研究目的
Investigating the synthesis, structure, and luminescent properties of Eu-doped layered yttrium hydroxides intercalated with benzenedicarboxylate and sulphobenzoate anions using hydrothermal microwave treatment.
研究成果
HTMW treatment enables rapid ion exchange and one-pot synthesis of intercalated LRHs, leading to sensitized Eu3+ luminescence with decreased local symmetry. The solved structure of Y3(OH)7(C7H4O5S)·H2O represents a new class of LRHs (LREH-III), expanding the potential for designing luminescent hybrid materials.
研究不足
Ion exchange reactions with sulphobenzoates other than 4-sulphobenzoate did not yield highly crystalline products under HTMW conditions. The one-pot synthesis was only successful for terephthalate and 4-sulphobenzoate anions, with others producing amorphous or nanocrystalline materials. The study is limited to specific anions and may not generalize to all organic anions.
1:Experimental Design and Method Selection:
The study used hydrothermal microwave (HTMW) treatment for ion exchange reactions and homogeneous hydrolysis to synthesize intercalated layered rare-earth hydroxides (LRHs). Two main approaches were employed: ion exchange between pre-synthesized LRHs and anion solutions, and one-pot synthesis by hydrolyzing rare-earth salts in the presence of anions.
2:Sample Selection and Data Sources:
Samples included Eu-doped yttrium hydroxynitrate and its ion exchange products with phthalate, isophthalate, terephthalate, 2-, 3-, and 4-sulphobenzoate anions. Reagents were sourced from suppliers like Lanhit, Sigma Aldrich, Vekton, Alfa Aesar, and Component-reaktiv.
3:List of Experimental Equipment and Materials:
Equipment included a Berghof Speedwave MWS-4 microwave unit, Teflon autoclaves, Bruker D8 Advance diffractometer, Carl Zeiss NVision 40 SEM, Carlo Erba Instruments EA 1108 CHN analyzer, Bruker ALPHA FTIR Spectrometer, Perkin Elmer LS-55 luminescence spectrophotometer, and synchrotron radiation sources. Materials included yttrium nitrate, europium nitrate, hexamethylenetetramine, various acids and salts, and deionized water.
4:Experimental Procedures and Operational Workflow:
For ion exchange, (Y0.95Eu0.05)2(OH)5NO3·nH2O was dispersed in anion solutions and treated at 25°C or 200°C via HTMW. For one-pot synthesis, mixtures of YCl3, HMTA, and anions were HTMW treated. Products were separated by centrifugation, washed, and dried. Characterization involved XRD, SEM, CHNS analysis, IR spectroscopy, luminescence measurements, and single-crystal X-ray diffraction.
5:95Eu05)2(OH)5NO3·nH2O was dispersed in anion solutions and treated at 25°C or 200°C via HTMW. For one-pot synthesis, mixtures of YCl3, HMTA, and anions were HTMW treated. Products were separated by centrifugation, washed, and dried. Characterization involved XRD, SEM, CHNS analysis, IR spectroscopy, luminescence measurements, and single-crystal X-ray diffraction. Data Analysis Methods:
5. Data Analysis Methods: XRD data were analyzed using Scherrer equation for particle size. IR spectra were interpreted for functional groups. Luminescence spectra were recorded and ratios calculated. Structural data were refined using SHELXTL software.
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Bruker D8 Advance diffractometer
D8 Advance
Bruker
Powder X-ray diffraction analysis
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Carl Zeiss NVision 40 SEM
NVision 40
Carl Zeiss
High-resolution scanning electron microscopy
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Bruker ALPHA FTIR Spectrometer
ALPHA
Bruker
Infrared spectroscopy
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Perkin Elmer LS-55 luminescence spectrophotometer
LS-55
Perkin Elmer
Luminescence spectra recording
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Carlo Erba Instruments EA 1108 CHN analyzer
EA 1108
Carlo Erba Instruments
Elemental analysis for carbon, hydrogen, nitrogen, sulphur
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Berghof Speedwave MWS-4 microwave unit
Speedwave MWS-4
Berghof
Hydrothermal microwave treatment
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Teflon autoclave
Reaction vessel for hydrothermal treatment
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