Pulsed Method Research Articles

PVD decorative coatings on polycarbonate and polyamide substrates for the automotive industry

Utilizing magnetron sputtering to incorporate metal onto polymer surfaces as a substitute for metal parts in the automobile industry offers an eco-friendly alternative. In this work, decorative titanium oxynitride (TiNxOy) coatings were sputter deposited over polycarbonate and polyamide 12 substrates using a low-temperature pulsed deposition method. In order to improve coating adhesion, all substrate surfaces were pre-treated for 30 s by reactive plasma etching. Four different film thicknesses were investigated to achieve various colours. The TiNxOy coatings were quasi-amorphous, and the oxygen content decreased with increasing film thickness. Overall, four distinct colours - green, purple, magenta, and blue - were produced, and all coatings showed excellent adhesion to the polymeric substrates. Colour fastness was assessed using adapted pin-on-disk tests to evaluate the film's applicability as decorative coatings for automotive parts, with all films achieving high ratings for colour fastness. This study provides insights into the deposition of thin films on polymeric substrates, showcasing successful approaches to achieve desired colours while preserving the film's optical properties after color fastness testing.

Enhancing the Kinetics of Vapor-based Polymerization by Pulsed Filament Approach.

Initiated chemical vapor deposition is a versatile technique for synthesizing conformal polymer films on both planar and porous surfaces. It can retain functional groups and avoid undesired cross-linking. However, there is still room for enhancing its performance without altering the feed parameters. Here, we investigate a pulsed iCVD approach to improve the deposition process, achieved by switching on and off the resistively heated filament periodically. By strategically switching off the filament, a shortage of thermally activated primary radicals was created, which allowed uninterrupted chain propagation with fewer termination reactions and potentially increased monomer conversion rates. This has caused significantly faster deposition kinetics with a higher molecular weight and longer chain length for poly(glycidyl methacrylate) compared to continuous deposition. Spectra analyses confirmed that the functionality and stoichiometry ratios remained intact throughout the pulsed deposition process. The pulsed iCVD method is therefore a competitive and sustainable tool, demonstrating fast deposition kinetics and a well-preserved functionality.

Pulsed-Mode Magnetic Field Measurements with a Single Stretched Wire System.

In synchrotrons, accurate knowledge of the magnetic field generated by bending dipole magnets is essential to ensure beam stability. Measurement campaigns are necessary to characterize the field. The choice of the measurement method for such campaigns is determined by the combination of magnet dimensions and operating conditions and typically require a trade-off between accuracy and versatility. The single stretched wire (SSW) is a well-known, polyvalent method to measure the integral field of magnets having a wide range of geometries. It, however, requires steady-state excitation. This work presents a novel implementation of this method called pulsed SSW, which allows the system to measure rapidly time-varying magnetic fields, as is often needed, to save power or gain beam time. We first introduce the measurement principle of the pulsed SSW, followed by a combined strategy to calculate the absolute magnetic field by incorporating the classic DC SSW method. Using a bending magnet from the Proton Synchrotron Booster located at the European Organization for Nuclear Research as a case study, we validate the pulsed SSW method and compare its dynamic measurement capabilities to a fixed induction coil, showing thereby how the coil calibration must be adjusted according to the field level. Finally, we assess the method's measurement accuracy using the standard SSW as a reference and present an analysis of the primary noise contributors.

Interface charge accumulation in bi-layer dielectrics between cable and accessory insulation under temperature gradient

Bi-layer dielectrics are a feature of high-voltage direct-current cable and accessory systems, giving rise to the interfaces between the cable and accessory insulation. The interfaces act as preference sites for space charge build-up and are therefore regarded as potential breakdown initiation sites. A further complication is that during the operation of cable, a temperature gradient (TG) will be produced across the bi-layer insulation. In this paper, carbon black (CB) nanoparticles with 0, 0.5, 1, 1.5, 3.5 and 5.5 wt% are doped into silicon rubber (SR), space charge distributions in bi-layer dielectrics composed of cross-linked polyethylene (XLPE) and CB/SR nanocomposites under DC voltage and TG are measured using the pulsed electroacoustic method, and the effects of the doping proportion of CB nanoparticles and the TG on the bi-layer interface charge behavior are investigated. The experimental results show that under the TG, CB nanoparticles doped into SR can effectively suppress the interface charge accumulation, the amount of the interface charge decreases with the increase of the doping proportion from 0 to 1.5 wt% but increases with the increase of the doping proportion from 1.5 to 5.5 wt%, and the CB nanoparticle with 1.5 wt% shows relatively better suppression effect on the interface charge accumulation. With the increase of the TG, the amount of the interface charge increases initially and then decreases.

Secondary electron emission yield in thick dielectric materials: a comparison between Kelvin probe and capacitive methods

The recent high demand of secondary electron emission yield (SEY) measurements in dielectric materials from space industry has driven SEY laboratories to improve their facilities and measurement techniques. SEY determination by the common capacitive method, also known as pulsed method, is well accepted and has given satisfactory results in most cases. Nevertheless, the samples under study must be prepared according to the experimental limitations of the technique, i.e. they should be manufactured separated from the devices representing faithfully the surface state of the own device and be as thin as possible. A method based on the Kelvin probe (KP) is proposed here to obtain the SEY characteristics of electrically floating Platinum, Kapton and Teflon placed over dielectric spacers with thicknesses ranging from 1.6 to 12.1 mm. The results are compared with those of the capacitive method and indicate that KP SEY curves are less sensitive to spacer thickness. An explanation based on the literature is also given. In all, we have established that KP is better suited for the analysis of dielectric samples thicker than 3 mm.

Sensitivity and perturbation analysis of alpha-eigenvalue with time-dependent Monte Carlo perturbation techniques

Sensitivity analysis and perturbation calculation methods for prompt neutron decay constants α using the Monte Carlo method, such as iterative fission probability (IFP), differential operator sampling (DOS), and correlated sampling (CS), have been proposed thus far. However, these methods require a significant amount of memory storage. The method developed in this study applies DOS and CS techniques during a time-dependent Monte Carlo simulation for the pulsed neutron method in subcritical systems. The time variation of the neutron flux is fitted to an exponential function during the time range when the flux decays with the fundamental mode α. By applying the least squares method to the results of time-dependent DOS and CS, the sensitivity coefficients with respect to nuclear data and the change in α due to perturbation can be calculated. In contrast to the existing methods that require storing the total fission or time sources per generation over several (∼10) generations, the proposed method only needs to store the weighting coefficient of a single source particle until it dies. The additional memory storage per parameter is comparable to that of conventional time-dependent Monte Carlo simulations and much less than that of existing methods. Numerical tests for the proposed method have demonstrated the accuracy and usefulness of the time-dependent DOS and CS methods.

Identification of interfacial strength between carbon fiber and epoxy matrix in CFRP laminates using pulse laser spallation method

Carbon fiber reinforced plastics (CFRP) have high specific strength and specific stiffness and are used in various fields such as aircraft, space structures, automobiles, and other transportation equipment. Since the internal structure of CFRP is very complex, it is very difficult to define failure criteria when external loads are applied. Various methods have been proposed to evaluate the interfacial shear strength between carbon fiber and resin matrix, such as microbond test, rupture test, and pull-out test, but currently no effective method has been proposed to evaluate the tensile strength of the CF/resin interface. In this study, we applied the pulsed laser spallation method, which has been confirmed to be effective for evaluating the adhesion strength of thin films and coating films on substrates, to the evaluation of CFRP. A finite element method based on the Laplace transform was used for the numerical analysis of the unsteady elastodynamic problem. The macroscopic stresses generated by ultrasonic waves excited by pulsed laser irradiation were calculated by inverse analysis using a transfer function with the displacement history of the back surface of the CFRP specimen as supplementary information. Microscopic stresses at the fiber/resin interface were evaluated by the homogenization method, taking into account the effects of fiber arrangement, distance between fibers, and molding residual stress in unidirectionally reinforced CFRP laminates. As a result, this series of investigations revealed that the vertical interfacial stress is dominant with respect to the strength of the fiber/resin interface with the strength of about 54MPa.

The Influence of Bias Voltage on the Structure and Properties of TiZrNbMo Coating Deposited by Magnetron Sputtering

TiZrNbMo coatings have been deposited using the direct current pulsed magnetron sputtering method in an argon atmosphere. The synthesis processes have been conducted under various process parameters. The structure (chemical and phase composition) and mechanical properties of the obtained multicomponent coatings are investigated as a function of plasma modulation frequency (10 Hz and 1000 Hz) and substrate bias (0 to −150 V). It is the case that an increase in the substrate bias decreases the deposition rate and alters the coating’s chemical composition. The latter leads to a Ti concentration decrease and a simultaneous increase in Mo and Nb concentrations in the final coating material. X-ray diffraction measurements indicate a single-phase BCC structure, with grain size decreasing as substrate bias increases. This ultimately forms an amorphous–nanocrystalline structure at −150 V. The mechanical properties of the multicomponent TiZrNbMo coatings have been determined using the nanoindentation method. The maximum values of hardness (13.45 GPa) and elastic modulus (188.6 GPa) are achieved at a substrate bias of −150 V. We also show that the minimum elastic modulus (41.8 GPa) is achieved at an intermediate substrate bias of −100 V.

Interrogation of Oxidative Pulsed Methods for the Stabilization of Copper Electrodes for CO2 Electrolysis.

Using copper (Cu) as an electrocatalyst uniquely produces multicarbon products (C2+-products) during the CO2 reduction reaction (CO2RR). However, the CO2RR stability of Cu is presently 3 orders of magnitude shorter than required for commercial operation. One means of substantially increasing Cu catalyst lifetimes is through periodic oxidative processes, such as cathodic-anodic pulsing. Despite 100-fold improvements, these oxidative methods only delay, but do not circumvent, degradation. Here, we provide an interrogation of chemical and electrochemical Cu oxidative processes to identify the mechanistic processes leading to stable CO2RR through electrochemical and in situ Raman spectroscopy measurements. We first examine chemical oxidation using an open-circuit potential (OCP), identifying that copper oxidation is regulated by the transient behavior of the OCP curve and limited by the rate of the oxygen reduction reaction (ORR). Increasing O2 flux to the cathode subsequently increased ORR rates, both extending lifetimes and reducing "off" times by 3-fold. In a separate approach, the formation of Cu2O is achieved through electrochemical oxidation. Here, we establish the minimum electrode potentials required for fast Cu oxidation (-0.28 V vs Ag/AgCl, 1 M KHCO3) by accounting for transient local pH changes and tracking oxidation charge transfer. Lastly, we performed a stability test resulting in a 20-fold increase in stable ethylene production versus the continuous case, finding that spatial copper migration is slowed but not mitigated by oxidative pulsing approaches alone.

Electro-assisted photothermal synergy for removal of volatile organic compounds over Au single atoms anchored TiO2 nanotubes

Gas-phase photoelectrocatalysis (GPEC) systems for treating gas pollution may lead to a Joule-heat effect and form photothermal synergy under an external bias voltage. However, such a synergistic effect and mechanism remain unclear. Herein, a electro-assisted photothermal synergistic removal of VOCs by defective TiO2 nanotube array decorated with atomically dispersed Au species was chosen as a prototypical illustration. By introducing single Au atoms, the carrier concentration and mobility of the catalytically active layer, i.e., TiO2 nanotube arrays anchored with Au single atoms, were substantially increased to the semi-metal level through an electrochemical reduction step and square-wave pulse method for anchoring single atoms. This not only contributes to the photogenerated carrier separation at low external bias but also significantly enhances the Joule heating effect on the catalyst surface. As a result, the catalyst used exhibited an excellent electro-assisted photothermal synergistic effect and outstanding efficiency in toluene removal in the designed tubular reactor. SynopsisA novel electro-assisted photothermal synergy system was constructed, which combines the advantages of gas-phase photoelectrocatalysis and electrothermal catalysis to remove VOCs with high efficiency and low energy consumption.

Enhancing bacterial inhibition in beetroot beverages: The potent combination of sappan heartwood extracts via accelerated solvent extraction and pulsed electric field methods

This study aimed to investigate the potential of sappan heartwood extract as an inhibitor of foodborne pathogenic bacteria in beetroot juice. The extract was obtained using an accelerated solvent extraction process (using an ethanol/water solvent mixture (3:1 w/w) at 120 °C and 1500 psi for 5 min), yielding 10.04 g per 73.6 g of dried sappan heartwood powder, with a percentage yield of 13.64 and 2.69 % brazilin. The extract was combined with pulsed electric fields (PEF) at different strengths and tested against Escherichia coli (E. coli), Staphylococcus aureus (S. aureus), Bacillus cereus (B. cereus), and Salmonella typhimurium (S. typhimurium). Results showed that the combination of sappan heartwood extract and PEF at 15 kV/cm and concentrations of 3.91, 5.86, and 11.73 mg/mL effectively reduced the total plate count and coliform bacteria count, and completely eliminated B. cereus and S. typhimurium during 7 days of storage at 4 °C. Furthermore, this combination was found to be more efficient in bacterial elimination compared to thermal pasteurization and potassium sorbate addition. These findings suggest that sappan heartwood extract can be used as a natural antimicrobial agent in food products, especially in beetroot juice, where regulatory standards restrict the addition of preservatives. Using sappan heartwood extract in combination with PEF is highly effective in killing foodborne pathogens, reducing the risk of consumer harm and ensuring food safety.

Solving the Annealing of Mo Interconnects for Next‐Gen Integrated Circuits

AbstractRecent surge in demand for computational power combined with strict constraints on energy consumption requires persistent increase in the density of transistors and memory cells in integrated circuits. Metal interconnects in their current form struggle to follow the size downscaling due to materials limitations at the nanoscale, causing severe performance losses. Next‐generation interconnects need new materials, and molybdenum (Mo) is considered the best choice, offering low resistivity, good scalability, and barrierless integration at a low cost. However, it requires annealing at temperatures far exceeding the currently accepted limit. In this work, the challenges of high‐temperature annealing of patterned Mo nanowires are looked into, and a new approach is presented to overcome them. It is demonstrated that while a conventional annealing process improves the average grain size, it can also reduce the cross‐section area, thus increasing the resistivity. Using high‐resolution transmission electron microscopy (TEM) with in situ heating, the evolution of structural features in real time is directly observed. Using insights from these experiments, a cyclic pulsed annealing method is developed, and it is shown that the desired grain structure is achieved in only a few seconds, without forming the surface grooves. These findings can radically facilitate Mo integration, boosting the efficiency of future integrated circuits.

Grain-Boundary Engineering Boosted Undercoordinated Active Sites for Scalable Conversion of CO2 to Ethylene.

The development of highly selective and energy efficient technologies for electrochemical CO2 reduction combined with renewable energy sources holds great promise for advancing the field of sustainable chemistry. The engineering of copper-based electrodes facilitates the conversion of CO2 into high-value multicarbon products (C2+). However, the ambiguous determination of the intrinsic CO2 activity and the maximization of the density of exposed active sites have severely limited the use of Cu for the realization of practical electrocatalytic devices. Here, we report a scalable strategy to obtain a high density of undercoordinated sites by maximizing the exposure of grain-boundary active sites using a direct chronoamperometric pulse method. Our numerical investigations predicted that grain boundaries modulate the adsorption behavior of *CO on the Cu surface, which acts as a key intermediate species associated with the production of multicarbon species. We investigated the consequence of grain-boundary density on dendric Cu catalysts (GB-Cu) by combining transmission electron microscopy, in situ Raman spectroscopy, and X-ray photoelectron spectroscopy with electrochemical measurements. A linear relationship between the Faradaic efficiency of the C2+ product and the presence of undercoordinated sites was observed, which allowed to directly quantify the contribution of the grain boundary in Cu-based catalysts on the CO2RR properties and the formation of multicarbon products. Using a membrane electrode assembly electrolyzer, the high grain-boundary density Cu electrodes achieved a maximum Faradaic efficiency of 73.2% for C2+ product formation and a full-cell energy efficiency of 20.2% at a specific current density of 303.6 mA cm-2. The GB-Cu was implemented in a 25 cm2 MEA electrolyzer and demonstrated selectivity of over 62% for 70 h together with current retention of 88.4% at the applied potential of -3.80 V. The catalysts and electrolyzer were further coupled to an InGaP/GaAs/Ge triple-junction solar cell to demonstrate a solar-to-fuel (STF) conversion efficiency of 8.33%. This work designed an undercoordinated Cu-based catalyst for the realization of solar-driven fuel production.

Study of aging mechanisms in LiFePO4 batteries with various SOC levels using the zero-sum pulse method

Investigating the correlation between aging mechanisms and state of charge (SOC) can optimize cycling conditions and prolong the life cycle of lithium-ion batteries (LIBs). A long-term cycle between a certain SOC range is usually employed to study this correlation. However, this method necessitates a lengthy period, running from months to years, prolonging the research duration significantly. The aging mechanisms obtained through this method are a result of the coupling of various SOC levels; the aging mechanisms at a specific SOC level are not accurately decoupled and analyzable. The proposed Zero-sum pulse method, using symmetrical pulses with small SOC amplitude variations on SOC, can explore aging mechanisms of LIBs at a specific SOC level and reduce the time to less than a week, which significantly expedite the research process. The aging mechanisms at 30%, 50%, 70%, and 90% SOC levels are explored to verify the accuracy and timeliness of this method.

Optical and structural characterization of ZnO:NiO nano composite prepared by pulsed laser deposition method

Optical and structural characterization of ZnO:NiO nano composite prepared by pulsed laser deposition method

Structural and optical properties of Ni-doped ZnO thin films as TCO material, fabricated by pulsed laser deposition method

Thin transparent layers of zinc oxide doped with nickel ions were obtained using the pulsed laser deposition method. The content of nickel ions in the initial solid solution was 1–10 %. The crystallographic structure was studied by X-ray diffraction. Measurements show that the fabricated layer crystallizes in the wurtzite phase and has a dominant orientation along the c-axis. The texture coefficient, grain size, and crystal lattice constants were calculated. The absorption coefficient of the layers was calculated from the transmission spectra of ultraviolet–visible light - near infrared. Photocurrent spectra were investigated. The composition of the layers significantly affects the optical constants. Ni-doped ZnO layers can find applications in optoelectronic devices.

Dynamic convergent shock compression initiated by return current in high-intensity laser–solid interactions

We investigate the dynamics of convergent shock compression in solid cylindrical targets irradiated by an ultrafast relativistic laser pulse. Our particle-in-cell simulations and coupled hydrodynamic simulations reveal that the compression process is initiated by both magnetic pressure and surface ablation associated with a strong transient surface return current with density of the order of 1017 A/m2 and lifetime of 100 fs. The results show that the dominant compression mechanism is governed by the plasma β, i.e., the ratio of thermal pressure to magnetic pressure. For targets with small radius and low atomic number Z, the magnetic pressure is the dominant shock compression mechanism. According to a scaling law, as the target radius and Z increase, the surface ablation pressure becomes the main mechanism generating convergent shocks. Furthermore, an indirect experimental indication of shocked hydrogen compression is provided by optical shadowgraphy measurements of the evolution of the plasma expansion diameter. The results presented here provide a novel basis for the generation of extremely high pressures exceeding Gbar (100 TPa) to enable the investigation of high-pressure physics using femtosecond J-level laser pulses, offering an alternative to nanosecond kJ-laser pulse-driven and pulsed power Z-pinch compression methods.

3D Nanostructured Electrodes Based on Anodic Alumina Templates for Stable Pseudocapacitors

This study investigates the preparation of nickel nanostructured electrodes for the enhancement of supercapacitor performance. The nanostructured electrodes are synthesized using nanoporous anodic alumina (NAA) as a template via the pulsed electrodeposition method. Structural properties are examined using field‐emission scanning electron microscopy, while electrochemical characterization is conducted through cyclic voltammetry (CV) and electrochemical impedance spectroscopy. The results reveal that Ni nanorod arrays can be obtained embedded in the NAA matrix and with electrical contact with the aluminum substrate. On average, the rods are spaced 90 nm apart, with a diameter of 70 nm and a length of 2 μm. The Ni@NAA electrode exhibits an enlarged active area and exceptional electrochemical performance, demonstrating remarkable stability over 5000 cycles of CV at a scan rate of 50 mV s−1. Specific capacitance values exceeding 100 mF cm−2 and maximum charging times of less than 10 min are reported, highlighting its suitability for high‐power energy devices requiring pseudo‐supercapacitance. The study underscores the significance of nanostructured electrodes in advancing energy storage technologies and presents promising prospects for practical applications.

Continuous Wave Ultrasound Testing Techniques

Currently, the primary method employed for ultrasound inspection is based on sending and detecting ultrasound pulses. Typically, pulse-based methods are essentially time-domain back-reflection methods, and the time-of-flight is the main measured parameter. Recently, continuous-wave methods have been developed in the radar and the fiber-optics fields, which demonstrate significantly better spatial resolution, higher signal-to-noise ratio, and ability to detect reflecting objects at very short distances. It is proposed to use the same approach to develop continuous-wave ultrasound inspection systems. The two main differences between the proposed continuous-wave ultrasonic testing and the classical pulsed ultrasound inspection method are: (i) in the continuous-wave ultrasonic testing method, the transmitted and received signals overlap in the time domain, while in the pulsed ultrasound inspection method the transmitted and received signals are separated in the time; and (ii) in the pulsed ultrasound inspection method the most important parameter is the time delay between the transmitted and received signals, while in the continuous-wave ultrasonic testing method the most informative parameters are the frequency and phase changes in the received signal in respect to modulated transmitted signal. This allows for additional flexibility in the continuous-wave ultrasonic measurements, through control of the frequency modulation. Also, the continuous-wave ultrasonic method potentially offers improved detection range and resolution; improved signal-to-noise ratio due to better energy efficiency and easier filtering; and reduced requirements on the voltage applied to the transducer, which in turn allows the use of simplified low-cost electronics. The theoretical basis of several continuous-wave ultrasound inspection technique is explained, and their advantages and limitations are discussed. Implementation of several prototype continuous-wave ultrasound testing systems is presented. Examples of the use of the systems for non-destructive testing are described.

Influence of Laser Energy on the Structural and Optical Properties of Sn Nanoparticles produced with Laser-Induced Plasma

This study aimed to investigate the structure and optical properties of Sn nanostructures. Thin tin (Sn) films were deposited on glass substrates using the pulsed laser deposition method. Nd:YAG laser with fundamental wavelengths of 532 nm and 1064 nm was used to create Sn nanostructures with varying energies of 400 mJ to 700 mJ and the same frequency of 6 Hz. The tin powder was compressed into a disc with a one-centimetre diameter to serve as a sample. The X-ray diffraction (XRD) pattern showed a crystalline structure with several Sn nanostructures peaks at various energies (400–700 mJ). The results revealed a crystalline size of 65.90 nm and 86.55 nm at 700 mJ, while the size was 40.19 nm and 17.19 at 400 mJ for the given wavelengths (532nm and 1064 nm), respectively. The appearance of Sn nanostructures and the aggregation of, particularly in the form of cauliflower, were revealed in Field emission scanning electron microscopy (FE-SEM) images. The results of the dispersive energy X-ray spectroscopy (EDS) analysis showed that various amounts of tin, carbon, and oxygen were present. Additionally, the optical characteristics were investigated of each film using absorbance spectra, which covered a range of wavelengths from 190 to 1100 nm. As the laser power increased, the band gap energy values in the optical properties decreased, falling into the ranges of 3.06 to 1.65 eV and 3.22 to 1.82 eV at 1064nm and 532nm, respectively.