研究目的
Investigating the effects of experimental parameters on the conversion of red phosphorus to black phosphorus using high-energy ball milling to optimize the synthesis process.
研究成果
The BtPw ratio is the most critical parameter for efficient RP to BP conversion, enabling near 100% yields with short milling times and moderate rotation speeds. Solid-state NMR is the most reliable quantification method. The process is energy-sustainable and cost-effective, with optimal conditions identified for high conversion efficiency.
研究不足
The study assumes energy transfer only from ball-wall collisions, neglecting ball-powder interactions. XRD and Raman provide semiquantitative data due to factors like particle size and orientation. NMR is more reliable but requires careful parameter setting. The BtPw ratio affects batch size scalability.
1:Experimental Design and Method Selection:
The study uses a mathematical model of energy transfer in ball milling to investigate the effects of rotation speed, milling time, and BtPw ratio on RP to BP conversion. High-energy ball milling (HEBM) is employed as the synthesis method, with characterization via solid-state NMR, Raman spectroscopy, XRD, and SEM.
2:Sample Selection and Data Sources:
Commercial red phosphorus (Sigma-Aldrich, >97%) is used as the starting material. Samples are prepared with varying parameters: rotation speed (250-500 rpm), milling time (15-3240 min), and BtPw ratio (10:1 to 110:1). All handling is done in an Ar-filled glovebox to prevent oxidation.
3:1). All handling is done in an Ar-filled glovebox to prevent oxidation. List of Experimental Equipment and Materials:
3. List of Experimental Equipment and Materials: Equipment includes a planetary ball milling apparatus (specific model not mentioned), Bruker D8 Advanced powder diffractometer for XRD, Zeiss EVO MA10 microscope for SEM, Bruker Avance III 400 MHz spectrometer for NMR, and Labram Dilor spectrometer for Raman spectroscopy. Materials include stainless steel bowls and balls, and commercial RP.
4:Experimental Procedures and Operational Workflow:
RP is weighed and placed in sealed stainless steel bowls with balls in a glovebox. Milling is performed at specified parameters. After milling, samples are characterized immediately using NMR, XRD, Raman, and SEM to analyze phase composition and morphology.
5:Data Analysis Methods:
XRD data are analyzed using intensity ratios of RP and BP reflections. NMR spectra are deconvolved using Gaussian and Lorentzian fits. Raman spectra are analyzed using peak intensities and fitting procedures. SEM images are used for morphological analysis.
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Red Phosphorus
>97%
Sigma-Aldrich
Starting material for mechanochemical synthesis to produce black phosphorus.
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X-ray Diffractometer
D8 Advanced
Bruker
Used for X-ray diffraction analysis to identify and quantify phases in the samples.
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Scanning Electron Microscope
EVO MA10
Zeiss
Used for morphological analysis and energy dispersive microanalysis of samples.
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NMR Spectrometer
Avance III 400 MHz
Bruker
Used for solid-state 31P NMR spectroscopy to quantify phases in the samples.
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Planetary Ball Milling Apparatus
Used for high-energy ball milling to convert red phosphorus to black phosphorus.
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Raman Spectrometer
Labram Dilor
Used for Raman spectroscopy to characterize structural evolution and quantify phases.
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Glovebox
Used for handling samples in an inert atmosphere to prevent oxidation.
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