CN107299252B - A kind of high intensity, the preparation method of high-ductility Ni-Mn-Ga-Nb memorial alloys - Google Patents
A kind of high intensity, the preparation method of high-ductility Ni-Mn-Ga-Nb memorial alloys Download PDFInfo
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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 60
- 239000000956 alloy Substances 0.000 title claims abstract description 60
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 230000032683 aging Effects 0.000 claims abstract description 37
- 238000011282 treatment Methods 0.000 claims abstract description 21
- 238000002844 melting Methods 0.000 claims abstract description 19
- 230000008018 melting Effects 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 7
- 238000010791 quenching Methods 0.000 claims abstract description 5
- 230000000171 quenching effect Effects 0.000 claims abstract description 5
- 238000000265 homogenisation Methods 0.000 claims abstract description 4
- 230000006698 induction Effects 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 238000005520 cutting process Methods 0.000 claims description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 229910052756 noble gas Inorganic materials 0.000 claims description 4
- 238000003723 Smelting Methods 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 229910052733 gallium Inorganic materials 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- 239000005457 ice water Substances 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 3
- 238000005498 polishing Methods 0.000 claims description 3
- 239000010453 quartz Substances 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 229910052748 manganese Inorganic materials 0.000 claims description 2
- 239000003708 ampul Substances 0.000 claims 1
- 229910052758 niobium Inorganic materials 0.000 claims 1
- -1 special Sign is Substances 0.000 claims 1
- 230000008859 change Effects 0.000 abstract description 7
- 238000013459 approach Methods 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 2
- 238000004140 cleaning Methods 0.000 abstract 1
- 238000001000 micrograph Methods 0.000 description 10
- 239000000463 material Substances 0.000 description 9
- 229910000807 Ga alloy Inorganic materials 0.000 description 4
- 238000011161 development Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 230000018109 developmental process Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000005291 magnetic effect Effects 0.000 description 3
- 230000009471 action Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 230000005294 ferromagnetic effect Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000003446 memory effect Effects 0.000 description 2
- 229910001285 shape-memory alloy Inorganic materials 0.000 description 2
- 229910000952 Be alloy Inorganic materials 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000005672 electromagnetic field Effects 0.000 description 1
- 230000005674 electromagnetic induction Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000003694 hair properties Effects 0.000 description 1
- 229910000734 martensite Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000000879 optical micrograph Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000012781 shape memory material Substances 0.000 description 1
- 238000004901 spalling Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 238000010257 thawing Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
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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
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/023—Alloys based on nickel
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/007—Alloys based on nickel or cobalt with a light metal (alkali metal Li, Na, K, Rb, Cs; earth alkali metal Be, Mg, Ca, Sr, Ba, Al Ga, Ge, Ti) or B, Si, Zr, Hf, Sc, Y, lanthanides, actinides, as the next major constituent
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/006—Resulting in heat recoverable alloys with a memory effect
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/10—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of nickel or cobalt or alloys based thereon
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Abstract
The present invention relates to a kind of high intensity, the preparation method of high-ductility Ni-Mn-Ga-Nb memorial alloys, this method is：According to atomic percent feeding, vacuumize, melting plus Mn elements continue melting, cleaning, keep the temperature, carry out Homogenization Treatments in water of quenching, then change aging temp and aging time to get to timeliness Ni53Mn25Ga21Nb1Alloy.Ni prepared by the present invention53Mn25Ga21Nb1Alloy has many advantages, such as that good toughness, intensity are big.The alloy property that the method for the present invention is easy to operate, prepares is stablized, and new approaches have been expanded in the field for high intensity and high-ductility marmem.
Description
Technical field
The present invention relates to a kind of high intensity, high-ductility Ni-Mn-Ga-Nb memorial alloy preparation methods.
Background technology
Ni-Mn-Ga marmems are a kind of intelligent ferromagnetic shape memory materials, have thermoelastic martensitic transformation concurrently
And ferromagnetic transition, not only with conventional shape-memory alloy by the shape memory effect of Temperature Field Control, but also can be in magnetic
Shape memory effect is generated under field action.The response frequency of its magneto-shape-memory effect connects close to piezoelectric ceramics, output strain
Nearly traditional temperature control marmem, is a kind of intellectual material of great future in engineering applications.Because its unique feature makes it
It is also able to extensive use in terms of driver and sensor.
But Ni-Mn-Ga block materials still have the shortcomings of brittleness is big, intensity is low and restoring force is small, it significantly limits
The engineer application of the material and its development.These become the main bottleneck that magnetic driven memory alloy is applied and developed.So how
The intensity of alloy is improved, brittleness is reduced, improves alloy mechanical performance, obtains big magnetic entropy change and giant magnetoresistance effect, it has also become note
Recall the main direction of studying of Alloyapplication and development.
Invention content
Big in order to solve existing NiMnGa alloys brittleness, the shortcomings of intensity is low and restoring force is small, we take the side of timeliness
Method increases the intensity of alloy and increases plasticity.By changing aging temp and time, to provide a kind of high intensity, high-ductility
Ni53Mn25Ga21Nb1The preparation method of memorial alloy.
The high intensity Ni that inventor is prepared using vacuum intermediate-frequency induction melting furnace53Mn25Ga21Nb1Alloy, then to it
Ageing treatment is carried out, it is found that the fracture strength of alloy and breaking strain present first to increase with the increase of aging temp and reduces afterwards
Trend, when aging temp reaches 700 DEG C, the fracture strength of alloy is up to 3827MPa；It is closed when aging temp reaches 600 DEG C
Gold breaking strain be up to 18.9%, this never Leader in NiMnGa alloys is crossed, this can become memorial alloy apply and
A kind of new material of development.Therefore shape memory aging alloy Ni53Mn25Ga21Nb1Development by opening up to the application sum of material
A new road is warded off in expansion.
The marmem of the present invention is prepared as follows：
(1) 53 parts of Ni, 25 parts of Mn, 21 parts of Ga and 1 part of Nb are taken to be put into vacuum intermediate-frequency induction melting furnace according to atomic percent
In, it is sequentially placed raw material in the following order：Nb is placed first, is subsequently placed with Ni, is finally putting into Ga, since the height of Mn elements is waved
Mn is first placed on spare in vacuum intermediate-frequency induction melting furnace material alloying device, close side fire door by hair property, when charging；
(2) before melting, 6.67 × 10 are evacuated down to-3-10×10-3Pa is re-filled with noble gas to 1-0.2Pa, starts melting,
Control monitor system 350-500Kw.Due to the Principle of Melting of Medium frequency induction itself, the metal liquid after thawing will be in electromagnetic field
Under the action of flow stirring, Mn is eventually adding after the metal liquid being melted is mixed well, by alloy liquid after 3-5min
It pours into mold, obtains sample, wait for that its cooling is taken out；
(3) by sample through wire cutting and mechanical polishing removal surface impurity, it is 10 that vacuum degree is enclosed after cleaning-1The quartz of Pa
Guan Zhong keeps the temperature in 5 hours, then ice water of quenching under conditions of 1000 DEG C and carries out Homogenization Treatments；Followed by wire cutting by sample
Product are cut into pillar and small pieces, in the ageing treatment that 500-800 DEG C carries out 0.5-5h to get to high intensity, high-ductility
Ni53Mn25Ga21Nb1Marmem.
Further, noble gas is high-purity argon gas in the step (2).
Further, acetone washed samples are used in the step (3).
Further, described vacuumize using equipment can be mechanical pump or lobe pump.
Vacuum intermediate-frequency induction melting furnace is that eddy heating for heating is generated in metallic conductor using electromagnetic induction under vacuum
Furnace charge is come the method that carries out melting.Small with melting, pumpdown time and melting cycle are short, controlled convenient for temperature, pressure,
The features such as being easily recycled Volatile Elements and accurate composition control.
Volatile since Mn element saturated vapour pressures are higher, in existing preparation method, the volatile quantity of Mn is not easy to control,
Can not in exact alloy Mn content, inventor using placing Hf first, then puts Ni, is subsequently placed into Ga, be finally putting into Mn's plus
Material mode solves the problems, such as that component content accurately controls.
The marmem Ni that the method for the present invention is prepared53Mn25Ga21Nb1Different from using vacuum non-consumable smelting furnace
The Ni-Mn-Ga alloys of preparation, and have many advantages, such as that fracture strength is high, toughness is big by comparison, after Wetted constructures
Ni53Mn25Ga21Nb1Alloy fracture intensity increases, and breaking strain increases.The alloy property that the method for the present invention is easy to operate, prepares
Stablize, new approaches have been expanded in the field for high intensity and high-ductility marmem.
Description of the drawings
Fig. 1 is the high intensity of the preparation of the embodiment of the present invention 2, high-ductility Ni53Mn25Ga21Nb1The light micrograph of alloy；
Wherein (a) be without ageing treatment after light micrograph, (b) be optical microphotograph of the alloy after 500 DEG C/3h ageing treatments
Photo is (c) light micrograph of the alloy after 600 DEG C/3h ageing treatments, (d) figure be alloy through 700 DEG C/3h timeliness at
Light micrograph after reason, (e) figure is light micrograph of the alloy after 800 DEG C/3h ageing treatments；
Fig. 2 is the high-ductility of the preparation of the embodiment of the present invention 3, high intensity Ni53Mn25Ga21Nb1The light micrograph of alloy,
(a) figure is light micrograph of the alloy after 700 DEG C/0.5h ageing treatments, and (b) figure is alloy through 700 DEG C/1h ageing treatments
Light micrograph afterwards, (c) figure is light micrograph of the alloy after 700 DEG C/3h ageing treatments, and (d) figure is alloy warp
Light micrograph after 700 DEG C/5h ageing treatments；
Fig. 3 is the high intensity of the preparation of the embodiment of the present invention 2, high-ductility Ni53Mn25Ga21Nb1Memorial alloy is through 700 DEG C/3h
Room temperature compression stress after ageing treatment and strain curve；
Fig. 4 is the high intensity of the preparation of the embodiment of the present invention 2, high-ductility Ni53Mn25Ga21Nb1Memorial alloy is through different timeliness
The fracture strength situation of change of alloy after temperature ageing treatment；
Fig. 5 is the high intensity of the preparation of the embodiment of the present invention 2, high-ductility Ni53Mn25Ga21Nb1Memorial alloy is through different timeliness
The breaking strain situation of change of alloy after temperature ageing treatment；
Fig. 6 is 3 superhigh intensity Ni of the embodiment of the present invention53Mn25Ga21Nb1Memorial alloy through 700 DEG C of different time timeliness at
The fracture strength situation of change of alloy after reason；
Fig. 7 is 3 superhigh intensity Ni of the embodiment of the present invention53Mn25Ga21Nb1Memorial alloy through 700 DEG C of different time timeliness at
The breaking strain situation of change of alloy after reason.
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.Vacuum intermediate-frequency induction melting furnace is purchased from Shanghai Twilight electric furnace Co., Ltd.
Embodiment 1
The high intensity of present embodiment, high-ductility Ni53Mn25Ga21Nb1The preparation method of memorial alloy as follows into
It is prepared by row：It takes 53 parts of Ni, 25 parts of Mn, 21 parts of Ga and 1 part of Nb to be put into vacuum intermediate-frequency induction melting furnace according to atomic percent, presses
It is sequentially placed raw material according to following sequence：Rare element Nb is placed first, is subsequently placed with Ni, is finally put Ga, Mn is placed on smelting furnace
In spare, close side fire door.Before melting, 6.67 × 10 are evacuated down to using mechanical pump, lobe pump-3Pa is re-filled with high-purity argon gas
To 0.5Pa.Start melting, control monitor system is between 350-500Kw.After the metal liquid being melted is mixed well most
After Mn is added, 3-5min pours into alloy liquid in bar molds, obtains the bar samples of Φ 12mm × 60mm, waits for that its cooling takes
Go out.For test material through wire cutting and mechanical polishing removal surface impurity, it is 10 that vacuum degree is enclosed after being cleaned with acetone-1The quartz of Pa
Guan Zhong keeps the temperature in 5 hours, then ice water of quenching under conditions of 1000 DEG C and carries out Homogenization Treatments, followed by wire cutting by sample
Product are cut into the small pieces of the pillar and Φ 5mm × 2mm of Φ 5mm × 7.5mm, carried out respectively 500 DEG C/3h, 600 DEG C/3h, 700
DEG C/3h, 800 DEG C/3h and 700 DEG C/0.5h, 700 DEG C/1h, the ageing treatment of 700 DEG C/3h and 700 DEG C/5h to get to it is high-strength
Degree, high-ductility Ni53Mn25Ga21Nb1Marmem.
Embodiment 2
The high intensity of the present embodiment, high-ductility Ni53Mn25Ga21Nb1Difference lies in change memorial alloy with embodiment 1
Aging temp and aging time carry out, and fixed aging time is 3 hours.Specific steps are as follows：Sample is heated to respectively
To get to high intensity, high-ductility Ni in 500 DEG C, 600 DEG C, 700 DEG C and 800 DEG C heat preservations, 3 hours water of quenching again53Mn25Ga21Nb1
Marmem.
Embodiment 3
The present embodiment high intensity, high-ductility Ni53Mn25Ga21Nb1Difference lies in timeliness temperature with embodiment 1 for memorial alloy
It is respectively 0.5h, 1h, 3h and 5h that 700 DEG C of degree changes aging time under conditions of remaining unchanged.
High intensity prepared by the present embodiment 2 and embodiment 3, high-ductility Ni53Mn25Ga21Nb1Alloy microstructure point
Analysis, the precipitated phase in all alloys first increases with the increase of aging temp as seen in Figure 1 is reduced afterwards, in 700 DEG C/3h
The quantity of precipitated phase is most after effect processing.As can be seen from Figure 2 first with phase amount is precipitated in the increase alloy of aging time
It is reduced after increase.
The test of high intensity, high-ductile alloy progress fracture strength and breaking strain prepared by the present embodiment 2, test knot
Fruit is as shown in figure 3, Ni prepared by the present invention53Mn25Ga21Nb1Alloy fracture strength after 700 DEG C/3h ageing treatments exists
3827Mpa, than the Ni without ageing treatment53Mn25Ga21Nb1Fracture strength be about 1600MPa.
By obtained Ni in the present embodiment 2-353Mn25Ga21Nb1Fracture strength and breaking strain with aging temp and
The variation test result of aging time is as shown in Figure 4 and Figure 5；Ni prepared by the present invention53Mn25Ga21Nb1The highest of alloy is broken
Resistance to spalling is 3827MPa, and highest breaking strain is 18.9%, illustrates Ni prepared by the present invention53Mn25Ga21Nb1Alloy ductility
Greatly.
In summary, the Ni that prepared by the present invention53Mn25Ga21Nb1Alloy influenced by aging temp and aging time it is very big,
Ni prepared by the present invention53Mn25Ga21Nb1Alloy fracture intensity first increases with the increase of aging temp to be reduced afterwards, is increased from 2212MPa
It is added to 3827MPa, about 3000Mpa is improved than existing Ni-Mn-Ga alloys；Fracture strength is also first to increase with the increase of aging time
It is reduced after big, increases 3422MPa from 2212MPa, about 2700Mpa is improved than existing Ni-Mn-Ga alloys.Breaking strain is with timeliness
The increase of temperature first increases to be reduced afterwards, increases to 18.9% from 9.4%, and about 150%- is improved than existing Ni-Mn-Ga alloys
300%；Breaking strain first increases with the increase of aging time to be reduced afterwards, increases to 13% from 9.4%, is closed than existing Ni-Mn-Ga
Gold improves 150%-200%.
Claims (5)
1. the preparation method of a kind of high intensity, high-ductility Ni-Mn-Ga-Nb memorial alloys, which is characterized in that include the following steps：
(1) it takes 53 parts of Ni, 25 parts of Mn, 21 parts of Ga and 1 part of Nb to be put into vacuum intermediate-frequency induction melting furnace according to atomic percent, presses
It is sequentially placed raw material according to following sequence：Nb is placed first, is subsequently placed with Ni, is finally putting into Ga, and Mn, which is temporarily placed in smelting furnace, to be closed
It is spare in golden feeding device；
(2) before melting, 6.67 × 10 are evacuated down to-3-10×10-3Pa is re-filled with noble gas to 1-0.2Pa, starts melting, control is molten
Downlink power 350-500Kw, is eventually adding Mn after metal liquid Ni, Ga, Nb for being melted are mixed well, and 3-5min is by alloy
Liquid pours into mold, obtains sample, waits for that its cooling is taken out；
(3) by sample through wire cutting and mechanical polishing removal surface impurity, it is 10 that vacuum degree is enclosed after cleaning-1The quartz ampoule of Pa
In, it is kept the temperature in 5 hours, then ice water of quenching under conditions of 1000 DEG C and carries out Homogenization Treatments；Followed by wire cutting by sample
It is cut into pillar and small pieces, in the ageing treatment that 500-800 DEG C carries out 0.5-5h to get to high intensity, high-ductility
Ni53Mn25Ga21Nb1Marmem.
2. the preparation method of a kind of high intensity according to claim 1, high-ductility Ni-Mn-Ga-Nb memorial alloys, special
Sign is that noble gas is high-purity argon gas in the step (2).
3. the preparation method of a kind of high intensity according to claim 1, high-ductility Ni-Mn-Ga-Nb memorial alloys, special
Sign is, acetone washed samples are used in the step (3).
4. the preparation method of a kind of high intensity according to claim 1, high-ductility Ni-Mn-Ga-Nb memorial alloys, special
Sign is that described vacuumize using equipment can be mechanical pump or lobe pump.
5. a kind of method as described in claim 1 prepares high intensity, high-ductility Ni-Mn-Ga-Nb memorial alloys, which is characterized in that
The memorial alloy is Ni53Mn25Ga21Nb1。
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| Title |
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| Microstucture，phase transformation and mechanical property of Nb-doped Ni-Mn-Ga alloys;B.Tian et al.;《Intermetallics》;20151231;摘要 * |
| 时效Ni-Mn-Ga-Ti合金的相变和力学行为;董桂馥;《中国博士学位论文全文数据库工程I辑》;20100215;第3页倒数第1段，第19页第1段 * |
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Application publication date: 20171027 Assignee: ZYBODY CO.,LTD. Assignor: DALIAN University Contract record no.: X2023210000200 Denomination of invention: A Preparation Method of High Strength and High Plasticity Ni Mn Ga Nb Memory Alloy Granted publication date: 20181102 License type: Common License Record date: 20231127 |
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Application publication date: 20171027 Assignee: Dalian Funuo Machinery Co.,Ltd. Assignor: DALIAN University Contract record no.: X2023210000252 Denomination of invention: A Preparation Method of High Strength and High Plasticity Ni Mn Ga Nb Memory Alloy Granted publication date: 20181102 License type: Common License Record date: 20231129 Application publication date: 20171027 Assignee: Dalian Sanfengsheng Heavy Industry Machinery Co.,Ltd. Assignor: DALIAN University Contract record no.: X2023210000251 Denomination of invention: A Preparation Method of High Strength and High Plasticity Ni Mn Ga Nb Memory Alloy Granted publication date: 20181102 License type: Common License Record date: 20231129 Application publication date: 20171027 Assignee: DALIAN MENGYU MACHINERY CO.,LTD. Assignor: DALIAN University Contract record no.: X2023210000220 Denomination of invention: A Preparation Method of High Strength and High Plasticity Ni Mn Ga Nb Memory Alloy Granted publication date: 20181102 License type: Common License Record date: 20231129 |