CN107345279B - A kind of preparation method of superplasticity Ni-Mn-Ga-Ta high temperature shape memory alloy - Google Patents
A kind of preparation method of superplasticity Ni-Mn-Ga-Ta high temperature shape memory alloy Download PDFInfo
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- CN107345279B CN107345279B CN201710471014.5A CN201710471014A CN107345279B CN 107345279 B CN107345279 B CN 107345279B CN 201710471014 A CN201710471014 A CN 201710471014A CN 107345279 B CN107345279 B CN 107345279B
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- 229910001285 shape-memory alloy Inorganic materials 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 38
- 239000000956 alloy Substances 0.000 claims abstract description 38
- 238000002844 melting Methods 0.000 claims abstract description 32
- 230000008018 melting Effects 0.000 claims abstract description 32
- 238000010791 quenching Methods 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims abstract description 5
- 230000000171 quenching effect Effects 0.000 claims abstract description 5
- 230000006698 induction Effects 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 13
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- 229910052751 metal Inorganic materials 0.000 claims description 9
- 239000002184 metal Substances 0.000 claims description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- 238000005520 cutting process Methods 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 238000003723 Smelting Methods 0.000 claims description 5
- 239000010453 quartz Substances 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- 229910052715 tantalum Inorganic materials 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 4
- 229910052756 noble gas Inorganic materials 0.000 claims description 4
- 229910052748 manganese Inorganic materials 0.000 claims description 3
- 239000005457 ice water Substances 0.000 claims description 2
- 239000012535 impurity Substances 0.000 claims description 2
- 238000005498 polishing Methods 0.000 claims description 2
- 229910052733 gallium Inorganic materials 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 4
- 238000004140 cleaning Methods 0.000 abstract description 3
- 238000013459 approach Methods 0.000 abstract description 2
- 230000007704 transition Effects 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 8
- 238000001938 differential scanning calorimetry curve Methods 0.000 description 7
- 229910000734 martensite Inorganic materials 0.000 description 6
- 229910000807 Ga alloy Inorganic materials 0.000 description 5
- 239000003708 ampul Substances 0.000 description 4
- 238000011161 development Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 238000010257 thawing Methods 0.000 description 4
- 230000009466 transformation Effects 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 230000005611 electricity Effects 0.000 description 3
- 230000005672 electromagnetic field Effects 0.000 description 3
- 230000005291 magnetic effect Effects 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 230000005294 ferromagnetic effect Effects 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 230000003446 memory effect Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 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
- 239000004020 conductor Substances 0.000 description 1
- 238000007796 conventional method Methods 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
- 239000000203 mixture Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000012781 shape memory material Substances 0.000 description 1
- 229910002058 ternary alloy Inorganic materials 0.000 description 1
Classifications
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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
-
- 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
- C22F1/002—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working by rapid cooling or quenching; cooling agents used therefor
-
- 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
-
- 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
Abstract
The present invention relates to a kind of preparation methods of high-temperature shape memory alloy, more particularly to a kind of preparation method of superplasticity Ni-Mn-Ga-Ta high temperature shape memory alloy, this method be according to atomic percent feeding, vacuumize, melting plus Mn elements continue melting, cleaning, keep the temperature, in water of quenching to get to High-temperature Superplasticity Ni53Mn25Ga21Ta1Alloy.Ni prepared by the present invention53Mn25Ga21Ta1Alloy has many advantages, such as that good toughness, intensity are big, phase transition temperature is high, is the application extension new approaches of high temperature high-ductility marmem.
Description
Technical field
The present invention relates to a kind of High-temperature Superplasticity Ni-Mn-Ga-Ta memorial alloy preparation methods.
Background technology
Ni-Mn-Ga marmems are a kind of novel intelligent ferromagnetic shape memory materials, have thermo elastic martensite concurrently
Phase transformation and ferromagnetic transition, not only with conventional shape-memory alloy by the shape memory effect of Temperature Field Control, but also can
Shape memory effect is generated under magnetic fields.The response frequency of its magneto-shape-memory effect is answered close to piezoelectric ceramics, output
Become close to traditional temperature control marmem, is a kind of intellectual material of great future in engineering applications.Because of its unique feature
It is set also to be able to extensive use in terms of driver and sensor.But Ni-Mn-Ga block materials still have that brittleness is big, intensity
The shortcomings of low and restoring force is small, significantly limits engineer application and its development of the material.These become Magnetic driving memory and close
The main bottleneck of gold application and development.Especially Ni-Mn-Ga block magnetic memorial alloys are applied in high-temperature field, it is necessary to
Meet the material and is in martensitic state (120 DEG C of Ms >) at high temperature.
Invention content
Big in order to solve existing Ni-Mn-Ga suitable shape memory alloys brittleness, the low problem of restoring force is mixed into alloy
Miscellaneous rare element Ta, to provide a kind of High-temperature Superplasticity Ni53Mn25Ga21Ta1Memorial alloy preparation method.
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 Ta 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：Ta 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, 10 × 10 are evacuated down to-3-3×10-3Pa is re-filled with noble gas to 1-0.2Pa, starts melting, control
Monitor system is between 350-500Kw.Due to the Principle of Melting of Medium frequency induction itself, the metal liquid after thawing will be in electromagnetism
Stirring is flowed under the action of, is eventually adding Mn after metal liquid Ni, Ga, Ta for being melted are mixed well, after 3-5min
Alloy liquid is poured into mold, sample is obtained, 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-2-10-1Pa
Quartz ampoule in, under conditions of 1000 DEG C keep the temperature 5 hours, then ice water of quenching in；Obtain superplasticity Ni53Mn25Ga21Ta1Shape
Shape memory alloys.
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.
Another object of the present invention is claimed the above method and prepares superplasticity Ni-Mn-Ga-Ta high temperature shape memory alloy, should
Memorial alloy is Ni53Mn25Ga21Ta1。
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.
It is big to solve existing Ni-Mn-Ga suitable shape memory alloys brittleness, the shortcomings of intensity is low and restoring force is small, simultaneously
Ensure that the problem of martensitic transformation temperature of alloy is unlikely to drop too low, inventor select the Doped ions electricity into alloy for the first time
Valence is higher, radius is smaller, with the element T a compared with macroion field strength (for the ratio between ion electricity price and radius).It is prepared by the method for the present invention
The marmem Ni gone out53Mn25Ga21Ta1Ingredient difference with using vacuum non-consumable smelting furnace prepare Ni-Mn-Ga close
Gold has the characteristics that high temperature, high intensity and superplastic, and martensitic traoformation peak temperature is up to 256 DEG C, and fracture strength is up to
6713MPa, breaking strain 21.2%.This never Leader in Ni-Mn-Ga alloys is crossed, and memorial alloy application can be become
With a kind of new material of development.High-temperature shape memory alloy Ni53Mn25Ga21Ta1Development to the application of Material Field and will open up
New approaches are warded off in expansion.
Description of the drawings
Fig. 1 is Ni prepared by the present invention53Mn25Ga21Ta1The DSC curve figure of alloy, wherein curve 1 are Ni53Mn25Ga21Ta1
Alloy heats the DSC curve measured, and curve 2 is Ni53Mn25Ga21Ta1Alloy cools down the DSC curve measured；
Fig. 2 is Ni prepared by the present invention53Mn25Ga21Ta1Alloy At Room Temperature compression stress and strain curve；
Fig. 3 is Ni prepared by the present invention54Mn25Ga21Alloy At Room Temperature compression stress and strain curve.
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-temperature Superplasticity Ni of present embodiment53Mn25Ga21Ta1The preparation method of note memorial alloy carries out as follows
It prepares：53 parts of Ni, 25 parts of Mn, 21 parts of Ga and 0.5 part of rare element Ta is taken to be put into vacuum according to atomic percent
In frequency induction melting furnace, it is sequentially placed raw material in the following order：Rare element Ta is placed first, is subsequently placed with Ni, is finally put
Enter Ga, due to the high volatile of Mn elements, when charging first Mn pieces are placed on it is spare in vacuum intermediate-frequency induction melting furnace feeder,
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 450Kw.Due to the Principle of Melting of Medium frequency induction itself, metal liquid after thawing will be
Stirring is flowed under the action of electromagnetic field.It is eventually adding Mn pieces, 3- after metal liquid Ni, Ga, Ta for being melted are mixed well
5min pours into alloy liquid in bar molds, obtains the bar samples of Φ 12mm × 60mm, waits for that its cooling is taken out.Then it utilizes
Wire cutting is cut, the alloy barred body after cleaning cutting with acetone, and it is 10 to be then placed in vacuum degree-2In the quartz ampoule of Pa
It is kept the temperature in 12 hours, then water of quenching under conditions of 900 DEG C；Obtain High-temperature Superplasticity Ni53Mn25Ga21Ta1Memorial alloy.
Embodiment 2
The High-temperature Superplasticity Ni of present embodiment53Mn25Ga21Ta1The preparation method of note memorial alloy carries out as follows
It prepares：53 parts of Ni, 25 parts of Mn, 21 parts of Ga and 0.5 part of rare element Ta is taken to be put into vacuum according to atomic percent
In frequency induction melting furnace, it is sequentially placed raw material in the following order：Rare element Ta is placed first, is subsequently placed with Ni, is finally put
Enter Ga, Mn pieces are placed on to spare in vacuum intermediate-frequency induction melting furnace feeder, close side fire door.Before melting, using mechanical pump,
Lobe pump is evacuated down to 6.67 × 10-3Pa is re-filled with high pure nitrogen to 0.5Pa.Start melting, control monitor system 450Kw.By
In the Principle of Melting of Medium frequency induction itself, the metal liquid after thawing will flow stirring under the action of electromagnetic field.When being melted
Metal liquid Ni, Ga, Ta of change are eventually adding Mn pieces after being mixed well, and 3-5min pours into alloy liquid in bar molds,
The bar samples of Φ 12mm × 60mm are obtained, wait for that its cooling is taken out.Then it is cut using wire cutting, cutting is cleaned with acetone
Alloy barred body afterwards, it is 10 to be then placed in vacuum degree-2Keep the temperature 12 hours under conditions of 900 DEG C in the quartz ampoule of Pa, then quench into
In water；Obtain High-temperature Superplasticity Ni53Mn25Ga21Ta1Memorial alloy.
Embodiment 3
The High-temperature Superplasticity Ni of present embodiment53Mn25Ga21Ta1The preparation method of note memorial alloy carries out as follows
It prepares：53 parts of Ni, 25 parts of Mn, 21 parts of Ga and 0.5 part of rare element Ta is taken to be put into vacuum according to atomic percent
In frequency induction melting furnace, it is sequentially placed raw material in the following order：Rare element Ta is placed first, is subsequently placed with Ni, is finally put
Enter Ga, Mn pieces are placed on to spare in vacuum intermediate-frequency induction melting furnace feeder, close side fire door.Before melting, using mechanical pump,
Lobe pump is evacuated down to 6.67 × 10-3Pa is re-filled with high-purity argon gas to 0.5Pa.Start melting, controls monitor system 500Kw, electricity
Arc melting 8-12 minutes.Due to the Principle of Melting of Medium frequency induction itself, the metal liquid after thawing will be in the effect of electromagnetic field
Lower flowing stirring.It is eventually adding Mn pieces after metal liquid Ni, Ga, Ta for being melted are mixed well, 3-5min is by aluminium alloy
Body pours into bar molds, obtains the bar samples of Φ 12mm × 60mm, waits for that its cooling is taken out.Then it is cut using wire cutting
It cuts, the alloy barred body after cleaning cutting with acetone, it is 10 to be then placed in vacuum degree-2In the quartz ampoule of Pa under conditions of 900 DEG C
It keeps the temperature in 12 hours, then water of quenching；Obtain High-temperature Superplasticity Ni53Mn25Ga21Ta1Memorial alloy.
High-temperature Superplasticity Ni prepared by embodiment53Mn25Ga21Ta1Memorial alloy is in the item that heating rate is 10K/min
Heating DSC curve is measured under part, measures cooling DSC curve under conditions of cooling rate 10K/min, the results are shown in Figure 1.It is logical
The DSC curve crossed in figure can be seen that in High-temperature Superplasticity Ni manufactured in the present embodiment53Mn25Ga21Ta1Alloy is adding hot and cold
But all illustrate High-temperature Superplasticity Ni only there are one heat absorption and exothermic peak on DSC curve53Mn25Ga21Ta1Alloy has with use
Vacuum non-consumable smelting furnace prepares the same thermoelastic martensitic transformation feature of Ni-Mn-Ga alloy ternary alloy three-partalloys.
Ni prepared by embodiment 153Mn25Ga21Ta1Alloy and Ni54Mn25Ga21Alloy carries out fracture strength and fracture is answered
The test of change, test result is as shown in Figures 2 and 3, Ni prepared by present embodiment53Mn25Ga21Ta1The fracture strength of alloy exists
6713MPa improves about 6000Mpa than existing Ni-Mn-Ga alloys, is equivalent to and improves about 6 times than Ni-Mn-Ga alloy, fracture
Strain improves 400% than the existing breaking strain for preparing Ni-Mn-Ga alloys using vacuum non-consumable smelting furnace.Illustrate this hair
The Ni of bright preparation53Mn25Ga21Ta1Alloy ductility is big.Ni prepared by the present invention53Mn25Ga21Ta1The martensite of alloy starts phase transformation
Temperature is 256 DEG C, with the existing immediate Ni of ingredient prepared using vacuum non-consumable smelting furnace54Mn25Ga21Alloy almost phase
When.
Claims (5)
1. a kind of preparation method of superplasticity Ni-Mn-Ga-Ta high temperature shape memory alloy, 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 Ta 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：Ta is placed first, is subsequently placed with Ni, is finally putting into Ga, and Mn, which is placed on smelting furnace alloy, to be added
Expect spare, close side fire door in device；
(2) before melting, 10 × 10 are evacuated down to-3-3×10-3Pa is re-filled with noble gas to 1-0.2Pa, starts melting, control melting
Power is eventually adding Mn between 350-500Kw after metal liquid Ni, Ga, Ta for being melted are mixed well, and 3-5min will
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-2-10-1The quartz of Pa
Guan Zhong is kept the temperature under conditions of 1000 DEG C in 5 hours, then ice water of quenching；Obtain superplasticity Ni53Mn25Ga21Ta1Shape memory
Alloy.
2. a kind of preparation method of superplasticity Ni-Mn-Ga-Ta high temperature shape memory alloy according to claim 1, feature exist
In noble gas is high-purity argon gas in the step (2).
3. a kind of preparation method of superplasticity Ni-Mn-Ga-Ta high temperature shape memory alloy according to claim 1, feature exist
In using acetone washed samples in the step (3).
4. a kind of preparation method of superplasticity Ni-Mn-Ga-Ta high temperature shape memory alloy according to claim 1, feature exist
In described vacuumize using equipment can be mechanical pump or lobe pump.
5. a kind of method as described in claim 1 prepares superplasticity Ni-Mn-Ga-Ta high temperature shape memory alloy, which is
Ni53Mn25Ga21Ta1。
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| CN108620582B (en) * | 2018-06-05 | 2020-02-14 | 哈尔滨工程大学 | Composite material of magnetic memory alloy and copper and preparation method thereof |
| CN110923510B (en) * | 2019-12-16 | 2021-08-31 | 大连大学 | Preparation method of high preferred orientation NiMnGa magnetic memory alloy wire |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101709409A (en) * | 2009-12-10 | 2010-05-19 | 厦门大学 | Micro-tantalum modified nickel-manganese-cobalt-gallium based high-temperature shape memory alloy |
| CN104947052A (en) * | 2015-07-27 | 2015-09-30 | 大连大学 | Method for preparing Ni52Mn24Ga24 alloy film through laser pulse sputtering deposition |
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2017
- 2017-06-20 CN CN201710471014.5A patent/CN107345279B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101709409A (en) * | 2009-12-10 | 2010-05-19 | 厦门大学 | Micro-tantalum modified nickel-manganese-cobalt-gallium based high-temperature shape memory alloy |
| CN104947052A (en) * | 2015-07-27 | 2015-09-30 | 大连大学 | Method for preparing Ni52Mn24Ga24 alloy film through laser pulse sputtering deposition |
Non-Patent Citations (1)
| Title |
|---|
| Ni-Mn-Ga high-temperature shape memory alloys;H.B.Xu et.al;《Materials Science and Engineering A》;20061231;2.Experimental、图2、图5 * |
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Application publication date: 20171114 Assignee: Dalian wina fluid equipment Co.,Ltd. Assignor: DALIAN University Contract record no.: X2023980049065 Denomination of invention: Preparation method of a superplastic Ni Mn Ga Ta high-temperature memory alloy Granted publication date: 20181102 License type: Common License Record date: 20231130 |
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