Engineering Papers⌕ Search

SEARCH · Engineering Papers

Results for “Powder diffraction”

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 1,783 records · Page 99
All sourcesNASA NTRSDOE OSTI
DOE OSTI2015

Experimental and theoretical characterization of ordered MAX phases Mo{sub 2}TiAlC{sub 2} and Mo{sub 2}Ti{sub 2}AlC{sub 3}

Herein, we report on the phase stabilities and crystal structures of two newly discovered ordered, quaternary MAX phases—Mo{sub 2}TiAlC{sub 2} and Mo{sub 2}Ti{sub 2}AlC{sub 3}—synthesized by mixing and heating different elemental powder mixtures of mMo:(3-m)Ti:1.1Al:2C with 1.5 ≤ m ≤ 2.2 and 2Mo: 2Ti:1.1Al:2.7C to 1600 °C for 4 h under Ar flow. In general, for m ≥ 2 an ordered 312 phase, (Mo{sub 2}Ti)AlC{sub 2}, was the majority phase; for m < 2, an ordered 413 phase (Mo{sub 2}Ti{sub 2})AlC{sub 3}, was the major product. The actual chemistries determined from X-ray photoelectron spectroscopy (XPS) are Mo{sub 2}TiAlC{sub 1.7} and Mo{sub 2}Ti{sub 1.9}Al{sub 0.9}C{sub 2.5}, respectively. High resolution scanning transmission microscopy, XPS and Rietveld analysis of powder X-ray diffraction confirmed the general ordered stacking sequence to be Mo-Ti-Mo-Al-Mo-Ti-Mo for Mo{sub 2}TiAlC{sub 2} and Mo-Ti-Ti-Mo-Al-Mo-Ti-Ti-Mo for Mo{sub 2}Ti{sub 2}AlC{sub 3}, with the carbon atoms occupying the octahedral sites between the transition metal layers. Consistent with the experimental results, the theoretical calculations clearly show that M layer ordering is mostly driven by the high penalty paid in energy by having the Mo atoms surrounded by C in a face-centered configuration, i.e., in the center of the M{sub n+1}X{sub n} blocks. At 331 GPa and 367 GPa, respectively, the Young's moduli of the ordered Mo{sub 2}TiAlC{sub 2} and Mo{sub 2}Ti{sub 2}AlC{sub 3} are predicted to be higher than those calculated for their ternary end members. Like most other MAX phases, because of the high density of states at the Fermi level, the resistivity measurement over 300 to 10 K for both phases showed metallic behavior.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Magnetic properties and transformation of crystal structure in the ErFe{sub 2}-ErAl{sub 2} system

The modification of structural properties and magnetic behaviour of the ErFe{sub 2−x}Al{sub x} Laves phase intermetallic compounds have been studied while changing the Al content in the range 0.36 ≤ x ≤ 1.5. Powder X-ray diffraction study at room temperature showed the formation of the cubic C15 structure, in the samples with Al content of 0.36 ≤ x < 0.75 and 1.4 ≤ x ≤ 2.0. For the intermediate compositions with 0.75 ≤ x ≤ 1.4, the hexagonal C14 structure is observed. Magnetic and magnetocaloric properties of polycrystalline ErFe{sub 2−x}Al{sub x} intermetallic compounds were investigated experimentally using magnetic and heat capacity measurements. The Curie temperature T{sub C} decreases from 275 to 28 K as the Al content increases from x = 0.36 to x = 1.5, respectively. Magnetization measurements in strong magnetic fields showed the complex mechanism of magnetic saturation in the studied compounds. Under an external field change from 0 to 2 T, the maximum entropy change is 6 J/kg K at T = 28 K for the composition with x = 1.5. The minimum in the concentration dependence of the magnetic entropy change is observed in the vicinity of x equal to 1.25. Regularities of variations of magnetocaloric properties of ErFe{sub 2−x}Al{sub x} intermetallic compounds with increasing Al content are discussed from the point of view of their both structural and magnetic states.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Synthesis of ZnSnO{sub 3} nanostructure by sol gel method

Zinc Stannate (ZST) with composition ZnSnO{sub 3} is known for high electron mobility, optical, piezoelectric and charge storage properties. ZST crystalizes in different lattice structures, which allows a wide range of tunablity. We demonstrate successful synthesis of ZnSnO{sub 3} nanomaterial by sol-gel method. ZnSnO{sub 3} nanomaterials were calcined and sintered at different temperatures. Powder X-ray diffraction confirmed the single phase of the nanomaterial with rhombohedral R-3 space group. The Rietveld refinement of diffraction pattern yielded lattice parameter values a=5.26Å, c=14.09Å. Raman spectroscopy revealed higher activity towards higher wavenumbers. Raman shift around 530cm{sup −1} was found to be highly structure dependent, most probably due to anharmonic atomic vibrations in ZnO{sub 6}/SnO{sub 6} octahedra around center of mass. Sharp Peak around 650cm{sup −1} is characteristic of ZnSnO{sub 3} molecule.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2014

Synthesis of BiOI flowerlike hierarchical structures toward photocatalytic reduction of CO{sub 2} to CH{sub 4}

BiOI can be used for photocatalytic reduction of CO{sub 2} into hydrocarbon fuels under sunlight. - Highlights: • Room temperature synthesis of BiOI flowerlike hierarchical structures. • BiOI can be used for photocatalytic reduction of CO{sub 2} into hydrocarbon fuels under sunlight. • The photocatalytic activity of BiOI is higher than that of P25 TiO{sub 2}. - Abstract: BiOI flowerlike hierarchical structure was synthesized by the direct hydrolysis method – hydrolysis at room temperature in the presence of polyvinyl pyrrolidone. As-synthesized BiOI was characterized by powder X-ray diffraction, UV–vis diffuse reflectance spectra, X-ray photoelectron spectroscopy spectra, scanning electron microscopy, transmission electron microscopy, and high-resolution transmission electron microscopy. It is a facile way to obtain BiOI flowerlike hierarchical structure photocatalyst for photocatalytic reduction of CO{sub 2} into hydrocarbon fuels under simulated sunlight irradiation without cocatalyst. And the photocatalytic activity of as-synthesized BiOI is higher than that of P25 TiO{sub 2} and bulk BiOI.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Silver chromate and silver dichromate nanostructures: Sonochemical synthesis, characterization, and photocatalytic properties

Graphical abstract: In this work, Ag{sub 2}CrO{sub 4} and Ag{sub 2}Cr{sub 2}O{sub 7} nanostructures have been sonochemically prepared using silver salicylate. The effect of preparation parameters on the morphology of the products was investigated by SEM images. Highlights: ► Herein, Ag{sub 2}CrO{sub 4} and Ag{sub 2}Cr{sub 2}O{sub 7} nanostructures have been sonochemically prepared. ► The effect of preparation parameters on the morphology of the products was investigated. ► The photocatalytic activity of the as-prepared Ag{sub 2}CrO{sub 4} nanoparticles was tested. ► XPS spectra indicated the high purity of Ag{sub 2}Cr{sub 2}O{sub 7} nanostructures obtained. - Abstract: In this work, Ag{sub 2}CrO{sub 4} and Ag{sub 2}Cr{sub 2}O{sub 7} nanostructures have been produced via a sonochemical method using silver salicylate as precursor. Besides silver salicylate, Na{sub 2}CrO{sub 4} and (NH{sub 4}){sub 2}Cr{sub 2}O{sub 7} as starting reagents were applied. To investigate the effect of preparation parameters on the morphology and particle size of Ag{sub 2}CrO{sub 4} and Ag{sub 2}Cr{sub 2}O{sub 7}, sonication time, type of surfactant and its concentration were changed. The as-produced nanostructures were characterized by techniques like powder X-ray diffraction, scanning electron microscopy, and X-ray photoelectron spectroscopy. The scanning electron micrographs showed that particle-like and rod-like nanostructures of Ag{sub 2}CrO{sub 4} and Ag{sub 2}Cr{sub 2}O{sub 7} were produced using different surfactants. To investigate the catalytic properties of Ag{sub 2}CrO{sub 4} nanoparticles, photooxidation of methyl orange (MO) was performed. According to the obtained results, it was found that the methyl orange degradation was about 87.3% after 280 min irradiation of visible light.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Surfactant mediated hydrothermal synthesis, characterization and luminescent properties of GdPO{sub 4}: Ce{sup 3+}/Tb{sup 3+} @ GdPO{sub 4} core shell nanorods

Highlights: • Core shell nanorods were synthesised by surfactant assisted hydrothermal method. • Morphology of core shell nanorods resembles those of core nanorods indicating coating of shell on cores. • More uniform and non-aggregated core shell nanorods were prepared in presence of surfactants. • Surfactant assisted prepared core shell nanorods show intense emission as compared to uncoated core nanorods. - Abstract: Core shell GdPO{sub 4}: Ce{sup 3+}/Tb{sup 3+} @ GdPO{sub 4} nanorods were synthesized via hydrothermal route in the presence of different surfactants [cetyltrimethyl ammonium bromide (CTAB) and Sodium dodecyl sulphate (SDS)]. The nanorods were characterized by powder X-ray diffraction (PXRD), fourier transform infrared spectroscopy (FTIR), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), energy dispersive spectroscopy (EDS) and photoluminescence (PL) studies. The X-ray diffraction results indicate good crystallinity and effective doping in core and core shell nanorods. SEM and TEM micrographs show that all of the as prepared gadolinium phosphate products have rod like shape. The compositional analysis of GdPO{sub 4}: Ce{sup 3+}/Tb{sup 3+} core was done by EDS. The emission intensity of the GdPO{sub 4}: Ce{sup 3+}/Tb{sup 3+} @ GdPO{sub 4} core shell increased significantly with respect to those of GdPO{sub 4}: Ce{sup 3+}/Tb{sup 3+} core nanorods. The effect of surfactant on the uniformity, thickness and luminescence of the core shell nanorods was investigated.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Harnessing nanoscale densification for controlling gas selectivity in flexible zeolitic imidazolate frameworks

Flexible metal-organic frameworks (MOFs) are promising for gas separation due to their molecular recognition capabilities. However, gate-opening behavior in certain flexible MOFs can reduce gas selectivity, enabling simultaneous adsorption of multiple gases. We introduce a binder-free, pressure-free densification process to enhance gas selectivity in flexible zeolitic imidazolate frameworks (ZIF-7 and ZIF-9) by optimizing nanoparticle packing. Unlike powders, the densified ZIF-7 and ZIF-9 retain rhombohedral crystal structures after solvent removal, confirmed via synchrotron powder X-ray diffraction. This process modifies adsorption behavior by introducing a diffusion barrier, enabling diffusivity-driven kinetic separation and enhanced CO2/hydrocarbon selectivity. At 0.5 bar, ZIF-7 mono shows 2×, 4×, and 9.5× higher CO 2 selectivity over C 2 H 2 , C 2 H 4 , and C 2 H 6 , respectively, versus ZIF-7 pwd . ZIF-9 mono similarly shows 6.5×, 3×, and 39× improvements over ZIF-9 pwd . Both monoliths outperform powders in ternary gas mixtures. This study provides a novel strategy to control gate opening and enhance gas selectivity in flexible MOFs for practical separation applications.

CO2/hydrocarbon separation↗
DOE OSTI2016

Effect of the both texture and electrical properties of activated carbon on the CO{sub 2} adsorption capacity

Highlights: • A series of activated carbon pellet without binder was prepared by chemical activation. • Carbon dioxide storage isotherm at 30 °C and up to 25 bars was measured for the microporous carbon. • Adsorption enthalpies have been correlated with the carbon dioxide uptake. • Pyrolysis temperature effect on the electrical conductivity of the samples. • Impact of the both texture and electrical properties on CO{sub 2} adsorption capacity have been deducted - Abstract: A series of activated carbon pellets (ACP) based on olive stones were studied for CO{sub 2} storage application. The surface area, pore volume, and pore diameter were evaluated from the analysis of N{sub 2} adsorption isotherm data. The characterization of carbon materials was performed by scanning electron microscopy (SEM), the powder X-ray diffraction (PXRD) and transmission electron microscopy (TEM). The adsorption enthalpies were obtained by microcalorimetry. The effect of pyrolysis temperature on textural, electrical conductivity and gas adsorption capacities of the ACP were investigated by adsorbing CO{sub 2} at 303 K in the pressure range of 0–2.3 MPa. In fact the electrical conductivity is strongly affected by the microporosity of the samples and the size of the micropore. It increases when the pore size decreases which affect the CO{sub 2} adsorption. Also with increases temperature the free electrons concentration on the surface increases which affect the interaction of the adsorbed gas molecules.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Interesting electron storage phenomenon in the spherical Ag/TiO{sub 2} nanocomposites and its application for the decomposition of acetaldehyde in the dark

Highlights: • The Ag/TiO{sub 2} composites have been prepared by a facile solvothermal method. • The photogenerated charges transfer behaviors between the Ag and TiO{sub 2}. • The Ag/TiO{sub 2} composites can store photogenerated electrons for a relative long time. • The Ag/TiO{sub 2} composite could be further used to decompose acetaldehyde in the dark. - Abstract: Ag/TiO{sub 2} nanocomposite has been prepared by a facile one-step low-temperature solvothermal method. The powder X-ray diffraction (XRD) and transmission electron microscopy (TEM) measurements have been used to characterize the detailed structure of the as-synthesized nanocomposite and the results indicate that the nanocompoiste is with the spherical structure and Ag and TiO{sub 2} nanoparticles are homogeneously dispersed in the sphere. Surface photovoltage (SPV) and transient photovoltage (TPV) techniques were used to further investigate the charge transfer behavior between the TiO{sub 2} and Ag in this composite material, and the results reveal that the nanocomposites could store the electrons for a relative long time even under air. Furthermore, these stored electrons in the nanocomposites have been successfully applied to decompose the acetaldehyde in the dark.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Methods of chemical and phase composition analysis of gallstones

This review presents the instrumental methods used for chemical and phase composition investigation of gallstones. A great body of data has been collected in the literature on the presence of elements and their concentrations, obtained by fluorescence microscopy, X-ray fluorescence spectroscopy, neutron activation analysis, proton (particle) induced X-ray emission, atomic absorption spectroscopy, high-resolution gamma-ray spectrometry, electron paramagnetic resonance. Structural methods—powder X-ray diffraction, infrared spectroscopy, Raman spectroscopy—provide information about organic and inorganic phases in gallstones. Stone morphology was studied at the macrolevel with optical microscopy. Results obtained by analytical scanning and transmission electron microscopy with X-ray energy dispersive spectrometry are discussed. The chemical composition and structure of gallstones determine the strategy of removing stone from the body and treatment of patients: surgery or dissolution in the body. Therefore one chapter of the review describes the potential of dissolution methods. Early diagnosis and appropriate treatment of the disease depend on the development of clinical methods for in vivo investigation, which gave grounds to present the main characteristics and potential of ultrasonography (ultrasound scanning), magnetic resonance imaging, and X-ray computed tomography.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2016

Growth, structural, optical, thermal and mechanical properties of cytosinium hydrogen selenite: A novel nonlinear optical single crystal

Highlights: • Growth of bulk single crystals of cytosinium hydrogen selenite (CHS) is reported. • Dielectric constant of CHS is measured as a function of Frequency and temperature. • Lower cut off value of UV–vis-NIR spectrum of CHS crystal is observed at 210 nm. • Meyer’s index value of CHS crystal calculated identifies it as a soft material. • Powder SHG efficiency of CHS is about 1.5 times that of KDP crystal. - Abstract: A novel nonlinear optical single crystal of cytosinium hydrogen selenite was grown from aqueous solution of cytosinium hydrogen selenite by slow solvent evaporation method at room temperature. The structural properties of grown crystal have been studied by single crystal and powder X-ray diffraction analysis. Presence of various functional groups was identified from Fourier transform infrared spectroscopy. The optical transmittance and absorbance spectra were recorded by UV–vis-NIR spectrometer and the grown crystal possesses good transparency in the entire visible region. The dielectric constant and dielectric loss of the crystal were calculated as a function of frequency at different temperatures. The mechanical strength of the cytosinium hydrogen selenite crystal was estimated using Vicker’s microhardness tester. Etch patterns of the cytosinium hydrogen selenite crystal were obtained using distilled water as etchant for different etching time. Second harmonic generation efficiency tested using Nd:YAG laser is about 1.5 times that of KDP.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Open frameworks based on mono-lanthanide-substituted polyoxometaloaluminate building units: Syntheses, structures and properties

Metal-substituted polyoxometalates are one of the most important research branch in polyoxometalate chemistry and have attached an increasing attention due to not only their intriguing structural diversity but also their special properties applicable to material science. In this paper, A series of novel lanthanide-substituted polyoxometaloaluminates (LSPs), K{sub 2}(H{sub 2}O){sub 4}Ln(H{sub 2}O){sub 7}[Ln(H{sub 2}O){sub 3}HAlW{sub 11}O{sub 39}]·nH{sub 2}O (Ln=Pr 1, Nd 2, Sm 3, Eu 4, Gd 5, Tb 6; for 1, n=8; for 2,4,5,6, n=7; for 3, n=9), have been hydrothermally made and characterized by infrared (IR) spectra, thermal gravimetric analysis (TGA), powder X-ray diffraction (PXRD) and single-crystal X-ray diffraction, respectively. The experimental results indicate these compounds exhibit 3-D frameworks with Gra-type topology constructed by lanthanide cations, mono- lanthanide-substituted [Gd(H{sub 2}O){sub 3}HAlW{sub 11}O{sub 39}]{sup 5−} cluster units and K{sup +} cations. The photoluminescence measurements show that Compounds 2, 4, 6 exhibit the characteristic emission for Nd{sup 3+}, Eu{sup 3+} and Tb{sup 3+} cations, respectively. In addition, this series of LSPs show weak second harmonic generation effects and ferroelectric properties. The success in making 1−6 not only provides innovative examples in search of new POM species, but also may open up possibilities for the design of LSP-based materials with related functions. - Graphical abstract: A series of lanthanide-substituted polyoxometaloaluminates have been hydrothermally made and their photoluminescence, non-linear optical and ferroelectricity properties have also been investigated, respectively. - Highlights: • Six lanthanide-substituted Al-based polyoxometalates have first been made. • Eu/Nd/Tb-based compounds display photoluminescence property. • The nonlinear optical and ferroelectricity properties have been investigated.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2016

Layered vanadyl (IV) nitroprusside: Magnetic interaction through a network of hydrogen bonds

The hydrogen bond and π-π stacking are two non-covalent interactions able to support cooperative magnetic ordering between paramagnetic centers. This contribution reports the crystal structure and related magnetic properties for VO[Fe(CN){sub 5}NO]·2H{sub 2}O, which has a layered structure. This solid crystallizes with an orthorhombic unit cell, in the Pna2{sub 1} space group, with cell parameters a=14.1804(2), b=10.4935(1), c=7.1722(8) Å and four molecules per unit cell (Z=4). Its crystal structure was solved and refined from powder X-ray diffraction data. Neighboring layers remain linked through a network of hydrogen bonds involving a water molecule coordinated to the axial position for the V atom and the unbridged axial NO and CN ligands. An uncoordinated water molecule is found forming a triple bridge between these last two ligands and the coordinated water molecule. The magnetic measurements, recorded down to 2 K, shows a ferromagnetic interaction between V atoms located at neighboring layers, with a Curie-Weiss constant of 3.14 K. Such ferromagnetic behavior was interpreted as resulting from a superexchange interaction through the network of strong OH····O{sub H2O}, OH····N{sub CN}, and OH····O{sub NO} hydrogen bonds that connects neighboring layers. The interaction within the layer must be of antiferromagnetic nature and it was detected close to 2 K. - Graphical abstract: Coordination environment for the metals in vanadyl (II) nitroprusside dihydrate. Display Omitted - Highlights: • Crystal structure of vanadyl nitroprusside dehydrate. • Network of hydrogen bonds. • Magnetic interactions through a network of hydrogen bonds. • Layered transition metal nitroprussides.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2015

Syntheses, characterization and properties of silver, copper and palladium complexes from bis(oxazoline)-containing ligands

The reactions of 2,6-di(2-oxazolyl)pyridine (L{sup 1}) and 2,6-bis[(S)-4-phenyl-2-oxazolyl]pyridine (L{sup 2}) with silver, copper and palladium salts to yield six new complexes: ([Ag{sub 5}(L{sup 1}){sub 5}](BF{sub 4}){sub 5}){sub n} (1), ([Ag(L{sup 1})](SbF{sub 6})){sub n} (2), [Cu{sub 4}I{sub 4}(L{sup 1}){sub 2}] (3), [Cu{sub 6}I{sub 6}(L{sup 1}){sub 2}] (4), [Pd(L′{sup 1})(OAc)] (5), [Pd(L′{sup 2})Cl] (6), which were fully characterized by single-crystal and powder X-ray diffraction, IR, elemental and thermogravimetric analyses. 1 and 2 are a pair of Ag-oxazoline helical chain structure complexes. The spiral directions of chains are opposite in 1, while identical in 2; the measurement of CD spectra can further confirm their meso and chiral structures. Complexes 3 and 4 show eight-nuclear and twelve-nuclear iodine–cuprous cluster structure. Their structural diversity is induced by different molar ratios of CuI:L{sup 1}. Complexes 5 and 6 are discrete mononuclear palladium complexes. In situ oxazolyl-ring-opening reactions take place in the syntheses of them and the L{sup 1} and the L{sup 2} were transformed to their oxazolyl-ring opened derivatives L′{sup 1} and L′{sup 2}. Moreover, fluorescence, non-linear optical properties, and ferroelectric properties have been investigated. - Graphical abstract: 2,6-di(2-oxazolyl)pyridine (L{sup 1}) reacts with silver and copper salts to yield helical and cluster structure complexes. - Highlights: • Helical and cluster structure complexes. • In situ oxazolyl-ring-opening reactions. • Fluorescence, non-linear optical properties, and ferroelectric properties.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2014

Magnetic and optical properties of electrospun hollow nanofibers of SnO{sub 2} doped with Ce-ion

Cerium doped SnO{sub 2} hollow nanofibers were synthesized by electrospinning. High resolution scanning electron microscope (HRSEM) and transmission electron microscopy (TEM) analysis showed hollow nanofibers with diameters around ∼200 nm. The optimized substitution of Ce ion into SnO{sub 2} lattices happened above 6 mol. % doping as confirmed by Powder X-ray diffraction (XRD) studies. Optical band gap was decreased by the doping confirming the direct energy transfer between f-electrons of rare earth ion and the SnO{sub 2} conduction or valence band. The compound also exhibited room temperature ferromagnetism with the saturation magnetization of 19 × 10{sup −5} emu/g at 6 mol. %. This study demonstrates the Ce doped SnO{sub 2} hollow nanofibers for applications in magneto-optoelectronic devices.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2016

Crystallographic features related to a van der Waals coupling in the layered chalcogenide FePS{sub 3}

We investigated the crystallographic structure of FePS{sub 3} with a layered structure using transmission electron microscopy and powder X-ray diffraction. We found that FePS{sub 3} forms a rotational twin structure with the common axis along the c*-axis. The high-resolution transmission electron microscopy images revealed that the twin boundaries were positioned at the van der Waals gaps between the layers. The narrow bands of dark contrast were observed in the bright-field transmission electron microscopy images below the antiferromagnetic transition temperature, T{sub N} ≈ 120 K. Low-temperature X-ray diffraction showed a lattice distortion; the a- and b-axes shortened and lengthened, respectively, as the temperature decreased below T{sub N.} We propose that the narrow bands of dark contrast observed in the bright-field transmission electron microscopy images are caused by the directional lattice distortion with respect to each micro-twin variant in the antiferromagnetic phase.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2014

Soft chemical synthesis of Ag{sub 3}SbS{sub 3} with efficient and recyclable visible light photocatalytic properties

Highlights: • Highly crystalline Ag{sub 3}SbS{sub 3} synthesized using soft chemical approach. • First time report of photocatalytic activity of Ag{sub 3}SbS{sub 3}. • Ag{sub 3}SbS{sub 3} degraded the harmful organic dyes rapidly under visible radiation. • Pseudo first order kinetics have been followed in these sets of reactions. • Up to 90% of Methylene Blue degraded even after 4th cycle of catalyst reuse. • Structure of catalyst is intact after reuse. • As the catalyst is heavy, its separation after use is quite simple. - Abstract: Application of Ag{sub 3}SbS{sub 3}, obtained by soft chemical approach involving rapid reaction of air stable metal–thiourea complexes in ethylene glycol medium, as visible light photocatalyst for the degradation of dye solutions was investigated. Ag{sub 3}SbS{sub 3} was confirmed by high resolution powder X-ray diffraction pattern and its no defined morphology was present in SEM images. From UV–vis spectroscopy measurements, optical band gap of 1.77 eV was deduced for Ag{sub 3}SbS{sub 3}. Rapid degradation kinetics and recyclability was exhibited by Ag{sub 3}SbS{sub 3} towards Methylene Blue, Methyl Orange, Malachite Green, and Rhodamine 6G dye solutions under visible radiation. All these processes followed pseudo first order kinetics. High surface area (6.39 m{sup 2}/g), with mesopores (3.81 nm), arising from solvent mediated synthesis of Ag{sub 3}SbS{sub 3} has been correlated to its catalytic activity.

36 MATERIALS SCIENCE↗
DOE OSTI2017

New insights into the structure, chemistry, and properties of Cu 4 SnS 4

The ambient temperature structure of Cu 4 SnS 4 has been revisited and the recently reported low temperature structure has been confirmed from single-crystal X-ray diffraction data. A structural phase transition from a large monoclinic unit cell at low temperature to a smaller orthorhombic unit cell at high temperature has been observed. The room temperature phase exhibited disorder in the two copper sites, which is a different finding from earlier reports. The low temperature monoclinic form crystallizes in P2 1 /c space group, which is isostructural with Cu 4 GeS 4 . The phase transition has also been studied with variable temperature powder X-ray diffraction and 119 Sn Mössbauer spectroscopy. The Seebeck coefficients and electrical resistivity of polycrystalline Cu 4 SnS 4 are reported from 16 to 400 K on hot pressed pellets. Thermal conductivity measurements at high temperatures, 350 – 750 K exhibited very low thermal conductivities in the range 0.28 – 0.35 W K –1 m –1 . In all the transport measurements the phase transition has been observed at around 232 K. Resistivity decreases, while Seebeck coefficient increases after the phase transition during warming up from low to high temperatures. This change in resistivity has been correlated with the results of first-principles electronic band structure calculations using highly-accurate screened-exchange local density approximation. It was found that both the low hole effective mass of 0.63 me for the Γ→Y crystallographic direction and small band gap, 0.49 eV, are likely to contribute to the observed higher conductivity of the orthorhombic phase. Cu 4 SnS 4 is also electrochemically active and shows reversible reaction with lithium between 1.7 and 3.5 volts.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗