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DOE OSTI2015

Insights into the structure–photoreactivity relationships in well-defined perovskite ferroelectric KNbO 3 nanowires

Structure–function correlations are a central theme in heterogeneous (photo)catalysis. In this study, the geometric and electronic structure of perovskite ferroelectric KNbO 3 nanowires with respective orthorhombic and monoclinic polymorphs have been systematically addressed. By virtue of aberration-corrected scanning transmission electron microscopy, we directly visualize surface photocatalytic active sites, measure local atomic displacements at an accuracy of several picometers, and quantify ferroelectric polarization combined with first-principles calculations. The photoreactivity of the as-prepared KNbO 3 nanowires is assessed toward aqueous rhodamine B degradation under UV light. A synergy between the ferroelectric polarization and electronic structure in photoreactivity enhancement is uncovered, which accounts for the prominent reactivity order: orthorhombic > monoclinic. Additionally, by identifying new photocatalytic products, rhodamine B degradation pathways involving N-deethylation and conjugated structure cleavage are proposed. The findings not only provide new insights into the structure–photoreactivity relationships in perovskite ferroelectric photocatalysts, but also have broad implications in perovskite-based water splitting and photovoltaics, among others.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2013

Surface photoelectric and visible light driven photocatalytic properties of zinc antimonate-based photocatalysts

Highlights: ► N-doped and pristine ZnSb{sub 2}O{sub 6} photocatalysts were synthesized by a facile method. ► N-doped ZnSb{sub 2}O{sub 6} shows a significant enhanced visible light photocatalytic activity. ► The N-doped ZnSb{sub 2}O{sub 6} shows the reduced surface photovoltage signals. - Abstract: The N-doped and pristine ZnSb{sub 2}O{sub 6} photocatalysts were synthesized by a facile method. The samples were characterized by X-ray diffraction (XRD), UV–vis spectroscopy, surface photovoltage spectroscopy and scanning electron microscopy. The photocatalytic activities of the prepared samples were evaluated from the degradation of rhodamine B (RhB) under full arc and visible light irradiation of Xe lamp. The XRD and UV–vis results indicated that the N-doping did not change the crystal structure, but decrease the band gap in comparison with the pristine one. The N-doped ZnSb{sub 2}O{sub 6} shows the reduced surface photovoltage signals and the significantly enhanced photocatalytic activity under two irradiation conditions.

36 MATERIALS SCIENCE↗

DOE OSTI2012

Oriented growth of urchin-like zinc oxide micro/nano-scale structures in aqueous solution

Highlights: Black-Right-Pointing-Pointer Highly oriented and well-defined ZnO urchin-like crystals were successfully fabricated by a facile and effective hydrotherm method. Black-Right-Pointing-Pointer Polyvinylpyrrolidone- and hydrogen peroxide-assisted synthesis of ZnO could optimize its crystalline quality and the obtained ZnO have smooth surface, radial growth of morphology, obvious crystal edges and decreased defects. Black-Right-Pointing-Pointer The physicochemical properties of samples were studied by analysis of its structure, morphology, surface and optical properties. Black-Right-Pointing-Pointer This study represented a multistep mechanism based on [Zn(OH){sub 4}]{sup 2-} growth units about formation such urchin-like structure. -- Abstract: The urchin-like ZnO microcrystals with high crystallinity decomposed from [Zn(OH){sub 4}]{sup 2-} directly were obtained via a hydrothermal method. The morphology, particle size, crystalline structure and fluorescence of the as-prepared ZnO were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD) and photoluminescence (PL) analyses. The results demonstrated that the urchin-like ZnO crystals with wurtzite structure had a narrow distribution in size, which could be adjusted in the range of 30-80 {mu}m by varying reaction time. Broad visible light emission peak was also observed in the PL spectra of the synthesized ZnO products. A multistep growth process about how to form such a structure was proposed.

36 MATERIALS SCIENCE↗

DOE OSTI2010

Detection of exposure damage in composite materials using Fourier transform infrared technology.

Goal: to detect the subtle changes in laminate composite structures brought about by thermal, chemical, ultraviolet, and moisture exposure. Compare sensitivity of an array of NDI methods, including Fourier Transform Infrared Spectroscopy (FTIR), to detect subtle differences in composite materials due to deterioration. Inspection methods applied: ultrasonic pulse echo, through transmission ultrasonics, thermography, resonance testing, mechanical impedance analysis, eddy current, low frequency bond testing & FTIR. Comparisons between the NDI methods are being used to establish the potential of FTIR to provide the necessary sensitivity to non-visible, yet significant, damage in the resin and fiber matrix of composite structures. Comparison of NDI results with short beam shear tests are being used to relate NDI sensitivity to reduction in structural performance. Chemical analyses technique, which measures the infrared intensity versus wavelength of light reflected on the surface of a structure (chemical and physical information via this signature). Advances in instrumentation have resulted in hand-held portable devices that allow for field use (few seconds per scan). Shows promise for production quality assurance and in-service applications on composite aircraft structures (scarfed repairs). Statistical analysis on frequency spectrums produced by FTIR interrogations are being used to produce an NDI technique for assessing material integrity. Conclusions are: (1) Use of NDI to assess loss of composite laminate integrity brought about by thermal, chemical, ultraviolet, and moisture exposure. (2) Degradation trends between SBS strength and exposure levels (temperature and time) have been established for different materials. (3) Various NDI methods have been applied to evaluate damage and relate this to loss of integrity - PE UT shows greatest sensitivity. (4) FTIR shows promise for damage detection and calibration to predict structural integrity (short beam shear). (5) Detection of damage for medium exposure levels (possibly resin matrix degradation only) is more difficult and requires additional study. (6) These are initial results only - program is continuing with additional heat, UV, chemical and water exposure test specimens.

36 MATERIALS SCIENCE↗

DOE OSTI2017

Synthesis of m-LaVO{sub 4}/BiOBr composite photocatalysts and their photocatalytic performance under visible light

Highlights: • A hydrothermal route to m-LaVO{sub 4}/BiOBr composite photocatalysts was proposed. • Products exhibit excellent photocatalytic activity under visible light. • Enhanced photocatalytic activity can be ascribed to forming p-n heterojunction. - Abstract: Visible-light driven m-LaVO{sub 4}/BiOBr composite photocatalysts were synthesized by a two-step hydrothermal process, and were characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), photoluminescence spectroscopy (PL), and UV–vis diffuse reflectance spectroscopy, respectively. The results showed that 1.0 wt% LaVO{sub 4}/BiOBr sample exhibits the highest photodegradation rate of RhB under visible-light irradiation, within 60 mins, it achieved 83.37%. The enhanced photocatalytic performance can be ascribed to the formation of p-n heterojunction structure and the inhibition of m-LaVO{sub 4} to 2D growth of BiOBr to a certain extent.

36 MATERIALS SCIENCE↗

DOE OSTI2011

Interplay between Ferroelastic and Metal-Insulator Phase Transitions in Strained Quasi-2D VO[subscript 2] Nanoplatelets

Formation of ferroelastic twin domains in vanadium dioxide (VO{sub 2}) nanosystems can strongly affect local strain distributions, and hence couple to the strain-controlled metal-insulator transition. Here we report polarized-light optical and scanning microwave microscopy studies of interrelated ferroelastic and metal-insulator transitions in single-crystalline VO{sub 2} quasi-two-dimensional (quasi-2D) nanoplatelets (NPls). In contrast to quasi-1D single-crystalline nanobeams, the 2D geometric frustration results in emergence of several possible families of ferroelastic domains in NPls, thus allowing systematic studies of strain-controlled transitions in the presence of geometrical frustration. We demonstrate the possibility of controlling the ferroelastic domain population by the strength of the NPl-substrate interaction, mechanical stress, and by the NPl lateral size. Ferroelastic domain species and domain walls are identified based on standard group-theoretical considerations. Using variable temperature microscopy, we imaged the development of domains of metallic and semiconducting phases during the metal-insulator phase transition and nontrivial strain-driven reentrant domain formation. A long-range reconstruction of ferroelastic structures accommodating metal-insulator domain formation has been observed. These studies illustrate that a complete picture of the phase transitions in single-crystalline and disordered VO{sub 2} structures can be drawn only if both ferroelastic and metal-insulator strain effects are taken into consideration and understood.

36 MATERIALS SCIENCE↗

DOE OSTI2015

Tapioca starch: An efficient fuel in gel-combustion synthesis of photocatalytically and anti-microbially active ZnO nanoparticles

Zinc oxide nanoparticles were synthesized by gel-combustion method using novel bio-fuel tapioca starch pearls, derived from the tubers of Manihotesculenta. The product is characterized using various techniques. The X-ray diffraction pattern correspond to a hexagonal zincite structure. Fourier transform infrared spectrum showed main absorption peaks at 394 and 508 cm{sup −} {sup 1} due to stretching vibration of Zn–O. Ultravoilet–visible spectrum of zinc oxide nanoparticles showed absorption maximum at 373 nm whereas the maximum of the bulk zinc oxide was 377 nm. The morphology of the product was studied using scanning electron microscopy and transmission electron microscopy. The scanning electron microscopic images showed that the products are agglomerated and porous in nature. The transmission electron microscopic images revealed spherical particles of 40–50 nm in diameter. The photocatalytic degradation of methylene blue was examined using zinc oxide nanoparticles and found more efficient in sunlight than ultra-violet light due to reduced band gap. The antibacterial properties of zinc oxide nanoparticles were investigated against four bacterial strains Klebsiella aerogenes, Escherichia coli, Pseudomonas aeruginosa and Staphylococcus aereus, where Pseudomonas aeruginosa and Staphylococcus aereus exhibited significant antibacterial activity in agar well diffusion method when compared to positive control. - Highlights: • ZnO nanoparticles have been prepared from a new bio-fuel, tapioca starch by gel combustion method. • XRD pattern revealed hexagonal zincite crystal structure with crystallite size 33 nm. • ZnO nanoparticles exhibited a band gap of 2.70 eV. • The ZnO nanoparticles exhibited superior degradation in sunlight in comparison with UV light. • The product showed a good anti-bacterial activity against two bacterial strains.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

DOE OSTI2011

Scanning tunneling microscopic studies of laser-induced modifications of Si(001)-(2 x 1) surface

Scanning tunneling microscopic studies of Si(001)-2 x 1 surfaces excited with 532-nm laser pulses of intensities below melting and ablation thresholds have revealed two different modes of structural modifications, strongly depending on the intensity of laser lights. The excitation below 100 mJ/cm{sup 2} causes bond rupture at individual dimer-sites leading to the formation of vacancies selectively on the outermost layer. The bond rupture, which shows a strongly site-sensitive rate, forms efficiently vacancy-strings elongated along the surface dimer-rows. Selective removal of surface dimers results in the exposure of flat and defect-less underlying layer as reported previously, which is resistive to the excitation at this range of intensity. At intensities above 100 mJ/cm{sup 2}, on the other hand, the excitation forms not only vacancies but also ad-dimers on terraces. The number density of ad-dimers is in proportion to the square of that for vacancies, indicating strongly that silicon atoms released by laser-induced bond rupture are associated with each other to form ad-dimers. The repeated irradiations at this range of intensities induce anisotropic growth of ad-dimer islands and of vacancy clusters on terrace regions, leading to multiply terraced structure. The primary processes of the structural modifications are discussed based on the quantitative analyses of the growth of vacancy and ad-dimer under excitation.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Investigating Grain Structure and Microcracking in SiCf-SiCm Composites Using 4D-STEM

Silicon carbide (SiC) fiber-reinforced SiC matrix composites (SiCf-SiCm) are promising materials for accident-tolerant fuel (ATF) cladding in light water reactors. This paper, using four-dimensional scanning transmission electron microscopy (4D-STEM), studied the microstructure of SiCf-SiCm at nanoscale and provided grain statistics at the CVI/fiber region. Here, the results reveal that CVI region mainly contain irregular sub-micron grains (115 nm to 1800 nm) with a preferred orientation, while the fiber region has nano equiaxed grains (21 nm to 78 nm) with random orientations. Centered dark field imaging over the fiber regions verified the grain size measurement by 4D-STEM. Through 4D-STEM virtual dark field imaging and orientation mapping, intragranular propagation was identified as the fracture mechanism for a microcrack observed within the CVI region. The amorphous pyrolytic carbon layer was also shown to effectively arrest the microcrack.

4D-STEM↗

DOE OSTI2011

Facile synthesis of mesoporous core-shell TiO{sub 2} nanostructures from TiCl{sub 3}

Highlights: {yields} Stable TiCl{sub 3} solution is adopted as Ti sources. {yields} Low-cost glucose assisted facile solvothermal reactions. {yields} Exquisite core-shell morphology and mesoporous structure of TiO{sub 2} nanostructures. {yields} Superior photocatalytic activity of TiO{sub 2} nanostructures in UV light irradiation. -- Abstract: The present study reports the synthesis and formation process of mesoporous core-shell TiO{sub 2} nanostructures by employing a glucose-assisted solvothermal process using water-ethanol mixture as solvent and subsequent calcination process at 550 {sup o}C for 4 h. X-ray diffraction, field emission scanning electron microscopy, transmission electron microscopy and nitrogen adsorption-desorption analysis were used to investigate the structural properties of these nanostructures. By optimizing the preparation conditions, especially the contents of water and ethanol in the mixture solvent, mesoporous core-shell TiO{sub 2} nanostructures were obtained. These mesoporous nanostructures have anatase phase and exhibit the superior photocatalytic activity. This synthesis route is facile due to the usage of stable and low-cost Ti precursor such as TiCl{sub 3} and is thus applicable for large-scale production.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2014

Nonlinear optical propagation in a tandem structure comprising nonlinear absorption and scattering materials

Laser propagation in a tandem structure comprising carbon nanotubes and phthalocyanines is studied by Z-scan method. Due to the different mechanisms of the two materials, the laser beam can be attenuated with different absorptivities, by changing the sequence of light passing through each material. Numerical simulations considering the effect of path length and the change of nonlinear coefficient within each material are conducted for understanding the distribution of laser intensity in the tandem system and hence, fitting of the asymmetric Z-scan curves. The results are helpful for the design of nonlinear optical devices comprising multiple nonlinear materials and mechanisms.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

DOE OSTI2015

Single-photon single ionization of W + ions: experiment and theory

Experimental and theoretical results are reported for photoionization of Ta-like (W + ) tungsten ions. Absolute cross sections were measured in the energy range 16-245 eV employing the photon-ion merged-beam setup at the advanced light source in Berkeley. Detailed photon-energy scans at 100 meV bandwidth were performed in the 16-108 eV range. In addition, the cross section was scanned at 50 meV resolution in regions where fine resonance structures could be observed. Theoretical results were obtained from a Dirac-Coulomb R-matrix approach. Photoionization cross section calculations were performed for singly ionized atomic tungsten ions in their J = 1/2, ground level and the associated excited metastable levels with J = 3/2, 5/2, 7/2 and 9/2. Since the ion beams used in the experiments must be expected to contain long-lived excited states also from excited configurations, additional cross-section calculations were performed for the second-lowest term, J = 5/2, and for the 4 F term, with J = 3/2, 5/2, 7/2 and 9/2. Given the complexity of the electronic structure of W + the calculations reproduce the main features of the experimental cross section quite well.

74 ATOMIC AND MOLECULAR PHYSICS↗

DOE OSTI2010

Optical switches based on CdS single nanowire

CdS nanowires have been synthesized by a composite-hydroxide-mediated approach. The characterization of the nanowire with X-ray diffraction, scanning electron microscopy, and transmission electron microscopy indicated a single-crystalline hexagonal structure growing along [21-bar 1-bar 0] direction with length up to 100 {mu}m. The UV-visible reflection spectrum demonstrated a band gap of 2.36 eV. A strong light emission centered at 543 nm was observed under different excitation wavelengths of 300, 320, 360 and 400 nm, which was further confirmed by a bright fluorescent imaging of a single CdS nanowire. The photocurrent response based on a single CdS nanowire showed distinct optical switch under the intermittent illumination of white light. The rise and decay time were less than 1.0 and 0.2 s, respectively, indicating high crystallization with fewer trap centers in the CdS nanowires. It is possible that the undesirable trapping effects on grain-boundaries for photoconductors could be avoided thanks to the single-crystalline nature of the CdS nanowires.

36 MATERIALS SCIENCE↗

DOE OSTI2014

The site occupation and valence of Mn ions in the crystal lattice of Sr{sub 4}Al{sub 14}O{sub 25} and its deep red emission for high color-rendering white light-emitting diodes

Highlights: • Different valences of Mn ions in Sr{sub 4}Al{sub 14}O{sub 25} were identified using XANES and EPR. • Red luminescence was attributed to Mn{sup 4+} occupying the center of AlO{sub 6} octahedron. • The Mn{sup 3+} incorporated in the center of AlO{sub 4} tetrahedron was non-luminescent. • The bond-valence theory was used to analyze the effective valences of cations. • A white LED device with CRI up to Ra 93.23 was packaged by using the red phosphor. - Abstract: The synthesis and component of red phosphor, Sr{sub 4}Al{sub 14}O{sub 25}: Mn, were optimized for application in white light-emitting diodes. The microstructure and morphology were investigated by the X-ray diffraction and scanning electron microscopy. Different valences of Mn ions in Sr{sub 4}Al{sub 14}O{sub 25} were discriminated using the electron paramagnetic resonance and X-ray absorption near-edge structure spectroscopy techniques. The bond-valence theory was used to analyze the effective valences of Sr{sup 2+} and Al{sup 3+} in Sr{sub 4}Al{sub 14}O{sub 25}. As a result, the strong covalence of Al{sup 3+} in the AlO{sub 4} tetrahedron other than in the AlO{sub 6} octahedron is disclosed. The deep red emission is attributed to Mn{sup 4+} occupying the center of AlO{sub 6} octahedron. The mechanism of energy transfer is mainly through dipole–dipole interaction, revealed by the analyses of critical distance and concentration quench. A high color rendering white LED prototype with color-rendering index up to Ra 93.23 packaged by using the red phosphor demonstrates its applicability.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Plasmon 3D Electron Tomography and Local Electric-Field Enhancement of Engineered Plasmonic Nanoantennas

Plasmonic nano-antennas are pushing the limits of optical imaging resolution capabilities in near-field scanning optical microscopy (NSOM). Accordingly, these techniques are driving the basic understanding of photonic and optoelectronic nanoscale devices with applications in sensing, energy conversion, solid-state lighting and information technology. Imaging the localized surface plasmon resonance (LSPR) at the nanoscale is a key to understanding the optical responses of a given tip geometry in order to engineer better plasmonic nano-antennas for near-field experiments. In recent years the advancement of focused ion beam technology provides the ability to directly modify plasmonic structures with nanometer resolution. Also, scanning transmission electron microscopy (STEM) with electron energy loss spectroscopy (EELS) is an established technique allowing imaging of LSPR. Specifically, the combination of these two techniques provides spectrally sensitive two-dimensional (2D) imaging information to better visualize and understand LSPR on the nanometer scale. This can be combined with electron tomography to provide the three-dimensional LSPR distribution. Here in this paper we demonstrate the fabrication of Au nano-pyramids using helium ion microscopy, and analyze the LSPR in 3D reconstructions produced by total variation (TV)-norm minimization of a set of 2D STEM-EELS maps. Additionally, a boundary element simulation method was used to verify the experimentally observed nanopyramid LSPR modes. Finally, we show that the point-spread-functions (PSF) of LSPR mode hot spots in nanopyramids differ to local electric-field enhancement under optical excitation making direct comparison to NSOM experimental resolution difficult. Furthermore, the STEM-EELS results show how LSPR modes are influenced by the tip characteristics, which can inform the development of new nano-antenna designs.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

DOE OSTI2015

Synthesis, characterization and hydrophilic properties of ZnFe{sub 2}O{sub 4}–TiO{sub 2} composite film

Highlights: • ZnFe{sub 2}O{sub 4}–TiO{sub 2} composite films have been successfully prepared via a sol–gel method. • It was deposited on glass slides through dip coating process. • 7% ZnFe{sub 2}O{sub 4}–TiO{sub 2} film exhibits a superhydrophilic property with a contact angle 0°. • The self-cleaning glasses also display antifogging property. - Abstract: ZnFe{sub 2}O{sub 4}–TiO{sub 2} composite films have been successfully prepared via a sol–gel method and deposited on glass slides through dip coating process. The hydrophilicity of ZnFe{sub 2}O{sub 4}–TiO{sub 2} composite films was investigated by the contact angles measurements under different conditions, including heat treatment temperature, molar ratios of ZnFe{sub 2}O{sub 4} to TiO{sub 2} and coating layers. The results revealed that the 7 mol% ZnFe{sub 2}O{sub 4}-TiO{sub 2} composite film exhibits an excellent superhydrophilic performance with a contact angle 0°. Compared with normal glass, the self-cleaning glasses also display antifogging property. The transmittance of ZnFe{sub 2}O{sub 4}–TiO{sub 2} composite films was characterized by UV–vis spectra in details. Coating layers and different molar percents of ZnFe{sub 2}O{sub 4} all have impact on the light transmittance. Moreover, the structure and morphology of the ZnFe{sub 2}O{sub 4}–TiO{sub 2} sample were investigated by means of X-ray diffraction (XRD), energy dispersive X-ray spectrometry (EDS) and scanning electron microscopy (SEM)

36 MATERIALS SCIENCE↗

DOE OSTI2018

Probing Light Atoms at Subnanometer Resolution: Realization of Scanning Transmission Electron Microscope Holography

Atomic resolution imaging of light elements in electron-transparent materials has long been a challenge. Biomolecular materials, for example, are rapidly altered by incident electrons. We demonstrate a scanning transmission electron microscopy (STEM) technique, called STEM holography, capable of efficient structural analysis of beam-sensitive nanomaterials. STEM holography measures the absolute phase and amplitude of electrons passed through a specimen via interference with a vacuum reference wave. We use an amplitude-dividing nanofabricated grating to prepare multiple beams focused at the sample. We configure the postspecimen microscope imaging system to overlap the beams, forming an interference pattern. We record and analyze the pattern at each 2D-raster-scan-position, reconstructing the complex object wave. As a demonstration, we image gold nanoparticles on an amorphous carbon substrate at 2.4 Å resolution. In conclusion STEM holography offers higher contrast of the carbon while maintaining gold atomic lattice resolution compared to high angle annular dark field STEM.

4D-STEM↗

DOE OSTI2022

Stressing Halide Perovskites with Light and Electric Fields

Understanding the light and electric field-induced effects underlying the local changes in optoelectronic properties in lead halide perovskites is crucial to establish a detailed structure–function relationship. Here, in this study, we use single-molecule absorption scanning tunneling microscopy (SMA-STM) to probe the local surface inhomogeneity of a mixed A-site cation/mixed halide perovskite under pulsed 532 nm photoexcitation to gain insight into the varying grain-to-grain absorption behavior at the nanoscale and reduction in the electronic bandgap under illumination. To correlate the observed changes in the absorption signal to structural ones, we utilize synchrotron X-ray STM (SX-STM) where we find that photoexcitation induces changes in the X-ray absorption spectral signatures. Lastly, using pump–probe time-resolved wide-angle X-ray scattering, we show the presence of nonthermal lattice deformations upon photoexcitation which indicate that the excited photocarriers distort the perovskite lattice, corroborating the local electronic changes observed by our STM measurements.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗