Seznam abstraktů 2023: POSTEROVÁ SEKCE E
Datum: 19.10.2023
The increasing use of nanoparticles (NPs) requires the development of a new method for their preparation. One of these options is to prepare NPs by laser ablation synthesis (LAS). LAS is based on the ablation of the target, which is placed in different environments, either in liquid or ambient gas. The most common laser for these syntheses is neodymium-doped yttrium aluminum garnet (Nd:YAG). LAS synthesis in a liquid environment is usually performed in organic solvents (e.g. ethanol or acetone). The setup was constructed to respect the maximum use of commercially available components and flexibility. The main issue was developing a setup enabling synthesis in gas or liquid environments with lasers operating at different wavelengths. In the case of LAS in liquid, a preparation is provided at 1064 nm, 10 Hz. On the other hand, the synthesis in an ambient gas environment (helium or argon) can be provided at 266 nm, 10 Hz. This wavelength cannot be used for LAS in liquid due to the absorption by liquid. This preparation is placed in the ablation chamber and then trapped in an organic solvent (e.g. acetone). The reason for this trapping is for easier manipulation and to prevent the release of toxic NPs into the atmosphere. The main issue for developing a preparation method is the preparation of fresh NPs due to their rapid aggregation. ACKNOWLEDGEMENTS: Supported by the Grant Agency of Czech Republic: project no. GA22-07635S and Masaryk University: project no. MUNI/A/1298/2022 and MUNI/A/1301/2022.
The modern electronic, sensing or photovoltaic devices are more and more dependent on the materials and junctions made in dimensions of several nanometers. However, the practical use of nano-structures requires comprehensive understanding of the processes occurring in them. Out of layered devices, the inorganic - organic hybrid junctions merge the advances of versatility of organic materials, with precise electronic structure, and morphology control in the inorganic counterparts. Good representatives of versatile organic molecules are transition metal phthalocyanines (MePc, where Me = metal). In the group of inorganic materials, nonstoichiometric alumina (AlxOy) has recently gained attention.
Within presented work we propose the joint ab initio calculation and photoemission - based approach for investigation of the ZnPc / Al2O3-x (where 0.5<x<1) interface formation. First, we addressed the adsorption of ZnPc molecules on alumina surface through geometry optimizations based on DFT computations. Then, we prepared the interfaces in multi-chamber vacuum experimental setup by means of PVD and as a next step we applied (in-situ) X-ray and UV - photoelectron spectroscopies for thorough characterization of the chemical and electronic phenomena taking place at the sub-monolayer ZnPc adsorption. STM I-V spectroscopy is also performed.
Our results provide insights on ZnPc / Al2O3-x interface electronic structure through comprehensive description of adsorption processes governing the charge relocation at the interface.
The revealed phenomena not only expand the atom scale understanding of the interfacial processes, but also are expected to be extremely helpful to consciously design the future hybrid-based devices. ACKNOWLEDGEMENTS: The EU’s Horizon 2020 OCTA project (agreement No. 778158) is acknowledged.
Within the domain of molecular dynamics simulations investigating the ion implantation phenomena, the precise incorporation of the sputtering effect is important for accurate predictions of surface properties and the spatial distribution of implanted particles throughout the target material. However, this becomes computationally demanding task, especially for middle-to-high fluences, owing to the substantial number of atoms required for such simulations. In this study, a novel approach was introduced to address this issue. Sputtering effects based on yield data from the Monte Carlo TRIDYN software were integrated into the molecular dynamics simulations using an in-house algorithm implemented within the LAMMPS code. This integration significantly reduces the computational time, allowing for efficient simulations. The practicality of this algorithm is demonstrated by its application in predicting depth distributions of N particles implanted within an α-Ti target as a function of N fluence. The simulation results with and without the inclusion of the sputtering are compared, and validated with established TRIDYN simulations and experimental data obtained via SIMS. This work showcases an efficient and pertinent approach for predicting high-dose ion implantation effects.
Titanium dioxide (TiO2) is a transition metal oxide with excellent thermal and corrosion resistance. The nanoscale form of TiO2 is one of the unequivocally accepted materials with applications in energy storage, energy conversion, and biomedicine. In nature, it occurs in three crystalline forms, stable rutile, metastable anatase, and metastable brookite. Anatase is the most preferred form due to its high electrochemical activity and wide bandgap energy. Herein, TiO2 colloidal nanoparticles have been synthesized by the thermal decomposition method using Ti(acac)3 as a precursor and 1,2 hexadecanediol as a surfactant. Furthermore, a versatile oleic acid/oleylamine ligand pair is used to control particle size and prevent aggregation during synthesis and after dispersion in a carrier solvent. Based on the three-solvent model, a novel solvent system with high separation efficiency has been discovered to minimize aggregation of nanoparticles. The phase and structural investigations have been done using TEM, EELS, and XRD. We confirmed that the invented synthesis procedure led to the preparation of ~ 5 nm nanoparticles with different TiO2 phases, especially the desired anatase phase. REFERENCES: [1] Silvestri et al., Nanoscale, 2021, 13, 13665.; [2] Mourdikoudis et al., Nanoscale Horiz., 2022, 7, 941.; [3] Tan et al., Nanoscale, 2022, 14, 5482.
An iron sulfide represent suitable candidate for photocatalytic application because of its specific electron-transfer ability, band gap value, good adsorption characteristic, no toxicity, earth abundance and relatively low cost. A pulsed Nd:YAG laser ablation in water and ethanol and the precipitation from Na2S.6H2O and FeCl2.4H2O in sodium metasilicate or TEOS medium provide two distinct processes for the formation of iron sulfide nanoparticles. Comparison of these two pathways and their final products allows consideration of the potential of highly thermodynamically non-equilibrium (laser ablation) and equilibrium (precipitation) processes. Conditions of colloidal stability, particle size and zeta potential of the resulting nanoparticles were determined by Dynamic Light Scattering. Raman and XP spectroscopy and electron microscopy of laser induced colloidal nanoparticles revealed that their outer layer composed of ferric and ferrous sulfates, and that the nanoparticles produced in water are made of high-pressure orthorhombic FeS, cubic magnetite Fe3O4, and tetragonal maghemite γ-Fe2O3, while those formed in ethanol contain hexagonal FeS and cubic magnetite Fe3O4. In contrast to laser ablation process, the precipitation method leads to formation of iron sulfide nanoparticles which are enveloped with SiO2 layer, whereas iron sulfide is completely converted to wüestite FeO when SiO2 stabilization shell is removed by HF.
Coherent Fourier Scatterometry is an optical interference based method suitable for analysis of periodic structures, like diffraction gratings. By using interference of various diffraction orders, the method is very sensitive to both sample geometrical and optical parameters and to its lateral movement, which can be used for accurate non-contact calibration of samples used in nanometrology - i.e. for providing metrological traceability to nanoscience and nanotechnology.
In this contribution we present an experimental setup that can be used for diffraction gratings calibration and we compare it with Scanning Probe Microscopy, which is the typically used method for such a task.
We also present data interpretation tools based on the open source Finite Difference in Time Domain method package GSvit, that can be used for analyzing more complex surface structures, or for accessing more complex grating parameters, like sidewall angle. We discuss the software performance and various data loading options, which can be used when inverse problem solution has to be found during experimental data analysis.
Perfluorinated ionomers transport ions through micropores that are formed by hydrophilic end groups. The requirement of ion conductivity is crucial for perfluorinated ionomers utilized as polymer electrolyte membranes in PEMFCs. The sulfonic acid group, which is a hydrophilic end group present in ionomers is generated by polymerization. This process includes copolymerization of TFE and PSEPVE, which is then subjected to hydrolysis and acid treatment. The EW value represents the number of ion exchange groups.
In this study, Ionomers with varying EWs are synthesized by adjusting the polymerization conditions. To enhance the ionic conductivity, a blend of an ionomer with a high number of ion exchange groups and an ionomer with a low number of ion exchange groups was created. Through blending, ionomers with a higher number of ion exchange groups are oriented inwards, leading to improved ionic conductivity. Furthermore, the durability of the blended membrane is enhanced by blending ionomers with a lower number of ion exchange groups and a higher content of PTFE. To comprehensively evaluate the impact of the blended ionomers, the investigation encompassed an analysis of the pore size distribution utilizing the cryometry technique based on time-domain nuclear magnetic resonance (TD-NMR). Additionally, the surface characteristics of the membrane were rigorously examined through contact angle measurements, and the membrane's chemical durability was evaluated via exposure to the Fenton test. Finally, the ionic conductivity of the membrane was measured to complete the assessment.
The adjustment of surface free energy (SFE) of various substrates plays a major role in coating technology and is perceived as an important part in plenty fields such as medicine, building industry, food packaging and many more. Currently, there are not many processes for generating materials with desired SFE that fulfill economic requirements of being cheap, fast and easily integrable to in-line manufacturing. Wet-chemical methods, but also printing techniques like e.g. screen-printing fail especially in temporal aspects by asking for long-term drying procedures.
Atmospheric pressure plasma deposition is a promising method for thin film deposition. In our work, we demonstrate a fast procedure for generating HMDSO layers by using a diffuse coplanar surface barrier discharge (DCSBD) plasma reactor. To stabilize the layer different plasma post-treatments were examined, resulting in different chemical composition analyzed by Attenuated Total Reflexion Infrared Spectroscopy and X-ray Photon Spectroscopy. The C/O- relation of as received layers after coating varies between 1.4-0.7. By applying a plasma post-treatment, it could be reduced down to 0.1. Furthermore, the surface structure was analyzed by using scanning electron microscopy revealing different morphology depending on the thickness off the layer. The contact angle varies between 40 and 105 °. More hydrophilic (<70 °) layers appeared after plasma post-treatment, ended up at about 90 ° after strong recovery process that is typical for plasma treated surfaces.
In conclusion, modifying surface free energy via DCSBD offers multiple benefits compared to contemporary approaches. This method is rapid, eliminates the need for hazardous solvents and precursors, and obviates the requirement for expensive and time-consuming vacuum systems. ACKNOWLEDGEMENT: This research was supported by Ministry of Education, Youth and Sports of the Czech Republic via the bilateral Mobility project 8J22AT002 co-sponsored by Austrian WTZ-CZ16/2021. We also acknowledge CzechNanoLab Research Infrastructure supported by MEYS CR (LM2023051).
Pulse plating, an electrochemical deposition process that employs pulses of constant current, has proven to be a versatile and reliable method for the preparation of metallic nanostructures. It is an especially useful technique for achieving uniform deposition in recessed areas. Due to the depletion of metal ions, resulting in time-dependent variation of the concentration profiles over the layers adjacent to the metal surface, pulse plating allows for enhanced control over the physical properties of electrodeposited. We have constructed a custom pulse galvanostat based on the circuit design of the Howland current source capable of voltage-controlled current sourcing from microamperes up to a hundred milliamperes with a frequency of up to 100 kHz. The main intended application of this device is the preparation of special plasmonic nanostructures, in particular, Surface-Enhanced Raman Scattering (SERS) substrates. High-quality substrates for SERS are characterized by a high concentration of hot spots, uniformly distributed on their surface. The emphasis is on homogeneity rather than regularity. The highest amplification of the Raman signal occurs in close proximity to surface features with extreme curvature, e.g., narrow gaps, sharp edges, or tips. One of the strategies for the preparation of SERS-active substrates with controlled nanostructures is the use of templates, which are subsequently plated (typically with gold or silver). The results of our original development of the galvanostat, together with its possible application, will be shown and discussed.
Aligned and highly oriented Klockmannite Copper (II) Selenide (CuSe) nanosheets were synthesized by electrodeposition over 304-stainless steel foil. The as-synthesized product was further characterized by XRD and SEM. Aligned CuSe nanosheets possess average thickness 25 nm. Electrochemical capacitive studies of the aligned CuSe nanosheet electrode were carried out in three electrode system. The specific capacitance defined for a scan rate 2 mV/s was found to be 848.2 F/g and 335.6 F/g was obtained at a current density of 0.59 A/g. High surface area of CuSe nanosheets may find the superior applications in various field like, Solar cells, Sensor and Battery etc.
In this work, we reveal how the segregation of polymer additives to the surface (commonly known as blooming) can cause problems, like giant blistering with bubbles that are hundreds of microns or even a millimeter in diameter and increased level of cracking in the 50 nm thick alumina coating. We also demonstrate how the right pre-treatment can help mitigating this problem.
Titanium and its alloys are widely used in aerospace industry, in chemical industry and in total joint replacements because of their low density, high strength, good corrosion resistance, high toughness, and good biocompatibility. However, titanium materials have poor wear resistance and high friction. Implantation of nitrogen into titanium and its alloys significantly improves their properties such as hardness, friction, wear and corrosion resistance. Titanium nitride nanolayer was prepared by nitrogen ion implantation into titanium. The evolution of surface hardness and phase composition after annealing was investigated. The aim of this work is to examine the effect of post-implantation annealing on surface hardness of nitrogen ion implanted titanium.
The advantages of sol-gel coatings, including relatively simple low-temperature preparation processes and the ease of altering their dimensions combined with their diverse industrial applications, are of considerable interest for optimising their properties. The common challenge with most sol-gel deposited coatings is the need to use the curing post-deposition processes, which usually involve heating at elevated temperatures or the use of UV radiation. This leads to higher energy consumption and increased manufacturing complexity. In our work, we demonstrate an alternative way for simple and fast curing of sol-gel coatings by a combination of heating and treatment using various atmospheric pressure cold or hot plasma technologies: Plasma jet, Diffuse Coplanar Surface Barrier Discharge, Gliding arc and InoCoat plasma technology. Our work involves the simple preparation of light-transparent sol-gel coatings, potentially feasible as water and corrosion-resistant protective paints, by spin-coating method on stainless-steel substrates from the composition based on the unique combination of commercially available organic precursors. We focus on investigating the efficiency of plasma curing through nanoindentation hardness measurements and analysis of the morphological alterations, water adhesion, and chemical changes induced by plasma treatment using Atomic Force Microscopy, Water Contact Angle measurement, X-ray Photoelectron Spectroscopy, and Fourier Transform Infrared Spectroscopy, respectively. The enhancement in nanoindentation hardness from 0.75 GPa to 1 GPa and Young modulus from 1.4 GPa to 1.9 GPa exhibited similarity after 60 s of treatment across all employed plasma technologies. Nevertheless, the modification of surface chemistry and water adhesion revealed distinct variations with respect to each plasma technology used.
ACKNOWLEDGEMENT: This research was supported by Ministry of Education, Youth and Sports of the Czech Republic via the bilateral Mobility project 8J22AT002 co-sponsored by Austrian WTZ-CZ16/2021. We also acknowledge CzechNanoLab Research Infrastructure supported by MEYS CR (LM2023051).
Fibrous nanomaterials have enormous application potential, their resemblance to asbestos might, however, hinder their broader use. Nanofibres represent a wide range of different materials with different physicochemical and biological properties and behavior. It is, therefore, crucial to understand underlying mechanisms of their possible toxicity and assign them to specific types of nanofibres. In the present in vitro study, we investigated mechanisms of the effects of nanocellulose (NC) and multi-walled carbon nanotubes (MWCNT) towards macrophages. Macrophages are immune cells, residing in most body tissues and acting as the first line of defense. As such, they are among the most important cell types interacting with inhaled nanomaterials in the lungs and directing their fate in the exposed organism. Although both NC and MWCNT form long, thin, solid fibers, the response of macrophages to incubation with these substances differs. NC directed macrophages towards a pro-inflammatory M1 response, MWCNT contrarily towards an anti-inflammatory M2 phenotype. Through a series of experiments on cultures of mouse macrophages, it was found that the tubes trigger changes that affect gene activity, specifically altering the production of histone-modifying enzymes (proteins that hold DNA strands in an inactive state), DNA methylating enzymes (blocking the transcription of genes in a given DNA region), and the production of microRNAs (short RNA molecules that prevent the translation of the corresponding DNA strands through mRNA into proteins). These results indicate the importance of epigenetic changes in macrophage polarization induced by nanofibers. Excessive and prolonged polarization towards M2 response by MWCNT might lead to lung fibrosis manifested as tissue scaring and loss of function.
Textile yarn is a group of twisted fibers with diameters of a few micrometers, requiring a nano-resolution scanner to capture precise details of the single fibers perfectly to make a digital twine of the scanned yarn. Computed tomography (CT) technology can 3D digitally scan the sample and achieve a digital twin. The fine fibers' diameter requires a nano-CT to achieve a high-resolution yarn's digital twin; nano-cts are more expensive than micro-CTs and require about eight times the scanning time compared to micro-CTs, which means more computational power to reconstruct and analyze the scanned objects. This paper introduces a systematic MATLAB algorithm to regenerate distorted yarn's micro-CT low-resolution cross-section images. The algorithm segments the distorted images' fibers, identifies them, and regenerates the clean, high-resolution fibers. The algorithm performance is compared to the optical microscopic cross-section image measurements using ImageJ.
In this work the P(VDF-co-HFP) was chosen as a matrix due to the better mechanical properties compared to neat PVDF. Strontium titanate (SrTiO3) was chosen as one of the lead-free ceramics and to observe its impact of modification on nanocomposite properties. SrTiO3 nanoparticles were successfully coated with (2,2,2 triflouroethyl methacrylate) short polymer brushes using surface-initiated atom transfer radical polymerization (SI-ATRP). Polymer grafted from the particles surface was analyzed by gel permeation chromatography (polymer chain length and polydispersity) and nuclear magnetic resonance (monomer conversion). Both, neat SrTiO3 nanoparticles and their modified analogues were characterized and further compounded with poly(vinylidene fluoride-co-hexafluoropropylene) (PVDF-co-HFP) to obtain nanocomposites with different nanoparticle content. Mechanical properties were analyzed using DMA and tensile test. Beta phase content was obtained using FTIR. Finally, thermal properties and crystallinity were evaluated using DSC. It was found out that modification of nanoparticles has impact on final piezo properties and other related material properties as well. ACKNOWLEDGEMENTS: The author P. F. would like to gratefully acknowledge to Internal Grant Agency of Tomas Bata University in Zlin (IGA/CPS/2023/007) for financial support. This study was also performed during the implementation of the project Building-up Centre for advanced materials application of the Slovak Academy of Sciences, ITMS project code 313021T081 supported by Research & Innovation Operational Programme funded by the ERDF.
With the increasing environmental awareness, depletion of non-renewable petroleum resource and growing demand on sustainable product development, plant fibers are actually assigned to more technical applications through the development of polymer/ natural fiber composites. Indeed, owing to their important advantages, such as low density, renewability and biodegradability, plant organic fibers represent a viable alternative to inorganic fillers or synthetic fibers in composite materials. Spartium junceum (Sj) is a small shrub that belongs to the leguminosae family and grows in all countries around the Mediterranean Sea. Its fibers have been used as reinforcement for several polymer matrices. In this work the effects of Spartium junceum (Sj) fiber content on the thermal properties of polypropylene/Spartium junceum fiber (PP/Sj), thermoplastic polyurethane/Spartium junceum fiber (TPU/Sj) and polycarbonate/ Spartium junceum fiber (PC/Sj) composites were studied. The neat PP, TPU and PC as well as their composites were characterized by DSC and TGA techniques. DSC analysis measurements illustrates that the addition of Sj no effect on Tm and Tc of PP/Sj composites. The addition, as well as the increase in the content of Sj fibers, results in an increase in the thermal stability of the PP/SJ composite. DSC results showed that the Tg shifts to lower temperatures, while the values of the Tm do not change by increasing the Sj fibers content in TPU/Sj composites. Based on the TGA results the thermal stability of the TPU/Sj composites increased as the Sj fibers content increased. The Tg in PC/BRN composites shifted to lower temperatures compared to the neat PC due to the amorphous structure of lignin. TGA results showed that the thermal stability of PC/Sj composites decreased.
The paper focuses on preparing beta-titanium alloy Ti39Nb for nitrogen ion implantation, a process in which the surface is bombarded with nitrogen ions. To successfully introduce ions into the titanium surface, it is crucial to have a high-quality surface preparation. In addition to grinding and polishing, removing the mechanically affected surface layer is necessary to eliminate residual stress introduction by pre-treatments. In this case, the affected surface layer was removed using ion sputtering-etching. Several analytical methods were chosen to characterize the state of the titanium alloy surface after ion sputtering-etching. These methods included X-ray diffraction to verify residual stress removal, confocal microscopy, and atomic force microscopy to examine surface morphology. For experimental comparison to Ti39Nb, alpha titanium grade 2 was utilized.
Scanning Thermal Microscopy is a thermal measurement technique coming from the Scanning Probe Microscopy family. Using a small resistive heater and sensor integrated on the sharp probe apex, it can either sense the local temperature or local thermal conductivity with spatial resolution in the range of hundreds of nanometers, or even better. The disadvantage of the method is that the heat flow path between probe and sample is most suitable for out of plane components of the thermal conductivity measurements. When we want to measure samples like thin films or nanowires, it would be useful to measure also the in-plane components. Using two probes, where one acts as heat sink and second as heat source, we can better control the heat flow path and reach better this quantity. In this contribution we present a simple modification of a commercial Scanning Probe Microscope for running the two probe measurements, discuss the measurement uncertainties and methodology for measurement and data processing.
With the rise of nanostructured solar cells and electronics came the need for nano-characterisation of electrical properties and the best candidate to fulfil this need is, in many cases, scanning probe microscopy (SPM). For electrical characterization, conductive AFM (C-AFM) is the natural candidate of choice.
During any current-detecting AFM measurement, we detect current flowing through a circuit that consists of the microscope, the probe tip, cantilever and chip, sample and all the interfaces between them. Aside from spreading resistance of the sample we can see that the measurement is dependent on the resistance of the tip that changes with the tip material and shape. Most problematic part of the measurement circuit is, however, the electrical contact between the tip and the sample.
We would like to focus on closer understanding of the sample geometry, tip-sample electrical contact and its evolution with changing normal contact force between the probe and the sample and share findings and thoughts regarding the tip-sample contact resistance and its changes caused by sample topography as well as practical demonstration on how to out-smart these and other inherently present shortcomings of current-detecting AFM in regard to characterization of solar cell electrical properties. Application of two new techniques, Scalpel C-AFM and C-AFM Tomography will be demonstrated, on the silicon solar cell samples.
Modern metrology relies heavily on data fitting. Unfortunately, the most popular method, least squares, reaches its limit at the naonoscale. The concept of an exactly known independent variable and an uncertain dependent variable which is at the core of least squares looses its validity as the relative uncertainties increase. Furthermore, correlations may arise due to the increasing complexity of the measurement process. Typical sources of correlations include the use of reference samples and crosstalk between sensors. These problems can be treated with generalized least squares but only few implementations are available, none of which are suitable for general functions and general covariance matrices.
A new algorithm - Optimal Estimation of Function Parameters by Iterated Linearization (OEFPIL) - has been introduced recently which can handle a wide class of functions and general covariance matrices.
In this work we focus on two typical cases of data fitting in atomic force microscopy (AFM): the evaluation of mechanical properties from force distance curves and the determination of the radius of a spherical lens is a typical application. Ordinary least squares cannot correctly treat the covariance matrix which arises due to calibrations, measurement principles and various errors of AFM such as drift, cross talk, bow. We compare results obtained by both ordinary least squares and OEFPIL and discuss the strengths and weaknesses of this method. The effects of uncertainties and correlations on the parameter estimates and uncertainties are discussed. We further compare the uncertainty estimates obtained by OEFPIL and Monte Carlo method.
Functional surfaces generated by nanotechnological processes require advanced methods combining material and surface analysis. Chemical heterogeneity and lateral structuring at the scale of several nanometers are characteristics for which the simple application of basic microscopic procedures is, in today's time, no longer sufficient. The modern methodological approach involves the application of correlated analyses that combine two or more methods to characterize the functional details of the analyzed surfaces. This study presents atomic force microscopy (AFM) correlated with infrared spectroscopy (IR) of samples based on photothermal expansion (IR-neascope, attocube systems AG, Germany). This method is especially suitable for flat surfaces of organic origin that exhibit spectral absorption of IR radiation in the mid-IR region (fingerprint). This region is characteristic for identifying polymers and their chemical groups. Combining IR spectroscopy with AFM allows pushing the microscope's resolution for spectroscopic purposes to the nanometer range and identifying the presence of characteristic chemical structures through qualitative chemical mapping. Model systems analyzed include surfaces combining different organics and/or metallic elements, e.g. polystyrene particles embedded in polyethylene glycol, metal-organic frameworks (MOFs), and graphene derivate based multilayers. Thanks to these model samples, the study demonstrates methodological limitations and the strength of the method, which is crucial for material characterization, technological optimization, and finally for the synthesis of new nanomaterials in catalysis, photonics, sensors, and nanomedicine.
Correlative microscopy methods become significant due to the possibility of examining several material properties during one measurement. Atomic Force Microscopy in Scanning Electron Microscopy (AFM-in-SEM) is a correlative method that allows simultaneous detection and acquisition of signals from both methods. Graphene/hexagonal Boron Nitride heterostructures (G/hBN), due to the possibility of tuning electronic properties, are studied in many electronic applications. However, research on the structural and electrical properties at the edges of the G/hBN heterostructure is negligible. In this work, we study electronic properties on the edges of single layer G on hBN flakes of various thicknesses prepared on Si and SiO2 substrates. Electronic properties are studied by AFM-in-SEM correlative microscopy. G/hBN morphology correlates with SEM structure. G/hBN heterostructure flakes structures obtained in the secondary electron detector show an enhanced signal on the edges. The pronounced Raman signal is observed in the 2D and Si peaks on the G/hBN edges Si substrate. Enhanced Raman intensity along the G/hBN edge is probably related to localised electrons concentration and suitable perpendicular orientation of plasmonic vibrations. Observing an increased signal in SEM at the edges of the G/hBN heterostructures on the Si substrate confirms an electronic rather than an optical or structural effect. ACKNOWLEDGEMENTS: This work was partly supported by JSPS KAKENHI Grant Numbers JP 20H02191 and 20H00354 and the Technology Agency of the Czech Republic project TM03000033.
Measurements by scanning probe microscopy techniques can be lengthy when acquiring data point-by-point or line-by-line. Scanning the complete image is not needed when e.g. defect detection is desired. Compressed sensing techniques have therefore been developed to gradually increase the detail level, or to focus at specific regions during scanning. We present a tool enabling to quickly identify regions containing possible anomalies, and gather information from suspect regions in the first place. Employed for this are Gaussian processes (GP), which provide an infinite-dimensional generalization of multivariate normal distributions (i.e., distributions over functions with a continuous domain). They can be considered a form of machine learning, and be applied as an interpolation tool. GP can be implemented in computer using standard tools for linear algebra and optimization without need for large computation toolboxes. One can observe that GP prediction variance is higher in regions of data where measured values show a significant deviation. Our strategy is thus to quickly find such regions and perform the scan there, in order to reduce the overall uncertainty across the whole image. A custom software tool has been in development (not released yet), based on a free Fortran library improved by CMI. At present scanning is simulated by reading from an existing image file, later the tool should be integrated into a microscope controlling software.
