研究目的
To prepare a novel microporous terbium (III) framework and investigate its structural properties, gas adsorption, and luminescent sensing capabilities for acetone and Fe3+ ions in aqueous and isopropanol solutions.
研究成果
The Tb-MOF exhibits excellent luminescent properties with a high quantum yield (90.7%) and can serve as a sensitive sensor for acetone and Fe3+ ions, with detection limits as low as 10^-9 M for Fe3+ in aqueous solutions. The microporous structure contributes to its sensing capabilities, but further studies are needed to understand the quenching mechanisms and improve selectivity.
研究不足
The Tb-MOF has microporous properties but weak N2 adsorption, indicating limited porosity for some gases. The quenching mechanism for acetone and Fe3+ is not fully elucidated, and selectivity for metal ions in isopropanol is weak (e.g., multiple ions cause quenching). Potential optimizations include improving pore size for better gas adsorption and enhancing selectivity in mixed solvents.
1:Experimental Design and Method Selection:
The study involved synthesizing a Tb-MOF using hydrothermal methods, followed by structural characterization, gas adsorption measurements, and luminescence-based sensing experiments for solvents and metal ions. Theoretical models included crystal structure analysis and fluorescence quenching mechanisms.
2:Sample Selection and Data Sources:
The Tb-MOF was synthesized from Tb(OAc)3·6H2O and H3DBB ligand. Metal ion solutions (e.g., Fe3+, Cu2+) and organic solvents (e.g., acetone, isopropanol) were used as analytes.
3:List of Experimental Equipment and Materials:
Equipment included VarioEL elemental analyzer, NicoletAvatar 360 FT-IR spectrometer, Netzsch STA449 F3 thermogravimetric analyzer, SHIMADZU XRD-7000 X-ray diffractometer, Lingguang F97Pro fluorescence spectrophotometer, Edinburgh instruments FLS980 fluorescence spectrophotometer, ASAP 2020 surface area analyzer, and Bruker SMART APEX CCD diffractometer. Materials included Tb(OAc)3·6H2O, H3DBB, various solvents, and metal salts.
4:Experimental Procedures and Operational Workflow:
Synthesis was done via hydrothermal reaction at 140°C for 72 hours. Characterization involved elemental analysis, IR spectroscopy, TGA, XRD, fluorescence spectroscopy, and gas adsorption. Sensing experiments involved immersing Tb-MOF in solvents or ion solutions, ultrasonication, aging, and measuring fluorescence intensity.
5:Data Analysis Methods:
Data were analyzed using software like APEX-II and SHELXTL for crystal structure, and linear regression for quenching effects. Statistical methods included calculating detection limits and linear coefficients.
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NicoletAvatar 360 FT-IR spectrometer
NicoletAvatar 360
Thermo Fisher Scientific
Recording FT-IR spectra from KBr pellets in the range of 4000–400 cm?1.
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SHIMADZU XRD-7000 X-ray diffractometer
XRD-7000
Shimadzu
Determining phase of as-synthesized products by X-ray diffraction with Cu Kα radiation.
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Edinburgh instruments FLS980 fluorescence spectrophotometer
FLS980
Edinburgh Instruments
Measuring luminescent quantum yields.
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Bruker SMART APEX CCD diffractometer
SMART APEX CCD
Bruker
Carrying out single crystal X-ray diffraction analyses with Mo-Kα radiation.
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VarioEL elemental analyzer
VarioEL
Elementar
Performing elemental analyses (CHN) for chemical composition determination.
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Netzsch STA449 F3 thermogravimetric analyzer
STA449 F3
Netzsch
Measuring thermogravimetric experiments in air atmosphere.
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Lingguang F97Pro fluorescence spectrophotometer
F97Pro
Lingguang
Recording fluorescence spectra at room temperature.
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ASAP 2020 surface area analyzer
ASAP 2020
Micromeritics
Measuring N2 and CO2 adsorption isotherms at 77 and 195 K.
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