WO2020228709A1 - Method for preparing alloy powder material - Google Patents

Abstract

The present invention relates to a method for preparing alloy powder material. Using the feature of an alloy solidification structure containing a matrix phase and an inert dispersed particle phase, the matrix phase is removed by reaction with an acid solution, so that the dispersed particle phase is separated to obtain the alloy powder material. The method is simple in process, and can prepare a variety of alloy powder materials with different morphologies including nanometer, submicrometer, micrometer and millimeter level, which has good application prospects in the fields including catalysis, powder metallurgy, and 3D printing.

Description

Method for preparing alloy powder material Technical field

The invention relates to the technical field of metal materials, in particular to a method for preparing alloy powder materials.

Background technique

Micro-nano particle size alloy powder, due to its special surface effect, quantum size effect, quantum tunneling effect and Coulomb blocking effect, exhibits many unique properties different from traditional materials in optics, electricity, magnetism, catalysis, etc. Therefore, it is widely used in many fields such as optoelectronic devices, wave absorbing materials, and high-efficiency catalysts.

At present, the preparation methods of ultra-fine alloy powder are classified into solid phase method, liquid phase method and gas phase method from the state of matter. The solid phase method mainly includes mechanical crushing method, ultrasonic crushing method, thermal decomposition method, explosion method and so on. Liquid phase methods mainly include precipitation method, alkoxide method, carbonyl method, spray thermal drying method, freeze drying method, electrolysis method, chemical coagulation method, etc. The gas phase method mainly includes gas phase reaction method, plasma method, high temperature plasma method, evaporation method, chemical vapor deposition method, etc. Although there are many methods for preparing ultrafine alloy powders, each method has certain limitations. For example, the shortcomings of the liquid phase method are low yield, high cost, and complicated process. The disadvantage of the mechanical method is that it is difficult to classify after preparing the powder, and the purity, fineness and morphology of the product are difficult to guarantee. Rotating electrode method and gas atomization method are currently the main methods for preparing high-performance alloy powder, but the production efficiency is low, the yield of ultrafine powder is not high, and the energy consumption is relatively large; jet milling method and hydrogenation dehydrogenation method are suitable for large Industrial production in batches, but with strong selectivity to raw metals and alloys. Therefore, it is of great significance to develop new preparation methods for ultrafine alloy powder materials.

Summary of the invention

technical problem

The solution to the problem

Technical solutions

Based on this, it is necessary to provide a method for preparing alloy powder material with simple process and easy operation in response to the above technical problems.

A preparation method of alloy powder material includes the following steps:

Provide (M _x T _y ) _a RE _b alloy, wherein M is selected from at least one of Fe, Co, Ni, and T is selected from W, Cr, Mo, V, Ta, Nb, Zr, Hf, Ti At least one, RE is selected from at least one of Y, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, x, y, and a, b respectively represents the atomic percentage content of the corresponding composition, and 33%≤x≤75%, x+y=100%; 0.1%≤a≤40%, a+b=100%, the (MxTy) _a RE _b alloy The solidification structure of the is composed of a dispersed particle phase with a composition of M _x T _y and a matrix phase with a composition mainly of RE;

The (M _x T _y ) _a RE _b alloy is mixed with an acid solution, the matrix phase reacts with the acid solution to become ions into the solution, and the dispersed particle phase separates out, that is, M _x T _y Composition of alloy powder material.

Further, the (M _x T _y ) _a RE _b alloy is obtained in the following manner:

Weigh the alloy raw materials according to the ratio;

Fully melting the alloy raw materials to obtain an alloy melt;

The alloy melt is prepared into the (M _x T _y ) _a RE _b alloy by a solidification method, wherein the solidification rate of the alloy melt is 0.001 K/s to 10 ⁷ K/s.

Further, the vacuum degree during the melting of the alloy melt is 1×10 ^-4 Pa to 1.01325×10 ⁵ Pa.

Further, the particle shape of the dispersed particle phase includes at least one of a dendritic shape, a spherical shape, a nearly spherical shape, a square shape, a pie shape, and a rod shape, and the particle size of the dispersed particle phase is 2 nm to 100 mm.

Further, the acid in the acid solution is at least one of sulfuric acid, hydrochloric acid, nitric acid, perchloric acid, phosphoric acid, acetic acid, oxalic acid, formic acid, carbonic acid, gluconic acid, oleic acid, and polyacrylic acid. The solvent in the acid solution It is water, ethanol, methanol or a mixture of the three in any ratio.

Further, the molar concentration of the acid in the acid solution is 0.001 mol/L to 5 mol/L.

Further, in the step of reacting the (M _x T _y ) _a RE _b alloy with the acid solution, the reaction time is 0.1 min to 48 h, and the reaction temperature is 0°C to 100°C.

Further, the particle size of the M _x T _y alloy powder material is 2 nm to 100 mm.

Further, after the step of reacting the (M _x T _y ) _a RE _b alloy with the acid solution, the following step is further performed: the obtained alloy powder material with a particle size range of 1 μm to 1 mm is sieved, Plasma spheroidization is performed respectively, and finally alloy powder materials with different particle sizes and spherical shapes are obtained.

Further, the particle size of the spherical alloy powder material with different particle diameters is 1 μm to 1 mm.

In the preparation method of the alloy powder material of the present invention, a (M _x T _y ) _a RE _b alloy made of a specific type and content of metal M, metal T and rare earth RE is selected. The solidified structure of the alloy is composed of a dispersed particle phase with a composition of M _x T _y and a matrix phase with a composition mainly of RE. The structure is conducive to subsequent separation. Specifically, when the (M _x T _y ) _a RE _b alloy subsequently reacts with the dilute acid solution, the matrix phase reacts with the H ions in the acid solution to become ions into the solution, and the composition is a dispersed particle phase of M _x T _y It is difficult to react with the dilute acid solution, so that it can be dispersed and separated from the (M _x T _y ) _a RE _b alloy, and finally the M _x T _y alloy powder material is obtained.

In addition, rare earth elements not only have a good "absorbing" effect on oxygen, but also have a good "absorbing" effect on other various impurity elements in the alloy raw materials M and T. Therefore, the dispersed particle phase in the (M _x T _y ) _a RE _b alloy and the obtained M _x T _y alloy powder material tend to have higher purity than the raw materials M and T.

The method has low cost and simple operation, and can prepare various alloy powder materials with different morphologies including nanometer, submicrometer, micrometer and millimeter level. The alloy powder material has good application prospects in hydrogen storage, catalysis, powder metallurgy, 3D printing and other fields.

The beneficial effects of the invention

Brief description of the drawings

Description of the drawings

Figure 1 is a scanning electron micrograph of CoTi dendrites prepared in Example 1 of the present invention;

Fig. 2 is a high magnification photograph of the CoTi dendrites prepared in Example 1 of the present invention;

FIG. 3 is an energy spectrum diagram of CoTi dendrites prepared in Example 1 of the present invention.

Invention embodiment

Embodiments of the invention

The present invention will be further described in detail below with reference to the accompanying drawings and embodiments. It should be pointed out that the following embodiments are intended to facilitate the understanding of the present invention and do not have any limiting effect on it.

The method for preparing alloy powder material provided by the present invention includes the following steps:

S1, providing (M _x T _y ) _a RE _b alloy, wherein M is selected from at least one of Fe, Co, and Ni, and T is selected from W, Cr, Mo, V, Ta, Nb, Zr, Hf, Ti At least one of, RE is selected from at least one of Y, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, x, y, and a and b respectively represent the atomic percentage content of the corresponding composition, and 33%≤x≤75%, x+y=100%; 0.1%≤a≤40%, a+b=100%, the (MxTy) _a RE The solidification structure of _b alloy consists of a dispersed grain phase with a composition of M _x T _y and a matrix phase with a composition mainly of RE;

S2, mixing the (M _x T _y ) _a RE _b alloy with an acid solution, so that the matrix phase reacts with the acid solution to become ions into the solution, and the dispersed particle phase is separated, and the resulting M _x Alloy powder material composed of _Ty .

In step S1, the (M _x T _y ) _a RE _b alloy is obtained in the following manner:

(1) Weigh the alloy raw materials according to the ratio;

(2) Fully melt the alloy raw materials to obtain an alloy melt;

(3) The alloy melt is prepared into the (M _x T _y ) _a RE _b alloy by a solidification method, wherein the solidification rate of the alloy melt is 0.001 K/s to 10 ⁷ K/s.

In step (1), the raw materials required for smelting (M _x T _y ) _a RE _b alloy are prepared according to a specific composition and content.

In step (2), due to the presence of a large amount of rare earth elements in the alloy melt obtained by melting the alloy raw materials, even if oxygen enters the alloy melt during the smelting process, all oxygen will be quickly "absorbed" by the rare earth elements, forming a coating The dense rare earth oxide protective film on the surface of the alloy melt blocks the passage of oxygen from further entering the alloy melt. Therefore, even if the alloy is smelted under low vacuum conditions or even atmospheric conditions, the dispersed particles in the solidified structure of the alloy will still not be contaminated by oxygen. Therefore, when the vacuum degree in the melting process of the alloy melt is 1×10 ^-4 Pa˜1.01325×10 ⁵ Pa, the purity of the obtained dispersed particle phase can still be guaranteed.

In addition, rare earth elements not only have a good "absorbing" effect on oxygen, but also have a good "absorbing" effect on other various impurity elements in the alloy raw materials M and T. Therefore, the dispersed particle phase in the (M _x T _y ) _a RE _b alloy tends to have higher purity than the raw materials M and T.

It can be understood that if the alloy raw materials are metal M, metal T and rare earth RE, each element can be melted to prepare an alloy melt. If the alloy raw materials provided are directly (M _x T _y ) _a RE _b alloy, the (M _x T _y ) _a RE _b alloy can be remelted to obtain an alloy melt. Of course, it is also possible to melt the metal M, the metal T and the rare earth RE into a (M _x T _y ) _a RE _b alloy, and then remelt the (M _x T _y ) _a RE _b alloy to obtain an alloy melt.

In step (3), the solidified structure of the alloy melt is composed of a dispersed particle phase composed of M _x T _y and a matrix phase composed mainly of RE. Among them, the dispersed particle phase of the component M _x T _y is an inert component under the action of dilute acid, and it is difficult to react with acid; the matrix phase mainly composed of RE is an active component, which is very easy to react with acid. Therefore, the solidified structure of the (M _x T _y ) _a RE _b alloy facilitates subsequent separation.

Specifically, the solidification method is not limited, and may be methods such as casting, melt stripping, and melt drawing. The particle size and morphology of the finally formed alloy powder material is basically consistent with the particle size and morphology of the M _x T _y dispersed particle phase in the (M _x T _y ) _a RE _b alloy. The particle size of the M _x T _y dispersed particle phase is related to the solidification rate of the alloy melt during the preparation process. Generally speaking, the particle size of the M _x T _y dispersed particle phase has a negative correlation with the cooling rate of the alloy melt, that is, the greater the solidification rate of the alloy melt, the smaller the particle size of the dispersed particle phase. Wherein, the solidification rate of the alloy melt may be 0.001 K/s to 10 ⁷ K/s, and the particle size of the M _x T _y dispersed particle phase may be 2 nm to 100 mm.

The particle shape of the dispersed particle phase is not limited, and may include at least one of a dendritic shape, a spherical shape, a nearly spherical shape, a square shape, a pie shape, and a rod shape. When the particle shape is rod-shaped, the particle size specifically refers to the diameter of the rod-shaped cross-section.

In step S2, the acid solution is a solution containing H ⁺ . Because (M _x T _y ) _a RE _b alloy solidification structure is composed of a dispersed grain phase with a composition of M _x T _y and a matrix phase with a composition mainly of RE. Therefore, the H ⁺ in the dilute acid solution reacts with the rare earth elements in the matrix phase to dissolve the rare earth elements into ions and enter the solution, while the M _x T _y dispersed particle phase, which is difficult to react with the dilute acid solution, is removed from the original alloy Disperse out of it. After cleaning, the M _x T _y alloy powder material is obtained. The particle size of the alloy powder material can be nanometer, submicrometer, micrometer, or even millimeter.

Specifically, the acid in the acid solution may be at least one of sulfuric acid, hydrochloric acid, nitric acid, perchloric acid, phosphoric acid, acetic acid, oxalic acid, formic acid, carbonic acid, gluconic acid, oleic acid, and polyacrylic acid, preferably sulfuric acid, hydrochloric acid , At least one of nitric acid, perchloric acid, phosphoric acid, acetic acid, and oxalic acid. The solvent in the acid solution is water, ethanol, methanol or a mixture thereof mixed in any ratio.

The concentration of the dilute acid in the acid solution is not specifically limited, as long as it can react with the matrix phase and retain the primary crystal phase. The reaction time is not limited, and the reaction temperature is not limited. Preferably, the molar concentration of the acid in the acid solution may be 0.001 mol/L to 5 mol/L. The reaction time of this reaction can be 0.1min～48h, and the reaction temperature can be 0℃～100℃.

Further, after step S2, if the particle size of the obtained alloy powder material is in the range of 1 μm to 1 mm, the following steps may be performed: the obtained alloy powder material is sieved, and plasma spheroidization is performed respectively, and finally A spherical alloy powder material with different particle sizes is obtained.

The powder material after the screening can be spheroidized by plasma spheroidization.

The particle diameter of the spherical alloy powder material with different particle diameters is 1 μm to 1 mm.

Therefore, the method has low cost and simple operation, and can prepare a variety of alloy powder materials with different morphologies including nanometer, submicrometer, micrometer and millimeter level. The alloy powder material has good application prospects in hydrogen storage, catalysis, powder metallurgy, 3D printing and other fields.

The following will further illustrate through various embodiments.

Example 1:

This embodiment provides a method for preparing micron-sized CoTi powder, which includes the following steps:

(1) Select the alloy with the formula formula (Co ₅₀ Ti ₅₀ ) ₂₅ Gd ₇₅ , weigh the raw materials according to the formula, and fully smelt the (Co ₅₀ Ti ₅₀ ) ₂₅ Gd ₇₅ alloy under the vacuum condition of 10 ^-2 Pa. The melt is poured into a copper mold with an inner cavity cross-sectional dimension of 4mm×6mm, and a (Co ₅₀ Ti ₅₀ ) ₂₅ Gd ₇₅ alloy sheet with a size of 4mm×6mm×30mm is prepared by casting at a cooling rate of about 75K/s. The alloy solidification structure includes dispersed dendritic particles composed of CoTi and a matrix phase composed of Gd, and the size of the CoTi dendritic particles ranges from 2 μm to 40 μm.

(2) At room temperature, 0.5 g of the (Co ₅₀ Ti ₅₀ ) ₂₅ Gd ₇₅ alloy sheet prepared in step (1) was immersed in 300 mL of a 0.2 mol/L dilute hydrochloric acid aqueous solution for reaction. During the reaction process, the matrix phase composed of Gd reacts with dilute hydrochloric acid and enters the solution, while the CoTi dendritic particles that are difficult to react with dilute hydrochloric acid are gradually separated from the matrix and dispersed. After 20 minutes, the obtained CoTi dendritic particles are separated from the solution, washed and dried to obtain micron-sized CoTi dendritic powder, and the size of the dendritic particles ranges from 5 μm to 40 μm.

The alloy powder material was tested by scanning electron microscopy. As shown in Figure 1 and Figure 2, the alloy powder particles were in dendrite shape.

As shown in Figure 3, almost no other elements can be detected on the energy spectrum of the CoTi powder material, and its composition is about Co ₅₀ Ti ₅₀ .

Example 2:

This embodiment provides a method for preparing spherical micron-sized CoTi powder, which includes the following steps:

(1) Select the alloy with the formula formula (Co ₅₀ Ti ₅₀ ) ₂₅ Gd ₇₅ , weigh the raw materials according to the formula, and fully smelt the (Co ₅₀ Ti ₅₀ ) ₂₅ Gd ₇₅ alloy under the vacuum condition of 10 ^-2 Pa. The melt is poured into a copper mold with an inner cavity cross-sectional dimension of 4mm×6mm, and a (Co ₅₀ Ti ₅₀ ) ₂₅ Gd ₇₅ alloy sheet with a size of 4mm×6mm×30mm is prepared by casting at a cooling rate of about 75K/s. The alloy solidification structure includes dispersed dendritic particles composed of CoTi and a matrix phase composed of Gd, and the size of the CoTi dendritic particles ranges from 2 μm to 40 μm.

(2) At room temperature, 0.5 g of the (Co ₅₀ Ti ₅₀ ) ₂₅ Gd ₇₅ alloy sheet prepared in step (1) was immersed in 300 mL of a 0.2 mol/L dilute hydrochloric acid aqueous solution for reaction. During the reaction process, the matrix phase composed of Gd reacts with dilute hydrochloric acid and enters the solution, while the CoTi dendritic particles that are difficult to react with dilute hydrochloric acid are gradually separated from the matrix and dispersed. After 20 minutes, the obtained CoTi dendritic particles are separated from the solution, washed and dried to obtain micron-sized CoTi dendritic powder, and the size of the dendritic particles ranges from 2 μm to 40 μm.

Collect 0.5 kg of the micron-sized CoTi dendritic powder prepared in step (2), and sieving through 540 mesh, 1000 mesh, and 2000 mesh sieve. The dendrite size ranges are >26μm, 26μm-13μm, 13μm～ Graded CoTi dendritic powder of 6.5μm and less than 6.5μm. The CoTi dendritic powders with dendrite diameters ranging from 26μm to 13μm and 13μm to 6.5μm are selected respectively, and spherical Co ₅₀ Ti with particle sizes ranging from 26μm to 13μm and 13μm to 6.5μm are further prepared through mature plasma spheroidization technology. ₅₀ powder.

Example 3:

This embodiment provides a method for preparing nano-scale CoHf powder, including the following steps:

(1) Select the alloy with the formula formula (Co ₅₀ Hf ₅₀ ) ₂₅ Y ₇₅ , weigh the raw materials according to the formula, and fully smelt the (Co ₅₀ Hf ₅₀ ) ₂₅ Y ₇₅ alloy under the vacuum condition of 10 ^-2 Pa. The melt is used to prepare (Co ₅₀ Hf ₅₀ ) ₂₅ Y ₇₅ alloy strips with a thickness of 20-30 μm at a cooling rate of 10 ⁵ -10 ⁶ K/s through the melt stripping method. The solidified structure of the alloy strip is composed of nearly spherical dispersed particles with a composition of CoHf and a matrix phase with a composition of Y, and the size of the dispersed particles of CoHf is in the range of 10-200 nm.

(2) At room temperature, 0.5 g of the (Co ₅₀ Hf ₅₀ ) ₂₅ Y ₇₅ alloy strip prepared in step (1) is immersed in 300 mL of a 0.2 mol/L dilute sulfuric acid aqueous solution for reaction. During the reaction, the matrix phase composed of Y reacts with dilute sulfuric acid and enters the solution, while the CoHf nanoparticles that are difficult to react with dilute sulfuric acid are gradually separated from the matrix and dispersed. After 5 minutes, the obtained CoHf nanoparticles are separated from the solution, washed and dried to obtain nano-sized nearly spherical CoHf powder, the size of which is in the range of 10-200 nm.

Example 4:

This embodiment provides a method for preparing spherical micron CoCrMo powder, which includes the following steps:

(1) Choose the alloy with formula formula (Co ₆₃ Cr ₃₃ Mo ₄ ) ₂₅ Gd ₇₅ , weigh the raw materials according to the formula, and fully smelt (Co ₆₃ Cr ₃₃ Mo ₄ ) ₂₅ Gd ₇₅ alloy under vacuum conditions of 10 ^-2 Pa , Pour the alloy melt into a copper mold with a cavity cross-sectional dimension of 4mm×6mm, and cast at a cooling rate of about 75K/s to prepare (Co ₆₃ Cr ₃₃ Mo ₄ ) _{25 with} a size of 4mm×6mm×30mm The alloy solidification structure of the Gd ₇₅ alloy sheet includes dispersed dendritic particles composed of Co-Cr-Mo and a matrix phase composed of Gd, and the size of the Co-Cr-Mo dendritic particles ranges from 3 μm to 50 μm.

(2) At room temperature, 0.5 g of the (Co ₆₃ Cr ₃₃ Mo ₄ ) ₂₅ Gd ₇₅ alloy sheet prepared in step (1) was immersed in 300 mL of a 0.2 mol/L dilute hydrochloric acid aqueous solution for reaction. During the reaction, the matrix phase composed of Gd reacts with dilute hydrochloric acid and enters the solution, while the Co-Cr-Mo dendritic particles that are difficult to react with dilute hydrochloric acid are gradually separated from the matrix and dispersed. After 20 minutes, the obtained Co-Cr-Mo dendritic particles were separated from the solution, washed and dried, and then micron-sized Co-Cr-Mo dendritic powder was obtained, the composition of which was approximately Co ₆₃ Cr ₃₃ Mo ₄ , dendritic particles The size range of 3μm ~ 50μm.

Collect 0.5 kg of the micron-sized Co-Cr-Mo dendritic powder prepared in step (2), and sieving through 540 mesh, 1000 mesh, and 2000 mesh sieve. The dendrite size ranges are> 26 μm, 26 μm ~ Graded Co-Cr-Mo dendritic powder of 13μm, 13μm～6.5μm and less than 6.5μm. Co-Cr-Mo dendritic powders with dendrite particle sizes ranging from 26μm to 13μm and 13μm to 6.5μm are selected, and the particle size ranges from 26μm to 13μm and 13μm to 6.5μm are further prepared by mature plasma spheroidizing technology. Spherical Co ₆₃ Cr ₃₃ Mo ₄ powder.

Example 5:

This embodiment provides a method for preparing sub-micron CoTiHf powder, which includes the following steps:

(1) Select the alloy with formula formula (Co ₅₀ Ti ₂₅ Hf ₂₅ ) ₂₀ (Gd ₅₀ Y ₅₀ ) ₈₀ , weigh the raw materials according to the formula, and fully smelt it under 10 ^-2 Pa vacuum conditions (Co ₅₀ Ti ₂₅ Hf ₂₅ ) ₂₀ (Gd ₅₀ Y ₅₀ ) ₈₀ alloy, the alloy melt is prepared by melt ribbon spinning at a cooling rate of ~10 ⁴ K/s to prepare (Co ₅₀ Ti ₂₅ Hf ₂₅ ) ₂₀ (Gd ₅₀ Y ₅₀ ) ₈₀ alloy strip. Size range of the alloy strip the solidification structure of a nearly spherical component Co ₅₀ Ti ₂₅ Hf ₂₅ dispersed particles and the matrix component is a Gd ₅₀ Y ₅₀ phase composition, and the Co ₅₀ Ti ₂₅ Hf ₂₅ dispersed particles is 100-800nm.

(2) At room temperature, 0.5 g of the (Co ₅₀ Ti ₂₅ Hf ₂₅ ) ₂₀ (Gd ₅₀ Y ₅₀ ) ₈₀ alloy sheet prepared in step (1) is immersed in 300 mL of a 0.2 mol/L dilute sulfuric acid aqueous solution for reaction. During the reaction process, the matrix phase composed of GdY reacts with dilute sulfuric acid into the solution, and the submicron Co ₅₀ Ti ₂₅ Hf ₂₅ particles that are difficult to react with dilute sulfuric acid are gradually separated from the matrix and dispersed. After 10 minutes, the obtained Co ₅₀ Ti ₂₅ Hf ₂₅ sub-micron particles are separated from the solution, washed and dried to obtain nearly spherical Co ₅₀ Ti ₂₅ Hf ₂₅ sub-micron alloy powder, the particle size range is 100-800 nm.

Example 6:

This embodiment provides a method for preparing micro-nano CoTiZr powder, which includes the following steps:

(1) Choose the alloy with formula formula (Co ₅₀ Ti ₂₅ Zr ₂₅ ) ₃₀ Y ₇₀ , weigh the raw materials according to the formula, and obtain (Co ₅₀ Ti ₂₅ Zr ₂₅ ) ₃₀ Y after arc melting under 10 ^-2 Pa vacuum conditions ₇₀ alloy, the alloy is remelted by induction heating, and then a (Co ₅₀ Ti ₂₅ Zr ₂₅ ) ₃₀ Y ₇₀ alloy thin strip with a thickness of about 150 μm is prepared by a copper roll spinning method. The alloy structure includes a matrix composed of Y and a nearly spherical dispersed particle phase composed of Co ₅₀ Ti ₂₅ Zr ₂₅ ). The diameter of the dispersed particles ranges from 50-500nm.

(2) At room temperature, 0.5 g of the (Co ₅₀ Ti ₂₅ Zr ₂₅ ) ₃₀ Y ₇₀ alloy ribbon prepared in step (1) was immersed in 300 mL of a 0.2 mol/L hydrochloric acid aqueous solution for reaction. During the reaction process, the matrix composed of active element Y reacts with hydrochloric acid and enters the solution, while the Co ₅₀ Ti ₂₅ Zr ₂₅ dispersed particle phase which is difficult to react with dilute hydrochloric acid is gradually separated from the matrix phase and dispersed. After 10 minutes, the obtained Co ₅₀ Ti ₂₅ Zr ₂₅ dispersed particles are separated from the solution, washed and dried to obtain approximately spherical Co ₅₀ Ti ₂₅ Zr ₂₅ micro-nano alloy powder, the diameter of which is in the range of 50-500 nm.

The technical features of the above-mentioned embodiments can be combined arbitrarily. In order to make the description concise, all possible combinations of the technical features in the above-mentioned embodiments are not described. However, as long as there is no contradiction in the combination of these technical features, All should be considered as the scope of this specification.

The above-mentioned embodiments only express several embodiments of the present invention, and the descriptions are more specific and detailed, but they should not be understood as limiting the scope of the invention patent. It should be pointed out that for those of ordinary skill in the art, without departing from the concept of the present invention, several modifications and improvements can be made, and these all fall within the protection scope of the present invention. Therefore, the protection scope of the patent of the present invention should be subject to the appended claims.

Claims (10)

1. A preparation method of alloy powder material is characterized in that it comprises the following steps:

   Provide (M _x T _y ) _a RE _b

   Alloy, wherein M is selected from at least one of Fe, Co, Ni, T is selected from at least one of W, Cr, Mo, V, Ta, Nb, Zr, Hf, Ti, and RE is selected from Y, La At least one of, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, x, y and a, b respectively represent the atomic percentage content of the corresponding composition, And 33%≤x≤75%, x+y=100%; 0.1%≤a≤40%, a+b=100%, the solidified structure of the (M _x T _y ) _a RE _b alloy is composed of M The dispersed particle phase of _x T _y and the matrix phase composed mainly of RE;

   The (M _x T _y ) _a RE _b alloy is mixed with an acid solution, the matrix phase reacts with the acid solution to become ions into the solution, and the dispersed particle phase separates out, that is, M _x T _y Composition of alloy powder material.
2. The method for preparing an alloy powder material according to claim 1, wherein the (M _x T _y ) _a RE _b alloy is obtained in the following manner:

   Weigh the alloy raw materials according to the ratio;

   Fully melting the alloy raw materials to obtain an alloy melt;

   The alloy melt is prepared into the (M _x T _y ) _a RE _b alloy by a solidification method, wherein the solidification rate of the alloy melt is 0.001 K/s to 10 ⁷ K/s.
3. The method for preparing alloy powder materials according to claim 1, wherein the vacuum degree during the melting of the alloy melt is 1×10 ^-4 Pa to 1.01325×10 ⁵ Pa.
4. The method for preparing a metal powder material according to claim 1, wherein the particle shape of the dispersed particle phase includes at least one of a dendritic shape, a spherical shape, a nearly spherical shape, a square shape, a pie shape, and a rod shape. The particle size of the dispersed particle phase is 2nm-100mm.
5. The method for preparing alloy powder materials according to claim 1, wherein the acid in the acid solution is sulfuric acid, hydrochloric acid, nitric acid, perchloric acid, phosphoric acid, acetic acid, oxalic acid, formic acid, carbonic acid, gluconic acid, oil At least one of acid and polyacrylic acid, and the solvent in the acid solution is water, ethanol, methanol, or a mixture of the three in any ratio.
6. The method for preparing alloy powder materials according to claim 5, wherein the molar concentration of the acid in the acid solution is 0.001 mol/L to 5 mol/L.
7. The method for preparing alloy powder material according to claim 1, wherein the (M _x T _y ) _a R _b

   In the step of reacting the alloy with the acid solution, the reaction time is 0.1 min to 48 h, and the reaction temperature is 0°C to 100°C.
8. The method for preparing an alloy powder material according to claim 1, wherein the particle size of the M _x T _y alloy powder material is 2 nm to 100 mm.
9. The method for preparing an alloy powder material according to any one of claims 1 to 8, wherein after the step of reacting the (M _x T _y ) _a R _b alloy with the acid solution The following steps are carried out: sieving the obtained alloy powder materials with a particle size ranging from 1 μm to 1 mm, and respectively performing plasma spheroidizing treatment, and finally obtaining spherical alloy powder materials with different particle sizes.
10. The method for preparing an alloy powder material according to claim 9, wherein the particle size of the spherical alloy powder material with different particle sizes is 1 μm to 1 mm.

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