CN102407329A - Method for preparing nickel-silver coreshell structure nanoparticles - Google Patents
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- CN102407329A CN102407329A CN2011103658673A CN201110365867A CN102407329A CN 102407329 A CN102407329 A CN 102407329A CN 2011103658673 A CN2011103658673 A CN 2011103658673A CN 201110365867 A CN201110365867 A CN 201110365867A CN 102407329 A CN102407329 A CN 102407329A
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Abstract
The invention relates to the field of a functional nanometer material and a material preparation, particularly to a method for preparing nickel-silver coreshell structure nanoparticles. The method particularly comprises the following steps of: dissolving silver nitrate in water, adding sodium hydroxide and adjusting solution by ammonia water until the solution becomes transparent again to obtain a main salt; dissolving glucose and tartaric acid in a mixed solution of ethanol and water to obtain a reducing solution; and washing sensitized nanometer nickel powders, adding the washed powders to the main salt, dripping the reducing solution in the main salt while stirring, separating the product by a magnet after stirring for 1h at normal temperature, washing the separated product by de-ionized water and absolute ethanol, and vacuum-drying the washed product for 12h at the temperature of 40 degrees centigrade to obtain the nickel-silver coreshell structure nanoparticles. The nickel-silver coreshell structure nanoparticles are synthesized on the basis of the prepared nanometer nickel particles; the operation method is simple and easy to implement; the reaction condition is moderate; the required equipment is simple; the shell layers of the prepared nickel-silver coreshell structure nanoparticles have strong bonding force and good dispersity and are covered densely; and the thickness of the silver shell can be controlled by changing the quantity of the silver nitrate.
Description
Technical field
The present invention relates to function nano material and field of material preparation, refer in particular to the preparation method of a kind of nickel-galactic nucleus shell structural nano particle.
Background technology
Composite nanoparticle comprises two kinds or more kinds of components; Has unique or various character; Therefore have wider application than single nano particle, therefore, in recent years; In persistent exploration process to the high-performance new material; Synthesizing, prepare and using of composite nanoparticle more and more causes people's attention, and a noticeable research focus is exactly the nuclear shell structure nano bimetallic material in the field, for single metal and traditional double metal component (alloy or binary metal) nano particle; Nucleocapsid structure bimetallic particle has special electronic structure and surface nature; It has not only kept the physical and chemical performance of original metal core, but also has the good metallic character of clad, so the nuclear shell structure nano bimetallic material has a wide range of applications in fields such as electronics, biology sensor, optics and catalysis.
Hud typed nickel-Yin composite micro-powder is meant that with a kind of metal nickel powder particulate be nuclear, and coats the structure that another kind of argent forms shell on its surface, and the development of this composite particles is to be based upon on the basis of nickel powder microparticle surfaces passivation.Because there is big specific area in the nickel powder particulate; The surface state of particulate is to chemistry, the physical property important influence of particulate; Utilize various organic and inorganic material that the nickel powder surface is modified, can eliminate blemish effectively, thereby realize macro-control nickel powder character; This nucleocapsid structure has not only kept the physical and chemical performance of original metallic nickel core; Also have the good metallic character of silver coating, improved the non-oxidizability and the heat endurance of simple nickel powder, kept the high conductivity of nickel with silver; And nickel can suppress silver-colored dissolving in the coated composite powder; Can overcome the defective of silver migration in the silver conductive adhesive; Reach the purpose of practicing thrift noble metal, protection environment, therefore, all have a good application prospect in many fields such as optics, magnetics, catalysis, biochemistry, biomedical sector, electric slurry, conductive filler, electrically-conducting paint, electronic shield materials; But because in most cases metal-back coating degree is lower; Coat inhomogeneously, therefore, nickel-galactic nucleus shell structure that preparation coats evenly, fully remains a kind of challenge.
The preparation method of nuclear shell structure nano metal powder comprises thermal decomposition-reducing process, electroless plating method, colloidal particle template, polyol reduction method, co-electrodeposition method, displacement method, electrochemical process etc.Wherein, electroless plating method is not have under the situation of impressed current, utilizes reducing agent that the reduction of solution metal ion chemistry is had the matrix surface of catalytic activity; Make it to form the coat of metal, originally, chemical plating just is plated on the material surface of bulk or sheet; To 20th century the mid-80s, electroless plating technology is used for reference in the surface treatment of powder, has the report at powder surface plating gold, silver, platinum, nickel, copper, cobalt etc. at present; This method is easy to operate, and technology is simple, and thickness of coating evenly and be easy to control; Outward appearance is good, and at present, the report of relevant nanometer nickeline nucleocapsid structure preparation is less; Prepared nano particle coating degree is lower, and needs to add protective agent in the course of reaction, and the present invention is on existing basis; Do not add the nanometer nickel-galactic nucleus shell structural nano particle that has prepared good dispersion under protectant condition with electroless plating method, and adopting various modern analysis means such as X-ray diffraction, transmission electron microscope that its structure is characterized.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of nickeline core-shell structure nanometer particle.
The concrete operations step is following: the 1) preparation of main salt: silver nitrate is water-soluble, add NaOH, and it is transparent again to transfer to solution with ammoniacal liquor, and wherein the concentration of silver nitrate is 0.2molL
-12) preparation of reducing solution: glucose and tartaric acid are joined stir in the mixed solution of second alcohol and water and make its dissolving, wherein concentration of glucose is 0.25 molL
-1, tartaric acid concentration is 0.025 molL
-1, the volume ratio of main salt and reducing solution is 1:1, the mol ratio of NaOH and glucose is 2.5:1; 4) chemical silvering: add after the nano-nickel powder washes clean with sensitization and become owner of in the salt; The mol ratio of nickel powder and silver nitrate is 3 ~ 8:2 ~ 8; Stir down reducing solution is splashed in the main salt; Use the magnet products of separated behind the stirring at normal temperature 1h, with deionized water, absolute ethanol washing, 40 ℃ of vacuum drying 12h obtain product.
Among the above-mentioned preparation method, said reducing solution is with 1mlmin
-1Speed splash in the main salt.
Among the above-mentioned preparation method, the preparation method of the nano-nickel powder of said sensitization is following: it is 5% SnCl that nano-nickel powder is joined to mass fraction
2Hydrochloric acid solution in soak, the time is 5min, after the washing repeatedly of nickel powder after the sensitization, filter liquor is used AgNO
3Whether the adularescent deposition generates in the solution titration, can check to have or not Cl
-Exist.
Among the above-mentioned preparation method, used nano-nickel powder average grain diameter is 104nm.
Among the above-mentioned preparation method, the volume ratio of second alcohol and water is 1:9.
Among the above-mentioned preparation method, whether the adularescent deposition generates with the watery hydrochloric acid titration to separate the supernatant that obtains with magnet after reaction finishes, and can check to have or not Ag
+Exist, thereby judge whether reaction is complete; With having or not the Ag nano particle to exist in the atomic absorption spectrophotometer test supernatant, can check Ag whether to wrap in Ni nuclear surface fully.
Description of drawings
Fig. 1 is the XRD spectra according to instance 1 prepared sample, and the silver nitrate consumption is 4mmol, and the nickel consumption is a) 3mmol, b) 5mmol, c) 8mmol;
Fig. 2 is the transmission electron microscope picture according to instance 1 prepared sample, and the silver nitrate consumption is 4mmol, and the nickel consumption is respectively a) 3mmol, b) 5mmol, c) 8mmol;
Fig. 3 is the transmission electron microscope picture according to instance 2 prepared samples, and the nickel consumption is 3mmol, and the silver nitrate consumption is respectively d) 2mmol, e) 4mmol, f) 6mmol, g) 8mmol;
Fig. 4 is the transmission electron microscope picture according to instance 3 prepared samples, and the nickel consumption is 3mmol, and the silver nitrate consumption is respectively 4mmol, and the consumption of NaOH is respectively 0g, 0.5g;
Fig. 5 is the transmission electron microscope picture according to instance 4 prepared samples, and the nickel consumption is 3mmol, and the silver nitrate consumption is respectively 4mmol, adds surfactant.
The specific embodiment
Below in conjunction with the practical implementation instance the present invention is further specified.
Embodiment 1:
The 4mmol silver nitrate is water-soluble, add the NaOH of 0.5g, it is transparent again to transfer to solution with ammoniacal liquor, adds water liquor capacity is adjusted to 20ml, is mixed with main salt; With 0.9g glucose, 0.0793g tartaric acid (D type-anhydride) is dissolved in the mixed solution of 2ml ethanol and 18ml water, is mixed with reducing solution; Add after the nano-nickel powder washes clean with sensitization and become owner of in the salt, stir with reducing solution with 1mlmin
-1Speed reducing solution is splashed in the main salt, use the magnet products of separated behind the stirring at normal temperature 1h, with deionized water, absolute ethanol washing, 40 ℃ of vacuum drying 12h obtain product; The amount of the nickel of investigating in this experiment is respectively 3mmol, 5mmol, 8mmol.
Adopt XRD, transmission electron microscope characterizes sample:
Fig. 1 is the XRD spectra of prepared sample, can find out through checking the card of answering, and has the characteristic peak of nickel and silver in the spectrogram, does not have the characteristic peak of its oxide; Be 38.2 ° at 2 θ wherein, 44.4 °, 64.6 °, 77.6 ° characteristic peak is (111) of corresponding A g respectively; (200), (220), (311) diffraction crystal face, 2 θ are (200) diffraction crystal face of 51.8 ° the corresponding Ni of characteristic peak; And 2 θ are 44.5 ° (111), and the characteristic peak of the nickel of 76.4 ° (220) is 44.4 ° (200) with silver-colored 2 θ respectively, the characteristic peak overlaid of 77.6 ° (311); This shows that this thermometal-powder is the mixed metal powder of nickeline, cleaning surfaces, oxide-free existence.
Fig. 2 is respectively 3mmol (a) for the nickel consumption, 5mmol (b), and the transmission electron microscope picture of prepared sample during 8mmol (c) as can be seen from the figure, is 5mmol at the nickel consumption, during 8mmol, it is more serious that sample is reunited, and consumption is when being 3mmol, sample dispersion property is good.
Embodiment 2:
Silver nitrate is water-soluble, add a certain amount of NaOH, it is transparent again to transfer to solution with ammoniacal liquor, is mixed with main salt, and wherein the concentration of silver nitrate is 0.2molL
-1With a certain proportion of glucose, tartaric acid is dissolved in the mixed solution of second alcohol and water, is mixed with reducing solution, and wherein concentration of glucose is 0.25molL
-1, tartaric acid concentration is 0.025molL
-1, the volume ratio of second alcohol and water is 1:9; Add after the nano-nickel powder washes clean with the 3mmol sensitization and become owner of in the salt, stir with reducing solution with 1mlmin
-1Speed splash in the main salt, the volume ratio of wherein main salt and reducing solution is 1:1, uses the magnet products of separated behind the stirring at normal temperature 1h, with deionized water, absolute ethanol washing, 40 ℃ of vacuum drying 12h obtain product; The amount of the silver nitrate of investigating in this experiment is respectively 2mmol, 4mmol, 6mmol, 8mmol., the volume of the water of adding is respectively 10ml, 20ml, and 30ml, 40ml, the NaOH of adding is respectively 0.25g, 0.5g, 0.75g, 1g.
Adopt transmission electron microscope that sample is characterized:
Fig. 3 is respectively 2mmol (d) for the silver nitrate consumption, 4mmol (e), and 6mmol (f), the transmission electron microscope picture of prepared sample during 8mmol (g), as can be seen from the figure, when the consumption of silver nitrate increased gradually, the silver-colored shell of prepared nickeline nucleocapsid structure was thick more.Therefore, the thickness of silver-colored shell can be controlled through the amount that changes silver nitrate.
Embodiment 3:
The 4mmol silver nitrate is water-soluble, add NaOH, it is transparent again to transfer to solution with ammoniacal liquor, adds water liquor capacity is adjusted to 20ml, is mixed with main salt; With 0.9g glucose, 0.0793g tartaric acid (D type-anhydride) is dissolved in the mixed solution of 2ml ethanol and 18ml water, is mixed with reducing solution; Add after the nano-nickel powder washes clean with the 3mmol sensitization and become owner of in the salt, stir with reducing solution with 1mlmin
-1Speed reducing solution is splashed in the main salt, use the magnet products of separated behind the stirring at normal temperature 1h, with deionized water, absolute ethanol washing, 40 ℃ of vacuum drying 12h obtain product.The consumption of the NaOH of investigating in this experiment is respectively 0g, 0.8 g.
Utilize transmission electron microscope that sample is characterized:
The transmission electron microscope picture of prepared sample when Fig. 4 is respectively 0g for the consumption of NaOH.The transmission electron microscope picture of sample relatively can be found out when being 0.5g with sodium hydroxide concentration, and whether the existence of NaOH does not have obvious influence to pattern, the coating degree of product.But we find in the experimentation, under all the same situation of no NaOH in the system and other conditions, react and still have Ag in the solution more than five hours
+Exist, and add after the NaOH, reaction only needed to accomplish in one hour, therefore, added NaOH and can promote reaction speed and Ag greatly
+Utilization rate.
Embodiment 4:
The 4mmol silver nitrate is water-soluble, add the NaOH of 0.5g, it is transparent again to transfer to solution with ammoniacal liquor, adds water liquor capacity is adjusted to 20ml, is mixed with main salt; With 0.9g glucose, 0.0793g tartaric acid is dissolved in the mixed solution of 2ml ethanol and 18ml water, is mixed with reducing solution; Add after the nano-nickel powder washes clean with the 3mmol sensitization and become owner of in the salt, and add certain amount of surfactant, stir with reducing solution with 1mlmin
-1Speed reducing solution is splashed in the main salt, use the magnet products of separated behind the stirring at normal temperature 1h, with deionized water, absolute ethanol washing, 40 ℃ of vacuum drying 12h obtain product; The surfactant of the adding of investigating in this experiment is respectively 0.5gSDS, 0.5gPVP.
Utilize transmission electron microscope that sample is characterized:
Fig. 5 is for adding surfactant SDS 0.5g (i); The transmission electron microscope picture of the prepared sample of PVP0.5g (j); As can be seen from the figure; Surfactant does not have obvious influence to pattern, the uniformity coefficient of product, and therefore, the present invention can synthesize the nickel-galactic nucleus shell structural nano particle of favorable dispersibility under the situation that does not add surfactant.
?
Claims (6)
1. the preparation method of nickel-galactic nucleus shell structural nano particle, the concrete operations step is following: the 1) preparation of main salt: silver nitrate is water-soluble, add NaOH, it is transparent again to transfer to solution with ammoniacal liquor, and wherein the concentration of silver nitrate is 0.2molL
-12) preparation of reducing solution: glucose and tartaric acid are joined stir in the mixed solution of second alcohol and water and make its dissolving, wherein concentration of glucose is 0.25 molL
-1, tartaric acid concentration is 0.025 molL
-1, the volume ratio of main salt and reducing solution is 1:1, the mol ratio of NaOH and glucose is 2.5:1; 4) chemical silvering: add after the nano-nickel powder washes clean with sensitization and become owner of in the salt; The mol ratio of nickel powder and silver nitrate is 3 ~ 8:2 ~ 8; Stir down reducing solution is splashed in the main salt; Use the magnet products of separated behind the stirring at normal temperature 1h, with deionized water, absolute ethanol washing, 40 ℃ of vacuum drying 12h obtain product.
2. the preparation method of a kind of nickel as claimed in claim 1-galactic nucleus shell structural nano particle, it is characterized in that: said reducing solution is with 1mlmin
-1Speed splash in the main salt.
3. the preparation method of a kind of nickel as claimed in claim 1-galactic nucleus shell structural nano particle, it is characterized in that: the preparation method of the nano-nickel powder of said sensitization is following: it is 5% SnCl that nano-nickel powder is joined to mass fraction
2Hydrochloric acid solution in soak, the time is 5min, after the washing repeatedly of nickel powder after the sensitization, filter liquor is used AgNO
3Whether the adularescent deposition generates in the solution titration, and check has or not Cl
-Exist.
4. the preparation method of a kind of nickel as claimed in claim 1-galactic nucleus shell structural nano particle is characterized in that: used nano-nickel powder average grain diameter is 104nm.
5. the preparation method of a kind of nickel as claimed in claim 1-galactic nucleus shell structural nano particle is characterized in that: the volume ratio of second alcohol and water is 1:9.
6. the preparation method of a kind of nickel as claimed in claim 1-galactic nucleus shell structural nano particle is characterized in that: whether the adularescent deposition generates with the watery hydrochloric acid titration to separate the supernatant that obtains with magnet after reaction finishes, and check has or not Ag
+Exist, thereby judge whether reaction is complete; With having or not the Ag nano particle to exist in the atomic absorption spectrophotometer test supernatant, whether check Ag has wrapped in Ni nuclear surface fully.
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Cited By (10)
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|---|---|---|---|---|
| CN102723142A (en) * | 2012-04-24 | 2012-10-10 | 江苏大学 | Preparation method of nickel-based silver conductive slurry |
| CN102728852A (en) * | 2012-07-10 | 2012-10-17 | 国家钽铌特种金属材料工程技术研究中心 | Preparation method of oxide or meta-coated nickel ultrafine powder |
| CN103071788A (en) * | 2012-10-31 | 2013-05-01 | 江苏大学 | Method of preparing nickel-silver nuclear shell structure nano-particles |
| CN103506620A (en) * | 2013-09-22 | 2014-01-15 | 陕西师范大学 | Barium ferrite/barium titanate core-shell particle |
| CN105598467A (en) * | 2016-01-20 | 2016-05-25 | 哈尔滨工业大学深圳研究生院 | High-temperature-resistant silver-coated and nickel-coated copper conductive powder of core-shell structure and preparation method thereof |
| CN106583712A (en) * | 2016-11-28 | 2017-04-26 | 清华大学 | Preparation method for silver-coated copper nanoparticles |
| 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 |
| CN112323086A (en) * | 2020-10-27 | 2021-02-05 | 澳门大学 | Nickel-platinum composite nano catalyst, preparation method and application thereof, and carbon-supported composite electrocatalyst |
| CN113426999A (en) * | 2021-07-14 | 2021-09-24 | 重庆邮电大学 | Magnetic nanowire with core-shell heterostructure and preparation method and application thereof |
| CN113909472A (en) * | 2020-06-22 | 2022-01-11 | 中国石油化工股份有限公司 | Nano composite particle, preparation method and application thereof |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102723142A (en) * | 2012-04-24 | 2012-10-10 | 江苏大学 | Preparation method of nickel-based silver conductive slurry |
| CN102723142B (en) * | 2012-04-24 | 2014-04-02 | 江苏大学 | Preparation method of nickel-based silver conductive slurry |
| CN102728852B (en) * | 2012-07-10 | 2014-11-12 | 国家钽铌特种金属材料工程技术研究中心 | Preparation method of oxide or meta-coated nickel ultrafine powder |
| CN102728852A (en) * | 2012-07-10 | 2012-10-17 | 国家钽铌特种金属材料工程技术研究中心 | Preparation method of oxide or meta-coated nickel ultrafine powder |
| CN103071788A (en) * | 2012-10-31 | 2013-05-01 | 江苏大学 | Method of preparing nickel-silver nuclear shell structure nano-particles |
| CN103506620B (en) * | 2013-09-22 | 2016-01-20 | 陕西师范大学 | Iron/barium titanate core-shell particles |
| CN103506620A (en) * | 2013-09-22 | 2014-01-15 | 陕西师范大学 | Barium ferrite/barium titanate core-shell particle |
| CN105598467A (en) * | 2016-01-20 | 2016-05-25 | 哈尔滨工业大学深圳研究生院 | High-temperature-resistant silver-coated and nickel-coated copper conductive powder of core-shell structure and preparation method thereof |
| CN106583712A (en) * | 2016-11-28 | 2017-04-26 | 清华大学 | Preparation method for silver-coated copper nanoparticles |
| 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 |
| CN113909472A (en) * | 2020-06-22 | 2022-01-11 | 中国石油化工股份有限公司 | Nano composite particle, preparation method and application thereof |
| CN112323086A (en) * | 2020-10-27 | 2021-02-05 | 澳门大学 | Nickel-platinum composite nano catalyst, preparation method and application thereof, and carbon-supported composite electrocatalyst |
| CN112323086B (en) * | 2020-10-27 | 2023-10-27 | 澳门大学 | Nickel-platinum composite nano-catalyst, preparation method and application thereof, and carbon-supported composite electrocatalyst |
| CN113426999A (en) * | 2021-07-14 | 2021-09-24 | 重庆邮电大学 | Magnetic nanowire with core-shell heterostructure and preparation method and application thereof |
| CN113426999B (en) * | 2021-07-14 | 2022-09-30 | 重庆邮电大学 | Magnetic nanowire with core-shell heterostructure and preparation method and application thereof |
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