研究目的
Investigating the electrochemical oxidation of selenide and polyselenide solutions to deposit selenium, and the role of polyselenides as intermediates in the process.
研究成果
The research demonstrates that polyselenides form as intermediates during the anodic electrodeposition of selenium from selenide solutions. Amorphous selenium deposits at 25°C and crystalline at 70°C. Potentiostatic deposition reaches a steady-state between deposition and dissolution, while galvanostatic deposition allows thicker layers up to 300 ? from polyselenide solutions. The findings highlight the potential for selenium films in technologies like photoelectrochemical cells, with recommendations for future studies on optimizing deposition conditions and exploring applications.
研究不足
The study is limited to specific pH (9.2) and temperature conditions (25°C and 70°C). The use of selenide solutions requires oxygen-free handling due to instability in air. The self-limiting growth mechanism due to selenium's high resistivity may restrict deposition thickness without external factors like light illumination.
1:Experimental Design and Method Selection:
The study uses cyclic voltammetry, potentiostatic and galvanostatic deposition experiments to investigate selenium deposition from selenide and polyselenide solutions at pH 9.2 and temperatures of 25°C and 70°C. Theoretical models include Pourbaix diagrams and formal potentials for redox reactions.
2:2 and temperatures of 25°C and 70°C. Theoretical models include Pourbaix diagrams and formal potentials for redox reactions. Sample Selection and Data Sources:
2. Sample Selection and Data Sources: Solutions were prepared using potassium selenide (K2Se) and polyselenides in carbonate buffer (pH 9.2). Fresh solutions were used for each measurement under oxygen-free conditions.
3:2). Fresh solutions were used for each measurement under oxygen-free conditions. List of Experimental Equipment and Materials:
3. List of Experimental Equipment and Materials: Glassy carbon working electrode (diameter 3 mm), graphite rod counter electrode, saturated calomel reference electrode, Autolab PGSTAT12 potentiostat, PANalytical Empyrean X-ray diffractometer, Zeiss EVO MA10 SEM, Oxford Instruments X-act EDX system, polishing materials (aluminum oxide slurries), chemicals (selenium, KCl, K2CO3, KHCO3), deionized water.
4:Experimental Procedures and Operational Workflow:
Electrodes were polished and sonicated. Cyclic voltammetry was performed with potential sweeps. Deposition experiments were conducted potentiostatically at 0.2 V and galvanostatically with varying current densities. Samples were analyzed using PXRD, SEM, and EDX.
5:2 V and galvanostatically with varying current densities. Samples were analyzed using PXRD, SEM, and EDX. Data Analysis Methods:
5. Data Analysis Methods: Data were analyzed using GPES or NOVA software, WinXPow for PXRD, AzTec for EDX, and OriginLab2017 for figure preparation. Diffusion coefficients were estimated using the Randles-?ev?ík equation.
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Glassy Carbon Electrode
diameter 3 mm
CH Instruments
Working electrode for electrochemical experiments
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X-ray Diffractometer
PANalytical Empyrean
PANalytical
Powder X-ray diffraction measurements
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Scanning Electron Microscope
Zeiss EVO MA10
Zeiss
Taking SEM images of deposited selenium
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Energy Dispersive X-ray System
Oxford Instruments X-act
Oxford Instruments
EDX analysis for elemental composition
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Graphite Rod
Sigma-Aldrich
Counter electrode in electrochemical setup
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Saturated Calomel Electrode
SCE
BAS Inc.
Reference electrode for potential measurements
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Potentiostat
Autolab PGSTAT12
EcoChemie
Computer-controlled instrument for voltammetric measurements
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pH Meter
Hannah pH 213
Hannah
Measuring pH of solutions
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Water Purification System
Millipore UHQ
Vivendi
Producing deionized water
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