CN113077954A - 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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- CN113077954A CN113077954A CN202110320209.6A CN202110320209A CN113077954A CN 113077954 A CN113077954 A CN 113077954A CN 202110320209 A CN202110320209 A CN 202110320209A CN 113077954 A CN113077954 A CN 113077954A
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- 229910001338 liquidmetal Inorganic materials 0.000 title claims abstract description 108
- 239000002131 composite material Substances 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 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 10
- 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
- 229910000846 In alloy Inorganic materials 0.000 claims description 10
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims description 8
- 229910052733 gallium Inorganic materials 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- OBACEDMBGYVZMP-UHFFFAOYSA-N iron platinum Chemical compound [Fe].[Fe].[Pt] OBACEDMBGYVZMP-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
- 239000007788 liquid Substances 0.000 claims 3
- 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
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 239000000696 magnetic material Substances 0.000 description 6
- 230000004043 responsiveness Effects 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 239000012298 atmosphere Substances 0.000 description 4
- 229910052742 iron Inorganic materials 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
- 238000001000 micrograph Methods 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 229910052688 Gadolinium Inorganic materials 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000008151 electrolyte solution Substances 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000005389 magnetism Effects 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
- 239000002994 raw material Substances 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
- 238000005406 washing Methods 0.000 description 2
- 229910018979 CoPt 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
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000010586 diagram Methods 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
- 239000001995 intermetallic alloy Substances 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
- 239000011859 microparticle Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
Images
Classifications
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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
- 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 inside the liquid metal, the saturation magnetization of the composite material is 1.3-10.0emu/g, and the coercive force is 2.2-8.6 kOe. The hard magnetic liquid metal paste composite material has strong coercive force and magnetic saturation strength and high 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 be 0.2-0.5MPa, and stirring for 0.5-2 h; (2) and continuously introducing inert gas, adding the hard magnetic nanoparticles, 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 responsiveness of the magnetic material, and has fluidity, high heat conductivity and electric conductivity of the liquid metal, so that the magnetic liquid metal paste composite material 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 comprise soft magnetic Fe, Ni and Gd micron particles and hard magnetic NdFeB micron particles. Patent No. CN109003773B discloses a multifunctional liquid metal, which uses liquid metal as core, and the liquid metal band has magnetism and no film on the surface of the liquid metal. 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, and rolling liquid metal on the alloy powder to ensure that the alloy powder is uniformly wrapped outside the liquid metal to obtain magnetic liquid metal; (2) adding hydrochloric acid into the magnetic liquid metal for treatment, and forming a film on the surface of the magnetic liquid metal; (3) providing a channel, wherein an electrolyte solution is placed in the channel; (4) placing the magnetic liquid metal processed in the step (2) in an electrolyte solution, and applying a direct-current power supply; (5) the magnetic liquid metal breaks the film and flows 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 switched off. However, Fe, Ni, Gd and NdFeB microparticles are easily oxidized and chemically unstable; meanwhile, Fe and Ni are easy to react with liquid metal to form intermetallic alloy (Gd)5Fe6) And the like, thereby causing deterioration in properties and reduction in stability of the composite material. Therefore, the composite material loses the inherent mobility and self-repairing function of the liquid metal, reduces the electric conduction and heat conduction properties, and limits the application of the magnetic liquid metal paste composite material in the fields of flexible elastic electronic devices, self-repairing robots, particularly bioengineering.
In order to fully utilize the excellent magnetic responsiveness of the magnetic liquid metal paste and the flexibility, stretchability, self-repairing, high electric conductivity and thermal conductivity of the liquid metal, it is particularly important to prepare the magnetic liquid metal paste composite material with stable chemical properties.
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 to prevent the magnetic particles from directly contacting 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 the liquid metal and the magnetic particles, a dilute HCl solution is usually used as a solvent, and then the magnetic liquid metal paste composite material is obtained through water washing and drying processes. The dilute HCl solution can be used for removing oxides on the surface of the liquid metal and preventing the liquid metal from being further oxidized in the stirring process, but the dilute HCl solution is washed by deionized water, so that the preparation process is more complicated, the preparation cost is increased, the residual dilute HCl solution has a corrosion effect on the magnetic particles, and the magnetic performance of the magnetic particles is reduced.
Disclosure of Invention
The invention provides a hard magnetic liquid metal paste composite material, wherein the hard magnetic liquid metal has higher chemical stability and stronger hard magnetism, and the preparation method is simple and environment-friendly.
A matrix of the composite material is liquid metal, hard magnetic nanoparticles are wrapped inside the liquid metal, the saturation magnetization of the composite material is 1.3-10.0emu/g, and the coercive force is 2.2-8.6 kOe.
A compact oxide film is formed on the surface of the hard magnetic liquid metal, so that oxygen and moisture in the air can be prevented from entering the liquid metal to oxidize the liquid metal and the hard magnetic nano particles, and the high conductivity is realized; the hard magnetic nanoparticles have good 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 nanoparticles is 99:1-70: 30.
The content of the magnetic particles directly influences the fluidity and the magnetic responsiveness of the liquid metal, when the content of the hard magnetic nanoparticles is too low, the fluidity of the liquid metal is good, the magnetic field 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 field responsiveness is enhanced.
The particle size of the hard magnetic nano particles is 5-200 nm.
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 iron platinum (fct/L1) with a face-centered tetragonal structure0-FePt), iron palladium (fct-FePd) and cobalt platinum (fct-CoPt). Further preferably, the hard magnetic nano material 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 the 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 be 0.2-0.5MPa, and stirring for 0.5-2 h;
(2) and continuously introducing inert gas, adding the hard magnetic nanoparticles, and stirring to obtain the hard magnetic liquid metal paste composite material.
In the step (1), air and moisture in the reaction container can be removed 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 action of proper stirring time, speed and pressure of a reaction container, inert gas enters the liquid metal and flows in the liquid metal to form micropores, so that the liquid metal has higher surface energy, and under the synergistic action of the surface energy and the capillary force of the micropores, the hard magnetic nanoparticles are tightly combined in the liquid metal, so that the combining capacity with the hard magnetic nanoparticles is enhanced; the hard magnetic nanoparticles do not react with the liquid metal, so that the hard magnetic liquid metal paste composite material has good hard magnetic performance and chemical stability.
The hard magnetic nano material has high magnetocrystalline anisotropy, extremely small superparamagnetic limit size, high Curie temperature and excellent chemical stability; the high curie temperature allows it to be used in medium and high temperature environments while having good hard magnetic properties.
In the step (1), the reaction container is a multi-mouth 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 300-1000 rpm.
And the fct-FePt nanoparticles are filled in the microporous structure of the liquid metal through proper stirring time, stirring speed and pressure of the reaction vessel, so that the hard magnetic liquid metal paste composite material has good structural stability.
In the step (1), the preparation temperature is a temperature above 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 100-800 rpm.
Compared with the prior art, the invention has the beneficial effects that:
(1) as the hard magnetic material in the paste composite material provided by the invention does not react with the liquid metal, the hard magnetic material is prevented from being polluted, and the paste composite material provided by the invention has higher coercive force and magnetic saturation strength and good chemical stability.
(2) The paste composite material provided by the invention has good wettability, and hard magnetic iron and platinum particles enter liquid metal, and the surface of the paste composite material is a liquid metal layer, so that air and moisture in the external environment are prevented from entering the liquid metal, and the paste composite material provided by the invention has high oxidation resistance.
(3) The method for preparing the paste composite material provided by the invention does not use acid solutions such as hydrochloric acid and the like as solvents, 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 present invention for preparing a hard magnetic liquid metal paste composite material, 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 adding liquid metal, 4 in b represents an air inlet pipe, 5 represents liquid metal, c is a reaction device after adding magnetic particles, 6 in c represents hard magnetic nanoparticles, d is a reaction device after reaction, and 7 in d represents a hard magnetic liquid metal paste composite material;
FIG. 2 is a picture of a hard magnetic liquid metal paste composite 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 a fct-FePt @ eGaIn paste composite prepared in example 1 of the present invention;
FIG. 5 is a magnetic hysteresis loop diagram of a fct-FePt @ eGaIn paste composite prepared in example 1 of the present invention;
FIG. 6 is a scanning electron microscope image of a cross section of a hard magnetic liquid metal paste composite material prepared in example 1 of the present invention;
FIG. 7 is a picture of a hard magnetic liquid metal paste composite prepared in example 2 of the present invention;
FIG. 8 is a scanning electron microscope image of a hard magnetic liquid metal paste composite material prepared in example 2 of the present invention;
FIG. 9 is an X-ray diffraction pattern of a fct-FePt @ eGaIn paste composite prepared in example 2 of the present invention;
FIG. 10 is a magnetic hysteresis loop plot of fct-FePt @ eGaIn paste composite 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, which are intended to illustrate some, but not all, embodiments of the invention. Given the embodiments of the present invention, all other embodiments that can be obtained by a person of ordinary skill in the art without any inventive step are within the scope of the present invention.
Example 1
In this example, the hard magnetic material used was fct-FePt nanoparticles of 30nm, and the liquid metal was gallium indium alloy. Wherein the mass ratio of fct-FePt nanoparticles to the gallium-indium alloy is 5:95, namely the mass fraction of the hard magnetic nanoparticles is 5%;
the reaction apparatus was connected as shown in FIG. 1a and checked for gas tightness. The gallium indium alloy was pretreated under nitrogen atmosphere according to FIG. 1 b. Adding hard magnetic fct-FePt nanoparticles according to the mass ratio and mixing as shown in figure 1c to obtain a hard magnetic fct-FePt @ eGaIn paste composite material as shown in figure 1 d;
the specific method comprises the following steps:
step 1: the reactor device is connected and sealed by a raw material belt. Opening a nitrogen pressure reducing valve, filling nitrogen, and checking the air tightness;
step 2: under inert atmosphere, 1.9g of gallium-indium alloy is added into a reactor, and air and moisture in the reactor are removed for 1 h. Starting stirring, and continuously stirring for 1h to pretreat the liquid metal.
And step 3: and continuously adding 0.1g of fct-FePt nano particles in an 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 nanoparticles is 5%, the fct-FePt @ eGaIn has good fluidity, and automatically shrinks to form a spherical shape and has a smooth surface like pure eGaIn.
As shown in fig. 3, fct-FePt nanoparticles have good wettability with eGaIn, and all enter the eGaIn, and a layer of eGaIn metal film is formed on the surface. Some bulges were also observed, formed by fct-FePt nanoparticles entering the interior of the eGaIn.
As shown in fig. 4, characteristic peaks of fct-FePt nanoparticles and characteristic peaks of eGaIn can be clearly observed.
As shown in FIG. 5, the saturation magnetization and the 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 nanoparticles to the gallium-indium alloy is 79:21, namely the mass fraction of the hard magnetic nanoparticles is 21%;
the reaction apparatus was connected as shown in FIG. 1a and checked for gas tightness. The gallium indium alloy was pretreated under nitrogen atmosphere according to FIG. 1 b. Adding hard magnetic fct-FePt nanoparticles according to the mass ratio and mixing as shown in figure 1c to obtain a hard magnetic fct-FePt @ eGaIn paste composite material as shown in figure 1 d;
the specific method comprises the following steps:
step 1: the reactor device is connected and sealed by a raw material belt. Opening a nitrogen pressure reducing valve, filling nitrogen, and checking the air tightness;
step 2: under inert atmosphere, 1.58g of gallium-indium alloy is added into a reactor, and air and moisture in the reactor are removed for 1 h. Starting stirring, continuously stirring for 1h, and pretreating the liquid metal;
and step 3: and continuously adding 0.42g of fct-FePt nano particles in an inert atmosphere, and stirring to obtain the hard magnetic fct-FePt @ eGaIn paste composite material.
As shown in fig. 7, as the fct-FePt nanoparticle content increases, the liquid metal viscosity and hardness increases, the fluidity decreases, and the fct-FePt @ eGaIn paste can 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 relatively decreases.
As shown in FIG. 10, the saturation magnetization and the coercive force were 6.8emu/g and 6.6kOe, respectively.
Claims (10)
1. The hard magnetic liquid metal paste composite material is characterized in that a matrix of the composite material is liquid metal, hard magnetic nanoparticles are wrapped inside the liquid metal, the saturation magnetization of the composite material is 1.3-10.0emu/g, and the coercive force is 2.2-8.6 kOe.
2. The hard magnetic liquid metal paste composite according to claim 1, characterized in that the mass ratio of the liquid metal and the hard magnetic nanoparticles is 1:99-70: 30.
3. The hard magnetic liquid metal paste composite according to claim 1, characterized in that the hard magnetic nanoparticles have a particle size of 5-200 nm.
4. The hard magnetic liquid metal paste composite 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 nano material is one or more of iron platinum, iron palladium or cobalt platinum with a face-centered tetragonal structure.
6. Method for the preparation of a hard magnetic liquid metal paste composite according to any of claims 1-5, comprising:
(1) adding liquid metal into a reaction container, adding inert gas, adjusting the pressure of the reaction container to be 0.2-0.5MPa, and stirring for 0.5-2 h;
(2) and continuously introducing inert gas, adding the hard magnetic nanoparticles, and stirring to obtain the hard magnetic liquid metal paste composite material.
7. The method for preparing a hard magnetic liquid metal-paste composite material according to claim 6, wherein in step (1), the reaction vessel is a multi-port bottle, an inert gas operation box or a glove box.
8. The method of claim 6, wherein the inert gas is one or more of nitrogen, argon, helium.
9. The method for preparing a hard magnetic liquid metal-paste composite material according to claim 6, 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 300-1000 rpm.
10. The method for preparing a hard magnetic liquid metal-paste composite material according to claim 6, 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 100-800 rpm.
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| CN115725869A (en) * | 2021-08-30 | 2023-03-03 | 中国科学院理化技术研究所 | Preparation method of composite thermal interface material, composite thermal interface material and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| US20070218282A1 (en) * | 2006-03-16 | 2007-09-20 | Fujitsu Limited | Hard-magnetic nanoparticles, manufacturing method therefor, magnetic fluid and magnetic recording medium |
| 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 |
| US20070218282A1 (en) * | 2006-03-16 | 2007-09-20 | Fujitsu Limited | Hard-magnetic nanoparticles, manufacturing method therefor, magnetic fluid and magnetic recording medium |
| 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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| CN115725869A (en) * | 2021-08-30 | 2023-03-03 | 中国科学院理化技术研究所 | Preparation method of composite thermal interface material, composite thermal interface material and application thereof |
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