CN109604628A - A kind of preparation method of ordered phase nanometer Fe-Pt particle and cobalt platinum nano particle - Google Patents
A kind of preparation method of ordered phase nanometer Fe-Pt particle and cobalt platinum nano particle Download PDFInfo
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- CN109604628A CN109604628A CN201910104158.6A CN201910104158A CN109604628A CN 109604628 A CN109604628 A CN 109604628A CN 201910104158 A CN201910104158 A CN 201910104158A CN 109604628 A CN109604628 A CN 109604628A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The invention discloses the preparation methods of a kind of ordered phase nanometer Fe-Pt particle and cobalt platinum nano particle, ferric acetyl acetonade (or cobalt) and chloroplatinic acid are dissolved in organic solvent as maceration extract, impregnate sodium chloride powder, it is restored under sodium chloride fusing point after drying, iron platinum (or cobalt platinum) nano particle is obtained after washing.The present invention can prepare polymolecularity ordered phase nanometer Fe-Pt particle and cobalt platinum nano particle, and particle size uniformity with rapid batch.
Description
Technical field
The present invention relates to the preparation methods of a kind of ordered phase nanometer Fe-Pt particle and cobalt platinum nano particle, belong to magnetic alloy
Particle preparation field.
Background technique
Ordered phase (also known as L10Phase, face-centered tetragonal phase) iron platinum (FePt) and cobalt platinum (CoPt) nano particle have high magnetic
Anisotropic crystalline constant, and therefore have extra small superparamagnetic critical dimension (D=2.8~3.3nm), while ordered phase iron platinum and
Cobalt platinum nano particle has high-coercive force, high energy product, high Curie temperature (Tc=480 DEG C) and good physics, chemistry steady
It is qualitative.Therefore, ordered phase iron platinum and cobalt platinum nano particle are constantly subjected to extensive concern, and are situated between in the following ultra high density magnetic recording
Matter, nanometer PABX networking magnet new material, high performance catalyst material etc. have good application prospect.
FePt/CoPt mainly has two kinds of structures of face-centered cubic and face-centered tetragonal.Wherein face-centered cubic (fcc) structure is chemistry
Unordered phase, Fe/Co and Pt atom occupy each lattice point at random, and probability is 50%.Unordered phase structure is shown as in terms of magnetism
Superparamagnetism cannot function as magnetic recording material.And face-centered tetragonal (fct) structure is chemically-ordered phase, Fe, Pt atom are in c-axis
It is in alternate layers on direction.Ordered phase FePt/CoPt has very strong magnetocrystalline anisotropy and very big coercivity, is not
Carry out the preferred material of ultra high density magnetic recording media.
FePt/CoPt nano particle is usually using oily phase thermal decomposition method preparation, but the nano particle of this method preparation is nothing
Sequence phase does not have high magnetocrystalline anisotropy.Unordered phase FePt/CoPt nano particle must pass through 500 DEG C or more high annealings, side
Ordered phase can be obtained.But after high annealing, though FePt/CoPt nano particle can be changed into ordered phase, nano particle can occur sternly
Reheating knot and curing are grown up, it is difficult to keep its ultra-small grain size and monodispersity.Currently, solving the problems, such as that this thinking mainly has:
(1) nucleocapsid cladding process.Nucleocapsid cladding is carried out to FePt/CoPt nano particle using MgO or MnO, pickling obtains after high annealing
Ordered phase FePt/CoPt nano particle.But nucleocapsid cladding process step is various, and acid cleaning process easily leads to lattice damage, magnetic property
Decline；(2) water soluble salt isolation method.The method prepares unordered FePt/CoPt nano particle as presoma, by nothing first
Sequence FePt/CoPt particle grinds in organic solvent with NaCl salt (801 DEG C of fusing point), mixes, high annealing after solvent evaporation, water
Ordered phase FePt/CoPt particle is obtained after washing.But this method not only needs previously prepared unordered phase FePt/CoPt particle out, and
And need to grind salt particle, complex procedures, preparation cost are excessively high, are only applicable to laboratory and prepare a small amount of sample.
In conclusion there are preparation cost height, complex process for the ordered phase FePt/CoPt nano particle of prior art preparation
The deficiencies of, the short-cut method still without prepare with scale ordered phase FePt/CoPt nano particle at present.
Summary of the invention
Technical problem: the present invention provides it is a kind of it is simple and easy to do, be able to produce particle dispersion, size more it is uniform orderly
The preparation method of the ordered phase nanometer Fe-Pt particle of phase nano particle and the preparation method of ordered phase cobalt platinum nano particle, preparation
Ordered phase nanometer Fe-Pt particle has good crystallinity and dispersibility, has excellent magnetic characteristics.
Technical solution: the preparation method of ordered phase nanometer Fe-Pt particle of the invention, comprising the following steps:
1) ferric acetyl acetonade of equimolar amounts and chloroplatinic acid are dissolved in organic solvent, as maceration extract；
2) organic solvent is evaporated after removing extra maceration extract with maceration extract dipping sodium chloride powder；
3) the water soluble salt powder after dipping is calcined in high-temperature reductibility atmosphere；
4) by powder washing, the drying after reduction, nanometer Fe-Pt particle is obtained.
Further, organic molten in the step 1) in the preparation method of ordered phase nanometer Fe-Pt particle of the invention
Agent is ethyl alcohol, ethylene glycol or acetone.
Further, in the preparation method of ordered phase nanometer Fe-Pt particle of the invention, dipping that the step 1) obtains
The concentration of liquid is 0.001mol/L~1mol/L.
Further, in the preparation method of ordered phase nanometer Fe-Pt particle of the invention, the high temperature model in the step 3)
It encloses between 500 DEG C to 800 DEG C.
Further, in the preparation method of ordered phase nanometer Fe-Pt particle of the invention, the reproducibility in the step 3)
Atmosphere refers to hydrogen, nitrogen and hydrogen mixture or carbon monoxide.
The preparation method of ordered phase cobalt platinum nano particle of the invention, comprising the following steps:
1) acetylacetone cobalt of equimolar amounts and chloroplatinic acid are dissolved in organic solvent, as maceration extract；
2) organic solvent is evaporated after removing extra maceration extract with maceration extract dipping sodium chloride powder；
3) the water soluble salt powder after dipping is calcined in high-temperature reductibility atmosphere；
4) by powder washing, the drying after reduction, cobalt platinum nano particle is obtained.
Further, organic molten in the step 1) in the preparation method of ordered phase cobalt platinum nano particle of the invention
Agent is ethyl alcohol, ethylene glycol or acetone.
Further, in the preparation method of ordered phase cobalt platinum nano particle of the invention, dipping that the step 1) obtains
The concentration of liquid is 0.001mol/L~1mol/L.
Further, in the preparation method of ordered phase cobalt platinum nano particle of the invention, the high temperature model in the step 3)
It encloses between 500 DEG C to 800 DEG C.
Further, in the preparation method of ordered phase cobalt platinum nano particle of the invention, the reproducibility in the step 3)
Atmosphere refers to hydrogen, nitrogen and hydrogen mixture or carbon monoxide.
The utility model has the advantages that compared with prior art, the present invention having the advantage that
The existing method for preparing ordered phase FePt/CoPt nano particle mainly has nucleocapsid cladding process and water soluble salt isolation
Method.Both methods is required to previously prepared unordered phase FePt/CoPt nano particle out and then passes through particle again as presoma
Surface coats or grinds together with water soluble salt particle, and then high annealing generates ordered phase again, not only complex procedures, cost
Height is difficult to scale, and the FePt/CoPt nanoparticle size prepared is difficult to control, and magnetic property is bad.
The present invention prepares ordered phase FePt/CoPt nano particle using easy-to-use infusion process, first by levulinic
Ketone iron (acetylacetone cobalt) and chloroplatinic acid are dissolved in organic solvent (sodium chloride cannot have larger solubility in organic solvent), as
Maceration extract.Sodium chloride powder is impregnated using this maceration extract, after organic solvent evaporation is fallen, iron (cobalt) and platinum element are present in
Sodium chloride particle surface.Then it is calcined in high temperature reducing atmospheres, can react and generate ordered phase FePt/CoPt, use water after cooling
Washing can remove sodium chloride, the ordered phase FePt/CoPt nano particle dispersed.
Dispersion ordered phase FePt/CoPt nano particle is prepared using the method, on condition that ferric acetyl acetonade, acetyl can be made
Acetone cobalt and chloroplatinic acid can uniformly be sprawled in sodium chloride salt particle surface, rather than with the presence of aggregated particle state.We study
It was found that these three raw materials are in the selected organic solvent of the present invention, there are stronger suction-operated, You Jirong with sodium chloride
Agent can be uniformly distributed after being evaporated on sodium chloride particle surface.Therefore, equally distributed iron (cobalt) and platinum element can at high temperature
Produce particle dispersion, the more uniform ordered phase FePt/CoPt nano particle of size.
The present invention can prepare the ordered phase FePt/CoPt nano particle of favorable dispersibility with rapid batch, prepared
Ordered phase FePt/CoPt nano particle crystallinity is good.Moreover, preparation method of the present invention do not need it is previously prepared unordered mutually orderly
Phase FePt/CoPt nano particle, technique is very easy, is easy to large-scale production.
Detailed description of the invention
Fig. 1 is ordered phase nanometer Fe-Pt particle prepared by the present invention.
Specific embodiment
Below with reference to embodiment and Figure of description, the present invention is further illustrated.
Embodiment 1: being configured to the ethanol solution that concentration is 0.1mol/L with the ferric acetyl acetonade of equimolar amounts and chloroplatinic acid,
Sodium chloride powder is impregnated, it is after removing extra maceration extract, powder is dry.By the powder after drying in 800 DEG C of hydrogen reducings, water
Wash, dry after ordered phase nanometer Fe-Pt particle can be obtained.
Embodiment 2: it is molten that the ethyl alcohol that concentration is 0.01mol/L is configured to the ferric acetyl acetonade of equimolar amounts and chloroplatinic acid
Liquid impregnates sodium chloride powder, after removing extra maceration extract, powder is dry.By the powder after drying in 800 DEG C of hydrogen reducings,
Ordered phase nanometer Fe-Pt particle can be obtained after washing, drying.
Embodiment 3: being configured to the ethanol solution that concentration is 1mol/L with the ferric acetyl acetonade of equimolar amounts and chloroplatinic acid, leaching
Stain sodium chloride powder, it is after removing extra maceration extract, powder is dry.By the powder after drying in 800 DEG C of hydrogen reducings, wash,
Ordered phase nanometer Fe-Pt particle can be obtained after drying.
Embodiment 4: being configured to the ethylene glycol solution that concentration is 1mol/L with the ferric acetyl acetonade of equimolar amounts and chloroplatinic acid,
Sodium chloride powder is impregnated, it is after removing extra maceration extract, powder is dry.By the powder after drying in 800 DEG C of hydrogen reducings, water
Wash, dry after ordered phase nanometer Fe-Pt particle can be obtained.
Embodiment 5: being configured to the acetone soln that concentration is 1mol/L with the ferric acetyl acetonade of equimolar amounts and chloroplatinic acid, leaching
Stain sodium chloride powder, it is after removing extra maceration extract, powder is dry.By the powder after drying in 800 DEG C of hydrogen reducings, wash,
Ordered phase nanometer Fe-Pt particle can be obtained after drying.
Embodiment 6: being configured to the ethanol solution that concentration is 1mol/L with the ferric acetyl acetonade of equimolar amounts and chloroplatinic acid, leaching
Stain sodium chloride powder, it is after removing extra maceration extract, powder is dry.By the powder after drying in 800 DEG C of hydrogen reducings, wash,
Ordered phase nanometer Fe-Pt particle can be obtained after drying.
Embodiment 7: it is molten that the ethylene glycol that concentration is 0.1mol/L is configured to the ferric acetyl acetonade of equimolar amounts and chloroplatinic acid
Liquid impregnates sodium chloride powder, after removing extra maceration extract, powder is dry.By the powder after drying in 800 DEG C of hydrogen reducings,
Ordered phase nanometer Fe-Pt particle can be obtained after washing, drying.
Embodiment 8: being configured to the acetone soln that concentration is 0.1mol/L with the ferric acetyl acetonade of equimolar amounts and chloroplatinic acid,
Sodium chloride powder is impregnated, it is after removing extra maceration extract, powder is dry.By the powder after drying in 800 DEG C of hydrogen reducings, water
Wash, dry after ordered phase nanometer Fe-Pt particle can be obtained.
Embodiment 9: being configured to the ethanol solution that concentration is 0.1mol/L with the ferric acetyl acetonade of equimolar amounts and chloroplatinic acid,
Sodium chloride powder is impregnated, it is after removing extra maceration extract, powder is dry.By the powder after drying in 800 DEG C of Carbon monoxide reductions,
Ordered phase nanometer Fe-Pt particle can be obtained after washing, drying.
Embodiment 10: it is molten that the ethyl alcohol that concentration is 0.1mol/L is configured to the ferric acetyl acetonade of equimolar amounts and chloroplatinic acid
Liquid impregnates sodium chloride powder, after removing extra maceration extract, powder is dry.By the powder after drying in 800 DEG C of nitrogen and hydrogen mixtures
Ordered phase nanometer Fe-Pt particle can be obtained after washing, drying in reduction.
Embodiment 11: it is molten that the ethyl alcohol that concentration is 0.1mol/L is configured to the ferric acetyl acetonade of equimolar amounts and chloroplatinic acid
Liquid impregnates sodium chloride powder, after removing extra maceration extract, powder is dry.By the powder after drying, hydrogen is also between 500 DEG C
Ordered phase nanometer Fe-Pt particle can be obtained after washing, drying in original.
Embodiment 12: it is molten that the ethyl alcohol that concentration is 0.1mol/L is configured to the ferric acetyl acetonade of equimolar amounts and chloroplatinic acid
Liquid impregnates sodium chloride powder, after removing extra maceration extract, powder is dry.By the powder after drying in 700 DEG C of hydrogen reducings,
Ordered phase nanometer Fe-Pt particle can be obtained after washing, drying.
Embodiment 13: it is molten that the ethyl alcohol that concentration is 0.1mol/L is configured to the acetylacetone cobalt of equimolar amounts and chloroplatinic acid
Liquid impregnates sodium chloride powder, after removing extra maceration extract, powder is dry.By the powder after drying in 800 DEG C of hydrogen reducings,
Ordered phase cobalt platinum nano particle can be obtained after washing, drying.
Embodiment 14: it is molten that the ethyl alcohol that concentration is 0.01mol/L is configured to the acetylacetone cobalt of equimolar amounts and chloroplatinic acid
Liquid impregnates sodium chloride powder, after removing extra maceration extract, powder is dry.By the powder after drying in 800 DEG C of hydrogen reducings,
Ordered phase cobalt platinum nano particle can be obtained after washing, drying.
Embodiment 15: being configured to the ethanol solution that concentration is 1mol/L with the acetylacetone cobalt of equimolar amounts and chloroplatinic acid,
Sodium chloride powder is impregnated, it is after removing extra maceration extract, powder is dry.By the powder after drying in 800 DEG C of hydrogen reducings, water
Wash, dry after ordered phase cobalt platinum nano particle can be obtained.
Embodiment 16: it is molten that the ethylene glycol that concentration is 1mol/L is configured to the acetylacetone cobalt of equimolar amounts and chloroplatinic acid
Liquid impregnates sodium chloride powder, after removing extra maceration extract, powder is dry.By the powder after drying in 800 DEG C of hydrogen reducings,
Ordered phase cobalt platinum nano particle can be obtained after washing, drying.
Embodiment 17: being configured to the acetone soln that concentration is 1mol/L with the acetylacetone cobalt of equimolar amounts and chloroplatinic acid,
Sodium chloride powder is impregnated, it is after removing extra maceration extract, powder is dry.By the powder after drying in 800 DEG C of hydrogen reducings, water
Wash, dry after ordered phase cobalt platinum nano particle can be obtained.
Embodiment 18: being configured to the ethanol solution that concentration is 1mol/L with the acetylacetone cobalt of equimolar amounts and chloroplatinic acid,
Sodium chloride powder is impregnated, it is after removing extra maceration extract, powder is dry.By the powder after drying in 800 DEG C of hydrogen reducings, water
Wash, dry after ordered phase cobalt platinum nano particle can be obtained.
Embodiment 19: it is molten that the ethylene glycol that concentration is 0.1mol/L is configured to the acetylacetone cobalt of equimolar amounts and chloroplatinic acid
Liquid impregnates sodium chloride powder, after removing extra maceration extract, powder is dry.By the powder after drying in 800 DEG C of hydrogen reducings,
Ordered phase cobalt platinum nano particle can be obtained after washing, drying.
Embodiment 20: it is molten that the acetone that concentration is 0.1mol/L is configured to the acetylacetone cobalt of equimolar amounts and chloroplatinic acid
Liquid impregnates sodium chloride powder, after removing extra maceration extract, powder is dry.By the powder after drying in 800 DEG C of hydrogen reducings,
Ordered phase cobalt platinum nano particle can be obtained after washing, drying.
Embodiment 21: it is molten that the ethyl alcohol that concentration is 0.1mol/L is configured to the acetylacetone cobalt of equimolar amounts and chloroplatinic acid
Liquid impregnates sodium chloride powder, after removing extra maceration extract, powder is dry.By the powder after drying 800 DEG C of carbon monoxide also
Ordered phase cobalt platinum nano particle can be obtained after washing, drying in original.
Embodiment 22: it is molten that the ethyl alcohol that concentration is 0.1mol/L is configured to the acetylacetone cobalt of equimolar amounts and chloroplatinic acid
Liquid impregnates sodium chloride powder, after removing extra maceration extract, powder is dry.By the powder after drying in 800 DEG C of nitrogen and hydrogen mixtures
Ordered phase cobalt platinum nano particle can be obtained after washing, drying in reduction.
Embodiment 23: it is molten that the ethyl alcohol that concentration is 0.1mol/L is configured to the acetylacetone cobalt of equimolar amounts and chloroplatinic acid
Liquid impregnates sodium chloride powder, after removing extra maceration extract, powder is dry.By the powder after drying, hydrogen is also between 500 DEG C
Ordered phase cobalt platinum nano particle can be obtained after washing, drying in original.
Embodiment 24: it is molten that the ethyl alcohol that concentration is 0.1mol/L is configured to the acetylacetone cobalt of equimolar amounts and chloroplatinic acid
Liquid impregnates sodium chloride powder, after removing extra maceration extract, powder is dry.By the powder after drying in 700 DEG C of hydrogen reducings,
Ordered phase cobalt platinum nano particle can be obtained after washing, drying.
Claims (10)
1. a kind of preparation method of ordered phase nanometer Fe-Pt particle, which is characterized in that method includes the following steps:
1) ferric acetyl acetonade of equimolar amounts and chloroplatinic acid are dissolved in organic solvent, as maceration extract；
2) organic solvent is evaporated after removing extra maceration extract with maceration extract dipping sodium chloride powder；
3) the water soluble salt powder after dipping is calcined in high-temperature reductibility atmosphere；
4) by powder washing, the drying after reduction, nanometer Fe-Pt particle is obtained.
2. a kind of preparation method of ordered phase nanometer Fe-Pt particle according to claim 1, which is characterized in that the step
1) organic solvent in is ethyl alcohol, ethylene glycol or acetone.
3. a kind of preparation method of ordered phase nanometer Fe-Pt particle according to claim 1, which is characterized in that the step
1) concentration of the maceration extract obtained is 0.001mol/L~1mol/L.
4. a kind of preparation method of ordered phase nanometer Fe-Pt particle according to claim 1, which is characterized in that the step
3) high temperature range in is between 500 DEG C to 800 DEG C.
5. a kind of preparation method of ordered phase nanometer Fe-Pt particle according to claim 1, which is characterized in that the step
3) reducing atmosphere in refers to hydrogen, nitrogen and hydrogen mixture or carbon monoxide.
6. a kind of preparation method of ordered phase cobalt platinum nano particle, which is characterized in that method includes the following steps:
1) acetylacetone cobalt of equimolar amounts and chloroplatinic acid are dissolved in organic solvent, as maceration extract；
2) organic solvent is evaporated after removing extra maceration extract with maceration extract dipping sodium chloride powder；
3) the water soluble salt powder after dipping is calcined in high-temperature reductibility atmosphere；
4) by powder washing, the drying after reduction, cobalt platinum nano particle is obtained.
7. a kind of preparation method of ordered phase cobalt platinum nano particle according to claim 1, which is characterized in that the step
1) organic solvent in is ethyl alcohol, ethylene glycol or acetone.
8. a kind of preparation method of ordered phase cobalt platinum nano particle according to claim 1, which is characterized in that the step
1) concentration of the maceration extract obtained is 0.001mol/L~1mol/L.
9. a kind of preparation method of ordered phase cobalt platinum nano particle according to claim 1, which is characterized in that the step
3) high temperature range in is between 500 DEG C to 800 DEG C.
10. a kind of preparation method of ordered phase cobalt platinum nano particle according to claim 1, which is characterized in that the step
It is rapid 3) in reducing atmosphere refer to hydrogen, nitrogen and hydrogen mixture or carbon monoxide.
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| CN115064718A (en) * | 2022-06-03 | 2022-09-16 | 北京亿华通科技股份有限公司 | Small-particle-size PtFe structure ordered fuel cell catalyst and preparation method and application thereof |
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