CN101433965A - Method for preparing monodisperse nickel nanoparticle - Google Patents
Method for preparing monodisperse nickel nanoparticle Download PDFInfo
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- CN101433965A CN101433965A CNA2008100724050A CN200810072405A CN101433965A CN 101433965 A CN101433965 A CN 101433965A CN A2008100724050 A CNA2008100724050 A CN A2008100724050A CN 200810072405 A CN200810072405 A CN 200810072405A CN 101433965 A CN101433965 A CN 101433965A
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Abstract
The invention discloses a method for preparing a monodispersed nickel nanoparticles, and relates to nickel nanoparticles. The invention provides a method for preparing monodispersed nickel nanoparticles which have common ferromagnetic property as well as high performance, monodispersion, insusceptibility to oxidizationm, non-agglomeration, nonferromagnetic property and other characteristics and expand application range of nickel nanoparticles. Under protection of inert gases, an organic metal salt of nickel, alkylamine, a surface stabilizer and an organic solvent are mixed, stirred, kept at 106 to 160 DEG C and then heated to 180 to 350 DEG C. Reaction products are collected, washed by using the organic solvent, centrifuged and subjected to vacuum drying to obtain monodispersed nickel nanoparticles. The method is simple in process, short in preparation period, rich in raw material resources and relatively low in cost and can prepare nickel nanoparticles which can be used as high-performance catalysts, magnetic materials, welding materials, electrode materials and so on.
Description
Technical field
The present invention relates to a kind of nickel nano particle, especially relate to a kind of preparation method of monodisperse nickel nanoparticle.
Background technology
The technology of preparing of nano particle is a key link of nano materials research, development and application.Nickel is a kind of important magnetic magnesium-yttrium-transition metal.Nickel nano particle has a wide range of applications in numerous field such as magnetics, electricity, catalysis, medicine and biology.Developed in recent years and some and prepare the method for nickel nano particle.Wherein one of topmost preparation method is the wet chemistry method reduction of metallic compound.Compare with the general physical preparation method, this method has advantages such as cost is cheap relatively, the simple relatively and easy realization amplification of technology path production, this method has been widely used in the preparation of noble metal (gold, platinum and palladium etc.), but because the electronegativity of nickel is higher, the reduction reaction of its compound is difficulty relatively.Chen D.H. etc. (J.Mater.Chem., 2002, reported at aqueous phase prepared nickel nano particle 12:2412) that though this method is comparatively simple, the nano particle diameter of preparing is inhomogeneous, and easily reunited by hydrazine hydrate reduction nickel inorganic salts.Toneguzzo P. etc. (J.Mater.Sci., 2000,35:3767) adopt how pure reducing process to prepare particle diameter nickel nano particle relatively uniformly, but the size of particle is difficult to be controlled at below 20 nanometers generally at submicron order.Domestic Liu Xiansong etc. (Rare Metals Materials and engineering, 2006,35:1457) the how pure reducing process of assisting with microwave has prepared the nickel nanosphere of diameter range 100～180nm.Gong Jie etc. (SCI, 2007,28:1232) reported with sol-gel process and prepare the nickel nano particle that average grain size is the tightly packed phase of six sides of 12 nanometers, but the particle diameter of product distributes and do not reach single dispersion as yet.(Adv.Mater. such as the Park J. of Korea S, 2005,17:429) adopt the high-temperature liquid-phase reducing process successfully to prepare the nickel nano particle of single dispersion, non-reunion, be solvent but this method adopts the higher alkylphosphines thing of cost, and the easy oxidation of nano particle can only obtain single crystal phase.
In sum, though reported both at home and abroad the preparation method of many nickel nano particles, these methods in the control grain size, be difficult to the control particle diameter distribute with crystal mutually.In addition, how to prevent that nickel nano particle oxidation and reunion from also being a difficult point.
Summary of the invention
The present invention aims to provide a kind of nickel nano particle of preparing not only can have general ferromagnetic characteristic, and have high-performance, singly disperse, be difficult for characteristics such as oxidation, non-reunion and nonferromagnetic, can expand the preparation method of the monodisperse nickel nanoparticle of nickel nano particle application space.
Technical scheme of the present invention is that organic metal salt with nickel is as the nickel source; under the protection of inert gas; it is mixed containing alkylamine/surface stabilizer or contain in the reaction system of high boiling organic solvent/surface stabilizer of non-conformability, be heated to the monodisperse nickel nanoparticle that reaction temperature prepares the different crystal phase rapidly.
The present invention includes following steps:
1) under the protection of inert gas, after organic metal salt, alkylamine, surface stabilizer and the organic solvent mixing stirring with nickel,, rise to 180～350 ℃ of reactions again 100～160 ℃ of insulations, get product;
2) product of step 1) gained is cleaned with organic solvent, centrifugal, vacuum drying gets monodisperse nickel nanoparticle.
In step 1), the organic metal salt of nickel is selected from nickel acetylacetonate, anhydrous formic acid nickel, contains crystallization water nickel formate, anhydrous acetic acid nickel, contain a kind of in crystallization water nickel acetate and the oleic acid nickel etc., alkylamine is selected from a kind of in octylame, lauryl amine, cetylamine, oleyl amine and the trioctylamine etc., surface stabilizer is selected from the alkylphosphines thing, and organic solvent is selected from a kind of in octadecylene, diphenyl ether and the benzyl ether etc.; The alkylphosphines thing can be selected from a kind of in tributylphosphine, tri octyl phosphine, trioctylphosphine oxide (TOPO) and the triphenylphosphine etc., and the molar concentration of the organic metal salt of nickel is 0.05～0.5mol/L, and the mol ratio of the organic metal salt of surface stabilizer and nickel is 0.1～5; Press mass ratio, the organic metal salt of nickel: alkylamine: surface stabilizer: the proportioning of organic solvent is 1: (5～80): (0.3～10): (5～80); The time of mixing stirring is preferably 1～20min, and the time of insulation can be 1min～6h, is preferably 45min.
In step 2) in, organic solvent can be selected ethanol or hexane etc. for use.
The organic solvent that organic metal salt, alkylamine, surface stabilizer and the organic solvent mixing of nickel are stirred is a kind of high boiling organic solvent of non-conformability, in preparation process, the particle size of nickel nano particle is controlled by the concentration of reaction temperature and surface stabilizer, and crystal is then controlled by the alkylamine of different proportion and the high boiling organic solvent of non-conformability mutually.
Compare with the similar preparation method of domestic and international report, the present invention is owing to employing " one-step method ", so preparation technology is simple, and manufacturing cycle is short, and cost is cheap relatively, is convenient to amplificationization production.Because the nickel nano particle that the present invention prepares presents the monodispersity of height, not only the size of nano particle can be regulated and control, its crystal also can be controlled mutually, and the nickel nano particle that obtains has non-reunion and is difficult for advantages such as oxidation, therefore it is applied widely, can be used as high performance catalyst, self assembly magnetic material, welding material and electrode material etc.Especially prepare the nickel nano particle of six side's close-packed structures, shown and all right different magnetism characteristic of ferromagnetism nickel, expanded the application space of nickel nano particle.
Description of drawings
Fig. 1 is the transmission electron microscope photo of the prepared nickel nano particle of embodiment 1.In Fig. 1, scale is 20nm.
Fig. 2 is the X-ray powder diffraction figure of the prepared nickel nano particle of embodiment 1.In Fig. 2, abscissa is the angle of diffraction 2 θ (degree), and ordinate is diffracted intensity Intensity (a.u.); Diffraction maximum is respectively (111), (200), (220).
Fig. 3 is the transmission electron microscope photo of the prepared nickel nano particle of embodiment 2.In Fig. 3, scale is 50nm.
Fig. 4 is the X-ray powder diffraction figure of the prepared nickel nano particle of embodiment 2.In Fig. 4, abscissa is the angle of diffraction 2 θ (degree), and ordinate is diffracted intensity Intensity (a.u.); Diffraction maximum is respectively (111), (200), (220).
Fig. 5 is the transmission electron microscope photo of the prepared nickel nano particle of embodiment 3.
Fig. 6 is the X-ray powder diffraction figure of the prepared nickel nano particle of embodiment 3.In Fig. 6, abscissa is the angle of diffraction 2 θ (degree), and ordinate is diffracted intensity Intensity (a.u.); Diffraction maximum is respectively (111), (200), (220), (311), (222).
Fig. 7 is the transmission electron microscope photo of the prepared nickel nano particle of embodiment 4.In Fig. 7, scale is 100nm.
Fig. 8 is the X-ray powder diffraction figure of the prepared nickel nano particle of embodiment 4.In Fig. 8, abscissa is the angle of diffraction 2 θ (degree), and ordinate is diffracted intensity Intensity (a.u.); Diffraction maximum is respectively (111), (200), (220).
Fig. 9 is the transmission electron microscope photo of the prepared nickel nano particle of embodiment 5.In Fig. 9, scale is 50nm.
Figure 10 is the X-ray powder diffraction figure of the prepared nickel nano particle of embodiment 5.In Figure 10, abscissa is the angle of diffraction 2 θ (degree), and ordinate is diffracted intensity Intensity (a.u.); Diffraction maximum is respectively (010), (002), (011), (012), (110), (103), (112), (201).
Figure 11 is the transmission electron microscope photo of the prepared nickel nano particle of embodiment 6.In Figure 11, scale is 100nm.
Figure 12 is the X-ray powder diffraction figure of the prepared nickel nano particle of embodiment 6.In Figure 12, abscissa is the angle of diffraction 2 θ (degree), and ordinate is diffracted intensity Intensity (a.u.); Diffraction maximum is respectively (010), (002), (011), (012), (110), (103), (112), (201).
Figure 13 is the transmission electron microscope photo of the prepared nickel nano particle of embodiment 7.
Figure 14 is the X-ray powder diffraction figure of the prepared nickel nano particle of embodiment 7.In Figure 14, abscissa is the angle of diffraction 2 θ (degree), and ordinate is diffracted intensity Intensity (a.u.); Diffraction maximum is respectively (010), (002), (011), (012), (110), (103), (112), (201).
Figure 15 is the typical room temperature hysteresis curve of the fcc phase nickel nano particle of the embodiment of institute 3 preparations.In Figure 15, abscissa is magnetic field Magnetic field (Oe), and ordinate is intensity of magnetization Magnetization (emu/g).
Figure 16 is the typical room temperature hysteresis curve of the prepared hcp phase nickel nano particle of embodiment 7.In Figure 16, abscissa is magnetic field Magnetic field (Oe), and ordinate is intensity of magnetization Magnetization (emu/g).
The specific embodiment
Embodiment 1 fcc is the preparation of 4 nanometer monodisperse nickel nanoparticles mutually
The 0.26g nickel acetylacetonate is mixed under the protection of argon gas with 6ml oleyl amine, 1ml trioctylamine and 1.38ml tri octyl phosphine; rise to 130 ℃ of insulation 20min after stirring 20min; rise to 205 ℃ more fast; insulation 30min; be cooled to room temperature then; through centrifugation and with the washing of ethanol and hexane mixed liquor for several 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, narrow particle size distribution, and average grain diameter is about 4nm.Fig. 2 is the X-ray powder diffraction figure of this product, and its diffraction maximum is consistent with fcc nickel.
The 0.26g nickel acetylacetonate is mixed under the protection of argon gas with 7ml oleyl amine, 0.66mL tri octyl phosphine and 0.15mL oleic acid; rise to 130 ℃ of insulation 20min after stirring 20min; rise to 215 ℃ more fast; insulation 30min; be cooled to room temperature then; through centrifugation and with the washing of ethanol and hexane mixed liquor for several times, last vacuum drying obtains the powder of black.Fig. 3 is the transmission electron microscope photo of this product, and the nano particle average grain diameter is about 9.3nm, and is spherical in shape, narrow particle size distribution.Fig. 4 is the X-ray powder diffraction figure of this product, and its diffraction maximum is consistent with fcc nickel.
Embodiment 3 fcc are the preparation of 11.3 nanometer monodisperse nickel nanoparticles mutually
0.25g four water nickel acetates are mixed under the protection of argon gas with 7ml oleyl amine, 1ml lauryl amine and 0.8ml tri octyl phosphine; rise to 150 ℃ behind the stirring 20min and vacuumize 40min; logical again argon gas insulation 20min; rise to 240 ℃ then fast; insulation 30min is cooled to room temperature, washs for several times through centrifugation with ethanol and hexane mixed liquor; last vacuum drying obtains the powder of black.Fig. 5 is its transmission electron microscope photo, and nano particle is spherical in shape as can be seen, narrow particle size distribution, and average grain diameter is about 11.3nm.Fig. 6 is the X-ray powder diffraction figure of this product, and its diffraction maximum is consistent with fcc nickel.This product magnetic hysteresis at room temperature line of whirling is seen Figure 15, and is consistent with the hysteresis curve of ferromagnetism nickel nano particle.
Embodiment 4 fcc are the preparation of 17.5 nanometer monodisperse nickel nanoparticles mutually
The 0.26g nickel acetylacetonate is mixed under the protection of argon gas with 7ml oleyl amine, 0.1ml tri octyl phosphine and 0.2 gram trioctylphosphine oxide (TOPO); rise to 130 ℃ of insulation 20min after stirring 20min; rise to 250 ℃ more fast; insulation 30min; be cooled to room temperature then; through centrifugation and with the washing of ethanol and hexane mixed liquor for several times, last vacuum drying obtains the powder of black.Fig. 7 is its transmission electron microscope photo, and nano particle is spherical in shape as can be seen, narrow particle size distribution, and average grain diameter is about 17.5nm.Fig. 8 is the X-ray powder diffraction figure of this product, and its diffraction maximum is consistent with fcc nickel.
Embodiment 5 hcp are the preparation of 6.5 nanometer monodisperse nickel nanoparticles mutually
0.25g four water nickel acetates are mixed under the protection of argon gas with 6ml octadecylene, 1.0ml oleyl amine and 0.66ml tri octyl phosphine; rise to 150 ℃ behind the stirring 20min and vacuumize 40min; logical again argon gas insulation 20min; rise to 230 ℃ more fast; insulation 60min is cooled to room temperature then, washs for several times through centrifugation with ethanol and hexane mixed liquor; last vacuum drying obtains the powder of black.Fig. 9 is its transmission electron microscope photo, and nano particle is spherical in shape as can be seen, narrow particle size distribution, and average grain diameter is about 6.5nm.Figure 10 is the X-ray powder diffraction figure of this product, and its diffraction maximum is consistent with hcp nickel.
Embodiment 6 hcp are the preparation of 9.5 nanometer monodisperse nickel nanoparticles mutually
The 0.26g nickel acetylacetonate is mixed under the protection of argon gas with 6ml two Bian ethers, 1.0ml oleyl amine and 0.44ml tri octyl phosphine; stir 20min and rise to 130 ℃ of insulation 20min; rise to 220 ℃ more fast; insulation 60min; be cooled to room temperature then; through centrifugation and with the washing of ethanol and hexane mixed liquor for several times, last vacuum drying obtains the powder of black.Figure 11 is its transmission electron microscope photo, and nano particle is spherical in shape as can be seen, narrow particle size distribution, and average grain diameter is about 9.5nm.Figure 12 is the X-ray powder diffraction figure of this product, and its diffraction maximum is consistent with hcp nickel.
Embodiment 7 hcp are the preparation of 27 nanometer monodisperse nickel nanoparticles mutually
The 0.26g nickel acetylacetonate is mixed under the protection of argon gas with 6ml octadecylene, 1.0ml oleyl amine and 0.3ml tri octyl phosphine; rise to 130 ℃ of insulation 20min after stirring 20min; rise to 240 ℃ more fast; insulation 45min; be cooled to room temperature then; through centrifugation and with the washing of ethanol and hexane mixed liquor for several times, last vacuum drying obtains the powder of black.Figure 13 is its transmission electron microscope photo, and nano particle is spherical in shape as can be seen, narrow particle size distribution, and average grain diameter is about 27nm.Figure 14 is the X-ray powder diffraction figure of this product, and its diffraction maximum is consistent with hcp nickel.Figure 16 is the room temperature hysteresis curve of this product, and it has the very low intensity of magnetization, demonstrates the magnetism characteristic different with ferromagnetism nickel.
Claims (10)
1. the preparation method of a monodisperse nickel nanoparticle is characterized in that may further comprise the steps:
1) under the protection of inert gas, after organic metal salt, alkylamine, surface stabilizer and the organic solvent mixing stirring with nickel,, rise to 180～350 ℃ of reactions again 100～160 ℃ of insulations, get product;
2) product of step 1) gained is cleaned with organic solvent, centrifugal, vacuum drying gets monodisperse nickel nanoparticle.
2. the preparation method of a kind of monodisperse nickel nanoparticle as claimed in claim 1, it is characterized in that in step 1) the organic metal salt of nickel is selected from nickel acetylacetonate, anhydrous formic acid nickel, contains crystallization water nickel formate, anhydrous acetic acid nickel, contain a kind of in crystallization water nickel acetate and the oleic acid nickel.
3. the preparation method of a kind of monodisperse nickel nanoparticle as claimed in claim 1 is characterized in that in step 1), and alkylamine is selected from a kind of in octylame, lauryl amine, cetylamine, oleyl amine and the trioctylamine.
4. the preparation method of a kind of monodisperse nickel nanoparticle as claimed in claim 1 is characterized in that in step 1), and surface stabilizer is the alkylphosphines thing.
5. the preparation method of a kind of monodisperse nickel nanoparticle as claimed in claim 1 is characterized in that in step 1), and organic solvent is selected from a kind of in octadecylene, diphenyl ether and the benzyl ether.
6. the preparation method of a kind of monodisperse nickel nanoparticle as claimed in claim 1 is characterized in that in step 1), and the alkylphosphines thing is selected from a kind of in tributylphosphine, tri octyl phosphine, trioctylphosphine oxide (TOPO) and the triphenylphosphine.
7. the preparation method of a kind of monodisperse nickel nanoparticle as claimed in claim 1 is characterized in that in step 1), and the molar concentration of the organic metal salt of nickel is 0.05～0.5mol/L, and the mol ratio of the organic metal salt of surface stabilizer and nickel is 0.1～5.
8. the preparation method of a kind of monodisperse nickel nanoparticle as claimed in claim 1, it is characterized in that pressing mass ratio in step 1) the organic metal salt of nickel: alkylamine: surface stabilizer: the proportioning of organic solvent is 1: 5～80: 0.3～10: 5～80.
9. the preparation method of a kind of monodisperse nickel nanoparticle as claimed in claim 1 is characterized in that in step 1), and mixing the time of stirring is 1～20min, but the time 1min～6h of insulation.
10. the preparation method of a kind of monodisperse nickel nanoparticle as claimed in claim 1 is characterized in that in step 2) in, organic solvent is ethanol or hexane.
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| CN109243850A (en) * | 2018-11-05 | 2019-01-18 | 南京晓庄学院 | Ni-Co oxide nanocrystalline and its controllable synthesis method and application |
| CN109243850B (en) * | 2018-11-05 | 2020-11-27 | 南京晓庄学院 | Ni-Co oxide nanocrystalline and controllable synthesis method and application thereof |
| CN110576191A (en) * | 2019-10-18 | 2019-12-17 | 济宁学院 | Method for preparing copper-nickel alloy nano material with bevel bipyramid morphology characteristics in hydrophobic phase |
| CN115608361A (en) * | 2021-10-08 | 2023-01-17 | 厦门大学 | Catalyst for reductive amination and preparation method and application thereof |
| CN115608361B (en) * | 2021-10-08 | 2024-04-23 | 厦门大学 | Catalyst for reductive amination and preparation method and application thereof |
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