CN114855008A - Nickel-titanium alloy double-pass shape memory effect training method with high nickel-rich content - Google Patents
Nickel-titanium alloy double-pass shape memory effect training method with high nickel-rich content Download PDFInfo
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Abstract
The invention relates to a nickel-titanium alloy two-way shape memory effect training method with high nickel-rich content, which comprises the following steps of preparing a strip-shaped alloy from a high-purity nickel block and high-purity sponge titanium according to a ratio; enclosing the nickel-titanium alloy strip with high nickel-rich content in a quartz tube filled with inert gas for homogenization treatment, and then carrying out water-cooling quenching and thickness reduction treatment to obtain a sample strip; and bending all the sample strips in a semi-cylindrical constraint mould with an arc-shaped groove, carrying out constraint aging treatment on the semi-cylindrical constraint mould loaded with the sample strips, and immediately carrying out water quenching after the treatment is finished. The nickel-titanium sample strip with high nickel content has excellent two-way shape memory, the strength is obviously higher than that of nickel-titanium alloy with near equal atomic ratio, and the R phase transition temperature of more than 25 ℃ is also achieved, namely the temperature corresponding to deformation generated during cooling is higher than room temperature, so that the material meets the loose service condition, and the nickel-titanium alloy with high nickel content can be subjected to constraint aging treatment in batch and high efficiency.
Description
Technical Field
The invention relates to the technical field of heat treatment processes, in particular to a nickel-titanium alloy two-way shape memory effect training method with high nickel content.
Background
Nickel titanium alloys have been widely used in the fields of daily life, aerospace, biomedical, mechanical engineering, etc. due to their excellent shape memory effect, high strength and good biocompatibility, and are the most successful and widely used alloys in all shape memory alloys. The unique functional properties of Ni-rich Ni-Ti alloys are a two-way shape memory effect that allows the alloys to repeatedly change shape during heating and cooling cycles, while the one-way shape memory effect is limited to only a single change in shape. The two-way shape memory effect is not an inherent property of nitinol, but rather requires some "training" process to provide the two-way shape memory effect. The purpose of "training" is to introduce specific dislocation fields or specific orientations of Ni into the nickel-titanium alloy 4 Ti 3 Thereby generating a specific internal force in the matrix. Under the influence of an internal stress field, martensite of the nickel-titanium alloy takes a specific orientation and macroscopically shows a shape change in the process of martensitic transformation. As long as this internal stress field is present, the nitinol can be changed back and forth between the high temperature and low temperature shapes as the temperature increases and decreases. Due to Ni 4 Ti 3 The coherent precipitated phase structure can maintain higher stability in repeated phase change cycles and mechanical cycles relative to the dislocation structure, so that specific orientation Ni is introduced into the matrix 4 Ti 3 Coherent precipitated phases are the common practice in the industry at present. The nickel-titanium alloy is aged by adopting a constrained aging process, so that a large amount of Ni arranged along a certain direction can be precipitated in a matrix 4 Ti 3 Coherent precipitated phases to introduce into the matrixThe stable coherent internal stress field enables the nickel-titanium alloy to have excellent two-way shape memory effect.
The nickel-titanium alloy is extremely sensitive to the change of nickel atom content, and the change of nickel content of every 1 percent can cause the properties of the alloy, such as phase change temperature, hardness, strength and the like, to be greatly changed. At present, the application of the nickel-titanium alloy two-way shape memory effect mainly focuses on the nickel-titanium alloy with the near-equal atomic ratio of 50-51 at.%, and related researches on the nickel-nickel alloy two-way shape memory effect with the high nickel-rich content of more than 51 at.% are rarely reported. The hardness of the nickel-titanium alloy with high nickel-rich content is generally over 400HV and is far greater than that of the nickel-titanium alloy with nearly equal atomic ratio, the defects of difficult smelting preparation and forming and difficult processing exist, and meanwhile, the alloy is broken due to excessive strain in the training process, so that the training fails. Under the influence of the above disadvantages, the "training" method for the two-way shape memory effect of nickel-titanium alloys with high nickel-rich content relative to near-equiatomic ratio nickel-titanium alloys is still lacking in systematic studies. Compared with the nickel-titanium alloy with the approximate equal atomic ratio, the nickel-titanium alloy with the high nickel-rich content has the excellent properties of high strength, high wear resistance, high corrosion resistance and the like, and has lower density compared with the traditional structural steel, so that the nickel-titanium alloy with the high nickel-rich content has greater application potential in equipment and devices with high mechanical and corrosion resistance requirements in the fields of aerospace, machinery, petroleum, electric power, chemical engineering, ocean engineering and the like. The nickel-titanium alloy with high nickel content and double-pass shape memory effect can be used as the core material of driving device suitable for the above severe service environment, and the nickel-titanium alloy with high nickel content can be used as an intelligent device driven by temperature change and applied to the working platforms of scientific research deep submergence vehicles, deep sea mining, transportation ships and the like in the ocean field, and has great development potential.
In view of the fact that no training process for nickel-titanium alloy rich in nickel exists at present, an efficient short-time constraint aging process is provided, and the nickel-titanium alloy rich in nickel has an excellent two-way shape memory effect and a high phase transition temperature.
Disclosure of Invention
Aiming at the technical problems in the prior art, the invention aims to: the nickel-titanium alloy with high nickel content has excellent two-way shape memory effect in a short time, and the R phase transition temperature of the nickel-titanium alloy can be controlled to be 25.1-53.6 ℃, so that the nickel-titanium alloy can be widely applied to intelligent devices with the working occasions above room temperature.
In order to achieve the purpose, the invention adopts the following technical scheme:
a nickel-titanium alloy two-way shape memory effect training method with high nickel-rich content comprises the following steps:
(1) repeatedly smelting the high-purity titanium sponge and the electrolytic nickel block for 6 times by using a vacuum arc smelting furnace to obtain a nickel-titanium alloy ingot with high nickel-rich content; then melting the obtained nickel-titanium alloy ingot with high nickel content again and carrying out suction casting to obtain a nickel-titanium alloy sample strip;
(2) enclosing the nickel-titanium alloy strip with high nickel-rich content in a quartz tube filled with inert gas for homogenization treatment, and performing water-cooling quenching after the homogenization treatment is finished; then, carrying out thickness reduction treatment on the sample to obtain a sample strip;
(3) and bending all the sample strips in a semi-cylindrical constraint mould with an arc-shaped groove, carrying out constraint aging treatment on the semi-cylindrical constraint mould loaded with the sample strips at the temperature of 400-500 ℃ for 3-5 h, and immediately carrying out water quenching after the treatment. The "training" is completed.
Preferably, the inert atmosphere is argon.
Preferably, the temperature of the homogenization treatment is 1000 ℃, and the time of the homogenization treatment is 3 h.
Preferably, the thickness of the sample strip is measured by a vernier caliper, and the thickness of the sample strip is recorded as t according to the formula
Is calculated to obtain wherein ∈ max Is the maximum strain value of the sample strip, 0 < epsilon max Less than or equal to 2 percent; and R is the curvature radius of the arc-shaped groove of the semi-cylindrical constraint mould.
Preferably, the thickness of the sample strip is 0.4-0.5 mm; the curvature radius of the arc-shaped groove of the semi-cylindrical constraint mould is 33 mm.
Preferably, the nickel-titanium alloy strip with high nickel-rich content is prepared by a rapid solidification process.
Preferably, the rapid solidification process is performed in the following manner: after vacuum arc melting, suction casting the molten alloy into a water-cooled oxygen-free copper mold; the corresponding dimension of the alloy strip is 50-100 mm (length) multiplied by 8-10 mm (width) multiplied by 0.5-1.5 mm (thickness).
Preferably, the nickel content in the nickel-titanium alloy strip with high nickel-rich content is as follows: the titanium atomic ratio is 52-53: 48-47.
Preferably, the thinning treatment uses a steel mould, the surface of the mould is ensured to be flat, the mould is well contacted with the surface of a sample during adhesion, the sample cannot be inclined in the thinning process, and the thickness of the sample is ensured to uniformly meet the design requirement.
Preferably, the semi-cylindrical constraint mould is in a mould with multiple cavities, and the mould is positioned and locked by using screws; more preferably 3 arc-shaped recesses, the mould being positioned and locked using 4 screws.
The principle of the invention is as follows:
nickel titanium alloys with nickel content greater than 50 at.% will precipitate Ni during aging 4 Ti 3 Metastable phases which, at the beginning of growth, are coherent with the matrix of the nickel-titanium alloy, due to Ni 4 Ti 3 The lattice parameter of the phase is different from that of the matrix, and therefore, the matrix is distorted to generate a coherent internal stress field in the alloy. However, the coherent internal stress field without a specific direction cannot enable the nickel-titanium alloy to have a two-way shape memory effect, and only the strong stress field with consistent orientation can enable the nickel-titanium alloy to generate the characteristic. The constraint aging process respectively applies tensile stress and compressive stress to the outer side and the inner side of the nickel-titanium alloy spline so as to lead Ni to be 4 Ti 3 The phases precipitate during the aging process in a manner parallel to the tensile stress and perpendicular to the compressive stress. Ni 4 Ti 3 The specific precipitation mode of the phases causes a strong coherent internal stress field to be generated in the nickel-titanium alloyUnder the influence of the field, the alloy generates martensite variants with specific orientation when undergoing martensite phase transformation during cooling, thereby forming a two-way shape memory effect macroscopically.
Ni 4 Ti 3 The nucleation and growth process of the precipitated phase is controlled by diffusion type phase change, the nucleation stage is mainly controlled by short-range diffusion of nickel atoms, and the growth process is determined by the long-range diffusion of the nickel atoms. The constraint aging temperature is selected to be a medium-high temperature of 400-500 ℃, and the aim is to improve the diffusion rate of the concentration of nickel atoms in the B2 matrix and enable a precipitated phase to grow rapidly in a short time. The grown precipitated phases form preferred orientation arrangement in a matrix, and then stable directional coherent stress field is introduced to dominate the variant selection of phase change behavior, so that a normal two-way shape memory effect is formed macroscopically.
At present, the research on the nickel-titanium alloy two-way shape memory effect mainly focuses on the nickel-rich nickel-titanium alloy with a near-equal atomic ratio and a nickel content of 50-51 at.%, and the report of the nickel-rich nickel-nickel alloy two-way shape memory effect with a nickel content of more than 51 at.% does not appear. This is because the nickel-titanium alloy with high nickel-rich content has poor fluidity in the molten state, and the alloy prepared by melting has more defects, and meanwhile, the nickel-titanium alloy with high nickel-rich content has higher hardness, so that the nickel-titanium alloy is easy to break when deformed in training.
Compared with the prior art, the invention has the following advantages:
(1) short time and high efficiency. The middle-high temperature constraint aging process provided by the invention can effectively shorten the time of the training process, can efficiently carry out constraint aging treatment on the nickel-titanium alloy with high nickel content in batches, and can increase the training efficiency by times in terms of yield.
(2) The training mode is simple, and the training effect is obvious. According to the invention, through the middle-high temperature constraint aging training process, the nickel-titanium alloy has a two-way shape memory effect superior to that of a sample under the traditional repeated deformation process, the recovery rate can reach 98.7%, and the nickel-rich nickel-titanium alloy can be comparable to the nickel-rich nickel-titanium alloy with the similar atomic ratio; meanwhile, the training mode is simple, and the method is particularly suitable for mass production in engineering application.
(3) The method is suitable for scenes above room temperature. The nickel-titanium sample strip with high nickel content has excellent two-way shape memory, and also has R phase transition temperature higher than 25 ℃, namely the temperature corresponding to deformation generated during cooling is higher than room temperature, so that the material meets the loose service condition, and can be widely applied to intelligent devices with the temperature higher than room temperature in working occasions.
(4) The material performance is excellent. Compared with nickel-rich nickel-titanium alloy with near-equal atomic ratio, the nickel-rich nickel-titanium alloy with high nickel-rich content and excellent two-way shape memory effect has the advantage of high strength and can adapt to more complex environment.
Drawings
FIG. 1 is a schematic view of a restraint mold and a sample strip holding state of the present invention.
FIG. 2 is a graph of a thermal processing process of an embodiment of the present invention.
FIG. 3 shows Ni after two-step aging process in an embodiment of the present invention 52 Ti 48 DSC curve of alloy bars.
FIG. 4 shows Ni treated by the two-step aging process in the examples of the present invention 52 Ti 48 And (3) bright field image of the alloy strip by a transmission electron microscope.
FIG. 5 is a graph comparing the hardness of nickel-rich nickel-titanium alloy with near-equiatomic ratio and nickel-rich nickel-titanium alloy after aging for 3h at 400 ℃.
FIG. 6 shows Ni treated by a two-step constrained aging process in an embodiment of the present invention 52 Ti 48 Deformation of the alloy strip at different temperatures.
Description of the reference numerals:
1-semicircular ring fixing sleeve, 2-inner hexagon screw, 3-arc groove and 4-semicircular column base.
Detailed Description
The present invention will be described in further detail below.
A nickel-titanium alloy two-way shape memory effect training method with high nickel-rich content comprises the following steps:
(1) the nickel-titanium alloy (Ni) with high nickel-rich content and the original number quantum ratio of nickel to titanium of 52:48 is prepared by vacuum arc melting 52 Ti 48 Alloy bars) and then using pressureThe molten nitinol was suction cast into a water cooled copper mold to produce nitinol strips with corresponding dimensions of 70mm (length) x 8mm (width) x 1mm (thickness).
(2) Putting the nickel-titanium alloy strip in the step (1) into a quartz tube, and vacuumizing the tube to 5 x 10 by using a molecular pump matched with a vacuum tube sealing machine -3 Pa, filling only protective gas high-purity argon into the tube, and then sealing the alloy strip in the quartz tube.
(3) And (3) placing the sample after the tube sealing into a tube sintering furnace, and carrying out solution treatment at the temperature of 1000 ℃ for 3 hours. And immediately taking out the sample for water quenching after the solid solution is finished.
(4) And (4) thinning the material processed in the step (3) through a stainless steel thinning die to enable the thickness of the sample to reach 0.5 mm.
(5) As shown in fig. 1, all the thinned alloy strips are placed into the arc-shaped groove 3 of a semi-cylindrical base 4 with the radius of 33mm, a semi-circular ring fixing sleeve 1 is placed above the arc-shaped groove, and then the base and the semi-circular ring sleeve are fixed by using an inner hexagonal screw 2, so that the alloy strips are restrained in a die. And (3) putting the mould loaded with the alloy strip into a box-type resistance furnace, performing medium-high temperature constraint aging treatment at the temperature of 450 ℃ for 3 hours, and immediately performing water quenching after the medium-high temperature constraint aging treatment to finish the two-way shape memory effect training of the nickel-titanium alloy with high nickel content.
The shape memory effect of the nickel-titanium alloy sample strip is characterized by using a photographic method, which comprises the following steps: the sample is placed in media with different temperatures, the camera is used for recording the bending state photos of the sample with different temperatures, the automatic CAD software is used for extracting the chord tangent angles of the sample strip at different temperatures (100 ℃ and-196 ℃), and the two-way shape memory recovery rate of the sample in the martensite state is calculated. In the embodiment, after the nickel-titanium sample strip is subjected to the two-step constraint aging, the recovery rate is as high as 98.7 percent and exceeds that of most nickel-rich nickel-titanium alloy samples with nearly equal atomic ratios.
FIG. 3 shows Ni after the two-step aging process in the example 52 Ti 48 DSC curve of the alloy strip, and R phase transition starting temperature R measured by a tangent method s And an end temperature R f Both are above room temperature, 53.6 ℃ and 25.1 ℃ respectively. This illustrates the two-step aging processThe obtained sample completely meets the application of room temperature or above in the working occasion.
FIG. 4 shows Ni treated by the two-step aging process in the examples 52 Ti 48 And (3) a transmission electron microscope bright field image of the alloy strip. As can be seen in fig. 4: ni with preferred orientation is distributed in B2 matrix 4 Ti 3 A phase precipitated. Through statistics of Image-Pro of statistical analysis software, the average size of the precipitated phase is found to be 46.8 +/-8.7 nm, and the size is within the demerged coherent size (300nm) reported in the literature, so that the length, the density and the coherent relation with a matrix of the precipitated phase achieve a good matching relation, an ideal coherent stress field is introduced into the matrix of the precipitated phase, and therefore, a sample shows an excellent two-way shape memory effect macroscopically.
FIG. 5 is a graph comparing the hardness of nickel-rich nickel-titanium alloy with near-equiatomic ratio and nickel-rich nickel-titanium alloy after aging for 3h at 400 ℃. Ni 52 Ti 48 Alloy and Ni 53 Ti 47 The hardness of the alloy is obviously higher than that of Ni 51 Ti 49 The alloy shows that the nickel-titanium alloy with high nickel-rich content has higher mechanical strength compared with the nickel-rich nickel-titanium alloy with the nearly equal atomic ratio.
FIG. 6 shows Ni treated by the two-step constrained aging process in the examples 52 Ti 48 Deformation of the alloy strip at different temperatures. As the temperature is lowered, the alloy strip tends to straighten and then reverse bending occurs at lower temperatures.
The results show that Ni can be obtained by reasonable medium-high temperature constraint aging process 52 Ti 48 The alloy obtains excellent two-way shape memory effect, has a temperature response range above room temperature, and has broad application prospect.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. A nickel-titanium alloy two-way shape memory effect training method with high nickel-rich content is characterized in that: comprises the following steps of (a) carrying out,
(1) repeatedly smelting high-purity titanium sponge and electrolytic nickel blocks by using a vacuum arc smelting furnace to obtain a nickel-titanium alloy ingot with high nickel-rich content; then melting the obtained nickel-titanium alloy ingot with high nickel content again and carrying out suction casting to obtain a nickel-titanium alloy sample strip;
(2) sealing the nickel-titanium alloy strip with high nickel-rich content in a quartz tube filled with inert gas for homogenization treatment, and performing water-cooling quenching after the homogenization treatment is finished; then, carrying out thickness reduction treatment on the sample to obtain a sample strip;
(3) and bending all the sample strips in a semi-cylindrical constraint mould with an arc-shaped groove, carrying out constraint aging treatment on the semi-cylindrical constraint mould loaded with the sample strips at the temperature of 400-500 ℃ for 3-5 h, and immediately carrying out water quenching after the treatment.
2. The nickel-titanium alloy high-nickel-content two-way shape memory effect training method as claimed in claim 1, wherein: the thickness of the sample strip is measured by a vernier caliper, and the thickness of the sample strip is recorded as t according to a formula
Is calculated to obtain, wherein max Is the maximum strain value of the sample strip, 0 < epsilon max Less than or equal to 2 percent; and R is the curvature radius of the arc-shaped groove of the semi-cylindrical constraint mould.
3. The training method for nickel-titanium alloy with high nickel-rich content to have two-way shape memory effect according to claim 1, wherein; in the nickel-titanium alloy strip with high nickel-rich content, the weight ratio of nickel: the titanium atomic ratio is 52-53: 48-47.
4. The training method for nickel-titanium alloy with high nickel-rich content to have two-way shape memory effect according to claim 1, wherein; the temperature of the homogenization treatment is 1000 ℃, and the time of the homogenization treatment is 3 h.
5. The training method for nickel-titanium alloy with high nickel-rich content to have two-way shape memory effect according to claim 1, wherein; the thickness of the sample strip is 0.4-0.5 mm.
6. The training method for nickel-titanium alloy with high nickel-rich content to have two-way shape memory effect according to claim 1, wherein; the inert gas is argon.
7. The training method for nickel-titanium alloy with high nickel-rich content to have two-way shape memory effect according to claim 1, wherein; the curvature radius of the arc-shaped groove of the semi-cylindrical constraint mould is 33 mm.
8. The training method for nickel-titanium alloy with high nickel-rich content to have two-way shape memory effect according to claim 1, wherein; the nickel-titanium alloy strip with high nickel-rich content is prepared by a rapid solidification process.
9. The training method of nickel-titanium alloy with high nickel-rich content for two-way shape memory effect as claimed in claim 8, wherein; the rapid solidification process is characterized in that after vacuum arc melting, molten alloy is suction cast into a water-cooled oxygen-free copper mold; the corresponding dimension of the alloy strip is 50-100 mm multiplied by 8-10 mm multiplied by 0.5-1.5 mm.
10. The training method for nickel-titanium alloy with high nickel-rich content to have two-way shape memory effect according to claim 1, wherein; the thinning treatment uses a steel mould, the inner surface of the mould is ensured to be flat, the contact with the surface of a sample is good when the mould is adhered, the sample level is kept in the thinning process, and the thickness of the sample is controlled to be 0.4-0.5 mm.
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Cited By (2)
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| CN116516270A (en) * | 2023-04-03 | 2023-08-01 | 华南理工大学 | Two-step training method for efficiently improving nickel-titanium alloy double-pass shape memory effect |
| CN117802357A (en) * | 2024-01-02 | 2024-04-02 | 武汉科技大学 | Nickel-titanium alloy with four-way shape memory effect, preparation method, application and component |
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| CN111534770A (en) * | 2020-05-12 | 2020-08-14 | 华南理工大学 | Near-equal atomic ratio nickel-rich nickel-titanium alloy two-way shape memory effect training method |
| CN111957966A (en) * | 2020-08-28 | 2020-11-20 | 东南大学 | Method for preparing nickel-titanium two-way memory deformation component and intelligent structure through 4D printing |
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| CN116516270A (en) * | 2023-04-03 | 2023-08-01 | 华南理工大学 | Two-step training method for efficiently improving nickel-titanium alloy double-pass shape memory effect |
| CN117802357A (en) * | 2024-01-02 | 2024-04-02 | 武汉科技大学 | Nickel-titanium alloy with four-way shape memory effect, preparation method, application and component |
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