CN110202166B - Chemical method for synthesizing fct-FePt nano particle by liquid phase assisted solid phase sintering - Google Patents

Chemical method for synthesizing fct-FePt nano particle by liquid phase assisted solid phase sintering Download PDF

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CN110202166B
CN110202166B CN201910549952.1A CN201910549952A CN110202166B CN 110202166 B CN110202166 B CN 110202166B CN 201910549952 A CN201910549952 A CN 201910549952A CN 110202166 B CN110202166 B CN 110202166B
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powder
nacl
metal precursor
ethyl alcohol
heating
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CN110202166A (en
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裴文利
赵东
吴纯
***
王凯
王强
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Northeastern University China
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    • 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
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/30—Making metallic powder or suspensions thereof using chemical processes with decomposition of metal compounds, e.g. by pyrolysis
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • 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

Abstract

The invention discloses a chemical method for synthesizing fct-FePt nano particles by liquid-phase assisted solid-phase sintering, which comprises the following steps: mixing metal precursor powder and NaCl/KCl powder with a low-boiling-point solvent according to a ratio, heating and stirring to uniformly dissolve the metal precursor powder and the NaCl/KCl powder in the low-boiling-point solvent, heating and continuously stirring to evaporate the solvent to form uniformly mixed powder of the metal precursor and the NaCl/KCl, annealing the mixed powder, cooling to room temperature, dissolving and dispersing in a mixed solution of deionized water and absolute ethyl alcohol, centrifuging to remove the NaCl/KCl, and pouring off the upper-layer centrifugate; adding absolute ethyl alcohol, dissolving and dispersing, adding deionized water with the same ratio as the absolute ethyl alcohol, centrifugally separating, and pouring off the upper layer of the centrifugate; and (3) repeating the dissolving and centrifuging operation of adding absolute ethyl alcohol and deionized water for 3-5 times to prepare the fct-FePt nano particles. The method is simple in operation process, low-carbon and environment-friendly, and the prepared nanoparticles are small and uniform in size, uniform in shape, good in dispersity and high in order degree.

Description

Chemical method for synthesizing fct-FePt nano particle by liquid phase assisted solid phase sintering
The technical field is as follows:
the invention belongs to the technical field of magnetic nano materials, and particularly relates to a chemical method for synthesizing fct-FePt nano particles by liquid-phase assisted solid-phase sintering.
Background art:
the fct-FePt nano material has high magnetocrystalline anisotropy (K)μ≈7×106J/cm3) Low superparamagnetic critical dimension (2.8-3.3 nm) and excellent catalytic performance, and has wide application prospect in the fields of high-density magnetic recording, permanent magnets, biomedicine, electrochemical catalysis and the like. The application performance of the fct-FePt nano material is closely related to the uniformity of the shape and the size of the fct-FePt nano material and the phase structure of the fct-FePt nano material. The existing method for synthesizing the fct-FePt nano particle mainly comprises the following steps: physical methods and chemical methods. The physical method mainly comprises a ball milling method and a magnetron sputtering method, and the synthesized FePt nano material has the problems of difficult shape control, uneven size and the like; the chemical method can obtain more uniform nano materials, but the FePt directly prepared has an fcc structure, and has lower magnetic property and catalytic property, so the FePt can not be directly preparedThe application is satisfied. High-temperature heat treatment above 550 ℃ is required to convert FePt nanoparticles from fcc to fct (L1)0) However, the high-temperature heat treatment causes the agglomeration and abnormal growth of the nanoparticles, so how to obtain fct-FePt nano-material with good dispersibility, small size and uniformity is a bottleneck problem in the field.
The invention content is as follows:
the invention aims to provide a chemical method for synthesizing fct-FePt nanoparticles by liquid-phase assisted solid-phase sintering, aiming at solving the problems in the prior art. The chemical components of the product can be adjusted by adjusting and controlling the proportion of the precursor; the mixing ratio of NaCl/KCl and the precursor with the isolation effect is adjusted by changing the proportion of the low-boiling-point solvent, the NaCl/KCl and the precursor, so that the size of the particles is regulated and controlled; the shape, size and order degree of the product are controlled by adjusting the temperature and time of solid-phase calcination.
In order to achieve the purpose, the invention adopts the following technical scheme:
a chemical method for synthesizing fct-FePt nanoparticles by liquid-phase assisted solid-phase sintering comprises the following steps:
step 1: pretreatment of precursors
(1) Ball-milling NaCl/KCl particles to obtain NaCl/KCl powder with the particle size of 500 nm-500 microns for later use;
(2) weighing a metal precursor powder comprising the metal precursor Fe (acac)3Powder and Metal precursor Pt (acac)2Powder with the molar ratio of 0.3-2 for later use;
step 2: mixing of precursors
(1) Adding metal precursor powder and a low-boiling-point solvent into a container according to the proportion of 1: 300-500 in unit g: ml;
(2) uniformly dissolving metal precursor powder in a low-boiling-point solvent by heating and stirring, wherein the heating temperature is 50-100 ℃ and the time is 10-30 min;
(3) adding NaCl/KCl powder in the step 1(1) with the mass being 50-400 times that of the metal precursor powder into the dissolved metal salt precursor, heating and continuously stirring to sequentially dissolve the NaCl/KCl powder, volatilize the low-boiling-point solvent, separate out the NaCl/KCl and the metal precursor, and finally forming mixed powder of the metal precursor and the NaCl/KCl, wherein the heating temperature is 50-150 ℃, and the heating time is 60-150 min;
and step 3: sintering of precursor
Putting the metal precursor and NaCl/KCl mixed powder into a crucible, putting the crucible into a vacuum heat treatment furnace, and annealing in an oxygen-free atmosphere at the annealing temperature of 550-750 ℃ for 30-150 min to form annealed mixed powder;
and 4, step 4: NaCl/KCl removal
(1) Cooling the annealed mixed powder to room temperature, taking a mixed solution of deionized water and absolute ethyl alcohol, dissolving and dispersing the annealed mixed powder, centrifuging at the speed of 6000-10000 rpm for 5-10 min, removing NaCl/KCl, and pouring out the upper-layer centrifugate;
(2) adding absolute ethyl alcohol for dissolving and dispersing, wherein the addition amount of the absolute ethyl alcohol is in a ratio of 1: 30-50 after annealing, and the unit is g: ml;
(3) adding deionized water with the same ratio as the absolute ethyl alcohol in the step (2), performing centrifugal separation again, and pouring off the upper layer of the centrifugal liquid; wherein the centrifugal rotating speed is 6000-10000 rpm, and the centrifugal time is 5-10 min;
(4) repeating the steps (2) - (3) for 3-5 times to prepare the fct-FePt nano particle.
In the step 1(1), the NaCl/KCl particles mean that one of the NaCl particles or the KCl particles is taken and treated; the same applies later.
In the steps 2, (2) and 2(3), the stirring speed is 1000-2500 rpm.
In the step 2(3), after NaCl/KCl powder is added, the heating is carried out at 50-150 ℃ for 60-150 min, and the specific change process is as follows: heating at 50-150 ℃ for 40-100 min to dissolve the NaCl/KCl powder to form a dissolved solution; and continuously heating at 150-150 ℃ for 20-50 min to volatilize the low-boiling-point solvent, and separating out the metal precursor and the NaCl/KCl to form mixed powder of the metal precursor and the NaCl/KCl.
In the step 2(3), the NaCl/KCl and the metal precursor are precipitated in the solution, so that the NaCl/KCl and the metal precursor can be sufficiently mixed together, and the mixed powder of the NaCl/KCl and the metal precursor is uniform mixed powder.
In the step 3, the mixed powder is pre-treated with 95% Ar + 5% H2And after the mixed gas is subjected to gas scrubbing, annealing treatment is performed.
In the step 3, the oxygen-free atmosphere is 95% Ar + 5% H2Mixed gas atmosphere.
In the step 4(1), the deionized water and the absolute ethyl alcohol in the mixed solution of the deionized water and the absolute ethyl alcohol are mixed in equal volume.
In the step 4(1), the mixture ratio of the annealed mixed powder to the mixed solution of the deionized water and the absolute ethyl alcohol is 1: 60-100, and the unit g is ml.
In the step 2(1), the low-boiling point solvent is one or two of ethanol, ethyl acetate, petroleum ether or n-hexane.
In the step 4(4), the obtained fct-FePt nanoparticles are dispersed in n-hexane for storage.
In the step 4(4), the magnetic property of the nanoparticles is measured by a comprehensive Physical Property Measurement System (PPMS), the morphology and distribution of the nanoparticles are observed by adopting a field emission transmission electron microscope, the phase of the nanoparticles is analyzed by utilizing X-ray diffraction, and the fct-FePt nanoparticles are confirmed to be obtained.
In the step 4(4), the average size of the prepared fct-FePt nanoparticles is 4-15 nm.
In the step 4(4), the prepared fct-FePt nano particles have high degree of order, and the coercive force reaches 2.0-2.4T.
The invention adopts a preparation method combining liquid phase assistance and solid phase sintering chemical reaction to directly synthesize the fct-FePt nano particles with small, uniform and high order degree. Firstly, NaCl/KCl particles and metal precursor powder (Fe and Pt) with a certain proportion are added into a low-boiling point solvent, and are uniformly mixed and fully dissolved. And then heating the solution, volatilizing the low-boiling-point solvent in a temperature environment, and separating NaCl/KCl and the metal precursor out of the solution to form a uniform mixture. And then calcining the mixture at a certain temperature for a period of time to directly synthesize the monodisperse fct-FePt nano particles. The method uses a low-boiling-point liquid phase auxiliary technology to reduce the size of the precursor, improve the uniform distribution of the precursor and improve the local concentration of the precursor, uses NaCl/KCl medium to induce heterogeneous nucleation to improve the nucleation rate, ensures the sufficient mixing of the precursor and NaCl/KCl particles and improves the size uniformity of subsequent sintering products. After the metal precursor is calcined and reacted, nano particles are formed, and due to the isolation effect of NaCl/KCl particles, a uniform mixture of salt and the metal precursor is formed, so that the particles can be prevented from agglomerating and abnormally growing at high temperature.
The invention has the beneficial effects that:
(1) dissolving the metal precursor and NaCl/KCl by using a low-boiling-point solvent, uniformly separating out the metal precursor and the NaCl/KCl by stirring and heating, and forming a precursor and NaCl/KCl mixed powder which are fully and uniformly mixed, wherein the low-boiling-point solvent is easy to volatilize, easy to operate, low in carbon and environment-friendly;
(2) the mixed powder with the metal precursor dispersed uniformly has uniform distribution of Fe and Pt precursors in the annealing process, and the coercive force of the fct-FePt nano-particle can reach 2.4T by a reasonable process. The particle size is small, the appearance is uniform, and the dispersibility is good;
(4) the annealed mixed powder adopts deionized water and ethanol to remove NaCl/KCl, so that the cleaning effect is good, and the mixed powder is non-toxic and pollution-free;
(5) because fct-FePt has important application in the fields of electronics, information, biomedicine, electrochemical catalysis and the like, but the high preparation cost limits the application range of the fct-FePt, the invention promotes the practicability of the one-step synthesis fct-FePt technology, simplifies the prior process, further saves the cost, has good dispersion effect and excellent magnetic property after annealing, and has wide theoretical and application significance.
Description of the drawings:
FIG. 1 is a hysteresis loop of fct-FePt nanoparticles prepared by the method of example 1 of the present invention;
FIG. 2 is an XRD pattern of fct-FePt nanoparticles prepared by the method of example 1 of the present invention;
FIG. 3 is a TEM image of fct-FePt nanoparticles prepared by the method of example 1 of the present invention;
FIG. 4 is a particle size distribution diagram of fct-FePt nanoparticles prepared by the method of example 1 of the present invention;
FIG. 5 is a hysteresis loop of fct-FePt nanoparticles prepared by the method of example 2 of the present invention;
FIG. 6 is an XRD pattern of fct-FePt nanoparticles prepared by the method of example 2 of the present invention;
FIG. 7 is a TEM image of fct-FePt nanoparticles prepared by the method of example 2 of the present invention;
FIG. 8 is a particle size distribution diagram of fct-FePt nanoparticles prepared by the method of example 2 of the present invention;
FIG. 9 is a hysteresis loop of fct-FePt nanoparticles prepared by the method of example 3 of the present invention;
fig. 10 is an XRD pattern of fct-FePt nanoparticles prepared by the method of example 3 of the present invention.
The specific implementation mode is as follows:
the present invention will be described in further detail with reference to examples.
In the following examples:
the preparation equipment is commercially available and can be purchased in the market, and the preparation equipment comprises: quartz crucible, wide-mouth flask, mechanical stirring heating jacket, vacuum drying oven, vacuum heat treatment furnace, centrifuge, ball mill, etc.
The commercial NaCl/KCl powder is processed by a ball mill to obtain reasonable NaCl/KCl granularity (500 nm-500 mu m);
the mechanical stirring heating sleeve mainly aims at enabling the materials to be mixed more uniformly and heating the materials to enable the low-boiling-point solvent to volatilize;
the vacuum drying oven adopts a blowing type vacuum drying oven;
vacuum heat treatment furnace, tubular heat treatment furnace using commercially available vacuum pump and diffusion pump, vacuum degree of 10-3Pa；
Wide-mouth flasks and quartz mortars are commercially available in the market;
the centrifuge is a high-speed centrifuge of HC-2066 type.
Platinum acetylacetonate [ Pt (acac) ] used in examples of the present invention2]And iron acetylacetonate [ Fe (acac)3]All are commercial products (purity > 98%) purchased from the market;
the expressions of the absolute ethyl alcohol A, B and the deionized water A, B are only used for convenience of distinguishing, and the absolute ethyl alcohol and the deionized water are both commercially used for dissolving and dispersing the mixed powder after annealing;
the ball mill is a PBM-V-2L-AD type high-speed rotary ball mill.
The low boiling solvents used in the examples were: one or two of ethanol, ethyl acetate, petroleum ether and n-hexane.
When the number of the low-boiling point solvents is 2, the volume ratio of the ethanol to the ethyl acetate is 1: 1; the volume ratio of the ethanol to the petroleum ether is 1: 1; the volume ratio of the ethanol to the n-hexane is 1: 1; the volume ratio of the ethyl acetate to the petroleum ether is 1: 1; the volume ratio of the ethyl acetate to the n-hexane is 1: 1.
The unit of the ratio of the metal precursor mixed powder to the low-boiling point solvent is g: ml;
the proportion unit of the mixed powder after annealing to the mixed solution of the deionized water A and the absolute ethyl alcohol A is g: ml;
the proportion unit of the mixed powder and the absolute ethyl alcohol B after annealing is g: ml;
in the heating process after the NaCl/KCl powder is dissolved and uniformly dispersed to form the dissolved solution, the NaCl/KCl and the metal precursor are separated out from the solution, so that the NaCl/KCl and the metal precursor can be fully mixed together, and the mixed powder of the NaCl/KCl and the metal precursor is uniformly mixed powder.
Example 1:
first, NaCl powder was ground by a ball mill to obtain NaCl powder having a particle size of 20 μm. Weighing the Metal precursor Fe (acac)3And Pt (acac)2Adding the powder (the molar ratio is 1) and a low-boiling point solvent into a wide-mouth bottle, wherein the low-boiling point solvent is n-hexane, and the ratio of the metal precursor mixed powder to the low-boiling point solvent is 1: 400. Firstly, get throughHeating and stirring the mixture by a mechanical stirring heating sleeve at the stirring speed of 1000 revolutions per minute, fully dissolving the metal precursor mixed powder in a low-boiling-point solvent, and heating the mixture for 24min at 70 ℃ to uniformly dissolve the metal salt precursor; adding NaCl powder with the mass being 100 times of that of the metal precursor, continuously heating and stirring at the same stirring speed, and heating at 90 ℃ for 60min to dissolve and uniformly disperse the NaCl powder to form a dissolved solution; and continuously heating at 90 ℃, continuously volatilizing the low-boiling-point solvent in the solution in the heating process, separating out partial NaCl, taking the NaCl as a heterogeneous nucleation medium, uniformly nucleating the NaCl surface firstly separated out by the metal precursor until heating for 40min, completely volatilizing the low-boiling-point solvent, completely separating out the NaCl and the metal precursor, and obtaining the mixed powder of which the NaCl surface is uniformly covered with the metal precursor.
The mixed powder was placed in a quartz crucible and placed in a tube-type vacuum heat treatment furnace using 95% Ar + 5% H2And (4) washing gas in a reducing atmosphere, and heating to 700 ℃ under the atmosphere condition for annealing for 60 min. Then cooling the annealed mixed powder to room temperature, taking a mixed solution of deionized water A and absolute ethyl alcohol A with the volume ratio of 1:1, and dissolving and dispersing the annealed mixed powder; wherein, according to the proportion, the mixed powder, the mixed solution of deionized water A and absolute ethyl alcohol A are 1: 60 after annealing; after dissolving and dispersing, centrifuging at 8000rpm at a high speed for 10min to remove NaCl, pouring out the supernatant centrifugate, adding absolute ethyl alcohol B for dissolving and dispersing, wherein the mixed powder after annealing and the absolute ethyl alcohol B are 1: 30, adding deionized water B with the same volume ratio with the absolute ethyl alcohol B, centrifuging again, the centrifugation speed is 6000rpm, the centrifugation time is 10min, pouring out the supernatant centrifugate, and repeating: adding absolute ethyl alcohol B for dissolving and dispersing, and carrying out centrifugal separation on deionized water B for 3 times to obtain fct-FePt nanoparticles, and dispersing the fct-FePt nanoparticles in n-hexane for storage. The magnetic property of the nanoparticles was determined by a comprehensive Physical Properties Measurement System (PPMS), and the coercivity was 2.4T, as shown in fig. 1. The phase structure of the sample was measured by X-ray diffractometry to contain fct characteristic peaks (110), (001), and (002), as shown in fig. 2. The sample particles of the nanoparticles observed by the field emission transmission electron microscope have uniform appearance and good dispersibilityAs shown in FIG. 3, the average size was 7.5nm, and the particle size distribution is shown in FIG. 4.
Example 2:
first, NaCl powder was ground by a ball mill to obtain NaCl powder having a particle size of 25 μm. Weighing the Metal precursor Fe (acac)3And Pt (acac)2(the molar ratio is 0.8), adding the mixed powder and a low-boiling point solvent into a wide-mouth bottle, wherein the low-boiling point solvent is a mixed solution of ethanol and ethyl acetate in the equal volume ratio, and the ratio of the metal precursor mixed powder to the low-boiling point solvent is 1: 500. Firstly, heating and stirring through a mechanical stirring heating sleeve, wherein the stirring speed is 1000 revolutions per minute, fully dissolving metal precursor mixed powder in a low-boiling-point solvent, heating for 20min at 75 ℃, adding NaCl powder with the mass being 400 times of that of the metal precursor after the metal salt precursor is uniformly dissolved, continuously stirring at the same stirring speed, and heating for 50min at 100 ℃ to ensure that the NaCl powder is uniformly dissolved and dispersed to form a dissolved solution; and continuously heating at 100 ℃, continuously volatilizing the low-boiling-point solvent in the solution in the heating process, separating out partial NaCl, taking the NaCl as a heterogeneous nucleation medium, uniformly nucleating the NaCl surface firstly separated out by the metal precursor until heating for 30min, completely volatilizing the low-boiling-point solvent, completely separating out the NaCl and the metal precursor, and obtaining the mixed powder of which the NaCl surface is uniformly covered with the metal precursor.
The mixed powder was placed in a quartz crucible and placed in a tube-type vacuum heat treatment furnace using 95% Ar + 5% H2And (4) washing gas in a reducing atmosphere, and heating to 750 ℃ under the atmosphere condition for annealing for 60 min. Then cooling the annealed mixed powder to room temperature, taking a mixed solution of deionized water A and absolute ethyl alcohol A with the volume ratio of 1:1, and dissolving and dispersing the annealed mixed powder; wherein, according to the proportion, the mixed powder, the mixed solution of deionized water A and absolute ethyl alcohol A are 1: 100 after annealing; dissolving and dispersing, centrifuging at high speed of 7000rpm for 8min, removing NaCl, pouring off supernatant centrifugate, adding anhydrous ethanol B for dissolving and dispersing, annealing, mixing powder and anhydrous ethanol B at ratio of 1: 30, adding deionized water B at equal volume ratio to anhydrous ethanol B, centrifuging again, and transferring to rotary centrifugeAt 6000rpm, centrifuge time 10min, pour off the supernatant, repeat: adding absolute ethyl alcohol B for dissolving and dispersing, and carrying out centrifugal separation on deionized water B for 4 times to prepare fct-FePt nano particles which are dispersed in normal hexane for storage. The magnetic property of the nano-particles is determined by a comprehensive Physical Property Measurement System (PPMS), and the coercive force is 2.2T as shown in the attached figure 5. The phase structure of the sample measured by the X-ray diffractometer contains fct characteristic peaks (110), (001) and (002) as shown in FIG. 6. A field emission transmission electron microscope is used for observing the sample particles of the nanoparticles, the morphology is uniform, the dispersity is better as shown in figure 7, the average size is 6.1nm, and the particle size distribution diagram is shown in figure 8.
Example 3:
first, NaCl powder was ground by a ball mill to obtain NaCl powder having a particle size of 500 nm. Weighing the Metal precursor Fe (acac)3And Pt (acac)2(the molar ratio is 1.2) and a low-boiling point solvent are added into a wide-mouth bottle, wherein the low-boiling point solvent is ethanol, and the ratio of the metal precursor mixed powder to the low-boiling point solvent is 1: 300. Firstly, heating and stirring through a mechanical stirring heating sleeve, wherein the stirring speed is 1000 revolutions per minute, fully dissolving metal precursor mixed powder in a low-boiling-point solvent, heating for 15min at 85 ℃, adding NaCl powder with the mass being 50 times of that of a metal precursor after the metal salt precursor is uniformly dissolved, continuously stirring at the same stirring speed, and heating for 40min at 120 ℃ to ensure that the NaCl powder is uniformly dissolved and dispersed to form a dissolved solution; and continuously heating at 120 ℃, continuously volatilizing the low-boiling-point solvent in the solution in the heating process, separating out partial NaCl, taking the NaCl as a heterogeneous nucleation medium, uniformly nucleating the NaCl surface firstly separated out by the metal precursor until heating for 20min, completely volatilizing the low-boiling-point solvent, completely separating out the NaCl and the metal precursor, and obtaining the mixed powder of which the NaCl surface is uniformly covered with the metal precursor.
The mixed powder was placed in a quartz crucible and placed in a tube-type vacuum heat treatment furnace using 95% Ar + 5% H2And (4) washing gas in a reducing atmosphere, and heating to 650 ℃ under the atmosphere condition for annealing for 30 min. Then cooling the annealed mixed powder to room temperature, and taking deionized water A and anhydrous water in a volume ratio of 1:1The mixed solution of the ethanol A is used for dissolving and dispersing the mixed powder after annealing; wherein, according to the proportion, the mixed powder, the mixed solution of deionized water A and absolute ethyl alcohol A are 1: 80 after annealing; after dissolving and dispersing, centrifuging at 6000rpm at high speed for 5min, removing NaCl, pouring out supernatant centrifugate, adding absolute ethyl alcohol B for dissolving and dispersing, wherein the mixed powder of the annealed absolute ethyl alcohol B is 1: 50, adding deionized water B with the same volume ratio with the absolute ethyl alcohol B, centrifuging again, the centrifugation speed is 6000rpm, the centrifugation time is 10min, pouring out the supernatant centrifugate, and repeating: adding absolute ethyl alcohol B for dissolving and dispersing, and carrying out centrifugal separation on deionized water B for 5 times to prepare fct-FePt nano particles which are dispersed in n-hexane for storage. The magnetic property of the nano-particles is determined by a comprehensive Physical Property Measurement System (PPMS), and the coercive force is 2.3T as shown in the attached figure 9. The phase structure of the sample measured by the X-ray diffractometer contains fct characteristic peaks (110), (001) and (002) as shown in FIG. 10. The average particle size of the sample of the nanoparticles was 8.7nm as observed by a field emission transmission electron microscope.
Example 4:
first, NaCl powder was ground by a ball mill to obtain NaCl powder having a particle size of 500. mu.m. Weighing the Metal precursor Fe (acac)3And Pt (acac)2(the molar ratio is 0.5) and a low-boiling point solvent are added into a wide-mouth bottle, the low-boiling point solvent is ethyl acetate, and the ratio of the metal precursor mixed powder to the low-boiling point solvent is 1: 500. Firstly, heating and stirring through a mechanical stirring heating sleeve, wherein the stirring speed is 1000 revolutions per minute, fully dissolving metal precursor mixed powder in a low-boiling-point solvent, heating for 20min at 75 ℃, adding NaCl powder with the mass being 400 times of that of the metal precursor after the metal salt precursor is uniformly dissolved, continuously stirring at the same stirring speed, and heating for 55min at 100 ℃ to ensure that the NaCl powder is uniformly dissolved and dispersed to form a dissolved solution; heating at 100 deg.C, continuously volatilizing low boiling point solvent in the solution during the heating process, separating out partial NaCl, taking NaCl as heterogeneous nucleation medium, uniformly nucleating the NaCl on the NaCl surface previously separated out by the metal precursor, heating for 35min, completely volatilizing low boiling point solvent, completely separating out NaCl and metal precursor, and obtaining NaThe Cl surface was uniformly covered with the mixed powder of the metal precursor.
The mixed powder was placed in a quartz crucible and placed in a tube-type vacuum heat treatment furnace using 95% Ar + 5% H2And (4) washing gas in a reducing atmosphere, and heating to 750 ℃ under the atmosphere condition for annealing for 150 min. Then cooling the annealed mixed powder to room temperature, taking a mixed solution of deionized water A and absolute ethyl alcohol A with the volume ratio of 1:1, and dissolving and dispersing the annealed mixed powder; wherein, according to the proportion, the mixed powder, the mixed solution of deionized water A and absolute ethyl alcohol A are 1: 100 after annealing; after dissolving and dispersing, centrifuging at a high speed of 10000rpm for 8min, removing NaCl, pouring out supernatant centrifugate, adding absolute ethyl alcohol B for dissolving and dispersing, wherein the mixed powder after annealing and the absolute ethyl alcohol B are i: 40, adding deionized water B with the same volume ratio with the absolute ethyl alcohol B, performing centrifugal separation again, the centrifugal speed is 8000rpm, the centrifugal time is 8min, pouring out the supernatant centrifugate, and repeating: adding absolute ethyl alcohol B for dissolving and dispersing, and carrying out centrifugal separation on deionized water B for 3 times to obtain fct-FePt nano particles which are dispersed in n-hexane for storage. The coercive force of the nano-particles is 2.1T determined by a comprehensive Physical Property Measurement System (PPMS), and the average size of the sample particles of the nano-particles is 15nm observed by a field emission transmission electron microscope.
Example 5:
first, NaCl powder was ground by a ball mill to obtain NaCl powder having a particle size of 400 μm. Weighing the Metal precursor Fe (acac)3And Pt (acac)2(the molar ratio is 0.3) and a low-boiling point solvent are added into the wide-mouth bottle, the low-boiling point solvent is petroleum ether, and the ratio of the metal precursor mixed powder to the low-boiling point solvent is 1: 400. Firstly, heating and stirring through a mechanical stirring heating sleeve, wherein the stirring speed is 1500 rpm, fully dissolving metal precursor mixed powder in a low-boiling-point solvent, heating for 28min at 60 ℃, adding NaCl powder with the mass being 300 times of that of a metal precursor after the metal salt precursor is uniformly dissolved, continuously stirring at the same stirring speed, and heating for 80min at 80 ℃ to dissolve and uniformly disperse the NaCl powder to form a dissolved solution; heating at 80 deg.C, wherein the solution has low boiling pointAnd continuously volatilizing the point solvent, separating out partial NaCl serving as a heterogeneous nucleation medium, uniformly nucleating the NaCl surface on which the metal precursor is firstly separated out until heating for 60min, completely volatilizing the low-boiling point solvent, completely separating out NaCl and the metal precursor, and obtaining mixed powder of which the NaCl surface is uniformly covered with the metal precursor.
The mixed powder was placed in a quartz crucible and placed in a tube-type vacuum heat treatment furnace using 95% Ar + 5% H2And (4) washing gas in a reducing atmosphere, and heating to 700 ℃ under the atmosphere condition for annealing for 60 min. Then cooling the annealed mixed powder to room temperature, taking a mixed solution of deionized water A and absolute ethyl alcohol A with the volume ratio of 1:1, and dissolving and dispersing the annealed mixed powder; wherein, according to the proportion, the mixed powder, the mixed solution of deionized water A and absolute ethyl alcohol A are 1: 80 after annealing; after dissolving and dispersing, centrifuging at 8000rpm at high speed for 10min, removing NaCl, pouring off the supernatant centrifugate, adding absolute ethyl alcohol B for dissolving and dispersing, wherein the ratio of the mixed powder to the absolute ethyl alcohol B is 1: 40 after annealing, adding deionized water B with the same volume ratio with the absolute ethyl alcohol B, centrifuging again at 8000rpm for 8min, pouring off the supernatant centrifugate, and repeating: adding absolute ethyl alcohol B for dissolving and dispersing, and carrying out centrifugal separation on deionized water B for 3 times to prepare fct-FePt nano particles which are dispersed in n-hexane for storage. The coercive force of the nano-particles is 2.2T determined by a comprehensive Physical Property Measurement System (PPMS), and the average size of the sample particles of the nano-particles is 6.5nm observed by a field emission transmission electron microscope.
Example 6:
first, NaCl powder was ground by a ball mill to obtain NaCl powder having a particle size of 10 μm. Weighing the Metal precursor Fe (acac)3And Pt (acac)2(the molar ratio is 0.5) and a low-boiling point solvent are added into a wide-mouth bottle, the low-boiling point solvent is a mixed solution of ethanol and petroleum ether in the same volume ratio, and the ratio of the metal precursor mixed powder to the low-boiling point solvent is 1: 500. Firstly, heating and stirring the mixture by a mechanical stirring heating sleeve at the stirring speed of 1500 rpm, fully dissolving the metal precursor mixed powder in a low-boiling-point solvent, heating the mixture for 15min at the temperature of 85 ℃, and obtaining metal saltAfter the precursor is dissolved uniformly, adding NaCl powder with the mass being 400 times that of the metal precursor, continuously stirring at the same stirring speed, and heating at 120 ℃ for 40min to dissolve and uniformly disperse the NaCl powder to form a dissolved solution; and continuously heating at 120 ℃, continuously volatilizing the low-boiling-point solvent in the solution in the heating process, separating out partial NaCl, taking the NaCl as a heterogeneous nucleation medium, uniformly nucleating the NaCl surface firstly separated out by the metal precursor until heating for 20min, completely volatilizing the low-boiling-point solvent, completely separating out the NaCl and the metal precursor, and obtaining the mixed powder of which the NaCl surface is uniformly covered with the metal precursor.
The mixed powder was placed in a quartz crucible and placed in a tube-type vacuum heat treatment furnace using 95% Ar + 5% H2And (4) washing gas in the reducing atmosphere, and heating to 550 ℃ under the atmosphere condition for annealing for 120 min. Then cooling the annealed mixed powder to room temperature, taking a mixed solution of deionized water A and absolute ethyl alcohol A with the volume ratio of 1:1, and dissolving and dispersing the annealed mixed powder; wherein, according to the proportion, the mixed powder, the mixed solution of deionized water A and absolute ethyl alcohol A are 1: 60 after annealing; after dissolving and dispersing, centrifuging at 6000rpm at high speed for 6min, removing NaCl, pouring off the supernatant centrifugate, adding absolute ethyl alcohol B for dissolving and dispersing, wherein the mixed powder of the annealed absolute ethyl alcohol B is 1: 50, adding deionized water B with the same volume ratio with the absolute ethyl alcohol B, centrifuging again at 8000rpm for 8min, pouring off the supernatant centrifugate, and repeating: adding absolute ethyl alcohol B for dissolving and dispersing, and carrying out centrifugal separation on deionized water B for 3 times to prepare fct-FePt nano particles which are dispersed in n-hexane for storage. The coercive force of the nano-particles is 2.2T measured by a comprehensive Physical Property Measurement System (PPMS), and the average size of the sample particles of the nano-particles is 4.0nm observed by a field emission transmission electron microscope.
Example 7:
KCl powder was first ground by means of a ball mill to obtain KCl powder having a particle size of 100 μm. Weighing the Metal precursor Fe (acac)3And Pt (acac)2(the molar ratio is 2) and a low-boiling point solvent are added into the wide-mouth bottle, wherein the low-boiling point solvent is petroleum ether and acetic acidThe volume ratio of the ethyl ester to the mixed solution is 1: 300, and the ratio of the metal precursor mixed powder to the low-boiling-point solvent is 1: 300. Firstly, heating and stirring through a mechanical stirring heating sleeve, wherein the stirring speed is 1500 rpm, fully dissolving metal precursor mixed powder in a low-boiling-point solvent, heating for 30min at 50 ℃, adding KCl powder with the mass 50 times that of the metal precursor after the metal salt precursor is uniformly dissolved, continuously stirring at the same stirring speed, and heating for 100min at 50 ℃ to dissolve and uniformly disperse the KCl powder to form a dissolved solution; and continuously heating at 50 ℃, wherein the low-boiling-point solvent in the dissolving solution is continuously volatilized in the heating process, partial KCl is separated out, the KCl is used as a heterogeneous nucleation medium, the KCl surface previously separated out by the metal precursor is uniformly nucleated, the low-boiling-point solvent is completely volatilized until heating is carried out for 50min, the KCl and the metal precursor are completely separated out, and the mixed powder with the KCl surface uniformly covered with the metal precursor is obtained.
The mixed powder was placed in a quartz crucible and placed in a tube-type vacuum heat treatment furnace using 95% Ar + 5% H2And (4) washing gas in a reducing atmosphere, and heating to 700 ℃ under the atmosphere condition for annealing for 60 min. Then cooling the annealed mixed powder to room temperature, taking a mixed solution of deionized water A and absolute ethyl alcohol A with the volume ratio of 1:1, and dissolving and dispersing the annealed mixed powder; wherein, according to the proportion, the mixed powder, the mixed solution of deionized water A and absolute ethyl alcohol A are 1: 80 after annealing; after dissolving and dispersing, centrifuging at 8000rpm at high speed for 8min to remove KCl, pouring off the supernatant, adding anhydrous ethanol B for dissolving and dispersing, wherein the ratio of the mixed powder to the anhydrous ethanol B is 1: 40 after annealing, adding deionized water B in the same volume ratio with the anhydrous ethanol B, centrifuging again at 8000rpm for 8min, pouring off the supernatant, and repeating the steps: adding absolute ethyl alcohol B for dissolving and dispersing, and carrying out centrifugal separation on deionized water B for 3 times to prepare fct-FePt nano particles which are dispersed in n-hexane for storage. The coercive force of the nano-particles is 2.3T measured by a comprehensive Physical Property Measurement System (PPMS), and the average size of the sample particles of the nano-particles is 8.6nm observed by a field emission transmission electron microscope.
Example 8:
KCl powder was first ground by means of a ball mill to obtain KCl powder having a particle size of 150 μm. Weighing the Metal precursor Fe (acac)3And Pt (acac)2(the molar ratio is 1) and a low-boiling point solvent are added into a wide-mouth bottle, the low-boiling point solvent is a mixed solution of n-hexane and ethanol in the same volume ratio, and the ratio of the metal precursor mixed powder to the low-boiling point solvent is 1: 400. Firstly, heating and stirring through a mechanical stirring heating sleeve, wherein the stirring speed is 2000 r/min, fully dissolving metal precursor mixed powder in a low-boiling-point solvent, heating for 20min at 75 ℃, adding KCl powder with the mass being 200 times of that of the metal precursor after the metal salt precursor is uniformly dissolved, continuously stirring at the same stirring speed, and heating for 60min at 100 ℃ to ensure that the KCl powder is dissolved and uniformly dispersed to form a dissolved solution; and continuously heating at 100 ℃, continuously volatilizing the low-boiling-point solvent in the dissolving solution in the heating process, precipitating partial KCl, taking the KCl as a heterogeneous nucleation medium, uniformly nucleating the KCl surface previously precipitated by the metal precursor until heating for 40min, completely volatilizing the low-boiling-point solvent, completely precipitating the KCl and the metal precursor, and obtaining the mixed powder with the KCl surface uniformly covered with the metal precursor.
The mixed powder was placed in a quartz crucible and placed in a tube-type vacuum heat treatment furnace using 95% Ar + 5% H2And (4) washing gas in a reducing atmosphere, and heating to 600 ℃ under the atmosphere condition for annealing for 60 min. Then cooling the annealed mixed powder to room temperature, taking a mixed solution of deionized water A and absolute ethyl alcohol A with the volume ratio of 1:1, and dissolving and dispersing the annealed mixed powder; wherein, according to the proportion, the mixed powder, the mixed solution of deionized water A and absolute ethyl alcohol A are 1: 60 after annealing; after dissolving and dispersing, centrifuging at 8000rpm at a high speed for 8min to remove KCl, pouring out supernatant centrifugate, adding absolute ethyl alcohol B for dissolving and dispersing, wherein the mixed powder of the annealed absolute ethyl alcohol B is 1: 50, adding deionized water B with the same volume ratio with the absolute ethyl alcohol B, centrifuging again, the centrifugation speed is 10000rpm, the centrifugation time is 5min, pouring out the supernatant centrifugate, and repeating: adding absolute ethyl alcohol B for dissolving and dispersing, and performing centrifugal separation on deionized water B for 3 times to obtain fct-FePt nanoThe rice grains are dispersed in n-hexane for storage. The coercive force of the nano-particles is 2.1T determined by a comprehensive Physical Property Measurement System (PPMS), and the average size of the sample particles of the nano-particles is 13.0nm observed by a field emission transmission electron microscope.
Example 9:
KCl powder was first ground by means of a ball mill to obtain KCl powder having a particle size of 50 μm. Weighing the Metal precursor Fe (acac)3And Pt (acac)2(the molar ratio is 0.8) and a low-boiling point solvent are added into a wide-mouth bottle, the low-boiling point solvent is a mixed solution of n-hexane and ethyl acetate in the same volume ratio, and the ratio of the metal precursor mixed powder to the low-boiling point solvent is 1: 350. Firstly, heating and stirring through a mechanical stirring heating sleeve, wherein the stirring speed is 2000 r/min, fully dissolving metal precursor mixed powder in a low-boiling-point solvent, heating for 15min at 85 ℃, adding KCl powder with the mass being 100 times of that of the metal precursor after the metal salt precursor is uniformly dissolved, continuously stirring at the same stirring speed, and heating for 50min at 120 ℃ to ensure that the KCl powder is dissolved and uniformly dispersed to form a dissolved solution; and continuously heating at 120 ℃, wherein in the heating process, the low-boiling-point solvent in the dissolving solution is continuously volatilized, partial KCl is separated out, the KCl is used as a heterogeneous nucleation medium, the KCl surface previously separated out by the metal precursor is uniformly nucleated until heating is carried out for 30min, the low-boiling-point solvent is completely volatilized, the KCl and the metal precursor are completely separated out, and the mixed powder with the KCl surface uniformly covered with the metal precursor is obtained.
The mixed powder was placed in a quartz crucible and placed in a tube-type vacuum heat treatment furnace using 95% Ar + 5% H2And (4) washing gas in a reducing atmosphere, and heating to 700 ℃ under the atmosphere condition for annealing for 150 min. Then cooling the annealed mixed powder to room temperature, taking a mixed solution of deionized water A and absolute ethyl alcohol A with the volume ratio of 1:1, and dissolving and dispersing the annealed mixed powder; wherein, according to the proportion, the mixed powder, the mixed solution of deionized water A and absolute ethyl alcohol A are 1: 100 after annealing; dissolving and dispersing, centrifuging at high speed of 7000rpm for 8min, removing KCl, pouring off supernatant centrifugate, adding anhydrous ethanol B, dissolving and dispersing, annealing, and mixing with powder and anhydrous ethanol B1: 50, adding deionized water B with the same volume ratio as the absolute ethyl alcohol B, performing centrifugal separation again, wherein the centrifugal speed is 10000rpm, the centrifugal time is 5min, pouring out the upper layer of centrifugal liquid, and repeating: adding absolute ethyl alcohol B for dissolving and dispersing, and carrying out centrifugal separation on deionized water B for 3 times to prepare fct-FePt nano particles which are dispersed in n-hexane for storage. The coercive force of the nano-particles is 2.4T determined by a comprehensive Physical Property Measurement System (PPMS), and the average size of the sample particles of the nano-particles is 14.4nm observed by a field emission transmission electron microscope.
Example 10:
KCl powder was first ground by means of a ball mill to obtain KCl powder having a particle size of 300. mu.m. Weighing the Metal precursor Fe (acac)3And Pt (acac)2(the molar ratio is 1.5) and a low-boiling point solvent are added into a wide-mouth bottle, the low-boiling point solvent is a mixed solution of n-hexane and petroleum ether in the same volume ratio, and the ratio of the metal precursor mixed powder to the low-boiling point solvent is 1: 400. Firstly, heating and stirring by a mechanical stirring heating sleeve at the stirring speed of 2500 rpm, fully dissolving metal precursor mixed powder in a low-boiling-point solvent, heating at the temperature of 100 ℃ for 10min, adding KCl powder with the mass being 200 times of that of the metal precursor after the metal salt precursor is uniformly dissolved, continuously stirring at the same stirring speed of 150 ℃ for 40min, and dissolving and uniformly dispersing the KCl powder to form a dissolved solution; and (2) continuously heating at 150 ℃, wherein in the heating process, the low-boiling-point solvent in the dissolving solution is continuously volatilized, partial KCl is separated out, the KCl is used as a heterogeneous nucleation medium, the KCl surface previously separated out by the metal precursor is uniformly nucleated until heating is carried out for 20min, the low-boiling-point solvent is completely volatilized, the KCl and the metal precursor are completely separated out, and the mixed powder with the KCl surface uniformly covered with the metal precursor is obtained.
The mixed powder was placed in a quartz crucible and placed in a tube-type vacuum heat treatment furnace using 95% Ar + 5% H2And (4) washing gas in a reducing atmosphere, and heating to 750 ℃ under the atmosphere condition for annealing for 30 min. Then cooling the annealed mixed powder to room temperature, taking a mixed solution of deionized water A and absolute ethyl alcohol A with the volume ratio of 1:1, and dissolving and dispersing the annealed mixed powder; wherein, according to the proportion, the step ofMixing the powder after fire with a mixed solution of deionized water A and absolute ethyl alcohol A at a ratio of 1: 60; after dissolving and dispersing, centrifuging at a high speed of 10000rpm for 8min to remove KCl, pouring out supernatant centrifugate, adding absolute ethyl alcohol B for dissolving and dispersing, wherein the mixed powder of the annealed absolute ethyl alcohol B is 1: 30, adding deionized water B with the same volume ratio with the absolute ethyl alcohol B, performing centrifugal separation again, centrifuging at a rotating speed of 10000rpm for 5min, pouring out the supernatant centrifugate, and repeating: adding absolute ethyl alcohol B for dissolving and dispersing, and carrying out centrifugal separation on deionized water B for 3 times to prepare fct-FePt nano particles which are dispersed in n-hexane for storage. The coercive force of the nano-particles is 2.2T determined by a comprehensive Physical Property Measurement System (PPMS), and the average size of the sample particles of the nano-particles is 13.6nm observed by a field emission transmission electron microscope.
The embodiment shows that the fct-FePt nanoparticles are synthesized by one step by adopting the chemical solid phase method, so that the high magnetic property and the high order degree are obtained, the nanoparticles are uniform in appearance and good in dispersity.

Claims (5)

1. A chemical method for synthesizing fct-FePt nanoparticles by liquid-phase assisted solid-phase sintering is characterized by comprising the following steps:
step 1: pretreatment of precursors
(1) Grinding NaCl particles by ball milling to obtain NaCl powder with the particle size of 500 nm-500 mu m for later use;
(2) weighing a metal precursor powder comprising the metal precursor Fe (acac)3Powder and Metal precursor Pt (acac)2Powder with the molar ratio of 0.3-0.8 for later use;
step 2: mixing of precursors
(1) According to the proportion, the metal precursor powder: the low-boiling-point solvent =1 (300-500), the unit g: ml, add both into container, wherein, the said low-boiling-point solvent is petroleum ether, or the mixed solvent of ethanol and ethyl acetate, or the mixed solvent of ethanol and n-hexane, wherein, in the case of the mixed solvent of ethanol and ethyl acetate, the volume ratio of both is 1:1, in the case of the mixed solvent of ethanol and n-hexane, the volume ratio of both is 1: 1;
(2) uniformly dissolving metal precursor powder in a low-boiling-point solvent by heating and stirring, wherein the heating temperature is 50-100 ℃ and the time is 10-30 min;
(3) adding NaCl powder with the mass being 300-400 times of that of the metal precursor powder into the dissolved metal salt precursor, heating and continuously stirring to sequentially dissolve the NaCl powder, volatilizing the low-boiling-point solvent, and separating the NaCl and the metal precursor to finally form metal precursor and NaCl mixed powder, wherein the heating temperature is 50-150 ℃, the heating time is 60-150 min, and the specific change process of heating for 60-150 min at 50-150 ℃ after adding the NaCl powder is as follows: heating at 50-150 ℃ for 40-100 min to dissolve the NaCl powder to form a dissolved solution; continuously heating at 50-150 ℃ for 20-50 min to volatilize the low-boiling-point solvent, and separating out NaCl and the metal precursor to form mixed powder of the metal precursor and the NaCl;
and step 3: sintering of precursor
Putting the mixed powder of the metal precursor and NaCl into a crucible, putting the crucible into a vacuum heat treatment furnace, annealing in an oxygen-free atmosphere at the annealing temperature of 550-750 ℃, and keeping the temperature for 60-120 min to form annealed mixed powder, wherein the oxygen-free atmosphere is 95% Ar + 5% H2Mixed gas atmosphere;
and 4, step 4: NaCl removal
(1) Cooling the annealed mixed powder to room temperature, taking a mixed solution of deionized water and absolute ethyl alcohol, dissolving and dispersing the annealed mixed powder, centrifuging at the speed of 6000-10000 rpm for 5-10 min, removing NaCl, and pouring out the upper-layer centrifugate;
(2) and adding absolute ethyl alcohol for dissolving and dispersing, wherein the addition amount of the absolute ethyl alcohol is in proportion, and the powder is mixed after annealing: absolute ethyl alcohol =1 (30-50), unit is g: ml;
(3) adding deionized water with the same ratio as the absolute ethyl alcohol in the step (2), performing centrifugal separation again, and pouring off the upper layer of the centrifugal liquid; wherein the centrifugal rotating speed is 6000-10000 rpm, and the centrifugal time is 5-10 min;
(4) repeating the steps (2) to (3) for 3-5 times to prepare the fct-FePt nano particle.
2. The chemical method for synthesizing fct-FePt nanoparticles through liquid-phase assisted solid-phase sintering as claimed in claim 1, wherein in the step 2(2), the stirring speed is 1000-2500 rpm.
3. The chemical method for synthesizing fct-FePt nanoparticles through liquid-phase assisted solid-phase sintering as claimed in claim 1, wherein in the step 3, the mixed powder is pre-treated with 95% Ar + 5% H2And after the mixed gas is subjected to gas scrubbing, annealing treatment is performed.
4. The chemical method for synthesizing fct-FePt nanoparticles through liquid-phase assisted solid-phase sintering as claimed in claim 1, wherein in step 4(1), the deionized water and the absolute ethyl alcohol are mixed in equal volume in the mixed solution of the deionized water and the absolute ethyl alcohol.
5. The chemical method for synthesizing fct-FePt nanoparticles through liquid-phase assisted solid-phase sintering according to claim 1, wherein in step 4(1), the mixture ratio of the annealed mixed powder to the mixed solution of deionized water and absolute ethyl alcohol is 1: (60-100) in unit g: ml.
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