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At least 757 records · Page 42

Atomic Force Microscope Controlled Topographical Imaging and Proximal Probe Thermal Desorption/Ionization Mass Spectrometry Imaging

This paper reports on the development of a hybrid atmospheric pressure atomic force microscopy/mass spectrometry imaging system utilizing nano-thermal analysis probes for thermal desorption surface sampling with subsequent atmospheric pressure chemical ionization and mass analysis. The basic instrumental setup and the general operation of the system were discussed and optimized performance metrics were presented. The ability to correlate topographic images of a surface with atomic force microscopy and a mass spectral chemical image of the same surface, utilizing the same probe without moving the sample from the system, was demonstrated. Co-registered mass spectral chemical images and atomic force microscopy topographical images were obtained from inked patterns on paper as well as from a living bacterial colony on an agar gel. Spatial resolution of the topography images based on pixel size (0.2 m x 0.8 m) was better than the resolution of the mass spectral images (2.5 m x 2.0 m), which were limited by current mass spectral data acquisition rate and system detection levels.

Ovchinnikova, Olga S↗

Depth-sensing indentation of nanomaterials and nanostructures

Due to its capacity for applying ultralow loads and detecting nanometer-scale deflections, nanoindentation has been used to investigate the mechanical behavior of various material configurations at the micro- and nano-scales. The emphasis of the article is on the nanoscale deformation of nanoparticles, micro/nanopillars, microbeams, micro/nanofibers, nanocomposites, membranes and monolayer films, which are all ubiquitous structures in nanotechnology. The small volumes of these structures have led to the elucidation of material deformation mechanisms that are not the same as their bulk counterparts. Advances in instrumentation have enabled nanoindentation experiments to be conducted in situ in conjunction with scanning electron microscopy (SEM), electron backscatter diffraction (EBSD), transmission electron microscopy (TEM), electrical contact resistance (ECR) measurements, atomic force microscopy (AFM), among others, and examples of these studies will be discussed.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Applications of Subsurface Microscopy

Exploring the interior of a cell is of tremendous importance in order to assess the effects of nanomaterials on biological systems. Outside of a controlled laboratory environment, nanomaterials will most likely not be conveniently labeled or tagged so that their translocation within a biological system cannot be easily identified and quantified. Ideally, the characterization of nanomaterials within a cell requires a nondestructive, label-free, and subsurface approach. Subsurface nanoscale imaging represents a real challenge for instrumentation. Indeed the tools available for high resolution characterization, including optical, electron or scanning probe microscopies, mainly provide topography images or require tagants that fluoresce. Although the intercellular environment holds a great deal of information, subsurface visualization remains a poorly explored area. Recently, it was discovered that by mechanically perturbing a sample, it was possible to observe its response in time with nanoscale resolution by probing the surface with a micro-resonator such as a microcantilever probe (Figure 1). Microcantilevers are used as the force-sensing probes in Atomic Force Microscopy (AFM), where the nanometer-scale probe tip on the microcantilever interacts with the sample in a highly controlled manner to produce high-resolution raster-scanned information of the sample surface. Taking advantage of the existing capabilities of AFM, we present a novel technique, Mode Synthesizing Atomic Force Microscopy (MSAFM) (Figure 1), which has the ability to probe subsurface structures such as non-labeled nanoparticles embedded in a cell. In MSAFM mechanical actuators (PZTs) excite the probe and the sample at different frequencies as depicted in Figure 1. The nonlinear nature of the tip-sample interaction, at the point of contact of the probe and the surface of the sample, in the contact mode AFM configuration permits the mixing of the elastic waves. The new dynamic system comprises new synthesized imaging modes, resulting from sum- and difference-frequency generation of the driving frequencies. The specific electronics of MSAFM allows the selection of individual modes and the monitoring of their amplitude and phase. From these quantities of various synthesized modes a series of images can be acquired. The new images contain subsurface information, thus revealing the presence of nanoparticles inside the cells.

Tetard, Laurene↗

From surface to intracellular non-invasive nanoscale study of living cells impairments

Among the enduring challenges in nanoscience, subsurface characterization of live cells holds major stakes. Developments in nanometrology for soft matter thriving on the sensitivity and high resolution benefits of atomic force microscopy have enabled detection of subsurface structures at the nanoscale (1,2,3). However, measurements in liquid environments remain complex (4,5,6,7), in particular in the subsurface domain. Here we introduce liquid-Mode Synthesizing Atomic Force Microscopy (l-MSAFM) to study both the inner structures and the chemically induced intracellular impairments of living cells. Specifically, we visualize the intracellular stress effects of glyphosate on living keratinocytes skin cells. This new approach for living cell nanoscale imaging, l-MSAFM, in their physiological environment or in presence of a chemical stress agent confirmed the loss of inner structures induced by glyphosate. The ability to monitor the cell's inner response to external stimuli, non-destructively and in real time, has the potential to unveil critical nanoscale mechanisms of life science.

Ewald, Dr. Maxime↗

Surface science analysis of GaAs photocathodes following sustained electron beam delivery

Degradation of the photocathode materials employed in photoinjectors represents a challenge for sustained operation of nuclear physics accelerators and high power Free Electron Lasers (FEL). Photocathode quantum efficiency (QE) degradation is due to residual gasses in the electron source vacuum system being ionized and accelerated back to the photocathode. These investigations are a first attempt to characterize the nature of the photocathode degradation, and employ multiple surface and bulk analysis techniques to investigate damage mechanisms including sputtering of the Cs-oxidant surface monolayer, other surface chemistry effects, and ion implantation. Surface and bulk analysis studies were conducted on two GaAs photocathodes, which were removed from the JLab FEL DC photoemission gun after delivering electron beam, and two control samples. The analysis techniques include Helium Ion Microscopy (HIM), Rutherford Backscattering Spectrometry (RBS), Atomic Force Microscopy (AFM) and Secondary Ion Mass Spectrometry (SIMS). In addition, two high-polarization strained superlattice GaAs photocathode samples, one removed from the Continuous Electron Beam Accelerator Facility (CEBAF) photoinjector and one unused, were also analyzed using Transmission Electron Microscopy (TEM) and SIMS. It was found that heat cleaning the FEL GaAs wafer introduces surface roughness, which seems to be reduced by prolonged use. The bulk GaAs samples retained a fairly well organized crystalline structure after delivering beam but shows evidence of Cs depletion on the surface. Within the precision of the SIMS and RBS measurements the data showed no indication of hydrogen implantation or lattice damage from ion back bombardment in the bulk GaAs wafers. In contrast, SIMS and TEM measurements of the strained superlattice photocathode show clear crystal damage in the wafer from ion back bombardment.

36 MATERIALS SCIENCE↗

Modification of Structural, Chemical and Process Properties of Rare Metal Minerals under Treatment by High-Voltage Nanosecond Pulses

The authors have studied the mechanism of controlled modification of composition, structure, chemistry, physicochemical and process properties of columbite, tantalite, zircon and feldspar at the meso-, micro- and nanoscales after nonthermal treatment by high-voltage nanosecond electromagnetic pulses. The studies used methods: X-ray photoelectron spectroscopy, scanning electron and atomic force microscopy, potentiometric titration, electromigration chromatography, Kelvin probe force microscopy, microhardness metering and assessment of hydrophobic behavior and flotation activity of the minerals. It is found that changes in the chemical state of atoms on the surface of minerals are mainly connected with the sequential transformation of stages in the process of formation and modification of a functional cover of mineral surface, with variation in a ratio of different type hydroxyl groups on the surface of columbite, zircon and feldspar, which conditions contrast physicochemical properties of rare metal minerals and improves selectivity of their separation by flotation.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Investigation of Antirelaxation Coatings for Alkali-metal Vapor Cells using Surface Science Techniques

Many technologies based on cells containing alkali-metal atomic vapor benefit from the use of antirelaxation surface coatings in order to preserve atomic spin polarization. In particular, paraffin has been used for this purpose for several decades and has been demonstrated to allow an atom to experience up to 10,000 collisions with the walls of its container without depolarizing, but the details of its operation remain poorly understood. We apply modern surface and bulk techniques to the study of paraffin coatings in order to characterize the properties that enable the effective preservation of alkali spin polarization. These methods include Fourier transform infrared spectroscopy, differential scanning calorimetry, atomic force microscopy, near-edge x-ray absorption fine structure spectroscopy, and x-ray photoelectron spectroscopy. We also compare the light-induced atomic desorption yields of several different paraffin materials. Experimental results include the determination that crystallinity of the coating material is unnecessary, and the detection of C=C double bonds present within a particular class of effective paraffin coatings. Further study should lead to the development of more robust paraffin antirelaxation coatings, as well as the design and synthesis of new classes of coating materials.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Comparative quantification and statistical analysis of η′ and η precipitates in aluminum alloy AA7075-T651 by TEM and AFM

Quantification of nanometric precipitates in metallic alloys has been traditionally performed using transmission electron microscopy, which is nominally a low throughput technique. This work presents a comparative study of quantification of η′ and η precipitates in aluminum alloy AA7075-T651 using transmission electron microscopy (TEM) and non-contact atomic force microscopy (AFM). AFM quantification was compared with 2-D stereological results reported elsewhere. Also, a method was developed, using specialized software, to characterize nanometric size precipitates observed in dark-field TEM micrographs. Statistical analysis of the quantification results from both measurement techniques supports the use of AFM for precipitate characterization. Once the precipitate stoichiometry has been determined by appropriate analytical techniques like TEM, as it is the case for η′ and η in AA7075-T651, the relative ease with which specimens are prepared for AFM analysis could be advantageous in product and process development, and quality control, where a large number of samples are expected for analysis on a regular basis. - Highlights: • Nanometric MgZn{sub 2} precipitates in AA7075-T651 were characterized using AFM and TEM. • Phase-contrast AFM was used to differentiate metal matrix from MgZn{sub 2} precipitates. • TEM and AFM micrographs were analyzed using commercially available software. • AFM image analysis and TEM 2-D stereology render statistically equivalent results.

36 MATERIALS SCIENCE↗

Investigation of anti-Relaxation coatings for alkali-metal vapor cells using surface science techniques

Many technologies based on cells containing alkali-metal atomic vapor benefit from the use of antirelaxation surface coatings in order to preserve atomic spin polarization. In particular, paraffin has been used for this purpose for several decades and has been demonstrated to allow an atom to experience up to 10?000 collisions with the walls of its container without depolarizing, but the details of its operation remain poorly understood. We apply modern surface and bulk techniques to the study of paraffin coatings in order to characterize the properties that enable the effective preservation of alkali spin polarization. These methods include Fourier transform infrared spectroscopy, differential scanning calorimetry, atomic force microscopy, near-edge x-ray absorption fine structure spectroscopy, and x-ray photoelectron spectroscopy. We also compare the light-induced atomic desorption yields of several different paraffin materials. Experimental results include the determination that crystallinity of the coating material is unnecessary, and the detection of C=C double bonds present within a particular class of effective paraffin coatings. Further study should lead to the development of more robust paraffin antirelaxation coatings, as well as the design and synthesis of new classes of coating materials.

36 MATERIALS SCIENCE↗

Silver nanoparticle production by Rhizopus stolonifer and its antibacterial activity against extended spectrum {beta}-lactamase producing (ESBL) strains of Enterobacteriaceae

Highlights: {yields} Silver nanoparticle production by using Rhizopus stolonifer. {yields} Antibacterial activity of silver nanoparticles against extended spectrum {beta}-lactamase producing (ESBL) strains of Enterobacteriaceae. {yields} Synergistic effect of antibiotics with silver nanoparticles towards ESBL-strains. {yields} Characterization of silver nanoparticles made by UV-vis spectra, scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transformed infrared (FTIR) spectroscopy, atomic force microscopy (AFM). -- Abstract: This report focuses on the synthesis of silver nanoparticles using the fungus, Rhizopus stolonifer and its antimicrobial activity. Research in nanotechnology highlights the possibility of green chemistry pathways to produce technologically important nanomaterials. Characterization of newly synthesized silver nanoparticles was made by UV-visible absorption spectroscopy, scanning electron microscope (SEM), transmission electron microscope (TEM), Fourier transform infrared (FTIR) spectroscopy and atomic force microscope (AFM). TEM micrograph revealed the formation of spherical nanoparticles with size ranging between 3 and 20 nm. The biosynthesized silver nanoparticles (AgNPs) showed excellent antibacterial activity against ESBL-strains which includes E. coli, Proteus. sp. and Klebsiella sp.

36 MATERIALS SCIENCE↗

Kelvin probe force microscopy under ambient conditions

Kelvin probe force microscopy (KPFM) is a technique derived from atomic force microscopy that provides maps of surface potential or work function differences across material systems, with nanometre-scale resolution. KPFM is a useful tool for investigating electrical phenomena such as dipole orientation, interfacial charge transfer, charge accumulation, band bending and doping levels. This Primer aims to provide an overview of typical ambient-condition KPFM measurements, covering their underlying principles, experimental implementations and wide-ranging applications. Key KPFM variants, including amplitude and frequency modulation, heterodyne detection schemes and innovative open loop and pulsed force techniques, are discussed, with practical guidance on optimizing signal acquisition and reducing errors. Specialized approaches, such as time-resolved KPFM and multimodal KPFM, are discussed for their ability to capture dynamic charge processes and chemical information, respectively. Here, we highlight recent advances in KPFM applications, spanning metal alloys, soft matter, ferroelectrics, photovoltaics and 2D materials, showcasing its versatility across research domains. By addressing current limitations and identifying future opportunities, this Primer underscores the transformative potential of KPFM in advancing the understanding of nanoscale electrical phenomena.

Zahmatkeshsaredorahi, Amirhossein [Lehigh Univ., B↗

Surface ripple evolution by argon ion irradiation in polymers

In this report, an attempt has been made to investigate the morphological evolution of nanoscale surface ripples on aliphatic (polypropylene, PP) and aromatic (polyethylene terephthalate, PET) polymeric substrates irradiated with 50 keV Ar{sup +} ions. The specimens were sputtered at off normal incidence of 30° with 5 × 10{sup 16} Ar{sup +} cm{sup −2}. The topographical features and structural behavior of the specimens were studied using Atomic Force Microscopy (AFM) and UV-Visible spectroscopy techniques, respectively. The Stopping and Range of Ions in Matter simulations were performed to calculate sputtering yield of irradiated PP and PET polymers. Sputtering yield of carbon atoms has been found to be smaller for PP (0.40) as compared to PET (0.73), which is attributed to the different structures of two polymers. AFM analysis demonstrates the evolution of ripple like features with amplitude (2.50 nm) and wavelength (690 nm) on PET while that of lower amplitude (1.50 nm) and higher wavelength (980 nm) on PP specimen. The disorder parameter (Urbach energy) has been found to increase significantly from 0.30 eV to 1.67 eV in case of PP as compared to a lesser increase from 0.35 eV to 0.72 eV in case of PET as revealed by UV-Visible characterization. A mutual correlation between ion beam sputtering induced topographical variations with that of enhancement in the disorder parameter of the specimens has been discussed.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

PbI 2 Nanocrystal Growth by Atomic Layer Deposition from Pb(tmhd) 2 and HI

Atomic layer deposition (ALD) allows for fine control over the thickness, stoichiometry, and structural defects of materials. ALD provides a suitable route to deposit lead halides, which can further be converted to perovskites for photovoltaics, photoemission, and photodetection, among other applications. Deposition of lead halides by ALD has already begun to be explored; however, the precursors used in published processes are highly hazardous, require expensive fabrication processes, or contain impurities that can jeopardize the optoelectronic properties of metal halide perovskites after conversion. In this work, we deposited lead iodide (PbI 2 ) by a facile ALD process involving only two readily accessible and low-cost precursors. PbI 2 nanocrystals were grown on soda-lime glass (SLG), silicon dioxide support grids, and silicon wafer substrates and provided the groundwork for further investigation into developing lead halide perovskite processes by ALD. Further, the ALD-grown PbI 2 was characterized by annular dark-field scanning transmission electron microscopy (ADF-STEM), atomic force microscopy (AFM), high resolution transmission electron microscopy (HRTEM), X-ray fluorescence (XRF), and X-ray photoemission spectroscopy (XPS), among other methods. This work presents the first step to synthesize lead halide perovskites with atomic control for applications such as interfacial layers in photovoltaics and for deposition in microcavities for lasing.

36 MATERIALS SCIENCE↗

Studies of Multiferroic Palladium Perovskites

Abstract We have studied the atomic force microscopy (AFM), X-ray Bragg reflections, X-ray absorption spectra (XAS) of the Pd L-edge, Scanning electron microscopey (SEM) and Raman spectra, and direct magnetoelectric tensor of Pd-substituted lead titanate and lead zirconate-titanate. A primary aim is to determine the percentage of Pd +4 and Pd +2 substitutional at the Ti-sites (we find that it is almost fully substitutional). The atomic force microscopy data uniquely reveal a surprise: both threefold vertical (polarized out-of-plane) and fourfold in-plane domain vertices. This is discussed in terms of the general rules for Voronoi patterns (Dirichlet tessellations) in two and three dimensions. At high pressures Raman soft modes are observed, as in pure lead titanate, and X-ray diffraction (XRD) indicates a nearly second-order displacive phase transition. However, two or three transitions are involved: First, there are anomalies in c/a ratio and Raman spectra at low pressures (P = 1 − 2 GPa); and second, the c/a ratio reaches unity at ca. P = 10 GPa, where a monoclinic (M c ) but metrically cubic transition occurs from the ambient tetragonal P4 mm structure in pure PbTiO 3 ; whereas the Raman lines (forbidden in the cubic phase) remain until ca. 17 GPa, where a monoclinic-cubic transition is known in lead titanate.

36 MATERIALS SCIENCE↗

Preparation and atomic structure of reconstructed (0001) InGaN surfaces

The preparation and surface structure of high quality group-III-polar (0001) InGaN layers grown by metal-organic vapor phase epitaxy have been investigated. In order to obtain a clean and well-ordered surface we studied the preparation by annealing at various temperatures under ultra high vacuum and nitrogen-rich conditions in nitrogen-plasma. We show that different InGaN surface reconstructions such as (1 Multiplication-Sign 1), (1 + 1/6), (2 Multiplication-Sign 2), and ({radical}(3) Multiplication-Sign {radical}(3))R30 Degree-Sign can be obtained as observed by low energy electron diffraction. Dependent on the annealing temperature and nitrogen supply these surfaces exhibit significant differences in stoichiometry and morphology as determined by Auger electron spectroscopy and atomic force microscopy measurements. The (1 Multiplication-Sign 1), (2 Multiplication-Sign 2), and ({radical}(3) Multiplication-Sign {radical}(3))R30 Degree-Sign superstructures are terminated by single group-III-adatoms, whereas the (1 + 1/6) exhibits a incommensurate overlayer of group-III-atoms. We show that the (2 Multiplication-Sign 2) and ({radical}(3) Multiplication-Sign {radical}(3))R30 Degree-Sign an In depletion in the first group-III layer and In or Ga adatoms in ontop position. Strain-relaxation is suggested to explain this structure formation.

36 MATERIALS SCIENCE↗

Probing three-dimensional surface force fields with atomic resolution: Measurement strategies, limitations, and artifact reduction

Noncontact atomic force microscopy (NC-AFM) is being increasingly used to measure the interaction force between an atomically sharp probe tip and surfaces of interest, as a function of the three spatial dimensions, with picometer and piconewton accuracy. Since the results of such measurements may be affected by piezo nonlinearities, thermal and electronic drift, tip asymmetries, and elastic deformation of the tip apex, these effects need to be considered during image interpretation. In this paper, we analyze their impact on the acquired data, compare different methods to record atomic-resolution surface force fields, and determine the approaches that suffer the least from the associated artifacts. The related discussion underscores the idea that since force fields recorded by using NC-AFM always reflect the properties of both the sample and the probe tip, efforts to reduce unwanted effects of the tip on recorded data are indispensable for the extraction of detailed information about the atomic-scale properties of the surface.

36 MATERIALS SCIENCE↗

Growth of boron doped hydrogenated nanocrystalline cubic silicon carbide (3C-SiC) films by Hot Wire-CVD

Highlights: • Boron doped nc-3C-SiC films prepared by HW-CVD using SiH{sub 4}/CH{sub 4}/B{sub 2}H{sub 6}. • 3C-Si-C films have preferred orientation in (1 1 1) direction. • Introduction of boron into SiC matrix retard the crystallanity in the film structure. • Film large number of SiC nanocrystallites embedded in the a-Si matrix. • Band gap values, E{sub Tauc} and E{sub 04} (E{sub 04} > E{sub Tauc}) decreases with increase in B{sub 2}H{sub 6} flow rate. - Abstract: Boron doped nanocrystalline cubic silicon carbide (3C-SiC) films have been prepared by HW-CVD using silane (SiH{sub 4})/methane (CH{sub 4})/diborane (B{sub 2}H{sub 6}) gas mixture. The influence of boron doping on structural, optical, morphological and electrical properties have been investigated. The formation of 3C-SiC films have been confirmed by low angle XRD, Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), Fourier transform infra-red (FTIR) spectroscopy and high resolution-transmission electron microscopy (HR-TEM) analysis whereas effective boron doping in nc-3C-SiC have been confirmed by conductivity, charge carrier activation energy, and Hall measurements. Raman spectroscopy and HR-TEM analysis revealed that introduction of boron into the SiC matrix retards the crystallanity in the film structure. The field emission scanning electron microscopy (FE-SEM) and non contact atomic force microscopy (NC-AFM) results signify that 3C-SiC film contain well resolved, large number of silicon carbide (SiC) nanocrystallites embedded in the a-Si matrix having rms surface roughness ∼1.64 nm. Hydrogen content in doped films are found smaller than that of un-doped films. Optical band gap values, E{sub Tauc} and E{sub 04} decreases with increase in B{sub 2}H{sub 6} flow rate.

36 MATERIALS SCIENCE↗