研究目的
Synthesizing and characterizing two new tetra-Zr(IV)-substituted sandwich-type Keggin polyoxometalates functionalized by chiral D-tartaric acid and glycolic acid, and studying their optical and electrochemical properties.
研究成果
Two new organic-functionalized Zr4-cluster-substituted POMs were successfully synthesized and characterized. Compound 1 is chiral and exhibits nonlinear optical properties, while both compounds show good electrocatalytic activity for H2O2 reduction, indicating their potential in optical and electrochemical applications.
研究不足
The study is limited to specific synthesis conditions and characterization techniques; potential optimizations could include exploring other organic ligands or varying synthesis parameters to enhance properties.
1:Experimental Design and Method Selection:
Hydrothermal synthesis was used to prepare the compounds. Characterization methods included FT-IR spectra, elemental analysis, single-crystal X-ray structure analysis, PXRD, TGA, UV-vis spectroscopy, and cyclic voltammetry.
2:Sample Selection and Data Sources:
Compounds 1 and 2 were synthesized from precursors like K8Na2[A-α-GeW9O34]·25H2O and Na10[A-α-SiW9O34]·19H2O, with D-tartaric acid or glycolic acid and ZrOCl2·8H2O.
3:2O. List of Experimental Equipment and Materials:
3. List of Experimental Equipment and Materials: Equipment included Bruker D8 Advance XRD diffractometer, Nicolet iS10 FTIR spectrometer, PE2400 II elemental analyzer, Mettler Toledo TGA/DSC 1/1100 analyzer, PerkinElmer Lamda-950 UV-vis spectrophotometer, Q-switched Nd:YAG solid-state laser, CHI 660E electrochemical workstation, and Gemini A Ultra diffractometer. Materials were commercially available chemicals.
4:Experimental Procedures and Operational Workflow:
Synthesis involved stirring reagents in buffer solutions, heating in a stainless steel reactor with Teflon-liner at 100°C for 5 days, cooling, filtration, and drying. Characterization followed standard procedures for each technique.
5:Data Analysis Methods:
Data were analyzed using software like SHELXTL-97 for structure refinement, Kubelka-Munk equation for UV-vis, and standard electrochemical analysis for CV.
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XRD diffractometer
D8 Advance
Bruker
Collecting powder XRD patterns for phase purity confirmation
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Elemental analyzer
PE2400 II
PerkinElmer
Measuring elemental analysis for C, H, and N
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UV-vis spectrophotometer
Lamda-950
PerkinElmer
Measuring optical diffuse reflectance spectra
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Electrochemical workstation
CHI 660E
CH Instruments
Conducting cyclic voltammetry experiments
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FTIR spectrometer
iS10
Nicolet
Recording FT-IR spectra with KBr pellets
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TGA analyzer
TGA/DSC 1/1100
Mettler Toledo
Performing thermogravimetric analysis under N2 atmosphere
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Laser
Q-switched Nd:YAG solid-state laser
Performing powder SHG signals for nonlinear optical properties
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Diffractometer
Gemini A Ultra
Single-crystal X-ray structure analysis
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