Controlled Stepwise Growth of Siloxane Chains Using Bivalent Building Units With Different Functionalities

2010 ◽  
Vol 1272 ◽  
Author(s):  
Nils Salingue ◽  
Dominic Lingenfelser ◽  
Pavel Prunici ◽  
Hess Peter
Keyword(s):  
Photoelectron Spectroscopy ◽  
Attenuated Total Reflection ◽  
Silicon Surfaces ◽  
Chain Growth ◽  
One Dimensional ◽  
X Ray ◽  
Sioh Group ◽  
Wet Chemical ◽  
Chemical Condensation

AbstractOrganic/inorganic hybrids of silicon and their subsequent chemical modification are of interest for tailoring and structuring surfaces on the nanoscale. The formation of monolayers on hydroxylated silicon surfaces was employed to synthesize molecular dimethylsiloxane chains by wet-chemical condensation reactions, using dimethylmonochlorosilane as the precursor. The SiH group of the resulting dimethylsilyl termination could be selectively oxidized to the SiOH group, which opened the possibility of bonding another species. By repeating the condensation and oxidation cycle the stepwise growth of one-dimensional dimethylsiloxane chains was achieved. The ongoing chain growth was characterized by attenuated total reflection (ATR) Fourier transform infrared (FTIR) spectroscopy, x-ray photoelectron spectroscopy (XPS), spectroscopic ellipsometry (SE), and determination of the surface energy by contact-angle experiments.

Chemical Structures of Native Oxides Formed During Wet Chemical Treatments on NH4F Treated Si(111) Surfaces

1992 ◽  
Vol 259 ◽  
Author(s):  
Takeo Hattori ◽  
Hiroki Ogawa
Keyword(s):  
Photoelectron Spectroscopy ◽  
Attenuated Total Reflection ◽  
Native Oxide ◽  
X Ray ◽  
Chemical Treatments ◽  
Chemical Structures ◽  
Native Oxides ◽  
Ft Ir ◽  
Wet Chemical ◽  
Silicon Interface

ABSTRACTChemical structures of native oxides formed during wet chemical treatments on NH4F treated Si(111) surfaces were investigated using X-ray Photoelectron Spectroscopy (XPS) and Fourier Transformed Infrared Attenuated Total Reflection(FT-IR-ATR). It was found that the amounts of Si-H bonds in native oxides and those at native oxide/silicon interface are negligibly small in the case of native oxides formed in H2SO4-H2O2-H2O solution. Based on this discovery, it was confirmed that native oxides can be characterized by the amount of Si-H bonds in native oxides. Furthermore, it was found that the combination of various wet chemical treatments with the treatment in NH4OH-H2O2-H2O solution results in the drastic decrease in the amount of Si-H bonds in native oxides.

scholarly journals An Insight into Chemistry and Structure of Colloidal 2D-WS2 Nanoflakes: Combined XPS and XRD Study

Nanomaterials ◽  
2021 ◽  
Vol 11 (8) ◽  
pp. 1969
Author(s):  
Riccardo Scarfiello ◽  
Elisabetta Mazzotta ◽  
Davide Altamura ◽  
Concetta Nobile ◽  
Rosanna Mastria ◽  
...  
Keyword(s):  
Photoelectron Spectroscopy ◽  
Xrd Analysis ◽  
Crystal Habit ◽  
Phase Identification ◽  
X Ray Diffraction ◽  
X Ray ◽  
Morphological Evaluation ◽  
Rational Understanding ◽  
Structural Inspection

The surface and structural characterization techniques of three atom-thick bi-dimensional 2D-WS2 colloidal nanocrystals cross the limit of bulk investigation, offering the possibility of simultaneous phase identification, structural-to-morphological evaluation, and surface chemical description. In the present study, we report a rational understanding based on X-ray photoelectron spectroscopy (XPS) and structural inspection of two kinds of dimensionally controllable 2D-WS2 colloidal nanoflakes (NFLs) generated with a surfactant assisted non-hydrolytic route. The qualitative and quantitative determination of 1T’ and 2H phases based on W 4f XPS signal components, together with the presence of two kinds of sulfur ions, S22− and S2−, based on S 2p signal and related to the formation of WS2 and WOxSy in a mixed oxygen-sulfur environment, are carefully reported and discussed for both nanocrystals breeds. The XPS results are used as an input for detailed X-ray Diffraction (XRD) analysis allowing for a clear discrimination of NFLs crystal habit, and an estimation of the exact number of atomic monolayers composing the 2D-WS2 nanocrystalline samples.

Formalism for the determination of intermediate stress gradients using X-ray diffraction

2009 ◽  
Vol 42 (2) ◽  
pp. 192-197 ◽  
Author(s):  
Thomas Gnäupel-Herold
Keyword(s):  
Lattice Strain ◽  
Narrow Line ◽  
X Ray Diffraction ◽  
Beam Spot ◽  
Strain Measurements ◽  
One Dimensional ◽  
X Ray ◽  
Stress Gradients ◽  
Shaped Beam

A method is outlined that allows the determination of one-dimensional stress gradients at length scales greater than 0.2 mm. By using standard four-circle X-ray diffractometer equipment and simple aperture components, length resolutions down to 0.05 mm in one direction can be achieved through constant orientation of a narrow, line-shaped beam spot. Angle calculations are given for the adjustment of goniometer angles, and for the effective azimuth and tilt of the scattering vector for general angle settings in a four-circle goniometer. The latter is necessary for the computation of stresses from lattice strain measurements.

Incorporation and Role of Nitrogen During Oxynitridation of Silicon Studied by Photoelectron Spectroscopy

1999 ◽  
Vol 567 ◽  
Author(s):  
Masayuki Suzuki ◽  
Yoji Saito
Keyword(s):  
Photoelectron Spectroscopy ◽  
High Vacuum ◽  
Oxide Films ◽  
Silicon Surfaces ◽  
Gaseous Mixtures ◽  
X Ray ◽  
Initial Stage ◽  
Thermal Stability Of

ABSTRACTWe tried direct oxynitridation of silicon surfaces by remote-plasma-exited nitrogen and oxygen gaseous mixtures at 700°C in a high vacuum. The oxynitrided surfaces were investigated with in-situ X-ray photoelectron spectroscopy. With increase of the oxynitridation time, the surface density of nitrogen gradually increases, but that of oxygen shows nearly saturation behavior after the rapid increase in the initial stage. We also annealed the grown oxynitride and oxide films to investigate the role of the contained nitrogen. The desorption rate of oxygen from the oxynitride films is much less than that from oxide films. We confirmed that nitrogen stabilizes the thermal stability of these oxynitride films.

A Two-step Electrodeposition of Pd-Cu/Cu2O Nanocomposite on FTO Substrate for Non-enzymatic Hydrogen Peroxide Sensor

2021 ◽  
Vol 17 ◽  
Author(s):  
Ke Huan ◽  
Li Tang ◽  
Dongmei Deng ◽  
Huan Wang ◽  
Xiaojing Si ◽  
...  
Keyword(s):  
Hydrogen Peroxide ◽  
Cyclic Voltammetry ◽  
Photoelectron Spectroscopy ◽  
Chemical Structure ◽  
Pd Nanoparticles ◽  
Optimal Conditions ◽  
Potential Oscillation ◽  
X Ray Diffraction ◽  
X Ray

Background: Hydrogen peroxide (H2O2) is a common reagent in the production and living, but excessive H2O2 may enhance the danger to the human body. Consequently, it is very important to develop economical, fast and accurate techniques for detecting H2O2. Methods: A simple two-step electrodeposition process was applied to synthesize Pd-Cu/Cu2O nanocomposite for non-enzymatic H2O2 sensor. Cu/Cu2O nanomaterial was firstly electrodeposited on FTO by potential oscillation technique, and then Pd nanoparticles were electrodeposited on Cu/Cu2O nanomaterial by cyclic voltammetry. The chemical structure, component, and morphology of the synthesized Pd-Cu/Cu2O nanocomposite were characterized by X-ray diffraction, scanning electron microscopy and X-ray photoelectron spectroscopy. The electrochemical properties of Pd-Cu/Cu2O nanocomposite were studied by cyclic voltammetry and amperometry. Results: Under optimal conditions, the as-fabricated sensor displayed a broad linear range (5-4000 µM) and low detection limit (1.8 µM) for the determination of H2O2. The proposed sensor showed good selectivity and reproducibility. Meanwhile, the proposed sensor has been successfully applied to detect H2O2 in milk. Conclusion: The Pd-Cu/Cu2O/FTO biosensor exhibits excellent electrochemical activity for H2O2 reduction, which has great potential application in the field of food safety.

scholarly journals Graphitic Nitrogen in Carbon Catalysts Important for the Reduction of Nitrite Revealed by 15N NMR Spectroscopy at Natural Abundance

2020 ◽  
Author(s):  
Zheng Chen ◽  
Aleksander Jaworski ◽  
Jianhong Chen ◽  
Tetyana Budnyak ◽  
Ireneusz Szewczyk ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Photoelectron Spectroscopy ◽  
Reduction Reaction ◽  
Nitrite Reduction ◽  
15N Nmr ◽  
Carbon Catalyst ◽  
X Ray ◽  
Wide Range ◽  
Alkaline Conditions

Metal-free nitrogen-doped carbon is considered as a green functional material, but the structural determination of the atomic positions of nitrogen remains challenging. We recently demonstrated that directly-excited solid state <sup>15</sup>N NMR (ssNMR) spectroscopy is a powerful tool for the determination of such positions in an N-doped carbon at natural <sup>15</sup>N isotope abundance. Here we present a green chemistry approach to the synthesis of N-doped carbon using cellulose as precursor, and a study of the catalytic properties and atomic structures of the related catalyst. The N-doped carbon (NH<sub>3</sub>) was obtained by oxidation of cellulose with HNO<sub>3</sub> followed by ammonolysis at 800°C. It had a N content of 6.5 wt.% and a surface area of 557 m<sup>2 </sup>g<sup>–1</sup>, and <sup>15</sup>N ssNMR spectroscopy provided evidence for graphitic nitrogen besides of regular pyrrolic and pyridinic nitrogen. This structure determination enabled probing the role of graphitic nitrogen for electrocatalytic reactions, such as the hydrogen evolution reaction (HER), oxygen evolution reaction (OER), and nitrite reduction reaction. The N-doped carbon catalyst (NH<sub>3</sub>) had higher electrocatalytic activities in OER and HER under alkaline conditions and a higher activity for nitrite reduction, as compared with a catalyst prepared by carbonization of the HNO<sub>3</sub>-treated cellulose in N<sub>2</sub>. The electrocatalytic selectivity for nitrite reduction of the N-doped carbon catalyst (NH<sub>3</sub>) was directly related to the graphitic nitrogen functions. Complementary structural analysis by means of <sup>13</sup>C and <sup>1</sup>H ssNMR, scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, and low-temperature N<sub>2 </sub>adsorption were preformed and provided support to the findings. The results show that directly-excited <sup>15</sup>N ssNMR at natural <sup>15</sup>N abundance is generally capable to provide information on N-doped carbon materials, and it is expected that the approach can be applied to a wide range of solids with an intermediate amount of N atoms.

Chemical Structure of Native Oxide Grown on Hydrogenterminated Silicon Surfaces

1992 ◽  
Vol 259 ◽  
Author(s):  
M. Takakura ◽  
T. Yasaka ◽  
S. Miyazaki ◽  
M. Hirose
Keyword(s):  
Photoelectron Spectroscopy ◽  
Chemical Structure ◽  
Pure Water ◽  
Silicon Surfaces ◽  
Native Oxide ◽  
Appreciable Amount ◽  
X Ray ◽  
Thermal Oxide ◽  
Phonon Peak ◽  
Strained Bonds

ABSTRACTChemical bonding features and suboxide compositions in native oxide grown on chemically-cleaned hydrogen-terminated Si(100) surfaces stored in pure water have been studied by using surface sensitive infrared spectroscopy and x-ray photoelectron spectroscopy. The LO phonon peak for the native oxide is located at 1210cm−1, which is shifted to a significantly lower wavenumber side than the ultrathin thermal oxide peak at 1250cm−1. This is because an appreciable amount of SiHx bonds are incorporated in the native oxide/Si interface and such hydrogen termination in the network dramatically reduces strained bonds in the interface. Very weak Si2+ suboxide signal from the oxide grown in pure water is also explained by the incorporated SiHx bonds which interrupt the Si2+ suboxide formation in the interface.

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