CN109022864B - Method for synthesizing NiMnGaCo magnetic memory alloy at high temperature through combustion reaction - Google Patents
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- 229910001285 shape-memory alloy Inorganic materials 0.000 title claims abstract description 30
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- 238000002485 combustion reaction Methods 0.000 title claims abstract description 9
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 7
- 239000000463 material Substances 0.000 claims abstract description 10
- 238000005245 sintering Methods 0.000 claims abstract description 10
- 239000000843 powder Substances 0.000 claims description 46
- 238000003825 pressing Methods 0.000 claims description 9
- 238000012360 testing method Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 abstract description 6
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- 229910045601 alloy Inorganic materials 0.000 description 34
- 239000000956 alloy Substances 0.000 description 34
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- 229910052751 metal Inorganic materials 0.000 description 8
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- 229910000807 Ga alloy Inorganic materials 0.000 description 7
- 238000011160 research Methods 0.000 description 7
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- 229910000734 martensite Inorganic materials 0.000 description 4
- 229910052733 gallium Inorganic materials 0.000 description 3
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- 230000007704 transition Effects 0.000 description 2
- 229910003310 Ni-Al Inorganic materials 0.000 description 1
- 229910018102 Ni-Mn-Al Inorganic materials 0.000 description 1
- 229910018548 Ni—Mn—Al Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
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Abstract
A method for synthesizing NiMnGaCo magnetic memory alloy at high temperature through combustion reaction relates to a preparation method of magnetic shape memory alloy. The invention synthesizes a novel magnetic shape NiMnGaCo memory alloy by adopting combustion reaction for the first time, and develops the idea for the application of the high-temperature high-plasticity shape memory alloy. The high-strength and high-plasticity NiMnGaCo disclosed by the invention is prepared by the following steps: taking materials according to atomic percentage, mixing evenly and sintering to obtain the NiMnGaCo with high strength, high strength and high plasticity. The magnetic shape memory alloy NiMnGaCo prepared by the invention has the advantages of good toughness, large strength, fine structure and the like.
Description
Technical Field
The invention relates to a method for synthesizing NiMnGaCo magnetic memory alloy at high temperature through combustion reaction.
Background
Magnetic-driven shape memory alloys have both the advantages of high response frequency and large output strain, and have been receiving great attention in recent years. Magnetically driven shape memory effects are currently found in many alloys, mainly including: Ni-Mn-Ga, Ni-Fe-Ga, Fe-Pd, Fe-Pt, Ni-Mn-Al, Co-Ni-Ga, Co-Ni-Al, and Ni-Mn-X (X ═ In, Sn, Sb) alloys, and the like. Among them, Ni-Mn-Ga is the first to be found and is also the most potential magnetic drive shape memory alloy.
In 1996, Ullakko et al first in Ni2The achievement of a reversible strain of about 0.2% in MnGa single crystals has since pulled the research screen for magnetically driven memory alloys and has become a research hotspot in the field of shape memory alloys. Researchers at home and abroad successively develop the research on the magnetic drive memory alloy, and make great progress in the aspects of alloy design and preparation, martensite phase transformation, mechanical behavior, magnetic characteristics, magnetic induced strain, microscopic mechanism and the like. Free sample (without applied stress or pre-stress) Ni where the physical location of the Chinese academy of sciences is52Mn24Ga24Up to 1.2% of the magnetic induction strain induced solely by the magnetic field is obtained. In 2000, Murray et al in Ni47.4Mn32.1Ga20.5A magnetically induced strain of 5.7% was obtained in the single-variant 5M martensite. In 2002, Sozinov et al reported that Ni has a 7M martensitic structure48.8Mn29.7Ga21.5In single crystals, up to 9.5% magnetically induced strain was obtained under 1T magnetic field, which is the largest magnetically induced strain currently found. However, since the segregation of components is caused by the segregation effect in the production of Ni-Mn-Ga single-crystal materials, it is difficult to obtain single-crystal materials having a large size and a uniform compositionCrystal material, poor quality repeatability and stability and high cost. For this reason, research is being focused on polycrystalline Ni-Mn-Ga alloys. Ullakko et al in Ni49.6Mn28.4Ga22The polycrystalline alloy obtains 0.3% of magnetic induced strain, and obtains preferentially oriented martensite by a thermo-mechanical training method, so that the magnetic induced strain is increased to 4%. Researches show that Ni-Mn-Ga alloy has larger brittleness, and the polycrystal of the Ni-Mn-Ga alloy is more brittle than single crystal, and various toughening methods are adopted, wherein the toughening methods comprise adding Fe and rare earth elements, refining crystal grains by powder metallurgy and the like, so that the brittleness of the Ni-Mn-Ga polycrystal is improved. Wang et al prepared Ni by spark plasma sintering under conditions of 80MPa of working pressure, 1173K of sintering temperature and 600s of sintering time2The MnGa alloy has a compressive fracture strain of 24 percent which is far higher than that of the alloy with the same component prepared by a fusion casting method (nearly 8 percent).
In conclusion, over 20 years of effort, the research driving memory alloys, particularly Ni-Mn-Ga alloys, has made great progress, but still has a critical problem of polycrystalline brittleness, which restricts the development and application thereof. Therefore, the exploration of improving the polycrystalline brittleness of the Ni-Mn-Ga alloy is one of the important development directions and research focuses in the field of the magnetic drive memory alloy.
The Ni-Mn-Ga alloy has large brittleness and poor mechanical processing performance, and is typically fractured along the crystal after being fractured under the action of stress. The current relatively consistent view on intrinsic brittleness is as follows: the grain boundary bonding force is low due to the heterogeneous environment formed near the grain boundary due to the difference of atomic size, valence and other electrochemical properties of the constituent alloys. Meanwhile, the ordered intermetallic compound has higher ordered energy, and the atoms of the grain boundary move less, so that the atoms at the grain boundary can be regarded as the atomic arrangement on one side of the grain boundary or belong to the atomic arrangement on the other side, and the columnar holes caused by the mismatch on two sides of the grain boundary cause the brittleness of the grain boundary; in addition, the larger unit cell volume leads the dislocation motion Berth vector to be larger, the independent slip system is less, the special structure of the grain boundary causes slip to be difficult to pass through the grain boundary, and the alloy is also the reason of intrinsic crystal brittleness. Scholars at home and abroad improve the plasticity of the Ni-Mn-Ga alloy and the toughness thereof through a great deal of work, but no better solution is explored.
Disclosure of Invention
In order to solve the problems of large brittleness and poor machining performance of the existing NiMnGa series magnetic memory alloy, the invention provides a method for synthesizing the NiMnGaCo magnetic memory alloy at high temperature through combustion reaction, and the inventive concept of the invention is as follows: the alloy phase transition temperature is obviously changed and the mechanical property and the physical property are improved by utilizing fine grain strengthening and alloying, a proper amount of Co element is doped in the NiMnGa alloy, and then the NiMnGaCo magnetic memory alloy is synthesized at high temperature through combustion reaction to improve the mechanical property of the alloy and improve the shape memory effect.
The invention adopts the following technical scheme that a method for synthesizing NiMnGaCo magnetic memory alloy at high temperature through combustion reaction: taking 46-50 parts of Ni powder, 25 parts of Mn powder, 25 parts of Ga powder and 1-4 parts of Co powder according to atomic percentage, uniformly mixing the materials by a stirrer, pouring the materials into a pressure forming die, pressing the die by a jack, pressing the powder into a cylindrical sample, placing the sample in a specific clamp, applying a certain pressure to clamp the sample, finally placing the clamp for clamping the sample into a box-type resistance furnace for sintering, keeping the temperature of the resistance furnace at 1000-1200 ℃ for 20-40 minutes, cooling the sample along with the furnace to room temperature, and taking out the sample to obtain the NiMnGaCo magnetic memory alloy.
The clamp comprises an upper pressure plate and a lower pressure plate, and two ends of each pressure plate are fixed by bolts or screws. When the device works, the distance between the upper pressure plate and the lower pressure plate is adjusted through the bolts or the screws, the sample is placed in a space formed between the upper pressure plate and the lower pressure plate, the surface of the sample is in contact with the pressure plate, two ends of the pressure plate are fixed, and pressure is applied to the clamp.
Further, the particle diameters of Ni powder, Mn powder, Ga powder and Co powder are 5 micrometers.
Further, the metal powder is stirred in the stirrer at a speed of 200 to 500 revolutions per minute to be uniformly mixed.
Further, the mold was pressed with a jack, and the powder was pressed into a cylindrical sample having a diameter of 10mm and a height of 10mm by pressurizing to a pressure of 400-1000MPa and maintaining the pressure for 2-4 minutes.
Furthermore, the grain diameter of the NiMnGaCo magnetic memory alloy is 20-30 microns.
Furthermore, the sintering temperature of the box-type resistance furnace is 1200 ℃, and the heat preservation time is 30 minutes.
The shape memory alloy NiMnGaCo prepared by the method is different from the existing magnetic shape memory alloy NiMnGaCo prepared by smelting in a smelting furnace, and has the following advantages compared with the existing magnetic shape memory alloy NiMnGaCo prepared by smelting in a smelting furnace:
1. the rupture strength of the NiMnGaCo alloy prepared by the invention is 7400MPa, which is about 6800MPa higher than that of the existing NiMnGaCo alloy;
2. the fracture strain of the alloy prepared by the method is 16.6 percent, which is improved by 6.6 percent compared with the fracture strain of the existing NiMnGaCo alloy, and the fracture strain of the NiMnGaCo alloy prepared by the method has high toughness.
3. The NiMnGaCo alloy prepared by the invention has the advantages that the grain size is obviously reduced, the diameter is about 20-30 microns, and the structure of the NiMnGaCo alloy is fine.
4. The phase transition temperature of the NiMnGaCo alloy prepared by the invention is about 62 ℃.
Drawings
Fig. 1 is a graph showing the fracture strength and strain at break of the high strength and high plasticity NiMnGaCo alloy prepared in example 1.
FIG. 2 is a DSC curve of the NiMnGaCo alloy prepared in example 2;
fig. 3 is an optical microscope photograph at room temperature of the high strength and high plasticity NiMnGaCo alloy prepared in example 1.
FIG. 4 is a room temperature transmission electron microphase and corresponding electron diffraction pattern for the NiMnGaCo alloy of example 1, where a is the fracture morphology and b is an enlarged view of a.
Detailed Description
The invention is described in more detail below with reference to specific examples, without limiting the scope of the invention. Unless otherwise specified, the experimental methods adopted by the invention are all conventional methods, and experimental equipment, materials, reagents and the like used in the experimental method can be obtained from commercial sources. The press machine referred to in the following examples was a YLJ-303 type micro press machine (JA2003N), and the box type resistance furnace was an SXZ-10-12 box type resistance furnace.
Example 1
The preparation method of the high-strength and high-plasticity NiMnGaCo magnetic memory alloy is prepared according to the following method: mixing 46 parts of Ni powder, 25 parts of Mn powder, 25 parts of Ga powder and 4 parts of Co powder with the grain diameter of 5 microns according to atomic percentage, stirring the metal powder in a stirrer at the speed of 200-500 revolutions/min to uniformly mix the metal powder, then pouring the metal powder into a pressure forming die, pressing the die by a jack, pressing the powder into a cylindrical sample with the diameter of 10mm and the height of 10mm by pressurizing to the pressure of 400-1000MPa and maintaining the pressure for 2-4 minutes, finally sintering the cylindrical sample at the temperature of 1000-1200 ℃ for 20-40 minutes by a sintering process, and finally obtaining the NiMnGaCo magnetic memory alloy with the grain diameter of 20-30 microns.
Example 2
The preparation method of the high-strength and high-plasticity NiMnGaCo magnetic memory alloy is prepared according to the following method: taking 50 parts of Ni powder with the grain diameter of 5 microns, 25 parts of Mn powder, 25 parts of Ga powder and 1 part of Co powder according to atomic percentage, mixing the Ni powder, the Mn powder and the Ga powder in a stirrer at the speed of 200-500 r/min to uniformly mix the metal powder, pouring the metal powder into a pressure forming die, pressing the die by a jack, pressing the powder into a cylindrical sample with the diameter of 10mm and the height of 10mm under the pressure of 400-1000MPa and the pressure maintaining for 2-4 minutes, and finally sintering at the temperature of 1000-1200 ℃ for the heat preservation time of 30 minutes to obtain the NiMnIn magnetic memory alloy with the grain diameter of 20-30 microns.
Example 3
The preparation method of the high-strength and high-plasticity NiMnGaCo magnetic memory alloy is prepared according to the following method: 47 parts of Ni powder with the grain diameter of 5 microns, 25 parts of Mn powder, 25 parts of Ga powder and 3 parts of Co powder are taken according to atomic percentage and mixed, the metal powder is stirred in a stirrer at the speed of 200-500 revolutions/min to be uniformly mixed, then the metal powder is poured into a pressure forming die, a jack is used for pressing the die, the powder is pressed into a cylindrical sample with the diameter of 10mm and the height of 10mm under the pressure of 400-1000MPa and the pressure is maintained for 2-4 minutes, finally, the cylindrical sample is sintered at the temperature of 1200 ℃ and the heat preservation time of 20-40 minutes, and finally the NiMnGaCo magnetic memory alloy with the grain diameter of 20-30 microns is obtained.
The high strength and high plasticity NiMnGaCo alloy prepared in example 1 was subjected to the test of breaking strength and breaking strain, and the test results are shown in fig. 1. The DSC test results of the alloy of NiMnGaCo obtained in example 2 are shown in fig. 2; the fracture strength of the NiMnGaCo alloy prepared by the embodiment is improved by about 6800MPa compared with the NiMnGaCo alloy smelted by a smelting furnace, and the fracture strain is improved by more than about 0.5 times compared with NiMnGa.
The high strength and high plasticity NiMnGaCo alloy prepared in example 1 was subjected to texture observation and analysis at room temperature, and the results are shown in fig. 3. It can be seen from fig. 3 that the NiMnGaCo alloy prepared in the present embodiment has fine grains, and thus plays a role of grain refinement.
The high-strength and high-plasticity NiMnGaCo alloy prepared in example 1 is subjected to fracture strength and fracture strain test and then subjected to mechanism analysis, the fracture morphology is shown in FIG. 4, and a large number of dimples appear in the fracture and almost no cavities appear in the fracture as can be seen from a diagram, which indicates that the alloy has high density at the moment. In addition, a crack almost throughout the cross section is clearly visible, with some small cracks remaining in other directions. The b picture is an enlarged fracture morphology of the A area, grain boundaries can be clearly seen from the b picture, and local grain boundaries are tightly bonded and show good bonding force; however, the bonding between partial grain boundaries is not tight, and a certain gap exists, so that the situation that a crystal face with smooth grains exists locally can be seen from the figure, and the mechanical property of the alloy is weakened. Meanwhile, a certain sliding mark appears in a part of areas, and a certain tearing mark accompanies the inside of the crystal grain, which shows that the alloy mainly has ductile fracture, and has a certain amount of cleavage fracture and crystal-edge fracture caused by defects introduced by material preparation.
The above description is only for the purpose of creating a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can substitute or change the technical solution and the inventive concept of the present invention within the technical scope of the present invention.
Claims (5)
1. A method for synthesizing NiMnGaCo magnetic memory alloy at high temperature through combustion reaction is characterized in that 46-50 parts of Ni powder, 25 parts of Mn powder, 25 parts of Ga powder and 1-4 parts of Co powder are uniformly mixed through a stirrer according to atomic percentage, then the mixture is poured into a pressure forming mold, a jack is used for pressing the mold, the powder is pressed into a cylindrical sample, then the sample is placed in a clamp, the clamp is pressed to 400-plus-material pressure for clamping, the pressure is maintained for 2-4 minutes, finally the clamp for clamping the sample is placed in a box type resistance furnace for sintering, the temperature of the resistance furnace is 1000-plus-material temperature, 1200 ℃ is kept for 20-40 minutes, and then the NiMnGaCo magnetic memory alloy is obtained after the furnace is cooled to room temperature.
2. The method of claim 1, wherein the Ni powder, Mn powder, Ga powder, and Co powder have a particle size of 5 μm.
3. The method according to claim 1, wherein the stirring speed in the stirrer is from 200 to 500 revolutions/min.
4. The method according to claim 1, wherein the powder is pressed after pressing into a cylindrical test piece having a diameter of 10mm and a height of 10 mm.
5. The method of claim 1, wherein the box-type resistance furnace has a sintering temperature of 1200 ℃ and a holding time of 30 minutes.
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| CN107142389A (en) * | 2017-05-04 | 2017-09-08 | 大连大学 | High-strength, the high-ductility Ni of one kind50Mn34In16‑xCoxThe preparation method of Magnetic Memory alloy |
| CN108060330A (en) * | 2017-12-25 | 2018-05-22 | 大连大学 | It is a kind of to inhibit the preparation method of the Ni-Mn-Ga memorial alloys of γ Phase Proportions by powder sintered |
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| CN107142389A (en) * | 2017-05-04 | 2017-09-08 | 大连大学 | High-strength, the high-ductility Ni of one kind50Mn34In16‑xCoxThe preparation method of Magnetic Memory alloy |
| CN108060330A (en) * | 2017-12-25 | 2018-05-22 | 大连大学 | It is a kind of to inhibit the preparation method of the Ni-Mn-Ga memorial alloys of γ Phase Proportions by powder sintered |
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Application publication date: 20181218 Assignee: DALIAN MENGYU MACHINERY CO.,LTD. Assignor: DALIAN University Contract record no.: X2023210000220 Denomination of invention: A method for high-temperature synthesis of NiMnGaCo magnetic memory alloy through combustion reaction Granted publication date: 20200407 License type: Common License Record date: 20231129 |
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