Scanning electron microscopy electrochemical deposition

Figure 3. Scanning electron microscopy images of gold electrodes coated by the nanostructured TMPP/C12 monolayer after the electrochemical platinum deposition. The deposition charge was 41 and 160Cm for the left and right images, respectively. (Reprinted from Ref [18], 2005, with permission from Wiley-VCH.)...

The microstructuie of films of the ferrocene dendrimers electrochemically deposited on platinum wire working electrodes was examined by scanning electron microscopy (SEM). The SEM micrograph in Figure 7 corresponding to a film of the octanuclear dendrimer 2 shows a sheet-like compact morphology and exhibits small agglutinations and some porosity. 

Semiconducting thin films of CdSe were electrochemically deposited on Ti substrates [186,187]. The film electrodes were characterized with photoelectrochemical imaging, optical microscopy, and scanning electron microscopy (SEM)/energy-dispersive X-ray analysis. 

The ingress of electrolyte cations into the MOF framework was confirmed by scanning electron microscopy/energy-dispersive x-ray (EDX) analysis of electrochemically treated deposits of Cu-MOF. Results obtained after application of a reductive potential step to Cu-MOF crystals in contact with acetate buffers are shown in Figure 5.3. Here, EDX spectra for (a) pristine Cu-MOF and (b) Cu-MOF after application of a constant potential of-1.0 V for 10 min are shown. EDX spectra of original Cu-MOF crystals exhibits prominent Cu peaks at 1.0, 8.0, and 8.4 keV accompanied by a Si signal at 1.9 keV. After the electrolysis step, an additional Na peak at 1.1 keV appears. 

Thin films of Cu, Co and Ni on Si were prepared from different aqueous electrolytes containing sulfates of the respective metals as well as some supporting electrolyte/additive. Voltammetry and current transients were used to analyze the electrochemical aspects of the deposition. The electrodeposited layers were investigated by scanning electron microscopy (SEM), Rutherford backscattering (RBS), magnetooptical Kerr effect (MOKE), X-ray diffractometry (XRD) as well as by electrical measurements. 

The research involves the development of techniques for deposition of porous catalyst layers by defining the conditions of pressure, sputter rates, and target configurations that will result in appropriate compositions and morphology for the catalyst layer. The effect of catalyst structure and composition on the activity of the catalyst layers will be characterized by x-ray diffraction (XRD), x-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), x-ray absorption spectroscopy (XAS), and electrochemical polarization studies in half cells and full cells. New base metal and noble metal alloys and oxides will also be studied with an aim to identify new compositions that will result in enhanced activity. The catalyst activity target is 2500 mW/mg of anode catalyst. 

Pb by ac electrochemical preparation while the alumina layers remained on the Al-substrate. Deposited metal wires were characterized by atomic force, scanning electron microscopy and Auger-spectroscopy. 

Figure 7.2 Scanning electron microscopy (SEM) images of an electrochemically deposited PPy/LiFePO composite film on a stainless-steel mesh, (a) Around a hole and (b) enlarged image (scale bars 85.7 and 19.9 pm, respectively), (c) Charge-discharge curves and (d) rate capabilities of PPy/LiFePO and PPy/C/PTFE composite electrodes. Panels (a, b, c, and d) are reproduced with permission [40]. Copyright 2007, WUey.

Highly boron-doped diamond films, which have been widely studied in electrochemistry, can be grown by chemical vapor deposition (CVD) and are electrically conductive. Different electrochemical properties of boron-doped diamond films have been studied, such as reactivity [133] and electronic structure [134]. Different characterization techniques have been used to study the electrochemistry of diamond, such as scanning electron microscopy [123, 135] and Raman spectroscopy [125,136]. 

In another investigation [17] it was shown by metallography, X-ray microprobe analysis and scanning electron microscopy that the cathodic incorporation of hafnium into copper primarily yields a HfCu4 compound at the electrode surface. Cu-Hf alloy formation is possible, by electrochemical deposition and also by interdiffiision of the metals. 

Scanning electron microscopy indicates that thin films of polythiophene (100-200 A), which are grown electrochemically and then peeled off the electrode, have smooth homogeneous surfaces [277]. Defects and contours develop when the film thickness is increased to 0.5-11 /u,m. Powdery deposits were observed at several micrometers. Transmission electron microscopy indicates that undoped polythiophenes exhibit a fibrillar morphology. When undoped, the randomly oriented fibrils are approximately 250 A in diameter when doped to 25%, the fibrils swell to approximately 800 A. The doping process appears to be inhomogeneous as some undoped fibrils remain. 

Template synthesis is a relatively simple and easy procedure which has made the fabrication of rather sophisticated nanomaterials accessible to almost any laboratory. Template synthesis reqnires access to instmmentation capable of metal sputtering and electrochemical deposition. The characterization of the fabricated nanostructures can be done using instmmental techniques including spectrophotometry, voltanunetry, optical microscopy, atomic force microscopy, and electronic microscopies (scanning electron microscopy (SEM) and transmission electron microscopy (TEM)). 

Miyashita and Kaneko [1109] studied vapor-deposited films of PPP using cyctic voltammetry and in situ UV-vis spectroscopy. In nonaqueous solutions, reversible anion as well as cation doping and dedoping that involve at least two different doping sites with a dose correlation between electrochemical and spectroscopical data were found. In an aqueous solution, the electrochemical processes were considerably slower. As an explanation, hindered diffusion of hydrated counterions into the film was proposed. Scanning electron microscopy pictures were considered to support this suggestion. The additional optical absorption bands of the doped PPP film were ascribed to transitions from the valence band into the bipolaron state. 

The research activities in the field of electrochemical materials science included electrochemical studies of metals and alloys, which were conducted, employing such methods as cychc voltammetry, electrochemical impedance spectroscopy, quartz crystal nanogravimetry, etc. These investigations in all cases were supported by the characterization of crystalline structure and chemical and phase composition of deposited layers, by means of transmission electron microscopy (TEM), electron diffi action, scanning electron microscopy with microprobe (EDX) analysis. X-ray and Auger electron spectroscopies (XPS), and X-ray diffraction (XRD) techniques. The latter studies were conducted in collaboration with the colleagues from the ICh department of materials strucmre characterization (R. Juskenas, A. Selskis, and V. Jasulaitiene). 

Therefore, innovative layers composed of siloxane/cerium and deposited by atmospheric pressure plasma have been tested. In this study, HMDSO was atomised and introduced as a precursor in an atmospheric pressure DBD plasma. The hybrid coating was obtained by mixing liquid precursor and nanoparticles (HMDSO and nanoAlCeOs) before atomisation. The properties of these different coatings were studied by scanning electron microscopy (SEM) and interferometry measurements. Their corrosion resistance has been determined electrochemically and their self-healing properties have been demonstrated by a combination of electrochemical impedance spectroscopy (EIS) and a nanoscratch method. 

Figure 20 Schematic diagram of a nanoporous BCP template prepared from athickfilm of PS-A-PMMA oriented with an electric field. The PMMA was removed leaving a template. Subsequent electrochemical deposition generated nanowires in a cross-linked PS matrix. On the right is a scanning electron microscopy image of cobalt nanowires electrochemically deposited in the cross-linked PS template.

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