CN111468553B - Nickel-titanium shape memory alloy plate with gradient grain structure - Google Patents
Nickel-titanium shape memory alloy plate with gradient grain structure Download PDFInfo
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- 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
A nickel-titanium shape memory alloy plate with a gradient grain structure is rolled and deformed by a sheath, the initiation and the expansion of cracks in the rolling deformation process are inhibited by means of the compressive stress applied to the rolling surface of the nickel-titanium shape memory alloy plate in the rolling process of the sheath plate, then sufficient plastic strain is synchronously accumulated on the surface layer and the middle layer of the nickel-titanium shape memory alloy plate, then continuous bending deformation is carried out, the difference of the plastic strain distribution of the surface layer and the middle layer of the plate is realized, finally, recrystallization annealing treatment is carried out, nano-scale grains are formed on the surface of the prepared nickel-titanium shape memory alloy plate, micron-scale grains are formed in the middle layer of the plate, the production cost can be obviously reduced, and the plate is prevented from being oxidized at high temperature.
Description
Technical Field
The invention belongs to the technical field of alloy materials, and particularly relates to a nickel-titanium shape memory alloy material.
Background
The most remarkable feature of the shape memory nickel-titanium alloy as a functional material is that the shape memory effect is achieved, namely, the shape memory nickel-titanium alloy is in a certain shape in an austenite phase and is cooled to a martensite phase transformation starting temperature (a)M s) The nickel-titanium shape memory alloy is transformed into a twinned martensite phaseDeforming, and then heating to austenite transformation starting temperature: (A s) Above, austenite transformation starts to occur, and when the temperature rises to the austenite transformation end temperature (S) ((S))A f) With the above, the shape memory nickel titanium alloy will fully return to its original shape in the austenite phase.
The nickel-titanium shape memory alloy has the shape memory effect, so the nickel-titanium shape memory alloy is widely applied to the field of biomedicine, wherein a nickel-titanium shape memory alloy bone fracture plate is a very typical application case. The nickel-titanium shape memory alloy bone fracture plate is required to have good shape memory effect and good biocompatibility on the surface in the service environment of a human body. Research shows that the nickel-titanium shape memory alloy with the nanometer grain size has good biocompatibility, but the shape memory is correspondingly poor. The nickel-titanium shape memory alloy with micron grain size has good shape memory effect but poor biocompatibility.
At present, most of the nickel-titanium shape memory alloy bone fracture plates are prepared based on nickel-titanium shape memory alloy plates, however, the nickel-titanium shape memory alloy plates are plates with single grain size, and because the widely adopted plate processing means (synchronous rolling, asynchronous rolling, equal-diameter angle rolling and the like) can only realize the preparation of the plates with single grain size, the nickel-titanium shape memory alloy plates with the gradient grain structure, the surface layer of which is nano-scale grains and the middle layer of which is micron-scale grains, cannot be prepared. In addition, the nickel-titanium shape memory alloy has high deformation resistance under the condition of lower temperature, obvious strain hardening and lower plasticity, so the processing and preparation of the nickel-titanium shape memory alloy plate are mostly carried out under the condition of medium-high temperature, which relates to the problem that the plate is oxidized at high temperature due to multiple heating treatments of the plate, and the production cost is higher.
Disclosure of Invention
In view of the above-mentioned disadvantages of the prior art, the present invention provides a nickel titanium shape memory alloy sheet with a gradient grain structure, which can be prepared to significantly reduce the production cost and prevent the sheet from being oxidized at high temperature.
The technical scheme of the invention is as follows:
a method for preparing nickel titanium shape memory alloy plate with gradient grain structure, the plate is a nickel titanium shape memory alloy plate with a gradient grain structure, the surface of the plate has nanometer-scale grains, and the middle layer of the plate has micron-scale grains, and the nickel titanium shape memory alloy plate is prepared by the following method:
(1) sheathing the plates: sheathing a steel plate outside the nickel-titanium shape memory alloy plate and fixing the nickel-titanium shape memory alloy plate;
(2) deformation: rolling the sheathed plate, wherein the rolling pass reduction is 40-60%, and the reduction rate of the nickel-titanium shape memory alloy plate is not lower than 35%; then continuously bending and deforming the rolled plate, wherein the radius of an inner fillet at the corner of the continuous bending die is 12-18 mm;
(3) and (3) annealing stage: and cutting a flat plate to be continuously bent and output, separating the deformed nickel-titanium shape memory alloy plate, performing high-temperature oxidation prevention treatment, and performing recrystallization annealing treatment to obtain the nickel-titanium shape memory alloy plate with the gradient grain structure.
The technical proposal shows that the nickel-titanium shape memory alloy plate with the gradient grain structure is rolled and deformed by a sheath, and the initiation and the expansion of cracks in the rolling deformation process are inhibited by the compressive stress applied to the rolling surface of the nickel-titanium shape memory alloy plate by the sheath plate in the rolling process, further, sufficient plastic strain is synchronously accumulated on the surface layer and the middle layer of the nickel-titanium shape memory alloy sheet material (the thinning rate of the nickel-titanium shape memory alloy sheet material is not less than 35 percent), and then continuous bending deformation is carried out, the method has the advantages that large plastic strain is accumulated on the surface layer of the nickel-titanium shape memory alloy plate, small plastic strain is accumulated on the middle layer of the nickel-titanium shape memory alloy plate, and the difference of the plastic strain distribution of the surface layer and the middle layer of the plate is realized, namely the difference of the deformation storage energy distribution (the deformation storage energy of the surface layer is high, and the deformation storage energy of the middle layer is low). Finally, the nickel-titanium shape memory alloy plate is prepared by recrystallization annealing treatment, so that nano-scale grains are formed on the surface of the nickel-titanium shape memory alloy plate, and micro-scale grains are formed in the middle layer of the plate, as shown in figure 2.
Preferably, the sheathing plate in the step (1) is formed by placing a steel plate on the upper surface and the lower surface of the nickel-titanium shape memory alloy plate to form a sandwich stack structure, and winding and fixing the end of the steel plate entering the rolling mill by using a steel wire, so that the sheathing plate and the nickel-titanium shape memory alloy plate are effectively prevented from being dislocated in the rolling process.
Further preferably, when the sheathed plate is rolled in the step (2), the rotating speed of an upper roller and a lower roller of a rolling mill is 10-50m/min, so as to effectively ensure that the sheathed rolled plate without obvious edge crack is obtained.
It is further preferred that the continuous bending mould has at least 6 corners to achieve an efficient bending deformation.
Further preferably, the cut plate is cut at a position 3-7mm after the last corner position of the continuous bending die, so that the flatness of the plate is ensured.
Further preferably, the high-temperature oxidation prevention treatment is to wrap the plate by using tin foil paper, and the high-temperature oxidation prevention treatment has the advantages of low price, easiness in operation and good protection effect.
Further preferably, the recrystallization annealing treatment is to heat the plate to a predetermined temperature, then preserve heat, and finally quench. Further preferably, the heating temperature of the recrystallization annealing treatment is 300-500 ℃, the heating rate is 10-15 ℃/min, after the recrystallization annealing treatment is heated to a preset temperature, the temperature is kept for 10-40min, and then the plate is placed into water for quenching, so that an ideal plate recrystallization annealing grain structure is obtained.
Further preferably, the thickness of the steel plate and the nickel-titanium shape memory alloy plate is 1-2: 1; the steel plate is made of Q235 low-carbon steel or other high-quality low-carbon steel, the room-temperature plastic deformation capacity of the steel plate is strong, and sufficient compressive stress can be applied to the rolled surface of the nickel-titanium shape memory alloy plate.
Further preferably, the surface of the plate is coated with a substance for reducing the friction coefficient of the plate, such as graphite, before the step (2) of deforming.
The invention has the following beneficial effects:
1. the invention combines the sheath rolling-continuous bending process, and realizes the difference of the distribution of plastic strain of the surface layer and the middle layer of the deformed nickel-titanium shape memory alloy plate, namely the difference of the distribution of deformation storage energy (the deformation storage energy of the surface layer is high, and the deformation storage energy of the middle layer is low). Then, the nickel-titanium shape memory alloy plate with the gradient grain structure of the surface layer nanometer-scale grain and the middle layer nanometer-scale grain is prepared through recrystallization annealing treatment, and the coordination and matching of the shape memory effect and the biocompatibility of the nickel-titanium shape memory alloy plate are realized.
2. The invention only needs 1 set of detachable continuous bending die, and can realize the processing and preparation of the nickel-titanium shape memory alloy plate with the gradient grain structure on a common rolling mill. In addition, because the deformation of the nickel-titanium shape memory alloy plate is carried out at room temperature, the problem of high-temperature oxidation is avoided, the process flow is simple, the production cost is obviously reduced, and the method is suitable for nickel-titanium shape memory alloys with various components.
3. According to the jacket rolling structure adopted by the invention, the jacket plate applies compressive stress to the rolling surface of the nickel-titanium shape memory alloy plate in the rolling process, so that the initiation and the expansion of cracks in the rolling deformation process are inhibited, and the large-strain deformation of the nickel-titanium shape memory alloy plate is favorably realized.
Drawings
FIG. 1 is a flow chart of the preparation of a nickel-titanium shape memory alloy plate with a gradient grain structure;
FIG. 2 is a schematic view of the microstructure of the cross section of a nickel titanium shape memory alloy plate with a gradient grain structure.
Detailed Description
The invention is further illustrated by the following examples in conjunction with the accompanying drawings:
in general, the process of the invention is embodied to include the steps of:
1. a preparation stage: firstly, sheathing a Q235 low-carbon steel plate 1 or other high-quality low-carbon steels with the thickness of 2.0mm-4.0mm and a nickel-titanium shape memory alloy plate 2 with the thickness of 2.0mm-4.0mm, polishing to remove surface burrs and an oxide layer, then stacking and compounding the sheathing plate and the nickel-titanium shape memory alloy plate according to a sandwich structure, and winding and fixing the sheathing plate and the nickel-titanium shape memory alloy plate by using steel wires at the end of a feeding mill.
2. And (3) deformation stage: coating graphite on the surface of the prepared composite plate to reduce the friction coefficient of the plate, then transferring the composite plate to a rolling mill 3, adjusting the rotating speed of an upper roller and a lower roller to be 10-50m/min, and adjusting the rolling pass reduction to be 40-60% (ensuring that the reduction rate of the nickel-titanium shape memory alloy plate is not lower than 35%), entering a continuous bending die 4 arranged at the outlet of the rollers to perform continuous bending deformation under the action of rolling friction, wherein the radius of an inner circular angle at a corner R1-R6 is 12-18 mm.
3. And (3) annealing stage: cutting the composite plate 5 at a position 3-7mm behind a corner R6 of a continuous bending die (ensuring the flatness of the plate), mechanically separating the deformed nickel-titanium shape memory alloy plate from the composite plate, wrapping the composite plate with tinfoil paper (preventing high-temperature oxidation), heating in a heating furnace 6 at the heating temperature of 300-500 ℃ at the heating rate of 10-15 ℃/min, keeping the temperature for 10-40min after heating to a preset temperature, and then putting the composite plate into water for quenching.
Finally obtaining the nickel-titanium shape memory alloy plate with the gradient grain structure of the surface layer nanometer-scale grain and the middle layer nanometer-scale grain, and referring to figure 2.
Example 1: for a nickel-titanium shape memory alloy plate with the thickness of 2.5mm, Ni50.9at% Ti49.1at% adopts the following process steps and parameters:
(1) 1 nickel titanium shape memory alloy plate with 200mm x 120mm x 2.5mm atomic ratio of Ni50.9at% Ti49.1at% is ground to remove burrs and oxide skin, 2Q 235 low carbon steel plates with 200mm x 120mm x 3mm are ground to remove burrs and oxide skin, then the two are stacked and compounded according to a 'sandwich' structure, and the steel wires are wound and fixed on a rolling mill end.
(2) Coating graphite on the surface of the prepared composite plate to reduce the friction coefficient of the friction plate, then transferring the composite plate to a rolling mill, adjusting the rotating speed of an upper roller and a lower roller to be 25m/min, and adjusting the rolling pass reduction to be 50% (ensuring that the reduction rate of the nickel-titanium shape memory alloy plate is not lower than 35%), wherein the composite plate enters a continuous bending die arranged at the outlet of the rollers to perform continuous bending deformation under the action of rolling friction, and the radius of an inner circular angle at a corner No. R1-R6 of the continuous bending die is 13 mm.
(3) Cutting off the composite board (ensuring the smoothness of the board) at a position 5mm behind a corner R6 of a continuous bending die, separating the deformed nickel-titanium shape memory alloy board from the composite board in a mechanical knocking mode, wrapping the composite board with tinfoil paper (preventing high-temperature oxidation), heating in a heating furnace at the heating temperature of 450 ℃ and the heating rate of 10-15 ℃/min, continuing to preserve heat for 12min after heating to a preset temperature, and then putting the composite board into water for quenching to obtain the gradient grain structure nickel-titanium shape memory alloy board with the surface layer grain size of 260-350nm and the middle layer grain size of 5-10 mu m.
Example 2: the following process steps and parameters are adopted for a nickel-titanium shape memory alloy plate with the thickness of 3.0mm, wherein the nickel-titanium shape memory alloy plate is Ni47at%, Ti50at%, Fe3 at%:
(1) 1 nickel titanium shape memory alloy plate with the atomic ratio of Ni47at% Ti50at% Fe3at% and 200mm 120mm 3.5mm Q235 low carbon steel plate are ground to remove burrs and scale, and then the two are stacked and compounded according to a sandwich structure, and the steel wire is wound and fixed at the end of a rolling mill.
(2) Coating graphite on the surface of the prepared composite plate to reduce the friction coefficient of the friction plate, then transferring the composite plate to a rolling mill, adjusting the rotating speed of an upper roller and a lower roller to 35m/min, and adjusting the rolling pass reduction to 43% (ensuring that the reduction rate of the nickel-titanium shape memory alloy plate is not lower than 35%), wherein the composite plate enters a continuous bending die arranged at the outlet of the rollers to perform continuous bending deformation under the action of rolling friction, and the radius of an inner circular corner at a corner No. R1-R6 of the continuous bending die is 15 mm.
(3) Cutting the composite board 4mm after the position of a corner R6 of a continuous bending die (ensuring the flatness of the board), separating the deformed nickel-titanium shape memory alloy board from the composite board in a mechanical knocking mode, wrapping the composite board with tinfoil paper (preventing high-temperature oxidation), heating in a heating furnace at the heating temperature of 380 ℃ at the heating rate of 10-15 ℃/min, continuing to preserve heat for 25min after heating to a preset temperature, and then putting the composite board into water for quenching to obtain the gradient grain structure nickel-titanium shape memory alloy board with the surface grain size of 300-400 nm and the middle layer grain size of 6-12 mu m.
Claims (10)
1. A preparation method of a nickel-titanium shape memory alloy plate with a gradient grain structure is characterized in that the plate is a nickel-titanium shape memory alloy plate with a gradient grain structure, wherein the surface of the nickel-titanium shape memory alloy plate is provided with nano-scale grains, and the middle layer of the nickel-titanium shape memory alloy plate is provided with micro-scale grains, and the nickel-titanium shape memory alloy plate is prepared by the following steps:
(1) sheathing the plates: sheathing a steel plate outside the nickel-titanium shape memory alloy plate and fixing the nickel-titanium shape memory alloy plate;
(2) deformation: rolling the sheathed plate, wherein the rolling pass reduction is 40-60%, and the reduction rate of the nickel-titanium shape memory alloy plate is not lower than 35%; then continuously bending and deforming the rolled plate, wherein the radius of an inner fillet at the corner of the continuous bending die is 12-18 mm;
(3) and (3) annealing stage: and cutting a flat plate which is output after continuous bending deformation, separating the deformed nickel-titanium shape memory alloy plate, performing high-temperature oxidation prevention treatment, and then performing recrystallization annealing treatment to obtain the nickel-titanium shape memory alloy plate with the gradient grain structure.
2. The method for preparing a ni-ti shape memory alloy plate with a gradient grain structure according to claim 1, wherein the sheathing plate in the step (1) is formed by placing steel plates on the upper and lower surfaces of the ni-ti shape memory alloy plate to form a sandwich stack structure, and winding and fixing the steel wires at the end of the steel plate entering the rolling mill.
3. The method for preparing a nickel titanium shape memory alloy plate with a gradient grain structure according to claim 1 or 2, wherein the rotation speed of upper and lower rollers of a rolling mill is 10-50m/min when the sheathed plate is rolled in the step (2).
4. The method of claim 1 or 2, wherein the continuous bending mold has at least 6 corners.
5. The method for preparing a nickel titanium shape memory alloy plate with a gradient grain structure as claimed in claim 1 or 2, wherein the flat plate output after the continuous bending deformation is cut in the step (3) and is cut at a position 3-7mm after the last corner position of the continuous bending die.
6. The method for preparing the nickel titanium shape memory alloy plate with the gradient grain structure as claimed in claim 1 or 2, wherein the high temperature oxidation prevention treatment in the step (3) is to wrap the plate with tinfoil paper.
7. The method for preparing the nickel titanium shape memory alloy plate with the gradient grain structure as claimed in claim 1 or 2, wherein the recrystallization annealing treatment comprises the steps of heating the plate to a preset temperature, then preserving the temperature and finally quenching.
8. The method for preparing the nickel titanium shape memory alloy plate with the gradient grain structure according to claim 7, wherein the heating temperature of the recrystallization annealing treatment is 300-500 ℃, the heating rate is 10-15 ℃/min, after the nickel titanium shape memory alloy plate is heated to a preset temperature, the temperature is kept for 10-40min, and then the nickel titanium shape memory alloy plate is put into water for quenching.
9. The method for preparing the nickel titanium shape memory alloy plate with the gradient grain structure according to the claim 1 or 2, wherein the thickness ratio of the steel plate to the nickel titanium shape memory alloy plate is 1-2: 1; the steel plate is Q235 low-carbon steel.
10. The method for preparing a nickel titanium shape memory alloy plate with a gradient grain structure as claimed in claim 1 or 2, wherein the surface of the plate is coated with a substance for reducing the friction coefficient of the plate before the step (2) of deforming.
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| CN113046665A (en) * | 2021-03-09 | 2021-06-29 | 江苏盛玛特新材料科技有限公司 | Nickel-titanium alloy preparation method for improving radial stability and medical device |
| CN112899596A (en) * | 2021-03-09 | 2021-06-04 | 清华大学 | Method for improving refrigeration performance by regulating stress-strain response of nickel-titanium alloy |
| CN115519847B (en) * | 2022-10-10 | 2024-07-26 | 太原理工大学 | Metal composite thin strip with double-pass shape memory effect and forming method thereof |
| CN116039178A (en) * | 2023-02-15 | 2023-05-02 | 湖北振华化学股份有限公司 | Nickel composite layer plate and preparation method and application thereof |
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