HIGH FREQUENCY RAMAN MODES IN NANOCRYSTALLINE LEAD (II) FLUORIDE

2006 ◽  
Vol 05 (04n05) ◽  
pp. 585-591
Author(s):  
P. THANGADURAI ◽  
S. RAMASAMY ◽  
R. KESAVAMOORTHY

Nanocrystalline PbF 2 was prepared by inert gas condensation technique. Structural studies using X-ray diffraction showed that as-prepared and annealed samples contained both orthorhombic and cubic phases of PbF 2. The annealed samples contain dominantly the cubic phase. For the first time Raman scattering and PL experiments were carried out on these nano- PbF 2. In addition to regular lattice vibrational modes such as T2g for cubic phase and Ag and B1g for orthorhombic phases, a few new Raman modes have been observed at high frequencies. PL studies confirmed that the new Raman modes are due to the presence of electronic centers. The regular modes agree well with the theoretically calculated values and previously reported experimental values.

2000 ◽  
Vol 643 ◽  
Author(s):  
P. Weisbecker ◽  
G. Bonhomme ◽  
A. Cael ◽  
L. Zhang ◽  
J.M. Dubois

AbstractUsing powder X-ray diffraction, we have studied the transformation of an atomized powder of nominal composition Al62Cu25.5Fe12.5 upon annealing at 500°C in air or in vacuum. The initial mixture of icosahedral and B2 cubic phases transforms within 2 hours into a nearly pure icosahedral compound. We observe however that a small amount of residual cubic phase is still present after annealings as long as 65 hours. Furthermore, the initial cubic phase splits in two components, a CsCl-type and a disordered bcc cubic phase. By comparison of the heat treatments in air and in vacuum, we point out that oxygen atoms diffuse into the icosahedral lattice.


1996 ◽  
Vol 431 ◽  
Author(s):  
Jianping Yang ◽  
Syed Qadri ◽  
Banahalli Ratna

AbstractBicontinuous cubic phase of lipid has been utilized for the first time as a matrix to synthesize II–VI (CdS) and IV–VI (PbS) semiconductor nanocrystallites. The nanoparticles were isolated from the lipid matrix and stabilized by capping with a thiol compound before purification. Two different sizes (2.3 nm and 3.0 nm) of CdS particles were prepared by varying the conditions of preparation. The size was determined by a combination of UV-vis absorption spectra and X-ray diffraction (XRD). The steep absorption edges of the two CdS samples indicate very narrow size distribution. XRD and transmission electron microscopic imaging of PbS nanocrystallites revealed that the size was 4.9 nm with nearly monodispersed size distribution.


Minerals ◽  
2021 ◽  
Vol 11 (7) ◽  
pp. 767
Author(s):  
Sytle M. Antao

Two isotropic grossular (ideally Ca3Al2Si3O12) samples from (1) Canada and (2) Tanzania, three optically anisotropic grossular samples (3, 4, 5) from Mexico, and one (6) anisotropic sample from Italy were studied. The crystal structure of the six samples was refined in the cubic space group Ia3¯d, using monochromatic synchrotron high-resolution powder X-ray diffraction (HRPXRD) data and the Rietveld method. The compositions of the samples were obtained from electron microprobe analyses (EPMA). The HRPXRD traces show a single cubic phase for two isotropic samples, whereas the four anisotropic samples contain two different cubic phases that were also resolved using X-ray elemental line scans, backscattered electron (BSE) images, and elemental maps. Structural mismatch from two cubic phases intergrown in the birefringent samples gives rise to strain-induced optical anisotropy. Considering the garnet general formula, [8]X3[6]Y2[4]Z3[4]O12, the results of this study show that with increasing unit-cell parameter, the Y-O distance increases linearly and rather steeply, the average <X-O> distance increases just slightly in response to substitution mainly on the Y site, while the Z-O distance remains nearly constant. The X and Z sites in grossular contain Ca and Si atoms, respectively; both sites show insignificant substitutions by other atoms, which is supported by a constant Z-O distance and only a slight increase in the average <X-O> distance. The main cation exchange is realized in the Y site, where Fe3+ (ionic radius = 0.645 Å) replaces Al3+ (ionic radius = 0.545 Å), so the Y-O distance increases the most.


Author(s):  
John M Seddon ◽  
Adam M Squires ◽  
Charlotte E Conn ◽  
Oscar Ces ◽  
Andrew J Heron ◽  
...  

In this paper, we give an overview of our studies by static and time-resolved X-ray diffraction of inverse cubic phases and phase transitions in lipids. In §1 , we briefly discuss the lyotropic phase behaviour of lipids, focusing attention on non-lamellar structures, and their geometric/topological relationship to fusion processes in lipid membranes. Possible pathways for transitions between different cubic phases are also outlined. In §2 , we discuss the effects of hydrostatic pressure on lipid membranes and lipid phase transitions, and describe how the parameters required to predict the pressure dependence of lipid phase transition temperatures can be conveniently measured. We review some earlier results of inverse bicontinuous cubic phases from our laboratory, showing effects such as pressure-induced formation and swelling. In §3 , we describe the technique of pressure-jump synchrotron X-ray diffraction. We present results that have been obtained from the lipid system 1 : 2 dilauroylphosphatidylcholine/lauric acid for cubic–inverse hexagonal, cubic–cubic and lamellar–cubic transitions. The rate of transition was found to increase with the amplitude of the pressure-jump and with increasing temperature. Evidence for intermediate structures occurring transiently during the transitions was also obtained. In §4 , we describe an IDL-based ‘ AXcess ’ software package being developed in our laboratory to permit batch processing and analysis of the large X-ray datasets produced by pressure-jump synchrotron experiments. In §5 , we present some recent results on the fluid lamellar– Pn 3 m cubic phase transition of the single-chain lipid 1-monoelaidin, which we have studied both by pressure-jump and temperature-jump X-ray diffraction. Finally, in §6 , we give a few indicators of future directions of this research. We anticipate that the most useful technical advance will be the development of pressure-jump apparatus on the microsecond time-scale, which will involve the use of a stack of piezoelectric pressure actuators. The pressure-jump technique is not restricted to lipid phase transitions, but can be used to study a wide range of soft matter transitions, ranging from protein unfolding and DNA unwinding and transitions, to phase transitions in thermotropic liquid crystals, surfactants and block copolymers.


Minerals ◽  
2021 ◽  
Vol 11 (6) ◽  
pp. 611
Author(s):  
Celia Marcos ◽  
María de Uribe-Zorita ◽  
Pedro Álvarez-Lloret ◽  
Alaa Adawy ◽  
Patricia Fernández ◽  
...  

Chert samples from different coastal and inland outcrops in the Eastern Asturias (Spain) were mineralogically investigated for the first time for archaeological purposes. X-ray diffraction, X-ray fluorescence, transmission electron microscopy, infrared and Raman spectroscopy and total organic carbon techniques were used. The low content of moganite, since its detection by X-ray diffraction is practically imperceptible, and the crystallite size (over 1000 Å) of the quartz in these cherts would be indicative of its maturity and could potentially be used for dating chert-tools recovered from archaeological sites. Also, this information can constitute essential data to differentiate the cherts and compare them with those used in archaeological tools. However, neither composition nor crystallite size would allow distinguishing between coastal and inland chert outcrops belonging to the same geological formations.


Crystals ◽  
2021 ◽  
Vol 11 (2) ◽  
pp. 218
Author(s):  
Carlos Alberto Ríos-Reyes ◽  
German Alfonso Reyes-Mendoza ◽  
José Antonio Henao-Martínez ◽  
Craig Williams ◽  
Alan Dyer

This study reports for the first time the geologic occurrence of natural zeolite A and associated minerals in mudstones from the Cretaceous Paja Formation in the urban area of the municipality of Vélez (Santander), Colombia. These rocks are mainly composed of quartz, muscovite, pyrophyllite, kaolinite and chlorite group minerals, framboidal and cubic pyrite, as well as marcasite, with minor feldspar, sulphates, and phosphates. Total organic carbon (TOC), total sulfur (TS), and millimeter fragments of algae are high, whereas few centimeters and not biodiverse small ammonite fossils, and other allochemical components are subordinated. Na–A zeolite and associated mineral phases as sodalite occur just beside the interparticle micropores (honeycomb from framboidal, cube molds, and amorphous cavities). It is facilitated by petrophysical properties alterations, due to processes of high diagenesis, temperatures up to 80–100 °C, with weathering contributions, which increase the porosity and permeability, as well as the transmissivity (fluid flow), allowing the geochemistry remobilization and/or recrystallization of pre-existing silica, muscovite, kaolinite minerals group, salts, carbonates, oxides and peroxides. X-ray diffraction analyses reveal the mineral composition of the mudstones and scanning electron micrographs show the typical cubic morphology of Na–A zeolite of approximately 0.45 mμ in particle size. Our data show that the sequence of the transformation of phases is: Poorly crystalline aluminosilicate → sodalite → Na–A zeolite. A literature review shows that this is an unusual example of the occurrence of natural zeolites in sedimentary marine rocks recognized around the world.


Materials ◽  
2021 ◽  
Vol 14 (10) ◽  
pp. 2623
Author(s):  
Monika Wójcik-Bania ◽  
Jakub Matusik

Polymer–clay mineral composites are an important class of materials with various applications in the industry. Despite interesting properties of polysiloxanes, such matrices were rarely used in combination with clay minerals. Thus, for the first time, a systematic study was designed to investigate the cross-linking efficiency of polysiloxane networks in the presence of 2 wt % of organo-montmorillonite. Montmorillonite (Mt) was intercalated with six quaternary ammonium salts of the cation structure [(CH3)2R’NR]+, where R = C12, C14, C16, and R’ = methyl or benzyl substituent. The intercalation efficiency was examined by X-ray diffraction, CHN elemental analysis, and Fourier transform infrared (FTIR) spectroscopy. Textural studies have shown that the application of freezing in liquid nitrogen and freeze-drying after the intercalation increases the specific surface area and the total pore volume of organo-Mt. The polymer matrix was a poly(methylhydrosiloxane) cross-linked with two linear vinylsiloxanes of different siloxane chain lengths between end functional groups. X-ray diffraction and transmission electron microscopy studies have shown that the increase in d-spacing of organo-Mt and the benzyl substituent influence the degree of nanofillers’ exfoliation in the nanocomposites. The increase in the degree of organo-Mt exfoliation reduces the efficiency of hydrosilylation reaction monitored by FTIR. This was due to physical hindrance induced by exfoliated Mt particles.


Author(s):  
Tianlei Ma ◽  
Marek Nikiel ◽  
Andrew G. Thomas ◽  
Mohamed Missous ◽  
David J. Lewis

AbstractIn this report, we prepared transparent and conducting undoped and molybdenum-doped tin oxide (Mo–SnO2) thin films by aerosol-assisted chemical vapour deposition (AACVD). The relationship between the precursor concentration in the feed and in the resulting films was studied by energy-dispersive X-ray spectroscopy, suggesting that the efficiency of doping is quantitative and that this method could potentially impart exquisite control over dopant levels. All SnO2 films were in tetragonal structure as confirmed by powder X-ray diffraction measurements. X-ray photoelectron spectroscopy characterisation indicated for the first time that Mo ions were in mixed valence states of Mo(VI) and Mo(V) on the surface. Incorporation of Mo6+ resulted in the lowest resistivity of $$7.3 \times 10^{{ - 3}} \Omega \,{\text{cm}}$$ 7.3 × 10 - 3 Ω cm , compared to pure SnO2 films with resistivities of $$4.3\left( 0 \right) \times 10^{{ - 2}} \Omega \,{\text{cm}}$$ 4.3 0 × 10 - 2 Ω cm . Meanwhile, a high transmittance of 83% in the visible light range was also acquired. This work presents a comprehensive investigation into impact of Mo doping on SnO2 films synthesised by AACVD for the first time and establishes the potential for scalable deposition of SnO2:Mo thin films in TCO manufacturing. Graphical abstract


Crystals ◽  
2021 ◽  
Vol 11 (3) ◽  
pp. 313
Author(s):  
Mohamad M. Ahmad ◽  
Hicham Mahfoz Kotb ◽  
Celin Joseph ◽  
Shalendra Kumar ◽  
Adil Alshoaibi

La2/3Cu3Ti4O12 (LCTO) powder has been synthesized by the mechanochemical milling technique. The pelletized powder was conventionally sintered for 10 h at a temperature range of 975–1025 °C, which is a lower temperature process compared to the standard solid-state reaction. X-ray diffraction analysis revealed a cubic phase for the current LCTO ceramics. The grain size of the sintered ceramics was found to increase from 1.5 ± 0.5 to 2.3 ± 0.5 μm with an increase in sintering temperature from 975 to 1025 °C. The impedance results show that the grain conductivity is more than three orders of magnitude larger than the grain boundary conductivity for LCTO ceramics. All the samples showed a giant dielectric constant (1.7 × 103–3.4 × 103) and dielectric loss (0.09–0.17) at 300 K and 10 kHz. The giant dielectric constant of the current samples was attributed to the effect of internal barrier layer capacitances due to their electrically inhomogeneous structure.


Surfaces ◽  
2021 ◽  
Vol 4 (2) ◽  
pp. 106-114
Author(s):  
Yannick Hermans ◽  
Faraz Mehmood ◽  
Kerstin Lakus-Wollny ◽  
Jan P. Hofmann ◽  
Thomas Mayer ◽  
...  

Thin films of ZnWO4, a promising photocatalytic and scintillator material, were deposited for the first time using a reactive dual magnetron sputtering procedure. A ZnO target was operated using an RF signal, and a W target was operated using a DC signal. The power on the ZnO target was changed so that it would match the sputtering rate of the W target operated at 25 W. The effects of the process parameters were characterized using optical spectroscopy, X-ray diffraction, and scanning electron microscopy, including energy dispersive X-ray spectroscopy as well as X-ray photoelectron spectroscopy. It was found that stoichiometric microcrystalline ZnWO4 thin films could be obtained, by operating the ZnO target during the sputtering procedure at a power of 55 W and by post-annealing the resulting thin films for at least 10 h at 600 °C. As FTO coated glass substrates were used, annealing led as well to the incorporation of Na, resulting in n+ doped ZnWO4 thin films.


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