WO2018188178A1 - Matériau composite métallique mm'x-y fonctionnel et son procédé de préparation - Google Patents

Matériau composite métallique mm'x-y fonctionnel et son procédé de préparation Download PDF

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WO2018188178A1
WO2018188178A1 PCT/CN2017/086889 CN2017086889W WO2018188178A1 WO 2018188178 A1 WO2018188178 A1 WO 2018188178A1 CN 2017086889 W CN2017086889 W CN 2017086889W WO 2018188178 A1 WO2018188178 A1 WO 2018188178A1
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metal composite
functional material
composite functional
material according
preparing
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PCT/CN2017/086889
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English (en)
Chinese (zh)
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张虎
陶坤
龙克文
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佛山市程显科技有限公司
佛山市川东磁电股份有限公司
北京科技大学
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Priority to US16/311,562 priority Critical patent/US20200024693A1/en
Publication of WO2018188178A1 publication Critical patent/WO2018188178A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C30/00—Alloys containing less than 50% by weight of each constituent
    • 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
    • B22F1/14—Treatment of metallic powder
    • B22F1/142—Thermal or thermo-mechanical treatment
    • 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
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12—Both compacting and sintering
    • B22F3/16—Both compacting and sintering in successive or repeated steps
    • 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
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
    • C09K5/08—Materials not undergoing a change of physical state when used
    • C09K5/14—Solid materials, e.g. powdery or granular
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/10—Alloys containing non-metals
    • C22C1/1036—Alloys containing non-metals starting from a melt
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/02—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
    • 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
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/044—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by jet milling
    • 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
    • B22F2301/00—Metallic composition of the powder or its coating
    • B22F2301/15—Nickel or cobalt
    • 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
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their steps
    • 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
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D2211/00—Microstructure comprising significant phases
    • C21D2211/008—Martensite
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C2202/00—Physical properties
    • C22C2202/02—Magnetic

Definitions

  • the invention relates to the technical field of metal materials, in particular to a metal composite functional material of MM'X-Y (M and M' are transition group elements, X is a group IIIA or IVA element) and a preparation method thereof.
  • Martensitic transformation is a very important non-diffusion crystal structure phase transition in solid phase transition, and the phase transition property is one stage.
  • the high-temperature mother phase lattice point has no diffusion-displacement shear at the atomic scale, so it is also called displacement phase transition.
  • the chemical composition of the two phases remains unchanged before and after the phase change, but the crystal structure of the material changes significantly.
  • the high temperature parent phase is austenite and the low temperature product is martensite.
  • Martensitic transformation materials have many applications in steel reinforcement, material toughening, reduction of quenching deformation, shape memory effect, superelasticity and pseudoelasticity, and are good functional materials.
  • the martensitic transformation process is often accompanied by dramatic crystal structure changes.
  • This effect is applied to the shape memory alloy, that is, it has a certain shape.
  • the material is cooled from a high temperature higher than the martensitic transformation temperature (T M ) to form a low temperature martensite phase, in which state the deformation is applied, and then the material is heated to the martensitic reverse transformation temperature (T A Above, the material returns to its original shape.
  • Conventional shape memory alloys mainly control their deformation by temperature and stress changes, which results in low response frequency and difficulty in sensitivity improvement.
  • ferromagnetic martensitic transition alloys Due to the magnetic phase transition and structural phase transition coupling, the crystal structure, magnetic properties and electrical properties change at the same time, so that the ferromagnetic shape memory alloy exhibits abundant magnetic functional properties, such as shape memory effect, magnetostriction, magnetoresistance effect, Hall effect, magnetocaloric effect, etc. Rich magnetic properties and potential application value make ferromagnetic horse
  • the austenitic phase change alloy has become a new type of functional material that has received much attention.
  • ferromagnetic martensitic transformation alloys include Ni-Mn-Ga, Ni-Mn-Al, Ni-Mn-In, Ni-Mn-Sn and the like.
  • MM'X ferromagnetic martensitic transformation material
  • M and M' are transition group elements, X is a group IIIA or IVA element
  • the MM'X alloy also exhibits a magnetic field-induced ferromagnetic martensitic transformation through composition and process adjustment, accompanied by large crystal structure changes and magnetocaloric effects during the phase transition, and its phase transition temperature can be very wide. Adjustment in the temperature zone. Therefore, it can be regarded as a multi-functional material such as a shape memory effect material, a negative expansion material, and a magnetic refrigeration material, and is considered as a new-generation ferromagnetic martensitic transformation functional material.
  • the object of the present invention is to provide a MM'XY metal composite functional material and a preparation method thereof, which can prepare a MM'XY metal composite functional material which has good mechanical properties and ferromagnetic martensitic transformation, and exhibits good performance. Magnetic refrigeration performance can greatly advance the application of this functional material.
  • a MM'XY metal composite functional material comprising the following components and their volume percentages: A% of M a M' b X c and B% of Y, wherein:
  • M, M' is any one of transition elements or an alloy of more than one element
  • X is any one of the elements of group IIIA or IVA or an alloy of more than one element
  • Y is any one of Group IB, Group IIB, Group IIIA, Group IVA or an alloy of more than one element;
  • a, b, and c are in the range of 0.8 to 1.2;
  • the A% is 50% to 95%
  • the B% is 5% to 50%.
  • the A% is 60% to 90%, and the B% is 10% to 40%.
  • a preparation method of MM'X-Y metal composite functional material comprises the following steps:
  • the molding material is cured to obtain a product MM'X metal composite functional material.
  • Mn is added in an excess of 1% to 10% by atomic ratio to compensate for volatilization and burning during the preparation, thereby obtaining a single phase.
  • Mn when the M or M' is a Mn element, Mn is added in an excess of 2% to 5% by atomic ratio.
  • the pressure after the vacuuming of the melting furnace is controlled to be less than or equal to 3 ⁇ 10 -3 Pa, the melting temperature is 1300 ° C or higher, and the melting time is 0.5 to 10 min.
  • the pressure after the vacuuming of the melting furnace is 2 ⁇ 10 -3 to 3 ⁇ 10 -3 Pa
  • the melting temperature is 1300 to 1700 ° C
  • the melting time is 2 to 3 min.
  • the vacuum annealing temperature is 600 to 1100 ° C and the time is 1 to 30 days.
  • the vacuum annealing temperature is 700 to 900 ° C and the time is 5 to 15 days.
  • the crushing is performed by any one or a combination of grinding, vibration grinding, rolling mill, ball milling, jet milling, etc.
  • the screening is a standard sieve exceeding 10 mesh
  • the powder of the powder The diameter is less than 2mm.
  • the sieving is a standard sieve of 100 to 300 mesh, and the powder has a particle diameter of 0 to 0.2 mm.
  • the press molding is to press the powder into a desired size and shape by a calendering method, a molding method, an extrusion method, a powder injection molding method, or a discharge plasma sintering method, and the press molding pressure is 300. ⁇ 1500 MPa, temperature is 0-900 ° C, time is 1-240 min, and the strength of the magnetic field is 0-5T.
  • the pressure of the press molding is 600 to 1000 MPa
  • the temperature is 0 to 500 ° C
  • the time is 5 to 60 min
  • the strength of the magnetic field is 0 to 2 T.
  • the curing temperature is 0 to 900 ° C and the time is 1 to 15 days.
  • the curing temperature is 0 to 500 ° C and the time is 2 to 7 days.
  • the present invention provides a novel MM'XY metal composite functional material; 2) The MM'XY metal composite functional material prepared by the present invention has higher mechanical properties than the conventional MM'X material; 3) The preparation of the present invention MM'XY metal composite functional material has good magnetocaloric effect and can be applied to the manufacture of magnetic refrigeration materials. 4) The preparation method of the present invention can be fabricated into MM'XY metal composite functional materials of any shape and size according to actual needs. 5) The preparation method of the invention is simple in process, easy to operate and realizes industrial production, and has important significance for practical application.
  • Example 1 is a topographical view of smelted Mn 0.6 Fe 0.4 NiSi 0.5 Ge 0.5 obtained in Example 1 of the present invention
  • Example 2 is a topographical view of a 70% Mn 0.6 Fe 0.4 NiSi 0.5 Ge 0.5 +30% In metal composite functional material prepared in Example 1 of the present invention
  • Example 3 is a graph showing a stress-strain curve of a 70% Mn 0.6 Fe 0.4 NiSi 0.5 Ge 0.5 +30% In metal composite functional material prepared in Example 1 of the present invention
  • Example 4 is a graph showing dependence of ⁇ S on temperature of a 70% Mn 0.6 Fe 0.4 NiSi 0.5 Ge 0.5 +30% In composite metal functional material prepared in Example 1 of the present invention under different magnetic fields;
  • Example 5 is a graph showing a stress-strain curve of a 75% Mn 0.6 Fe 0.4 NiSi 0.5 Ge 0.5 +25% In metal composite functional material prepared in Example 2 of the present invention
  • Fig. 6 is a graph showing the stress-strain curve of an 80% Mn 0.6 Fe 0.4 NiSi 0.5 Ge 0.5 + 20% In metal composite functional material obtained in Example 3 of the present invention.
  • Embodiment 1 see Figures 1 to 4:
  • the invention provides a 70%Mn 0.6 Fe 0.4 NiSi 0.5 Ge 0.5 +30%In metal composite functional material and a preparation method thereof, comprising the following steps:
  • the raw material is prepared according to the chemical formula of Mn 0.6 Fe 0.4 NiSi 0.5 Ge 0.5 , and the raw material is commercially available metal Mn, Fe, Ni, Si, Ge with a purity higher than 99.9 wt.%, wherein Mn is added in excess of 5% atomic ratio. Used to compensate for its volatilization and burning during the preparation process;
  • the prepared raw materials are placed in a smelting furnace, the smelting furnace is vacuumed to 2 ⁇ 10 -3 Pa, and then washed with argon gas, and then the prepared raw materials are protected at 1500 ° C under argon gas protection. After smelting for 3 min, the ingot Mn 0.6 Fe 0.4 NiSi 0.5 Ge 0.5 was obtained ;
  • Fig. 1 The morphology of the smelted Mn 0.6 Fe 0.4 NiSi 0.5 Ge 0.5 sample prepared in this example is shown in Fig. 1. It can be seen from the figure that after the conventional smelting, the sample undergoes martensite transformation due to cooling from high temperature to room temperature. The large internal stress generated during the phase change causes the sample to be fragmented and cannot be formed and machined, which limits the application of such functional materials.
  • the appearance of the product of this embodiment is shown in Fig. 2, and the product has good molding and processing properties, and the above problems are well solved.
  • MM'X alloys have poor mechanical properties due to sample fragmentation and are not capable of stress-strain curve testing.
  • the mechanical properties of the product of this embodiment are significantly improved, and the mechanical property test can be completely performed.
  • the stress-strain curve of the product of this example was measured on a WDW200D type microcomputer-controlled universal material testing machine. As shown in Fig. 3, the compressive strength of the product of this example was 45 MPa, and the corresponding strain was 9.2%.
  • the isothermal magnetization curve (MH curve) of the product of this example was measured on a magnetic measurement system (Versalab Free measurement system designed by Quantum Design, USA), and then according to Maxwell's relationship:
  • the magnetic entropy change ⁇ S can be calculated from the isothermal magnetization curve.
  • Fig. 4 shows the dependence of ⁇ S on the temperature of the product in the present embodiment under different magnetic fields. It can be seen that the maximum value of the magnetic entropy change occurs in the sample near the phase transition temperature 311K, and the magnetic field changes are 0-1T, 0, respectively. At -2T and 0-3T, the maximum magnetic entropy change of the samples was 4.5 J/kg K, 9.9 J/kg K, and 15.3 J/kg K, respectively.
  • the invention provides a 75% Mn 0.6 Fe 0.4 NiSi 0.5 Ge 0.5 + 25% In metal composite functional material and a preparation method thereof, comprising the following steps:
  • the raw material is prepared according to the chemical formula of Mn 0.6 Fe 0.4 NiSi 0.5 Ge 0.5 , and the raw material is commercially available metal Mn, Fe, Ni, Si, Ge with a purity higher than 99.9 wt.%, wherein Mn is added in excess of 5% atomic ratio. Used to compensate for its volatilization and burning during the preparation process;
  • the prepared raw materials are placed in a smelting furnace, the smelting furnace is vacuumed to 2.5 ⁇ 10 -3 Pa, and then washed with argon gas, and then the prepared raw materials are protected at 1700 ° C under argon gas protection. After smelting for 2 min, the ingot Mn 0.6 Fe 0.4 NiSi 0.5 Ge 0.5 was obtained ;
  • the stress-strain curve of the 75% Mn 0.6 Fe 0.4 NiSi 0.5 Ge 0.5 +25% In metal composite of the product of this example was measured on a WDW200D type microcomputer-controlled universal material testing machine. As shown in FIG. 5, the compression resistance of the product of this example was as shown in FIG. The strength is 48 MPa and the corresponding strain is 15.6%. At the same time, the magnetothermal effect of the product of this embodiment is higher than that of the conventional room temperature magnetic refrigeration material Gd.
  • the invention provides an 80% Mn 0.6 Fe 0.4 NiSi 0.5 Ge 0.5 +20% In metal composite functional material and a preparation method thereof, comprising the following steps:
  • the raw material is prepared according to the chemical formula of Mn 0.6 Fe 0.4 NiSi 0.5 Ge 0.5 , and the raw material is a commercially available metal Mn, Fe, Ni, Si, Ge having a purity higher than 99.9 wt.%, wherein Mn is excessively added in an atomic ratio of 3%. Used to compensate for its volatilization and burning during the preparation process;
  • the prepared raw materials are placed in a smelting furnace, the smelting furnace is vacuumed to 3 ⁇ 10 -3 Pa, and then washed with argon gas, and then the prepared raw materials are protected at 1700 ° C under argon gas protection. After smelting for 2 min, the ingot Mn 0.6 Fe 0.4 NiSi 0.5 Ge 0.5 was obtained ;
  • the stress-strain curve of the 80% Mn 0.6 Fe 0.4 NiSi 0.5 Ge 0.5 +20% In metal composite of the product of this example was measured on a WDW200D type microcomputer-controlled universal material testing machine. As shown in Fig. 6, the compression resistance of the product of this example was as shown in Fig. 6. The strength is 41 MPa and the corresponding strain is 14.9%.
  • the invention provides a 60% MnCoCu 0.08 Ge 0.92 +40%Sn metal composite functional material and a preparation method thereof, comprising the following steps:
  • the raw material is prepared according to the chemical formula of MnCoCu 0.08 Ge 0.92 , and the raw material is commercially available metal Mn, Co, Cu, Ge having a purity higher than 99.9 wt.%, wherein Mn is excessively added in an atomic ratio of 3% to compensate for Volatilization and burning during preparation;
  • the prepared raw materials are placed in a smelting furnace, the smelting furnace is vacuumed to 2 ⁇ 10 -3 Pa, and then washed with argon gas, and then the prepared raw materials are protected at 1600 ° C under argon gas protection. After smelting for 3 min, the ingot MnCoCu 0.08 Ge 0.92 was obtained .
  • the invention provides a 75% Mn 0.95 CoCe 0.9 Si 0.1 +25% InSn metal composite functional material and a preparation method thereof, comprising the following steps:
  • the raw material is prepared according to the chemical formula of Mn 0.95 CoCe 0.9 Si 0.1 , and the raw material is commercially available metal Mn, Co, Ge, Si with a purity higher than 99.9 wt.%, wherein Mn is added in excess of 4% atomic ratio for compensation Its volatilization and burning during the preparation process;
  • the prepared raw materials are placed in a smelting furnace, the smelting furnace is vacuumed to 3 ⁇ 10 -3 Pa, and then washed with argon gas, and then the prepared raw materials are protected at 1400 ° C under argon gas protection. After smelting for 3 min, the ingot Mn 0.95 CoCe 0.9 Si 0.1 was obtained .

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Abstract

L'invention concerne un matériau composite métallique MM'X-Y fonctionnel et son procédé de préparation, ses constituants étant, en pourcentage en volume : A % de MaM'bXc et B % de Y, M et M' étant des éléments du groupe de transition ; X étant un élément du groupe IIIA ou IVA ; Y étant un élément choisi parmi ou un alliage de plusieurs éléments choisis parmi les éléments du groupe IB, du groupe IIB, du groupe IIIA et du groupe IVA ; les plages de valeurs de a, b et c étant de 0,8 à 1,2 ; et la somme de A % et B % étant égale à 100 %. Ce matériau est préparé à l'aide d'étapes de fusion, recuit, broyage, mélange, pressage, solidification, etc. Ce matériau présente des propriétés mécaniques supérieures et un bon effet thermomagnétique.
PCT/CN2017/086889 2017-04-13 2017-06-01 Matériau composite métallique mm'x-y fonctionnel et son procédé de préparation WO2018188178A1 (fr)

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CN201710238382.5A CN106917029B (zh) 2017-04-13 2017-04-13 一种铁磁马氏体相变mm′x-y金属复合功能材料及其制备方法

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WO2016104739A1 (fr) * 2014-12-26 2016-06-30 大電株式会社 Procédé de production d'un matériau de réfrigération magnétique
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CN105714173A (zh) * 2016-04-27 2016-06-29 上海电力学院 一种锰钴锗基合金磁制冷材料及其制备

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CN106917029B (zh) 2018-08-21
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