Multilayer Samples Research Articles

Magnetic force microscopy: High quality-factor two-pass mode

Magnetic force microscopy (MFM) is a well-established technique in scanning probe microscopy that allows for the imaging of magnetic samples with a spatial resolution of tens of nm and stray fields down to the mT range. The spatial resolution and field sensitivity can be significantly improved by measuring in vacuum conditions. This improvement originates from the higher quality-factor (Q-factor) of the cantilever’s oscillation in vacuum compared to ambient conditions. However, while high Q-factors are desirable as they directly enhance the magnetic measurement signal, they pose a challenge when performing standard MFM two-pass (lift) mode measurements. At high Q-factors, amplitude-based topography measurements become impossible, and the MFM phase response behaves non-linearly. Here, we present a modified two-pass mode implementation in a vacuum atomic force microscope that addresses these issues. By controlling the Q-factor in the first pass and using a phase-locked loop technique in the second pass, high Q-factor measurements in vacuum are enabled. Measuring the cantilever’s frequency shift instead of the phase shift eliminates the issue of emerging nonlinearities. The improvements in MFM signal-to-noise ratio are demonstrated using a nano-patterned magnetic sample. The elimination of non-linear responses is highlighted through measurements performed on a well-characterized multilayer reference sample. Finally, we discuss a technique that avoids topography-induced artifacts by following the average sample slope. The newly developed, sensitive, and distortion-free high quality-factor two-pass mode has the potential to be widely implemented in commercial setups, facilitating high-resolution MFM measurements and advancing studies of modern magnetic materials.

Circumventing cracking in grading 316L stainless steel to Monel400 through compositional modifications in directed energy deposition

In joining Fe-alloys and Cu-containing alloys to access the high strength of steels and corrosion resistance of Cu-alloy, cracking is widely observed due to the significant Cu microsegregation during the solidification process, resulting in an interdendritic Cu-rich liquid film at the end of solidification. By fabricating functionally graded materials (FGMs) that incorporate additional elements like Ni in the transition region between these terminal alloy classes, the hot cracking can be reduced. In the present work, the joining of stainless steel 316L (SS316L) and Monel400 by modifying the Ni concentration in the gradient region was studied. A new hot cracking criterion based on hybrid Scheil-equilibrium approach was developed and validated with monolithic multi-layer samples within the SS316L-Ni-Monel400 three-alloy system and a SS316L to 55/45 wt% SS316L/Ni to Monel400 FGM sample fabricated by direct energy deposition (DED). The new hot cracking criterion, based on the hybrid Scheil-equilibrium approach, is expected to help design FGM paths between other Fe-alloys and Cu-containing alloys as well.

Determining Bandgaps in the Layered Group‐10 2D Transition Metal Dichalcogenide PtSe2

AbstractUnlike traditional group‐6 transition metal dichalcogenides (TMDs), group‐10 TMDs such as PtSe2 and PdTe2 possess highly tuneable indirect bandgaps, transitioning from semiconducting in the near‐infrared to semimetal behavior with a number of monolayers (MLs). This opens up the possibility of TMD‐based mid‐infrared and terahertz optoelectronics. Despite this large potential, the optical properties of such materials have shown an extremely large disparity between that predicted and measured. For example, simulations show that a few MLs is required for the semiconductor–semimetal transition, whilst tens of MLs is found experimentally. This is a result of widely used optical extrapolation methods to determine bandgaps, such as the Tauc plot approach, that are not adapted here owing to i) nearby direct transitions, ii) the material dimensionality and iii) large changes in the non‐parabolic bandstructure with MLs. Here, uniquely combining optical ellipsometry to determine the complex permittivity, terahertz time resolved spectroscopy for the complex conductivity and in‐depth density functional theory (DFT) simulations, it is shown that the optical properties and bandstructure can be determined reliably and demonstrate clearly that the semiconductor‐semimetal transition occurs for PtSe2 layers ≈5 MLs. The microscopic origins of the observed transitions and the crucial role of the Coulomb interaction for thin semiconducting layers, and that of interlayer van der Waals forces for multilayer semimetallic samples are also demonstrated. This work of combining complimentary experimental techniques and extensive simulations avoids the application of constrained extrapolation methods to determine the optical properties of group‐10 TMDs, and will be of importance for future mid‐infrared and terahertz applications.

Attainment of high critical current in thick BaZrO3-doped YBa2Cu3O7 multilayer nanocomposite films

High critical current (Ic) in high magnetic fields (B) with minimal variations with respect to the orientation of the B field is demanded by many applications such as high-field magnets for fusion systems. Motivated by this, this work studies 6 vol. % BaZrO3/YBa2Cu3O7 (BZO/YBCO) multilayer nanocomposite films by stacking two 10 nm thick Ca0.3Y0.7Ba2Cu3O7 (CaY-123) spacers with three BZO/YBCO layers of thickness varied from 50 to 330 nm to make the total film thickness of 150–1000 nm. The Ca diffusion from the spacers into BZO/YBCO was shown to dramatically enhance pinning efficiency of c-axis aligned BZO nanorods, which yields high and almost thickness independent critical current density (Jc) in the BZO/YBCO multilayer nanocomposite films. Remarkably, enhanced Jc was observed in these multilayer samples at a wide temperature range of 20–80 K and magnetic fields up to 9.0 T. In particular, the thicker BZO/YBCO multilayer films outperform their thinner counterparts in both higher value and less anisotropy of Jc at lower temperatures and higher fields. At 20 K and 9.0 T, Ic is up to 654 A/cm-width at B//c in the 6% multilayer (1000 nm) sample, which is close to 753 A/cm-width at B//ab due to the intrinsic pinning. This result illustrates the critical role of the Ca cation diffusion into the YBCO lattice in achieving high and isotropic pinning in thick BZO/YBCO multilayer films.

Multi-spectroscopic characterization system for cultural heritage materials analysis (SYSPECTRAL): Conception and example

A comprehensive understanding of chemical composition of cultural heritage materials usually requires several complementary analytical techniques. Given the fragility and value of artworks, minimizing or avoiding sampling and performing in situ analysis under ambient light is an important goal. This article outlines a novel prototype designed to merge LIBS, laser-induced fluorescence spectroscopy (LIF), Raman spectroscopy using a single pulsed laser, and reflectance spectroscopy in a multi-spectroscopic characterization system for cultural heritage analysis (SYSPECTRAL). The aim is to analyze cultural heritage materials in their original place, obtaining both elemental and molecular information at such same point that is not always insured with several separated experimental settings. The SYSPECTRAL system focuses on compactness, mobility, and ease of operation. Software designed for the prototype controls multi-spectroscopic measurements, allows for image capture, precise localization, and data acquisition. Reflectance spectra examined the material and colors at the surface, and the LIBS-LIF-Raman package examines the stratigraphic structure of a multi-layered painted sample.

An Investigation of Thermomechanical Behavior in Laser Hot Wire Directed Energy Deposition of NAB: Finite Element Analysis and Experimental Validation

Laser Hot Wire (LHW) Directed Energy Deposition (DED) Additive Manufacturing (AM) processes are capable of manufacturing parts with a high deposition rate. There is a growing research interest in replacing large cast Nickel Aluminum Bronze (NAB) components using LHW DED processes for maritime applications. Understanding thermomechanical behavior during LHW DED of NAB is a critical step towards the production of high-quality NAB parts with desired performance and properties. In this paper, finite element simulations are first used to predict the thermomechanical time histories during LHW DED of NAB test coupons with an increasing geometric complexity, including single-layer and multilayer depositions. Simulation results are experimentally validated through in situ measurements of temperatures at multiple locations in the substrate as well as displacement at the free end of the substrate during and immediately following the deposition process. The results in this paper demonstrate that the finite element predictions have good agreement with the experimental measurements of both temperature and distortion history. The maximum prediction error for temperature is 5% for single-layer samples and 6% for multilayer samples, while the distortion prediction error is about 12% for single-layer samples and less than 4% for multilayer samples. In addition, this study shows the effectiveness of including a stress relaxation temperature at 500 °C during FE modeling to allow for better prediction of the low cross-layer accumulation of distortion in multilayer deposition of NAB.

An assessment of PLA/wood with PLA core sandwich multilayer component tensile strength under different 3D printing conditions

Material extrusion is increasingly used to make functional parts in small batches that are challenging to produce with traditional machining. Also, intensive efforts are being made to develop new eco–friendly materials. This work investigates the strength of multilayer samples made in sandwich form with 4–5–4 layers of 0.3 mm layer thickness, externally with polylacticacid wood (PLA/wood, 61.5 % of specimens' material) and internally with pure PLA (38.5 % of specimens' material), under tensile loads. The intent is to investigate the possibility of manufacturing biocompatible components that take advantage of the excellent surface properties of wood externally and the durability properties of PLA internally. For this purpose, a designed experiment following the Taguchi L9 orthogonal array was prepared, and nine samples were fabricated: three with pure PLA, three with a sandwich PLA/wood–PLA–PLA/wood form, and three with composite PLA/wood form. Printing speed and temperature were varied during the experiment, and the results were examined using the analysis of means and residuals. Sandwich specimens improve tensile strength and elastic modulus by 100 % and 50 % compared to PLA/wood components while exhibiting slightly better surface roughness parameters, i.e., Ra and Rz, about ∼10 % lower values. Additionally, even if PLA parts showed better strength and surface texture than sandwich parts (∼100 % and ∼56 % higher tensile strength and elastic modulus), they had lower performance in terms of PLA–PLA/wood material ratio, i.e., 160 % more PLA than sandwich parts. The findings of this research, with the potential to design functional and sustainable new products with optimal performance, are significant and can be exploited in various industries.

R&D status of FARICH option for PID

The Super Charm-Tau Factory project is a future electron–positron colliding beam experiment with unprecedented high luminosity of 10[Formula: see text][Formula: see text]cm[Formula: see text][Formula: see text]s[Formula: see text] at the center of mass energy range from 3 to 7[Formula: see text]GeV. To perform the broad physics program, the high-performance universal detector is proposed. One of the main detector subsystems is the FARICH (Focusing Aerogel RICH) detector. The proposed FARICH scheme combined with abilities of tracking system will provide the excellent [Formula: see text]-separation for the whole operation momentum range and [Formula: see text]-separation up to momentum of 1.5[Formula: see text]GeV/c. In 2023 two multilayer focusing aerogel samples with record overall sizes [Formula: see text][Formula: see text]mm were produced in Novosibirsk. The results of the beam tests of these aerogel samples and comparison with simulation are presented. Conceptual design and some technical issues of the dedicated particle identification system based on FARICH technique are discussed as well.

The influence of ultrasonic vibration on the microstructure and properties of laser-cladded Fe-Ni-Ti composite coatings

To enhance the service life of brake discs for rail transit vehicles, an experimental platform for ultrasonic-assisted laser cladding was established. Single-layer and multi-layer overlapping Fe-Ni-Ti coatings were prepared on the surface of 316 L steel with and without ultrasonic assistance. The study investigated the influence of ultrasonic vibration on the microstructure and residual stress of composite coatings, and conducted tests on hardness, frictional wear, and corrosion resistance of the coatings. Results showed that ultrasonic vibration can refine grain structures.Under ultrasonic assistance, residual tensile and compressive stresses of the multi-layer cladding decreased by 12 % and 13 %, respectively. Under ultrasonic assistance, the average microhardness of single-pass samples increased to 515 HV, while the average microhardness of multi-pass overlapping samples increased to 460 HV. After adding ultrasonic vibration, the wear rate of single-layer samples decreased by 18.1 %, and that of multi-layer samples decreased by 12.9 %. Electrochemical impedance spectroscopy shows that under the action of ultrasound, the composite coating has better corrosion resistance performance.

Anisogrid lattice structure in thermoplastic composite by filament gun deposition

A new method to manufacture thermoplastic composite parts has been used to produce anisogrid lattice structures. Filament gun deposition consists of a hot-melt gun loaded with narrow thermoplastic prepreg tapes. Anisogrid lattice structures have been prototyped with 3 different geometries and 5 different numbers of layers (from 4 to 8) by using a metallic pattern and E-glass/polypropylene prepregs. Scanning calorimetry and bending tests of multi-layer samples have been used to characterize thermoplastic prepregs. Anisogrid lattice structures have been tested under tensile loads. A finite element model has been used to predict mechanical stiffness of these structures by using material properties coming from the sample characterization. Numerical models have been developed with a batch-type parametric approach to rapidly evaluate the combined effect of geometric and material parameters. A good agreement has been found between experimental and numerical data with an average difference about 4%.

Microstructure evolution and grain refinement in 2319 aluminium alloy via wire arc additive manufacturing coupled with multi-pass friction stir processing

The present study investigates the alterations in 2319 aluminium alloy microstructure and properties induced by the WAAM-FSP process, including grain size, microhardness and tensile strength. The effects of multiple stirring friction processing and remelting on the grains were systematically investigated. The results demonstrated that the grains within the stirring zone underwent enlargement due to thermal remelting, while the size of the stirring zone decreased. Furthermore, multiple thermo-mechanical factors significantly intensified grain growth in the bottom of the stirring zone, resulting in an increase of up to 3.4 μm.Upon a second remelting process conducted on the top of the sample, the grain size in the stirring zone can reach 3.7 μm. Additionally, the bottom stirring zone exhibited a higher prevalence of deformed grains (21.7 %) of deformed grains caused by the extrusion during multiple stirring friction processing. The top region was subjected to less thermo-mechanical influence, resulting in a smaller grain size and an ultimate tensile strength of 192.6 MPa and a hardness of 90 HV0.2. This finding demonstrates highlights the impact of thermomechanical cycling on the grains within the multilayer samples prepared by the WAAM-FSP technique.

Fabrication and thermoelectric properties of multilayer textured Sr-doped Ca3Co4O9/Ag laminar composites

This work presents a comparative analysis of pure and Ag-intercalated Ca3Co4O9 multilayer thermoelectric materials prepared through the hot-uniaxial pressing technique. Samples were prepared by attrition milling and hot-pressed at 900 °C and 55 MPa for 1 h. They were mirror polished, and some of them were stacked with and without intermediate Ag foil and hot-pressed again at 900 °C and 52 MPa for 1 h. Out-of-plane XRD showed that samples are nearly single-phase, and the grains are well oriented with their ab-plane perpendicular to the pressure direction. Microstructural studies confirmed perfect welding in the multilayer samples accompanied by the formation of a very thin layer containing larger grains and notable Ag diffusion close to the Ca3Co4O9/Ag interface. Three-point bending stresses have been increased in Ag-containing samples, while microhardness has been raised in all samples hot-pressed twice. Thermoelectric measurements showed a decrease of thermal gradient along the Ag-containing sample, together with a drastic decrease of electrical resistivity when compared to the Ag-free ones. However, the Ag-layers have promoted a drastic decrease in the Seebeck coefficient, reflected in a notable reduction of the power factor of Ca3Co4O9/Ag multilayer composites. Nevertheless, these results show that it is possible to use these materials to reduce Joule heating and increasing the compatibility with the welding compounds when building thermoelectric modules. Moreover, they open a new research line searching for larger S compounds to be intercalated with Ag foils.

Thermal Property Estimation of Thin-Layered Structures by Means of Thermoreflectance Measurement and Network Identification by Deconvolution Algorithm

Abstract Laser-induced forward transfer (LIFT) is a powerful tool for micro and nanoscale digital printing of metals for electronic packaging. In the metal LIFT process, the donor thin metal film is propelled to the receiving substrate and deposited on it. Morphology of the deposited metal varies with the thermodynamic responses of the donor thin film during and after the laser heating. Thus, the thermophysical properties of the multilayered donor sample are important to predict the LIFT process accurately. Here, we investigated thermophysical properties of a 100 nm-thick gold coated on 0.5 mm-thick sapphire and silicon substrates by means of the nanosecond time-domain thermoreflectance (ns-TDTR) analyzed by the network identification by deconvolution (NID) algorithm, which does not require numerical simulation or analytical solution. The NID algorithm enabled us to extract the thermal time constants of the sample from the nanosecond thermal decay of the sample surface. Furthermore, the cumulative and differential structure functions allowed us to investigate the heat flow path, giving the interfacial thermal resistance and the thermal conductivity of the substrate. After calibration of the NID algorithm using the thermal conductivity of the sapphire, the thermal conductivity of the silicon was determined to be 107–151 W/(m K), which is in good agreement with the widely accepted range of 110–148 W/(m K). Our study shows the feasibility of the structure function obtained from the single-shot TDTR experiments for thermal property estimation in laser processing and electronics packaging applications.

Enhancing Ni–Ti shape memory alloy diffusion bonding with Ti/Ni reactive multilayer foils

This study investigates the utilization of Ti/Ni reactive multilayer foils as an energy source for facilitating the joining of Ni–Ti shape memory alloys through diffusion bonding. Multilayered samples were prepared using a 10-cycle accumulative roll bonding (ARB) process to be used for the bonding process. Diffusion bonding employing reactive multilayers was conducted over a temperature range of 600 °C to 900 °C, at 5 MPa pressure, with a 1-h hold time. Additionally, a comparison was made with a diffusion-bonded Nitinol sample at 900 °C without a reactive multilayer. Materials characterization and testing involved scanning electron microscopy (SEM), energy-dispersive spectroscopy (EDS), shear strength testing, and differential scanning calorimetry (DSC), which were conducted on the bonded samples. The findings underscored the advantages of using reactive multilayers for diffusion bonding. These benefits included the formation of TiNi and the induction of a shape memory effect in the joint region, alongside a 1.5 times shear strength compared to identical diffusion bonding conditions without reactive multilayers. Moreover, employing reactive multilayers in the diffusion bonding of Nitinol holds promise for significantly reducing the energy needed to achieve robust and seamless bonded boundaries in the joining area.

Novel Fast-X-Ray Reflectivity Setup for Studying Electrochemical Interfaces

A fundamental understanding of atomic scale processes occurring at electrochemical interfaces is crucial for advancing the development of energy-related electrochemical systems such as ion batteries or fuel cells. For this purpose, operando experiments are imperative. X-ray reflectivity (XRR) is a non-destructive technique that enables operando analysis of buried structures with atomic resolution [1,2]. However, the time-resolution of typical XRR setups of minutes per XRR scan is limited by diffractometer motor motion and detector read-out times; this resolution is in many cases too slow to observe interfacial electrochemical phenomena [1,2].To overcome these limitations, we developed a novel fast-XRR setup, which employs a fast quasi-continuous rotation stage in combination with a stationary, high frame rate area detector. With this setup, the sample can be rotated with a frequency of up to 10 Hz, yielding sub-second time resolution for an individual XRR scan. In contrast to complementary fast-XRR setups [3,4], the presented setup can easily be combined with complex sample environments, as typically required for the investigation of electrochemical interfaces.We present first fast-XRR results obtained at PETRA III beamline P08 at DESY using 18 keV and a Dectris Eiger1M detector. We reached a time resolution below one second for an incident angular range between 0° – 6° (≙ 0 – 2 Å-1, i.e., covering the Fresnel XRR range). We measured several multilayer samples (e.g., 2 nm Ti / 20 nm Au coating on a Si substrate) and benchmarked the results to “standard” XRR measurements, where the measurements took several minutes. We find good agreement and conclude, that our novel setup provides significant XRR data within less than one second, demonstrating its usability for operando XRR measurements.Literature:[1] C. Cao, H.-G. Steinrück, Encyclopedia of Solid-Liquid Interfaces, 391–416, Elsevier, 2024.[2] C. Cao, H.-G. Steinrück et al., Nano Letters, 16, 12, 7394–7401, 2016.[3] M. Lippmann et al. Review of Scientific Instruments, 87, 113904, 2016.[4] H. Jorres et al., Applied Physics Letters, 114, 081904, 2019.

Faktor Penentu Pembayaran Zakat Masyarakat Islam di Negeri Terengganu

The statistics of zakat collection by the Terengganu Islamic Religious and Malay Customs Council (MAIDAM) which is increasing from year to year is a very good development for MAIDAM and the Muslim community of Terengganu. Researchers are interested in identifying the factors that influence the compliance of zakat payment by the Muslim community in Terengganu. Thus, this study aims to (i) identify the relationship between the factors of knowledge, exposure, self-efficacy, attitude, and awareness towards zakat payment and (ii) propose a model related to the relationship between knowledge, exposure, self-efficacy, attitude and understanding towards zakat payment. Using quantitative methods, a set of questionnaires developed based on previous studies were distributed to 384 people in the Terengganu Muslim community using multi-layer area sampling techniques and random sampling. The collected data was analyzed using SPSS Version 22 and Smart-PLS Version 3.2.7 software. The findings found that the factors of knowledge, exposure, self-efficacy, and attitude showed a significant relationship to the payment of zakat, while the factor of understanding did not influence respondents in paying zakat. This finding can help related parties in formulating strategies to increase the amount of zakat collection from the Muslim community in the future. However, the findings of this study are only limited to five determining factors. Hence, future research should expand its scope to encompass additional determining factors for more comprehensive outcomes. Keywords: ; ; ; ;

Fracture and Wear Behavior of Functionally Graded 316L–TiC Composite Fabricated by Selective Laser Melting Additive Manufacturing

Herein, the tribological and fracture behavior of multilayer 316L–TiC composites produced by the selective laser melting additive manufacturing process is investigated. The results show a robust interface between the layers and no cracks are detected even after a flexural strain of 0.4. The hardness of the composite layers with 5 and 10 wt% TiC increases by 75.5 and 104.8% compared to the hardness of the pure 316L stainless steel layer. Transverse rupture strength measurements show that a layer of pure 316L significantly improves the rupture strength of the multilayer samples. Wear test results show that the inclusion of TiC particles increases wear resistance, with the composite layer containing 10 wt% TiC demonstrating the highest wear resistance.

Comprehensive electrochemical imaging analyses of redox activities correlated to multilayer graphene and graphite structures

The utilization of two-dimensional (2D) materials within electrochemical devices constitutes a pivotal area of investigation, particularly pertinent to energy-related materials. Scanning electrochemical cell microscopy (SECCM) stands as a valuable characterization tool for the in-situ visualization of electrochemical processes transpiring within nanoscale structures. In the context of this investigation, SECCM was employed to scrutinize the influence of atomic structures in multilayer graphene and graphite samples, emblematic of 2D materials, upon a spectrum of electrochemical reactions, encompassing redox reactions of Ru(NH3)63+/2+. By visualizing and locally evaluating electrochemical reactions with various atomic structures, this research can be applied to design materials to promote more electrochemical reactions, as well as to other electrochemical energy devices (such as lithium-ion batteries and electrocatalysts). Furthermore, it extends its purview to assess the applicability of graphene substrates as platforms for the evaluation of other two-dimensional materials.

Layer-resolved vector magnetometry using generalized magneto-optical ellipsometry

We demonstrate the ability of a single magneto-optical reflection experiment to achieve layer-resolved vector magnetometry in multilayer films. For this purpose, we designed, fabricated, and measured a set of epitaxial ferromagnetic/non-magnetic/ferromagnetic heterostructure multilayer samples that exhibit in-plane uniaxial anisotropy and a tunable ferromagnetic interlayer coupling strength through the non-magnetic interlayer. By means of generalized magneto-optical ellipsometry measurements, we obtain the magnetization angles of the two different ferromagnetic layers independently as a function of the applied field. Hereby, we observe that the magnetization switching of one layer can trigger a discontinuous shift of the magnetization angle in the second layer if ferromagnetic interlayer coupling is present. Moreover, we reproduce the obtained behavior using a model of two coupled macrospins, which corroborates even the unexpected aspects of our experimental results and thus reinforces the sensitivity and reliability of our experimental layer-resolved vector magnetometry.

Effects of highly-textured and untextured polycrystalline layers on deformation mechanisms in amorphous submicron-layered materials

Amorphous alloys have high strength, but softening can lead to room temperature brittleness, limiting their applications. Typically, soft means low hardness and yield strength, and the lower the yield stress, the higher the fracture toughness. Two amorphous/crystalline multilayer samples with submicron single layer thickness were prepared. The crystalline layer of one sample is composed of highly-textured (111) nanocrystalline grains, and the other sample is untextured. Indentation experiments proved that the samples were plastically deformed, while the amorphous layer did not form shear bands with decreased layer thickness. The thickness reduction of the amorphous layer in the sample with highly-textured crystalline layers is greater than in the sample with untextured crystalline layers. The strain-hardening ability of the textured crystalline layer is higher, while the corresponding amorphous layer is deformed more severely with free volume annihilation and greater flow with more compact atoms. The amorphous layer corresponding to the untextured crystalline layer absorbs dislocations, and activates shear transformation zones (STZs), increasing the free volume near the interface. The annihilation of the free volume is less than the sample with highly-textured crystalline layers.