研究目的
To unveil a novel hexagonal polymorph of tungsten oxide (h’-WO3) with enhanced electrochromic properties through a soft chemistry synthesis route.
研究成果
The novel h’-WO3 polymorph exhibits superior electrochromic properties with fast proton insertion/deinsertion, high coloration efficiency, and stability, making it promising for applications in electrochromic devices and other energy-related fields.
研究不足
The material is sensitive to beam damage in electron microscopy, and precise proton positions in the structure require further investigation. The study is limited to proton insertion; other cations and substitutions are not fully explored.
1:Experimental Design and Method Selection:
The study employed a soft chemistry aqueous route for synthesis, using pH adjustment and hydrothermal conditions. Structural characterization involved XRD, TEM, SEM, STEM, and spectroscopic methods. Electrochemical properties were evaluated using a three-electrode cell setup.
2:Sample Selection and Data Sources:
Samples were synthesized from sodium tungstate dihydrate and hydrazine in water, with pH adjusted to 0.6. Data were obtained from laboratory experiments and computational modeling (DFT).
3:Data were obtained from laboratory experiments and computational modeling (DFT). List of Experimental Equipment and Materials:
3. List of Experimental Equipment and Materials: Equipment included PanAlytical X’Pert Pro diffractometer, Hitachi S3400-N SEM, Tecnai spirit G2 TEM, JEOL JEMARM200cF STEM, Perkin Elmer Lambda 900 UV/Vis/NIR spectrometer, Omicron XPS apparatus, Bruker X-band ESR spectrometer, Mettler LF1600 TGA/DTA, BEL Belsorp Max and Belprep II for sorption, Solartron Modilab potentiostat. Materials included Na2WO4·2H2O, hydrazine, HCl, ethanol, FTO substrates, H2SO4 electrolyte.
4:Experimental Procedures and Operational Workflow:
Synthesis involved dissolving Na2WO4·2H2O in water, adding hydrazine, adjusting pH to 0.6 with HCl, aging, heating at 120°C for 12h, washing, and drying. Characterization steps included XRD for structure resolution, microscopy for nanostructure imaging, spectroscopy for optical and electronic properties, and electrochemical testing for electrochromic performance.
5:6 with HCl, aging, heating at 120°C for 12h, washing, and drying. Characterization steps included XRD for structure resolution, microscopy for nanostructure imaging, spectroscopy for optical and electronic properties, and electrochemical testing for electrochromic performance. Data Analysis Methods:
5. Data Analysis Methods: Data were analyzed using Rietveld refinement for XRD, DFT calculations for electronic structure, and standard electrochemical and spectroscopic techniques for property evaluation.
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X-ray diffractometer
X’Pert Pro
PanAlytical
Recording XRD patterns for structural analysis
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Scanning electron microscope
S3400-N
Hitachi
Obtaining SEM images of nanostructures
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Transmission electron microscope
Tecnai spirit G2
FEI
Recording TEM images and SAED patterns
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STEM microscope
JEMARM200cF
JEOL
Atomic resolution characterization with HAADF and ABF detection
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UV/Vis/NIR spectrometer
Lambda 900
Perkin Elmer
Measuring absorption spectra and reflectance
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ESR spectrometer
X-band
Bruker
Electron spin resonance measurements
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XPS apparatus
Omicron
Performing X-ray photoelectron spectroscopy
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TGA/DTA apparatus
LF1600
Mettler
Thermogravimetric and differential temperature analysis
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Sorption apparatus
Belsorp Max
BEL
Nitrogen sorption for specific surface area measurement
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Potentiostat
Modilab
Solartron
Electrochemical measurements and applying voltage functions
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Sodium tungstate dihydrate
Sigma
Precursor for synthesis
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FTO substrate
Conductive substrate for electrode fabrication
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