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At least 73 records · Page 4

Ground-based research of crystal growth of II-VI compound semiconductors by physical vapor transport

Ground-based investigation of the crystal growth of II-VI semiconductor compounds, including CdTe, CdS, ZnTe, and ZnSe, by physical vapor transport in closed ampoules was performed. The crystal growth experimental process and supporting activities--preparation and heat treatment of starting materials, vapor partial pressure measurements, and transport rate measurements are reported. The results of crystal characterization, including microscopy, microstructure, optical transmission photoluminescence, synchrotron radiation topography, and chemical analysis by spark source mass spectrography, are also discussed.

Volz, M. P.↗

Vapor Growth of ZnSe-based Compound Semiconductors in Low Gravity environment on International Space Station

Six low-gravity experiments of crystal growth of ZnSe-based compound semiconductors by physical vapor transport (PVT) are scheduled to be processed inside Low Gradient Furnace (LGF) on Materials Science Research Rack (MSRR) in Material Science Laboratory (MSL) on International Space Station (ISS) starting from February 27th, 2023. The flight samples consist of three unseeded growths of ZnSe, Cr-doped ZnSe and ZnSeTe as well as growth of ZnSe on top of three single crystal ZnSe seeds with orientation of (100), (110) and (111). The main scientific objective of the flight experiments is to establish the effects of gravity-driven fluid flows on Earth to (i) the non-uniform incorporation of impurities and defects and (ii) the deviation from stoichiometry observed in the grown crystals caused by growth interface fluctuations and evolution as the results of buoyancy-driven convection and irregular fluid-flows. The investigation will also evaluate the effects of gravity on the PVT process by examining (i) the growth kinetics on various seed orientations, (ii) the dopant segregation and distribution in the Cr doped ZnSe, and (iii) the compositional segregation and distribution in the ternary ZnSeTe crystal grown by PVT. Additionally, from X-ray diffraction/topography and by measuring the density and distribution of various crystalline defects it will assess the self-induced strain effects developed during processing at elevated temperatures caused by the weight of the crystals. During the ground-based preparations, the following tasks have been accomplished: • Establish the thermodynamic properties of the ZnSe binary and related ternary systems by measuring the partial pressures of the vapor phase coexisting with the condensed phases and perform phase diagram calculations for comparison. • Evaluate the effects of gravity-driven convection in the growth process by performing experiments under various vapor transport orientations relative to gravity vector, i.e., horizontal, vertically stabilized and destabilized configurations. • Establish a quantitative correlation between growth parameters and the characteristics and properties of the grown crystals by characterizing the crystals using a variety of techniques. • Evaluate the fundamentals of the current theories on vapor transport and crystal growth kinetics by performing in-situ and real-time monitoring techniques during growth. • Develop a one-dimensional diffusion limited theory of mass transport and two- and three-dimensional numerical simulations of both mass transport and heat transfer and thus establish the microgravity requirements for the flight experiments and to predict the characteristics of the grown crystals such as the solid-vapor interface shapes… etc. and establish a fundamental understanding of the crystal growth process from the comparison with experimental results.

ZnSe↗

Characterization of Scintillating Crystal for High Energy Radiation Detection and Applications

Cesium Hafnium Chloride (Cs2Hfl6) is a promising metal halide scintillating detector due to its excellent characteristics such as non-hygroscopicity, high light yield without doping. Scintillators plays an important role in nuclear security applications as detectors at border monitoring stations. We grew and characterized CHC crystals to be fabricated for gamma detection. Photoluminescence was performed using the Duetta Fluorescence and Absorbance Spectrometer. The energy response to Cs-137 and Co-60 reference sources was recorded for a representative sodium iodide (NaI) scintillating detector.

Reeder, Angel↗

Instrument for in situ hard x-ray nanobeam characterization during epitaxial crystallization and materials transformations

Solid-phase epitaxy (SPE) and other three-dimensional epitaxial crystallization processes pose challenging structural and chemical characterization problems. The concentration of defects, the spatial distribution of elastic strain, and the chemical state of ions each vary with nanoscale characteristic length scales and depend sensitively on the gas environment and elastic boundary conditions during growth. The lateral or three-dimensional propagation of crystalline interfaces in SPE has nanoscale or submicrometer characteristic distances during typical crystallization times. Here, an in situ synchrotron hard x-ray instrument allows these features to be studied during deposition and crystallization using diffraction, resonant scattering, nanobeam and coherent diffraction imaging, and reflectivity. The instrument incorporates a compact deposition system allowing the use of short-working-distance x-ray focusing optics. Layers are deposited using radio-frequency magnetron sputtering and evaporation sources. The deposition system provides control of the gas atmosphere and sample temperature. The sample is positioned using a stable mechanical design to minimize vibration and drift and employs precise translation stages to enable nanobeam experiments. Results of in situ x-ray characterization of the amorphous thin film deposition process for a SrTiO 3 /BaTiO 3 multilayer illustrate implementation of this instrument.

47 OTHER INSTRUMENTATION↗

Crystal Structure and Characterization of Human Heavy-Chain Only Antibodies Reveals a Novel, Stable Dimeric Structure Similar to Monoclonal Antibodies

We report the novel crystal structure and characterization of symmetrical, homodimeric humanized heavy-chain-only antibodies or dimers (HC2s). HC2s were found to be significantly coexpressed and secreted along with mAbs from transient CHO HC/LC cotransfection, resulting in an unacceptable mAb developability attribute. Expression of full-length HC2s in the absence of LC followed by purification resulted in HC2s with high purity and thermal stability similar to conventional mAbs. The V H and C H 1 portion of the heavy chain (or Fd) was also efficiently expressed and yielded a stable, covalent, and reducible dimer (Fd2). Mutagenesis of all heavy chain cysteines involved in disulfide bond formation revealed that Fd2 intermolecular disulfide formation was similar to Fabs and elucidated requirements for Fd2 folding and expression. For one HC2, we solved the crystal structure of the Fd2 domain to 2.9 Å, revealing a highly symmetrical homodimer that is structurally similar to Fabs and is mediated by conserved (C H 1) and variable (V H ) contacts with all CDRs positioned outward for target binding. Interfacial dimer contacts revealed by the crystal structure were mutated for two HC2s and were found to dramatically affect HC2 formation while maintaining mAb bioactivity, offering a potential means to modulate novel HC2 formation through engineering. These findings indicate that human heavy-chain dimers can be secreted efficiently in the absence of light chains, may show good physicochemical properties and stability, are structurally similar to Fabs, offer insights into their mechanism of formation, and may be amenable as a novel therapeutic modality.

60 APPLIED LIFE SCIENCES↗

Growth and characterization of single crystal insulators on silicon

An overview of the growth and characterization of epitaxial insulators on semiconductors is presented. The potential applications include semiconductor-on-insulator structures, three-dimensional and/or high-density integrated circuits, optoelectronic applications such as integrated waveguides and improved gate insulators. The growth and physical characterization of epitaxial fluorides on semiconductors are discussed. Consideration is also given to the epitaxial overgrowth of epitaxial metal layers with CaF2 as well as to the formation of a novel superlattice of Ca particles in epitaxial CaF2.

Schowalter, Leo J.↗

Latent Tracks in Ion-Irradiated LiTaO 3 Crystals: Damage Morphology Characterization and Thermal Spike Analysis

Systematic research on the response of crystal materials to the deposition of irradiation energy to electrons and atomic nuclei has attracted considerable attention since it is fundamental to understanding the behavior of various materials in natural and manmade radiation environments. This work examines and compares track formation in LiTaO3 induced by separate and combined effects of electronic excitation and nuclear collision. Under 0.71–6.17 MeV/u ion irradiation with electronic energy loss ranging from 6.0 to 13.8 keV/nm, the track damage morphologies evolve from discontinuous to continuous cylindrical zone. Based on the irradiation energy deposited via electronic energy loss, the subsequently induced energy exchange and temperature evolution processes in electron and lattice subsystems are calculated through the inelastic thermal spike model, demonstrating the formation of track damage and relevant thresholds of lattice energy and temperature. Combined with a disorder accumulation model, the damage accumulation in LiTaO3 produced by nuclear energy loss is also experimentally determined. The damage characterizations and inelastic thermal spike calculations further demonstrate that compared to damage-free LiTaO3, nuclear-collision-damaged LiTaO3 presents a more intense thermal spike response to electronic energy loss owing to the decrease in thermal conductivity and increase in electron–phonon coupling, which further enhance track damage.

36 MATERIALS SCIENCE↗

Overview of Characterization Techniques for High Speed Crystal Growth

Features of characterization requirements for crystals, devices and completed products are discussed. Key parameters of interest in semiconductor processing are presented. Characterization as it applies to process control, diagnostics and research needs is discussed with appropriate examples.

Ravi, K. V.↗

Characterization of Semi-Insulating CdTe Crystals Grown by Horizontal Seeded Physical Vapor Transport

CdTe crystals were grown by horizontal seeded physical vapor transport technique in uncoated and boron nitride coated fused silica ampoules with the source materials near the congruent sublimation condition. The grown crystals were characterized by current-voltage measurements, low temperature photoluminescence spectroscopy, near IR transmission optical microscopy, spark source mass spectroscopy and chemical etching. The measured resistivities of the crystals were in the high-10(exp 8) ohm-cm range. Although the crystal grown in the boron nitride coating was contaminated with boron from the photoluminescence measurements, the coating yielded a single crystal with no inclusions or precipitates.

Chattopadhyay, K.↗

Single crystal growth and characterization of new Zintl phase Ca 9 Zn 3.1 In 0.9 Sb 9

Complex Zintl phases have yielded a large variety of promising new thermoelectric materials. Here we report the discovery of the new Zintl phase Ca 9 (Zn 1– x In x ) 4 Sb 9 ( x ~ 0.9), needle-like crystals of which were serendipitously obtained from an In- and Sb-rich flux. Although its composition is reminiscent of Ca 9 Zn 4+ x Sb 9 , an excellent thermoelectric material with zT > 1, the substitution of In on the Zn site leads to the formation of an entirely new structure type. Single crystal X-ray diffraction revealed a structure characterized by T Sb 4 tetrahedra ( T = statistically disordered Zn and In atoms) and ZnSb 3 triangular units, which share common corners to form [ T 4 Sb 9 ] 18– polyanions. The average structure was found to have hexagonal symmetry. The valence electron count in this heavily-disordered structure appears to follows the Zintl-Klemm rules, suggesting semiconducting behavior. Single crystal electrical conductivity and Seebeck coefficient measurements support this conclusion, suggesting that the as-grown crystals are degenerate p -type semiconductors.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Crystal Growth and Characterization of Bil3

Bismuth tri-iodide (BiI3) have been grown by physical vapor transport (PVT), and by the Bridgman (melt) method. These crystals along with pure and stoichiometric BiI3 powder have been investigated by differential scanning calorimetry (DSC). The DSC results show that pure BiI3 powder has no phase transition and melts around 408 C. While we found no evidence for the high temperature dissociation of BiI3, the DSC measurements show that crystals grown from melt method contain a significantly large amount of Bi-rich phases than crystals grown from PVT method, as indicated by phase transition detected at 270, 285, 298 and 336 C.

Hayes, Julia↗

Developing techniques for crystal growth synthesis and characterization of rare earth-silicon-germanium magnetoresponsive alloys

In this study, a crystal growth technique was developed for the family of intermetallic, magnetoresponsive RE 5 (Si 1-x Ge x ) 4 alloys in order to access the intrinsic and anisotropic properties. Initial bulk properties measured on polycrystalline samples alluded to the properties being obscured or averaged and high-quality, well-characterized, single crystals would clarify this. Successful crystal growth led to development of oriented sample preparation techniques specific for the crystal structures (monoclinic and orthorhombic) and mechanical properties (hard and brittle) of these alloys, and customized for the various measurement techniques undertaken. Here we describe our journey, sometimes circuitous, from crystal growth to sample preparation and cite the scientific discoveries that came about as a result.

36 MATERIALS SCIENCE↗

Multiparameter laser performance characterization of liquid crystals for polarization control devices in the nanosecond regime

Abstract Interactions of liquid crystals (LC’s) with polarized light have been studied widely and have spawned numerous device applications, including the fabrication of optical elements for high-power and large-aperture laser systems. Currently, little is known about both the effect of incident polarization state on laser-induced–damage threshold (LIDT) and laser-induced functional threshold (LIFT) behavior at sub-LIDT fluences under multipulse irradiation conditions. This work reports on the first study of the nanosecond-pulsed LIDT’s dependence on incident polarization for several optical devices employing oriented nematic and chiral-nematic LC’s oriented by surface alignment layers. Accelerated lifetime testing was also performed to characterize the ability of these devices to maintain their functional performance under multipulse irradiation as a function of the laser fluence at both 1053 nm and 351 nm. Results show that the LIDT varies as a function of input polarization by 30–80% within the same device, while the multipulse LIFT (which can differ from the nominal LIDT) depends on irradiation conditions such as laser fluence and wavelength.

47 OTHER INSTRUMENTATION↗

Crystal Growth and Characterization of Europium-Doped Rubidium Calcium Bromide Scintillators

National security strategies like gamma spectroscopy and high-energy X-ray radiography are limited, in part, by the scintillator used, prompting research into novel materials with improved properties. In this paper, Eu 2+ activated rubidium calcium bromide scintillators were grown via the vertical Bridgman method with a range of dopant concentrations. Light yield, energy resolution, and the afterglow of Rb 4 CaBr 6 :Eu and RbCaBr 3 :Eu improved with increasing Eu 2+ concentration, and scintillation decay time increased. The highest light yields of Rb 4 CaBr 6 :Eu and RbCaBr 3 :Eu were 71000 and 45000 ph/MeV, respectively.

36 MATERIALS SCIENCE↗

Formation of U(VI) peroxide nanoclusters from cascade reactions with a persulfate radical initiator

Radiolysis of water in high radiation fields generates a variety of reactive oxygen species that influence the chemical behavior and complexation of hexavalent uranium. This study investigates the behavior of interaction of a uranyl cation (UO 2 2+ (VI)) with a series of free radicals that are formed in situ via activation of the free radical initiator persulphate (S 2 O 8 2− ), which releases both SO 4 ˙ − and ˙OH species in the solution. Electron Paramagnetic Resonance (EPR) and Raman spectroscopy were used to evaluate the presence of the hydroperoxyl radical (HO 2 ˙) and superoxide radicals (O 2 ˙ − ) that are formed within the solution through radical cascade reactions. In addition, a uranyl peroxide cluster solid (NaU 24 ) was crystallized and characterized using single crystal X-ray diffraction (SCXRD), vibrational spectroscopy, and EPR spectroscopy. The presence of the hydroperoxyl radical (HO 2 ˙) and superoxide radicals (O 2 ˙ − ) was also observed in the solid-state compound, but spectroscopic evidence suggests that it was associated with the Na + network and not the cluster itself. Density functional theory (DFT) calculations were also utilized to further confirm the radical species produced and determine the potential stabilization of radicals detected within the cluster and lattice.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗