CN113308656B - Post-treatment method for additive manufacturing of super-elastic nickel-titanium alloy and application thereof - Google Patents
Post-treatment method for additive manufacturing of super-elastic nickel-titanium alloy and application thereof Download PDFInfo
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Abstract
The invention provides a post-treatment method for preparing a super-elastic nickel-titanium alloy by nickel additive manufacturing and application thereof, wherein the method comprises the steps of carrying out heat treatment on a nickel-titanium alloy piece, wherein the heat treatment temperature is 150-350 ℃, and the heat treatment time is 0.1-72 h; the nickel-titanium alloy part is processed by a selective laser melting method, and in the nickel-titanium alloy part, the atomic percent of nickel element is 50.2-52%, and the balance is titanium element. The method can realize that the nickel-titanium alloy piece simultaneously considers high damping performance and super-elastic performance under a wide temperature range, and widens the application range of the nickel-titanium alloy piece.
Description
Technical Field
The invention relates to a post-processing method of an alloy part, in particular to a post-processing method of a super-elastic nickel-titanium alloy manufactured by additive manufacturing and application thereof, and belongs to the technical field of alloys.
Background
The nickel-titanium alloy has a specific shape memory function, high damping, superelasticity and good biocompatibility, and has been applied to the fields of aerospace, medical treatment, machinery and the like. But the method is limited by the poor machining and welding performance of the NiTi alloy, and the NiTi alloy part with a complex structure is difficult to manufacture by adopting the traditional metallurgical process, so that the popularization and the application of the NiTi alloy part are limited. In recent years, Selective Laser Melting (SLM) technology has received much attention and research to form nitinol parts.
The damping mechanism of the titanium-nickel alloy is derived from martensite phase transformation, and energy can be absorbed by the hysteretic elastic migration of the interface by generating rich phase interfaces and substructure interfaces (twin planes and variant interfaces) in the martensite phase, so that the titanium-nickel alloy has good damping performance. Particularly, the damping coefficient (expressed by loss tangent tan delta) is the highest and can reach 10 in the process of martensite transformation-1Orders of magnitude. However, the martensitic transformation temperature range of the titanium-nickel alloy is generally narrow (about 30 ℃ variation range), and is difficult to apply in a wide temperature range. Meanwhile, the damping measured in the phase change process comprises a very high proportion of instantaneous damping, namely the damping performance is not high when the temperature fluctuation does not exist in the application environment. Therefore, even though a nickel titanium alloy piece having a complicated structure can be obtained by the SLM technique, its damping performance in a wide temperature range is generally only in its martensitic state, and thus the tan δ value is generally less than 0.03.
In addition, the research shows that the super-elastic performance of the SLM forming titanium-nickel alloy part is obviously lower than that of the NiTi alloy part prepared by the traditional method.
Therefore, how to obtain a titanium-nickel alloy part with both high damping performance and super-elastic performance under a wide temperature range is a technical problem to be solved in the field.
Disclosure of Invention
The invention provides a post-treatment method for additive manufacturing of a super-elastic nickel-titanium alloy, which can realize that a nickel-titanium alloy piece has both high damping performance and super-elastic performance under a wide temperature range, broadens the application range of the nickel-titanium alloy piece and further exerts the advantages of the nickel-titanium alloy material.
The invention also provides a high-damping super-elastic nickel-titanium alloy part which not only has super-elastic performance, but also has excellent damping performance in a wide temperature range, and meets the requirements of high-efficiency and stable operation of high-precision instruments in the fields of aerospace, medical treatment and the like at the present stage.
The invention also provides an application of the high-damping superelastic nickel-titanium alloy part.
The invention provides a post-treatment method for additive manufacturing of super-elastic nickel-titanium alloy, which comprises the following steps of carrying out heat treatment on a nickel-titanium alloy piece, wherein the heat treatment temperature is 150-350 ℃, and the heat treatment time is 0.1-72 h;
the nickel-titanium alloy part is processed by a selective laser melting technology, and in the nickel-titanium alloy part, the atomic percent of nickel element is 50.2-52%, and the balance is titanium element.
The post-treatment method as described above, wherein the time of the heat treatment is 5 to 72 hours.
The post-treatment method comprises the steps of performing heat treatment at the temperature of 210-280 ℃ for 20-30 h.
The post-treatment method as described above, wherein before the heat treatment, the method further comprises pre-treating the nitinol piece;
the temperature of the pretreatment is 650-780 ℃.
The post-treatment method as described above, wherein the time of the pre-treatment is 0.5 to 24 hours.
The post-treatment method as described above, wherein the time of the heat treatment is 0.1 to 48 hours.
The post-treatment method comprises the steps of, wherein the temperature of the pretreatment is 680-780 ℃, and the time of the pretreatment is 0.5-4.5 h; the temperature of the heat treatment is 210-280 ℃, and the time of the heat treatment is 20-30 h.
The post-treatment method as described above, wherein the nickel-titanium alloy member contains 50.2 to 51.5 atomic% of nickel element and the balance of titanium element.
The invention also provides a high-damping super-elastic nickel-titanium alloy part, which is obtained by the post-treatment method of any one of the parts.
The invention also provides application of the high-damping superelastic nickel-titanium alloy part in the aerospace field and the medical field.
The post-treatment method for the additive manufacturing of the superelastic nickel-titanium alloy takes a nickel-titanium alloy piece processed by a selective laser melting method as an object, limits the composition and post-treatment parameters of the nickel-titanium alloy piece, not only enables the nickel-titanium alloy piece to be overlapped in a wide temperature range to form R phase transformation and B19 'martensite phase transformation, greatly widens the coexistence temperature of an alloy B2 parent phase, an R phase and a B19' martensite phase, but also can form a nanoscale nickel atom segregation region in the nickel-titanium alloy piece to improve the yield strength of the parent phase, so that the nickel-titanium alloy piece obtained by post-treatment can have both high damping performance and superelasticity performance in the wide temperature range.
The high-damping superelastic nickel-titanium alloy part is obtained by adopting SLM forming, so that the high-damping superelastic nickel-titanium alloy part has the characteristics of high geometric complexity and high precision; in addition, the high damping performance and the super-elastic performance under a wide temperature range are considered. Therefore, the high-damping superelastic nickel-titanium alloy part can be used in the aerospace field and the medical field, and particularly can be used as a part in a high-precision instrument, so that the long-term stable and efficient operation of the high-precision instrument is ensured.
Drawings
FIG. 1 is a comparison of DSC curves of high damping Nitinol articles according to examples 1 and 6 of the present invention and Nitinol article according to comparative example 5;
FIG. 2 is an XRD pattern of a highly damped superelastic nickel-titanium alloy part according to example 6 of the present invention;
FIG. 3 is an XRD integral curve of a high damping superelastic nickel-titanium alloy part according to example 6 of the present invention;
FIG. 4 is a DMA curve of example 6 of the present invention;
FIG. 5 is a high angle annular dark field image of a high damping nitinol part of example 11 according to the present invention;
FIG. 6 is a line scan quantitative analysis of the EDS energy spectrum at the white line in FIG. 5;
FIG. 7a is a tensile stress-strain curve of an untreated nickel titanium alloy part of example 11 of the present invention;
FIG. 7b is a tensile stress-strain curve of a high damping superelastic nickel-titanium alloy article according to example 11 of the present invention;
FIG. 8a is a graph of compressive stress versus strain for a nickel titanium alloy part without post-treatment according to example 11 of the present invention;
FIG. 8b is a graph of compressive stress-strain curves for a high damping Nitinol article according to example 11 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a post-treatment method for additive manufacturing of a super-elastic nickel-titanium alloy, which comprises the following steps of carrying out heat treatment on a nickel-titanium alloy piece, wherein the heat treatment temperature is 150-350 ℃, and the heat treatment time is 0.1-72 h;
the nickel-titanium alloy part is processed by a selective laser melting method, and in the nickel-titanium alloy part, the atomic percent of nickel element is 50.2-52%, and the balance is titanium element.
The nickel-titanium alloy part is subjected to post-treatment, specifically, the nickel-titanium alloy part is obtained by processing and forming nickel-titanium alloy powder through a Selective Laser Melting (SLM), so that the nickel-titanium alloy part has the characteristics of high precision and complex structure. Moreover, the nickel-titanium alloy piece obtained by SLM forming has no obvious cracks and air holes inside, and the compactness is more than 99%, so that the mechanical property is excellent.
The inventors have also found that when the nickel-titanium alloy piece consisting of 50.2 to 52 atomic% of nickel and the balance of titanium is subjected to the above post-treatment, the microstructure of the nickel-titanium alloy piece of the composition can be effectively improved. Specifically, R phase transformation and B19 'martensite phase transformation in a wide temperature range can be introduced into the nickel-titanium alloy piece, so that a B2 parent phase, an R phase and a B19' martensite phase can coexist in a wide temperature range, and finally, the damping performance of tan delta not less than 0.08 is achieved.
In addition, the SLM-formed nickel-titanium alloy piece has coarse grains, and the grain size is between several microns and tens of microns, so that the yield strength of the parent phase of the alloy is low, dislocation slip is easy to occur in the stress-induced martensite phase transformation process, irreversible plastic deformation is introduced, and the superelasticity is deteriorated. The super-elastic performance of the nickel-titanium alloy piece formed by SLM is obviously improved after the nickel-titanium alloy piece is subjected to the specific heat treatment of the invention. Specifically, a uniformly dispersed nanoscale nickel atom segregation zone is formed in the nickel-titanium alloy part, the nickel atom segregation zone is small in size, large in quantity and uniform in dispersion, dislocation slippage can be effectively inhibited, the yield strength of a parent phase of the nickel-titanium alloy part is improved, stress-induced martensite phase transformation of the nickel-titanium alloy part cannot be obviously inhibited, and therefore the super-elastic performance of the nickel-titanium alloy part is improved. It is emphasized here that the superelastic properties of the present invention include tensile superelastic and compressive superelastic.
The present invention is not limited to the specific operation of performing the heat treatment as long as the time and parameters of the heat treatment satisfy the limitations of the present invention. In one embodiment, the heat treatment operation described above may be performed using a muffle furnace.
The post-treatment method is simple and convenient to operate, and the nickel-titanium alloy piece processed and formed by the SLM can have excellent high damping performance in a wide temperature range only by carrying out heat treatment on the nickel-titanium alloy piece, and meanwhile, the superelasticity performance of the nickel-titanium alloy piece is obviously improved.
To further promote the positive effect of heat treatment on the microstructure of the nitinol part, the tan δ of the nitinol part is further increased and the superelastic stress decay and residual strain of the nitinol part are further reduced when the heat treatment is carried out for a period of 5-72 hours.
In a specific embodiment, when the temperature of the heat treatment is 210-280 ℃ and the time of the heat treatment is 20-30h, the damping performance and the superelastic performance of the nickel-titanium alloy part are more excellent. Preferably, the temperature of the heat treatment is 250 ℃ and the time of the heat treatment is 24 h.
Further, the inventors have found that pre-treating the nitinol piece prior to heat treatment can further improve the damping and superelastic properties of the nitinol piece. Wherein the temperature of the pretreatment is 650-780 ℃. The inventors speculate that the combination of pretreatment and heat treatment may further broaden the coexisting temperature ranges of the B2 parent phase, R phase, and B19' martensite phase, and further reduce the size of the nickel atom segregation zone to coherent combination with the nickel titanium alloy matrix. Namely, the pretreatment is beneficial to enhancing the treatment effect of subsequent heat treatment, and the damping performance and the superelasticity performance of the nickel-titanium alloy part are further improved. Further, the pretreatment time is 0.5-24 h.
When the step of pre-treatment is performed before the heat treatment, the time for the heat treatment can be shortened, for example, from 0.1 to 48 hours.
It will be appreciated that when the parameters of the pretreatment and heat treatment are adjusted within the above ranges, the damping and superelastic properties of the resulting nickel-titanium alloy part will be affected to varying degrees. Thus, in general, in one specific embodiment, the post-treatment of the nitinol part comprises a pretreatment and a heat treatment in this order, wherein the temperature of the pretreatment is 680-780 ℃ and the time of the pretreatment is 0.5-4.5 h; the heat treatment temperature is 210-280 ℃, and the heat treatment time is 20-30h, so that the damping performance and the superelasticity performance of the processed nickel-titanium alloy part can be basically ensured to be in a more satisfactory state. Preferably, the temperature of the pretreatment is 700 ℃, and the time of the pretreatment is 4.5 h; the heat treatment temperature is 250 ℃, and the heat treatment time is 24 h. Particularly, when the atomic percent of nickel element in the nickel-titanium alloy part is 50.2-51.5%, and the balance is titanium element, the treatment effect of pretreatment and heat treatment on the nickel-titanium alloy part can be further exerted, and particularly the effect of improving the super-elastic property is more remarkable.
The invention also provides a high-damping superelastic titanium alloy part, which is obtained according to any one of the post-treatment methods. The high-damping super-elastic titanium alloy part has excellent damping performance and super-elastic performance.
In one embodiment, the high-damping super-elastic titanium alloy part has high damping performance with tan delta being more than or equal to 0.08 in a wide temperature range of-100-30 ℃ (temperature range window exceeding 120 ℃); furthermore, the maximum superelastic strain in compression mode is up to 7% and the superelastic strain in tension mode exceeds 5%. Meanwhile, the high-damping superelastic titanium alloy part has high superelastic cycle stability, and after 10 times of 6% stretching and unloading cycles, the superelastic strain attenuation of the high-damping superelastic titanium alloy part is less than 0.5%, and the residual strain is less than 1%.
The invention also provides application of the high-damping superelastic nickel-titanium alloy part in the aerospace field and the medical field. The high-damping superelastic nickel-titanium alloy part can be used as a spare part in a high-precision instrument, and long-term stable and efficient operation of the high-precision instrument is guaranteed.
The following describes in detail the post-treatment method for additive manufacturing of the super elastic nickel titanium alloy and the high damping super elastic nickel titanium alloy part according to the present invention with specific embodiments.
Example 1
And (3) carrying out heat treatment on the nickel-titanium alloy piece (the content of nickel atoms is 50.6 at.%, and the balance is titanium atoms) obtained by SLM processing and molding at 350 ℃, wherein the heat treatment time is 1h, and thus the high-damping superelastic nickel-titanium alloy piece is obtained.
Example 2
And (3) carrying out heat treatment on the nickel-titanium alloy piece (the content of nickel atoms is 50.6 at.%, and the balance is titanium atoms) obtained by SLM processing and molding at 200 ℃, wherein the heat treatment time is 48h, and thus the high-damping super-elastic nickel-titanium alloy piece is obtained.
Example 3
And (3) carrying out heat treatment on the nickel-titanium alloy piece (the content of nickel atoms is 50.6 at.%, and the balance is titanium atoms) obtained by SLM processing and molding at 250 ℃ for 24h to obtain the high-damping super-elastic nickel-titanium alloy piece.
Example 4
The post-treatment method of the nickel-titanium alloy part comprises the following steps:
1) pretreating a nickel-titanium alloy piece (the content of nickel atoms is 50.6 at.%, and the balance is titanium atoms) obtained by SLM processing and molding at 700 ℃, wherein the pretreatment time is 2 h;
2) and (3) carrying out heat treatment on the pretreated nickel-titanium alloy piece at the temperature of 250 ℃ for 24 hours to obtain the high-damping super-elastic nickel-titanium alloy piece.
Example 5
And (3) carrying out heat treatment on the nickel-titanium alloy piece (the content of nickel atoms is 51.2 at.%, and the balance is titanium atoms) obtained by SLM processing and molding at 250 ℃ for 24h to obtain the high-damping super-elastic nickel-titanium alloy piece.
Example 6
The post-treatment method of the nickel-titanium alloy part comprises the following steps:
1) pretreating a nickel-titanium alloy piece (the content of nickel atoms is 50.6 at.%, and the balance is titanium atoms) obtained by SLM processing and molding at 700 ℃, wherein the pretreatment time is 4.5 h;
2) and (3) carrying out heat treatment on the pretreated nickel-titanium alloy piece, wherein the heat treatment temperature is 250 ℃, and the heat treatment time is 24 hours, so as to obtain the high-damping superelastic nickel-titanium alloy piece.
Example 7
The post-treatment method of the nickel-titanium alloy part comprises the following steps:
1) pretreating a nickel-titanium alloy piece (the content of nickel atoms is 50.6 at.%, and the balance is titanium atoms) obtained by SLM (selective laser melting) at 680 ℃ for 4.5 h;
2) and (3) carrying out heat treatment on the pretreated nickel-titanium alloy piece, wherein the heat treatment temperature is 250 ℃, and the heat treatment time is 24 hours, so as to obtain the high-damping superelastic nickel-titanium alloy piece.
Example 8
The post-treatment method of the nickel-titanium alloy part comprises the following steps:
1) pretreating a nickel-titanium alloy piece (the content of nickel atoms is 50.6 at.%, and the balance is titanium atoms) obtained by SLM processing and molding at 780 ℃ for 4.5 h;
2) and (3) carrying out heat treatment on the pretreated nickel-titanium alloy piece, wherein the heat treatment temperature is 250 ℃, and the heat treatment time is 24 hours, so as to obtain the high-damping superelastic nickel-titanium alloy piece.
Example 9
The post-treatment method of the nickel-titanium alloy part comprises the following steps:
1) pretreating a nickel-titanium alloy piece (the content of nickel atoms is 50.6 at.%, and the balance is titanium atoms) obtained by SLM processing and molding at 700 ℃, wherein the pretreatment time is 4.5 h;
2) and (3) carrying out heat treatment on the pretreated nickel-titanium alloy piece, wherein the heat treatment temperature is 350 ℃, and the heat treatment time is 1h, so as to obtain the high-damping superelastic nickel-titanium alloy piece.
Example 10
The post-treatment method of the nickel-titanium alloy part comprises the following steps:
1) pretreating a nickel-titanium alloy piece (the content of nickel atoms is 50.6 at.%, and the balance is titanium atoms) obtained by SLM processing and molding at 700 ℃, wherein the pretreatment time is 0.5 h;
2) and (3) carrying out heat treatment on the pretreated nickel-titanium alloy piece, wherein the heat treatment temperature is 250 ℃, and the heat treatment time is 24 hours, so as to obtain the high-damping superelastic nickel-titanium alloy piece.
Example 11
The post-treatment method of the nickel-titanium alloy part comprises the following steps:
1) pretreating a nickel-titanium alloy piece (the content of nickel atoms is 50.6 at.%, and the balance is titanium atoms) obtained by SLM processing and molding at 700 ℃, wherein the pretreatment time is 1 h;
2) and (3) carrying out heat treatment on the pretreated nickel-titanium alloy piece, wherein the heat treatment temperature is 250 ℃, and the heat treatment time is 24 hours, so as to obtain the high-damping superelastic nickel-titanium alloy piece.
Example 12
The post-treatment method of the nickel-titanium alloy part comprises the following steps:
1) pretreating a nickel-titanium alloy piece (the content of nickel atoms is 51.2 at.%, and the balance is titanium atoms) obtained by SLM processing and molding at 700 ℃, wherein the pretreatment time is 4.5 h;
2) and (3) carrying out heat treatment on the pretreated nickel-titanium alloy piece, wherein the heat treatment temperature is 250 ℃, and the heat treatment time is 24 hours, so as to obtain the high-damping superelastic nickel-titanium alloy piece.
Example 13
The post-treatment method of the nickel-titanium alloy part comprises the following steps:
1) pretreating a nickel-titanium alloy piece (the content of nickel atoms is 51.6 at.%, and the balance is titanium atoms) obtained by SLM processing and molding at 700 ℃, wherein the pretreatment time is 4.5 h;
2) and (3) carrying out heat treatment on the pretreated nickel-titanium alloy piece, wherein the heat treatment temperature is 250 ℃, and the heat treatment time is 24 hours, so as to obtain the high-damping superelastic nickel-titanium alloy piece.
Example 14
The post-treatment method of the nickel-titanium alloy part comprises the following steps:
1) pretreating a nickel-titanium alloy piece (the content of nickel atoms is 51.8 at.%, and the balance is titanium atoms) obtained by SLM processing and molding at 700 ℃, wherein the pretreatment time is 4.5 h;
2) and (3) carrying out heat treatment on the pretreated nickel-titanium alloy piece, wherein the heat treatment temperature is 250 ℃, and the heat treatment time is 24 hours, so as to obtain the high-damping superelastic nickel-titanium alloy piece.
Example 15
The post-treatment method of the nickel-titanium alloy part comprises the following steps:
and (3) carrying out heat treatment on the nickel-titanium alloy piece (the content of nickel atoms is 51.6 at.%, and the balance is titanium atoms) obtained by SLM processing and molding at 250 ℃ for 24h to obtain the high-damping super-elastic nickel-titanium alloy piece.
Comparative example 1
And (3) carrying out heat treatment on the nickel-titanium alloy piece (the content of nickel atoms is 50.6 at.%, and the balance is titanium atoms) obtained by SLM processing and molding at 500 ℃, wherein the heat treatment time is 1h, and thus the treated nickel-titanium alloy piece is obtained.
Comparative example 2
And (3) carrying out heat treatment on the nickel-titanium alloy piece (the content of nickel atoms is 50.0 at.%, and the balance is titanium atoms) obtained by SLM processing and molding at 350 ℃, wherein the heat treatment time is 1h, and thus the treated nickel-titanium alloy piece is obtained.
Comparative example 3
And (3) carrying out heat treatment on the nickel-titanium alloy piece (the content of nickel atoms is 50.0 at.%, and the balance is titanium atoms) obtained by SLM processing and molding at 500 ℃, wherein the heat treatment time is 1h, and thus the treated nickel-titanium alloy piece is obtained.
Comparative example 4
1) Pretreating a nickel-titanium alloy piece (the content of nickel atoms is 50.6 at.%, and the balance is titanium atoms) obtained by SLM processing and molding at 700 ℃, wherein the pretreatment time is 4.5 h;
2) and (3) carrying out heat treatment on the nickel-titanium alloy piece (the content of nickel atoms is 50.6 at.%, and the balance is titanium atoms) obtained by SLM processing and molding at 500 ℃, wherein the heat treatment time is 1h, and thus the treated nickel-titanium alloy piece is obtained.
Comparative example 5
The post-treatment method of the nickel-titanium alloy part comprises the following steps:
and (3) carrying out heat treatment on the nickel-titanium alloy piece (the content of nickel atoms is 50.6 at.%, and the balance is titanium atoms) obtained by SLM (selective laser melting) at 700 ℃, wherein the heat treatment time is 4.5h, and thus the treated nickel-titanium alloy piece is obtained.
Comparative example 6
And (4) performing SLM (selective laser melting) machining forming without any post-treatment to obtain the nickel-titanium alloy piece.
In the above examples and comparative examples, the SLM processing parameters of the nitinol pieces obtained by SLM processing and forming were completely the same.
The following tests were carried out on the high damping superelastic nickel titanium alloy pieces of the above examples and the nickel titanium alloy pieces of the comparative examples.
1. Differential scanning calorimetry detection
FIG. 1 is a DSC curve comparison of high damping Nitinol articles of examples 1 and 6 of the present invention and Nitinol articles of comparative example 5.
As can be seen from fig. 1: in the cooling process of the high damping super elastic nickel titanium alloy pieces in the examples 1 and 6, obvious R phase transformation occurs, the temperature range of B19' martensite phase transformation is seriously widened, and the DSC curve is obviously different from that of the comparative example 5. Therefore, the heat treatment method of the present invention can effectively widen the coexistence temperature range of the B2 parent phase, the R phase, and the B19' martensite phase.
2. X-ray diffraction analysis
FIG. 2 is an XRD pattern of a highly damped superelastic nickel-titanium alloy article according to example 6 of the present invention. FIG. 3 is an XRD integral curve of the high damping superelastic nickel-titanium alloy article of example 6 of the present invention.
As shown in fig. 2 and 3, the phase transformation process of the SLM-formed ni-ti alloy piece after post-treatment was monitored in situ by synchrotron radiation high-energy XRD. The results show that the samples underwent R-phase transformation (Rs 36 ℃, Rf-39 ℃) and B19 'phase transformation (Ms 3 ℃, Mf-163 ℃) at 60 ℃ to-180 ℃, and the phase transformation temperature range windows were 75 ℃ and 166 ℃, respectively (the temperature range windows for the R-phase transformation and B19' phase transformation of the titanium-nickel alloy part without post-treatment were-15 ℃ and-25 ℃, respectively). As is evident from the fact that Ms is significantly higher than Rf, the B2 → B19 'or R → B19' phase transition has begun to occur before the B2 → R phase transition is completed; from the phenomenon that when the temperature is lower than Rf, the reduction speed of the diffraction peak intensity of the R phase is higher than the increase speed of the diffraction peak intensity of the B19 'phase, when the temperature is reduced to Rf, the B2 phase is not completely converted into the R phase, and the residual B2 phase undergoes the phase change of B2 → B19' in the process of continuously reducing the temperature; as a result, when the temperature was lowered to-180 ℃, the diffraction peak of the R phase did not disappear, and the R phase did not completely transform into the B19' phase even at-180 ℃. In summary, the post-treatment method of the present invention can significantly widen the temperature range of the thermally induced phase transition, and different phase transitions can be performed in an overlapping manner within the same wide temperature range, so that the B2 and R, B19' phases coexist for a long time.
3. Dynamic thermomechanical analysis
Wherein, the ring temperature interval and the temperature rise and fall rate are as follows: and circularly heating and cooling at the speed of 5 ℃/min under the condition of-150 to 100 ℃. The clamp type is a film stretching clamp, the pre-stress interval is 0.01N, the dynamic force tracking is 125%, the amplitude range is 15-25 μm, the frequency is 0.4, 1, 4, 10 and 20Hz respectively, and the holding time is 5 min.
FIG. 4 is a DMA curve of example 6 of the present invention. As can be seen from FIG. 4, the nickel-titanium alloy part treated by the post-treatment method of the present invention has a high damping plateau of approximately 0.14 at-130 ℃ to 10 ℃.
4. EDS energy spectrum detection
Fig. 5 is a high angle annular dark field image of a high damping nitinol part according to example 11 of the present invention. FIG. 6 is a line scan quantitative analysis of the EDS energy spectrum at the white line in FIG. 5. In FIG. 5, the bright regions are nickel atom segregation regions.
As shown in FIG. 5, the high damping superelastic nickel-titanium alloy part of example 11 has homogeneously dispersed nanometer nickel atom segregation areas formed inside. As shown by the energy spectrum line scanning of FIG. 6, the nickel atom enrichment region in the material has a diameter of about 5nm and an interval of about 3nm, and the nickel element content in the enrichment region is about 53 percent.
5. Compression, tension detection
FIG. 7a is a tensile stress-strain curve of a nickel titanium alloy part without post-treatment according to example 11 of the present invention, and FIG. 7b is a tensile stress-strain curve of a high damping superelastic nickel titanium alloy part according to example 11 of the present invention. As shown in fig. 7a and 7b, the tensile superelasticity of the high-damping superelastic nickel-titanium alloy part after the post-treatment of the invention is obviously improved, and the high-damping superelastic nickel-titanium alloy part has good superelastic cycle stability. Wherein the tensile superelastic strain reaches 5.5 percent and is far higher than the reported maximum tensile superelastic strain (< 3 percent) of the nickel-titanium alloy piece formed by SLM; the super elastic stress attenuation after 10 times of 6% stretching and unloading cycles is not more than 60MPa and is far lower than that of a nickel-titanium alloy piece (143 MPa) which is not post-treated; the residual strain after 10 cycles of stretch-add-unload was less than 0.5% and much lower than the untreated nitinol piece (-2.05%).
FIG. 8a is a graph of compressive stress vs. strain for a nickel titanium alloy part without post-treatment according to example 11 of the present invention, and FIG. 8b is a graph of compressive stress vs. strain for a high damping superelastic nickel titanium alloy part according to example 11 of the present invention. In fig. 8a and 8b, the compressibility is 4%, 6%, 8%, 10%, 12% and compression to fracture, respectively. As shown in fig. 8a and 8b, the compressive superelastic performance of the high damping nitinol piece of example 11 was significantly improved, with a residual strain after 12% compressive strain unloading of only 3%, significantly less than 7.2% of the un-post treated nitinol piece.
6. Detection of related parameters
The relevant parameters of the above examples and comparative examples were examined and the results are shown in table 1.
TABLE 1
From table 1, it can be seen that: the post-treatment method for additive manufacturing of the super-elastic nickel-titanium alloy not only can realize the super-elastic performance of the nickel-titanium alloy piece, but also has high damping performance in a wide temperature range.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (7)
1. A post-treatment method for additive manufacturing of super-elastic nickel-titanium alloy is characterized by comprising the steps of carrying out heat treatment on a nickel-titanium alloy piece, wherein the heat treatment temperature is 150-350 ℃, and the heat treatment time is 5-72 h;
before the heat treatment, the method also comprises the step of pretreating the nickel-titanium alloy piece; the temperature of the pretreatment is 650-780 ℃;
the nickel-titanium alloy part is processed by a selective laser melting method, and in the nickel-titanium alloy part, the atomic percent of nickel element is 50.2-52%, and the balance is titanium element.
2. The post-treatment method as claimed in claim 1, wherein the temperature of the heat treatment is 210-280 ℃, and the time of the heat treatment is 20-30 h.
3. The post-treatment process according to claim 1, characterized in that the pre-treatment time is comprised between 0.5 and 24 h.
4. The post-treatment method as claimed in claim 1, wherein the temperature of the pre-treatment is 680-780 ℃, and the time of the pre-treatment is 0.5-4.5 h; the temperature of the heat treatment is 210-280 ℃, and the time of the heat treatment is 20-30 h.
5. The method of any of claims 1 to 4, wherein the nickel-titanium alloy part comprises 50.2 to 51.5 atomic percent nickel, and the balance titanium.
6. A high damping superelastic nickel-titanium alloy part, wherein said high damping superelastic nickel-titanium alloy part is obtained according to the post-treatment method of any one of claims 1-5.
7. The high damping super elastic nickel titanium alloy part of claim 6 for use in aerospace and medical fields.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1780924A (en) * | 2003-05-01 | 2006-05-31 | Ati资产公司 | Methods of processing nickel-titanium shape memory alloys |
| EP2952276A1 (en) * | 2014-06-03 | 2015-12-09 | Airbus Defence and Space GmbH | Method for the heat treatment of a workpiece made from a nickel based alloy |
| CN107475652A (en) * | 2017-08-22 | 2017-12-15 | 哈尔滨工程大学 | In a kind of regulation and control TiNi base memorial alloys there is the method in section in R phases |
| CN110508815A (en) * | 2019-10-09 | 2019-11-29 | 山东大学 | A method of niti-shaped memorial alloy phase transition temperature is regulated and controled based on increasing material manufacturing |
| CN111945089A (en) * | 2020-07-15 | 2020-11-17 | 佛山市逸合生物科技有限公司 | Additive manufacturing titanium part and heat treatment process thereof |
| 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 |
-
2021
- 2021-05-28 CN CN202110590562.6A patent/CN113308656B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1780924A (en) * | 2003-05-01 | 2006-05-31 | Ati资产公司 | Methods of processing nickel-titanium shape memory alloys |
| EP2952276A1 (en) * | 2014-06-03 | 2015-12-09 | Airbus Defence and Space GmbH | Method for the heat treatment of a workpiece made from a nickel based alloy |
| CN107475652A (en) * | 2017-08-22 | 2017-12-15 | 哈尔滨工程大学 | In a kind of regulation and control TiNi base memorial alloys there is the method in section in R phases |
| CN110508815A (en) * | 2019-10-09 | 2019-11-29 | 山东大学 | A method of niti-shaped memorial alloy phase transition temperature is regulated and controled based on increasing material manufacturing |
| CN111945089A (en) * | 2020-07-15 | 2020-11-17 | 佛山市逸合生物科技有限公司 | Additive manufacturing titanium part and heat treatment process thereof |
| 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 |
Non-Patent Citations (3)
| Title |
|---|
| 4D 打印技术的现状与未来;宋波 等;《电加工与模具》;20181220;P1-8 * |
| Texture, aging, and superelasticity of selective laser melting fabricated Nirich NiTi alloys;Soheil Saedi et al.;《Materials Science & Engineering A》;20170104;P1-10 * |
| The influence of heat treatment on the thermomechanical response of Ni-rich NiTi alloys manufactured by selective laser melting;Soheil Saedi et al.;《Journal of Alloys and Compounds》;20160324;P204-210 * |
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