scholarly journals Surface Topography of PVD Hard Coatings

Coatings ◽  
2021 ◽  
Vol 11 (11) ◽  
pp. 1387
Author(s):  
Peter Panjan ◽  
Aljaž Drnovšek ◽  
Nastja Mahne ◽  
Miha Čekada ◽  
Matjaž Panjan

The primary objective of this study was to investigate and compare the surface topography of hard coatings deposited by three different physical vapor deposition methods (PVD): low-voltage electron beam evaporation, unbalanced magnetron sputtering and cathodic arc evaporation. In these deposition systems, various ion etching techniques were applied for substrate cleaning. The paper summarizes our experience and the expertise gained during many years of development of PVD hard coatings for the protection of tools and machine components. Surface topography was investigated using scanning electron microscopy (SEM), atomic force microscopy (AFM), scanning transmission electron microscopy (STEM) and 3D stylus profilometry. Observed similarities and differences among samples deposited by various deposition methods are discussed and correlated with substrate material selection, substrate pretreatment and deposition conditions. Large variations in the surface topography were observed between selected deposition techniques, both after ion etching and deposition processes. The main features and implications of surface cleaning by ion etching are discussed and the physical phenomena involved in this process are reviewed. During a given deposition run as well as from one run to another, a large spatial variation of etching rates was observed due to the difference in substrate geometry and batching configurations. Variations related to the specific substrate rotation (i.e., temporal variations in the etching and deposition) were also observed. The etching efficiency can be explained by the influence of different process parameters, such as substrate-to-source orientation and distance, shadowing and electric field effects. The surface roughness of PVD coatings mainly originates from growth defects (droplets, nodular defects, pinholes, craters, etc.). We briefly describe the causes of their formation.

Author(s):  
Marek Malecki ◽  
J. Victor Small ◽  
James Pawley

The relative roles of adhesion and locomotion in malignancy have yet to be clearly established. In a tumor, subpopulations of cells may be recognized according to their capacity to invade neighbouring tissue,or to enter the blood stream and metastasize. The mechanisms of adhesion and locomotion are themselves tightly linked to the cytoskeletal apparatus and cell surface topology, including expression of integrin receptors. In our studies on melanomas with Fluorescent Microscopy (FM) and Cell Sorter(FACS), we noticed that cells in cultures derived from metastases had more numerous actin bundles, then cells from primary foci. Following this track, we attempted to develop technology allowing to compare ultrastructure of these cells using correlative Transmission Electron Microscopy(TEM) and Low Voltage Scanning Electron Microscopy(LVSEM).


Author(s):  
Marek Malecki ◽  
James Pawley ◽  
Hans Ris

The ultrastructure of cells suspended in physiological fluids or cell culture media can only be studied if the living processes are stopped while the cells remain in suspension. Attachment of living cells to carrier surfaces to facilitate further processing for electron microscopy produces a rapid reorganization of cell structure eradicating most traces of the structures present when the cells were in suspension. The structure of cells in suspension can be immobilized by either chemical fixation or, much faster, by rapid freezing (cryo-immobilization). The fixation speed is particularly important in studies of cell surface reorganization over time. High pressure freezing provides conditions where specimens up to 500μm thick can be frozen in milliseconds without ice crystal damage. This volume is sufficient for cells to remain in suspension until frozen. However, special procedures are needed to assure that the unattached cells are not lost during subsequent processing for LVSEM or HVEM using freeze-substitution or freeze drying. We recently developed such a procedure.


Author(s):  
Peter K. Mueller ◽  
Glenn R. Smith ◽  
Leslie M Carpenter ◽  
Ronald L. Stanley

At the present time the primary objective of the electron microscopy group of the Air and Industrial Hygiene Laboratory is the development of a method suitable for use in establishing an air quality standard for asbestos in ambient air and for use in its surveillance. The main concept and thrust of our approach for the development of this method is to obtain a true picture of fiber occurrence as a function of particle size and asbestos type utilizing light and electron microscopy.We have now available an electron micrographic atlas of all asbestos types including selected area diffraction patterns and examples of fibers isolated from air samples. Several alternative approaches for measuring asbestos in ambient air have been developed and/or evaluated. Our experiences in this regard will be described. The most promising method involves: 1) taking air samples on cellulose ester membrane filters with a nominal pore size of 0.8 micron; 2) ashing in a low temperature oxygen plasma for several hours;


Author(s):  
S. J. Krause ◽  
W.W. Adams ◽  
S. Kumar ◽  
T. Reilly ◽  
T. Suziki

Scanning electron microscopy (SEM) of polymers at routine operating voltages of 15 to 25 keV can lead to beam damage and sample image distortion due to charging. Imaging polymer samples with low accelerating voltages (0.1 to 2.0 keV), at or near the “crossover point”, can reduce beam damage, eliminate charging, and improve contrast of surface detail. However, at low voltage, beam brightness is reduced and image resolution is degraded due to chromatic aberration. A new generation of instruments has improved brightness at low voltages, but a typical SEM with a tungsten hairpin filament will have a resolution limit of about 100nm at 1keV. Recently, a new field emission gun (FEG) SEM, the Hitachi S900, was introduced with a reported resolution of 0.8nm at 30keV and 5nm at 1keV. In this research we are reporting the results of imaging coated and uncoated polymer samples at accelerating voltages between 1keV and 30keV in a tungsten hairpin SEM and in the Hitachi S900 FEG SEM.


Author(s):  
E. Dupré ◽  
G. Schatten

Sperm of decapod crustaceans are formed by a round or cup-shaped body, a complex acrosome and one a few appendages emerging from the main body. Although this sperm does not have motility, it has some components of the cytoskeleton like microtubules, which are found inside the appendages. Actin filaments have been found in the spike of penaeidae sperms. The actual participation of the crustacean decapod sperm cytoskeleton during fertilization is not well understood. Actin is supposed to play an active role in drawing the penaeidae shrimp sperm closer to the egg after bending of the spike. The present study was aimed at the localization of actin filaments in sperm of the Robinson Crusoe island lobster, Jasus frontalis and in the crayfish Orconectes propincus, by fluorescent probes and low voltage scanning electron microscopy.


Author(s):  
Quintin J. Lai ◽  
Stuart L. Cooper ◽  
Ralph M. Albrecht

Thrombus formation and embolization are significant problems for blood-contacting biomedical devices. Two major components of thrombi are blood platelets and the plasma protein, fibrinogen. Previous studies have examined interactions of platelets with polymer surfaces, fibrinogen with platelets, and platelets in suspension with spreading platelets attached to surfaces. Correlative microscopic techniques permit light microscopic observations of labeled living platelets, under static or flow conditions, followed by the observation of identical platelets by electron microscopy. Videoenhanced, differential interference contrast (DIC) light microscopy permits high-resolution, real-time imaging of live platelets and their interactions with surfaces. Interference reflection microscopy (IRM) provides information on the focal adhesion of platelets on surfaces. High voltage, transmission electron microscopy (HVEM) allows observation of platelet cytoskeletal structure of whole mount preparations. Low-voltage, high resolution, scanning electron microscopy allows observation of fine surface detail of platelets. Colloidal gold-labeled fibrinogen, used to identify the Gp Ilb/IIIa membrane receptor for fibrinogen, can be detected in all the above microscopies.


Author(s):  
Arthur V. Jones

In comparison with the developers of other forms of instrumentation, scanning electron microscope manufacturers are among the most conservative of people. New concepts usually must wait many years before being exploited commercially. The field emission gun, developed by Albert Crewe and his coworkers in 1968 is only now becoming widely available in commercial instruments, while the innovative lens designs of Mulvey are still waiting to be commercially exploited. The associated electronics is still in general based on operating procedures which have changed little since the original microscopes of Oatley and his co-workers.The current interest in low-voltage scanning electron microscopy will, if sub-nanometer resolution is to be obtained in a useable instrument, lead to fundamental changes in the design of the electron optics. Perhaps this is an opportune time to consider other fundamental changes in scanning electron microscopy instrumentation.


Author(s):  
W.W. Adams ◽  
G. Price ◽  
A. Krause

It has been shown that there are numerous advantages in imaging both coated and uncoated polymers in scanning electron microscopy (SEM) at low voltages (LV) from 0.5 to 2.0 keV compared to imaging at conventional voltages of 10 to 20 keV. The disadvantages of LVSEM of degraded resolution and decreased beam current have been overcome with the new generation of field emission gun SEMs. In imaging metal coated polymers in LVSEM beam damage is reduced, contrast is improved, and charging from irregularly shaped features (which may be unevenly coated) is reduced or eliminated. Imaging uncoated polymers in LVSEM allows direct observation of the surface with little or no charging and with no alterations of surface features from the metal coating process required for higher voltage imaging. This is particularly important for high resolution (HR) studies of polymers where it is desired to image features 1 to 10 nm in size. Metal sputter coating techniques produce a 10 - 20 nm film that has its own texture which can obscure topographical features of the original polymer surface. In examining thin, uncoated insulating samples on a conducting substrate at low voltages the effect of sample-beam interactions on image formation and resolution will differ significantly from the effect at higher accelerating voltages. We discuss here sample-beam interactions in single crystals on conducting substrates at low voltages and also present the first results on HRSEM of single crystal morphologies which show some of these effects.


Author(s):  
William Krakow ◽  
Alec N. Broers

Low-loss scanning electron microscopy can be used to investigate the surface topography of solid specimens and provides enhanced image contrast over secondary electron images. A high resolution-condenser objective lens has allowed the low-loss technique to resolve separations of Au nucleii of 50Å and smaller dimensions of 25Å in samples coated with a fine grained carbon-Au-palladium layer. An estimate of the surface topography of fine grained vapor deposited materials (20 - 100Å) and the surface topography of underlying single crystal Si in the 1000 - 2000Å range has also been investigated. Surface imaging has also been performed on single crystals using diffracted electrons scattered through 10−2 rad in a conventional TEM. However, severe tilting of the specimen is required which degrades the resolution 15 to 100 fold due to image forshortening.


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