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At least 1,729 records · Page 96

A facile synthesis of metal nanoparticle - graphene composites for better absorption of solar radiation

Herein, a facile chemical approach has been adopted to prepare silver nanoparticles (AgNPs)- graphene (G) composite to study photothermal effect. Sodium borohydride (SBH), a strong reducing agent has been selected for this work. Effect of SBH concentrations on optical behavior of AgNPs-G composite was also investigated. Resultant materials were characterized by various techniques including X-ray diffraction (XRD), fourier transform infrared spectroscopy (FTIR), optical absorption, scanning electron microscopy (SEM) and transmission electron microscopy (TEM). SEM micrographs confirm wrapping of AgNPs into graphene whereas XRD analysis reveals their particle size variation between 47 nm to 69 nm. Optical studies throw a light on their strong absorption behavior towards solar radiation.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Study on metal nanoparticles induced third-order optical nonlinearity in phenylhydrazone derivatives with DFWM technique

The third-order nonlinear optical properties of newly synthesized phenylhydrazone derivatives and the influence of noble metal nanoparticles (Ag and Au) on their nonlinear optical responses were investigated by employing Degenerate Four wave Mixing (DFWM) technique with a 7 nanosecond, 10Hz Nd: YAG laser pulses at 532nm. Metal nanoparticles were prepared by laser ablation and the particle formation was confirmed using UV-Visible spectroscopy, Transmission Electron Microscopy (TEM). The nonlinear optical susceptibility were measured and found to be of the order 10{sup −13}esu. The results are encouraging and conclude that the materials are promising candidate for future optical device applications.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Advanced Instrumentation for Metal Additive Manufacturing

Laser powder bed fusion (LPBF) is the most widely used process for metal additive manufacturing (AM), particularly where complex geometries provide performance advantages unattainable with traditional manufacturing techniques. However, LPBF is highly sensitive to innate variability in both the powder spreading and fusion steps, often leading to defects such as pores that are difficult to detect yet significantly impair component mechanical properties and fatigue life. This thesis presents a range of novel instruments enabling both precise assessment of powder layer characteristics and in-situ thermal metrology of metal AM to advance the quality control of LPBF. First, leveraging a custom X-ray microscope and a radiation-transport model developed through this work, transmission X-ray imaging is used to study spreading of thin metal powder layers. Effective layer depth is directly mapped at a process-relevant size scale, surpassing optical techniques that can only estimate local deposition from layer surface topography. Layer packing density and quality are shown to be influenced by powder flowability and particle size relative to nominal powder layer thickness. Layer quality is additionally connected to the geometry of the spreading implement and its velocity. This technique and its presented findings enable pairing feedstocks with spreading strategies that create layers with consistent packing density and uniformity. Second, a twofold approach is employed to optically interrogate the laser fusion step of LPBF for observing signatures of defect formation. Aperture division multiplexing is conceptualized, providing for simultaneous laser delivery and high-fidelity infrared (IR) process monitoring through a common optic. In-situ microscopy at 50 μm spatial resolution and at mid-wave IR wavelengths is proven readily achievable with the first purpose-built optic of this type. Next, a bespoke imaging spectrometer, along with a temperature-emissivity separation technique, is used to retrieve accurate process temperatures over a 1000 K range. Data from these instruments are correlated to porosity as fine as 4.3 μm in two LPBF test artifacts, as verified using computed tomography (CT), establishing the viability of robust optically-based component qualification.

Penny, Ryan↗

Layer-dependent ferromagnetism in a van der Waals crystal down to the monolayer limit

Since the celebrated discovery of graphene, the family of two-dimensional (2D) materials has grown to encompass a broad range of electronic properties. Recent additions include spin-valley coupled semiconductors, Ising superconductors that can be tuned into a quantum metal, possible Mott insulators with tunable charge-density waves, and topological semi-metals with edge transport. Despite this progress, there is still no 2D crystal with intrinsic magnetism, which would be useful for many technologies such as sensing, information, and data storage. Theoretically, magnetic order is prohibited in the 2D isotropic Heisenberg model at finite temperatures by the Mermin-Wagner theorem. However, magnetic anisotropy removes this restriction and enables, for instance, the occurrence of 2D Ising ferromagnetism. Here, we use magneto-optical Kerr effect (MOKE) microscopy to demonstrate that monolayer chromium triiodide (CrI 3 ) is an Ising ferromagnet with out-of-plane spin orientation. Its Curie temperature of 45 K is only slightly lower than the 61 K of the bulk crystal, consistent with a weak interlayer coupling. Moreover, our studies suggest a layer-dependent magnetic phases, showcasing the hallmark thickness dependent physical properties typical of van der Waals crystals. Remarkably, bilayer CrI3 displays suppressed magnetization with a metamagnetic effect, while in trilayer the interlayer ferromagnetism observed in the bulk crystal is restored. Our work creates opportunities for studying magnetism by harnessing the unique features of atomically-thin materials, such as electrical control for realizing magnetoelectronics, and van der Waals engineering for novel interface phenomena.

36 MATERIALS SCIENCE↗

Effect of tilt on circular zone plate performance

Fresnel zone plates are frequently used as focusing and imaging optics in x-ray microscopy, as they provide the ease of use of normal incidence optics. We consider here the effects of tilt misalignment on their optical performance, both in the thin optics limit and in the case of zone plates that are sufficiently thick so that volume diffraction effects come into play. Using multislice propagation, we show that simple analytical models describe the tilt sensitivity of thin zone plates and the thickness at which volume diffraction must be considered, and examine numerically the performance of example zone plates for soft x-ray focusing at 0.5 keV and hard x-ray focusing at 10 keV.

47 OTHER INSTRUMENTATION↗

Single-Molecule Tracking Measurements Reveal the Detailed Mechanisms of Molecular Diffusion in Solvent Mixtures under Nanoconfinement

Understanding mass transport mechanisms in nanopores is important for developing advanced materials for chemical separations, chemical sensing, and energy storage. This paper reports a novel imaging platform that is employed for the first time to investigate the detailed diffusion dynamics of single rhodamine B (RhB) dye molecules confined within solution-filled cylindrical anodic aluminum oxide (AAO) nanopores. The imaging platform relies on illumination of horizontally-oriented AAO nanopores in a highly inclined and laminated optical (HILO) light sheet microscopy geometry. The method was used to investigate the translational and orientational dynamics of single rhodamine B (RhB) molecules within horizontally-oriented 5- and 10-nm diameter AAO nanopores filled with water–ethanol mixtures. The established platform enabled the observation of one-dimensional motion along the pore axis involving occasional short- or long-term immobilization at the single-molecule level. Analysis of cumulative squared-displacement distributions revealed fast (5 – 30 µm²/s), intermediate (1 – 5 µm²/s), and slow (< 1 µm²/s) diffusion components. From the effects of mixture composition and pore size on the contributions of these three components, we inferred that the fast, intermediate, and slow components could be assigned to desorption-mediated hopping, crawling, and wiggling motions, respectively. The platform based on the horizontally-oriented AAO nanopores also permitted single-molecule emission polarization measurements that revealed the negligible steric confinement of individual diffusing RhB molecules within the AAO nanopores. The imaging platform based on AAO membranes and HILO microscopy provided a unique means to investigate how solvation-mediated surface interactions and nanoconfinement govern molecular transport in nanoporous environments.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Laboratory-size three-dimensional x-ray microscope with Wolter type I mirror optics and an electron-impact water window x-ray source

We constructed a laboratory-size three-dimensional water window x-ray microscope that combines wide-field transmission x-ray microscopy with tomographic reconstruction techniques, and observed bio-medical samples to evaluate its applicability to life science research fields. It consists of a condenser and an objective grazing incidence Wolter type I mirror, an electron-impact type oxygen Kα x-ray source, and a back-illuminated CCD for x-ray imaging. A spatial resolution limit of around 1.0 line pairs per micrometer was obtained for two-dimensional transmission images, and 1-μm scale three-dimensional fine structures were resolved.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Effect of substrate rotation on domain structure and magnetic relaxation in magnetic antidot lattice arrays

Microdimensional triangular magnetic antidot lattice arrays were prepared by varying the speed of substrate rotation. The pre-deposition patterning has been performed using photolithography technique followed by a post-deposition lift-off. Surface morphology taken by atomic force microscopy depicted that the growth mechanism of the grains changes from chain like formation to island structures due to the substrate rotation. Study of magnetization reversal via magneto optic Kerr effect based microscopy revealed reduction of uniaxial anisotropy and increase in domain size with substrate rotation. The relaxation measured under constant magnetic field becomes faster with rotation of the substrate during deposition. The nature of relaxation for the non-rotating sample can be described by a double exponential decay. However, the relaxation for the sample with substrate rotation is well described either by a double exponential or a Fatuzzo-Labrune like single exponential decay, which increases in applied field.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Growth from Solutions, Structure, and Photoluminescence of Single-Crystal Plates of p-Terphenyl and Its Trimethylsilyl Derivative

Samples of single-crystal plates of p-terphenyl (3Р) and its derivative with terminal substituents–Si(CH{sub 3}){sub 3} (TMS-3P-TMS), up to 25–30 mm in size and 400 μm thick, have been obtained for the first time by the solvent–antisolvent growth method. The crystal structure at temperatures of 293 and 85 K is refined for 3Р and solved (for the first time) for TMS-3P-TMS using X-ray diffraction. The habit of crystals and their surface morphology are investigated by methods of optical and laser confocal microscopy. The influence of substituent terminal groups -Si(CH{sub 3}){sub 3} on the growth and structure of TMS-3P-TMS crystals is analyzed based on experimental data. The optical absorption and photoluminescence spectra of solutions and crystalline samples are investigated.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Structural and optical changes induced by incorporation of antimony into InAs/GaAs(001) quantum dots

We present experimental evidence of Sb incorporation inside InAs/GaAs(001) quantum dots exposed to an antimony flux immediately before capping with GaAs. The Sb composition profile inside the nanostructures as measured by cross-sectional scanning tunneling and electron transmission microscopies show two differentiated regions within the quantum dots, with an Sb rich alloy at the tip of the quantum dots. Atomic force microscopy and transmission electron microscopy micrographs show increased quantum-dot height with Sb flux exposure. The evolution of the reflection high-energy electron-diffraction pattern suggests that the increased height is due to changes in the quantum-dot capping process related to the presence of segregated Sb atoms. These structural and compositional changes result in a shift of the room-temperature photoluminescence emission from 1.26 to 1.36 {mu}m accompanied by an order of magnitude increase in the room-temperature quantum-dot luminescence intensity.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Femtosecond laser ablation of dielectric materials in the optical breakdown regime: Expansion of a transparent shell

Phase transition pathways of matter upon ablation with ultrashort laser pulses have been considered to be understood long-since for metals and semiconductors. We provide evidence that also certain dielectrics follow the same pathway, even at high pulse energies triggering optical breakdown. Employing femtosecond microscopy, we observe a characteristic ring pattern within the ablating region that dynamically changes for increasing time delays between pump and probe pulse. These transient Newton rings are related to optical interference of the probe beam reflected at the front surface of the ablating layer with the reflection at the interface of the non-ablating substrate. Analysis of the ring structure shows that the ablation mechanism is initiated by a rarefaction wave leading within a few tens of picoseconds to the formation of a transparent thin shell of reduced density and refractive index, featuring optically sharp interfaces. The shell expands and eventually detaches from the solid material at delays of the order of 100 ps.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Squeezing Noise in Microscopy with Quantum Light

Quantum-enhanced microscopes capable of probing classically inaccessible material properties have drawn increasing interest, but most proof-of-principle quantum microscopes have not surpassed classical limits. Here, we discuss the promise and obstacles associated with the use of quantum light with reduced noise (‘squeezed’ light) for quantum-enhanced atomic force microscopy, bioimaging, magneto-optical measurements, and Raman spectroscopy.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Effects of excitation laser wavelength on Ly-{alpha} and He-{alpha} line emission from nitrogen plasmas

Laser-produced nitrogen plasmas emitting radiation at 2.48 nm (Ly-{alpha}) and 2.88 nm (He-{alpha}) are considered potential efficient sources for water-window (WW) microscopy. The atomic and optical properties of nitrogen plasma and influence of the laser wavelength on the line emission in the WW range are investigated. It is found that the optimal temperatures for maximum emission from Ly-{alpha} and He-{alpha} spectral lines are 40-60 eV and 80-100 eV, respectively. The WW line emission and the conversion efficiency (CE) are estimated for three distinct Nd:YAG laser wavelengths (1064 nm, 532 nm, and 266 nm). The calculated CEs are compared with experimentally observed CE values. It is found that 1064 nm wavelength provides the highest CE from laser to Ly-{alpha} and He-{alpha} radiation.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Scanning microscopy in microcircuit failure analysis

A three-phase microcircuit failure analysis procedure is presented. In the first phase, the device is nondestructively tested and the data obtained is correlated with the circumstances surrounding the failure event. The device is then subjected to a limited nondestructive analysis dominated by optical and scanning electron microscopy (SEM). Knowing that microcircuits usually fail from manufacturing defects or misuse, the analyst looks for one of the probable mechanisms. The SEM has two special operating modes that provide unique data for nondestructive analysis: voltage contrast and conductive current. These are used with other SEM modes and surface analysis techniques to analyze complicated microcircuits. The last phase includes the destructive procedures. The end product of these analyses is a corrective action that will yield a highly reliable system.

Nicolas, D. P.↗

Effect of substrates on microstructure and mechanical properties of nano-eutectic 1080 steel produced by aluminothermic reaction

Nano-eutectic bulk 1080 carbon steel was prepared on glass and copper substrates by an aluminothermic reaction casting. The microstructure of the steel was analyzed by an optical microscope, transmission electron microscopy, an electron probe micro-analyzer, a scanning electron microscope and X-ray diffraction. Results show that the microstructure of the steel consisted of a little cementite and lamellar eutectic pearlite. Average lamellar spacing of the pearlite prepared on copper and glass substrates was about 230 nm and 219 nm, respectively. Volume fraction of the pearlite of the two steels was about 95%. Hardness of the steel was about 229 and 270 HV. Tensile strength was about 610 and 641 MPa and tensile elongation was about 15% and 8%. Compressive strength was about 1043 and 1144 MPa. Compared with the steel prepared on copper substrate, the steel prepared on glass substrate had smaller lamellar spacing of the pearlite phase and higher strength, and low ductility due to the smaller spacing. - Highlights: • 1080-carbon steels were successfully prepared by an aluminothermic reaction casting. • Lamellar spacing of the nanoeutetic pearlite is less than 250 nm. • The compressive strength of the steel is about 1144 MPa. • The tensile ductility of the steel is about 15%.

36 MATERIALS SCIENCE↗

Optical tuning of the diamond Fermi level measured by correlated scanning probe microscopy and quantum defect spectroscopy

Quantum technologies based on quantum point defects in crystals require control over the defect charge state. Here we tune the charge state of shallow nitrogen-vacancy and silicon-vacancy centers by locally oxidizing a hydrogenated surface with moderate optical excitation and simultaneous spectral monitoring. The loss of conductivity and change in work function due to oxidation are measured in atmosphere using conductive atomic force microscopy and Kelvin probe force microscopy (KPFM). We correlate these scanning probe measurements with optical spectroscopy of the nitrogen-vacancy and silicon-vacancy centers created via implantation 15–25 nm beneath the diamond surface and annealing. The observed charge state of the defects as a function of optical exposure demonstrates that laser oxidation provides a way to precisely tune the Fermi level over a range of at least 2.00 eV. We also observe a significantly larger oxidation rate for implanted surfaces compared to unimplanted surfaces under ambient conditions. Here, combined with knowledge of the electron affinity of a surface, these results suggest KPFM is a powerful, high-spatial-resolution technique to advance surface Fermi level engineering for charge stabilization of quantum defects.

36 MATERIALS SCIENCE↗

SYNTHESIS AND CHARACTERIZATION OF SMART FUNCTIONAL COATINGS BY CHEMICAL SOLUTION DEPOSITION METHODS

New coating technology enables the fabrication of low cost structural health monitoring (SHM) and tamper indication devices that can be employed to strengthen national and international safeguards objectives. In particular, such innovations could serve the safeguards community by improving both the timeliness of detection and confidence in verification and monitoring. This work investigates the synthesis of functional surface coatings using chemical solutions deposition methods. Chemical solution deposition has recently received attention in the materials research community due to its unique advantages such as low temperature processing, high homogeneity of final products and the ability to fabricate materials with controlled surface properties and pore structures. The synthesis of functional coatings aimed at modifying the materials conductivity and optical properties was investigated by the incorporation of transition element (e.g. Cr{sup +3}) and rare earth (e.g. Er{sup +3}) serving as dopants in a polymer or gel matrix. The structural and morphological investigation of the as-deposited films was carried out using UV/Vis and photoluminescence (PL) spectroscopy. The as deposited coating was further investigated by scanning electron microscopy and energy dispersive x-ray microscopy.

98 NUCLEAR DISARMAMENT, SAFEGUARDS, AND PHYSICAL P↗

XRD, Electron Microscopy and Vibrational Spectroscopy Characterization of Simulated SB6 HLW Glasses - 13028

Sample glasses have been made using SB6 high level waste (HLW) simulant (high in both Al and Fe) with 12 different frit compositions at a constant waste loading of 36 wt.%. As follows from X-ray diffraction (XRD) and optical and scanning electron microscopy (SEM) data, all the samples are composed of primarily glass and minor concentration of spinel phases which form both isometric grains and fine cubic (∼1 μm) crystals. Infrared spectroscopy (IR) spectra of all the glasses within the range of 400-1600 cm{sup -1} consist of the bands due to stretching and bending modes in silicon-oxygen, boron-oxygen, aluminum-oxygen and iron-oxygen structural groups. Raman spectra showed that for the spectra of all the glasses within the range of 850-1200 cm{sup -1} the best fit is achieved by suggestion of overlapping of three major components with maxima at 911-936 cm{sup -1}, 988-996 cm{sup -1} and 1020-1045 cm{sup -1}. The structural network is primarily composed of metasilicate chains and rings with embedded AlO{sub 4} and FeO{sub 4} tetrahedra. Major BO{sub 4} tetrahedra and BO{sub 3} triangles form complex borate units and are present as separate constituents. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗