scholarly journals In-Operando Diffraction and Spectroscopic Evaluation of Pure, Zr-, and Ce-Doped Vanadium Dioxide Thermochromic Films Derived via Glycolate Synthesis

Nanomaterials ◽  
2020 ◽  
Vol 10 (12) ◽  
pp. 2537
Author(s):  
Stanislav Kurajica ◽  
Vilko Mandić ◽  
Ivana Panžić ◽  
Mattia Gaboardi ◽  
Katarina Mužina ◽  
...  
Keyword(s):  
Intermediate Phase ◽  
Solar Spectrum ◽  
Structural Evolution ◽  
Grazing Incidence ◽  
X Ray Diffraction ◽  
X Ray ◽  
Powder Samples ◽  
Zirconium Doping ◽  
In Operando ◽  
Transmission And Reflection

Pure and doped vanadia (VO2, V0.98Zr0.02O2, V0.98Ce0.02O2) samples were prepared by wet chemistry synthesis from vanadyl glycolate intermediate phase and tape casted into films. Combining in-operando grazing incidence synchrotron X-ray diffraction and Raman spectroscopy, we studied the structural evolution of the films under isothermal conditions. The setup allowed assessment of the thermochromic functionality with continuous monitoring of the monoclinic to tetragonal transition in pure and doped vanadia phases, responsible for the transmission and reflection of light in the infrared part of the solar spectrum. The materials characterisation by X-ray diffraction beamline (MCX) goniometer demonstrated ideal performance, combining flexible geometry, high resolution, and the potential to accommodate the multi-channel equipment for in-operando characterisation. This method proved viable for evaluating the relevant structural and physical, and thereof functional properties of these systems. We revealed that dopants reduce the transition temperature by 5 °C on average. The synthetic route of the films was held responsible for the observed phase separation. The more favourable behaviour of cerium-doped sample was attributed to cerium alkoxide behaviour. In addition, structural, microstructural, thermal, and spectroscopic characterisation on powder samples was performed to gain more insight into the development of the phases that are responsible for thermochromic features in a broader range of doping ratios. The influence of the dopants on the extent of the thermochromic transition (transmission to reflection hysteresis) was also evaluated using (micro) structural, thermal and spectroscopic methods of powder samples. Characterisations showed that zirconium doping in 2, 4, and 6 mol% significantly influenced the phase composition and morphology of the precursor. Vanadium oxides other than VO2 can easily crystallise; however, a thermal treatment regime that allowed crystallisation of VO2 as a single phase was established.

scholarly journals Structure-Dependent Mechanical Properties of ALD-Grown Nanocrystalline BiFeO3Multiferroics

2016 ◽  
Vol 2016 ◽  
pp. 1-7 ◽  
Author(s):  
Anna Majtyka ◽  
Anna Nowak ◽  
Benoît Marchand ◽  
Dariusz Chrobak ◽  
Mikko Ritala ◽  
...  
Keyword(s):  
Mechanical Properties ◽  
Photoelectron Spectroscopy ◽  
Present Report ◽  
Structural Evolution ◽  
Atomic Layer ◽  
Grazing Incidence ◽  
X Ray Diffraction ◽  
X Ray ◽  
Layer Deposition ◽  
Pertinent Information

The present paper pertains to mechanical properties and structure of nanocrystalline multiferroic BeFiO3(BFO) thin films, grown by atomic layer deposition (ALD) on the Si/SiO2/Pt substrate. The usage of sharp-tip-nanoindentation and multiple techniques of structure examination, namely, grazing incidence X-ray diffraction, X-ray photoelectron spectroscopy, scanning electron microscopy, and energy dispersive X-ray spectrometry, enabled us to detect changes in elastic properties(95 GPa≤E≤118 GPa)and hardness(4.50 GPa≤H≤7.96 GPa)of BFO after stages of annealing and observe their relation to the material’s structural evolution. Our experiments point towards an increase in structural homogeneity of the samples annealed for a longer time. To our best knowledge, the present report constitutes the first disclosure of nanoindentation mechanical characteristics of ALD-fabricated BeFiO3, providing a new insight into the phenomena that accompany structure formation and development of nanocrystalline multiferroics. We believe that our systematic characterization of the BFO layers carried out at consecutive stages of their deposition provides pertinent information which is needed to control and optimize its ALD fabrication.

Structural Transformations During Growth of Epitaxial Fe(001) Thin Films on Cu(001) and Pt(001)

1996 ◽  
Vol 436 ◽  
Author(s):  
B. M. Clemens ◽  
T. C. Hufnagel ◽  
M. C. Kautzky ◽  
J.-F. Bobo
Keyword(s):  
Thin Films ◽  
Structural Evolution ◽  
Grazing Incidence ◽  
Structural Transformations ◽  
X Ray Diffraction ◽  
X Ray ◽  
Bulk Chemical ◽  
Sputter Deposited ◽  
Fcc Phase ◽  
Bcc Phase

AbstractWe have used grazing incidence x-ray diffraction to observe the structural evolution during growth of sputter-deposited epitaxial Fe films on Cu(001) and Pt(001). We find that on Cu(001), Fe is fcc up to a thickness of 10–12 monolayers, whereupon bcc Fe is observed in first the Pitsch and then the Bain orientations. The fcc Fe shows some relaxation of the misfit from the Cu, as do the Pitsch orientation bcc, which is in tension, and the Bain orientation bcc, which is in compression. All three Fe variants exist in a 40 monolayer thick film. On Pt(001) the Fe grows as bcc with the Bain orientation. However, a thin (20 å) bcc Fe film is transformed to fcc Fe with cube-on-cube orientation by subsequent deposition of Pt. This behavior is consistent with intermixing of Pt into the Fe layer, which lowers the mismatch and bulk chemical energies of the fcc phase relative to that of the bcc phase.

scholarly journals Structural evolution in thermoelectric zinc antimonide thin films studied by in situ X-ray scattering techniques

IUCrJ ◽  
2021 ◽  
Vol 8 (3) ◽  
Author(s):  
Lirong Song ◽  
Martin Roelsgaard ◽  
Anders B. Blichfeld ◽  
Ann-Christin Dippel ◽  
Kirsten Marie Ørnsbjerg Jensen ◽  
...  
Keyword(s):  
Amorphous Phase ◽  
Intermediate Phase ◽  
Function Analysis ◽  
Structural Evolution ◽  
X Ray Diffraction ◽  
X Ray ◽  
X Ray Scattering ◽  
Intermediate Phases ◽  
Long Range Ordering

Zinc antimonides have been widely studied owing to their outstanding thermoelectric properties. Unlike in the bulk state, where various structurally unknown phases have been identified through their specific physical properties, a number of intermediate phases in the thin-film state remain largely unexplored. Here, in situ X-ray diffraction and X-ray total scattering are combined with in situ measurement of electrical resistivity to monitor the crystallization process of as-deposited amorphous Zn-Sb films during post-deposition annealing. The as-deposited Zn-Sb films undergo a structural evolution from an amorphous phase to an intermediate crystalline phase and finally the ZnSb phase during heat treatment up to 573 K. An intermediate phase (phase B) is identified to be a modified β-Zn8Sb7 phase by refinement of the X-ray diffraction data. Within a certain range of Sb content (∼42–55 at%) in the films, phase B is accompanied by an emerging Sb impurity phase. Lower Sb content leads to smaller amounts of Sb impurity and the formation of phase B at lower temperatures, and phase B is stable at room temperature if the annealing temperature is controlled. Pair distribution function analysis of the amorphous phase shows local ordered units of distorted ZnSb4 tetrahedra, and annealing leads to long-range ordering of these units to form the intermediate phase. A higher formation energy is required when the intermediate phase evolves into the ZnSb phase with a significantly more regular arrangement of ZnSb4 tetrahedra.

New Structure of CTAB Templated Silica Films as revealed by GISAXS coupled to HRTEM

2000 ◽  
Vol 628 ◽  
Author(s):  
Sophie Besson ◽  
Catherine Jacquiod ◽  
Thierry Gacoin ◽  
André Naudon ◽  
Christian Ricolleau ◽  
...  
Keyword(s):  
Cetyltrimethylammonium Bromide ◽  
Grazing Incidence ◽  
Hexagonal Structure ◽  
X Ray Diffraction ◽  
Electronic Microscopy ◽  
Silica Films ◽  
X Ray ◽  
X Ray Scattering ◽  
Hexagonal Arrangement ◽  
Spherical Micelles

ABSTRACTA microstructural study on surfactant templated silica films is performed by coupling traditional X-Ray Diffraction (XRD) and Transmission Electronic Microscopy (TEM) to Grazing Incidence Small Angle X-Ray Scattering (GISAXS). By this method it is shown that spin-coating of silicate solutions with cationic surfactant cetyltrimethylammonium bromide (CTAB) as a templating agent provides 3D hexagonal structure (space group P63/mmc) that is no longer compatible with the often described hexagonal arrangement of tubular micelles but rather with an hexagonal arrangement of spherical micelles. The extent of the hexagonal ordering and the texture can be optimized in films by varying the composition of the solution.

STRUCTURAL EVOLUTION OF EXCEPTIONALLY IRON-DEFICIENT HEMATITE NANOCRYSTALS AS OBSERVED BY IN SITU SYNCHROTRON X-RAY DIFFRACTION

2019 ◽  
Author(s):  
Si Athena Chen ◽  
◽  
Peter Heaney ◽  
Jeffrey E. Post ◽  
Peter J. Eng ◽  
...  
Keyword(s):  
Structural Evolution ◽  
X Ray Diffraction ◽  
X Ray ◽  
Iron Deficient

scholarly journals Surface Stoichiometry and Depth Profile of Tix-CuyNz Thin Films Deposited by Magnetron Sputtering

Materials ◽  
2021 ◽  
Vol 14 (12) ◽  
pp. 3191
Author(s):  
Arun Kumar Mukhopadhyay ◽  
Avishek Roy ◽  
Gourab Bhattacharjee ◽  
Sadhan Chandra Das ◽  
Abhijit Majumdar ◽  
...  
Keyword(s):  
Magnetron Sputtering ◽  
Photoelectron Spectroscopy ◽  
Film Surface ◽  
Grazing Incidence ◽  
X Ray Diffraction ◽  
X Ray ◽  
Relative Composition ◽  
Transmission Electron ◽  
Deposited Film ◽  
Deposited Films

We report the surface stoichiometry of Tix-CuyNz thin film as a function of film depth. Films are deposited by high power impulse (HiPIMS) and DC magnetron sputtering (DCMS). The composition of Ti, Cu, and N in the deposited film is investigated by X-ray photoelectron spectroscopy (XPS). At a larger depth, the relative composition of Cu and Ti in the film is increased compared to the surface. The amount of adventitious carbon which is present on the film surface strongly decreases with film depth. Deposited films also contain a significant amount of oxygen whose origin is not fully clear. Grazing incidence X-ray diffraction (GIXD) shows a Cu3N phase on the surface, while transmission electron microscopy (TEM) indicates a polycrystalline structure and the presence of a Ti3CuN phase.

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