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To minimize the stress shielding effect of metallic biomaterials in mimicking bone, the body-centered cubic (bcc) unit cell-based porous CoCrMo alloys with different, designed volume porosities of 20, 40, 60, and 80% were produced via a selective laser melting (SLM) process. A heat treatment process consisting of solution annealing and aging was applied to increase the volume fraction of an ε-hexagonal close-packed (hcp) structure for better mechanical response and stability. In the present study, we investigated the impact of different, designed volume porosities on the compressive mechanical properties in as-built and heat-treated CoCrMo alloys. The elastic modulus and yield strength in both conditions were dramatically decreased with increasing designed volume porosity. The elastic modulus and yield strength of the CoCrMo alloys with a designed volume porosity of 80% exhibited the closest match to those of bone tissue. Different strengthening mechanisms were quantified to determine their contributing roles to the measured yield strength in both conditions. The experimental results of the relative elastic modulus and yield strength were compared to the analytical and simulation modeling analyses. The Gibson–Ashby theoretical model was established to predict the deformation behaviors of the lattice CoCrMo structures.

We examined fatigue-crack-growth behaviors of CoCrFeMnNi high-entropy alloys (HEAs) under as-fatigued and tensile-overloaded conditions using neutron-diffraction measurements coupled with diffraction peak-profile analyses. We applied both high-resolution transmission electron microscopy (HRTEM) and neutron-diffraction strain mapping for the complementary microstructure examinations. Immediately after a single tensile overload, the crack-growth-retardation period was obtained by enhancing the fatigue resistance, as compared to the as-fatigued condition. The combined mechanisms of the overload-induced larger plastic deformation, the enlarged compressive residual stresses and plastic-zone size, the crack-tip blunting ahead of the crack tip, and deformation twinning governed the pronounced macroscopic crack-growth-retardation behavior following the tensile overload. A remarkable fracture surface of highly-periodic serrated features along the crack-propagation direction was found in the crack-growth region immediately after the tensile overload. Moreover, a transition of plastic deformation from planar dislocation slip-dominated to twinning-dominated microstructures in the extended plastic zone was clearly observed at room temperature in the overloaded condition, in accordance with the simulated results by a finite element method (FEM). The above tensile overload-induced simultaneously combined effects in the coarse-grained CoCrFeMnNi shed light on the improvement of fatigue resistance for HEAs applications.

Gray cast iron comprises α-Fe, Fe3C and graphite with their different anisotropies in terms of structure and mechanical behavior. We perform two different deformation paths as tension-compression and compression-tension on bulk gray iron to capture the stress partitioning. Using in situ neutron diffraction, the composite-like deformation behaviors of α-Fe and Fe3C are revealed simultaneously. Within the elastic deformation stage, both deformation paths do not cause load transfer. However, when the applied compressive stress exceeds 300 MPa, there is a clear load sharing in both paths. From microscopic examinations, the debonding between matrix and graphite is clarified.

The present work extends the examination of selective laser melting (SLM)-fabricated 15-5 PH steel with the 8%-transient-austenite-phase towards fully-reversed strain-controlled low-cycle fatigue (LCF) test. The cyclic-deformation response and microstructural evolution were investigated via in-situ neutron-diffraction measurements. The transient-austenite-phase rapidly transformed into the martensite phase in the initial cyclic-hardening stage, followed by an almost complete martensitic transformation in the cyclic-softening and steady stage. The compressive stress was much greater than the tensile stress at the same strain amplitude. The enhanced martensitic transformation associated with lower dislocation densities under compression predominantly governed such a striking tension-compression asymmetry in the SLM-built 15-5 PH.

Coaxial core/shell electrospun nanofibers consisting of ferroelectric P(VDF-TrFE) and relaxor ferroelectric P(VDF-TrFE-CTFE) are tailor-made with hierarchical structures to modulate their mechanical properties with respect to their constituents. Compared with two single and the other coaxial membranes prepared in the research, the core/shell-TrFE/CTFE membrane shows a more prominent mechanical anisotropy between revolving direction (RD) and cross direction (CD) associated with improved resistance to tensile stress for the crystallite phase stability and good strength-ductility balance. This is due to the better degree of core/shell-TrFE-CTFE nanofiber alignment and the crystalline/amorphous ratio. The coupling between terpolymer P(VDF-TrFE-CTFE) and copolymer P(VDF-TrFE) is responsible for phase stabilization, comparing the core/shell-TrFE/CTFE with the pristine terpolymer. Moreover, an impressive collective deformation mechanism of a two-length scale in the core/shell composite structure is found. We apply in-situ synchrotron X-ray to resolve the two-length scale simultaneously by using the small-angle X-ray scattering to characterize the nanofibers and the wide-angle X-ray diffraction to identify the phase transformations. Our findings may serve as guidelines for the fabrication of the electrospun nanofibers used as membranes-based electroactive polymers.

We have examined the effect of different bath temperatures on residual stress of both the random-oriented Cu films and the highly (111)-oriented nanotwinned Cu films by synchrotron radiation x-ray measurements. The bath temperature varied from 15°C to 40°C. The results indicate that the average residual stress in the highly (111)-oriented nanotwinned films is higher than that in the randomly oriented Cu films. However, the stress in the highly (111)-oriented Cu decreases with increasing bath temperature. The average residual stress can be reduced from 253 MPa electroplated at 15°C to 95 MPa under a bath temperature of 35°C. We could successfully tune and measure residual stress of the Cu thin films. The films with low residual stress prevent warpage from occurring on the substrate and lower the processing failure in copper direct bonding and other processes that need alignment.

We applied Simmons–Balluffi methods, positron measurements, and neutron diffraction to estimate the vacancy of CoCrFeNi and CoCrFeMnNi high-entropy alloys (HEAs) using Cu as a benchmark. The corresponding formation enthalpies and associated entropies of the HEAs and Cu were calculated. The vacancy-dependent effective free volumes in both CoCrFeNi and CoCrFeMnNi alloys are greater than those in Cu, implying the easier formation of vacancies by lattice structure relaxation of HEAs at elevated temperatures. Spatially resolved synchrotron X-ray measurements revealed different characteristics of CoCrFeNi and CoCrFeMnNi HEAs subjected to quasi-equilibrium conditions at high temperatures. Element-dependent behavior revealed by X-ray fluorescence (XRF) mapping indicates the effect of Mn on the Cantor Alloy.

An equiatomic CoCrFeMnNi high-entropy alloy under hydrostatic compression is investigated using in-situ angular-dispersive X-ray diffraction to explore the polymorphism in high entropy alloy systems. The metallic system is of face-centered-cubic structure at ambient condition and applied hydrostatic pressures up to 20 GPa via diamond anvil cell. The angle-resolved diffraction-intensity evolutions of multiple diffraction peaks were collected simultaneously to elucidate the phase stability examinations. The phase transformation from face-centered-cubic to hexagonal-close-packed structure was evidently observed in CoCrFeMnNi alloy accompanied by a deviatoric strain subjected to the hydrostatic compression. We found lattice-asymmetric crossover before and after the phase transformation subjected to hydrostatic compression surroundings. Deviatoric strain triggers fcc-hcp phase transformation as local heterogeneity-driven lattice distortion is significant for CoCrFeMnNi alloy.

In the present work, the tensile properties of 15–5 PH steel fabricated by selective laser melting (SLM) were examined with respect to the transient austenite phase. Compared with the 8%-transient-phase sample, the 18%-transient-phase one shows higher ultimate tensile strength and relatively low yield strength, as well as hardening behavior. We conducted in-situ neutron-diffraction study to examine the microstructure evolution for mechanistic understanding. After applying the external load, most non-equilibrium, retained austenite in the 8%-transient-phase sample transforms before the yield strength, whereas in the 18%-transient-phase sample only 50% of the austenite transforms. Accompanying with the phase transformation, a decrease in the dislocation density and the dislocation strain energy-assisted phase transformation of the ferrite phase are found in the 8%-transient-phase sample even before yielding, which, however, is not the case in the 18%-transient-phase sample. The study demonstrates the SLM enables tuning the amount of transient-phase ratio and coherency between phases to realize a mechanical property control for additive manufactured steel.

Long term success of metallic fusion cages depends on mechanobiological processes through the bone incorporation and rich osseointegration. An optimal configuration of porous titanium-aluminum-vanadium (Ti 6Al 4V) implant fabricated via the additive manufacturing was evaluated in complimentary structure examinations to investigate the growth of autologous osseous at multi-length scales. X-ray microcomputed tomography (micro-CT) and transmission X-ray microscopy (TXM) using newly-built analysis method indicate the porous Ti 6Al 4V is much better for bone ingrowth compared to commercially non-porous titanium (Ti) and porous tantalum (Ta) implants at the ultramicrostructural level. The evolution of bone formation and remodeling acquired by nano X-ray Laue diffraction mapping exhibits the isotropic orientation and low crystallinity of all newly formed bone whereas mature bone in Ti 6Al 4V discloses the preferential alignment and higher crystallinity volumes of constituent hydroxyapatite (HA) crystallites. The high degree in mineral crystallinity of the fully mature bone suggests additive manufactured Ti 6Al 4V pores enhance the collagen-regulated mineralization.

We demonstrated the design of pre-additive manufacturing microalloying elements in tuning the microstructure of iron (Fe)-based alloys for their tunable mechanical properties. We tailored the microalloying stoichiometry of the feedstock to control the grain sizes of the metallic alloy systems. Two specific microalloying stoichiometries were reported, namely biodegradable iron powder with 99.5% purity (BDFe) and that with 98.5% (BDFe-Mo). Compared with the BDFe, the BDFe-Mo powder was found to have lower coefficient of thermal expansion (CTE) value and better oxidation resistance during consecutive heating and cooling cycles. The selective laser melting (SLM)-built BDFe-Mo exhibited high ultimate tensile strength (UTS) of 1200 MPa and fair elongation of 13.5%, while the SLM-built BDFe alloy revealed a much lower UTS of 495 MPa and a relatively better elongation of 17.5%, indicating the strength enhancement compared with the other biodegradable systems. Such an enhanced mechanical behavior in the BDFe-Mo was assigned to the dominant mechanism of ferrite grain refinement coupled with precipitate strengthening. Our findings suggest the tunability of outstanding strength-ductility combination by tailoring the pre-additive manufacturing microalloying elements with their proper concentrations.

CoFeB/MgO-based magnetic tunnel junctions (MTJs) have considerable potential in magnetic random access memory (MRAM), thanks to their tunable perpendicular magnetic anisotropy (PMA). We found significant reduction of dead-layer by inserting additional MgO into the MTJ structure. Interface, electronic and transport characterizations were utilized to approach the modified magnetic properties driven by the dual-MgO structure in this work. The dual-MgO structure appeared to hinder boron (B) diffusion into the metallic layer and prevent capping-layer (Ta) penetration across the interface. This suppressed the dead-layer effect and promoted overall magnetization despite PMA degradation. A robust BOx phase that formed within the dual-MgO structure presented a superparamagnetic ground state. In the single-MgO structure, any reduction in the thickness of the CoFeB promoted PMA, albeit at the cost of spin-polarization. The dual-MgO structure could restore spin-polarization by preferentially populating spin electrons into Fe/Co minority states. X-ray magnetic spectroscopy and anomalous Hall effect suggest that, the dual-MgO differs from the single-MgO with a favorable longitudinal polarized spin-channel. This makes the dual-MgO structure applicable to applications requiring in-plane rather than out-of-plane sensing.

An equal-molar CoCrFeMnNi, face-centered-cubic high-entropy alloy system is investigated using in-situ angular-dispersive X-ray diffraction under hydrostatic compression up to 20 GPa via diamond anvil cell. The evolutions of multiple diffraction peaks are collected simultaneously to elucidate the phase stability field. The results indicated that an irreversible phase transformation had occurred in the high entropy alloy upon decompression to ambient pressure. A reference material (n-type silicon-doped gallium arsenide) was investigated following the same protocol to demonstrate the different deformation mechanisms. It is suggested that the atomic bonding characteristics on the phase stability may play an important role in the high entropy alloys.

La1−xSrxMnO3 (LSMO) is well known as an efficient spin-injection electrode in ferromagnetic–organic hybrid-based organic spin valves (OSV). Herein, we examine the influence of three terminating layers of LSMO films (mixed-, MnO2-, and LaSrO- (LSO-) terminated) on the spin filter at the bottom interface of tri (8-hydroxyquinoline) aluminum (Alq3) deposited on these substrates. Angle-dependent X-ray photoelectron spectra (XPS) demonstrated the presence of SrO segregation at the outermost layer for three types of LSMO films but in different amounts that might contribute to their magnetic properties. A weak surface coupling between LSMO and Alq3 was obtained through a small increase of Mn L-edge X-ray magnetic circular dichroism (XMCD) but it does not vary the bulk magnetic properties of LSMO films upon Alq3 adsorption (LSMO/Alq3). The surface dipoles due to the interaction between LSMO films and Alq3 were found to be 0.5, 0.5, and 0.7 eV for the mixed-ter/Alq3, MnO2-ter/Alq3, and LSO-ter/Alq3 interfaces, respectively. Our results indicate that the segregated SrO layer plays an important role in the surface electronic and magnetic properties at LSMO/Alq3 interfaces, which contributes to a fundamental understanding of the spin injection and transport in LSMO-Alq3 hybrid-based OSV devices.

The coaxial core/shell composite electrospun nanofibers consisting of relaxor ferroelectric P(VDF-TrFE-CTFE) and ferroelectric P(VDF-TrFE) polymers are successfully tailored towards superior structural, mechanical, and electrical properties over the individual polymers. The core/shell-TrFE/CTFE membrane discloses a more prominent mechanical anisotropy between the revolving direction (RD) and cross direction (CD) associated with a higher tensile modulus of 26.9 MPa and good strength-ductility balance, beneficial from a better degree of nanofiber alignment, the increased density, and C-F bonding. The interfacial coupling between the terpolymer P(VDF-TrFE-CTFE) and copolymer P(VDF-TrFE) is responsible for comparable full-frequency dielectric responses between the core/shell-TrFE/CTFE and pristine terpolymer. Moreover, an impressive piezoelectric coefficient up to 50.5 pm/V is achieved in the core/shell-TrFE/CTFE composite structure. Our findings corroborate the promising approach of coaxial electrospinning in efficiently tuning mechanical and electrical performances of the electrospun core/shell composite nanofiber membranes-based electroactive polymers (EAPs) actuators as artificial muscle implants.

In this study, we optimized the geometry and composition of additive-manufactured pedicle screws. Metal powders of titanium-aluminum-vanadium (Ti-6Al-4V) were mixed with reactive glass-ceramic biomaterials of bioactive glass (BG) powders. To optimize the geometry of pedicle screws, we applied a novel numerical approach to proposing the optimal shape of the healing chamber to promote biological healing. We examined the geometry and composition effects of pedicle screw implants on the interfacial autologous bone attachment and bone graft incorporation through in vivo studies. The addition of an optimal amount of BG to Ti-6Al-4V leads to a lower elastic modulus of the ceramic-metal composite material, effectively reducing the stress-shielding effects. Pedicle screw implants with optimal shape design and made of the composite material of Ti-6Al-4V doped with BG fabricated through additive manufacturing exhibit greater osseointegration and a more rapid bone volume fraction during the fracture healing process 120 days after implantation, per in vivo studies.

We report an annealing method which significantly enhances the piezoelectric performance by simultaneously tuning morphology and crystalline phase of electrospun P(VDF-TrFE) nanofibers. Annealing process-induced transformation, from α to β crystalline phase at lattice scale, also changes fiber morphology at micrometer scale. The underlying differences between as-spun and annealed P(VDF-TrFE) nanofibers for their stretch-hold deformation were examined via in-situ synchrotron for both small and wide angle X-ray scattering (SAXS and WAXS). Transmission X-ray microscopy (TXM) characterization reveals the underneath fiber orientation subjected to different levels of deformation. Multi-length scale microstructural evolution demonstrates distinct deformation behaviors of the as-spun and annealed nanofibers during uniaxial tensile loading. The findings can be applied for multi-scale structure modulation for the design of future piezoelectric devices.

Understanding the interfacial behavior at FM-OSC-FM hybrid structures for both the bottom contact (Alq 3 adsorption on Co, Co/Alq 3 ) and the top contact (Co atop Alq 3 , Alq 3 /Co) is crucial for efficient spin filtering with transport of spin-polarized charge carriers through these interfaces. X-ray photoelectron spectroscopy (XPS) spectra indicate a symmetry of charge transfer from Co to Alq 3 and the corresponding orbital hybridization to a certain extent at both contacts. The alignment of energy levels at both Alq 3 /Co and Co/Alq 3 heterostructures is depicted with ultraviolet photoelectron spectroscopy (UPS). Through magnetic images acquired with a X-ray photoemission electron microscope (XPEEM), the strong hybridization of the top contact presents no micromagnetic domain but still shows magnetic coupling, to some extent, to the bottom contact in the Co–Alq 3 –Co trilayer structure. Measurements of X-ray magnetic circular dichroism (XMCD) demonstrate the induced spin-polarization of non-magnetic Alq 3 at both contacts, proving Alq 3 a unique and promising organic material for spin filtering in OSV.

To realize the origin of efficient spin injection at organic-ferromagnetic contact in organic spintronics, we have implemented the formation of quasi-molecular magnet via surface restructuring of a strong organic acceptor, tetrafluoro-tetracyano-quinodimethane (F4-TCNQ), in contact with ferromagnetic cobalt. Our results demonstrate a spin-polarized F4-TCNQ layer and a remarkably enhanced magnetic anisotropy of the Co film. The novel magnetic properties are contributed from strong magnetic coupling caused by the molecular restructuring that displays an angular anchoring conformation of CN and upwardly protruding fluorine atoms. We conclude that the π bonds of CN, instead of the lone-pair electrons of N atoms, contribute to the hybridization-induced magnetic coupling between CN and Co and generate a superior magnetic order on the surface.

The interfacial regions at organic-ferromagnetic hybrid structures are critical to affect the spin injection and transport in organic spin valves (OSVs) since spin-polarized charge carriers across these interfaces. Understanding the interfacial behavers at FM-OSC-FM heterostructures is crucial for the design and operation of OSV devices. Herein, we investigated influence of different termination layers of lanthanum strontium manganite (LSMO) on the interfacial electronic and magnetic properties of LSMO/Alq 3 heterostructures. Different termination layers of LSMO with LSO, MnO 2 and mixed terminations were prepared to examine the spin interface of LSMO/Alq 3 . From experimental results, the outermost layer of LSO and mixed terminations exhibited significant SrO segregation while less segregation was found for MnO 2 . In addition, the surface SrO segregation correlates to the variation of surface magnetic properties and the formation of surface dipole at the mixed LMSO/Alq 3 , MnO 2 -ter/Alq 3 , and LSO-ter/Alq 3 interfaces.

Nitrogen-doped TiO2 nanotube arrays (N-TNAs) were successfully fabricated by a simple thermal annealing process in ambient N2 gas at 450 &deg, C for 3 h. TNAs with modified morphologies were prepared by a two-step anodization using an aqueous NH4F/ethylene glycol solution. The N-doping concentration (0&ndash, 9.47 at %) can be varied by controlling N2 gas flow rates between 0 and 500 cc/min during the annealing process. Photocatalytic performance of as-prepared TNAs and N-TNAs was studied by monitoring the methylene blue degradation under visible light (&lambda, &ge, 400 nm) illumination at 120 mW&middot, cm&minus, 2. N-TNAs exhibited appreciably enhanced photocatalytic activity as compared to TNAs. The reaction rate constant for N-TNAs (9.47 at % N) reached 0.26 h&minus, 1, which was a 125% improvement over that of TNAs (0.115 h&minus, 1). The significant enhanced photocatalytic activity of N-TNAs over TNAs is attributed to the synergistic effects of (1) a reduced band gap associated with the introduction of N-doping states to serve as carrier reservoir, and (2) a reduced electron‒hole recombination rate.

This paper reports on a magnetic device with a [Co40Pd60/Cu]10/Fe structure for use in the detection of H2. In a magneto-optical, transport, and gas-detection system, the proposed device presented sharp, reproducible H2-dependent magnetic/electrical properties. The device's saturation magnetization (induced resistance change) dropped (increased) by a factor of ∼5 when a H2 pressure of 75 kPa is given. Besides, the electrical signal-to-noise ratio of the device can be restored ∼50% by exposing it to a magnetic field of 1000 Oe, even when the sensitivity of the device dropped at a low H2 pressure (0.7 KPa). This demonstrates the applicability of the device for use as a low-pressure H2 detector. Operando x-ray spectroscopy revealed that changes in H2-induced magnetism arose from a Co-Pd charge transfer effect coupled to changes in the local-structure symmetry.

We report on the successful fabrication of epitaxial-discrete Co x Fe3−x O4/CoO magnetic nanostructures on a SrTiO3 substrate as well as the results of a thorough investigation of the magnetic cross-reactions of the two phases in the vicinity of the epitaxial junction. These nanostructures were originally prepared as Fe3O4-CoO core-shell structures through the phase decomposition of bismuth perovskite precursors by pulsed-laser deposition. An antiphase boundary emerged during the structural/electronic transition from the CoO core to the Co1−x Fe2+X O4 shell; this then developed into a ferrimagnetic/antiferromagnetic interface. Uncompensated spins (UCS) arose from the Co x Fe3−x O4/CoO interface as a result of strong ferrimagnetic–antiferromagnetic interactions. A notable exchange bias as well as a significant exchange enhancement was observed owing to the UCS, which had a locking effect because of the decoupling of the Co1−x Fe2+X O4/CoO reversal from the antiphase boundary. Control of the precursor ratio allowed for the fine-tuning of the Co1−x Fe2+X O4 phase and the associated locking behaviors. This, in turn, allowed the anisotropy and coercivity of the nanostructures to be manipulated. Thus, we were able to create and thoroughly understand a complex epitaxial configuration with tunable structural and magnetic properties. This study should open new opportunities with regard to current magnetic oxide technology, which requires novel methods for pursuing extremity of controllable properties over an atomic landscape.

Using synchrotron x-ray techniques, we studied the Co2FeAl spin-polarization state that generates the half-metallicity of the compound during an A2 (low-spin) → B2 (high-spin) phase transition. Given the advantage of element specificity of x-ray techniques, we could fingerprint the structural and magnetic cross-reactions between Co and Fe within a complex Co2FeAl structure deposited on a MgO (0 0 1) substrate. X-ray diffraction and extended x-ray absorption fine structure investigations determined that the Co atoms preferably populate the (1/4,1/4,1/4) and (3/4,3/4,3/4) sites during the development of the B2 phase. X-ray magnetic spectroscopy showed that although the two magnetic elements were ferromagnetically coupled, they interacted in a competing manner via a charge-transfer effect, which enhanced Co spin polarization at the expense of Fe spin polarization during the phase transition. This means that the spin-polarization of Co2FeAl was electronically dominated by Fe in A2 whereas the charge transfer turned the dominance to Co upon B2 formation. Helicity-dependent x-ray absorption spectra also revealed that only the minority state of Co/Fe was involved in the charge-transfer effect whereas the majority state was independent of it. Despite an overall increase of Co2FeAl magnetization, the charge-transfer effect created an undesired trade-off during the Co–Fe exchange interactions, because of the presence of twice as many X sites (Co) as Y sites (Fe) in the Heusler X 2 YZ formula. This suggests that the spin-polarization of Co2FeAl is unfortunately regulated by compromising the enhanced X (Co) sites and the suppressed Y (Fe) sites, irrespective of the development of the previously known high-spin-polarization phase of B2. This finding provides a possible cause for the limited half-metallicity of Co2FeAl discovered recently. Electronic tuning between the X and Y sites is necessary to further increase the spin-polarization, and likely the half-metallicity as well, of the compound.