Study on the c-axis preferred orientation of ZnO film on various metal electrodes

ZnO thin film was deposited on various metal electrodes by reactive sputtering, and c-axis preferred orientation of the film has been studied. ZnO, which has high piezoelectricity, is promising for oscillators or filter devices such as surface acoustic wave (SAW) device, gas sensor, and film bulk acoustic resonator (FBAR). But, for the application of ZnO film for these devices, the film should be grown with c-axis normal to the electrode. In this study, Pt, Al, and Au were deposited on Si wafer, and the surface roughness and crystal structure of the ZnO film on the electrode were investigated using AFM, scanning electron microscopy (SEM), and X-ray diffraction (XRD). Columnar structures of ZnO films were grown with c-axis normal to all electrodes, and among them Pt electrode showed the highest preferred orientation of ZnO film.     

STM imaging of metal-coated cell plugs of the archaeobacterium Methanospirillum hungatei GP1

Scanning tunnelling microscopy (STM) images of Pt/Ir- and Pt/Ir/C-coated cell plugs of Methanospirillum hungatei showed paracrystalline structures with P6 symmetry and an 18-nm lattice constant, in agreement with electron microscopy studies. The three-dimensional STM images unambiguously distinguished the two morphologically different proteinaceous plug assemblies and led to an improved understanding of the natural internal organization of whole plugs. Tip convolution effects and the grain size of the metal coating complicated interpretation of finer structures. We discuss possible imaging mechanisms to explain observations in which part of the film was removed but the remaining part of the structure was still imaged reproducibly.     

A method for preparing cross sections of films on wear surfaces for transmission electron microscopy study

A method for preparing cross sections of surface layers which exist on bulk metal substrates for transmission electron microscopy (TEM) study is described. The surface layer or film is protected by a vacuum-deposited or sputtered coating of a suitable metal. A mask is placed over the surface and non-masked areas are subjected to ion beam etching until the substrate is exposed. A thick electroplated layer is then applied to the surface. This layer adheres well to the ion-etched substrate and seals the coated surface film against damage during the usual slicing and grinding steps which are required for the preparation from bulk materials of thin foils for TEM study. The method was developed specifically for the analysis of boundary and extreme pressure lubrication films on wear surfaces together with the near-surface region of the substrate. However, it is also applicable to the investigation of oxide, corrosion and other surface films.     

Lift-off patterning of thin Au films on Si surfaces with atomic force microscopy

We studied a new lift-off process of thin Au film on silicon surfaces in nanometer-scale, combining anodic oxidation patterning with AFM, deposition of Au thin film on the patterned substrate and chemical etching processes of the Si oxide underneath the Au film. For Au films of thickness of 2-5 nm, the Au films on the Si oxide patterns were left unbroken and bent down to stick to Si surface after the removal of the oxide by the chemical etching. For an Au film of 1 nm in thickness, it was possible to lift-off the Au film on oxide patterns of the lines and dots in nanometer-scale using Si oxide as a sacrificial mask.     

Observation of very thin gold island films vacuum-deposited onto MoS2 surface by STM

A gold film of about half a monolayer in thickness was vacuum-deposited onto air-cleaved MoS₂ surface at room temperature at a pressure of 10^?5 Pa. Quasi-two-dimensionally grown gold islands made of several atomic layers were observed by scanning an area of 40×30 nm². The shape of them was oblate and about 20 nm in diameter. Atomic corrugations which reflect the Au(111) surface were observed. The islands were found to move and changed their shape during the microscopy.     

Behaviour of TEM metal grids during in-situ heating experiments

The stability of Ni, Cu, Mo and Au transmission electron microscope (TEM) grids coated with ultra-thin amorphous carbon (α-C) or silicon monoxide film is examined by in-situ heating up to a temperature in the range 500–850 °C in a transmission electron microscope. It is demonstrated that some grids can generate nano-particles either due to the surface diffusion of metal atoms on amorphous film or due to the metal evaporation/redeposition. The emergence of nano-particles can complicate experimental observations, particularly in in-situ heating studies of dynamic behaviours of nano-materials in TEM. The most widely used Cu grid covered with amorphous carbon is unstable, and numerous Cu nano-particles start to form once the heating temperature reaches 600 °C. In the case of Ni grid covered with α-C film, a large number of Ni nano-crystals occur immediately when the temperature approaches 600 °C, accompanied by the graphitization of amorphous carbon. In contrast, both Mo and Au grids covered with α-C film exhibit good stability at elevated temperature, for instance, up to 680 and 850 °C for Mo and Au, respectively, and any other metal nano-particles are detected. Cu grid covered Si monoxide thin film is stable up to 550 °C, but Si nano-crystals appear under intensive electron beam. The generated nano-particles are well characterized by spectroscopic techniques (EDXS/EELS) and high-resolution TEM. The mechanism of nano-particle formation is addressed based on the interactions between the metal grid and the amorphous carbon film and on the sublimation of metal.     

Study on the c-axis preferred orientation of ZnO film on various metal electrodes

ZnO thin film was deposited on various metal electrodes by reactive sputtering, and c-axis preferred orientation of the film has been studied. ZnO, which has high piezoelectricity, is promising for oscillators or filter devices such as surface acoustic wave (SAW) device, gas sensor, and film bulk acoustic resonator (FBAR). But, for the application of ZnO film for these devices, the film should be grown with c-axis normal to the electrode. In this study, Pt, Al, and Au were deposited on Si wafer, and the surface roughness and crystal structure of the ZnO film on the electrode were investigated using AFM, scanning electron microscopy (SEM), and X-ray diffraction (XRD). Columnar structures of ZnO films were grown with c-axis normal to all electrodes, and among them Pt electrode showed the highest preferred orientation of ZnO film.     

High-resolution force microscopy of in-plane magnetization

We have shown for the first time, in previous studies, that the force microscope fitted with a magnetic tip could be used to image magnetic domains in TbFe thin films. In this report we show that the information provided by the magnetic force microscope can also include a measurement of the component of magnetization in the sample which is parallel to the surface. Measurements were taken with a magnetized tip tilted at 45° with respect to the surface normal. In a first experiment, we imaged 1 μm diameter domains thermomagnetically written in a TbFe thin film. In a second measurement, we imaged a series of alternating domains in a thin film Co-alloy disc which was decorated with small magnetized particles, allowing unambiguous identification of the domain boundaries. In both cases we interpret the asymmetric portion of the images to the in-plane component of the sample magnetization.     

Rationale for the application of thin,continuous metal films in high magnification electron microscopy

Various metal films of different thicknesses were deposited on to a particle test specimen and their effects on topographic contrast generation and specimen preservation were determined. Tobacco mosaic virus adsorbed on to thin carbon supports or silicon chips was imaged in TEM or high resolution SE-I SEM at a magnification of 350,000×. Tantalum films of 1–2 nm (average mass) thickness produced best contrasts and prevented volume loss of the particles from electron beam damage. Excessively thick films of 5–10 nm thickness blanketed fine structures and caused severe volume losses. Discontinuous 2 nm thick films of gold or platinum decorated the surfaces, caused a loss in topographic contrasts and induced very high volume losses. Thin continuous metal films were necessary to generate high topographic contrast and to prevent volume loss from beam damage by providing sufficient mechanical stability for small topographic features and increased thermal conductivity of the specimen surface.     

Study of Golgi-impregnated material using the confocal tandem scanning reflected light microscope

The tandem scanning reflected-light microscope (TSM) is a real-time, direct-view confocal microscope. Only those points in the specimen situated in the focal plane contribute information to the image. A Tracor Northern TMS with piezo-electric control of the objective lens was used to generate 3-D images from Golgi-impregnated hamster cerebral cortex. Stereoscopic pairs of images were recorded as 35-mm colour film transparencies by photographing while automatically through-focusing along inclined axes. Transferring the image via a TV camera to the computer, stereo-pairs were obtained by oblique through-focusing and summing, displaying maximum intensity data in each line of sight. Pseudocolour topographic displays were generated by assigning the pixel value in a z map image as the focal depth at which the back-scattered light signal was maximal. The TSM was also modified so that a conventional transmitted-light image with a large depth of field could be obtained simultaneously as the very shallow depth of field confocal back-scattered-light image seen at any focus level. The conventional image is a silhouette of the impregnated neurons: the top surface of the cell is not visible and the relationships of processes that cross over cell bodies cannot be discerned. TSM gives a high-contrast image. The Golgi precipitate over the neuronal surface is resolved as globular or ovoid, coloured particles. The smaller particles also cover the dendritic spines. All the confocal range (extended focus) image display methods satisfactorily demonstrated the 3-D arrangement of cell bodies and processes in the chosen volume.     

激光织构和碳基薄膜复合处理提高钛合金摩擦学性能研究

在重载滑动干摩擦条件下，对比不同织构密度的钛合金表面的摩擦学性能；在耐磨性最好的织构密度钛合金表面再制备碳基薄膜，并与直接在钛合金表面制备的碳基薄膜的摩擦学性能进行对比。结果表明：3种低织构密度条件下，TC4钛合金的摩擦因数减小、磨损率降低；随着织构密度的增大，钛合金材料的摩擦因数变化极小，磨损率有所增加；在织构密度5.95%的钛合金表面制备的碳基薄膜，因织构微凹处产生的小微湍流，减少了摩擦阻力，使得其摩擦因数相比直接在钛合金表面制备的碳基薄膜的摩擦因数有所减小。织构化碳基薄膜的磨损率比钛合金的磨损率降低了99.31%，比直接在钛合金表面制备碳基薄膜的磨损率也降低了约60%，这是因为高接触应力摩擦过程中触发石墨化转变，被磨损的石墨化颗粒碎片嵌入织构微凹中，抑制了摩擦接触界面的磨损行为。     

Development of a parallel detection and processing system using a multidetector array for wave field restoration in scanning transmission electron microscopy

A parallel image detection and image processing system for scanning transmission electron microscopy was developed using a multidetector array consisting of a multianode photomultiplier tube arranged in an 8 x 8 square array. The system enables the taking of 64 images simultaneously from different scattered directions with a scanning time of 2.6 s. Using the 64 images, phase and amplitude contrast images of gold particles on an amorphous carbon thin film could be separately reconstructed by applying respective 8 shaped bandpass Fourier filters for each image and multiplying the phase and amplitude reconstructing factors.     

In-situ STM studies of electrochemical underpotential deposition of Pb on Au(111)

A modified scanning tunnelling microscope (STM) has been used to observe in-situ deposition and stripping of an electrochemical film. With STM tip and sample immersed in an acid electrolyte, single atomic steps on Au(111) have been imaged during the deposition and stripping of a monolayer-thick, underpotential deposit (UPD) of Pb. Integration of the electrochemical current passed during the film deposition and evidence from the STM images themselves confirm monolayer coverage. Our images show enhanced film growth at step edges and defect sites. Observations of single plating and stripping cycles indicate that the Au substrate returns unaltered. Except for atomic resolution images of Au(111), which we have not yet achieved in an electrolyte, all types of Au surface features seen in air are reproduced under the electrolytic solution. The modifications made to our STM in order to perform in-situ electrochemical experiments are described.     

A New Method for the Measurement of Real Area of Contact by the Adhesive Transfer of Thin Au film

In this study, a new experimental method is proposed to measure the real area of contact between a ceramic sphere and an Al surface based on the adhesive transfer of the Au film and the scanning electron microscope (SEM) in the back-scattered mode. A thin film of Au is sputtered on the ceramic sphere before the indentation with the Al surface. The success of this method relies on the fundamental assumption that the adhesive transfer of Au only occurs everywhere inside the contact area. A thin polymer (PMMA) film is deposited between gold film and the ceramic surface to further reduce adhesive strength. After indentation, the interfaces of the ceramic sphere and Al surface are observed by SEM. Experimental evidence that the adhesive transfer of the Au film occurs inside the contact area is given. The entire contact regions on the ceramic sphere and the Al surface are captured in the second electron and back-scattered images with a magnification of 220× (resolution: 432 nm, i.e., distance between neighboring pixels). The contact area can be identified based on both the distributions of the ceramic and Au on the ceramic sphere and Al surface, respectively. The back-scattered images with the magnifications of 5000× and 10,000× (resolution: 20 and 4 nm) are captured at four different locations along the radial direction (starting from the contact center), respectively. The real area of contact decreases from the center to the contact edge.     

Assessing conformal thin film growth under nonstochastic deposition conditions: application of a phenomenological model of roughness replication to synthetic topographic images

In this work, a simple method to follow the evolution of the surface of thin films during growth on substrates characterised by high roughness is detailed. To account for real cases as much as possible, the approach presented is based on the hypothesis that deposition takes place under nonstochastic conditions, such as those typical of many thin film processes in industry and technology. In this context, previous models for roughness replication, which are mainly based on idealised deposition conditions, cannot be applied and thus ad hoc approaches are required for achieving quantitative predictions. Here it is suggested that under nonstochastic conditions a phenomenological relation can be proposed, mainly based on local roughening of surface, to monitor the statistical similarity between the film and the substrate during growth or, in other words, to detect changes of the bare substrate morphological profile occurring during the film growth on top. Such approximation is based on surface representation in terms of power spectral density of surface heights, derived from topographic images; in this work, such method will be tested on two separate batches of synthetic images which simulate thin films growth onto a real rough substrate. In particular, two growth models will be implemented: the first reproduces the surface profile obtained during an atomic force microscopy measurement by using a simple geometrical envelope of surface, regardless the thin film growth mechanism; the second reproduces the columnar growth expected under nonstochastic deposition conditions. It will be shown that the approach introduced is capable to highlight differences between the two batches and, in the second case, to quantitatively account for the replication of the substrate roughness during growth. The results obtained here are potentially interesting in that they account essentially for the geometrical features of the surfaces, and as such they can be applied to synthetic depositions that reproduce different thin film depositions and experimental contexts.     

Characterizing inorganic crystals grown on organic self‐assembled bilayers with scanning probe and electron microscopies

Combined microscopy techniques are used to establish the usability of phosphonic acid layers as promoters of hydroxyapatite (HAp) growth. Using spread coating, octadecylphosphonic acid (OPA) self‐assembled bilayers are delivered to the thin natural oxide layer of a titanium film surface with no prior treatment. These bilayers aggregate two major advantages of phosphonic moieties to titanium surfaces: nucleation of hydroxyapatite crystals from ionic solution and affinity for both titanium oxide surface and HAp crystals. The functionalized substrates and bare titanium (control) samples are immersed in an aqueous solution containing calcium and phosphorus ions. Over a 4‐week immersion time, OPA‐functionalized substrates present numerous large agglomerates of inorganic crystals, in contrast to control samples, with no significant amount of deposits. Initial sample characterization was performed with atomic force microscopy (AFM). Compositional and structural characterization of these agglomerates (using TEM, EDS, and electron diffraction), revealed that they are indeed HAp, the main component of the inorganic bone matrix. Microsc. Res. Tech. 76:1278–1283, 2013. © 2013 Wiley Periodicals, Inc.     

Statistical analysis of support films and the visibility of atoms

The statistical properties of an image of an EM support film could be completely specified by evaluating all orders of joint probabilities of the image optical density values. The probability of random fluctuations in the support image interfering with the identification of images of atoms at the vertices of an n-sided polygon can be determined from the nth order statistics. This probability has been calculated as a function of the OD at specified points, for n= 1, 2 and 3. The first order statistics amount to the probability of finding a particular OD in the image, where the width of the distribution gives the standard deviation of the OD values, or contrast. The second order statistics or covariance (correlation) function provide an intuitive understanding of the granularity of the image. We have measured the first and second order statistics of carbon and aluminum oxide films imaged under a variety of conditions, and have found them useful in quantitative assessment and comparison of the images. The lower contrast of the aluminum oxide films is reflected in both the OD distribution and covariance function. The contrast of both types of films is found to be a non-monotonic function of film thickness.     

Pressure Dependence of Shear Strengths of Thin Films on Metal Surfaces Measured in Ultrahigh Vacuum

The friction coefficient is measured for systems consisting of a thin potassium chloride film deposited onto a variety of clean, flat metal substrates, namely Pb, Sn, Au, Ag, Cu, Pd, Fe, Ta, and two types of steel, which are rubbed by a tungsten carbide pin in an ultrahigh vacuum. The friction coefficients are plotted versus 1/H _S, the inverse of the substrate hardness, where two regimes are found. In the first regime, where deformation at the asperity tips is suggested to be plastic, the observed variation in friction coefficient with substrate hardness is rationalized by assuming that the shear strength S for sliding on a KCl film varies with contact pressure P as S = S ₀ + aP, yielding values for a of 0.14 ± 0.02 and S ₀ of ~60–70 MPa. In the second regime, it is proposed that the softer, film-covered Pb and Sn substrates are closer to being in conformal contact with the rough tribopin. These values of S ₀ and a, along with the measured surface asperity height distribution of the tribopin and the value of the friction coefficient for a KCl monolayer on the metal, are used to rationalize the observed increase in friction coefficient with increasing film thickness.     

Tribology of Co-sputtered Nanocomposite Au/MoS2 Solid Lubricant Films over a Wide Contact Stress Range

Co-sputtered nanocomposite metal/MoS₂ solid lubricant films are traditionally used in high contact stress applications (typically around 1 GPa) because they are hard and conform to the Hertzian contact model, i.e., the coefficient of friction () decreases with increasing contact stress. We are investigating whether appropriate modifications can be made in these films that could make them also work in low contact stress applications, especially sliding electrical contacts (e.g., slip rings) that would benefit from the higher conductivity and environmental robustness of these films. To this end, and also more generally to increase our understanding of how film composition affects performance, we studied the friction and endurance of co-sputtered Au/MoS₂ films in sliding contact in N₂ gas at two vastly different contact stresses, 730 and 0.1 MPa. Seven different film compositions were studied, with Au contents in the range 42-100 at.%, as well as pure MoS₂. The results showed that co-sputtered Au/MoS₂ films outperformed both pure sputtered MoS₂ films and pure sputtered Au films. Optimum films at high contact stress (i.e., those that exhibited the lowest and highest endurance) were films with lower Au contents (i.e., 42 and 59 at.% Au). In contrast, at low contact stress, films with moderately high Au contents (i.e., 75 and 89 at.% Au) performed the best. For films that did not fail by the end of the 2000 m test, Auger Nanoprobe analysis revealed that lubrication was provided by a thin film (1 nm thick) of relatively pure MoS₂, regardless of the contact stress. Based on these results, we hypothesize that at high contact stresses, the low Au content provides optimum amounts of MoS₂ in the contact region, while at low contact stresses, the higher Au contents limit the amount/size of MoS₂ particles that are transferred to the opposing surface, providing a thinner, more uniform transfer film. The results indicate that with appropriate optimization of the metal:MoS₂ ratio, co-sputtered nanocomposite metal/MoS₂ films can be applied to a much wider range of contact stresses than previously studied.