Surface Characterization of Carbon-Bearing Magnetite (CBM) and Carbon-Bearing Ni(II)-Ferrite (CBNF)

1994 ◽  
Vol 344 ◽  
Author(s):  
T. Sano ◽  
K. Akanuma ◽  
M. Tsuji ◽  
Y. Tamaura
Keyword(s):  
Photoelectron Spectroscopy ◽  
Spinel Structure ◽  
Surface Characterization ◽  
Carbon Deposition ◽  
X Ray Diffraction ◽  
Xps Spectra ◽  
X Ray ◽  
Oxygen Ions ◽  
Diffraction Patterns

AbstractOxygen-deficient magnetite (ODM; Fe3O4-δ, δ>0) synthesized by reduction of magnetite with H2 at 300°C decomposed CO2 to carbon with an efficiency of nearly 100% at 300°C. In this reaction, two oxygen ions of the CO2 were incorporated into the spinel structure of ODM and carbon was deposited on the surface of ODM with zero valence to form visible particles. The particles of carbon separated from ODM were studied by Raman, energy-dispersive X-ray and wave-dispersive X-ray spectroscopies. The carbon which had been deposited on the ODM was found to be a mixture of graphite and amorphous carbon in at least two levels of crystallization. X-ray photoelectron spectroscopy and X-ray diffraction patterns of the carbon-bearing magnetite (CBM) showed no indication of carbide (Fe3C) or metallic iron (α-Fe) phase formation. In the C 1s XPS spectra of the CBM, no peaks were observed which could be assigned to CO2 or CO. X-ray diffractometry, chemical analysis and TG-MS measurement showed that the carbon-bearing Ni(II)-ferrite (CBNF) (Ni(II)/Fetotal = 0.15) synthesized by the carbon deposition reaction from CO2 with the H2-reduced Ni(II)-ferrite was represented by (Ni0.28Fe2.72O4.00)1-δ (Ni2+06.9Fe2+2.31O3.00)δCτ (δ= 0.27, τ= 0.17). The carbon of the CBNF gave the CIOlayer-like oxide containing some Ni2+ ions.

scholarly journals PECHINI SYNTHESIS AND CHARACTERIZATION OF Eu3+ DOPED ZnCo2O4 SPINELS

2005 ◽  
Vol 03 (2) ◽  
pp. 24-29
Author(s):  
P.M. PIMENTEL ◽  
A.M.G. PEDROSA ◽  
H.K.S. SOUZA ◽  
C.N.S. JÚNIOR ◽  
R.C.A. PINTO ◽  
...  
Keyword(s):  
Spinel Structure ◽  
Pechini Method ◽  
Synthesis Temperature ◽  
X Ray Diffraction ◽  
X Ray ◽  
Spinel Oxides ◽  
Diffraction Patterns ◽  
Pechini Synthesis ◽  
Spinel Structures

Spinel oxides with the composition ZnCo2O4 and ZnCo2O4:Eu3+ have been synthesized by the Pechini method and characterized by X-ray diffraction, infrared spectroscopy, thermal analysis and scanning electron microscopy. IR spectroscopy revealed the presence of n1 and n2 bands, typical of spinel structures. The formation of monophase cubic spinel structure was confirmed by X-ray diffraction patterns. Extra lines corresponding to other phase has been observed in the powders calcined at 900 ºC. The results showed the extremely lower synthesis temperature than those presents in conventional methods.

scholarly journals A multi-method characterization of natural terrestrial birnessites

2020 ◽  
Vol 105 (6) ◽  
pp. 833-847
Author(s):  
Florence T. Ling ◽  
Jeffrey E. Post ◽  
Peter J. Heaney ◽  
Cara M. Santelli ◽  
Eugene S. Ilton ◽  
...  
Keyword(s):  
Photoelectron Spectroscopy ◽  
Large Set ◽  
X Ray Diffraction ◽  
Full Spectrum ◽  
X Ray ◽  
High Concentrations ◽  
Diffraction Patterns ◽  
X Ray Absorption ◽  
Crystal Structure And Chemistry

Abstract With a focus on a large set of natural birnessites collected from terrestrial, freshwater systems, we applied and compared the capabilities of X-ray diffraction (XRD), extended X-ray absorption fine structure (EXAFS), Fourier-transform infrared spectroscopy (FTIR), and X-ray photoelectron spectroscopy (XPS) to characterize crystal structure and chemistry. Using XRD, we successfully identified 3 of the 11 natural birnessite samples as hexagonal ranciéite-like phases, but the remaining samples yielded less interpretable “3-line” diffraction patterns with broad, asymmetrical peaks at d-spacings of ~7.2, ~2.4, and ~1.4 Å. EXAFS analysis suggested that many of these samples had characteristics of both triclinic and hexagonal birnessite. However, application of EXAFS to the ranciéite-like phases yielded unreasonably high concentrations of triclinic birnessite as an intergrowth, calling into question the use of synthetic hexagonal H-birnessite as an appropriate standard in the linear combination fitting of EXAFS data for natural birnessites. FTIR spectroscopy of the “3-line” birnessite samples successfully distinguished triclinic and hexagonal constituents, and analyses of peak positions suggested that natural birnessites occur as a full spectrum of triclinic and hexagonal intergrowths. XPS analysis of these samples revealed that higher Mn3+ concentrations relative to Mn2+ and Mn4+ are correlated to increased proportions of triclinic birnessite.

CO2 Adsorption Performance of N-Doped Ordered Microporous Carbons Templated from Zeolite HY

2011 ◽  
Vol 284-286 ◽  
pp. 2102-2105 ◽  
Author(s):  
Jin Zhou ◽  
Wen Li ◽  
Shu Ping Zhuo
Keyword(s):  
Photoelectron Spectroscopy ◽  
Carbon Deposition ◽  
X Ray Diffraction ◽  
Step Method ◽  
X Ray ◽  
Microporous Carbons ◽  
Adsorption Performance ◽  
Basic Nitrogen ◽  
Diffraction Patterns ◽  
Very High

Several microporous carbons were prepared by a two-step method using zeolite HY as a template, and were used as CO2 adsorbents. X-ray diffraction patterns present that the structure regularity of the zeolite has been well-replicated by the templated carbons. X-ray photoelectron spectroscopy confirms that the prepared carbons possess abundant nitrogen-containing groups due to the carbon deposition of acetonitrile. The prepared carbons show high CO2 adsorption capacity due to its very high microporous surface area and abundant basic nitrogen-containing groups.

scholarly journals Calcined Co(II)-Triethylenetetramine, Co(II)- Polyaniline-Thiourea as the Cathode Catalyst of Proton Exchanged Membrane Fuel Cell

Polymers ◽  
2020 ◽  
Vol 12 (12) ◽  
pp. 3070
Author(s):  
Wen-Yao Huang ◽  
Li-Cheng Jheng ◽  
Tar-Hwa Hsieh ◽  
Ko-Shan Ho ◽  
Yen-Zen Wang ◽  
...  
Keyword(s):  
Photoelectron Spectroscopy ◽  
Linear Sweep Voltammetry ◽  
Conducting Medium ◽  
Membrane Electrode ◽  
X Ray Diffraction ◽  
Xps Spectra ◽  
X Ray ◽  
Co Catalysts ◽  
Electrode Assemblies ◽  
Diffraction Patterns

Triethylenetetramine (TETA) and thiourea complexed Cobalt(II) (Co(II)) ions are used as cathode catalysts for proton exchanged membrane fuel cells (PEMFCs) under the protection of polyaniline (PANI) which can become a conducting medium after calcination. Fourier-transform infrared spectroscopy (FTIR) and X-ray photoelectron spectroscopy (XPS) spectra clearly reveal the presence of typical carbon nitride and sulfide bonds of the calcined Nitrogen (N)- or Sulfur (S)-doped co-catalysts. Clear (002) and (100) planes of carbon-related X-ray diffraction patterns are found for co-catalysts after calcination, related to the formation of a conducting medium after the calcination of PANI. An increasing intensity ratio of the D to G band of the Raman spectra reveal the doping of N and S elements. More porous surfaces of co-catalysts are found in scanning electronic microscopy (SEM) micropictures when prepared in the presence of both TETA and thiourea (CoNxSyC). Linear sweep voltammetry (LSV) curves show the highest reducing current to be 4 mAcm−2 at 1600 rpm for CoNxSyC, indicating the necessity for both N- and S-doping. The membrane electrode assemblies (MEA) prepared with the cathode made of CoNxSyC produces the highest maximum power density, close to 180 mW cm−2.

Surface Characterization of Calcium-Stabilized Zirconia Film by X-Ray Photoelectron Spectroscopy

1997 ◽  
Vol 495 ◽  
Author(s):  
E. O. Bensadon ◽  
P. A. P. Nascente ◽  
L.O.S. Bulhões ◽  
E. C. Pereira
Keyword(s):  
Photoelectron Spectroscopy ◽  
Surface Characterization ◽  
Oxide Films ◽  
Depth Profiling ◽  
Cubic Phase ◽  
X Ray Diffraction ◽  
Stabilized Zirconia ◽  
X Ray ◽  
Zirconia Film

ABSTRACTA new methodology was developed to stabilized zirconia films at room temperature. The zirconium oxide films were prepared electrochemically by anodic oxidation of metallic zirconium at constant curcent density. X-ray diffraction (XRD) revealed the partial stabilization of the cubic phase in the ZrO2 films obtained in the presence of calcium. On the other hand, the films obtained in H3PO4 presented monoclinic phase. Scanning electron microscopy (SEM) showed that the oxide films obtained in calcium medium were porous, while the films obtained in H3PO4 were compact. X-ray photoelectron spectroscopy (XPS) identified ZrO2 and the intercalation of Na, N, P and CaO, as well as adventitious carbon. Using depth profiling, we observed that the concentrations of ZrO2, P and CaO increased with sputtering time.

The Use of Advanced Analytical Techniques for Characterization of the Chemical, Physical, and Crystallographic Nature of a Surface

1973 ◽  
Vol 31 ◽  
pp. 132-133 ◽  
Author(s):  
R. E. Herfert
Keyword(s):  
Surface Characterization ◽  
Analytical Techniques ◽  
X Ray Diffraction ◽  
Depth Of Penetration ◽  
X Ray ◽  
The Past ◽  
Transmission Electron ◽  
Scanning Electron

Studies of the nature of a surface, either metallic or nonmetallic, in the past, have been limited to the instrumentation available for these measurements. In the past, optical microscopy, replica transmission electron microscopy, electron or X-ray diffraction and optical or X-ray spectroscopy have provided the means of surface characterization. Actually, some of these techniques are not purely surface; the depth of penetration may be a few thousands of an inch. Within the last five years, instrumentation has been made available which now makes it practical for use to study the outer few 100A of layers and characterize it completely from a chemical, physical, and crystallographic standpoint. The scanning electron microscope (SEM) provides a means of viewing the surface of a material in situ to magnifications as high as 250,000X.

scholarly journals Optical, XPS and XRD Studies of Semiconducting Copper Sulfide Layers on a Polyamide Film

2009 ◽  
Vol 2009 ◽  
pp. 1-8 ◽  
Author(s):  
Valentina Krylova ◽  
Mindaugas Andrulevičius
Keyword(s):  
Photoelectron Spectroscopy ◽  
Copper Sulfide ◽  
Diffusion Method ◽  
X Ray Diffraction ◽  
Xps Spectra ◽  
X Ray ◽  
Xrd Studies ◽  
Polyamide Film ◽  
Indirect Band Gap ◽  
Xrd Method

Copper sulfide layers were formed on polyamide PA 6 surface using the sorption-diffusion method. Polymer samples were immersed for 4 and 5 h in 0.15 mol⋅  solutions and acidified with HCl (0.1 mol⋅) at . After washing and drying, the samples were treated with Cu(I) salt solution. The samples were studied by UV/VIS, X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) methods. All methods confirmed that on the surface of the polyamide film a layer of copper sulfide was formed. The copper sulfide layers are indirect band-gap semiconductors. The values of are 1.25 and 1.3 eV for 4 h and 5 h sulfured PA 6 respectively. Copper XPS spectra analyses showed Cu(I) bonds only in deeper layers of the formed film, while in sulfur XPS S 2p spectra dominating sulfide bonds were found after cleaning the surface with ions. It has been established by the XRD method that, beside , the layer contains as well. For PA 6 initially sulfured 4 h, grain size forchalcocite, , was  nm and fordjurleite, , it was 54.17 nm. The sheet resistance of the obtained layer varies from 6300 to 102 .

Preparation and Application of Lead Dioxide Electrode for Zinc Electrolysis

2013 ◽  
Vol 785-786 ◽  
pp. 1125-1129
Author(s):  
Xiao Yong Yang ◽  
Pei Xian Zhu ◽  
Yun Sen Si
Keyword(s):  
Surface Characterization ◽  
Catalytic Properties ◽  
Lead Dioxide ◽  
Manufacturing Cost ◽  
X Ray Diffraction ◽  
Simulation Test ◽  
X Ray ◽  
Zinc Smelter ◽  
Lead Dioxide Electrode

According to the process of anodic oxygen evolution in sulfate system for zinc electrolysis,Ti-base lead dioxide electrode can be prepared to use in this case.The surface characterization of the electrode was studied by Scanning electron microscopy(SEM) and X-ray diffraction(XRD).The electrode lifetime was tested in 1mol/L H2SO4solution at 60°C,and the electro-catalytic properties was examined by polarization curves.Then these samples was enlarged and simulation test was conducted at Mengzi marriage zinc smelter in Yunnan.The results show that the electro-catalytic properties is better and the electrodes lifetime is longer compared to the traditional lead electrode.Moreover,it has a significant effect in reducing energy consumption, manufacturing cost and improving the production and grade of zinc.

scholarly journals Fabrication and Characterization of Al/NiO Energetic Nanomultilayers

2015 ◽  
Vol 2015 ◽  
pp. 1-6 ◽  
Author(s):  
YiChao Yan ◽  
Wei Shi ◽  
HongChuan Jiang ◽  
Jie Xiong ◽  
WanLi Zhang ◽  
...  
Keyword(s):  
Photoelectron Spectroscopy ◽  
Total Thickness ◽  
X Ray Diffraction ◽  
Dc Magnetron Sputtering ◽  
Metallic Oxide ◽  
Promising Candidate ◽  
X Ray ◽  
Thermal Boundary Conductance ◽  
Fabrication And Characterization

The redox reaction between Al and metallic oxide has its advantage compared with intermetallic reaction and Al/NiO nanomutlilayers are a promising candidate for enhancing the performance of energetic igniter. Al/NiO nanomutlilayers with different modulation periods are prepared on alumina substrate by direct current (DC) magnetron sputtering. The thicknesses of each period are 250 nm, 500 nm, 750 nm, 1000 nm, and 1500 nm, respectively, and the total thickness is 3 μm. The X-ray diffraction (XRD) and scanning electron microscope (SEM) results of the as-deposited Al/NiO nanomutlilayers show that the NiO films are amorphous and the layered structures are clearly distinguished. The X-ray photoelectron spectroscopy (XPS) demonstrates that the thickness of Al2O3increases on the side of Al monolayer after annealing at 450°C. The thermal diffusion time becomes greater significantly as the amount of thermal boundary conductance across the interfaces increases with relatively smaller modulation period. Differential scanning calorimeter (DSC) curve suggests that the energy release per unit mass is below the theoretical heat of the reaction due to the nonstoichiometric ratio between Al and NiO and the presence of impurities.

Preparation and Characterization of γ-Fe2O3-ZnFe2O4 Composite Nanoparticles

2013 ◽  
Vol 873 ◽  
pp. 152-157
Author(s):  
Long Long Chen ◽  
Jun Ming Li ◽  
Xiao Min Gong ◽  
Jian Li
Keyword(s):  
Photoelectron Spectroscopy ◽  
Chemical Species ◽  
Composite Nanoparticles ◽  
X Ray Diffraction ◽  
Ferrite Core ◽  
Phase Synthesis ◽  
X Ray ◽  
Transmission Electron ◽  
Chemically Induced

Using a chemically induced transition in an FeCl2 solution, γ-Fe2O3 nanoparticles can be prepared from an amorphous precursor composed of FeOOH and Mg (OH)2. Surface modification by adding ZnCl2 during liquid-phase synthesis was attempted. The magnetization, morphology, crystal structure, and chemical species of as-prepared samples were characterized by vibrating sample magnetometer (VSM), transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray energy-dispersive spectroscopy (EDX), and X-ray photoelectron spectroscopy (XPS). The experimental results showed that the surface of the γ-Fe2O3 nanoparticles can be modified by adding ZnCl2 to form composite nanoparticles with a γ-Fe2O3/ZnFe2O4 ferrite core coated with Zn (OH)2 and absorbed FeCl36H2O; this modification can be enhanced by additional NaOH.

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