High-Temperature and High-Speed Atomic Force Microscopy Using a qPlus Sensor in Liquid via Quadpod Scanner and Hybrid-Loop Frequency Demodulation

TL;DR

This paper presents a high-temperature, high-speed atomic force microscopy technique using a qPlus sensor and hybrid frequency demodulation, enabling atomic-resolution imaging of molten metal/solid interfaces above 200°C.

Contribution

The development of a robust high-temperature, high-speed AFM system with a novel scanner and demodulation method for atomic-resolution imaging in liquid environments.

Findings

Achieved atomic-resolution imaging of molten Ga/PtGa_x interface at ~210°C.

Developed a Quadpod scanner with high resonant frequencies for thermal drift tolerance.

Established a hybrid-loop frequency demodulation technique with wider bandwidth.

Abstract

Atomic-resolution imaging on molten metal/solid interfaces at temperatures above 200 {\deg}C was achieved using a high-temperature, high-speed atomic force microscope (AFM) equipped with a qPlus sensor. A tip-scanning high-speed Quadpod scanner for a large mass load of qPlus sensor (2.3 g) was developed to enhance thermal drift tolerance by high-speed scanning and thermal insulation from the heated specimen. This scanner has dominant resonant frequencies of 7.05 kHz (lateral) / 29.7 kHz (vertical) without a load. In addition, the Hybrid-loop frequency demodulation technique for low-resonant-frequency ($f_0$) sensors with a wider bandwidth than conventional phase-locked loop was also established, providing a demodulation bandwidth of $B_{\Delta f_\mathrm{inst}}\sim 0.26 f_0$ without exceeding the theoretical noise of the input deflection signal. Combining these techniques enabled atomic-resolution imaging on the molten $\mathrm{Ga/PtGa_x}$ interface at $\sim$210 {\deg}C. The topographic images obtained at $\sim$210 {\deg}C showed a relatively low-symmetry surface with an oblique lattice with a superstructure, which differed from the primitive rectangular lattice observed in the non-heated sample left at room temperature for 96 h. This demonstrates that the developed high-temperature, high-speed AFM techniques for qPlus sensors enable visualization of non-aqueous liquid/solid interfaces above 200 {\deg}C at atomic resolution, which has various potential applications, such as injection modeling, soldering, and the fabrication of liquid-metal-based catalysts.