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Results for “atomic force microscopy”
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An insight into microscopy and analytical techniques for morphological, structural, chemical, and thermal characterization of cellulose
Cellulose obtained from plants is a bio-polysaccharide and the most abundant organic polymer on earth that has immense household and industrial applications. Hence, the characterization of cellulose is important for determining its appropriate applications. In this article, we review the characterization of cellulose morphology, surface topography using microscopic techniques including optical microscopy, transmission electron microscopy, scanning electron microscopy, and atomic force microscopy. Additionally, other physicochemical characteristics like crystallinity, chemical composition, and thermal properties are studied using techniques including X-ray diffraction, Fourier transform infrared, Raman spectroscopy, nuclear magnetic resonance, differential scanning calorimetry, and thermogravimetric analysis. This review may contribute to the development of using cellulose as a low-cost raw material with anticipated physicochemical properties.
Dynamics of High Molecular Weight Cylindrical and Lamellar Block Copolymers with X‐ray Photon Correlation Spectroscopy
Here, the structure and dynamics of polystyrene (PS)-b-poly(ethylene oxide) block copolymers (BCPs) are studied. The BCPs exhibit microphase-separated cylindrical and lamellar morphologies. Structural dynamics are measured with X-ray photon correlation spectroscopy in the small-angle regime. Morphologies and domain sizes are evaluated using small-angle X-ray scattering (SAXS), scanning electron microscopy, and atomic force microscopy. Different solvent processing conditions are investigated. Grain sizes evaluated using SAXS are found to depend on processing only for the rubbery majority BCP. The structural relaxation times are examined as a function of PS volume fraction, temperature, morphology, and structural sizes. Well above the glass transition temperature (T g ) of PS, all samples exhibit stretched autocorrelation decays and diffusive dynamics. Near T g of PS, the dynamics of all samples are anomalous with compressed autocorrelation decays and hyperdiffusive dynamics. This transition occurs at 153 °C or 1.13 T g of PS. In the diffusive regime (at high temperature), structural relaxation times are dependent on the processing method. Near PS T g (at low temperature), structural relaxation times scale with the PS volume fraction. Structural relaxation times do not correlate with grain size, indicating that the out-of-equilibrium state of PS dominates the structural dynamics of these strongly phase-segregated BCPs.
Fast Scanning Probe Microscopy via Machine Learning: Non-Rectangular Scans with Compressed Sensing and Gaussian Process Optimization
Fast scanning probe microscopy enabled via machine learning allows for a broad range of nanoscale, temporally resolved physics to be uncovered. However, such examples for functional imaging are few in number. Here, using piezoresponse force microscopy (PFM) as a model application, a factor of 5.8 reduction in data collection using a combination of sparse spiral scanning with compressive sensing and Gaussian process regression reconstruction is demonstrated. It is found that even extremely sparse spiral scans offer strong reconstructions with less than 6% error for Gaussian process regression reconstructions. Further, the error associated with each reconstructive technique per reconstruction iteration is analyzed, finding the error is similar past ≈15 iterations, while at initial iterations Gaussian process regression outperforms compressive sensing. Finally, this study highlights the capabilities of reconstruction techniques when applied to sparse data, particularly sparse spiral PFM scans, with broad applications in scanning probe and electron microscopies.
Electron beam irradiation effects on bulk metals: a comparative study of polycrystalline versus single-crystalline structures
This study investigates the effects of electron beam (e-beam) irradiation on the mechanical and structural properties of eight bulk metallic samples, comprising both polycrystalline (PC) and single-crystalline (SC) forms of Ni, Cr, V, and Ti. These metals were evaluated as potential candidates for beam exit windows in high-power (MW-class) particle accelerators. The primary objective is to identify metals capable of withstanding the conditions of high-power/MW-class e-beam accelerators and serve effectively as exit windows. Selection criteria were based on each metal’s intrinsic properties, power dissipation capability, and irradiation-induced changes in mechanical behavior, including hardness, elastic modulus, and defect density. Comprehensive characterization was conducted using field-emission scanning electron microscopy (FESEM), atomic force microscopy (AFM), scanning electron microscopy with energy-dispersive X-ray spectroscopy (SEM–EDS), X-ray diffraction (XRD), high-resolution transmission electron microscopy (HRTEM), selected area electron diffraction (SAED), and nanoindentation, performed both before and after exposure to a ~¿66 kGy dose from a 10 MeV e-beam accelerator. Results revealed that e-beam irradiation induced hardening in PC Ni, whereas PC Ti, commonly used in beam exit windows, exhibited softening. The observed softening in PC Ti is attributed to grain coarsening, elongation, and the formation of twins and twin boundaries, in contrast to the smaller, compressed grains in the pristine (Pr) PC Ti samples, consistent with the Hall–Petch relationship. The stresses due to twinning are small and insignificant in influencing the overall hardening of the PC Ti irradiated sample when compared to the stresses due to the dislocation density. Conversely, SC Ti samples exhibited irradiation-induced hardening. The SC Ti irradiated samples developed additional irradiation-induced modifications in crystallographic texture of (100), (101), (110), (200), (112), (004), and (211) as evidenced from the XRD results, which could probably explain the hardening effect that is caused by irradiation.
The Effects of an Alkaline Treatment on the Ferroelectric Properties of Poly(vinylidene fluoride trifluoroethylene) Films
The effects of an alkaline treatment on the ferroelectric properties of poly(vinylidene fluoride trifluoroethylene) [P(VDF-TrFE)] copolymer films are investigated. The alkaline treatment resulted in a small change in the surface roughness but no significant change in the grain shape or size of P(VDF-TrFE) copolymer films, as evidenced by both scanning electron microscopy and atomic force microscopy images. However, x-ray photoelectron spectroscopy results indicated that the alkaline etchant of a KOH solution reacted with P(VDF-TrFE) films to decrease the number of C-F bonds while creating new carbon conjugated double bonds, which decreased the remanent polarization of the P(VDF-TrFE) films. These results can improve our understanding of the degradation mechanism of an alkaline treatment.
Nanoindentation study of niobium nitride thin films on niobium fabricated by reactive pulsed laser deposition
Nanomechanical and structural properties of NbN x films deposited on single crystal Nb using pulsed laser deposition for different substrate temperature were previously investigated as a function of film/substrate crystal structure (Mamun et al. (2012) [30]). In this study we focus on the effect of laser fluences and background nitrogen pressure on the nanomechanical and structural properties of NbN x films. The crystal structure and surface morphology of the thin films were tested by X-ray diffraction, scanning electron microscopy, and atomic force microscopy. Using nanoindentation, the investigation of the nanomechanical properties revealed that the hardness of the NbN x films was directly influenced by the laser fluence for low background nitrogen pressure, whereas the nanomechanical hardness showed no apparent correlation with laser fluence at high background nitrogen pressure. The NbN x film hardness measured at 30% film thickness increased from 14.0 ± 1.3 to 18.9 ± 2.4 GPa when the laser fluence was increased from 15 to 25 J/cm 2 at 10.7 Pa N 2 pressure. X-ray diffraction showed NbN x films with peaks that correspond to δ-NbN cubic and β-Nb 2 N hexagonal phases in addition to the δ'-NbN hexagonal phase. Finally, increasing the laser fluence resulted in NbN x films with larger grain sizes.
Characterization of surface layers formed on DU10Mo ingots after processing steps and high humidity exposure
The design of monolithic U-Mo fuel elements fabricated from low-enriched uranium for use in high-power research reactors requires bonding of the fuel foil to either Al cladding or a Zr barrier layer. Processing of the U-Mo ingot to final foil form has the potential to generate surface layers on the foil that differ from the bulk, metallic U-Mo. The interfacial properties between the U-Mo and Zr or Al cladding layers will then be determined by these surface layers. We use x-ray photoelectron spectroscopy, cross-sectional scanning electron microscopy, and atomic force microscopy to characterize the composition, oxidation state, and morphology of the surface layers that form after hot rolling and cold rolling depleted U–10 wt% Mo alloy (DU10Mo). A thick uranium nitride layer is observed after hot rolling, although its origin is likely from a previous processing step. The surface composition of cold-rolled DU10Mo varied significantly between two foils, with a strongly Mo-depleted surface oxide layer observed on one foil but nominal Mo composition observed on the other. The efficacy of acid etching in HNO 3 is compared to that of electropolishing in H 2 SO 4 to remove the surface layers, and both methods are found to be similarly effective. Both laboratory (low humidity) air exposure and longer rinse times in water are shown to promote the formation of surface oxide layers. Exposure of both acid-etched and electropolished DU10Mo foils to humid air (97% relative humidity) for six weeks results in formation of a thick oxide layer due to corrosion. The oxide layer on the acid-etched foil is thicker and more highly oxidized than the oxide layer that forms on the electropolished foil, and these differences in oxidation behavior are attributed to higher surface roughness on the acid-etched foil. In general, Mo is found to play a role as a sacrificial element, typically exhibiting a larger ratio of Mo 6+ / Mo 4+ than U 6+ / U 4+ . This is unexpected, given the greater thermodynamic driving force to form U oxides than Mo oxides.
Evolution of solid electrolyte interphase and active material in the silicon wafer model system
Alloying anode materials for lithium-ion batteries, such as silicon (Si), are an important focus of materials research due to the demand for increased energy density for electric vehicles and stationary grid storage. However, progress towards next generation anode materials has been hindered by poor capacity retention due to the instability of the Si active material and the solid electrolyte interphase (SEI). Herein, the evolution of the active Si material and the SEI are simultaneously investigated from the perspective of chemical, structural, morphological, and electronic evolution in the Si wafer model system through its cycling life, using time-of-flight secondary ion mass spectrometry (TOF-SIMS), scanning transmission electron microscopy (STEM), atomic force microscopy (AFM), and scanning spreading resistance microscopy (SSRM). The results illustrate a dynamic evolution of the SEI and active Si material through cycling. Through an improved understanding of evolution of SEI and Si active material within the Si wafer model system, mitigation strategies may be designed to extend the lifetime of Si anodes.
In situ fabrication and characterization of cobalt ferrite nanorods/graphene composites
Cobalt ferrite nanorods/graphene composites were prepared by a one-step hydrothermal process using NaHSO{sub 3} as the reducing agent and 1-propyl-3-hexadecylimidazolium bromide as the structure growth-directing template. The reduction of graphene oxide and the in situ formation of cobalt ferrite nanorods were accomplished in a one-step reaction. The structure and morphology of as-obtained composites were characterized by field emission scanning electron microscopy, transmission electron microscopy, high resolution transmission electron microscopy, atomic force microscope, X-ray diffractometer, Fourier transform infrared spectra, X-ray photoelectron spectroscopy and Raman spectroscopy. Uniform rod-like cobalt ferrites with diameters of about 100 nm and length of about 800 nm were homogeneously distributed on the graphene sheets. The hybrid materials showed a saturation magnetization of 42.5 emu/g and coercivity of 495.1 Oe at room temperature. The electromagnetic parameters were measured using a vector network analyzer. A minimum reflection loss (RL) of − 25.8 dB was observed at 16.1 GHz for the cobalt ferrite nanorods/graphene composites with a thickness of 2 mm, and the effective absorption frequency (RL < − 10 dB) ranged from 13.5 to 18.0 GHz. The composites exhibited better absorbing properties than the cobalt ferrite nanorods and the mixture of cobalt ferrite nanorods and graphene. - Highlights: • Reduction of GO and formation of ferrites were accomplished in a one-step reaction. • Ionic liquid was used to control 1D growth of ferrite nanorods for the first time. • Cobalt ferrite nanorods/graphene composites showed dielectric and magnetic loss. • Cobalt ferrite nanorods/graphene composites exhibited better absorbing properties.
Fabrication and characterization of poly(l-lactic acid) gels induced by fibrous complex crystallization with solvents
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Thickness dependence of Al 0.88 Sc 0.12 N thin films grown on silicon
The thickening behavior of aluminum scandium nitride (Al 0.88 Sc 0.12 N) films grown on Si(111) substrates has been investigated experimentally using X-ray diffraction (XRD), transmission electron microscopy (TEM), atomic force microscopy, and residual stress measurement. Al 0.88 Sc 0.12 N films were grown with thicknesses spanning 14 nm to 1.1 um. TEM analysis shows that the argon sputter etch used to remove the native oxide prior to deposition produced an amorphous, oxygen-rich surface, preventing epitaxial growth. XRD analysis of the films show that the A1ScN(002) orientation improves as the films thicken and the XRD A1ScN(002) rocking curve full width half maximum decreases to 1.34 q for the 1.1 pm thick film. XRD analysis shows that the unit cell is expanded in both the a- and c-axes by Sc doping; the a-axis lattice parameter was measured to be 3.172 ± 0.007 A and the c-axis lattice parameter was measured to be 5.000 ± 0.001 A, representing 1.96% and 0.44% expansions over aluminum nitride lattice parameters, respectively. The grain size and roughness increase as the film thickness increases. A stress gradient forms through the film; the residual stress grows more tensile as the film thickens, from -1.24 GPa to +8.5MPa.
Effects of varying gelatin coating concentrations on RANKL induced osteoclastogenesis
Here, we assessed the effects of varying concentrations of gelatin coating on Receptor Activator of Nuclear Factor κ-B Ligand (RANKL)-induced RAW264.7 murine macrophage differentiation into osteoclast (OC) via osteoclastogenesis. The microstructures of coating surfaces with different concentrations of gelatin were examined by scanning electron microscopy and atomic force microscopy. Increased gelatin coating concentrations led to decreased gel rigidity but increased surface adhesion force attenuated OC differentiation and the decreased actin ring formation in RANKL-induced osteoclastogenesis. The decreased actin ring formation is associated with decreased lysosomal-associated membrane protein 1 (LAMP1) activity and bone resorption in the differentiated OCs with different gelatin coating concentrations as compared to the cells differentiated without gelatin coatings. In addition, increasing concentrations of gelatin coating attenuated the medium TGF-β1 protein levels and the expression levels of TGF-β and type-I (R1) and type-II (R2) TGF-β receptors in OCs, suggesting the gelatin-induced suppression of TGF-β signaling for the regulation of RNAKL-induced OC differentiation. Taken together, these findings showed that changes in gelatin coating concentrations, which were associated with altered gel thickness and substrate rigidity, might attenuate TGF-β signaling events to modulate OC differentiation and concomitant actin ring formation and bone matrix resorption in RANKL-induced osteoclastogenesis.
Self-Healing Thermal Annealing: Surface Morphological Restructuring Control of GaN Nanorods
With advances in nanolithography and dry etching, top-down methods of nanostructuring have become a widely used tool for improving the efficiency of optoelectronics. These nano dimensions can offer various benefits to the device performance in terms of light extraction and efficiency, but often at the expense of emission color quality. Broadening of the target emission peak and unwanted yellow luminescence are characteristic defect-related effects due to the ion beam etching damage, particularly for III–N based materials. In this article we focus on GaN based nanorods, showing that through thermal annealing the surface roughness and deformities of the crystal structure can be “self-healed”. Correlative electron microscopy and atomic force microscopy show the change from spherical nanorods to faceted hexagonal structures, revealing the temperature-dependent surface morphology faceting evolution. The faceted nanorods were shown to be strain- and defect-free by cathodoluminescence hyperspectral imaging, micro-Raman, and transmission electron microscopy (TEM). In-situ TEM thermal annealing experiments allowed for real time observation of dislocation movements and surface restructuring observed in ex-situ annealing TEM sampling. This thermal annealing investigation gives new insight into the redistribution path of GaN material and dislocation movement post growth, allowing for improved understanding and in turn advances in optoelectronic device processing of compound semiconductors.
Optical-Vibrational Properties of the Cs 2 SnX 6 (X = Cl, Br, I) Defect Perovskites and Hole-Transport Efficiency in Dye-Sensitized Solar Cells
We report the vibrational and optical properties of the ‘defect’ perovskites Cs 2 SnX 6 (X = Cl, Br, I) as well as their use as hole-transporting materials (HTMs) in solar cells. All three air-stable compounds were characterized using powder X-ray diffraction and Rietveld refinement. Far-IR reflectance, Raman, and UV–vis spectroscopy as well as electronic band structure calculations show that the compounds are direct band gap semiconductors with a pronounced effect of the halogen atom on the size of the energy gap and the vibrational frequencies. Scanning electron microscopy and atomic force microscopy confirmed that the morphology of the perovskite films deposited from $N,N$-dimethylformamide solutions on TiO 2 substrates also strongly depends on the chemical composition of the materials. The Cs 2 SnX 6 perovskites were introduced as hole-transporting materials in dye-sensitized solar cells, based on mesoporous titania electrodes sensitized with various organic and metal–organic dyes. The solar cells based on Cs 2 SnI 6 HTM and the Z907 dye performed best with a maximum power conversion efficiency of 4.23% at 1 sun illumination. The higher performance of Cs 2 SnI 6 is attributed to efficient charge transport in the bulk material and hole extraction at the perovskite-Pt interface, as evidenced by electrochemical impedance spectroscopy.
Structure and Dynamics Investigations of Sr/Ca-Doped LaPO 4 Proton Conductors
Proton conductors loom out of the pool of candidate materials with great potential to boost hydrogen alternatives to fossil-based resources for energy. Acceptor doped lanthanum orthophosphates are considered for solid oxide fuel cells (SOFCs) for their potential stability and conductivity at high temperature. By exploring the crystal and defect structure of x% Sr/Ca-doped LaPO 4 with different nominal Sr/Ca concentrations (x = 0 – 10) with Neutron powder diffraction (NPD) and X-ray powder diffraction (XRD), we confirm that Sr/Ca-doped LaPO 4 can exist as self-supported structures at high temperatures during solid oxide fuel cell operation. Thermal stability, surface topography, size distribution are also studied to better understand the proton conductivity for dry and wet compounds obtained at sintering temperatures ranging from 1200 to 1400 °C using a combination of scanning electron microscopy (SEM), Atomic Force Microscopy (AFM), Fourier transform infrared spectroscopy (FTIR) and electrochemical impedance spectroscopy (EIS). In conclusion, the results suggest that Sr doped samples exhibit the highest proton conductivity of our samples and illustrate the impact of material design and versatile characterization schemes on the development of proton conductors with superior functionality.
Domain-Dependent Surface Adhesion in Twisted Few-Layer Graphene: Platform for Moiré-Assisted Chemistry
Twisted van der Waals multilayers are widely regarded as a rich platform to access novel electronic phases thanks to the multiple degrees of freedom available for controlling their electronic and chemical properties. Here, in this work, we propose that the stacking domains that form naturally due to the relative twist between successive layers act as an additional ”knob” for controlling the behavior of these systems and report the emergence and engineering of stacking domain-dependent surface chemistry in twisted few-layer graphene. Using mid-infrared near-field optical microscopy and atomic force microscopy, we observe a selective adhesion of metallic nanoparticles and liquid water at the domains with rhombohedral stacking configurations of minimally twisted double bi- and trilayer graphene. Furthermore, we demonstrate that the manipulation of nanoparticles located at certain stacking domains can locally reconfigure the moiré superlattice in their vicinity at the micrometer scale. Our findings establish a new approach to controlling moiré-assisted chemistry and nanoengineering.
Ultra-scalable Multifunctional Nanoengineered Cu and Al surfaces for anti-biofouling applications
Biofouling disrupts surface functionality and integrity of engineered substrates. A variety of natural materials such as plant leaves and insect wings have evolved sophisticated physical mechanisms capable of preventing biofouling. Over the past decade, several reports have pinpointed nanoscale surface topography as an important regulator of the surface adhesion and growth of bacteria. Although artificial nanoengineered features have been used to create bactericidal materials that kill adhered bacteria, functional surfaces capable of synergistically providing anti-biofouling and bactericidal properties remain to be developed. Furthermore,fundamental questions pertaining to the need for intrinsic hydrophobicity to achieve bactericidal performance or the crucial role played by structure length scale (nano vs. micro), remain to be answered. Here, we demonstrate highly scalable, cost effective, and efficient nanoengineered multifunctional surfaces that possess both anti-biofouling and bactericidal properties on industrially relevant copper (Cu) and aluminum (A1) substrates. We characterize biofouling and bactericidal performance using a combination of scanning electron microscopy (SEM), atomic force microscopy (AFM), live-dead bacterial staining and imaging, as well as solution phase measurements of bacterial viability. SEM results showed that nanostructures created on both Cuand Al were capable of physical deformation of adhered E. coli . Bacterial viability measurements on both Cu and Al indicated a complex interaction between the anti-biofouling and bactericidal nature of these materials and their surface topography, chemistry, and structure. We found that nano-length structures, as compared to micro-length, provide improved bactericidal properties,and that increased hydrophobicity greatly decreased the of adhered bacteria while also modestly increasing the surfaces killing capacity. This study provides additional insights into design guidelines for materials that are not only bactericidal, but also anti-biofouling, using a simple and economic method.