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Millisecond X-ray reflectometry and neural network analysis: unveiling fast processes in spin coating
David Schumi-Mareček1, Florian Bertram2, Petr Mikulík3
1Physikalische Chemie, Graz University, Heinrichstraße 28, Graz, Steiermark 8010, Austria.
Summary
This study introduces Quick X-ray Reflectometry (XRR), a millisecond technique for real-time monitoring of nanoscale processes like thin film formation. This rapid method enables unprecedented insights into fast structural changes during material deposition and other dynamic events.
Area of Science:
- Nanotechnology and Materials Science
- Surface Science and Thin Film Analysis
Background:
- X-ray Reflectometry (XRR) is crucial for characterizing nanoscale films and layered structures in semiconductor and optics manufacturing.
- Existing XRR methods are often too slow for real-time monitoring of rapid nanoscale processes.
Purpose of the Study:
- To develop and demonstrate a novel, high-speed XRR technique for quantitative, millisecond-scale measurements.
- To enable real-time, in situ monitoring of fast nanoscale processes, such as thin film formation.
Main Methods:
- Development of a novel millisecond monochromatic X-ray Reflectometry (XRR) system, termed Quick XRR (qXRR).
- Demonstration of qXRR with a record acquisition time of 1.4 ms for static gold thin films.
- Application of qXRR for dynamic in situ measurements during PMMA spin coating, coupled with machine learning for rapid data fitting.
Main Results:
- Achieved millisecond acquisition times, an order of magnitude faster than previous methods.
- Successfully monitored dynamic in situ processes like thin film formation during spin coating.
- Resolved initial film thinning via mass transport and later thinning via solvent evaporation.
Conclusions:
- Millisecond qXRR is a significant advancement for in situ studies of fast thin film deposition processes.
- The technique can track intrinsically fast phenomena like high deposition rate growth and spin coating.
- qXRR has broad implications for studying rapid structural changes, including photostriction and diffusion.

