CN108691007B - Method for producing metal single crystal particle - Google Patents
Method for producing metal single crystal particle Download PDFInfo
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- CN108691007B CN108691007B CN201810577812.0A CN201810577812A CN108691007B CN 108691007 B CN108691007 B CN 108691007B CN 201810577812 A CN201810577812 A CN 201810577812A CN 108691007 B CN108691007 B CN 108691007B
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B1/00—Single-crystal growth directly from the solid state
- C30B1/02—Single-crystal growth directly from the solid state by thermal treatment, e.g. strain annealing
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/52—Alloys
Abstract
The invention provides a method for manufacturing metal single crystal particles, which comprises the following specific steps: 1) preparing metal particles; 2) uniformly mixing metal particles with an inert solid dispersing agent; 3) single crystallization treatment of metal particles: annealing the uniformly mixed powder at a temperature below the melting point of the metal to obtain metal single crystal particles, preferably at an annealing temperature in the range of 50 ℃ to 200 ℃ below the melting point of the metal; 4) removing the solid dispersing agent to obtain metal single crystal particle powder. The present invention separates metal particles with an inert solid dispersant and utilizes the strong growth ability of metal grains at high temperature to produce single crystal particles. If the metal particles are prepared in a spherical shape in step 1, spherical metal single crystal particles can be prepared by the subsequent step processes of the present invention. The present invention relates to the manufacture of single crystal particles of metals, including elemental metals, metal alloys, and metal compound materials.
Description
Technical Field
The invention relates to a method for manufacturing metal single crystal particles, which is suitable for the field of functional materials such as magnetic materials, shape memory alloys, semiconductor photoelectric materials, metal 3D printing and the like.
Background
The metal single crystal is a solid substance formed by periodically arranging structural units in a three-dimensional space, the complete ordered arrangement determines that the metal single crystal has good uniformity and strong anisotropy, and the metal single crystal has important application in the fields of functional materials such as shape memory alloys, high-performance soft magnetism, magnetostriction, semiconductor photoelectricity and the like. However, the preparation of large-size single crystal materials is often limited by the type of materials and the preparation process. Generally, the preparation process of the metal single crystal material is complex, the production cost is high, and the preparation of the single crystal material with large-size components and uniform performance is difficult. As an alternative method, metal single crystal powder can be prepared and made into a composite material with other materials, such as resin-based powder, and can exhibit physical properties similar to bulk single crystal materials. For example, by mixing ferromagnetic single crystal particles with a resin-based powder and then molding the mixture under a magnetic field, a high degree of orientation of the magnetic single crystal particles can be obtained, and the composite material can exhibit magnetic anisotropy similar to that of a single crystal material.
The existing preparation method of single crystal particles is a solvent-assisted method, which is a method for growing crystals from molten salt flux at high temperature, and each material needs to find a proper fluxing agent for growing single crystals. The cosolvent method can grow single crystal particles of metal compounds, but it is difficult to grow single crystal particles of elemental metals and alloys.
In addition, a mechanical crushing method is a commonly used method for producing metal single crystal particles. There are two main ways: first, mechanical breaking of ingots or rapid-set wafers: annealing the ingot or the rapid hardening crystal plate at high temperature to grow crystal grains, and obtaining single crystal particles by a mechanical crushing method, wherein the particles are irregular flaky; the second is melt drawing and mechanical crushing. Preparing ferromagnetic metal fibers from molten ferromagnetic metal melt by a wire drawing method, annealing at high temperature to grow crystal grains, and crushing the crystal grains into nodular single crystal particles. At present, the defects of the two methods for preparing the single crystal particles still exist, which are mainly reflected in that the metal types are limited, the proportion of the single crystal particles in the powder is not high enough, and the shapes of the particles are irregular. Mechanical crushing of an ingot or a rapidly solidified wafer and mechanical crushing of a melt by pulling out are both performed to obtain powder by using mechanical crushing, so that the kinds of metallic materials are limited, and materials having high brittleness such as metal compounds are required, and alloy solid solutions are not suitable for this method. In addition, although a magnetic intermetallic compound having a large brittleness is easily broken between crystals during mechanical crushing, a part of particles are broken in the crystal, and it is difficult to obtain a high proportion of single crystal particles in the powder. In addition, the powder after mechanical crushing has a large flaky shape and has sharp water chestnuts, and high density is difficult to obtain when the powder is mixed with other materials to prepare a composite material. If the particles are ferromagnetic metal single crystal particles, the flaky particles are greatly hindered by surrounding powder and a dispersing agent when the magnetic field is applied for orientation, unlike spherical particle powder, the rotational orientation of the particles when the magnetic field is applied is easy to realize, and high orientation degree is difficult to obtain.
Disclosure of Invention
The present invention is directed to a method for producing metal single crystal particles by mixing metal particles with an inert solid dispersing agent, separating the metal particles by the inert solid dispersing agent, annealing the mixture at a temperature lower than the melting point of the metal, and utilizing the property that the metal does not react with or diffuse into the solid dispersing agent, thereby producing metal single crystal particles having a strong ability to grow metal crystal grains at high temperatures. If the spherical metal particles are isolated from the inert solid dispersant, spherical metal single crystal particles can be prepared by the subsequent steps of the present invention.
The technical scheme of the invention is that the manufacturing method of the metal single crystal particles comprises the following steps:
(1) preparing metal particles;
(2) uniformly mixing metal particles with an inert solid dispersing agent;
(3) single crystallization treatment of metal particles: annealing the uniformly mixed powder at a temperature below the melting point of the metal to obtain single crystal particles;
(4) removing the solid dispersing agent to obtain metal single crystal particles.
The metal comprises copper, aluminum, gallium, tin, iron, cobalt, nickel, manganese, titanium, gold, silver and rare earth elementary metal; the alloy and intermetallic compound formed between two or more elementary metals, and the alloy and compound formed by the elementary metal or alloy and boron, silicon, carbon, sulfur, phosphorus, germanium, nitrogen and selenium nonmetal.
The step of preparing the metal particles includes obtaining metal particles of a desired size by mechanical crushing, atomization, shredding or punching remelting, droplet spraying, electrical discharge, plasma spheroidization, or by purchase.
The metal particles are less than 500 μm in size, with a preferred size range of 1 μm to 200 μm.
The metal particles are separated by an inert solid dispersant comprising carbon material powder (graphite, graphene, diamond, carbon powder, and the like, and mixtures thereof) or ceramic material powder (carbide ceramic, boride ceramic, oxide ceramic, nitride ceramic, and the like, and mixtures thereof). The step of mixing materials is that the metal particles and a solid dispersant are mechanically mixed or uniformly mixed by stirring in liquid (water, ethanol and the like) or uniformly mixed by the aid of the dispersant.
The solid dispersant may be any size smaller than the size of the metal particles, preferably in the size range of 1 μm to 100 μm, and may be in the form of a sheet, sphere, wire, tube or other shape.
The mass ratio of the metal particles to the dispersant is such that the metal particles are completely separated by the solid dispersant.
The step of annealing treatment to realize single crystallization of the metal particles comprises the following steps: 1) annealing the mixed powder of the metal particles and the solid dispersant in a high vacuum or atmosphere (including hydrogen, nitrogen, argon); 2) the annealing temperature is lower than the melting point of the metal particles, the preferred annealing temperature is in the range of 50-200 ℃ lower than the melting point of the metal, and the preferred annealing time is 0.5-5 hours; 3) a cooling mode: slow cooling or fast cooling.
The step of removing the solid dispersant to obtain metal single crystal particles comprises: 1) after soaking in liquid, carrying out ultrasonic cleaning for many times to remove the solid dispersing agent, and obtaining metal single crystal particles; 2) after soaking in liquid, obtaining metal single crystal particles by adopting a method of centrifugation, filtration or external magnetic field; 3) and separating the metal and the solid dispersing agent by using a wind power sorting method by utilizing the density difference of the metal and the solid dispersing agent to obtain metal single crystal particles.
The size of the metal single crystal particles is less than 500 μm. The size of the metal single crystal particles is preferably in the range of 1 μm to 200. mu.m.
Advantageous effects
The invention separates metal particles from inert solid dispersant, anneals at a temperature lower than the melting point of metal, and prepares single crystal particles by utilizing the strong growing ability of metal crystal grains at high temperature through the characteristic that metal and solid dispersant do not react and diffuse. According to the invention, the principle of preparing the metal single crystal particles is clear, the process method for preparing the metal single crystal particles is simple, the production efficiency is high, and the method is simple and feasible and can be used for producing the metal single crystal particles in a large scale. The size of the produced metal particles is less than 500 μm, and the size of the metal single crystal particles is preferably in the range of 1 μm to 200 μm. The metal particles have high single crystallinity, and can be widely applied to the fields of magnetic materials, shape memory alloys, semiconductor photoelectric materials, metal 3D printing and the like.
Drawings
FIG. 1 is a scanning electron microscope picture of CoMnSi intermetallic compound particles obtained by the manufacturing method of the present invention;
FIG. 2 magnetic field oriented and unoriented XRD of single crystal particles of CoMnSi intermetallic compound after mixing with epoxy resin.
FIG. 3 Ni obtained by the production method of the present invention2Scanning electron microscope pictures of MnGa alloy spherical particles;
FIG. 4 Ni2Mixing MnGa alloy spherical single crystal particles with epoxy resin, and then carrying out magnetic field orientation and non-orientation XRD;
Detailed Description
As described above, the inventors of the present application found that: the metal particles are mixed with an inert solid dispersant such that the metal particles are separated by the solid dispersant. Annealing at a certain temperature below the melting point of the metal, and preparing the single crystal particles by utilizing the strong growth capability of metal grains at high temperature through the characteristic that the metal does not react with and diffuse the solid dispersing agent. The method for producing the metal single crystal grains of the present invention will be described in detail below.
The present invention first prepares or purchases metal particles of a desired size. Method for preparing metal particles: 1) mechanical crushing, 2) atomization, 3) shredding or punching remelting, 4) droplet spraying, 5) electric spark, 6) plasma spheroidization, and 7) purchasing metal particles of desired size in addition to metal particles.
The metal particles are uniformly mixed with a solid dispersant of suitable size and quantity to achieve the purpose of separating the metal particles with the solid dispersant. The mixing method comprises the following steps: 1) uniformly mixing by adopting a mechanical method; 2) stirring and mixing in liquid (water, ethanol, etc.); 3) the uniform mixing is achieved by the dispersion aid of the dispersant.
Annealing the uniformly mixed metal/solid dispersant mixed powder, wherein the temperature is as follows: the temperature is lower than the melting point of the metal, and the preferred temperature is 50-200 ℃ lower than the melting point of the metal; a cooling mode: slow cooling or fast cooling.
Removing the solid dispersing agent in the annealed metal/solid dispersing agent to obtain metal single crystal particles. The cleaning method comprises the following steps: 1) in a liquid (e.g.: water or organic solvent, etc.), removing the solid dispersant by ultrasonic cleaning for many times by utilizing the density difference of the metal and the solid dispersant to obtain metal single crystal particles; 2) after soaking in liquid, obtaining metal single crystal particles by adopting a method of centrifugation, filtration or external magnetic field; 3) and separating the metal and the solid dispersing agent by using a wind power sorting method by utilizing the density difference of the metal and the solid dispersing agent to obtain metal single crystal particles.
The method for producing metal single crystal grains of the present invention is most suitable for metal single crystal grains having a size of 1 to 200 μm.
Example 1
Preparation of single crystal particles of CoMnSi intermetallic compound
The CoMnSi intermetallic compound (subscript is atomic percent) is obtained by a smelting method, and is mechanically crushed to obtain powder with the average size of about 10-50 mu m as a raw material. 2 g of CoMnSi intermetallic compound powder and magnesium oxide powder with the size of about 1 mu m are mixed according to the weight ratio of 1:3, and are mechanically stirred and then evenly mixed.
Putting the mixed CoMnSi intermetallic compound/magnesia powder into a quartz tube, and vacuumizing the quartz tube to 6 x 10-3And Pa, introducing argon to 0.06MPa, sealing the tube, putting the quartz tube filled with the mixed CoMnSi intermetallic compound/magnesium oxide powder under the protection of the argon into an annealing furnace for heating to 950 ℃, preserving heat for 2 hours, and cooling to room temperature at a cooling speed of 10 ℃/min.
Soaking the CoMnSi intermetallic compound/magnesium oxide mixed powder by using alcohol, and obtaining CoMnSi intermetallic compound particles by ultrasonic cleaning. FIG. 1 is a scanning electron micrograph of the resulting CoMnSi intermetallic compound particles, the particle size being in the range of 10 μm to 50 μm. FIG. 2 is a magnetic field orientation and non-orientation XRD of the particles after mixing with epoxy, and a comparison shows that the applied magnetic field achieves good orientation, indicating that the particles are single crystals. According to the method for producing metal particles of the present invention, it was confirmed that single crystal particles of a CoMnSi intermetallic compound can be obtained.
Example 2
Ni2Preparation of MnGa alloy single crystal particles
Obtaining Ni by smelting process2MnGa alloy (subscript is atomic percent) is mechanically crushed to obtain powder with the size of 40-80 mu m as a raw material. 2 g of Ni2The MnGa alloy powder and the alumina powder with the size of about 5 mu m are mixed according to the weight ratio of 1:3, and are mechanically stirred and then uniformly mixed. Mixing well Ni2Putting the MnGa alloy/alumina mixed powder into a quartz tube, and vacuumizing the quartz tube to 6 multiplied by 10-3Pa, introducing argon to 0.06MPa, sealing the tube, and filling Ni protected by argon2And putting the quartz tube of the MnGa alloy/alumina mixed powder into an annealing furnace heated to 1200 ℃, preserving heat for 8 minutes, cooling to 1000 ℃ at a cooling speed of 10 ℃/minute, preserving heat for 2 hours, and cooling to room temperature along with the furnace at a cooling speed of 10 ℃/minute.
Soaking Ni in alcohol2MnGa alloy/alumina mixed powder, combining ultrasonic cleaning and external magnetic field to make ferromagnetic Ni2Method for separating MnGa alloy particles from nonmagnetic alumina powder to obtain Ni2MnGa alloy spherical particles. FIG. 3 shows the Ni obtained2The scanning electron microscope picture of the MnGa alloy particles has the particle size of 40-80 mu m. FIG. 4 is a XRD, Ni, of magnetic field orientation and non-orientation of particles after mixing with epoxy resin2The crystal structure of the MnGa alloy particles is a non-modulated martensite phase, and after comparison, the external magnetic field can realize good orientation, which indicates that the particles are good single crystals. According to the method for producing metal particles of the present invention, it was confirmed that Ni could be obtained2MnGa alloy single crystal particles.
Example 3
Copper single crystal grain preparation
Spherical particles of metallic copper having an average size of about 10 μm were purchased as a raw material. 2 g of spherical metal copper particles and graphite powder with the size of about 0.5 mu m are mixed according to the weight ratio of 1:1, mechanically stirred and uniformly mixed. And (3) loading the mixed metal copper particle/graphite mixed powder into an alumina crucible, and feeding into an annealing furnace. The annealing furnace is vacuumized to 6 x 10-3Pa, heating the hearth to 900 ℃ at a heating speed of 20 ℃/min under vacuum, preserving heat for 3 hours, and cooling to room temperature along with the furnace.
And soaking the metal copper particle/graphite mixed powder in water, and carrying out ultrasonic cleaning to obtain copper spherical particles. The copper spherical particles were single crystalline as characterized by Electron Back Scattering Diffraction (EBSD). According to the method for producing metal particles of the present invention, it was confirmed that copper single crystal particles could be obtained.
Example 4
TiNi alloy single crystal particle preparation
TiNi shape memory alloy particles having an average size of about 40 μm were purchased as a raw material. Taking 2 g of alloy particles and boron nitride powder with the size of about 1 mu m, mixing the alloy particles and the boron nitride powder according to the weight ratio of 1:1, and mechanically stirring and uniformly mixing the alloy particles and the boron nitride powder. And (3) loading the mixed TiNi alloy particles/boron nitride mixed powder into an alumina crucible, and feeding into an annealing furnace. The annealing furnace is vacuumized to 6 x 10-3And Pa, introducing nitrogen to one atmosphere, heating the hearth to 1120 ℃ at a heating speed of 20 ℃/min, preserving heat for 3 hours, and cooling to room temperature along with the furnace.
Soaking the TiNi alloy particles/boron nitride mixed powder in alcohol, and carrying out ultrasonic cleaning to obtain the TiNi alloy particles. The TiNi alloy particles were single crystalline as characterized by Electron Back Scattering Diffraction (EBSD). According to the method for producing metal particles of the present invention, it was confirmed that single crystal particles of a TiNi alloy could be obtained.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and it should be understood that any modification and improvement made by those skilled in the art within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. A method for producing metal single crystal particles, comprising the steps of:
(1) preparing metal particles;
(2) uniformly mixing metal particles with an inert solid dispersing agent;
(3) single crystallization treatment of metal particles: annealing the uniformly mixed powder at a temperature below the melting point of the metal to obtain single crystal particles, wherein the annealing temperature is in the range of 50-200 ℃ below the melting point of the metal, and the annealing time is 0.5-5 hours;
(4) removing the solid dispersing agent to obtain metal single crystal particles;
the metal comprises copper, aluminum, gallium, tin, iron, cobalt, nickel, manganese, titanium, gold, silver and rare earth elementary metal; alloys and intermetallic compounds formed between two or more elementary metals, and alloys and compounds formed by the elementary metals or the alloys and nonmetal of boron, silicon, carbon, sulfur, phosphorus, germanium, nitrogen or selenium;
the step of preparing said metal particles comprises obtaining metal particles of a desired size by mechanical crushing, atomization, shredding or punching remelting, droplet spraying, electrical discharge, plasma spheroidization or by purchasing;
the metal particle size is less than 500 microns;
separating the metal particles with an inert solid dispersant comprising carbon material powder of graphite, graphene, diamond, carbon powder or mixtures thereof, or ceramic material powder comprising carbide ceramic, boride ceramic, oxide ceramic, nitride ceramic or mixtures thereof; the step of mixing materials is that the metal particles and a solid dispersant are mechanically mixed or are uniformly mixed by stirring in water and ethanol liquid or are uniformly mixed by the aid of the dispersion of the solid dispersant;
the solid dispersing agent is in any size smaller than the size of the metal particles, the size range is 1-100 micrometers, and the shape of the solid dispersing agent is sheet, spherical, linear or tubular.
2. The method for producing metal single crystal particles according to claim 1, wherein: the size range of the metal particles is 1-200 microns.
3. The method for producing metal single crystal particles according to claim 1, wherein: the mass ratio of the metal particles to the solid dispersing agent is such that the metal particles can be completely separated by the solid dispersing agent.
4. A method for producing metal single crystal particles according to any one of claims 1 to 3, characterized in that: the step of annealing treatment to realize single crystallization of the metal particles comprises the following steps: 1) annealing the mixed powder of the metal particles and the solid dispersant in a high vacuum or an atmosphere including hydrogen, nitrogen, or argon; 2) the annealing temperature is 50-200 deg.C lower than the melting point of the metaloC, annealing time is 0.5-5 hours; 3) a cooling mode: slow cooling or fast cooling.
5. The method for producing metal single crystal particles according to claim 1, wherein: the step of removing the solid dispersant to obtain metal single crystal particles comprises: 1) after soaking in liquid, carrying out ultrasonic cleaning for many times to remove the solid dispersing agent, and obtaining metal single crystal particles; 2) after soaking in liquid, obtaining metal single crystal particles by adopting a method of centrifugation, filtration or external magnetic field; 3) and separating the metal and the solid dispersing agent by using a wind power sorting method by utilizing the density difference of the metal and the solid dispersing agent to obtain metal single crystal particles.
6. The method for producing metal single crystal particles according to any one of claims 1 to 3 or 5, characterized in that: the size of the metal single crystal particles is less than 500 microns.
7. The method for producing metal single crystal particles according to claim 6, wherein: the size of the metal single crystal particles is in the range of 1-200 microns.
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| CN111326303A (en) * | 2020-03-04 | 2020-06-23 | 南京大学 | Method for manufacturing rare earth alloy spherical single crystal magnetic powder and <111> oriented rare earth giant magnetostrictive material |
| WO2023153943A1 (en) * | 2022-02-09 | 2023-08-17 | Auckland Uniservices Limited | High-entropy oxides |
| CN116550975B (en) * | 2023-07-04 | 2023-09-26 | 赣州金顺科技有限公司 | Preparation method of diamond/copper composite material |
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