CN102672168A - Preparation method for core-shell structural nickel-silver bimetallic powder - Google Patents
Preparation method for core-shell structural nickel-silver bimetallic powder Download PDFInfo
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- CN102672168A CN102672168A CN2012100036220A CN201210003622A CN102672168A CN 102672168 A CN102672168 A CN 102672168A CN 2012100036220 A CN2012100036220 A CN 2012100036220A CN 201210003622 A CN201210003622 A CN 201210003622A CN 102672168 A CN102672168 A CN 102672168A
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Abstract
The invention relates to the technical field of the preparation of metal powder materials and particularly discloses a preparation method for core-shell structural nickel-silver bimetallic powder. The preparation method comprises the following steps of: adding nickel powder and a dispersing agent in an ethanol-water mixed solvent, and stirring to obtain a nickel powder dispersing solution; preparing hydrazine hydrate solution with the hydrazine hydrate concentration of 2.5 mol/L, and adjusting the pH value of the hydrazine hydrate solution to more than 10 to obtain a reducing agent solution; mixing the nickel powder dispersing solution with the reducing agent solution to obtain a reaction solution A; dropwise adding an ammonia-silver solution in the reaction solution A and reacting for 70-100 minutes to obtain turbid liquid; performing centrifugal separation, washing and vacuum-drying the obtained solid to obtain the core-shell structural nickel-silver bimetallic powder. The preparation method provided by the invention has simple process; the obtained core-shell structural nickel-silver bimetallic powder has the advantages of controllable thickness of a silver coating layer, narrow distribution of grain diameter, good dispersing property and high vibrating density.
Description
Technical field
The present invention relates to the metal powder material preparing technical field, be specifically related to the preparation method of a kind of nucleocapsid structure nickel-silver bimetal powder.
Background technology
Metal dust is a kind of important raw material, both can directly disperse to use, and also can and sinter block materials into its press forming, can also process film material etc.With hyundai electronics industry is example, and multilayer ceramic capacitor (Multilayer ceramic capacitors is called for short MLCC) has become the main product of capacitor industry, is widely used in communication, computer and consumer electronics product.One of main developing direction of MLCC shows as the lowpriced metallization of electrode, promptly adopts the base metal of low price to replace noble metals such as expensive palladium, silver to reduce cost, and interior electrode can be saved 2～5 times cost behind lowpriced metallization.Nickel is cheap and easy to get, has high melt point and good electrical conductivity, and high frequency stability is better than gold, silver, and is compatible with most of scolders, and not diffusion or reaction in ceramic dielectric when sintering to the not influence of ceramic dielectric performance, is comparatively desirable inner electrode.But nickel powder at high temperature is prone to oxidation generates the non-conductor oxide-film, therefore, modification is carried out on the nickel powder surface, and improving its high-temperature oxidation resistance is to solve one of electrode base metal important approach.
To the problem of oxidation of nickel powder in MLCC electrode and the electromagnetic shielding material, in order to improve the high-temperature oxidation resistance of nickel powder, the method for existing at present employing nickel powder electroplate improves the report of the antioxygenic property of nickel powder.Silver-plated nickel powder not only can improve the antioxygenic property of nickel powder, and can not influence its prerequisite decline low electrode of leading performance, the cost of electric slurry.The technology that nickel powder surface clad silver adopts at present mainly is the electroless plating technology of nickel powder, and is at first in the nickel powder Electroless copper, then silver-plated through copper and silver ion displacement reaction.This method complex process need repeatedly be washed, filtered, and is unfavorable for the reduction of the stable and production cost of properties of product.
Summary of the invention
The object of the present invention is to provide the preparation method of a kind of nucleocapsid structure nickel-silver bimetal powder.
In order to realize above purpose, the technical scheme that the present invention adopted is: the preparation method of a kind of nucleocapsid structure nickel-silver bimetal powder may further comprise the steps:
(1) nickel powder, dispersant are joined in the ethanol-water mixed solvent, place water-bath then, keeping bath temperature is 50 ℃; Stir; Make the nickel powder dispersion soln, the concentration of nickel powder is 25.0g/l in the said nickel powder dispersion soln, and the concentration of dispersant is 8.33g/l in the said nickel powder dispersion soln;
(2) the reducing agent hydrazine hydrate is mixed with water, make the hydrazine hydrate aqueous solution that hydrazine hydrate concentration is 2.5mol/L, regulate more than the pH value to 10 of hydrazine hydrate aqueous solution, promptly get reductant solution;
(3) with said nickel powder dispersion soln and said reductant solution with volume ratio nickel powder dispersion soln: reductant solution=mix at 2.4: 1; Get reactant liquor A, in said reactant liquor A, drip silver ammino solution 50ml and react, the control reaction time is 70～100 minutes; Get suspension; Centrifugation, the gained solid makes nucleocapsid structure nickel-silver bimetal powder through washing, vacuum drying.
Said nickel powder is that the spherical nickel particle of 1.0 μ m is formed by average grain diameter.
Said dispersant is PVP or sodium tartrate.
The volume ratio of second alcohol and water is in the said ethanol-water mixed solvent: ethanol: water=2: 5.
The preparation method of nucleocapsid structure nickel provided by the invention-silver bimetal powder selects appropriate reductant and reaction system through thermodynamic analysis, is fully suppressing under the situation of displacement reaction; It is silver-plated to be implemented in nickel powder surface direct chemical, promptly adopts liquid phase reduction, directly at the metal nickel powder electroplate; In ethanol-water system, be reducing agent with the hydrazine hydrate, through the control inhibition displacement reaction of reaction condition; Make silver ammino solution that the liquid-phase reduction reaction preferentially take place; In the plating process, the solution metal silver ion is constantly reduced and is deposited on the matrix surface, has made and former nickel powder particle diameter and the roughly the same core-shell type nickel-silver bimetal powder of pattern.
The preparation method of nucleocapsid structure nickel provided by the invention-silver bimetal powder adopts that particle diameter is less, the nickel powder of narrow diameter distribution, good dispersion is made matrix; Because matrix nickel powder itself can serve as catalyst, matrix surface need not to carry out sensitization, activation processing.The preparation method of nucleocapsid structure nickel provided by the invention-silver bimetal powder has the following advantages: the present invention adopts the chemical plating new technology that nickel powder is directly coated; Avoid complicated in the past technology, helped the reduction of the stable and production cost of properties of product; In the chemical plating process, adopt the dripping method new technology, add silver ammino solution quantitatively, continuously, reaction is maintained under the low metal ion concentration always carry out, efficiently solve a difficult problem that hinders the powder electroless large-scale production; The present invention changes the morphology control of nickel-silver bimetal powder into morphology control that ripe relatively nickel powder prepares process; Thickness through silver-colored addition controlling diaphragm.
Nucleocapsid structure nickel-silver bimetal the powder that adopts the inventive method to make, its silver coating controllable thickness, narrow diameter distribution, good dispersion, tap density is high.Nickel-silver bimetal the powder that adopts the inventive method to make has kept original pattern of nickel powder, and powder dispersity is good, and no agglomeration produces.The surperficial silver content of the nickel-silver bimetal powder that after secondary coats, makes can reach more than 90%, and silver forms continuous silverskin on the nickel particle surface, forms the nickel-silver bimetal powder of nucleocapsid structure.Can know through the DSC-TG atlas analysis; The initial oxidation resistance temperature of the nickel-silver bimetal powder that after secondary coats, makes has lifting by a relatively large margin; High-temperature oxidation resistance also significantly improves, maybe for serving as under nickel-silver metal powder body hypothermia that electrocondution slurry, electromagnetic wave absorption material provide.
Description of drawings
Fig. 1 is the SEM figure of nickel powder material in the embodiment of the invention 1;
Fig. 2 is the SEM figure of the nucleocapsid structure nickel-silver bimetal powder that once coats that makes in the embodiment of the invention 1;
Fig. 3 is the XRD figure spectrum of the nucleocapsid structure nickel-silver bimetal powder that once coats that makes in the embodiment of the invention 1;
Fig. 4 composes for the XRD figure of nucleocapsid structure nickel-silver bimetal powder that the secondary that makes in the embodiment of the invention 1 coats;
Fig. 5 is the SEM figure of the nucleocapsid structure nickel-silver bimetal powder that once coats that makes in the embodiment of the invention 2;
Fig. 6 is the DSC-TG collection of illustrative plates of nickel powder material in the embodiment of the invention 2;
The DSC-TG collection of illustrative plates of nucleocapsid structure nickel-silver bimetal powder that Fig. 7 coats for the secondary that makes in the embodiment of the invention 2.
The specific embodiment
Embodiment 1
The preparation method of present embodiment nucleocapsid structure nickel-silver bimetal powder may further comprise the steps:
(1) 25g nickel powder, 8.33g dispersant PVP are joined in the 1L ethanol-water mixed solvent; Place water-bath then, keeping bath temperature is 50 ℃, stirs 1 hour; Mixing speed 500rpm; Make the nickel powder dispersion soln, wherein nickel powder is that the spherical nickel particle of 1.0 μ m is formed by average grain diameter, and the volume ratio of second alcohol and water is in the ethanol-water mixed solvent: ethanol: water=2: 5;
(2) the reducing agent hydrazine hydrate is mixed with water, make the hydrazine hydrate aqueous solution that hydrazine hydrate concentration is 2.5mol/L, regulate the pH value to 11 of hydrazine hydrate aqueous solution, get reductant solution;
(3) with nickel powder dispersion soln and reductant solution with volume ratio nickel powder dispersion soln: reductant solution=mix at 2.4: 1; Get reactant liquor A, in reactant liquor A, drip silver ammino solution 50ml and react, the control reaction time is 70 minutes; Get suspension; Centrifugation, gained solid make the nucleocapsid structure nickel-silver bimetal powder that once coats through washing, vacuum drying.
Nucleocapsid structure nickel-silver bimetal powder once to coat replaces the nickel powder in the present embodiment step (1), can prepare nucleocapsid structure nickel-silver bimetal powder that secondary coats, and promptly may further comprise the steps:
(1) the nucleocapsid structure nickel-silver bimetal powder, the 8.33g dispersant PVP that 25g are once coated join in the 1L ethanol-water mixed solvent; Place water-bath then; Keeping bath temperature is 50 ℃, stirs mixing speed 500rpm 1 hour; Make dispersion soln, the volume ratio of second alcohol and water is in the ethanol-water mixed solvent: ethanol: water=2: 5;
(2) the reducing agent hydrazine hydrate is mixed with water, make the hydrazine hydrate aqueous solution that hydrazine hydrate concentration is 2.5mol/L, regulate the pH value to 11 of hydrazine hydrate aqueous solution, get reductant solution;
(3) with dispersion soln and reductant solution with the volume ratio dispersion soln: reductant solution=mix at 2.4: 1; Get reactant liquor A, in reactant liquor A, drip silver ammino solution 50ml and react, the control reaction time is 70 minutes; Get suspension; Centrifugation, gained solid make nucleocapsid structure nickel-silver bimetal powder that secondary coats through washing, vacuum drying.
Fig. 1 is the SEM figure of present embodiment nickel powder material, and as can be seen from Figure 1, nickel powder material is a spheric granules, and particle diameter is even, average grain diameter 1.0 μ m, and distributed area is narrow; Fig. 2 schemes for the SEM of the nucleocapsid structure nickel-silver bimetal powder that once coats that present embodiment makes; As can be seen from Figure 2; Nucleocapsid structure nickel-silver bimetal the powder that once coats has kept original pattern of nickel powder material; Average grain diameter is 1.2 μ m, and powder dispersity is good, and no agglomeration produces; Fig. 3 composes for the XRD figure of the nucleocapsid structure nickel-silver bimetal powder that once coats that present embodiment makes, and as can be seen from Figure 3, Ag and Ni characteristic peak is arranged in the diffraction maximum; Show that nickel powder is through coating; Formed nickel-silver metal powder, the nucleocapsid structure nickel-silver bimetal powder surface silver content that once coats that present embodiment makes reaches 32.53%, explains that the surface is except that containing silver atoms; Also have nickle atom, silver does not have to form continuous silverskin on the nickel particle surface; Fig. 4 is the XRD figure spectrum of nucleocapsid structure nickel-silver bimetal powder of coating of the secondary that makes; As can be seen from Figure 4; The surperficial silver content of nucleocapsid structure nickel-silver bimetal powder that the secondary that makes coats can reach 90.96%, though nickle atom also exists, proportion is very little; Silver atoms has accounted for absolute predominance, and silver has formed continuous silverskin on the nickel particle surface.
Embodiment 2
The preparation method of present embodiment nucleocapsid structure nickel-silver bimetal powder may further comprise the steps:
(1) 25g nickel powder, 8.33g dispersant sodium tartrate are joined in the 1L ethanol-water mixed solvent; Place water-bath then, keeping bath temperature is 50 ℃, stirs 1 hour; Mixing speed 500rpm; Make the nickel powder dispersion soln, wherein nickel powder is that the spherical nickel particle of 1.0 μ m is formed by average grain diameter, and the volume ratio of second alcohol and water is in the ethanol-water mixed solvent: ethanol: water=2: 5;
(2) the reducing agent hydrazine hydrate is mixed with water, make the hydrazine hydrate aqueous solution that hydrazine hydrate concentration is 2.5mol/L, regulate the pH value to 12 of hydrazine hydrate aqueous solution, get reductant solution;
(3) with nickel powder dispersion soln and reductant solution with volume ratio nickel powder dispersion soln: reductant solution=mix at 2.4: 1; Get reactant liquor A, in reactant liquor A, drip silver ammino solution 50ml and react, the control reaction time is 100 minutes; Get suspension; Centrifugation, gained solid make the nucleocapsid structure nickel-silver bimetal powder that once coats through washing, vacuum drying.
Nucleocapsid structure nickel-silver bimetal powder once to coat replaces the nickel powder in the present embodiment step (1), and nucleocapsid structure nickel-silver bimetal powder that the preparation secondary coats may further comprise the steps:
(1) the nucleocapsid structure nickel-silver bimetal powder, the 8.33g dispersant sodium tartrate that 25g are once coated join in the 1L ethanol-water mixed solvent; Place water-bath then; Keeping bath temperature is 50 ℃, stirs mixing speed 500rpm 1 hour; Make dispersion soln, the volume ratio of second alcohol and water is in the ethanol-water mixed solvent: ethanol: water=2: 5;
(2) the reducing agent hydrazine hydrate is mixed with water, make the hydrazine hydrate aqueous solution that hydrazine hydrate concentration is 2.5mol/L, regulate the pH value to 12 of hydrazine hydrate aqueous solution, get reductant solution;
(3) with dispersion soln and reductant solution with the volume ratio dispersion soln: reductant solution=mix at 2.4: 1; Get reactant liquor A, in reactant liquor A, drip silver ammino solution 50ml and react, the control reaction time is 100 minutes; Get suspension; Centrifugation, gained solid make nucleocapsid structure nickel-silver bimetal powder that secondary coats through washing, vacuum drying.
Fig. 5 schemes for the SEM of the nucleocapsid structure nickel-silver bimetal powder that once coats that present embodiment makes; As can be seen from Figure 5; Nucleocapsid structure nickel-silver bimetal the powder that once coats that present embodiment makes is a spheric granules, and distributed area is narrow, average grain diameter 1.2 μ m; Good dispersion property does not have agglomeration to take place.Fig. 6 is the DSC-TG collection of illustrative plates of present embodiment nickel powder material; Fig. 7 is the DSC-TG collection of illustrative plates of the nucleocapsid structure nickel-silver bimetal powder of present embodiment secondary coating; As can be seen from Figure 6, the initial oxidation temperature of nickel powder material is 290.45 ℃, and weightening finish is up to 25.89% in the time of 732.62 ℃; After this no longer weightening finish is so the high-temperature oxidation resistance of nickel powder material is very poor; As can be seen from Figure 7, the initial oxidation temperature of nucleocapsid structure nickel-silver bimetal powder that the present embodiment secondary coats is 389.36 ℃, in the time of 732.62 ℃; It is maximum that weightening finish reaches; Weightening finish 7.584% this shows, nucleocapsid structure nickel-initial oxidation resistance temperature of silver bimetal powder that the present embodiment secondary coats promotes significantly; Approximately promote 100 ℃, high-temperature oxidation resistance also obviously improves.Because the initial oxidation resistance temperature of nucleocapsid structure nickel-silver bimetal powder that secondary coats significantly promotes, for serve as electrocondution slurry under its low temperature, electromagnetic wave absorption material provides maybe.
In order to obtain nucleocapsid structure nickel-silver bimetal powder that covered effect is good, high-temperature oxidation resistance is good, can repeat preparation method 1-2 time of nucleocapsid structure nickel provided by the invention-silver bimetal powder.
Claims (4)
1. the preparation method of nucleocapsid structure nickel-silver bimetal powder is characterized in that, may further comprise the steps:
(1) nickel powder, dispersant are joined in the ethanol-water mixed solvent, place water-bath then, keeping bath temperature is 50 ℃; Stir; Make the nickel powder dispersion soln, the concentration of nickel powder is 25.0g/l in the said nickel powder dispersion soln, and the concentration of dispersant is 8.33g/l in the said nickel powder dispersion soln;
(2) the reducing agent hydrazine hydrate is mixed with water, make the hydrazine hydrate aqueous solution that hydrazine hydrate concentration is 2.5mol/L, regulate more than the pH value to 10 of hydrazine hydrate aqueous solution, promptly get reductant solution;
(3) with said nickel powder dispersion soln and said reductant solution with volume ratio nickel powder dispersion soln: reductant solution=mix at 2.4: 1; Get reactant liquor A, in said reactant liquor A, drip silver ammino solution 50ml and react, the control reaction time is 70～100 minutes; Get suspension; Centrifugation, the gained solid makes nucleocapsid structure nickel-silver bimetal powder through washing, vacuum drying.
2. the preparation method of nucleocapsid structure nickel according to claim 1-silver bimetal powder is characterized in that, said nickel powder is that the spherical nickel particle of 1.0 μ m is formed by average grain diameter.
3. the preparation method of nucleocapsid structure nickel according to claim 1-silver bimetal powder is characterized in that said dispersant is PVP or sodium tartrate.
4. the preparation method of nucleocapsid structure nickel according to claim 1-silver bimetal powder is characterized in that the volume ratio of second alcohol and water is in the said ethanol-water mixed solvent: ethanol: water=2: 5.
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Cited By (7)
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| CN103008674A (en) * | 2013-01-08 | 2013-04-03 | 安徽工业大学 | Nickel/copper oxide composite nanometer wave absorbing material and preparation method thereof |
| CN103567437A (en) * | 2013-10-11 | 2014-02-12 | 国家钽铌特种金属材料工程技术研究中心 | Preparation method of nickel powder with high tap density and degree of crystallinity |
| CN104588679A (en) * | 2015-01-15 | 2015-05-06 | 黑龙江大学 | Preparation method of nano silver-nickel alloy powder |
| CN106378448A (en) * | 2016-09-20 | 2017-02-08 | 杨海波 | Silver coating surface modification method of nickel powder for circuit protection device material |
| CN108296478A (en) * | 2018-01-11 | 2018-07-20 | 宁波广新纳米材料有限公司 | Silver-nickel powder and preparation method thereof and electrocondution slurry containing the silver-nickel powder |
| CN111468739A (en) * | 2020-03-26 | 2020-07-31 | 浙江师范大学 | Magnetic recyclable Ni-coated Ag core-shell structure composite nanoparticle, preparation method thereof and dye degradation method |
| CN112916851A (en) * | 2021-01-25 | 2021-06-08 | 江苏博迁新材料股份有限公司 | Preparation method of silver-nickel composite powder |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104588679B (en) * | 2015-01-15 | 2017-09-22 | 黑龙江大学 | Nano Silver nickel alloy raw powder's production technology |
| CN106378448A (en) * | 2016-09-20 | 2017-02-08 | 杨海波 | Silver coating surface modification method of nickel powder for circuit protection device material |
| CN108296478A (en) * | 2018-01-11 | 2018-07-20 | 宁波广新纳米材料有限公司 | Silver-nickel powder and preparation method thereof and electrocondution slurry containing the silver-nickel powder |
| CN111468739A (en) * | 2020-03-26 | 2020-07-31 | 浙江师范大学 | Magnetic recyclable Ni-coated Ag core-shell structure composite nanoparticle, preparation method thereof and dye degradation method |
| CN112916851A (en) * | 2021-01-25 | 2021-06-08 | 江苏博迁新材料股份有限公司 | Preparation method of silver-nickel composite powder |
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