CN107699667B - A method of preparing magnetic Fe-Mn-Si base marmem - Google Patents
A method of preparing magnetic Fe-Mn-Si base marmem Download PDFInfo
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- CN107699667B CN107699667B CN201710858157.1A CN201710858157A CN107699667B CN 107699667 B CN107699667 B CN 107699667B CN 201710858157 A CN201710858157 A CN 201710858157A CN 107699667 B CN107699667 B CN 107699667B
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- 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
- C21D6/00—Heat treatment of ferrous alloys
- C21D6/004—Heat treatment of ferrous alloys containing Cr and Ni
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- 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
- C21D6/00—Heat treatment of ferrous alloys
- C21D6/005—Heat treatment of ferrous alloys containing Mn
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- 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
- C21D6/00—Heat treatment of ferrous alloys
- C21D6/007—Heat treatment of ferrous alloys containing Co
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- 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
- C21D6/00—Heat treatment of ferrous alloys
- C21D6/008—Heat treatment of ferrous alloys containing Si
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/10—Ferrous alloys, e.g. steel alloys containing cobalt
- C22C38/105—Ferrous alloys, e.g. steel alloys containing cobalt containing Co and Ni
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/12—Ferrous alloys, e.g. steel alloys containing tungsten, tantalum, molybdenum, vanadium, or niobium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/14—Ferrous alloys, e.g. steel alloys containing titanium or zirconium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
- C22C38/44—Ferrous alloys, e.g. steel alloys containing chromium with nickel with molybdenum or tungsten
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
- C22C38/46—Ferrous alloys, e.g. steel alloys containing chromium with nickel with vanadium
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
- C22C38/48—Ferrous alloys, e.g. steel alloys containing chromium with nickel with niobium or tantalum
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
- C22C38/50—Ferrous alloys, e.g. steel alloys containing chromium with nickel with titanium or zirconium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
- C22C38/52—Ferrous alloys, e.g. steel alloys containing chromium with nickel with cobalt
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
- C22C38/58—Ferrous alloys, e.g. steel alloys containing chromium with nickel with more than 1.5% by weight of manganese
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- 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
- C21D2201/00—Treatment for obtaining particular effects
- C21D2201/01—Shape memory effect
Abstract
The invention discloses a kind of methods for preparing magnetic Fe-Mn-Si base marmem, belong to marmem field.It is difunctional that Fe-Mn-Si base marmem prepared by the present invention possesses magnetic and shape memory effect.Fe-Mn-Si base marmem of the present invention contains Fe, Mn and Si element, it and include one of Cr, Ni, Ti, Nb, Cu, Co, V, Mo, Al, C and N element or a variety of, the specific method is as follows: first handling above-mentioned Fe-Mn-Si base marmem >=30 minutes with 1000 DEG C ~ 1300 DEG C in the environment of vacuum degree≤1Pa, subsequent air-cooled or oil cooling or water cooling to room temperature；There are one layer of ferrite, and ferrite lamellae average thickness >=3 micron in the surface of the magnetic Fe-Mn-Si base marmem of above method preparation.Fe-Mn-Si base marmem is in high temperature ferrite monophase field at 1250 DEG C ~ 1300 DEG C.
Description
Technical field
The present invention relates to marmem fields, and in particular to a kind of to prepare magnetic Fe-Mn-Si base marmem
Method.Compared with conventional Fe-Mn-Si base marmem, the Fe-Mn-Si base marmem of this method preparation possesses magnetic
Property and shape memory are difunctional, to expand the application field of such alloy, such as magnetic sensor and driver etc..
Background technique
Compared with NiTi base memorial alloy, Fe-Mn-Si base marmem has low cost and excellent processability
The characteristics of energy and weldability, so since the advent of the world just has received widespread attention.The memory of Fe-Mn-Si base marmem
Stress induces martensite transfor mation and its heating of the austenite of face-centred cubic structure to close-packed hexagonal structure when effect is derived from deformation
Reverted austenite in the process.It is worth noting that the austenite of face-centred cubic structure and the martensite of close-packed hexagonal structure are paramagnetic
Property, without magnetism.If it is magnetic to assign ferrimanganic silicon-base alloy, we will obtain one kind and possess magnetic and shape memory
The difunctional marmem of effect.In this case, the application range of ferrimanganic silicon-base alloy is by further expansion, such as can
It is used to prepare magnetic sensor and driver.Kanada in 1999 etc. is by the method for oxidation on FeMnSiCr memorial alloy surface
Form one layer of magnetic Fe3O4Oxide layer is obtained for the first time with shape memory effect and magnetic difunctional ferrimanganic silicon substrate shape note
Recall alloy (Journal of Magnetism and Magnetic Materials, 1999,196-197:349-350).
However, when the FeMnSiCr memorial alloy deformation prepared to this method, magnetic Fe3O4Oxide layer will fall off.Todaka etc. is then
Be be prepared for using the method for fast melt-quenching it is a series of there are magnetic and memory performance iron-base marmems, such as
FeMnCrNiCoSi strip (Journal of Applied Physics, 91:7448-7450; Journal of
Magnetism and Magnetic Materials, 2003,254-255:410-412), FeCrNiSiMn strip
(Journal of Materials Processing Technology, 2007,181:217-221) SiFe/FeMnSi is bis-
Layer strip (IEEE Transactions on Magnetics, 2011,47:3184-3187), SiFe/FeMnCrSiB are bis-
Layer strip (IEEE Transactions on Magnetics, 2014,50:2501304).Valeanu etc. also uses melt
The method of fast quenching is prepared for magnetic Fe MnSi base marmem strip (Journal of Magnetism and
Magnetic Materials, 2008,320:e164-e167).It is worth noting that melt-quenching method is to equipment requirement
Height, and strip two-dimensional material can only be obtained, limit to the application of magnetic Fe-Mn-Si base marmem.Therefore, how to use
The magnetic Fe-Mn-Si base marmem that conventional equipment can prepare needles of various sizes is current urgent problem to be solved.
Summary of the invention
The object of the present invention is to provide a kind of methods for preparing magnetic Fe-Mn-Si base marmem.
Fe-Mn-Si base marmem mainly contains tri- kinds of elements of Fe, Mn and Si, and include Cr, Ni, Ti, Nb, Cu,
One of Co, V, Mo, Al, C and N element or a variety of, the weight percent content of each element in alloy are as follows: Mn 12 ~ 32%, Si
4 ~ 7%, Cr 0 ~ 14%, Ni 0 ~ 8%, Ti 0 ~ 1%, Nb 0 ~ 2%, Cu 0 ~ 1%, Co 0 ~ 2%, V 0 ~ 2%, Mo 0 ~ 2%, Al 0 ~ 3%,
C 0 ~ 0.2%, N 0 ~ 0.2%, Yu Wei Fe and inevitable impurity.Obviously, manganese is most heavy in Fe-Mn-Si base marmem
One of basic component wanted.It is worth noting that, the vapour pressure of manganese is high, it is caused easily to wave under vacuum environment
Hair.So when carrying out high-temperature process under vacuum conditions, since manganese atom is from a large amount of volatilizations on surface, ferrimanganic silicon-base alloy
The poor manganese layer that surface will form one layer of manganese content and be substantially less than core.And manganese is austenite former, its reduction will lead to
Ferritic formation.And ferrite is ferromagnetism, is magnetic phase.Therefore, the present invention just can be obtained by the method for vacuum heat treatment
Obtaining surface has one layer of ferritic Fe-Mn-Si base marmem, to impart the function of alloy magnetism.
Preparing magnetic Fe-Mn-Si base marmem using vacuum heat treatment, the specific method is as follows: by mentioned component
Fe-Mn-Si base marmem is handled >=30 minutes in the environment of vacuum degree≤1Pa with 1000 DEG C ~ 1300 DEG C, then air-cooled
Or oil cooling or water cooling is to room temperature.When heat treatment temperature is lower than 900 DEG C or less, Fe-Mn-Si base marmem will have the second phase
It is precipitated, destroys the uniformity of tissue.In addition, heat treatment temperature is higher, the vapour pressure of manganese is also higher, is more advantageous to vacuum in this way
It is heat-treated lower volatilization of the manganese from alloy surface, to guarantee the ferritic formation in surface layer.In order to avoid the second phase precipitation and
Be conducive to the volatilization of manganese, heat treatment temperature of the invention is 1000 DEG C ~ 1300 DEG C.The magnetic ferrimanganic silicon substrate shape of above method preparation
There are one layer of ferrite, and weight percent content≤10% of the manganese in this layer of ferrite in the surface of shape memory alloys.Meanwhile magnetic
Average layer thickness >=3 micron of the ferrite lamellae on property Fe-Mn-Si base marmem surface.In order to possess higher magnetic property,
Average thickness >=21 micron of the ferrite lamellae on magnetic Fe-Mn-Si base marmem surface.
In order to obtain best ferrite surface layer and excellent shape memory effect, Fe-Mn-Si base marmem is best
In vacuum degree≤2.0 × 10-1It is handled in the environment of Pa；Time >=2 hour are preferably handled under vacuum conditions；Preferably in vacuum ring
It is handled under border with 1000 DEG C ~ 1250 DEG C, subsequent air-cooled or oil cooling or water cooling to room temperature；With 1250 DEG C preferably under vacuum degree environment
~ 1300 DEG C of processing, are then air-cooled to room temperature.Patent ZL201410102165.X, which is disclosed, is changed into Ovshinsky using high temperature ferrite
The method for training Fe-Mn-Si base marmem is exempted from the solid-state phase changes preparation of body.Therefore, it is imitated to obtain more preferably shape memory
It answers, Fe-Mn-Si base marmem is at 1250 DEG C ~ 1300 DEG C preferably at high temperature ferrite monophase field.
The present invention has the advantage that (1) is not limited by material shape, the Armco magnetic iron of needles of various sizes and shape can be prepared
Manganese silicon substrate marmem.(2) surface ferrite layer is in-situ preparation, therefore very good with basal body binding force, and deformation will not
Lead to falling off for ferrite lamellae.
Detailed description of the invention
It in vacuum degree is 2.3 × 10 that Fig. 1, which is embodiment 13,-2It is air-cooled to after being handled 80 hours in the environment of Pa with 1200 DEG C
The section metallographic microscope of room temperature.Illustrate that Fe-Mn-Si base marmem forms one layer of ferrite on surface after above-mentioned processing
Layer.
It in vacuum degree is 2.3 × 10 that Fig. 2, which is embodiment 13,-2It is air-cooled to after being handled 80 hours in the environment of Pa with 1200 DEG C
The XRD spectrum to surface test of room temperature.Illustrate that Fe-Mn-Si base marmem is formed really by above-mentioned processing rear surface
One layer of ferrite lamellae.
Specific embodiment
The invention will be further described with embodiment with reference to the accompanying drawing.It is worth noting that the embodiment provided is not
It can be interpreted as limiting the scope of the invention, the person skilled in the art in the field is according to the content of aforementioned present invention to this hair
The bright some nonessential modifications and adaptations made still should belong to the scope of the present invention.
Comparative example 1 and embodiment 1 to 21.The weight percent of each element of the Fe-Mn-Si base marmem of selection
Are as follows: Mn 18.61%, Si 5.75%, Cr 9.23%, Ni 4.35%, C 0.01%, Yu Wei Fe and inevitable impurity.Work as temperature
When higher than 1260 DEG C, which is in high temperature ferrite monophase field.Comparative example and embodiment be deformation section be sectional area 2 ×
2mm2Dog bone sample.In order to compare effect of the invention, comparative example 1 is only handled 0.5 hour with 1100 DEG C under protection of argon gas,
Subsequent water cooling is to room temperature.It is 8.0 × 10 that embodiment 1 to 21, which is in vacuum degree,-1~9.3×10-3In the environment of with 1000 DEG C ~
1290 DEG C are handled 0.5 hour ~ 200 hours, subsequent air-cooled or oil cooling or water cooling to room temperature.Comparative example 1 and reality are tested with magnet
Apply whether example 1 to 21 is magnetic, as a result as follows: comparative example 1 cannot be sucked in magnet, show comparative example 1 without magnetism；The equal energy of magnet
Embodiment 1 to 21 is sucked easily, shows that embodiment 1 to 21 is magnetic.Using metallographic and XRD characterization embodiment 13, Fig. 1 is seen
And Fig. 2, the results showed that the one layer of average thickness that truly have on surface of magnetism Fe-Mn-Si base marmem prepared by the present invention be
239 microns of ferrite lamellae exists.Using the shape memory effect of 5% pulling method characterization alloy, steps are as follows: first alloy existing
Then room temperature tensile deformation 5% restores alloy 5 minutes in 600 DEG C of heating, the recovery strain of last test alloy.Table 1
Data clearly illustrate: 1 surface layer of comparative example does not have ferrite lamellae to be formed, and the surface of embodiment 1 to 21 form 3 microns ~
411 microns of ferrite lamellae；For the sample being vacuum-treated at 1000 DEG C ~ 1250 DEG C, ferrite lamellae thickness is bigger, can restore to become
Shape amount is also lower；For the sample being vacuum-treated at 1270 DEG C ~ 1290 DEG C, ferrite lamellae thickness is bigger, recovery strain
Also lower, but it is all remarkably higher than the sample being vacuum-treated at 1000 DEG C ~ 1250 DEG C, this illustrates that high temperature ferrite is changed into Austria
The solid-state phase changes of family name's body significantly improve its recovery strain.
The preparation method and shape-memory properties and surface ferrite layer of 1 comparative example 1 of table and embodiment 1 to 21 are average
Thickness
The preparation method and shape-memory properties and surface ferrite layer of 2 comparative example 2 of table and embodiment 22 to 28 are average
Thickness
Claims (5)
1. a kind of method for preparing magnetic Fe-Mn-Si base marmem, the Fe-Mn-Si base marmem contain Fe,
Mn, Si and C element, and include one of Cr, Ni, Ti, Nb, Cu, Co, V, Mo, Al and N element or a variety of, each member in alloy
The weight percent content of element are as follows: Mn 12 ~ 32%, Si 4 ~ 7%, Cr 0 ~ 14%, Ni 0 ~ 8%, Ti 0 ~ 1%, Nb 0 ~ 2%, Cu 0 ~
1%, Co 0 ~ 2%, V 0 ~ 2%, Mo 0 ~ 2%, Al 0 ~ 3%, C 0.01 ~ 0.2%, N 0 ~ 0.2%, Yu Wei Fe and inevitably it is miscellaneous
Matter, which is characterized in that handle Fe-Mn-Si base marmem with 1000 DEG C ~ 1100 DEG C in the environment of vacuum degree≤1Pa
>=30 minutes, subsequent air-cooled or oil cooling or water cooling to room temperature；The magnetic Fe-Mn-Si base marmem of above method preparation
There is one layer of ferrite on surface.
2. a kind of method for preparing magnetic Fe-Mn-Si base marmem according to claim 1, which is characterized in that will
Fe-Mn-Si base marmem is in vacuum degree≤2.0 × 10-1It is handled in the environment of Pa.
3. a kind of method for preparing magnetic Fe-Mn-Si base marmem according to claim 1, which is characterized in that will
Fe-Mn-Si base marmem handles time >=2 hour under vacuum conditions.
4. a kind of method for preparing magnetic Fe-Mn-Si base marmem according to claim 1, which is characterized in that magnetic
Average thickness >=3 micron of the ferrite lamellae on property Fe-Mn-Si base marmem surface.
5. a kind of method for preparing magnetic Fe-Mn-Si base marmem according to claim 4, which is characterized in that magnetic
Average thickness >=21 micron of the ferrite lamellae on property Fe-Mn-Si base marmem surface.
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109477175B (en) * | 2016-09-06 | 2021-02-12 | 国立大学法人东北大学 | Fe-based shape memory alloy material and method for producing same |
| CN108588368B (en) * | 2018-04-02 | 2019-06-25 | 四川大学 | The method that prediction ferrimanganic silicon-base alloy austenite increases temperature ferrite dual phase area warm area |
| CN109182662B (en) * | 2018-10-15 | 2020-02-07 | 四川大学 | Method for improving recoverable strain of iron-manganese-silicon-based shape memory alloy |
| CN109457091B (en) * | 2018-10-15 | 2020-02-07 | 四川大学 | Method for preparing coarse-grain Fe-Mn-Si-based shape memory alloy |
| CN111041387B (en) * | 2019-12-25 | 2020-10-27 | 南京龙浩新材料科技有限公司 | Multi-element iron-based shape memory alloy and preparation method thereof |
| CN112011745A (en) * | 2020-08-17 | 2020-12-01 | 中南大学 | Fe-Mn-Si-based shape memory alloy powder, preparation method and application thereof, 3D printing method and shape memory alloy |
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| US4929289A (en) * | 1988-04-05 | 1990-05-29 | Nkk Corporation | Iron-based shape-memory alloy excellent in shape-memory property and corrosion resistance |
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| CN101215678A (en) * | 2008-01-17 | 2008-07-09 | 四川大学 | Training-free casting iron-base shape memory alloy containing high temperature ferrite |
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| CN101202144A (en) * | 2007-11-12 | 2008-06-18 | 上海工程技术大学 | Method for preparing Fe-Mn-Si magnetic shape memory alloy film |
| CN101215678A (en) * | 2008-01-17 | 2008-07-09 | 四川大学 | Training-free casting iron-base shape memory alloy containing high temperature ferrite |
| CN102719721A (en) * | 2012-06-19 | 2012-10-10 | 大连大学 | Magnetic shape memory alloy and preparation method thereof |
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| Oxidation behavior of an austenitic stainless FeMnSiCrNi shape memory alloy;Rui Ma;《Corrosion Science》;20130131;第66卷;第269-277页 |
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