CN111243817A - Amorphous nano-particle liquid metal magnetic fluid and preparation method thereof - Google Patents

Amorphous nano-particle liquid metal magnetic fluid and preparation method thereof Download PDF

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CN111243817A
CN111243817A CN202010096981.XA CN202010096981A CN111243817A CN 111243817 A CN111243817 A CN 111243817A CN 202010096981 A CN202010096981 A CN 202010096981A CN 111243817 A CN111243817 A CN 111243817A
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liquid
liquid metal
amorphous
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nanoparticles
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杨春成
刘忠
赵素彦
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Hebei GEO University
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Hebei GEO University
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/44—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of magnetic liquids, e.g. ferrofluids
    • H01F1/442—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of magnetic liquids, e.g. ferrofluids the magnetic component being a metal or alloy, e.g. Fe
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y25/00—Nanomagnetism, e.g. magnetoimpedance, anisotropic magnetoresistance, giant magnetoresistance or tunneling magnetoresistance
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties

Abstract

The invention provides an amorphous nano-particle liquid metal magnetic fluid and a preparation method thereof2O3The amorphous nano particles are used as magnetic particles, and the stable, nontoxic and nonvolatile amorphous nano particle liquid metal magnetic fluid is prepared in the liquid metal carrier liquid.

Description

Amorphous nano-particle liquid metal magnetic fluid and preparation method thereof
Technical Field
The invention relates to the field of functional materials, in particular to an amorphous nanoparticle liquid metal magnetic fluid and a preparation method thereof.
Background
Magnetic fluid is a novel functional material, and has attracted extensive attention and attention due to the liquidity of liquid and the magnetism of solid. The carrier liquid is an important component of the magnetic fluid, and when the magnetic fluid is selected, the type of the carrier liquid needs to be selected according to different purposes of the magnetic fluid. The carrier liquid of the magnetic fluid reported at home and abroad at present mainly comprises organic matters and water. However, these organic magnetic fluids such as polyphenylene ethers, toluene or n-hexane are generally very volatile and have a certain toxicity, and are not suitable for applications in the fields of biomedicine and the like; the magnetic fluid prepared by using water as carrier liquid is not suitable for engineering application fields with higher ambient temperature, such as high-temperature sealing, high-temperature cooling and the like, because the boiling point of water is lower and higher than 100 ℃, the water can boil.
Conventional magnetic fluids have limited further research and application due to limitations in the nature of the carrier fluid. Therefore, metals existing in liquid state at normal temperature and pressure are good choices for magnetic fluid carrier liquid due to their characteristics of low melting point, high boiling point, low vapor pressure, etc. However, the liquid metal magnetic fluid obtained with liquid metal has insufficient stability.
Disclosure of Invention
Therefore, in order to overcome the defects of the prior art, the invention provides an amorphous nanoparticle liquid metal magnetic fluid and a preparation method thereof, wherein a GaSn liquid metal eutectic alloy is used as a carrier liquid of the magnetic fluid, and Fe-Co-B @ Al is used as the carrier liquid2O3The amorphous nano particles are used as magnetic particles, and the stable, nontoxic and nonvolatile amorphous nano particle liquid metal magnetic fluid is prepared in the liquid metal carrier liquid.
The invention provides a preparation method of amorphous nanoparticle liquid metal magnetic fluid, which is characterized by comprising the following steps: preparing Fe-Co-B amorphous nanoparticles; preparing Fe-Co-B @ Al by using the Fe-Co-B amorphous nano particles and an Al salt solution2O3A nanoparticle; preparing a liquid metal carrier liquid; to the addition of said Fe-Co-B @ Al2O3Mixing and dispersing the liquid metal carrier liquid of the magnetic particles to obtain a metal mixed liquid to be treated; annealing the metal mixed solution to be processed in a muffle furnace at 350-600 ℃ to obtain the stable amorphous nano-particle liquid metal magnetic fluid, wherein the preparation of the liquid metal carrier liquid comprises the following steps: and smelting pure metal Ga and pure metal Sn according to a first mass ratio to prepare the GaSn eutectic liquid alloy carrier liquid.
In one embodiment, the preparing the Fe-Co-B amorphous nanoparticles comprises: and preparing the Fe-Co-B amorphous nano particles by adopting a chemical reduction method or a chemical coprecipitation method.
In one embodiment, the preparation of the Fe-Co-B amorphous nanoparticles by a chemical reduction method comprises: using FeCl2·4H2O and CoCl2·6H2Preparing a mixed solution from O, wherein Fe is contained in the mixed solution2+And Co2+The molar ratio of (A) to (B) is 2-3: 1-2; adding a first predetermined volume of NaBH to the mixed solution with stirring4Solution, adding NaBH regulated by NaOH4The pH value of the mixed solution after the solution is 10-12; mechanically stirring and ultrasonically dispersing the mixed solution after the pH is adjusted within first treatment time to obtain suspension, wherein the first treatment time is not less than 0.5 hour; and (4) carrying out high-speed centrifugation on the suspension to obtain the Fe-Co-B amorphous nano-particles.
In one embodiment, a first predetermined volume of NaBH is added to the mixed solution with agitation4A solution comprising: under the conditions of mechanical stirring and ultrasonic dispersion, adding NaBH with a first preset volume into the mixed solution at a constant speed4And (3) solution.
In one embodiment, the Fe-Co-B @ Al solution and the Fe-Co-B amorphous nanoparticles are used to prepare Fe-Co-B @ Al2O3A nanoparticle comprising: taking a first predetermined mass of Fe-Co-B nano particles, adding Al (NO)3)3Obtaining a suspension in the solution; adding PEG-2000 and PEG-400 serving as dispersing agents into the suspension, and uniformly stirring by magnetic force to obtain suspension; slowly adding ammonia water into the suspension, adjusting the pH value of the suspension to 9, and mechanically stirring for a second treatment time, wherein the second treatment time is not less than 4 hours; filtering the stirred suspension, washing the precipitate with distilled water, drying and grinding the precipitate to obtain Al (OH)3Coated Fe-Co-B nanoparticles; mixing the Al (OH)3Coated Fe-Co-B nanoparticles with MgSO4Mixing the solution, and performing ultrasonic dispersion, wherein the atomic percentages of Mg and Al in the dispersion are Mg: 20 of Al: 1; heating and continuously stirring the dispersion to obtain a powder mixture, and heating the powder mixture at 180 ℃ to obtain Al (OH)3Conversion to Al2O3(ii) a Cleaning mixtureRemoving MgSO from the compound4Powder is dried to obtain Fe-Co-B @ Al2O3And (3) nanoparticles.
In one embodiment, said heating and continuously stirring said dispersion to provide a powder mixture, said powder mixture is heated at 180 ℃ to al (oh)3Conversion to Al2O3The method comprises the following steps: heating at 60-90 deg.C under stirring to evaporate water solvent completely, heating the obtained mixture at 180 deg.C for 2 hr to remove Al (OH)3Conversion to Al2O3。
In one embodiment, the pair adds the Fe-Co-B @ Al2O3And mixing and dispersing the liquid metal carrier liquid of the magnetic particles to obtain a metal mixed liquid to be treated: adding the Fe-Co-B @ Al by adopting mechanical stirring and/or ultrasonic dispersion2O3The liquid metal carrier liquid of the magnetic particles is mixed and dispersed.
In one embodiment, the pair adds the Fe-Co-B @ Al2O3And mixing and dispersing the liquid metal carrier liquid of the magnetic particles to obtain a metal mixed liquid to be treated: stirring the liquid metal carrier liquid by a mechanical stirring device, simultaneously dispersing and combining by ultrasonic dispersion, and adding a second predetermined mass of Fe-Co-B @ Al into the liquid metal carrier liquid2O3And (3) mixing and dispersing the nanoparticles at the temperature of 35-50 ℃ for a third treatment time, wherein the third treatment time is not less than 1 hour.
In one embodiment, the annealing treatment of the mixed solution of metals to be treated in a muffle furnace at 400-550 ℃ comprises: and annealing the metal mixed solution to be treated in a muffle furnace at 450-550 ℃, wherein the annealing time is 120 min.
The invention also provides an amorphous nanoparticle liquid metal magnetic fluid, which is characterized in that: the amorphous nanoparticle liquid metal magnetic fluid is prepared by any one of the methods.
Compared with the prior art, the invention has the advantages that: using a gallium-tin eutectic alloy which is liquid at room temperatureFor the carrier liquid of the magnetic fluid, Al2O3The coated Fe-Co-B amorphous nano particles are used as magnetic particles and dispersed in the liquid metal eutectic alloy, so that the prepared amorphous nano particles liquid metal magnetic fluid has good stability, good fluidity and excellent magnetic performance. And the amorphous nano-particle liquid metal magnetic fluid has no toxicity, is not easy to volatilize, can resist high and low temperatures, has high thermal conductivity and electric conductivity of metal, and solves the problems of the traditional magnetic fluid.
Drawings
FIG. 1 is an XRD spectrum of Fe-Co-B amorphous magnetic nanoparticles prepared by the first embodiment of the present invention;
FIG. 2 is a DSC curve of Fe-Co-B amorphous magnetic nanoparticles prepared according to the first embodiment of the present invention;
FIG. 3 is a transmission electron microscope image of Fe-Co-B amorphous magnetic nanoparticles prepared according to the first embodiment of the present invention;
FIG. 4 shows Fe-Co-B @ Al prepared in the first embodiment of the present invention2O3Scanning electron micrographs of magnetic nanoparticles;
FIG. 5 shows a Fe-Co-B @ Al-based alloy prepared in accordance with example one of the present invention2O3Ga of magnetic nanoparticles91.6Sn8.4A hysteresis loop of the liquid metal eutectic alloy magnetic fluid;
FIG. 6 shows a Fe-Co-B @ Al-based alloy prepared in accordance with example one of the present invention2O3Ga of magnetic nanoparticles91.6Sn8.4Stability curve of liquid metal eutectic alloy magnetic fluid.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to specific embodiments and the accompanying drawings.
< example one >
The method comprises the following steps: preparation of Fe-Co-B amorphous nanoparticles
The Fe-Co-B amorphous nano-particles can be prepared by a chemical reduction method or a chemical coprecipitation method. In this example, the chemical reduction method was used to prepare Fe-Co-B amorphous nanoparticlesAnd (4) granulating. Configuring FeCl2·4H2O and CoCl2·6H2100ml of mixed solution of O, wherein Fe is contained in the mixed solution2+And Co2+In a molar ratio of 2: 1. Adding a first predetermined volume of NaBH to the mixed solution with stirring4And (3) solution. Under the conditions of mechanical stirring and ultrasonic dispersion, NaBH with a first preset volume can be added into the mixed solution at a constant speed4And (3) solution. First predetermined capacity according to Fe2+And Co2+Is determined. The mixed solution was placed in a three-necked flask for mechanical stirring and ultrasonic dispersion, and then 30 ml of 0.8 mol NaBH was added at room temperature at a rate of 1.5ml per minute4And (3) solution. NaBH is added with NaOH regulation4And (3) the pH value of the mixed solution after the solution is 10-12. In this example, the pH of the solution was adjusted to 10 using NaOH. And (3) carrying out mechanical stirring and ultrasonic dispersion treatment on the mixed solution after the pH is adjusted within first treatment time to obtain suspension, wherein the first treatment time is not less than 0.5 hour. In this example, the magnetic particles were dispersed for 1 hour by mechanical stirring and ultrasonic dispersion, and then the suspension was centrifuged at high speed to obtain amorphous Fe-Co-B magnetic particles.
Step two: preparation of Fe-Co-B @ Al by using Fe-Co-B amorphous nanoparticles and Al salt solution2O3Nanoparticles
4g of Fe-Co-B nanoparticles were weighed out and added to 75ml of Al (NO)3)3Obtaining a suspension in solution, Al (NO)3)3The concentration of the solution was 0.5 mol/L. 0.4g PEG-2000 and 1.5g PEG-400 were added to the suspension as dispersing agents and stirred magnetically. Wherein the mass (g) of Fe-Co-B nanoparticles and Al (NO)3)3The ratio between the volumes (ml) of the solutions was 1: 18.75; the proportion of the dispersing agent PEG-2000 to PEG-400 to the Fe-Co-B nano particles is 1: 3.75: 10. slowly dropping 25% NH3·H2And O solution, adjusting the pH value of the suspension to 9, and mechanically stirring for a second treatment time, wherein the second treatment time is not less than 4 hours. Stirring mechanically for 5h, filtering, washing precipitate with distilled water, drying and grinding precipitate to obtain Al (OH)3Coated Fe-Co-B nanoparticles. The obtained Al (OH)3Coated Fe-Co-BNanoparticles with MgSO4And ultrasonically dispersing the solution, wherein the atomic percentages of Mg and Al in the suspension are Mg: 20 of Al: 1. heating at 60-90 deg.C under stirring to evaporate water solvent completely, and heating the obtained mixture at 180 deg.C for 2 hr to remove Al (OH)3Conversion to Al2O3. Specifically, heating at 60 deg.C under stirring for 1.5 hr to evaporate water solvent completely, heating the obtained mixture at 180 deg.C for 2 hr to remove Al (OH)3Conversion to Al2O3Washing the mixture several times to remove MgSO4Powdering and drying to obtain Al2O3Coated Fe-Co-B nanoparticles.
Step three: preparation of liquid Metal Carrier liquid
And smelting pure metal Ga and pure metal Sn according to a first mass ratio to prepare the GaSn eutectic liquid alloy carrier liquid. Specifically, 99.999% pure gallium and tin are used, and the ratio of Ga to Sn in atomic mass is 91.6: 8.4, proportioning, smelting by using a high-frequency induction furnace to obtain Ga of gallium-tin91.6Sn8.4Eutectic alloys, such alloys being in a liquid state at room temperature. Then, 25ml of liquid metal was taken into the crucible for the subsequent operation.
Step four: for adding Fe-Co-B @ Al2O3Mixing and dispersing liquid metal carrier liquid of magnetic particles to obtain metal mixed liquid to be treated
Adding Fe-Co-B @ Al2O3Magnetic particles are added into a crucible which is filled with liquid metal, and Fe-Co-B @ Al is added by mechanical stirring and/or ultrasonic dispersion2O3The liquid metal carrier liquid of the magnetic particles is mixed and dispersed. Specifically, a micro-mechanical stirring device is used for stirring the liquid metal eutectic alloy in the crucible, ultrasonic dispersion is used for dispersion combination, and a certain mass of Fe-Co-B @ Al is added into the liquid metal eutectic alloy2O3And (3) controlling the temperature of the nano particles at 35 ℃, mechanically stirring and ultrasonically treating for 1 hour, and then cooling and standing.
Step five: preparation of amorphous nanoparticle liquid metal magnetic fluid
And annealing the metal mixed solution to be treated in a muffle furnace at 350-600 ℃ to obtain the stable amorphous nano-particle liquid metal magnetic fluid. And putting the crucible into a muffle furnace for annealing treatment, wherein the annealing treatment temperature is 400 ℃, and the annealing time is 120 min. After annealing treatment, stable amorphous nanoparticle liquid metal magnetic fluid can be obtained.
FIG. 1 is an XRD spectrum of Fe-Co-B amorphous magnetic nanoparticles prepared by the first embodiment of the present invention; FIG. 2 is a DSC curve of Fe-Co-B amorphous magnetic nanoparticles prepared according to the first embodiment of the present invention; FIG. 3 is a transmission electron microscope image of Fe-Co-B amorphous magnetic nanoparticles prepared according to the first embodiment of the present invention; FIG. 4 shows Fe-Co-B @ Al prepared in the first embodiment of the present invention2O3Scanning electron micrographs of magnetic nanoparticles; FIG. 5 shows a Fe-Co-B @ Al-based alloy prepared in accordance with example one of the present invention2O3Ga of magnetic nanoparticles91.6Sn8.4A hysteresis loop of the liquid metal eutectic alloy magnetic fluid; FIG. 6 shows a Fe-Co-B @ Al-based alloy prepared in accordance with example one of the present invention2O3Ga of magnetic nanoparticles91.6Sn8.4Stability curve of liquid metal eutectic alloy magnetic fluid.
The XRD map of the Fe-Co-B magnetic nano particles can show that the XRD map has obvious amorphous diffraction peaks and shows amorphous characteristics; from the DSC curve, the Fe-Co-B magnetic nano-particles have two exothermic peaks, which represent the exothermic heat in the crystallization process and are consistent with the structure of the XRD pattern; the transmission electron microscope picture shows that the size of the Fe-Co-B amorphous magnetic particles is in the nanometer level, and is about 13 nm.
The scanning electron microscope picture shows that Fe-Co-B @ Al2O3The size of the magnetic nano particles is nano-scale and slightly larger than that of the Fe-Co-B particles; from the hysteresis loop, Fe-Co-B @ Al can be seen2O3The magnetic nanoparticles exhibit superparamagnetism; from the stability curve, it can be seen that Fe-Co-B @ Al2O3The magnetic nanoparticles have good stability.
< example two >
The method comprises the following steps: preparation of Fe-Co-B amorphous nanoparticles
Configuring FeCl2·4H2O and CoCl2·6H2100ml of mixed solution of O, wherein Fe2+And Co2+Is 3: 1. The mixed solution was placed in a three-necked flask for mechanical stirring and ultrasonic dispersion, and then 30 ml of 0.8 mol NaBH was added at room temperature at a rate of 1.5ml per minute4And (3) solution. The pH of the solution was adjusted to 11 using NaOH. Mechanically stirring and ultrasonically dispersing for 1 hour, and then centrifuging the suspension at high speed to obtain the amorphous Fe-Co-B magnetic particles.
Step two: preparation of Fe-Co-B @ Al by using Fe-Co-B amorphous nanoparticles and Al salt solution2O3Nanoparticles
4g of Fe-Co-B nanoparticles were weighed out and added to 75ml of Al (NO)3)3Obtaining a suspension in solution, Al (NO)3)3The concentration of the solution was 0.5 mol/L. 0.4g PEG-2000 and 1.5g PEG-400 were added to the suspension as dispersing agents and stirred magnetically. Slowly dropping 25% NH3·H2O solution, adjusting the pH value of the suspension to 9, mechanically stirring for 5h, filtering, washing with distilled water, drying and grinding to obtain Al (OH)3Coated Fe-Co-B nanoparticles. The obtained Al (OH)3Coated Fe-Co-B nanoparticles with MgSO4And ultrasonically dispersing the solution, wherein the atomic percent of Mg and Al in the suspension is Mg/Al of 20. Heating at 70 deg.C under stirring for 1.5 hr to evaporate water solvent completely, and heating the obtained mixture at 180 deg.C for 2 hr to remove Al (OH)3Conversion to Al2O3Washing the mixture several times to remove MgSO4Powdering and drying to obtain Al2O3Coated Fe-Co-B nanoparticles.
Step three: preparation of liquid Metal Carrier liquid
Using 99.999% pure gallium and tin according to the Ga: Sn atomic mass ratio of 91.6: 8.4, proportioning, smelting by using a high-frequency induction furnace to obtain Ga of gallium-tin91.6Sn8.4Eutectic alloys, such alloys being in a liquid state at room temperature. 25ml of liquid metal was taken and placed in the crucible.
Step four: for adding Fe-Co-B @ Al2O3Mixing and dispersing liquid metal carrier liquid of magnetic particles to obtain metal mixed liquid to be treated
Stirring liquid metal eutectic alloy in a crucible by a micro mechanical stirring device, simultaneously dispersing and combining by ultrasonic dispersion, and adding a certain mass of Fe-Co-B @ Al into the liquid metal eutectic alloy2O3Controlling the temperature of the nano particles at 45 ℃, mechanically stirring and ultrasonically treating for 1 hour, and then cooling and standing.
Step five: preparation of amorphous nanoparticle liquid metal magnetic fluid
And (3) putting the crucible into a muffle furnace for annealing treatment, wherein the annealing treatment temperature is 450 ℃, and the annealing time is 120 min. After annealing treatment, stable amorphous particle liquid metal magnetic fluid can be obtained.
< example three >
The method comprises the following steps: preparation of Fe-Co-B amorphous nanoparticles
Configuring FeCl2·4H2O and CoCl2·6H2100ml of mixed solution of O, wherein Fe2+And Co2+Is 3: 2. The mixed solution was placed in a three-necked flask for mechanical stirring and ultrasonic dispersion, and then 35 ml of 0.8 mol NaBH was added at room temperature at a rate of 1.5ml per minute4And (3) solution. The pH of the solution was adjusted to 12 using NaOH. Mechanically stirring and ultrasonically dispersing for 1 hour, and then centrifuging the suspension at high speed to obtain the amorphous Fe-Co-B magnetic particles.
Step two: preparation of Fe-Co-B @ Al by using Fe-Co-B amorphous nanoparticles and Al salt solution2O3Nanoparticles
4g of Fe-Co-B nanoparticles were weighed out and added to 75ml of Al (NO)3)3Obtaining a suspension in solution, Al (NO)3)3The concentration of the solution was 0.5 mol/L. 0.4g PEG-2000 and 1.5g PEG-400 were added to the suspension as dispersing agents and stirred magnetically. Slowly dropping 25% NH3·H2O solution, adjusting the pH value of the suspension to 9, mechanically stirring for 5h, filtering, washing with distilled water, drying and grinding to obtain Al (OH)3Coated Fe-Co-B nanoparticles. The obtained Al (OH)3Coated Fe-Co-B nanoparticles with MgSO4Ultrasonic dispersing the solution, wherein atoms of Mg and Al in the suspensionThe percentage is Mg/Al 20. Heating at 80 deg.C under stirring for 1.5 hr to evaporate water solvent completely, and heating the obtained mixture at 180 deg.C for 2 hr to remove Al (OH)3Conversion to Al2O3Washing the mixture several times to remove MgSO4Powdering and drying to obtain Al2O3Coated Fe-Co-B nanoparticles.
Step three: preparation of liquid Metal Carrier liquid
Using 99.999% pure gallium and tin according to the Ga: Sn atomic mass ratio of 91.6: 8.4, proportioning, smelting by using a high-frequency induction furnace to obtain Ga of gallium-tin91.6Sn8.4Eutectic alloys, such alloys being in a liquid state at room temperature. 25ml of liquid metal was taken and placed in the crucible.
Step four: for adding Fe-Co-B @ Al2O3Mixing and dispersing liquid metal carrier liquid of magnetic particles to obtain metal mixed liquid to be treated
Stirring liquid metal eutectic alloy in a crucible by a micro mechanical stirring device, simultaneously dispersing and combining by ultrasonic dispersion, and adding a certain mass of Fe-Co-B @ Al into the liquid metal eutectic alloy2O3Controlling the temperature of the nano particles at 50 ℃, mechanically stirring and ultrasonically treating for 1 hour, and then cooling and standing.
Step five: preparation of amorphous nanoparticle liquid metal magnetic fluid
And (3) putting the crucible into a muffle furnace for annealing treatment, wherein the annealing treatment temperature is 550 ℃, and the annealing time is 120 min. After annealing treatment, stable amorphous particle liquid metal magnetic fluid can be obtained.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention. The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.

Claims (10)

1. A preparation method of amorphous nanoparticle liquid metal magnetic fluid is characterized by comprising the following steps:
preparing Fe-Co-B amorphous nanoparticles;
preparing Fe-Co-B @ Al by using the Fe-Co-B amorphous nano particles and an Al salt solution2O3A nanoparticle;
preparing a liquid metal carrier liquid;
to the addition of said Fe-Co-B @ Al2O3Mixing and dispersing the liquid metal carrier liquid of the magnetic particles to obtain a metal mixed liquid to be treated;
annealing the metal mixed solution to be treated in a muffle furnace at 400-550 ℃ to obtain stable amorphous nano-particle liquid metal magnetic fluid,
wherein the preparing a liquid metal carrier liquid comprises: and smelting pure metal Ga and pure metal Sn according to a first mass ratio to prepare the GaSn eutectic liquid alloy carrier liquid.
2. The method of claim 1, wherein the step of preparing Fe-Co-B amorphous nanoparticles comprises:
and preparing the Fe-Co-B amorphous nano particles by adopting a chemical reduction method or a chemical coprecipitation method.
3. The method of claim 2, wherein the step of preparing Fe-Co-B amorphous nanoparticles by chemical reduction comprises:
using FeCl2·4H2O and CoCl2·6H2Preparing a mixed solution from O, wherein Fe is contained in the mixed solution2+And Co2+The molar ratio of (A) to (B) is 2-3: 1-2;
adding a first predetermined volume of NaBH to the mixed solution with stirring4Solution, adding NaBH regulated by NaOH4The pH value of the mixed solution after the solution is 10-12;
mechanically stirring and ultrasonically dispersing the mixed solution after the pH is adjusted within first treatment time to obtain suspension, wherein the first treatment time is not less than 0.5 hour;
and (4) carrying out high-speed centrifugation on the suspension to obtain the Fe-Co-B amorphous nano-particles.
4. The method of claim 3, wherein the NaBH of a first predetermined volume is added to the mixed solution under stirring4A solution comprising:
under the conditions of mechanical stirring and ultrasonic dispersion, adding NaBH with a first preset volume into the mixed solution at a constant speed4And (3) solution.
5. The method of claim 1, wherein the Fe-Co-B amorphous nanoparticle and Al salt solution are used to prepare Fe-Co-B @ Al2O3A nanoparticle comprising:
taking a first predetermined mass of Fe-Co-B nano particles, adding Al (NO)3)3Obtaining a suspension in the solution;
adding PEG-2000 and PEG-400 serving as dispersing agents into the suspension, and uniformly stirring by magnetic force to obtain suspension;
slowly adding ammonia water into the suspension, adjusting the pH value of the suspension to 9, and mechanically stirring for a second treatment time, wherein the second treatment time is not less than 4 hours;
filtering the stirred suspension, washing the precipitate with distilled water, drying and grinding the precipitate to obtain Al (OH)3Coated Fe-Co-B nanoparticles;
mixing the Al (OH)3Coated Fe-Co-B nanoparticles with MgSO4Mixing the solution, and performing ultrasonic dispersion, wherein the atomic percentages of Mg and Al in the dispersion are Mg: 20 of Al: 1;
heating and continuously stirring the dispersion to obtain a powder mixture, and mixing the powder mixtureHeating at 180 deg.C to cause Al (OH)3Conversion to Al2O3；
Washing the mixture to remove MgSO4Powder is dried to obtain Fe-Co-B @ Al2O3And (3) nanoparticles.
6. The method of claim 5, wherein the dispersion is heated and continuously stirred to obtain a powder mixture, and the powder mixture is heated at 180 ℃ to cause Al (OH) to form3Conversion to Al2O3The method comprises the following steps:
heating at 60-90 deg.C under stirring to evaporate water solvent completely, heating the obtained mixture at 180 deg.C for 2 hr to remove Al (OH)3Conversion to Al2O3。
7. The method of claim 1, wherein the Fe-Co-B @ Al is added to the pair2O3And mixing and dispersing the liquid metal carrier liquid of the magnetic particles to obtain a metal mixed liquid to be treated:
adding the Fe-Co-B @ Al by adopting mechanical stirring and/or ultrasonic dispersion2O3The liquid metal carrier liquid of the magnetic particles is mixed and dispersed.
8. The method of claim 7, wherein the pair of additions of Fe-Co-B @ Al is provided as a solution to the amorphous nanoparticle liquid metal magnetic fluid2O3And mixing and dispersing the liquid metal carrier liquid of the magnetic particles to obtain a metal mixed liquid to be treated:
stirring the liquid metal carrier liquid by a mechanical stirring device, simultaneously dispersing and combining by ultrasonic dispersion, and adding a second predetermined mass of Fe-Co-B @ Al into the liquid metal carrier liquid2O3And (3) mixing and dispersing the nanoparticles at the temperature of 35-50 ℃ for a third treatment time, wherein the third treatment time is not less than 1 hour.
9. The method for preparing amorphous nanoparticle liquid metal magnetic fluid according to claim 1, wherein the annealing the mixed solution of the metals to be treated in a muffle furnace at 400-550 ℃ comprises:
and annealing the metal mixed solution to be treated in a muffle furnace at 450-550 ℃, wherein the annealing time is 120 min.
10. An amorphous nanoparticle liquid metal magnetic fluid, characterized by:
the amorphous nanoparticle liquid metal magnetic fluid is prepared by the method of any one of claims 1 to 9.
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