Combinatorial Exploration and Mapping of Phase Transformation in a Ni-Ti-Co Thin Film Library.

Combinatorial synthesis and high-throughput characterization of a Ni-Ti-Co thin film materials library are reported for exploration of reversible martensitic transformation. The library was prepared by magnetron co-sputtering, annealed in vacuum at 500 °C without atmospheric exposure, and evaluated for shape memory behavior as an indicator of transformation. Composition, structure, and transformation behavior of the 177 pads in the library were characterized using high-throughput wavelength dispersive spectroscopy (WDS), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), and four-point probe temperature-dependent resistance (R(T)) measurements. A new, expanded composition space having phase transformation with low thermal hysteresis and Co > 10 at. % is found. Unsupervised machine learning methods of hierarchical clustering were employed to streamline data processing of the large XRD and XPS data sets. Through cluster analysis of XRD data, we identified and mapped the constituent structural phases. Composition-structure-property maps for the ternary system are made to correlate the functional properties to the local microstructure and composition of the Ni-Ti-Co thin film library.

Electrodeposition of a magnetic and redox-active chitosan film for capturing and sensing metabolic active bacteria.

Rapid and portable detection of viable pathogen is highly desired to minimize the risk of foodborne pathogen outbreaks. Here we report a proof-of-concept fabrication methodology of a multifunctional film that allows established methods from bacterial recognition (antibodies) and nanotechnology (magnetic nanoparticles) to be coupled with electrochemical signal processing methods for detection of viable bacteria. Specifically, we enlist a sequence of externally applied electrical and magnetic signals to: i) guide the self-assembly of stimuli-responsive biopolymer; ii) incorporate magnetic nanoparticles to form a magnetic layer; iii) electro-synthesize a signal processing layer (redox-capacitor). The function of the magnetic layer is collecting and concentrating MMP-bacteria through magnetic attractions between MMP-bacteria and the magnetic layer. The function of the signal processing layer is amplifying electrochemical detection of the collected bacteria by engaging the redox-active mediators with the redox capacitor. Importantly, the fabrication demonstrated here is simple, controllable, and reagentless.

Rapid Construction of Fe-Co-Ni Composition-Phase Map by Combinatorial Materials Chip Approach.

One hundred nanometer thick Fe-Co-Ni material chips were prepared and isothermally annealed at 500, 600, and 700 °C, respectively. Pixel-by-pixel composition and structural mapping was performed by microbeam X-ray at synchrotron light source. Diffraction images were recorded at a rate of 1 pattern/s. The XRD patterns were automatically processed, phase-identified, and categorized by hierarchical clustering algorithm to construct the composition-phase map. The resulting maps are consistent with corresponding isothermal sections reported in the ASM Alloy Phase Diagram Database, verifying the effectiveness of the present approach in phase diagram construction.

Combinatorial study of Fe-Co-V hard magnetic thin films.

Thin film libraries of Fe-Co-V were fabricated by combinatorial sputtering to study magnetic and structural properties over wide ranges of composition and thickness by high-throughput methods: synchrotron X-ray diffraction, magnetometry, composition, and thickness were measured across the Fe-Co-V libraries. In-plane magnetic hysteresis loops were shown to have a coercive field of 23.9 kA m-1 (300 G) and magnetization of 1000 kA m-1. The out-of-plane direction revealed enhanced coercive fields of 207 kA m-1 (2.6 kG) which was attributed to the shape anisotropy of column grains observed with electron microscopy. Angular dependence of the switching field showed that the magnetization reversal mechanism is governed by 180° domain wall pinning. In the thickness-dependent combinatorial study, co-sputtered composition spreads had a thickness ranging from 50 to 500 nm and (Fe70Co30)100-xVx compositions of x = 2-80. Comparison of high-throughput magneto-optical Kerr effect and traditional vibrating sample magnetometer measurements show agreement of trends in coercive fields across large composition and thickness regions.

Electric-Field Induced Reversible Switching of the Magnetic Easy Axis in Co/BiFeO3 on SrTiO3.

Electric-field (E-field) control of magnetism enabled by multiferroic materials has the potential to revolutionize the landscape of present memory devices plagued with high energy dissipation. To date, this E-field controlled multiferroic scheme has only been demonstrated at room temperature using BiFeO3 films grown on DyScO3, a unique and expensive substrate, which gives rise to a particular ferroelectric domain pattern in BiFeO3. Here, we demonstrate reversible electric-field-induced switching of the magnetic state of the Co layer in Co/BiFeO3 (BFO) (001) thin film heterostructures fabricated on (001) SrTiO3 (STO) substrates. The angular dependence of the coercivity and the remanent magnetization of the Co layer indicates that its easy axis reversibly switches back and forth 45° between the (100) and the (110) crystallographic directions of STO as a result of alternating application of positive and negative voltage pulses between the patterned top Co electrode layer and the (001) SrRuO3 (SRO) layer on which the ferroelectric BFO is epitaxially grown. The coercivity (HC) of the Co layer exhibits a hysteretic behavior between two states as a function of voltage. A mechanism based on the intrinsic magnetoelectric coupling in multiferroic BFO involving projection of antiferromagnetic G-type domains is used to explain the observation. We have also measured the exact canting angle of the G-type domain in strained BFO films for the first time using neutron diffraction. These results suggest a pathway to integrating BFO-based devices on Si wafers for implementing low power consumption and nonvolatile magnetoelectronic devices.

Self-assembly with orthogonal-imposed stimuli to impart structure and confer magnetic function to electrodeposited hydrogels.

A magnetic nanocomposite film with the capability of reversibly collecting functionalized magnetic particles was fabricated by simultaneously imposing two orthogonal stimuli (electrical and magnetic). We demonstrate that cathodic codeposition of chitosan and Fe3O4 nanoparticles while simultaneously applying a magnetic field during codeposition can (i) organize structure, (ii) confer magnetic properties, and (iii) yield magnetic films that can perform reversible collection/assembly functions. The magnetic field triggered the self-assembly of Fe3O4 nanoparticles into hierarchical "chains" and "fibers" in the chitosan film. For controlled magnetic properties, the Fe3O4-chitosan film was electrodeposited in the presence of various strength magnetic fields and different deposition times. The magnetic properties of the resulting films should enable broad applications in complex devices. As a proof of concept, we demonstrate the reversible capture and release of green fluorescent protein (EGFP)-conjugated magnetic microparticles by the magnetic chitosan film. Moreover, antibody-functionalized magnetic microparticles were applied to capture cells from a sample, and these cells were collected, analyzed, and released by the magnetic chitosan film, paving the way for applications such as reusable biosensor interfaces (e.g., for pathogen detection). To our knowledge, this is the first report to apply a magnetic field during the electrodeposition of a hydrogel to generate magnetic soft matter. Importantly, the simple, rapid, and reagentless fabrication methodologies demonstrated here are valuable features for creating a magnetic device interface.

On-the-fly machine-learning for high-throughput experiments: search for rare-earth-free permanent magnets.

Advanced materials characterization techniques with ever-growing data acquisition speed and storage capabilities represent a challenge in modern materials science, and new procedures to quickly assess and analyze the data are needed. Machine learning approaches are effective in reducing the complexity of data and rapidly homing in on the underlying trend in multi-dimensional data. Here, we show that by employing an algorithm called the mean shift theory to a large amount of diffraction data in high-throughput experimentation, one can streamline the process of delineating the structural evolution across compositional variations mapped on combinatorial libraries with minimal computational cost. Data collected at a synchrotron beamline are analyzed on the fly, and by integrating experimental data with the inorganic crystal structure database (ICSD), we can substantially enhance the accuracy in classifying the structural phases across ternary phase spaces. We have used this approach to identify a novel magnetic phase with enhanced magnetic anisotropy which is a candidate for rare-earth free permanent magnet.