Experimental Characterization Research Articles

Stability Assessment in Aqueous and Organic Solvents of Metal-Organic Framework PCN 333 Nanoparticles through a Combination of Physicochemical Characterization and Computational Simulations.

Mesoporous metal-organic frameworks (MOFs) have been recognized as powerful platforms for drug delivery, especially for biomolecules. Unfortunately, the application of MOFs is restricted due to their relatively poor stability in aqueous media, which is crucial for drug delivery applications. An exception is the porous coordination network (PCN)-series (e.g., PCN-333 and PCN-332), a series of MOFs with outstanding stability in aqueous media at the pH range from 3 to 9. In this study, we fabricate PCN-333 nanoparticles (nPCN) and investigate their stability in different solvents, including water, ethanol, and methanol. Surprisingly, the experimental characterizations in terms of X-ray diffraction, Brunauer-Emmett-Teller (BET), and scanning electron microscopy demonstrated that nPCN is not as stable in water as previously reported. Specifically, the crystalline structure of nPCN lost its typical octahedral shape and even decomposed into an irregular amorphous form when exposed to water for only 2 h, but not when ethanol and methanol were used. Meanwhile, the porosity of nPCN substantially diminished while being exposed to water, as demonstrated by the BET measurement. With the assistance of computational simulations, the mechanism behind the collapse of PCN-333 is illuminated. By molecular dynamics simulation and umbrella sampling, we elucidate that the degradation of PCN-333 occurs by hydrolysis, wherein polar solvent molecules initiate the attack and subsequent breakage of the metal-ligand reversible coordination bonds.

Experimental characterization of indented dry connections for precast double‐curved concrete shells

Experimental characterization of indented dry connections for precast double‐curved concrete shells

Experimental characterization and numerical analysis of 3D woven preforms torsional deformation

Experimental characterization and numerical analysis of <scp>3D</scp> woven preforms torsional deformation

Single-Step PECVD Synthesis of Graphene@Carbon Nanotubes Electrocatalyst.

Graphene (Gr) and carbon nanotubes (CNTs), the two intriguing carbon nanomaterials, have presented great potential in serving as high-performance electrocatalysts in lithium-sulfur (Li-S) chemistry. The concurrent management of both materials would achieve a promoted synergistic effect. Nevertheless, there still remains a lack of an effective material synthesis route. Herein, a single-step plasma-enhanced chemical vapor deposition (PECVD) strategy is devised to prepare Gr@CNTs heterostructures with strong bonded connections. In the PECVD system, the damaged sidewalls generated in CNT tubes can serve as appropriate nucleation sites for further Gr growth. The formation mechanisms are thoroughly explored in aspects of both experimental characterizations and theoretical calculations. To confirm the validity of this approach, thus-constructed Gr@CNTs architectures are employed as the sulfur host, enabling boosted redox kinetics of polysulfides. This project provides fundamental insight into the mechanism exploration for single-step PECVD growth of Gr@CNTs heterostructure, hence promoting the practical application prospect of carbon nanomaterials toward Li-S systems.

Thermomechanical behavior of alumina–magnesia castables and numerical modeling of the steel ladle thermal process

AbstractBy experimental characterization and numerical modeling, the dependence of thermophysical properties on time and temperature as well as its influence on the thermomechanical behavior of alumina–magnesia castables has been studied in this work. The thermal conductivity, thermal expansion coefficient, and Young's modulus are the most important parameters, which evolve with temperature and piecewise change with the thermal processes of drying, preheating, and service. It is mainly related to the sintering degree and amount of formed calcium aluminate and spinel phases. The sensitivity analysis of parallel simulations for multilayer steel ladle with different numbers of temperature‐dependent thermophysical parameters demonstrates that the thermal conductivity is the most influential parameter, as it dominates the temperature distribution and affects the succeeding thermal expansion as well as deformation. The increase of thermal expansion coefficient and decrease of Young's modulus with temperature counterbalance the deformation of linings under thermal process. Meanwhile, compared with the simulation using temperature‐independent parameters, the model with temperature‐dependent thermophysical parameters exhibits more severe damage in outer surface of both the working lining and the permanent lining. This gives new insight into the adoption of temperature‐dependent parameters for actual thermomechanical behavior evaluation of refractories.

Hydrogen Spillover Mechanism of Superaerophobic NiSe2‐Ni5P4 Electrocatalyst to Promote Hydrogen Evolution in Saline Water

AbstractThe hydrogen spillover mechanism of metal‐supported electrocatalyst can significantly improve HER activity. However, the rational design of binary heterojunction hydrogen spillover electrocatalysts remains a challenge. Here, a NiSe2‐Ni5P4 heterojunction electrocatalyst with superaerophobic structure is synthesized by using a simple substrate self‐derived strategy. Experimental characterization and theoretical calculation reveal the hydrogen spillover mechanism of NiSe2‐Ni5P4 heterogeneous electrocatalyst. NiSe2 and Ni5P4 synergistically promote the adsorption/dissociation of H2O and the adsorption of H*, respectively. The smaller ΔΦ effectively reduced the electron density at the interface, weakening the proton adsorption at the interface and promoting the migration of H* from NiSe2 to Ni5P4. The NiSe2‐Ni5P4 exhibits excellent HER activity in alkaline electrolyte, requiring only a potential of 65, 270 mV to achieve a current density of 10, 500 mA cm−2, respectively, and a stability of up to 200 h. Moreover, the design of NiSe2‐Ni5P4 with superaerophobic structure can reduce the deposition of impurity ions on the electrode surface and avoid Cl− corrosion of the electrode, which results in NiSe2‐Ni5P4 showing better HER activity and stability than commercial Pt/C in brackish water. This study deepens the understanding of hydrogen spillover mechanism of binary heterojunction electrocatalysts, broadens the application of hydrogen production in complex water quality.

Degradation Mechanism and Enhanced Stability of Organolithium for Chemical Lithiation

AbstractOrganolithium solutions, especially Li‐arene solutions (LASs) with high reactivity and controllable redox potentials, have gained significant attention because of their wide applications in chemical lithiation, liquid anodes, and battery recycling. However, the sudden loss of reactivity when stored or applied at room temperature is still puzzling and inhibits the application of LASs. In this work, the degradation mechanism of LASs is fully investigated and revealed by combining various experimental characterization and computational simulations. A hierarchical reaction mechanism for lithium biphenyl/2‐methyl tetrahydrofuran (Li‐Bp‐2MT), a lithiation solution used for most anodes, explains degradation and side product formation. Specifically, the dimerization of the active component Li1Bp[2MT]1 forms an inactive dimer that is irreversibly reduced in the presence of locally accumulated highly reductive Li0. This reaction mechanism reveals the atomic origins of lithiation solution deactivation and accounts for all solid and gaseous byproducts. LiH is identified as the dominating solid byproduct, indicating irreversible destruction of the active components and facilitating side reactions producing H2 and CH4. Based on reaction mechanism insights, modifying molecular interactions and reaction kinetics are experimentally shown to inhibit Li0 aggregation kinetics, enhancing long‐term prelithiation performance. This research provides comprehensive guidelines for practical applications of LASs.

Reinforced Nacre-Like MXene/Sodium Alginate Composite Films for Bioinspired Actuators Driven by Moisture and Sunlight.

MXene-based soft actuators have attracted increasing attention and shown competitive performance in various intelligent devices such as supercapacitors, bionic robots and artificial muscles. However, the development of robust MXene-based actuators with multi-stimuli responsiveness remains challenging. In this study, a nacre-like structure soft actuator based on MXene and sodium alginate (SA) composite films is prepared using a straightforward solvent casting self-assembly method, which not only enhances the mechanical performance (tensile strength of 72MPa) but also diversifies the stimuli responsiveness of the material. The composite actuators can be powered by external stimuli from renewable energy sources, from moisture inducing a maximum bending angle of 190 degrees at a relative humidity (RH) of 91%, and sunlight irradiation generating a maximum curvature of 1.45 cm-1 under 100mW cm-2. The feasibility of practical applications, including moisture-responsive flowers and walkers, sunlight-responsive oscillators, and smart switches, is demonstrated through comprehensive experimental characterization and performance evaluation. The work presented here provides insight into the design of robust actuators via the utilization and conversion of environmentally renewable energy sources.

Experimental characterization and thin-layer convective drying modeling of Jamun (Indian Blackberry) slices

Experimental characterization and thin-layer convective drying modeling of Jamun (Indian Blackberry) slices

Poroelasticity and acoustic properties of bio-based materials : from characterization to the understanding of mechanical dissipation effects

The building sector is a key element in reducing the effects of climate change. To operate sustainably and efficiently, solutions based on building materials having a low environmental impact, such as bio-based materials, are needed. In fact, they present high-level multi-functional properties and they capture atmospheric carbon dioxide. However, even if a number of works has examined visco-thermal dissipation effects, the understanding of the mechanical dissipation effects on the acoustic performances of bio-based materials is still incomplete and little data are available in the literature. Therefore, it seems particularly relevant to investigate by experimental characterizations and modelling methods the effects of mechanical dissipation on the acoustic properties of a representative variety of bio-based materials such as vegetal wools, vegetal aggregate stacks and vegetal concretes. To do this, Young's modulus, Poisson's ratio and structural damping were measured on the various typology of materials by a quasi-static analysis method. The non-linear elastic behaviour in compression of bio-based samples is analyzed. Finally, the influence of Young's modulus and structural damping on the acoustic absorption and attenuation properties of bio-based materials is described using modelling approaches.

Vibration reduction of an electric vehicle heat exchanger by controlling the polarization of its ferroelectric ceramics

The growing requirements in terms of CO2 emissions reduction in transports renders necessary the development of new electric traction technologies. This results in new technical constraints for equipment manufacturers, forcing them to reduce the acoustic emissivity of their new products inside and outside vehicles. Heat exchangers for electric cars are part of this new product category. High voltage supplied by the battery of electrical vehicles requires introduction of a new energy conversion process and technology. To this end, components based on ceramics containing barium titanate (BaTiO3) with high electrocaloric coupling properties are selected to provide the heating function. Baryum titanate is ferroelectric. This category of materials is subjected to piezoelectric and electrostrictive effects. The vibrations induced in the components (rods) containing the BaTiO3 ceramics are transmitted through the system, and cause undesired acoustic radiation. This coupling is a suffered effect and is not taken into account in the integration process during the rods manufacturing. In this study, an experimental characterization is proposed to identify the involved electromechanical coupling coefficients. Numerical simulations of the vibrations induced by BaTiO3 are carried out and used to study the possibility of attenuating them by controlling the polarisation of the ceramics or by geometric modifications.

Predicting the impact of wind turbine noise: general overview and results of the PIBE project

The PIBE project aims to improve wind turbine noise prediction methods and to explore new solutions for noise reduction. This five years project brought together French experts in aeroacoustics, sound propagation, experimental noise characterization and wind engineering, and was structured around three work packages. The first one aimed to study amplitude modulation phenomena and focused particularly the characterization of dynamic stall noise. Specific aerodynamic and acoustic measurements were carried out in a wind tunnel, showing the influence of several stall regimes on noise production. The second work package focused on quantifying the uncertainties of noise prediction methods. It developed an open-access online application (WindTUNE) that quantifies uncertainties on noise prediction of a wind farm, and a parametric and uncertainties calculation tool for the engineering application Code-TYMPAN. This axe also produced an open-access database of a 400 days campaign of meteorological and acoustical measurements around a wind farm. The last work package investigated new noise reduction devices using blades with modified leading and/or trailing edges. The efficiency of the solutions were characterized in a wind tunnel, both acoustically and aerodynamically. The paper presents the main results obtained at the end of the project.

An innovative approach for enclosure design of power generators to meet noise regulation targets

The use of diesel-powered engine generators as a power source is very common for various industrial and residential applications. There are strict regulatory requirements and legislations to limit the noise levels from these generators below statutory limits. The purpose of the paper is to present an approach using statistical energy analysis (SEA) augmented by experimental inputs for the prediction of noise levels for the generators and propose strategies for optimized enclosure design that effectively mitigate noise to achieve regulatory requirements. The study begins by developing an SEA model that represents the acoustic behavior of the generator and enclosure. The airborne sources such as engine, alternator, radiator fan and exhaust are modelled explicitly using experimental noise source characterization. Based on the established SEA model and excitation sources, noise levels are predicted through the calculation of energy flow between subsystems. The predicted sound levels for an existing Diesel Generator with enclosure were validated with its test data to ensure correctness of SEA model. Parametric studies were carried out using simulations on key variables, including critical noise paths, panel thickness, and noise control treatments. These investigations helped identify optimal process parameters that reduce noise levels emitted by genset in adherence to noise regulations.

Acoustic characterization of a bi-directional turbine

A thermoacoustic engine converts thermal energy into acoustic energy, which can then be converted into electricity using an alternator. The conversion of acoustic-to-electric energy in thermoacoustic electricity generators usually relies on electromagnetic transducers. A bi-directional turbine coupled to a DC motor offers a plausible alternative due to its simplified mechanical design, cost-effectiveness, and relatively good performance. Efficient coupling of a bi-directional turbine with a thermoacoustic engine requires a comprehensive understanding of its operating behavior. This study aims to extend existing research by carrying out experimental characterization of a bi-directional turbine. This will involve measuring its transfer matrix and impedance under various acoustic conditions. The experimental results are then analyzed and compared with the predictions of an electro-acoustic model.

Uncertainties in numerical predictions and experimental characterization of wind farm noise

Wind Turbine Noise (WTN) variability is often related to the influence of local micrometeorology as well as to space and time variations in the ground properties. Thus, the PIBE Project (2020-2024) aims to estimate these variabilities and their associated uncertainties. Its objective is to enable engineering companies or wind farm developers to estimate more accurately the risk of noise. In the WP2 of the PIBE project, 3 approaches are explored: (i) a NUMerical approach through the development of a metamodel, (ii) an EXPerimental approach through a major in-situ measurement campaign lasting more than 1 year, and (iii) a STATistical approach consisting in the evaluation of WTN variability. The NUM approach consists in sound emission calculation of each wind turbine using the Amiet's theory, and sound propagation calculation using a wide-angle Parabolic Equation (WAPE) modelling. The EXP part of the PIBE project has led to the development of a large database, accessible via a dedicated Shiny application. The last approach (STAT) has been carried out using both an open-access online tool called WindTUNE and an open-source tool based on Code_TYMPANTM, namely OCP. The 3 approaches (NUM + EXP + STAT) are presented and the corresponding results are discussed.

Effect of relative humidity on the interlayer spacing of phosphate intercalated Mg, Al layered double hydroxide (hydrotalcite‐like) crystals

AbstractThe availability of water and the type of interlayer anions present affect the arrangement and interlayer spacing of layered double hydroxide (LDH). A systematic study of the effect of relative humidity (RH) on the basal spacing of phosphate intercalated, magnesium aluminum LDHs (MgAl–PO4 LDH) was conducted, confirming that MgAl‐PO4 LDH exhibit distinct interlayer spacing corresponding to separate low‐ and high‐hydration states produced when exposed to low and high humidity conditions. The transition from the low‐ to high‐hydration form begins when RH exceeds 33% and is accompanied by the transition from one to two interlayers of water. An improved understanding of the effect of RH on MgAl–PO4 LDHs will enable more accurate atomistic modeling and experimental characterization of MgAl–PO4 LDHs and may lead to improvements in the tunability of MgAl‐PO4 LDHs for commercial applications such as slow‐release fertilizer.

Experimental characterization of stall noise on a pitching airfoil in an anechoic wind tunnel

Dynamic stall noise is one of the potential source of amplitude modulations associated with wind turbine noise. This phenomenon is related to the periodic separation and reattachment of the boundary layer on the wind turbine blade suction side during its rotation. Within the framework of the PIBE project (Predicting the Impact of Wind Turbine Noise), experiments were conducted in an anechoic wind tunnel in order to characterize stall noise on a pitching airfoil in both static and dynamic conditions. A first set of measurements was performed using an airfoil equiped with pressure taps to measure both steady and unsteady wall pressure as well as far-field acoustic pressure. These measurements were used to identify the noise regimes associated with different angles of attack, and to relate them with the boundary layer evolution. In a second experiment, synchronized flow and acoustic measurements have been obtained to identify the coherent aerodynamic structures responsible for the noise radiation. The velocity fluctuations evaluated from the time-resolved particle image velocimetry (TR-PIV) data are correlated with acoustic pressure to localize aeroacoustic sources, and various tools such as vortex detection methods and spectral proper orthogonal decomposition are applied to identify the nature of these sources.

Metagratings for underwater acoustic wavefront manipulation

Metagratings are flat periodic assemblies of small scatterers, engineered to achieve effects such as steering, beamforming, or absorption. They have recently received attention in both electromagnetism and acoustic fields. In this work, we report the design, modeling, and experimental characterization of metagratings to steer underwater acoustic wavefronts towards anomalous directions (i.e. not classically allowed by Snell-Decartes relationships) with high efficiency (close to 100%). They are build from simple assemblies of small brass cylinders, hold by 3D-printed plastic supports, and can redirect ultrasonic wavefronts either in reflection mode (when placed in front of a reflective surface like e.g. the water / air interface) or in transmission mode. Furthermore, we demonstrate how metagratings build from an asymmetrical pattern of multiple basic elements can achieve near perfect asymmetrical transmission: a wavefront incident from side of the structure is fully transmitted, while a similar wavefront incoming from the other side is fully reflected, achieving an acoustic one-way mirror effect. This work combine theoretical analysis, finite element modeling, and experimentation in water tanks to explore and demonstrate the potential of such metagratings for various applications in underwater acoustics, like communication, noise mitigation, and stealth.

Experimental characterization of the effective acoustic properties of anisotropic porous materials via free-field measurements

Porous media are commonly described as effective isotropic fluid materials, such that their acoustic properties can be adequately determined from their bulk modulus and dynamic density. Most acoustic absorbents, however, possess a marked anisotropy, which influences their acoustical behavior and the parameters necessary to deduce it. Specifically, the influence of anisotropy translates into a full symmetric density tensor (in place of a scalar). This study presents a method for retrieving the bulk modulus and all six components of the density tensor of a layer of porous material from reflection coefficients measured in free field with an array of microphones. The procedure consists in expressing the sound field measured in the vicinity of the layer as a superposition of plane waves, from which the surface impedance and the reflection coefficient are reconstructed. The reflection properties, as well as the pressure at the rigid backing interface, are estimated for various source positions (i.e., various angles of incidence) and an inverse problem is formulated to infer the effective fluid parameters. The validity of the method is examined experimentally on a manufactured porous material, and the resulting fluid parameters compared with experimental results obtained from reflection and transmission coefficients measured in an impedance tube.

Experimental FTIR characterization of kidney stones, DFT analysis of CaC2O4 and its interactions with lysozyme

Experimental FTIR characterization of kidney stones, DFT analysis of CaC2O4 and its interactions with lysozyme