CN107142389B - High-strength, the high-ductility Ni of one kind50Mn34In16-xCoxThe preparation method of Magnetic Memory alloy - Google Patents
High-strength, the high-ductility Ni of one kind50Mn34In16-xCoxThe preparation method of Magnetic Memory alloy Download PDFInfo
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- 229910001285 shape-memory alloy Inorganic materials 0.000 title claims abstract description 33
- 230000005291 magnetic effect Effects 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 238000005245 sintering Methods 0.000 claims abstract description 18
- 239000000843 powder Substances 0.000 claims description 66
- 239000000956 alloy Substances 0.000 claims description 38
- 229910045601 alloy Inorganic materials 0.000 claims description 37
- 239000002184 metal Substances 0.000 claims description 30
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- 238000002156 mixing Methods 0.000 abstract description 8
- 238000005238 degreasing Methods 0.000 abstract description 5
- 230000008901 benefit Effects 0.000 abstract description 3
- 238000000465 moulding Methods 0.000 abstract 1
- 238000001746 injection moulding Methods 0.000 description 7
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- 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
- C22C1/0433—Nickel- or cobalt-based alloys
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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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
-
- 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
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/103—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material containing an organic binding agent comprising a mixture of, or obtained by reaction of, two or more components other than a solvent or a lubricating agent
-
- 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
- B22F3/115—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by spraying molten metal, i.e. spray sintering, spray casting
Abstract
The present invention relates to a kind of preparation method of magnetic shape memory alloy, especially a kind of high-strength, high-ductility Ni50Mn34In16‑xCoxThe preparation method of Magnetic Memory alloy.According to atomic percent feeding, mixing, molding, degreasing, sintering to get high-strength to high intensity, high-ductility Ni50Mn34In16‑xCox(x=2,3,4,5).Magnetic shape memory alloy Ni prepared by the present invention50Mn34In16‑xCox(x=2,3,4,5) has many advantages, such as that good toughness, intensity is big, fine microstructures.For the application extension thinking of high temperature high-ductility marmem.
Description
Technical field
The present invention relates to high-strength, the high-ductility Ni of one kind50Mn34In16-xCoxThe preparation method of Magnetic Memory alloy.
Background technology
1996, Ullakko et al. was for the first time in Ni2The reversible strain that about 0.2% is obtained in MnGa monocrystalline, is pulled open since then
The research prelude of magnetic driven memory alloy, has become the research hotspot in marmem field.Current research is wide
Magnetic driven memory alloy includes mainly：Ni-Mn-Ga (Al), Ni-Fe-Ga, Co-Ni-Ga (Al) and novel Ni-Mn-In
(Sn, Sb) alloy.Ni-Mn-Ga based alloys are to find earliest and study most commonly used magnetic marmem at present,
Magnetic-field-induced strain derives from martensitic twin variant under external magnetic field and resets the macro-strain generated, has such deformation mechanism
Alloy to obtain the key of big magnetic-field-induced strain be to have high magnetocrystalline anisotropy energy and low twin boundary migration limit stress.
At present in Ni-Mn-Ga series alloys, monocrystalline maximum reversible strain property reaches 10%, but due to defeated caused by variant rearrangement
It is smaller to go out stress, only 2MPa or so, it is difficult to meet the application requirement of Practical Project.In the recent period, novel magnetic driven memory alloy system
Ni-Mn-X (X=In, Sn, Sb) causes the attention of various countries researcher.Series Heulser alloys are in nonstoichiometry ratio
With thermoelastic martensitic transformation, magnetic truly is realized in certain composition range or after the ferromagnetic Elements C o of doping
Driving phase transformation, generates macro-strain, the essence of the series alloy magnetic-field-induced strain be martensitic phase with parent phase with larger
Saturation magnetization is poor, and alloy transformation temperature significantly reduces under external magnetic field, applies external magnetic field in certain temperature range
Martensite reverse transformation can then be brought it about to have shape memory effect, and export larger stress.But Ni-Mn-In is closed
The defects such as that there are still brittleness is big for golden system, and the threshold value of field drives phase transformation is high, and Curie temperature is low, limit it to a certain extent
Practical application.So how to improve magnetic field life strain, field drives threshold value is reduced, improves alloy mechanical performance, obtains big
Magnetic entropy becomes and giant magnetoresistance effect, it has also become memorial alloy is applied and the main direction of studying of development.
Refined crystalline strengthening can significantly change alloy transformation temperature and improve its mechanical performance and physical property.Therefore pass through gold
Belong to injection moulding and sintering process combines and prepares Ni50Mn34In16Magnetic Memory alloy improves alloy mechanical property and improves magnetics
One of effective ways of performance.
Metal injection moulding (Metal Injection Molding, abbreviation MIM) is a kind of from injection molding of plastics industry
In the novel powder metallurgy forming technique extending out, it is well known that the cheap price production of injection molding of plastics technology is various
The product of complicated shape, but plastic products intensity is not high, in order to improve its performance, can add metal or ceramic powder in the plastic
End is to obtain the product that intensity is higher, wearability is good.In recent years, development evolvement is to improve solid to the maximum extent to this idea
The content of particle and in subsequent sintering process completely remove no-bonder and make forming base be densified.
Invention content
It is big in order to solve existing Ni-Mn-In-Co suitable shape memory alloys brittleness, the high problem of driving magnetic field threshold value,
The present invention provide it is a kind of by metal injection moulding and sintering process in conjunction with preparing Ni50Mn34In16-xCox(x=2,3,4,5)
The method of Magnetic Memory alloy.
The marmem of the present invention is prepared as follows：According to atomic percent take 50 parts Ni powder, 34
The Mn powder, 11-14 parts of In powder and 2-5 parts of Co powder of part are uniformly mixed by blender, and a certain amount of binder is then added and carries out
It is kneaded, is then injection moulded by metallic injection machine, it is last degreasing sintered, Ni is made50Mn34In16-xCox(x=2,3,4,
5) Magnetic Memory alloy.
More specifically, Ni of the present invention50Mn34In16-xCoxThe preparation method of (x=2,3,4,5) Magnetic Memory alloy is as follows：
Before sintering, the Ni powder that grain size is 300 mesh, Mn powder, In powder and Co powder is taken to mix according to atomic percent, with 200 in blender
Turn/min-500 turns/min is uniformly mixed to stir metal powder, the binder of metal powder gross mass 2%-5% is then added
So that it is sufficiently mixed uniformly with metal powder, be then added in metallic injection machine, makes to glue by being heated to 200 DEG C -400 DEG C
Tie agent to melt, then 20-40 kilograms of pressure 10h-48h applied to mold, obtain injection embryo, finally will injection base through degreasing at
Reason, uses 1500 DEG C -1700 DEG C of temperature, 200-400 kilograms of pressure, vacuum degree 10-3-10-4MPa, time are 20-40 minutes
Sintering process is sintered, and finally obtains the Ni that grain size is about 50-60 microns50Mn34In16-xCox(x=2,3,4,5) Magnetic Memory closes
Gold.
Preferably, the binder is epoxy resin and polyamide with 4：1 mass ratio mixes.
Binder is the core of Metal Injection Molding, and binder has enhancing mobility to be suitble to injection in MIM
It is molded and maintains the effect of briquet shape, it should also have the characteristics that readily removed, pollution-free, non-toxic, cost is reasonable in addition,
Occur various binders thus, Recent study personnel just gradually select from rule of thumb to according to degreasing method
And the requirement to binder function, the direction for targetedly designing binder system are developed.Inventor is by repeatedly
Test of many times obtains most suitable Ni50Mn34In16-xCoxThe binder of (x=2,3,4,5) Magnetic Memory alloy, in the binder
Under effect, make metal powder that there is good cavity filling, while there is good degreasing, keeps the consistency of alloy high, burning
Good performance is obtained after knot.Ni50Mn34In12The reason of Co4 gold excellent in mechanical performance, the crystal grain of mainly alloy was more tiny, and
And there is (Co, Ni) in the alloyxThe second phases of In, therefore the mechanical property of alloy is made to be greatly improved.
Advantageous effect
The marmem Ni that the method for the present invention is prepared50Mn34In16-xCox(x=2,3,4,5) different existing warps
Magnetic shape memory alloy Ni prepared by arc melting method50Mn34In16-xCox(x=2,3,4,5), and by comparison have with
Lower advantage：
Ni prepared by the present invention50Mn34In16-xCoxThere is (x=2,3,4,5) alloy higher fracture strength and fracture to answer
Become, the magnetic shape memory alloy fine microstructures, good toughness, intensity is big, with excellent magnetic performance, is high temperature high-ductility shape
The application extensions of shape memory alloys thinking.
Description of the drawings
Fig. 1 is Ni prepared by embodiment 450Mn34In11Co5Alloy carries out the test curve of fracture strength and breaking strain
Figure；
Fig. 2 a are Ni prepared by the present invention50Mn34In16-xCoxThe fracture strength of (x=2,3,4,5) alloy is with Co contents
Variation relation；
Fig. 2 b are Ni prepared by the present invention50Mn34In16-xCoxThe breaking strain of (x=2,3,4,5) alloy is with Co contents
Variation relation；
Fig. 3 a are Ni prepared by the present invention50Mn34In14Co2Alloy optical microscope photograph at room temperature；
Fig. 3 b are Ni prepared by the present invention50Mn34In11Co5Alloy optical microscope photograph at room temperature.
Specific implementation mode
The present invention is described in further detail below by embodiment, but is not limited the scope of the invention.Such as without spy
Different explanation, experimental method of the present invention is conventional method, and experiment equipment used, material, reagent etc. can be chemically
Company buys.Preferably, the equipment that sintering process selects in the embodiment of the present invention is the production of Japanese Zhu You coals Co., Ltd.
SPS 1050.The highest pulse current of the equipment is 5000A, and maximum sintering temperature can reach 2000 DEG C, maximum axial pressure
Power is 100KN, and vacuum degree is up to 6Pa.
Embodiment 1
High-strength, high-ductility Ni50Mn34In14Co2Magnetic Memory alloy is prepared as follows：It is taken according to atomic percent
Grain size is 14 parts of 34 parts of 50 parts of Ni powder, Mn powder, In powder and 2 parts of mixing of Co powder of 300 mesh, is turned with 200 turns/min in blender
Speed stirring metal powder, makes it be uniformly mixed, binder (the m epoxy resin of metal powder gross mass 2wt% is then added：M is poly-
Amide=4：1) so that it is sufficiently mixed uniformly, then said mixture is added in metallic injection machine, by being heated to 200
So that binder is melted drives metal powder to enter in mold cavity, is applying 20-40 kilograms of pressure/10h- to mold
Then 48h obtains injection embryo, finally through ungrease treatment, finally utilize 1500 DEG C -1700 DEG C, it is 200-400 kilograms of pressure, true
Reciprocal of duty cycle is 10-3-10-4MPa, time are that 20-40 minutes sintering process are sintered, and it is about 50-60 microns to finally obtain grain size
Ni50Mn34In14Co2Magnetic Memory alloy.
Embodiment 2
High-strength, high-ductility Ni50Mn34In13Co3Magnetic Memory alloy is prepared as follows：It is taken according to atomic percent
Grain size is 13 parts of 34 parts of 50 parts of Ni powder, Mn powder, In powder and 3 parts of mixing of Co powder of 300 mesh, is turned with 200 turns/min in blender
Speed stirring metal powder, makes it be uniformly mixed, binder (the m epoxy resin of metal powder gross mass 2wt% is then added：M is poly-
Amide=4：1) so that it is sufficiently mixed uniformly, then said mixture is added in metallic injection machine, by being heated to 200
So that binder is melted drives metal powder to enter in mold cavity, is applying 20-40 kilograms of pressure/10h- to mold
Then 48h obtains injection embryo, finally through ungrease treatment, finally utilize 1500 DEG C -1700 DEG C, it is 200-400 kilograms of pressure, true
Reciprocal of duty cycle is 10-3-10-4MPa, time are that 20-40 minutes sintering process are sintered, and it is about 50-60 microns to finally obtain grain size
Ni50Mn34In13Co3Magnetic Memory alloy.
Embodiment 3
High-strength, high-ductility Ni50Mn34In12Co4Magnetic Memory alloy is prepared as follows：It is taken according to atomic percent
Grain size is 12 parts of 34 parts of 50 parts of Ni powder, Mn powder, In powder and 4 parts of mixing of Co powder of 300 mesh, is turned with 200 turns/min in blender
Speed stirring metal powder, makes it be uniformly mixed, binder (the m epoxy resin of metal powder gross mass 2wt% is then added：M is poly-
Amide=4：1) so that it is sufficiently mixed uniformly, then said mixture is added in metallic injection machine, by being heated to 200
So that binder is melted drives metal powder to enter in mold cavity, is applying 20-40 kilograms of pressure/10h- to mold
Then 48h obtains injection embryo, finally through ungrease treatment, finally utilize 1500 DEG C -1700 DEG C, it is 200-400 kilograms of pressure, true
Reciprocal of duty cycle is 10-3-10-4MPa, time are that 20-40 minutes sintering process are sintered, and it is about 50-60 microns to finally obtain grain size
Ni50Mn34In12Co4Magnetic Memory alloy.
Embodiment 4
High-strength, high-ductility Ni50Mn34In11Co5Magnetic Memory alloy is prepared as follows：It is taken according to atomic percent
Grain size is 11 parts of 34 parts of 50 parts of Ni powder, Mn powder, In powder and 5 parts of mixing of Co powder of 300 mesh, is turned with 200 turns/min in blender
Speed stirring metal powder, makes it be uniformly mixed, binder (the m epoxy resin of metal powder gross mass 2wt% is then added：M is poly-
Amide=4：1) so that it is sufficiently mixed uniformly, then said mixture is added in metallic injection machine, by being heated to 200
So that binder is melted drives metal powder to enter in mold cavity, is applying 20-40 kilograms of pressure/10h- to mold
Then 48h obtains injection embryo, finally through ungrease treatment, finally utilize 1500 DEG C -1700 DEG C, it is 200-400 kilograms of pressure, true
Reciprocal of duty cycle is 10-3-10-4MPa, time are that 20-40 minutes sintering process are sintered, and it is about 50-60 microns to finally obtain grain size
Ni50Mn34In11Co5Magnetic Memory alloy.
Embodiment 5
High-strength, high-ductility Ni50Mn34In11Co5Magnetic Memory alloy is prepared as follows：It is taken according to atomic percent
Grain size is 11 parts of 34 parts of 50 parts of Ni powder, Mn powder, In powder and 5 parts of mixing of Co powder of 300 mesh, is turned with 200 turns/min in blender
Speed stirring metal powder, makes it be uniformly mixed, binder (the m epoxy resin of metal powder gross mass 2wt% is then added：M is poly-
Amide=4：1) so that it is sufficiently mixed uniformly, then said mixture is added in metallic injection machine, by being heated to 400
So that binder is melted drives metal powder to enter in mold cavity, is applying 20-40 kilograms of pressure/10h- to mold
Then 48h obtains injection embryo, finally through ungrease treatment, finally utilize 1500 DEG C -1700 DEG C, it is 200-400 kilograms of pressure, true
Reciprocal of duty cycle is 10-3-10-4MPa, time are that 20-40 minutes sintering process are sintered, and it is about 50-60 microns to finally obtain grain size
Ni50Mn34In11Co5Magnetic Memory alloy.
Embodiment 6
High-strength, high-ductility Ni50Mn34In14Co2Magnetic Memory alloy is prepared as follows：It is taken according to atomic percent
Grain size is 14 parts of 34 parts of 50 parts of Ni powder, Mn powder, In powder and 2 parts of mixing of Co powder of 300 mesh, is turned with 400 turns/min in blender
Speed stirring metal powder, makes it be uniformly mixed, binder (the m epoxy resin of metal powder gross mass 5wt% is then added：M is poly-
Amide=4：1) so that it is sufficiently mixed uniformly, then said mixture is added in metallic injection machine, by being heated to 200
So that binder is melted drives metal powder to enter in mold cavity, is applying 40 kilograms of pressure 48h to mold, then
To injection embryo, finally in pressure, the vacuum degree 10 for through ungrease treatment, finally utilizing 1600 DEG C, 200 kilograms-3MPa, time is
Sintering process sintering in 30 minutes, finally obtains the Ni that grain size is about 50-60 microns50Mn34In14Co2Magnetic Memory alloy.
Comparative example
Ni is prepared using arc melting method50Mn34In11Co5Alloy：It is the Ni of 300 mesh to take grain size according to atomic percent
5 parts of 50 parts of powder, 34 parts of Mn powder, 11 parts of In powder and Co powder mixing are positioned over smelting furnace melting, be made after sample through cooling, cleaning,
Heat preservation obtains Ni50Mn34In11Co5Alloy.
Alloy prepared by embodiment 4 and comparative example is carried out to the test of fracture strength and breaking strain, the survey of embodiment 4
Test result is as shown in Figure 1.Ni prepared by the present invention50Mn34In11Co5Alloy fracture intensity is in 8805 Mpa, arc melting method side
Ni prepared by method50Mn34In16The fracture strength of alloy is about Ni prepared by the 400MPa present invention50Mn34In11Co5Alloy ratio compares
Example improves about 8300Mpa；And the Ni only prepared by the method for sintering50Mn29Ga21Its fracture strength of alloy is about 1700MPA.
By obtained Ni in the present embodiment 1-450Mn34In16-xCoxThe fracture strength of (x=2,3,4,5) and fracture are answered
Become as shown in Figure 2 a and 2 b with the variation test result of Co contents；Ni prepared by the present invention50Mn34In16-xCox(x=2,3,
4,5) Ni of the fracture strength of alloy than arc melting method50Mn34In16-xCoxAlloy improves about 200, and as x=5, fracture is answered
Become 20, than existing Ni50Mn34In11Co5The breaking strain of alloy improves 15%, improves 4 times than Ni-Mn-Ga alloy, says
Ni prepared by the bright present invention50Mn34In11Co5Alloy ductility is big.
High-strength, high-ductility Ni prepared by embodiment 1 and embodiment 450Mn34In14Co2Alloy and Ni50Mn34In11Co5
Alloy carries out structure observation analysis at room temperature, and the results are shown in Figure 3.The alloy that as seen in Figure 3 prepared by the present invention is brilliant
More tiny, the Ni of grain50Mn34In11Co2The crystallite dimension of alloy significantly reduces, probably about 50 microns of diameter, and Ni50Mn34In11Co5
The fine microstructures of alloy, are dispersed with the second more tiny phase in crystal grain, and this method plays the role of crystal grain refinement.
In conclusion magnetic shape memory alloy Ni prepared by the method for the present invention50Mn34In16-xCox(x=2,3,4,5)
Have many advantages, such as that good toughness, intensity is big, fine microstructures.
Claims (2)
1. high-strength, the high-ductility Ni of one kind50Mn34In16-xCoxThe preparation method of Magnetic Memory alloy, which is characterized in that step is specific
For：Before sintering, it is 50 parts of Ni powder, 34 parts of Mn powder, 11-14 parts of In powder and the 2-5 parts of Co of 300 mesh to take grain size according to atomic percent
Powder mixes, and is uniformly mixed with 200 turns/min-500 turns/min to stir metal powder in blender, metal powder is then added
The binder of gross mass 2%-5% makes it be sufficiently mixed uniformly with metal powder, is then added in metallic injection machine, passes through
Being heated to 200 DEG C -400 DEG C makes binder melt, then applies 20-40 kilograms of pressure 10h-48h to mold, obtains injection embryo,
Base will finally be injected through ungrease treatment, use 1500 DEG C -1700 DEG C of temperature, 200-400 kilograms of pressure, vacuum degree 10-3-10- 4MPa, time are that 20-40 minutes sintering process are sintered, and finally obtain the Ni that grain size is about 50-60 microns50Mn34In16-xCoxMagnetic
Memorial alloy, the binder are epoxy resin and polyamide with 4:1 mass ratio mixes, wherein x=2, and 3,4,5.
2. high-strength, the high-ductility Ni of one kind50Mn34In16-xCoxMagnetic Memory alloy, which is characterized in that according to side described in claim 1
It is prepared by method.
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| CN201710306539.3A CN107142389B (en) | 2017-05-04 | 2017-05-04 | High-strength, the high-ductility Ni of one kind50Mn34In16-xCoxThe preparation method of Magnetic Memory alloy |
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| CN108950275B (en) * | 2018-08-02 | 2020-09-22 | 大连大学 | Method for synthesizing NiCoMnin magnetic memory alloy at high temperature through combustion reaction |
| CN108929963B (en) * | 2018-08-02 | 2020-02-18 | 大连大学 | High-wear-resistance Ni50Mn34In16-xCoxPreparation method of magnetic memory alloy |
| CN109022864B (en) * | 2018-08-02 | 2020-04-07 | 大连大学 | Method for synthesizing NiMnGaCo magnetic memory alloy at high temperature through combustion reaction |
| CN108950274B (en) * | 2018-08-02 | 2020-05-19 | 大连大学 | Preparation method of high-corrosion-resistance NiMnInCo magnetic shape memory alloy |
| CN113684390A (en) * | 2021-08-16 | 2021-11-23 | 大连大学 | Method for preparing hyperelastic NiMnInCo magnetic memory alloy by liquid die forging |
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| CN105296925B (en) * | 2015-07-27 | 2018-07-06 | 大连大学 | The method that laser pulse sputtering sedimentation prepares Ni-Mn-Co-In alloy firms |
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| CN105448443A (en) * | 2015-11-26 | 2016-03-30 | 北京科技大学 | Preparation method of bonding martensitic phase change material |
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Application publication date: 20170908 Assignee: Dalian Funuo Machinery Co.,Ltd. Assignor: DALIAN University Contract record no.: X2023210000252 Denomination of invention: A Preparation Method for High Strength and High Plasticity Ni50Mn34In16-xCoxMagnetic Memory Alloy Granted publication date: 20181102 License type: Common License Record date: 20231129 Application publication date: 20170908 Assignee: Dalian Sanfengsheng Heavy Industry Machinery Co.,Ltd. Assignor: DALIAN University Contract record no.: X2023210000251 Denomination of invention: A Preparation Method for High Strength and High Plasticity Ni50Mn34In16-xCoxMagnetic Memory Alloy Granted publication date: 20181102 License type: Common License Record date: 20231129 Application publication date: 20170908 Assignee: DALIAN MENGYU MACHINERY CO.,LTD. Assignor: DALIAN University Contract record no.: X2023210000220 Denomination of invention: A Preparation Method for High Strength and High Plasticity Ni50Mn34In16-xCoxMagnetic Memory Alloy Granted publication date: 20181102 License type: Common License Record date: 20231129 |