CN102407329B - Method for preparing nickel-silver coreshell structure nanoparticles - Google Patents
Method for preparing nickel-silver coreshell structure nanoparticles Download PDFInfo
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- CN102407329B CN102407329B CN 201110365867 CN201110365867A CN102407329B CN 102407329 B CN102407329 B CN 102407329B CN 201110365867 CN201110365867 CN 201110365867 CN 201110365867 A CN201110365867 A CN 201110365867A CN 102407329 B CN102407329 B CN 102407329B
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- 239000002105 nanoparticle Substances 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title abstract description 13
- 239000011258 core-shell material Substances 0.000 title abstract description 5
- MOFOBJHOKRNACT-UHFFFAOYSA-N nickel silver Chemical compound [Ni].[Ag] MOFOBJHOKRNACT-UHFFFAOYSA-N 0.000 title abstract 4
- 239000010956 nickel silver Substances 0.000 title abstract 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 66
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 54
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 44
- 239000000243 solution Substances 0.000 claims abstract description 36
- 150000003839 salts Chemical class 0.000 claims abstract description 26
- 238000002360 preparation method Methods 0.000 claims abstract description 25
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000000843 powder Substances 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 20
- 238000003756 stirring Methods 0.000 claims abstract description 16
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims abstract description 12
- 239000008103 glucose Substances 0.000 claims abstract description 12
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims abstract description 10
- 235000002906 tartaric acid Nutrition 0.000 claims abstract description 10
- 239000011975 tartaric acid Substances 0.000 claims abstract description 10
- 238000005406 washing Methods 0.000 claims abstract description 10
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims abstract description 7
- 239000011259 mixed solution Substances 0.000 claims abstract description 7
- 238000001291 vacuum drying Methods 0.000 claims abstract description 7
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims abstract description 6
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims abstract description 4
- 239000000047 product Substances 0.000 claims description 14
- 206010070834 Sensitisation Diseases 0.000 claims description 10
- 230000008313 sensitization Effects 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N hydrochloric acid Substances Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000012546 transfer Methods 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 5
- 238000001556 precipitation Methods 0.000 claims description 4
- 239000006228 supernatant Substances 0.000 claims description 4
- 238000004448 titration Methods 0.000 claims description 4
- 101710134784 Agnoprotein Proteins 0.000 claims description 2
- 238000010521 absorption reaction Methods 0.000 claims description 2
- 238000012360 testing method Methods 0.000 claims description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 abstract description 8
- 239000000463 material Substances 0.000 abstract description 8
- 229910052709 silver Inorganic materials 0.000 abstract description 7
- 239000004332 silver Substances 0.000 abstract description 7
- 239000002245 particle Substances 0.000 abstract description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 abstract 1
- 230000005540 biological transmission Effects 0.000 description 14
- 229910052751 metal Inorganic materials 0.000 description 8
- 239000002184 metal Substances 0.000 description 8
- 239000004094 surface-active agent Substances 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
- UIFOTCALDQIDTI-UHFFFAOYSA-N arsanylidynenickel Chemical compound [As]#[Ni] UIFOTCALDQIDTI-UHFFFAOYSA-N 0.000 description 4
- 239000002131 composite material Substances 0.000 description 4
- 238000007772 electroless plating Methods 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 239000011246 composite particle Substances 0.000 description 1
- 239000011231 conductive filler Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000011549 displacement method Methods 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 230000005291 magnetic effect Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000011859 microparticle Substances 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 230000002085 persistent effect Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 239000003223 protective agent Substances 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001507 sample dispersion Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
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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-silvercoreshell 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 the component of two or more, has unique or various character, therefore has wider application than single nano particle, therefore, in recent years, in the persistent exploration process to the high-performance new material, synthesizing of composite nanoparticle, preparation and application more and more attract much attention, 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 have the good metallic character of clad, so the nuclear shell structure nano bimetallic material is at electronics, biology sensor, field such as optics and catalysis has a wide range of applications.
Hud typed nickel-Yin composite micro-powder refers to 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 the macro-control to nickel powder character, this nucleocapsid structure has not only kept the physical and chemical performance of original metallic nickel core, also has the good metallic character of silver coating, improve non-oxidizability and the heat endurance of simple nickel powder, kept the high conductivity of nickel and 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 saving 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 inhomogeneous; therefore, the nickel-galactic nucleus shell structure for preparing evenly, coats 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; utilize 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; have at present in the powder surface plated with gold; silver; platinum; nickel; copper; the report of cobalt etc.; this method is easy to operate, and technology is simple, and thickness of coating evenly and be easy to control; outward appearance is good; at present, the report of relevant nanometer nickeline nucleocapsid structure preparation is less, and prepared nano particle coating degree is lower; and need to add protective agent in the course of reaction; the present invention is not adding the nanometer nickel-galactic nucleus shell structural nano particle that has prepared good dispersion under protectant condition with electroless plating method on existing basis, and adopts X-ray diffraction; various modern analysis means such as transmission electron microscope characterize its structure.
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 as follows: 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, described 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 described sensitization is as follows: 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 AgNO
3Whether the adularescent precipitation 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 precipitation 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 example 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 example 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 example 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 example 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 example 4 prepared samples, and the nickel consumption is 3mmol, and the silver nitrate consumption is respectively 4mmol, adds surfactant.
The specific embodiment
The present invention will be further described below in conjunction with concrete embodiment.
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, by checking the card of answering as can be seen, the characteristic peak that has nickel and silver in the spectrogram, the characteristic peak that does not have its oxide, it is 38.2 ° at 2 θ wherein, 44.4 °, 64.6 °, 77.6 ° characteristic peak (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 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, wherein the volume ratio of 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 more thick.Therefore, the thickness of silver-colored shell can be controlled by 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.When being 0.5g with sodium hydroxide concentration the transmission electron microscope picture of sample more as can be seen, whether the existence of NaOH does not have obvious influence to pattern, the coating degree of product.But we find in the experimentation, when no NaOH in the system and other conditions all under the same situation, react and still have Ag in the solution more than five hours
+Exist, and add after the NaOH, reaction only needed to finish 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, 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 as follows: 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; 3) 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: described 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 described sensitization is as follows: it is 5% SnCl that nano-nickel powder is joined mass fraction
2Hydrochloric acid solution in soak, the time is 5min, after the washing repeatedly of nickel powder after the sensitization, filter liquor AgNO
3Whether the adularescent precipitation 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, it 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: step 2) in the volume ratio of second alcohol and water be 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: reaction finishes the back and separates the supernatant that obtains with magnet whether the adularescent precipitation generates with the watery hydrochloric acid titration, 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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| 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 |
| 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 |
| CN105598467B (en) * | 2016-01-20 | 2018-11-27 | 哈尔滨工业大学深圳研究生院 | A kind of preparation method of the high temperature resistant silver nickel coat copper-clad conductive powder body with core-shell structure |
| CN106583712B (en) * | 2016-11-28 | 2018-08-28 | 清华大学 | A kind of preparation method of wicker copper nano particle |
| 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 |
| 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 |
| 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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| CN102228994A (en) * | 2011-06-20 | 2011-11-02 | 厦门大学 | Method for preparing monodisperse silver core-nickel shell nanoparticles |
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| Ag nanoshell-induced dual-frequency electromagnetic wave absorption of Ni nanoparticles;Chung-Che Lee and Dong-Hwang Chen;《Applied Physics Letters》;20070507;1-3 * |
| Chen, Dong-Hwang et al.,.Protective agent-free synthesis of Ni–Ag core–shell nanoparticles.《Materials Chemistry and Physics》.2006,468-471. |
| Chung-Che Lee and Dong-Hwang Chen.Ag nanoshell-induced dual-frequency electromagnetic wave absorption of Ni nanoparticles.《Applied Physics Letters》.2007, |
| Large-scale synthesis of Ni-Ag core-shell nanoparticles with magnetic, optical and anti-oxidation properties;Lee CC and Chen DH;《NANOTECHNOLOGY》;20060714;第17卷(第13期);3094-3099 * |
| LeeCCandChenDH.Large-scalesynthesisofNi-Agcore-shellnanoparticleswithmagnetic optical and anti-oxidation properties.《NANOTECHNOLOGY》.2006 |
| Protective agent-free synthesis of Ni–Ag core–shell nanoparticles;Chen, Dong-Hwang et al.,;《Materials Chemistry and Physics》;20060221;468-471 * |
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|---|---|
| CN102407329A (en) | 2012-04-11 |
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