Quantitative Element-Sensitive Analysis of Individual Nanoobjects.

A reliable and quantitative material analysis is crucial for assessing new technological processes, especially to facilitate a quantitative understanding of advanced material properties at the nanoscale. To this end, X-ray fluorescence microscopy techniques can offer an element-sensitive and non-destructive tool for the investigation of a wide range of nanotechnological materials. Since X-ray radiation provides information depths of up to the microscale, even stratified or buried arrangements are easily accessible without invasive sample preparation. However, in terms of the quantification capabilities, these approaches are usually restricted to a qualitative or semi-quantitative analysis at the nanoscale. Relying on comparable reference nanomaterials is often not straightforward or impossible because the development of innovative nanomaterials has proven to be more fast-paced than any development process for appropriate reference materials. The present work corroborates that a traceable quantification of individual nanoobjects can be realized by means of an X-ray fluorescence microscope when utilizing rather conventional but well-calibrated instrumentation instead of reference materials. As a proof of concept, the total number of atoms forming a germanium nanoobject is quantified using soft X-ray radiation. Furthermore, complementary dimensional parameters of such objects are reconstructed.

A new type of nanoscale reference grating manufactured by combined laser-focused atomic deposition and x-ray interference lithography and its use for calibrating a scanning electron microscope.

Calibration of magnification and nonlinearity of scanning electron microscopy (SEM) is an essential task. In this paper, we proposed a new type of 1D grating sample fabricated by combining laser-focused atomic deposition and x-ray interference lithography as a lateral standard for calibrating SEMs. The calibrations of the grating pattern by a metrological large-range atomic force microscope indicate that the grating sample exhibits outstanding pattern uniformity that surpasses conventional samples fabricated by e-beam lithography: (1) the nonlinear deviation of the grating structures is below +/- 0.5 nm over a measurement range of 5 µm; (2) the maximal variation of the calibrated mean pitch values is lower than 0.01 nm at different locations randomly selected all over the pattern area. The proposed new sample is applied for accurately calibrating the magnification and nonlinearity of a commercial SEM, showing its advantages of easy-of-use and high accuracy. The influence of the defocus level of SEM on the calibration result is also demonstrated. This research offers a feasible solution for highly accurate SEM calibration needed for 3D nanometrology and hybrid metrology demanded in metrology of modern nanoelectronics devices and systems.

Hybrid application of laser-focused atomic deposition and extreme ultraviolet interference lithography methods for manufacturing of self-traceable nanogratings.

A novel hybrid method that combines the laser-focused atomic deposition (LFAD) and extreme ultraviolet (EUV) interference lithography has been introduced. The Cr grating manufactured by LFAD has advantages of excellent uniformity, low line edge roughness and its pitch value determined directly by nature constants (i.e. self-traceable). To further enhance the density of the Cr grating, the EUV interference lithography with 13.4 nm wavelength was employed, which replicated the master Cr grating onto a Si wafer with its pitch reduced to half. In order to verify the performance of the gratings manufactured by this novel method, both mask grating (Cr grating) and replicated grating (silicon grating) were calibrated by the metrological large range scanning probe microscope (Met.LR-SPM) at Physikalisch-Technische Bundesanstalt (PTB). The calibrated results show that both gratings have excellent short-term and long-term uniformity: (i) the calibrated position deviation (i.e. nonlinearity) of the grating is below ±1 nm; (ii) the deviation of mean pitch values of 6 randomly selected measurement locations is below 0.003 nm. In addition, the mean pitch value of the Cr grating is calibrated as 212.781 ± 0.008 nm (k = 2). It well agrees with its theoretical value of 212.7787 ± 0.0049 nm, confirming the self-traceability of the manufactured grating by the LFAD. The mean pitch value of the Si grating is calibrated as 106.460 ± 0.012 nm (k = 2). It corresponds to the shrinking factor of 0.500 33 of the applied EUV interference lithographic technique. This factor is very close to its theoretical value of 0.5. The uniform, self-traceable gratings fabricated using this novel approach can be well applied as reference materials in calibrating, e.g. the magnification and uniformity of almost all kinds of high resolution microscopes for nanotechnology.

True 3D Nanometrology: 3D-Probing with a Cantilever-Based Sensor.

State of the art three-dimensional atomic force microscopes (3D-AFM) cannot measure three spatial dimensions separately from each other. A 3D-AFM-head with true 3D-probing capabilities is presented in this paper. It detects the so-called 3D-Nanoprobes CD-tip displacement with a differential interferometer and an optical lever. The 3D-Nanoprobe was specifically developed for tactile 3D-probing and is applied for critical dimension (CD) measurements. A calibrated 3D-Nanoprobe shows a selectivity ratio of 50:1 on average for each of the spatial directions x, y, and z. Typical stiffness values are kx = 1.722 ± 0.083 N/m, ky = 1.511 ± 0.034 N/m, and kz = 1.64 ± 0.16 N/m resulting in a quasi-isotropic ratio of the stiffness of 1.1:0.9:1.0 in x:y:z, respectively. The probing repeatability of the developed true 3D-AFM shows a standard deviation of 0.18 nm, 0.31 nm, and 0.83 nm for x, y, and z, respectively. Two CD-line samples type IVPS100-PTB, which were perpendicularly mounted to each other, were used to test the performance of the developed true 3D-AFM: repeatability, long-term stability, pitch, and line edge roughness and linewidth roughness (LER/LWR), showing promising results.

Tip wear and tip breakage in high-speed atomic force microscopes.

Tip abrasion is a critical issue particularly for high-speed atomic force microscopy (AFM). In this paper, a quantitative investigation on the tip abrasion of diamond-like-carbon (DLC) coated tips in a high-speed metrological large range AFM device has been detailed. Wear tests are conducted on four different surfaces made of silicon, niobium, aluminum and steel. During the tests, different scanning speeds up to 1 mm/s and different vertical load forces up to approximately 33.2 nN are applied. Various tip characterization techniques such as scanning electron microscopy (SEM) and AFM tip characterizers have been jointly applied to measure the tip form change precisely. The experimental results show that tip form changes abruptly rather than progressively, particularly when structures with steep sidewalls were measured. This result indicates the increased tip breakage risk in high-speed AFM measurements. To understand the mechanism of tip breakage, tip-sample interaction is modelled, simulated and experimentally verified. The results indicate that the tip-sample interaction force increases dramatically in measurement scenarios of steep surfaces.

Metrological large range magnetic force microscopy.

A new metrological large range magnetic force microscope (Met. LR-MFM) has been developed. In its design, the scanner motion is measured by using three laser interferometers along the x, y, and z axes. Thus, the scanner position and the lift height of the MFM can be accurately and traceably determined with subnanometer accuracy, allowing accurate and traceable MFM measurements. The Met. LR-MFM has a measurement range of 25 mm × 25 mm × 5 mm, larger than conventional MFMs by almost three orders of magnitude. It is capable of measuring samples from the nanoscale to the macroscale, and thus, it has the potential to bridge different magnetic field measurement tools having different spatially resolved scales. Three different measurement strategies referred to as Topo&MFM, MFMXY, and MFMZ have been developed. The Topo&MFM is designed for measuring topography and MFM phase images, similar to conventional MFMs. The MFMXY differs from the Topo&MFM as it does not measure the topography profile of surfaces at the second and successive lines, thus reducing tip wear and saving measurement time. The MFMZ allows the imaging of the stray field in the xz- or yz-planes. A number of measurement examples on a multilayered thin film reference sample made of [Co(0.4 nm)/Pt(0.9 nm)]100 and on a patterned magnetic multilayer [Co(0.4 nm)/Pt(0.9 nm)]10 with stripes with a 9.9 µm line width and 20 µm periodicity are demonstrated, indicating excellent measurement performance.

Spatial dimensions in atomic force microscopy: Instruments, effects, and measurements.

Atomic force microscopes (AFMs) are commonly and broadly regarded as being capable of three-dimensional imaging. However, conventional AFMs suffer from both significant functional constraints and imaging artifacts that render them less than fully three dimensional. To date a widely accepted consensus is still lacking with respect to characterizing the spatial dimensions of various AFM measurements. This paper proposes a framework for describing the dimensional characteristics of AFM images, instruments, and measurements. Particular attention is given to instrumental and measurement effects that result in significant non-equivalence among the three axes in terms of both data characteristics and instrument performance. Fundamentally, our position is that no currently available AFM should be considered fully three dimensional in all relevant aspects.

A metrological large range atomic force microscope with improved performance.

A metrological large range atomic force microscope (Met. LR-AFM) has been set up and improved over the past years at Physikalisch-Technische Bundesanstalt (PTB). Being designed as a scanning sample type instrument, the sample is moved in three dimensions by a mechanical ball bearing stage in combination with a compact z-piezostage. Its topography is detected by a position-stationary AFM head. The sample displacement is measured by three embedded miniature homodyne interferometers in the x, y, and z directions. The AFM head is aligned in such a way that its cantilever tip is positioned on the sample surface at the intersection point of the three interferometer measurement beams for satisfying the Abbe measurement principle. In this paper, further improvements of the Met. LR-AFM are reported. A new AFM head using the beam deflection principle has been developed to reduce the influence of parasitic optical interference phenomena. Furthermore, an off-line Heydemann correction method has been applied to reduce the inherent interferometer nonlinearities to less than 0.3 nm (p-v). Versatile scanning functions, for example, radial scanning or local AFM measurement functions, have been implemented to optimize the measurement process. The measurement software is also improved and allows comfortable operations of the instrument via graphical user interface or script-based command sets. The improved Met. LR-AFM is capable of measuring, for instance, the step height, lateral pitch, line width, nanoroughness, and other geometrical parameters of nanostructures. Calibration results of a one-dimensional grating and a set of film thickness standards are demonstrated, showing the excellent metrological performance of the instrument.