CN101037737A - Magnetic material having magnetic field driven martensitic transformation effect and preparation method thereof - Google Patents
Magnetic material having magnetic field driven martensitic transformation effect and preparation method thereof Download PDFInfo
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- CN101037737A CN101037737A CN 200710064895 CN200710064895A CN101037737A CN 101037737 A CN101037737 A CN 101037737A CN 200710064895 CN200710064895 CN 200710064895 CN 200710064895 A CN200710064895 A CN 200710064895A CN 101037737 A CN101037737 A CN 101037737A
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Abstract
The invention discloses a magnetic material with magnetic-field-driving-martensite phase change effect, the formula of which is: NimConMnoGap, wherein 30<m<55, 2<n<20, 25<o<37, 13<p<25, m+n+o+p=100, m, n, o and p represent atom percentage composition. The invention also discloses a method for preducing the said magnetic material with magnetic-field-driving-martensite phase change effect, including the steps of: (1) weighing the material according to the formula NimConMnoGap, (2)placing weighed material in the crucible, and producing NimConMnoGap magnetic single crystal or multi crystal using normal pulling method, (3) keeping the material in the crucible at the fused temperature of 1000-1330 DEG C for 10-30 minutes and then producing single crystal or multi crystal. The magnetic material NimConMnoGap of the invention has higher controllability than existing alloy, is usable for preparing actuator, temperature and/or magnetic sensitive element, magnetic refrigerating device and apparatus, magnetic memory, micro-electromechanical device and system, ect.
Description
Technical field
The present invention relates to a kind of shape-memory material, have ferromegnetism and bidirectional shape memory effect, particularly relate to and have magnetic field and can drive martensitic transformation and big magneto-resistor and NiCoMnGa magneticsubstance of magnetic entropy character and preparation method thereof.
Background technology
The general shape memorial alloy has a kind of crystalline structure (hereinafter referred to as parent phase) under high relatively temperature, and under low relatively temperature spontaneous another crystalline structure that becomes, generally be referred to as martensitic phase.When from higher greenhouse cooling to lower temperature, material changes martensitic phase into from parent phase, and this changes mutually and is called martensitic transformation.Conversely, from low relatively temperature heating material, alloy can change parent phase into from martensitic phase, and this opposite transformation mutually is called the martensite reverse transformation.Generally, be called M with the starting point and the terminal point of martensitic transformation
sPoint and M
fPoint, beginning and terminal point with the martensite reverse transformation are called A
sPoint and A
fThe point.If M
sAnd A
sBetween difference less, such as be the several years or tens the degree, this martensitic transformation of material is called as thermoelastic martensitic transformation.
Usually, certain alloy material is cooled off with the shape of determining at parent phase, behind martensitic phase, change original shape more artificially, then, alloy material is heated up, when 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 shape of parent phase is out of shape constantly in the phase transformation that cooling causes, the reverse transformation redeformation constantly that causes in subsequently intensification again, and partly or entirely be transformed into the shape of original parent phase, be referred to as bidirectional shape memory effect.
Type purposes that shape memory alloy is widely used in various " intelligence ", as various driving mechanisms, temperature-sensing element, medicine equipment etc.
Some magnetic shape memory alloys of recent findings, as the NiMnIn alloy, this alloy has had the not available new property of a kind of shape-memory material in the past, can drive martensitic transformation by magnetic field that is:.That is to say that it not only has the character of common shape-memory material phase transformation: drive martensitic transformation by temperature variation (heat energy) or external stress (mechanical energy), and its martensitic transformation can be driven by magnetic field.But owing to have the new property of magnetic control phase transformation, thereby this memorial alloy compares with temperature control phase transformation memorial alloy in the past, has better controllability, and its range of application is more extensive.Just because of the good controllability that the magnetic control memorial alloy is showed, make numerous scientists all make great efforts the new memorial alloy that development more has the magnetic control characteristic.
Summary of the invention
Primary and foremost purpose of the present invention is to provide a kind of magneticsubstance with magnetic field driven martensitic transformation effect, this magneticsubstance not only has the character of common shape-memory material phase transformation: drive martensitic transformation by temperature variation (heat energy) or external stress (mechanical energy), and its martensitic transformation can be driven by magnetic field.The controllability of material is improved greatly, and range of application is more extensive.Further aim of the present invention is, a kind of above-mentioned this method with magneticsubstance of magnetic field driven martensitic transformation effect for preparing also is provided.
For achieving the above object, the present invention synthesizes a kind of magneticsubstance with magnetic field driven martensitic transformation effect, and its chemical formula is: Ni
mCo
nMn
oGa
pWherein, 30≤m＜55,2≤n≤20,25＜o＜37,13≤p＜25, m+n+o+p=100, m, n, o, p represent atom percentage content.
Further, described Ni
mCo
nMn
oGa
pThe form of magneticsubstance comprises single crystal structure and polycrystalline structure.
The preparation method of the magneticsubstance with magnetic field driven martensitic transformation effect that the present invention proposes comprises the steps:
(1) presses chemical formula Ni
mCo
nMn
oGa
pRaw materials weighing, wherein, 30≤m＜55,2≤n≤20,25＜o＜37,13≤p＜25, m+n+o+p=100, m, n, o, p represent atom percentage content;
(2) material that will weigh up is contained in the crucible, adopts conventional Czochralski grown Ni
mCo
nMn
oGa
pMagnetic mono crystal, its growth conditions is: the heating mentioned component former expect make it fusion; Its fusion environment is 1 * 10
-2To 5 * 10
-5The argon shield gas of the vacuum of Pa or 0.01～1MPa positive pressure; A seed crystal is fixed in seed rod lower end with 0.5～50 rev/min speed rotation; Described seed crystal is a composition monocrystalline identical or approaching, that have needed orientation;
(3) under 1000～1330 ℃ melt temperature condition, kept 10～30 minutes, liquid level with end in contact melt under the seed crystal, with 3～80mm/ hour uniform rate lifting seed rod, lift on the single crystal direction with solidification and crystallization then, and make the single crystal diameter of growth become big or keep certain;
(4) when the monocrystalline of growth reaches desired size, single crystal pulling is broken away from fused raw material surface, slowly reduce temperature with 0.5～20 ℃/minute rate of temperature fall and be cooled to room temperature, take out at last.
Further, the above-mentioned sample for preparing was annealed in 500～1200 ℃ temperature range 0.01～100 hour again, and then cool off with 0.01～1000 ℃/second rate of temperature fall.
Described growth type of heating can heat or the resistive heating mode with the radio frequency of 50～245 kilohertzs.Described crucible can be magnetic levitation cold crucible, plumbago crucible or quartz crucible.
Magneticsubstance with magnetic field driven martensitic transformation effect provided by the invention, its eigenwert dT/dH (size that unit magnetic field is moved transformation temperature) that shows that magnetic field driven martensitic transformation is renderd a service can be by changing Ni, Co, Mn, Ga ratio of components and changed or adjusted according to purposes.This material under martensitic state because the increase of the magneticstrength that adds can produce the phase transformation (contrary martensitic transformation) from martensite to austenitic field drives.After this reverse transformation has taken place, along with the reduction in magnetic field, material will occur from austenite to martensitic positive martensitic transformation.Thereby show separately by martensitic transformation circulation field drives, recoverable.In above-mentioned circulation, material shows the martensitic transformation that is accompanied by field drives and reverses magneticstrain (magnetostrain) effect that becomes, and numerical value can reach 6.0%.In above-mentioned circulation, material also shows the character (large magnetic resistance effect) of the resistance change with change of magnetic field strength, and the numerical value change amplitude can reach 20-50%.Simultaneously, material also shows the character (magneto-caloric effect) that changes the Entropy Changesization that causes with the phase transformation of field drives and magnetic order degree, changes numerical value and can reach Δ S=9J/Kkg.So, the martensitic transformation magneticsubstance Ni with field drives provided by the invention
mCo
nMn
oGa
pHas purposes widely, driving mechanism for example, temperature and/or magnetic sensor, magnetic refrigeration device and equipment, magneticstorage, micro-electro-mechanical device and system etc.
Description of drawings
Accompanying drawing 1 is Ni of the present invention
mCo
nMn
oGa
pTransformation temperature under the material field drives moves the dT/dH performance;
Accompanying drawing 2 is Ni of the present invention
mCo
nMn
oGa
pMagnetzation curve under the material field drives;
Accompanying drawing 3 is Ni of the present invention
mCo
nMn
oGa
pThe curve in the strain-magnetic field under the monocrystalline field drives;
Accompanying drawing 4 is Ni of the present invention
mCo
nMn
oGa
pThe curve in the resistance-magnetic field under the material field drives.
Embodiment:
Embodiment 1
Preparation consists of: Ni
41Co
9Mn
31Ga
19The magneticalloy with magnetic field driven martensitic transformation effect; adopting growth parameter(s) is the radio frequency heating of 245 kilohertzs, arrives the argon gas of 1MPa positive pressure as shielding gas, in magnetic levitation cold crucible with 0.01; heating power is 20 kilowatts, and its preparation method is undertaken by following concrete steps:
(1) weighing purity respectively is 99.9% Ni, Co, Mn, Ga;
(2) material that will weigh up is put into crucible, is heated to 1230 ℃ of fusions, keeps 10～30 minutes;
(3) with the NiCoMnGa[001 of 2 * 2 * 7mm size] oriented single crystal is the seeded growth monocrystalline; The seed rod speed of rotation is 30 rev/mins in its process of growth, and pulling growth speed is 30mm/ hour;
(4) be 10 millimeters when obtaining diameter, when length is 100 millimeters high quality single crystal, single crystal pulling broken away from fused raw material surface, slowly reduce temperature with 0.5～20 ℃/minute rate of temperature fall and be cooled to room temperature, take out at last;
(5) sample for preparing was annealed in 500-1200 ℃ temperature range 0.01～100 hour again, and then cools off with 0.01～1000 ℃/second rate of temperature fall.
Monocrystalline is cut into the small sample of 4 * 4 * 8mm and the large sample of 10 * 10 * 100mm along [001] direction, measure above-mentioned various character, obtain various characteristics curve as shown in drawings, respective value sees Table 1.
Preparation consists of: Ni
48Co
2Mn
30Ga
20The magneticalloy with magnetic field driven martensitic transformation effect; Different is in quartz crucible, is heated by resistive the method growth, and removing the seed rod speed of rotation is 20 rev/mins, pulling growth speed is outside 20mm/ hour, and all the other measure above-mentioned various character with embodiment 1, obtain various characteristics curve as shown in drawings, respective value sees Table 1.
Embodiment 3
Preparation consists of: Ni
45Co
5Mn
30Ga
20The magneticalloy with magnetic field driven martensitic transformation effect; Removing the seed rod speed of rotation is 10 rev/mins, and pulling growth speed is outside 50mm/ hour, and all the other are with embodiment 1.Measure above-mentioned various character, obtain various characteristics curve as shown in drawings, respective value sees Table 1.
Preparation consists of Ni
39Co
11Mn
31Ga
19The magneticalloy with magnetic field driven martensitic transformation effect; Removing the seed rod speed of rotation is 5 rev/mins, and pulling growth speed is outside 40mm/ hour, and all the other measure above-mentioned various character with embodiment 1, obtain various characteristics curve as shown in drawings, and respective value sees Table 1.
Embodiment 5
Preparation consists of: Ni
37Co
13Mn
32Ga
18The magneticalloy with magnetic field driven martensitic transformation effect; Removing the seed rod speed of rotation is 15 rev/mins, and pulling growth speed is outside 45mm/ hour, and all the other measure above-mentioned various character with embodiment 1, obtain various characteristics curve as shown in drawings, and respective value sees Table 1.
Preparation consists of: Ni
35Co
15Mn
33Ga
17The magneticalloy with magnetic field driven martensitic transformation effect; Removing the seed rod speed of rotation is 20 rev/mins, and pulling growth speed is outside 35mm/ hour, and all the other measure above-mentioned various character with embodiment 1, obtain various characteristics curve as shown in drawings, and respective value sees Table 1.
Embodiment 7
Preparation consists of: Ni
30Co
20Mn
35Ga
15The magneticalloy with magnetic field driven martensitic transformation effect; Removing the seed rod speed of rotation is 25 rev/mins, and pulling growth speed is outside 25mm/ hour, and all the other measure above-mentioned various character with embodiment 1, obtain various characteristics curve as shown in drawings, and respective value sees Table 1.
Preparation consists of: Ni
40Co
7Mn
35Ga
18The magneticalloy with magnetic field driven martensitic transformation effect; Removing the seed rod speed of rotation is 25 rev/mins, and pulling growth speed is outside 25mm/ hour, and all the other measure above-mentioned various character with embodiment 1, obtain various characteristics curve as shown in drawings, and respective value sees Table 1.
Embodiment 9
Preparation consists of: Ni
40Co
14Mn
33Ga
13The magneticalloy with magnetic field driven martensitic transformation effect; Removing the seed rod speed of rotation is 35 rev/mins, and pulling growth speed is outside 25mm/ hour, and all the other measure above-mentioned various character with embodiment 1, obtain various characteristics curve as shown in drawings, and respective value sees Table 1.
Preparation consists of: Ni
39Co
17Mn
30Ga
14The magneticalloy with magnetic field driven martensitic transformation effect; It is 60 rev/mins that its growth conditions removes the seed rod speed of rotation, and pulling growth speed is outside 80mm/ hour, and all the other measure above-mentioned various character with embodiment 1, obtain various characteristics curve as shown in drawings, and respective value sees Table 1.
Embodiment 11
Preparation consists of: Ni
45Co
13Mn
28Ga
14The magneticalloy with magnetic field driven martensitic transformation effect; It is 40 rev/mins that its growth conditions removes the seed rod speed of rotation, and pulling growth speed is outside 15mm/ hour, and all the other measure above-mentioned various character with embodiment 1, obtain various characteristics curve as shown in drawings, and respective value sees Table 1.
The Ni of table 1 heterogeneity
mCo
nMn
oGa
pThe dT/dH numerical value of material, magneticstrain (magnetostrain) value λ, magneto-resistor MR value and magnetic entropy become (Δ S) numerical value
| Composition | dT/dH (K/T) | λ (％) | MR (％) | ΔS (J/Kkg) |
| Ni 41Co 9Mn 31Ga 19 | 10 | 4.1 | 30 | 7.1 |
| Ni 48Co 2Mn 30Ga 20 | 2.7 | 5.0 | 21 | 5 |
| Ni 45Co 5Mn 30Ga 20 | 3.5 | 4.8 | 25 | 5.5 |
| Ni 39Co 11Mn 31Ga 19 | 11.6 | 5.5 | 32 | 5.7 |
| Ni 37Co 13Mn 32Ga 18 | 13.2 | 4 | 35 | 5.8 |
| Ni 35Co 15Mn 33Ga 17 | 15.5 | 3.8 | 37 | 6.2 |
| Ni 30Co 20Mn 35Ga 15 | 18.3 | 3.5 | 42 | 5.9 |
| Ni 40Co 7Mn 35Ga 18 | 5.8 | 4.8 | 28 | 8.6 |
| Ni 40Co 14Mn 33Ga 13 | 14.9 | 3.0 | 33 | 7.5 |
| Ni 46Co 7Mn 25Ga 22 | 2.1 | 5.1 | 20 | 4.1 |
| Ni 45Co 13Mn 28Ga 14 | 20 | 4.2 | 31 | 6.9 |
Claims (5)
1. magneticsubstance with magnetic field driven martensitic transformation effect, its chemical formula is: Ni
mCo
nMn
oGa
pWherein, 30≤m＜55,2≤n≤20,25＜o＜37,13≤p＜25, m+n+o+p=100, m, n, o, p represent atom percentage content.
2. the magneticsubstance with magnetic field driven martensitic transformation effect as claimed in claim 1 is characterized in that, described Ni
mCo
nMn
oGa
pThe form of magneticsubstance comprises single crystal structure and polycrystalline structure.
3. one kind prepares claim 1 or 2 described methods with magneticsubstance of magnetic field driven martensitic transformation effect, comprises the steps:
(1) presses chemical formula Ni
mCo
nMn
oGa
pRaw materials weighing, wherein, 30＜m＜55,2＜n＜20,25＜0＜37,13＜p＜25, m+n+o+p=100, m, n, o, p represent atom percentage content;
(2) raw material that weighs up is contained in the crucible, adopts conventional Czochralski grown Ni
mCo
nMn
oGa
pMagnetic mono crystal or polycrystalline, its growth conditions is: the heating mentioned component former expect make it fusion; Its fusion environment is 1 * 10
-2To 5 * 10
-5The argon shield state of the vacuum state of Pa or 0.01～1MPa positive pressure; Fix a seed crystal in the seed rod lower end that rotates with 0.5～50 rev/min speed; Described seed crystal is composition monocrystalline identical or approaching, that have needed orientation or polycrystalline;
(3) raw material in the crucible was kept 10～30 minutes under 1000～1330 ℃ fused temperature condition, liquid level with end in contact melt under the seed crystal, promote seed rod with 3～80mm/ hour uniform rate then, the monocrystalline or the polycrystalline of solidification and crystallization are upwards lifted, and make the monocrystalline of growth or polycrystalline diameter become big or keep certain;
(4) when the monocrystalline of growth or polycrystalline when reaching desired size, it is lifted break away from fused raw material surface, be cooled to room temperature with 0.5～20 ℃/minute rate of temperature fall, take out at last.
4. as a kind of method for preparing magneticsubstance as described in the claim 3, it is characterized in that, also comprise step (5): the above-mentioned magneticalloy for preparing was annealed 0.01～100 hour again, and then be cooled to room temperature with 0.01～1000 ℃/second rate of temperature fall in 500～1200 ℃ temperature range.
5. as a kind of method for preparing magneticsubstance as described in the claim 3, it is characterized in that the growth type of heating described in the above-mentioned steps (2) can adopt the radio frequency heating or the resistive heating mode of 50～245 kilohertzs; Described crucible can be magnetic levitation cold crucible or plumbago crucible or quartz crucible.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102228964A (en) * | 2011-06-21 | 2011-11-02 | 哈尔滨工业大学 | Method for preparing Ni-Mn-Ga ferromagnetic shape memory alloy continuous fibers by adopting spinning method |
| CN103334043A (en) * | 2013-03-22 | 2013-10-02 | 中国科学院物理研究所 | Magnetic alloy serving as magnetic refrigeration material |
| CN103741003A (en) * | 2014-01-07 | 2014-04-23 | 大连大学 | Novel high-temperature magnetic shape memory alloy and preparation method thereof |
| CN105714378A (en) * | 2014-12-05 | 2016-06-29 | 中国科学院福建物质结构研究所 | Crystal material, preparation method thereof and magnetic refrigerating material applying crystal material |
| CN106282865A (en) * | 2015-06-29 | 2017-01-04 | 中国科学院宁波材料技术与工程研究所 | The method of refrigeration temperature area when expansion primary magnetic phase change material is applied as magnetic cooling material |
| CN108950277A (en) * | 2018-08-02 | 2018-12-07 | 大连大学 | A kind of method of combustion reaction high―temperature nuclei NiMnGa Magnetic Memory alloy |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP3881741B2 (en) * | 1997-03-19 | 2007-02-14 | Ｎｅｃトーキン株式会社 | NiMnGa alloy |
| JP2002285269A (en) * | 2001-03-27 | 2002-10-03 | Daido Steel Co Ltd | Ferromagnetic shape memory alloy |
| CN1310257C (en) * | 2004-09-24 | 2007-04-11 | 中国科学院物理研究所 | Magnetic material with bidirectional shape memory effect and single-crystal producing method thereof |
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- 2007-03-28 CN CNB2007100648955A patent/CN100465314C/en not_active Expired - Fee Related
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102228964A (en) * | 2011-06-21 | 2011-11-02 | 哈尔滨工业大学 | Method for preparing Ni-Mn-Ga ferromagnetic shape memory alloy continuous fibers by adopting spinning method |
| CN102228964B (en) * | 2011-06-21 | 2012-09-26 | 哈尔滨工业大学 | Method for preparing Ni-Mn-Ga ferromagnetic shape memory alloy continuous fibers by adopting spinning method |
| CN103334043A (en) * | 2013-03-22 | 2013-10-02 | 中国科学院物理研究所 | Magnetic alloy serving as magnetic refrigeration material |
| CN103334043B (en) * | 2013-03-22 | 2015-07-08 | 中国科学院物理研究所 | Magnetic alloy serving as magnetic refrigeration material |
| CN103741003A (en) * | 2014-01-07 | 2014-04-23 | 大连大学 | Novel high-temperature magnetic shape memory alloy and preparation method thereof |
| CN105714378A (en) * | 2014-12-05 | 2016-06-29 | 中国科学院福建物质结构研究所 | Crystal material, preparation method thereof and magnetic refrigerating material applying crystal material |
| CN105714378B (en) * | 2014-12-05 | 2018-06-15 | 中国科学院福建物质结构研究所 | A kind of crystalline material, preparation method and the magnetic refrigerating material using the crystal |
| CN106282865A (en) * | 2015-06-29 | 2017-01-04 | 中国科学院宁波材料技术与工程研究所 | The method of refrigeration temperature area when expansion primary magnetic phase change material is applied as magnetic cooling material |
| CN106282865B (en) * | 2015-06-29 | 2017-11-10 | 中国科学院宁波材料技术与工程研究所 | The method for expanding refrigeration temperature area when primary magnetic phase change material is applied as magnetic cooling material |
| CN108950277A (en) * | 2018-08-02 | 2018-12-07 | 大连大学 | A kind of method of combustion reaction high―temperature nuclei NiMnGa Magnetic Memory alloy |
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