研究目的
To investigate the evolution of microstructure and mechanical properties of a graded TiAlON thin film with stepwise increasing oxygen content across the film thickness using cross-sectional characterization techniques.
研究成果
The study revealed a transition from a wurtzite to a face-centered cubic structure with the addition of oxygen, accompanied by an increasing amorphous phase fraction. The hardness initially increased due to the phase transition but decreased at higher oxygen contents due to the increasing amorphous phase fraction. The complementary use of advanced cross-sectional characterization methods provided a comprehensive understanding of the microstructure and mechanical properties evolution in the graded TiAlON thin film.
研究不足
The study focuses on the microstructural and mechanical properties evolution of a graded TiAlON thin film with increasing oxygen content. The limitations include the specific deposition conditions (e.g., substrate temperature, deposition time) and the characterization techniques used, which may not capture all aspects of the film's properties. Additionally, the presence of residual oxygen in the deposition chamber and surface oxidation of the TEM lamella could affect the results.
1:Experimental Design and Method Selection:
A graded TiAl(O)N film was synthesized on Si substrates using a laboratory-scale unbalanced d.c. magnetron sputter deposition system. The deposition was performed in constant current mode with a stepwise increasing oxygen partial pressure over the film thickness.
2:Sample Selection and Data Sources:
Single crystalline Si(100) substrates were used. The elemental and phase composition was investigated by transmission electron microscopy (TEM), electron energy loss spectroscopy (EELS), energy dispersive X-ray spectroscopy (EDX), and selected area electron diffraction (SAED). Synchrotron X-ray nanodiffraction was applied to study the phase composition and in-plane strain. Cross-sectional μ-Raman spectroscopy and nanoindentation were performed to investigate the phase evolution and mechanical properties.
3:List of Experimental Equipment and Materials:
Zeiss Auriga field emission gun scanning electron microscope (SEM), Orsay Physics Cobra Z-05 focused ion beam (FIB) workstation, FEI Tecnai F20 TEM, FEI Tecnai 12 TEM, Hitachi IM4000Plus ion milling system, Hysitron TriboIndenter TI 950 nanoindenter, LabRAM HR800 spectrometer.
4:Experimental Procedures and Operational Workflow:
The film was deposited with increasing oxygen partial pressure in four steps. TEM lamella was prepared using FIB. TEM, EELS, EDX, and SAED were performed to study the microstructure and phase composition. Synchrotron X-ray nanodiffraction was used to validate the phase information and evaluate the in-plane strain. Cross-sectional μ-Raman spectroscopy and nanoindentation were performed to study the phase evolution and mechanical properties.
5:Data Analysis Methods:
The data from TEM, EELS, EDX, SAED, synchrotron X-ray nanodiffraction, μ-Raman spectroscopy, and nanoindentation were analyzed to determine the phase composition, microstructure, and mechanical properties of the film.
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