scholarly journals The in situ synthesis of PbS nanocrystals from lead(II) n -octylxanthate within a 1,3-diisopropenylbenzene–bisphenol A dimethacrylate sulfur copolymer

2017 ◽  
Vol 4 (8) ◽  
pp. 170383 ◽  
Author(s):  
P. D. McNaughter ◽  
J. C. Bear ◽  
A. G. Mayes ◽  
I. P. Parkin ◽  
P. O'Brien

The synthesis of lead sulfide nanocrystals within a solution processable sulfur ‘inverse vulcanization’ polymer thin film matrix was achieved from the in situ thermal decomposition of lead(II) n -octylxanthate, [Pb(S 2 COOct) 2 ]. The growth of nanocrystals within polymer thin films from single-source precursors offers a faster route to networks of nanocrystals within polymers when compared with ex situ routes. The ‘inverse vulcanization’ sulfur polymer described herein contains a hybrid linker system which demonstrates high solubility in organic solvents, allowing solution processing of the sulfur-based polymer, ideal for the formation of thin films. The process of nanocrystal synthesis within sulfur films was optimized by observing nanocrystal formation by X-ray photoelectron spectroscopy and X-ray diffraction. Examination of the film morphology by scanning electron microscopy showed that beyond a certain precursor concentration the nanocrystals formed were not only within the film but also on the surface suggesting a loading limit within the polymer. We envisage this material could be used as the basis of a new generation of materials where solution processed sulfur polymers act as an alternative to traditional polymers.

2002 ◽  
Vol 17 (7) ◽  
pp. 1622-1633 ◽  
Author(s):  
Xiaowu Fan ◽  
Mi-Kyoung Park ◽  
Chuanjun Xia ◽  
Rigoberto Advincula

Nanostructured montmorillonite/poly(diallyldimethylammonium chloride) multilayer thin films were fabricated up to 100 layers thick by stepwise alternating polyelectrolyte and clay deposition from solution. The structure and morphology of the films were characterized by x-ray diffraction, ellipsometry, atomic force microscopy, and quartz crystal microbalance ex situ and in situ measurements. The mechanical properties were tested by nanoindentation. The hardness of the multilayer thin film was 0.46 GPa. The thin film's modulus was correlated to its ordering and anisotropic structure. Both hardness and modulus of this composite film were higher than those of several other types of polymer thin films.


1999 ◽  
Vol 14 (2) ◽  
pp. 436-441 ◽  
Author(s):  
S. Logothetidis ◽  
E. I. Meletis ◽  
G. Kourouklis

In situ and ex situ spectroscopic ellipsometry (SE), Raman spectroscopy (RS), x-ray photoelectron spectroscopy (XPS), and Auger electron spectroscopy (AES) have been used to study the stoichiometry and characterize TiNx thin films deposited by magnetron sputtering at various stoichiometries. In situ SE can provide parameters, such as the plasma energy, that can be utilized for monitoring of the film stoichiometry. Besides plasma energy, optical phonon position in RS was also found to be a sensitive probe of TiNx stoichiometry as detected by RS, XPS, and ex situ SE. Under these conditions, AES faces difficulties for reliable film characterization, and the complementary use of other techniques is required for determining the exact film stoichiometry.


Author(s):  
Maurizio De Santis ◽  
Aude Bailly ◽  
Ian Coates ◽  
Stéphane Grenier ◽  
Olivier Heckmann ◽  
...  

Cobalt ferrite ultrathin films with the inverse spinel structure are among the best candidates for spin filtering at room temperature. High-quality epitaxial CoFe2O4 films about 4 nm thick have been fabricated on Ag(001) following a three-step method: an ultrathin metallic CoFe2 alloy was first grown in coherent epitaxy on the substrate and then treated twice with O2, first at room temperature and then during annealing. The epitaxial orientation and the surface, interface and film structure were resolved using a combination of low-energy electron diffraction, scanning tunnelling microscopy, Auger electron spectroscopy and in situ grazing-incidence X-ray diffraction. A slight tetragonal distortion was observed, which should drive the easy magnetization axis in-plane due to the large magneto-elastic coupling of such a material. The so-called inversion parameter, i.e. the Co fraction occupying octahedral sites in the ferrite spinel structure, is a key element for its spin-dependent electronic gap. It was obtained through in situ resonant X-ray diffraction measurements collected at both the Co and Fe K edges. The data analysis was performed using FDMNES, an ab initio program already extensively used to simulate X-ray absorption spectroscopy, and shows that the Co ions are predominantly located on octahedral sites with an inversion parameter of 0.88 (5). Ex situ X-ray photoelectron spectroscopy gives an estimation in accordance with the values obtained through diffraction analysis.


1990 ◽  
Vol 191 ◽  
Author(s):  
Ming Y. Chen ◽  
P. Terrence Murray

ABSTRACTThin films of TiO2 have been grown by pulsed laser evaporation. The films were analyzed by in-situ Auger and x-ray photoelectron spectroscopy as well as by ex-situ grazing incidence xray diffraction. Films grown at room temperature and at a pressure of 5×10minus; 3 Torr were oxygen deficient. Films grown at 500°C and higher were found to be stoichiometric TiO2.The effect of substrate temperature and evaporation conditions on film properties will be discussed.


Author(s):  
Tianlei Ma ◽  
Marek Nikiel ◽  
Andrew G. Thomas ◽  
Mohamed Missous ◽  
David J. Lewis

AbstractIn this report, we prepared transparent and conducting undoped and molybdenum-doped tin oxide (Mo–SnO2) thin films by aerosol-assisted chemical vapour deposition (AACVD). The relationship between the precursor concentration in the feed and in the resulting films was studied by energy-dispersive X-ray spectroscopy, suggesting that the efficiency of doping is quantitative and that this method could potentially impart exquisite control over dopant levels. All SnO2 films were in tetragonal structure as confirmed by powder X-ray diffraction measurements. X-ray photoelectron spectroscopy characterisation indicated for the first time that Mo ions were in mixed valence states of Mo(VI) and Mo(V) on the surface. Incorporation of Mo6+ resulted in the lowest resistivity of $$7.3 \times 10^{{ - 3}} \Omega \,{\text{cm}}$$ 7.3 × 10 - 3 Ω cm , compared to pure SnO2 films with resistivities of $$4.3\left( 0 \right) \times 10^{{ - 2}} \Omega \,{\text{cm}}$$ 4.3 0 × 10 - 2 Ω cm . Meanwhile, a high transmittance of 83% in the visible light range was also acquired. This work presents a comprehensive investigation into impact of Mo doping on SnO2 films synthesised by AACVD for the first time and establishes the potential for scalable deposition of SnO2:Mo thin films in TCO manufacturing. Graphical abstract


2010 ◽  
Vol 89-91 ◽  
pp. 503-508 ◽  
Author(s):  
J. Sheng ◽  
U. Welzel ◽  
Eric J. Mittemeijer

The stress evolution during diffusion annealing of Ni-Cu bilayers (individual layer thicknesses of 50 nm) was investigated employing ex-situ and in-situ X-ray diffraction measurements. Annealing at relatively low homologous temperatures (about 0.3 - 0.4 Tm) for durations up to about 100 hours results in considerable diffusional intermixing, as demonstrated by Auger-electron spectroscopy investigations (in combination with sputter-depth profiling). In addition to thermal stresses due to differences of the coefficients of thermal expansion of layers and substrate, tensile stress con-tributions in the sublayers arise during the diffusion anneals. The obtained stress data have been discussed in terms of possible mechanisms of stress generation. The influence of diffusion on stress development in the sublayers of the diffusion couple during heating and isothermal annealing was investigated by comparing stress changes in the bilayer system with corresponding results obtained under identical conditions for single layers of the components in the bilayer system. The specific residual stresses that emerge due to diffusion between the (sub)layers in the bilayer could thereby be identified.


Surfaces ◽  
2021 ◽  
Vol 4 (2) ◽  
pp. 106-114
Author(s):  
Yannick Hermans ◽  
Faraz Mehmood ◽  
Kerstin Lakus-Wollny ◽  
Jan P. Hofmann ◽  
Thomas Mayer ◽  
...  

Thin films of ZnWO4, a promising photocatalytic and scintillator material, were deposited for the first time using a reactive dual magnetron sputtering procedure. A ZnO target was operated using an RF signal, and a W target was operated using a DC signal. The power on the ZnO target was changed so that it would match the sputtering rate of the W target operated at 25 W. The effects of the process parameters were characterized using optical spectroscopy, X-ray diffraction, and scanning electron microscopy, including energy dispersive X-ray spectroscopy as well as X-ray photoelectron spectroscopy. It was found that stoichiometric microcrystalline ZnWO4 thin films could be obtained, by operating the ZnO target during the sputtering procedure at a power of 55 W and by post-annealing the resulting thin films for at least 10 h at 600 °C. As FTO coated glass substrates were used, annealing led as well to the incorporation of Na, resulting in n+ doped ZnWO4 thin films.


2021 ◽  
pp. 150898
Author(s):  
Makoto Takayanagi ◽  
Takashi Tsuchiya ◽  
Shigenori Ueda ◽  
Tohru Higuchi ◽  
Kazuya Terabe

2012 ◽  
Vol 90 (1) ◽  
pp. 39-43 ◽  
Author(s):  
X. Xiang ◽  
D. Chang ◽  
Y. Jiang ◽  
C.M. Liu ◽  
X.T. Zu

Anatase TiO2 thin films are deposited on K9 glass samples at different substrate temperatures by radio frequency magnetron sputtering. N ion implantation is performed in the as-deposited TiO2 thin films at ion fluences of 5 × 1016, 1 × 1017, and 5 × 1017 ions/cm2. X-ray diffraction, atomic force microscope, X-ray photoelectron spectroscopy (XPS), and UV–visible spectrophotometer are used to characterize the films. With increasing N ion fluences, the absorption edges of anatase TiO2 films shift to longer wavelengths and the absorbance increases in the visible light region. XPS results show that the red shift of TiO2 films is due to the formation of N–Ti–O compounds. As a result, photoactivity is enhanced with increasing N ion fluence.


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