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At least 703 records · Page 39

Quantitative Nonlinear Optical Polarimetry with High Spatial Resolution

Nonlinear optical microscopy such as in the optical second-harmonic generation (SHG) modality has become a popular tool today for probing materials in the physical and biological sciences. While imaging and spectroscopy are widely used in the microscopy mode, nonlinear polarimetry, which can shed light on materials’ symmetry and microstructure, is relatively underdeveloped. This is partly because quantitative analytical modeling of the optical SHG response for anisotropic crystals and films largely assumes low-numerical aperture (NA) focusing of light, where the plane-wave approximation is sufficient. Tight focusing provides unique benefits in revealing out-of-plane polarization responses, which cannot be detected by near-plane-wave illumination at normal incidence. Here, we outline a method for quantitatively analyzing SHG polarimetry measurements obtained under high-NA focusing within a microscope geometry. Experiments and simulations of a variety of standard samples, from single crystals to thin films, are in good agreement, including measured and simulated spatial SHG maps of ferroelectric domains. A solution to the inverse problem is demonstrated, where the spatial distribution of an SHG tensor with unknown tensor coefficient magnitudes is determined by experimentally measured polarimetry. The ability to extract the out-of-plane component of the nonlinear polarization in normal incidence is demonstrated, which can be valuable for high-resolution polarimetry of 2D materials, thin films, heterostructures, and uniaxial crystals with a strong out-of-plane response.

36 MATERIALS SCIENCE↗

Estimation of position resolution for DOI-PET detector using diameter 0.2 mm WLS fibers [ANIMMA--2015-IO-x5]

We have been developing a submillimeter resolution and low-cost DOI-PET detector using wavelength shifting fibers (WLSF), scintillating crystal plates and MPPCs (Hamamatsu Photonics). Conventional design of DOI-PET detectors had approximately mm{sup 3} of resolution by using some scintillating blocks with a volume of 1 mm{sup 3}, which detects gamma-ray. They are expensive due to difficulties in processing scintillating crystals and a large number of photo-detectors, and these technologies are likely to reach the limit of the resolution. Development of a lower cost DOI-PET detector with higher resolution is challenging to popularize the PET diagnosis. We propose two type of PET detector. One is a whole body PET system, and the other is a PET system for brain or small animals. Each PET system consists 6 blocks. The former consists of 6 layers of crystal plates with 300 mm x 300 mm x 4 mm. The latter consists of 16 crystal layers, forming 4 x 4 crystal arrays. The size of the crystal plate is 40 mm x 40 mm x 1 mm. Wavelength shifting fiber (WLSF) sheets are attached to above and up and down side of crystal planes. The whole PET system has 8 MPPCs attached on each side. For the brain PET detector, 9 WLSF fibers are attached on the each side. The expected position resolution would be less than 1 mm at the former system. We have performed an experimental performance estimation for the system component using {sup 22}Na radioactive source. We achieved a collection efficiency of 10% using the WLSF sheet and Ce:Gd{sub 3}(Al,Ga){sub 5}O{sub 12} (GAGG) crystals at 511 keV. The linear relationship between reconstruction position and incident position was obtained, and a resolution of 0.7 mm (FWHM) for x-axis of DOI by the WLSF readout was achieved. (authors)

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

The Role of Ice Splintering on Microphysics of Deep Convective Clouds Forming Under Different Aerosol Conditions: Simulations Using the Model With Spectral Bin Microphysics

Observations during the Ice in Clouds Experiment-Tropical (ICE-T) field experiment show that the ice particles concentration in a developing deep convective clouds at the level of T = -15 °C reached about 500 L -1 , that is, many orders higher than that of ice-nucleating particle. To simulate microphysics of these clouds, the 2-D Hebrew University Cloud model (HUCM) with spectral bin microphysics was used in which two main types of ice multiplication mechanisms were included in addition to the Hallet-Mossop mechanism. In the first ice multiplication mechanism ice splinters form by drop freezing and drop-ice collisions. Ice multiplication of this type dominates during developing stage of cloud evolution, when liquid water content is significant. At later stage when clouds become nearly glaciated, ice crystals are produced largely by ice splintering during ice-ice collisions (the second ice multiplication mechanism). Simulations show that droplet size distributions, as well as size distributions of ice particles, agree well with the measurements during ICE-T. Simulations with different cloud condensation nuclei concentrations show the existence of the “optimum” cloud condensation nuclei concentration (or droplet concentration), at which concentration of ice splinters reaches maximum. In these simulations ice nucleation caused by the direct formation of ice crystals upon ice-nucleating particles, as well as the Hallett-Mossop process, has a negligible contribution to the ice crystal concentration.

54 ENVIRONMENTAL SCIENCES↗

Rapid Crystallization of Zeolites with Controllable Defects: Disentangling Fluoride Concentration and pH Using NH 4 F

Zeolite synthesis is typically conducted either under basic conditions or in neutral fluoride media using hydrofluoric acid (HF). While basic (OH − ) conditions generally result in faster zeolite crystallization, they can also increase the likelihood of framework defects and crystal intergrowths. In contrast, synthesis in neutral fluoride media tends to produce fewer defects because fluoride balances positive charges from structure-directing agents. However, this method often requires significantly longer crystallization times and involves the handling of dangerous HF. In the present study, we pursue the best of both synthesis conditions, rapid syntheses with controllable defect concentrations, by disentangling of mineralizing agent and chargebalancing agent using ammonium fluoride (NH 4 F) as an alternative to HF. We have investigated the use of NH 4 F in the syntheses of siliceous and aluminum-containing zeolite A (LTA, small pore), ZSM-5 (MFI, medium pore), and siliceous Beta(*BEA, large pore). The crystallization times of all four zeolites decreased substantially with an increasing NH 4 F concentration. Crystallization times were reduced from 24 to 4 h (Si-LTA), 96 to 36 h (Al-LTA), 240 to 6 h (ZSM-5), and 24 to 3 h (Si-*BEA). Additionally, increasing the NH 4 F concentration in the synthesis mixtures decreases the defect densities of siliceous zeolites. Raman spectroscopy, along with 29 Si MAS NMR, 19 F MAS NMR, 13 C MAS NMR, and fluorine elemental analysis of Si-LTA samples confirms that the reduction in charged defects (Si−O − ) is due to the higher incorporation of F − within the double four-membered ring (D4R) present in the LTA samples. We show that the accelerated crystallization is due to the role of F − in enhancing the silica mineralization rate (formation of silicon hexafluoride species) and stabilizing D4Rs under basic conditions. As a result, combining basic and fluoride-mediated synthesis could therefore be advantageous for faster zeolite production and improved control over structural properties for a wide variety of zeolite structures.

Anions↗

Cs 2 Hg 3 S 4 : A Low-Dimensional Direct Bandgap Semiconductor

Cs2Hg3S4 was synthesized by slowly cooling a melted stoichiometric mixture of Hg and Cs2S4. Cs2Hg3S4 crystallizes in the Ibam spacegroup with a = 6.278(1) angstrom, b = 11.601(2) angstrom, and c = 14.431(3)angstrom; d(calc) = 6.29 g/cm(3). Its crystal structure consists of straight chains of [Hg3S4](n)(2n-) that engage in side-by-side weak bonding interactions forming layers and are charge balanced by Cs+ cations. The thermal stability of this compound was investigated with differential thermal analysis and temperature dependent in situ synchrotron powder diffraction. The thermal expansion coefficients of the a, b, and c axes were assessed at 1.56 x 10(-5), 2.79 x10(-5), and 3.04 x 10(-5) K-1, respectively. Large single-crystals up to similar to 5 cm in length and similar to 1 cm in diameter were grown using a vertical Bridgman method. Electrical conductivity and photoconductivity measurements on naturally cleaved crystals of Cs2Hg3S4 gave resistivity rho of >= 10(8) Omega.cm and carrier mobility-lifetime (mu tau) products of 4.2 x 10(-4) and 5.82 x 10(-5) cm(2) V-1 for electrons and holes, respectively. Cs2Hg3S4 is a semiconductor with a bandgap E-g similar to 2.8 eV and exhibits photoluminescence (PL) at low temperature. Electronic band structure calculations within the density functional theory (DFT) framework employing the nonlocal hybrid functional within Heyd-Scuseria-Ernzerhof (HSE) formalism indicate a direct bandgap of 2.81 eV at Gamma. The theoretical calculations show that the conduction band minimum has a highly dispersive and relatively isotropic mercury-based s-orbital-like character while the valence band maximum features a much less dispersive and more anisotropic sulfur orbital-based band.

Islam, Saiful M.↗

Self-selecting vapor growth of transition-metal-halide single crystals

Transition-metal halides can host a large variety of novel phenomena, such as magnetism in the monolayer limit, quantum spin liquid and spiral spin liquid states, topological magnons, and chiral phonons. Sizable high-quality single crystals are necessary for investigations of magnetic and lattice excitations by, for example, inelastic neutron scattering. In this paper, we review a less well-known vapor transport technique, self-selecting vapor growth, and report our growths of transition-metal halides using this technique. We report the growth and characterizations of sizable single crystals of α–RuCl 3 , CrCl 3 , Ru 1–x Cr x Cl 3 , and CrBr 3 . In order to expedite the conversion of starting powder to single crystals, we modified the technique by cooling the growth ampoule through an appropriate temperature range. Our work shows that the self-selecting vapor transport technique can provide large single crystals of transition-metal halides, demonstrating its potential for providing high-quality single crystals of quantum materials.

2-dimensional systems↗

Effect of adjusting composition on the crystallization and luminescence properties in NaYF{sub 4}:Er{sup 3+} embedded glass ceramics

Highlights: • Intense 2.7 μm emission was achieved in transparent glass ceramics containing NaYF{sub 4}:Er{sup 3+} nanocrystals. • The crystallization and luminescence properties of the nanocrystals embedded glass ceramics are tuned by adjusting the Na{sub 2}O/NaF ratio. • Modifying the properties of glass ceramics through adjusting the glass composition is an effective route. - Abstract: Intense 2.7 μm emission was achieved in transparent glass ceramics containing NaYF{sub 4}:Er{sup 3+} nanocrystals. The effect of adjusting Na{sub 2}O/NaF ratio in glass composition on the crystallizing and luminescence behavior in the glass ceramics was investigated. The controllable crystallization property of NaYF{sub 4} nanocrystals was remained after modifying the glass composition and the crystallization temperature was largely reduced for the samples with high Na{sub 2}O content. The X-ray diffraction and transmission electron microscopy analysis evidenced the shrink of lattice parameter with increasing Na{sub 2}O content. High transparency was kept for these glass ceramic samples, and intense upconversion, near- and mid-infrared emissions were obtained in Er{sup 3+}-doped glass ceramics with an increase of red/green ratio and prominent Stark splits in the sample with high Na{sub 2}O content, indicating the change of crystal field around Er{sup 3+} in the host matrix. Our results indicate that the crystallization and luminescence properties of glass ceramics could be modified through adjusting the glass composition, and it is an effective route to develop glass ceramics with favorable properties.

36 MATERIALS SCIENCE↗

X-Ray Sources and High-Throughput Data Collection Methods

X-ray diffraction experiments on protein crystals are at the core of the structure determination process. An overview of X-ray sources and data collection methods to support structure-based drug design (SBDD) efforts is presented in this chapter. First, methods of generating and manipulating X-rays for the purpose of protein crystallography, as well as the components of the diffraction experiment setup are discussed. SBDD requires the determination of numerous protein-ligand complex structures in a timely manner, and the second part of this chapter describes how to perform diffraction experiments efficiently on a large number of crystals, including crystal screening and data collection.

59 BASIC BIOLOGICAL SCIENCES↗

Stability of Y-Ba-Cu-oxide phases in salt flux

The results of an investigation into the possibility of growing YBa2Cu3O7 (or Y123) single crystals from a NaCl-KCl flux (salt flux) are presented. They are compared with results for Y123 crystals grown from a Ba-Cu-oxide flux system. The chosen salt flux composition was 1:1 (NaCl:KCl). The preparation method of the solutes is presented, with particular attention given to the compounds surrounding the Y123 phase, such as Y2BaCuO6 (Y211). Optical microscopy was introduced to study the morphology of the sample; X-ray diffraction was used for phase identification; and a chemical analysis was effected. The Y123, Y211, and BaCuO2 phases were shown to be dissociated in the NaCl-KCl flux, and could not be recrystallized. A small amount of the flux could be added to create large-grain Y123 crystals, but single-crystal growth was not possible in a top-seeded NaCl-KCl solution. This is attributed to significant differences in solubility of the crystal elements, and phase separation caused by CuO crystal formation.

Tao, Y. K.↗

The Mu2e crystal calorimeter

The Mu2e experiment at Fermilab will search for the charged-lepton flavour violating conversion of negative muons into electrons in the coulomb field of an Al nucleus, planning to reach a single event sensitivity of about $3\cdot10^{−17}$, four orders of magnitude beyond the current best limit.The conversion electron has a clear monoenergetic signature at 104.967 MeV, slightly below the muon rest mass, and will be identified by a complementary measurement carried out by a high-resolution tracker and an electromagnetic calorimeter (EMC). The calorimeter is composed of 1348 pure CsI crystals, each read by two custom UV-extended SiPMs, that are arranged in two annular disks. The EMC should achieve better than 10% energy resolution and 500 ps timing resolution for 100 MeV electrons and maintain extremely high levels of reliability and stability and in a harsh operating environment with high vacuum, 1 T B-field and radiation exposures up to 100 krad and $10^{12} \rm{n}_\rm{1MeVeq}/\rm{cm}^{2}$.The calorimeter technological choice, along with the design of the custom front-end electronics, cooling and mechanical systems were validated through an electron beam test on a large-scale 51-crystals prototype (Module-0) and extensive test campaigns that characterised and verified the performance of crystals, photodetectors, analogue and digital electronics. This included hardware stress tests and irradiation campaigns with neutrons, protons, and photons.The production and QC phases of all calorimeter components is completed apart for the digital electronics that has been revised for improving its resilience to SEU and SEL. A series of vertical slice tests with the final electronics is being carried out on the Module-0 at LNF along with the implementation and validation of the calibration procedures. The first disk has been assembled in 2022 while the second disk is under assembly at the moment of writing. Status of construction will be summarised, along with plans for commissioning and first calibration of the fully assembled disks.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

A Catastrophic Charge Density Wave in BaFe 2 Al 9

Charge density waves (CDWs) are modulations of the electron density and the atomic lattice that develop in some crystalline materials at low temperatures. We report an unusual example of a CDW in BaFe 2 Al 9 below 100 K. In contrast to the canonical CDW phase transition, temperature-dependent physical properties of single crystals reveal a first-order phase transition. This is accompanied by a discontinuous change in the size of the crystal lattice. In fact, this large strain has catastrophic consequences for the crystals causing them to physically shatter. Single-crystal X-ray diffraction reveals superlattice peaks in the low-temperature phase signaling the development of a CDW lattice modulation. No similar low-temperature transitions are observed in BaFe 2 Al 9 . Electronic structure calculations provide one hint to the different behavior of these two compounds; the d-orbital states in the Fe compound are not completely filled. Iron compounds are renowned for their magnetism, and partly filled d-states play a key role. Finally, it is therefore surprising that BaFe 2 Al 9 develops a structural modulation at low temperature instead of magnetic order.

36 MATERIALS SCIENCE↗

Evaluation of GOES encoder lamps

Aging characteristics and life expectancies of flight quality, tungsten filament, encoder lamps are similar to those of 'commercial' grade gas filled lamps of similar construction, filament material and filament temperature. The aging and final failure by filament burnout are caused by single crystal growth over large portions of the filament with the concomitant development of facets and notches resulting in reduction of cross section and mechanical weakening of the filament. The life expectancy of presently produced lamps is about one year at their nominal operating voltage of five volts dc. At 4.5 volts, it is about two years. These life times are considerably shorter, and the degradation rates of lamp current and light flux are considerably higher, than were observed in the laboratory and in orbit on lamps of the same type manufactured more than a decade ago. It is speculated that the filaments of these earlier lamps contained a crystallization retarding dopant, possibly thorium oxide. To obtain the desired life expectancy of or = to four years in present lamps, operating voltages of or = to four volts dc would be required.

Viehmann, W.↗

Materials Chemistry Issues in the Development of a Single-Crystal Solar/Thermal Refractive Secondary Concentrator

A translucent crystal concentrates and transmits energy to a heat exchanger, which in turn heats a propellant gas, working gas of a dynamic power system, or a thermopile. Materials are the limiting issue in such a system. Central is the durability of the crystal, which must maintain the required chemical, physical/optical, and mechanical properties as it is heated and cooled. This report summarizes available data to date on the materials issues with this system. We focus on the current leading candidate materials, which are sapphire (Al2O3) for higher temperatures and silica (SiO2) for lower temperatures. We use data from thermochemical calculations; laboratory coupon tests with silica and sapphire; and system tests with sapphire. The required chemical properties include low-vapor pressure and interfacial stability with supporting structural materials. Optical properties such as transmittance and index of refraction must be maintained. Thermomechanical stability is a major challenge for a large, single-crystal ceramic and has been discussed in another report. In addition to the crystal, other materials in the proposed system include refractory metals (Nb, Ta, Mo, W, and Re), carbon (C), and high-temperature ceramic insulation. The major issue here is low levels of oxygen, which lead to volatile refractory metal oxides and rapid consumption of the refractory metal. Interfacial reactions between the ceramic crystal and refractory metal are also discussed. Finally, high-temperature ceramic insulating materials are also likely to be used in this system. Outgassing is a major issue for these materials. The products of outgassing are typically reactive with the refractory metals and must be minimized.

Jacobson, Nathan S.↗

Intrinsic surface passivation of CdTe

Recombination is critically limiting in CdTe devices such as solar cells and detectors, with much of it occurring at or near the surface. In this work, we explore different routes to passivate p-type CdTe surfaces without any intentional extrinsic passivation layers. To provide deeper insight into the passivation routes, we uniquely correlate a set of characterization methods: surface analysis and time-resolved spectroscopy. We study two model systems: nominally undoped single crystals and large-grain polycrystalline films. We examine several strategies to reduce surface recombination velocity. First, we study the effects of removing surface contaminants while maintaining a near-stoichiometric surface. Then we examine stoichiometric thermally reconstructed surfaces. Here, we also investigate the effects of shifting the surface stoichiometry by both “subtractive” (wet chemical etches) and “additive” (ampoule anneals and epitaxial growth) means. We consistently find for a variety of methods that a highly ordered stoichiometric to Cd-rich surface shows a significant reduction in surface recombination, whereas a Te-rich surface has high recombination and propose a mechanism to explain this. While as-received single crystals and as-deposited polycrystalline films have surface recombination velocities in the range of 10 5 –10 6 cm/s, we find that several routes can reduce surface recombination velocities to <2.5 × 10 4 cm/s.

14 SOLAR ENERGY↗

Designing functionality in perovskite thin films using ion implantation techniques: Assessment and insights from first-principles calculations

Ion implantation has been widely used in the semiconductor industry for decades to selectively control electron/hole doping for device applications. Recently, experimental studies on ion implantation into more structurally and electronically complex materials have been undertaken in which defect generation has been used to control a variety of functional phenomena. Of particular interest, are recent findings demonstrating that low doses of low energy helium ions into single crystal films can be used to tailor the structural properties. These initial experimental studies have shown that crystal symmetry can be continuously controlled by applying increasingly large doses of He ions into a crystal. The observed changes in lattice structure were then observed to correlate with functional changes, such as metal-insulator transition temperature2 and optical bandgap3. In these preliminary experimental studies, changes to lattice expansion was proposed to be the direct result of chemical pressure originating predominantly from the implanted He applying chemical pressure at interstitial sites. However, the influence of possible secondary knock-on damage arising from the He atoms transferring energy to the lattice through nuclear-nuclear collision with the crystal lattice remains largely unaddressed. In this work, we focus on a SrRuO3 model system to provide a comprehensive examination of the impact of common defects on structural and electronic properties, obtain calculated defect formation energies, and define defect migration barriers. Our model indicates that, while interstitial He can modify the crystal properties, a dose significantly larger than those reported in experimental studies would be required. The true origin of the observed structural changes is likely the result of a combination of secondary defects created during He implantation. Of particular importance, we observe that different defect types can generate greatly varied local electronic structures and that the formation energies and migration energy barriers vary by defect type. Thus, we may have identified a new method of selectively inducing controlled defect complexes into single crystal materials. Development of this approach would have a broad impact on both our ability to probe specific defect contributions in fundamental studies and allow a new level of control over functional properties driven by specific defect complexes.

36 MATERIALS SCIENCE↗

Understanding the Crystallographic Phase Relations in Alkali-Trihalogeno-Germanates in Terms of Ferroelectric or Antiferroelectric Arrangements of the Tetrahedral GeX 3 Units

The alkali-trihalogeno-germanates AGeX 3 with A: Rb or Cs and X a halogen (I, Br, Cl) along with the corresponding stannates (ASnX 3 ) and plumbates (APbX 3 ) reflect a large variety of crystal structures, some of which are of the perovskite type. These materials, better known as “halide perovskites” have recently gained worldwide attention as promising photovoltaic and more broadly opto-electronic materials. Yet, their stability problems relative to the non-perovskite phases are a major issue. It is shown that some of the phase relations in these materials can be understood in terms of the relative orientation of the GeX 3 tetrahedral units, which is ferroelectric (FE) in the perovskite phase but antiferroelectric (AFE) in the competing monoclinic phase. Electrostatic dipole interactions favor the AFE phase and the additional bond formation favors the FE phase. The change in phase is accompanied by a large change in band gap.

36 MATERIALS SCIENCE↗

Ultralow Thermal Conductivity and High-Temperature Thermoelectric Performance in n-Type K 2.5 Bi 8.5 Se 14

We studied the narrow band-gap (0.55 eV) semiconductor K 2.5 Bi 8.5 Se 14 as a potential thermoelectric material for power generation. Samples of polycrystalline K 2.5 Bi 8.5 Se 14 prepared by spark plasma sintering exhibit exceptionally low lattice thermal conductivities (κ lat ) of 0.57-0.33 W m -1 K -1 in the temperature range of 300-873 K. The physical origin of such low κ lat in K 2.5 Bi 8.5 Se 14 is related to the strong anharmonicity and low phonon velocity caused by its complex low symmetry, large unit cell crystal structure, and mixed occupancy of Bi and K atoms in the lattice. High-resolution scanning transmission electron microscopy studies and microanalysis indicate that the K 2.5 Bi 8.5 Se 14 sample is a single phase without intergrowth of the structurally related K 2 Bi 8 Se 13 phase. The undoped material exhibits an n-type character and a figure-of-merit (ZT) value of 0.67 at 873 K. Electronic band structure calculations indicate that K 2.5 Bi 8.5 Se 14 is an indirect band-gap semiconductor with multiple conduction bands close to the Fermi level. Phonon dispersion calculations suggest that K 2.5 Bi 8.5 Se 14 has low phonon velocities and large Grüneisen parameters that can account for the observed ultralow κ lat . The degree of n-type doping can be controlled by introducing Se deficiencies in the structure, providing a simple route to increase the ZT to ~1 at 873 K.

36 MATERIALS SCIENCE↗