EELS characterization of “Smut” layer films on steel surface prepared for chrome plating by anodic etching

Author(s):  
E Y. Wang ◽  
J. T. Cherian ◽  
A. Madsen ◽  
R. M. Fisher

Many steel parts are electro-plated with chromium to protect them against corrosion and to improve their wear-resistance. Good adhesion of the chrome plate to the steel surface, which is essential for long term durability of the part, is extremely dependent on surface preparation prior to plating. Recently, McDonnell Douglas developed a new pre-treatment method for chrome plating in which the steel is anodically etched in a sulfuric acid and hydrofluoric acid solution. On carbon steel surfaces, this anodic pre-treatment produces a dark, loosely adhering material that is commonly called the “smut” layer. On stainless steels and nickel alloys, the surface is only darkened by the anodic pre-treatment and little residue is produced. Anodic pre-treatment prior to hard chrome plating results in much better adherence to both carbon and alloy steels.We have characterized the anodic pre-treated steel surface and the resulting “smut” layer using various techniques including electron spectroscopy for chemical analysis (ESCA) on bulk samples and transmission electron microscopy (TEM) and electron energy-loss spectroscopy (EELS) on stripped films.

2020 ◽  
Vol 57 (12) ◽  
pp. 1832-1843 ◽  
Author(s):  
Yongfeng Deng ◽  
Jun Wu ◽  
Yunzhi Tan ◽  
Yujun Cui ◽  
Chao-sheng Tang ◽  
...  

Municipal mud consists of organic matter naturally deposited in a microbial-rich environment, and its common pre-treatment in the laboratory is normally different from that in situ. In this study, an improved pre-loading method and the common pre-treatment method (by air or oven drying) were first applied to investigate the effect of microorganisms within organic matter on performance of the solidified soils. Results reveal that (i) Atterberg limits in the pre-loading method were higher than those in the drying method; (ii) the time-dependent strength became stable for the solidified soils pre-treated by the drying method, while strength decreased for the soils pre-treated by the pre-loading method; (iii) pH value of solidified soils by the pre-loading method decreased more significantly. After excluding the possible porosity influence on solidified soils, the effects of microorganisms within organic matter were investigated by microbial identification tests, including fluorescence detection and high-throughput sequencing. The pre-treatment procedure changed the vitality and diversity of microorganisms, leading to a rebalance between acid erosion and cement hydration during long-term curing. At the end, the long-term strength of the solidified municipal mud by the traditional pre-treatment method (by air or oven drying) could be overevaluated.


Author(s):  
S. L. Ngoh ◽  
S. C. Tan ◽  
C. S. Goh ◽  
J. Wei

Adhesive bonding offers many advantages, such as light weight, ease of manufacturing, corrosion resistance and more uniform stress distribution at joint. In order to achieve good initial adhesion and durability of adhesive bonded aluminum joint, pre-treatment of the aluminum substrate is essential. Some of the surface pre-treatment procedures commonly used are chromium-based chemical and electro-chemical methods. However, due to the environmental and health concerns, and legislation to ban the use of hexavalent chromium, there is a need to omit the use of chromium-based pre-treatment methods in the surface preparation process. Therefore, this work aims to study the effect of the developed hybrid chromium-free surface pre-treatment method on the bonding strength of adhesive bonded aluminum joint. The study on the effects of solution concentration level and processing time of the hybrid treatment on the bonding strength suggests that bonding strength can be improved through enhancement of mechanical interlocking and increase of bonding area between the adhesive and adherend. Even though comparable or rougher surface morphologies were obtained from hybrid treatments as compared to the chromium-based treatment, lower bonding strengths were observed. This further suggests that the nano-scale level interaction between the adhesive and adherend has vital effect on the bonding performance.


Author(s):  
Dennis Maher ◽  
David Joy ◽  
Peggy Mochel

A variety of standard specimens is needed in order to systematically investigate the instrumentation, specimen, data reduction and quantitation variables in electron energy-loss spectroscopy (EELS). Pure single element specimens (e.g. various forms of carbon) have received considerable attention to date but certain elements of interest cannot be prepared directly as thin films. Since studies of the first and second row elements in two- or multicomponent systems will be of considerable importance in microanalysis using EELS, there is a need for convenient standards containing these species. For many investigations a standard should contain the desired element, or elements, homogeneously dispersed through a suitable matrix and at an accurately known concentration. These conditions may be met by the technique of implantation.Silicon was chosen as the host lattice since its principal ionization energies, EL23 = 98 eV and Ek = 1843 eV, are well removed from the K-edges of most elements of major interest such as boron (Ek = 188 eV), carbon (Ek = 283 eV), nitrogen (Ek = 400 eV) and oxygen (Ek = 532 eV).


Author(s):  
R. W. Ditchfield ◽  
A. G. Cullis

An energy analyzing transmission electron microscope of the Möllenstedt type was used to measure the electron energy loss spectra given by various layer structures to a spatial resolution of 100Å. The technique is an important, method of microanalysis and has been used to identify secondary phases in alloys and impurity particles incorporated into epitaxial Si films.Layers Formed by the Epitaxial Growth of Ge on Si Substrates Following studies of the epitaxial growth of Ge on (111) Si substrates by vacuum evaporation, it was important to investigate the possible mixing of these two elements in the grown layers. These layers consisted of separate growth centres which were often triangular and oriented in the same sense, as shown in Fig. 1.


Author(s):  
E.G. Bithell ◽  
W.M. Stobbs

It is well known that the microstructural consequences of the ion implantation of semiconductor heterostructures can be severe: amorphisation of the damaged region is possible, and layer intermixing can result both from the original damage process and from the enhancement of the diffusion coefficients for the constituents of the original composition profile. A very large number of variables are involved (the atomic mass of the target, the mass and energy of the implant species, the flux and the total dose, the substrate temperature etc.) so that experimental data are needed despite the existence of relatively well developed models for the implantation process. A major difficulty is that conventional techniques (e.g. electron energy loss spectroscopy) have inadequate resolution for the quantification of any changes in the composition profile of fine scale multilayers. However we have demonstrated that the measurement of 002 dark field intensities in transmission electron microscope images of GaAs / AlxGa1_xAs heterostructures can allow the measurement of the local Al / Ga ratio.


Author(s):  
John F. Mansfield

One of the most important advancements of the transmission electron microscopy (TEM) in recent years has been the development of the analytical electron microscope (AEM). The microanalytical capabilities of AEMs are based on the three major techniques that have been refined in the last decade or so, namely, Convergent Beam Electron Diffraction (CBED), X-ray Energy Dispersive Spectroscopy (XEDS) and Electron Energy Loss Spectroscopy (EELS). Each of these techniques can yield information on the specimen under study that is not obtainable by any other means. However, it is when they are used in concert that they are most powerful. The application of CBED in materials science is not restricted to microanalysis. However, this is the area where it is most frequently employed. It is used specifically to the identification of the lattice-type, point and space group of phases present within a sample. The addition of chemical/elemental information from XEDS or EELS spectra to the diffraction data usually allows unique identification of a phase.


Author(s):  
J P Cassella ◽  
V Salih ◽  
T R Graham

Left ventricular assist systems are being developed for eventual long term or permanent implantation as an alternative to heart transplantation in patients unsuitable for or denied the transplant option. Evaluation of the effects of these devices upon normal physiology is required. A preliminary study was conducted to evaluate the morphology of aortic tissue from calves implanted with a pneumatic Left Ventricular Assist device-LVAD. Two 3 month old heifer calves (calf 1 and calf 2) were electively explanted after 128 days and 47 days respectively. Descending thoracic aortic tissue from both animals was removed immediately post mortem and placed into karnovsky’s fixative. The tissue was subsequently processed for transmission electron microscopy (TEM). Some aortic tissue was fixed in neutral buffered formalin and processed for routine light microscopy.


Author(s):  
John B. Vander Sande ◽  
Thomas F. Kelly ◽  
Douglas Imeson

In the scanning transmission electron microscope (STEM) a fine probe of electrons is scanned across the thin specimen, or the probe is stationarily placed on a volume of interest, and various products of the electron-specimen interaction are then collected and used for image formation or microanalysis. The microanalysis modes usually employed in STEM include, but are not restricted to, energy dispersive X-ray analysis, electron energy loss spectroscopy, and microdiffraction.


2014 ◽  
Vol 24 (2) ◽  
pp. 48-58 ◽  
Author(s):  
Lakshmi Kollara ◽  
Graham Schenck ◽  
Jamie Perry

Studies have investigated the applications of Continuous Positive Airway Pressure (CPAP) therapy in the treatment of hypernasality due to velopharyngeal dysfunction (VPD; Cahill et al., 2004; Kuehn, 1991; Kuehn, Moon, & Folkins, 1993; Kuehn et al., 2002). The purpose of this study was to examine the effectiveness of CPAP therapy to reduce hypernasality in a female subject, post-traumatic brain injury (TBI) and pharyngeal flap, who presented with signs of VPD including persistent hypernasality. Improvements in mean velopharyngeal orifice size, subjective perception of hypernasality, and overall intelligibility were observed from the baseline to 8-week post-treatment assessment intervals. Additional long-term assessments completed at 2, 3, and 4 months post-treatment indicated decreases in immediate post-treatment improvements. Results from the present study suggest that CPAP is a safe, non-invasive, and relatively conservative treatment method for reduction of hypernasality in selected patients with TBI. More stringent long-term follow up may indicate the need for repeated CPAP treatment to maintain results.


2020 ◽  
Vol 82 (5) ◽  
pp. 11-20
Author(s):  
D.R. Abdulina ◽  
◽  
L.M. Purish ◽  
G.O. Iutynska ◽  
◽  
...  

The studies of the carbohydrate composition of the sulfate-reducing bacteria (SRB) biofilms formed on the steel surface, which are a factor of microbial corrosion, are significant. Since exopolymers synthesized by bacteria could activate corrosive processes. The aim of the study was to investigate the specificity of commercial lectins, labeled with colloidal gold to carbohydrates in the biofilm exopolymeric matrix produced by the corrosive-relevant SRB strains from man-caused ecotopes. Methods. Microbiological methods (obtaining of the SRB biofilms during cultivation in liquid Postgate B media under microaerophilic conditions), biochemical methods (lectin-binding analysis of 10 commercial lectins, labeled with colloidal gold), transmission electron microscopy using JEM-1400 JEOL. Results. It was shown using transmission electron microscopy that the binding of lectins with carbohydrates in the biofilm of the studied SRB strains occurred directly in the exopolymerіс matrix, as well as on the surfaces of bacterial cells, as seen by the presence of colloidal gold particles. For detection of the neutral carbohydrates (D-glucose and D-mannose) in the biofilm of almost all studied bacterial strains PSA lectin was the most specific. This lectin binding in biofilms of Desulfotomaculum sp. К1/3 and Desulfovibrio sp. 10 strains was higher in 90.8% and 94.4%, respectively, then for ConA lectin. The presence of fucose in the SRB biofilms was detected using LABA lectin, that showed specificity to the biofilm EPS of all the studied strains. LBA lectin was the most specific to N-аcetyl-D-galactosamine for determination of amino sugars in the biofilm. The amount of this lectin binding in D. vulgaris DSM644 biofilm was 30.3, 10.1 and 9.3 times higher than SBA, SNA and PNA lectins, respectively. STA, LVA and WGA lectins were used to detect the N-acetyl-Dglucosamine and sialic acid in the biofilm. WGA lectin showed specificity to N-acetyl-D-glucosamine in the biofilm of all the studied SRB; maximum number of bounded colloidal gold particles (175 particles/μm2) was found in the Desulfotomaculum sp. TC3 biofilm. STA lectin was interacted most actively with N-acetyl-D-glucosamine in Desulfotomaculum sp. TC3 and Desulfomicrobium sp. TC4 biofilms. The number of bounded colloidal gold particles was in 9.2 and 7.4 times higher, respectively, than using LVA lectin. The lowest binding of colloidal gold particles was observed for LVA lectin. Conclusions. It was identified the individual specificity of the 10 commercial lectins to the carbohydrates of biofilm matrix on the steel surface, produced by SRB. It was estimated that lectins with identical carbohydrates specificity had variation in binding to the biofilm carbohydrates of different SRB strains. Establishing of the lectin range selected for each culture lead to the reduction of the scope of studies and labor time in the researching of the peculiarities of exopolymeric matrix composition of biofilms formed by corrosiverelevant SRB.


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