研究目的
To synthesize and characterize a new photochromic inorganic-organic hybrid material based on phenethyl viologen and bismuth(III) chloride, and to investigate its photochromic properties.
研究成果
The study successfully synthesized a new photochromic hybrid material (PeV)3(Bi2Cl9)2, which exhibits reversible color change due to electron transfer between viologen species. The in situ synthesis method is more efficient and less toxic, offering potential for developing new viologen-based materials with enhanced properties.
研究不足
The photochromic properties may be influenced by factors such as the size of inorganic oligomers and π-π interactions, which are not fully predictable. The toxicity of viologen compounds is a concern, though the in situ synthesis reduces intermediate formation.
1:Experimental Design and Method Selection:
The synthesis was conducted under solvothermal conditions to facilitate in situ generation of the viologen cation and self-assembly of the hybrid material. Single crystal X-ray diffraction was used for structural characterization, and UV-vis diffuse-reflectance spectroscopy and electron spin resonance (ESR) measurements were employed to study photochromic behavior.
2:Sample Selection and Data Sources:
The compound (PeV)3(Bi2Cl9)2 was synthesized from BiCl3, 4,4′-bipyridine, phenylethyl alcohol, and concentrated HCl. Single crystals were obtained for structural analysis.
3:List of Experimental Equipment and Materials:
BiCl3, 4,4′-bipyridine, phenylethyl alcohol, concentrated HCl (36-38%), ethanol, Teflon-lined autoclave, Rigaku SATURN70 CCD diffractometer, Bruker A300 spectrometer, PE Lambda 900 UV-vis spectrometer, Rigaku MiniFlex2 diffractometer, Elementar Vario EL III microanalyzer.
4:Experimental Procedures and Operational Workflow:
BiCl3 and 4,4′-bipyridine were mixed with concentrated HCl and phenylethyl alcohol in an autoclave, heated to 150 °C at 2 °C/min, held for 3 days, then cooled to room temperature at 2 °C/hour. Crystals were washed with ethanol. Characterization included elemental analysis, PXRD, single crystal X-ray diffraction, UV-vis spectroscopy, and ESR measurements.
5:Data Analysis Methods:
Crystal structure was solved using SHELXTL-2014 and refined with OLEX2. UV-vis data were analyzed for absorption peaks, and ESR spectra were recorded to detect radical formation.
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Rigaku SATURN70 CCD diffractometer
SATURN70
Rigaku
Used for single crystal X-ray diffraction measurements to determine crystal structure.
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Bruker A300 spectrometer
A300
Bruker
Used for electron spin resonance (ESR) measurements to detect radical species.
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PE Lambda 900 UV-vis spectrometer
Lambda 900
PE
Used for UV-vis diffuse-reflectance spectroscopy to study photochromic behavior.
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Rigaku MiniFlex2 diffractometer
MiniFlex2
Rigaku
Used for powder X-ray diffraction (PXRD) to check phase purity.
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Teflon-lined autoclave
25 mL
Used for solvothermal synthesis reactions under high temperature and pressure.
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Elementar Vario EL III microanalyzer
Vario EL III
Elementar
Used for elemental analysis of C, H, and N.
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