研究目的
Investigation of the possibility to use the indenter-objective for the in-situ collection of Raman spectra during an indentation.
研究成果
The indenter-objective enables simultaneous indentation and in-situ Raman spectroscopy measurements, allowing investigation of phases under load and after unloading. It is applicable to non-transparent samples and not limited to edge measurements, though the diamond tip's Raman peak is always present but has negligible effect for materials with peaks far from it, such as silicon.
研究不足
Scattering of light in the diamond tip introduces a peak at 1332 cm?1, which may interfere with spectra. Quality and resolution are limited by tip manufacturing accuracy, and using objective magnifications higher than 20x is unreasonable due to image distortion. The approach is not fully optimized for accuracy.
1:Experimental Design and Method Selection:
A special load application unit was designed to be used with a standard laboratory Raman spectrometer, incorporating a transparent diamond indenter that functions as an optical objective. The method involves simultaneous indentation and Raman spectroscopy measurements.
2:Sample Selection and Data Sources:
A silicon sample with (100) surface orientation and thickness of about 0.4 mm was used, selected based on known phase transformations during indentation.
3:4 mm was used, selected based on known phase transformations during indentation.
List of Experimental Equipment and Materials:
3. List of Experimental Equipment and Materials: Equipment includes a linear translation stage with a stepper motor, resistive load cell, sample holder, housing, transparent diamond indenter (Berkovich pyramid shape), and a Raman spectrometer with a 20x objective (NA = 0.4). Materials include the silicon sample.
4:4). Materials include the silicon sample.
Experimental Procedures and Operational Workflow:
4. Experimental Procedures and Operational Workflow: The sample was indented up to a maximum load of 50 N using the linear translator to push the sample into the fixed indenter. Raman spectra were collected at loads of 3 N, 10 N, 20 N, 30 N, 40 N, and 50 N during loading and unloading. The optical image was observed through the indenter, and spectra were measured directly through it.
5:Data Analysis Methods:
Raman peak shifts were analyzed to identify phases (e.g., Si-I, Si-II, Si-XII/Si-III) under different loads, using literature references for comparison and pressure estimation.
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