Versatile Experimental Setup Research Articles

Chemical and Structural In-Situ Characterization of Model Electrocatalysts by Combined Infrared Spectroscopy and Surface X-ray Diffraction.

New diagnostic approaches are needed to drive progress in the field of electrocatalysis and address the challenges of developing electrocatalytic materials with superior activity, selectivity, and stability. To this end, we developed a versatile experimental setup that combines two complementary in-situ techniques for the simultaneous chemical and structural analysis of planar electrodes under electrochemical conditions: high-energy surface X-ray diffraction (HE-SXRD) and infrared reflection absorption spectroscopy (IRRAS). We tested the potential of the experimental setup by performing a model study in which we investigated the oxidation of preadsorbed CO on a Pt(111) surface as well as the oxidation of the Pt(111) electrode itself. In a single experiment, we were able to identify the adsorbates, their potential dependent adsorption geometries, the effect of the adsorbates on the surface morphology, and the structural evolution of Pt(111) during surface electro-oxidation. In a broader perspective, the combined setup has a high application potential in the field of energy conversion and storage.

The long view of triadic resonance instability in finite-width internal gravity wave beams

This article presents our exploration into how a finite-width internal gravity wave beam is modified by triadic resonance instability. We present both experimental and weakly nonlinear modelling to examine this instability mechanism, in which a primary wave beam generates two secondary wave beams of lower frequencies and shorter length scales. Through a versatile experimental set-up, we examine how this instability evolves over hundreds of buoyancy periods. Unlike predictions from previous zero-dimensional weakly nonlinear theory, we find that the wave does not monotonically approach a saturated equilibrium of triadic interactions; rather, the amplitudes and structures of the constituent beams continue to modulate without ever reaching a steady equilibrium. To understand this behaviour, we develop a weakly nonlinear approach to account for the spatiotemporal evolution of the amplitudes and structures of the beams over slow time scales and long distances, and explore the consequences using a numerical scheme to solve the resulting equations. Through this approach, we establish that the evolution of the instability is remarkably sensitive to the spatiotemporal triadic configuration for the system and how part of the observed modulations can be attributed to a competition between the linear growth rate of the secondary wave beams and the finite residence time of the triadic perturbations within the underlying primary beam.

Novel Experimental Setup for Coulometric Signal Transduction of Ion-Selective Electrodes.

In this work, a novel and versatile experimental setup for coulometric signal transduction of ion-selective electrodes (ISEs) is introduced and studied. It is based on a constant potential coulometric measurement carried out using a one-compartment three-electrode electrochemical cell. In the setup, a potassium ion-selective electrode (K+- ISE) is connected as the reference electrode (RE). A poly(3,4-ethylenedioxythiophene) doped with polystyrene sulfonate (PEDOT:PSS)-based electrode with a dummy membrane (DM) and a glassy carbon (GC) rod are connected as the working electrode (WE) and counter electrode (CE), respectively. Adding a non-selective dummy membrane to the structure of the WE facilitates the regulation of the measured signal and response time. The results from electrochemical impedance spectroscopy measurements carried out on the WE showed that the time constant is profoundly influenced by the dummy membrane thickness. In addition, the redox capacitance of the PEDOT:PSS film shows a better correlation with the electrode area than the film thickness. Sequential addition/dilution experiments showed the improvement of current and cumulated charge signals in the new setup studied in this work compared to the setup used in the original coulometric signal transduction method. Both conventional ISEs and solid-contact ISEs (SCISEs) were used in this work. The results showed that the coulometric response was independent of the type of ISE used as RE, confirming the versatility of the novel set-up.

Versatile experimental setup for FTJ characterization

Ferroelectric Tunnel Junctions (FTJ) are intriguing electron devices which can be operated as memristors and artificial synapses for hardware neural networks. In this work, two virtual–grounded amplifiers have been designed to extract the hysteretic I–V and Q–V characteristics directly, and good agreement between repeated measurements on both circuits demonstrates the accuracy and flexibility of the two setups. Optimal measurement conditions have also been assessed and, finally, wake–up, fatigue, and the preset–dependent early breakdown have been studied.

Challenges and Accomplishments in Mechanical Testing Instrumented by In Situ Techniques: Infrared Thermography, Digital Image Correlation, and Acoustic Emission

A current trend in mechanical testing technologies is to equip researchers and industrial practitioners with the facilities for non-destructive characterisation of the deformation and fracture processes occurring on different scales. The synergistic effect of such a combination of destructive and non-destructive techniques both widens and deepens existing knowledge in the field of plasticity and fracture of materials and provides the feedback sought to develop new non-destructive testing approaches and in situ monitoring techniques with enhanced reliability, accuracy and a wider scope of applications. The macroscopic standardised mechanical testing is still dominant in the research laboratories and industrial sector worldwide. The present paper reviews multiple challenges commonly faced by experimentalists, aiming at enhancing the capability of conventional mechanical testing by a combination of contemporary infrared thermography (IRT), rapid video imaging (RVI) with non-contact strain mapping possibilities enabled by the digital image correlation (DIC) method, and the acoustic emission (AE) technique providing unbeatable temporal resolution of the stochastic defect dynamics under load. Practical recommendations to address these challenges are outlined. A versatile experimental setup uniting the unique competencies of all named techniques is described alone with the fascinating possibilities it offers for the comprehensive characterisation of damage accumulation during plastic deformation and fracture of materials. The developed toolbox comprising practical hardware and software solutions brings together measuring technologies, data, and processing in a single place. The proposed methodology focuses on the characterisation of the thermodynamics, kinematics and dynamics of the deformation and fracture processes occurring on different spatial and temporal scales. The capacity of the proposed combination is illustrated using preliminary results on the tensile and fatigue behaviour of the fcc Inconel-625 alloy used as a representative example. Dissipative processes occurring in this alloy are assessed through the complex interplay between the released heat, acoustic emission waves, and expended and stored elastic energy.

Experimental characterization of quantum processes: A selective and efficient method in arbitrary finite dimensions

The temporal evolution of a quantum system can be characterized by quantum process tomography, a complex task that consumes a number of physical resources scaling exponentially with the number of subsystems. An alternative approach to the full reconstruction of a quantum channel is the selective and efficient quantum process tomography, a method that allows estimating, individually and up to the required accuracy, each element of the matrix that describes the process, using only a polynomial amount of resources. The implementation of this protocol is closely related to the possibility of building a complete set of mutually unbiased bases (MUBs), whose existence is known only when the dimension of the Hilbert space is the power of a prime number. However, an extension of the method that uses tensor products of maximal sets of MUBs has been recently introduced. Here we explicitly describe how to implement the algorithm for a selective and efficient estimation of a quantum process in a nonprime power dimension and conduct, an experimental verification of the method in a Hilbert space of dimension $d=6$. This is the smallest space for which a complete set of MUBs is not known to exist, but it can be decomposed as a tensor product of two Hilbert spaces of dimensions ${D}_{1}=2$ and ${D}_{2}=3$, in which a complete set of MUBs is already known. The six-dimensional states were codified in the discretized transverse linear momentum of photons. The state preparation and detection stages are dynamically programed with the use of only-phase spatial light modulators, in a versatile experimental setup that allows one to implement the algorithm in any finite dimension.

Versatile Device for the Study of Coupling Properties in Multifunctional Materials. Example: Ni-(Co)-Mn-In Heusler Materials

We report on a versatile experimental setup for the study of the electro-magneto-elasto-thermal coupling for bulk materials having coupling properties. The setup enables measurement of stress and electrical resistivity in a 80-450 K temperature range under controlled uniaxial pressure in a magnetic field up to 8 T. The strong influence of uniaxial pressure and magnetic field on strain and transport properties is shown for Ni-Co-Mn-In Heusler single crystal material. Phase transformation, magnetostress and magnetic field-induced phase transformation, and elastocaloric effect can be estimated using this versatile setup. This device is very complementary to the studies focused on the modeling of thermo-electro-magneto-mechanical behavior for functional materials.

Bright, polarization-tunable high repetition rate extreme ultraviolet beamline for coincidence electron–ion imaging

After decades of supremacy of the Titanium:Sapphire technology, Ytterbium-based high-order harmonic sources are emerging as a promising alternative for experiments requiring high flux of ultrashort extreme ultraviolet (XUV) radiation. In this article we describe a versatile experimental setup delivering XUV photons in the 10–50 eV range. The use of cascaded high-order harmonic generation enables us to reach 1.9 mW of average power at 18 eV. Several spectral selection schemes are presented, to isolate a single high-harmonic or a group of them. In the perspective of circular dichroism experiments, we produce highly elliptical XUV radiation using resonant elliptical high-harmonic generation, and circularly polarized XUV by bichromatic bicircular high-harmonic generation. As an illustration of the capacities of the beamline, we focus the XUV beam in a coincidence electron–ion imaging spectrometer, where we measure the photoelectron momentum angular distributions of xenon monomers and dimers.

A versatile low-cost experimental set-up and measurement protocol for temperature dependent electrical measurements in the temperature range 100 K – 500 K

A versatile low-cost experimental set-up and adjoining measurement protocol for continuous temperature dependent electrical measurements in the temperature range of 100 K – 500 K is described. The set-up can perform continuous measurements of DC and AC electrical properties of a sample under test (SUT) as a function of its temperature in the mentioned temperature range without any artefacts. The SUT can be in the form of film, or, powders pressed into pellets. The set-up comprises of automatic data acquisition system equipped with LabVIEW programme for real time data acquisition during measurements. The errors involved in the measurements using the set-up have been calculated by measuring the temperature dependent resistance of standard Pt100 RTD temperature sensor and from temperature response of dielectric constant of standard polycrystalline BaTiO3. The high measurement accuracy of the present set-up in artefact-free AC and DC electrical measurements has been demonstrated by measuring the temperature response of the electrical properties of standard polycrystalline BaTiO3, standard polycrystalline SnO2 and nano polycrystalline SnO2 samples.

On-Line Analysis of the Heterogeneous Pd-Catalyzed Transfer Hydrogenation of p-Nitrophenol in Water with Formic Acid in a Flow Reactor

An versatile experimental setup composed of a fixed-bed reactor and an HPLC apparatus has been developed for the study of heterogeneous catalytic reactions under transient conditions. The transfer hydrogen reaction of formic acid in water to give p-nitrophenol catalyzed by Pd@Al2O3 support was chosen as the model reaction in a flow reactor. On one hand, this setup allowed the first experimental on-line measurements of p-aminophenol in an acidic medium, indicating that it is the only product of the reaction at steady state. On the other hand, the setup evidenced a quite long transient period before stationary conditions were reached, involving a transient component that is quite instable and can transform to p-aminophenol without a catalyst. Results of numerical simulations indicate that only a change in the reaction mechanism, due to a change in the catalyst activity after few minutes of reaction, can explain the transient production of this intermediate and that this occurs when the active hydrogen coverage of the catalyst is low.

Revealing the formation dynamics of the electric double layer by means of in-situ Rutherford backscattering spectrometry.

We report on a new versatile experimental setup for in situ Rutherford backscattering spectrometry at solid-liquid interfaces which enables investigations of electric double layers directly and in a quantitative manner. A liquid cell with a three-electrode arrangement is mounted in front of the beam line, and a thin Si3N4 window (thickness down to 150 nm) separates the vacuum of the detector chamber from the electrolyte in the cell. By minimizing the contribution of the window to the measurement, a large variety of elements at the solid-liquid interface with sensitivities far below one monolayer can be monitored. The attachment of Ba onto the Si3N4 surface as a function of contact time and pH value of the electrolyte solution was chosen as an example system. From our measurement, we can not only follow the evolution of the double layer but also derive limits for the point of zero charge for the Si3N4 surface. Our findings of 5.7≤pHPZC≤6.2 are in good agreement with values found in the literature obtained by other techniques. Despite focusing on a specific system in this work, the presented setup allows for a large variety of in situ investigations at solid-liquid interfaces such as, but not limited to, tracing electrochemical reactions and monitoring segregation, adsorption, and dissolution and corrosion processes.

Dipolar Quantum Mixtures of Erbium and Dysprosium Atoms.

We report on the first realization of heteronuclear dipolar quantum mixtures of highly magnetic erbium and dysprosium atoms. With a versatile experimental setup, we demonstrate binary Bose-Einstein condensation in five different Er-Dy isotope combinations, as well as one Er-Dy Bose-Fermi mixture. Finally, we present first studies of the interspecies interaction between the two species for one mixture.

An Apparatus for the Performance Estimation of Pressure Fluctuation Energy Harvesters

Hydraulic pressure fluctuation energy harvesters are promising alternatives to power up wireless sensor nodes in hydraulic systems. The characterization of these harvesters under dynamic and band-limited pressure signals is imperative for the research and development of novel concepts. To generate and control these signals in a hydraulic medium, a versatile apparatus capable of reproducing pressure signals is proposed. In this paper, a comprehensive discussion of the design considerations for this apparatus and its performance is given. The suggested setup enables the investigation of devices tailored for the harvesting of energy in conventional hydraulic systems. To mimic these systems, static pressures can be tuned up to 300 bar, and the pressure amplitudes with a maximum of 28 Bar at 40 Hz and 0.5 bar at 1000 Hz can be generated. In addition, pressure signals found in commercial hydraulic systems can be reproduced with good accuracy. This apparatus proves to be an accessible, robust, and versatile experimental setup to create environments for the complete performance estimation of pressure fluctuation energy harvesters.

Characterisation of the electric drive of EV: on‐road versus off‐road method

For system design, analysis of global performance and energy management of electric vehicles (EVs), it is common to use the efficiency map of electric traction drive. The characterisation of the efficiency map with high accuracy is then an important issue. In this study, an on-road method and an off-road method are compared experimentally to determine the efficiency map of electric drive of EVs. The off-road method requires a dedicated experimental test bed, which is expensive and time consuming. The on-road method is achieved directly in-vehicle. Experimental data, recorded during an on-road driving cycle, are used to determine the efficiency map using non-intrusive measurements from global positioning system antenna, voltage and current sensors. A versatile experimental setup is used to compare both methods on the same platform. A maximal efficiency difference of 6% is achieved in most of the torque–speed plane. It is shown that, in an energetic point of view, both methods yield similar results. © The Institution of Engineering and Technology 2017

RhizoTubes as a new tool for high throughput imaging of plant root development and architecture: test, comparison with pot grown plants and validation.

BackgroundIn order to maintain high yields while saving water and preserving non-renewable resources and thus limiting the use of chemical fertilizer, it is crucial to select plants with more efficient root systems. This could be achieved through an optimization of both root architecture and root uptake ability and/or through the improvement of positive plant interactions with microorganisms in the rhizosphere. The development of devices suitable for high-throughput phenotyping of root structures remains a major bottleneck.ResultsRhizotrons suitable for plant growth in controlled conditions and non-invasive image acquisition of plant shoot and root systems (RhizoTubes) are described. These RhizoTubes allow growing one to six plants simultaneously, having a maximum height of 1.1 m, up to 8 weeks, depending on plant species. Both shoot and root compartment can be imaged automatically and non-destructively throughout the experiment thanks to an imaging cabin (RhizoCab). RhizoCab contains robots and imaging equipment for obtaining high-resolution pictures of plant roots. Using this versatile experimental setup, we illustrate how some morphometric root traits can be determined for various species including model (Medicago truncatula), crops (Pisum sativum, Brassica napus, Vitis vinifera, Triticum aestivum) and weed (Vulpia myuros) species grown under non-limiting conditions or submitted to various abiotic and biotic constraints. The measurement of the root phenotypic traits using this system was compared to that obtained using “classic” growth conditions in pots.ConclusionsThis integrated system, to include 1200 Rhizotubes, will allow high-throughput phenotyping of plant shoots and roots under various abiotic and biotic environmental conditions. Our system allows an easy visualization or extraction of roots and measurement of root traits for high-throughput or kinetic analyses. The utility of this system for studying root system architecture will greatly facilitate the identification of genetic and environmental determinants of key root traits involved in crop responses to stresses, including interactions with soil microorganisms.

Tunable Polarons of Slow-Light Polaritons in a Two-Dimensional Bose-Einstein Condensate

When an impurity interacts with a bath of phonons it forms a polaron. For increasing interaction strengths the mass of the polaron increases and it can become self-trapped. For impurity atoms inside an atomic Bose-Einstein condensate (BEC) the nature of this transition is not understood. While Feynman's variational approach to the Fröhlich model predicts a sharp transition for light impurities, renormalization group studies always predict an extended intermediate-coupling region characterized by large phonon correlations. To investigate this intricate regime and to test polaron physics beyond the validity of the Fröhlich model we suggest a versatile experimental setup that allows us to tune both the mass of the impurity and its interactions with the BEC. The impurity is realized as a dark-state polariton (DSP) inside a quasi-two-dimensional BEC. We show that its interactions with the Bogoliubov phonons lead to photonic polarons, described by the Bogoliubov-Fröhlich Hamiltonian, and make theoretical predictions using an extension of a recently introduced renormalization group approach to Fröhlich polarons.

Observation of giant Goos-Hänchen and angular shifts at designed metasurfaces.

Metasurfaces with sub-wavelength features are useful in modulating the phase, amplitude or polarization of electromagnetic fields. While several applications are reported for light manipulation and control, the sharp phase changes would be useful in enhancing the beam shifts at reflection from a metasurface. In designed periodic patterns on metal film, at surface plasmon resonance, we demonstrate Goos-Hanchen shift of the order of 70 times the incident wavelength and the angular shifts of several hundred microradians. We have designed the patterns using rigorous coupled wave analysis (RCWA) together with S-matrices and have used a complete vector theory to calculate the shifts as well as demonstrate a versatile experimental setup to directly measure the shifts. The giant shifts demonstrated could prove to be useful in enhancing the sensitivity of experiments ranging from atomic force microscopy to gravitational wave detection.

Combining structural and chemical information at the nanometer scale by correlative transmission electron microscopy and atom probe tomography.

In many cases, the three-dimensional reconstructions from atom probe tomography (APT) are not sufficiently accurate to resolve crystallographic features such as lattice planes, shear bands, stacking faults, dislocations or grain boundaries. Hence, correlative crystallographic characterization is required in addition to APT at the exact same location of the specimen. Also, for the site-specific preparation of APT tips containing regions of interest (e.g. grain boundaries) correlative electron microscopy is often inevitable. Here we present a versatile experimental setup that enables performing correlative focused ion beam milling, transmission electron microscopy (TEM), and APT under optimized characterization conditions. The setup was designed for high throughput, robustness and practicability. We demonstrate that atom probe tips can be characterized by TEM in the same way as a standard TEM sample. In particular, the use of scanning nanobeam diffraction provides valuable complementary crystallographic information when being performed on atom probe tips. This technique enables the measurement of orientation and phase maps as known from electron backscattering diffraction with a spatial resolution down to one nanometer.

A flexible experimental setup for femtosecond time-resolved broad-band ellipsometry and magneto-optics.

A versatile experimental setup for femtosecond time-resolved ellipsometry and magneto-optical Kerr effect measurements in the visible light range is described. The apparatus is based on the pump-probe technique and combines a broad-band probing beam with an intense near-infrared pump. According to Fresnel scattering matrix formalism, the analysis of the reflected beam at different polarization states of the incident probe light allows one to determine the diagonal and the off-diagonal elements of the dielectric tensor in the investigated sample. Moreover, the pump-probe method permits to study the dynamics of the dielectric response after a short and intense optical excitation. The performance of the experimental apparatus is tested on CrO2 single crystals as a benchmark.

Gas-phase volatile organic chloride electroreduction: A versatile experimental setup for electrolytic dechlorination and voltammetric analysis

Silver is a well-known and largely studied electrocatalytic material for (hydro)dehalogenation reactions of organic halides, a class which includes several priority pollutants. Silver nanoparticles are particularly attractive since exhibit similar or even better performances than bulk silver allowing a significant reduction of precious metal loading. In this study the hydrodehalogenation of CHCl3 is selected as model reaction in order to evaluate the electrocatalytic activity of 2–15nm silver nanoparticles. For the electrochemical characterization a versatile experimental setup was purportedly in-house designed and assembled that allows both cyclic voltammetry and electrolysis investigations. All the tests are performed in aqueous solution using a gas diffusion electrode as working cathode. The progressive conversion of gaseous trichloromethane to less chlorinated compounds is quantitatively evaluated in terms of concentration Cl− ions produced in the aqueous electrolyte solution.