scholarly journals Impact of high temperatures on aluminoceladonite studied by Mössbauer, Raman, X-ray diffraction and X-ray photoelectron spectroscopy

2021 ◽  
Author(s):  
Mariola Kądziołka-Gaweł ◽  
Maria Czaja ◽  
Mateusz Dulski ◽  
Tomasz Krzykawski ◽  
Magdalena Szubka
Keyword(s):  
Photoelectron Spectroscopy ◽  
Integral Intensity ◽  
Photoelectron Spectra ◽  
X Ray Diffraction ◽  
Structural Reorganization ◽  
Oh Groups ◽  
X Ray ◽  
Al Content ◽  
Integral Intensity Ratio ◽  
Higher Temperature

AbstractMössbauer, Raman, X-ray diffraction and X-ray photoelectron spectroscopies were used to examine the effects of temperature on the structure of two aluminoceladonite samples. The process of oxidation of Fe2+ to Fe3+ ions started at about 350 °C for the sample richer in Al and at 300 °C for the sample somewhat lower Al-content. Mössbauer results show that this process may be associated with dehydroxylation or even initiate it. The first stage of dehydroxylation takes place at a temperature > 350 °C when the adjacent OH groups are replaced with a single residual oxygen atom. Up to ~500 °C, Fe ions do not migrate from cis-octahedra to trans-octahedra sites, but the coordination number of polyhedra changes from six to five. This temperature can be treated as the second stage of dehydroxylation. The temperature dependence on the integral intensity ratio between bands centered at ~590 and 705 cm−1 (I590/I705) clearly reflects the temperature at which six-coordinated polyhedra are transformed into five-coordinated polyhedra. X-ray photoelectron spectra obtained in the region of the Si2p, Al2p, Fe2p, K2p and O1s core levels, highlighted a route to identify the position of Si, Al, K and Fe cations in a structure of layered silicates with temperature. All the measurements show that the sample with a higher aluminum content and a lower iron content in octahedral sites starts to undergo a structural reorganization at a relatively higher temperature than the less aluminum-rich sample does. This suggests that iron may perform an important role in the initiation of the dehydroxylation of aluminoceladonites.

Large-scale and facile fabrication of PbSe nanostructures by selenization of a Pb sheet

2015 ◽  
Vol 08 (05) ◽  
pp. 1550063 ◽  
Author(s):  
Sara Hoomi ◽  
Ramin Yousefi ◽  
Farid Jamali-Sheini ◽  
Abdolhossein Sáaedi ◽  
Mohsen Cheraghizade ◽  
...  
Keyword(s):  
Large Scale ◽  
Chemical Vapor ◽  
Infrared Region ◽  
Photoelectron Spectra ◽  
X Ray Diffraction ◽  
X Ray ◽  
Facile Fabrication ◽  
Higher Temperature ◽  
Set Up ◽  
Lower Temperature

PbSe nanostructures were synthesized by selenization of lead sheets in a chemical vapor deposition (CVD) set-up under a selenium ambiance. The lead sheets were placed in the different temperature zones, between 300°C and 450°C. Field emission scanning electron microscope (FESEM) images showed that, PbSe nanostructures grown on the lead sheets with different morphologies. PbSe nanostructures with flakes shape were grown on the lead sheets that were placed in the lower temperature, while PbSe nanocubes and nanorods, which were grown on the nanocubes, were grown on the lead sheets in the higher temperature. The phase and composition of the product were identified by X-ray diffraction (XRD) pattern and X-ray photoelectron spectra (XPS). The XRD and XPS results showed that, the PbSe phase was started to form after 350°C and completed at 450°C. However, the XPS results showed that the Se concentration was different in the samples. In addition, Raman measurements confirmed the XRD and XPS results and indicated three Raman active modes, which belonged to PbSe phase for the nanostructures. The optical properties of the products were characterized by UV–Vis. The optical characterization results showed a band gap for the PbSe nanostructures in the infrared region.

scholarly journals Green synthesis and characterization of cuprous oxide nanoparticles in presence of a bio-surfactant

2014 ◽  
Vol 32 (4) ◽  
pp. 702-708 ◽  
Author(s):  
M. Behera ◽  
G. Giri
Keyword(s):  
Green Synthesis ◽  
Photoelectron Spectroscopy ◽  
Broad Band ◽  
X Ray Diffraction ◽  
Oh Groups ◽  
X Ray ◽  
Transmission Electron ◽  
Fcc Lattice ◽  
Perennial Shrub ◽  
A Charge

AbstractHerein, we report a facile green synthesis of Cu2O nanoparticles (NPs) using copper sulfate as precursor salt and hydrazine hydrate as reducing agent in presence of bio-surfactant (i.e. leaves extract of arka — a perennial shrub) at 60 to 70 °C in an aqueous medium. A broad band centered at 460 nm in absorption spectrum reveals the formation of surfactant stabilized Cu2O NPs. X-ray diffraction pattern of the surfactant stabilized NPs suggests the formation of only Cu2O phase in assistance of a bio-surfactant with the crystallite size of ∼8 nm. A negative zeta potential of −12 mV at 8.0 pH in surfactant stabilized Cu2O NPs hints non-bonding electron transfer from O-atom of saponin to the surface of NP. Red-shift in the vibrational band (Cu-O stretching) of Cu2O from 637 cm−1 to 640 cm−1 in presence of bio-surfactant suggests an interfacial interaction between NPs and O-atoms of -OH groups of saponin present in the plant (i.e. Calotropis gigantean) extract. From X-ray photoelectron spectroscopy spectra, a decrease in binding energy of both 2p3/2 and 2p1/2 bands in Cu2O with saponin molecules as compared to bulk Cu atom reveals a charge transfer interaction between NP and saponin surfactant molecules. Transmission electron microscopy images show crystalline nature of Cu2O NPs with an fcc lattice.

Synthesis of Ferromagnetic Germanides in 40Ge/60Mn Films: Magnetic and Structural Properties

2014 ◽  
Vol 215 ◽  
pp. 167-172
Author(s):  
Victor G. Myagkov ◽  
A.A. Matsunin ◽  
Y.L. Mikhlin ◽  
Victor S. Zhigalov ◽  
Liudmila E. Bykova ◽  
...  
Keyword(s):  
Solid State ◽  
Curie Temperature ◽  
Photoelectron Spectroscopy ◽  
Magnetic Measurements ◽  
Atomic Ratio ◽  
Photoelectron Spectra ◽  
Solid State Reactions ◽  
Ferromagnetic Phase ◽  
X Ray Diffraction ◽  
X Ray

Solid-state reactions between Ge and Mn films are systematically examined using X-ray diffraction, photoelectron spectroscopy and magnetic measurements. The films have a nominal atomic ratio Ge:Mn = 40:60 and are investigated at temperatures from 50 to 500 °С. It is established that after annealing at ~120 °С, the ferromagnetic Mn5Ge3 phase is the first phase to form at the 40Ge/60Mn interface. Increasing the annealing temperature to 500 °С leads to the formation of the ferromagnetic phase with a Curie temperature TC ~ 360 K and magnetization MS ~ 140-200 emu/cc at room temperature. Analysis of X-ray diffraction patterns and the photoelectron spectra suggests that the increased Curie temperature and magnetization are related to the migration of C and O atoms into the Mn5Ge3 lattice and the formation of the Nowotny phase Mn5Ge3СxOy. The initiation temperature (~120 °С) of the Mn5Ge3 phase is the same both for solid-state reactions in Ge/Mn films, as well as for phase separation in GexMn1-x diluted semiconductors. We conclude that the synthesis of the Mn5Ge3 phase is the moving force for the spinodal decomposition of the GexMn1-x diluted semiconductors.

EVIDENCE OF POLARIZATION SWITCHING INDUCED BY MAGNETIC FIELD IN BiFeO3 THIN FILM

2013 ◽  
Vol 27 (11) ◽  
pp. 1350077
Author(s):  
J. N. WANG ◽  
W. L. LI ◽  
X. L. LI ◽  
W. D. FEI
Keyword(s):  
Magnetic Field ◽  
Thin Film ◽  
Domain Switching ◽  
Integral Intensity ◽  
Film Surface ◽  
Residual Tensile Stress ◽  
X Ray Diffraction ◽  
X Ray ◽  
Integral Intensity Ratio ◽  
The Magnetic Field

A BiFeO 3 thin film was prepared on the (111) Pt / Ti / SiO 2/ Si substrate by the solution coating method. In order to detect the effect of an external magnetic field on the BiFeO 3 thin film, a fine scan X-ray diffraction with a scan ratio of 0.002°/s was carried out under the magnetic field parallel to the film surface. The result of the in situ analysis of X-ray diffraction for the thin film in the magnetic field indicates that the magnetic field leads to an increase of the integral intensity ratio of [Formula: see text] compared with that under no magnetic field. The increase of [Formula: see text] implies a domain switching under the magnetic field, where the domain switching comes from the decreasing residual tensile stress induced by the magnetostriction of BiFeO 3 in the magnetic field.

Structural and Band-Edge Properties of Cu(AlxIn1-X)S2 (0≤x≤1) Series Chalcopyrite Semiconductors

2012 ◽  
Vol 194 ◽  
pp. 133-138 ◽  
Author(s):  
Ching Hwa Ho ◽  
Chia Chi Pan ◽  
Jian Rong Cai ◽  
Guan Tzu Huang ◽  
Dumitru O. Dumcenco ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Photoelectron Spectroscopy ◽  
Measurement Techniques ◽  
X Ray Diffraction ◽  
Valence Band Structure ◽  
X Ray ◽  
Al Content ◽  
Chalcopyrite Semiconductors ◽  
Structural And Electronic Properties ◽  
Enhanced Strain

We have demonstrated structural and electronic properties of a series solar energy crystals Cu(AlxIn1-x)S2 (0<=x<=1) by using measurement techniques of X-ray diffraction, polarized thermoreflectance (PTR), and X-ray photoelectron spectroscopy (XPS). Single crystals of Cu(AlxIn1-x)S2 (0<=x<=1) (0 and E ^ polarizations. The PTR spectra clearly showed that the energy value of D increases with the increase of Al content x in the Cu(AlxIn1-x)S2 (0<=x<=1) series due to the enhanced strain in the lattice. The composition-dependent crystal-field-splitting energies can be evaluated and determined to be D(x)= (10±2)+( 139±5)×x meV. Based on the experimental analyses, the crystal structure and valence-band structure of the Cu(AlxIn1-x)S2 (0<=x<=1) (0<=x<=1) series are thus realized.

scholarly journals Magnetron-Sputtered Ni-Cr and Ti-Si Layers to Protect Ti-46Al-8Nb (at.%) Substrates Against Gas Absorption

2019 ◽  
Vol 28 (10) ◽  
pp. 6258-6267
Author(s):  
Marzena Mitoraj-Królikowska ◽  
Elzbieta Godlewska
Keyword(s):  
Mechanical Properties ◽  
Cross Sections ◽  
Photoelectron Spectroscopy ◽  
Analytical Techniques ◽  
Gas Absorption ◽  
X Ray Diffraction ◽  
Surface Layers ◽  
Surface Protection ◽  
X Ray ◽  
Higher Temperature

Abstract Ni-Cr and Ti-Si layers were deposited by magnetron sputtering on Ti-46Al-8Nb (at.%) substrates to suppress penetration of gases, which brings about undesirable changes in mechanical properties. Alloy samples with and without surface protection were subjected to interrupted oxidation at elevated temperature (700 and 800 °C) for up to 300 h. Selected mechanical properties as well as adhesion of surface layers were examined in the as-received and oxidized state. Analytical techniques used to characterize surfaces and cross sections of the samples included scanning electron microscopy and light microscopy, energy-dispersive x-ray spectroscopy, x-ray photoelectron spectroscopy and x-ray diffraction. Both investigated layers were sufficiently adherent and effective in hindering gas absorption at 700 °C; however, only Ni-Cr showed promising properties for higher-temperature applications.

Tribological Behavior of CrN and Al-Cr-N Coatings

2008 ◽  
Author(s):  
Nicholaos G. Demas ◽  
Andreas A. Polycarpou ◽  
Kyriaki Polychronopoulou ◽  
Claus Rebholz
Keyword(s):  
Photoelectron Spectroscopy ◽  
Tribological Behavior ◽  
Electron Beam Evaporation ◽  
X Ray Diffraction ◽  
X Ray ◽  
Mechanical And Tribological Properties ◽  
Al Content ◽  
Composition Structure ◽  
Crn Coatings ◽  
Ball On Disc

The tribological behavior of CrN and Al-Cr-N coatings prepared by twin electron-beam evaporation at 450°C was investigated. The composition, structure, mechanical and tribological properties of the coatings were determined using X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD) in combination with nanoindentation mechanical property measurements, scanning electron microscopy (SEM), and laboratory controlled ball-on-disc sliding experiments. It was found that all of the Al-Cr-N coatings exhibit higher hardness compared to CrN coatings. Also, the compositions of Al-Cr-N coatings with the lower Al content and lower Al/Cr ratios showed better tribological performance than the rest of the coatings.

Investigation of the Effect of Uv-Assisted Oxidation and Nitridation of Hafnium Metal Films

2003 ◽  
Vol 780 ◽  
Author(s):  
C. Essary ◽  
V. Craciun ◽  
J. M. Howard ◽  
R. K. Singh
Keyword(s):  
Uv Radiation ◽  
Photoelectron Spectroscopy ◽  
Grazing Angle ◽  
X Ray Diffraction ◽  
Metal Thin Films ◽  
X Ray ◽  
Force Microscopy ◽  
Si Substrates ◽  
Atomic Force ◽  
Silicon Interface

AbstractHf metal thin films were deposited on Si substrates using a pulsed laser deposition technique in vacuum and in ammonia ambients. The films were then oxidized at 400 °C in 300 Torr of O2. Half the samples were oxidized in the presence of ultraviolet (UV) radiation from a Hg lamp array. X-ray photoelectron spectroscopy, atomic force microscopy, and grazing angle X-ray diffraction were used to compare the crystallinity, roughness, and composition of the films. It has been found that UV radiation causes roughening of the films and also promotes crystallization at lower temperatures.Furthermore, increased silicon oxidation at the interface was noted with the UVirradiated samples and was shown to be in the form of a mixed layer using angle-resolved X-ray photoelectron spectroscopy. Incorporation of nitrogen into the film reduces the oxidation of the silicon interface.

scholarly journals Modification of Wood with Monoethanolamino-borate by The Data of X-Ray Photoelectron Spectroscopy

2018 ◽  
Vol 196 ◽  
pp. 04005
Author(s):  
Irina Stepina ◽  
Irina Kotlyarova
Keyword(s):  
Particle Size ◽  
Photoelectron Spectroscopy ◽  
Model Compound ◽  
Hydrolytic Stability ◽  
Photoelectron Spectra ◽  
Wood Cellulose ◽  
Rapid Loss ◽  
X Ray ◽  
Wood Protection ◽  
Cellulose Materials

The difficulty of wood protection from biocorrosion and fire is due to the fact that modifiers in use are washed out from the surface of the substrate under the influence of environmental factors. This results in a rapid loss of the protective effect and other practically important wood characteristics caused by the modification. To solve this problem is the aim of our work. Here, monoethanolaminoborate is used as a modifier, where electron-donating nitrogen atom provides a coordination number equal to four to a boron atom, which determines the hydrolytic stability of the compounds formed. Alpha-cellulose ground mechanically to a particle size of 1 mm at most was used as a model compound for the modification. X-ray photoelectron spectra were recorded on the XSAM-800 spectrometer (Kratos, UK). Prolonged extraction of the modified samples preceded the registration of the photoelectron spectra to exclude the fixation of the modifier molecules unreacted with cellulose. As a result of the experiment, boron and nitrogen atoms were found in the modified substrate, which indicated the hydrolytic stability of the bonds formed between the modifier molecules and the substrate. Therefore monoethanolaminoborate can be considered as a non-extractable modifier for wood-cellulose materials.

scholarly journals α-Cellulose Fibers of Paper-Waste Origin Surface-Modified with Fe3O4 and Thiolated-Chitosan for Efficacious Immobilization of Laccase

Polymers ◽  
2021 ◽  
Vol 13 (4) ◽  
pp. 581
Author(s):  
Gajanan S. Ghodake ◽  
Surendra K. Shinde ◽  
Ganesh D. Saratale ◽  
Rijuta G. Saratale ◽  
Min Kim ◽  
...  
Keyword(s):  
Enzyme Immobilization ◽  
Photoelectron Spectroscopy ◽  
Cellulose Fibers ◽  
Relative Activity ◽  
Significant Activity ◽  
X Ray Diffraction ◽  
X Ray ◽  
Transmission Electron ◽  
Laccase Immobilization ◽  
Surface Modified

The utilization of waste-paper-biomass for extraction of important α-cellulose biopolymer, and modification of extracted α-cellulose for application in enzyme immobilization can be extremely vital for green circular bio-economy. Thus, in this study, α-cellulose fibers were super-magnetized (Fe3O4), grafted with chitosan (CTNs), and thiol (-SH) modified for laccase immobilization. The developed material was characterized by high-resolution transmission electron microscopy (HR-TEM), HR-TEM energy dispersive X-ray spectroscopy (HR-TEM-EDS), X-ray diffraction (XRD), vibrating sample magnetometer (VSM), X-ray photoelectron spectroscopy (XPS), and Fourier transform infrared spectroscopy (FT-IR) analyses. Laccase immobilized on α-Cellulose-Fe3O4-CTNs (α-Cellulose-Fe3O4-CTNs-Laccase) gave significant activity recovery (99.16%) and laccase loading potential (169.36 mg/g). The α-Cellulose-Fe3O4-CTNs-Laccase displayed excellent stabilities for temperature, pH, and storage time. The α-Cellulose-Fe3O4-CTNs-Laccase applied in repeated cycles shown remarkable consistency of activity retention for 10 cycles. After the 10th cycle, α-Cellulose-Fe3O4-CTNs possessed 80.65% relative activity. Furthermore, α-Cellulose-Fe3O4-CTNs-Laccase shown excellent degradation of pharmaceutical contaminant sulfamethoxazole (SMX). The SMX degradation by α-Cellulose-Fe3O4-CTNs-Laccase was found optimum at incubation time (20 h), pH (3), temperatures (30 °C), and shaking conditions (200 rpm). Finally, α-Cellulose-Fe3O4-CTNs-Laccase gave repeated degradation of SMX. Thus, this study presents a novel, waste-derived, highly capable, and super-magnetic nanocomposite for enzyme immobilization applications.

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