研究目的
Investigating the luminescence properties of Eu3+-doped barium borogermanate phosphors with controllable morphologies and their thermal conversion products.
研究成果
Three morphologies of Ba3[Ge2B7O16(OH)2](OH)(H2O):Eu3+ were successfully synthesized, with hexagonal-flake morphology showing the highest quantum yield (54.1%) and longest lifetime (1.67 ms). The precursor calcination method for Ba3Ge2B6O16:Eu3+ resulted in red emission, while solid-state method gave orange emission, indicating different Eu3+ site occupations. The hexagonal-flake morphology phosphor is promising for WLED applications due to its high efficiency.
研究不足
The study is limited to specific boron sources and synthesis conditions; other parameters or materials were not explored. The thermal stability is only up to 673 K, and the concentration quenching effect occurs above 3% Eu3+ doping. The morphologies are dependent on pH and cations from boron sources, which may not be generalizable.
1:Experimental Design and Method Selection:
The study used hydrothermal synthesis to prepare Ba3[Ge2B7O16(OH)2](OH)(H2O):Eu3+ phosphors with different morphologies by varying boron sources (H3BO3, NH4B5O8·4H2O, Na2B4O7·10H2O). Ba3Ge2B6O16:Eu3+ was prepared by calcining the precursor at 900°C for 5 hours and compared with a sample made by high-temperature solid-state reaction. Characterization methods included XRD, EDS, FT-IR, TG-DTA, SEM, HRTEM, PL spectroscopy, lifetime measurements, and quantum yield measurements.
2:Sample Selection and Data Sources:
Analytical grade reagents (BaCO3, Eu2O3, GeO2, H3BO3, NH4B5O8·4H2O, Na2B4O7·10H2O) were used without purification. Samples were synthesized in a Teflon-lined autoclave at 200°C for varying times (24-96 hours).
3:List of Experimental Equipment and Materials:
Autoclave, oven, filter, deionized water, ethanol, drying oven. Characterization equipment: XRD (Rigaku D/MAX-C, Cu Kα radiation), FT-IR (Nicolet NEXUS 670 spectrometer), TG-DTA (TA-SDT Q600), EDS (Hitachi JEOL-6700F), SEM (Philips-FEI Quanta 200), TEM (Tecnai G2 F20), PL spectrometer (FL-4600 Hitachi), lifetime apparatus (FLS920P Edinburgh Analytical Instrument), quantum yield apparatus (Hamamatsu C9920-02G).
4:Experimental Procedures and Operational Workflow:
For hydrothermal synthesis, raw materials were sealed in an autoclave, heated at 200°C for specified times, cooled, filtered, washed, and dried. Calcination was done at 900°C for 5 hours. Characterization involved standard procedures for each technique, e.g., XRD for structure, SEM for morphology, PL for emission spectra.
5:Data Analysis Methods:
XRD patterns were compared with simulated structures. FT-IR peaks were assigned based on literature. PL spectra were analyzed for emission peaks and intensities. Lifetime decay curves were fitted with double-exponential functions. Quantum yield was calculated as the ratio of emitted to absorbed photons.
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X-ray Diffractometer
D/MAX-C
Rigaku
Characterize the structure of samples by X-ray powder diffraction
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EDS Spectrometer
JEOL-6700F
Hitachi
Energy-dispersive X-ray spectroscopy for elemental analysis
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SEM
Quanta 200
Philips-FEI
Investigate morphology and size of products
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TEM
Tecnai G2 F20
FEI
Characterize inter-planar spacing by field transmittance electron microscopy
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Fluorescence Spectrometer
FL-4600
Hitachi
Record photoluminescence spectra
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Quantum Yield Apparatus
C9920-02G
Hamamatsu
Measure absolute photoluminescence quantum yield
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FT-IR Spectrometer
NEXUS 670
Nicolet
Record FT-IR spectra of samples
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TG-DTA Analyzer
SDT Q600
TA
Perform thermogravimetric and differential thermal analysis
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Lifetime Apparatus
FLS920P
Edinburgh Analytical Instrument
Measure lifetime of phosphors
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Autoclave
Used for hydrothermal synthesis reactions
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