CN113077954B - Hard magnetic liquid metal paste composite material and preparation method thereof - Google Patents
Hard magnetic liquid metal paste composite material and preparation method thereof Download PDFInfo
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- CN113077954B CN113077954B CN202110320209.6A CN202110320209A CN113077954B CN 113077954 B CN113077954 B CN 113077954B CN 202110320209 A CN202110320209 A CN 202110320209A CN 113077954 B CN113077954 B CN 113077954B
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- 229910001338 liquidmetal Inorganic materials 0.000 title claims abstract description 112
- 239000002131 composite material Substances 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000003756 stirring Methods 0.000 claims abstract description 33
- 239000002122 magnetic nanoparticle Substances 0.000 claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- 239000011261 inert gas Substances 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 9
- 230000005415 magnetization Effects 0.000 claims abstract description 5
- 239000011159 matrix material Substances 0.000 claims abstract description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims description 10
- 229910000846 In alloy Inorganic materials 0.000 claims description 10
- 229910052733 gallium Inorganic materials 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- OBACEDMBGYVZMP-UHFFFAOYSA-N iron platinum Chemical compound [Fe].[Fe].[Pt] OBACEDMBGYVZMP-UHFFFAOYSA-N 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 238000003760 magnetic stirring Methods 0.000 claims description 4
- 238000010907 mechanical stirring Methods 0.000 claims description 4
- 239000002086 nanomaterial Substances 0.000 claims description 4
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical group [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 claims description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- GUBSQCSIIDQXLB-UHFFFAOYSA-N cobalt platinum Chemical compound [Co].[Pt].[Pt].[Pt] GUBSQCSIIDQXLB-UHFFFAOYSA-N 0.000 claims description 2
- 239000001307 helium Substances 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
- 229910052738 indium Inorganic materials 0.000 claims description 2
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims description 2
- SORXVYYPMXPIFD-UHFFFAOYSA-N iron palladium Chemical compound [Fe].[Pd] SORXVYYPMXPIFD-UHFFFAOYSA-N 0.000 claims description 2
- 229910052718 tin Inorganic materials 0.000 claims description 2
- 239000000126 substance Substances 0.000 abstract description 9
- 229910005335 FePt Inorganic materials 0.000 description 31
- 239000002105 nanoparticle Substances 0.000 description 18
- 239000006249 magnetic particle Substances 0.000 description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- 239000000696 magnetic material Substances 0.000 description 6
- 239000000243 solution Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 239000012298 atmosphere Substances 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 230000004043 responsiveness Effects 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000008151 electrolyte solution Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 230000005389 magnetism Effects 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 229910001172 neodymium magnet Inorganic materials 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 229910018979 CoPt Inorganic materials 0.000 description 1
- 229910015187 FePd Inorganic materials 0.000 description 1
- 229910052688 Gadolinium Inorganic materials 0.000 description 1
- 229910001260 Pt alloy Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- AJNVQOSZGJRYEI-UHFFFAOYSA-N digallium;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ga+3].[Ga+3] AJNVQOSZGJRYEI-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910001195 gallium oxide Inorganic materials 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 239000011859 microparticle Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
Classifications
-
- 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
- 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
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/108—Mixtures obtained by warm mixing
-
- 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
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/06—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys in the form of particles, e.g. powder
-
- 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
- H01F41/02—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 for manufacturing cores, coils, or magnets
- H01F41/0253—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 for manufacturing cores, coils, or magnets for manufacturing permanent magnets
Abstract
The invention discloses a hard magnetic liquid metal paste composite material, wherein a matrix of the composite material is liquid metal, hard magnetic nano particles are wrapped in the liquid metal, the saturation magnetization intensity of the composite material is 1.3-10.0emu/g, and the coercive force of the composite material is 2.2-8.6kOe. The hard magnetic liquid metal paste composite material has stronger coercive force and magnetic saturation strength and higher chemical stability. The invention also discloses a preparation method of the hard magnetic liquid metal paste composite material, which comprises the following steps: (1) Adding liquid metal into a reaction container, adding inert gas, adjusting the pressure of the reaction container to 0.2-0.5MPa, and stirring for 0.5-2h; (2) Continuously introducing inert gas, adding hard magnetic nano particles, and stirring to obtain the hard magnetic liquid metal paste composite material. The method is simple to prepare and is environment-friendly.
Description
Technical Field
The invention belongs to the field of flexible electronics, and particularly relates to a hard magnetic liquid metal paste composite material and a preparation method thereof.
Background
The magnetic liquid metal paste composite material has good magnetic response of magnetic materials, fluidity of liquid metal, high heat conduction and electric conductivity, and has important application value in the fields of elastic wires, self-repairing circuits, bioengineering and the like.
The magnetic materials currently used for preparing the magnetic liquid metal paste composite material are soft magnetic Fe, ni and Gd micron particles and hard magnetic NdFeB micron particles. The patent number CN109003773B discloses a multifunctional liquid metal, which takes the liquid metal as a core, the liquid metal belt has magnetism, and the surface of the liquid metal is not provided with a film. The invention also relates to a preparation method of the multifunctional liquid metal, which comprises the following steps: (1) Providing a substrate, placing alloy powder on the substrate, rolling liquid metal on the alloy powder, and uniformly coating the alloy powder outside the liquid metal to obtain magnetic liquid metal; (2) Adding hydrochloric acid into the magnetic liquid metal for treatment, wherein a film is formed on the surface of the magnetic liquid metal; (3) Providing a channel in which an electrolyte solution is placed; (4) Placing the magnetic liquid metal treated in the step (2) in an electrolyte solution, and applying a direct current power supply; (5) The magnetic liquid metal breaks through the film to flow out and drags the film to move towards the cathode, and when the magnetic liquid metal is separated from the film, the direct current power supply is turned off. However, fe, ni, gd and NdFeB microparticles are susceptible to oxidation and are chemically unstable; meanwhile, fe and Ni are easy to chemically react with liquid metal to form intermetallic metal alloy (Gd 5Fe6) and the like, so that the property of the composite material is deteriorated and the stability is reduced. The composite material not only loses the inherent fluidity and self-repairing function of the liquid metal, but also reduces the electric and thermal conductivity, and limits the application of the magnetic liquid metal paste composite material in the fields of flexible elastic electronic devices and self-repairing robots, in particular bioengineering.
In order to fully utilize the excellent magnetic response of the magnetic liquid metal paste and the flexibility, the stretchability, the self-repairing property, the high electric conductivity and the high thermal conductivity of the liquid metal, the preparation of the magnetic liquid metal paste composite material with stable chemical properties is particularly important.
Meanwhile, as the liquid metal is easy to oxidize in the air, a gallium oxide layer is formed on the surface of the liquid metal, and the magnetic particles are prevented from being in direct contact with the liquid metal, so that the magnetic particles are adhered to the oxide layer on the surface, and the wettability of the magnetic particles and the liquid metal is reduced. In order to improve the wettability of liquid metal and magnetic particles, HCl dilute solution is generally used as a solvent, and then the magnetic liquid metal paste composite material is obtained through water washing and drying processes. The oxide on the surface of the liquid metal can be removed by utilizing the HCl dilute solution, so that the liquid metal is prevented from being further oxidized in the stirring process, but the preparation process is complicated by washing the HCl dilute solution by deionized water, the preparation cost is increased, and the residual HCl dilute solution has a corrosion effect on magnetic particles, so that the magnetic performance of the magnetic particles is reduced.
Disclosure of Invention
The invention provides a hard magnetic liquid metal paste composite material, which has higher chemical stability and stronger hard magnetism, and the preparation method is simple and environment-friendly.
The matrix of the hard magnetic liquid metal paste composite material is liquid metal, hard magnetic nano particles are wrapped in the liquid metal, and the composite material has saturation magnetization intensity of 1.3-10.0emu/g and coercive force of 2.2-8.6kOe.
The surface of the hard magnetic liquid metal forms a compact oxide film, so that oxygen and moisture in air can be prevented from entering the liquid metal to oxidize the liquid metal and the hard magnetic nano particles, and the hard magnetic liquid metal has higher conductivity; the hard magnetic nano particles have better wettability with liquid metal and do not react with the liquid metal, so that the hard magnetic liquid metal has good hard magnetic performance and chemical stability.
The mass ratio of the liquid metal to the hard magnetic nano particles is 99:1-70:30.
The content of the magnetic particles directly affects the fluidity and magnetic responsiveness of the liquid metal, and when the content of the hard magnetic nanoparticles is too low, the fluidity of the liquid metal is good and the magnetic responsiveness is weak, and when the content of the hard magnetic nanoparticles is too high, the fluidity of the liquid metal is reduced and the magnetic responsiveness is enhanced.
The particle size of the hard magnetic nano particles is 5-200nm.
The liquid metal is one or more of gallium (Ga), indium (In), tin (Sn), ga-In alloy and gallium (Ga).
The hard magnetic nano material is one or more of iron platinum (fct/L1 0 -FePt), iron palladium (fct-FePd) and cobalt platinum (fct-CoPt) with a face-centered tetragonal structure. Further preferably, the hard magnetic nanomaterial is iron platinum (fct-FePt) with a face-centered tetragonal structure.
The fct-FePt nano particles have excellent chemical stability and do not react with liquid metal, so that the chemical property and structural stability of the magnetic liquid metal are improved, and the platinum metal and the liquid metal have good wettability, so that the iron-platinum alloy and the liquid metal also have good wettability.
The invention also provides a preparation method of the hard magnetic liquid metal paste composite material, which comprises the following steps:
(1) Adding liquid metal into a reaction container, adding inert gas, adjusting the pressure of the reaction container to 0.2-0.5MPa, and stirring for 0.5-2h;
(2) Continuously introducing inert gas, adding hard magnetic nano particles, and stirring to obtain the hard magnetic liquid metal paste composite material.
The step (1) can remove air and moisture in the reaction vessel through inert gas, nitrogen enters the liquid metal to form inert bubble micropores, the bonding strength of the liquid metal and the magnetic particles is enhanced, and the structural stability of the magnetic liquid metal paste is improved.
Under the synergistic effect of proper stirring time, speed and pressure of a reaction container, inert gas enters liquid metal, micropores are formed by flowing in the liquid metal, so that the liquid metal has higher surface energy, and under the synergistic effect of the surface energy and capillary force of the micropores, hard magnetic nano particles are tightly combined in the liquid metal, and the combination capability with the hard magnetic nano particles is enhanced; the hard magnetic nano particles do not react with the liquid metal, so that the hard magnetic liquid metal paste composite material has good hard magnetic property and chemical stability.
The hard magnetic nano material has high magnetocrystalline anisotropy energy, extremely small superparamagnetic limit size, high Curie temperature and excellent chemical stability; the high curie temperature can make it useful in medium and high temperature environments while having good hard magnetic properties.
In the step (1), the reaction container is a multi-port bottle, an inert gas operation box or a glove box.
In the step (1), the inert gas is one or more of nitrogen, argon or helium.
In the step (1), the stirring conditions are as follows: the stirring mode is one or two of magnetic stirring and mechanical stirring, the stirring time is 0.5-2h, and the stirring speed is 300-1000rpm.
The fct-FePt nano particles are filled in the micropore structure of the liquid metal through proper stirring time, stirring speed and pressure of a reaction container, so that the hard magnetic liquid metal paste composite material has good structural stability.
In the step (1), the preparation temperature is a temperature equal to or higher than the melting point of the liquid metal.
In the step (2), the stirring conditions are as follows: the stirring mode is mechanical stirring or magnetic stirring, the stirring time is 1-10h, and the stirring speed is 100-800rpm.
Compared with the prior art, the invention has the beneficial effects that:
(1) The hard magnetic material in the paste composite material provided by the invention does not react with the liquid metal, so that the pollution of the hard magnetic material is prevented, and the paste composite material provided by the invention has higher coercive force and magnetic saturation strength and good chemical stability.
(2) Because the paste composite material provided by the invention has good wettability, hard magnetic iron platinum particles enter liquid metal, and the surface is a liquid metal layer, air and moisture in the external environment are prevented from entering the liquid metal, so that the paste composite material provided by the invention has higher oxidation resistance.
(3) The method for preparing the paste composite material does not use acid solution such as hydrochloric acid and the like as a solvent, avoids the influence of a water washing process and a drying process on the environment, and is simple.
Drawings
FIG. 1 is a flow chart of the preparation of a hard magnetic liquid metal paste composite material according to the invention, wherein a is a reaction device, 1 in a is a reactor, 2 represents a stirring device, 3 represents an air outlet pipe, b is a reaction device after liquid metal is added, 4 in b represents an air inlet pipe, 5 represents liquid metal, c is a reaction device after magnetic particles are added, 6 in c represents hard magnetic nano particles, d is a reaction device after the reaction is finished, and 7 in d represents a hard magnetic liquid metal paste composite material;
FIG. 2 is a physical picture of the hard magnetic liquid metal paste composite material prepared in example 1 of the present invention;
FIG. 3 is a scanning electron microscope image of the hard magnetic liquid metal paste composite material prepared in example 1 of the present invention;
FIG. 4 is an X-ray diffraction pattern of the fct-FePt@eGaIn paste composite material prepared in example 1 of the invention;
FIG. 5 is a hysteresis loop diagram of the fct-FePt@eGaIn paste composite material prepared in example 1 of the present invention;
FIG. 6 is a cross-sectional scanning electron microscope picture of the hard magnetic liquid metal paste composite material prepared in example 1 of the present invention;
FIG. 7 is a physical image of the hard magnetic liquid metal paste composite material prepared in example 2 of the present invention;
FIG. 8 is a scanning electron microscope image of the hard magnetic liquid metal paste composite material prepared in example 2 of the present invention;
FIG. 9 is an X-ray diffraction pattern of the fct-FePt@eGaIn paste composite material prepared in example 2 of the present invention;
FIG. 10 is a hysteresis loop diagram of the fct-FePt@eGaIn paste composite material prepared in example 2 of the present invention.
Detailed Description
The present invention will be further described with reference to the accompanying drawings and examples, wherein it is to be understood that the examples described below are some, but not all embodiments of the invention. Given the embodiments of the present invention, all other embodiments that would be obvious to one of ordinary skill in the art without making any inventive effort are within the scope of the present invention.
Example 1
In this example, the hard magnetic material used was fct-FePt nanoparticles at 30nm, and the liquid metal was gallium indium alloy. Wherein the mass ratio of the fct-FePt nano particles to the gallium indium alloy is 5:95, namely the mass fraction of the hard magnetic nano particles is 5%;
The reaction apparatus was connected as shown in FIG. 1a, and the air tightness was checked. The gallium indium alloy was pretreated under nitrogen atmosphere according to fig. 1b. According to the figure 1c, adding hard magnetic fct-FePt nano particles according to the mass ratio, and mixing to obtain the hard magnetic fct-FePt@eGaIn paste composite material as shown in the figure 1 d;
The specific method comprises the following steps:
Step 1: the reactor device was connected and sealed with a green tape. Opening a nitrogen pressure reducing valve to charge nitrogen, and checking the air tightness;
Step 2: under inert atmosphere, 1.9g of gallium-indium alloy is added into the reactor, and the air and water gas in the reactor are removed for 1h. Stirring is started, stirring is continued for 1h, and pretreatment is carried out on the liquid metal.
Step 3: and continuously adding 0.1g of fct-FePt nano particles under inert atmosphere, and stirring to obtain the hard magnetic fct-FePt@eGaIn paste composite material.
As shown in FIG. 2, when the doping amount of the fct-FePt nano particles is 5%, the fct-FePt@eGaIn has good fluidity, and the fct-FePt@eGaIn is automatically contracted to form a sphere like a pure eGaIn, so that the surface is smooth.
As shown in FIG. 3, fct-FePt nanoparticles and eGaIn have good wettability, all enter eGaIn, and a layer of eGaIn metal film is formed on the surface. Some protrusions were also observed, formed by fct-FePt nanoparticles entering eGaIn.
As shown in FIG. 4, characteristic peaks of fct-FePt nanoparticles and eGaIn can be clearly observed.
As shown in FIG. 5, the saturation magnetization and coercive force were 1.3emu/g and 4.75kOe, respectively.
As shown in fig. 6, a large number of hard magnetic fct-FePt nanoparticles are uniformly distributed inside the liquid metal eGaIn.
Example 2
In this example, the hard magnetic material used was 34nm fct-FePt nanoparticles and the liquid metal was gallium indium alloy. Wherein the mass ratio of fct-FePt nano particles to gallium indium alloy is 79:21, namely the mass fraction of hard magnetic nano particles is 21%;
The reaction apparatus was connected as shown in FIG. 1a, and the air tightness was checked. The gallium indium alloy was pretreated under nitrogen atmosphere according to fig. 1b. According to the figure 1c, adding hard magnetic fct-FePt nano particles according to the mass ratio, and mixing to obtain the hard magnetic fct-FePt@eGaIn paste composite material as shown in the figure 1 d;
The specific method comprises the following steps:
Step 1: the reactor device was connected and sealed with a green tape. Opening a nitrogen pressure reducing valve to charge nitrogen, and checking the air tightness;
Step 2: under inert atmosphere, 1.58g of gallium-indium alloy was added to the reactor, and the air and water gas in the reactor were purged for 1 hour. Stirring is started, stirring is continued for 1h, and pretreatment is carried out on the liquid metal;
Step 3: and continuously adding 0.42g of fct-FePt nano particles under inert atmosphere, and stirring to obtain the hard magnetic fct-FePt@eGaIn paste composite material.
As shown in fig. 7, as the content of fct-FePt nanoparticles increases, viscosity and hardness of the liquid metal increase, fluidity decreases, and the fct-fept@egain paste may be fixed in a cylindrical shape.
As shown in fig. 8, it can be seen that fct-FePt nanoparticles are uniformly distributed on the surface of the liquid metal.
As shown in FIG. 9, as the content of fct-FePt nanoparticles increases, the peak intensity of the fct-FePt phase in the XRD pattern increases, while the peak intensity of the liquid metal is relatively decreased.
As shown in FIG. 10, the saturation magnetization and coercive force were 6.8emu/g and 6.6kOe, respectively.
Claims (9)
1. The hard magnetic liquid metal paste composite material is characterized in that a matrix of the composite material is liquid metal, hard magnetic nano particles are wrapped in the liquid metal, the saturation magnetization intensity of the composite material is 1.3-10.0emu/g, and the coercive force of the composite material is 2.2-8.6kOe;
the preparation method of the hard magnetic liquid metal paste composite material comprises the following steps:
(1) Adding liquid metal into a reaction container, adding inert gas, adjusting the pressure of the reaction container to 0.2-0.5MPa, and stirring for 0.5-2h;
(2) Continuously introducing inert gas, adding hard magnetic nano particles, and stirring to obtain the hard magnetic liquid metal paste composite material.
2. The hard magnetic liquid metal paste composite material according to claim 1, wherein the mass ratio of the liquid metal to the hard magnetic nanoparticles is 1:99-70:30.
3. The hard magnetic liquid metal paste composite material according to claim 1, wherein the hard magnetic nanoparticles have a particle diameter of 5-200nm.
4. The hard magnetic liquid metal paste composite material according to claim 1, wherein the liquid metal is one or more of gallium, indium, tin, gallium indium alloy.
5. The hard magnetic liquid metal paste composite material according to claim 1, wherein the hard magnetic nanomaterial is one or more of iron platinum, iron palladium or cobalt platinum in a face-centered tetragonal structure.
6. The method for preparing a composite material of a hard magnetic liquid metal paste according to claim 1, wherein in the step (1), the reaction vessel is a multi-necked flask, an inert gas operation box or a glove box.
7. The method for preparing a hard magnetic liquid metal paste composite material according to claim 1, wherein the inert gas is one or more of nitrogen, argon and helium.
8. The method for preparing a hard magnetic liquid metal paste composite material according to claim 1, wherein in the step (1), the stirring conditions are as follows: the stirring mode is one or two of magnetic stirring and mechanical stirring, the stirring time is 0.5-2h, and the stirring speed is 300-1000rpm.
9. The method for preparing a hard magnetic liquid metal paste composite material according to claim 1, wherein in the step (2), the stirring conditions are as follows: the stirring mode is mechanical stirring or magnetic stirring, the stirring time is 1-10h, and the stirring speed is 100-800rpm.
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| CN1955252A (en) * | 2005-10-24 | 2007-05-02 | 中国科学院理化技术研究所 | Nano metal fluid with high heat-transfer performance |
| CN107545973A (en) * | 2017-06-26 | 2018-01-05 | 中国科学院理化技术研究所 | A kind of liquid metal magnetohydrodynamic and preparation method thereof |
| CN108085519A (en) * | 2016-11-21 | 2018-05-29 | 云南科威液态金属谷研发有限公司 | A kind of method and its application that micro-nano granules are adulterated into liquid metal |
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| CN1955252A (en) * | 2005-10-24 | 2007-05-02 | 中国科学院理化技术研究所 | Nano metal fluid with high heat-transfer performance |
| CN108085519A (en) * | 2016-11-21 | 2018-05-29 | 云南科威液态金属谷研发有限公司 | A kind of method and its application that micro-nano granules are adulterated into liquid metal |
| CN107545973A (en) * | 2017-06-26 | 2018-01-05 | 中国科学院理化技术研究所 | A kind of liquid metal magnetohydrodynamic and preparation method thereof |
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