CN108500284B - Fe/L10Preparation method of-FePt composite nano material - Google Patents
Fe/L10Preparation method of-FePt composite nano material Download PDFInfo
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Abstract
The invention discloses a Fe/L10A preparation method of the-FePt composite nano material. The preparation method comprises: mixing Fe nanoparticles with PtCl4Uniformly mixing the aqueous solution to form a mixed solution; further dropping a part of PtCl into the mixed solution4Water solution, and ultrasonic reaction is carried out at normal temperature to obtain a reaction product; annealing the reaction product in a reducing atmosphere at 500-750 ℃ to obtain Fe/L10-FePt composite nanomaterial. The preparation method is a water-based synthesis method, the used reagent is a common non-toxic water-based reagent, organic matters are not needed to participate, toxic byproducts are not generated in the reaction process, the synthesis steps are simple and easy to implement, and the preparation method is a green and environment-friendly preparation process. Fe/L1 obtained by the preparation method of the invention0Fe in the FePt composite nano material is not easy to be oxidized in the interior, so that the composite nano material has good chemical stability.
Description
Technical Field
The invention relates to Fe/L10-FePt composite nano material and a preparation method thereof, belonging to the field of magnetic nano material.
Background
The nano double-phase composite material can obtain the high coercive force of a hard magnetic phase and also has the high saturation magnetization intensity of a soft magnetic phase, so that an ideal maximum magnetic energy product is obtained, and a high-performance permanent magnetic material can be prepared. Skomsk predicts that an exchange-spring type highly oriented nanocomposite magnetic material with appropriate exchange coupling can achieve 1096kJ/m3The magnetic energy product of (1) is about the theoretical limit of Nd-Fe-B [516kJ/m3]Twice as much. Due to L10FePt of the structure not only has extremely high chemical stability, but also has very high magnetocrystalline anisotropy constant and high corrosion resistance, thereby attracting great attention. Currently, the preparation of Fe/L1 is adopted in the industry0The mainstream method of-FePt is a high-temperature organic liquid phase chemical synthesis method. The nano particles prepared by the high-temperature organic liquid phase chemical synthesis method are annealed to obtain Fe/L10-FePt. However, the high-temperature organic liquid phase chemical synthesis method adopts oil synthesis, most of the reagents are toxic, and organic matters or toxic byproducts are continuously volatilized in the reaction process, thereby causing environmental pollution. And the replacement reaction method adopted by usThe method is an environment-friendly synthesis method, and no organic matters participate in the reaction process and no toxic by-products are generated in the reaction process.
Disclosure of Invention
The invention mainly aims to provide Fe/L10A preparation method of FePt composite nano material, which overcomes the defects in the prior art.
In order to achieve the purpose, the technical scheme adopted by the invention comprises the following steps:
the embodiment of the invention provides Fe/L10-a method for preparing a FePt composite nanomaterial comprising:
mixing Fe nanoparticles with PtCl4Uniformly mixing the aqueous solution to form a mixed solution;
further dropping a part of PtCl into the mixed solution4Water solution, and ultrasonic reaction is carried out at normal temperature to obtain a reaction product;
annealing the reaction product in a reducing atmosphere at 500-750 ℃ to obtain Fe/L10-FePt composite nanomaterial.
In some embodiments, the method of making comprises:
providing PtCl4An aqueous solution;
reacting part of PtCl4Uniformly mixing the water solution and the Fe nano particles to form a mixed solution;
the residual PtCl is removed4And dripping the aqueous solution into the mixed solution, and carrying out ultrasonic reaction at normal temperature to obtain the reaction product.
Preferably, the preparation method comprises the following steps: dropping the residual PtCl at a dropping rate of 0.1-0.4 ml/min4And (3) slowly dripping the aqueous solution into the mixed solution, wherein the dripping speed is particularly preferably 0.1-0.15 ml/min.
Preferably, the preparation method comprises the following steps: the residual PtCl is removed4And (3) dripping the aqueous solution into the mixed solution, and carrying out ultrasonic reaction for 15-45 min at normal temperature, particularly preferably for 30-45 min to obtain the reaction product.
In some embodiments, the method of making further comprises: and washing and drying the obtained reaction product, and then carrying out the annealing treatment in the reducing atmosphere.
In some embodiments, the PtCl is4The concentration of the aqueous solution is 0.005-0.02 mol/L, preferably 0.005-0.015 mol/L.
In some embodiments, PtCl in the mixed solution4The molar ratio to Fe is 1: 2.91-1: 4.49, preferably 1: 3-1: 4, particularly preferably 1: 3.1.
in some embodiments, the Fe nanoparticles comprise Fe nanoparticles.
Preferably, the particle size of the Fe nano-particles is 30-500 nm.
Further, the preparation method of the Fe nanoparticles comprises the following steps: and carrying out reduction annealing on the FeOOH nano particles for 2-10 h at 350-550 ℃ in a reducing atmosphere to obtain Fe nano particles.
In some embodiments, the method of making comprises: and placing the reaction product in a reducing atmosphere, heating to the annealing temperature at a heating rate of 5-10 ℃/min, and preserving heat for 30-240 min, thereby finishing the annealing treatment.
Preferably, the annealing temperature is 550-750 ℃, and particularly preferably 550-650 ℃.
Preferably, the time of the annealing treatment is 30-120 min.
In some embodiments, the method of making comprises: placing the reaction product in a reaction chamber, removing air in the reaction chamber, introducing reducing gas to form the reducing atmosphere, and then carrying out annealing treatment; preferably, the flow rate of the reducing gas is 200 to 400 ml/min.
Preferably, the reducing atmosphere is formed by a reducing gas, and the reducing gas comprises a mixed gas of hydrogen and an inert gas; preferably, the reducing gas comprises 0-95 v/v% argon and 5-100 v/v% hydrogen.
The embodiment of the invention also provides Fe/L1 prepared by the method0-FePt composite nanomaterial.
Compared with the prior art, the invention has the advantages that:
(1) the invention provides Fe/L10The preparation method of the-FePt composite nano material is a water-based synthesis method, the used reagent is a common non-toxic water-based reagent, no organic matter participates, no toxic by-product is generated in the reaction process, the synthesis steps are simple and easy to implement, and the preparation method is a green and environment-friendly preparation process;
(2) Fe/L1 obtained by the preparation method of the invention0Fe in the FePt composite nano material is not easy to be oxidized in the interior, so that the composite nano material has good chemical stability.
Drawings
FIG. 1 is L1 obtained in example 1 of the present invention0-XRD pattern of FePt nanomaterial;
FIG. 2 is L1 obtained in example 1 of the present invention0-VSM spectra of FePt nanomaterials;
FIG. 3 is L1 obtained in example 1 of the present invention0-TEM spectra of FePt nanomaterials;
FIG. 4 shows Fe/L1 obtained in example 2 of the present invention0-XRD pattern of FePt composite nanomaterial;
FIG. 5 shows Fe/L1 obtained in example 2 of the present invention0-VSM profile of FePt composite nanomaterial;
FIG. 6 shows Fe/L1 obtained in example 2 of the present invention0-VSM profile of FePt composite nanomaterial after one week of standing in air;
FIG. 7 shows Fe/L1 obtained in example 2 of the present invention0-TEM spectra of FePt composite nanomaterials;
FIG. 8 shows Fe/L1 obtained in example 3 of the present invention0-XRD pattern of FePt composite nanomaterial;
FIG. 9 shows Fe/L1 obtained in example 3 of the present invention0-VSM profile of FePt composite nanomaterial;
FIG. 10 shows Fe/L1 obtained in example 3 of the present invention0-TEM spectra of FePt composite nanomaterials;
FIG. 11 is Fe/L1 obtained in example 4 of the present invention0VSM plot of-FePt composite nanomaterialA spectrum;
FIG. 12 shows Fe/L1 obtained in example 5 of the present invention0-VSM profile of FePt composite nanomaterial.
Detailed Description
In view of the defects of the prior art, the inventor of the present invention has made long-term research and great practice to provide the technical scheme of the present invention, which mainly adopts a displacement reaction method, is aqueous synthesis, has no participation of organic matters in the reaction process, and has no generation of toxic by-products, and is an environment-friendly synthesis method. The technical solution, its implementation and principles, etc. will be further explained as follows.
One aspect of an embodiment of the present invention provides a Fe/L10-a method for preparing a FePt composite nanomaterial comprising:
mixing Fe nanoparticles with PtCl4Uniformly mixing the aqueous solution to form a mixed solution;
further dropping PtCl into the mixed solution4Water solution, and ultrasonic reaction is carried out at normal temperature to obtain a reaction product;
annealing the reaction product in a reducing atmosphere at 500-750 ℃ to obtain Fe/L10-FePt composite nanomaterial.
In some embodiments, the method of making comprises:
providing PtCl4An aqueous solution;
reacting part of PtCl4Uniformly mixing the water solution and the Fe nano particles to form a mixed solution;
the residual PtCl is removed4And dripping the aqueous solution into the mixed solution, and carrying out ultrasonic reaction at normal temperature to obtain the reaction product.
According to the invention, all the PtCl4 aqueous solution and the Fe nanoparticles are not mixed at one time, but a batch adding mode is adopted, so that the phenomenon that the reaction is uneven and the tested hysteresis loop has a waist collapse phenomenon if all the PtCl4 aqueous solution and the Fe nanoparticles are mixed at one time can be avoided.
Preferably, the preparation method comprises the following steps: dropping the residual PtCl at a dropping rate of 0.1-0.4 ml/min4And (3) slowly dripping the aqueous solution into the mixed solution, wherein the dripping speed is particularly preferably 0.1-0.15 ml/min.
Preferably, the preparation method comprises the following steps: the residual PtCl is removed4And (3) dripping the aqueous solution into the mixed solution, and carrying out ultrasonic reaction for 15-45 min at normal temperature, particularly preferably for 30-45 min to obtain the reaction product.
In some embodiments, the method of making further comprises: and washing and drying the obtained reaction product, and then carrying out the annealing treatment in the reducing atmosphere.
In some embodiments, the PtCl is4The concentration of the aqueous solution is 0.005-0.02 mol/L, preferably 0.005-0.015 mol/L.
In some embodiments, PtCl in the mixed solution4The molar ratio to Fe is 1: 2.91-1: 4.49, preferably 1: 3-1: 4, particularly preferably 1: 3.1.
when the molar ratio of PtCl4 to Fe in the mixed solution is 1: 2.91-1: 4.49 to obtain L10-FePt or Fe/L10-FePt, but the ratio of 1: 3-1: 4, the obtained L10-FePt or Fe/L10-FePt has higher performance, and Fe/L10-FePt can be obtained when the molar ratio of PtCl4 to Fe reaches 1: 3.1.
In some embodiments, the Fe nanoparticles include Fe nanoparticles, and may also be Fe nanorods formed from Fe nanoparticles.
Preferably, the particle size of the Fe nano-particles is 30-500 nm.
Further, the preparation method of the Fe nanoparticles comprises the following steps: and carrying out reduction annealing on the FeOOH nano particles for 2-10 h at 350-550 ℃ in a reducing atmosphere to obtain Fe nano particles.
In some embodiments, the method of making comprises: and placing the reaction product in a reducing atmosphere, heating to the annealing temperature at a heating rate of 5-10 ℃/min, and preserving heat for 30-240 min, thereby finishing the annealing treatment.
Preferably, the annealing temperature is 550-750 ℃, and particularly preferably 550-650 ℃.
Preferably, the time of the annealing treatment is 30-120 min.
In some embodiments, the method of making comprises: placing the reaction product in a reaction chamber, removing air in the reaction chamber, introducing reducing gas to form the reducing atmosphere, and then carrying out annealing treatment; preferably, the flow rate of the reducing gas is 200 to 400 ml/min.
Preferably, the reducing atmosphere is formed by a reducing gas, and the reducing gas comprises a mixed gas of hydrogen and an inert gas; preferably, the reducing gas comprises 0-95 v/v% argon and 5-100 v/v% hydrogen.
In some more typical embodiments, the preparation method may include the steps of:
(1) preparing Fe nanoparticles;
(2) reacting PtCl4Placing the mixture in deionized water for ultrasonic dispersion to obtain uniform PtCl4An aqueous solution;
(3) taking part of the PtCl4Mixing the water solution with the Fe nano particles and carrying out ultrasonic treatment to obtain a mixed solution;
(4) leaving the PtCl4Dropwise adding the aqueous solution into the mixed solution to perform ultrasonic reaction at normal temperature to obtain a reaction product;
(5) centrifugally washing the reaction product, and then drying;
(6) annealing the obtained reaction product to obtain Fe/L10-FePt composite nanomaterial.
Another aspect of an embodiment of the invention also provides Fe/L1 prepared by the foregoing method0-FePt composite nanomaterial.
In summary, the present invention first prepares PtCl with a certain concentration4Then taking part of the above PtCl4Mixing the aqueous solution with Fe nanoparticles prepared in advance and performing ultrasonic treatment, and then adding the rest PtCl4The aqueous solution was added dropwise to PtCl4And carrying out ultrasonic reaction on the mixed solution of the aqueous solution and the Fe nano particles at normal temperature to obtain a reaction product. Centrifuging, washing, drying, and annealingThus obtaining Fe/L10-FePt composite nanomaterial.
The technical solution of the present invention is further described in detail by the following examples. However, the examples are chosen only for the purpose of illustrating the invention and are not to be construed as limiting the scope of the invention.
Example 1
(1) Preparing Fe nanoparticles:
1.0812g of FeCl were weighed3·6H2Dissolving O and 0.48048g urea in 64mL of deionized water to obtain a transparent and uniform mixed solution, transferring the mixed solution into a high-pressure reaction kettle, then reacting at 120 ℃ for 10 hours, washing the obtained reaction product by alternately centrifuging water and ethanol (6000 rpm multiplied by 3 minutes), and then drying in vacuum for 2 hours to obtain the FeOOH nanorod. Then 0.1g FeOOH is weighed out in Ar/H2(95％Ar+5％H2) And annealing for 10 hours at 350 ℃ in a mixed atmosphere to obtain the Fe nanorod.
(2)L10-preparation of FePt nanomaterial:
0.020g of PtCl was weighed4Placing the mixture in 5.94mL deionized water for ultrasonic dispersion to obtain uniform PtCl4Aqueous solution of the PtCl4PtCl in aqueous solution4The concentration of (A) is 0.01 mol/L; then 1/2 the PtCl mentioned above is taken4The aqueous solution was mixed with 0.009974g of Fe nanorods to obtain a mixed solution (PtCl)4And Fe in a total molar ratio of 1: 3.0); finally, 1/2 of PtCl was left over by using a peristaltic pump4The aqueous solution was dropwise added to PtCl at a dropping rate of 0.1mL/min4Carrying out ultrasonic reaction at normal temperature in the mixed solution of the aqueous solution and the Fe nano-rods, and reacting for 30min to obtain a reaction product; washing the obtained reaction product by alternately centrifuging (6500 r/min. times.3 min) with water and ethanol, and then vacuum drying for 30 min; the reaction product obtained in the above is reacted in Ar/H2Heating to 550 ℃ at the heating rate of about 10 ℃/min for annealing for 2H under the mixed atmosphere of (95% Ar + 5% H2) to obtain L10-FePt nanomaterial.
FIG. 1 shows L1 obtained in this example0-XRD pattern of FePt nanomaterial, from which it can be seen that the material contains only one phase, which is: l10-FePt. FIG. 2 shows L1 obtained in this example0-FePt nanoparticlesThe material has a VSM spectrum, and the coercive force of the material is 12053Oe, and the saturation magnetization of the material is 37.47 emu/g. Fig. 1 and 2 can prove that a single-phase L1 is obtained0-FePt nanoparticles. FIG. 3 shows L1 obtained in the present example0-TEM spectra of FePt nanomaterials.
Example 2
(1) Preparing Fe nanoparticles:
1.0812g of FeCl were weighed3·6H2Dissolving O and 0.48048g urea in 64mL of deionized water to obtain a transparent and uniform mixed solution, transferring the mixed solution into a high-pressure reaction kettle, then reacting at 120 ℃ for 10 hours, washing the obtained reaction product by alternately centrifuging water and ethanol (6000 rpm multiplied by 3 minutes), and then drying in vacuum for 2 hours to obtain the FeOOH nanorod. Then 0.1g FeOOH is weighed out in Ar/H2(95％Ar+5％H2) And annealing for 10 hours at 350 ℃ in a mixed atmosphere to obtain the Fe nanorod.
(2)Fe/L10-preparation of FePt composite nanomaterial:
0.020g of PtCl was weighed4Placing the mixture in 5.94mL deionized water for ultrasonic dispersion to obtain uniform PtCl4Aqueous solution of the PtCl4PtCl in aqueous solution4The concentration of (A) is 0.01 mol/L; then 1/2 the PtCl mentioned above is taken4The aqueous solution was mixed with 0.01097g of Fe nanorods to obtain a mixed solution (PtCl)4And Fe in a total molar ratio of 1: 3.3); finally, 1/2 of PtCl was left over by using a peristaltic pump4The aqueous solution was dropwise added to PtCl at a dropping rate of 0.1mL/min4Carrying out ultrasonic reaction at normal temperature in the mixed solution of the aqueous solution and the Fe nano-rods, and reacting for 30min to obtain a reaction product; washing the obtained reaction product by alternately centrifuging (6500 r/min. times.3 min) with water and ethanol, and then vacuum drying for 30 min; the reaction product obtained in the above is reacted in Ar/H2Heating to 550 ℃ at the heating rate of about 10 ℃/min and annealing for 2H under the mixed atmosphere of (95% Ar + 5% H2) to obtain Fe/L10-FePt composite nanomaterial.
FIG. 4 shows Fe/L1 obtained in this example0-XRD pattern of FePt composite nanomaterial, from which it can be seen that the material contains two phases, respectively: fe and L10-FePt. FIG. 5 shows this embodimentExample obtained Fe/L10The VSM spectrum of the FePt composite nano material shows that the coercive force is 10281Oe, and the saturation magnetization is 46.36 emu/g. FIGS. 4 and 5 prove that Fe/L1 is obtained0-FePt composite nanomaterial with a higher saturation magnetization than the material obtained in example 1. FIG. 6 shows Fe/L1 obtained in example 2 of the present invention0The VSM map of the FePt composite nano material after being placed in air for one week shows that the coercive force is 10189Oe, the saturation magnetization is 44.47emu/g, and the comparison between the FIG. 5 and the FIG. 6 can prove that the Fe/L1 obtained by the embodiment0the-FePt composite nano material has good chemical stability. FIG. 7 shows Fe/L1 obtained in this example0-TEM spectra of FePt composite nanomaterials.
Example 3
(1) Preparing Fe nanoparticles:
1.0812g of FeCl were weighed3·6H2Dissolving O and 0.48048g urea in 64mL of deionized water to obtain a transparent and uniform mixed solution, transferring the mixed solution into a high-pressure reaction kettle, then reacting at 120 ℃ for 10 hours, washing the obtained reaction product by alternately centrifuging water and ethanol (6000 rpm multiplied by 3 minutes), and then drying in vacuum for 2 hours to obtain the FeOOH nanorod. Then 0.1g FeOOH is weighed out in Ar/H2(95％Ar+5％H2) And annealing for 10 hours at 350 ℃ in a mixed atmosphere to obtain the Fe nanorod.
(2)Fe/L10-preparation of FePt composite nanomaterial:
0.020g of PtCl was weighed4Placing the mixture in 5.94mL deionized water for ultrasonic dispersion to obtain uniform PtCl4Aqueous solution of the PtCl4PtCl in aqueous solution4The concentration of (A) is 0.01 mol/L; then 1/2 the PtCl mentioned above is taken4The aqueous solution was mixed with 0.01230g of Fe nanorods to obtain a mixed solution (PtCl)4And Fe in a total molar ratio of 1: 3.7); finally, 1/2 of PtCl was left over by using a peristaltic pump4The aqueous solution was dropwise added to PtCl at a dropping rate of 0.1mL/min4Carrying out ultrasonic reaction at normal temperature in the mixed solution of the aqueous solution and the Fe nano-rods, and reacting for 30min to obtain a reaction product; the obtained reaction product is alternately centrifuged by water and ethanol (6500 r/min)3 minutes) and then dried in vacuum for 30 minutes; the reaction product obtained in the above is reacted in Ar/H2Heating to 550 ℃ at the heating rate of about 10 ℃/min and annealing for 2H under the mixed atmosphere of (95% Ar + 5% H2) to obtain Fe/L10-FePt composite nanomaterial.
FIG. 8 shows Fe/L1 obtained in this example0-XRD pattern of FePt composite nanomaterial, from which it can be seen that the material contains two phases, respectively: fe and L10-FePt. FIG. 9 shows Fe/L1 obtained in this example0The VSM spectrum of the FePt composite nano material shows that the coercive force is 4311.4Oe, and the saturation magnetization is 67.54 emu/g. FIGS. 8 and 9 demonstrate that Fe/L1 with a higher Fe content than in example 2 is obtained0-FePt composite nanomaterial with higher saturation magnetization. FIG. 10 shows Fe/L1 obtained in this example0-TEM spectra of FePt composite nanomaterials.
Example 4
(1) Preparing Fe nanoparticles:
1.0812g of FeCl were weighed3·6H2Dissolving O and 0.48048g urea in 64mL of deionized water to obtain a transparent and uniform mixed solution, transferring the mixed solution into a high-pressure reaction kettle, then reacting at 120 ℃ for 10 hours, washing the obtained reaction product by alternately centrifuging water and ethanol (6000 rpm multiplied by 3 minutes), and then drying in vacuum for 2 hours to obtain the FeOOH nanorod. Then 0.1g FeOOH is weighed out in Ar/H2(95％Ar+5％H2) And annealing for 10 hours at 350 ℃ in a mixed atmosphere to obtain the Fe nanorod.
(2)Fe/L10-preparation of FePt composite nanomaterial:
0.020g of PtCl was weighed4Placing the mixture in 5.94mL deionized water for ultrasonic dispersion to obtain uniform PtCl4Aqueous solution of the PtCl4PtCl in aqueous solution4The concentration of (A) is 0.01 mol/L; then 1/2 the PtCl mentioned above is taken4The aqueous solution was mixed with 0.01097g of Fe nanorods to obtain a mixed solution (PtCl)4And Fe in a total molar ratio of 1: 3.3); finally, 1/2 of PtCl was left over by using a peristaltic pump4The aqueous solution was dropwise added to PtCl at a dropping rate of 0.1mL/min4In the mixed solution of the aqueous solution and the Fe nano-rodCarrying out ultrasonic reaction at normal temperature for 30min to obtain a reaction product; washing the obtained reaction product by alternately centrifuging (6500 r/min. times.3 min) with water and ethanol, and then vacuum drying for 30 min; the reaction product obtained in the above is reacted in Ar/H2Heating to 650 ℃ at the heating rate of about 10 ℃/min and annealing for 2H under the mixed atmosphere of (95% Ar + 5% H2) to obtain Fe/L10-FePt composite nanomaterial.
FIG. 11 shows Fe/L1 obtained in this example0The VSM spectrum of the FePt composite nano material shows that the coercive force of the material is 9427.1Oe, and the saturation magnetization is 40.85 emu/g.
Example 5
(1) Preparing Fe nanoparticles:
1.0812g of FeCl were weighed3·6H2Dissolving O and 0.48048g urea in 64mL of deionized water to obtain a transparent and uniform mixed solution, transferring the mixed solution into a high-pressure reaction kettle, then reacting at 120 ℃ for 10 hours, washing the obtained reaction product by alternately centrifuging water and ethanol (6000 rpm multiplied by 3 minutes), and then drying in vacuum for 2 hours to obtain the FeOOH nanorod. Then 0.1g FeOOH is weighed out in Ar/H2(95％Ar+5％H2) And annealing for 10 hours at 350 ℃ in a mixed atmosphere to obtain the Fe nanorod.
(2)Fe/L10-preparation of FePt composite nanomaterial:
0.020g of PtCl was weighed4Placing the mixture in 5.94mL deionized water for ultrasonic dispersion to obtain uniform PtCl4Aqueous solution of the PtCl4PtCl in aqueous solution4The concentration of (A) is 0.01 mol/L; then 1/2 the PtCl mentioned above is taken4The aqueous solution was mixed with 0.01097g of Fe nanorods to obtain a mixed solution (PtCl)4And Fe in a total molar ratio of 1: 3.3); finally, 1/2 of PtCl was left over by using a peristaltic pump4The aqueous solution was dropwise added to PtCl at a dropping rate of 0.1mL/min4Carrying out ultrasonic reaction at normal temperature in the mixed solution of the aqueous solution and the Fe nano-rods, and reacting for 30min to obtain a reaction product; washing the obtained reaction product by alternately centrifuging (6500 r/min. times.3 min) with water and ethanol, and then vacuum drying for 30 min; the reaction product obtained in the above is reacted in Ar/H2(95% Ar + 5% H2) at a temperature of about 1 deg.CHeating to 750 ℃ at the heating rate of 0 ℃/min and annealing for 2h to obtain Fe/L10-FePt composite nanomaterial.
FIG. 12 shows Fe/L1 obtained in this example0The VSM spectrum of the FePt composite nano material shows that the coercive force of the material is 9200.3Oe, and the saturation magnetization is 39.87 emu/g. A comparison of FIGS. 5, 11 and 12 demonstrates that Fe/L1 increases with annealing temperature0The magnetic property of the-FePt composite nano material is slightly reduced.
Furthermore, the inventors have conducted experiments under other process conditions described in the present specification by referring to examples 2 to 5, and have found that Fe/L1 is obtained0the-FePt composite nano material has excellent magnetic performance and the like.
In conclusion, the Fe/L1 obtained by the technical scheme of the invention0Fe in the FePt composite nano material is not easy to be oxidized in the interior, so that the composite nano material has good chemical stability. The preparation method is a water-based synthesis method, the used reagent is a common non-toxic water-based reagent, no organic matter participates, no toxic by-product is generated in the reaction process, the synthesis steps are simple and easy to implement, and the method is green and environment-friendly.
It should be understood that the above describes only some embodiments of the present invention and that various other changes and modifications may be affected therein by one of ordinary skill in the related art without departing from the scope or spirit of the invention.
Claims (22)
1. Fe/L10-a method for preparing a FePt composite nanomaterial, characterized by comprising:
mixing Fe nanoparticles with PtCl4Uniformly mixing the aqueous solution to form a mixed solution;
further dropping a part of PtCl into the mixed solution4Water solution, and ultrasonic reaction is carried out at normal temperature to obtain a reaction product;
annealing the reaction product in a reducing atmosphere at 500-750 ℃ to obtain Fe/L10-FePt composite nanomaterial.
2. The method of manufacturing according to claim 1, comprising:
providing PtCl4An aqueous solution;
reacting part of PtCl4Uniformly mixing the water solution and the Fe nano particles to form a mixed solution;
the residual PtCl is removed4And dripping the aqueous solution into the mixed solution, and carrying out ultrasonic reaction at normal temperature to obtain the reaction product.
3. The method of manufacturing according to claim 2, comprising: dropping the residual PtCl at a dropping rate of 0.1-0.4 ml/min4The aqueous solution was slowly dropped into the mixed solution.
4. The production method according to claim 3, characterized in that: the dropping rate is 0.1-0.15 ml/min.
5. The method of manufacturing according to claim 2, comprising: the residual PtCl is removed4And (3) dripping the aqueous solution into the mixed solution, and carrying out ultrasonic reaction for 15-45 min at normal temperature to obtain the reaction product.
6. The method of manufacturing according to claim 5, comprising: the residual PtCl is removed4And (3) dripping the aqueous solution into the mixed solution, and carrying out ultrasonic reaction for 30-45 min at normal temperature to obtain the reaction product.
7. The method of claim 1, further comprising: and washing and drying the obtained reaction product, and then carrying out the annealing treatment in the reducing atmosphere.
8. The method of claim 1, wherein: the PtCl4Of aqueous solutionsThe concentration is 0.005-0.02 mol/L.
9. The method of claim 8, wherein: the PtCl4The concentration of the aqueous solution is 0.005-0.015 mol/L.
10. The method of claim 1, wherein: PtCl in the mixed solution4The molar ratio to Fe is 1: 2.91-1: 4.49.
11. the method of manufacturing according to claim 10, wherein: PtCl in the mixed solution4The molar ratio to Fe is 1: 3-1: 4.
12. the method of claim 11, wherein: PtCl in the mixed solution4The molar ratio to Fe is 1: 3.1.
13. the method of claim 1, wherein:
the Fe nano-particles comprise Fe nano-particles, and the particle size of the Fe nano-particles is 30-500 nm;
the preparation method of the Fe nano-particles comprises the following steps: and carrying out reduction annealing on the FeOOH nano particles for 2-10 h at 350-550 ℃ in a reducing atmosphere to obtain Fe nano particles.
14. The production method according to claim 1, characterized by comprising: and placing the reaction product in a reducing atmosphere, heating to the annealing temperature at a heating rate of 5-10 ℃/min, and preserving heat for 30-240 min, thereby finishing the annealing treatment.
15. The method of claim 14, wherein: the annealing temperature is 550-750 ℃.
16. The method of claim 15, wherein: the annealing temperature is 550-650 ℃.
17. The method of claim 14, wherein: the annealing time is 30-120 min.
18. The production method according to claim 1, characterized by comprising: and placing the reaction product in a reaction chamber, removing air in the reaction chamber, introducing a reducing gas to form the reducing atmosphere, and then carrying out annealing treatment.
19. The method of claim 18, wherein: the flow rate of the reducing gas is 200-400 ml/min.
20. The production method according to any one of claims 1 to 19, characterized in that: the reducing atmosphere is formed by a reducing gas including a mixed gas of hydrogen and an inert gas.
21. The method of claim 20, wherein: the reducing gas comprises 0-95 v/v% argon and 5-100 v/v% hydrogen.
22. Fe/L1 prepared by the method of any one of claims 1-210-FePt composite nanomaterial.
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