XPS study of protein adsorption onto nanocrystalline aluminosilicate microparticles

X-ray photoelectron spectroscopy (XPS) was used to study the interaction of two different sized proteins, bovine serum albumin (BSA) and fibrinogen, with an aluminosilicate system containing yttrium and iron that is a potential biomaterial. Serum albumin and fibrinogen are two major plasma proteins and the most relevant proteins adsorbed on the surface of biomaterials in blood contact.The aluminosilicate samples were incubated for several exposure times, up to 24 h, in simulated body fluid enriched with BSA, and in buffered fibrinogen solution. Time dependence of proteins adsorption onto surface of the investigated samples is reflected by the evolution of the new N 1s photoelectron peak and by the modification of C 1s core-level spectra recorded from the samples immersed in protein solution.     

X-ray photoelectron spectroscopy of Sm-doped CaO-MgO-Al2O3-SiO2 glasses and glass ceramics

Sm³⁺ doped CaO-MgO-Al₂O₃-SiO₂ glass and glass ceramics have been prepared. The diopside crystal (CaMgSi₂O₆) was identified in the glass ceramics by X-ray diffraction analysis. X-ray photoelectron spectra of the glass and glass ceramics were measured by a monochromatised Al-Kα XPS instrument. Sm 3d core level spectra for the Sm doped samples showed that Sm ions are predominantly in the Sm (III) state in glass and glass ceramics. The O 1s core spectra could be fitted by summing the contributions from bridging oxygen (BO) and non bridging oxygen (NBO) for samarium undoped glass, BO, NBO and Si-O-Sm for the doped glass. The O 1s XPS spectrum of undoped glass ceramics was curve fitted with BO and NBO in glass phase, as well as SiOSi, SiOMg and SiOCa in diopside. In addition to the five components above mentioned, SiOSm in diopside also appeared in O 1s XPS spectra of samarium doped glass ceramics. According to the fitting results, we demonstrate that the Sm₂O₃ exist in glass network as a glass modifier. After heat treatment, nearly all the Sm³⁺ existed in diopside phase as the substitution for Ca²⁺.     

ToF-SIMS and XPS study of ancient papers

The surface composition of 18th century papers was investigated by means of ToF-SIMS and XPS. The aim of the present study was to explore the possibility of using these surface sensitive methods to obtain information which can help to determine the manufacturing process, provenance and state of conservation of ancient papers. The ToF-SIMS results indicate that the analyzed papers were sized by gelatin and that alum was added as hardening agent. The paper sheets produced in near geographical areas but in different paper mills exhibit a similar surface composition and morphology of the fibers as shown by the ToF-SIMS measurements. The ToF-SIMS and the XPS results indicate that a significant fraction of the cellulose fibers is not covered by the gelatin layer. This was observed for the ancient papers and for a modern handmade paper manufactured according to the old recipes.     

Amphiphobicity of polyvinylidene fluoride porous films after atmospheric pressure plasma intermittent etching

This study modified the surface of polyvinylidene fluoride (PVDF) films and characterized their surface physicochemical properties. The main aim of this study was to examine how to provide the surface with a specific property, e.g., not only hydrophobic but also oleophobic (amphiphobicity) after argon atmospheric pressure plasma (APP) treatment. The surface free energy calculated using the Owens-Wendt (OW) method decreased significantly while showing a very small value of the polar component. Scanning electron microscopy indicated that a small amount of hydrophilic solid spines and many superamphiphobic uniform micro air pockets formed in the plasma-modified PVDF film, which made it amphiphobic but not superamphiphobic.     

Valence control of cobalt oxide thin films by annealing atmosphere

The cobalt oxide (CoO and Co₃O₄) thin films were successfully prepared using a spin-coating technique by a chemical solution method with CH₃OCH₂CH₂OH and Co(NO₃)₂·6H₂O as starting materials. The grayish cobalt oxide films had uniform crystalline grains with less than 50 nm in diameter. The phase structure is able to tailor by controlling the annealing atmosphere and temperature, in which Co₃O₄ thin film was obtained by annealing in air at 300-600, and N₂ at 300, and transferred to CoO thin film by raising annealing temperature in N₂. The fitted X-ray photoelectron spectroscopy (XPS) spectra of the Co2p electrons are distinguishable from different valence states of cobalt oxide especially for their satellite structure. The valence control of cobalt oxide thin films by annealing atmosphere contributes to the tailored optical absorption property.     

Effect of C60 ion sputtering on the compositional depth profiling in XPS for Li(Ni,Co,Mn)O2 electrodes

The performance of a Li-ion cell strongly depends on the solid-electrolyte interface (SEI) on electrodes. The depth distribution of composition in SEI is normally determined by means of X-ray Photoelectron Spectroscopy (XPS) via Ar ion sputtering. Recently, a new kind of ion gun using C60 ions as sputtering source was introduced. In this report, a comparison between the effects of these two kinds of ion guns on the quantification of Li(Ni,Co,Mn)O₂ electrodes was made. It was found that the C60 ion gun is more suitable for analyzing the composition and chemical state of Li(Ni,Co,Mn)O₂ electrode since that it causes lower chemical damage in the superficial layer.     

Modification of surface properties of polyamide 6 films with atmospheric pressure plasma

To investigate the effect of the different plasma gases treatment on the surface modification of atmospheric pressure plasma, polyamide 6 films were treated using pure helium (He), He/O₂ and He/CF₄, respectively. Atomic force microscopy (AFM) showed rougher surface, while X-ray photoelectron spectroscopy (XPS) revealed increased oxygen and fluorine contents after the plasma treatments. The plasma treated samples had lower water contact angles and higher T-peel strength than that of the control. The addition of small amount of O₂ or CF₄ to He plasma increases the effectiveness of the plasma treatment in polymer surface modification in terms of surface roughness, surface hydrophilic groups, etching rate, water contact angle and bonding strength.     

Carbon nitride films by RF plasma assisted PLD: Spectroscopic and electronic analysis

Carbon nitride (CNx) thin films have been grown on Si 〈1 0 0〉 by 193 nm ArF ns pulsed laser ablation of a pure graphite target in a low pressure atmosphere of a RF generated N₂ plasma and compared with samples grown by PLD in pure nitrogen atmosphere. Composition, structure and bonding of the deposited materials have been evaluated by X-ray photoelectron spectroscopy (XPS), and Raman scattering. Significant chemical and micro-structural changes have been registered, associated to different nitrogen incorporation in the two types of films analyzed. The intensity of the reactive activated species is, indeed, increased by the presence of the bias confined RF plasma, as compared to the bare nitrogen atmosphere, thus resulting in a different nitrogen uptake in the growing films. The process has been also investigated by some preliminary optical emission studies of the carbon plume expanding in the nitrogen atmosphere. Optical emission spectroscopy reveals the presence of many excited species like C⁺ ions, C atoms, C₂, N₂; and CN radicals, and N₂⁺ molecular ions, whose relative intensity appears to be increased in the presence of the RF plasma. The films were also characterised for electrical properties by the “four-probe-test method” determining sheet resistivity and correlating surface conductivity with chemical composition.     

Oxidation kinetics of thin copper films and wetting behaviour of copper and Organic Solderability Preservatives (OSP) with lead-free solder

The oxide formation on thin copper films deposited on Si wafer was studied by XPS, SEM and Sequential Electrochemical Reduction Analysis SERA. The surfaces were oxidized in air with a reflow oven as used in electronic assembly at temperatures of 100 °C, 155 °C, 200 °C, 230 °C and 260 °C. The SERA analyses detected only the formation of Cu₂O but the XPS analysis done for the calibration of the SERA equipment proved also the presence of a CuO layer smaller than 2 nm above the Cu₂O oxide. The oxide growth follows a power-law dependence on time within this temperature range and an activation energy of 33.1 kJ/mol was obtained. The wettability of these surfaces was also determined by measuring the contact angle between solder and copper substrate after the soldering process. A correlation between oxide thickness and wetting angle was established. It was found that the wetting is acceptable only when the oxide thickness is smaller than 16 nm. An activation energy of 27 kJ/mol was acquired for the spreading of lead free solder on oxidized copper surfaces.From wetting tests on copper surfaces protected by Organic Solderability Preservatives (OSP), it was possible to calculate the activation energy for the thermal decomposition of these protective layers.