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1.
J Fluoresc ; 2024 Jul 03.
Article in English | MEDLINE | ID: mdl-38958905

ABSTRACT

Pedalium Murex leaf extract was used in this study to create Nickel-doped Cerium oxide (Ni-CeO2) nanoparticles at 3 mol% and 5 mol% molar concentrations. The biosynthesized process was applied for the fabrication of Ni-CeO2 NPs. The X-ray diffraction method was used to identify their crystal structure. The XRD measurements showed that the Ni-CeO2 NPs crystallized into the face-centred cubic system. Fourier transform infrared spectral study was applied to explore the molecular vibrations and chemical bonding. The surface texture and chemical ingredients of Ni-CeO2 NPs were studied using field-emission scanning electron microscopy and energy-dispersive X-ray analysis. The EDX mapping spectra illustrate the uniform dispersal of Ce, Ni, and O atoms over the sample's surface. X-ray photoelectron spectroscopy (XPS) was conducted to confirm the chemical state of the Ni-CeO2 NPs. UV-Vis spectrum study was performed to ascertain the photon absorption, bandgap, and Urbach edge of Ni-CeO2 NPs. Photoluminescence (PL) research has been used to study the light-emitting characteristic of Ni-CeO2 NPs. The emissive intensity transition corresponding to Ni-CeO2 NPs was found to increase with the dopant level. The CIE 1931 chromaticity map was plotted to find the aptness of the samples for optical uses. The antifungal ability of Ni-CeO2 NPs was evaluated against the fungi candida albicans and candida krusein with the agar well-diffusion process. The fungicidal activity of the 3 mol% Ni doped CeO2 nanoparticles has shown a maximum zone of inhibition. The experimental findings illustrate the utility of Ni-CeO2 NPs for optical and antifungal applications.

2.
Mol Pharm ; 21(8): 4074-4081, 2024 Aug 05.
Article in English | MEDLINE | ID: mdl-39008633

ABSTRACT

Amorphous solid dispersions (ASDs) can be used to enhance the solubility and bioavailability of poorly soluble drugs. An ASD is often a ternary system containing a drug, a surfactant, and a polymer. Recent work on binary ASDs has observed significant differences between surface and bulk compositions, with impacts on wettability and stability. Here we investigate a ternary ASD composed of the antifungal posaconazole, the surfactant Span 80, and a dispersion polymer (PVP or PVP/VA). The surfactant loading was fixed at the typical level of 5 wt %, and the drug/polymer ratio was varied. We observed strong surface enrichment of the surfactant and simultaneous depletion of the drug. This effect is already pronounced in the binary drug-surfactant system and is enhanced by the addition of the polymers. Between the two polymers, the more hydrophilic PVP causes a stronger enhancement of the surface enrichment effect. These results demonstrate the impact of component interactions on the surface composition of ASDs and the performance.


Subject(s)
Hydrophobic and Hydrophilic Interactions , Polymers , Solubility , Surface-Active Agents , Surface-Active Agents/chemistry , Polymers/chemistry , Wettability , Triazoles/chemistry , Antifungal Agents/chemistry , Povidone/chemistry , Hexoses
3.
Polymers (Basel) ; 16(14)2024 Jul 20.
Article in English | MEDLINE | ID: mdl-39065389

ABSTRACT

Sodium alginate (NaAlg) is widely used as a food additive. To study the effect of irradiation with X-ray quanta with energies of 1253.6 eV and 1486.6 eV on the composition of NaAlg, thick films with a smooth surface were prepared, which did not differ in IR spectra from the original powders. The films were irradiated in a high vacuum (3 × 10-10 mbar) in the chamber of a Specs PHOIBOS 150 MCD9 XPS spectrometer with an X-ray source power of 150 W and an irradiation duration of up to 300 min, which significantly exceeded the time required to obtain an XPS spectrum. This made it possible to use XPS to monitor changes in the composition of the NaAlg surface directly during irradiation. As a result of the research, it has been established that NaAlg degrades with prolonged irradiation, which is accompanied by a significant decrease in the O/C ratio. When analyzing the dependence of the intensities of individual peaks in the C1s spectrum on the irradiation time, it was found that after 100 min of irradiation, a peak due to the carbonate group appears in the spectrum. The decomposition was also accompanied by a change in the color of NaAlg from white to yellow-brown. In the IR spectrum of the NaAlg film irradiated for 300 min, an absorption band was detected at 1910 cm-1, which is usually associated with the presence of allene groups.

4.
Micromachines (Basel) ; 15(7)2024 Jul 20.
Article in English | MEDLINE | ID: mdl-39064441

ABSTRACT

In this work, Ni3V2O8 (NVO) and Ni3V2O8-reduced graphene oxide (NVO-rGO) are synthesized hydrothermally, and their extensive structural, morphological, and electrochemical characterizations follow subsequently. The synthetic materials' crystalline structure was confirmed by X-ray diffraction (XRD), and its unique marigold-like morphology was observed by field emission scanning electron microscopy (FESEM). The chemical states of the elements were investigated via X-ray photoelectron spectroscopy (XPS). Electrochemical impedance spectroscopy (EIS), Galvanostatic charge-discharge (GCD), and cyclic voltammetry (CV) were used to assess the electrochemical performance. A specific capacitance of 132 F/g, an energy density of 5.04 Wh/kg, and a power density of 187 W/kg were demonstrated by Ni3V2O8-rGO. Key electrochemical characteristics were b = 0.67; a transfer coefficient of 0.52; a standard rate constant of 6.07 × 10-5 cm/S; a diffusion coefficient of 5.27 × 10-8 cm2/S; and a series resistance of 1.65 Ω. By employing Ni3V2O8-rGO and activated carbon, an asymmetric supercapacitor with a specific capacitance of 7.85 F/g, an energy density of 3.52 Wh/kg, and a power density of 225 W/kg was achieved. The series resistance increased from 4.27 Ω to 6.63 Ω during cyclic stability tests, which showed 99% columbic efficiency and 87% energy retention. The potential of Ni3V2O8-rGO as a high-performance electrode material for supercapacitors is highlighted by these findings.

5.
Micromachines (Basel) ; 15(7)2024 Jul 20.
Article in English | MEDLINE | ID: mdl-39064440

ABSTRACT

Preparing elastic substrates as a carrier for dual-end supported nickel chromium thin film strain sensors is crucial. Wet etching is a vital microfabrication process widely used in producing microelectronic components for various applications. This article combines lithography and wet etching methods to microprocess the external dimensions and rectangular grooves of 304 stainless steel substrates. The single-factor variable method was used to explore the influence mechanism of FeCl3, HCl, HNO3, and temperature on the etching rate, etching factor, and etching surface roughness. The optimal etching parameter combination was summarized: an FeCl3 concentration of 350 g/L, HCl concentration of 150 mL/L, HNO3 concentration of 100 mL/L, and temperature of 40 °C. In addition, by comparing the surface morphology, microstructure, and chemical and mechanical properties of a 304 stainless steel substrate before and after etching treatment, it can be seen that the height difference of the substrate surface before and after etching is between 160 µm and -70 µm, which is basically consistent with the initial design of 0.2 mm. The results of an XPS analysis and Raman spectroscopy analysis both indicate that the surface C content increases after etching, and the corrosion resistance of the surface after etching decreases. The nano-hardness after etching increased by 26.4% compared to before, and the ζ value decreased by 7%. The combined XPS and Raman results indicate that the changes in surface mechanical properties of 304 stainless steel substrates after etching are mainly caused by the formation of micro-nanostructures, grain boundary density, and dislocations after wet etching. Compared with the initial rectangular substrate, the strain of the I-shaped substrate after wet etching increased by 3.5-4 times. The results of this study provide the preliminary process parameters for the wet etching of a 304 stainless steel substrate of a strain measuring force sensor and have certain guiding significance for the realization of simple steps and low cost of 304 stainless steel substrate micro-nano-processing.

6.
Gels ; 10(7)2024 Jul 17.
Article in English | MEDLINE | ID: mdl-39057491

ABSTRACT

In this research, the influence of the thermal treatment of geopolymer gels at 300 °C, 600 °C and 900 °C when incorporated with 5% rare earth elements (REEs) in the form of (GP-Sm) Sm2O3 and (GP-Nd) Nd2O3 was investigated. Changes in the chemical and structural properties of the geopolymer gels during thermal treatment for 1 h were monitored. Physico-chemical characterization was performed using the following methods: diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS), scanning electron microscopy with energy dispersive spectrometry (SEM-EDS), and X-ray photoelectron spectroscopy (XPS). Besides the characterization of the fundamental properties, some practical macroscopic properties were analyzed as well: sorptivity, open porosity, and Archimedean density. The stretching vibrations of Nd-O-Si and Sm-O-Si were confirmed at a value of around 680 cm-1and an Nd-O-Si absorption band at a higher value, together with the most dominant band of Si-O stretching vibration similar for all the samples. No significant chemical changes occurred. Structural analysis showed that for GP-Nd, the largest pore diameter was obtained at 900 °C, while for GP-Sm, the largest pore diameter was obtained at 600 °C. EDS confirmed the amount of dopant to be about 5%. X-ray photoelectron spectroscopy showed that for GP-Nd, the ratio of Si and Al changed the most, while for GP-Sm, the ratio of Si and Al decreased with increasing temperature. The contributions of both dopants in the GP-gel structure remained almost unchanged and stable at high temperatures. The atomic percentages obtained by XPS analysis were in accordance with the expected trend; the amount of Si increased with the temperature, while the amount of Al decreased with increasing temperature. The sorptivity and open porosity showed the highest values at 600 °C, while the density of both geopolymers decreased linearly with increasing temperature.

7.
ACS Appl Mater Interfaces ; 16(30): 40210-40221, 2024 Jul 31.
Article in English | MEDLINE | ID: mdl-39037739

ABSTRACT

Chalcogenide perovskites exhibit optoelectronic properties that position them as potential materials in the field of photovoltaics. We report a detailed investigation into the electronic structure and chemical properties of polycrystalline BaZrS3 perovskite powder by X-ray photoelectron spectroscopy, complemented by an analysis of its long- and short-range geometric structures using X-ray diffraction and X-ray absorption spectroscopy. The results obtained for the powdered BaZrS3 are compared to similar measurements on a sputtered polycrystalline BaZrS3 thin film prepared through rapid thermal processing. While bulk characterization confirms the good quality of the powder, depth-profiling achieved by photoelectron spectroscopy utilizing Al Kα (1.487 keV) and Ga Kα (9.25 keV) radiations shows that, regardless of the fabrication method, the oxidation effects extend beyond 10 nm from the sample surface, with zirconium oxides specifically distributing deeper than the oxidized sulfur species. A hard X-ray photoelectron spectroscopy study on the powder and thin film detects signals with minimal contamination contributions and allows for the determination of the valence band maximum position with respect to the Fermi level. Based on these measurements, we establish a correlation between the experimental valence band spectra and the theoretical density of states derived from density functional theory calculations, thereby discerning the orbital constituents involved. Our analysis provides an improved understanding of the electronic structure of BaZrS3 developed through different synthesis protocols by linking it to material geometry, surface chemistry, and the nature of doping. This methodology can thus be adapted for describing electronic structures of chalcogenide perovskite semiconductors in general, a knowledge that is significant for interface engineering and, consequently, for device integration.

8.
ACS Appl Mater Interfaces ; 16(28): 37275-37287, 2024 Jul 17.
Article in English | MEDLINE | ID: mdl-38959130

ABSTRACT

Titanium dioxide (TiO2) shows significant potential as a self-cleaning material to inactivate severe acute respiratory syndrome coronavirus 2 (SARS-CoV-2) and prevent virus transmission. This study provides insights into the impact of UV-A light on the photocatalytic inactivation of adsorbed SARS-CoV-2 virus-like particles (VLPs) on a TiO2 surface at the molecular and atomic levels. X-ray photoelectron spectroscopy, combined with density functional theory calculations, reveals that spike proteins can adsorb on TiO2 predominantly via their amine and amide functional groups in their amino acids blocks. We employ atomic force microscopy and grazing-incidence small-angle X-ray scattering (GISAXS) to investigate the molecular-scale morphological changes during the inactivation of VLPs on TiO2 under light irradiation. Notably, in situ measurements reveal photoinduced morphological changes of VLPs, resulting in increased particle diameters. These results suggest that the denaturation of structural proteins induced by UV irradiation and oxidation of the virus structure through photocatalytic reactions can take place on the TiO2 surface. The in situ GISAXS measurements under an N2 atmosphere reveal that the virus morphology remains intact under UV light. This provides evidence that the presence of both oxygen and UV light is necessary to initiate photocatalytic reactions on the surface and subsequently inactivate the adsorbed viruses. The chemical insights into the virus inactivation process obtained in this study contribute significantly to the development of solid materials for the inactivation of enveloped viruses.


Subject(s)
SARS-CoV-2 , Titanium , Ultraviolet Rays , Titanium/chemistry , Titanium/radiation effects , SARS-CoV-2/radiation effects , SARS-CoV-2/chemistry , Virus Inactivation/radiation effects , Virus Inactivation/drug effects , Humans , Spike Glycoprotein, Coronavirus/chemistry , Spike Glycoprotein, Coronavirus/metabolism , COVID-19/virology , COVID-19/prevention & control , Adsorption , Surface Properties
9.
ACS Appl Mater Interfaces ; 16(29): 37915-37926, 2024 Jul 24.
Article in English | MEDLINE | ID: mdl-38989828

ABSTRACT

Nickel/yttria-stabilized zirconia (YSZ) composites are the most commonly used fuel electrodes for solid oxide cells. While microstructural changes of Ni/YSZ during operational conditions have been thoroughly investigated, there is limited knowledge regarding Ni/YSZ surface chemistry under working conditions. In this study, we examine the interaction between Ni/YSZ electrodes and water vapor under open circuit and polarization conditions, utilizing near ambient pressure soft and hard X-ray photoelectron spectroscopies. Miniature cells with conventional porous Ni/YSZ composite cermet cathodes were modified to facilitate the direct spectroscopic observation of the functional electrode's areas close to the interface with the YSZ electrolyte. The results highlight dynamic changes in the oxidation state and composition of Ni/YSZ under H2 and H2O atmospheres. We also quantify the accumulation of impurities on the electrode surface. Through adjustments in the pretreatment of the cell, the correlation between the nickel surface oxidation state and the cell's electrochemical performance during H2O electroreduction is established. It is unequivocally shown that nickel surface oxidation in H2O electrolysis favors NiO over Ni(OH)x, providing critical insights into the mechanism of Ni-phase redistribution within the electrode during long-term operation. Depth-dependent photoemission measurements, combined with theoretical quantitative simulations, reveal that NiO and Ni phases are uniformly mixed on the surface during H2O electrolysis. This differs from the conventional expectation of a NiO-shell/Ni-core configuration in gas phase oxidation. These findings provide crucial insights into the surface chemistry of Ni/YSZ electrodes under conditions relevant to H2O electrolysis, elucidating their impact on the electrochemical performance of the cell.

10.
Int J Mol Sci ; 25(13)2024 Jul 05.
Article in English | MEDLINE | ID: mdl-39000514

ABSTRACT

The peculiar behavior of arsenoplatin-1, ([Pt(µ-NHC(CH3)O)2ClAs(OH)2], AP-1), in aqueous solution and the progressive appearance of a characteristic and intense blue color led us to carry out a more extensive investigation to determine the nature of this elusive chemical species, which we named "AsPt blue". A multi-technique approach was therefore implemented to describe the processes involved in the formation of AsPt blue, and some characteristic features of this intriguing species were revealed.


Subject(s)
Oxidation-Reduction , Water/chemistry , Solutions , Organoplatinum Compounds/chemistry
11.
Polymers (Basel) ; 16(11)2024 May 30.
Article in English | MEDLINE | ID: mdl-38891498

ABSTRACT

This study continues the discussion on the surface modification of polymers using an atmospheric pressure plasma (APP) reactor in air. These results complement prior research focusing on nonpolar polymers. Polymers, such as polyethylene terephthalate, polyetheretherketone, and polymethyl methacrylate, containing structurally bonded oxygen are studied, representing a range of properties such as oxygen content, crystalline/amorphous structure, polarity, functionality, and aliphatic/aromatic structure. APP induces superior wetting properties on the hydrophilic polymer surfaces with rapid and uniform modification within 0.5 s of exposure. The amorphous structures undergo additional modification for longer exposure. Moreover, the aliphatic chain structures require longer plasma exposure to reach surface modification equilibrium. The polar polymers reach a limit level of modification corresponding to a minimum water contact angle of about 50°. The surface polarity increases on average by a factor of approximately two. The equilibrium values of the adhesion work attained after post-processing recovery fall within a limited range of about 100-120 mJ/m2. The enhancement of surface functionality through the creation of oxidized groups primarily depends on the initial oxygen content and reaches a limit of about 40 at.% oxygen. The surface properties of the treated polar surfaces exhibit good stability, comparable to that of the previously tested nonpolar polymers.

12.
ACS Nano ; 18(25): 16248-16256, 2024 Jun 25.
Article in English | MEDLINE | ID: mdl-38861269

ABSTRACT

Herein, we report the assembly behavior of triptycenes with aldehyde (Trip-1) and amino (Trip-2) groups on pristine and iodine-passivated Au(111) surfaces by a combination of scanning tunneling microscopy (STM), X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, and density functional theory (DFT) calculation. On Au(111) surface, Trip-1 forms long trimer chains and two-dimensional islands via aldehyde-aldehyde hydrogen bonding in one dimension and π-π stacking of adjacent benzene rings in the other dimension. In contrast, Trip-2 lies as individuals or in disorderly stacked islands. Trip-2 and Trip-1 can be mixed in an arbitrary ratio. And Trip-2 molecules disrupt the ordered self-assembly structure of Trip-1 due to the formation of stronger aldehyde-amino hydrogen bonding. DFT, XPS, and Raman spectra confirm the conformational difference of Trip-1 and -2, as well as the aldehyde-amino hydrogen bonding formation in Trip-1 and Trip-2 mixture. On the iodine-passivated Au(111) surface, Trip-1 forms single-molecule chains and a hexagonal closely packed structure due to iodine interlayer mediation. Trip-2 molecules disrupt the hexagonal closely packed structure of Trip-1.

13.
Materials (Basel) ; 17(12)2024 Jun 13.
Article in English | MEDLINE | ID: mdl-38930251

ABSTRACT

This study investigates the simultaneous decoration of vertically aligned molybdenum disulfide nanostructure (VA-MoS2) with Ag nanoparticles (NPs) and nitrogen functionalization. Nitrogen functionalization was achieved through physical vapor deposition (PVD) DC-magnetron sputtering using nitrogen as a reactive gas, aiming to induce p-type behavior in MoS2. The utilization of reactive sputtering resulted in the growth of three-dimensional silver structures on the surface of MoS2, promoting the formation of silver nanoparticles. A comprehensive characterization was conducted to assess surface modifications and analyze chemical and structural changes. X-ray photoelectron spectroscopy (XPS) showed the presence of silver on the MoS2 surface. Scanning electron microscopy (SEM) confirmed successful decoration with silver nanoparticles, showing that deposition time affects the size and distribution of the silver on the MoS2 surface.

14.
Micromachines (Basel) ; 15(6)2024 May 31.
Article in English | MEDLINE | ID: mdl-38930712

ABSTRACT

In this paper, one of the great challenges faced by silicon-based biosensors is resolved using a biomaterial multilayer. Tiny biomolecules are deposited on silicon substrates, producing devices that have the ability to act as iridescent color sensors. The color is formed by a coating of uniform microstructures through the interference of light. The system exploits a flat, RNA-aptamer-coated silicon-based surface to which captured microbes are covalently attached. Silicon surfaces are encompassed with the layer-by-layer deposition of biomolecules, as characterized by atomic force microscopy and X-ray photoelectron spectroscopy. Furthermore, the results demonstrate an application of an RNA aptamer chip for sensing a specific bacterium. Interestingly, the detection limit for the microbe was observed to be 2 × 106 CFUmL-1 by visually observed color changes, which were confirmed further using UV-Vis reflectance spectrophotometry. In this report, a flexible method has been developed for the detection of the pathogen Sphingobium yanoikuyae, which is found in non-beverage alcohols. The optimized system is capable of detecting the specific target microbe. The simple concept of these iridescent color changes is mainly derived from the increase in thickness of the nano-ordered layers.

15.
Nanotechnology ; 35(36)2024 Jun 18.
Article in English | MEDLINE | ID: mdl-38888294

ABSTRACT

In this perspective we discuss the progress made in the mechanistic studies of the surface chemistry associated with the atomic layer deposition (ALD) of metal films and the usefulness of that knowledge for the optimization of existing film growth processes and for the design of new ones. Our focus is on the deposition of late transition metals. We start by introducing some of the main surface-sensitive techniques and approaches used in this research. We comment on the general nature of the metallorganic complexes used as precursors for these depositions, and the uniqueness that solid surfaces and the absence of liquid solvents bring to the ALD chemistry and differentiate it from what is known from metalorganic chemistry in solution. We then delve into the adsorption and thermal chemistry of those precursors, highlighting the complex and stepwise nature of the decomposition of the organic ligands that usually ensued upon their thermal activation. We discuss the criteria relevant for the selection of co-reactants to be used on the second half of the ALD cycle, with emphasis on the redox chemistry often associated with the growth of metallic films starting from complexes with metal cations. Additional considerations include the nature of the substrate and the final structural and chemical properties of the growing films, which we indicate rarely retain the homogeneous 2D structure often aimed for. We end with some general conclusions and personal thoughts about the future of this field.

16.
Sci Rep ; 14(1): 14770, 2024 Jun 26.
Article in English | MEDLINE | ID: mdl-38926594

ABSTRACT

The core and surface structure, and magnetism of mechano-synthesized LaFeO3 nanoparticles (30-40 nm), Eu3+-doped (La0.70Eu0.30FeO3), and Eu3+/Cr3+ co-doped (La0.70Eu0.30Fe0.95Cr0.05O3) are reported. Doping results in a transition from the O'-type to the O-type distorted structure. Traces of reactants, intermediate phases, and a small amount of Eu2+ ions were detected on the surfaces of the nanoparticles. The nanoparticles consist of antiferromagnetic cores flanked by ferromagnetic shells. The Eu3+ dopant ions enhance the magnetization values relative to those of the pristine nanoparticles and result in magnetic susceptibilities compatible with the presence of Eu3+ van Vleck paramagnetism of spin-orbit coupling constant (λ = 363 cm-1) and a low temperature Curie-Weiss like behavior associated with the minority Eu2+ ions. Anomalous temperature-dependent magnetic hardening due to competing magnetic anisotropy and magnetoelectric coupling effects together with a temperature-dependent dopant-sensitive exchange bias, caused by thermally activated spin reversals at the core of the nanoparticles, were observed.

17.
Nanomaterials (Basel) ; 14(11)2024 May 28.
Article in English | MEDLINE | ID: mdl-38869571

ABSTRACT

Due to their unique physical and chemical properties, complex nanostructures based on carbon nanotubes and transition metal oxides are considered promising electrode materials for the fabrication of high-performance supercapacitors with a fast charge rate, high power density, and long cycle life. The crucial role in determining their efficiency is played by the properties of the interface in such nanostructures, among them, the type of chemical bonds between their components. The complementary theoretical and experimental methods, including dispersion-corrected density functional theory (DFT-D3) within GGA-PBE approximation, scanning electron microscopy (SEM), X-ray diffraction (XRD), Raman, X-ray photoelectron, and X-ray absorption spectroscopies, were applied in the present work for the comprehensive investigation of surface morphology, structure, and electronic properties in CuOx/MWCNTs and NiOx/MWCNTs. As a result, the type of interfacial interaction and its correlation with electrochemical characteristics were determined. It was found that the presence of both Ni-O-C and Ni-C bonds can increase the contact between NiO and MWCNTs, and, through this, promote electron transfer between NiO and MWCNTs. For NiOx/MWCNTs, better electrochemical characteristics were observed than for CuOx/MWCNTs, in which the interfacial interaction is determined only by bonding through Cu-O-C bonds. The electrochemical properties of CuOx/MWCNTs and NiOx/MWCNTs were studied to demonstrate the effect of interfacial interaction on their efficiency as electrode materials for supercapacitor applications.

18.
Beilstein J Nanotechnol ; 15: 603-611, 2024.
Article in English | MEDLINE | ID: mdl-38887529

ABSTRACT

Thin silicon oxide films deposited on a polypropylene substrate by plasma-enhanced chemical vapor deposition were investigated using atomic force microscopy-based infrared (AFM-IR) nanospectroscopy in contact and surface-sensitive mode. The focus of this work is the comparison of the different measurement methods (i.e., contact mode and surface-sensitive mode) with respect to the chemical surface sensitivity. The use of the surface-sensitive mode in AFM-IR shows an enormous improvement for the analysis of thin films on the IR-active substrate. As a result, in this mode, the signal of the substrate material could be significantly reduced. Even layers that are so thin that they could hardly be measured in the contact mode can be analyzed with the surface-sensitive mode.

19.
Microsc Res Tech ; 2024 Jun 10.
Article in English | MEDLINE | ID: mdl-38856214

ABSTRACT

Field emission finds a vital space in numerous scientific and technological applications, including high-resolution imaging at micro- and nano-scales, conducting high-energy physics experiments, molecule ionization in spectroscopy, and electronic uses. A continuous effort exists to develop new materials for enhanced field emission applications. In the present work, two-dimensional (2D) well-aligned CdSSe flake flowers (CdSSe-FFs) were successfully grown on gold-coated silicon substrate utilizing a simple and affordable chemical bath deposition approach at ambient temperature. The time-dependent growth mechanism from nanoparticles to FFs was observed at optimized parameters such as concentration of precursors, pH (~11), deposition time, and solution temperature. The crystalline nature of CdSSe-FFs is confirmed by high-resolution transmission electron microscopy (HRTEM) results, and selected area electron diffraction (SAED) observations reveal a hexagonal crystal structure. Additionally, the CdSSe-FFs thickness was confirmed by TEM analysis and found to be ~20-30 nm. The optical, photoelectric, and field emission (FE) characteristics are thoroughly explored which shows significant enhancement due to the formation of heterojunction between the gold-coated silicon substrate and CdSSe-FFs. The UV-visible absorption spectra of CdSSe-FFs show enhanced absorption at 700 nm, corresponding to the energy band gap (Eg) of 1.77 eV. The CdSSe-FFs exhibited field emission and photosensitive field emission (PSFE) characteristics. In FE study CdSSe-FFs shows an increase in current density of 387.2 µ A cm-2 in an applied field of 4.1 V m-1 which is 4.08 fold as compared to without light illumination (95.1 µ A cm-2). Furthermore, it shows excellent emission current stability at the preset value of 1.5 µA over 3 h with a deviation of the current density of less than 5% respectively. RESEARCH HIGHLIGHTS: Novel CdSSe flake flowers were grown on Au-coated Si substrate by a cost-effective chemical bath deposition route. The growth mechanism of CdSSe flake flowers is studied in detail. Field emission and Photoluminescence study of CdSSe flake flowers is characterized. CdSSe flake flowers with nanoflakes sharp edges exhibited enhanced field emission properties.

20.
ACS Appl Mater Interfaces ; 16(27): 35675-35685, 2024 Jul 10.
Article in English | MEDLINE | ID: mdl-38932607

ABSTRACT

In electrochemical energy storage devices, the interface between the electrode and the electrolyte plays a crucial role. A solid electrolyte interphase (SEI) is formed on the electrode surface due to spontaneous decomposition of the electrolyte, which in turn controls the dynamics of ion migration during charge and discharge cycles. However, the dynamic nature of the SEI means that its chemical structure evolves over time and as a function of the applied bias; thus, a true operando study is extremely valuable. X-ray photoelectron spectroscopy (XPS) is a widely used technique to understand the surface electronic and chemical properties, but the use of ultrahigh vacuum in standard instruments is a major hurdle for their utilization in measuring wet electrochemical processes. Herein, we introduce a 3-electrode electrochemical cell to probe the behavior of Na ions and the formation of SEI at the interface of an ionic liquid (IL) electrolyte and an aluminum electrode under operando conditions. A system containing 0.5 molar NaTFSI dissolved in the IL [BMIM][TFSI] was investigated using an Al working electrode and Pt counter and reference electrodes. By optimizing the scan rate of both XPS and cyclic voltammetry (CV) techniques, we captured the formation and evolution of SEI chemistry using real-time spectra acquisition techniques. A CV scan rate of 2 mVs-1 was coupled with XPS snapshot spectra collected at 10 s per core level. The technique demonstrated here provides a platform for the chemical analysis of materials beyond batteries.

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