advantages of the present general inventive concept will be set forth in part in the description which follows and, in part, will be apparent from the description, or may be learned by practice of the general inventive concept.

According to an embodiment of the invention, the invention may provide a production method of nickel nanoparticles including: forming an aqueous solution including nickel precursor, surfactant, and hydrophobic solvent; forming nickel-hydrazine complex by adding a reducing agent that includes hydrazine to the mixture; and producing nickel nanoparticles by adding a reducing agent to the mixture that includes the nickel-hydrazine complex.

Here the nickel precursor may be one or more compounds selected from the group consisting of NiCl2, Ni(NO3)2, NiSO4, and (CH3COO)2Ni. Here, the surfactant may be one or more compounds selected from the group consisting of cetyltrimethylammonium bromide, sodium dodecyl sulfate, sodium carboxymethyl cellulose, and polyvinylpyrrolidone. The surfactant may further include one or more cosurfactants selected from the group consisting of ethanol, propanol, and butanol. Here, the hydrophobic solvent may be one or more compounds selected from the group consisting of hexane, cyclohexane, heptane, octane, isooctane, decane, tetradecane, hexadecane, toluene, xylene, 1-octadecene, and 1-hexadecene.

Here, the nickel precursor may be included by 0.1-10 parts by weight with respect to 100 parts by weight of the aqueous solution.

Here, the surfactant may be included by 0.1-20 mole with respect to 1 mole of the distilled water that is added to the aqueous solution.

Further, the cosurfactant may be included by 20-40 part by weight with respect to 100 parts by weight of the distilled water.

Here, the hydrophobic solvent may be included by 30-60 parts by weight with respect to 100 parts by weight of the aqueous solution.

Further, the compound including the hydrazine may be one or more compounds selected from the group consisting of hydrazine, hydrazine hydrate, and hydrazine hydrochloride. According to an embodiment, the compound including the hydrazine may be included by 1-10 moles with respect to 1 mole of nickel ions supplied by the nickel precursor.

Here, the reducing agent may be sodium borohydride. According to an embodiment, the sodium borohydride may be included by 0.1-1 mole with respect to 1 mole of nickel ion supplied by the nickel precursor.

Further, the step of forming the aqueous solution to the step of producing nickel nanoparticles may be performed at 25-60° C., and the step of producing nickel nanoparticles may be performed for 0.5-2 hours.

Here, 10-50 nm of uniform particles having smooth surface and superior dispersion stability may be generated.

According to another aspect of the invention, in a manufacturing method of nickel nanoparticles by reverse microemulsion method, the invention may provide a method of producing nickel nanoparticles having uniform size, superior dispersion stability and smooth surface, the method includes: forming nickel hydrazine complex with a compound having hydrazine; and reducing this nickel hydrazine complex.

According to another aspect of the invention, the invention may provide nickel nanoparticles manufactured by the method set forth above.

Here, the invention may provide 10-50 nm of uniform nickel nanoparticles, having smooth surface and superior dispersion stability and including 90-97 weight % of nickel content.

According to another aspect of the invention, the invention may provide conductive ink including nickel nanoparticles set forth above.

According to another aspect of the invention, the invention may provide multi layer ceramic condenser including nickel nanoparticles set forth above as an electrode material.

BRIEF DESCRIPTION OF THE DRAWINGS

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These and/or other aspects and advantages of the present general inventive concept will become apparent and more readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings of which:

FIG. 1 is a graph representing the result of XRD analysis for the nickel nanoparticles produced according to an embodiment;

FIG. 2 is a graph representing the result of TGA analysis for the nickel nanoparticles produced according to an embodiment;

FIG. 3 is a graph representing the result of particle distribution of the metal nanoparticles produced according to embodiments;




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stats Patent Info
Application #
US 20100078604 A1
Publish Date
04/01/2010
Document #
File Date
12/31/1969
USPTO Class
Other USPTO Classes
International Class
/
Drawings
0


Hydrazine

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Samsung Electro-mechanics Co., Ltd.


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Compositions   Electrically Conductive Or Emissive Compositions   Metal Compound Containing   Iron, Cobalt, Or Nickel Compound  

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20100401|20100078604|nickel nanoparticles|Nickel nanoparticles including an aqueous solution including a nickel precursor, a surfactant, a hydrophobic solvent, and distilled water, the hydrophobic solvent being one or more compounds selected from the group consisting of hexane, cyclohexane, heptane, octane, isooctane, decane, tetradecane, hexadecane, toluene, xylene, 1-octadecene, and 1-hexadecene; a compound including hydrazine which |Samsung-Electro-mechanics-Co-Ltd
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