Application Example 7: Sample Surface Preparation by Ultramicrotomy Using a Diamond Knife for Cross-Sectional Examination of Various Coatings on Metals

2009 ◽  
pp. 23-24
Author(s):  
Kenichi Shimizu ◽  
Tomoaki Mitani
Keyword(s):  
Surface Preparation ◽  
Sample Surface ◽  
Cross Sectional ◽  
Diamond Knife

A technique to prepare cross-sectional TEM specimens of semiconducting devices

1986 ◽  
Vol 44 ◽  
pp. 742-743
Author(s):  
A. K. Rai ◽  
P. P. Pronko
Keyword(s):  
Thin Films ◽  
Surface Region ◽  
Sample Surface ◽  
Specific Region ◽  
Cross Sectional ◽  
Thin Sections ◽  
The Past ◽  
Device Structures ◽  
Ion Implanted

Several techniques have been reported in the past to prepare cross(x)-sectional TEM specimen. These methods are applicable when the sample surface is uniform. Examples of samples having uniform surfaces are ion implanted samples, thin films deposited on substrates and epilayers grown on substrates. Once device structures are fabricated on the surfaces of appropriate materials these surfaces will no longer remain uniform. For samples with uniform surfaces it does not matter which part of the surface region remains in the thin sections of the x-sectional TEM specimen since it is similar everywhere. However, in order to study a specific region of a device employing x-sectional TEM, one has to make sure that the desired region is thinned. In the present work a simple way to obtain thin sections of desired device region is described.

Comparison of Ion-Milling Techniques For Cross-Sectional TEM of Semiconductors

1985 ◽  
Vol 43 ◽  
pp. 166-167
Author(s):  
Julia T. Luck ◽  
C. W. Boggs ◽  
S. J. Pennycook
Keyword(s):  
Analytical Techniques ◽  
Sample Surface ◽  
Ion Milling ◽  
Cross Sectional ◽  
Reliable Technique ◽  
Near Surface ◽  
Transmission Electron ◽  
Thin Region ◽  
Transient Thermal

The use of cross-sectional Transmission Electron Microscopy (TEM) has become invaluable for the characterization of the near-surface regions of semiconductors following ion-implantation and/or transient thermal processing. A fast and reliable technique is required which produces a large thin region while preserving the original sample surface. New analytical techniques, particularly the direct imaging of dopant distributions, also require good thickness uniformity. Two methods of ion milling are commonly used, and are compared below. The older method involves milling with a single gun from each side in turn, whereas a newer method uses two guns to mill from both sides simultaneously.

An Infrared Interferometer for Elastoplastic Crack-Tip Field Investigation of Homogeneous and Bimaterial Beams: A Study of Three-Dimensional Effects and J-Dominance

1998 ◽  
Vol 65 (4) ◽  
pp. 1032-1041
Author(s):  
J. K. Sinha ◽  
H. V. Tippur
Keyword(s):  
Plane Deformation ◽  
Three Dimensional ◽  
Surface Preparation ◽  
Field Measurements ◽  
Sample Surface ◽  
Field Investigation ◽  
Crack Tip Field ◽  
Full Field ◽  
Infrared Wavelength ◽  
Dimensional Effects

An infrared interferometer capable of performing real-time full-field noncontacting deformation field measurements on optically rough surfaces is proposed as a tool for elastoplastic fracture mechanics investigations. The choice of the infrared wavelength allows interferometric measurements on fracture samples with little or no surface preparation and is more tolerant of the damage accumulation near the crack. The interferometer also bridges a sensitivity gap among existing techniques for out-of-plane deformation measurement. First, a rigorous Fourier optics analysis is provided for the interferometer and the range of surface roughness that can be studied using this interferometer is examined. The interferometer is then used for mapping deformations near elastoplastically deformed cracks in aluminum beams and solder-copper bimaterials. The regions of dominant three-dimensional effects and J-dominance are examined on the sample surface by evaluating measurements along with companion finite element analyses and the HRR fields.

scholarly journals Cross-sectional TEM Sample Preparation for Nanowires or Porous Films Grown on a Substrate

2007 ◽  
Vol 15 (1) ◽  
pp. 44-45
Author(s):  
Chengyu Song
Keyword(s):  
Low Temperature ◽  
Sample Preparation ◽  
Traditional Method ◽  
Sample Surface ◽  
Specimen Preparation ◽  
Air Bubbles ◽  
Ion Milling ◽  
Porous Films ◽  
Cross Sectional ◽  
Single Section

Nanowires or porous films grown on a substrate normally lack mechanical strength, and may be subject to damage during specimen preparation. When we made cross-sectional TEM specimen for this type of sample, we modified the traditional method by covering the sample with epoxy to improve the film strength, and applying single-section ion milling to protect the film from over-milling.The sample surface is first covered with G1 epoxy. We choose G1 for this application because it is relatively thick and cures at low temperature. For samples with a dense-growth of nanowires or a thick porous film, a brief moment in vacuum helps to get rid of the air bubbles in the epoxy. The glue is cured at 100 degree C for 10 minutes, until its color turns to a reddish brown. To remove the excess glue and flatten the surface, the sample is then ground and polished until the glue is less than 0.1 mm thick.

scholarly journals Improved Sectioning of Polymers Using an Oscillating Diamond Knife for Transmission Electron Microscopy

2006 ◽  
Vol 14 (5) ◽  
pp. 20-21 ◽  
Author(s):  
J.D. Harris ◽  
J.S. Vastenhout
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Wedge Angle ◽  
Cutting Speed ◽  
Sample Surface ◽  
Section Thickness ◽  
Thin Sections ◽  
Transmission Electron ◽  
Surface Section ◽  
Diamond Knife

Polymers are viscoelastic materials that can often deform during microtome sectioning. Similar to plastic embedded biological materials, many methods have been developed over the years to not only improve the image contrast of these materials but also to harden the material for improved sectioning during microtomy. Even with these improvements, a common artifact, compression, during the sectioning of this class of materials remains problematic.Compression is caused by several factors: hardness of the sample, embedding media, wedge angle of the knife, interaction between the diamond and sample surface, section thickness and cutting speed. It has been found that reducing the knife angle from 45º to 35° leads to a reduction in compression. Recent efforts to further reduce the compression of ultra-thin sections have led to the invention of an oscillating diamond knife.

Epitaxial cerium oxide buffer layers and YBa2Cu3O7−δ thin films for microwave device applications

1999 ◽  
Vol 14 (6) ◽  
pp. 2385-2393 ◽  
Author(s):  
Sissel N. Jacobsen ◽  
Lynnette D. Madsen ◽  
Ulf Helmersson
Keyword(s):  
Thin Films ◽  
Surface Morphology ◽  
Rf Magnetron Sputtering ◽  
Sample Surface ◽  
Columnar Structure ◽  
Buffer Layers ◽  
Ex Situ ◽  
Epitaxial Relationship ◽  
Cross Sectional ◽  
Appreciable Change

CeO2 films with thicknesses ranging from 8.8 to 199 nm were grown on Al2O3 (1102) (R-cut) substrates by off-axis rf magnetron sputtering. X-ray diffraction showed an epitaxial relationship with the CeO2 (001) planes parallel to the Al2O3 (1102) planes for all film thicknesses. Atomic force microscopy (AFM) revealed a rough surface morphology consisting of crystallites with lateral dimensions of 10–90 nm. In the thinnest film, these crystallites were regularly shaped and uniformly distributed on the substrate, while they were rectangularly shaped and oriented mainly in two directions, orthogonal to each other, in the thicker films. The surface roughness of the films increased with increasing layer thickness. Characterization of the microstructure was done by cross-sectional transmission electron microscopy (XTEM) and showed a polycrystalline, highly oriented, columnar structure with a top layer terminated by (111)-facets. High-quality YBa2Cu3O7−δ (YBCO) thin films were deposited directly onto the CeO2 layers. XTEM, rather surprisingly, showed a smooth interface between the YBCO and CeO2 layer. Postdeposition ex situ annealing was carried out on two CeO2 films and evaluated by AFM. Upon annealing samples at 930 °C, a relatively smooth morphology without facets was obtained. Annealing films at 800 °C caused no appreciable change in surface morphology, whereas igniting a YBCO plasma during a similar anneal clearly altered the sample surface, giving facets that were rounded.

scholarly journals Rock Sample Surface Preparation Influences Thermal Infrared Spectra

2018 ◽  
Author(s):  
Evelien Rost ◽  
Christoph Hecker ◽  
Martin C. Schodlok ◽  
Freek D. van der Meer
Keyword(s):  
Surface Roughness ◽  
Rock Sample ◽  
Surface Preparation ◽  
Thermal Infrared ◽  
Sample Surface ◽  
Spectral Shape ◽  
Spectral Signature ◽  
Rock Surface ◽  
Spectral Signatures ◽  
Spectral Contrast

High-resolution laboratory-based thermal infrared spectroscopy is an up-and-coming tool in the field of geological remote sensing. Its spatial resolution allows for detailed analyses at centimeter to sub-millimeter scale. However, this increase in resolution creates challenges with sample characteristics such as grain size, surface roughness and porosity that can influence the spectral signature. This research explores the effect of rock sample surface preparation on the TIR spectral signatures. We applied three surface preparation methods (split, saw and polish) to determine how the resulting differences in surface roughness affects both the spectral shape as well as the spectral contrast. The selected samples are a pure quartz sandstone, a quartz sandstone containing a small percentage of kaolinite, and an intermediate-grained gabbro. To avoid instrument or measurement type biases we conducted measurements on three TIR instruments, resulting in directional hemispherical reflectance spectra, emissivity spectra and bi-directional reflectance images. Surface imaging and analyses were performed with scanning electron microscopy and profilometer measurements. We demonstrate that surface preparation affects the TIR spectral signatures influencing both the spectral contrast as well as the spectral shape. The results show that polished surfaces predominantly display a high spectral contrast while the sawed and split surfaces display up to 25% lower reflectance values. Furthermore, the sawed and split surfaces display spectral signature shape differences at specific wavelengths, which we link to mineral transmission features, surface orientation effects and multiple reflections in fine-grained minerals. Hence, the influence of rock surface preparation should be taken in consideration to avoid an inaccurate geological interpretation.

Comparison of the effect of the feldspathic sample surface preparation method on the strength of the bond with orthodontic aesthetic brackets

2018 ◽  
Vol 14 (3) ◽  
pp. 167-177
Author(s):  
Olga Włodarczyk-Górniak ◽  
Agata Szczesio ◽  
Joanna Nowak ◽  
Leszek Klimek ◽  
Joanna Szczepańska ◽  
...  
Keyword(s):  
Bonding Strength ◽  
Preparation Method ◽  
Testing Machine ◽  
Surface Preparation ◽  
Sample Surface ◽  
Shear Resistance ◽  
Resistance Test ◽  
Cohesive Fracture ◽  
Orthodontic Bracket ◽  
Roughness Profile

As the amount of orthodontically treated adults is steadily increasing, the need arose of adhesive cementation of brackets for crowns and other ceramic restorations. The surface of dentist porcelain does not undergo etching with phosphoric acid (H3PO4) and requires a different procedure protocol. <b>Aim.</b> The aim of the research was to evaluate the strength of the polycrystalline bracket bonds with feldspathic ceramics processed using some selected methods. <b>Material and methods.</b> Feldspathic ceramic samples fired onto a metal cylinder were divided into five groups and processed with the selected methods. The surface was subjected to scanning electron microscope (SEM) imaging and roughness profile examination. Next, after cementing the polycrystalline brackets and after conducting a thermocycling process (24h, 1450 cycles), a technical shear resistance test was performed in a strength testing machine. The resulting adhesive-cohesive fracture was evaluated as well as the ARI (Adhesive Remnant Index). The findings were subjected to statistical analysis. <b>Results.</b> All the samples tested demonstrated that the orthodontic bracket bonding strength with ceramics examined using the shear resistance test amounted to more than 7 MPa, with such bonding strength being considered sufficient to conduct orthodontic treatment. The highest mean strength was obtained and the most frequent adhesive-cohesive fracture with damage to the ceramics was observed in group HF (12,85 MPa). The preparation applied in group MEP (10,03 MPa) had the lowest influence on the ceramics structure. This was observed in the roughness profile test and in the SEM test. The surface structure of the samples in the MEP group did not significantly differ from that in the K group. <b>Conclusions.</b> The tests demonstrated that the alternative procedure methods applied during the feldspathic ceramics surface preparation for adhesive cementing comply with the requirements set by the contemporary orthodontics. <b>(Włodarczyk-Górniak O, Szczesio A, Nowak J, Klimek L, Szczepańska J, Pawłowska E. Comparison of the effect of the feldspathic sample surface preparation method on the strength of the bond with orthodontic aesthetic brackets. Orthod Forum 2018; 14: 167-77).</b>

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