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Determination of nanoscale titanium oxide thin film phase composition using X-ray photoelectron spectroscopy valence band analysis
摘要： The phase compositions of nanoscale thick titania films on the titanium were determined using X-ray photoelectron spectroscopy valence band analysis for the first time, by deconvoluting the two-peak structure of valence band into five peaks and analysing the relative peak area. The titania films of thickness varying from about 2 nm to 8 μm were obtained by the air oxidation of commercially pure titanium at different temperatures. The titania films formed on titanium for oxidizing temperatures up to 200 °C were amorphous, with thickness < 10 nm. The sub-stoichiometric oxides present at the TiO2-Ti interface were composed of Ti3+, Ti2+ and Ti1+ states when the film of thickness was < 10 nm. At 300 °C, when the titania film thickness was < 20 nm, it was fully converted to rutile phase and remained stable up to 1000 °C. A broadening of full-width half-maxima of the core level peaks for the titania layers was attributed to the presence of surface hydroxyl group and stress gradient within the oxide layer. The absence of metastable anatase phase in the titania layers at lower temperatures was attributed to the presence of high stresses within the oxide layers owing to their nanoscale thickness.
关键词： X-ray Photoelectron Spectroscopy,Thin film,Valence band,Surface phase composition,Titania,Titanium
更新于2025-11-21 11:24:58
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Full color carbon dots through surface engineering for constructing white light-emitting diodes
摘要： White light-emitting diodes (WLEDs) devices are replacing the filament lamp and they can provide a light close to the natural sunlight, which have thus drawn considerable attention in these recent years. It remains a scientific challenge to develop WLEDs using environmentally friendly, easy-to-process and cost-effective phosphors. Here we synthesized blue-, green- and red-carbon dots (denoted as B-, G- and R-CDs) by a facile solvothermal method with high dispersity both in aqueous and organic solvent. The quantum yield (QY) of the R-CDs achieved up to 24.7%. These CDs can be easily dissolved in polyvinylpyrrolidone (PVP) colloid, leading to the production of ultraviolet (UV)-excited LED devices to avoid the retinal damage caused by blue ray excitation. The fluorescence emission of the WLED has a wide band, covering the whole visible light region. Importantly, the influence of doping that gives rise to the change of emissive colors has been elucidated by X-ray photoelectron spectroscopy (XPS) combined with a computation method in order to provide a systematic controllable tuning on the functionalization of CDs. As such, WLEDs were demonstrated with color coordinates of (0.33, 0.33), a color temperature of 5612 K in the CIE chromaticity diagram with good anti-photobleaching and a color rendering index (CRI) of 89.
关键词： polyvinylpyrrolidone,White light-emitting diodes,solvothermal method,UV-excited LED devices,density functional theory,quantum yield,X-ray photoelectron spectroscopy,carbon dots
更新于2025-11-14 15:18:02
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Low-damage nitrogen incorporation in graphene films by nitrogen plasma treatment: Effect of airborne contaminants
摘要： Graphene films grown on copper by chemical vapor deposition were exposed to the late afterglow of a reduced-pressure N2 plasma sustained by microwave electromagnetic fields. X-ray photoelectron and Raman spectroscopies reveal extremely high incorporation of plasma-generated N atoms into the graphene film (N/C = 29%) while maintaining an unprecedentedly low-damage generation (D:G = 0.35-0.45) compared to the literature (0.5 to 2.5). The incorporation dynamics between graphene on copper and graphene on copper oxide are also compared and discussed. After transfer on SiO2/Si substrate, the N/C content decrease to only 6%. This reveals that a large part of the N atoms are weakly bonded to the graphene surface. Most of the nitrogen incorporation seems linked to the functionalization of weakly bonded hydrocarbons initially adsorbed from air exposure or carbon-nitrogen structures arising from plasma-surface interactions.
关键词： X-Ray photoelectron spectroscopy,Raman spectroscopy,graphene,downstream plasma treatment,N-incorporation
更新于2025-09-23 15:23:52
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Chemical Analysis of the Interface between Hybrid Organic-Inorganic Perovskite and Atomic Layer Deposited Al2O3
摘要： Ultrathin metal oxides prepared by atomic layer deposition (ALD) have gained utmost attention as moisture and thermal stress barrier layers in perovskite solar cells (PSCs). We have recently shown that 10 cycles of ALD Al2O3 deposited directly on top of the CH3NH3PbI3-xClx perovskite material, are effective in delivering a superior PSC performance with 18% efficiency (compared to 15% of the Al2O3-free cell) with a long-term humidity-stability of more than 60 days. Motivated by these results, the present contribution focuses on the chemical modification which the CH3NH3PbI3-xClx perovskite undergoes upon growth of ALD Al2O3. Specifically, we combine in situ Infrared (IR) spectroscopy studies during film growth, together with X-ray Photoelectron Spectroscopy (XPS) analysis of the ALD Al2O3/perovskite interface. The IR-active signature of the NH3+ stretching mode of the perovskite undergoes minimal changes upon exposure to ALD cycles, suggesting no diffusion of ALD precursor and co-reactant (Al(CH3)3 and H2O) into the bulk of the perovskite. However, by analyzing the difference between the IR spectra associated with the Al2O3 coated perovskite and the pristine perovskite, respectively, changes occurring at the surface of perovskite are monitored. The abstraction of either NH3 or CH3NH2 from the perovskite surface is observed as deduced by the development of negative N-H bands associated to its stretching and bending modes. The IR investigations are corroborated by XPS study, confirming the abstraction of CH3NH2 from the perovskite surface, whereas no oxidation of its inorganic framework is observed within the ALD window process investigated in this work. In parallel, the growth of ALD Al2O3 on perovskite is witnessed by the appearance of characteristic IR-active Al-O-Al phonon and (OH)-Al=O stretching modes. Based on the IR and XPS investigations, a plausible growth mechanism of ALD Al2O3 on top of perovskite is presented.
关键词： infrared spectroscopy,x-ray photoelectron spectroscopy,atomic layer deposition,Al2O3,perovskite
更新于2025-09-23 15:23:52
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Evaluating the Surface Chemistry of Black Phosphorus during Ambient Degradation
摘要： Black Phosphorus (BP) is emerging as a promising candidate for electronic, optical and energy storage applications, however its poor ambient stability remains a critical challenge. Evaluation of few-layer liquid exfoliated BP during ambient exposure using x-ray photoelectron spectroscopy (XPS) and attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR) allows its surface chemistry to be investigated. Oxidation of liquid exfoliated few-layer BP initially occurs through non-bridging oxide species, which convert to bridging oxide species after ambient exposure. We demonstrate the instability of these bridging oxide species, which undergo hydrolysis to form volatile phosphorus oxides and evaporate from the BP surface. FTIR spectroscopy, scanning transmission electron microscopy and atomic force microscopy were used to confirm the formation of liquid oxides through a continuous oxidation cycle that results in the decomposition of BP. Furthermore, we show that the instability of few-layer BP originates from the formation of bridging oxide species.
关键词： Fourier transform infrared spectroscopy,Black phosphorus,phosphorene,x-ray photoelectron spectroscopy,2D materials,degradation,ambient stability,oxidation
更新于2025-09-23 15:23:52
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X-ray photoelectron spectroscopy and Raman microscopy of a ferroan platinum crystal from the Kondyor Massif, Russian Far East
摘要： X-ray Photoelectron Spectroscopy was used to study a ferroan platinum crystal from the Kondyor Massif, Russian Far East. Prior to the X-ray Photoelectron Spectroscopic analyses, the nature of the crystal was confirmed by X-ray diffraction. The survey scan showed mainly the presence of Pt and Fe, with smaller amounts of O and Si. The high resolutions spectra of the Pt 4f and Fe 2p showed 18.3 atom% Fe in the crystal, which puts the composition on the lower boundary for ferroan platinum and confirms earlier analyses using other methods such as Scanning Electron Microscopy-Energy Dispersive X-ray analysis/microprobe. The binding energy of the Pt 4f5/2 was 74.0 eV and Pt 4f7/2 70.5 eV, while the Fe 2p3/2 for metallic Fe was observed at 707.2 eV. The Fe 2p3/2 for metallic Fe was significantly sharper than that of Fe 2p3/2 at 710.7 eV associated with surface material. The Raman spectrum was dominated by the Pt–Pt stretching mode at 253 cm?1. Changed orientation resulted in the observation of two bands at 127 and 139 cm?1, interpreted as being due to stretching modes of two Pt–Pt bonds with the third bond to Fe and Pt fixed. The presence of Ca-Fe-Al-Mg-Si-O on the surface was probably associated with the presence of a clinopyroxene. These minerals can be expected since the crystal came originally from a clinopyroxenite-dunite matrix. The spectra showed a variety of interferences, e.g. Al 2p with Pt 4f, Mg 2p with Fe 3p, and Ca 2p1/2 with Mg Auger, making exact determinations of the ratios of these elements difficult.
关键词： surface chemistry,platinum group minerals,X-ray photoelectron spectroscopy,Raman spectroscopy,Platinum
更新于2025-09-23 15:23:52
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Diamond like carbon films with embedded Cu nanoclusters deposited by reactive high power impulse magnetron sputtering: Pulse length effects
摘要： In the present study diamond like carbon films with embedded Cu nanoclusters (DLC:Cu films) were deposited by reactive high power impulse magnetron sputtering (HIPIMS). HIPIMS pulse length (pulse on time) effects were considered. The dependence of the chemical composition on pulse length was found. Structure of diamond like carbon matrix of the nanocomposite films studied by Raman scattering spectroscopy has indicated weak increase of the sp3/sp2 carbon bond ratio with HIPIMS pulse length. Studies of the shape and dimensions of copper nanoclusters performed by He ion microscopy have shown that increase of the HIPIMS pulse on time resulted in increased number of the nanoclusters and subsequent increase of the Cu nanoclusters size. Study of optical properties revealed surface plasmon resonance effect in all investigated films. Correlation between the optical absorption spectra and photoexcited charge carrier relaxation time recorded by the pump probe spectroscopy was found. The highest relaxation time was observed at the excitation wavelength close to the absorption surface plasmon resonance peak wavelength The highest maximum relaxation time was observed for the DLC:Cu film deposited by using HIPIMS pulse of 400 μs on time. It was explained by the dependence of the relaxation time on Cu nanocluster size.
关键词： Pulse length,Diamond-like carbon,High-power pulsed magnetron sputtering,Structure,Optical properties,X-ray photoelectron spectroscopy,Copper,Nanoclusters
更新于2025-09-23 15:23:52
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Signal enhancement in laser diode thermal desorption-triple quadrupole mass spectrometry analysis using microwell surface coatings
摘要： Laser diode thermal desorption (LDTD) is an ionization source usually coupled to triple quadrupole mass spectrometry (QqQMS) and specifically designed for laboratories requiring high-throughput analysis. It has been observed that surface coatings on LDTD microwell plates can improve the sensitivity of the analysis of small polar molecules. The objective of the present study is to understand and quantify the effect of microwell surface coatings on signal intensity of small organic molecules of clinical, environmental and forensic interest. Experiments showed that the peak areas of diclofenac, chloramphenicol, salicylic acid and 11-nor-9-carboxy-Δ9-tetrahydrocannabinol obtained by LDTD-QqQMS increased by up to 3 orders of magnitude when using microwells coated with ethylenediaminetetraacetic acid (EDTA). Tests with different chelating agents and polytetrafluoroethylene as microwell surface coatings showed that nitrilotriacetic acid gave significantly higher peak areas for five out of the nine compounds that showed signal enhancement using chelating agents as coatings. Scanning electron microscopy studies of EDTA-coated and uncoated microwells showed that analytes deposited in the former formed more uniform and thinner films than in the latter. The enhancement effect of surface coatings in LDTD-QqQMS was explained mainly by the formation of homogenous and thinner layers of nanocrystals of analytes that are easier to desorb thermally than the layers formed when the analytes dry in direct contact with the bare stainless steel surface. Chemisorption of some analytes to the stainless steel surface of the microwell plate appeared to be a minor factor. Surface coatings widen the number of compounds analyzable by LDTD-QqQMS and can also improve sensitivity and limits of detection.
关键词： pharmaceuticals,high-throughput,hormones,pesticides,x-ray photoelectron spectroscopy,scanning electron microscopy,stainless steel,small organic molecules,chelating agents
更新于2025-09-23 15:23:52
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Effect of Oxygen on Thermal and Radiation Induced Chemistries in a Model Organotin Photoresist
摘要： Organotin photoresists have shown promise for next generation lithography due to their high extreme ultraviolet (EUV) absorption cross sections, their radiation sensitive chemistries, and their ability to enable high-resolution patterning. To better understand both temperature and radiation induced reaction mechanisms, we have studied a model EUV photoresist, which consists of a charge-neutral butyl-tin cluster. Temperature programmed desorption (TPD) showed very little outgassing of the butyl-tin resist in ultrahigh vacuum, and excellent thermal stability of the butyl groups. TPD results indicated that decomposition of the butyl-tin resist was first order with a fairly constant decomposition energy between 2.4 and 3.0 eV, which was determined by butyl group desorption. Electron stimulated desorption (ESD) showed that butyl groups were the primary decomposition product for electron kinetic energies expected during EUV exposures. XPS was performed before and after low energy electron exposure to evaluate the compositional and chemical changes in the butyl-tin resists after interaction with radiation. The effect of molecular oxygen during ESD experiments was evaluated and it was found to enhance butyl group desorption during exposure, and resulted in a significant increase in the ESD cross section by over 20%. These results provide mechanistic information that can be applied to organotin EUV photoresists, where a significant increase in photoresist sensitivity may be obtained by varying the ambient conditions during EUV exposures.
关键词： X-ray photoelectron spectroscopy,electron stimulated desorption,Extreme ultraviolet lithography,organotin photoresist,temperature programmed desorption
更新于2025-09-23 15:23:52
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Biodegradability of Disulfide-Organosilica Nanoparticles Evaluated by Soft X-ray Photoelectron Spectroscopy: Cancer Therapy Implications
摘要： Two kinds of organosilica nanoparticles (NPs) that were fabricated from thiol-containing precursors, (3-mercaptopropyl)trimethoxysilane and (3-mercaptopropyl)methyldimethoxysilane (MPDMS), are potential delivery vehicles of anticancer drugs. MPMS can form three siloxane bonds, but MPDMS forms two siloxane bonds as the maximum limit. Hence, disulfide bonds can be involved in the three-dimensional morphology of MPDMS NPs. In addition, NPs containing disulfide bonds are potentially degraded by a reduced form of glutathione (GSH). To examine reactions between the organosilica NPs and GSH, the NPs were incubated in 10 mM GSH aqueous solution at 37 °C for 7 d and the products were analyzed using field-emission scanning electron microscopy (FE-SEM), Raman spectroscopy, and soft X-ray photoelectron spectroscopy (XPS). The Raman spectra showed the presence of disulfide bonds in the MPDMS NPs and the absence of disulfide bonds in MPMS NPs. The results of XPS measurements suggested that the disulfide bonds in the outer layer of MPDMS NPs were reduced to thiol groups. FE-SEM observations of MPDMS NPs detected changes in NP morphology after the GSH incubation. These results support the idea that MPDMS NPs contain disulfide bonds and are degradable by GSH. Therefore, MPDMS NPs possess a biodegradable feature that is advantageous for clinical translation, that is, nanomedicine.
关键词： (3-mercaptopropyl)methyldimethoxysilane,nanoparticles,(3-mercaptopropyl)trimethoxysilane,biodegradability,glutathione,X-ray photoelectron spectroscopy,Raman spectroscopy
更新于2025-09-23 15:22:29