CN114574730B - Large intrinsic internal consumption nickel-manganese-gallium alloy and preparation method thereof - Google Patents

Large intrinsic internal consumption nickel-manganese-gallium alloy and preparation method thereof Download PDF

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CN114574730B
CN114574730B CN202210207137.9A CN202210207137A CN114574730B CN 114574730 B CN114574730 B CN 114574730B CN 202210207137 A CN202210207137 A CN 202210207137A CN 114574730 B CN114574730 B CN 114574730B
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manganese
nickel
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CN114574730A (en
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宁睿
赵云东
孙思博
高智勇
蔡伟
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Harbin Institute of Technology
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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
    • 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
    • C22C19/005—Alloys based on nickel or cobalt with Manganese as the next major constituent
    • 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
    • C22F1/10—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
    • 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
    • C22F3/00—Changing the physical structure of non-ferrous metals or alloys by special physical methods, e.g. treatment with neutrons
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Abstract

The invention belongs to the technical field of alloys, and particularly relates to a high intrinsic internal consumption nickel-manganese-gallium alloy and a preparation method thereof. The invention provides a preparation method of a large intrinsic internal consumption nickel-manganese-gallium alloy, which comprises the following steps: providing an ingot of nickel-manganese-gallium alloy; and sequentially carrying out solid solution treatment and electron irradiation treatment on the cast ingot to obtain the large intrinsic internal consumption nickel-manganese-gallium alloy. The electron irradiation treatment can introduce a large amount of defects such as vacancies, dislocation and the like into the alloy, the twin crystal interface can be subjected to the pinning effect of the irradiation defects in the movement process, and the defects are gradually increased along with the increase of the electron irradiation dose, so that the friction energy of the martensite variant and the twin crystal interface is obviously improved, more energy can be consumed, the internal consumption of the alloy is increased, and the intrinsic internal consumption value of the alloy is improved. The test result of the embodiment shows that the damping value of the large intrinsic internal consumption nickel-manganese-gallium alloy obtained by the preparation method provided by the invention is 0.044-0.095.

Description

Large intrinsic internal consumption nickel-manganese-gallium alloy and preparation method thereof
Technical Field
The invention belongs to the technical field of alloys, and particularly relates to a high intrinsic internal consumption nickel-manganese-gallium alloy and a preparation method thereof.
Background
Damping is a physical property of an alloy material that dissipates kinetic energy into thermal energy when excited vibration. Reducing vibration and noise can extend the useful life of high precision instruments when operating in a spatial environment, thus requiring the device to maintain high and stable damping over a range of temperatures. The memory alloy contains a large number of twin crystal interfaces, the movement of the twin crystal interfaces can generate a high damping value, and meanwhile, the phase interface motion in the martensite phase transformation process can also bring energy dissipation.
The damping internal loss of the memory alloy is mainly positioned in two temperature intervals, one is a martensite phase transformation temperature interval, and the internal loss mainly consists of phase transformation internal loss and comes from the transition of a phase interface in the phase transformation process; the other temperature interval is below the martensite phase transformation finishing temperature, and the alloy is in a martensite state, and the internal friction mainly consists of intrinsic internal friction and is derived from the movement of a martensite twin crystal interface. The internal loss of phase transformation is related to a phase transformation mechanism, is only generated in the temperature range of martensite phase transformation, has a small application temperature range, and the intrinsic internal loss is unrelated to the temperature rise and reduction rate and can stably exist in the martensite state, so that the damping performance of the alloy in the martensite state does not need to be changed in temperature, has a wider application temperature range and stable damping performance, and has wider application value.
Intrinsic internal loss mainly depends on the structural characteristics of a microstructure, and the movement of a martensite twin crystal interface can be regulated and controlled by methods of doping, introducing defects and the like. The existing common method for improving the damping characteristic of the alloy is to increase the number of martensite twin crystal interfaces in the alloy, while the method for increasing the twin crystal interfaces is usually through a heat treatment method and mechanical training, but the methods cannot obtain larger intrinsic internal consumption in a brittle material, such as nickel manganese gallium alloy with large intrinsic internal consumption.
Disclosure of Invention
In view of the above, the present invention aims to provide a nickel-manganese-gallium alloy with large intrinsic internal consumption and a preparation method thereof.
In order to achieve the purpose of the invention, the invention provides the following technical scheme:
the invention provides a preparation method of a large intrinsic internal consumption nickel-manganese-gallium alloy, which comprises the following steps:
providing an ingot of nickel-manganese-gallium alloy;
and sequentially carrying out solid solution treatment and electron irradiation treatment on the cast ingot to obtain the large intrinsic internal loss nickel-manganese-gallium alloy.
Preferably, the conditions of the electron irradiation treatment include: the irradiation dose is 1 × 10 17 ～4×10 17 e/cm 2 Dose rate of 1X 10 10 ～1×10 12 e/cm 2 ·S -1 。
Preferably, the energy loss of electrons in the electron irradiation treatment is more than or equal to 95 percent.
Preferably, the temperature of the electron irradiation treatment is 20 to 50 ℃.
Preferably, the nickel manganese gallium alloy comprises one or more of Ni50Mn25Ga25, ni54Mn25Ga21 and Ni50Mn28Ga 22.
Preferably, the temperature of the solution treatment is 850-950 ℃, and the holding time is 12-36 h.
Preferably, ice water quenching is further performed after the solution treatment and before the electron irradiation treatment.
The invention also provides the large intrinsic internal consumption nickel-manganese-gallium alloy obtained by the preparation method in the technical scheme, and the damping value of the large intrinsic internal consumption nickel-manganese-gallium alloy is 0.044-0.095.
The invention provides a preparation method of a large intrinsic internal consumption nickel-manganese-gallium alloy, which comprises the following steps: providing an ingot of nickel-manganese-gallium alloy; and sequentially carrying out solid solution treatment and electron irradiation treatment on the cast ingot to obtain the large intrinsic internal consumption nickel-manganese-gallium alloy. In the invention, a large amount of defects such as vacancies, dislocations and the like are introduced into the alloy in the electron irradiation treatment, the martensite twin crystal interface can be subjected to the pinning effect of irradiation defects in the movement process, and the defects are gradually increased along with the increase of the electron irradiation dose, so that the friction energy of the martensite variant and the twin crystal interface is obviously improved, more energy can be consumed, the internal consumption of the alloy is increased, and the intrinsic internal consumption value of the alloy is improved.
The test result of the embodiment shows that the damping value of the large intrinsic internal consumption nickel-manganese-gallium alloy obtained by the preparation method provided by the invention is 0.044-0.095.
Drawings
FIG. 1 is a diagram showing the movement locus and energy distribution of electrons of different energies in NiMnGa alloy in examples 1-3;
FIG. 2 is an XRD pattern of a nickel-manganese-gallium alloy obtained in example 3 and comparative examples 1 and 2;
FIG. 3 is a graph showing the damping curves with temperature of the Ni-Mn-Ga alloys obtained in example 3 and comparative examples 1 to 2.
Detailed Description
The invention provides a preparation method of a large intrinsic internal consumption nickel-manganese-gallium alloy, which comprises the following steps:
providing an ingot of nickel-manganese-gallium alloy;
and sequentially carrying out solid solution treatment and electron irradiation treatment on the cast ingot to obtain the large intrinsic internal consumption nickel-manganese-gallium alloy.
The invention provides an ingot of nickel-manganese-gallium alloy.
In the present invention, the method for preparing the nickel-manganese-gallium alloy ingot preferably comprises the following steps: mixing pure nickel, pure manganese and pure gallium raw materials according to the chemical composition of the nickel-manganese-gallium alloy, smelting, and casting the obtained molten metal to obtain the cast ingot.
In the present invention, the purity of the pure nickel, pure manganese and pure gallium is preferably independently more than or equal to 99.99wt.%.
In the present invention, the nickel manganese gallium alloy preferably includes one or more of Ni50Mn29Ga21, ni50Mn25Ga25, ni54Mn25Ga21 and Ni50Mn28Ga 22.
In the present invention, the melting method is preferably vacuum induction melting. In the present invention, the melting apparatus is preferably a water-cooled copper crucible.
In the present invention, the temperature of the melting is preferably 1300 to 1450 ℃, more preferably 1350 to 1450 ℃.
The casting is not particularly limited in the present invention, and casting known to those skilled in the art may be employed.
After obtaining the cast ingot, the invention carries out solid solution treatment and electron irradiation treatment on the cast ingot in sequence to obtain the large intrinsic internal consumption nickel-manganese-gallium alloy.
In the present invention, the temperature of the solution treatment is preferably 850 to 950 ℃, more preferably 870 to 930 ℃, and most preferably 900 ℃; the holding time is preferably 12 to 36 hours, more preferably 18 to 30 hours, and most preferably 24 hours. In the present invention, the solution treatment is preferably: and placing the cast ingot in a quartz tube, vacuumizing, sealing, and carrying out solution treatment and heat preservation. In the present invention, the degree of vacuum in the evacuated quartz tube is preferably 10 -4 ～10 -3 Pa。
In the present invention, the irradiation dose in the electron irradiation treatment is preferably 1 × 10 17 ～4×10 17 e/cm 2 More preferably 1.5X 10 17 ～3.5×10 17 e/cm 2 (ii) a The dose rate is preferably 1X 10 10 ～1×10 12 e/cm 2 ·S -1 More preferably 1X 10 11 ～1×10 12 e/cm 2 ·S -1 。
In the present invention, the energy loss of electrons in the electron irradiation treatment is preferably not less than 95%.
In the present invention, when the thickness of the ingot is 6cm, the irradiation energy in the electron irradiation treatment is preferably 0.6MeV to 1.2MeV.
In the present invention, the temperature of the electron irradiation treatment is preferably 20 to 50 ℃, more preferably 25 to 45 ℃. In the present invention, the method of maintaining the temperature of the electron irradiation treatment is preferably: and (3) placing the alloy ingot subjected to the solution treatment on a copper plate, introducing cooling water below the copper plate, and maintaining the temperature of the alloy ingot in the electron irradiation treatment through heat transfer.
In the present invention, the apparatus for electron irradiation treatment is preferably an electron accelerator.
After the solution treatment and before the electron irradiation treatment, the invention preferably further comprises the step of performing ice water quenching on the alloy ingot after the solution treatment. The present invention is not particularly limited to the ice water quenching, and the ice water quenching known to those skilled in the art may be used.
After the ice is quenched, the present invention preferably further comprises: and (3) carrying out surface oxide scale removal treatment on the ice water quenched alloy ingot obtained by ice water quenching. In the present invention, the method of the surface descaling treatment preferably includes mechanical grinding. The mechanical polishing is not particularly limited in the present invention, and may be performed by mechanical polishing known to those skilled in the art.
In the present invention, the irradiation energy of the electron irradiation treatment is related to the thickness of the alloy ingot subjected to the electron irradiation treatment. In order to ensure that the energy loss of electrons in the electron irradiation treatment is not less than 95%, when the thickness of the alloy ingot is too large and the irradiation energy in the electron irradiation treatment is not enough to ensure that the energy loss of the electrons is not less than 95%, the method preferably further comprises the steps of cutting the ice water quenched alloy ingot and then removing surface oxide skin; the cutting is subject to guarantee that the energy loss of electrons in the electron irradiation treatment is more than or equal to 95 percent. In the present invention, the cutting device is preferably a wire electric discharge machine.
The invention also provides the large intrinsic internal consumption Ni-Mn-Ga alloy obtained by the preparation method of the technical scheme, and the damping value of the large intrinsic internal consumption Ni-Mn-Ga alloy is 0.044-0.095.
In order to further illustrate the present invention, the following examples are provided to describe the large intrinsic internal consumption nickel-manganese-gallium alloy and the preparation method thereof in detail, but they should not be construed as limiting the scope of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
According to the element proportion of the Ni50Mn29Ga21 alloy, mixing pure nickel, pure manganese and pure gallium raw materials, smelting at 1450 ℃, and casting the obtained molten metal to obtain an ingot;
placing the cast ingot in a quartz tube, and vacuumizing until the vacuum degree is 10 -4 Pa, then preserving heat at 900 ℃ for 24 hours for solution treatment, taking out the alloy ingot after solution treatment, quenching with ice water, obtaining an alloy ingot with the thickness of 6cm by utilizing a wire-electrode cutting machine, mechanically polishing to remove surface oxide skin, placing the obtained ice water quenched alloy ingot on a copper plate, introducing cooling water below the copper plate to keep the thickness of the ice water quenched alloy ingot at 25 ℃, and performing electron irradiation treatment by utilizing an electron accelerator, wherein the irradiation energy in the electron irradiation treatment is 0.6MeV, and the irradiation dose is 2 multiplied by 10 17 e/cm 2 Dose rate of 1X 10 12 e/cm 2 ·S -1 And obtaining the large intrinsic internal loss Ni-Mn-Ga alloy with the damping value of 0.054.
Example 2
According to the element proportion of the Ni50Mn29Ga21 alloy, mixing pure nickel, pure manganese and pure gallium raw materials, smelting at 1450 ℃, and casting the obtained molten metal to obtain an ingot;
placing the cast ingot in a quartz tube, and vacuumizing until the vacuum degree is 10 -4 Pa, then preserving heat at 900 ℃ for 24 hours for solution treatment, taking out the alloy ingot after solution treatment, quenching with ice water, obtaining an alloy ingot with the thickness of 6cm by utilizing a wire-electrode cutting machine, mechanically polishing to remove surface oxide skin, placing the obtained ice water quenched alloy ingot on a copper plate, introducing cooling water below the copper plate to keep the thickness of the ice water quenched alloy ingot at 25 ℃, and performing electron irradiation treatment by utilizing an electron accelerator, wherein the irradiation energy in the electron irradiation treatment is 0.8MeV, and the irradiation dose is 2 multiplied by 10 17 e/cm 2 Dose rate of 1X 10 12 e/cm 2 ·S -1 And obtaining the large intrinsic internal consumption nickel-manganese-gallium alloy with the damping value of 0.044.
Example 3
According to the element proportion of the Ni50Mn29Ga21 alloy, mixing pure nickel, pure manganese and pure gallium raw materials, smelting at 1450 ℃, and casting the obtained molten metal to obtain a cast ingot;
placing the cast ingot in a quartz tube, and vacuumizing until the vacuum degree is 10 -4 Pa, then preserving heat at 900 ℃ for 24 hours for solution treatment, taking out the alloy ingot after solution treatment, quenching with ice water, obtaining an alloy ingot with the thickness of 6cm by utilizing a wire-electrode cutting machine, mechanically polishing to remove surface oxide skin, placing the obtained ice water quenched alloy ingot on a copper plate, introducing cooling water below the copper plate to keep the thickness of the ice water quenched alloy ingot at 25 ℃, and performing electron irradiation treatment by utilizing an electron accelerator, wherein the irradiation energy in the electron irradiation treatment is 1.2MeV, and the irradiation dose is 2 multiplied by 10 17 e/cm 2 Dose rate of 1X 10 12 e/cm 2 ·S -1 And obtaining the large intrinsic internal loss Ni-Mn-Ga alloy with the damping value of 0.095.
Comparative example 1
According to the element proportion of the Ni50Mn29Ga21 alloy, mixing pure nickel, pure manganese and pure gallium raw materials, smelting at 1450 ℃, and casting the obtained molten metal to obtain a cast ingot;
placing the cast ingot in a quartz tube, and vacuumizing until the vacuum degree is 10 -4 Pa, then preserving heat at 900 ℃ for 24h for solution treatment, taking out the alloy ingot after solution treatment, quenching with ice water, and obtaining the thickness by utilizing a wire-electrode spark cutting machineMechanically polishing 6cm alloy ingot to remove surface oxide skin, placing the obtained ice water quenched alloy ingot on a copper plate, introducing cooling water under the copper plate to maintain the ice water quenched alloy ingot at 25 deg.C, and performing electron irradiation treatment with an electron accelerator, wherein the irradiation energy is 1.2MeV and the irradiation dose is 1 × 10 17 e/cm 2 Dose rate of 1X 10 12 e/cm 2 ·S -1 And obtaining the large intrinsic internal consumption nickel-manganese-gallium alloy with the damping value of 0.058.
Comparative example 2
According to the element proportion of the Ni50Mn29Ga21 alloy, mixing pure nickel, pure manganese and pure gallium raw materials, smelting at 1450 ℃, and casting the obtained molten metal to obtain a cast ingot;
placing the cast ingot in a quartz tube, and vacuumizing until the vacuum degree is 10 -4 Pa, then preserving heat at 900 ℃ for 24 hours for solution treatment, taking out the alloy ingot after solution treatment, quenching with ice water, obtaining an alloy ingot with the thickness of 6cm by utilizing a wire-electrode cutting machine, mechanically polishing to remove surface oxide skin, placing the obtained ice water quenched alloy ingot on a copper plate, introducing cooling water below the copper plate to keep the thickness of the ice water quenched alloy ingot at 25 ℃, and performing electron irradiation treatment by utilizing an electron accelerator, wherein the irradiation energy in the electron irradiation treatment is 1.2MeV, and the irradiation dose is 3 multiplied by 10 17 e/cm 2 Dose rate of 1X 10 12 e/cm 2 ·S -1 And obtaining the large intrinsic internal consumption nickel-manganese-gallium alloy with the damping value of 0.081.
The motion locus and energy distribution of electrons with different energies in the nickel-manganese-gallium alloy of the embodiments 1 to 3 are simulated by using the CASSINO software, and the simulation chart is shown in FIG. 1, wherein in FIG. 1, the first column is embodiment 1, the second column is embodiment 2, and the third column is embodiment 3. As can be seen from fig. 1, electrons collide with lattice atoms on the alloy surface, the movement locus of the electrons is changed, the lattice atoms deviate from the initial position, and point defects such as vacancies and interstitial atoms are generated.
The nickel manganese gallium alloys obtained in example 3 and comparative examples 1 and 2 were subjected to X-ray diffraction measurement, and the XRD patterns obtained are shown in FIG. 2. As can be seen from FIG. 2, the Ni-Mn-Ga alloy is in a martensite phase at room temperature, and the main peak of the martensite gradually moves towards a large angle direction with the increase of the electron irradiation dose, which shows that the defect introduced by the electron irradiation reduces the mirror surface distance, and the introduced defect is more with the increase of the irradiation dose.
The damping characteristics of the nickel-manganese-gallium alloy before and after the electron irradiation treatment in the example 3 and the comparative examples 1 to 2 are measured by using a single-arm beam mode of a dynamic mechanical thermal analyzer, and the test method comprises the following steps: the nickel-manganese-gallium alloy sample has the dimensions of 1mm multiplied by 25mm, the vibration frequency is 1Hz, the vibration amplitude is 15 mu m, the measurement temperature range is-75-150 ℃, and the temperature change rate is 5K/min; the test results are shown in FIG. 3. As can be seen from FIG. 3, the damping values of the Ni-Mn-Ga alloy obtained in example 3 in the martensitic state were 2X 10 from 0.055 in the non-irradiated state 17 e/cm 2 After the irradiation dose is irradiated, the increase is increased to 0.095, the improvement is very obvious, and the irradiation dose can exist stably in a wider range.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (5)

1. The preparation method of the large intrinsic internal consumption nickel-manganese-gallium alloy is characterized by comprising the following steps of:
providing an ingot of nickel-manganese-gallium alloy;
sequentially carrying out solid solution treatment and electron irradiation treatment on the cast ingot to obtain the large intrinsic internal loss nickel-manganese-gallium alloy; the damping value of the large intrinsic internal loss nickel-manganese-gallium alloy is 0.095;
the nickel-manganese-gallium alloy is Ni50Mn29Ga21;
the conditions of the electron irradiation treatment are as follows: the irradiation dose is 2X 10 17 e/cm 2 Dose rate of 1X 10 12 e/cm 2 ·S -1 ；
The irradiation energy in the electron irradiation treatment is 1.2MeV;
the temperature of the electron irradiation treatment is 20-50 ℃.
2. The method according to claim 1, wherein the energy loss of electrons in the electron irradiation treatment is 95% or more.
3. The preparation method according to claim 1, wherein the temperature of the solution treatment is 850-950 ℃ and the holding time is 12-36 h.
4. The method according to claim 1, further comprising performing ice water quenching after the solution treatment and before the electron irradiation treatment.
5. The large intrinsic internal consumption Ni-Mn-Ga alloy obtained by the preparation method of any one of claims 1 to 4, wherein the damping value of the large intrinsic internal consumption Ni-Mn-Ga alloy is 0.095.
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