CN113046659A - Method for preparing nickel-titanium shape memory alloy with gradient nanocrystalline grain structure - Google Patents
Method for preparing nickel-titanium shape memory alloy with gradient nanocrystalline grain structure Download PDFInfo
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- CN113046659A CN113046659A CN202110258415.9A CN202110258415A CN113046659A CN 113046659 A CN113046659 A CN 113046659A CN 202110258415 A CN202110258415 A CN 202110258415A CN 113046659 A CN113046659 A CN 113046659A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/02—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B1/00—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
- B21B1/22—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling plates, strips, bands or sheets of indefinite length
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
- B21C1/00—Manufacture of metal sheets, metal wire, metal rods, metal tubes by drawing
- B21C1/003—Drawing materials of special alloys so far as the composition of the alloy requires or permits special drawing methods or sequences
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
- B21C23/00—Extruding metal; Impact extrusion
- B21C23/002—Extruding materials of special alloys so far as the composition of the alloy requires or permits special extruding methods of sequences
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
- B21C23/00—Extruding metal; Impact extrusion
- B21C23/02—Making uncoated products
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B29/00—Machines or devices for polishing surfaces on work by means of tools made of soft or flexible material with or without the application of solid or liquid polishing agents
- B24B29/02—Machines or devices for polishing surfaces on work by means of tools made of soft or flexible material with or without the application of solid or liquid polishing agents designed for particular workpieces
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
- C21D9/0081—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for slabs; for billets
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/10—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of nickel or cobalt or alloys based thereon
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B1/00—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
- B21B1/22—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling plates, strips, bands or sheets of indefinite length
- B21B2001/221—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling plates, strips, bands or sheets of indefinite length by cold-rolling
Abstract
The invention provides a method for preparing a nickel-titanium shape memory alloy with a gradient nanocrystalline grain structure, which is characterized by comprising the following steps: step 1, preparing an ultrafine nanocrystalline nickel-titanium alloy matrix with the average grain size of about 5-20 nm by a forced plastic deformation process; step 2, polishing the surface of the superfine nanocrystalline nickel-titanium alloy obtained in the step 1 to a mirror surface; and 3, carrying out surface heat treatment on the superfine nanocrystalline matrix obtained in the step 2 by using continuous laser with the power of 50-300W, wherein the laser scanning speed is 400-2000 mm/s, and the scanning line interval is 5-100 mu m. The nickel-titanium alloy with the gradient nano-grain structure is prepared by combining the traditional cold processing technology and the emerging laser processing technology, the nickel-titanium alloy with the gradient structure can give consideration to both the strength and the ductility of the material, and simultaneously, the energy dissipation in the phase change process is reduced, so that the service life is prolonged, and the mechanical property stability is improved. In addition, the process is simple to operate, high in precision, low in cost, capable of being rapidly produced in mass and put into use, and wide in application prospect.
Description
Technical Field
The invention belongs to the field of regulating and controlling macroscopic mechanical properties through metal microstructure design, and particularly relates to a method for preparing a nickel-titanium shape memory alloy with a gradient nanocrystalline grain structure.
Background
The nickel-titanium shape memory alloy is widely applied to the fields of aerospace, microelectronic devices, biomedical treatment, solid state refrigeration and the like due to unique superelasticity, shape memory, corrosion resistance and biocompatibility. The traditional commercial coarse-grain nickel-titanium alloy has good ductility and considerable latent heat of phase change, but the huge energy dissipation (hysteresis loop area) in the phase change process can accelerate the mechanical property decline and fatigue failure of the material, and simultaneously reduce the stability of the component in the service process. Furthermore, the applications of commercial macrocrystalline nickel titanium alloys tend to be limited by their limited strength and fatigue life. The obtained nanocrystalline nickel-titanium alloy after strong plastic deformation (plastic deformation) has ultrahigh strength, stable superelasticity and considerable fatigue life, but the performance is improved at the expense of ductility and latent heat of phase change of the material. Therefore, a method for preparing the nickel-titanium alloy with the gradient grain structure is urgently needed, so that the large latent heat and the high ductility of coarse grains and the high strength, the high stability and the fatigue resistance of fine grains are considered.
Disclosure of Invention
Aiming at the problems in the prior art, the technical scheme adopted by the invention for solving the problems in the prior art is as follows:
a method for preparing a nickel-titanium shape memory alloy with a gradient nanocrystalline grain structure is characterized by comprising the following steps:
step 1, preparing an ultra-fine nanocrystalline nickel-titanium alloy thin plate substrate with the average grain size of about 5-20 nm through a forced plastic deformation cold rolling process;
step 2, polishing the surface of the superfine nanocrystalline nickel-titanium alloy obtained in the step 1 to a mirror surface;
and 3, carrying out surface heat treatment on the superfine nanocrystalline matrix obtained in the step 2 by using continuous laser with the power of 50-300W, wherein the laser scanning speed is 400-2000 mm/s, and the scanning line interval is 5-100 mu m.
The ultra-fine nanocrystalline nickel-titanium alloy matrix in the step 1 can be other pure metals or alloys, such as nickel, titanium, molybdenum, nickel-based alloy, titanium-based alloy, various stainless steels, high-entropy alloy and the like.
The geometric shape of the superfine nanocrystalline nickel-titanium alloy matrix prepared in the step 1 can be a plate, a cylinder, a pipe, a wire or a cuboid, and the superfine nanocrystalline nickel-titanium alloy matrix is prepared by a cold rolling method, an equal-channel extrusion method, a cold drawing method or a high-pressure torsion method and other strong plastic deformation methods, wherein the processing temperature is below the metal recrystallization temperature and generally needs to be lower than 100 ℃.
The raw material in the step 1 is a common commercial nickel-titanium alloy plate with coarse crystals and approximately equal atomic ratio, a stainless steel plate is wrapped outside the nickel-titanium alloy plate, the pressing amount of a roller is controlled within 0.05mm each time in the cold rolling process, the nickel-titanium alloy plate is rolled in multiple passes, and finally the thickness of the nickel-titanium alloy plate is uniformly reduced by 20-70% and no obvious micro cracks exist on the surface.
In the step 2, the polishing method comprises the steps of firstly sequentially grinding by using 240,800,2000,4000-mesh silicon carbide abrasive paper, and then mechanically polishing by using a polishing solution until the surface of the sample is rough and the surface of the sample does not contain microcracks under a light mirror.
In the step 3, the laser power, the laser scanning speed and the scanning line interval are adjusted according to actual conditions, so that the crystal grain size is distributed in a gradient manner along the thickness direction, and the situation that the crystal grain of the substrate is completely grown due to overhigh laser input energy or a coarse crystal area is difficult to generate due to overlow input power is avoided.
In the step 3, the element on the surface of the substrate is prevented from evaporating to form a pit due to overhigh laser input energy, and meanwhile, the whole laser processing process needs to be carried out under inert protective gas.
The invention has the following advantages:
the nickel-titanium shape memory alloy with the gradient nanocrystalline grain structure is prepared by combining the traditional cold processing technology and the emerging laser processing technology, the nickel-titanium shape memory alloy with the gradient nanocrystalline grain structure can give consideration to both the strength and the ductility of the material, and simultaneously, the energy dissipation in the phase change process is reduced, so that the service life is prolonged, and the mechanical property stability is improved. In addition, the process is simple to operate, high in precision, low in cost, capable of being rapidly produced in mass and put into use, and wide in application prospect.
Drawings
FIG. 1 is a schematic view of the processing of the method of the present invention;
FIG. 2 is a graph showing the evolution of the microstructure of a gradient nanocrystalline nitinol alloy prepared by the method of the present invention along the thickness d of the plate;
FIG. 3 is a graph of the average grain size of nickel titanium with gradient grains prepared by the method of the present invention along the thickness of the sheet;
FIG. 4 is a graph of stress strain versus stress strain for nickel titanium in a graded grain structure, severely plastically deformed nickel titanium, and conventional commercial macrocrystalline nickel titanium.
Detailed Description
Referring to fig. 1, a method for preparing a nickel-titanium shape memory alloy with a gradient nanocrystalline grain structure, according to an embodiment of the present invention, a commercial coarse-grained superelastic nickel-titanium alloy sheet with an initial thickness of 1.5mm, a chemical composition of 50.8% atomic nickel and 49.2% titanium is processed according to the following steps:
A. repeatedly cold rolling to make the final thickness of the plate be 1mm and the average grain size be about 14 nm;
B. polishing all the surfaces of the superfine nanocrystalline to a mirror surface;
C. and performing surface scanning on the polished superfine nanocrystalline nickel-titanium matrix by using a continuous laser with the power of 100W, wherein the scanning speed is 1000mm/s, and the scanning line spacing is 30 mu m.
In the step A, the superfine nanocrystalline nickel-titanium alloy matrix can be other pure metals or alloys, such as nickel, titanium, molybdenum, nickel-based alloy, titanium-based alloy, various stainless steels, high-entropy alloy and the like, the geometric shape can be a plate, a cylinder, a pipe, a wire or a cuboid, the superfine nanocrystalline nickel-titanium alloy matrix is prepared by a cold rolling method, an equal-channel extrusion method, a cold drawing method or a high-pressure torsion method, and the processing temperature is below the metal recrystallization temperature and generally needs to be lower than 100 ℃. The raw material is a nickel-titanium alloy plate with common commercial coarse crystals and approximately equal atomic ratio, a stainless steel plate is wrapped outside the nickel-titanium alloy plate, the pressing amount of a roller is controlled within 0.05mm each time in the cold rolling process, the nickel-titanium alloy plate is rolled in multiple times, the thickness of the nickel-titanium plate is reduced by 33% uniformly, and the surface of the nickel-titanium plate is free of obvious microcracks.
In the step B, the polishing method comprises the steps of firstly sequentially grinding by using 240,800,2000,4000-mesh silicon carbide abrasive paper, and then mechanically polishing by using a polishing solution until the surface of the sample is rough and the surface of the sample does not contain microcracks under a light mirror.
In the step C, the laser power, the laser scanning speed and the scanning line spacing are adjusted according to actual conditions, so that the grain sizes are distributed in a gradient manner along the thickness direction. The crystal grains of the matrix are prevented from growing completely due to the over-high input energy of the laser, and the coarse crystal area is prevented from being generated due to the over-low input power. Coarse crystals are generated on the surface of the processed sample, ultrafine nanocrystals are still kept in the matrix, and the size of the crystals is gradually reduced from 100nm of the surface to 14nm of the core along the depth.
The results of experiments conducted based on the examples of the present invention show that the nickel titanium alloy treated according to the method of the present invention gradually decreases in thickness from 100nm at the surface to 14nm at the center, and the grain boundaries evolve from being clearly visible to dislocation loops, as shown in fig. 2 and 3. As can be seen from FIG. 4, the nickel titanium with the gradient grain structure prepared by the method has both high ductility of commercial coarse grains and high strength of ultra-fine grains, which indicates that the method can break the barrier between the strength and the ductility of the material. In addition, the hysteresis loop area in the phase change process of the nickel-titanium with the gradient structure is greatly reduced, so that the nucleation and the expansion of microcracks in the cyclic deformation process can be effectively inhibited, and the fatigue life of the structure is prolonged. From fig. 4, a significantly reduced hysteresis and a significantly increased hardening capacity can enhance the mechanical stability of the material during service. In conclusion, the method can prepare the nickel titanium with the gradient grain structure, so that the nickel titanium has high strength and high ductility, and simultaneously reduces energy dissipation in the phase change process, thereby prolonging the service life and improving the stability of mechanical properties.
The scope of the present invention is not limited to the above examples, and it is apparent that those skilled in the art can make various modifications and variations to the present invention without departing from the scope and spirit of the invention. It is intended that the present invention cover the modifications and variations of this invention provided they come within the scope of the appended claims and their equivalents.
Claims (7)
1. A method for preparing a nickel-titanium shape memory alloy with a gradient nanocrystalline grain structure is characterized by comprising the following steps:
step 1, preparing an ultra-fine nanocrystalline nickel-titanium alloy thin plate substrate with the average grain size of about 5-20 nm through a strong plastic deformation (strong plastic deformation) cold rolling process;
step 2, polishing the surface of the superfine nanocrystalline nickel-titanium alloy obtained in the step 1 to a mirror surface;
and 3, carrying out surface heat treatment on the superfine nanocrystalline matrix obtained in the step 2 by using continuous laser with the power of 50-300W, wherein the laser scanning speed is 400-2000 mm/s, and the scanning line interval is 5-100 mu m.
2. The method of claim 1, wherein the gradient nanocrystalline grain nitinol is formed by a method comprising: the superfine nanocrystalline nickel-titanium alloy matrix in the step 1 can be other pure metals or alloys, such as nickel, titanium, molybdenum, nickel-based alloy, titanium-based alloy, various stainless steels, high-entropy alloy and the like.
3. The method of claim 1, wherein the gradient nanocrystalline grain nitinol is formed by a method comprising: the geometric shape of the superfine nanocrystalline nickel-titanium alloy matrix prepared in the step 1 can be a plate, a cylinder, a pipe, a wire or a cuboid, and the superfine nanocrystalline nickel-titanium alloy matrix is prepared by a cold rolling method, an equal-channel extrusion method, a cold drawing method or a high-pressure torsion method and other strong plastic deformation methods, wherein the processing temperature is below the metal recrystallization temperature and generally needs to be lower than 100 ℃.
4. The method of claim 1, wherein the gradient nanocrystalline grain nitinol is formed by a method comprising: the raw material in the step 1 is a common commercial nickel-titanium alloy plate with coarse crystals and approximately equal atomic ratio, a stainless steel plate is wrapped outside the nickel-titanium alloy plate, the secondary pressing amount of a roller is controlled within 0.05mm in the cold rolling process, the nickel-titanium alloy plate is rolled in multiple passes, and finally the thickness of the nickel-titanium alloy plate is uniformly reduced by 20-70% and no obvious micro cracks exist on the surface.
5. The method of claim 1, wherein the gradient nanocrystalline grain nitinol is formed by a method comprising: in the step 2, the polishing method comprises the steps of firstly sequentially grinding by using 240,800,2000,4000-mesh silicon carbide abrasive paper, and then mechanically polishing by using a polishing solution until the surface of the sample is rough and the surface of the sample does not contain microcracks under a light mirror.
6. The method of claim 1, wherein the gradient nanocrystalline grain nitinol is formed by a method comprising: in the step 3, the laser power, the laser scanning speed and the scanning line interval are adjusted according to actual conditions, so that the grain size is distributed in a gradient manner along the thickness direction, and simultaneously, the situation that the grain of the substrate is completely grown due to overhigh laser input energy or a coarse crystal area is difficult to generate due to overlow input power is avoided.
7. The method of claim 1, wherein the gradient nanocrystalline grain nitinol is formed by a method comprising: in the step 3, the element on the surface of the substrate is prevented from evaporating to form a pit due to overhigh laser input energy, and meanwhile, the whole laser processing process needs to be carried out under inert protective gas.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN114260330A (en) * | 2021-11-29 | 2022-04-01 | 中国兵器工业第五九研究所 | Accurate preparation method of ultrafine-grained tissue thin-wall conical part |
CN114411074A (en) * | 2021-12-13 | 2022-04-29 | 四川大学 | Multilayer biphase trans-scale structure pure titanium and preparation method thereof |
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CN106148658A (en) * | 2015-03-26 | 2016-11-23 | 西安思维金属材料有限公司 | A kind of Ti-Ni alloy adds refractory metal powder distributing method |
CN108517441A (en) * | 2018-04-15 | 2018-09-11 | 烟台浩忆生物科技有限公司 | Low transformation temperature titanium zirconium niobium tantalum marmem, preparation method and applications |
CN109518103A (en) * | 2018-12-28 | 2019-03-26 | 武汉大学 | A method of Nitinol refrigeration efficiency is improved than, service life and temperature stability |
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2021
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US20090165898A1 (en) * | 2007-11-30 | 2009-07-02 | Abbott Laboratories | Fatigue-resistant nickel-titanium alloys and medical devices using same |
US20130205567A1 (en) * | 2007-11-30 | 2013-08-15 | Abbott Laboratories | Fatigue-resistant nickel-titanium alloys and medical devices using same |
CN106148658A (en) * | 2015-03-26 | 2016-11-23 | 西安思维金属材料有限公司 | A kind of Ti-Ni alloy adds refractory metal powder distributing method |
CN108517441A (en) * | 2018-04-15 | 2018-09-11 | 烟台浩忆生物科技有限公司 | Low transformation temperature titanium zirconium niobium tantalum marmem, preparation method and applications |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN114260330A (en) * | 2021-11-29 | 2022-04-01 | 中国兵器工业第五九研究所 | Accurate preparation method of ultrafine-grained tissue thin-wall conical part |
CN114260330B (en) * | 2021-11-29 | 2023-09-12 | 中国兵器工业第五九研究所 | Accurate preparation method of superfine crystal tissue thin-wall conical part |
CN114411074A (en) * | 2021-12-13 | 2022-04-29 | 四川大学 | Multilayer biphase trans-scale structure pure titanium and preparation method thereof |
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