CN102228994A - Method for preparing monodisperse silver core-nickel shell nanoparticles - Google Patents
Method for preparing monodisperse silver core-nickel shell nanoparticles Download PDFInfo
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- CN102228994A CN102228994A CN2011101650022A CN201110165002A CN102228994A CN 102228994 A CN102228994 A CN 102228994A CN 2011101650022 A CN2011101650022 A CN 2011101650022A CN 201110165002 A CN201110165002 A CN 201110165002A CN 102228994 A CN102228994 A CN 102228994A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
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Abstract
The invention relates to metal nanoparticles of a core-shell structure and provides a method for preparing monodisperse silver core-nickel shell nanoparticles and application of monodisperse silver core-nickel shell nanoparticles to catalysis of sodium borohydride for hydrolysis hydrogen production, wherein the method has a simple process and can ensure the monodispersity of products. The method comprises the steps of: adding a mixed solution of metal salt of nickel, metal salt of silver, a surface stabilizing agent, alkylamine or alkylamine and a high-boiling-point organic solvent into a reaction vessel under the protection of inert gas, homogenizing the mixture, heating to 170-240 DEG C and preserving the temperature for 20min-3h to obtain a reaction product; and cleaning the obtained reaction product with an organic solvent mixed solution, centrifuging for separation, and vacuum-drying to obtain the monodisperse silver core-nickel shell nanoparticles. The monodisperse silver core-nickel shell nanoparticles can be applied to catalysis of the sodium borohydride for hydrolysis hydrogen production. The method has the advantages of simple preparation process, relatively low cost and convenience for industrial production.
Description
Technical field
The present invention relates to a kind of metal core-shell structure nanometer particle, especially relating to a kind of is that nuclear, nickel are shell with silver, is preparation method and its application on the catalysis preparing hydrogen by sodium borohydride hydrolysis of monodispersed nuclear shell structured nano-particle.
Background technology
Along with deepening continuously of nanotechnology research, it is found that two kinds or two or more nano particles are combined effectively by certain mechanism, can cause a lot of excellent physics and the appearance of chemical property.Wherein the core-shell nano structure is the most typical.The core-shell nano structure is assembled the shell material in order on nuclear by chemical bond or other interaction and is formed.The nano particle of this structure is except can combining the multiple function of nuclear and shell, also because the synergy at its interface produces new performance.Thereby the nano particle of nucleocapsid structure has abundant and excellent more physics, chemical property than single component nano particle, has important use to be worth in fields such as medical science, biology, catalysis, electricity, magnetics and optics.
An important application of metal core-shell structure nanometer particle is catalysis.Hud typed structure nano particle catalyst can be by the control shell thickness and distribute realize control to catalytic reaction.This type of catalyst mainly contains noble metal-noble metal type, noble metal-transition metal type, metal-oxide type, oxide-oxide type etc.Wherein metal-metal type catalyst all has catalytic activity and stability preferably to reactions such as the CO selective oxidation under the reduction of the electroxidation in the fuel cell, organic matter hydrogenation, the rich hydrogen condition, environmental catalysis.Along with the aggravation of environmental pollution, society becomes very urgent to the demand of clean energy resource in recent years, and hydrogen energy source causes that as a kind of clean energy resource people pay close attention to greatly.There is very big application potential in the boron hydride salt as a kind of storage hydrogen compound of cheapness aspect hydrogen energy source.It can be under the effect of catalyst hydrolysis and generation hydrogen that can continuous controllable.Yet the catalyst of participating in hydrolysis generally is difficult to reclaim, and this has not only caused very big waste, and has polluted environment.Therefore, develop a kind of easy method synthetic callable, stable catalyst is imperative.
Magnesium-yttrium-transition metal has a wide range of applications at catalytic field.Block cobalt, nickel and the Raney's nickel that has been found that (Raney nickel) all has the ability (J.Chem.Soc.Dalton.Trans.1985 that the catalysis sodium borohydride decomposes, 307), but its catalytic activity is not high enough, can not satisfy the requirement that quick decomposition produces hydrogen.Ru nano particle (the J.Hydrogen Energ.2000 of report such as Amendola, 25,969) and Ni-Ru nano particle (the Int.J.Hydrogen Energ. of report such as Liu, 2009,34,2153), though have advantages of high catalytic activity, but its complex process, and the costing an arm and a leg of Ru are unfavorable for that heavy industrialization uses.
For silver-colored nickel binary system core-shell nano, report before is the structure that silver coats nickel substantially, though this structure has important application at biological, medical domain, its catalytic effect is not ideal enough.The catalysis characteristics of nickel excellence then can be given full play to and promote to the structure of nickel coated with silver.About the preparation of galactic nucleus-nickel core/shell nanoparticles, still there is not report at home, external report is also few.(Chem.Mater.2009,21,5222) such as nearest zhang have been reported with " two step method " preparation galactic nucleus-nickel core/shell nanoparticles, have promptly been prepared silver-colored seed earlier, coat nickel again.Owing to do not introduce suitable surface stabilizer, prepared product particle diameter distributes even inadequately, fails to reach single dispersion, and the report of catalytic applications is not arranged yet.
Summary of the invention
It is simple that purpose of the present invention aims to provide a kind of technology, can guarantee single preparation method who disperses galactic nucleus-nickel core/shell nanoparticles of the monodispersity of product.
Another object of the present invention is to provide the described single galactic nucleus-application of nickel core/shell nanoparticles on the catalysis preparing hydrogen by sodium borohydride hydrolysis that disperse.
Single preparation method of galactic nucleus-nickel core/shell nanoparticles that disperses of the present invention adopts " one-step method "; with the organic metal salt of nickel as the nickel source; inorganic or organic metal salt with silver is silver-colored source; under the protection of inert gas; it is mixed in the mixed system that contains alkylamine and surface stabilizer, slowly be heated to reaction temperature, and insulation is worn out and prepared the monodispersed core-shell structural nano particle under this temperature.
Single preparation method of galactic nucleus-nickel core/shell nanoparticles that disperses of the present invention may further comprise the steps:
1) under the protection of inert gas, the slaine of nickel, slaine, surface stabilizer, alkylamine or the alkylamine of silver and the mixed liquor of high boiling organic solvent are added in the reaction vessel, make the mixture homogenising, be warming up to 170～240 ℃ and under this temperature, be incubated 20min～3h again, obtain product;
In step 1), the described temperature of mixture homogenising that makes can be 60～100 ℃, and is incubated 5～20min down at 60～100 ℃; The slaine of described nickel can be selected from a kind of in nickel acetylacetonate, nickel formate, the nickel acetate etc., and the slaine of described silver can be selected from silver nitrate or silver acetate etc.; Described surface stabilizer can be selected from triphenylphosphine or tri octyl phosphine etc.; Described alkylamine can be selected from a kind of in oleyl amine, lauryl amine, the cetylamine etc.; Described high boiling organic solvent can be selected from a kind of in octadecylene, diphenyl ether, the benzyl ether etc.; The ratio range of slaine, surface stabilizer, alkylamine or the alkylamine of the slaine of described nickel, silver and the mixed liquor of high boiling organic solvent can be: the slaine of nickel is 0.1～1mmol; The slaine of silver is 0.1～0.5mmol; Surface stabilizer is 0.05～2mmol; The amount of the mixture of alkylamine and high boiling organic solvent is 4～20ml, and wherein alkylamine content can be 20%～100%.
2) product of step 1) gained is cleaned with the organic solvent mixed liquor, centrifugation, vacuum drying obtains single galactic nucleus-nickel core/shell nanoparticles that disperses at last.
In step 2) in, described organic solvent can be selected from a kind of in n-hexane, ethanol, the acetone etc.
Spherical in shape substantially with single galactic nucleus-nickel core/shell nanoparticles pattern that disperses that the present invention obtains, the galactic nucleus size is constant substantially, and about 12nm, the nickel shell thickness then can be regulated by the organic metal salt content that changes reaction temperature, temperature retention time and nickel.
The prepared single galactic nucleus-nickel core/shell nanoparticles that disperses of the present invention can be used for the reaction of catalysis preparing hydrogen by sodium borohydride hydrolysis, concrete steps are: prepared single galactic nucleus-nickel core/shell nanoparticles that disperses is positioned in the 10ml microreactor, reactor is put into the isothermal reaction groove, behind the insulation 10min, inject 3～10ml alkalescence sodium borohydride solution, the hydrolysis of catalysis sodium borohydride produces hydrogen under magnetic agitation, use downward drainage to collect hydrogen, calculate the generation speed of hydrogen by timing, reaction adds magnetic field after finishing, and reclaims catalyst.
Compare with the method for preparing core-shell structure nanometer particle of bibliographical information, the present invention uses " one-step method ", settles the synthetic kernel shell structure at one go in a temperature-rise period, and preparation technology is simple, and cost is cheap relatively, is convenient to suitability for industrialized production.The galactic nucleus that the present invention prepares-nickel core/shell nanoparticles monodispersity is good, the galactic nucleus with single-size, and nickel layer thickness is adjustable, and then can regulate the magnetism characteristic of nano particle, makes it have characteristics such as can utilizing reclaim in magnetic field, separation.Simultaneously, nano particle has non-reunion and is difficult for advantages such as oxidation, so it is applied widely, not only can be used as high performance catalyst, and can be used for self assembly magnetic material, welding material and electrode material etc.Fully demonstrated the superiority of bimetallic nucleocapsid structure aspect catalysis, can be used widely in the Industrial Catalysis field.
Description of drawings
Fig. 1 is the transmission electron microscope photo of the prepared galactic nucleus-nickel core/shell nanoparticles of embodiment 1.In Fig. 1, scale is 20nm.
Fig. 2 is the high power transmission electron microscope photo of the prepared galactic nucleus-nickel core/shell nanoparticles of embodiment 1.In Fig. 2, scale is 5nm.
Fig. 3 is the X-ray diffractogram of the prepared galactic nucleus-nickel core/shell nanoparticles of embodiment 1.In Fig. 3, abscissa is angle of diffraction 2Theta (degree), and ordinate is diffracted intensity Intensity (a.u.); Diffraction maximum is respectively the mixing diffraction maximum of fcc structure silver and fcc structure nickel, Ag (111) is wherein arranged, Ag (200), Ag (220), Ni (111), Ni (200).
Fig. 4 is the prepared galactic nucleus-nickel core/shell nanoparticles transmission electron microscope photo of embodiment 2.In Fig. 4, scale is 100nm.
Fig. 5 is the high power transmission electron microscope photo of the galactic nucleus-nickel core/shell nanoparticles of embodiment 2 preparations.In Fig. 5, scale is 5nm.
Fig. 6 is the transmission electron microscope photo of the prepared galactic nucleus-nickel core/shell nanoparticles of embodiment 3.In Fig. 6, scale is 100nm.
Fig. 7 is the high power transmission electron microscope photo of the galactic nucleus-nickel core/shell nanoparticles of embodiment 3 preparations.In Fig. 7, scale is 5nm.
The transmission electron microscope photo of galactic nucleus-nickel core/shell nanoparticles that Fig. 8 embodiment 4 is prepared.In Fig. 8, scale is 20nm.
Fig. 9 is that the galactic nucleus-nickel core/shell nanoparticles of preparation among the embodiment 2 produces the output V of hydrogen and the curve of time t 40 ℃ of following catalysis sodium borohydride hydrolysis.In Fig. 9, abscissa is time (s), and ordinate is hydrogen output Volune (mL).
(curve a) and the hysteresis curve that records under the 300K (curve b) at 5K for galactic nucleus-nickel core/shell nanoparticles among the embodiment 2 for Figure 10.Abscissa is magnetic field intensity H (Oe), and ordinate is specific magnetization Magnetization (emu/g).
The specific embodiment
Embodiment 1
0.4mmol nickel acetylacetonate, 0.1mmol silver nitrate, 0.6mmol triphenylphosphine and 6ml oleyl amine are added in the there-necked flask; under the protection of argon gas, mix; be warming up to 80 ℃ after stirring 10min; insulation 15min fully mixes reactant; slowly be warming up to 180 ℃ then; insulation 40min naturally cools to room temperature then in air.Add ethanol nanoparticle precipitate is got off, by centrifugal taking-up reaction mother liquor, use acetone and n-hexane mixed solution cyclic washing then three times, last vacuum drying obtains the powder of black.Fig. 1 is the transmission electron microscope photo of this product, and its pattern is spherical, and narrow particle size distribution, particle diameter are about 15 nanometers; Fig. 2 is the high power transmission electron microscope photo of this product, can obviously observe nucleocapsid structure, and the thickness of nickel dam is about 1.6 nanometers.Fig. 3 is the X-ray diffractogram of this product, and its diffraction maximum is the compound of fcc structure silver and fcc structure nickel.
Embodiment 2
0.4mmol nickel acetylacetonate, 0.1mmol silver nitrate, 0.3mmol triphenylphosphine and 6ml oleyl amine are added in the there-necked flask; under the protection of argon gas, mix; be warming up to 80 ℃ after stirring 10min; insulation 15min fully mixes reactant; slowly be warming up to 200 ℃ then; insulation 60min naturally cools to room temperature then in air.Add ethanol nanoparticle precipitate is got off, by centrifugal taking-up reaction mother liquor, use acetone and n-hexane mixed solution cyclic washing then three times, last vacuum drying obtains the powder of black.Fig. 4 is the transmission electron microscope photo of this product, and its pattern is spherical, and narrow particle size distribution, particle diameter are about 17 nanometers; Fig. 5 is the high power transmission electron microscope photo of this product, can obviously observe nucleocapsid structure, and the thickness of nickel dam is about 2.5 nanometers.The X-ray diffractogram of this product is consistent with Fig. 3, illustrates that product is nickel compound of the silver of fcc structure and fcc structure.
Embodiment 3
0.4mmol nickel acetylacetonate, 0.1mmol silver nitrate, 0.1mmol triphenylphosphine and 6ml oleyl amine are added in the there-necked flask; under the protection of argon gas, mix; be warming up to 80 ℃ after stirring 10min; insulation 15min fully mixes reactant; slowly be warming up to 220 ℃ then; insulation 60min naturally cools to room temperature then in air.Add ethanol nanoparticle precipitate is got off, by centrifugal taking-up reaction mother liquor, use acetone and n-hexane mixed solution cyclic washing then three times, last vacuum drying obtains the powder of black.Fig. 6 is the transmission electron microscope photo of this product, and its pattern is spherical, and narrow particle size distribution, particle diameter are about 19 nanometers; Fig. 7 is the high power transmission electron microscope photo of this product, can obviously observe nucleocapsid structure, and the thickness of nickel dam is about 3.5 nanometers.The X-ray diffractogram of this product is consistent with Fig. 3, illustrates that product is nickel compound of the silver of fcc structure and fcc structure.
Embodiment 4
0.5mmol nickel acetylacetonate, 0.1mmol silver acetate, 0.5mmol tri octyl phosphine and 4ml octadecylene and 3ml oleyl amine are added in the there-necked flask; under the protection of argon gas, mix; be warming up to 80 ℃ after stirring 10min; insulation 15min fully mixes reactant; slowly be warming up to 200 ℃ then; insulation 45min naturally cools to room temperature then in air.Add ethanol nanoparticle precipitate is got off, by centrifugal taking-up reaction mother liquor, use acetone and n-hexane mixed solution cyclic washing then three times, last vacuum drying obtains the powder of black.Fig. 8 is the transmission electron microscope photo of this product, and its pattern is spherical, and narrow particle size distribution, particle diameter are about 14 nanometers.The X-ray diffractogram of this product is consistent with Fig. 3, illustrates that product is nickel compound of the silver of fcc structure and fcc structure.
Adopt example 2 prepared galactic nucleus-nickel core/shell nanoparticles catalyst 25mg, produce hydrogen in the solution hydrolysis of 40 ℃ of following catalysis 4ml alkalescence sodium borohydrides (10wt% sodium borohydride and 10wt% NaOH).Fig. 9 is the curve of hydrogen output V and time t.The generation speed of hydrogen is: 1928ml/ming.
Embodiment 6
The recyclable aptitude tests of magnetic.Embodiment 2 prepared galactic nucleus-nickel shell structural nano particle is dispersed in the toluene, and ultrasonic concussion back obtains uniform colloid, adds magnetic field then, and all particles are inhaled on tube wall behind about 1min, remain limpid toluene solution.Can illustrate after prepared nanoparticulate dispersed is in solution and be easy to collect by adding before the magnetic field toluene solution of the galactic nucleus-nickel core/shell nanoparticles of (left side) back (right side) by externally-applied magnetic field.The prepared nano particle of Figure 10 5K (curve a) and the hysteresis curve that records under the 300K (curve b) illustrates that prepared nano particle at room temperature is superparamagnetism, and next at 5K be ferromagnetism.
Claims (10)
1. single preparation method who disperses galactic nucleus-nickel core/shell nanoparticles is characterized in that may further comprise the steps:
1) under the protection of inert gas, the slaine of nickel, slaine, surface stabilizer, alkylamine or the alkylamine of silver and the mixed liquor of high boiling organic solvent are added in the reaction vessel, make the mixture homogenising, be warming up to 170～240 ℃ and under this temperature, be incubated 20min～3h again, obtain product;
2) product of step 1) gained is cleaned with the organic solvent mixed liquor, centrifugation, vacuum drying obtains single galactic nucleus-nickel core/shell nanoparticles that disperses at last.
2. a kind of single preparation method who disperses galactic nucleus-nickel core/shell nanoparticles as claimed in claim 1 is characterized in that in step 1), and described to make the temperature of mixture homogenising be 60～100 ℃, and at 60～100 ℃ of insulation 5～20min down.
3. a kind of single preparation method who disperses galactic nucleus-nickel core/shell nanoparticles as claimed in claim 1 is characterized in that in step 1), and the slaine of described nickel is selected from a kind of in nickel acetylacetonate, nickel formate, the nickel acetate.
4. a kind of single preparation method who disperses galactic nucleus-nickel core/shell nanoparticles as claimed in claim 1 is characterized in that in step 1) the slaine of described silver is selected from silver nitrate or silver acetate.
5. a kind of single preparation method who disperses galactic nucleus-nickel core/shell nanoparticles as claimed in claim 1 is characterized in that in step 1) described surface stabilizer is selected from triphenylphosphine or tri octyl phosphine.
6. a kind of single preparation method who disperses galactic nucleus-nickel core/shell nanoparticles as claimed in claim 1 is characterized in that in step 1), and described alkylamine is selected from a kind of in oleyl amine, lauryl amine, the cetylamine.
7. a kind of single preparation method who disperses galactic nucleus-nickel core/shell nanoparticles as claimed in claim 1 is characterized in that in step 1), and described high boiling organic solvent is selected from a kind of in octadecylene, diphenyl ether, the benzyl ether.
8. a kind of single preparation method who disperses galactic nucleus-nickel core/shell nanoparticles as claimed in claim 1, it is characterized in that in step 1) the ratio range of slaine, surface stabilizer, alkylamine or the alkylamine of the slaine of described nickel, silver and the mixed liquor of high boiling organic solvent is: the slaine of nickel is 0.1～1mmol; The slaine of silver is 0.1～0.5mmol; Surface stabilizer is 0.05～2mmol; The amount of the mixture of alkylamine and high boiling organic solvent is 4～20ml, and wherein alkylamine content is 20%～100%.
9. a kind of single preparation method who disperses galactic nucleus-nickel core/shell nanoparticles as claimed in claim 1 is characterized in that in step 2) in, described organic solvent is selected from a kind of in n-hexane, ethanol, the acetone.
10. be used for the reaction of catalysis preparing hydrogen by sodium borohydride hydrolysis as a kind of single prepared single galactic nucleus-nickel core/shell nanoparticles that disperses of preparation method of galactic nucleus-nickel core/shell nanoparticles that disperses as described in one of in the claim 1～9.
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102407329A (en) * | 2011-11-18 | 2012-04-11 | 江苏大学 | Method for preparing nickel-silver coreshell structure nanoparticles |
| CN103008660A (en) * | 2012-12-21 | 2013-04-03 | 大连理工大学 | Method for preparing shape-controlled core-shell uniform particles |
| CN103071788A (en) * | 2012-10-31 | 2013-05-01 | 江苏大学 | Method of preparing nickel-silver nuclear shell structure nano-particles |
| CN103769584A (en) * | 2014-01-03 | 2014-05-07 | 西北师范大学 | Method for preparing nanometer particles of nickel-carbide nickel core-shell structure |
| CN104507600A (en) * | 2012-08-02 | 2015-04-08 | 国立大学法人山形大学 | Process for producing covered silver fine particles and covered silver fine particles produced by said process |
| CN104959626A (en) * | 2015-06-30 | 2015-10-07 | 厦门大学 | Method for preparing multifunctional core-shell nano-material by using alloy to wrap copper nanowires |
| CN105414558A (en) * | 2015-11-11 | 2016-03-23 | 中国科学院山西煤炭化学研究所 | Preparation method of mono-dispersed spherical nano copper and ferrum |
| CN106077699A (en) * | 2016-06-30 | 2016-11-09 | 青岛科技大学 | A kind of preparation method of silver ferrite composite nanometer particle |
| CN106141171A (en) * | 2015-04-27 | 2016-11-23 | 中国科学院宁波材料技术与工程研究所 | Hud typed superstructure nano material, its preparation method and application |
| CN108311710A (en) * | 2018-02-28 | 2018-07-24 | 深圳市航天新材科技有限公司 | A kind of preparation method of the anti-oxidant nanoscale nickel powder of monodisperse |
| CN110294969A (en) * | 2018-03-21 | 2019-10-01 | Tcl集团股份有限公司 | Ink and preparation method thereof |
| 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 |
| 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 (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102407329A (en) * | 2011-11-18 | 2012-04-11 | 江苏大学 | Method for preparing nickel-silver coreshell structure nanoparticles |
| CN102407329B (en) * | 2011-11-18 | 2013-09-11 | 江苏大学 | Method for preparing nickel-silver coreshell structure nanoparticles |
| CN104507600A (en) * | 2012-08-02 | 2015-04-08 | 国立大学法人山形大学 | Process for producing covered silver fine particles and covered silver fine particles produced by said process |
| CN103071788A (en) * | 2012-10-31 | 2013-05-01 | 江苏大学 | Method of preparing nickel-silver nuclear shell structure nano-particles |
| CN103008660A (en) * | 2012-12-21 | 2013-04-03 | 大连理工大学 | Method for preparing shape-controlled core-shell uniform particles |
| CN103008660B (en) * | 2012-12-21 | 2014-11-12 | 大连理工大学 | Method for preparing shape-controlled core-shell uniform particles |
| CN103769584A (en) * | 2014-01-03 | 2014-05-07 | 西北师范大学 | Method for preparing nanometer particles of nickel-carbide nickel core-shell structure |
| CN106141171B (en) * | 2015-04-27 | 2018-06-05 | 中国科学院宁波材料技术与工程研究所 | Hud typed superstructure nano material, its preparation method and application |
| CN106141171A (en) * | 2015-04-27 | 2016-11-23 | 中国科学院宁波材料技术与工程研究所 | Hud typed superstructure nano material, its preparation method and application |
| CN104959626B (en) * | 2015-06-30 | 2017-02-22 | 厦门大学 | Method for preparing multifunctional core-shell nano-material by using alloy to wrap copper nanowires |
| CN104959626A (en) * | 2015-06-30 | 2015-10-07 | 厦门大学 | Method for preparing multifunctional core-shell nano-material by using alloy to wrap copper nanowires |
| CN105414558A (en) * | 2015-11-11 | 2016-03-23 | 中国科学院山西煤炭化学研究所 | Preparation method of mono-dispersed spherical nano copper and ferrum |
| CN106077699A (en) * | 2016-06-30 | 2016-11-09 | 青岛科技大学 | A kind of preparation method of silver ferrite composite nanometer particle |
| CN108311710A (en) * | 2018-02-28 | 2018-07-24 | 深圳市航天新材科技有限公司 | A kind of preparation method of the anti-oxidant nanoscale nickel powder of monodisperse |
| CN110294969A (en) * | 2018-03-21 | 2019-10-01 | Tcl集团股份有限公司 | Ink and preparation method thereof |
| 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 |
| 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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