Within the European iMERA-Plus project 'Traceable Characterisation of Nanoparticles' various particle measurement procedures were developed and finally a measurement comparison for particle size was carried out among seven laboratories across six national metrology institutes. Seven high quality particle samples made from three different materials and having nominal sizes in the range from 10 to 200 nm were used. The participants applied five fundamentally different measurement methods, atomic force microscopy, dynamic light scattering (DLS), small-angle x-ray scattering, scanning electron microscopy and scanning electron microscopy in transmission mode, and provided a total of 48 independent, traceable results. The comparison reference values were determined as weighted means based on the estimated measurement uncertainties of the participants. The comparison reference values have combined standard uncertainties smaller than 1.4 nm for particles with sizes up to 100 nm. All methods, except DLS, provided consistent results.
Atomic layer deposition (ALD) raises global interest through its unparalleled conformality. This work describes new microscopic lateral high-aspect-ratio (LHAR) test structures for conformality analysis of ALD. The LHAR structures are...
Traceability of measurements and calibration of devices are needed also at the nanometre scale. Calibration of a commercial atomic force microscope (AFM) was studied as part of a dimensional nanometrology project at MIKES. The calibration procedure and results are presented here. The metrological properties of the AFM were characterized by several measurements. A method developed to calibrate the z scale by a laser interferometer during a normal measurement mode of an AFM is presented. x and y movements were studied with a laser interferometer and the scales were also calibrated using a calibration grid, which was calibrated at MIKES using a laser diffraction method. The advantages and disadvantages of the two methods are discussed. Orthogonalities of the axes were determined by calibration grids and an error separation method. Out-of-plane deviation was measured with a flatness standard. Uncertainty estimates for the coordinate system of the AFM scanner are presented.
In this work we have studied the feasibility of DNA origami nanostructures as dimensional calibration standards for atomic force microscopes (AFMs) at the nanometre scale. The stability of the structures and repeatability of the measurement have been studied, and the applicability for calibration is discussed. A cross-like Seeman tile (ST) was selected for the studies and it was found suitable for repeatable calibration of AFMs. The height of the first height step of the ST was 2.0 nm. Expanded standard uncertainty (k = 2) of the measurement Uc was 0.2 nm. The width of the ST was 88 nm and width of its arm was 28 nm with Uc = 3 nm. In addition, prepared dry samples were found out to be stable at least for 12 months.
Laser diffractometer constructed at MIKES for calibration of pitches of 1D and 2D gratings is based on the Littrow configuration. The grating is rotated by a rotary table. In order to obtain optimal beam quality a fibre-coupled frequency-doubled stabilized Nd:YAG laser is used as a light source and a CCD without internal reflections is used to detect the diffracted beam position. The angle corresponding to the Littrow null position is calculated using a linear fit to equidistantly spaced angles around the null position, which reduces the effect of nonlinearity of the angle encoder scale. Pitch is calculated as a weighted average of the diffraction orders. Novel use of an uncalibrated 1D grating applied to classical error separation methods for angle calibration by full-circle subdivision is described. Diffraction angle measurements are repeated in many sample holder alignments rotated relative to the absolute angle scale. The sequences overlap so that the full circle of the angle scale is covered with multiple evenly distributed sequences, needed for circle-subdivision metrology. The average grating pitch over all sequences is used to separate angle scale errors and a correction table for the rotary table is calculated. The method was verified using a calibrated polygon and an autocollimator. Uncertainty estimates for the grating pitch calibration are given, e.g. the standard uncertainty of 9 pm for 2 µm grating.
This paper describes methods for dynamic measurement and correction of laser interferometer periodic nonlinearity down to the picometre level. A capacitive sensor is used as an external reference for measuring and calculating the periodic interferometer nonlinearity correction function. The experimental interferometer setup is a heterodyne interferometer with symmetrical paths to detectors and time-interval-based phase detection. The periodic nonlinearity is represented as harmonic Fourier components. The time evolution of the nonlinearity function is tracked during measurement. The method is verified by spatial and temporal repeatability of the measured nonlinearity. Linearization repeatability in the 10 pm range is observed.
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