Search results for: x-ray photoelectron (XPS)

Authors: Marie Kudrnová, Jana Rejková

Abstract:

The samples of supplied INCONEL 601, 617, 625, and HASTELLOY C-22 alloys and experimental nickel alloy MoNiCr were examined by XPS (X-ray photoelectron spectroscopy) before and after exposure. The experiment was performed in a mixture of LiCl-KCl salt (58.2-41.8 wt. %). The exposure conditions were 440°C, pressure 0.2 MPa, 500 hours in an inert argon atmosphere. The XPS analysis shows that a thin oxide layer composed of metal oxides such as NiO, Cr₂O₃, and Nb₂O₅ was formed. After sputtering the exposed surface with Ar ions, metals were also detected in the elemental state, indicating a very thin protective oxide layer with a thickness in units of up to tens of nanometers.

Keywords: XPS, MSR, nickel alloy, metal oxides

Procedia PDF Downloads 47

Authors: Xingguo Feng, Hui Zhou, Kaifeng Zhang, Zhao Jiang, Hanjun Hu, Jun Zheng, Hong Hao

Abstract:

TiN and TiC films have been prepared on Ti6Al4V alloy substrates by plasma-based ion implantation. The effect of N+C and Ti+N hybrid ion implantation at 50 kV, and Ti+C hybrid ion implantation at 20 kV, 35 kV and 50 kV extraction voltages on mechanical properties at a dose of 2×10¹⁷ ions / cm² was studied. The chemical states and microstructures of the implanted samples were investigated using X-ray photoelectron (XPS), and X-ray diffraction (XRD), together with the mechanical and tribological properties of the samples were characterized using nano-indentation and ball-on-disk tribometer. It was found that the modified layer by Ti+C implanted at 50 kV was composed of mainly TiC and Ti-O bond and the layer of Ti+N implanted at 50 kV was observed to be TiN and Ti-O bond. Hardness tests have shown that the hardness values for N+C, Ti+N, and Ti+C hybrid ion implantation samples were much higher than the un-implanted ones. The results of wear tests showed that both Ti+C and Ti+N ion implanted samples had much better wear resistance compared un-implanted sample. The wear rate of Ti+C implanted at 50 kV sample was 6.7×10⁻⁵mm³ / N.m, which was decreased over one order than unimplanted samples.

Keywords: plasma ion implantation, x-ray photoelectron (XPS), hardness, wear

Procedia PDF Downloads 382

Authors: Marie Kudrnova, Jana Petru

Abstract:

This study is part of the international research - Materials for Molten Salt Reactors (MSR) and addresses the part of the project dealing with the corrosion behavior of candidate construction materials. Inconel 625 was characterized by x-ray photoelectron spectroscopy (XPS) before and after high–temperature experiment in molten salt. The experiment was performed in a horizontal tube furnace molten salt reactor, at 450 °C in argon, at atmospheric pressure, for 150 hours. Industrially produced HITEC salt was used (NaNO3, KNO3, NaNO2). The XPS study was carried out using the ESCAProbe P apparatus (Omicron Nanotechnology Ltd.) equipped with a monochromatic Al Kα (1486.6 eV) X-ray source. The surface layer on alloy 625 after exposure contains only Na, C, O, and Ni (as NiOx) and Nb (as NbOx BE 206.8 eV). Ni was detected in the metallic state (Ni0 – Ni 2p BE-852.7 eV, NiOx - Ni 2p BE-854.7 eV) after a short Ar sputtering because the oxide layer on the surface was very thin. Nickel oxides can form a protective layer in the molten salt, but only future long-term exposures can determine the suitability of Inconel 625 for MSR.

Keywords: Inconel 625, molten salt, oxide layer, XPS

Procedia PDF Downloads 121

Authors: Ruchi Jain, Chinnakonda S. Gopinath

Abstract:

The CO oxidation is a primary reaction in heterogeneous catalysis due to its potential to overcome the air pollution caused by various reasons. Indeed, in the study of sustainable catalysis, the role played by water is very important. The present work is focused on studying the effect of moisture on the sustainability of Co3O4 NR catalyst for CO oxidation reaction at ambient temperature. The catalytic activity, electronic structure and the mechanistic aspects of spinel Co3O4 nanorod surfaces have been explored in dry and wet atmosphere by near-ambient pressure photoelectron spectroscopic techniques (NAP-PES) with conventional x-ray (Al kα) and ultraviolet sources (He-I).Comparative NAPPES studies have been employed to understand the elucidation of the catalytic reaction pathway and the evolution of various surface species. The presence of water with CO+O2 plummet the catalytic activity due to the change in electronic nature from predominantly oxidic (without water in the feed) to few intermediates covered Co3O4 surface. However, ≥ 375 K Co3O4 surface recovers and regain oxidation activity, at least partially, even in the presence of water. Above mentioned observations are fully supported by the changes observed in the work function of Co3O4 in the presence of wet (H2O+CO+O2) compared to dry (CO+O2) conditions. Various type of surface species, such as CO(ads), carbonate, formate, are found to be on the catalyst surface depending on the reaction conditions. Under dry condition, CO couples with labile O atoms to form CO2, however under wet conditions it also interacts with surface OH groups results in the formation carbonate and formate intermediate. The carbonate acts at reaction inhibitor at room temperature, however proves as active intermediate at temperature 375 K or above. On the other hand, formate has proved to be reaction spectator due to its high stability. The intrinsic role of these species to suppress the oxidation has been demonstrated through a possible reaction mechanism under different reaction conditions.

Keywords: heterogeneous catalysis, surface chemistry, photoelectron spectroscopy, ambient oxidation

Procedia PDF Downloads 227

Authors: Hina Verma, Karine Le Guen, Renaud Dalaunay, Iyas Ismail, Vita Ilakovac, Jean Pascal Rueff, Yunlin Jacques Zheng, Philippe Jonnard

Abstract:

To the extent of our knowledge, X-ray emission spectroscopy (XES) has been applied in the soft x-ray region (photon energy ≤ 2 keV) to study the buried layers and interfaces of stacks of nanometer-thin films. Now we extend the methodology to study the buried interfaces in the hard X-ray region (i.e., ≥ five keV). The emission spectra allow us to study the interactions between elements in the buried layers from the analysis of their valence states, thereby providing sensitive information about the physical-chemical environment of the emitting element in multilayers. We exploit the chemical sensitivity of XES to study the interfaces between Fe and Si layers in the Fe/Si multilayer from the Fe Kβ₂,₅ emission spectra (7108 eV). The Fe Kβ₅ emission line results from the electronic transition from occupied 3d to 1s levels (i.e., valence to core transition) and is hence sensitive to the chemical state of emitting Fe atoms. The comparison of emission spectra recorded for Fe/Si multilayer with Fe and FeSi₂ references reveal the formation of FeSi₂ at the Fe-Si interfaces inside the multilayer stack. The interfacial thickness was calculated to be 1.4 ± 0.2 nm by taking into consideration the intensity of Fe atoms emitted from the interface and the Fe layer. The formation of FeSi₂ at the interface was further confirmed by the X-ray diffraction and X-ray photoelectron spectroscopy done on the Fe/Si multilayer. Hence, we can conclude that the XES in the hard X-ray range could be used to study multilayers and their interfaces and obtain information both qualitatively and quantitatively.

Keywords: buried interfaces, hard X-ray emission spectroscopy, X-ray diffraction, X-ray photoelectron spectroscopy

Procedia PDF Downloads 118

Authors: R. S. Yadav, J. Havlica, I. Kuřitka, Z. Kozakova, J. Masilko, L. Kalina, M. Hajdúchová, V. Enev, J. Wasserbauer

Abstract:

In this work, copper ferrite CuFe2O4 spinel ferrite nanoparticles with different particle size at different annealing temperature were synthesized using the starch-assisted sol-gel auto-combustion method. The synthesized nanoparticles were characterized by conventional powder X-ray diffraction (XRD) spectroscopy, Raman Spectroscopy, Fourier Transform Infrared Spectroscopy, Field-Emission Scanning Electron Microscopy, X-ray Photoelectron Spectroscopy, and Vibrating Sample Magnetometer. The XRD patterns confirmed the formation of CuFe2O4 spinel ferrite nanoparticles. Field-Emission Scanning Electron Microscopy revealed that particles are of spherical morphology with particle size 5-20 nm at lower annealing temperature. An infrared spectroscopy study showed the presence of two principal absorption bands in the frequency range around 530 cm-1 (ν1) and around 360 cm-1 (ν2); which indicate the presence of tetrahedral and octahedral group complexes, respectively, within the spinel ferrite nanoparticles. Raman spectroscopy study also indicated the change in octahedral and tetrahedral site related Raman modes in copper ferrite nanoparticles with change of particle size. This change in magnetic behavior with change of particle size of CuFe2O4 nanoparticles was also observed. The change in magnetic properties with change of particle size is due to cation redistribution, which was confirmed by X-Ray photoelectron study.

Keywords: copper ferrite, nanoparticles, magnetic property, CuFe2O4

Procedia PDF Downloads 417

Authors: Reza Vakili, Xiaolei Fan, Alex Walton

Abstract:

The first near ambient pressure (NAP)-XPS study of CO oxidation over Pt nanoparticles (NPs) incorporated into Zr-based UiO (UiO for Universitetet i Oslo) MOFs was carried out. For this purpose, the MOF-based Catalysts were prepared by wetness impregnation (WI-PtNPs@UiO-67) and linker design (LD-PtNPs@UiO-67) methods along with PtNPs@ZrO₂ as the control catalyst. Firstly, the as-synthesized catalysts were reduced in situ prior to the operando XPS analysis. The existence of Pt(II) species was proved in UiO-67 by observing Pt 4f core level peaks at a high binding energy of 72.6 ± 0.1 eV. However, by heating the WI-PtNPs@UiO-67 catalyst in situ to 200 °C under vacuum, the higher BE components disappear, leaving only the metallic Pt 4f doublet, confirming the formation of Pt NPs. The complete reduction of LD-PtNPs@UiO-67 is achieved at 250 °C and 1 mbar H₂. To understand the chemical state of Pt NPs in UiO-67 during catalytic turnover, we analyzed the Pt 4f region using operando NAP-XPS in the temperature-programmed measurements (100-260 °C) with reference to PtNPs@ZrO₂ catalyst. CO conversion during NAP-XPS experiments with the stoichiometric mixture shows that LD-PtNPs@UiO-67 has a better CO turnover frequency (TOF, 0.066 s⁻¹ at 260 °C) than the other two (ca. 0.055 s⁻¹). Pt 4f peaks only show one chemical species present at all temperatures, but the core level BE shifts change as a function of reaction temperature, i.e., Pt 4f peak from 71.8 eV at T < 200 °C to 71.2 eV at T > 200 °C. As this higher BE state of 71.8 eV was not observed after in situ reductions of the catalysts and only once the CO/O₂ mixture was introduced, we attribute it to the surface saturation of Pt NPs with adsorbed CO. In general, the quantitative analysis of Pt 4f data from the operando NAP-XPS experiments shows that the surface chemistry of the Pt active phase in the two PtNPs@UiO-67 catalysts is the same, comparable to that of PtNPs@ZrO₂. The observed difference in the catalytic activity can be attributed to the particle sizes of Pt NPs, as well as the dispersion of active phase in the support, which are different in the three catalysts.

Keywords: CO oxidation, heterogeneous catalysis, MOFs, Metal Organic Frameworks, NAP-XPS, Near Ambient Pressure X-ray Photoelectron Spectroscopy

Procedia PDF Downloads 109

Authors: Jose Alberto Duarte Moller, Cynthia Deisy Gomez Esparza

Abstract:

The cobalt-titanium system was grown as thin films in an INTERCOVAMEX V3 sputtering system, equipped with four magnetrons assisted by DC pulsed and direct DC. A polished highly oriented (400) silicon wafer was used as substrate and the growing temperature was 500 oC. Xray Absorption Spectroscopy experiments were carried out in the SSRL in the 4-3 beam line. The Extenden X-Ray Absorption Fine Structure spectra have been numerically processed by WINXAS software from the background subtraction until the normalization and FFT adjustment. Analyzing the absorption spectra of cobalt in the CoTi2 phase we can appreciate that they agree in energy with the reference spectra that corresponds to the CoO, which indicates that the valence where upon working is Co2+. The RDF experimental results were then compared with those RDF´s generated theoretically by using FEFF software, from a model compound of CoTi2 phase obtained by XRD. The fitting procedure is a highly iterative process. Fits are also checked in R-space using both the real and imaginary parts of Fourier transform. Finally, the presence of overlapping coordination shells and the correctness of the assumption about the nature of the coordinating atom were checked.

Keywords: XAS, EXAFS, FEFF, CoTi

Procedia PDF Downloads 263

Authors: G. Balaji, R. Balasundaraprabhu, S. Prasanna, M. D. Kannan, K. Sivakumaran, David Mcilroy

Abstract:

Copper Zin tin sulphide (Cu2ZnSnS4 or CZTS) is found to be better alternative to Copper Indium gallium diselenide as absorber layers in thin film based solar cells due to the utilisation of earth-abundant materials in the midst of lower toxicity. In the present study, Cu2ZnSnS4 thin films were prepared on soda lime glass using (CuS, ZnS, SnS) targets and were deposited by three different stacking orders, using RF Magnetron sputtering. The substrate temperature was fixed at 300 °C during the depositions. CZTS thin films were characterized using X-ray diffraction, X-ray photoelectron spectroscopy, Raman spectroscopy and UV-Vis-NIR spectroscopy. All the samples exhibited X-ray peaks pertaining to (112) kesterite phase of CZTS, along with the presence of a predominant wurtzite CZTS phase. X-ray photoelectron spectroscopy revealed the presence of all the elements in all the samples. The change in stacking order clearly shows that it affects the structural and phase properties of the films. Relative atomic concentrations of Zn, Cu, Sn and S, which are determined by high-resolution XPS core level spectra integrated peak areas revealed that the CZTS films exhibit inhomogeneity in both stoichiometry and elemental composition. Raman spectroscopy studies on the film showed the presence of CZTS phase. The energy band gap of the CZTS thin films was found to be in the range of 1.5 eV to 1.6 eV. The films were then annealed at 450 °C for 5 hrs and it was found that the predominant nature of the X-ray peaks has transformed from Wurtzite to Kesterite phase which is highly desirable for absorber layers in thin film solar cells. The optimized CZTS layer was used as an absorber layer in thin film solar cells. ZnS and CdS were used as buffer layers which in turn prepared by Hot wall epitaxy technique. Gallium doped Zinc oxide was used as a transparent conducting oxide. The solar cell structure Glass/Mo/CZTS/CdS or ZnS/GZO has been fabricated, and solar cell parameters were measured.

Keywords: earth-abundant, Kesterite, RF sputtering, thin film solar cells

Procedia PDF Downloads 260

Authors: Haruka Kaji, Jae-Ho Kim, Yonezawa Susumu

Abstract:

The surface of polycarbonate (PC) was modified with fluorine gas at 25℃ and 10-380 Torr for one h. The surface roughness of the fluorinated PC samples was approximately five times larger than that (1.2 nm) of the untreated thing. The results of Fourier transform infrared spectroscopy, and X-ray photoelectron spectroscopy showed that the bonds (e.g., -C=O and C-Hx) derived from raw PC decreased and were converted into fluorinated bonds (e.g., -CFx) after surface fluorination. These fluorinated bonds showed higher electronegativity according to the zeta potential results. Fluorinated PC could be strained with the methylene blue basic dye because of the increased surface roughness and the negatively charged surface.

Keywords: dyeable layer, polycarbonate, surface fluorination, zeta potential

Procedia PDF Downloads 148

Authors: M. Ertas, A. C. Onel, G. Ekinci, B. Toydemir, S. Durdu, M. Usta, L. Colakerol Arslan

Abstract:

To develop AZ91D magnesium alloys with improved properties, we have applied TiN and VN/TiN multilayer coatings using DC magnetron sputter technique. Coating structure, surface morphology, chemical bonding and corrosion resistance of coatings were analyzed by x-ray diffraction (XRD), scanning electron microscope (SEM), x-ray photoelectron spectroscopy (XPS), and tafel extrapolation method, respectively. XPS analysis reveal that VN overlayer reacts with oxygen at the VN/TiN interface and forms more stable TiN layer. Morphological investigations and the corrosion results show that VN/TiN multilayer thin film coatings are quite effective to optimize the corrosion resistance of Mg alloys.

Keywords: AZ91D Mg alloys, high corrosion resistance, transition metal nitride coatings, magnetron sputter

Procedia PDF Downloads 450

Authors: Zineb Benouahmane, Zhang Lifeng

Abstract:

Experimental oxidation tests at high temperature (1300°C-1500°C) on α-SiC samples have been performed with different holding times and atmosphere (air, argon). Oxidized samples were then analyzed using X-ray photoelectron spectroscopy coupled to SEM and DAKTEK surface profiler verification. The oxidation rate and the mas gain were found to increase with temperature and holding times, corresponding to a passive oxidation regime which lead to the formation of SiO2 layer. The sessile drop method is employed in order to measure the wetting angles between Si/SiC system at high temperature (1430°C-1550°C). Contact angle can be varied between 44 °C to 85°C, by controlling the oxygen content in α-SiC. Increasing the temperature occurred the infiltration of liquid silicon and deoxidation of the coating.

Keywords: oxidation, wettability, silicon, SiC

Procedia PDF Downloads 431

Authors: Meltem Bolluk, Ismail Duman

Abstract:

Boron exhibits the properties of high melting temperature (2273K to 2573 K), high hardness (Mohs: 9,5), low density (2,340 g/cm3), high chemical resistance, high strength, and semiconductivity (band gap:1,6-2,1 eV). These superior properties enable to use it in several high-tech areas from electronics to nuclear industry and especially in high temperature metallurgy. Amorphous boron and crystalline boron have different application areas. Amorphous boron powder (directly amorphous and/or α-rhombohedral) is preferred in rocket firing, airbag inflating and in fabrication of superconducting MgB2 wires. The conventional ways to produce elemental boron with a purity of 85 pct to 95 prc are metallothermic reduction, fused salt electrolysis and mechanochemical synthesis; but the only way to produce high-purity boron powders is Chemical Vapour Deposition (Hot Surface CVD). In this study; amorphous boron powders with a minimum purity of 99,9 prc were synthesized in quartz tubes using BCl3-H2 gas mixture by CVD. Process conditions based on temperature and gas flow rate were determined. Thermodynamical interpretation of BCl3-H2 system for different temperatures and molar rates were performed using Fact Sage software. The characterization of powders was examined by using Xray diffraction (XRD), Scanning Electron Microscope (SEM) and Transmission Electron Microscope (TEM), Stereo Microscope (SM), Helium gas pycnometer analysis. The purities of final products were determined by titration after lime fusion.

Keywords: amorphous boron, CVD, powder production, powder characterization

Procedia PDF Downloads 188

Authors: Mingmei Zhang, Xinyong Li

Abstract:

AgInS₂/SnS₂ (AIS) nanocomposites were synthesized by a simple hydrothermal method. The morphology and composition of the fabricated AIS nanocomposites were investigated by field-emission scanning electron microscopy (SEM), X-ray diffraction (XRD), high resolution transmission electron microscopy (HRTEM) and X-ray photoelectron spectroscopy (XPS). Moreover, the as-prepared AIS photocatalysts exhibited excellent photocatalytic activities for the degradation of Norfloxacin (NOR), mainly due to its high optical absorption and separation efficiency of photogenerated electron-hole pairs, as evidenced by UV–vis diffusion reflection spectra (DRS) and Surface photovoltage (SPV) spectra. Furthermore, the interfacial charges transfer mechanism was also discussed by DFT calculations.

Keywords: AIS nanocomposites, electron-hole pairs, charges transfer, DFTcaculations

Procedia PDF Downloads 159

Authors: Le Nguyen Binh, Luong Xuan Binh, Le Van Tuan, Tran Binh Duong, Truong Nguyen Khanh Hung, Do Le Hoang Son, Pham Quang Vinh, Hoang Quoc Huy, Nguyen Bach, Nguyen Quoc Khanh Le, Jiunn Horng Kang

Abstract:

Introduction: Traumatic hip dislocation is an emergency in young adult which can cause avascular necrosis of femoral head or osteoarthritis of hip joint. The reasons for these may be the loose body of bony or chondral fragments, which are difficult to be detected on CT scan or MRI. In those cases, Hip arthroscopy may be the method of choice for diagnosis and treatment of loose bodies in hip joint after traumatic dislocation. Methods: A case report is performed. A 55-year-old male patient was under hip arthroscopy to retrieve the loose body in the right hip joint. Results: The patient’s hip was reduced under anesthesia in the opeation room. Xray and CT scan post-reduction showed that his right hip was wide and a small fragment of femoral head (< 5mm) locking inside the joint. A hip arthroscopy was done to take the fragment out. Post-operation, the patient went under rehabilition. After 6 months, he can walk with full-weight bearing; no further dislocaion was noted, and the Harris score was 84 points. Conclusions: Although acute traumatic injury of hip joint is usually treated with open surgeries, these methods have many drawbacks, such as soft tissue destruction, blood-loss,….Despite its technical requirement, hip arthroscopy is less invasive and effective treatment. Therefore, it may be an alternative treatment for a traumatic hip injury and can be applied frequently in the near future.

Keywords: hip dislocation, hip arthroscopy, hip osteoarthritis, acute hip trauma

Procedia PDF Downloads 49

Authors: Natsumi Murakami, Jae-Ho Kim, Susumu Yonezawa

Abstract:

The calcium fluorosilicate (CaSiF₆) was prepared from calcium silicate (CaSiO₃) with fluorine gas at 25 ~ 200 ℃ and 760 Torr for 1~24 h. Especially, the pure CaSiF₆ could be prepared at 25 ℃ for 24 h with F₂ gas from the results of X-ray diffraction. Increasing temperature to higher than 100 ℃, the prepared CaSiF₆ was decomposed into CaF₂ and SiF₄. The release of SiF₄ gas was confirmed by the results of gas-phase infrared spectroscopy. In this study, we tried to modify the surface of polycarbonate (PC) resin using the SiF₄ gas released from CaSiF₆ particles. By using the prepared CaSiF₆, the surface roughness of fluorinated PC samples was approximately four times larger than that (1.4 nm) of the untreated sample. The results of X-ray photoelectron spectroscopy indicated the formation of fluorinated bonds (e.g., -CFx) on the surface of PC after surface fluorination. Consequently, the CaSiF₆ particles can be useful for a new fluorinating agent.

Keywords: calcium fluorosilicate, fluorinating agent, polycarbonate, surface fluorination

Procedia PDF Downloads 86

Authors: Muhammad A. Nadeem, Shaheed Ullah

Abstract:

The article reports the synthesis of Cr2O3/C nanocomposites obtained by the direct carbonization of PFA/MIL-101(Cr) bulk composite. The nanocomposites were characterized by various instrumental techniques like powder X-ray diffraction (PXRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), transmission electron microscopy (TEM), selected area electron diffraction (SAED) and the surface characterized were investigated via N2 adsorption/desorption analysis. TEM and SAED analysis shows that turbostatic graphitic carbon was obtained with high crystallinity. The nanocomposites were tested for electrochemical supercapacitor and the faradic and non-Faradic processes were checked through cyclic voltammetry (CV). The maximum specific capacitance calculated for Cr2O3/C 900 sample from CV measurement is 301 F g-1 at 2 mV s-1 due to its maximum charge storing capacity as confirm by frequency response analysis.

Keywords: nanocomposites, transmission electron microscopy, non-faradic process

Procedia PDF Downloads 410

Authors: R. S. Yadav, J. Havlica, I. Kuřitka, Z. Kozakova, J. Masilko, M. Hajdúchová, V. Enev, J. Wasserbauer

Abstract:

In this present work, CoFe2-xNdxO4 (0.0 ≤ x ≥0.1) spinel ferrite nanoparticles were synthesized by starch-assisted sol-gel auto-combustion method. Powder X-ray diffraction patterns were revealed the formation of cubic spinel ferrite with the signature of NdFeO3 phase at higher Nd3+ concentration. The field emission scanning electron microscopy study demonstrated the spherical nanoparticle in the size range between 5-15 nm. Raman and Fourier Transform Infrared spectra supported the formation of the spinel ferrite structure in the nanocrystalline form. The X-ray photoelectron spectroscopy (XPS) analysis confirmed the presence of Co2+ and Fe3+ at octahedral as well as a tetrahedral site in CoFe2-xNdxO4 nanoparticles. The change in magnetic properties with a variation of concentration of Nd3+ ions in cobalt ferrite nanoparticles was observed.

Keywords: nanoparticles, spinel ferrites, sol-gel auto-combustion method, CoFe2-xNdxO4

Procedia PDF Downloads 468

Authors: Anna V. Zaporozhchenko, Dmytro Kutnyakhov, Katherina Medjanik, Christian Tusche, Hans-Joachim Elmers, Olena Fedchenko, Sergey Chernov, Martin Ellguth, Sergej A. Nepijko, Gerd Schoenhense

Abstract:

Graphene reveals a unique electronic structure that predetermines many intriguing properties such as massless charge carriers, optical transparency and high velocity of fermions at the Fermi level, opening a wide horizon of future applications. Hence, a detailed investigation of the electronic structure of graphene is crucial. The method of choice is angular resolved photoelectron spectroscopy ARPES. Here we present experiments using time-of-flight (ToF) momentum microscopy, being an alternative way of ARPES using full-field imaging of the whole Brillouin zone (BZ) and simultaneous acquisition of up to several 100 energy slices. Unlike conventional ARPES, k-microscopy is not limited in simultaneous k-space access. We have recorded the whole first BZ of graphene on Ir(111) including all six Dirac cones. As excitation source we used synchrotron radiation from BESSY II (Berlin) at the U125-2 NIM, providing linearly polarized (both polarizations p- and s-) VUV radiation. The instrument uses a delay-line detector for single-particle detection up the 5 Mcps range and parallel energy detection via ToF recording. In this way, we gather a 3D data stack I(E,kx,ky) of the full valence electronic structure in approx. 20 mins. Band dispersion stacks were measured in the energy range of 14 eV up to 23 eV with steps of 1 eV. The linearly-dispersing graphene bands for all six K and K’ points were simultaneously recorded. We find clear features of hybridization with the substrate, in particular in the linear dichroism in the angular distribution (LDAD). Recording of the whole Brillouin zone of graphene/Ir(111) revealed new features. First, the intensity differences (i.e. the LDAD) are very sensitive to the interaction of graphene bands with substrate bands. Second, the dark corridors are investigated in detail for both, p- and s- polarized radiation. They appear as local distortions of photoelectron current distribution and are induced by quantum mechanical interference of graphene sublattices. The dark corridors are located in different areas of the 6 Dirac cones and show chirality behaviour with a mirror plane along vertical axis. Moreover, two out of six show an oval shape while the rest are more circular. It clearly indicates orientation dependence with respect to E vector of incident light. Third, a pattern of faint but very sharp lines is visible at energies around 22eV that strongly remind on Kikuchi lines in diffraction. In conclusion, the simultaneous study of all six Dirac cones is crucial for a complete understanding of dichroism phenomena and the dark corridor.

Keywords: band structure, graphene, momentum microscopy, LDAD

Procedia PDF Downloads 310

Authors: Maryam Kiani, Abdul Basit Kiani

Abstract:

Simple hydrothermal method to synthesize new nanocomposites consisting of nitrogen-doped graphene and NiFe₂O₄. By analyzing the X-Ray Powder Diffraction (XRD) images, we confirmed that the NiFe₂O₄ phase is pure and has a Face Centered Cubic (FCC) structure. The average size of the NiFe₂O₄ nanoparticles is approximately 40±2 nm. Additionally, we used X-ray photoelectron spectroscopy (XPS) to study the surface chemical composition and cation oxidation states of both the NiFe₂O₄ nanoparticles and the nitrogen-doped graphene/NiFe₂O₄ nanocomposites. A magnetic interaction between nitrogen doped graphene/NiFe₂O₄ was studied. Increases in hydrothermal synthesis temperature lead to the improved crystalline structure of NiFe₂O₄ nanoparticles, which improves the magnetic properties.

Keywords: nickel ferrite spinal, nitrogen doped graphene, magnetic nanocomposite, hydrothermal synthesis

Procedia PDF Downloads 83

Authors: Lucky Malise, Hilary Rutto, Tumisang Seodigeng

Abstract:

The use of tires in automobiles is very important in the automobile industry. However, there is a serious environmental problem concerning the disposal of these rubber tires once they become worn out. The main aim of this study was to prepare activated carbon from waste tire pyrolysis char by impregnating KOH on pyrolytic char. Adsorption studies on lead onto chemically activated carbon was carried out using response surface methodology. The effect of process parameters such as temperature (°C), adsorbent dosage (g/1000ml), pH, contact time (minutes) and initial lead concentration (mg/l) on the adsorption capacity were investigated. It was found that the adsorption capacity increases with an increase in contact time, pH, temperature and decreases with an increase in lead concentration. Optimization of the process variables was done using a numerical optimization method. Fourier Transform Infrared Spectra (FTIR) analysis, XRay diffraction (XRD), Thermogravimetric analysis (TGA) and scanning electron microscope was used to characterize the pyrolytic carbon char before and after activation. The optimum points 1g/ 100 ml for adsorbent dosage, 7 for pH value of the solution, 115.2 min for contact time, 100 mg/l for initial metal concentration, and 25°C for temperature were obtained to achieve the highest adsorption capacity of 93.176 mg/g with a desirability of 0.994. Fourier Transform Infrared Spectra (FTIR) analysis and Thermogravimetric analysis (TGA) show the presence of oxygen-containing functional groups on the surface of the activated carbon produced and that the weight loss taking place during the activation step is small.

Keywords: waste tire pyrolysis char, chemical activation, central composite design (CCD), adsorption capacity, numerical optimization

Procedia PDF Downloads 191

Authors: Andrea Alfaro Barajas, Arturo I. Martinez

Abstract:

3D photothermal structure of carbon was synthesized using PET bottles waste and sodium chloride through controlled carbonization. Characterization techniques such as X-ray photoelectron spectroscopy, X-ray diffraction, BET, scanning electron microscopy (SEM), transmission electron microscopy (TEM), Raman spectroscopy, spectrophotometry, and mechanical compression were carried out. The carbon showed physical integrity > 90%, an absorbance > 90% between 300-1000nm of the solar spectrum, and a high specific surface area from 450 to 620 m2/g. The X-ray was employed to examine the phase structure; the obtained pattern shows an amorphous material. A higher intensity of band D with respect to band G was confirmed by Raman Spectroscopy. C-OH, COOH, C-O, and C-C bonds were obtained from the deconvolution of the high-resolution C1s orbital. Macropores of 160 to 180µm and micropores of 0.5 to 2nm were observed by SEM and TEM images, respectively. Such combined characteristics of carbon confer efficient evaporation of water under 1 sun irradiation > 60%.

Keywords: solar-absorber, carbon, water-evaporation, interfacial

Procedia PDF Downloads 125

Authors: Mingmei Zhang, Xinyong Li

Abstract:

Novel AgInS2/SnS2/RGO (AISR) heterojunctions photocatalysts were synthesized by simple hydrothermal method. The morphology and composition of the fabricated AISR nanocomposites were investigated by field-emission scanning electron microscopy (SEM), X-ray diffraction (XRD), high resolution transmission electron microscopy (HRTEM) and X-ray photoelectron spectroscopy (XPS). Moreover, the as-prepared AISR photocatalysts exhibited excellent photocatalytic activities for the degradation of Norfloxacin (NOR), mainly due to its high optical absorption and separation efficiency of photogenerated electron-hole pairs, as evidenced by UV–vis diffusion reflection spectra (DRS) and Surface photovoltage (SPV) spectra. Furthermore, laser flash photolysis technique was conducted to test the lifetime of charge carriers of the fabricated nanocomposites. The interfacial charges transfer mechanism was also discussed.

Keywords: AISR heterojunctions, electron-hole pairs, SPV spectra, charges transfer mechanism

Procedia PDF Downloads 148

Authors: M. P. Joshi, F. Deganello, L. F. Liotta, V. La Parola, G. Pantaleo

Abstract:

For the first time, commercial iron nitrate was replaced by rust wastes, as a source of Iron for the preparation of LaFeO₃ powders by solution combustion synthesis (SCS). A detailed comparison with a reference powder obtained by SCS, starting from a commercial iron nitrate, was also performed. Several techniques such as X-ray diffraction combined with Rietveld refinement, mass plasma atomic emission spectroscopy, nitrogen adsorption measurements, temperature programmed reduction, X-ray photoelectron spectroscopy, Fourier transform analysis and scanning electron microscopy were used for the characterization of the rust wastes as well as of the perovskite powders. The performance of this ecofriendly material was evaluated by testing the activity and selectivity in the propylene oxidation, in order to use it for the benefit of the environment. Characterization and performance results clearly evidenced limitations and peculiarities of this new approach.

Keywords: perovskite type catalysts, solution combustion synthesis, X-ray diffraction, rust wastes

Procedia PDF Downloads 304

Authors: Yasaman Tabari-Saadi, Kaiwen Sun, Jialiang Huang, Martin Green, Xiaojing Hao

Abstract:

Optical and electrical properties of p-type AgBiS₂ absorber material have been improved by copper doping on silver sites. X-Ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) analysis suggest that complete solid solutions of Ag₁₋ₓCuₓBiS₂ thin film have been formed. The carrier concentration of pure AgBiS₂ thin film deposited by the chemical process is 4.5*E+14 cm⁻³, and copper doping leads to the improved carrier concentration despite the semiconductor AgBiS₂ remains p-type semiconductor. Copper doping directly changed the absorption coefficient and increased the optical band gap (~1.5eV), which makes it a promising absorber for thin-film solar cell applications.

Keywords: copper doped, AgBiS₂, thin-film solar cell, carrier concentration, p-type semiconductor

Procedia PDF Downloads 92

Authors: Surjyakanta Rana, Sreekantha B. Jonnalagadda

Abstract:

Synthesis of well distributed Pd nanoparticles (3 – 7 nm) on organo amine-functionalized graphene is reported, which demonstrated excellent catalytic activity towards Suzuki coupling reaction. The active material was characterized by X-ray diffraction (XRD), BET surface area, X-ray photoelectron spectra (XPS), Fourier-transfer infrared spectroscopy (FTIR), Raman spectra, Scanning electron microscope (SEM), Transmittance electron microscopy (TEM) analysis and HRTEM. FT-IR revealed that the organic amine functional group was successfully grafted onto the graphene oxide surface. The formation of palladium nanoparticles was confirmed by XPS, TEM and HRTEM techniques. The catalytic activity in the coupling reaction was superb with 100% conversion and 98 % yield and also activity remained almost unaltered up to six cycles. Typically, an extremely high turnover frequency of 185,078 h-1 is observed in the C-C Suzuki coupling reaction using organo di-amine functionalized graphene as catalyst.

Keywords: Di-amine, graphene, Pd nanoparticle, suzuki coupling

Procedia PDF Downloads 348

Authors: Dina M. Abd El-Aty, D. Aman, E. G. Zaki, Heba M. Salem

Abstract:

A friendly environmental source of energy as hydrogen was produced by photo-hydrolysis of hydrogen storage material as sodium borohydride (NaBH4), which is non-toxic and stores a high percentage of hydrogen. The photoreaction was produced under visible light and nano-alumina as a catalyst. In this study, we use more economical and friendly environmental oil as a template to produce a nano-catalyst. The prepared catalyst was characterized by X-Ray diffraction, N2-adsorption-desorption, Fourier Transforms Infrared, Scanning Electron microscope and X-Ray Photoelectron Spectroscopy. Different parameters such as catalyst weight, NaBH4 weight and time of irradiation were studied to obtain a highly efficient photo-hydrolysis reaction. The reaction is pseudo-first order and the hydrogen production rate was determined as 1500 ml min-1 g-1 at the optimum conditions.

Keywords: photo-reaction, nano-alumina, hydrogen production, sodium borohydride, visible light

Procedia PDF Downloads 56

Authors: Kohei Yamamoto, Jae-Ho Kim, Susumu Yonezawa

Abstract:

The surface of polyethylene terephthalate (PET) was modified with fluorine gas at 25 ℃ and 100 Torr for one h. Moreover, the effect of ethanol washing on surface modification was investigated in this study. The surface roughness of the fluorinated and washed PET samples was approximately six times larger than that (0.6 nm) of the untreated thing. The results of Fourier transform infrared spectroscopy, and X-ray photoelectron spectroscopy showed that the bonds such as -C=O and -C-Hx derived from raw PET decreased and were converted into fluorinated bonds such as -CFx after surface fluorination. Even after washing with ethanol, the fluorinated bonds stably existed on the surface. These fluorinated bonds showed higher electronegativity according to the zeta potential results. The negative surface charges were increased by washing the ethanol, and it caused to increase in the number of polar groups such as -CHF- and -C-Fx. The fluorinated and washed surface of PET could promote the adsorption of Ag+ ions in AgNO₃ solution because of the increased surface roughness and the negatively charged surface.

Keywords: Ag+ ions adsorption, polyethylene terephthalate, surface fluorination, zeta potential

Procedia PDF Downloads 96

Authors: Lamia L. G. Al-Mahamad, Benjamin R. Horrocks, Andrew Houlton

Abstract:

Hydrogels based on metal coordination polymers of nucleosides and a range of metal ions (Au, Ag, Cu) have been prepared and characterized by atomic force microscopy (AFM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy, Fourier transform infrared spectroscopy, ultraviolet-visible absorption spectroscopy, and powder X-ray diffraction. AFM images of the xerogels revealed the formation of extremely long polymer molecules (> 10 micrometers, the maximum scan range). This result is also consistent with TEM images which show a fibrous morphology. Oxidative doping of the Au-nucleoside fibres produces an electrically conductive nanowire. No sharp Bragg peaks were found at the at the X-ray diffraction pattern for metal ions hydrogels indicating that the samples were amorphous, but instead the data showed broad peaks in the range 20 < Q < 40 and correspond to distances d=2μ/Q. The data was analysed using a simplified Rietveld method by fitting a regression model to obtain the distance between atoms.

Keywords: hydrogel, metal ions, nanowire, nucleoside

Procedia PDF Downloads 230

Authors: Mohamed H. Gabr, Kiyoshi Uzawa

Abstract:

The current study aims to investigate the effect of fillers with different geometries and sizes on the interfacial shear properties of PA6 composites with de-sized carbon fiber. The fillers which have been investigated are namely; nano-layer silicates (nanoclay), sub-micro aluminum titanium (ALTi) particles, and multiwall carbon nanotube (MWCNT). By means of X-ray photoelectron spectroscopy (XPS), epoxide group which defined as a sizing agent, has been removed. Sizing removal can reduce the acid parameter of carbon fibers surface promoting bonding strength at the fiber/matrix interface which is a desirable property for the carbon fiber composites. Microdroplet test showed that the interfacial shear strength (IFSS) has been enhanced with the addition of 10wt% ALTi by about 23% comparing with neat PA6. However, with including other types of fillers into PA6, the results did not show enhancement of IFSS.

Keywords: sub-micro particles, nano-composites, interfacial shear strength, polyamide 6

Procedia PDF Downloads 216