Adsorption and Thermal Decomposition of Tetrakis(dimethylamido)titanium on Si and SiO2/Si Surfaces: an XPS Study

1995 ◽  
Vol 60 (3) ◽  
pp. 372-382 ◽  
Author(s):  
Michaela Janovská ◽  
Zdeněk Bastl

X-Ray photoelectron spectroscopy (XPS) has been used to study adsorption of tetrakis(dimethylamido)titanium (TDMT) on a clean Si surface and surface on which an oxide layer was grown prior to TDMT adsorption. Measurements were carried out at temperatures 80 and 295 K. In addition, decomposition of TDMT on the above substrates yielding titanium nitride coatings was investigated. The change in surface composition as a function of TiNx layer thickness was monitored by XPS. Adsorption at 80 K proceeds without dissociation on both substrates. Photoelectron spectra measured at 295 K indicate presence of surface species containing C-N multiple bond on both substrates and on SiO2/Si substrate formation of species that contain Ti-N-C rings. At 580 K an overlayer consisting predominantly of TiNx was produced by pyrolysis of TDMT. The photoelectron spectra revealed also presence of species with C-N-C, Si-CHx and Ti-C bonds the concentration of which depended on an overlayer thickness. On SiO2/Si substrate decomposition of SiO2 accompanied by titanium oxide formation occurs during initial stages of TDMT pyrolysis.

1989 ◽  
Vol 154 ◽  
Author(s):  
P.V. Nagarkar ◽  
E.K. Sichela ◽  
G.L. Doll

AbstractAn x-ray photoelectron spectroscopy (XPS) study of laser treated and heat treated Kapton®indicates that both the treatments result in depleting the carbonyl groups from the sample and leave behind a conducting residue that still contains significant amounts of oxygen and nitrogen. The rapid changes in surface composition coincide with a substantial decrease in the electrical resistivity of the polyimide samples.


2020 ◽  
Author(s):  
Jennifer A. Rudd ◽  
Ewa Kazimierska ◽  
Louise B. Hamdy ◽  
Odin Bain ◽  
Sunyhik Ahn ◽  
...  

The utilization of carbon dioxide is a major incentive for the growing field of carbon capture. Carbon dioxide could be an abundant building block to generate higher value products. Herein, we describe the use of porous copper electrodes to catalyze the reduction of carbon dioxide into higher value products such as ethylene, ethanol and, notably, propanol. For <i>n</i>-propanol production, faradaic efficiencies reach 4.93% at -0.83 V <i>vs</i> RHE, with a geometric partial current density of -1.85 mA/cm<sup>2</sup>. We have documented the performance of the catalyst in both pristine and urea-modified foams pre- and post-electrolysis. Before electrolysis, the copper electrode consisted of a mixture of cuboctahedra and dendrites. After 35-minute electrolysis, the cuboctahedra and dendrites have undergone structural rearrangement. Changes in the interaction of urea with the catalyst surface have also been observed. These transformations were characterized <i>ex-situ</i> using scanning electron microscopy, X-ray diffraction, and X-ray photoelectron spectroscopy. We found that alterations in the morphology, crystallinity, and surface composition of the catalyst led to the deactivation of the copper foams.


2018 ◽  
Vol 196 ◽  
pp. 04005
Author(s):  
Irina Stepina ◽  
Irina Kotlyarova

The difficulty of wood protection from biocorrosion and fire is due to the fact that modifiers in use are washed out from the surface of the substrate under the influence of environmental factors. This results in a rapid loss of the protective effect and other practically important wood characteristics caused by the modification. To solve this problem is the aim of our work. Here, monoethanolaminoborate is used as a modifier, where electron-donating nitrogen atom provides a coordination number equal to four to a boron atom, which determines the hydrolytic stability of the compounds formed. Alpha-cellulose ground mechanically to a particle size of 1 mm at most was used as a model compound for the modification. X-ray photoelectron spectra were recorded on the XSAM-800 spectrometer (Kratos, UK). Prolonged extraction of the modified samples preceded the registration of the photoelectron spectra to exclude the fixation of the modifier molecules unreacted with cellulose. As a result of the experiment, boron and nitrogen atoms were found in the modified substrate, which indicated the hydrolytic stability of the bonds formed between the modifier molecules and the substrate. Therefore monoethanolaminoborate can be considered as a non-extractable modifier for wood-cellulose materials.


Author(s):  
Mariola Kądziołka-Gaweł ◽  
Maria Czaja ◽  
Mateusz Dulski ◽  
Tomasz Krzykawski ◽  
Magdalena Szubka

AbstractMössbauer, Raman, X-ray diffraction and X-ray photoelectron spectroscopies were used to examine the effects of temperature on the structure of two aluminoceladonite samples. The process of oxidation of Fe2+ to Fe3+ ions started at about 350 °C for the sample richer in Al and at 300 °C for the sample somewhat lower Al-content. Mössbauer results show that this process may be associated with dehydroxylation or even initiate it. The first stage of dehydroxylation takes place at a temperature > 350 °C when the adjacent OH groups are replaced with a single residual oxygen atom. Up to ~500 °C, Fe ions do not migrate from cis-octahedra to trans-octahedra sites, but the coordination number of polyhedra changes from six to five. This temperature can be treated as the second stage of dehydroxylation. The temperature dependence on the integral intensity ratio between bands centered at ~590 and 705 cm−1 (I590/I705) clearly reflects the temperature at which six-coordinated polyhedra are transformed into five-coordinated polyhedra. X-ray photoelectron spectra obtained in the region of the Si2p, Al2p, Fe2p, K2p and O1s core levels, highlighted a route to identify the position of Si, Al, K and Fe cations in a structure of layered silicates with temperature. All the measurements show that the sample with a higher aluminum content and a lower iron content in octahedral sites starts to undergo a structural reorganization at a relatively higher temperature than the less aluminum-rich sample does. This suggests that iron may perform an important role in the initiation of the dehydroxylation of aluminoceladonites.


Materials ◽  
2018 ◽  
Vol 11 (9) ◽  
pp. 1725 ◽  
Author(s):  
Xiaohong Liu ◽  
Ming Li ◽  
Xuemei Zheng ◽  
Elias Retulainen ◽  
Shiyu Fu

As a type of functional group, azo-derivatives are commonly used to synthesize responsive materials. Cellulose nanocrystals (CNCs), prepared by acid hydrolysis of cotton, were dewatered and reacted with 2-bromoisobuturyl bromide to form a macro-initiator, which grafted 6-[4-(4-methoxyphenyl-azo) phenoxy] hexyl methacrylate (MMAZO) via atom transfer radical polymerization. The successful grafting was supported by Fourier transform infrared spectroscopy (FT-IR) and Solid magnetic resonance carbon spectrum (MAS 13C-NMR). The morphology and surface composition of the poly{6-[4-(4-methoxyphenylazo) phenoxy] hexyl methacrylate} (PMMAZO)-grafted CNCs were confirmed with Transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS). The grafting rate on the macro-initiator of CNCs was over 870%, and the polydispersities of branched polymers were narrow. The crystal structure of CNCs did not change after grafting, as determined by X-ray diffraction (XRD). The polymer PMMAZO improved the thermal stability of cellulose nanocrystals, as shown by thermogravimetry analysis (TGA). Then the PMMAZO-grafted CNCs were mixed with polyurethane and casted to form a composite film. The film showed a significant light and pH response, which may be suitable for visual acid-alkali measurement and reversible optical storage.


2018 ◽  
Vol 122 (10) ◽  
pp. 2695-2702 ◽  
Author(s):  
E. Antonsson ◽  
C. Raschpichler ◽  
B. Langer ◽  
D. Marchenko ◽  
E. Rühl

2006 ◽  
Vol 600 (18) ◽  
pp. 3749-3752 ◽  
Author(s):  
C. Biswas ◽  
S. Banik ◽  
A.K. Shukla ◽  
R.S. Dhaka ◽  
V. Ganesan ◽  
...  

2014 ◽  
Vol 16 (39) ◽  
pp. 21486-21495 ◽  
Author(s):  
Josephina Werner ◽  
Jan Julin ◽  
Maryam Dalirian ◽  
Nønne L. Prisle ◽  
Gunnar Öhrwall ◽  
...  

The water–vapor interface of aqueous solutions of succinic acid, where pH values and bulk concentrations were varied, has been studied using surface sensitive X-ray photoelectron spectroscopy (XPS) and molecular dynamics (MD) simulations.


Author(s):  
Changqing Liu ◽  
David A. Hutt ◽  
Dezhi Li ◽  
Paul P. Conway

This paper aims to gain an insight into the correlation between the microstructure and surface composition of electroless Ni-P and its behaviour during soldering with Pb free alloys including Sn-3.8Ag-0.7Cu, Sn-3.5Ag and Sn-0.7Cu. Ni-P coatings with different P contents were produced through an industrial process on copper metal substrates. The surface morphology of these coatings was observed by Scanning Electron Microscopy (SEM) and the bulk composition was analyzed by means of Energy Dispersive X-ray analysis (EDX). The mechanical properties of the coatings were evaluated by nano-indentation testing under different maximum loads. However, to understand the behaviour of P in Ni-P coatings and deterioration of the coating surfaces during exposure to air, the surfaces of the coatings were also characterised by X-ray Photoelectron Spectroscopy (XPS) for storage at different temperatures. The dependence of the solderability of Ni-P coatings on the storage time and temperature was investigated by wetting balance testing, using an inactive or active flux with or without an inert N2 atmosphere. Finally, the solderability of Ni-P coatings to Pb free solders is correlated with their composition and microstructure (e.g. surface characteristics).


2002 ◽  
Vol 57 (2) ◽  
pp. 193-201 ◽  
Author(s):  
Gülsün Gökağaç ◽  
Brendan J. Kennedy

11% Pt/C, 10% Pt + 1%Os/C, 9% Pt + 2%Os/C, 8% Pt + 3%Os/C, 7% Pt + 4%Os/C, 6% Pt + 5%Os/C and 5%Pt + 6% Os/C catalysts have been prepared for methanol oxidation reaction. Transmission electron microscopy, X-ray photoelectron spectroscopy, X-ray diffraction and cyclic voltammetry have been used to understand the nature of the species present in these catalysts. 7% Pt + 4% Os/C was the most active catalyst, while 8% Pt + 3% Os/C was the least active one. It is found that the metal particle size and distribution on the carbon support, the surface composition and the oxidation states of the metal particles, the metal-metal and metal support interactions are important parameters to define the activity of the catalyst.


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