CN114643365B - Interface induction synthesis of ordered L1 0 Method for structuring permanent magnetic nanoparticles - Google Patents

Interface induction synthesis of ordered L1 0 Method for structuring permanent magnetic nanoparticles Download PDF

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CN114643365B
CN114643365B CN202210309658.5A CN202210309658A CN114643365B CN 114643365 B CN114643365 B CN 114643365B CN 202210309658 A CN202210309658 A CN 202210309658A CN 114643365 B CN114643365 B CN 114643365B
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seed crystal
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CN114643365A (en
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裴文利
赵东
白羽丰
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Northeastern University China
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
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Abstract

The invention belongs to the technical field of magnetic nano materials, and particularly relates to interface-induced synthesis of ordered L1 0 Method for structuring permanent magnetic nanoparticles. Firstly, adding a certain proportion of a seed crystal core metal precursor, a surfactant and a reducing agent into a solvent, heating the mixed solution to a certain temperature, preserving the temperature, then cooling to room temperature, and reducing the seed crystal core metal precursor to form a seed crystal core. Then adding a certain proportion of shell metal precursor, slowly heating to a certain temperature, then cooling to room temperature after heat preservation, reducing the shell metal precursor by a reducing agent, and growing under the induction of the interface of the seed crystal core to form L1 0 The shell of the structure is finally centrifugally cleaned to obtain ordered L1 0 The structure of the black powder of the permanent magnetic nano particles. Monodisperse high coercivity ordered L1 synthesis by ordered metal seed interface induction 0 The structure nano material has lower synthesis temperature and simple operation.

Description

Interface induction synthesis of ordered L1 0 Method for structuring permanent-magnet nanoparticles
The technical field is as follows:
the invention belongs to the technical field of magnetic nano materials, and particularly relates to interface-induced synthesis of ordered L1 0 A method of structuring permanent magnetic nanoparticles.
Background art:
some transition group intermetallic compounds have abundant phase structure and diverse intrinsic magnetism, such as: feCo and FeNi generally have A2 and B2 structures, show high saturation magnetization and low coercive force and are good soft magnetic materials; common MnAl and MnGa have a tau-phase structure and exhibit ferrimagnetism. If these intermetallic compounds can be made chemically ordered L1 0 Tetragonal phase, L1 0 -FeCo、L1 0 -FeNi、L1 0 -MnAl、L1 0 MnGa, the crystal structure of which has high symmetry, presents large magnetocrystalline anisotropy, high Curie temperature and high coercivity, is an excellent permanent magnetic material, the intermetallic compound does not contain rare earth elements, has low cost and wide application prospectThe alloy is made into nano particles, and has important application value in the aspects of high-density magnetic storage, electrochemical catalysis, micro-nano devices, biomedicine and the like.
However, it is difficult to obtain ordered tetragonal phases with high magnetocrystalline anisotropy with the usual direct preparation of FeCo, feNi, mnAl, mnGa nanoparticles, because the process window for obtaining this structural alloy is narrow, for example: l1 0 MnAl is a metastable phase formed by quenching and subsequent annealing (usually at 500℃.) of a Mn-rich epsilon phase, and is susceptible to decomposition into a non-magnetic phase. L1 0 the-FeNi phase diffuses slowly at 593K of order-disorder transition temperature, L1 0 FeNi is only present in meteorites that have cooled at very low cooling rates over billions of years. L1 0 FeCo has a ratio L1 0 FeNi more desirable magnetic properties, but L1 due to limited knowledge of the thermodynamics of phase formation 0 The preparation of FeCo remains to be studied and, to date, L1 has not been successfully synthesized in any laboratory 0 -a FeCo phase. However, the existing chemical synthesis method generally directly reduces the metal precursor, the atoms form FeCo, feNi, mnAl or MnGa alloy nuclei in a certain reaction environment, and then grow into FeCo, feNi, mnAl or MnGa nanoparticles, and because the metal atoms are randomly stacked in the growth process, the metal atoms are difficult to control to form an ordered structure, the L1 is difficult to prepare by the common process 0 FeCo, feNi, mnAl and MnGa nano materials with the structure. How to induce atoms to grow orderly in the nucleation growth process to prepare L1 with good controllability and high order degree 0 FeCo, feNi, mnAl and MnGa nano particles are the bottleneck problem in the field.
The invention content is as follows:
the invention aims to provide an interface induced synthesis ordered L1 0 The method for structuring permanent magnetic nano particles is the ordered L1 0 The structural permanent magnetic nanoparticles refer to transition group intermetallic compound nanoparticles, and particularly form ordered L1 difficultly by a conventional method 0 The intermetallic compound of the structure specifically includes an intermetallic compound permanent magnetic nanoparticle such as FeCo, feNi, mnAl, mnGa, and the like.
The idea of the invention patent is as follows:
L1 0 the structural nano particles of FeCo, feNi, mnAl, mnGa and the like are difficult to obtain by direct synthesis, so that the structural nano particles need to be induced to form an ordered structure in the synthesis process. Chemically synthesized nanoparticles are generally carried out in a nucleation growth manner, first forming a crystal nucleus, and then growing into large-sized particles or various nanomaterials. During the growth process, different atoms are generally stacked along the surface of the crystal nucleus, and epitaxial growth along the interface is the main growth mode, so that the structure of the crystal nucleus has inheritance to the synthesized nano particle. If it is to have L1 0 Putting seed crystal of the structure into a reaction system, taking the seed crystal as a mass point of heterogeneous nucleation, stacking the reduced atoms along the surface of the seed crystal core, and when the lattice constant of the seed crystal is close to that of the particle to be synthesized, the lattice matching degree of the seed crystal is higher, the atoms can grow along the original crystal face in an epitaxial way, thereby continuing to grow into ordered L1 0 Structured nanoparticles.
Intermetallic compounds such as AuCu, mnNi, fePt and the like exist stably at lower temperature, are easy to obtain by chemical synthesis, and have lattice lattices and order L1 0 The lattice lattices of FeCo, feNi, mnAl and MnGa have higher matching degree and are easy to form epitaxial growth. Thus L1 can be synthesized first 0 AuCu, mnNi and FePt in the structure are used as crystal seeds, and then the crystal seeds are used as cores, and through interface induction of crystal lattices, ordered L1 can be obtained 0 Permanent magnetic nanoparticles of these transition group intermetallics of structure (e.g., feCo, feNi, mnAl, mnGa, etc., as described above).
The permanent magnetic nanoparticles thus formed have a magnetic permeability of L1 0 The crystal seed of intermetallic compound of AuCu, mnNi, fePt, etc. with structure is used as core and L1 0 Transition intermetallic compounds such as FeCo, feNi, mnAl, mnGa and the like with the structure are taken as shells, and the shape, the order degree and the magnetic property of the product can be controlled by adjusting the proportion of precursors, controlling the chemical components of the product, changing the reaction temperature, the reaction time and the like.
In order to achieve the purpose, the invention adopts an interface to induce and synthesize the ordered L1 0 A method of structuring permanent magnetic nanoparticles. HeadFirstly adding a seed crystal core metal precursor, a surfactant and a reducing agent in a certain proportion into a solvent, heating the mixed solution to a certain temperature, preserving the temperature, then cooling to room temperature, and reducing the seed crystal core metal precursor to form L1 0 The crystal seed core of intermetallic compound of AuCu, mnNi, fePt, etc. Then FeCo, feNi, mnAl or MnGa shell metal precursor with a certain proportion is added, the temperature is slowly raised to a certain temperature, then the heating source is removed after heat preservation, the temperature is cooled to room temperature, the shell metal precursor is reduced by a reducing agent and grows under the induction of an interface of a seed crystal core to form L1 0 FeCo, feNi, mnAl or MnGa shell with the structure is finally centrifugally cleaned to obtain ordered L1 0 The structure of the black powder of the permanent magnetic nano particles.
The method specifically comprises the following steps:
s1: the seed core metal precursor and the reducing agent are weighed.
The seed crystal core metal precursor can form a highly ordered structure L1 0 The metal source mixture of two metals of the metal alloy can be reduced to produce L1 0 Seed core of the structure. Specifically, the intermetallic compound or metal alloy as the seed core may be AuCu, mnNi, fePt, and thus the seed core metal precursor may be a mixture of a gold source and a copper source, a manganese source and a nickel source, or an iron source and a platinum source, and the molar ratio of metal ions in the two metal sources is preferably (0.1 to 1): (0.1-1).
Specifically, in the seed core metal precursor: the gold source is chloroauric acid HAuCl 4 Potassium tetrachloroaurate KAuCl 4 One or more of (a); the copper source is copper acetylacetonate Cu (acac) 2 Copper acetate Cu (Ac) 2 Copper chloride CuCl 2 One or more of (a); the manganese source is manganese acetate Mn (Ac) 2 MnCl, manganese chloride 2 Manganese acetylacetonate Mn (acac) 2 One or more of (a); the nickel source is nickel acetate Ni (Ac) 2 Nickel nitrate Fe (NO) 3 ) 3 Nickel sulfate Fe 2 (SO 4 ) 3 Nickel chloride NiCl 2 Nickel acetylacetonate Ni (acac) 2 One or more of (a); the iron source being chlorineIron FeCl 3 FeNO, iron nitrate 3 Iron (Fe) sulfate 2 (SO 4 ) 3 Fe acetylacetonate (acac) 3 One or more of (a); the platinum source is chloroplatinic acid H 2 PtCl 6 Platinum acetylacetonate Pt (acac) 2 Chloroplatinic acid K 2 PtCl 6 One or more of (a).
The reducing agent is potassium borohydride KBH 4 Sodium borohydride NaBH 4 1, 2-hexadecanediol C 16 H 34 O 2 Lithium aluminum hydride LiAlH, sodium cyanoborohydride CH 3 One or more BNNa. The actual total addition amount of the reducing agent is not less than the theoretical addition amount, and the theoretical addition amount of the reducing agent is the amount capable of reducing all metal ions in the seed crystal core metal precursor and the shell metal precursor into 0-valent metal. Specifically, the ratio of the actual amount of the reducing agent to the theoretical amount may be (1 to 10): 1.
S2: adding the crystal seed core metal precursor into a solvent, carrying out dehydration treatment under the action of a protective atmosphere, and adding a surfactant after the dehydration treatment to form a mixed solution.
Preferably, the solvent is hexadecylamine C 16 H 35 N, trioctylamine C 24 H 51 N, octadecylamine C 18 H 39 N, icosanamine C 20 H 43 N, oleylamine C 18 H 37 One or more of N, and the surfactant is decaalkyl quaternary ammonium bromide C 16 H 38 Br 2 N 2 Lecithin C 42 H 80 NO 8 P, glyceryl monostearate C 21 H 42 O 4 Oleylamine C 18 H 37 N and oleic acid C 18 H 34 O 2 The two substances in the surfactant are mixed, and the two substances in the surfactant are mixed according to the volume ratio (0.1-1): (0.1-1) mixing and adding. The above-mentioned solvent and surfactant can promote more favorable growth of the metal atom generated after the seed core metal precursor is reduced to L1 0 The structure also promotes the metal atoms of the shell metal precursor after being reduced to grow into L1 better under the induction of the crystal lattice interface of the seed crystal core 0 And (5) structure. The solvent isThe growth of the two provides a good platform, and the surfactant can retain the synthesized L1 to the maximum extent 0 The surface activity of the structure and various groups on the surface of the structure provide guarantee for subsequent various applications.
The molar ratio of metal ions to solvent in the seed crystal core metal precursor is 1: (10-30), wherein the molar ratio of the solvent to the surfactant (the surfactant is the total amount of the two substances) is 10: (1.0-5.0).
Preferably, said protective atmosphere is 93% Ar +7% 2 、95％Ar+5％H 2 High purity argon Ar or high purity nitrogen N 2 One of (1) and (b). The method for water removal treatment comprises the following steps: under the action of protective atmosphere, heating to 100-120 ℃ at a heating rate of 1-10 ℃/min, and preserving heat for 30-120 min. The water removal treatment is more beneficial to the function of the surfactant.
S3: and heating the mixed solution to a first reaction temperature, preserving the temperature, carrying out a reaction for generating a seed crystal core, cooling, weighing and adding a shell metal precursor.
In the process of temperature rise and heat preservation, the seed crystal core metal precursor is reduced into 0-valent metal atoms and assembled into an intermetallic compound to form L1 0 Seed core of the structure. It is therefore necessary to ensure that there is a sufficient amount of reducing agent in solution prior to this process, i.e. prior to the reaction that produces the seed cores.
Preferably, the first reaction temperature is 280-360 ℃, the heat preservation time is 30-300 min, and the mixed solution is cooled to 60-120 ℃ after the reaction.
The shell metal precursor is an ordered L1 to be prepared 0 A metal source mixture of two metals of the structured permanent magnetic nanoparticles, such as FeCo, feNi, mnAl or MnGa, and thus in particular the shell metal precursor may be a mixture of an iron source and a cobalt source, an iron source and a nickel source, a manganese source and an aluminum source or a manganese source and a gallium source.
As mentioned previously, these metals are generally difficult to form ordered L1 s 0 Intermetallic compounds or gold nanoparticles of the structure, and in the present invention, under the premise of existence of seed crystal core and interface induction,the difficulty of forming intermetallic compounds of such a structure is greatly reduced.
Preferably, the molar ratio of the two metal ions in the shell metal precursor metal source is (0.2-1): (0.2-1). In the shell metal precursor, the iron source is ferric chloride FeCl 3 Carbonyl iron Fe (CO) 5 Fe acetylacetonate (acac) 3 Iron oleate C 54 H 99 FeO 6 One or more of the above; the cobalt source is cobalt acetylacetonate Co (acac) 2 Octacarbonyldicobalt Co 2 (CO) 8 Cobalt acetate Co (Ac) 2 One or more of the above; the nickel source is nickel acetate Ni (Ac) 2 Nickel nitrate Fe (NO) 3 ) 3 Nickel sulfate Fe 2 (SO 4 ) 3 Nickel chloride NiCl 2 Nickel acetylacetonate Ni (acac) 2 One or more of (a); the manganese source is manganese acetate Mn (Ac) 2 Manganese chloride MnCl 2 Manganese acetylacetonate Mn (acac) 2 One or more of (a); the aluminum source is aluminum chloride AlCl 3 Aluminum acetylacetonate Al (acac) 3 One or more of (a); the gallium source is gallium acetate Ga (Ac) 2 Gallium chloride GaCl 2 Ga acetylacetonate (acac) 2 One or more of (a).
When the shell metal precursor is added into the mixed solution, the molar ratio of the total amount of metal ions in the shell metal precursor to the total amount of metal ions in the seed crystal core metal precursor is (0.4-1): (0.2-1).
S4: heating the mixed solution to a second reaction temperature, preserving heat, carrying out a shell generation reaction, cooling to room temperature, and carrying out centrifugal cleaning on the mixed solution to obtain black powder, namely the ordered L1 0 Structure permanent magnetic nanoparticles.
In the process of temperature rise and heat preservation, the shell metal precursor is reduced into 0-valent metal atoms, and ordered L1 is formed under the induction of the interface of the seed crystal core 0 Structural intermetallic compounds. It is therefore necessary to ensure that a sufficient amount of reducing agent is contained in the mixed solution before the process, i.e. before the reaction to produce the shell.
Preferably, the second reaction temperature is 200-300 ℃, and the heat preservation time is 10-60 min.
Preferably, in the step S3 and the step S4, the temperature of the mixed solution is increased to the reaction temperature by a slow temperature increase method with a temperature increase rate of 1 to 10 ℃/min, so as to ensure sufficient reduction of the precursor and to allow sufficient growth time of the intermetallic compound.
A method for obtaining black powder by centrifugal cleaning of the mixed solution is described as follows:
adopting two mixed solvents for centrifugal cleaning, wherein the mixed solvent A is absolute ethyl alcohol and chloroform according to the volume ratio of (1-5): (5-1), wherein the mixed solvent B is deionized water and absolute ethyl alcohol according to the volume ratio of (1-5): (5-1).
The mixed solution is first washed by a mixed solvent a: the volume ratio of the mixed solution is (1-5): 1, then carrying out centrifugal separation, and pouring out upper liquid after the centrifugal separation to obtain black powder;
then cleaning the black powder by using the mixed solvent A and centrifugally separating, and repeating for 3-5 times;
then, cleaning and centrifugally separating the black powder by adopting a mixed solvent B and a mixed solvent A in turn, wherein the process of centrifugally separating after cleaning the mixed solvent B and after cleaning the mixed solvent A is called as 1 time, and the process is repeated for 3-5 times;
finally, storing the black powder after the last cleaning and centrifugal separation in absolute ethyl alcohol.
In the method, the rotating speed of a centrifugal machine for centrifugal separation is 6000-12000 rpm, and the time for each centrifugation is 3-10 min.
In the above method, it is described that in the reaction of producing the seed crystal core and producing the shell in step S3 and step S4, it is necessary to ensure a sufficient amount of the reducing agent in the mixed solution. Specifically, the reducing agent is added in one of two ways:
the method A comprises the following steps: all reducing agents are added before the seed core generation reaction of step S3, for example, all reducing agents may be added to the solvent in step S2 together with the seed core metal precursor.
The method B comprises the following steps: a first portion of reducing agent, for example a solvent, may be added together with the seed core metal precursor prior to the seed core generation reaction of step S3, the first portion being added in an amount not less than the amount capable of fully reducing the seed core metal precursor, and a second portion of the remaining reducing agent, for example a solvent, may be added together with the shell metal precursor prior to the shell generation reaction of step S4, ensuring full reduction of the shell metal precursor.
By the method, ordered L1 can be successfully synthesized by utilizing interface induction 0 The degree of order of the product of the structured nano-particle is 0.85-0.95. The coercive force Hc reaches 850.5-1500.8 Oe, and the saturation magnetization Ms reaches 61.2-185.8 emu/g.
The invention has the beneficial effects that:
(1) Monodisperse high coercivity ordered L1 synthesis by ordered metal seed interface induction 0 The structure nano material has lower synthesis temperature and simple operation;
(2) By optimizing the synthesis process, the ordered L1 with excellent dispersibility, high order degree and excellent magnetic property can be obtained 0 A structured nanomaterial;
(3) The invention aims to prepare high-order L1 by adopting interface induction 0 The structure nano particle avoids the phenomena of aggregation and abnormal growth caused in the heat treatment process, and is used for preparing high-order L1 0 The structural nano material provides theoretical support and promotes the practical process.
Description of the drawings:
FIG. 1 is an XRD pattern of the product synthesized in example 1 of the process of the present invention;
FIG. 2 is a hysteresis loop of a synthesized product in example 1 of the present invention;
FIG. 3 is a TEM image of a synthesized product of example 1 of the method of the present invention;
FIG. 4 is an XRD pattern of the product synthesized in example 2 of the process of the present invention;
FIG. 5 is a hysteresis loop of the synthesized product in example 2 of the present invention;
FIG. 6 is a TEM image of a synthesized product of example 2 of the method of the present invention;
FIG. 7 is an XRD pattern of the product synthesized by method example 3 of the present invention;
FIG. 8 is a hysteresis loop of the product synthesized in example 3 of the method of the present invention;
FIG. 9 is a TEM image of a synthesized product of example 3 of the method 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 experimental equipment, instruments and experimental reagents are all purchased commercially.
The experimental apparatus and instruments include: a three-neck flask, a condenser pipe, an electronic balance, a mechanical stirring heating sleeve, a centrifuge and the like;
the experimental reagent comprises: chloroauric acid, potassium tetrachloroaurate, copper acetylacetonate, copper acetate, copper chloride, manganese acetate, manganese chloride, manganese acetylacetonate, nickel acetate, nickel nitrate, nickel sulfate, nickel chloride, nickel acetylacetonate, iron chloride, iron nitrate, iron sulfate, iron acetylacetonate, chloroplatinic acid, platinum acetylacetonate, potassium chloroplatinate, iron carbonyl, iron oleate, cobalt acetylacetonate, cobaltoctacarbonyl, cobalt acetate, nickel nitrate, nickel sulfate, nickel chloride, nickel acetylacetonate, manganese acetate, manganese chloride, manganese acetylacetonate, manganese chloride, aluminum acetylacetonate, gallium acetate, gallium chloride, gallium acetylacetonate, potassium borohydride, sodium borohydride, 1, 2-hexadecanediol, lithium aluminum hydride, sodium cyanoborohydride, hexadecylamine, trioctylamine, octadecylamine, eicosylamine, oleylamine, oleic acid, 93 Ar 7H + H 2 、 95％Ar+5％H 2 High-purity argon Ar and high-purity nitrogen N 2 Chloroform, absolute ethyl alcohol and deionized water, all purchased from the market.
The magnetic properties of the product were measured with a Vibrating Sample Magnetometer (VSM), the morphology of the product was observed with a field emission Transmission Electron Microscope (TEM), and the phase of the product was analyzed by x-ray diffraction (XRD).
In the following examples, the reducing agent was added in one of two ways:
the method A comprises the following steps: all reducing agents are added prior to the seed core generation reaction, e.g., all reducing agents may be added to the solvent in step S2 together with the seed core metal precursor.
The method B comprises the following steps: a first portion of the reducing agent, for example, a solvent may be added together with the seed core metal precursor prior to the reaction to generate the seed core, the first portion being added in an amount not less than the amount capable of reducing the seed core metal precursor in its entirety, and a second portion of the remaining reducing agent is added prior to the reaction to generate the shell in step S4, ensuring the total reduction of the shell metal precursor.
The reducing agent is not particularly described in the following examples, and only the kind and amount of the reducing agent are described, as long as the reducing agent can ensure that all of the metal sources in the seed core metal precursor and the shell metal precursor can be reduced in two reactions of the seed core formation and the shell formation.
Example 1:
(1) Firstly, weighing seed crystal core metal precursor copper source acetylacetone copper and gold source chloroauric acid by adopting an electronic balance, wherein the molar ratio of the copper source acetylacetone copper to the gold source chloroauric acid is 0.3:0.2, weighing a reducing agent 1, 2-hexadecanediol, wherein the ratio of the theoretical value to the actual value of the using amount of the reducing agent is 1:1.
(2) Adding weighed crystal seed core metal precursor powder (a copper source and a gold source) and a reducing agent 1, 2-hexadecanediol into a three-neck flask filled with a solvent hexadecylamine, wherein the molar ratio of the crystal seed core metal precursor to the solvent is 1:10. the content of Ar +7% in protective atmosphere 93 2 Under the action of the temperature, the temperature is raised to 120 ℃ at the temperature rise rate of 10 ℃/min and is kept for 120min, the water removal treatment is carried out, and then the surfactant (oleylamine + oleic acid) is added into the mixed solution according to the volume ratio, the oleylamine: oleic acid =1:1; in terms of molar ratio, solvent: surfactant =10:1.0.
(3) Slowly heating the mixed solution to 280 ℃ at the heating rate of 1 ℃/min, preserving the temperature for 300min to obtain a black mixed solution, then cooling to 60 ℃, adding shell metal precursor powder iron source ferric chloride and cobalt source cobalt acetylacetonate into the mixed solution, wherein the molar ratio of metal in the shell metal precursor powder to metal in the seed crystal core metal precursor powder is 1:0.5, the molar ratio of two metal ions in the shell metal precursor is 0.5:0.5.
(4) And heating the mixed solution to 300 ℃ at a heating rate of 1 ℃/min, then preserving the heat for 60min, and cooling to room temperature to obtain a black mixed solution.
Carrying out centrifugal cleaning by adopting two mixed solvents, wherein the mixed solvent A is absolute ethyl alcohol and chloroform according to the volume ratio of 5:1, wherein the mixed solvent B is deionized water and absolute ethyl alcohol according to a volume ratio of 1:5, a mixed solvent; firstly, cleaning the mixed solution by using a mixed solvent A, wherein the mixed solvent A: the volume ratio of the mixed solution is 1:1, then carrying out centrifugal separation, and pouring out upper liquid after the centrifugal separation to obtain black powder; then cleaning the black powder by using a mixed solvent A, carrying out centrifugal separation, and repeating for 3 times; then, cleaning and centrifugally separating the black powder by adopting a mixed solvent B and a mixed solvent A in turn, and repeating for 3 times; finally, storing the black powder after the last cleaning and centrifugal separation in absolute ethyl alcohol; the rotating speed of the centrifugal machine for centrifugal separation is 12000rpm, and the time of each centrifugation is 10min.
Characterization of the product phase by X-ray diffractometry to be L1 0 FeCo, which contains ordered phase characteristic peaks (001), (110) and (002) with an order degree of 0.92, and an XRD pattern as shown in figure 1. Measuring the magnetic hysteresis loop of the product at room temperature by using a vibrating sample strong magnetometer, and the coercive force H of the product c 1175.6Oe, and the saturation magnetization Ms is 89.9emu/g, the hysteresis loop is shown in FIG. 2. The morphology of the product is observed to be uniformly dispersed core-shell morphology by a field emission transmission electron microscope, and a TEM image is shown in figure 3. The coercivity of the core-shell Nano-particles obtained by heat treatment at 380 ℃ is 846 Oe, which is similar to the result in the example.
Example 2:
(1) Firstly, weighing seed crystal core metal precursors of copper source copper acetate and gold source potassium tetrachloroaurate by using an electronic balance, wherein the molar ratio of the copper source copper acetate to the gold source potassium tetrachloroaurate is 0.5:0.2, weighing a certain amount of reducing agent potassium borohydride, wherein the ratio of the theoretical value to the actual value of the amount of the reducing agent is 1:1.
(2) Adding weighed seed crystal core metal precursor powder (a copper source and a gold source) and a reducing agent potassium borohydride into a three-neck flask filled with a solvent trioctylamine, wherein the molar ratio of the seed crystal core metal precursor to the solvent is 1:15. 95% in protective atmosphere Ar +5% 2 Under the action of the mixed solution, heating to 100 ℃ at a heating rate of 1 ℃/min, preserving the temperature for 120min, removing water, then adding a surfactant (brominated decahydrocarbon quaternary amine + oleic acid) into the mixed solution, and mixing the brominated decahydrocarbon quaternary amine: oleic acid =1:0.5; in terms of molar ratio, solvent: surfactant =10:2.0.
(3) Slowly heating the mixed solution to 290 ℃ at a heating rate of 2 ℃/min, preserving the temperature for 200min to obtain a black mixed solution, then cooling to 120 ℃, adding shell metal precursor powder iron carbonyl iron and cobalt source octacarbonyl dicobalt into the mixed solution, wherein the molar ratio of metal in the shell metal precursor powder to metal in the seed crystal core metal precursor powder is 1:0.2.
(4) Heating the mixed solution to 270 ℃ at a heating rate of 2 ℃/min, then preserving the heat for 10min, and cooling to room temperature to obtain a black mixed solution.
Carrying out centrifugal cleaning by adopting two mixed solvents, wherein the mixed solvent A is absolute ethyl alcohol and chloroform according to the volume ratio of 5:2, wherein the mixed solvent B is deionized water and absolute ethyl alcohol according to a volume ratio of 3:5 in a mixed solvent; first, the mixed solution is washed by a mixed solvent a: the volume ratio of the mixed solution is 2:1, then carrying out centrifugal separation, and pouring out upper liquid after the centrifugal separation to obtain black powder; then cleaning the black powder by using a mixed solvent A, carrying out centrifugal separation, and repeating for 3 times; then cleaning and centrifugally separating the black powder by adopting a mixed solvent B and a mixed solvent A in turn, and repeating for 3 times; finally, storing the black powder after the last cleaning and centrifugal separation in absolute ethyl alcohol; the rotating speed of the centrifugal machine for centrifugal separation is 8000-12000 rpm, and the time for each centrifugation is 3min.
Characterization of the product phase by X-ray diffractometry to be L1 0 FeCo, which contains ordered phase characteristic peaks (001), (110) and (002) with an order degree of 0.90, and an XRD pattern is shown in figure 4. Measuring the magnetic hysteresis loop of the product at room temperature by a vibrating sample magnetometer, and the coercive force H of the product c 1028.9Oe, a saturation magnetization Ms of 91.0emu/g, and a hysteresis loop as shown in FIG. 5. By passingThe morphology of the product observed by a field emission transmission electron microscope is a uniformly dispersed core-shell morphology, and a TEM image is shown in figure 6. The coercivity of the core-shell Nano-particles obtained by heat treatment at 380 ℃ is 846 Oe, which is similar to the result in the example.
Example 3:
(1) Firstly, weighing a seed crystal core metal precursor copper source chloride and gold source chloroauric acid by using an electronic balance, wherein the molar ratio of the copper source chloride to the gold source chloroauric acid is 0.1:1, weighing a certain amount of reducing agent sodium borohydride, wherein the ratio of the theoretical value to the actual value of the using amount of the reducing agent is 1:2.
(2) Adding weighed seed crystal core metal precursor powder (a copper source and a gold source) and a reducing agent sodium borohydride into a three-neck flask filled with a solvent trioctylamine, wherein the molar ratio of the seed crystal core metal precursor to the solvent is 1:20. under the action of high-purity argon Ar in protective atmosphere, heating to 105 ℃ at the heating rate of 2 ℃/min, preserving the temperature for 100min, removing water, then adding a surfactant (decahydroquaternary ammonium bromide + oleic acid) into the mixed solution, and according to the volume ratio, brominating the decahydroquaternary ammonium: oleic acid =0.4:1; in terms of molar ratio, solvent: surfactant =10:3.0.
(3) Slowly heating the mixed solution to 300 ℃ at a heating rate of 3 ℃/min, preserving heat for 250min to obtain a black mixed solution, then cooling to 100 ℃, adding shell metal precursor powder iron source ferric acetylacetonate and cobalt source cobalt acetate into the mixed solution, wherein the molar ratio of metal in the shell metal precursor powder to metal in the seed crystal core metal precursor powder is 1:0.5.
(4) And (3) heating the mixed solution to 260 ℃ at a heating rate of 5 ℃/min, then preserving the heat for 20min, and cooling to room temperature to obtain a black mixed solution.
Carrying out centrifugal cleaning by adopting two mixed solvents, wherein the mixed solvent A is absolute ethyl alcohol and chloroform according to the volume ratio of 5:4, wherein the mixed solvent B is deionized water and absolute ethyl alcohol according to a volume ratio of 5:5 in a mixed solvent; firstly, cleaning the mixed solution by using a mixed solvent A, wherein the mixed solvent A: the volume ratio of the mixed solution is 3:1, then carrying out centrifugal separation, and pouring out upper-layer liquid after the centrifugal separation to obtain black powder; then cleaning the black powder by using a mixed solvent A, performing centrifugal separation, and repeating for 4 times; then cleaning and centrifugally separating the black powder by adopting a mixed solvent B and a mixed solvent A in turn, and repeating for 4 times; finally, storing the black powder after the last cleaning and centrifugal separation in absolute ethyl alcohol; the rotating speed of the centrifugal machine for centrifugal separation is 8000-10000 rpm, and the time for each centrifugation is 4-8 min.
Characterization of the product phase by X-ray diffractometry to be L1 0 FeCo, which contains ordered phase characteristic peaks (001), (110) and (002) with an order degree of 0.91, and the XRD pattern is shown in figure 7. Measuring the magnetic hysteresis loop of the product at room temperature by using a vibrating sample strong magnetometer, and the coercive force H of the product c 1093.1Oe, the saturation magnetization Ms is 76.4emu/g, and the hysteresis loop is shown in FIG. 8. The morphology of the product is observed to be a uniformly dispersed core-shell morphology by a field emission transmission electron microscope, and a TEM image is shown in figure 9. The coercivity of the core-shell Nano-particles obtained by heat treatment at 380 ℃ is 846 Oe, which is similar to the result in the example.
Example 4:
(1) Firstly, weighing seed crystal core metal precursor copper source acetylacetone copper and gold source potassium tetrachloroaurate by using an electronic balance, wherein the molar ratio of the copper source acetylacetone copper to the gold source potassium tetrachloroaurate is 0.5:1, weighing a certain amount of reducing agent 1, 2-hexadecanediol, wherein the proportion relation between the theoretical value and the actual value of the using amount of the reducing agent is 1:2.
(2) Adding weighed crystal seed core metal precursor powder (a copper source and a gold source) and a reducing agent 1, 2-hexadecanediol into a three-neck flask filled with a solvent octadecylamine, wherein the molar ratio of the crystal seed core metal precursor to the solvent is 1:25. high purity nitrogen N in protective atmosphere 2 Under the action of the temperature, the temperature is raised to 110 ℃ at the temperature rise rate of 10 ℃/min and is kept for 80min, the water removal treatment is carried out, and then the surfactant (oleylamine + lecithin) is added into the mixed solution according to the volume ratio, the ratio of oleylamine: lecithin =0.3:1; in terms of molar ratio, solvent: surfactant =10:4.0.
(3) Slowly heating the mixed solution to 320 ℃ at a heating rate of 5 ℃/min, preserving heat for 150min to obtain a black mixed solution, then cooling to 90 ℃, adding shell metal precursor powder iron source ferric oleate and cobalt source cobalt acetylacetonate into the mixed solution, wherein the molar ratio of metal in the shell metal precursor powder to metal in the seed crystal core metal precursor powder is 1:1.
(4) And (3) heating the mixed solution to 200 ℃ at the heating rate of 1 ℃/min, then preserving the heat for 30min, and cooling to room temperature to obtain a black mixed solution.
Carrying out centrifugal cleaning by adopting two mixed solvents, wherein the mixed solvent A is absolute ethyl alcohol and chloroform according to a volume ratio of 4:5, wherein the mixed solvent B is deionized water and absolute ethyl alcohol according to a volume ratio of 5:4 in a mixed solvent; first, the mixed solution is washed by a mixed solvent a: the volume ratio of the mixed solution is 4:1, then carrying out centrifugal separation, and pouring out upper-layer liquid after the centrifugal separation to obtain black powder; then cleaning the black powder by using a mixed solvent A, performing centrifugal separation, and repeating for 4 times; then cleaning and centrifugally separating the black powder by adopting a mixed solvent B and a mixed solvent A in turn, and repeating for 4 times; finally, storing the black powder after the last cleaning and centrifugal separation in absolute ethyl alcohol; the rotating speed of the centrifugal machine for centrifugal separation is 8000-10000 rpm, and the time for each centrifugation is 6-8 min.
Characterization of the product phase by X-ray diffractometry to be L1 0 FeCo, which contains ordered phase characteristic peaks (001), (110) and (002), with an order degree of 0.95. Measuring the magnetic hysteresis loop of the product at room temperature by using a vibrating sample strong magnetometer, and the coercive force H of the product c 1405.5Oe, and the saturation magnetization Ms is 92.5emu/g. The morphology of the product is observed to be uniformly dispersed core-shell morphology through a field emission transmission electron microscope.
Example 5:
(1) Firstly, weighing seed crystal core metal precursors of manganese source manganese acetate and nickel source nickel acetate by using an electronic balance, wherein the molar ratio of the manganese source manganese acetate to the nickel source nickel acetate is 0.3:1, weighing a certain amount of reducing agent lithium aluminum hydride, wherein the proportion relation between the theoretical value and the actual value of the reducing agent is 1:3.
(2) Adding weighed crystal seed core metal precursor powder (a manganese source and a nickel source) and a reducing agent lithium aluminum hydride into a three-neck flask filled with a solvent icosamine, wherein the molar ratio of the crystal seed core metal precursor to the solvent is 1:30. under the action of high-purity argon Ar in a protective atmosphere, heating to 115 ℃ at a heating rate of 5 ℃/min, preserving heat for 50min, removing water, and then adding a surfactant (oleylamine + glyceryl monostearate) into the mixed solution, wherein the volume ratio of oleylamine: glycerol monostearate =1:0.3; in terms of molar ratio, solvent: surfactant =10:5.0.
(3) Slowly heating the mixed solution to 340 ℃ at a heating rate of 8 ℃/min, keeping the temperature for 100min to obtain a black mixed solution, then cooling to 80 ℃, adding shell metal precursor powder nickel acetate and iron oleate into the mixed solution, wherein the molar ratio of metal in the shell metal precursor powder to metal in the seed crystal core metal precursor powder is 1.4: 1.
(4) And (3) heating the mixed solution to 245 ℃ at the heating rate of 8 ℃/min, then preserving the heat for 40min, and cooling to room temperature to obtain a black mixed solution.
And (2) carrying out centrifugal cleaning by adopting two mixed solvents, wherein the mixed solvent A is absolute ethyl alcohol and chloroform according to a volume ratio of 2:5, wherein the mixed solvent B is deionized water and absolute ethyl alcohol according to a volume ratio of 5: 2; first, the mixed solution is washed by a mixed solvent a: the volume ratio of the mixed solution is 5:1, then carrying out centrifugal separation, and pouring out upper-layer liquid after the centrifugal separation to obtain black powder; then cleaning the black powder by using a mixed solvent A, carrying out centrifugal separation, and repeating for 5 times; then cleaning and centrifugally separating the black powder by adopting a mixed solvent B and a mixed solvent A in turn, and repeating for 3 times; finally, storing the black powder after the last cleaning and centrifugal separation in absolute ethyl alcohol; the rotating speed of the centrifugal machine for centrifugal separation is 8000-10000 rpm, and the time for each centrifugation is 3-10 min.
Characterization of the product phase by X-ray diffractometry to be L1 0 FeNi, which contains ordered phase characteristic peaks (001), (110) and (002), and has an order degree of 0.95. Measuring the magnetic hysteresis loop of the product at room temperature by using a vibrating sample strong magnetometer, and the coercive force H of the product c 1405.5Oe, and the saturation magnetization Ms is 92.5emu/g. The morphology of the product is observed to be uniformly dispersed core-shell morphology through a field emission transmission electron microscope.
Example 6:
(1) Firstly, weighing a seed crystal core metal precursor manganese source manganese chloride and nickel source nickel nitrate by using an electronic balance, wherein the molar ratio of the manganese source manganese chloride to the nickel source nickel nitrate is 1:0.5, weighing a certain amount of reducing agent sodium cyanoborohydride, wherein the ratio of the theoretical value to the actual value of the amount of the reducing agent is 1:4.
(2) Adding weighed seed crystal core metal precursor powder (a manganese source and a nickel source) and a reducing agent sodium cyanoborohydride into a three-neck flask filled with oleylamine as a solvent, wherein the molar ratio of the seed crystal core metal precursor to the solvent is 1:25. 95% in protective atmosphere Ar +5% 2 Under the action of the temperature, the temperature is raised to 120 ℃ at the temperature raising rate of 8 ℃/min and is kept for 30min, the water removing treatment is carried out, then, the surfactant (decahydroquaternary ammonium bromide + lecithin) is added into the mixed solution, and the decahydroquaternary ammonium bromide is prepared by the following steps: lecithin =1:1; in terms of molar ratio, solvent: surfactant =10:2.0.
(3) Slowly heating the mixed solution to 360 ℃ at a heating rate of 10 ℃/min, preserving heat for 30min to obtain a black mixed solution, then cooling to 60 ℃, adding shell metal precursor powder iron source ferric acetylacetonate and nickel source nickel nitrate into the mixed solution, wherein the molar ratio of metal in the shell metal precursor powder to metal in the seed crystal core metal precursor powder is 1:1.
(4) Heating the mixed solution to 240 ℃ at a heating rate of 10 ℃/min, then preserving the heat for 50min, and cooling to room temperature to obtain a black mixed solution.
And (2) carrying out centrifugal cleaning by adopting two mixed solvents, wherein the mixed solvent A is absolute ethyl alcohol and chloroform according to a volume ratio of 1:5, wherein the mixed solvent B is deionized water and absolute ethyl alcohol according to a volume ratio of 5:1, a mixed solvent; first, the mixed solution is washed by a mixed solvent a: the volume ratio of the mixed solution is 5:1, then carrying out centrifugal separation, and pouring out upper-layer liquid after the centrifugal separation to obtain black powder; then cleaning the black powder by using a mixed solvent A, carrying out centrifugal separation, and repeating for 5 times; then, cleaning and centrifugally separating the black powder by adopting a mixed solvent B and a mixed solvent A in turn, and repeating for 5 times; finally, storing the black powder after the last cleaning and centrifugal separation in absolute ethyl alcohol; the rotating speed of the centrifugal machine for centrifugal separation is 6000-12000 rpm, and the time for each centrifugation is 3-10 min.
Characterization of the product phase by X-ray diffractometry to be L1 0 FeNi, which contains ordered phase characteristic peaks (001), (110) and (002), and has an order degree of 0.95. Measuring the magnetic hysteresis loop of the product at room temperature by a vibrating sample magnetometer, and the coercive force H of the product c 1500.8Oe and 85.6emu/g of saturation magnetization Ms. The morphology of the product is observed to be uniformly dispersed core-shell morphology by a field emission transmission electron microscope.
Example 7:
(1) Firstly, weighing seed crystal core metal precursors of manganese source acetylacetone manganese and nickel source nickel sulfate by using an electronic balance, wherein the molar ratio of the manganese source acetylacetone manganese to the nickel source nickel sulfate is 1:0.2, weighing a certain amount of 1, 2-hexadecanediol as a reducing agent, wherein the ratio of the theoretical value to the actual value of the amount of the reducing agent is 1:3.
(2) Weighing seed crystal core metal precursor powder (a manganese source and a nickel source) and 1, 2-hexadecanediol serving as a reducing agent into a three-neck flask filled with a solvent hexadecylamine, wherein the molar ratio of the seed crystal core metal precursor to the solvent is 1:10. h at a protective atmosphere of 93% Ar +7 2 Under the action of the temperature, heating to 100 ℃ at the heating rate of 1 ℃/min, preserving the temperature for 30min, removing water, and then adding a surfactant (oleylamine + oleic acid) into the mixed solution, wherein the volume ratio of oleylamine: oleic acid =1:1; in terms of molar ratio, solvent: surfactant =10:1.0.
(3) Slowly heating the mixed solution to 280 ℃ at a heating rate of 1 ℃/min, preserving heat for 30min to obtain a black mixed solution, then cooling to 60 ℃, adding shell metal precursor powder iron carbonyl iron and nickel sulfate, wherein the molar ratio of metal in the shell metal precursor powder to metal in the seed crystal core metal precursor powder is 0.8: 0.5.
(4) And heating the mixed solution to 280 ℃ at a heating rate of 1 ℃/min, then preserving the heat for 60min, and cooling to room temperature to obtain a black mixed solution.
Carrying out centrifugal cleaning by adopting two mixed solvents, wherein the mixed solvent A is absolute ethyl alcohol and chloroform according to a volume ratio of 1:5, wherein the mixed solvent B is deionized water and absolute ethyl alcohol according to a volume ratio of 1:5, a mixed solvent; first, the mixed solution is washed by a mixed solvent a: the volume ratio of the mixed solution is 1:1, then carrying out centrifugal separation, and pouring out upper-layer liquid after the centrifugal separation to obtain black powder; then cleaning the black powder by using a mixed solvent A, performing centrifugal separation, and repeating for 3 times; then, cleaning and centrifugally separating the black powder by adopting a mixed solvent B and a mixed solvent A in turn, and repeating for 3 times; finally, storing the black powder after the last cleaning and centrifugal separation in absolute ethyl alcohol; the rotation speed of the centrifugal machine for centrifugal separation is 6000rpm, and each time of centrifugation is 3min.
Characterization of the product phase by X-ray diffractometry to be L1 0 FeNi, containing ordered phase characteristic peaks (001), (110) and (002), with an order degree of 0.86. Measuring the magnetic hysteresis loop of the product at room temperature by using a vibrating sample strong magnetometer, and the coercive force H of the product c The saturation magnetization Ms was 896.8Oe and 163.8emu/g. The morphology of the product is observed to be uniformly dispersed core-shell morphology by a field emission transmission electron microscope.
Example 8:
(1) Firstly, weighing seed crystal core metal precursors of manganese source manganese chloride and nickel source nickel chloride by using an electronic balance, wherein the molar ratio of the manganese source manganese chloride to the nickel source nickel chloride is 0.5:1, weighing a certain amount of reducing agent potassium borohydride, wherein the ratio of the theoretical value to the actual value of the amount of the reducing agent is 1:7.
(2) Adding weighed seed crystal core metal precursor powder (a manganese source and a nickel source) and a reducing agent potassium borohydride into a three-neck flask filled with a solvent octadecylamine, wherein the molar ratio of the seed crystal core metal precursor to the solvent is 1:30. heating to 120 ℃ at a heating rate of 10 ℃/min under the action of high-purity argon in a protective atmosphere, preserving heat for 120min, removing water, adding a surfactant (oleylamine + lecithin) into the mixed solution, and mixing the oleylamine: lecithin =0.1:1; in terms of molar ratio, solvent: surfactant =10:5.0.
(3) Slowly heating the mixed solution to 360 ℃ at a heating rate of 10 ℃/min, preserving heat for 300min to obtain a black mixed solution, then cooling to 120 ℃, adding shell metal precursor powder iron source ferric chloride and nickel source nickel chloride into the mixed solution, wherein the molar ratio of metal in the shell metal precursor powder to metal in the seed crystal core metal precursor powder is 1:1.
(4) Heating the mixed solution to 340 ℃ at a heating rate of 10 ℃/min, then preserving the heat for 60min, and cooling to room temperature to obtain a black mixed solution.
Carrying out centrifugal cleaning by adopting two mixed solvents, wherein the mixed solvent A is absolute ethyl alcohol and chloroform according to a volume ratio of 1:1, wherein the mixed solvent B is deionized water and absolute ethyl alcohol according to a volume ratio of 1:1, a mixed solvent; firstly, cleaning the mixed solution by using a mixed solvent A, wherein the mixed solvent A: the volume ratio of the mixed solution is 5:1, then carrying out centrifugal separation, and pouring out upper-layer liquid after the centrifugal separation to obtain black powder; then cleaning the black powder by using a mixed solvent A, performing centrifugal separation, and repeating for 5 times; then, cleaning and centrifugally separating the black powder by adopting a mixed solvent B and a mixed solvent A in turn, and repeating for 4 times; finally, storing the black powder after the last cleaning and centrifugal separation in absolute ethyl alcohol; the rotating speed of the centrifugal machine for centrifugal separation is 12000rpm, and the time of each centrifugation is 10min.
Characterization of the product phase by X-ray diffractometry to be L1 0 FeNi, which contains ordered phase characteristic peaks (001), (110) and (002), and has an order degree of 0.89. Measuring the magnetic hysteresis loop of the product at room temperature by using a vibrating sample strong magnetometer, and the coercive force H of the product c 1096.8Oe, and the saturation magnetization Ms is 185.8emu/g. The morphology of the product is observed to be uniformly dispersed core-shell morphology through a field emission transmission electron microscope.
Example 9:
(1) Firstly, weighing seed crystal core metal precursors of manganese source acetylacetone manganese and nickel source acetylacetone nickel by an electronic balance, wherein the molar ratio of the two precursors is 0.8:1, weighing a certain amount of reducing agent sodium borohydride, wherein the ratio of the theoretical value to the actual value of the using amount of the reducing agent is 1:2.
(2) Adding weighed seed crystal core metal precursor powder (a manganese source and a nickel source) and a reducing agent sodium borohydride into a three-neck flask filled with a solvent trioctylamine, wherein the molar ratio of the seed crystal core metal precursor to the solvent is 1:20. heating to 110 ℃ at a heating rate of 5 ℃/min and keeping the temperature for 75min under the action of high-purity nitrogen in a protective atmosphere, removing water, adding a surfactant (brominated quaternary decahydrocarbon amine + oleic acid) into the mixed solution, and carrying out bromination on the quaternary decahydrocarbon amine: oleic acid =1:0.1; in terms of molar ratio, solvent: surfactant =10:3.0.
(3) Slowly heating the mixed solution to 320 ℃ at a heating rate of 5 ℃/min, preserving heat for 150min to obtain a black mixed solution, then cooling to 90 ℃, adding shell metal precursor powder iron source ferric oleate and nickel source nickel acetylacetonate into the mixed solution, wherein the molar ratio of metal in the shell metal precursor powder to metal in the seed crystal core metal precursor powder is 1:0.2.
(4) Heating the mixed solution to 300 ℃ at a heating rate of 5 ℃/min, then preserving the heat for 30min, and cooling to room temperature to obtain a black mixed solution.
And (2) carrying out centrifugal cleaning by adopting two mixed solvents, wherein the mixed solvent A is absolute ethyl alcohol and chloroform according to a volume ratio of 5:1, wherein the mixed solvent B is deionized water and absolute ethyl alcohol in a volume ratio of 5: 1; firstly, cleaning the mixed solution by using a mixed solvent A, wherein the mixed solvent A: the volume ratio of the mixed solution is 1:1, then carrying out centrifugal separation, and pouring out upper-layer liquid after the centrifugal separation to obtain black powder; then cleaning the black powder by using a mixed solvent A, carrying out centrifugal separation, and repeating for 4 times; then, cleaning and centrifugally separating the black powder by adopting a mixed solvent B and a mixed solvent A in turn, and repeating for 4 times; finally, storing the black powder after the last cleaning and centrifugal separation in absolute ethyl alcohol; the rotating speed of the centrifugal machine for centrifugal separation is 9000rpm, and the time of each centrifugation is 6min.
Characterization of the product phase by X-ray diffractometry to be L1 0 FeNi, containing ordered phase characteristic peaks (001), (110) and (002), with an order degree of 0.90. Measuring the magnetic hysteresis loop of the product at room temperature by a vibrating sample magnetometer, and the coercive force H of the product c The saturation magnetization Ms was 61.2emu/g at 1206.7 Oe. The morphology of the product is observed to be uniformly dispersed core-shell morphology through a field emission transmission electron microscope.
Example 10:
(1) Firstly, weighing seed crystal core metal precursors of manganese source manganese acetate and nickel source nickel chloride by using an electronic balance, wherein the molar ratio of the manganese source manganese acetate to the nickel source nickel chloride is 0.7:1, weighing a certain amount of reducing agent sodium cyanoborohydride, wherein the ratio of the theoretical value to the actual value of the amount of the reducing agent is 1:1.
(2) Adding weighed seed crystal core metal precursor powder (a manganese source and a nickel source) and a reducing agent sodium cyanoborohydride into a three-neck flask filled with a solvent eicosylamine, wherein the molar ratio of the seed crystal core metal precursor to the solvent is 1:10. in a protective atmosphere 93% Ar +7% 2 Under the action of the temperature, heating to 120 ℃ at a heating rate of 10 ℃/min, preserving the temperature for 120min, removing water, and then adding a surfactant (oleylamine + glyceryl monostearate) into the mixed solution, wherein the volume ratio of oleylamine: glycerol monostearate =1:1; in terms of molar ratio, solvent: surfactant =10:1.0.
(3) Slowly heating the mixed solution to 280 ℃ at a heating rate of 1 ℃/min, preserving the temperature for 300min to obtain a black mixed solution, then cooling to 60 ℃, adding shell metal precursor powder, namely manganese acetate and aluminum chloride, into the mixed solution, wherein the molar ratio of metal in the shell metal precursor powder to metal in the seed crystal core precursor powder is 0.4: 0.5.
(4) And heating the mixed solution to 280 ℃ at a heating rate of 1 ℃/min, then preserving the heat for 60min, and cooling to room temperature to obtain a black mixed solution.
Carrying out centrifugal cleaning by adopting two mixed solvents, wherein the mixed solvent A is absolute ethyl alcohol and chloroform according to the volume ratio of 5:1, wherein the mixed solvent B is deionized water and absolute ethyl alcohol in a volume ratio of 1:5, a mixed solvent; firstly, cleaning the mixed solution by using a mixed solvent A, wherein the mixed solvent A: the volume ratio of the mixed solution is 1:1, then carrying out centrifugal separation, and pouring out upper-layer liquid after the centrifugal separation to obtain black powder; then cleaning the black powder by using a mixed solvent A, performing centrifugal separation, and repeating for 3 times; then cleaning and centrifugally separating the black powder by adopting a mixed solvent B and a mixed solvent A in turn, and repeating for 5 times; finally, storing the black powder after the last cleaning and centrifugal separation in absolute ethyl alcohol; the rotating speed of the centrifugal machine for centrifugal separation is 6000-12000 rpm, and the time for each centrifugation is 10min.
Characterization of the product phase by X-ray diffractometry to be L1 0 MnAl, which contains ordered phase characteristic peaks (001), (110) and (002), and has an order degree of 0.92. Measuring the magnetic hysteresis loop of the product at room temperature by a vibrating sample magnetometer, and the coercive force H of the product c It was 1231.8Oe and the saturation magnetization Ms was 75.8emu/g. The morphology of the product is observed to be uniformly dispersed core-shell morphology through a field emission transmission electron microscope.
Example 11:
(1) Firstly, weighing a seed crystal core metal precursor gold source chloroauric acid and a copper source copper chloride by using an electronic balance, wherein the molar ratio of the gold source chloroauric acid to the copper source copper chloride is 1:0.7, weighing a certain amount of reducing agent 1, 2-hexadecanediol, wherein the proportion relation between the theoretical value and the actual value of the using amount of the reducing agent is 1:6.
(2) Weighing seed crystal core metal precursor powder (a gold source and a copper source) and a reducing agent 1, 2-hexadecanediol into a three-neck flask filled with a solvent hexadecylamine, wherein the molar ratio of the seed crystal core metal precursor to the solvent is 1:10. h at a protective atmosphere of 93% Ar +7 2 Under the action of the temperature, heating to 120 ℃ at the heating rate of 8 ℃/min, preserving the temperature for 120min, removing water, and then adding a surfactant (oleylamine + oleic acid) into the mixed solution according to the volume ratio, wherein the ratio of oleylamine: oleic acid =1:1; in terms of molar ratio, solvent: surfactant =10:1.0.
(3) Slowly heating the mixed solution to 280 ℃ at a heating rate of 1 ℃/min, preserving the temperature for 300min to obtain a black mixed solution, then cooling to 60 ℃, adding shell metal precursor powder, namely manganese source manganese chloride and aluminum source aluminum chloride, into the mixed solution, wherein the molar ratio of metal in the shell metal precursor powder to metal in the seed crystal core metal precursor powder is 1:0.2.
(4) And heating the mixed solution to 280 ℃ at a heating rate of 1 ℃/min, then preserving the heat for 60min, and cooling to room temperature to obtain a black mixed solution.
Carrying out centrifugal cleaning by adopting two mixed solvents, wherein the mixed solvent A is absolute ethyl alcohol and chloroform according to the volume ratio of 5:1, wherein the mixed solvent B is deionized water and absolute ethyl alcohol according to a volume ratio of 1:5 in a mixed solvent; firstly, cleaning the mixed solution by using a mixed solvent A, wherein the mixed solvent A: the volume ratio of the mixed solution is 1:1, then carrying out centrifugal separation, and pouring out upper liquid after the centrifugal separation to obtain black powder; then cleaning the black powder by using a mixed solvent A, carrying out centrifugal separation, and repeating for 3 times; then, cleaning and centrifugally separating the black powder by adopting a mixed solvent B and a mixed solvent A in turn, and repeating for 3 times; finally, storing the black powder after the last cleaning and centrifugal separation in absolute ethyl alcohol; the rotation speed of the centrifugal machine for centrifugal separation is 9000rpm, and each centrifugal time is 10min.
Characterization of the product phase by X-ray diffractometry to be L1 0 MnAl, which contains ordered phase characteristic peaks (001), (110) and (002), and has an order degree of 0.93. Measuring the magnetic hysteresis loop of the product at room temperature by using a vibrating sample strong magnetometer, and the coercive force H of the product c It was 1332.7Oe, and the saturation magnetization Ms was 71.5emu/g. The morphology of the product is observed to be uniformly dispersed core-shell morphology by a field emission transmission electron microscope.
Example 12:
(1) Firstly, weighing a seed crystal core metal precursor gold source potassium tetrachloroaurate and a copper source copper acetylacetonate by using an electronic balance, wherein the molar ratio of the gold source potassium tetrachloroaurate to the copper source copper acetylacetonate is 1:0.2, weighing a certain amount of 1, 2-hexadecanediol as a reducing agent, wherein the ratio of the theoretical value to the actual value of the amount of the reducing agent is 1:9.
(2) Adding weighed crystal seed core metal precursor powder (a gold source and a copper source) and a reducing agent 1, 2-hexadecanediol into a three-neck flask filled with a solvent hexadecylamine, wherein the molar ratio of the crystal seed core metal precursor to the solvent is 1:10. in a protective atmosphere of 93%Ar+7％H 2 Under the action of the temperature, heating to 100 ℃ at the heating rate of 1 ℃/min, preserving the temperature for 30min, removing water, and then adding a surfactant (oleylamine + oleic acid) into the mixed solution, wherein the volume ratio of oleylamine: oleic acid =1:1; in terms of molar ratio, solvent: surfactant =10:1.0.
(3) Slowly heating the mixed solution to 280 ℃ at a heating rate of 1 ℃/min, preserving the temperature for 30min to obtain a black mixed solution, then cooling to 60 ℃, adding shell metal precursor powder manganese source manganese acetylacetonate and aluminum source aluminum acetylacetonate into the mixed solution, wherein the molar ratio of metal in the shell metal precursor powder to metal in the seed crystal core metal precursor powder is 0.8: 0.5.
(4) And heating the mixed solution to 280 ℃ at a heating rate of 1 ℃/min, then preserving the heat for 60min, and cooling to room temperature to obtain a black mixed solution.
Carrying out centrifugal cleaning by adopting two mixed solvents, wherein the mixed solvent A is absolute ethyl alcohol and chloroform according to a volume ratio of 1:5, wherein the mixed solvent B is deionized water and absolute ethyl alcohol according to a volume ratio of 1:5 in a mixed solvent; first, the mixed solution is washed by a mixed solvent a: the volume ratio of the mixed solution is 1:1, then carrying out centrifugal separation, and pouring out upper liquid after the centrifugal separation to obtain black powder; then cleaning the black powder by using a mixed solvent A, performing centrifugal separation, and repeating for 3 times; then cleaning and centrifugally separating the black powder by adopting a mixed solvent B and a mixed solvent A in turn, and repeating for 3 times; finally, storing the black powder after the last cleaning and centrifugal separation in absolute ethyl alcohol; the rotation speed of the centrifugal machine for centrifugal separation is 6000rpm, and each time of centrifugation is 3min.
Characterization of the product phase by X-ray diffractometry to be L1 0 MnAl, which contains ordered phase characteristic peaks (001), (110) and (002), and has an order degree of 0.94. Measuring the magnetic hysteresis loop of the product at room temperature by a vibrating sample magnetometer, and the coercive force H of the product c It was 1231.8Oe, and the saturation magnetization Ms was 75.8emu/g. The morphology of the product is observed to be uniformly dispersed core-shell morphology by a field emission transmission electron microscope.
Example 13:
(1) Firstly, weighing iron source ferric chloride and platinum source platinum acetylacetonate serving as seed crystal core metal precursors by using an electronic balance, wherein the molar ratio of the iron source ferric chloride to the platinum source platinum acetylacetonate is 0.5:1, weighing a certain amount of reducing agent potassium borohydride, wherein the ratio of the theoretical value to the actual value of the using amount of the reducing agent is 1:2.
(2) Adding weighed seed crystal core metal precursor powder (an iron source and a platinum source) and a reducing agent potassium borohydride into a three-neck flask filled with a solvent octadecylamine, wherein the molar ratio of the seed crystal core metal precursor to the solvent is 1:30. heating to 120 ℃ at a heating rate of 10 ℃/min under the action of high-purity argon in a protective atmosphere, preserving heat for 120min, removing water, adding a surfactant (oleylamine + lecithin) into the mixed solution, and mixing the oleylamine: lecithin =0.1:1; in terms of molar ratio, solvent: surfactant =10:5.0.
(3) Slowly heating the mixed solution to 360 ℃ at a heating rate of 10 ℃/min, preserving heat for 300min to obtain a black mixed solution, then cooling to 120 ℃, adding shell metal precursor powder manganese acetylacetonate and gallium acetate into the mixed solution, wherein the molar ratio of the shell metal precursor powder to metal in the seed crystal core metal precursor powder is 1:1.
(4) And (3) heating the mixed solution to 340 ℃ at a heating rate of 10 ℃/min, then preserving the heat for 60min, and cooling to room temperature to obtain a black mixed solution.
And (2) carrying out centrifugal cleaning by adopting two mixed solvents, wherein the mixed solvent A is absolute ethyl alcohol and chloroform according to a volume ratio of 1:1, wherein the mixed solvent B is deionized water and absolute ethyl alcohol in a volume ratio of 1:1, a mixed solvent; firstly, cleaning the mixed solution by using a mixed solvent A, wherein the mixed solvent A: the volume ratio of the mixed solution is 5:1, then carrying out centrifugal separation, and pouring out upper-layer liquid after the centrifugal separation to obtain black powder; then cleaning the black powder by using a mixed solvent A, carrying out centrifugal separation, and repeating for 5 times; then cleaning and centrifugally separating the black powder by adopting a mixed solvent B and a mixed solvent A in turn, and repeating for 5 times; finally, storing the black powder after the last cleaning and centrifugal separation in absolute ethyl alcohol; the rotating speed of the centrifugal machine for centrifugal separation is 12000rpm, and the time of each centrifugation is 10min.
Characterization of the product phase by X-ray diffractometry to be L1 0 MnGa containing ordered phase characteristic peaks (001), (110) and (002) and having an order degree of 0.95. Measuring the magnetic hysteresis loop of the product at room temperature by using a vibrating sample strong magnetometer, and the coercive force H of the product c It was 1450.5Oe and the saturation magnetization Ms was 85.9emu/g. The morphology of the product is observed to be uniformly dispersed core-shell morphology by a field emission transmission electron microscope.
Example 14:
(1) Firstly, weighing iron source ferric nitrate and platinum source chloroplatinic acid serving as seed crystal core metal precursors by using an electronic balance, wherein the molar ratio of the iron source ferric nitrate to the platinum source chloroplatinic acid is 0.8:1, weighing a certain amount of reducing agent sodium borohydride, wherein the ratio of the theoretical value to the actual value of the using amount of the reducing agent is 1:2.
(2) Adding weighed seed crystal core metal precursor powder (an iron source and a platinum source) and a reducing agent sodium borohydride into a three-neck flask filled with a solvent trioctylamine, wherein the molar ratio of the seed crystal core metal precursor to the solvent is 1:20. under the action of high-purity nitrogen in protective atmosphere, heating to 110 ℃ at a heating rate of 5 ℃/min, keeping the temperature for 75min, removing water, adding a surfactant (brominated decahydrocarbon quaternary amine + oleic acid) into the mixed solution, and mixing the brominated decahydrocarbon quaternary amine: oleic acid =1:0.1; in terms of molar ratio, solvent: surfactant =10:3.0.
(3) Slowly heating the mixed solution to 320 ℃ at a heating rate of 5 ℃/min, preserving heat for 150min to obtain a black mixed solution, then cooling to 90 ℃, adding shell metal precursor powder manganese source manganese acetate and gallium source gallium chloride into the mixed solution, wherein the molar ratio of the shell metal precursor powder to the metal in the seed crystal core metal precursor powder is 1:0.2.
(4) And (3) heating the mixed solution to 300 ℃ at the heating rate of 5 ℃/min, then preserving the heat for 30min, and cooling to room temperature to obtain a black mixed solution.
Carrying out centrifugal cleaning by adopting two mixed solvents, wherein the mixed solvent A is absolute ethyl alcohol and chloroform according to the volume ratio of 5:1, wherein the mixed solvent B is deionized water and absolute ethyl alcohol according to a volume ratio of 5:1, a mixed solvent; firstly, cleaning the mixed solution by using a mixed solvent A, wherein the mixed solvent A: the volume ratio of the mixed solution is 1:1, then carrying out centrifugal separation, and pouring out upper-layer liquid after the centrifugal separation to obtain black powder; then cleaning the black powder by using a mixed solvent A, carrying out centrifugal separation, and repeating for 4 times; then, cleaning and centrifugally separating the black powder by adopting a mixed solvent B and a mixed solvent A in turn, and repeating for 4 times; finally, storing the black powder after the last cleaning and centrifugal separation in absolute ethyl alcohol; the rotating speed of the centrifugal machine for centrifugal separation is 9000rpm, and the time of each centrifugation is 6min.
Characterization of the product phase by X-ray diffractometry to be L1 0 MnGa containing ordered phase characteristic peaks (001), (110) and (002) and having an order degree of 0.90. Measuring the magnetic hysteresis loop of the product at room temperature by a vibrating sample magnetometer, and the coercive force H of the product c 1460.8Oe, and the saturation magnetization Ms of 160.5emu/g. The morphology of the product is observed to be uniformly dispersed core-shell morphology by a field emission transmission electron microscope.
Example 15:
(1) Firstly, weighing iron source ferric sulfate and platinum source potassium chloroplatinate serving as core metal precursors of the seed crystal by using an electronic balance, wherein the molar ratio of the iron source ferric sulfate to the platinum source potassium chloroplatinate is 0.7:1, weighing a certain amount of reducing agent sodium cyanoborohydride, wherein the ratio of the theoretical value to the actual value of the amount of the reducing agent is 1:6.
(2) Adding weighed seed crystal core metal precursor powder (an iron source and a platinum source) and a reducing agent sodium cyanoborohydride into a three-neck flask filled with a solvent eicosylamine, wherein the molar ratio of the seed crystal core metal precursor to the solvent is 1:10. in a protective atmosphere 93% Ar +7% 2 Under the action of the temperature, heating to 120 ℃ at the heating rate of 10 ℃/min, preserving the temperature for 120min, removing water, and then adding a surfactant (oleylamine + glyceryl monostearate) into the mixed solution according to the volume ratio, namely, oleylamine: glycerol monostearate =1:1; in terms of molar ratio, solvent: surfactant =10:1.0.
(3) Slowly heating the mixed solution to 280 ℃ at the heating rate of 1 ℃/min, preserving the temperature for 300min to obtain a black mixed solution, then cooling to 60 ℃, adding shell metal precursor powder manganese source manganese chloride and gallium source gallium acetylacetonate into the mixed solution, wherein the molar ratio of metal in the shell metal precursor powder to metal in the seed crystal core metal precursor powder is 0.4:1, the molar ratio of two metal ions in the shell metal precursor is 0.5:0.5.
(4) And (3) heating the mixed solution to 200 ℃ at the heating rate of 1 ℃/min, then preserving the heat for 60min, and cooling to room temperature to obtain a black mixed solution.
Carrying out centrifugal cleaning by adopting two mixed solvents, wherein the mixed solvent A is absolute ethyl alcohol and chloroform according to the volume ratio of 5:1, wherein the mixed solvent B is deionized water and absolute ethyl alcohol in a volume ratio of 1:5 in a mixed solvent; firstly, cleaning the mixed solution by using a mixed solvent A, wherein the mixed solvent A: the volume ratio of the mixed solution is 1:1, then carrying out centrifugal separation, and pouring out upper-layer liquid after the centrifugal separation to obtain black powder; then cleaning the black powder by using a mixed solvent A, carrying out centrifugal separation, and repeating for 3 times; then cleaning and centrifugally separating the black powder by adopting a mixed solvent B and a mixed solvent A in turn, and repeating for 5 times; finally, storing the black powder after the last cleaning and centrifugal separation in absolute ethyl alcohol; the rotating speed of the centrifugal machine for centrifugal separation is 6000-12000 rpm, and the time of each centrifugation is 10min.
Characterization of the product phase by X-ray diffractometry to be L1 0 MnGa containing ordered phase characteristic peaks (001), (110) and (002) and having an order degree of 0.92. Measuring the magnetic hysteresis loop of the product at room temperature by using a vibrating sample strong magnetometer, and the coercive force H of the product c It was 1492.4Oe and the saturation magnetization Ms was 126.8emu/g. The morphology of the product is observed to be uniformly dispersed core-shell morphology by a field emission transmission electron microscope.
Example 16:
(1) Firstly, weighing iron source ferric acetylacetonate and platinum source chloroplatinic acid serving as seed crystal core metal precursors by using an electronic balance, wherein the molar ratio of the iron source ferric acetylacetonate to the platinum source chloroplatinic acid is 0.2:0.3, weighing a certain amount of reducing agent 1, 2-hexadecanediol, wherein the proportion relation between the theoretical value and the actual value of the using amount of the reducing agent is 1:4.
(2) Before the weighed seed crystal core is metallizedAdding precursor powder (an iron source and a platinum source) and a reducing agent 1, 2-hexadecanediol into a three-neck flask filled with a solvent hexadecylamine, wherein the molar ratio of the seed crystal core metal precursor to the solvent is 1:10. the content of Ar +7% in protective atmosphere 93 2 Under the action of the temperature, heating to 100 ℃ at the heating rate of 1 ℃/min, preserving the temperature for 120min, removing water, and then adding a surfactant (oleylamine + oleic acid) into the mixed solution, wherein the volume ratio of oleylamine: oleic acid =0.2:1; in terms of molar ratio, solvent: surfactant =10:1.0.
(3) Slowly heating the mixed solution to 280 ℃ at a heating rate of 10 ℃/min, preserving the temperature for 200min to obtain a black mixed solution, then cooling to 60 ℃, adding shell metal precursor powder manganese source manganese acetate and gallium source gallium acetylacetonate into the mixed solution, wherein the molar ratio of metal in the shell metal precursor powder to metal in the seed crystal core metal precursor powder is 1:0.5, the molar ratio of two metal ions in the shell metal precursor is 0.5:0.5.
(4) And heating the mixed solution to 280 ℃ at a heating rate of 10 ℃/min, then preserving the heat for 15min, and cooling to room temperature to obtain a black mixed solution.
Carrying out centrifugal cleaning by adopting two mixed solvents, wherein the mixed solvent A is absolute ethyl alcohol and chloroform according to the volume ratio of 5:1, wherein the mixed solvent B is deionized water and absolute ethyl alcohol in a volume ratio of 1:5, a mixed solvent; firstly, cleaning the mixed solution by using a mixed solvent A, wherein the mixed solvent A: the volume ratio of the mixed solution is 1:1, then carrying out centrifugal separation, and pouring out upper liquid after the centrifugal separation to obtain black powder; then cleaning the black powder by using a mixed solvent A, performing centrifugal separation, and repeating for 3 times; then, cleaning and centrifugally separating the black powder by adopting a mixed solvent B and a mixed solvent A in turn, and repeating for 3 times; finally, storing the black powder after the last cleaning and centrifugal separation in absolute ethyl alcohol; the rotating speed of the centrifugal machine for centrifugal separation is 6000-12000 rpm, and the time of each centrifugation is 10min.
Characterization of the product phase by X-ray diffractometry to be L1 0 MnGa containing ordered phase characteristic peaks (001), (110) and (002) and having an order degree of 0.91. Measuring hysteresis of product at room temperature using vibrating sample magnetometerLoop of coercive force H c At 1358.6Oe, the saturation magnetization Ms was 143.8emu/g. The morphology of the product is observed to be uniformly dispersed core-shell morphology by a field emission transmission electron microscope.
Example 17:
(1) Firstly, weighing iron source ferric sulfate and platinum source potassium chloroplatinate serving as core metal precursors of the seed crystal by using an electronic balance, wherein the molar ratio of the iron source ferric sulfate to the platinum source potassium chloroplatinate is 0.2:1, weighing a certain amount of reducing agent potassium borohydride, wherein the ratio of the theoretical value to the actual value of the amount of the reducing agent is 1:1.
(2) Adding weighed seed crystal core metal precursor powder (an iron source and a platinum source) and a reducing agent potassium borohydride into a three-neck flask filled with a solvent trioctylamine, wherein the molar ratio of the seed crystal core metal precursor to the solvent is 1:10. 95% in protective atmosphere Ar +5% 2 Under the action of the temperature, heating to 120 ℃ at the heating rate of 3 ℃/min, preserving the temperature for 100min, removing water, then adding a surfactant (brominated decahydrocarbon quaternary amine + oleic acid) into the mixed solution, and according to the volume ratio, brominating the decahydrocarbon quaternary amine: oleic acid =0.8:1; in terms of molar ratio, solvent: surfactant =10:4.1.
(3) Slowly heating the mixed solution to 320 ℃ at a heating rate of 7 ℃/min, preserving the temperature for 300min to obtain a black mixed solution, then cooling to 120 ℃, adding shell metal precursor powder iron source ferric chloride and cobalt source cobalt acetylacetonate into the mixed solution, wherein the molar ratio of metal in the shell metal precursor powder to metal in the seed crystal core metal precursor powder is 1:0.8, wherein the molar ratio of two metal ions in the shell metal precursor is 0.2:1.
(4) And (3) heating the mixed solution to 220 ℃ at the heating rate of 1 ℃/min, then preserving the heat for 60min, and cooling to room temperature to obtain a black mixed solution.
Carrying out centrifugal cleaning by adopting two mixed solvents, wherein the mixed solvent A is absolute ethyl alcohol and chloroform according to a volume ratio of 1:5, wherein the mixed solvent B is deionized water and absolute ethyl alcohol according to a volume ratio of 5:1, a mixed solvent; firstly, cleaning the mixed solution by using a mixed solvent A, wherein the mixed solvent A: the volume ratio of the mixed solution is 5:1, then carrying out centrifugal separation, and pouring out upper liquid after the centrifugal separation to obtain black powder; then cleaning the black powder by using a mixed solvent A, performing centrifugal separation, and repeating for 5 times; then cleaning and centrifugally separating the black powder by adopting a mixed solvent B and a mixed solvent A in turn, and repeating for 5 times; finally, storing the black powder after the last cleaning and centrifugal separation in absolute ethyl alcohol; the rotating speed of the centrifugal machine for centrifugal separation is 6000-12000 rpm, and the time for each centrifugation is 3-4 min.
Characterization of the product phase by X-ray diffractometry to be L1 0 FeCo, which contains ordered phase characteristic peaks (001), (110) and (002), with an order degree of 0.93. Measuring the magnetic hysteresis loop of the product at room temperature by a vibrating sample magnetometer, and the coercive force H of the product c It was 1434.5Oe and the saturation magnetization Ms was 120.7emu/g. The morphology of the product is observed to be uniformly dispersed core-shell morphology by a field emission transmission electron microscope.
Example 18:
(1) Firstly, weighing a seed crystal core metal precursor gold source chloroauric acid and a copper source copper acetylacetonate by using an electronic balance, wherein the molar ratio of the two precursors is 1:0.4, weighing a certain amount of reducing agent sodium borohydride, wherein the ratio of the theoretical value to the actual value of the using amount of the reducing agent is 1:3.
(2) Adding weighed seed crystal core metal precursor powder (a gold source and a copper source) and a reducing agent sodium borohydride into a three-neck flask filled with a solvent octadecylamine, wherein the molar ratio of the seed crystal core metal precursor to the solvent is 1:10. under the action of high-purity argon Ar in protective atmosphere, heating to 110 ℃ at a heating rate of 5 ℃/min, preserving heat for 30min, removing water, and then adding a surfactant (oleylamine + lecithin) into the mixed solution, wherein the volume ratio of oleylamine: lecithin =1:0.1; in terms of molar ratio, solvent: surfactant =10:3.8.
(3) Slowly heating the mixed solution to 360 ℃ at a heating rate of 9 ℃/min, preserving heat for 100min to obtain a black mixed solution, then cooling to 110 ℃, adding shell metal precursor powder iron source ferric chloride and cobalt source cobalt acetylacetonate into the mixed solution, wherein the molar ratio of metal in the shell metal precursor powder to metal in the seed crystal core metal precursor powder is 1:0.8, the molar ratio of two metal ions in the shell metal precursor is 1:0.9.
(4) Heating the mixed solution to 240 ℃ at a heating rate of 7 ℃/min, then preserving the heat for 10min, and cooling to room temperature to obtain a black mixed solution.
Carrying out centrifugal cleaning by adopting two mixed solvents, wherein the mixed solvent A is absolute ethyl alcohol and chloroform according to a volume ratio of 3:4, wherein the mixed solvent B is deionized water and absolute ethyl alcohol according to a volume ratio of 1:4 in a mixed solvent; firstly, cleaning the mixed solution by using a mixed solvent A, wherein the mixed solvent A: the volume ratio of the mixed solution is 2:1, then carrying out centrifugal separation, and pouring out upper liquid after the centrifugal separation to obtain black powder; then cleaning the black powder by using a mixed solvent A, carrying out centrifugal separation, and repeating for 3 times; then, cleaning and centrifugally separating the black powder by adopting a mixed solvent B and a mixed solvent A in turn, and repeating for 4 times; finally, storing the black powder after the last cleaning and centrifugal separation in absolute ethyl alcohol; the rotating speed of the centrifugal machine for centrifugal separation is 7000-10000 rpm, and the time for each centrifugation is 3-7 min.
Characterization of the product phase by X-ray diffractometry to be L1 0 FeCo, which contains ordered phase characteristic peaks (001), (110) and (002), with an order degree of 0.86. Measuring the magnetic hysteresis loop of the product at room temperature by using a vibrating sample strong magnetometer, and the coercive force H of the product c 952.8Oe, saturation magnetization Ms is 85.2emu/g. The morphology of the product is observed to be uniformly dispersed core-shell morphology by a field emission transmission electron microscope.
Example 19:
(1) Firstly, weighing seed crystal core metal precursors of manganese source manganese acetate and nickel source nickel acetylacetonate by using an electronic balance, wherein the molar ratio of the manganese source acetate to the nickel source nickel acetylacetonate is 1:0.1, weighing a certain amount of reducing agent 1, 2-hexadecanediol, wherein the proportion relation between the theoretical value and the actual value of the using amount of the reducing agent is 1:5.
(2) Adding weighed crystal seed core metal precursor powder (a manganese source and a nickel source) and a reducing agent 1, 2-hexadecanediol into a three-neck flask filled with a solvent icosamine, wherein the molar ratio of the crystal seed core metal precursor to the solvent is 1:10. high purity nitrogen N in protective atmosphere 2 Under the action of the water, the temperature is raised to 117 ℃ at the temperature rise rate of 7 ℃/min and is kept for 70min, the water removal treatment is carried out, and then the surfactant (oleylamine + mono-amine) is addedGlyceryl stearate) is added into the mixed solution, and the volume ratio of oleylamine: glycerol monostearate =1:0.5; in terms of molar ratio, solvent: surfactant =10:1.9.
(3) Slowly heating the mixed solution to 300 ℃ at the heating rate of 1 ℃/min, preserving the temperature for 20min to obtain a black mixed solution, then cooling to 90 ℃, adding shell metal precursor powder iron source ferric chloride and cobalt source cobalt acetylacetonate into the mixed solution, wherein the molar ratio of metal in the shell metal precursor powder to metal in the seed crystal core metal precursor powder is 1:0.8, wherein the molar ratio of two metal ions in the shell metal precursor is 1:0.2.
(4) And (3) heating the mixed solution to 260 ℃ at a heating rate of 5 ℃/min, then preserving the heat for 40min, and cooling to room temperature to obtain a black mixed solution.
And (2) carrying out centrifugal cleaning by adopting two mixed solvents, wherein the mixed solvent A is absolute ethyl alcohol and chloroform according to a volume ratio of 5:2, wherein the mixed solvent B is deionized water and absolute ethyl alcohol according to a volume ratio of 4:1; firstly, cleaning the mixed solution by using a mixed solvent A, wherein the mixed solvent A: the volume ratio of the mixed solution is 3:1, then carrying out centrifugal separation, and pouring out upper-layer liquid after the centrifugal separation to obtain black powder; then cleaning the black powder by using a mixed solvent A, carrying out centrifugal separation, and repeating for 4 times; then cleaning and centrifugally separating the black powder by adopting a mixed solvent B and a mixed solvent A in turn, and repeating for 5 times; finally, storing the black powder after the last cleaning and centrifugal separation in absolute ethyl alcohol; the rotating speed of the centrifugal machine for centrifugal separation is 7000-8000 rpm, and the time of each centrifugation is 5-7 min.
Characterization of the product phase by X-ray diffractometry to be L1 0 FeCo, which contains ordered phase characteristic peaks (001), (110) and (002), with an order degree of 0.93. Measuring the magnetic hysteresis loop of the product at room temperature by a vibrating sample magnetometer, and the coercive force H of the product c It was 1168.4Oe and the saturation magnetization Ms was 106.8emu/g. The morphology of the product is observed to be uniformly dispersed core-shell morphology by a field emission transmission electron microscope.
Example 20:
(1) Firstly, weighing iron source ferric chloride and platinum source chloroplatinic acid serving as seed crystal core metal precursors by using an electronic balance, wherein the molar ratio of the iron source ferric chloride to the platinum source chloroplatinic acid is 0.9:1, weighing a certain amount of reducing agent lithium aluminum hydride, wherein the proportional relation between a theoretical value and an actual value of the amount of the reducing agent is 1:3.
(2) Adding weighed crystal seed core metal precursor powder (an iron source and a platinum source) and a reducing agent lithium aluminum hydride into a three-neck flask filled with oleylamine, wherein the molar ratio of the crystal seed core metal precursor to the solvent is 1:10. ar +7% in a protective atmosphere of 93% 2 Under the action of the temperature, the temperature is raised to 105 ℃ at the temperature raising rate of 10 ℃/min and is kept for 50min, the water removing treatment is carried out, then, the surfactant (decahydroquaternary ammonium bromide + lecithin) is added into the mixed solution, and the volume ratio of the decahydroquaternary ammonium bromide: lecithin =1:0.1; in terms of molar ratio, solvent: surfactant =10:5.0.
(3) Slowly heating the mixed solution to 340 ℃ at a heating rate of 3 ℃/min, preserving heat for 30min to obtain a black mixed solution, then cooling to 70 ℃, adding shell metal precursor powder iron source ferric chloride and nickel source nickel nitrate into the mixed solution, wherein the molar ratio of metal in the shell metal precursor powder to metal in the seed crystal core metal precursor powder is 1:0.8, the molar ratio of two metal ions in the shell metal precursor is 0.9:1.
(4) And (3) heating the mixed solution to 265 ℃ at the heating rate of 4 ℃/min, preserving the heat for 60min, and cooling to room temperature to obtain a black mixed solution.
Carrying out centrifugal cleaning by adopting two mixed solvents, wherein the mixed solvent A is absolute ethyl alcohol and chloroform according to a volume ratio of 3:5, wherein the mixed solvent B is deionized water and absolute ethyl alcohol according to a volume ratio of 2:5 in a mixed solvent; firstly, cleaning the mixed solution by using a mixed solvent A, wherein the mixed solvent A: the volume ratio of the mixed solution is 4:1, then carrying out centrifugal separation, and pouring out upper-layer liquid after the centrifugal separation to obtain black powder; then cleaning the black powder by using a mixed solvent A, carrying out centrifugal separation, and repeating for 5 times; then cleaning and centrifugally separating the black powder by adopting a mixed solvent B and a mixed solvent A in turn, and repeating for 3 times; finally, storing the black powder after the last cleaning and centrifugal separation in absolute ethyl alcohol; the rotating speed of the centrifugal machine for centrifugal separation is 9000rpm, and the time of each centrifugation is 5-9 min.
Characterization of the product phase by X-ray diffractometry to be L1 0 FeNi, containing ordered phase characteristic peaks (001), (110) and (002), with an order degree of 0.93. Measuring the magnetic hysteresis loop of the product at room temperature by using a vibrating sample strong magnetometer, and the coercive force H of the product c 1069.5Oe and a saturation magnetization Ms of 86.5emu/g. The morphology of the product is observed to be uniformly dispersed core-shell morphology by a field emission transmission electron microscope.
Example 21:
(1) Firstly, weighing a seed crystal core metal precursor gold source potassium tetrachloroaurate and a copper source copper acetylacetonate by using an electronic balance, wherein the molar ratio of the gold source potassium tetrachloroaurate to the copper source copper acetylacetonate is 0.3:0.8, weighing a certain amount of reducing agent sodium cyanoborohydride, wherein the proportion relation between the theoretical value and the actual value of the reducing agent is 1:1.
(2) Adding weighed seed crystal core metal precursor powder (a gold source and a copper source) and a reducing agent sodium cyanoborohydride into a three-neck flask filled with a solvent hexadecylamine, wherein the molar ratio of the seed crystal core metal precursor to the solvent is 1:10. 95% in protective atmosphere Ar +5% 2 Under the action of the temperature, the temperature is raised to 113 ℃ at the temperature raising rate of 8 ℃/min and is kept for 60min, the water removing treatment is carried out, and then a surfactant (oleylamine + oleic acid) is added into the mixed solution according to the volume ratio, the oleylamine: oleic acid =0.8:1; in terms of molar ratio, solvent: surfactant =10:2.2.
(3) Slowly heating the mixed solution to 350 ℃ at a heating rate of 4 ℃/min, keeping the temperature for 120min to obtain a black mixed solution, then cooling to 80 ℃, adding shell metal precursor powder manganese source manganese acetylacetonate and gallium source gallium chloride into the mixed solution, wherein the metal molar ratio of the shell metal precursor powder to the seed crystal core metal precursor powder is 1:0.4, the molar ratio of two metal ions in the shell metal precursor is 0.5:1.
(4) And heating the mixed solution to 235 ℃ at a heating rate of 9 ℃/min, then preserving the heat for 50min, and cooling to room temperature to obtain a black mixed solution.
And (2) carrying out centrifugal cleaning by adopting two mixed solvents, wherein the mixed solvent A is absolute ethyl alcohol and chloroform according to a volume ratio of 2:3, wherein the mixed solvent B is deionized water and absolute ethyl alcohol according to a volume ratio of 3:2 in a mixed solvent; first, the mixed solution is washed by a mixed solvent a: the volume ratio of the mixed solution is 3.2:1, then carrying out centrifugal separation, and pouring out upper-layer liquid after the centrifugal separation to obtain black powder; then cleaning the black powder by using a mixed solvent A, performing centrifugal separation, and repeating for 3 times; then cleaning and centrifugally separating the black powder by adopting a mixed solvent B and a mixed solvent A in turn, and repeating for 5 times; finally, storing the black powder after the last cleaning and centrifugal separation in absolute ethyl alcohol; the rotating speed of the centrifugal machine for centrifugal separation is 7500-10000 rpm, and the time for each centrifugation is 6-9 min.
Characterization of the product phase by X-ray diffractometry to be L1 0 MnGa, which contains ordered phase characteristic peaks (001), (110) and (002), and has an order degree of 0.92. Measuring the magnetic hysteresis loop of the product at room temperature by using a vibrating sample strong magnetometer, and the coercive force H of the product c 1086.7Oe and a saturation magnetization Ms of 96.5emu/g. The morphology of the product is observed to be uniformly dispersed core-shell morphology by a field emission transmission electron microscope.
As can be seen from the above examples, L1 was successfully synthesized by using ordered nanoparticle interfacial induction 0 -FeCo、 L1 0 -FeNi、L1 0 -MnAl、L1 0 -MnGa nanomaterial, which has excellent dispersibility, high degree of order and excellent magnetic properties.

Claims (4)

1. Interface induction synthesis orderL1 0 A method of structuring permanent magnetic nanoparticles, comprising the steps of:
s1: weighing a seed crystal core metal precursor and a reducing agent;
s2: adding a seed crystal core metal precursor into a solvent, performing dehydration treatment under the action of a protective atmosphere, and adding a surfactant after the dehydration treatment to form a mixed solution; the solvent is hexadecylamine C 16 H 35 N, trioctylamine C 24 H 51 N, octadecylamine C 18 H 39 N, icosanamine C 20 H 43 One or more of N; the surfactant is decabromodecaHydrocarbon quaternary amine C 16 H 38 Br 2 N 2 Lecithin C 42 H 80 NO 8 P, glyceryl monostearate C 21 H 42 O 4 And oleic acid C 18 H 34 O 2 Mixing the two substances in the (1), wherein the two substances of the surfactant are mixed according to a volume ratio of (0.1 to 1): (0.1 to 1) and adding the mixture; the molar ratio of metal ions to solvent in the seed crystal core metal precursor is 1: (10 to 30), wherein the molar ratio of the solvent to the surfactant is 10: (1.0 to 5.0); said protective atmosphere being 93% Ar +7% 2 、95%Ar + 5%H 2 High purity nitrogen N 2 One kind of (1);
the method for dewatering treatment comprises the steps of heating to 100-120 ℃ at a heating rate of 1-10 ℃/min for 30-120 min under the action of a protective atmosphere;
s3: heating the mixed solution to a first reaction temperature, preserving heat, carrying out a reaction for generating a seed crystal core, cooling, weighing and adding a shell metal precursor; the first reaction temperature is 280-360 ℃, the heat preservation time is 30-300 min, and the cooling temperature is 60-90 ℃;
s4: heating the mixed solution to a second reaction temperature, preserving heat, carrying out a shell generation reaction, cooling to room temperature, and carrying out centrifugal cleaning on the mixed solution to obtain black powder, namely the ordered powderL1 0 Structural permanent magnetic nanoparticles; the second reaction temperature is 240 to 300 ℃, and the heat preservation time is 40 to 60min;
the seed crystal core metal precursor can form a highly ordered structureL1 0 Metal source mixture of two metals of a metal alloy capable of forming a highly ordered structureL1 0 The two metals of the metal alloy are AuCu, mnNi or FePt; the molar ratio of two metal ions in the seed crystal core metal precursor is (0.1-1): (0.1 to 1);
the shell metal precursor is structured to be prepared in orderL1 0 Metal source mixture of two metals of structured permanent magnetic nanoparticles, said composition constituting the order to be producedL1 0 Two metals of the structural permanent magnetic nano particle are FeCo, feNi, mnAl or MnGa; in the metal precursor of the housingThe molar ratio of the two metal ions is (0.2 to 1): (0.2 to 1);
the molar ratio of the total amount of metal ions in the shell metal precursor to the total amount of metal ions in the seed crystal core metal precursor is (0.4 to 1): (0.2 to 1);
the total adding amount of the reducing agent is not less than the theoretical adding amount, and the theoretical adding amount of the reducing agent is the adding amount of the reducing agent capable of completely reducing the seed crystal core metal precursor and the shell metal precursor;
in the step S3 and the step S4, the temperature of the mixed solution is raised to the reaction temperature, and the heating rate is 1 to 10 ℃/min.
2. The interface-induced synthetic order of claim 1L1 0 A method of structuring permanent magnetic nanoparticles, characterized by:
in the seed core metal precursor: the gold source is potassium tetrachloroaurate KAuCl 4 The copper source is copper acetate Cu (Ac) 2 Copper chloride (CuCl) 2 The manganese source is manganese acetate Mn (Ac) 2 Manganese chloride MnCl 2 Manganese acetylacetonate Mn (acac) 2 The nickel source is nickel acetate Ni (Ac) 2 Nickel nitrate Fe (NO) 3 ) 3 Nickel sulfate Fe 2 (SO 4 ) 3 Nickel chloride NiCl 2 Nickel acetylacetonate Ni (acac) 2 The iron source is one or more of ferric chloride FeCl 3 FeNO, iron nitrate 3 Iron (Fe) sulfate 2 (SO 4 ) 3 Fe acetylacetonate (acac) 3 One or more of (A), the platinum source is chloroplatinic acid H 2 PtCl 6 Platinum acetylacetonate Pt (acac) 2 Chloroplatinic acid K 2 PtCl 6 One or more of (a);
in the shell metal precursor: the iron source is ferric chloride FeCl 3 Fe acetylacetonate (acac) 3 C, iron oleate 54 H 99 FeO 6 One or more of the above; the cobalt source is cobalt acetylacetonate Co (acac) 2 Cobalt acetate Co (Ac) 2 One or more of the above; the nickel source is nickel acetate Ni (Ac) 2 Nickel nitrate Fe (NO) 3 ) 3 Nickel sulfate Fe 2 (SO 4 ) 3 Nickel chloride NiCl 2 Nickel acetylacetonate Ni (acac) 2 One or more of (a); the manganese source is manganese acetate Mn (Ac) 2 Manganese chloride MnCl 2 Manganese acetylacetonate Mn (acac) 2 One or more of (a); the aluminum source is aluminum chloride AlCl 3 Aluminum acetylacetonate Al (acac) 3 One or more of (a); the gallium source is gallium acetate Ga (Ac) 2 Gallium chloride GaCl 2 Ga acetylacetonate (acac) 2 One or more of (a).
3. The interface-induced synthetic ordering of claim 1L1 0 The method for preparing the structural permanent magnetic nano particle is characterized in that the reducing agent is potassium borohydride KBH 4 Sodium borohydride NaBH 4 Lithium aluminum hydride LiAlH, sodium cyanoborohydride CH 3 One or more of BNNa; the reducing agent is added by one of the following two methods:
the method A comprises the following steps: adding all reducing agents before the reaction of generating the seed crystal cores in the step S3;
the method B comprises the following steps: a first portion of the reducing agent is added before the seed core generation reaction of step S3, the first portion being added in an amount not less than the amount of the reducing agent capable of reducing the seed core metal precursor in its entirety, and a second portion of the remaining reducing agent is added before the shell generation reaction of step S4.
4. The interface-induced synthetic order of claim 1L1 0 The method for preparing the structural permanent magnetic nanoparticles is characterized in that the method for obtaining the black powder by centrifugally cleaning the mixed solution in the step S4 comprises the following steps:
carrying out centrifugal cleaning by adopting two mixed solvents, wherein the mixed solvent A is absolute ethyl alcohol and chloroform according to a volume ratio of (1 to 5): (5 to 1), wherein the mixed solvent B is deionized water and absolute ethyl alcohol in a volume ratio of (1 to 5): (5 to 1) a mixed solvent;
first, the mixed solution is washed by a mixed solvent a: the volume ratio of the mixed solution is (1 to 5): 1, then carrying out centrifugal separation, and pouring out upper liquid after the centrifugal separation to obtain black powder;
then cleaning the black powder by using a mixed solvent A, carrying out centrifugal separation, and repeating for 3 to 5 times;
then cleaning and centrifugally separating the black powder by adopting a mixed solvent B and a mixed solvent A in turn, and repeating for 3 to 5 times; finally, storing the black powder after the last cleaning and centrifugal separation in absolute ethyl alcohol;
the rotation speed of the centrifugal machine for centrifugal separation is 6000 to 12000rpm, and the time for each centrifugation is 3 to 10min.
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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005183898A (en) * 2003-09-12 2005-07-07 Fuji Photo Film Co Ltd Magnetic particle, method of producing the same, and magnetic recording medium
JP2007118147A (en) * 2005-10-28 2007-05-17 Toyota Motor Corp Method of manufacturing core/shell conjugated nanoparticle
CN102218543A (en) * 2011-05-20 2011-10-19 湖北大学 Method for one-step synthesis of FePt nanoparticles with an fct (face centered tetragonal) structure and product thereof
CN104625046A (en) * 2015-02-06 2015-05-20 南京大学 Manufacturing method of micrometer and nanometer composite spherical metal powder of core-shell structure
JP2016153519A (en) * 2015-02-20 2016-08-25 新日鉄住金化学株式会社 Metal composite particle and method for producing the same
CN108031840A (en) * 2018-01-15 2018-05-15 国家纳米科学中心 A kind of heterogeneous nano-superstructure of self-supporting metal and its preparation method and application

Family Cites Families (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6262129B1 (en) * 1998-07-31 2001-07-17 International Business Machines Corporation Method for producing nanoparticles of transition metals
KR100438408B1 (en) * 2001-08-16 2004-07-02 한국과학기술원 Method for Synthesis of Core-Shell type and Solid Solution type Metallic Alloy Nanoparticles via Transmetalation Reactions and Their Applications
JP2003257719A (en) * 2002-02-27 2003-09-12 Fuji Photo Film Co Ltd Method of manufacturing hard magnetic regular alloy phase nano-particle
US8133332B2 (en) * 2009-02-12 2012-03-13 Seagate Technology Llc Method for preparing FePt media at low ordering temperature and fabrication of exchange coupled composite media and gradient anisotropy media for magnetic recording
EP2842667B1 (en) * 2012-04-23 2017-11-22 LG Chem, Ltd. Method for producing core-shell particles
CN102699346A (en) * 2012-06-14 2012-10-03 西北工业大学 Chemical method for synthesizing L10-FePt by sequentially coating nanopowder nuclear body
CN105664951B (en) * 2016-02-18 2018-07-31 厦门大学 Cupro-nickel-zinc oxide compound nano crystalline substance photochemical catalyst and the preparation method and application thereof
CN112893834B (en) * 2021-01-20 2021-12-21 东北大学 L10-FePt @ PtBi2/Bi core-shell structure nano-particle and one-step synthesis method thereof

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005183898A (en) * 2003-09-12 2005-07-07 Fuji Photo Film Co Ltd Magnetic particle, method of producing the same, and magnetic recording medium
JP2007118147A (en) * 2005-10-28 2007-05-17 Toyota Motor Corp Method of manufacturing core/shell conjugated nanoparticle
CN102218543A (en) * 2011-05-20 2011-10-19 湖北大学 Method for one-step synthesis of FePt nanoparticles with an fct (face centered tetragonal) structure and product thereof
CN104625046A (en) * 2015-02-06 2015-05-20 南京大学 Manufacturing method of micrometer and nanometer composite spherical metal powder of core-shell structure
JP2016153519A (en) * 2015-02-20 2016-08-25 新日鉄住金化学株式会社 Metal composite particle and method for producing the same
CN108031840A (en) * 2018-01-15 2018-05-15 国家纳米科学中心 A kind of heterogeneous nano-superstructure of self-supporting metal and its preparation method and application

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
核壳结构双金属纳米粒子的研究与应用;王锐等;《化学进展》;20100324;第22卷;第358-366页 *

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