Inorganic-oxide-based sample systems are popular for applications in catalysis, sensing, renewable energy, and fuel cells, in which electronic properties play important roles. Environmental conditions, e.g., temperature, can greatly impact the electronic properties and thereby the performance. The lack of basic knowledge of the local variation of electronic properties as a function of temperature limits the fundamental understanding of systems and hampers their robustness. Here, we present temperature-dependent scanning probe microscopy experiments to reveal the variation of contact potential difference (CPD) across different length scales. Our measurements demonstrate that the CPD of inorganic perovskites (e.g., SrTiO 3 ) and metal-oxide semiconductors (e.g., TiO 2 ) evolves significantly with temperature. We show that CPD variation depends on the locality of the measurement and originates from a thermodynamically driven intrinsic doping state. These results will facilitate a fundamental understanding of the electronic properties of oxides and thus ease emerging technologies, rationalized by engineering temperature-dependent electronic properties.
Atomic force microscopy (AFM) is an analytical surface characterization tool that reveals the surface topography at a nanometer length scale while probing local chemical, mechanical, and even electronic sample properties. Both contact (performed with a constant deflection of the cantilever probe) and dynamic operation modes (enabled by demodulation of the oscillation signal under tip–sample interaction) can be employed to conduct AFM-based measurements. Although surface topography is accessible regardless of the operation mode, the resolution and the availability of the quantified surface properties depend on the mode of operation. However, advanced imaging techniques, such as frequency modulation, to achieve high resolution, quantitative surface properties are not implemented in many commercial systems. Here, we show the step-by-step customization of an atomic force microscope. The original system was capable of surface topography and basic force spectroscopy measurements while employing environmental control, such as temperature variation of the sample/tip, etc. We upgraded this original setup with additional hardware (e.g., a lock-in amplifier with phase-locked loop capacity, a high-voltage amplifier, and a new controller) and software integration while utilizing its environmental control features. We show the capabilities of the customized system with frequency modulation-based topography experiments and automated voltage and/or distance spectroscopy, time-resolved AFM, and two-dimensional force spectroscopy measurements under ambient conditions. We also illustrate the enhanced stability of the setup with active topography and frequency drift corrections. We believe that our methodology can be useful for the customization and automation of other scanning probe systems.
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