Metal-induced reconstructions of the silicon(111) surface

We have used scanning tunnelling microscopy (STM) to study changes in the structure of the Si(111) surface induced by deposition of the group III metals In and Ga. For both metals, several different ordered reconstructions are seen as a function of coverage. The STM images provide new structural information on each of these reconstructions. With In metal deposition, we have seen the surface reconstructions √3×, √3, √31× √31, √7×√3 and 4×1 as the coverage increases. In the case of Ga on Si(111), we have studied structures that exist up to 0·7 ML. At 1/3 ML, there is a √3×√3 structure identical to that of In. Above 0·3 ML there is a different phase that may correspond to the (6·3times6·3) RHEED pattern reported in this coverage range. This surface tends to grow as triangular islands at higher coverages.     

Scanning probe microscopy of biological samples and other surfaces

Scanning probe microscopes derived from the scanning tunnelling microscope (STM) offer new ways to examine surfaces of biological samples and technologically important materials. The surfaces of conductive and semiconductive samples can readily be imaged with the STM. Unfortunately, most surfaces are not conductive. Three alternative approaches were used in our laboratory to image such surfaces. 1. Crystals of an amino acid were imaged with the atomic force microscope (AFM) to molecular resolution with a force of order 10^?8 N. However, it appears that for most biological systems to be imaged, the atomic force microscope should be able to operate at forces at least one and perhaps several orders of magnitude smaller. The substitution of optical detection of the cantilever bending for the measurement by electron tunnelling improved the reliability of the instrument considerably. 2. Conductive replicas of non-conductive surfaces enabled the imaging of biological surfaces with an STM with a lateral resolution comparable to that of the transmission electron microscope. Unlike the transmission electron microscope, the STM also measures the heights of the features. 3. The scanning ion conductance microscope scans a micropipette with an opening diameter of 0·04-0·1 μm at constant ionic conductance over a surface covered with a conducting solution (e.g., the surface of plant leaves in saline solution).     

STM and AFM investigations of high-Tc superconductors

We have studied the (001) surface of single crystal YBa₂Cu₃O_7-x high-T_c superconductors using scanning tunnelling microscopy (STM) and atomic force microscopy (AFM) at room temperature at ambient pressure. Both methods show flat terraces with steps which are multiples of the c-axis lattice constant (of 1·17 nm) high. Our results show that the bulk crystal structure extends to the surface and that the crystals were formed by island growth. Only occasionally tunnelling was possible with sample bias voltages below +1·0 V. We interpret the observed voltage dependence and the difficulty to get good STM images to be due to the presence of a less-conducting surface layer. Auger spectroscopy indicates that carbon is present at the surface, which is probably related to a contamination layer.     

Anomalous voltage dependence of tunnelling microscopy in WSe2

We present scanning tunnelling microscopy (STM) investigations of the layered semiconductor WSe₂. The tunnelling experiments were performed in air and under silicone oil with markedly different results. In air, atomic resolution images of the hexagonally structured surface could be obtained for sample-to-tip voltages of both negative and positive polarities, from ?1·5 to ?0·3 V for negative sample and from +0·6 to +1·6 V for positive sample, respectively. Under silicone oil, however, good atomic images could be seen for negative sample biases down to at least ?14 V, while for positive sample biases no difference with respect to the tunnelling in air was found.     

Photon emission experiments with the scanning tunnelling microscope

We have detected the light emitted from an STM at both ultraviolet (9·5 eV) and optical (1–4 eV) energies. We show that this light contains spectroscopic information on the sample surface comparable to conventional inverse photoelectric spectroscopy, but with nearly atomic spatial resolution. At optical energies we found sufficiently high intensities to allow spatial imaging of the emission probability. We propose that the high quantum efficiency is due to resonance phenomena, and present fluorescence spectra of the emitted light that support this view. We believe that atomic resolution inverse photoemission microscopy and spectroscopy will provide an important new dimension to surface studies.     

Imaging of hydrogen-induced Si(111) surface with the scanning tunnelling microscope

We have directly observed the hydrogen-induced changes of the Si(111)7times7 surface using a scanning tunnelling microscope (STM). The 7times7 reconstructed atomic structure was formed on a clean surface of Si(111). But when the clean surface was dosed with typically 1–2 L [1 L (Langmuir) = 1·33 times 10^?4 Pa. sec] hydrogen, the 7 times 7 image was gradually smeared out and then a 1 times 1 unreconstructed pattern appeared. After dosing with 5–10 L hydrogen, the STM image exhibited a new long-periodic structure together with the 1times1 structure underneath. These experimental results may be ascribed to the chemisorption of hydrogen atoms on clean Si surfaces.     

Study on tungsten electrode deposition effect of 3D metal micro-mold during laminated slip welding

3D metal micro-mold fabricated through the micro double-staged laminated object manufacturing process is formed via stacking and fitting of multi-layer 2D micro structures. In this paper, it is suggested that micro-electric resistance slip welding technology be adopted to optimize the connection of micro structures in 3D metal micro-mold. Moreover, the deposition effect of tungsten electrode which was formed on the micro-mold surface and produced during micro-electric resistance slip welding is also studied. Firstly, the temperature field of electric resistance slip welding was simulated by ANSYS software and the maximum temperature in the slip welding area is 1,219 °C when the number of slip welding discharge is 160, which is far lower than the melting point of tungsten electrode material (3,410 °C). Hence, bulk tungsten will not shed during slip welding; however, the wear of the tungsten electrode will be deposited on the surface of the micro-mold in micro-particle shape. Secondly, the influence of slip welding discharge and surface roughness of tungsten electrode on tungsten deposition effect is studied and the study shows that: the content of tungsten within the slip welding area increases gradually as the number of slip welding discharge increases, and decreases gradually as surface roughness of tungsten electrodes increases. Finally, under 160 time’s slip welding discharge and using tungsten electrodes (0.5-mm diameter and 0.12-μm surface roughness), the 3D metal micro-molds which contains 0.4 % tungsten in slip welding area and has a good quality surface was obtained.     

Preparation of STM tips for in-situ characterization of electrode surfaces

The total current between the tip and the sample in a scanning tunnelling microscopy study of a solid/liquid interface can be dominated by Faradaic charge transfer currents. In such a situation, feedback control of the tunnelling gap, and imaging, is precluded. In this contribution we describe the preparation of glass and polymer coated STM tips that possess < 100 Ų of exposed metal. These tips effectively discriminate against Faradaic current and enable STM imaging in the presence of reversible electroactive solution species at appreciable tip/sample biases.     

Low-temperature scanning tunnelling microscopy and spectroscopy on Pb and Au

We have designed and built a scanning tunnelling microscope (STM) in order to work at temperatures ranging from 1·2 to 300 K. Tunnelling spectroscopy has been performed in Au and Pb with this STM. Our results on Au show different conductance-voltage behaviours, their relation with the cleaning state of the tip being discussed. For Pb, the fitting of our I-V characteristics to a BCS density of states gives A = 1·25 meV for the superconducting energy gap at about 5 K.     

Characterization and local modification of atomically flat gold surfaces by STM

In order to characterize the surface of epitaxial gold on mica in air we have used a scanning tunnelling microscope (STM) to image and to modify this surface. It was possible to create controlled features by applying voltage pulses on the tip while scanning. The voltage threshold for writing (about 3 V, 100 ns pulses) was dependent of the tip condition. The lowest pulses were associated with sub-50 Å feature size. We observed that at ambient temperature the written features disappeared in a time scale of half an hour for the smallest (<30 Å) to a few hours for the bigger features (～500 Å). We have used the same surface as a substrate for organic imaging. We also present images of a polymer deposited on gold.     

Scanning tunnelling microscopy of biomacromolecules

When imaging biomacromolecules with a STM, coating of specimens with a conductive layer is a convenient preparation method which provides a good rate of success. Utilizing evaporated platinum/carbon as a coating film we have investigated two biomacromolecules of very different appearance. The first of these is the HPI-layer, a natural two-dimensional protein crystal with a period of 18 nm, which is found on the surface of the bacterium Deinococcus radiodurans. The second specimen is type IV collagen which forms long triple-helical strands approx. 1·5nm in diameter. The resulting STM pictures compare very well with electron microscopical images.     

Adhesive wear and frictional characteristics of UHMWPE and HDPE sliding against different counterfaces under dry contact condition

Abstract

The current work evaluates the wear and frictional performance of ultrahigh molecular weight polyethylene (UHMWPE) and high density polyethylene (HDPE) sliding against different metal counterfaces, stainless steel(SS), mild steel (MS) and aluminium (Al), under dry contact condition. The experiments were conducted using pin on disc machine at different sliding distances (0–40·32 km), 15 N applied load and 2·8 m s^–1 sliding velocity. Interface temperatures and frictional forces were measured simultaneously during the sliding, while specific wear rates were determined for every 1·68 km sliding distance. Based on the optical microscopy of the worn surface and wear track, frictional and wear results were analysed and discussed. The experimental results showed that the type of counterface material significantly influences both frictional and wear performances of the selected polymers. This was mainly due to the film transfer characteristics. Higher temperature and friction coefficient for UHMWPE and HDPE were evident when sliding took place against Al counterface. Sliding the polymers against stainless steel showed low friction coefficients compared to other counterfaces.     

MEMS-based fast scanning probe microscopes

Scanning probe microscopy is a frequently used nanometer-scale surface investigation technique. Unfortunately, its applicability is limited by the relatively low image acquisition speed, typically seconds to minutes per image. Higher imaging speeds are desirable for rapid inspection of samples and for the study of a range of dynamic surface processes, such as catalysis and crystal growth. We have designed a new high-speed scanning probe microscope (SPM) based on micro-electro mechanical systems (MEMS). MEMS are small, typically micrometer size devices that can be designed to perform the scanning motion required in an SPM system. These devices can be optimized to have high resonance frequencies (up to the MHz range) and have very low mass (10⁻¹¹ kg). Therefore, MEMS can perform fast scanning motion without exciting resonances in the mechanical loop of the SPM, and hence scan the surface without causing the image distortion from which conventional piezo scanners suffer. We have designed a MEMS z-scanner which we have integrated in commercial AFM (atomic force microscope) and STM (scanning tunneling microscope) setups. We show the first successful AFM experiments.     

STM imaging of molecular collagen and phospholipid membranes

The application of STM to biological materiais has been limited by poor conductivity, sample geometry and stability of biological materials. In this paper we describe an STM study of the monomeric helical forms of collagen, a stable, conductive and widely prevalent structural protein. We have also used STM to image artificial Langmuir DPE (dipalmitoyl phosphatidyl ethanolamine) phospholipid membranes. Both molecular collagen and the phospholipid membranes were dried in air on highly oriented pyrolytic graphite (HOPG). Our STM images of collagen dried on HOPG reveal strands 15Å in diameter with a periodicity of about 30Å which correlates with that known to occur in collagen. Spikes which periodically protrude from strands in our STM images of collagen appear to represent pyrrolidine ring structures in the amino acids proline and hydroxyproline. Thus, we report the first STM imaging of native biomolecules revealing intramolecular details and what appear to be specific amino acids. STM imaging of phospholipid membranes show a lattice pattern with densities spaced ～4–5Å apart. These are thought to represent individual phospholipid molecules in an artificial membrane formed on the HOPG. We believe STM and its related technologies will have great future utility in biomolecular studies.     

Silver nanoparticles/polymethacrylic acid (AgNPs/PMA) hybrid nanocomposites-modified electrodes for the electrochemical detection of nitrate ions

AgNPs/PMA hybrid nanocomposite materials with different Ag loadings have been synthesized using a simple chemical route assisted by UV irradiation. The hybrid composites were characterized by means of SEM and TEM, UV–vis spectroscopy and XPS. The as synthesized hybrid samples, composed of small Ag nanoparticles (AgNPs) embedded within the PMA (poly-methacrylic-acid) matrix, have been used to modify the working electrode of disposable screen printed carbon electrodes (SPCEs). It has been observed that hybrid composite with the lowest Ag loading forms dendritic silver structures on the surface of working electrode, whereas at higher loadings massive structures were formed. The electrocatalytic properties of the AgNPs/PMA/SPCEs were investigated toward the reduction of nitrate at neutral pH. Based on these modified electrodes, both voltammetric and amperometric sensors were developed for the electrochemical sensing of nitrate. Voltammetric sensor showed a wide linear range (0–20 mM) and high sensitivity (130 μA mM⁻¹ cm⁻²).     

Formation of large ordered domains in benzenethiol self-assembled monolayers on Au(1 1 1) observed by scanning tunneling microscopy

Benzenethiol (BT) self-assembled monolayers (SAMs) on Au(1 1 1) were prepared as a function of solution temperature after immersion in a 1 mM ethanol solution for 1 day. The surface structures of BT SAMs were examined by means of scanning tunneling microscopy (STM). Although BT molecules usually form disordered SAMs containing the Au adatom islands at room temperature, we found that they formed two-dimensional ordered SAMs containing a large size domain at a high solution temperature of 50 or 75 °C. High-resolution STM imaging revealed that BT SAMs on Au(1 1 1) formed at 50 °C have a (2×3√2)R23° packing structure. From our STM study, we revealed that two-dimensional ordered BT SAMs on Au(1 1 1) can be obtained by changing the solution temperature.     

半导体硅电极多通道放电机理研究

为了实现电火花加工同一时刻形成多个放电通道蚀除工件,克服现有放电加工理论中同一时刻仅有一个放电通道蚀除工件的限制,提出了采用半导体材料作为电极进行放电加工的新方法。首先,通过试验证明以半导体硅为电极加工金属可以形成多通道放电;其次,建立了半导体电极单通道放电等效电路模型,发现半导体电极在放电加工时不是一个等势体,并进行了电势差分布试验,验证了多通道放电形成的原因是远离放电点处的电势较高,可以同时形成击穿产生放电;最后,进行了半导体硅电极单脉冲放电试验及成型加工试验。试验结果显示,半导体硅电极通过1次脉冲放电同时形成多个放电通道,有效地分散放电能量,相较于金属电极,每个放电坑的直径和深度都显著减小。在相同放电参数下,对比钢电极,用硅电极进行电火花加工的表面粗糙度值下降71.7%。     

Observation of removal of an Fmoc protecting group by scanning tunneling microscopy

We demonstrate here by imaging successive surface reactions in self-assembled monolayers (SAMs) on Au(1 1 1) at molecular scale with a scanning tunneling microscope (STM): (i) SAM matrices formation with 1-octanethiol on Au(1 1 1) in ethanol, (ii) insertion of N-Fmoc-aminooctanethiol into the SAM matrices in ethanol, and (iii) removal of the Fmoc protecting group with tris(2-aminoethyl)amine (TAEA). The total reaction is formation of SAMs containing a small amount of NH₂ terminated molecules in the CH₃ terminated SAM matrices. After the reaction of the protecting group with TAEA, STM imaging revealed the decrease in heights of the inserted molecules on average. We attributed this observation to removal of the protecting group by taking account of a convolution of electronic and topographic contributions to observed STM heights. Apparent areas of the terminal groups, however, became larger on removal. The increase in the areas was attributed to water adsorption to the NH₂ terminal group under air.     

In situ,atomic scale observation of electrode topography and reactions

The topographical changes occurring on a Au(111) electrode during simple electrochemical reactions have been followed with an STM capable of operating in situ, i.e. in the electrochemical environment, and of yielding atomic scale resolution. Changes in the surface structure induced by adsorption and desorption of Cl^? ions could be observed and the effects of subjecting the sample to an oxidation-reduction cycle could be monitored.     

Two-photon excited lifetime imaging of autofluorescence in cells during UV A and NIR photostress

By monitoring coenzyme autofluorescence modifications. as an indicator of cell damage. the cellular response to femtosecond near-infrared (NIR) radiation (two-photon absorption) was compared with exposure to low-power UV A radiation (one-photon absorption). Excitation radiation from a tunable Ti-sapphire laser. focused through highnumerical- aperture microscope optics. provided diffractionlimited mlcrobeams of an adjustable peak power. Laser scanning NIR microscopy was used to detect spatially the intracellular distribution of fluorescent coenzymes by fluorescence intensity imaging as well as fluorescence lifetime imaging (_T-mapping). Upon the onset of UV or NIR exposure. Chinese hamster ovary cells exhibited blue/green autofluorescence witq a mean lifetime of 2·2 ns. which was attributed to NAD(P)H in mitochondria. Exposure to 365 nm radiation from a high-pressure mercury lamp (1 m W. 300 J cm^-2 ) resulted in oxidative stress correlated with increased autofluorescence intensity. onset of nuclear fluorescence. and a fluorescence lifetime decrease. The cellular response to femtosecond NIR micro beams depended significantly on peak power. Peak powers above a threshold value of about 0·5kW (average power: 6mW). 0·55kW (7mW) and 0·8kW (lOmW) at 730nm. 760nm and 800nm. respectively. resulted in the onset of short-lived luminescence with higher intensity (100x) than the intracellular NAD(P)H fluorescence. This luminescence. accompanied by destruction of cellular morphology. was localized and occurred in the mitochondrial region. In contrast. beams at a power of less than 0·5 kW allowed nondestructive fluorophore detection with high spatial and temporal resolution without modification of cellular redox state or cell morphology.