Engineering Papers⌕ Search

SEARCH · Engineering Papers

Results for “Large Crystal”

Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 145 records · Page 8

The effect of rare-earth substitution on the Debye temperature of inorganic phosphors

In the quest to predict photoluminescent efficiency in rare-earth substituted inorganic phosphors, research has shown that materials consisting of ordered, rigid crystal structures tend to possess the highest photoluminescent quantum yields. A compound's Debye temperature (Θ D ), which can be calculated using ab initio calculations, is an ideal proxy for quantitatively comparing structural rigidity among different inorganic compounds, allowing potentially efficient phosphors to be selected from large crystal structure databases. However, the high computational cost of these calculations limits estimating Θ D for unsubstituted host crystal structures only. It is assumed that the low substitution concentration of the rare-earth luminescent center does not significantly influence a material's Debye temperature. This work evaluates the validity of this approximation by examining the effect of luminescent center substitution on a host structure's Θ D . Two well-known phosphors, (Y 1– x Ce x ) 3 Al 5 O 12 ( x = 0 – 0.05) and Ba 1-δ Eu δ MgAl 10 O 17 (δ = 0 – 0.15), were synthesized with varying rare-earth concentrations, while Θ D was computationally estimated and then determined by ultrasonic pulse-echo speed-of-sound and low-temperature heat capacity measurements. Overall, the ensuing results provide key implications for using Θ D as a proxy for structural rigidity in substituted inorganic compounds.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

The effect of annealing on optical transmittance and structure of ZLANI fluorozirconate glass thin films

In this work, we report the effect of thermal annealing on structure, composition, optical transmittance and thickness of a novel fluorozirconate glass (ZLANI) containing Zr, La, Al, Na and In fluorides. In this work, pulsed laser depo- sition was used to grow thin films of ZLANI, and thermal annealing at different temperatures was performed on the films. Annealing did not change the composition, but a clear structural evolution of the ZLANI glass was observed by transmission electron microscopy (TEM), showing that we can control microstructure independent of composition. An increase in transmittance after the film was subject to a 100 °C thermal anneal was ascribed to the removal of defects and structural relaxation in the amorphous state. Following an anneal of 200 °C, the transmittance decreases due to heterogeneous formation of crystalline nuclei and changes in the local bonding. After the final annealing at 300 °C, a wider-scale crystallization occurred, with some major crystal phases formed as Zr 2 F 8 (H 2 O) 6 and ZrO 2 , which alters the shape of the transmittance curve. The crystalline content of the crystal phases that form in the annealed films was quantified using hollow cone dark field TEM imaging. The 100 °C or 200 °C annealing decreases the film thickness by inducing structural relaxation and densification of the amorphous films, while the thickness increase of the 300 °C annealed film resulted from the formed large crystals. These results provide insights for the design of multilayer nanocomposites with a ZLANI glass matrix, which have potential applications as up-/down-conversion luminescent materials and X-ray storage phosphors.

36 MATERIALS SCIENCE↗

Advances in the electron diffraction characterization of atomic clusters and nanoparticles

Nanoparticles and metallic clusters continue to make a remarkable impact on novel and emerging technologies. In recent years, there have been impressive advances in the controlled synthesis of clusters and their advanced characterization. One of the most common ways to determine the structures of nanoparticles and clusters is by means of X-ray diffraction methods. However, this requires the clusters to crystallize in a similar way to those used in protein studies, which is not possible in many cases. Novel methods based on electron diffraction have been used to efficiently study individual nanoparticles and clusters and these can overcome the obstacles commonly encountered during X-ray diffraction methods without the need for large crystals. These novel methodologies have improved with advances in electron microscopy instrumentation and electron detection. Here, we review advanced methodologies for characterizing metallic nanoparticles and clusters using a variety of electron diffraction procedures. These include selected area electron diffraction, nanobeam diffraction, coherent electron diffraction, precession electron diffraction, scanning transmission electron microcopy diffraction, and high throughput data analytics, which leverage deep learning to reduce the propensity for data errors and translate nanometer and atomic scale measurements into material data.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Design and expected performance of a variable-radii sinusoidal spiral x-ray spectrometer for the National Ignition Facility

A novel high-resolution x-ray spectrometer for point-like emission sources has been developed using a crystal shape having both a variable major and a variable minor radius of curvature. This variable-radii sinusoidal spiral spectrometer (VR-Spiral) allows three common spectrometer design goals to be achieved simultaneously: 1. reduction of aberrations and improved spectral (energy) resolution, 2. reduction of source size broadening, and 3. use of large crystals to improve total throughput. The VR-Spiral concept and its application to practical spectrometer design are described in detail. This concept is then used to design a spectrometer for an extreme extended x-ray absorption fine structure experiment at the National Ignition Facility looking at the Pb L 3 absorption edge at 13.0352 keV. The expected performance of this VR-Spiral spectrometer, both in terms of energy resolution and spatial resolution, is evaluated through the use of a newly developed raytracing tool, xicsrt. Finally, the expected performance of the VR-Spiral concept is compared to that of spectrometers based on conventional toroidal and variable-radii toroidal crystal geometries showing a greatly improved energy resolution.

47 OTHER INSTRUMENTATION↗

Process for Encapsulating Protein Crystals

A process for growing protein crystals encapsulated within membranes has been invented. This process begins with the encapsulation of a nearly saturated aqueous protein solution inside semipermeable membranes to form microcapsules. The encapsulation is effected by use of special formulations of a dissolved protein and a surfactant in an aqueous first liquid phase, which is placed into contact with a second, immiscible liquid phase that contains one or more polymers that are insoluble in the first phase. The second phase becomes formed into the semipermeable membranes that surround microglobules of the first phase, thereby forming the microcapsules. Once formed, the microcapsules are then dehydrated osmotically by exposure to a concentrated salt or polymer solution. The dehydration forms supersaturated solutions inside the microcapsules, thereby enabling nucleation and growth of protein crystals inside the microcapsules. By suitable formulation of the polymer or salt solution and of other physical and chemical parameters, one can control the rate of transport of water out of the microcapsules through the membranes and thereby create physicochemical conditions that favor the growth, within each microcapsule, of one or a few large crystals suitable for analysis by x-ray diffraction. The membrane polymer can be formulated to consist of low-molecular-weight molecules that do not interfere with the x-ray diffraction analysis of the encapsulated crystals. During dehydration, an electrostatic field can be applied to exert additional control over the rate of dehydration. This protein-crystal-encapsulation process is expected to constitute the basis of protein-growth experiments to be performed on the space shuttle and the International Space Station. As envisioned, the experiments would involve the exposure of immiscible liquids to each other in sequences of steps under microgravitational conditions. The experiments are expected to contribute to knowledge of the precise conditions under which protein crystals form. By enhancing the ability to grow crystals suitable for x-ray diffraction analysis, this knowledge can be expected to benefit not only the space program but also medicine and the pharmaceutical industry.

Morrison, Dennis R.↗

Cryotrapping peroxide in the active site of human mitochondrial manganese superoxide dismutase crystals for neutron diffraction

Structurally identifying the enzymatic intermediates of redox proteins has been elusive due to difficulty in resolving the H atoms involved in catalysis and the susceptibility of ligand complexes to photoreduction from X-rays. Cryotrapping ligands for neutron protein crystallography combines two powerful tools that offer the advantage of directly identifying hydrogen positions in redox-enzyme intermediates without radiolytic perturbation of metal-containing active sites. However, translating cryogenic techniques from X-ray to neutron crystallography is not straightforward due to the large crystal volumes and long data-collection times. Here, methods have been developed to visualize the evasive peroxo complex of manganese superoxide dismutase (MnSOD) so that all atoms, including H atoms, could be visualized. The subsequent cryocooling and ligand-trapping methods resulted in neutron data collection to 2.30 Å resolution. The P 6 1 22 crystal form of MnSOD is challenging because it has some of the largest unit-cell dimensions ( a = b = 77.8, c = 236.8 Å) ever studied using high-resolution cryo-neutron crystallography. The resulting neutron diffraction data permitted the visualization of a dioxygen species bound to the MnSOD active-site metal that was indicative of successful cryotrapping.

59 BASIC BIOLOGICAL SCIENCES↗

Improved liquid lithium surfaces in the Lithium Tokamak Experiment-β

Advances in vacuum, surface, and lithium conditioning techniques throughout five years of continuous operations in LTX-β have produced mirror-like liquid lithium surfaces and demonstrated the feasibility of high-performance tokamak discharges fully surrounded by liquid metal without significant operational problems. Improvements in conditioning techniques and procedures, including many weeks of baking and accumulation of 70 g of Li, led to reduced residual gasses and clean Li surfaces - all while still maintaining enough operational flexibility for multiple in-vacuum diagnostic upgrades and calibrations. Coatings had a visibly clean appearance, with reflective liquid metal demonstrating good wetting and surface adhesion with films that were now macroscopically thick. Solidified Li showed large crystal grains, while surface science measurements observed reduced impurities in the lithium. Steadily improved plasma performance was achieved with liquid lithium, with discharges able to match solid Li in terms of evolution of I p and n e , including rapid density pumping indicating low recycling. There were indications of moderately increased Li impurity influx, though few significant disturbances by the large liquid surfaces on tokamak operations over hundreds of discharges. Liquid metal plasma facing components are a potential solution to the extreme heat and particle fluxes that could cause unacceptable damage to solid materials, while liquid lithium also has the potential for greatly increased confinement in the low-recycling regime. While many liquid metal approaches are possible, and numerous experiments have been conducted in test stands and small modules in fusion devices, LTX-β is the only tokamak operated while fully surrounded by liquid metal.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Realization of flat bands by lattice intercalation in kagome metals

Recently there has been intense interest in kagome metals, which are expected to host flat bands (FBs). However, the observed “FBs” are not flat over the whole two-dimensional Brillouin zone and overlap strongly with other bands. In fact, the FB does not truly exist in a default d-orbital kagome lattice, and the conditions for its existence in kagome metals are unknown. Here, based on tight-binding model analyses of the interplay between orbital and lattice symmetry, we establish such conditions. Additionally, we show that for a single d-orbital kagome lattice assuming large crystal field splitting (CFS), only the d z 2 orbital gives rise to a FB, while d xy , d x 2 -y 2 , d x⁢z , and d yz orbitals can only produce a FB with a rotated d-orbital basis so that they conform with the underlying kagome lattice symmetry. Most importantly, we demonstrate that both conditions of d-orbital rotation and large CFS can be ideally satisfied by intercalating the kagome lattice with a hexagonal sublattice without disrupting the destructive interference of FB wave function. Furthermore, we propose layered metalorganic frameworks as promising candidate kagome metals to realize FBs.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Single crystal synthesis and magnetism of the Ba Ln 2 O 4 family ( Ln = lanthanide)

The series of compounds in the Ba Ln 2 O 4 family (Ln = La–Lu, Y) has been synthesized for the first time in single crystalline form, using a molten metal flux. The series crystallizes in the CaV 2 O 4 structure type with primitive orthorhombic symmetry (space group Pnma , #62), and a complete structural study of atomic positions, bonds, angles, and distortions across the lanthanide series is presented. With the exception of the Y, La, Eu, and Lu members, magnetic susceptibility measurements were performed between 2 K and 300 K. BaCe 2 O 4 and BaYb 2 O 4 display large crystal fields effects and suppression of magnetic ordering. As a result, all compounds show signs of magnetic frustration due to the trigonal arrangements of the trivalent lanthanide cations in the structure.

36 MATERIALS SCIENCE↗

Unexpected Hydride: Ce 4 B 2 C 2 H 2.42 , a Stuffed Variant of the Nd 2 BC Structure Type

Ce 4 B 2 C 2 H 2.42 was grown as large crystals from a cerium/copper eutectic flux. The structure was characterized by single-crystal X-ray and neutron diffraction and was found to be a stuffed variant of Nd 2 BC with the addition of two interstitial hydrogen positions. The tetrahedral hydrogen position is fully occupied, while the octahedral position has an occupancy of 42(3)%. Initial synthesis was due to hydrogen contamination of the cerium metal but has been successfully repeated using anthracene as a carbon and hydrogen source. Density of states calculations suggest that the incorporation of hydrogen stabilizes the compound with respect to the nonhydrided model. Magnetic susceptibility data show a complex magnetic ordering at 7.7 K that originates from the localized electron on the Ce 3+ in the structure. The trivalent state is also supported by X-ray photoelectron spectroscopy measurements. Heat capacity and electrical resistivity data show that the phase transition is broad in temperature, which may be due to structural disorder. Furthermore, the large low temperature value of C/T also indicates possible heavy fermion behavior.

36 MATERIALS SCIENCE↗

Nucleation and Growth of PbBrF Crystals at the Liquid Mercury–Electrolyte Interface Studied by Operando X-ray Scattering

In this work, detailed in operando studies of electrochemically induced PbBrF deposition at the liquid mercury/liquid electrolyte interface are presented. The nucleation and growth were monitored using time-resolved X-ray diffraction and reflectivity combined with electrochemical measurements, revealing a complex potential-dependent behavior. PbBrF deposition commences at potentials above –0.7 V with the rapid formation of an ultrathin adlayer of one unit cell thickness, on top of which (001)-oriented three-dimensional crystallites are formed. Two potential regimes are identified. At low overpotentials, slow growth of a low surface density film of large crystals is observed. At high overpotentials, crossover to a potential-independent morphology occurs, consisting of a compact PbBrF deposit with a saturation thickness of 25 nm, which forms within a few minutes. This potential behavior can be rationalized by the increasing supersaturation near the interface, caused by the potential-dependent Pb2+ deamalgamation, which changes from a slow reaction-controlled process to a fast transport-controlled process in this range of overpotentials. In addition, growth on the liquid substrate is found to involve complex micromechanical effects, such as crystal reorientation and film breakup during dissolution.

36 MATERIALS SCIENCE↗

Vapor transport and crystal growth of GeSe under normal and high acceleration

Physical vapor transport experiments on GeSe in the presence of 2 atm xenon and for a nominal temperature difference of 600-500 C were performed under 1 g, 5 g, and 10 g acceleration conditions. Under high acceleration and destabilizing conditions, the GeSe crystals are generally larger than those under 1 g, stabilizing, and up to three orders of magnitude larger in surface area than those under 1 g, destabilizing conditions. The mass transport rates of the 5 g and 10 g destabilizing experiments are considerably greater than those of the 10 g, stabilizing, and 1 g experiments. The observed increase in mass flux (under destabilizing conditions) with acceleration is significantly greater than the anticipated dependence (mass flux proportional to g exp 1/4) for laminar, boundary-layer driven free convection. In view of the considerable convection under high acceleration, destabilizing conditions, the surface morphology and bulk crystallinity of the large crystal platelets are unexpectedly good.

Wiedemeier, H.↗

Detecting Thin Cirrus in Multiangle Imaging Spectroradiometer Aerosol Retrievals

Thin cirrus clouds (optical depth (OD) < 03) are often undetected by standard cloud masking in satellite aerosol retrieval algorithms. However, the Mu]tiangle Imaging Spectroradiometer (MISR) aerosol retrieval has the potential to discriminate between the scattering phase functions of cirrus and aerosols, thus separating these components. Theoretical tests show that MISR is sensitive to cirrus OD within Max{0.05 1 20%l, similar to MISR's sensitivity to aerosol OD, and MISR can distinguish between small and large crystals, even at low latitudes, where the range of scattering angles observed by MISR is smallest. Including just two cirrus components in the aerosol retrieval algorithm would capture typical MISR sensitivity to the natural range of cinus properties; in situations where cirrus is present but the retrieval comparison space lacks these components, the retrieval tends to underestimate OD. Generally, MISR can also distinguish between cirrus and common aerosol types when the proper cirrus and aerosol optical models are included in the retrieval comparison space and total column OD is >-0.2. However, in some cases, especially at low latitudes, cirrus can be mistaken for some combinations of dust and large nonabsorbing spherical aerosols, raising a caution about retrievals in dusty marine regions when cirrus is present. Comparisons of MISR with lidar and Aerosol Robotic Network show good agreement in a majority of the cases, but situations where cirrus clouds have optical depths >0.15 and are horizontally inhomogeneous on spatial scales shorter than 50 km pose difficulties for cirrus retrieval using the MISR standard aerosol algorithm..

Pierce, Jeffrey R.↗

Revisiting two thiophosphate compounds constituting d 0 transition metal HfP 2 S 6 and d 10 transition metal α-Ag 4 P 2 S 6 as multifunctional materials for combining second harmonic generation response and photocurrent response

Two acentric thiophosphate compounds, HfP 2 S 6 and α-Ag 4 P 2 S 6 , are revisited and studied as infrared nonlinear optical materials. HfP 2 S 6 and α-Ag 4 P 2 S 6 were structurally characterized without any property measurements. Here, in this work, HfP 2 S 6 and α-Ag 4 P 2 S 6 were synthesized via high temperature salt flux reactions. Low-temperature polymorph acentric α-Ag 4 P 2 S 6 was purified and grown as mm-sized crystals with the aid of AgBr flux. The AgBr flux was revealed to play an important role in stabilizing the acentric α-Ag 4 P 2 S 6 . The acentric α-Ag 4 P 2 S 6 transforms to centrosymmetric β-Ag 4 P 2 S 6 at 850(5) K, which is revealed by differential scanning calorimetry (DSC) analysis and powder X-ray diffraction experiments. HfP 2 S 6 and α-Ag 4 P 2 S 6 are discovered by UV-vis spectrum measurements as indirect bandgap semiconductors with bandgaps of 2.2(1) eV and 2.5(1) eV, respectively, which is supported by DFT calculations and TB-LMTO-ASA calculations. The bonding pictures of α-Ag 4 P 2 S 6 were studied by crystal orbital Hamilton population calculations (COHP) coupled with electron localization function (ELF) analysis. DFT calculations predict that HfP 2 S 6 and α-Ag 4 P 2 S 6 would exhibit different optical performances regardless of being constructed from identical [P 2 S 6 ] motifs. HfP 2 S 6 exhibits a low second harmonic generation (SHG) response, ~0.21 × AGS (for the sample of particle size of 25 μm). α-Ag 4 P 2 S 6 possesses moderate SHG response, ~0.61 × AGS (for the sample of particle size of 225 μm) coupled with a high laser damage threshold (LDT) of ~3.2 × AGS. Characteristics of high ambient stability, moderate bandgap and SHG response, type-I phase-matching capability, and high LDT together with the easy growth of large crystals make α-Ag 4 P 2 S 6 attractive for future infrared nonlinear optical applications. Photocurrent measurements found that α-Ag 4 P 2 S 6 and β-Ag 4 P 2 S 6 have high photocurrent response, 165 nA cm -2 and 135 nA cm -2 , respectively. α-Ag 4 P 2 S 6 is a new multifunctional material of the ternary Ag–P–S system, which combines nonlinear optical (NLO) properties and photocurrent response.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Synthesis and structural characterization of the new Zintl phases Ba 3 Cd 2 P 4 and Ba 2 Cd 2 P 3 . Rare example of small gap semiconducting behavior with negative thermopower within the range 300 K-700 K

The new Zintl phases Ba 3 Cd 2 P 4 and Ba 2 Cd 2 P 3 have been synthesized using Pb flux, which allowed for the growth of 4-5 mm large crystals. The structures were determined utilizing single-crystal X-ray diffraction methods. Both compounds crystalize in the monoclinic crystal system (space group C2/m (No. 12)) and their structures are closely related. The structure of Ba 3 Cd 2 P 4 can be seen as being comprised of divalent Ba atoms and conjoined CdP 4 tetrahedra in the form of [Cd 2 P 4 ] 6- layers. Within the layers, homoatomic P–P bonds are present, which if cleaved, leave two infinite [CdP 3 ] 7- chains running along the crystallographic b-axis. The other structure, that of Ba 2 Cd 2 P 3 , can be rationalized as also having divalent Ba atoms and conjoined CdP4 tetrahedra in the form of [Cd 2 P 3 ] 6- layers. These layers, again, can be visualized as chains that run down the crystallographic b-axis, which are further connected by P-P dimers. Electronic band structure calculations show that each structure has an optimal number of valence electrons, and therefore conform to the Zintl-Klemm concept. Accordingly, the two compounds can be considered small band gap semiconductors, with band gaps of ca. 0.1 eV and 0.6 eV for Ba3Cd2P4 and Ba 2 Cd 2 P 3 , respectively. Electrical resistivity measurements show that Ba3Cd2P4 displays a large resistivity value at room temperature and an experimental band gap of ca. 0.05 eV, which fits reasonably well with the theoretical predictions. Thermopower measurements show that throughout the temperature range 300 K-700 K, Ba 3 Cd 2 P 4 displays a negative Seebeck coefficient. Here, the extremum value of -84 μV is reached at 630 K, suggestive of an n-type semiconductor, a rarity among Zintl phases.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Low Thermal Gradient Czochralski growth of large CdWO{sub 4} crystals and electronic properties of (010) cleaved surface

The crystal growth of large high-quality inclusion-free CdWO4 crystals, 110 mm in diameter and mass up to 20 kg, has been carried out by the Low Thermal Gradient Czochralski (LTG Cz) technique. The high-purity CdWO{sub 4}(010) surface has been prepared by cleavage and high structural quality of the surface has been verified by RHEED, revealing a system of Kikuchi lines. The chemical state and electronic structure of the surface have been studied using X-ray photoelectron spectroscopy (XPS) and X-ray emission spectroscopy (XES). The total and partial densities of states of the CdWO{sub 4} tungstate were calculated employing the first-principles full potential linearized augmented plane wave (FP-LAPW) method. The results indicate that the principal contributors to the valence band of CdWO{sub 4} are the Cd 4d, W 5d and O 2p states which contribute mainly at the bottom, in the central portion and at the top of the valence band, respectively, with also significant contributions of the mentioned states throughout the whole CdWO{sub 4} valence-band region. With respect to the occupation of the O 2p states, the results of the FP-LAPW calculations are confirmed by comparison on a common energy scale of the XPS valence-band spectrum and the XES band representing the energy distribution of the O 2p states in this compound. Additionally, the FP-LAPW data allow us to conclude that the CdWO{sub 4} tungstate is a non-direct semiconductor. - Highlights: • Large high-quality CdWO{sub 4} crystals, up to 115 mm in diameter and mass up to 20 kg, have been grown. • The high-purity cleaved CdWO{sub 4}(010) surface has been studied by the XPS and XES methods. • The principal contributors to the CdWO{sub 4} valence band are the Cd 4d, W 5d and O 2p states.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Surface Processes of Faceted Growth

Atomic force microscopy and high precision optical interferometry allow to analyze the processes that are in the core of our present understanding of faceted crystal growth. Some of these processes will be reviewed. Recent experiments suggest that the Gibbs-Thomson Law (GTL) may not be applicable to the weakly fluctuating strongly polygonized steps, with low kink density. Propagation rate of a straight short step segment changes with the segment length much steeper than predicted by GTL. If the step fluctuations are still well developed, the typical transition length may be determined just by the radius of rounded comers of the polygonized step. If fluctuations do not have enough time to develop, the kinetic effects may be essential. Indeed, 'communications' between comers of a short straight step segment may occur and, thus, the GTL may be implemented only via kink exchange. E.g., dissolutions of this short segment at macroscopic equilibrium occurs as follows: The kinks are split from one comer as a result of fluctuations, and annihilate with kinks of the opposite sign generated by another comer. Similarly, an exchange via chain of kinks on a rough step is the mechanism to implement the GT Law. If there is a supersaturation with respect to a large crystal, the kinks not only diffuse along the step, but move back the generating comers. This 'wind' prevents communication between the comers and places upper limit supersaturation only below which GTL is applicable. Steps replace kinks in the 3D case, though, of course, another dimensionality brings about another physics. Another specific problem to think about is if fluctuations are always fast enough to provide enough kinks for linear dependence of step rate on supersaturation. Increasing azimuthal polygonization of growth hillocks is a sign of insufficient fluctuation rate. Morphological stability of vicinal faces is usually considered on the basis of mutually parallel steps. Azimuthal anisotropy and interlacing of step bunches inducing the well known bunch splitting is another challenge. Among other challenging problems are: existence of surface diffusion on the crystal/so1ution interface, step interaction in solutions, achievement of step flow modes from liquids, impurity effects. New phenomena essential in biomacromolecular crystallization is another interesting area.

Chernov, A.↗

RFe{sub 2}Mg{sub x}Al{sub 8−x} (R=La–Nd and Sm; x≈0.8): Flux synthesis, structure, magnetic and electrical properties

Single crystals of Mg-substituted CeFe{sub 2}Al{sub 8} type intermetallics RFe{sub 2}Mg{sub x}Al{sub 8–x} (R=La–Nd and Sm; x≤1) were grown by reacting iron and rare earth metals in 1:1 Mg/Al mixed flux. The structure features mono-capped and bi-capped trigonal prismatic FeAl{sub 6} units. Electronic structure calculations indicate that magnesium substitution reduces the valence electron count, shifting the Fermi level away from a pseudo-gap. This changes the electronic nature of the cerium analog; the previously reported ternary CeFe{sub 2}Al{sub 8} shows strong hybridization between the cerium states and the conduction electrons, resulting in no magnetic moment on Ce atoms. On the other hand, magnetic susceptibility measurements on CeFe{sub 2}Mg{sub x}Al{sub 8–x} indicates a localized moment on cerium. The newly synthesized Pr, Nd and Sm analogs exhibit antiferromagnetic ordering at 2.8 K, 7.8 K and 12 K respectively. Solid state {sup 27}Al NMR of LaFe{sub 2}Mg{sub x}Al{sub 8–x} exhibits a broad Knight shift at ~1200 ppm, consistent with the metallic behavior shown by electrical resistivity data. - Graphical abstract: Mg substitution into CeFe{sub 2}Al{sub 8} modifies cerium valence due to changing valence electron count. - Highlights: • RFe{sub 2}Mg{sub x}Al{sub 8−x} (R=La–Nd, Sm) grow as large crystals from reactions in Mg/Al flux. • Products are magnesium-substituted variants of CeFe{sub 2}Al{sub 8}, with CaCo{sub 2}Al{sub 8} structure. • Ce magnetic moment in CeFe{sub 2}Mg{sub x}Al{sub 8−x} varies from that in CeFe{sub 2}Al{sub 8} due to VEC change. • Antiferromagnetic ordering observed for Pr, Nd, Sm analogs of RFe{sub 2}Mg{sub x}Al{sub 8−x}.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗