Commenced in January 2007
Frequency: Monthly
Edition: International
Paper Count: 10

XPS Related Abstracts

10 Chemical Modification of PVC and Its Surface Analysis by Means of XPS and Contact Angle Measurements

Authors: Ali Akrmi, Mohamed Beji, Ahmed Baklouti, Fatma Djouani, Philippe Lang, Mohamed M. Chehimi


Poly(vinyl chloride) (PVC) is a highly versatile polymer with excellent balance of properties and numerous applications such as water pipes, packaging and polymer materials of importance in the biomedical sector. However, depending on the applications, it is necessary to modify PVC by mixing with a plasticizer; surface modification using plasma, surface grafting or flame treatment; or bulk chemical modification which affects the entire PVC chains at an extent that can be tuned by the polymer chemist. The targeted applications are improvement of chemical resistance, avoiding or limitation of migration of toxic plasticizers, improvement of antibacterial properties, or control of blood compatibility.

Keywords: poly(vinyl chloride), nucleophilic substitution, sulfonylcarbamates, XPS

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9 Absorption Kinetic and Tensile Mechanical Properties of Swollen Elastomer/Carbon Black Nanocomposites using Typical Solvents

Authors: F. Elhaouzi, H. Lahlali, M. Zaghrioui, I. El Aboudi A. BelfKira, A. Mdarhri


The effect of physico chemical properties of solvents on the transport process and mechanical properties in elastomeric nano composite materials is reported. The investigated samples are formed by a semi-crystalline ethylene-co-butyl acrylate polymer filled with hard spherical carbon black (CB) nano particles. The swelling behavior was studied by immersion the dried samples in selected solvents at room temperature during 2 days. For this purpose, two chemical compounds methyl derivatives of aromatic hydrocarbons of benzene, i.e. toluene and xylene, are used to search for the mass and molar volume dependence on the absorption kinetics. Mass gain relative to the mass of dry material at specific times was recorded to probe the absorption kinetics. The transport of solvent molecules in these filled elastomeric composites is following a Fickian diffusion mechanism. Additionally, the swelling ratio and diffusivity coefficient deduced from the Fickian law are found to decrease with the CB concentration. These results indicate that the CB nano particles increase the effective path length for diffusion and consequently limit the absorption of the solvent by occupation free volumes in the material. According to physico chemical properties of the two used solvents, it is found that the diffusion is more important for the toluene molecules solvent due to their low values of the molecular weight and volume molar compared to those for the xylene. Differential Scanning Calorimetry (DSC) and X-ray photo electron (XPS) were also used to probe the eventual change in the chemical composition for the swollen samples. Mechanically speaking, the stress-strain curves of uniaxial tensile tests pre- and post- swelling highlight a remarkably decrease of the strength and elongation at break of the swollen samples. This behavior can be attributed to the decrease of the load transfer density between the matrix and the CB in the presence of the solvent. We believe that the results reported in this experimental investigation can be useful for some demanding applications e.g. tires, sealing rubber.

Keywords: Modelling, nanocomposite, Mechanical Behavior, diffusion, DSC, XPS, absorption kinetics

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8 Gypsum Composites with CDW as Raw Material

Authors: R. Santos Jiménez, A. San-Antonio-González, M. del Río Merino, M. González Cortina, C. Viñas Arrebola


On average, Europe generates around 890 million tons of construction and demolition waste (CDW) per year and only 50% of these CDW are recycled. This is far from the objectives determined in the European Directive for 2020 and aware of this situation, the European Countries are implementing national policies to prevent the waste that can be avoidable and to promote measures to increase recycling and recovering. In Spain, one of these measures has been the development of a CDW recycling guide for the manufacture of mortar, concrete, bricks and lightweight aggregates. However, there is still not enough information on the possibility of incorporating CDW materials in the manufacture of gypsum products. In view of the foregoing, the Universidad Politécnica de Madrid is creating a database with information on the possibility of incorporating CDW materials in the manufacture of gypsum products. The objective of this study is to improve this database by analysing the feasibility of incorporating two different CDW in a gypsum matrix: ceramic waste bricks (perforated brick and double hollow brick), and extruded polystyrene (XPS) waste. Results show that it is possible to incorporate up to 25% of ceramic waste and 4% of XPS waste over the weight of gypsum in a gypsum matrix. Furhtermore, with the addition of ceramic waste an 8% of surface hardness increase and a 25% of capillary water absorption reduction can be obtained. On the other hand, with the addition of XPS, a 26% reduction of density and a 37% improvement of thermal conductivity can be obtained.

Keywords: Construction Materials, Waste Materials, gypsum, Ceramic Waste, XPS, CDW

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7 O-Functionalized CNT Mediated CO Hydro-Deoxygenation and Chain Growth

Authors: K. Mondal, S. Talapatra, M. Terrones, S. Pokhrel, C. Frizzel, B. Sumpter, V. Meunier, A. L. Elias


Worldwide energy independence is reliant on the ability to leverage locally available resources for fuel production. Recently, syngas produced through gasification of carbonaceous materials provided a gateway to a host of processes for the production of various chemicals including transportation fuels. The basis of the production of gasoline and diesel-like fuels is the Fischer Tropsch Synthesis (FTS) process: A catalyzed chemical reaction that converts a mixture of carbon monoxide (CO) and hydrogen (H2) into long chain hydrocarbons. Until now, it has been argued that only transition metal catalysts (usually Co or Fe) are active toward the CO hydrogenation and subsequent chain growth in the presence of hydrogen. In this paper, we demonstrate that carbon nanotube (CNT) surfaces are also capable of hydro-deoxygenating CO and producing long chain hydrocarbons similar to that obtained through the FTS but with orders of magnitude higher conversion efficiencies than the present state-of-the-art FTS catalysts. We have used advanced experimental tools such as XPS and microscopy techniques to characterize CNTs and identify C-O functional groups as the active sites for the enhanced catalytic activity. Furthermore, we have conducted quantum Density Functional Theory (DFT) calculations to confirm that C-O groups (inherent on CNT surfaces) could indeed be catalytically active towards reduction of CO with H2, and capable of sustaining chain growth. The DFT calculations have shown that the kinetically and thermodynamically feasible route for CO insertion and hydro-deoxygenation are different from that on transition metal catalysts. Experiments on a continuous flow tubular reactor with various nearly metal-free CNTs have been carried out and the products have been analyzed. CNTs functionalized by various methods were evaluated under different conditions. Reactor tests revealed that the hydrogen pre-treatment reduced the activity of the catalysts to negligible levels. Without the pretreatment, the activity for CO conversion as found to be 7 µmol CO/g CNT/s. The O-functionalized samples showed very activities greater than 85 µmol CO/g CNT/s with nearly 100% conversion. Analyses show that CO hydro-deoxygenation occurred at the C-O/O-H functional groups. It was found that while the products were similar to FT products, differences in selectivities were observed which, in turn, was a result of a different catalytic mechanism. These findings now open a new paradigm for CNT-based hydrogenation catalysts and constitute a defining point for obtaining clean, earth abundant, alternative fuels through the use of efficient and renewable catalyst.

Keywords: dft, Liquid Fuels, XPS, CNT, CO Hydrodeoxygenation, XTL

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6 Streptavidin-Biotin Attachment on Modified Silicon Nanowires

Authors: Shalini Singh, Sanjay K. Srivastava, Govind, Mukhtar. A. Khan, P. K. Singh


Nanotechnology is revolutionizing the development of biosensors. Nanomaterials and nanofabrication technologies are increasingly being used to design novel biosensors. Sensitivity and other attributes of biosensors can be improved by using nanomaterials with unique chemical, physical, and mechanical properties in their construction. Silicon is a promising biomaterial that is non-toxic and biodegradable and can be exploited in chemical and biological sensing. Present study demonstrated the streptavidin–biotin interaction on silicon surfaces with different topographies such as flat and nanostructured silicon (nanowires) surfaces. Silicon nanowires with wide range of surface to volume ratio were prepared by electrochemical etching of silicon wafer. The large specific surface of silicon nanowires can be chemically modified to link different molecular probes (DNA strands, enzymes, proteins and so on), which recognize the target analytes, in order to enhance the selectivity and specificity of the sensor device. The interaction of streptavidin with biotin was carried out on 3-aminopropyltriethoxysilane (APTS) functionalized silicon surfaces. Fourier Transform Infrared Spectroscopy (FTIR) and X-ray Photoelectron Spectroscopy (XPS) studies have been performed to characterize the surface characteristics to ensure the protein attachment. Silicon nanowires showed the enhance protein attachment, as compared to flat silicon surface due to its large surface area and good molecular penetration to its surface. The methodology developed herein could be generalized to a wide range of protein-ligand interactions, since it is relatively easy to conjugate biotin with diverse biomolecules such as antibodies, enzymes, peptides, and nucleotides.

Keywords: Silicon Nanowires, FTIR, XPS, streptavidin-biotin

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5 Physicochemical Characterization of Mercerized Cellulose-Supported Nickel-Oxide

Authors: Sherif M. A. S. Keshk, Hisham S. M. Abd-Rabboh, Mohamed S. Hamdy, Ibrahim H. A. Badr


Microwave radiation was applied to synthesize nanoparticles of nickel oxide supported on pretreated cellulose with metal acetate in the presence of NaOH. Optimization, in terms of irradiation time and metal concentration, was investigated. FT-IR spectrum of cellulose/NiO spectrum shows a band at 445 cm^-1 that is related to the Ni–O stretching vibration of NiO6 octahedral in the cubic NiO structure. cellulose/NiO showed similar XRD pattern of cellulose I and exhibited sharpened reflection peak at 2q = 29.8°, corresponding to (111) plane of NiO, with two weak broad peaks at 48.5°, and 49.2°, representing (222) planes of NiO. XPS spectrum of mercerized cellulose/NiO composite showed did not show any peaks corresponding to Na ion.

Keywords: Cellulose, SEM, FTIR, XRD, XPS, Raman spectrum, mercerized cellulose, cellulose/zinc and nickeloxides composite

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4 Resistive Switching Characteristics of Resistive Random Access Memory Devices after Furnace Annealing Processes

Authors: Chi-Yan Chu, Kai-Chi Chuang, Huang-Chung Cheng


In this study, the RRAM devices with the TiN/Ti/HfOx/TiN structure were fabricated, then the electrical characteristics of the devices without annealing and after 400 °C and 500 °C of the furnace annealing (FA) temperature processes were compared. The RRAM devices after the FA’s 400 °C showed the lower forming, set and reset voltages than the other devices without annealing. However, the RRAM devices after the FA’s 500 °C did not show any electrical characteristics because the TiN/Ti/HfOx/TiN device was oxidized, as shown in the XPS analysis. From these results, the RRAM devices after the FA’s 400 °C showed the best electrical characteristics.

Keywords: Forming, XPS, RRAM, furnace annealing (FA), set and reset voltages

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3 Electronic Properties Study of Ni/MgO Nanoparticles by X-Ray Photoemission Spectroscopy (XPS)

Authors: Ouafek Nora, Keghouche Nassira, Dehdouh Heider, Untidt Carlos


A lot of knowledge has been accumulated on the metal clusters supported on oxide surfaces because of their multiple applications in microelectronics, heterogeneous catalysis, and magnetic devices. In this work, the surface state of Ni / MgO has been studied by XPS (X-ray Photoemission Spectroscopy). The samples were prepared by impregnation with ion exchange Ni²⁺ / MgO, followed by either a thermal treatment in air (T = 100 -350 ° C) or a gamma irradiation (dose 100 kGy, 25 kGy dose rate h -1). The obtained samples are named after impregnation NMI, NMR after irradiation, and finally NMC(T) after calcination at the temperature T (T = 100-600 °C). A structural study by XRD and HRTEM reveals the presence of nanoscaled Ni-Mg intermetallic phases (Mg₂Ni, MgNi₂, and Mg₆Ni) and magnesium hydroxide. Mg(OH)₂ in nanometric range (2- 4 nm). Mg-Ni compounds are of great interest in energy fields (hydrogen storage…). XPS spectra show two Ni2p peaks at energies of about 856.1 and 861.9 eV, indicating that the nickel is primarily in an oxidized state on the surface. The shift of the main peak relative to the pure NiO (856.1 instead of 854.0 eV) suggests that in addition to oxygen, nickel is engaged in another link with magnesium. This is in agreement with the O1s spectra which present an overlap of peaks corresponds to NiO and MgO, at a calcination temperature T ≤ 300 °C.

Keywords: XRD, XPS, nanoparticules, Ni-MgO

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2 Preparation and Characterization of Phosphate-Nickel-Titanium Composite Coating Obtained by Sol Gel Process for Corrosion Protection

Authors: Khalidou Ba, Abdelkrim Chahine, Mohamed Ebn Touhami


A strong industrial interest is focused on the development of coatings for anticorrosion protection. In this context, phosphate composite materials are expanding strongly due to their chemical characteristics and their interesting physicochemical properties. Sol-gel coatings offer high homogeneity and purity that may lead to obtain coating presenting good adhesion to metal surface. The goal behind this work is to develop efficient coatings for corrosion protection of steel to extend its life. In this context, a sol gel process allowing to obtain thin film coatings on carbon steel with high resistance to corrosion has been developed. The optimization of several experimental parameters such as the hydrolysis time, the temperature, the coating technique, the molar ratio between precursors, the number of layers and the drying mode has been realized in order to obtain a coating showing the best anti-corrosion properties. The effect of these parameters on the microstructure and anticorrosion performance of the films sol gel coating has been investigated using different characterization methods (FTIR, XRD, Raman, XPS, SEM, Profilometer, Salt Spray Test, etc.). An optimized coating presenting good adhesion and very stable anticorrosion properties in salt spray test, which consists of a corrosive attack accelerated by an artificial salt spray consisting of a solution of 5% NaCl, pH neutral, under precise conditions of temperature (35 °C) and pressure has been obtained.

Keywords: Corrosion, Coating, sol gel, XPS

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1 X-Ray Photoelectron Spectroscopy Characterization of the Surface Layer on Inconel 625 after Exposition in Molten Salt

Authors: Marie Kudrnova, Jana Petru


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: molten salt, XPS, oxide layer, Inconel 625

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