研究目的
To explain the structural changes in silicate glasses when the sodium oxide content is varied from 12 mol% to 20 mol% while maintaining the iron oxide (as Fe3O4) concentration at a fixed value of 8 mol%.
研究成果
The study confirms that iron ions in silicate glasses are predominantly in tetrahedral coordination with oxygen, with increasing distortion and Fe3+/Fe2+ ratios as sodium content increases. Raman spectroscopy shows that iron presence shifts the predominant linkage from Q3 to Q2, with Q3 linkages increasing with sodium due to Fe3+ network formers. The findings are based on thermodynamic considerations during cooling.
研究不足
The interpretation of spectra from disordered materials like glasses is not unambiguous due to variety of local iron environments. The study is limited to specific sodium and iron concentrations, and the techniques used may not capture all structural details.
1:Experimental Design and Method Selection:
The study uses Raman spectroscopy, EXAFS, and M?ssbauer spectroscopy to analyze the structural changes in silicate glasses with varying sodium and fixed iron contents. The rationale is to understand the coordination and linkages in the glass network.
2:Sample Selection and Data Sources:
Glass samples were synthesized with compositions as per Table 1, using oxides from Thomas Baker (purity ≥99%). Samples were prepared by melting and quenching, and confirmed vitreous by X-ray diffraction.
3:List of Experimental Equipment and Materials:
Equipment includes a Carbolite 1600 furnace, agate pestle and mortar, platinum crucible, X-ray diffractometer (MoKα X-rays), field-emission scanning electron microscope (Quanta FEG 250, FEI, Netherlands) with EDAX (Smart Insight, USA), confocal micro spectrometer imaging spectroscope (STR 500, AIRIX Corp., Tokyo, Japan) with a 532 nm laser, EXAFS beam line (BL-09) at Indus-2 Synchrotron Source, and M?ssbauer spectrometer with WissEI velocity drive.
4:Experimental Procedures and Operational Workflow:
Samples were synthesized by weighing oxides, homogenizing, heating to 900°C for decomposition, then to 1400°C for melting, quenching in air, and annealing at 350°C. EDX was used for composition analysis, Raman spectroscopy for vibrational studies, EXAFS for local structure analysis, and M?ssbauer spectroscopy for iron state analysis.
5:Data Analysis Methods:
Raman spectra were deconvoluted using Gaussian curve fitting. EXAFS data were analyzed using IFEFFIT software (ATHENA and ARTEMIS) for fitting parameters. M?ssbauer spectra were fitted using NORMOS DIST/SITE software to obtain hyperfine parameters.
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Scanning Electron Microscope
Quanta FEG 250
FEI
Imaging and composition analysis with EDX
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Sputter Coater
Auto fine coater Leica EM ACE 200
Leica
Coating samples with gold-palladium for SEM
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Furnace
Carbolite 1600
Carbolite
Heating samples to high temperatures for synthesis
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EDAX System
Smart Insight
EDAX
Energy-dispersive X-ray spectroscopy for composition analysis
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Confocal Micro Spectrometer
STR 500
AIRIX Corp.
Raman spectroscopy measurements
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Laser
532 nm solid state laser
Excitation source for Raman spectroscopy
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M?ssbauer Spectrometer
WissEI velocity drive
M?ssbauer spectroscopy measurements
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EXAFS Beam Line
BL-09
Indus-2 Synchrotron Source
Extended X-ray Absorption Fine Structure measurements
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Software
IFEFFIT
Analysis of EXAFS data
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Software
NORMOS DIST/SITE
Analysis of M?ssbauer spectra
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