Simultaneous enhancement of mechanical and shape memory properties by heat-treatment homogenization of Ti2Ni precipitates in TiNi shape memory alloy fabricated by selective laser melting

doi:10.1016/j.jmst.2021.06.019

Abstract

Abstract:

The excellent shape memory and mechanical properties of TiNi shape memory alloys (SMAs) fabricated using selective laser melting (SLM) are highly desirable for a wide range of critical applications. In this study, we examined the simultaneous enhancement of mechanical and shape memory properties using heat-treatment homogenization of Ti₂Ni precipitates in a Ti_50.6Ni_49.4 SMA fabricated using SLM. Specifically, because of the complete solution treatment, nanoscale spherical Ti₂Ni precipitates were homogeneously dispersed throughout the grain interior. Interestingly, the resultant SMA exhibited an ultrahigh tensile strength of 880 ± 13 MPa, a large elongation of 22.4 ± 0.4%, and an excellent shape memory effect, with a recovery rate of > 98% and ultrahigh recoverable strain of 5.32% after ten loading-unloading cycles. These simultaneously enhanced properties are considerably superior than those of most previously reported TiNi SMAs fabricated using additive manufacturing. Fundamentally, the enhancement in tensile strength is ascribed to precipitation strengthening and work hardening, and the large plasticity is mainly attributed to the homogeneous nanoscale globular Ti₂Ni precipitates, which effectively impeded the rapid propagation of microcracks. Furthermore, the enhanced shape memory properties are derived from the suppression of dislocation movement and formation of retained stabilized martensite by the presence of high-density dislocations, nanoscale Ti₂Ni precipitates, and abundant interfaces. The obtained results provide insight into the enhancement of the two types of properties in TiNi SMAs and will accelerate the wider application of SMAs.

Key words: Shape memory alloy, Selective laser melting, Heat treatment, Mechanical properties, Shape memory properties

H.Z. Lu, L.H. Liu, , X. Luo, C.H. Song, Z. Wang, J. Wang, Y.D. Su, Y.F. Ding, L.C. Zhang, Y.Y. Li. Simultaneous enhancement of mechanical and shape memory properties by heat-treatment homogenization of Ti₂Ni precipitates in TiNi shape memory alloy fabricated by selective laser melting[J]. J. Mater. Sci. Technol., 2022, 101: 205-216.

Figures/Tables 13

Fig. 1. (a) TiNi binary phase diagram and three heat treatment modes; (b) XRD patterns and change in the phase volume fraction of martensite and austenite of the as-SLMed and heat-treated TiNi SMAs.

Fig. 2. (a-c) SEM images and (d-f) proportion distribution histograms of the Ti2Ni phase for the as-SLMed (a and d) and heat-treated (SISA-800 (b and e) and SCSA-1000 (c and f)) TiNi SMAs. The insets in Fig. 2(d-f) show the corresponding size distributions and densities of the Ti2Ni phase.

Fig. 3. TEM microstructural images of sample SCSA-1000: (a) homogeneous distribution of Ti2Ni precipitates in the matrix, (b) high-density dislocations around Ti2Ni precipitates for the circular area in (a), (c) corresponding SAED patterns for the circular area in (b), and (d) high-resolution TEM image of the interface between Ti2Ni and B2 for the circular area in (b).

Fig. 4. TEM microstructural images of sample SCSA-1000: (a) homogeneous distribution of Ti2Ni precipitates around B19′ nanotwins, (b) SAED pattern for the circular area in (a), (c) high-resolution TEM image of the R phase and an FFT of the Ti2Ni phase (II), (d) interaction between B19′ nanotwins and Ti2Ni precipitates, (e) <011> type II and (100) compound twins, (f) SAED pattern of compound twins, (g) high-resolution TEM image of the interface between the Ti2Ni phase and B19′ nanotwins and corresponding inverse fast Fourier transform (IFFT) image, (h) IFFT image of the interface between the Ti2Ni and B2 phases based on Fig. 3d, and (i) IFFT image of the interface between the Ti2Ni and R phases based on Fig. 4c.

Fig. 5. DSC scans of the as-SLMed and heat-treated TiNi SMAs.

Table 1 Values of Ms, Mf, As, Af, Ms - Mf, and Af - As obtained from the DSC curves and chemical compositions based on EDS analysis of all samples.

Sample	M_s (°C)	M_f (°C)	A_s (°C)	A_f (°C)	M_s - M_f (°C)	A_f - A_s (°C)	Ti (at.%)	Ni (at.%)
as-SLMed	49.2	-6.8	30.2	80.8	56.0	50.6	50.79 ± 0.15	49.21 ± 0.15
S_SRA-500	56.7	5.1	40.5	83.7	51.6	43.2	50.85 ± 0.17	49.15 ± 0.17
S_ISA-800	58.5	18.2	44.3	87.2	40.3	42.9	50.90 ± 0.24	49.10 ± 0.24
S_CSA-1000	69.1	29.7	60.4	100.8	39.4	40.4	50.92 ± 0.10	49.08 ± 0.10

Fig. 6. (a) Room-temperature tensile engineering stress-strain curves of the as-SLMed and heat-treated TiNi SMAs. (b) Ultimate tensile strength vs. tensile strain of TiNi SMAs fabricated by SLM and directed laser deposition reported in related works [11,14,[49], [53], [50], [51], [52]], indicating that this work circumvents the strength-ductility trade-off.

Table 2 Summary of the tensile strain (δ) and ultimate tensile strength (σUTS) for the as-SLMed and heat-treated TiNi SMAs.

TiNi SMAs	as-SLMed	S_SRA-500	S_ISA-800	S_CSA-1000
δ (%)	7.2 ± 0.2	8.9 ± 0.3	8.0 ± 0.3	22.4 ± 0.4
σ_UTS (MPa)	776 ± 9	753 ± 14	705 ± 11	880 ± 13

Fig. 7. Stress-controlled cyclic tensile curves and resultant SME during heating for the SLMed and heat-treated TiNi SMAs: (a) as-SLMed, (b) SSRA-500, (c) SISA-800, and (d) SCSA-1000. εirrec is the irrecoverable strain after heating.

Table 3 Summary of εrec and η for the as-SLMed and heat-treated TiNi SMAs. For comparison, related results of representative TiNi SMAs fabricated by additive manufacturing are also presented. σmax: maximum loading stress in controlled cyclic tensile curves; εrec: recoverable strain after heating; LDED: laser-based directed energy deposition; *: compressive stress; RT: room temperature. M and A denote the martensite and austenite phases, respectively.

Alloy composition (at.%)	Processing method	σ_max (MPa)	ε_rec (%)	η (%)	Phase (RT)	Microstructure
TiNi (this work)	As-SLMed	400	3.54	91.0	M	Semicontinuous Ti₂Ni along GBs
	S_SRA-500	400	4.84	94.2	M	Semicontinuous Ti₂Ni along GBs
	S_ISA-800	400	3.53	85.9	M	Continuous Ti₂Ni along GBs
	S_CSA-1000	400	5.32	98.2	M	Homogeneous globular Ti₂Ni
Ti_49.9Ni_50.1 [53]	SLMed	300	3.54/2.79	75.2/87.2	M	/
Ti_49.6Ni_50.4 [37]	SLMed	150/220	3.91/5.55	97.7/92.5	M	Dislocations and Ni₄Ti₃
Ti_49.91Ni_50.09 [54]	SLMed	1300/290	3.2/2.2	48/100	M	Columnar grains (0.15 ± 0.05 mm) and Ti₂Ni
Ti_52.1Ni_47.9 [54]	LDED	1300/520	2.3/1.9	41/100	A	Equiaxed grains (0.7 ± 0.4 mm)
TiNi [55]	SLMed	900/220	3.6/0.9	58.6/97.1	M	Twinned M
Ti_49.8Ni_50.2 [56]	SLMed	900/250	4.6/1.6	92/100	A	Large M plates and fine elongated A
Ti_49.9Ni_50.1 [57]	SLMed	800*	5.5	97.3	M	/

Fig. 8. (a) Original shape of the TiNi SMA part (190 × 100 × 12 mm3) after CSA heat treatment at 1000 °C, (b) deformed state of the TiNi SMA part after bending, (c) recovery process of the TiNi SMA part after heating to above Af, and (d) recovered shape of the TiNi SMA part after heating.

Fig. 9. SEM fractographs of the as-SLMed and heat-treated TiNi SMAs. (a, b) Microcracks and quasi-cleavage facets across fracture surfaces and (c) nanoscale dimples for the as-SLMed SMA, and dimples for samples (d) SSRA-500, (e) SISA-800, and (f) SCSA-1000 (For interpretation of the references to color in this figure, the reader is referred to the web version of this article.).

Fig. 10. Schematic of microstructural evolution under the three heat treatment modes designed in this study.

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Simultaneous enhancement of mechanical and shape memory properties by heat-treatment homogenization of Ti₂Ni precipitates in TiNi shape memory alloy fabricated by selective laser melting

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