CN102554257A - Amorphous core-shell structure nanoparticle and preparation method thereof - Google Patents
Amorphous core-shell structure nanoparticle and preparation method thereof Download PDFInfo
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- CN102554257A CN102554257A CN2012100118201A CN201210011820A CN102554257A CN 102554257 A CN102554257 A CN 102554257A CN 2012100118201 A CN2012100118201 A CN 2012100118201A CN 201210011820 A CN201210011820 A CN 201210011820A CN 102554257 A CN102554257 A CN 102554257A
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Abstract
The invention discloses an amorphous core-shell structure nanomaterial and a preparation method thereof. The amorphous core-shell structure nanomaterial takes magnetic metal nanoparticles as a core, and takes a metal oxide as a shell. The preparation method, i.e., a chemical reduction method, comprises the following steps of: 1. preparing a salt-containing aqueous solution in which a polymer dispersant agent is dispersed; 2. preparing a reducing agent solution; 3. placing the prepared reaction solution in a microfluid reaction system to react and collecting a product; and 4: washing and separating to obtain the amorphous core-shell structure nanoparticles. The amorphous core-shell structure nanoparticles with uniform and dense shell layers can be obtained by one step by the preparation method provided by the invention, the further oxidation of the core can be effectively prevented by the shell layers, the stability of the material is improved, and the preparation method is simple.
Description
Technical field
The invention belongs to the nano composite material technical field, be specifically related to a kind of amorphous state nuclear shell structure nano particle and preparation method thereof.
Background technology
Owing to have unique magnetic performance, magnetic nanoparticle all enjoys biomedical sector and high content information storing material (as surpassing 1Tbit/in always
2) pay close attention to.The more magnetic Nano material of research mainly contains nanometer ferrite material, magnetic metal nanometer material at present.Two kinds of material compared, the magnetic metal nanometer material development relatively lags behind, and this mainly is because under nanoscale; Metal nanoparticle is too active, and chemical stability is very poor, and preservation condition is very harsh; The prepared nano particle that comes out tends to the oxidation by in various degree, simultaneously when size little after to a certain degree, it has become ultra paramagnetic by ferromagnetism; Though it similarly is useful that biomedicine is, be useless to the high density magnetic memory.
To this situation, scientists has also been taked some counter-measures, and what wherein comparatively approve is the surface-coated one deck noble metal gold, silver at the metal magnetic nano particle.Dai etc. have prepared hydrophilic three metal core-shell type CoPtAu nano particles; Document [1] sees reference: Dai J.T.; Du Y.K.; Yang P..Preparation and characterization of Pt/Co-CoreAu-Shell magneticnanoparticles [J] .Z.Anorg.A1lg.Chem, 2006,632 (6): 1108-1111.The result shows; Au shell in the CoPtAu nano particle has well anti-oxidation, anti-agglomeration to the CoPt nano particle of internal layer; In addition; Make this nucleocapsid structure material have a good application prospect at biomedical sector because outer field golden shell has excellent optical property, but basic for ultra paramagnetic under the said material room temperature, very difficult it is adjusted to has ferromagnetic property.Simultaneously, the preparation method of this core-shell nano particle is complicated, and output capacity is very low, therefore still is in conceptual phase at present.
Summary of the invention
The objective of the invention is to propose a kind of amorphous state nuclear shell structure nano particle with and preparation method thereof, it is to be nuclear with the metal magnetic nano particle, metal oxide is the sandwich of shell.Wherein magnetic core can be metal Fe, Co, CoFe, FeAl or CoAl; Shell is the oxide of nuclear metal, and this layer crystal can be full amorphous state mutually, also can be to be embroidered with a small amount of small nanocrystalline multiphase structure by point in the amorphous state, convenient for the purpose of, still be called amorphous structure.Different with crystal phase structure based on material composition, these materials promptly become ferrimagnet, can become superparamagnetism again.
The present invention proposes the preparation method of above-mentioned amorphous state nuclear shell structure nano granular materials, comprise following step:
Step 1: the slaine of 0.04～4.0g macromolecule dispersing agent, 0.15～15mmol is dissolved in the 50mL ultra-pure water, obtains the mixing salt solution that macromolecule dispersing agent disperses;
Step 2: configuration reductant solution;
Described reductant solution is the strong reductant with the anhydrous organic solvent dissolving, can be with 0.15～1.5gNaBH
4Be dissolved in the 50mLN-methyl pyrrolidone colourless transparent solution that obtains; Perhaps for being dissolved with LiBH (C
2H
5)
3Tetrahydrofuran solution.
Step 3: with the syringe solution 20mL that disposed of extraction step one and step 2 respectively; Place on the syringe pump; Flow velocity is adjusted to: 0.05mL/min～1ml/min; Two kinds of solution are reacted in the micro fluid reaction system, and product imports in the gathering-device of nitrogen protection, obtains the solution of the amorphous state nuclear shell structure nano particle of stable dispersion;
Step 4: the solution of the amorphous state nuclear shell structure nano particle of stable dispersion is carried out the sonic oscillation washing, and centrifugation settles down the nanometer ferrite particle from the aqueous solution, outwell supernatant, obtains precipitum.To join in the precipitum with the N-methyl pyrrolidone of the same volume of supernatant, sonic oscillation washing once more behind the cyclic washing, obtains amorphous state nuclear shell structure nano particle.
The invention has the advantages that:
1, a kind of amorphous state nuclear shell structure nano material of the present invention's proposition, its preparation principle is simple, only needs a step can obtain the nuclear shell structure nano particle;
2, a kind of amorphous state nuclear shell structure nano material of the present invention's proposition has unique amorphous structure;
3, a kind of amorphous state nuclear shell structure nano material of the present invention's proposition has the nucleocapsid double-decker, and shell is the fine and close oxide-film of one deck, can effectively stop the further oxidation of magnetic core, thereby has improved the chemistry and the magnetic property stability of this nano material.According to the magnetoelectricity coupling between nucleocapsid, through regulating the composition and the structure of material, these materials promptly become ferrimagnet, can become superparamagnetism again.
Description of drawings
Fig. 1: the sketch map of a kind of amorphous state nuclear shell structure nano preparation methods that the present invention proposes;
The amorphous state nuclear shell structure nano material transmission electron microscope photo of preparing among Fig. 2 a and 2b: the embodiment 1;
The XRD spectra of the amorphous state nuclear shell structure nano material of preparing among Fig. 3: the embodiment 1;
The room temperature hysteresis curve of the amorphous state nuclear shell structure nano material of preparing among Fig. 4: the embodiment 1.
The specific embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is elaborated.
A kind of amorphous state nuclear shell structure nano material that the present invention proposes uses one step of microfluid method synthetic, as shown in Figure 1, specifically comprises following step:
Step 1: the salt of 0.04～4.0g macromolecule dispersing agent, 0.15～15mmol is dissolved in the 50mL ultra-pure water, obtains the iron content mixing salt solution that macromolecule dispersing agent disperses; Described salt is molysite, aluminium salt or cobalt salt, is the mixing of above-mentioned any two kinds of salt perhaps, and mixed proportion is any, is preferably chlorate, and during the mixing of two kinds of salt, preferred molar ratio is 1: 1.Described molysite is FeCl
24H
2O, described aluminium salt is AlCl
3, described cobalt salt is CoCl
26H
2O.
Described macromolecule dispersing agent is one or both in the following material: PVP (PVP), polyvinyl alcohol (PVA), polyacrylamide (PAM), polyethylene glycol (PEG), polyacrylic acid (PPA), sodium lignin sulfonate and lignin carboxylic acid amine are preferably PVP.
Step 2: configuration reductant solution;
Described reductant solution is the strong reductant with the anhydrous organic solvent dissolving, can be with 0.015～1.5g NaBH
4Be dissolved in the 50mL N-methyl pyrrolidone colourless transparent solution that obtains; Also can be to be dissolved with LiBH (C
2H
5)
3Tetrahydrofuran solution.The solution concentration of reducing agent is identical.
Step 3: with the syringe solution 20mL that disposed of extraction step one and step 2 respectively; Place on the syringe pump, flow velocity v is adjusted to: 0.05mL/min～10ml/min, and as shown in Figure 1; Heater is the heater of reactor part, with adjustment to temperature required scope.Two kinds of solution are reacted in the micro fluid reaction system, and product imports in the gathering-device of nitrogen protection, obtains the solution by the amorphous state nuclear shell structure nano particle of stable dispersion; Described temperature range is regulated according to two kinds of SOLUTION PROPERTIES, and the principle of adjusting is for guaranteeing that two kinds of solution can react smoothly.
Step 4: the solution of the amorphous state nuclear shell structure nano particle of stable dispersion is carried out the sonic oscillation washing; Is centrifugal 20～60min under 3000～15000r/min with its solution at rotating speed; Nano particle is settled down from solution, outwell supernatant, obtain precipitum.To join in the precipitum with the N-methyl pyrrolidone of the same volume of supernatant, sonic oscillation washing once more, behind the cyclic washing, collect final bottom black precipitum and be final products of the present invention---amorphous state nuclear shell structure nano particle.Described cyclic washing, general preferred washing 2～3 times, purpose is that the macromolecule dispersing agent in the solution is washed off, also will guarantee the integrality of amorphous state nuclear shell structure nano particle simultaneously.
The amorphous state nuclear shell structure nano particle that method for preparing obtains is an amorphous state, has the nucleocapsid double-decker, and shell is the fine and close oxide-film of one deck, can effectively stop the further oxidation of magnetic core, thereby improve the stability of this nano-particle material.Resulting amorphous state nuclear shell structure nano particle is to be nuclear with the metal magnetic nano particle; Metal oxide is the sandwich of shell; Wherein magnetic core can be Fe, Co, CoFe, FeAl or CoAl, and shell is the oxide of inner layer metal, like the oxide Fe of iron
3O
4Amorphous state nuclear shell structure nano granular materials saturation magnetization at room temperature is 13.7～140emu/g, and coercivity is 0～560Oe.
Embodiment 1:
A kind of amorphous state nuclear shell structure nano preparation method of granules that proposes in the present embodiment specifically comprises following step:
Step 1: with the FeCl of 4.0g PVP (molecular weight is 10000), 15mmol
24H
2O is dissolved in the 50mL ultra-pure water, obtains the iron content mixing salt solution that macromolecule dispersing agent disperses;
Step 2: with 1.5g NaBH
4Be dissolved in the 50mL N-methyl pyrrolidone, obtain its colourless transparent solution;
Step 3: with the syringe solution 20mL that disposed of extraction step one and step 2 respectively; Place on the syringe pump; Flow velocity v is adjusted to: 0.05mL/min～0.1ml/min; Above-mentioned two kinds of solution are reacted in the micro fluid reaction system, and product imports in the gathering-device of nitrogen protection, obtains the solution by the amorphous state nuclear shell structure nano particle of stable dispersion;
Step 4: the solution of the amorphous state nuclear shell structure nano particle of stable dispersion is carried out the sonic oscillation washing, is centrifugal 20min under the 15000r/min with its solution at rotating speed, and nano particle is settled down from solution, outwells supernatant, obtains precipitum.To join in the precipitum with the N-methyl pyrrolidone of the same volume of supernatant, sonic oscillation washing once more behind the cyclic washing 2～3 times, is collected final bottom black precipitum and is final products of the present invention.
Can find out from the transmission electron microscope photo of this ferrite nanometer particle shown in Figure 2; Particle is for being amorphous structure; And among the figure in great circle and the ringlet contrast of material have evident difference; Explained that this amorphous state nuclear shell structure nano particle has the structure of nuclear and shell, this amorphous state nuclear shell structure nano particle has amorphous structure simultaneously.Fig. 3 is the X-ray diffraction analysis result of material; Locate to occur a diffuse scattering peak for 44.6 ° in this collection of illustrative plates; Its diffuse scattering peak position with Fe-based amorphous alloy is consistent; This result is combined with the experiment mechanism of material to infer that the prepared nano particle kernel that goes out is the iron-based non-crystalline nano particle, and skin is its oxide, is amorphous state (Fig. 2 A) basically on its Electronic Speculum.But can find out that from its XRD it locates to occur a diffuse scattering peak except 44.6 °, also has some faint small peaks; By analysis; They are the peak of crystalline state tri-iron tetroxide, also can find from the transmission electron microscope photo of some nano particles, and some the crystalline particle of particle diameter in the 0.5-2 nanometer occurred; Can think that in conjunction with XRD they are crystalline state tri-iron tetroxides, the crystalline region that is enclosed like Fig. 2 B dotted ellipse.The hysteresis curve of its room temperature is as shown in Figure 4.Show its saturation induction density M
sBe 130emu/g, its coercivity H
cBe 110Oe, can see the off-centered characteristics of its coercivity simultaneously, depart from a H
EbAbout 100Oe, its remanent magnetism M
rBe 20emu/g.Consider that these nano particles are connected with surface stabilizer usually, if the quality of surface stabilizer is removed, the M of this material
s, M
rCan be higher, so this material can be used as the ultrahigh density storing material (above 1Tbit/in
2).
Embodiment 2:
A kind of amorphous state nuclear shell structure nano preparation method of granules that proposes in the present embodiment specifically comprises following step:
Step 1: with the FeCl of 0.04g PVP (molecular weight is 10000), 0.15mmol
24H
2O is dissolved in the 50mL ultra-pure water, obtains the iron content mixing salt solution that macromolecule dispersing agent disperses;
Step 2: with 0.015g NaBH
4Be dissolved in the 50mL N-methyl pyrrolidone, obtain its colourless transparent solution;
Step 3: with the syringe solution 20mL that disposed of extraction step one and step 2 respectively; Place on the syringe pump; Flow velocity is adjusted to: 0.5mL/min～1ml/min; Above-mentioned two kinds of solution are reacted in the micro fluid reaction system, and product imports in the gathering-device of nitrogen protection, obtains the solution by the amorphous state nuclear shell structure nano particle of stable dispersion;
Step 4: the solution of the amorphous state nuclear shell structure nano particle of stable dispersion is carried out the sonic oscillation washing, is centrifugal 60min under the 3000r/min with its solution at rotating speed, and nano particle is settled down from solution, outwells supernatant, obtains precipitum.To join in the precipitum with the N-methyl pyrrolidone of the same volume of supernatant, sonic oscillation washing once more behind the cyclic washing 3 times, is collected final bottom black precipitum and is final products of the present invention.
The above-mentioned final products that prepare are carried out the high resolution electron microscopy analysis can know that material is shown as amorphous structure, and have the double-decker of shell and nuclear.
Embodiment 3:
A kind of amorphous state nuclear shell structure nano preparation method of granules that proposes in the present embodiment specifically comprises following step:
Step 1: with the FeCl of 0.4g PVP (molecular weight is 10000), 1.5mmol
24H
2O is dissolved in the 50mL ultra-pure water, obtains the iron content mixing salt solution that macromolecule dispersing agent disperses;
Step 2: with 0.15g NaBH
4Be dissolved in the 50mL N-methyl pyrrolidone, obtain its colourless transparent solution;
Step 3: with the syringe solution 20mL that disposed of extraction step one and step 2 respectively; Place on the syringe pump; Flow velocity is adjusted to: 1ml/min; Reactant liquor is reacted in the micro fluid reaction system, and product imports in the gathering-device of nitrogen protection, obtains the solution by the amorphous state nuclear shell structure nano particle of stable dispersion;
Step 4: the solution of the amorphous state nuclear shell structure nano particle of stable dispersion is carried out the sonic oscillation washing, is centrifugal 30min under the 10000r/min with its solution at rotating speed, and nano particle is settled down from solution, outwells supernatant, obtains precipitum.To join in the precipitum with the N-methyl pyrrolidone of the same volume of supernatant, sonic oscillation washing once more, behind the cyclic washing 3 times, collect final bottom black precipitum and be final products of the present invention---amorphous state nuclear shell structure nano particle.
Embodiment 4:
The difference of present embodiment and embodiment 1 only is, with the FeCl in embodiment 1 step 1
24H
2O is replaced by the cobalt salt CoCl with mole
26H
2O, the preparation process and the embodiment 1 of other each steps are identical.The saturation magnetization of (300K) is 13.7emu/g under this material room temperature,, coercivity is zero, this material can be as biomedical with magnetic resonance imaging reinforcing agent.
Embodiment 5:
The difference of present embodiment and embodiment 1 only is, with the FeCl in embodiment 1 step 1
24H
2O is replaced by with the cobalt salt of mole and molysite, and wherein the mol ratio of cobalt salt and molysite is 1: 1, and the preparation process and the embodiment 1 of other each steps are identical.Saturation magnetization under this nano material room temperature is 97.5emu/g, and coercivity is 499Oe.
Embodiment 6:
The difference of present embodiment and embodiment 1 only is, with the FeCl in embodiment 1 step 1
24H
2O is replaced by with the molysite of mole and aluminium salt, and wherein the mol ratio of cobalt salt and molysite is 1: 1, and the preparation process and the embodiment 1 of other each steps are identical.Saturation magnetization under this nano material room temperature is 52.7emu/g, and coercivity is 560Oe.
Embodiment 7:
The difference of present embodiment and embodiment 1 only is, with the FeCl in embodiment 1 step 1
24H
2O is replaced by with the cobalt salt of mole and aluminium salt, and wherein the mol ratio of cobalt salt and molysite is 1: 1, and the preparation process and the embodiment 1 of other each steps are identical, but the flow velocity of microfluid rises to 10mL/ minute.The core of the product that obtains is an amorphous state, and size is 4.5 nanometers, and shell is an amorphous state, and thickness is about 1.5 nanometers.Saturation magnetization under this nano material room temperature is 140emu/g, and coercivity is 280Oe.
Embodiment 8:
The difference of present embodiment and above embodiment only is, with the NaBH that is dissolved with in the above embodiment step 2
4N methyl pyrrolidone solution exchange be same concentrations be dissolved with LiBH (C
2H
5)
3Tetrahydrofuran solution.The preparation process and the embodiment 1 of other each steps are identical.Can prepare amorphous state nuclear shell structure nano particle equally.
In the above embodiments, described cobalt salt is CoCl
26H
2O, described molysite are FeCl
24H
2O, described aluminium salt is AlCl
3
Claims (7)
1. amorphous state nuclear shell structure nano preparation methods is characterized in that: specifically comprise following step:
Step 1: the salt of 0.04～4.0g macromolecule dispersing agent, 0.15～15mmol is dissolved in the 50mL ultra-pure water, obtains the mixed salt solution that contains of macromolecule dispersing agent dispersion;
Step 2: configuration reductant solution;
Step 3: with the syringe solution 20mL that disposed of extraction step one and step 2 respectively; Place on the syringe pump; Flow velocity is adjusted to: 0.05mL/min～1ml/min; Two kinds of solution are reacted in the micro fluid reaction system, and product imports in the gathering-device of nitrogen protection, obtains the solution of the amorphous state nuclear shell structure nano particle of stable dispersion;
Step 4: the solution of the amorphous state nuclear shell structure nano particle of stable dispersion is carried out the sonic oscillation washing, and centrifugation settles down the nanometer ferrite particle from the aqueous solution; Outwell supernatant; Obtain precipitum, will join in the precipitum, sonic oscillation washing once more with the N-methyl pyrrolidone of the same volume of supernatant; Behind the cyclic washing, obtain amorphous state nuclear shell structure nano particle.
2. a kind of amorphous state nuclear shell structure nano preparation methods according to claim 1 is characterized in that: the reductant solution that uses in the step 2 is for 0.15～1.5g NaBH
4Be dissolved in the 50mL N-methyl pyrrolidone, obtain its colourless transparent solution; Perhaps be dissolved with LiBH (C for same concentrations
2H
5)
3Tetrahydrofuran solution.
3. a kind of amorphous state nuclear shell structure nano preparation methods according to claim 1 is characterized in that: described macromolecule dispersing agent is the following material that comprises one or both: PVP, polyvinyl alcohol, polyacrylamide, polyethylene glycol, polyacrylic acid, sodium lignin sulfonate and lignin carboxylic acid amine.
4. a kind of amorphous state nuclear shell structure nano preparation methods according to claim 1; It is characterized in that: the salt in the described step 1 is the salt-mixture of salt-mixture, molysite and the aluminium salt of molysite, cobalt salt, aluminium salt, cobalt salt and molysite, perhaps cobalt salt and aluminium salt salt-mixture.
5. amorphous state nuclear shell structure nano material is characterized in that: said amorphous state nuclear shell structure nano material is to be nuclear with the metal magnetic nano particle, and metal oxide is the sandwich of shell, and nuclear and shell are amorphous structure.
6. a kind of amorphous state nuclear shell structure nano material according to claim 5; It is characterized in that: examine Fe, Co, CoFe, FeAl or CoAl into metal material; Shell is the oxide of inner layer metal, and this layer is for amorphous state or for being inlaid with the nanocrystalline multiphase alloy structure of small amount of crystalline attitude.
7. a kind of amorphous state nuclear shell structure nano material according to claim 5, it is characterized in that: material saturation magnetization at room temperature is 13.7～140emu/g, coercivity is 0～560Oe.
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| CN103646743A (en) * | 2013-09-26 | 2014-03-19 | 宋玉军 | Super-miniature core-shell structure nano-particles and preparing method thereof |
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| CN106984829A (en) * | 2017-05-03 | 2017-07-28 | 厦门大学 | A kind of synthetic method of the FeCoNi ternary asymmetric particles of core shell structure |
| CN109351964A (en) * | 2018-12-18 | 2019-02-19 | 吉林大学 | Compound iron-based powder with nucleocapsid structure and its preparation method and application |
| CN113453786A (en) * | 2019-03-28 | 2021-09-28 | 庄信万丰股份有限公司 | Exhaust gas treatment system and use thereof for exhaust gas treatment |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103646743A (en) * | 2013-09-26 | 2014-03-19 | 宋玉军 | Super-miniature core-shell structure nano-particles and preparing method thereof |
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| CN106984829B (en) * | 2017-05-03 | 2019-03-22 | 厦门大学 | A kind of synthetic method of the FeCoNi ternary asymmetric particle of core-shell structure |
| CN109351964A (en) * | 2018-12-18 | 2019-02-19 | 吉林大学 | Compound iron-based powder with nucleocapsid structure and its preparation method and application |
| CN109351964B (en) * | 2018-12-18 | 2020-12-22 | 吉林大学 | Composite iron-based powder with core-shell structure and preparation method and application thereof |
| CN113453786A (en) * | 2019-03-28 | 2021-09-28 | 庄信万丰股份有限公司 | Exhaust gas treatment system and use thereof for exhaust gas treatment |
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