研究目的
To utilize the Kirkendall effect in the Al-Au system to produce hollow AlAu2 nanoparticles attached to a sapphire substrate, and to understand the mechanism involving substrate-assisted oxidation and diffusion.
研究成果
Hollow AlAu2 nanoparticles were successfully fabricated on sapphire using solid state dewetting and annealing in air. The hollowing mechanism is driven by Al oxidation at the Au-sapphire interface, facilitated by oxygen diffusion through the Au film. The substrate plays an active role in the process, enabling homoepitaxial growth of alumina. This expands the applicability of the Kirkendall effect for creating porous nanostructures and highlights the potential for similar mechanisms in other systems with reactive substrates.
研究不足
The study is limited to the Al-Au system on sapphire substrates; applicability to other binary systems depends on diffusion rates and reaction kinetics. The model assumes steady-state conditions and homogeneous diffusion, which may not fully capture microstructural complexities. Experimental conditions such as film thickness and particle size affect pore morphology and kinetics, requiring further optimization.
1:Experimental Design and Method Selection:
The study employed solid state dewetting of Al thin films on sapphire, followed by Au deposition and annealing in different atmospheres to investigate pore formation and intermetallic phase growth. A kinetic model was developed to describe oxygen diffusion and Al oxidation.
2:Sample Selection and Data Sources:
C-plane oriented sapphire wafers with a miscut of 0.2° toward the m-plane were used. Thin Al and Au films were deposited via molecular beam epitaxy (MBE).
3:2° toward the m-plane were used. Thin Al and Au films were deposited via molecular beam epitaxy (MBE). List of Experimental Equipment and Materials:
3. List of Experimental Equipment and Materials: MBE tool for deposition and annealing, rapid thermal annealing furnace (ULVAC-RIKO MILA 5000 P-N), X-ray diffractometer (Rigaku SmartLab), high-resolution scanning electron microscope (Zeiss Ultra-Plus), focused ion beam system (FEI Helios NanoLab DualBeam G3 UC), transmission electron microscopes (FEI Titan 80-300 KeV S/TEM and FEI Themis G2 300 80-300 keV S/TEM), energy dispersive X-ray spectroscopy (EDS), electron backscattered diffraction (EBSD), and electron energy loss spectroscopy (EELS). Materials included Al and Au thin films, sapphire substrates, and gases (air, vacuum, forming gas).
4:Experimental Procedures and Operational Workflow:
A 10 nm Al film was deposited on sapphire and annealed at 600°C for 18 hours in MBE. A 20 nm Au film was then deposited. Subsequent annealing was performed at 170°C for 30 or 60 minutes in air, vacuum, or forming gas. Characterization involved XRD, HRSEM, FIB for cross-sections, TEM, EDS, EBSD, and EELS.
5:Data Analysis Methods:
XRD spectra were fitted with Gaussians for phase identification. EDS provided elemental maps and composition profiles. EBSD was used for grain size analysis. A kinetic model based on diffusion equations was developed and solved numerically.
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X-ray Diffractometer
SmartLab
Rigaku
Used for phase identification and analysis of samples through XRD measurements.
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High-Resolution Scanning Electron Microscope
Ultra-Plus
Zeiss
Used for acquiring secondary electron micrographs of samples.
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Focused Ion Beam System
Helios NanoLab DualBeam G3 UC
FEI
Used for preparing cross-sectional samples via lift-out method for TEM analysis.
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Transmission Electron Microscope
Titan 80-300 KeV S/TEM
FEI
Used for high-resolution imaging and analysis of samples at 300 keV.
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Transmission Electron Microscope
Themis G2 300 80-300 keV S/TEM
FEI
Used for high-resolution imaging and analysis of samples.
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Molecular Beam Epitaxy Tool
Used for deposition and annealing of thin films under high vacuum conditions.
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Rapid Thermal Annealing Furnace
MILA 5000 P-N
ULVAC-RIKO
Used for annealing samples in controlled atmospheres at specific temperatures.
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Energy Dispersive X-ray Spectroscopy
Used for elemental mapping and composition analysis in TEM.
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Electron Backscattered Diffraction
Used for grain orientation and size mapping.
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Electron Energy Loss Spectroscopy
Used for detecting oxygen presence in grain boundaries.
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