研究目的
To synthesize the red-emitting nitridosilicate phosphor Sr2Si5N8:Eu2+ using shock waves as a new method, aiming to provide an alternative synthesis route that may be easier and more cost-effective compared to conventional high-temperature methods.
研究成果
Shock wave synthesis successfully produces Sr2Si5N8:Eu2+ phosphor with high crystallinity and similar luminescence properties to conventional methods, but with lower intensity due to impurities and incomplete doping. The method shows potential for synthesizing complex materials but requires optimization in powder processing and parameter control to improve purity and performance.
研究不足
The reaction time is very short (≈1 ms), limiting diffusion and potentially leading to incomplete reaction and impurity phases. The method requires precise control of experimental parameters, and the incorporation of europium is sensitive to conditions, resulting in lower luminescence intensity compared to conventional methods. The use of moisture-sensitive starting materials and the need for inert handling add complexity. Temperature calculations are approximate due to unknown material parameters.
1:Experimental Design and Method Selection:
The study uses a shock wave-induced solid-state reaction method, where a detonation-driven shock wave apparatus generates high pressure and temperature to initiate the reaction. The method involves encapsulating a powder mixture in a steel container and subjecting it to shock waves from an explosive charge.
2:Sample Selection and Data Sources:
Starting materials include α-Si3N4 powder (H.C. Starck, type M11), in-house made Sr3N2 granules from strontium rods, and EuN powder (Materion). Powders are mixed under inert conditions to avoid contamination.
3:List of Experimental Equipment and Materials:
Equipment includes a vibration ball mill (Narva), hydraulic ram press, detonation-driven shock wave apparatus with explosive charge, steel containers, scanning electron microscope (Jeol JCM-5700), energy dispersive X-ray spectroscopy (Bruker), powder X-ray diffractometer (Seifert XRD 3000TT), Fourier-transform infrared spectrometer (Varian 670-IR), elemental analyzer (Leco ONH836), and spectrometer (CAS 140B). Materials include Si3N4, Sr3N2, EuN, explosives, and steel.
4:Experimental Procedures and Operational Workflow:
Powders are milled and mixed under nitrogen atmosphere. The mixture is pressed into a steel container and subjected to shock waves at varying pressures (18-41 GPa) and porosities. After shock treatment, samples are recovered and analyzed for phase composition, morphology, elemental content, and luminescence properties.
5:Data Analysis Methods:
Phase analysis is done using Rietveld refinement of XRD data. Elemental analysis uses hot gas extraction. Morphology and composition are analyzed via SEM and EDX. Luminescence properties are measured with excitation and emission spectra.
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Scanning electron microscope
JCM-5700
Jeol
Used to check grain size and morphology of powders.
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Spectrometer
CAS 140B
Instrument System
Used to measure luminescence properties (emission and excitation spectra).
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α-Si3N4 powder
M11
H.C. Starck
Starting material for the solid-state reaction to synthesize the phosphor.
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EuN powder
Materion
Doping material for europium incorporation into the phosphor.
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Vibration ball mill
Narva
Used for milling and mixing the starting powders under inert conditions.
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Energy dispersive X-ray spectroscopy
Bruker
Used for chemical composition and distribution analysis.
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Powder X-ray diffractometer
XRD 3000TT
Seifert
Used for phase analysis via powder XRD with Rietveld refinement.
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Fourier-transform infrared spectrometer
670-IR
Varian
Used to record FTIR spectra for purity checking.
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Elemental analyzer
ONH836
Leco
Used for hot gas extraction method to determine nitrogen and oxygen composition.
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