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Sharma, Sagar B., Vincent Maurice, Lorena H. Klein, and Philippe Marcus. "Local inhibition by 2-mercaptobenzothiazole of early stage intergranular corrosion of copper." Journal of The Electrochemical Society 167 (November 30, 2020): 161504. https://doi.org/10.1149/1945-7111/abcc36.
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Corrosion inhibition by 2-mercaptobenzothiazole (MBT) at the surface termination of various types of grain boundaries (GBs) was studied at the nanometer scale on microcrystalline copper in HCl acid solution using <em>in situ</em> electrochemical scanning tunneling microscopy (ECSTM). Macroscopic electrochemical analysis by cyclic voltammetry showed highly effective inhibition of Cu(I) active dissolution blocked by MBT pre-adsorption in a potential range of 0.15-0.2 V. ECSTM analysis of the initial stages of intergranular corrosion confirmed the mitigation of net intergranular dissolution by the pre-adsorbed MBT surface layer but also revealed the local accumulation of reaction products in the GB regions. For Coincidence Site Lattice boundaries other than coherent twins, intergranular dissolution, mitigated by the pre-adsorbed MBT layer, and protection by intergranular formation of a film of reaction products were observed. For random GBs, protection by reaction products was dominant, in agreement with their more reactive intrinsic character, generating more Cu(I) ions under anodic polarization and thus promoting the formation of a protective film of reaction products. Coherent twins did not show preferential intergranular reactivity compared to adjacent grains, indicating equally strong efficiency than on grains. These results bring new insight on how inhibition operates locally at various types of GBs.
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Schneeweiss, Marie Anne, Dieter M. Kolb, Dezhong Liu, and Daniel Mandler. "Anodic oxidation of Au(111)." Canadian Journal of Chemistry 75, no. 11 (1997): 1703–9. http://dx.doi.org/10.1139/v97-603.
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The initial stages of the anodic oxidation of Au(111) were investigated by means of cyclic voltammetry as well as in situ scanning tunneling microscopy (STM). The results suggest that the place exchange process, which initiates the oxide formation, starts at step edges. The oxide phase was imaged in situ by scanning tunneling and atomic force microscopy (AFM). The topographic information acquired by the two techniques is compared. Keywords: gold, gold oxide, corrosion, scanning tunneling microscopy (STM), atomic force microscopy (AFM).
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Müller, C., K. Németh, S. Vesztergom, T. Pajkossy, and T. Jacob. "The interface between HOPG and 1-butyl-3-methyl-imidazolium hexafluorophosphate." Physical Chemistry Chemical Physics 18, no. 2 (2016): 916–25. http://dx.doi.org/10.1039/c5cp05406k.
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The interface between highly oriented pyrolytic graphite (HOPG) and 1-butyl-3-metyl-imidazolium hexafluorophosphate (BMIPF<sub>6</sub>) has been studied using cyclic voltammetry, electrochemical impedance spectroscopy, immersion charge measurements and in situ scanning tunneling microscopy (in situ STM).
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Peña Román, Ricardo Javier, Yves Auad, Lucas Grasso, et al. "Design and implementation of a device based on an off-axis parabolic mirror to perform luminescence experiments in a scanning tunneling microscope." Review of Scientific Instruments 93, no. 4 (2022): 043704. http://dx.doi.org/10.1063/5.0078423.
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We present the design, implementation, and illustrative results of a light collection/injection strategy based on an off-axis parabolic mirror collector for a low-temperature Scanning Tunneling Microscope (STM). This device allows us to perform STM induced Light Emission (STM-LE) and Cathodoluminescence (STM-CL) experiments and in situ Photoluminescence (PL) and Raman spectroscopy as complementary techniques. Considering the Étendue conservation and using an off-axis parabolic mirror, it is possible to design a light collection and injection system that displays 72% of collection efficiency (considering the hemisphere above the sample surface) while maintaining high spectral resolution and minimizing signal loss. The performance of the STM is tested by atomically resolved images and scanning tunneling spectroscopy results on standard sample surfaces. The capabilities of our system are demonstrated by performing STM-LE on metallic surfaces and two-dimensional semiconducting samples, observing both plasmonic and excitonic emissions. In addition, we carried out in situ PL measurements on semiconducting monolayers and quantum dots and in situ Raman on graphite and hexagonal boron nitride (h-BN) samples. Additionally, STM-CL and PL were obtained on monolayer h-BN gathering luminescence spectra that are typically associated with intragap states related to carbon defects. The results show that the flexible and efficient light injection and collection device based on an off-axis parabolic mirror is a powerful tool to study several types of nanostructures with multiple spectroscopic techniques in correlation with their morphology at the atomic scale and electronic structure.
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Goritzka, Jan C., Benjamin Herd, Philipp P. T. Krause, Jens Falta, J. Ingo Flege, and Herbert Over. "Insights into the gas phase oxidation of Ru(0001) on the mesoscopic scale using molecular oxygen." Physical Chemistry Chemical Physics 17, no. 21 (2015): 13895–903. http://dx.doi.org/10.1039/c4cp06010e.
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We present an extensive mesoscale study of the initial gas phase oxidation of Ru(0001), employing in situ low-energy electron microscopy (LEEM), micro low-energy electron diffraction (μ-LEED) and scanning tunneling microscopy (STM).
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Tewari, Sumit, Koen M. Bastiaans, Milan P. Allan, and Jan M. van Ruitenbeek. "Robust procedure for creating and characterizing the atomic structure of scanning tunneling microscope tips." Beilstein Journal of Nanotechnology 8 (November 13, 2017): 2389–95. http://dx.doi.org/10.3762/bjnano.8.238.
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Scanning tunneling microscopes (STM) are used extensively for studying and manipulating matter at the atomic scale. In spite of the critical role of the STM tip, procedures for controlling the atomic-scale shape of STM tips have not been rigorously justified. Here, we present a method for preparing tips in situ while ensuring the crystalline structure and a reproducibly prepared tip structure up to the second atomic layer. We demonstrate a controlled evolution of such tips starting from undefined tip shapes.
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Zhang, Sun, Shen, et al. "Recent Progress with In Situ Characterization of Interfacial Structures under a Solid–Gas Atmosphere by HP-STM and AP-XPS." Materials 12, no. 22 (2019): 3674. http://dx.doi.org/10.3390/ma12223674.
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: Surface science is an interdisciplinary field involving various subjects such as physics, chemistry, materials, biology and so on, and it plays an increasingly momentous role in both fundamental research and industrial applications. Despite the encouraging progress in characterizing surface/interface nanostructures with atomic and orbital precision under ultra-high-vacuum (UHV) conditions, investigating in situ reactions/processes occurring at the surface/interface under operando conditions becomes a crucial challenge in the field of surface catalysis and surface electrochemistry. Promoted by such pressing demands, high-pressure scanning tunneling microscopy (HP-STM) and ambient pressure X-ray photoelectron spectroscopy (AP-XPS), for example, have been designed to conduct measurements under operando conditions on the basis of conventional scanning tunneling microscopy (STM) and photoemission spectroscopy, which are proving to become powerful techniques to study various heterogeneous catalytic reactions on the surface. This report reviews the development of HP-STM and AP-XPS facilities and the application of HP-STM and AP-XPS on fine investigations of heterogeneous catalytic reactions via evolutions of both surface morphology and electronic structures, including dehydrogenation, CO oxidation on metal-based substrates, and so on. In the end, a perspective is also given regarding the combination of in situ X-ray photoelectron spectroscopy (XPS) and STM towards the identification of the structure–performance relationship.
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ITAYA, KINGO. "Scanning Tunneling Microscopy(STM). Application for Chemistry. In-Situ STM of Solid-Liquid Interfaces." Nihon Kessho Gakkaishi 35, no. 2 (1993): 135–36. http://dx.doi.org/10.5940/jcrsj.35.135.
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Lo, W. K., and J. C. H. Spence. "STM imaging of the sample or the tip ? an in situ REM study." Proceedings, annual meeting, Electron Microscopy Society of America 50, no. 2 (1992): 1126–27. http://dx.doi.org/10.1017/s0424820100130262.
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Image interpretation for Scanning Tunneling Microscopy (STM) is complicated by inadequate tip characterization. Tip and surface features can be difficult to separate, especially for rough surfaces. Figure 1, an STM image of a gold platelet deposited onto graphite, illustrates some of the possible problems. The doubled image of the platelet and step, for example, is a commonly encountered image artifact caused by tunneling from multiple tip asperities. The shape of the platelet(s) may also be an artifact since they are usually round. Ordinarily, to confirm the interpretation of such objects, experiments would be repeated using different tips and specimens to test for reproducibility. This is not an ideal procedure since the exact experimental conditions are difficult to duplicate. Alternatively, by comparing images of the same topography taken by STM and an independent imaging method, one can expose these artifacts.STM image artifacts were studied using an STM operating inside a Philips EM 400T TEM. This allowed imaging of the same region by Reflection Electron Microscopy (REM) and STM, independently of each other.
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Schouteden, K., D. A. Muzychenko, and C. Van Haesendonck. "Spin-Polarized Scanning Tunneling Spectroscopy of Self-Organized Nanoscale Co Islands on Au(111) Surfaces." Journal of Nanoscience and Nanotechnology 8, no. 7 (2008): 3616–20. http://dx.doi.org/10.1166/jnn.2008.412.
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Magnetic monolayer and bilayer Co islands of only a few nanometer in size were grown by atomic deposition on atomically flat Au(111) films. The islands were studied in situ by scanning tunneling microscopy (STM) and spectroscopy at low temperatures. Spin-resolved tunneling spectroscopy, using an STM tip with a magnetic coating, revealed that the Co islands exhibit a net magnetization perpendicular to the substrate surface due to the presence of spin-polarized d-states. A random distribution of islands with either upward or downward pointing magnetization was observed, without any specific correlation of magnetization orientation with island size or island height.
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Serrano, Giulia, Beatrice Bonanni, Tomasz Kosmala, et al. "In situ scanning tunneling microscopy study of Ca-modified rutile TiO2(110) in bulk water." Beilstein Journal of Nanotechnology 6 (February 12, 2015): 438–43. http://dx.doi.org/10.3762/bjnano.6.44.
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Despite the rising technological interest in the use of calcium-modified TiO2 surfaces in biomedical implants, the Ca/TiO2 interface has not been studied in an aqueous environment. This investigation is the first report on the use of in situ scanning tunneling microscopy (STM) to study calcium-modified rutile TiO2(110) surfaces immersed in high purity water. The TiO2 surface was prepared under ultrahigh vacuum (UHV) with repeated sputtering/annealing cycles. Low energy electron diffraction (LEED) analysis shows a pattern typical for the surface segregation of calcium, which is present as an impurity on the TiO2 bulk. In situ STM images of the surface in bulk water exhibit one-dimensional rows of segregated calcium regularly aligned with the [001] crystal direction. The in situ-characterized morphology and structure of this Ca-modified TiO2 surface are discussed and compared with UHV-STM results from the literature. Prolonged immersion (two days) in the liquid leads to degradation of the overlayer, resulting in a disordered surface. X-ray photoelectron spectroscopy, performed after immersion in water, confirms the presence of calcium.
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Aiga, Norihiro, and Satoshi Takeuchi. "A straightforward optical alignment protocol for STM-based single molecule spectroscopy." Applied Physics Letters 121, no. 9 (2022): 091601. http://dx.doi.org/10.1063/5.0107414.
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A light-accessed scanning tunneling microscope (STM) is a powerful spectroscopic tool that enables chemical analysis at the single molecular level, but it requires highly precise optical alignments to pinpoint the nano-scale tunneling gap, leaving experimental challenges. Here we present straightforward procedures to align the optical setup for STM-luminescence and STM-based tip-enhanced Raman spectroscopy (TERS) performed with a reflection geometry in an ultrahigh vacuum chamber. Observing real-space images of the metal tip apex through a spectrograph set to the zeroth-order diffraction enables “ in situ” optimization of the detection path and introduction of the excitation light of TERS to the nanogap. The best spatial overlap with the nanogap can be achieved by monitoring plasmon-enhanced, low-frequency inelastic scattering of the metal. This protocol allows us to overcome such difficulties in STM-based spectroscopy and facilitates physicochemical study of single adsorbates on nontransparent substrates.
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Larsson, Magnus W., L. Reine Wallenberg, Ann I. Persson, and Lars Samuelson. "Probing of Individual Semiconductor Nanowhiskers by TEM-STM." Microscopy and Microanalysis 10, no. 1 (2004): 41–46. http://dx.doi.org/10.1017/s1431927604040176.
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Along with rapidly developing nanotechnology, new types of analytical instruments and techniques are needed. Here we report an alternative procedure for electrical measurements on semiconductor nanowhiskers, allowing precise selection and visual control at close to atomic resolution. We use a combination of two powerful microscope techniques, scanning tunneling microscopy (STM) and simultaneous viewing in a transmission electron microscope (TEM). The STM is mounted in the sample holder for the TEM. We describe here a method for creating an ohmic contact between the STM tip and the nanowhisker. We examine three different types of STM tips and present a technique for cleaning the STM tip in situ. Measurements on 1-μm-tall and 40-nm-thick epitaxially grown InAs nanowhiskers show an ohmic contact and a resistance of down to 7 kΩ.
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Schroefel, Fabian, Matthias Greve, Karsten Tarhouni, and Olaf M. Magnussen. "Development of a Fast in Situ Scanning Tunneling Microscope for Studies of Electrocatalyst Surfaces." ECS Meeting Abstracts MA2023-02, no. 54 (2023): 2587. http://dx.doi.org/10.1149/ma2023-02542587mtgabs.
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The atomic-scale understanding of processes at the interface between solid electrodes and liquid electrolytes is of high importance for electrochemical energy storage and conversion. Electrochemical scanning tunneling microscopy (ECSTM) is a key technique for the investigation of these interfaces and as such, it has seen widespread use. However, the image acquisition in a conventional ECSTM is a rather slow process, requiring tens of seconds or minutes per image. To help understand the precise reaction mechanisms of atomic and molecular species at solid-liquid interfaces, their movement and interactions need to be resolved. For this, much higher imaging rates are necessary. High-speed STMs (video STMs) are capable of operating at rates >10 images per second, which is sufficiently fast to observe and quantitatively study a wide range of surface dynamic processes, e.g., surface diffusion and growth [1]. However, this technique has not been widely employed, mainly because of the instrumental requirements. The development of an STM for fast in situ measurements poses a set of challenges, which require a carefully planned implementation. For operation in electrochemical environment, the potentials of both STM tip and sample need to be controlled and electrochemical currents at the tip need to be kept way below the tunneling current. Fast image acquisition requires a scanner with high mechanical stability to avoid the excitation of uncontrolled tip oscillations at its resonance frequencies. Additionally, high-bandwidth measurement and control electronics and a sophisticated control software with fast scan generation and data processing capabilities are essential. No commercial system that is capable of fulfilling these requirements exists up to now. For this reason, all existing video-rate STM studies have been performed with home-built setups that employ highly specialized hardware that is not easy to reproduce. In this contribution, we present a new ECSTM developed and built in our group. The setup is based on a Nanonis SPM controller by SPECS and a custom scanner, bipotentiostat, and coarse approach control that were integrated into this system. We show example data and images to demonstrate the performance of the STM. Furthermore, we reveal the modifications employed to make it capable of video-rate imaging. These include a novel scanner design with two independent piezo stacks for slow and high-speed movements and a custom high-bandwidth preamplifier integrated into the scan head as close as possible to the tip. Fast data acquisition is realized by an FPGA-based control software, which features a user-friendly frontend and a backend with good performance even at high image acquisition rates. This software is designed to run alongside the commercial control software for the slow STM operation so that switching between the slow and fast imaging modes is as frictionless as possible. We will show preliminary test results of the early implementation of the fast imaging mode. [1] O. M. Magnussen, Chem. Eur. J. 2019, 25, 12865.
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Bonanni, Beatrice, Massimo Fanfoni, Anna Sgarlata, Fabrizio Caroleo, Roberto Paolesse, and Claudio Goletti. "Perimeter fractal dimension analysis of corrole islands on Au(111) at the solid-water interface." Journal of Porphyrins and Phthalocyanines 24, no. 05n07 (2020): 959–63. http://dx.doi.org/10.1142/s1088424620500078.
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Corrole molecules deposited from aqueous solution on Au(111) arrange flat forming mesa-like clusters (islands), as evidenced by in situ scanning tunneling microscopy (STM). A morphology quantitative assessment of the entire image is given by STM data analysis, evaluating the islands’ fractal dimension as a whole. To this end, two methods are employed: the first exploits the power law that binds the perimeter and the area of all the islands; the second is simply a value of an appropriate average of the fractal dimensions of the islands. In fact the two methods return very close results.
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Lustemberg, P. G., C. Vericat, G. A. Benitez, et al. "Spontaneously Formed Sulfur Adlayers on Gold in Electrolyte Solutions: Adsorbed Sulfur or Gold Sulfide?" J. Phys. Chem. C 112 (July 2, 2008): 11394–402. https://doi.org/10.5281/zenodo.10579183.
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High coverage S phases (surface coverage grater than 0.33), spontaneously formed by immersion of Au(111) in Na2S aqueous solutions at room temperature, have been studied by scanning tunneling microscopy (STM), X-ray photoelectron spectroscopy (XPS), surface enhanced Raman spectroscopy (SERS), electrochemistry, and density functional theory (DFT) calculations. XPS data show no evidence of a AuS phase, as no oxidized gold isdetected. Voltammetric data are also inconsistent with the formation of a AuS phase with 0.5 stoichiometry.In situ and ex situ SERS measurements of S-covered nanostructured gold substrates demonstrate that thesurface species present at the gold surface consist of a mixture of chemisorbed S and polysulfide species, asalready proposed based on in situ STM images. A DFT surface model that is energetically feasible andreproduces well the experimental STM images is presented. The proposed model involves only a smallrearrangement of the upper Au layer and coexistence of monomeric and polymeric S. Therefore, the highcoverage S phase should be described as a mixture of monomeric and polymeric chemisorbed sulfur ratherthan as an extended 2D AuS phase.
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HASEGAWA, SHUJI, ICHIRO SHIRAKI, FUHITO TANABE, et al. "ELECTRICAL CONDUCTION THROUGH SURFACE SUPERSTRUCTURES MEASURED BY MICROSCOPIC FOUR-POINT PROBES." Surface Review and Letters 10, no. 06 (2003): 963–80. http://dx.doi.org/10.1142/s0218625x03005736.
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For in-situ measurements of the local electrical conductivity of well-defined crystal surfaces in ultrahigh vacuum, we have developed two kinds of microscopic four-point probe methods. One involves a "four-tip STM prober," in which four independently driven tips of a scanning tunneling microscope (STM) are used for measurements of four-point probe conductivity. The probe spacing can be changed from 500 nm to 1 mm. The other method involves monolithic micro-four-point probes, fabricated on silicon chips, whose probe spacing is fixed around several μm. These probes are installed in scanning-electron-microscopy/electron-diffraction chambers, in which the structures of sample surfaces and probe positions are observed in situ. The probes can be positioned precisely on aimed areas on the sample with the aid of piezoactuators. By the use of these machines, the surface sensitivity in conductivity measurements has been greatly enhanced compared with the macroscopic four-point probe method. Then the conduction through the topmost atomic layers (surface-state conductivity) and the influence of atomic steps on conductivity can be directly measured.
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Kosmala, Tomasz, Matías Blanco, Gaetano Granozzi, and Klaus Wandelt. "Potential Driven Non-Reactive Phase Transitions of Ordered Porphyrin Molecules on Iodine-Modified Au(100): An Electrochemical Scanning Tunneling Microscopy (EC-STM) Study." Surfaces 1, no. 1 (2018): 12–28. http://dx.doi.org/10.3390/surfaces1010003.
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The modelling of long-range ordered nanostructures is still a major issue for the scientific community. In this work, the self-assembly of redox-active tetra(N-methyl-4-pyridyl)-porphyrin cations (H2TMPyP) on an iodine-modified Au(100) electrode surface has been studied by means of Cyclic Voltammetry (CV) and in-situ Electrochemical Scanning Tunneling Microscopy (EC-STM) with submolecular resolution. While the CV measurements enable conclusions about the charge state of the organic species, in particular, the potentio-dynamic in situ STM results provide new insights into the self-assembly phenomena at the solid-liquid interface. In this work, we concentrate on the regime of positive electrode potentials in which the adsorbed molecules are not reduced yet. In this potential regime, the spontaneous adsorption of the H2TMPyP molecules on the anion precovered surface yields the formation of up to five different potential-dependent long-range ordered porphyrin phases. Potentio-dynamic STM measurements, as a function of the applied electrode potential, show that the existing ordered phases are the result of a combination of van der Waals and electrostatic interactions.
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AVERY, A. R., D. M. HOLMES, T. S. JONES, and B. A. JOYCE. "AN STM STUDY OF THE (2×4) AND c(4×4) RECONSTRUCTIONS FORMED ON GaAs(001) BY MOLECULAR BEAM EPITAXY." Surface Review and Letters 01, no. 04 (1994): 621–24. http://dx.doi.org/10.1142/s0218625x94000801.
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Atomic resolution scanning tunneling microscopy (STM) has been used to study the Asterminated (2×4) and c(4×4) reconstructions formed on GaAs(001) surfaces grown in situ by molecular beam epitaxy (MBE). Filled states STM images of the (2×4) surface always showed unit cells consisting of two As dimers in the top layer. Cooling this surface under an As flux led initially to a highly kinked (2×4) phase before the transition to the c(4×4) structure. At no point were three As dimers observed in the top layer for the (2×4) unit cell. The c(4×4) structure involves the chemisorption of a second layer of As onto an already As-terminated surface. STM images of this surface showed a series of bright rectangular blocks consisting, when complete, of three pairs of As atoms.
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Matsushima, Hisayoshi. "(Invited) In-Situ Observation of Electrodeposition Processes By High Speed Scanning Probe Microscope." ECS Meeting Abstracts MA2022-01, no. 23 (2022): 1154. http://dx.doi.org/10.1149/ma2022-01231154mtgabs.
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Electrodeposition is important technology for developing the novel functional materials such as MEMS. In nanotechnology term, the metal deposition is one of the hot topics since it can control the surface structure precisely and easily. Generally, in metal electrodeposition, an adatom deposited on the electrode diffuses and reaches a step or kink before forming a crystal. In the process, the solvents and additives adsorbed on the surface are often incorporated into the deposits. Since they works as an impurity in the film, they induce the crystal defects and surface defects, which may cause the performance degradation of the produces. Because each processes occur at high speeds and on the atomic scale, the deposition mechanism is difficult to understand. The methods for observing the nucleation have been developed in various ways. With the invention of the scanning probe microscope (SPM) in the 1980’s, we could directly observe the nanostructure. It has been applied to the electrodeposition in aqueous solution. However, since SPM usually takes some time to observe the surface, it is very difficult to catch the dynamic process such as the nucleation and growth of the deposits. Therefore, I believe that the high-speed SPM is the promising solution of both temporal and special problems. There are two types of SPM: scanning tunneling microscope (STM) and atomic force microscope (AFM). In the former type, there is a video rate STM (Video STM) that can capture up to 30 frames per second. Furthermore, the spatial resolution can reach the atomic scale. For example, the Bi kink growth along the step is reported and Pb surface diffusion on the Cu surface is clarified [1-3]. However, since the tunneling current flows continuously between the probe and the substrate during the measurement, it is necessary to sufficiently consider the effects on electrochemical reactions. Although the resolution of the high-speed scanning AFM (HS-AFM) is inferior to that of the STM, the influence of the probe can be less. Therefore, in addition to the nucleation phenomenon during Cu electrodeposition (Fig. 1-A) [4], we have observed the weak adsorption of PEG polymer that is known as the major additives during the electrodeposition (Fig.1-B). By taking the advantage of the low contact pressure of the probe, the transient behavior of nucleation and growth of electrolytic nanobubbles can be observed. In this presentation, the dynamic variations of the electrolytic nucleation & growth by using a high-speed SPM will be presented. References H. Matsushima et al., Faraday Discuss., 193 (2016) 171. A. Taranovskyy et al., Phys. Chem. Chem. Phys., 14 (2012) 10579. S. Guezo et al., J. Phys. Chem. C, 115 (2011) 19336. T. Yoshioka et al., Electrochim. Acta, 302 (2019) 422. Figure 1
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Tentschert, J., P. Fraundorf, and B. Armbruster. "In-situ measurements of scanned probe tip shape with etched nuclear tracks." Proceedings, annual meeting, Electron Microscopy Society of America 51 (August 1, 1993): 528–29. http://dx.doi.org/10.1017/s0424820100148472.
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In air based Scanning Tunneling Microscopy (STM), tip geometry is often unknown so effects in images due to tip shape are difficult to quantify. While the importance of tip structure is often discussed, the methods for getting this information tend to be unsatisfactory in that they often involve ad hoc assumptions (seeing carbon atoms means a good tip) or they lack the ability to make measurements necessary to make quantitative assertions about unknowns. By exploiting the reproducibility of etched nuclear track pits, we have measured the tip interaction profile for an STM tip in air to a resolution of better than 4 nm in three dimensions.As a source of nuclear track pits we coated Nuclepore filters to make them conductive for STM. We used holes in both the 50nm and 200nm range. As a height calibration we took an image of 30nm colloidal Au on HOPG. Our method was as follows: We took an image of an area containing several pits. Next, the image was flattened, several holes were cut and averaged, and a standard deviation image was calculated using the programming language Semper 6, see Figure 1.
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Sakamaki, Kenji, Kohichiroh Hinokuma, and Akira Fujishima. "In situ observation using a scanning tunneling microscope of a local morphological light-induced transformation of n-molybdenumdisulfide in contact with acetonitrile containing a small amount of water." Collection of Czechoslovak Chemical Communications 56, no. 1 (1991): 104–11. http://dx.doi.org/10.1135/cccc19910104.
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A scanning tunneling microscope (STM) under photoelectrochemical control was used to expand the understanding of nanometer scale in situ photoelectrochemical processes at an n-MoS2/acetonitrile interface. A local morphological light-induced transformation occurred around a MoS2(0001) surface depression. This morphological transformation was attributed to the n-MoS2 photoelectrochemical reaction which was controlled by a small amount of water contained in the acetonitrile. After visible light illumination (276 s), photoelectrochemical reactions under anodic polarization transformed the original depression into a "right-angled triangular" type depression.
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Garagnani, David, Paola De Padova, Carlo Ottaviani та ін. "Evidence of sp2-like Hybridization of Silicon Valence Orbitals in Thin and Thick Si Grown on α-Phase Si(111)√3 × √3R30°-Bi". Materials 15, № 5 (2022): 1730. http://dx.doi.org/10.3390/ma15051730.
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One-monolayer (ML) (thin) and 5-ML (thick) Si films were grown on the α-phase Si(111)√3 × √3R30°-Bi at a low substrate temperature of 200 °C. Si films have been studied in situ by reflection electron energy loss spectroscopy (REELS) and Auger electron spectroscopy, as a function of the electron beam incidence angle α and low-energy electron diffraction (LEED), as well as ex situ by grazing incidence X-ray diffraction (GIXRD). Scanning tunneling microscopy (STM), and scanning tunneling spectroscopy (STS) were also reported. The REELS spectra, taken at the Si K absorption edge (~1.840 KeV), reveal the presence of two distinct loss structures attributed to transitions 1s→π* and 1s→σ* according to their intensity dependence on α, attesting to the sp2-like hybridization of the silicon valence orbitals in both thin and thick Si films. The synthesis of a silicon allotrope on the α-phase of Si(111)√3 × √3R30°-Bi substrate was demonstrated by LEED patterns and GIXRD that discloses the presence of a Si stack of 3.099 (3) Å and a √3 × √3 unit cell of 6.474 Å, typically seen for multilayer silicene. STM and STS measurements corroborated the findings. These measurements provided a platform for the new √3 × √3R30° Si allotrope on a Si(111)√3 × √3 R30°-Bi template, paving the way for realizing topological insulator heterostructures from different two-dimensional materials, Bi and Si.
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Schweizer, T. F., U. Niemann, X. Que, et al. "Epitaxial growth and scanning tunneling microscopy of LiV2O4 thin films on SrTiO3(111)." APL Materials 11, no. 2 (2023): 021109. http://dx.doi.org/10.1063/5.0140576.
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LiV2O4 is a mixed-valent spinel oxide and one of a few transition-metal compounds to host a heavy fermion phase at low temperatures. Although numerous experimental studies have attempted to elucidate how its 3 d electrons undergo giant mass renormalization, spectroscopic probes that may provide crucial hints, such as scanning tunneling microscopy (STM), remain to be applied. A prerequisite is atomically flat and pristine surfaces, which, in the case of LiV2O4, are difficult to obtain by the cleavage of small, three-dimensional crystals. We report the epitaxial growth of LiV2O4 thin films with bulklike properties on SrTiO3(111) via pulsed laser deposition and stable STM imaging of the LiV2O4(111) surface. The as-grown films were transferred ex situ to a room-temperature STM, where subsequent annealing with optional sputtering in ultrahigh vacuum enabled compact islands with smooth surfaces and a hexagonal 1 × 1 atomic lattice to be resolved. Our STM measurements provide insights into the growth mechanisms of LiV2O4 on SrTiO3(111) as well as demonstrate the feasibility of performing surface-sensitive measurements of this heavy fermion compound.
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Ohmori, Takashi, Kenji Sakamaki, and Akira Fujishima. "In Situ Observations of Electrode/Solution Interfaces Using a Scanning Tunneling Microscope." CORROSION ENGINEERING 39, no. 10 (1990): 564–75. http://dx.doi.org/10.3323/jcorr1974.39.10_564.
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KUSHVAHA, SUNIL SINGH, ZHIJUN YAN, MAO-JIE XU, WENDE XIAO, and XUE-SEN WANG. "IN SITU STM INVESTIGATION OF Ge NANOSTRUCTURES WITH AND WITHOUT Sb ON GRAPHITE." Surface Review and Letters 13, no. 02n03 (2006): 241–49. http://dx.doi.org/10.1142/s0218625x06008098.
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Germanium was deposited onto highly oriented pyrolytic graphite (HOPG) with and without antimony in ultra-high vacuum. The surface morphology was analyzed using in situ scanning tunneling microscopy (STM) at room temperature (RT). The film grows exclusively in 3D island mode and was affected significantly by substrate defects. At initial stage, nucleation of cluster occurred at step edges and defect sites. Later, we found various types of Ge nanostructures on HOPG in different deposition conditions and stages, including cluster chains, cluster islands, nanowires, and double layer ramified islands at RT. Compact Ge islands were observed when depositing at a substrate temperature of 450 K or after an annealing at 600 K following RT deposition. In addition, the pre-deposited Sb on graphite enhances the sticking probability and suppresses the surface diffusion of Ge atoms, resulting in a significant increase in Ge cluster island density on HOPG terraces.
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Wang, Yi, Xinrui Miao, and Wenli Deng. "Halogen Bonds Fabricate 2D Molecular Self-Assembled Nanostructures by Scanning Tunneling Microscopy." Crystals 10, no. 11 (2020): 1057. http://dx.doi.org/10.3390/cryst10111057.
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Halogen bonds are currently new noncovalent interactions due to their moderate strength and high directionality, which are widely investigated in crystal engineering. The study about supramolecular two-dimensional architectures on solid surfaces fabricated by halogen bonding has been performed recently. Scanning tunneling microscopy (STM) has the advantages of realizing in situ, real-time, and atomic-level characterization. Our group has carried out molecular self-assembly induced by halogen bonds at the liquid–solid interface for about ten years. In this review, we mainly describe the concept and history of halogen bonding and the progress in the self-assembly of halogen-based organic molecules at the liquid/graphite interface in our laboratory. Our focus is mainly on (1) the effect of position, number, and type of halogen substituent on the formation of nanostructures; (2) the competition and cooperation of the halogen bond and the hydrogen bond; (3) solution concentration and solvent effects on the molecular assembly; and (4) a deep understanding of the self-assembled mechanism by density functional theory (DFT) calculations.
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Kurczak, Robert, Paulina Wira, Anna Futyma, Radosław Wasielewski, and Tomasz Kosmala. "Highly Reproducible Automated Tip Coater for In Situ and Operando EC-STM Measurements." Surfaces 7, no. 4 (2024): 990–1002. http://dx.doi.org/10.3390/surfaces7040065.
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High-quality, reproducible tip coatings are essential for minimizing faradaic currents in electrochemical scanning tunneling microscopy (EC-STM), especially during in situ and operando measurements. The variability inherent in manual coating methods, influenced by the operator’s skill and a lack of standardization, can lead to inconsistent results, increased research costs, and a greater workload. This study introduces an Automated Tip Coater (ATC) designed to automate and standardize the tip coating process. The ATC features a tip movement system using stepper motors, a rotation module with a DC motor, and a heating block based on a soldering iron. It is controlled by an Arduino development board, supported by motor drivers, and has a user-friendly interface with an OLED display and encoder. The ATC coating mechanism includes a redesigned plate with a reduced gap size and a milled tray to precisely control the amount of insulating material applied to the tip. A fast cyclic voltammetry test in a 0.1 M HClO4 electrolyte demonstrated that over 75% of ATC-coated tips achieved excellent insulation with leakage currents below ±50 pA—and 30% below ±10 pA—suitable for highly sensitive experiments. Further measurements with EC-STM using the newly coated tips investigated the electrochemical behavior of highly oriented pyrolytic graphite (HOPG), revealing detailed atomic structures under dynamic electrochemical conditions. The ATC significantly enhances reproducibility, reduces dependency on operator skills, and lowers research costs while improving the accuracy and reliability of EC-STM measurements.
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Matsushige, Kazumi. "Structural Evaluation and Molecular Control of Vacuum-Evaporated Organic Thin Films." MRS Bulletin 20, no. 6 (1995): 26–31. http://dx.doi.org/10.1557/s0883769400036940.
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Recently, organic molecules and their complexes with inorganic or metallic materials have drawn many researchers' interest as candidate materials for nanoscale electronic devices of the next generation, especially since Carter's proposal on molecular electronic devices (MEDs) with the functions of gating, switching, memory, etc. in one molecule. However, in order to build such nanoscopic organic electronic devices to replace conventional silicon-based inorganic devices, one must determine how to produce such nanoscale devices and to recognize the electronic states of a single molecule.The scanning tunneling microscope (STM) developed by G. Binning and H. Rohrer made it possible to visualize atoms and molecules in real space under various atmospheres. In addition, STMs can be used as nanoscopic tools for manipulation of individual atoms and molecules, thus realizing MEDs and nanotechnology.In this article, we present our recent achievements concerning the STM as well as in situ x-ray diffraction studies on the molecular structure of ultrathin films prepared by vacuum evaporation. STM observations with atomic resolution reveal the mechanism of nuclei formation and the crystal-growth process in organic molecules. Computer simulations based on STM images of polar organic molecules with electronic dipoles have elucidated the role of electronic interaction for their aggregation structures.Also, nanometer-sized molecular memory can be created by applying an electronic pulse to the evaporated organic films through the STM tip. Furthermore, we discuss the principle of a newly developed in situ total reflection x-ray diffraction (TRXD) apparatus and its application to the evaluation of crystal structure and molecular orientation in organic thin films during the evaporation process, particularly in regard to the role of the substrate, that is, epitaxial growth on organic molecular crystals.
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Fukui, Nobuyuki, Atsushi Taninaka, Toshiki Sugai, et al. "Placing and Imaging Individual Carbon Nanotubes on Cu(111) Clean Surface Using In Situ Pulsed-Jet Deposition-STM Technique." Journal of Nanoscience and Nanotechnology 7, no. 12 (2007): 4267–71. http://dx.doi.org/10.1166/jnn.2007.18106.
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We report pulsed-jet deposition of single-wall and double-wall carbon nanotubes (SWNTs and DWNTs; CNTs) onto a clean Cu(111) surface and their scanning tunneling microscopy(STM) observations under ultra-high vacuum (UHV). The clean Cu(111) surface prepared by a repeated Ar-sputtering and annealing is introduced into a load-lock chamber kept at a 10−5-Pa range vacuum, and the CNTs dispersed in a chloroform solution byultrasonication are pulse-injected onto the surface. Since the substrate is annealed at 700 K to remove the residual solvent molecules, high resolution lattice images of the CNTs are successfullyobserved bySTM. High-resolution chirality-resolved images of the two SWNTs with a metal cluster are also observed, supporting the well accepted growth mechanism of the CNTs from the metal-catalyst cluster. The present pulsed-jet deposition in high-vacuum is superior to the conventional spin-coating or drop-coating techniques for preparing clean and well-defined CNTs on clean surfaces for high-resolution and contamination-free UHV-STM observation.
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Mazur, Piotr, Agata Sabik, Rafał Lewandków, Artur Trembułowicz, and Miłosz Grodzicki. "Obtaining Niobium Nitride on n-GaN by Surface Mediated Nitridation Technique." Crystals 12, no. 12 (2022): 1847. http://dx.doi.org/10.3390/cryst12121847.
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In this work the n-GaN(1000) surface is used as a source of nitrogen atoms in order to obtain niobium nitride film by a surface-mediated nitridation technique. To this end, the physical vapor deposition of the niobium film on GaN is followed by sample annealing at 1123 K. A thermally induced decomposition of GaN and interfacial mixing phenomena lead to the formation of a niobium nitride compound, which contains Nb from thin film and N atoms from the substrate. The processes allowed the obtaining of ordered NbNx films on GaN. Structural and chemical properties of both the GaN substrate and NbNx films were studied in-situ by surface-sensitive techniques, i.e., X-ray and UV photoelectron spectroscopies (XPS/UPS) and a low-energy electron diffraction (LEED). Then, the NbNx/GaN surface morphology was investigated ex-situ by scanning tunneling microscopy (STM).
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Matsushima, H., S. W. Lin, S. Morin, and O. M. Magnussen. "In situ video-STM studies of the mechanisms and dynamics of electrochemical bismuth nanostructure formation on Au." Faraday Discussions 193 (2016): 171–85. http://dx.doi.org/10.1039/c6fd00086j.
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The microscopic mechanisms of Bi electrodeposition on Au(111) and Au(100) electrodes in the overpotential regime were studied by in situ scanning tunneling microscopy with high spatial and temporal resolution. Atomic resolution images of the needle-like Bi(110) deposits formed on Au(111) reveal the central influence of covalent Bi–Bi bonds on the deposit morphology. In the straight steps along the needle edges the Bi atoms are interlinked by these bonds, whereas at the needle tip and at kinks along the needle edges dangling bonds exist, explaining the rapid structural fluctuations at these sites. For ultrathin Bi deposits on Au(100) a more open atomic arrangement was found within the surface plane, which was tentatively assigned to an epitaxially stabilised Bi(111) film. Furthermore, well-defined nanowires, consisting of zigzag chains of Bi surface atoms, were observed on this surface.
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PAN, GE-BO, HUI-JUAN YAN, and LI-JUN WAN. "STRUCTURES OF Ni(II) OCTAETHYLPORPHYRIN AND C60 AT Au(111) SURFACE INVESTIGATED BY STM." Nano 01, no. 01 (2006): 95–100. http://dx.doi.org/10.1142/s1793292006000033.
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In situ scanning tunneling microscopy (STM) was employed to investigate the adsorption of C 60 on a Ni(II) octaethylporphyrin ( NiOEP ) adlayer at liquid/ Au (111) interface. It was found that C 60 molecules tend to form small islands without defined coordination to the underlying NiOEP array. Moreover, increasing the surface coverage of C 60 resulted in the formation of multilayers. The mixture of C 60 and NiOEP prepared in solution formed separated domains. The results suggested that the C 60– C 60 interaction is stronger than that of C 60– NiOEP and dominated the adsorption of C 60 on NiOEP -modified Au (111) surface. This work provides a direct evidence at molecular scale for the coordination of C 60 with NiOEP in a two-dimensional assembly, demonstrating that immobilizing C 60 at the geometric center of NiOEP on an Au (111) surface in solution is complicated.
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Grodzicki, M., P. Mazur, S. Zuber, J. Pers, and A. Ciszewski. "Pd/GaN(0001) interface properties." Materials Science-Poland 32, no. 2 (2014): 252–56. http://dx.doi.org/10.2478/s13536-013-0183-8.
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AbstractThis report concerns the properties of an interface formed between Pd films deposited onto the surface of (0001)-oriented n-type GaN at room temperature (RT) under ultrahigh vacuum. The surface of clean substrate and the stages of Pd-film growth were characterized in situ by X-ray photoelectron spectroscopy (XPS), scanning tunneling microscopy (STM), ultraviolet photoelectron spectroscopy (UPS), and low energy electron diffraction (LEED).As-deposited Pd films are grainy, cover the substrate surface uniformly and reproduce its topography. Electron affinity of the clean n-GaN surface amounts to 3.1 eV. The work function of the Pd-film is equal to 5.3 eV. No chemical interaction has been found at the Pd/GaN interface formed at RT. The Schottky barrier height of the Pd/GaN contact is equal to 1.60 eV.
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OTTAVIANO, L., S. di Nardo, L. LOZZI, M. PASSACANTANDO, P. PICOZZI, and S. SANTUCCI. "NiPC/Si(111)(7 × 7) STUDIED WITH XPS, STM AND TAPPING MODE AIR AFM." Surface Review and Letters 04, no. 01 (1997): 59–64. http://dx.doi.org/10.1142/s0218625x97000109.
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We evaporated a few angstroms of nickel phthalocyanine (NiPC) in ultrahigh vacuum (UHV) on clean single crystal substrates of Si (111)(7×7) and studied in situ the structural and electronic properties of the interface with X-ray photoelectron spectroscopy (XPS) and scanning tunneling microscopy (STM). The mesoscopic morphology of the samples has also been studied in air with a tapping mode atomic force microscope (TM-AFM). XPS measurements with variation of the NiPC thickness suggest planar adsorption of the first layer of admolecules; in particular, we found evidences for stronger chemisorption at the outer benzene rings of the PC molecule. UHV STM measurements confirm the XPS results; despite the lack of intermolecular resolution we show an image suggesting chemisorption commensurate with the substrate lattice and planar stacking consistent with the intermolecular stacking in the known crystalline phases of metal phthalocyanines. TM-AFM shows a growth mode in terms of flat islands of 20–35 Å typical height and a few hundreds of nm width. The potential of imaging with TM-AFM elastic sample properties of soft materials deposited on hard substrates is addressed.
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Pütz, Frederik, Richard Blättner, Yves Kurek, et al. "Liquid Phase Preparation of Organic Thin Films Consisting of Complex Molecules—The Example of the Metallacrown CuCu4." Solids 6, no. 1 (2025): 13. https://doi.org/10.3390/solids6010013.
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Large organic molecules and metal complexes are promising candidates for organic electronics, optoelectronics, and spintronics, with interfaces to metals being critical. Clean preparation in ultra-high vacuum (UHV) is ideal, but many systems are fragile and cannot be thermally sublimed. This study details the preparation of thin films of the metallacrown Cu(II)[12-MCCu(II)N(Shi)-4] (short: CuCu4) from the liquid phase using electrospray injection (ESI) and, in particular, liquid injection (LI). Both methods produce films with intact CuCu4 complexes, but they differ in the amount of co-adsorbed solvent molecules. Enhancements using an argon stream perpendicular to the molecular beam significantly reduce these contaminants. An additional effect occurs due to the counterions (HNEt3)2 of CuCu4. They are co-deposited by LI, but not by ESI. The advantages and limitations of the LI method are discussed in detail. The CuCu4 films prepared by different methods were analyzed with infrared (IR) spectroscopy, ultraviolet and X-ray photoelectron spectroscopy (UPS, XPS), and scanning tunneling microscopy (STM). For thicker films, ex situ and in situ prepared CuCu4 films to exhibit similar properties, but for studying interface effects or ultrathin films, in situ preparation is necessary.
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Santana, Santos Carla, Bright Nsolebna Jaato, Ignacio Sanjuán, Wolfgang Schuhmann, and Corina Andronescu. "Operando Scanning Electrochemical Probe Microscopy during Electrocatalysis." Chemical Reviews 123 (March 27, 2023): 4972–5019. https://doi.org/10.1021/acs.chemrev.2c00766.
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Scanning electrochemical probe microscopy (SEPM) techniques can disclose the local electrochemical reactivity of interfaces in single-entity and sub-entity studies. Operando SEPM measurements consist of using a SEPM tip to investigate the performance of electrocatalysts, while the reactivity of the interface is simultaneously modulated. This powerful combination can correlate electrochemical activity with changes in surface properties, e.g., topography and structure, as well as provide insight into reaction mechanisms. The focus of this review is to reveal the recent progress in local SEPM measurements of the catalytic activity of a surface toward the reduction and evolution of O<sub>2</sub> and H<sub>2</sub> and electrochemical conversion of CO<sub>2</sub>. The capabilities of SEPMs are showcased, and the possibility of coupling other techniques to SEPMs is presented. Emphasis is given to scanning electrochemical microscopy (SECM), scanning ion conductance microscopy (SICM), electrochemical scanning tunneling microscopy (EC-STM), and scanning electrochemical cell microscopy (SECCM).
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Haid, Richard W., Regina M. Kluge, Thorsten O. Schmidt, Federico Calle-Vallejo, and Aliaksandr S. Bandarenka. "(Digital Presentation) High-Resolution Imaging of Active Sites Under Reaction Conditions for Carbon-Based Electrocatalysis." ECS Meeting Abstracts MA2022-01, no. 7 (2022): 627. http://dx.doi.org/10.1149/ma2022-017627mtgabs.
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Due to the abundance and the electrochemical versatility of carbon, it is becoming an increasingly popular material for electrocatalytic applications. Whether it is used as a support material, as a catalyst, or even as a bifunctional catalyst, insights into the reaction processes are of fundamental value. In this light, we employ electrochemical scanning tunneling microscopy (EC-STM) to in-situ evaluate electrode surfaces' behavior and identify the nature of the active sites.[1] The experimental distinction between inactive and active sites of a catalytic system can be achieved by comparing the noise level of surface sites in the EC-STM signal while a reaction is ‘Off’ or ‘On’, respectively. The tunneling current will be stable under both conditions if the scanning tip is positioned over an inactive site. Over an active site, reactions occurring within the tunneling gap will influence the EC-STM signal, which can be observed as locally confined noise features superimposed on the surface morphology. Here, we examine highly ordered pyrolytic graphite (HOPG) in alkaline and acidic media as a model system for carbon-based structures. In an alkaline medium, we compare the activity of specific surface sites under oxygen reduction reaction (ORR) and oxygen evolution reaction (OER) conditions (Figure 1a).[2] In both cases, predominantly steps and defects are active. However, in the case of the OER, the terraces also play a role. For the hydrogen evolution reaction (HER) in acidic media, it was possible to identify individual active sites on the ‘honeycomb’ structured surface with down to atomic resolution (Figure 1b).[3] Apart from HOPG, the technique will be demonstrated for metal-organic frameworks, another class of promising catalysts for ORR and OER. References: [1] Pfisterer, J. H.; Liang, Y.; Schneider, O.; Bandarenka, A. S. Nature 2017, 549, 74. [2] Haid, R. W.; Kluge, R. M.; Schmidt, T. O.; Bandarenka, A. S. Electrochim. Acta 2021, 382, 138285. [3] Kluge, R. M.; Haid, R. W.; Stephens, I. E. L.; Calle-Vallejo, F.; Bandarenka, A. S. Phys. Chem. Figure Caption: Figure 1: a) n-EC-STM measurement of a step under ORR (red) and OER (green) conditions, as well as during reaction ‘Off’ (blue). The most active sites in both cases can be found at steps, indicated by the distinct noise spikes at these positions compared to reaction ‘Off’. Terraces are inactive towards the ORR. However, they do play a role in the OER.[2] © 2021 Elsevier Ltd. b) Atomically resolved active sites on HOPG under HER conditions. Bright spots in the measurements indicate active centers. They can be observed predominantly at step edges and defects, while the basal plane (terrace) remains inactive.[3] © 2021 The Royal Society of Chemistry Figure 1
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Yin, You, Jianfei Jiang, Qiyu Cai, and Bingchu Cai. "Scanning tunneling microscopy and in situ spectroscopy of ultra thin Ti films and nano sized TiOx dots induced by STM." Applied Surface Science 199, no. 1-4 (2002): 319–27. http://dx.doi.org/10.1016/s0169-4332(02)00893-0.
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Leonard, D. N., та P. E. Russell. "Using a Moderate Vacuum, Hot/Cryo-Stage Equipped AFM for In-Situ Observation of α-Phase Growth In 60SN40PB Hypoeutectic Solder". Microscopy and Microanalysis 4, S2 (1998): 316–17. http://dx.doi.org/10.1017/s143192760002170x.
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Atomic force microscopy (AFM) was introduced in 1984, and proved to be more versatile than scanning tunneling microscopy (STM) due to the AFM's capabilities to scan non-conductive samples under atmospheric conditions and achieve atomic resolution. Ultra high vacuum (UHV) AFM has been used in surface science applications when control of oxidation and corrosion of a sample's surface are required. Expensive equipment and time consuming sample exchanges are two drawbacks of the UHV AFM system that limit its use. Until recently, no hot/cryo-stage, moderate vacuum, controlled gas environment AFM was commonly available.We have demonstrated that phase transformations are easily observable in metal alloys and polymers with the use of a moderate vacuum AFM that has in-situ heating/cooling capabilities and quick (within minutes) sample exchange times. This talk will describe the results of experiments involving a wide range of samples designed to make use of the full capabilities of a hot/cryo-stage, controlled gas environment AFM.
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Doud, Evan A., Michael S. Inkpen, Giacomo Lovat, et al. "In Situ Formation of N-Heterocyclic Carbene-Bound Single-Molecule Junctions." Journal of the American Chemical Society 140, no. 28 (2018): 8944–49. https://doi.org/10.5281/zenodo.2579390.
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ABSTRACT: Self-assembled monolayers (SAMs) formed using N-heterocyclic carbenes (NHCs) have recently emerged as thermally and chemically ultrastable alternatives to those formed from thiols. The rich chemistry and strong σ-donating ability of NHCs offer unique prospects for applications in nanoelectronics, sensing, and electrochemistry. Although stable in SAMs, free carbenes are notoriously reactive, making their electronic characterization challenging. Here we report the first investigation of electron transport across single NHC-bound molecules using the scanning tunneling microscope-based break junction (STM-BJ) technique. We develop a series of air-stable metal NHC complexes that can be electrochemically reduced in situ to form NHC−electrode contacts, enabling reliable single- molecule conductance measurements of NHCs under ambient conditions. Using this approach, we show that the conductance of an NHC depends on the identity of the single metal atom to which it is coordinated in the junction. Our observations are supported by density functional theory (DFT) calculations, which also firmly establish the contributions of the NHC linker to the junction transport characteristics. Our work demonstrates a powerful method to probe electron transfer across NHC− electrode interfaces; more generally, it opens the door to the exploitation of surface-bound NHCs in constructing novel, functionalized electrodes and/or nanoelectronic devices.
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NIELSEN, L. PLETH, I. STENSGAARD, F. BESENBACHER, and E. LÆGSGAARD. "COMBINED STM AND RBS INVESTIGATION OF THE NUCLEATION AND GROWTH OF Au ON Ni(110): ALLOYING AND DEALLOYING." Surface Review and Letters 03, no. 05n06 (1996): 1713–19. http://dx.doi.org/10.1142/s0218625x96002655.
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We have performed in-situ Scanning Tunneling Microscopy (STM) and Rutherford Backscattering Spectroscopy (RBS) investigations of the room-temperature (RT) growth of Au on Ni(110) . At low coverages, we observe the formation of a Au/Ni surface alloy, even though Au is immiscible with bulk Ni at RT. At a critical Au coverage of θ Au = 0.4 ML (monolayer), we observe a “dealloying” phase transition where 0.16 ML of Au is “popping” out of the alloyed surface layer and nucleates into [001]-directed dimer/trimer Au chains. Increasing the Au coverage further causes the nucleation and growth of more [001]-directed chains, i.e. their mutual distance in the [Formula: see text] direction decreases until the chain structure finally saturates in a p(5 × 3) structure at θ Au = 0.93 ML . The formation of a surface alloy at low coverage is supported by theoretical calculations within the Effective-Medium Theory (EMT), and an atomic model for the [001]-directed Au chains is developed from a detailed interplay between experiments and theoretical calculations.
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Ren, Wei, Hao Ru, Kun Peng, et al. "Oxygen Adsorption Induced Superconductivity in Ultrathin FeTe Film on SrTiO3(001)." Materials 14, no. 16 (2021): 4584. http://dx.doi.org/10.3390/ma14164584.
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The phenomenon of oxygen incorporation-induced superconductivity in iron telluride (Fe1+yTe, with antiferromagnetic (AFM) orders) is intriguing and quite different from the case of FeSe. Until now, the microscopic origin of the induced superconductivity and the role of oxygen are far from clear. Here, by combining in situ scanning tunneling microscopy/spectroscopy (STM/STS) and X-ray photoemission spectroscopy (XPS) on oxygenated FeTe, we found physically adsorbed O2 molecules crystallized into c (2/3 × 2) structure as an oxygen overlayer at low temperature, which was vital for superconductivity. The O2 overlayer were not epitaxial on the FeTe lattice, which implied weak O2 –FeTe interaction but strong molecular interactions. The energy shift observed in the STS and XPS measurements indicated a hole doping effect from the O2 overlayer to the FeTe layer, leading to a superconducting gap of 4.5 meV opened across the Fermi level. Our direct microscopic probe clarified the role of oxygen on FeTe and emphasized the importance of charge transfer effect to induce superconductivity in iron-chalcogenide thin films.
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Sharma, Sagar B., Vincent Maurice, Lorena H. Klein, and Philippe Marcus. "In situ scanning tunneling microscopy study of 2-mercaptobenzimidazole local inhibition effects on copper corrosion at grain boundary surface terminations." Electrochimica Acta, March 15, 2021, 138150. https://doi.org/10.1016/j.electacta.2021.138150.
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New insight on local inhibition effects of 2-mercaptobenzimidazole (MBI) on early stage intergranular corrosion of copper in hydrochloric acid solution is reported from <em>in situ</em> analysis at the nanometer scale and comparison with 2-mercaptobenzothiazole (MBT) effects in the same pre-adsorption and corrosion testing conditions. Macroscopic cyclic voltammetry analysis, including grains and grain boundary (GB) network, showed a passivation-like behavior in the Cu(I) oxidation range, specific to MBI since not observed with MBT and assigned to the anodic formation of a surface film of Cu(I)-MBI reaction products protecting against dissolution. Electrochemical scanning tunneling microscopy analysis revealed net intergranular dissolution, mitigated by the imperfect protection provided by the anodically formed MBI layer. It also showed local accumulation of reaction products in the GB surface regions, blocking preferential dissolution. For random GBs, blocking by local accumulation of reaction products was dominant, in agreement with the expected higher reactivity of these GBs generating more Cu(I) ions under anodic polarization and thus less efficiently protected by the anodically formed MBI layer. For Coincidence Site Lattice (CSL) boundaries, mitigated net dissolution was more frequently observed. Coherent twins showed equally efficient inhibition in the GB surface region than on adjacent grains. MBI inhibition was less efficient than MBT inhibition with more Cu(I) reaction products generated on the grains to form a surface film and their preferential local accumulation more frequently observed in the GB surface regions.
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Kim, Y. C., M. J. Nowakowski, and D. N. Seidman. "In Situ Cross-Sectional Scanning Tunneling Microscopy Sample Preparation Technique." MRS Proceedings 399 (1995). http://dx.doi.org/10.1557/proc-399-129.
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ABSTRACTA novel in situ sample cleavage technique has been developed for fabricating specimens for cross-sectional scanning tunneling microscopy (XSTM) applications. This technique can be easily adapted to any ultrahigh vacuum (UHV) STM that has a coarse motion capability. A conducting diamond STM tip is used to create micron long scratches on Ge/GaAs or GaAs {001 }-type surfaces. These {001} surfaces are imaged with STM to observe scratch characteristics, and GaAs samples are cleaved to reveal {110}-type faces. Atomic resolution images of {110}-type GaAs surfaces are readily and reproducibly obtained.
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Kuwabara, M., D. A. Smith, and M. E. Welland. "Scanning Tunneling Microscope Study on Amorphous and Crystallized CoSi2 Films." MRS Proceedings 202 (1990). http://dx.doi.org/10.1557/proc-202-615.
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ABSTRACTCoSi2 films were investigated using a scanning tunneling microscope (STM) to understand the film surface topology. The STM images showed that the as-deposited amorphous film had a nano-meter scale roughness which agrees with cross-sectional transmission electron microscope (TEM) observations and also had a uniform granular structure. Images of the crystallized film clearly show the crystal grain structure at the surface and the surface topography change associated with crystallization. In-situ crystallization was accomplished by operating the STM with a high bias; dome shape crystallites were produced at the surface of the amorphous films.
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Thupakula, Umamahesh, We-Hyo Soe, Jimmy Faria, et al. "Low-temperature UHV scanning tunneling microscope double sample holder for in situ exchangeable clean room processed samples." Review of Scientific Instruments 96, no. 4 (2025). https://doi.org/10.1063/5.0228294.
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A generalization of the double sample holder (DSH) concept is presented for an ultra-high vacuum (UHV) low-temperature (LT) multi-probe scanning tunneling microscope (STM). In UHV, the DSH is carrying, side-by-side, a reference metal sample [Au(111) single crystal for STM tip apex preparation] and an ancillary stand-alone small sample holder (for samples originating from a clean room) that can be mounted in situ in/out of the DSH plate. STM tip navigation on both sample surfaces is performed using a UHV scanning electron microscope positioned above the STM stage. For demonstration, clean room nanofabricated graphene nano-gears (diameter down to 25 nm) on a sapphire sample are characterized using STM. The STM tip apices are cleaned on the atomically precise and UHV cleaned Au(111) reference sample surface. Using our new DSH plate and in situ STM tip apex re-preparation on the reference metallic sample, we demonstrate how a clean room originating sample can be imaged at the atomic resolution using our LT-UHV 4-STM.
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Yokota, Yasuyuki. "In situ and ex situ approaches for molecular scale understanding of electrochemical interfaces." Japanese Journal of Applied Physics, April 30, 2024. http://dx.doi.org/10.35848/1347-4065/ad455d.
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Abstract Microscopic studies on electrolyte solution / electrode interfaces provide the most fundamental information not only for understanding the electric double layer formed at the interfaces but also for designing sophisticated electrochemical (EC) devices. In this study, we developed tip-enhanced Raman spectroscopy (TERS), which is based on an electrochemical scanning tunneling microscope (EC-STM), and demonstrated electrochemical TERS (EC-TERS) measurements of benzenethiol monolayers on Au(111). A specially-designed cell enables us to carry out reproducible EC, EC-STM, and EC-TERS measurements, which indicates consistent results among these techniques for the oxidative desorption of the benzenethiol monolayers.
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Taber, Benjamen N., Matthew L. Neill, Trevor N. Thom, Octavia D. Clapp, Vartkess Ara Apkarian, and Joonhee Lee. "In situ plasmonic tip preparation and validation techniques for scanning tunneling microscopy." Journal of Vacuum Science & Technology A 41, no. 5 (2023). http://dx.doi.org/10.1116/6.0002807.
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Among the many parts constituting a scanning tunneling microscope, the metallic tip is the component that directly interacts with the specimen and plays a critical role in visualizing the physical quantity of interest. While tip materials such as W and Pt–Ir are commonly used for topographic imaging and their preparation is well-documented, the preparation of plasmonic materials such as Ag for tip-enhanced Raman spectroscopy is relatively less standardized. Here, we present several in situ Ag tip preparation and validation techniques for the microscopist to use depending on their intended application, including atomic resolution imaging, scanning tunneling spectroscopy (STM), and tip-enhanced Raman spectro-microscopy in ultrahigh vacuum. Besides optical applications, these methods are not limited to Ag but also applicable to other STM tip materials.
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Glade, S. C., T. W. Trelenberg, J. G. Tobin, and A. V. Hamza. "Characterization of Uranium Particles Produced via Pulsed Laser Deposition." MRS Proceedings 802 (2003). http://dx.doi.org/10.1557/proc-802-dd5.5.
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ABSTRACTWe have constructed an experimental apparatus for the synthesis (via pulsed laser deposition) and analysis of nanoparticles and thin films of plutonium and other actinides. In-situ analysis techniques include x-ray photoelectron spectroscopy (XPS), ultraviolet photoelectron spectroscopy (UPS), scanning tunneling microscopy (STM), and scanning tunneling spectroscopy (STS). Also, the oxidation kinetics and the reaction kinetics of actinides with other gaseous species can be studied with this experimental apparatus. Preliminary results on depleted uranium are presented.