CN102851545B - Ni-Mn-Ge magnetic shape memory alloy and preparation method thereof - Google Patents

Ni-Mn-Ge magnetic shape memory alloy and preparation method thereof Download PDF

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CN102851545B
CN102851545B CN201210383242.4A CN201210383242A CN102851545B CN 102851545 B CN102851545 B CN 102851545B CN 201210383242 A CN201210383242 A CN 201210383242A CN 102851545 B CN102851545 B CN 102851545B
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罗鸿志
刘国栋
孟凡斌
刘何燕
代学芳
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Hebei University of Technology
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Abstract

The invention relates to a Ni-Mn-Ge magnetic shape memory alloy of which the chemical formula is NixMnyGezMa, wherein M is a main group element or transition group element; and 51<x<55, 31<y<40, 5<z<20, a<5, x+y+z+a=100, and x, y, z and a represent atomic percents. The alloy is a monocrystalline material or polycrystalline material. The main group element is In, Sn, Sb, As or Si; and the transition group element is Ti, Fe or Co. The magnetic material with magnetic shape memory effect has shape memory effect and ferromagnetic property, and appears the property of entropic change (magnetic card effect) caused by magnetic-field-driven phase change and magnetic order degree change, wherein the change value is up to S=8J/Kkg.

Description

A kind of Ni-Mn-Ge is magnetic shape memory alloy and preparation method thereof
Technical field
The present invention relates to a kind of magnetic shape memory alloy, there is ferromegnetism and bidirectional shape memory effect, particularly relate to Ni-Mn-Ge magneticsubstance having controlled magnetic-field-induced strain and field drives phase transformation and preparation method thereof.
Background technology
Common shape memory alloy has a kind of crystalline structure (hereinafter referred to as parent phase) at relatively high temperature, and at relatively low temperature spontaneous another crystalline structure that becomes, be generally referred to as martensitic phase.When the greenhouse cooling from higher is during to lower temperature, material changes martensitic phase into from parent phase, and this changes mutually and is called martensitic transformation.Conversely, from relatively low temperature heating material, alloy can change parent phase into from martensitic phase, and this contrary transformation is mutually called martensite reverse transformation.General by the starting point of martensitic transformation and terminal, be called M spoint and M fpoint, by the beginning of martensite reverse transformation and terminal, is called A spoint and A fpoint.If M sand A sbetween difference less, such as be the several years or tens degree, this martensitic transformation of material is called as thermoelastic martensitic transformation.
Usually, certain alloy material is cooling with the shape of determining at parent phase, until after martensitic phase, change artificially more original shape, then, alloy material is heated up, until while being transformed into austenite, if the shape of alloy material completely or partially changes original shape into, this phenomenon is called shape memory effect.In addition, if in the circulation of same said temperature, the phase transformation that the shape of parent phase causes in cooling is out of shape constantly, then the reverse transformation redeformation constantly causing in intensification subsequently, and the shape that is partly or entirely transformed into original parent phase, is referred to as bidirectional shape memory effect.
General shape memory alloy component deformation is controlled by temperature variation, causes its response frequency lower, and promotes difficulty.And the martensite of magnetic shape memory alloy to reset can be field drives, action response speed is fast, is therefore widely used in various " intelligence " type purposes, as micro electro mechanical device etc.
The magnetic shape memory alloy having been found that at present mainly comprises Ni-Mn-Ga, Ni-Mn-Sb, Ni-Fe-Ga etc., but these materials transformation temperature be usually less than room temperature, and/or fragility is large, be easy to fracture, thereby limited this application of class material in engineering, so people still find the new magnetic shape memory material with better performance constantly.2006, reported that composition is Ni 50mn 25ge 25shape memory alloy, predict that this material may have higher transformation temperature, but this material that experiment shows into Heusler phase can only obtain film on substrate by film growth method, complicated process of preparation, cost is high, and is difficult to obtain massive material.
Summary of the invention
Primary and foremost purpose of the present invention is to overcome existing Ni 50mn 25ge 25the deficiency of alloy, the material that provides a kind of Ni-Mn-Ge cording to be magnetic shape memory effect, this material phase transformation temperature can change in larger temperature range, meets the needs of different application environment.Simultaneously its preparation technology and Ni 50mn 25ge 25film is compared easier, is beneficial to scale operation manufacture, can obtain being suitable for the massive material of different application environment.
Technical scheme of the present invention is:
Ni-Mn-Ge is a magnetic shape memory alloy, and its chemical formula is: Ni xmn yge zm a, M is main group element or transition element; Wherein, 51<x<55,31<y<40,5<z<20, a<5, x+y+z+a=100, x, y, z, a represent atom percentage content; Described alloy is monocrystal material or polycrystalline material.
Described main group element is In, Sn, Sb, As or Si;
Described transition element is Ti, Fe or Co;
Described Ni-Mn-Ge is the preparation method of magnetic shape memory alloy, and arbitrary for following two kinds of methods comprises the steps:
Method one, the preparation of polycrystalline material:
(1) press chemical formula Ni xmn yge zm araw materials weighing, wherein, 51<x<55,31<y<40,5<z<20, a<5, x+y+z+a=100, x, y, z, a represent atom percentage content;
(2) material weighing up is contained in smelting pot, adopts conventional arc melting method to obtain Ni xmn yge zm amagnetic polycrystalline, its melting condition is: at base vacuum, reach 2 * 10 -3when Pa is following, pass into argon gas, whole fusion process sample adopts argon shield, and then high-temperature homogenization is processed 3 days, then quenches to realize ingot casting homogenization of composition;
(3) ingot casting of processing through homogenizing is put into a bottom and be with foraminate silica tube, be placed to and get rid of in band machine furnace chamber, be evacuated down to 1 * 10 -3below Pa, in furnace chamber, pass into high-purity argon gas afterwards, adopt induction heating to make alloy molten, then from silica tube top, be blown into high-purity argon gas and molten alloy liquid be ejected on the copper wheel of high speed rotating from aperture throw away fast, obtain Polycrystalline Metals band.
Or, method two, the preparation of monocrystal material:
(1) press chemical formula Ni xmn yge zm araw materials weighing, wherein, 51<x<55,31<y<40,5<z<20, a<5, x+y+z+a=100, x, y, z, a represent atom percentage content;
(2) material weighing up is contained in smelting pot, adopts conventional arc melting method to obtain Ni xmn yge zm amagnetic polycrystalline, whole fusion process sample adopts argon shield, then carries out high-temperature homogenization and processes 3 days, then quenches to realize ingot casting homogenization of composition.
(3) by the Ni processing through homogenizing xmn yge zm araw material is placed in crucible, adopts conventional Czochralski grown Ni xmn yge zm amagnetic mono crystal, its growth conditions is: heating mentioned component former expect make it melting; Its melting environment is 5 * 10 -3-5 * 10 -5the argon shield gas of the vacuum of Pa or 0.01～1MPa positive pressure; Under the melt temperature condition of 1100～1330 ℃, keep 10～30 minutes;
(4) the fixing seed crystal in seed rod lower end rotating with the speed of 0.5～50 rev/min; Described seed crystal is composition monocrystalline identical or approaching, that have needed orientation, with the liquid level of end in contact melt under seed crystal, then, with the uniform rate lifting seed rod of 3～80mm/ hour, will on the single crystal direction of solidification and crystallization, lift, and keeps isodiametric growth;
(5) when the monocrystalline of growth reaches desired size, single crystal pulling is departed to the raw material surface of melting, with the rate of temperature fall of 0.5～20 ℃/min, slowly reduce temperature and be cooled to room temperature, finally take out.
Further comprising the steps of in described preparation method: the above-mentioned sample preparing is annealed 0.1～100 hour in the temperature range of 500～1200 ℃ again, and then cooling with the rate of temperature fall of 0.1～1000 ℃/sec.
Growth type of heating can be by radio frequency heating or the resistive heating mode of 50～245 kilohertzs in described step (3).
Single crystal growing crucible in described step (3) is magnetic levitation cold crucible, plumbago crucible or quartz crucible.
Provided by the invention have magnetic shape memory effect magneticsubstance, it is characterized by and there is shape memory effect and ferromegnetism simultaneously.By changing the ratio of components of Ni, Mn, Ge and M element in material, Ni xmn yge zm atransformation temperature and Curie temperature adjustable continuously within the scope of 100K-400K and 300K-450K respectively, to adapt to different occasions, the requirement of purposes.The martensitic phase twin generation reorientation of this material can be brought out in magnetic field, under the effect of field drives power, by twin boundary migration, realizes position to growing up of variant preferentially, and this will bring considerable magneto-strain.At Ni xmn yge zm ain Polycrystalline, can be different with composition, can obtain the magneto-strain value of 2%-4%.
Meanwhile, Ni xmn yge zm amaterial also shows the character (magneto-caloric effect) that changes the Entropy Changes causing with the phase transformation of field drives and magnetic order degree, for example Ni 52mn 33ge 12sn 3middle magnetic entropy variable value can reach S=8J/Kkg.So, magnetic shape memory alloy material Ni provided by the invention xmn yge zm apreparation method is simple and easy to do, can obtain large-sized material, and in magnetic functional material field, tool has been widely used, for example, as actuator, and temperature and/or magnetic sensor, magnetic refrigeration device and equipment, micro-electro-mechanical device and system etc.
Accompanying drawing explanation
Accompanying drawing 1 is the Ni that the embodiment of the present invention 1 obtains 52mn 33ge 12si 3the x ray diffraction spectra of alloy;
Accompanying drawing 2 is Ni that the embodiment of the present invention 2 obtains 52mn 33ge 12sn 3ac magnetic susceptibility-temperature relation figure of alloy;
Accompanying drawing 3 is Ni that the embodiment of the present invention 3 obtains 52mn 32ge 15co 1the magnetzation curve figure of alloy;
Accompanying drawing 4 is Ni that the embodiment of the present invention 6 obtains 54mn 35ge 7fe 4the x ray diffraction spectra of alloy
Accompanying drawing 5 is Ni that the embodiment of the present invention 2 obtains 52mn 33ge 12sn 3the magnetic entropy of alloy becomes result.
Embodiment:
Embodiment 1
Preparation consists of: the monocrystal material with magnetic shape memory effect, adopt the radio frequency heating that growth parameter(s) is 245KHz, with 0.01 argon gas to 1MPa positive pressure, as shielding gas, in magnetic levitation copper crucible, grow, heating power is 20 kilowatts,
Its preparation method is undertaken by following concrete steps:
(1) according to mole proportioning Ni:Mn:Ge:Si=52:33:12:3 of each material in forming, weighing respectively purity is above 99.9% Ni, Mn, Ge, Si, and the material weighing up is put into copper crucible, puts into smelting furnace, with mechanical pump forvacuum to 5 * 10 -1pa; With molecular pump, be evacuated down to 5 * 10 -4pa, passes into high-purity argon gas (purity is 99.9%), makes melting furnace chamber internal pressure reach 0.1MPa; Adopt arc melting method to obtain Ni 52mn 33ge 12si 3polycrystalline cast ingot.In fusion process, electric arc head remains on 2-5cm place, sample top and repeatedly swings among a small circle about 1min, and melting electric current 100A will be overturn after sample is cooling, repeat melting step above; Each sample upset three times, i.e. melting four times so repeatedly, so that it is even to prepare sample composition; Treat that furnace chamber is cooled to room temperature, finally take out, obtain Ni 52mn 33ge 12si 3polycrystalline cast ingot;
(2) Ni step (1) being obtained 52mn 33ge 12si 3polycrystalline cast ingot, carries out vacuum homogenizing thermal treatment 3 days with packing into after tantalum piece parcel in the vitreosil pipe of sealing at 800 ℃, in the room temperature water of then ingot casting being quenched to realize ingot casting homogenization of composition;
(3) ingot casting obtaining is put into single crystal growing crucible, adopt conventional Czochralski grown Ni 52mn 33ge 12si 3magnetic mono crystal, its growth conditions is: heating mentioned component ingot casting former expect make it melting; The argon shield gas that its melting environment is 0.01～1MPa positive pressure; 20 kilowatts of heating powers keep 25 minutes under the melt temperature condition of 1200 ℃;
(4) adopting the NiMnGe[001 of 2 * 2 * 7mm size] (seed crystal of use is along [001] direction orientation) direction oriented single crystal is as seed crystal; In its process of growth, seed rod speed of rotation is 25 revs/min, the liquid level of the seed crystal bottom surface contact melt of seed rod lower end will be fixed on, pulling growth speed is 30mm/ hour, lifts, and make the single crystal diameter of growth transfer isodiametric growth to after increasing to 10mm on the single crystal direction of solidification and crystallization;
(5) when obtaining diameter, be 10mm, the Ni that length is 100mm 52mn 33ge 12si 3after monocrystalline, single crystal pulling is departed to the raw material surface of melting, with the rate of temperature fall of 1 ℃/min, slowly reduce temperature and be cooled to room temperature, finally take out;
(6) monocrystalline step (5) being prepared carries out vacuum annealing 48 hours with packing into after tantalum piece parcel in the vitreosil pipe of sealing in 500-1200 ℃ of temperature range, and then is cooled to room temperature with 10 ° of rate of temperature fall of C/ minute.
The single crystal samples that step (6) is obtained utilizes line to be cut into appropriate size sample, measures various character, and sample becomes martensitic structure in room temperature, and its x ray diffraction spectra is shown in accompanying drawing 1; The sample martensitic transformation temperature obtaining and the value of Curie temperature are in Table 1.
Embodiment 2
Preparation consists of Ni 52mn 33ge 12sn 3the polycrystalline alloy with magnetic shape memory effect, adopt arc melting method, with the argon gas of 0.1MPa positive pressure, as shielding gas, in the copper crucible of water-cooled, prepare polycrystalline cast ingot, adopt afterwards and get rid of band method and obtain Polycrystalline.Its preparation method is undertaken by following concrete steps:
(1) according to mole proportioning Ni:Mn:Ge:Sn=52:33:12:3 of each material in forming, weighing respectively purity is above 99.9% Ni, Mn, Ge, Sn, and the material weighing up is put into copper crucible, puts into smelting furnace, with mechanical pump forvacuum to 5 * 10 -1pa; With molecular pump, be evacuated down to 1 * 10 -4pa, passes into high-purity argon gas, makes melting chamber internal pressure reach 0.1MPa; Produce electric arc, electric arc head remains on 2-5cm place, sample top and repeatedly swings among a small circle about 1min, and melting electric current 120A will be overturn after sample is cooling, repeat melting step above; Each sample upset 3 times, i.e. melting four times so repeatedly, so that it is even to prepare sample composition; Treat that furnace chamber is cooled to room temperature, finally take out;
(2) arc melting method is obtained to Ni 52mn 33ge 12sn 3polycrystalline cast ingot, carries out vacuum homogenizing thermal treatment 3 days with packing into after tantalum piece parcel in the vitreosil pipe of sealing at 850 ℃, in the room temperature water of then ingot casting being quenched to realize ingot casting homogenization of composition;
(3) ingot casting of processing through homogenizing is put into a bottom and be with foraminate silica tube, be placed to and get rid of in band machine furnace chamber, be evacuated down to 1 * 10 -3below Pa, in furnace chamber, pass into high-purity argon gas, pressure is-0.05MPa, adopt induction heating, 10 kilowatts of heating powers, make alloy in molten state, and the high-purity argon gas that is then blown into 0.08MPa from silica tube top is ejected on the copper wheel of high speed rotating that linear velocity is 20m/s molten alloy liquid to throw away fast from aperture, obtaining width is 3-5mm, and thickness is the Polycrystalline Metals band of 50-100 μ m.
Above-mentioned Polycrystalline is prepared into appropriate size sample, measure various character, susceptibility-the temperature relation of sample is shown in accompanying drawing 2, and the magnetic sample Entropy Changes value measuring can reach 8J/Kkg(and see accompanying drawing 5), the sample martensitic transformation temperature of acquisition and the value of Curie temperature are in Table 1.
Embodiment 3
Preparation consists of: Ni 52mn 32ge 15co 1the magnetic shape memory alloy polycrystalline with magnetic field driven martensitic transformation effect; Remove into be grouped into and become Ni:Mn:Ge:Co=52:32:15:1, and in step (3), getting rid of band process, to be blown into ar pressure be 0.05MPa, copper wheel rotating speed is that beyond 25m/s, all the other steps are with embodiment 2.Measure above-mentioned various character, gained magnetzation curve sees attached list 3, therefrom visible significantly field drives phase transformation, and the sample martensitic transformation temperature of acquisition and the value of Curie temperature are in Table 1.
Embodiment 4
Preparation consists of: Ni 54mn 36ge 8ti 2the magnetic shape memory alloy polycrystalline with high transformation temperature and magneto-strain effect; Remove into be grouped into and become Ni:Mn:Ge:Ti=54:36:8:2, and in step (3), to get rid of band process ar pressure be 0.06MPa, copper wheel rotating speed is that beyond 25m/s, all the other steps are with embodiment 2.The various character of the phase transformation of measure sample and magnetic properties, the sample martensitic transformation temperature of acquisition and the value of Curie temperature are in Table 1.The transformation temperature of visible sample is far above room temperature, can at higher temperature, keep shape memory effect, martensitic phase still has ferromegnetism simultaneously, can under field drives, produce magneto-strain, and this material will be widely used in magnetic action performer field.
Embodiment 5
Preparation consists of: Ni 52mn 37ge 8sb 3the monocrystal material with magnetic shape memory effect; Remove into be grouped into and become Ni:Mn:Ge:Sb=52:37:8:3, in step (3), melting environment is 5 * 10 -4the vacuum of Pa, and 15 revs/min of seed rod speed of rotation in its process of growth in step (4), pulling growth speed is that beyond 25mm/ hour, all the other steps are with embodiment 1.The various character of the phase transformation of measure sample and magnetic properties, the sample martensitic transformation temperature of acquisition and the value of Curie temperature are in Table 1.Visible sample is very little in the heat stagnation of room temperature, has shown obvious thermo-elasticity shape memory effect.
Embodiment 6
Preparation consists of: Ni 54mn 35ge 7fe 4the polycrystalline alloy with magnetic shape memory effect; Remove into and be grouped into that in the corresponding Ni:Mn:Ge:Fe=54:35:7:4 of becoming and step (3), to get rid of band process ar pressure be 0.04MPa, copper wheel rotating speed is that beyond 15m/s, all the other steps are with embodiment 2.Accompanying drawing 4 has provided the x ray diffraction spectra of this sample, in visible sample except main BCC mutually, also contain a small amount of γ phase (marking with an asterisk in figure), the existence of the second-phase of this high tenacity can effectively improve the mechanical property of material, solve traditional magnetic shape memory alloy fragility large, the problem of easy fracture.The sample martensitic transformation temperature obtaining and the value of Curie temperature are in Table 1.
The Ni of table 1 heterogeneity xmn yge zm athe Curie temperature T arriving that material is measured after the match at 10Oe cwith martensitic transformation temperature M s, austenite phase transformation temperature A s.
From above-described embodiment, can find out, it is simple that Ni-Mn-Ge is that shape memory alloy alloy has preparation method, the feature that can prepare massive material, it is wider that Ni-Mn-Ge has the composition variation range of martensitic transformation, therefore can adulterate by different compositions, in material, realize magnetic shape memory effect, magnetic field driven martensitic transformation, high tenacity shape memory alloy etc. has the function of practical value, thereby making Ni-Mn-Ge is that shape memory alloy alloy has been widely used at magnetic functional material field tool, for example, as actuator, temperature and/or magnetic sensor, magnetic refrigeration device and equipment, micro-electro-mechanical device and system etc.

Claims (4)

1. Ni-Mn-Ge is a preparation method for magnetic shape memory alloy, and the chemical formula that it is characterized by this alloy is: Ni xmn yge zm a, wherein M is main group element or transition element; Wherein, 51<x<55,31<y<40,5<z<20, a<5, x+y+z+a=100, x, y, z, a represent atom percentage content; Described alloy is monocrystal material or polycrystalline material;
Described main group element is In, Sn, Sb, As or Si;
Described transition element is Ti, Fe or Co;
The preparation method of this alloy is the arbitrary of following two kinds of methods, comprises the steps:
Method one, the preparation of polycrystalline material:
(1) press chemical formula Ni xmn yge zm araw materials weighing, wherein, 51<x<55,31<y<40,5<z<20, a<5, x+y+z+a=100, x, y, z, a represent atom percentage content;
(2) material weighing up is contained in smelting pot, adopts conventional arc melting method to obtain Ni xmn yge zm amagnetic polycrystalline, its melting condition is: at base vacuum, reach 2 * 10 -3when Pa is following, pass into argon gas, whole fusion process sample adopts argon shield, and then high-temperature homogenization is processed 3 days, then quenches to realize ingot casting homogenization of composition;
(3) ingot casting of processing through homogenizing is put into a bottom and be with foraminate silica tube, be placed to and get rid of in band machine furnace chamber, be evacuated down to 1 * 10 -3below Pa, in furnace chamber, pass into high-purity argon gas afterwards, adopt induction heating to make alloy molten, then from silica tube top, be blown into high-purity argon gas and molten alloy liquid be ejected on the copper wheel of high speed rotating from aperture throw away fast, obtain Polycrystalline Metals band;
Or, method two, the preparation of monocrystal material:
(1) press chemical formula Ni xmn yge zm araw materials weighing, wherein, 51<x<55,31<y<40,5<z<20, a<5, x+y+z+a=100, x, y, z, a represent atom percentage content;
(2) material weighing up is contained in smelting pot, adopts conventional arc melting method to obtain Ni xmn yge zm amagnetic polycrystalline, whole fusion process sample adopts argon shield, then carries out high-temperature homogenization and processes 3 days, then quenches to realize ingot casting homogenization of composition;
(3) by the Ni processing through homogenizing xmn yge zm araw material is placed in crucible, adopts conventional Czochralski grown Ni xmn yge zm amagnetic mono crystal, its growth conditions is: heating mentioned component former expect make it melting; Its melting environment is 5 * 10 -3-5 * 10 -5the argon shield gas of the vacuum of Pa or 0.01～1MPa positive pressure; Under the melt temperature condition of 1100～1330 ℃, keep 10～30 minutes;
(4) the fixing seed crystal in seed rod lower end rotating with the speed of 0.5～50 rev/min; Described seed crystal is composition monocrystalline identical or approaching, that have needed orientation, with the liquid level of end in contact melt under seed crystal, then, with the uniform rate lifting seed rod of 3～80mm/ hour, will on the single crystal direction of solidification and crystallization, lift, and keeps isodiametric growth;
(5) when the monocrystalline of growth reaches desired size, single crystal pulling is departed to the raw material surface of melting, with the rate of temperature fall of 0.5～20 ℃/min, slowly reduce temperature and be cooled to room temperature, finally take out.
2. Ni-Mn-Ge as claimed in claim 1 is the preparation method of magnetic shape memory alloy, it is characterized by described preparation method further comprising the steps of: the above-mentioned sample preparing is annealed 0.1～100 hour in the temperature range of 500～1200 ℃ again, and then cooling with the rate of temperature fall of 0.1～1000 ℃/sec.
3. Ni-Mn-Ge as claimed in claim 1 is the preparation method of magnetic shape memory alloy, it is characterized by described step (3) radio frequency heating or the resistive heating mode of 50～245 kilohertzs for growth type of heating.
4. Ni-Mn-Ge as claimed in claim 1 is the preparation method of magnetic shape memory alloy, and the single crystal growing crucible it is characterized by described step (3) is magnetic levitation cold crucible, plumbago crucible or quartz crucible.
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EP3065148A1 (en) * 2015-03-03 2016-09-07 Institute of Modern Physics, Chinese Academy of Sciences Magnetic phase-transformation material
CN110846551A (en) * 2019-11-26 2020-02-28 贵州师范大学 Preparation method of NiMnGaCoCu memory alloy thin strip
CN110846551B (en) * 2019-11-26 2020-12-08 贵州师范大学 Preparation method of NiMnGaCoCu memory alloy thin strip

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