International audienceSharp Pt/Ir tips have been reproducibly etched by an electrochemical process using an inverse geometry of an electrochemical cell and a dedicated electronic device which allows us to control the applied voltages waveform and the intensity of the etching current. Conductive tips with a radius smaller than 10 nm were routinely produced as shown by field emission measurements through FowlereNordheim plots. These etched tips were then fixed on a quartz tuning fork force sensor working in a qPlus configuration to check their performances for both scanning tunneling microscopy (STM) and atomic force microscopy (AFM) imaging. Their sharpness and conductivity are evidenced by the resolution achieved in STM and AFM images obtained of epitaxial graphene on 6H-SiC(0001) surface. The structure of an epitaxial graphene layer thermally grown on the 6H-SiC(0001) (6R3x6R3)R30° reconstructed surface, was successfully imaged at room temperature with STM, dynamic STM and by frequency modulated AFM

International audienceThe fabrication of ultra-sharp tips from carbon fiber (CF), which are mounted on a qPlus probe for combined dynamic scanning tunneling microscopy (STM) and frequency modulation atomic force microscopy (FM-AFM) experiments, is reported. The carbon fiber tips were electrochemically etched in a KOH or NaOH solution, using different electronic devices. CF tips with an apex radius ~10 nm, as deduced from the measured slopes of the Fowler–Nordheim plots (kR < 70 nm for k ~ 6), were routinely obtained with a home-made electronic device that controls the intensity of the etching current. Then, these conductive CF tips were also characterized by imaging the 6H-SiC(0001) surface covered by an epitaxial graphene layer in ultra-high vacuum (UHV). The lattice of the (6R3x6R3)R30° reconstruction was regularly imaged by STM working either in non-oscillating mode or in dynamic mode, which also maps the variations of the force gradient. From these measurements with a constant mean-tunneling-current of 20 pA, it was found that the STM tip suffered variations of the tip/surface force gradient in between 8.25 and 16.50 N/m when it scanned the epitaxial graphene layer on the reconstructed 6H-SiC(0001) surface

Reference samples are commonly used for the calibration and quantification of nanoscale electrical measurements of capacitances and dielectric constants in scanning microwave microscopy (SMM) and similar techniques. However, the traceability of these calibration samples is not established. In this work, we present a detailed investigation of most possible error sources that affect the uncertainty of capacitance measurements on the reference calibration samples. We establish a comprehensive uncertainty budget leading to a combined uncertainty of 3% in relative value (uncertainty given at one standard deviation) for capacitances ranging from 0.2 fF to 10 fF. This uncertainty level can be achieved even with the use of unshielded probes. We show that the weights of uncertainty sources vary with the values and dimensions of measured capacitances. Our work offers improvements on the classical calibration methods known in SMM and suggests possible new designs of reference standards for capacitance and dielectric traceable measurements. Experimental measurements are supported by numerical calculations of capacitances to reveal further paths for even higher improvements.

In this paper, a definition of the gain and added noise of impedance matching networks for scanning microwave microscopy is given. This definition can be used to compare different impedance matching techniques independently of the instrument used to measure the S-parameter. As a demonstration, impedance matching devices consisting of a Beatty line, a tuner, and interferometric setups with and without amplifiers have been investigated. Measurement frequencies up to 28 GHz are used, and the maximal resulting gain found was 9504.7 per Siemens.

Measuring resistances at the nanoscale has attracted recent attention for developing microelectronic components, memory devices, molecular electronics, and two-dimensional materials. Despite the decisive contribution of scanning probe microscopy in imaging resistance and current variations, measurements have remained restricted to qualitative comparisons. Reference resistance calibration samples are key to advancing the research-to-manufacturing process of nanoscale devices and materials through calibrated, reliable, and comparable measurements. No such calibration reference samples have been proposed so far. In this work, we demonstrate the development of a multi-resistance reference sample for calibrating resistance measurements in conductive probe atomic force microscopy (C-AFM) covering the range from 100 Ω to 100 GΩ. We present a comprehensive protocol for in situ calibration of the whole measurement circuit encompassing the tip, the current sensing device, and the system controller. Furthermore, we show that our developed resistance reference enables the calibration of C-AFM with a combined relative uncertainty (given at one standard deviation) lower than 2.5% over an extended range from 10 kΩ to 100 GΩ and lower than 1% for a reduced range from 1 MΩ to 50 GΩ. Our findings break through the long-standing bottleneck in C-AFM measurements, providing a universal means for adopting calibrated resistance measurements at the nanoscale in the industrial and academic research and development sectors.

The importance of high dielectric constant materials in the development of high frequency nano-electronic devices is undeniable. Their polarization properties are directly dependent on the value of their relative permittivity. We report here on the nanoscale metrological quantification of the dielectric constants of two high-κ materials, lead zirconate titanate (PZT) and lead magnesium niobate-lead titanate (PMN-PT), in the GHz range using scanning microwave microscopy (SMM). We demonstrate the importance of the capacitance calibration procedure and dimensional measurements on the weight of the combined relative uncertainties. A novel approach is proposed to correct lateral dimension measurements of micro-capacitive structures using the microwave electrical signatures, especially for rough surfaces of high-κ materials. A new analytical expression is also given for the capacitance calculations, taking into account the contribution of fringing electric fields. We determine the dielectric constant values ε_PZT = 445 and ε_PMN-PT = 641 at the frequency around 3.6 GHz, with combined relative uncertainties of 3.5% and 6.9% for PZT and PMN-PT, respectively. This work provides a general description of the metrological path for a quantified measurement of high dielectric constants with well-controlled low uncertainty levels.