CN107099698B - A kind of preparation method of superhigh intensity Ni-Mn-Ga-Hf memorial alloys - Google Patents
A kind of preparation method of superhigh intensity Ni-Mn-Ga-Hf memorial alloys Download PDFInfo
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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 69
- 239000000956 alloy Substances 0.000 title claims abstract description 69
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 230000032683 aging Effects 0.000 claims abstract description 40
- 238000011282 treatment Methods 0.000 claims abstract description 22
- 238000002844 melting Methods 0.000 claims abstract description 21
- 230000008018 melting Effects 0.000 claims abstract description 21
- 238000000265 homogenisation Methods 0.000 claims abstract description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- 230000006698 induction Effects 0.000 claims description 7
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 238000005520 cutting process Methods 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 4
- 239000012535 impurity Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 229910052756 noble gas Inorganic materials 0.000 claims description 4
- 238000005498 polishing Methods 0.000 claims description 4
- 239000010453 quartz Substances 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 239000003708 ampul Substances 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 229910052733 gallium Inorganic materials 0.000 claims description 2
- 229910052748 manganese Inorganic materials 0.000 claims description 2
- 238000012545 processing Methods 0.000 claims description 2
- 238000010791 quenching Methods 0.000 abstract description 3
- 229910001285 shape-memory alloy Inorganic materials 0.000 abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 3
- 230000000171 quenching effect Effects 0.000 abstract description 2
- 238000004140 cleaning Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 11
- 238000001000 micrograph Methods 0.000 description 11
- 229910000807 Ga alloy Inorganic materials 0.000 description 6
- 238000012360 testing method Methods 0.000 description 5
- 230000008859 change Effects 0.000 description 4
- 238000011161 development Methods 0.000 description 4
- 238000005275 alloying Methods 0.000 description 3
- 230000018109 developmental process Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000005291 magnetic effect Effects 0.000 description 3
- 238000003723 Smelting Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 230000005294 ferromagnetic effect Effects 0.000 description 2
- 229910052735 hafnium Inorganic materials 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 229910000734 martensite Inorganic materials 0.000 description 2
- 230000003446 memory effect Effects 0.000 description 2
- 238000004901 spalling Methods 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 229910000952 Be alloy Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000013459 approach 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
- 230000005674 electromagnetic induction Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 230000003694 hair properties Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000004321 preservation 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
- 238000001228 spectrum Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 229910002058 ternary alloy Inorganic materials 0.000 description 1
- 238000010257 thawing Methods 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
-
- 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 preparation method of New Shape Memory Alloys, particularly a kind of preparation method of superhigh intensity Ni Mn Ga Hf memorial alloys.Marmem Ni prepared by the present invention53Mn25Ga21Hf1Application extension for high temperature high-ductility marmem thinking.The Ni of the present invention53Mn25Ga21Hf1It is prepared as follows：According to atomic percent feeding, vacuumize, melting plus Mn elements continue melting, cleaning, keep the temperature, Homogenization Treatments are carried out in water of quenching, by changing aging temp and aging time to get to superhigh intensity Ni53Mn25Ga21Hf1Alloy.Ni prepared by the present invention53Mn25Ga21Hf1Alloy has many advantages, such as that good toughness, intensity are big.
Description
Technical field
The present invention relates to a kind of high intensity Ni-Mn-Ga-Hf 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.For the response frequency of its magneto-shape-memory effect close to piezoelectric ceramics, output should
Become close to traditional temperature control marmem, be a kind of intellectual material of great future in engineering applications.The characteristics of because of its uniqueness
It is made also to be 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, reduces brittleness, 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 Ni-Mn-Ga alloys brittleness, the shortcomings of intensity is low and restoring force is small, we take timeliness
Method increases the intensity of alloy and increases plasticity.It is strong to provide a kind of novel superelevation by changing aging temp and time
The Ni of degree53Mn25Ga21Hf1Memorial 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 Hf is 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：Hf is placed first, is subsequently placed with Ni, is finally putting into Ga, since the height of Mn elements is waved
Mn is placed on spare in material alloying device, close side fire door by hair property, when charging in advance；
(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 the metal liquid being melted is by abundant mixing, by aluminium alloy after 3-5min
Body is poured into bar molds, obtains sample, treats 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 5 hours under conditions of 1000 DEG C and carries out Homogenization Treatments；Then by obtained alloy carry out 500-800 DEG C,
The ageing treatment of 0.5-5h, you can obtain the Ni of superhigh intensity53Mn25Ga21Hf1Alloy.
Further, noble gas is high-purity argon gas in the step (2).
Further, acetone washed samples, then vacuum processing 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 superhigh intensity Ni-Mn-Ga-Hf memorial alloys
Ni53Mn25Ga21Hf1。
Alloying can significantly change alloy transformation temperature and improve its mechanical performance and physical property.Inventor by
In Ni-Mn-Ga ternary alloy three-partalloys with ion electricity price is higher, radius is smaller, have compared with macroion field strength (ion electricity price and radius it
Than) element Hf doping substitute part Ni members usually improve alloy mechanical property do not reduce or slightly reduce alloy martensite phase
Phase transition temperature, to provide a kind of novel high intensity Ni-Mn-Ga-Hf memorial alloys.Since Mn element saturated vapour pressures are higher,
Volatile, in existing preparation method, the volatile quantity of Mn is difficult to control, can not in exact alloy Mn content, inventor uses
Hf is placed first, then puts Ni, is subsequently placed into Ga, is finally putting into the feed way of Mn, and solve that component content accurately controls asks
Topic.
The high intensity Ni that inventor is prepared using vacuum intermediate-frequency induction melting furnace53Mn25Ga21Hf1Alloy, then to it
Carry out ageing treatment, find the fracture strength of alloy and breaking strain presented with the increase of aging temp gradually it is increased become
Gesture, when aging temp is higher than 600 DEG C, fracture strength presentation is quick increases, up to 7734MPa；Breaking strain is first quick to be increased
After be slowly increased, highest breaking strain be 17.8%, this never Leader in NiMnGa alloys is crossed, this can become memory close
Gold application and a kind of new material of development.Therefore shape memory aging alloy Ni53Mn25Ga21Hf1Development will be to material
Using and expand open up new thinking.
Vacuum intermediate-frequency induction melting furnace is that eddy heating for heating is generated in metallic conductor using electromagnetic induction under vacuum
Furnace charge carries out the method for 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.
The shape memory metal shape memorial alloy Ni that the method for the present invention is prepared53Mn25Ga21Hf1Different from using vacuum
Ni-Mn-Ga alloys prepared by non-consumable smelting furnace have many advantages, such as that fracture strength is high, toughness is big, and this method is grasped by comparison
Make alloy property that is simple, preparing to stablize, new approaches have been expanded in the field for high intensity and high-ductility marmem.
Description of the drawings
Fig. 1 is Ni prepared by the present invention53Mn25Ga21Hf1The light micrograph of alloy；Wherein (a) figure is alloy in room
Light micrograph under temperature, light micrograph of (b) figure alloy after 500 DEG C/3h ageing treatments, (c) figure are alloy warps
Light micrograph after 600 DEG C/3h ageing treatments, (d) figure are that optics of the alloy after 700 DEG C/3h ageing treatments is shown
Micro- photo, (e) figure are light micrograph of the alloy after 800 DEG C/3h ageing treatments；
Fig. 2 is Ni prepared by the present invention53Mn25Ga21Hf1The XRD spectrum of alloy；Wherein (a) figure be alloy through 700 DEG C/
Light micrograph after 0.5h ageing treatments, (b) figure are light micrograph of the alloy after 700 DEG C/1h ageing treatments,
(c) figure is light micrograph of the alloy after 700 DEG C/3h ageing treatments, and (d) figure is alloy through 700 DEG C/5h ageing treatments
Light micrograph afterwards；
Fig. 3 is Ni prepared by the present invention53Mn25Ga21Hf1Room temperature pressure of the memorial alloy after 800 DEG C/3h ageing treatments
Stress under compression and strain curve；
Fig. 4 is Ni prepared by the present invention53Mn25Ga21Hf1Memorial alloy alloy after different aging temp ageing treatments
Fracture strength changes；
Fig. 5 is Ni prepared by the present invention53Mn25Ga21Hf1Memorial alloy alloy after different aging temp ageing treatments
Breaking strain changes；
Fig. 6 is Ni53Mn25Ga21Hf1The fracture strength of memorial alloy alloy after 700 DEG C of different time ageing treatments；
Fig. 7 is Ni53Mn25Ga21Hf1The change of memorial alloy breaking strain of alloy after 700 DEG C of different time ageing treatments
Change.
Specific embodiment
The present invention is described in further detail, but does not limit the scope of the invention below by embodiment.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 Ni of the present embodiment53Mn25Ga21Hf1The preparation method of memorial alloy is prepared as follows：It presses
53 parts of Ni, 25 parts of Mn, 21 parts Ga and 1 part of rare element Hf is taken to be put into vacuum intermediate-frequency induction melting furnace according to atomic percent,
It is sequentially placed raw material in the following order：Rare element Hf is placed first, is subsequently placed with Ni pieces, is finally putting into Ga, and when charging is pre-
First Mn is placed on it is spare in material alloying device, after Hf, Ni, Ga melt uniformly after, add Mn.Before melting, using mechanical pump,
Lobe pump is evacuated down to 6.67 × 10-3Pa is re-filled with high-purity argon gas to 0.2Pa.Start melting, control monitor system 500Kw.When
The metal liquid being melted is eventually adding Mn pieces after abundant mixing, and 3-5min pours into alloy liquid in bar molds, obtains
The bar samples of Φ 12mm × 60mm treat that its cooling is taken out.Test material is used through wire cutting and mechanical polishing removal surface impurity
It is 10 that vacuum degree is enclosed after acetone cleaning-1In the quartz ampoule of Pa, under conditions of 1000 DEG C keeping the temperature 5 hours carries out at homogenization
Reason；Obtain Ni53Mn25Ga21Hf1Marmem.
Embodiment 2
The high intensity Ni of the present embodiment53Mn25Ga21Hf1The preparation method of memorial alloy is prepared as follows：It presses
It is carried out according to aging temp and aging time is changed, specific steps are as follows：Aging time fixed first, respectively heats sample
It is strong to get the superelevation handled to different aging times into 500 DEG C, 600 DEG C, 700 DEG C and 800 DEG C heat preservations, 3 hours water of quenching again
Spend Ni53Mn25Ga21Hf1Marmem.
Embodiment 3
Difference lies in 700 DEG C of aging temp changes aging time to the present embodiment under conditions of remaining unchanged with embodiment 1
Respectively 0.5h, 1h, 3h and 5h.It is other same as the specific embodiment one.
Embodiment 4
53 parts of Ni, 25 parts of Mn, 21 parts Ga and 1 part of rare element Hf is taken to be put into vacuum intermediate-frequency sensing according to atomic percent
In smelting furnace, rare element Hf being placed first, is subsequently placed with Ni pieces, is finally putting into Ga, Mn is placed on alloy in advance and added by when charging
It is spare in material device, after Hf, Ni, Ga melt uniformly, add Mn.Before melting, 10 are evacuated down to using mechanical pump, lobe pump
×10-3Pa is re-filled with high-purity argon gas to 0.2Pa.Start melting, control monitor system 350Kw.When the metal liquid quilt being melted
Mn pieces are eventually adding after abundant mixing, 3-5min pours into alloy liquid in bar molds, obtains the rodlike of Φ 12mm × 60mm
Sample treats that its cooling is taken out.Test material encloses vacuum through wire cutting and mechanical polishing removal surface impurity after being cleaned with acetone
Spend is 10-1In the quartz ampoule of Pa, 5 hours are kept the temperature under conditions of 1000 DEG C and carries out Homogenization Treatments；Then the alloy that will be obtained
3h are kept the temperature in 800 DEG C to quench again in water to get to Ni53Mn25Ga21Hf1Marmem.
Superhigh intensity Ni prepared by embodiment 2 and 353Mn25Ga21Hf1Alloy microstructure is analyzed, and Fig. 1 is superhigh intensity
The light micrograph that alloy structure changes with aging temp, the precipitated phase in all alloys is at any time as seen in Figure 1
The increase of effect temperature first increases to be reduced afterwards.
Fig. 2 is the light micrograph that changes with aging time of superstrength alloy tissue, as can be seen from Figure 2 with
It and phase amount increase is precipitated in the increase alloy of aging time.
Superstrength alloy prepared by the present invention carries out the test of fracture strength and breaking strain, test result such as Fig. 3
Shown, prepared by present invention Ni53Mn25Ga21Hf1Fracture strength is in 7734Mpa after 800 DEG C/3h ageing treatments for alloy, than not
Ni through ageing treatment53Mn25Ga21Hf1Fracture strength be about 3300MPa.Ni prepared by the present invention53Mn25Ga21Hf1Alloy breaks
Resistance to spalling increases with the increase of aging time, increases 594834MPa from 4684MPa, is improved about than existing Ni-Mn-Ga alloys
4000-5000Mpa。
By Ni obtained in the present embodiment 2-353Mn25Ga21Hf1Fracture 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 invention53Mn25Ga21Hf1The highest of alloy is broken
Resistance to spalling is 7734MPa, and highest breaking strain is 18%, illustrates Ni prepared by the present invention53Mn25Ga21Hf1Alloy ductility is big.
Ni prepared by the present invention53Mn25Ga21Hf1Alloy fracture intensity increases with the increase of aging temp, increases to from 4376MPa
7734MPa improves about 3500-7000Mpa than existing Ni-Mn-Ga alloys；Increase to 17.8% from 12.8%, than existing Ni-
Mn-Ga alloys improve about 200%-350%；Ni prepared by the present invention53Mn25Ga21Hf1Alloy fracture is strained with aging time
Increase first increases to be reduced afterwards, is increased to 16.7% from 12.8% and is dropped to 14.4, is improved about than existing Ni-Mn-Ga alloys
200%-350%.
Claims (5)
1. a kind of preparation method of superhigh intensity Ni-Mn-Ga-Hf memorial alloys, which is characterized in that include the following steps：
(1) 53 parts of Ni, 25 parts of Mn, 21 parts of Ga and 1 part of Hf is taken to be put into vacuum intermediate-frequency induction melting furnace according to atomic percent, pressed
Raw material is sequentially placed according to following sequence：Hf is placed first, is subsequently placed with Ni, is finally putting into Ga, and Mn is placed on conjunction by when charging in advance
It is spare in golden feeding device, close side fire door；
(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 in 350-500kW；Mn is eventually adding after metal liquid Ga, Hf, the Ni being melted are by abundant mixing, it will after 3-5min
Mixed alloy liquid is poured into bar molds, obtains sample, treats 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, 5 hours are kept the temperature under conditions of 1000 DEG C and carries out Homogenization Treatments；Then obtained alloy is subjected to 500-800 DEG C, 0.5-
The ageing treatment of 5h is up to Ni53Mn25Ga21Hf1Marmem.
2. a kind of preparation method of superhigh intensity Ni-Mn-Ga-Hf memorial alloys 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 superhigh intensity Ni-Mn-Ga-Hf memorial alloys according to claim 1, feature exist
In using acetone washed samples, then vacuum processing in the step (3).
4. a kind of preparation method of superhigh intensity Ni-Mn-Ga-Hf memorial alloys 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 superhigh intensity Ni-Mn-Ga-Hf memorial alloys, which is characterized in that the note
Alloy is recalled for Ni53Mn25Ga21Hf1。
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Application publication date: 20170829 Assignee: ZYBODY CO.,LTD. Assignor: DALIAN University Contract record no.: X2023210000200 Denomination of invention: Preparation method of ultra-high strength Ni Mn Ga Hf memory alloy Granted publication date: 20180622 License type: Common License Record date: 20231127 |
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Application publication date: 20170829 Assignee: Xiaosongxiong lianpute machinery manufacturing (Dalian) Co.,Ltd. Assignor: DALIAN University Contract record no.: X2023210000249 Denomination of invention: Preparation method of ultra-high strength Ni Mn Ga Hf memory alloy Granted publication date: 20180622 License type: Common License Record date: 20231129 Application publication date: 20170829 Assignee: DALIAN MENGYU MACHINERY CO.,LTD. Assignor: DALIAN University Contract record no.: X2023210000220 Denomination of invention: Preparation method of ultra-high strength Ni Mn Ga Hf memory alloy Granted publication date: 20180622 License type: Common License Record date: 20231129 |