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Influence of Contact Stresses on Shape Recovery in Sputter Deposited NiTiCu Thin FilmsGelli, N V R Vikram January 2016 (has links) (PDF)
NiTiCu is a shape memory alloy that regains its original shape after large amount of shape changing deformation when heated above a critical temperature called reverse martensitic trans-formation temperature( Af). When external load is applied on the sample in twinned martensite phase at low temperature, it deforms by detwinning, accommodating large amount of strains. When it is heated above Af, the shape recovers by transformation of the martensite to austenite phase. However, the amount of shape recovery degrades over time due to internal factors such as precipitates, residual strains and thermal history as well as external factors such as stresses. Severe localized stresses induced by contacts result in plastic deformation that affect the reverse martensitic transformation and hence the shape recovery. In this work, we study how varying levels of contact stresses induced in NiTiCu thin film affect its shape recovery. NiTiCu thin films of six different compositions are deposited on Si(100) wafer by co-sputtering from elemental targets. After deposition, the films are annealed at 500 C for 4 h to make them crystalline. The composition of the films varied linearly with applied power to the targets. Uniformity in composition over a 4 inch substrate area is achieved by substrate rotation. All the films show ne grain microstructure after annealing. The subsurface of the Ni-rich films is columnar. Ni-rich films have annealing cracks and the crack width increases with Ni composition in the films. The roughness of as-deposited films is found to be more for Ni-rich films compared to Ti-rich films. The roughness of the Ni-rich and Ti-rich films increased after annealing. From the X-ray diffraction studies, it was observed that the films are nanocrystalline.
Indentation is carried out using a Berkovich diamond indenter with spherical apex, at nine different locations with loads ranging from 0.25 mN to 25 mN. A predefined array is chosen for indentation such that the larger indents act as a guide to precisely locate minute indents generated at lower loads, with residual depth as small as 10 nm, for imaging in high-resolution microscopes like Scanning Electron Microscope as well as in Atomic Force Microscope . In Ti60 (a Ti-rich) lm, the residual indents generated at loads greater than 10 mN show radial cracks originating at corners. Average crack length increases with the maximum load used for generating the indent. Sequential sectioning of Ti48 (a Ni-rich) lm using Focused Ion Beam microscope, revealed that the cracks originate at the lm-substrate interface and reach the surface. In Ti48 lm, residual indents do not show any indentation cracks. The indentation stresses are accommodated by breaking of the columnar structure and the voids between them. Delamination of the film from the substrate is observed on either sides
of the indent in both the Ti60 and Ti48 films. The hardness of the films is high at low loads and decrease as the load increases.
The deformation by indentation at lower loads is mainly due to detwinning as only the apex of the indenter, which is nearly spherical, is in contact with the sample and the resulting stresses are low. As the load increases, the deformation starts getting accommodated through dislocations along with detwinning as the stress beneath the indenter increases. Spherical cavity model extended to SMA shows that inner hemisphere near the tip contains dislocations where stresses are very high, surrounded by detwinned region with stresses that are relatively low. When the sample is heated above reverse martensitic transformation temperature to induce shape recovery in the indents, only the detwinned region recovers to the original shape. Recovery ratio, quantification of shape recovery, is calculated from the depth of the indents before and after heating. Recovery ratio in Ti60 films is found to be large at low loads and decreases with increase in load. The decrease in shape recovery in Ti60 is attributed to the increase in the amount of plastic deformation at the expense of detwinning. Three-dimensional mapping of the surfaces shows that the recovery ratio is high at the apex of the indent at the maximum depth and reduces towards the edges of the indent. There is no evident recovery in Ti48 films.
The shape recovery of SMAs can be achieved by Joule heating. When electric current is passed through the material, it heats up by Joule heating because of the intrinsic resistivity. The resistivity and hence the resistance would get effected by the dislocation based plastic deformation induced by the contact. This might result in shape recovery through resistive heating. Towards understanding this, the effect of contact stresses on electrical contact resistance is studied. Experimental setup is designed, developed and calibrated for studying the variation of electrical contact resistance of the NiTiCu thin films as a function of load. Electrical contact resistance is found to decrease with increase in applied load. Contact stresses in sub-micron NiTiCu thin films are simulated by carrying out nanoindentation at different loads. The recovery ratio is high when the stresses induced by the contact is less, at lower loads. The shape recovery ratio is reduced when the induced contact stresses in-creases. There is no shape recovery at the sharp edges of the indentation where contact stresses are very high. Hence, by carefully designing the features to reduce the stress concentrations, the performance of the device can be improved.
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