WO2020228709A1 - Procédé de préparation d'un matériau d'alliage pulvérulent - Google Patents

Procédé de préparation d'un matériau d'alliage pulvérulent Download PDF

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WO2020228709A1
WO2020228709A1 PCT/CN2020/089895 CN2020089895W WO2020228709A1 WO 2020228709 A1 WO2020228709 A1 WO 2020228709A1 CN 2020089895 W CN2020089895 W CN 2020089895W WO 2020228709 A1 WO2020228709 A1 WO 2020228709A1
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alloy
acid
alloy powder
powder material
preparing
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PCT/CN2020/089895
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English (en)
Chinese (zh)
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刘丽
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刘丽
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C28/00—Alloys based on a metal not provided for in groups C22C5/00 - C22C27/00
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C3/00—Removing material from alloys to produce alloys of different constitution separation of the constituents of alloys
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C3/00—Removing material from alloys to produce alloys of different constitution separation of the constituents of alloys
    • C22C3/005—Separation of the constituents of alloys

Definitions

  • the invention relates to the technical field of metal materials, in particular to a method for preparing alloy powder materials.
  • 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.
  • 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.
  • 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.
  • a preparation method of alloy powder material includes the following steps:
  • (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
  • 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.
  • 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.
  • the vacuum degree during the melting of the alloy melt is 1 ⁇ 10 -4 Pa to 1.01325 ⁇ 10 5 Pa.
  • 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.
  • 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.
  • the molar concentration of the acid in the acid solution is 0.001 mol/L to 5 mol/L.
  • the reaction time is 0.1 min to 48 h, and the reaction temperature is 0°C to 100°C.
  • the particle size of the M x T y alloy powder material is 2 nm to 100 mm.
  • the following step is further performed: the obtained alloy powder material with a particle size range of 1 ⁇ m to 1 mm is sieved, Plasma spheroidization is performed respectively, and finally alloy powder materials with different particle sizes and spherical shapes are obtained.
  • the particle size of the spherical alloy powder material with different particle diameters is 1 ⁇ m to 1 mm.
  • 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.
  • 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.
  • 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.
  • 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.
  • the method for preparing alloy powder material provided by the present invention includes the following steps:
  • step S1 the (M x T y ) a RE b alloy is obtained in the following manner:
  • 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.
  • 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.
  • 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.
  • 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.
  • the alloy raw materials are metal M, metal T and rare earth RE, each element can be melted to prepare an alloy melt.
  • 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.
  • 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.
  • 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.
  • 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.
  • 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.
  • the solidification rate of the alloy melt may be 0.001 K/s to 10 7 K/s
  • 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.
  • the particle size specifically refers to the diameter of the rod-shaped cross-section.
  • the acid solution is a solution containing H + .
  • (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.
  • 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.
  • 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°C ⁇ 100°C.
  • step S2 if the particle size of the obtained alloy powder material is in the range of 1 ⁇ m 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 ⁇ m to 1 mm.
  • 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.
  • This embodiment provides a method for preparing micron-sized CoTi powder, which includes the following steps:
  • 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 ⁇ m to 40 ⁇ m.
  • 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.
  • This embodiment provides a method for preparing spherical micron-sized CoTi powder, which includes the following steps:
  • 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 ⁇ m to 40 ⁇ m.
  • the dendrite size ranges are >26 ⁇ m, 26 ⁇ m-13 ⁇ m, 13 ⁇ m ⁇ Graded CoTi dendritic powder of 6.5 ⁇ m and less than 6.5 ⁇ m.
  • the CoTi dendritic powders with dendrite diameters ranging from 26 ⁇ m to 13 ⁇ m and 13 ⁇ m to 6.5 ⁇ m are selected respectively, and spherical Co 50 Ti with particle sizes ranging from 26 ⁇ m to 13 ⁇ m and 13 ⁇ m to 6.5 ⁇ m are further prepared through mature plasma spheroidization technology. 50 powder.
  • This embodiment provides a method for preparing nano-scale CoHf powder, including the following steps:
  • This embodiment provides a method for preparing spherical micron CoCrMo powder, which includes the following steps:
  • 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 ⁇ m to 50 ⁇ m.
  • 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 3 ⁇ m ⁇ 50 ⁇ m.
  • the dendrite size ranges are> 26 ⁇ m, 26 ⁇ m ⁇ Graded Co-Cr-Mo dendritic powder of 13 ⁇ m, 13 ⁇ m ⁇ 6.5 ⁇ m and less than 6.5 ⁇ m.
  • Co-Cr-Mo dendritic powders with dendrite particle sizes ranging from 26 ⁇ m to 13 ⁇ m and 13 ⁇ m to 6.5 ⁇ m are selected, and the particle size ranges from 26 ⁇ m to 13 ⁇ m and 13 ⁇ m to 6.5 ⁇ m are further prepared by mature plasma spheroidizing technology.
  • Spherical Co 63 Cr 33 Mo 4 powder are further prepared by mature plasma spheroidizing technology.
  • This embodiment provides a method for preparing sub-micron CoTiHf powder, which includes the following steps:
  • This embodiment provides a method for preparing micro-nano CoTiZr powder, which includes the following steps:
  • 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.
  • 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.

Abstract

La présente invention concerne un procédé de préparation d'un matériau d'alliage pulvérulent. À l'aide de la caractéristique d'une structure de solidification d'alliage contenant une phase matricielle et une phase particulaire dispersée inerte, la phase matricielle est éliminée par réaction avec une solution acide, de sorte que la phase particulaire dispersée est séparée afin d'obtenir le matériau d'alliage pulvérulent. Le procédé est simple à mettre en œuvre, et permet de préparer une pluralité de matériaux d'alliage pulvérulents ayant différentes morphologies, notamment à l'échelle nanométrique, submicrométrique, micrométrique et millimétrique, et présente de bonnes perspectives d'application dans des domaines tels que la catalyse, la métallurgie des poudres et l'impression 3D.
PCT/CN2020/089895 2019-05-15 2020-05-13 Procédé de préparation d'un matériau d'alliage pulvérulent WO2020228709A1 (fr)

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WO2022100656A1 (fr) * 2019-11-28 2022-05-19 赵远云 Procédé de préparation de poudre d'alliage contenant de l'aluminium, son utilisation et bande d'alliage
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