In situ kinetic studies of the chemical bath deposition of zinc sulfide from acidic solutions

ZnS thin films are promising as a buffer layer in solar cells, which can be basis of photovoltaic cells, photoelectric sensors, and light-emitting diodes. For the preparation of thin ZnS films by chemical bath deposition, thioacetamide or thiourea is used as a chalcogenization agent, and ammonia, triethanolamine and sodium citrate are mainly used as ligands, carrying out the process in an alkaline medium. In the present work, in order to predict the conditions of hydrochemical deposition of ZnS films, we have analyzed ionic equilibria in two reaction systems “ZnCl2 – NH4OH – CH3CNH2” and “ZnCl2 – CH3CSNH2 – KHC8H4O4” that differ in acidity of the medium. An analysis of ionic equilibrium showed that in the first bath ~80% of the metal is in the form of a neutral hydroxo complex Zn(OH)2 at pH > 7, and in the second more than 98% of zinc is present as acetate complexes Zn(CH3COO)+ and Zn(CH3COO)2 in the range of pH from 0 to 7. The thermodynamic evaluation of the boundary conditions for the formation of zinc sulfide made it possible to conclude that a zinc sulfide film can be formed in both systems without the admixture of Zn(OH)2 hydroxide. ZnS films were obtained by hydrochemical deposition with thick about 100 nm from both systems. Using local energy-dispersive elemental analysis, it was found that the average ratio between the main elements of Zn and S in the layers obtained in an alkaline medium is 49.48 and 50.52 at.%, and in the synthesized from acidic solutions – 50.35 and 49.65 at.%. According to the data of electron microscopy, up to 85% of the agglomerates have an average size of 200-450 nm that formed from ZnS particles growing in an alkaline reaction bath. At the same time, there are aggregates whose dimensions reach 700 nm. The layers that deposited from relatively acidic solutions are distinguished by a higher degree of dispersion. Here up to ~90% of the film-forming particles is in the nanoscale range from 50 to 90 nm.

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Chemical Bath Deposition of CdS Thin Films: Electrochemical In Situ Kinetic Studies

Journal of The Electrochemical Society ◽

10.1149/1.2068984 ◽

1992 ◽

Vol 139 (10) ◽

pp. 2810-2814 ◽

Cited By ~ 67

Author(s):

J. M. Doña ◽

J. Herrero

Keyword(s):

Thin Films ◽

Chemical Bath Deposition ◽

Kinetic Studies ◽

Cds Thin Films

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Time-Resolved Morphology and Kinetic Studies of Pulsed Laser Deposition-Grown Pt Layers on Sapphire at Different Growth Temperatures by in Situ Grazing Incidence Small-Angle X-ray Scattering

Langmuir ◽

10.1021/acs.langmuir.0c02952 ◽

2021 ◽

Author(s):

Sondes Bauer ◽

Adriana Rodrigues ◽

Lukáš Horák ◽

Berkin Nergis ◽

Xiaowei Jin ◽

...

Keyword(s):

Pulsed Laser Deposition ◽

Small Angle ◽

Pulsed Laser ◽

Kinetic Studies ◽

Grazing Incidence ◽

Laser Deposition ◽

Time Resolved ◽

X Ray ◽

X Ray Scattering

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The AMPIX electrochemical cell: a versatile apparatus forin situX-ray scattering and spectroscopic measurements

Journal of Applied Crystallography ◽

10.1107/s0021889812042720 ◽

2012 ◽

Vol 45 (6) ◽

pp. 1261-1269 ◽

Cited By ~ 98

Author(s):

Olaf J. Borkiewicz ◽

Badri Shyam ◽

Kamila M. Wiaderek ◽

Charles Kurtz ◽

Peter J. Chupas ◽

...

Keyword(s):

Electrochemical Cell ◽

Function Analysis ◽

Kinetic Studies ◽

Spectroscopic Measurements ◽

Battery Materials ◽

X Ray ◽

Complex Processes ◽

Electrochemical Cycling ◽

Ray Scattering

This article presents a versatile easy-to-use electrochemical cell suitable forin operando,in situmeasurements of battery materials during electrochemical cycling using a variety of X-ray techniques. Argonne's multi-purposein situX-ray (AMPIX) cell provides reliable electrochemical cycling over extended periods owing to the uniform stack pressure applied by rigid X-ray windows and the formation of a high-fidelity hermetic seal. The suitability of the AMPIX cell for a broad range of synchrotron-based X-ray scattering and spectroscopic measurements has been demonstrated with studies at eight Advanced Photon Source beamlines to date. Compatible techniques include pair distribution function analysis, high-resolution powder diffraction, small-angle scattering and X-ray absorption spectroscopy. These techniques probe a broad range of electronic, structural and morphological features relevant to battery materials. The AMPIX cell enables experiments providing greater insight into the complex processes that occur in operating batteries by allowing the electrochemical reactions to be probed at fine reaction intervals with greater consistency (within the charge–discharge cycle and between different methodologies) with potential for new time-dependent kinetic studies or studies of transient species. Representative X-ray and electrochemical data to demonstrate the functionality of the AMPIX cell are presented.

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Structure of Microphase-Separated Silica/Siloxane Molecular Composites

MRS Proceedings ◽

10.1557/proc-171-57 ◽

1989 ◽

Vol 171 ◽

Cited By ~ 8

Author(s):

Dale W. Schaefer ◽

James E. Mark ◽

David Mccarthy ◽

Li Jian ◽

C. -C. Sun ◽

...

Keyword(s):

Phase Separation ◽

Kinetic Studies ◽

Organic Content ◽

Small Particles ◽

X Ray ◽

Filled Elastomers ◽

Polymeric Networks ◽

Large Particles ◽

Molecular Composites

ABSTRACTThe structure of several classes of silica/siloxane molecular composites is investigated using small-angle x-ray and neutron scattering. These filled elastomers can be prepared through different synthethic protocols leading to a range of fillers including particulates with both rough and smooth surfaces, particulates with dispersed interfaces, and polymeric networks. We also find examples of bicontinuous filler phases that we attribute to phase separation via spinodal decomposition. In-situ kinetic studies of particulate fillers show that the precipitate does not develop by conventional nucleation-and-growth. We see no evidence of growth by ripening whereby large particles grow by consumption of small particles. Rather, there appears to be a limiting size set by the elastomer network itself. Phase separation develops by continuous nucleation of particles and subsequent growth to the limiting size. We also briefly report studies of polymer-toughened glasses. In this case, we find no obvious correlation between organic content and structure.

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