CN109604628B - Preparation method of ordered phase iron platinum nano-particles and cobalt platinum nano-particles - Google Patents
Preparation method of ordered phase iron platinum nano-particles and cobalt platinum nano-particles Download PDFInfo
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Abstract
The invention discloses a preparation method of ordered phase iron platinum nano-particles and cobalt platinum nano-particles, which comprises the steps of dissolving iron acetylacetonate (or cobalt) and chloroplatinic acid in an organic solvent to be used as an impregnation solution, impregnating sodium chloride powder, reducing under a sodium chloride melting point after drying, and washing with water to obtain the iron platinum (or cobalt platinum) nano-particles. The invention can rapidly prepare the high-dispersity ordered phase iron platinum nanoparticles and cobalt platinum nanoparticles in batches, and the particle sizes are uniform.
Description
Technical Field
The invention relates to a preparation method of ordered phase iron platinum nano particles and cobalt platinum nano particles, belonging to the field of magnetic alloy particle preparation.
Background
Ordered phase (also known as L1)0Phase, face-centered tetragonal phase) iron platinum (FePt) and cobalt platinum (CoPt) nanoparticles have high magnetocrystalline anisotropy constants and therefore ultra-small superparamagnetic critical dimension (D ═ 2.8-3.3 nm), while ordered phase iron platinum and cobalt platinum nanoparticles have high coercivity, high magnetic energy product, high Curie temperature (Tc ═ 480 ℃) and good physical and chemical stability. Therefore, the ordered phase iron platinum and cobalt platinum nano-particles always receive wide attention, and have good application prospects in the aspects of future ultrahigh-density magnetic recording media, new nano exchange elastic magnet materials, high-performance catalyst materials and the like.
FePt/CoPt mainly has two structures of face-centered cubic and face-centered tetragonal. The face centered cubic (fcc) structure is a chemically disordered phase, Fe/Co and Pt atoms occupy each lattice randomly, and the probability is 50%. The disordered phase structure exhibits superparamagnetism in terms of magnetism and cannot be used as a magnetic recording material. The face-centered tetragonal (fct) structure is a chemical ordered phase, and Fe atoms and Pt atoms of the ordered phase are alternately arranged in a layer shape in the c-axis direction. The ordered phase FePt/CoPt has strong magnetocrystalline anisotropy and large coercive force, and is the first choice material of future ultra-high density magnetic recording media.
FePt/CoPt nanoparticles are typically prepared using an oil phase thermal decomposition process, but the nanoparticles prepared by this process are disordered phases and do not have high magnetocrystalline anisotropy. The disordered phase FePt/CoPt nano-particles need to be annealed at a high temperature of more than 500 ℃ to obtain an ordered phase. However, after high-temperature annealing, although FePt/CoPt nanoparticles can be converted into ordered phase, the nanoparticles can be seriously sintered and aged, and the ultra-small particle size and monodispersity of the nanoparticles are difficult to maintain. At present, the idea of solving the problem mainly comprises: core-shell coating method. Performing core-shell coating on the FePt/CoPt nano-particles by using MgO or MnO, and carrying out acid washing after high-temperature annealing to obtain the ordered phase FePt/CoPt nano-particles. However, the core-shell coating method has various steps, and the crystal lattice is easy to damage and the magnetic property is reduced in the acid washing process; and (II) a water-soluble salt isolation method. The method comprises the steps of firstly preparing disordered FePt/CoPt nano particles as a precursor, grinding and mixing the disordered FePt/CoPt particles and NaCl salt (with a melting point of 801 ℃) in an organic solvent, carrying out high-temperature annealing after the solvent is evaporated, and washing with water to obtain ordered-phase FePt/CoPt particles. However, the method not only needs to prepare disordered-phase FePt/CoPt particles in advance, but also needs to grind salt particles, has complex working procedures and overhigh preparation cost, and is only suitable for preparing a small amount of samples in a laboratory.
In summary, the ordered phase FePt/CoPt nanoparticles prepared by the prior art have the defects of high preparation cost, complex process and the like, and a simple method for preparing the ordered phase FePt/CoPt nanoparticles in a large scale does not exist at present.
Disclosure of Invention
The technical problem is as follows: the invention provides a preparation method of ordered phase iron platinum nano-particles and an ordered phase cobalt platinum nano-particles, which are simple and easy to implement, can produce the ordered phase iron platinum nano-particles with dispersed particles and uniform sizes, and the prepared ordered phase iron platinum nano-particles have good crystallinity and dispersibility and excellent magnetic performance.
The technical scheme is as follows: the preparation method of the ordered phase iron-platinum nano-particles comprises the following steps:
1) dissolving equimolar amounts of ferric acetylacetonate and chloroplatinic acid in an organic solvent to obtain an impregnation solution;
2) soaking sodium chloride powder in the soaking solution, removing redundant soaking solution, and evaporating the organic solvent to dryness;
3) calcining the impregnated water-soluble salt powder in a high-temperature reducing atmosphere;
4) and washing and drying the reduced powder to obtain the iron-platinum nano-particles.
Further, in the preparation method of the ordered phase iron-platinum nanoparticle of the present invention, the organic solvent in step 1) is ethanol, ethylene glycol or acetone.
Further, in the preparation method of the ordered phase iron-platinum nano-particles, the concentration of the impregnation liquid obtained in the step 1) is 0.001 mol/L-1 mol/L.
Further, in the preparation method of the ordered phase iron platinum nano-particles, the high temperature range in the step 3) is between 500 ℃ and 800 ℃.
Further, in the preparation method of the ordered phase iron-platinum nanoparticles, the reducing atmosphere in the step 3) refers to hydrogen, a nitrogen-hydrogen mixed gas or carbon monoxide.
The preparation method of the ordered phase cobalt-platinum nano-particles comprises the following steps:
1) dissolving equal molar amounts of cobalt acetylacetonate and chloroplatinic acid in an organic solvent to obtain an impregnation solution;
2) soaking sodium chloride powder in the soaking solution, removing redundant soaking solution, and evaporating the organic solvent to dryness;
3) calcining the impregnated water-soluble salt powder in a high-temperature reducing atmosphere;
4) and washing and drying the reduced powder to obtain the cobalt-platinum nano-particles.
Further, in the preparation method of the ordered phase cobalt platinum nanoparticle of the present invention, the organic solvent in the step 1) is ethanol, ethylene glycol or acetone.
Further, in the preparation method of the ordered-phase cobalt-platinum nanoparticles, the concentration of the impregnation liquid obtained in the step 1) is 0.001 mol/L-1 mol/L.
Further, in the preparation method of the ordered phase cobalt platinum nanoparticles, the high temperature range in the step 3) is between 500 ℃ and 800 ℃.
Further, in the preparation method of the ordered phase cobalt platinum nanoparticles, the reducing atmosphere in the step 3) refers to hydrogen, a nitrogen-hydrogen mixed gas or carbon monoxide.
Has the advantages that: compared with the prior art, the invention has the following advantages:
the existing method for preparing the ordered phase FePt/CoPt nano-particles mainly comprises a core-shell coating method and a water-soluble salt isolation method. Both methods need to prepare disordered phase FePt/CoPt nanoparticles as a precursor in advance, then coat the particle surface or grind the particles together with water-soluble salt particles, and then anneal the particles at high temperature to generate ordered phase, so that the method has the advantages of complex working procedure, high cost and difficult scale production, and the prepared FePt/CoPt nanoparticles are difficult to control in size and poor in magnetic performance.
The invention adopts a simple and easy impregnation method to prepare the ordered phase FePt/CoPt nano-particles, firstly, ferric acetylacetonate (cobalt acetylacetonate) and chloroplatinic acid are dissolved in an organic solvent (sodium chloride can not have larger solubility in the organic solvent) to be used as an impregnation solution. The sodium chloride powder is impregnated with the impregnation solution, and after the organic solvent is evaporated, iron (cobalt) and platinum elements are present on the surface of the sodium chloride particles. And then calcining the mixture in a high-temperature reducing atmosphere to react to generate the ordered phase FePt/CoPt, cooling and washing the mixture with water to remove sodium chloride, thereby obtaining the dispersed ordered phase FePt/CoPt nano-particles.
The method is used for preparing the dispersed ordered phase FePt/CoPt nano particles, and the premise is that the ferric acetylacetonate, the cobalt acetylacetonate and the chloroplatinic acid can be uniformly spread on the surfaces of sodium chloride salt particles, but do not exist in an aggregated particle state. The research shows that the three raw materials have stronger adsorption with sodium chloride in the organic solvent selected by the invention, and the organic solvent can be uniformly distributed on the surface of sodium chloride particles after being dried by distillation. Therefore, iron (cobalt) and platinum elements which are uniformly distributed at high temperature can produce ordered phase FePt/CoPt nanoparticles with dispersed particles and uniform size.
The invention can rapidly prepare the ordered phase FePt/CoPt nano-particles with good dispersibility in batches, and the prepared ordered phase FePt/CoPt nano-particles have good crystallinity. In addition, the preparation method does not need to prepare disordered phase ordered phase FePt/CoPt nano particles in advance, has simple and convenient process and is easy for large-scale production.
Drawings
Fig. 1 is ordered phase iron platinum nano-particles prepared by the invention.
Detailed Description
The invention is further described with reference to the following examples and the accompanying drawings.
Example 1: soaking sodium chloride powder in 0.1mol/L ethanol solution prepared from iron acetylacetonate and chloroplatinic acid in equimolar amount, removing excessive soaking solution, and drying the powder. And reducing the dried powder with hydrogen at 800 ℃, washing with water, and drying to obtain the ordered phase iron-platinum nano-particles.
Example 2: soaking sodium chloride powder in 0.01mol/L ethanol solution prepared from iron acetylacetonate and chloroplatinic acid in equimolar amount, removing excessive soaking solution, and drying the powder. And reducing the dried powder with hydrogen at 800 ℃, washing with water, and drying to obtain the ordered phase iron-platinum nano-particles.
Example 3: soaking sodium chloride powder in ethanol solution with concentration of 1mol/L prepared from equimolar amount of ferric acetylacetonate and chloroplatinic acid, removing excessive soaking solution, and drying the powder. And reducing the dried powder with hydrogen at 800 ℃, washing with water, and drying to obtain the ordered phase iron-platinum nano-particles.
Example 4: sodium chloride powder was impregnated with an ethylene glycol solution prepared with equimolar amounts of iron acetylacetonate and chloroplatinic acid to a concentration of 1mol/L, and after removing the excess impregnation solution, the powder was dried. And reducing the dried powder with hydrogen at 800 ℃, washing with water, and drying to obtain the ordered phase iron-platinum nano-particles.
Example 5: sodium chloride powder was impregnated with an acetone solution prepared with equimolar amounts of iron acetylacetonate and chloroplatinic acid to a concentration of 1mol/L, and after removing the excess impregnation solution, the powder was dried. And reducing the dried powder with hydrogen at 800 ℃, washing with water, and drying to obtain the ordered phase iron-platinum nano-particles.
Example 6: soaking sodium chloride powder in ethanol solution with concentration of 1mol/L prepared from equimolar amount of ferric acetylacetonate and chloroplatinic acid, removing excessive soaking solution, and drying the powder. And reducing the dried powder with hydrogen at 800 ℃, washing with water, and drying to obtain the ordered phase iron-platinum nano-particles.
Example 7: sodium chloride powder was impregnated with an ethylene glycol solution having a concentration of 0.1mol/L prepared from equimolar amounts of iron acetylacetonate and chloroplatinic acid, and after removing the excess impregnation solution, the powder was dried. And reducing the dried powder with hydrogen at 800 ℃, washing with water, and drying to obtain the ordered phase iron-platinum nano-particles.
Example 8: sodium chloride powder was impregnated with an acetone solution prepared with equimolar amounts of iron acetylacetonate and chloroplatinic acid to a concentration of 0.1mol/L, and after removing the excess impregnation solution, the powder was dried. And reducing the dried powder with hydrogen at 800 ℃, washing with water, and drying to obtain the ordered phase iron-platinum nano-particles.
Example 9: soaking sodium chloride powder in 0.1mol/L ethanol solution prepared from iron acetylacetonate and chloroplatinic acid in equimolar amount, removing excessive soaking solution, and drying the powder. Reducing the dried powder with carbon monoxide at 800 ℃, washing with water, and drying to obtain the ordered phase iron platinum nanoparticles.
Example 10: soaking sodium chloride powder in 0.1mol/L ethanol solution prepared from iron acetylacetonate and chloroplatinic acid in equimolar amount, removing excessive soaking solution, and drying the powder. And reducing the dried powder at 800 ℃ by using a nitrogen-hydrogen mixed gas, washing with water, and drying to obtain the ordered phase iron-platinum nano-particles.
Example 11: soaking sodium chloride powder in 0.1mol/L ethanol solution prepared from iron acetylacetonate and chloroplatinic acid in equimolar amount, removing excessive soaking solution, and drying the powder. And reducing the dried powder with hydrogen at 500 ℃, washing with water, and drying to obtain the ordered phase iron-platinum nano-particles.
Example 12: soaking sodium chloride powder in 0.1mol/L ethanol solution prepared from iron acetylacetonate and chloroplatinic acid in equimolar amount, removing excessive soaking solution, and drying the powder. And reducing the dried powder with hydrogen at 700 ℃, washing with water, and drying to obtain the ordered phase iron-platinum nano-particles.
Example 13: soaking sodium chloride powder in 0.1mol/L ethanol solution prepared from cobalt acetylacetonate and chloroplatinic acid in equal molar amount, removing excessive soaking solution, and drying the powder. And reducing the dried powder with hydrogen at 800 ℃, washing with water, and drying to obtain the ordered-phase cobalt-platinum nano-particles.
Example 14: soaking sodium chloride powder in 0.01mol/L ethanol solution prepared from cobalt acetylacetonate and chloroplatinic acid in equimolar amount, removing excessive soaking solution, and drying the powder. And reducing the dried powder with hydrogen at 800 ℃, washing with water, and drying to obtain the ordered-phase cobalt-platinum nano-particles.
Example 15: soaking sodium chloride powder in 1mol/L ethanol solution prepared from cobalt acetylacetonate and chloroplatinic acid in equal molar amounts, removing excessive soaking solution, and drying the powder. And reducing the dried powder with hydrogen at 800 ℃, washing with water, and drying to obtain the ordered-phase cobalt-platinum nano-particles.
Example 16: the sodium chloride powder was impregnated with an ethylene glycol solution prepared with equimolar amounts of cobalt acetylacetonate and chloroplatinic acid to a concentration of 1mol/L, and after removing the excess impregnation solution, the powder was dried. And reducing the dried powder with hydrogen at 800 ℃, washing with water, and drying to obtain the ordered-phase cobalt-platinum nano-particles.
Example 17: the sodium chloride powder was impregnated with an acetone solution prepared with equimolar amounts of cobalt acetylacetonate and chloroplatinic acid to a concentration of 1mol/L, and after removing the excess impregnation solution, the powder was dried. And reducing the dried powder with hydrogen at 800 ℃, washing with water, and drying to obtain the ordered-phase cobalt-platinum nano-particles.
Example 18: soaking sodium chloride powder in 1mol/L ethanol solution prepared from cobalt acetylacetonate and chloroplatinic acid in equal molar amounts, removing excessive soaking solution, and drying the powder. And reducing the dried powder with hydrogen at 800 ℃, washing with water, and drying to obtain the ordered-phase cobalt-platinum nano-particles.
Example 19: sodium chloride powder was impregnated with an ethylene glycol solution having a concentration of 0.1mol/L prepared from cobalt acetylacetonate and chloroplatinic acid in equimolar amounts, and after removing the excess impregnation solution, the powder was dried. And reducing the dried powder with hydrogen at 800 ℃, washing with water, and drying to obtain the ordered-phase cobalt-platinum nano-particles.
Example 20: sodium chloride powder was impregnated with an acetone solution having a concentration of 0.1mol/L prepared from equimolar amounts of cobalt acetylacetonate and chloroplatinic acid, and after removing the excess impregnation solution, the powder was dried. And reducing the dried powder with hydrogen at 800 ℃, washing with water, and drying to obtain the ordered-phase cobalt-platinum nano-particles.
Example 21: soaking sodium chloride powder in 0.1mol/L ethanol solution prepared from cobalt acetylacetonate and chloroplatinic acid in equal molar amount, removing excessive soaking solution, and drying the powder. Reducing the dried powder with carbon monoxide at 800 ℃, washing with water, and drying to obtain the ordered-phase cobalt-platinum nanoparticles.
Example 22: soaking sodium chloride powder in 0.1mol/L ethanol solution prepared from cobalt acetylacetonate and chloroplatinic acid in equal molar amount, removing excessive soaking solution, and drying the powder. And reducing the dried powder at 800 ℃ by using a nitrogen-hydrogen mixed gas, washing with water, and drying to obtain the ordered-phase cobalt-platinum nano-particles.
Example 23: soaking sodium chloride powder in 0.1mol/L ethanol solution prepared from cobalt acetylacetonate and chloroplatinic acid in equal molar amount, removing excessive soaking solution, and drying the powder. And reducing the dried powder with hydrogen at 500 ℃, washing with water, and drying to obtain the ordered-phase cobalt-platinum nano-particles.
Example 24: soaking sodium chloride powder in 0.1mol/L ethanol solution prepared from cobalt acetylacetonate and chloroplatinic acid in equal molar amount, removing excessive soaking solution, and drying the powder. And reducing the dried powder with hydrogen at 700 ℃, washing with water, and drying to obtain the ordered-phase cobalt-platinum nano-particles.
Claims (6)
1. A method for preparing ordered phase iron-platinum nano particles is characterized by comprising the following steps:
1) dissolving equimolar amounts of ferric acetylacetonate and chloroplatinic acid in an organic solvent to obtain an impregnation solution, wherein the organic solvent is ethanol, ethylene glycol or acetone, and the concentration of the impregnation solution is 0.001-1 mol/L;
2) soaking sodium chloride powder in the soaking solution, removing redundant soaking solution, and evaporating the organic solvent to dryness;
3) calcining the impregnated water-soluble salt powder in a high-temperature reducing atmosphere;
4) and washing and drying the reduced powder to obtain the iron-platinum nano-particles.
2. The method for preparing ordered phase FePt nanoparticles according to claim 1, wherein the high temperature in step 3) is in the range of 500-800 ℃.
3. The method for preparing ordered phase FePt nanoparticles according to claim 1, wherein the reducing atmosphere in step 3) is hydrogen, mixed gas of nitrogen and hydrogen, or carbon monoxide.
4. A method for preparing ordered phase cobalt-platinum nano particles is characterized by comprising the following steps:
1) dissolving equal molar amounts of cobalt acetylacetonate and chloroplatinic acid in an organic solvent to obtain an impregnation solution, wherein the organic solvent is ethanol, ethylene glycol or acetone, and the concentration of the impregnation solution is 0.001-1 mol/L;
2) soaking sodium chloride powder in the soaking solution, removing redundant soaking solution, and evaporating the organic solvent to dryness;
3) calcining the impregnated water-soluble salt powder in a high-temperature reducing atmosphere;
4) and washing and drying the reduced powder to obtain the cobalt-platinum nano-particles.
5. The method for preparing ordered cobalt-platinum nanoparticles as claimed in claim 4, wherein the high temperature in step 3) is in the range of 500 ℃ to 800 ℃.
6. The method for preparing ordered cobalt-platinum nanoparticles as claimed in claim 4, wherein the reducing atmosphere in step 3) is hydrogen, a mixture of nitrogen and hydrogen, or carbon monoxide.
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