On radiation damage in FIB-prepared softwood samples measured by scanning X-ray diffraction

2015 ◽  
Vol 22 (2) ◽  
pp. 267-272 ◽  
Author(s):  
Selina Storm ◽  
Malte Ogurreck ◽  
Daniel Laipple ◽  
Christina Krywka ◽  
Manfred Burghammer ◽  
...  
Keyword(s):  
Cell Wall ◽  
Radiation Damage ◽  
Focused Ion Beam ◽  
Complex Geometry ◽  
Ion Beam ◽  
Wall Structure ◽  
X Ray Diffraction ◽  
X Ray ◽  
First Time ◽  
Interesting System

The high flux density encountered in scanning X-ray nanodiffraction experiments can lead to severe radiation damage to biological samples. However, this technique is a suitable tool for investigating samples to high spatial resolution. The layered cell wall structure of softwood tracheids is an interesting system which has been extensively studied using this method. The tracheid cell has a complex geometry, which requires the sample to be prepared by cutting it perpendicularly to the cell wall axis. Focused ion beam (FIB) milling in combination with scanning electron microscopy allows precise alignment and cutting without splintering. Here, results of a scanning X-ray diffraction experiment performed on a biological sample prepared with a focused ion beam of gallium atoms are reported for the first time. It is shown that samples prepared and measured in this way suffer from the incorporation of gallium atoms up to a surprisingly large depth of 1 µm.

Oxidation of Alloy-X in Subcritical, Transition, and Supercritical Water

CORROSION ◽  
10.5006/3881 ◽  
2021 ◽  
Author(s):  
Zachary Karmiol ◽  
Dev Chidambaram
Keyword(s):  
Supercritical Water ◽  
Photoelectron Spectroscopy ◽  
Focused Ion Beam ◽  
Elevated Temperatures ◽  
Subcritical Water ◽  
Ion Beam ◽  
X Ray Diffraction ◽  
X Ray ◽  
Nickel Based Superalloy ◽  
Before And After

This work investigates the oxidation of a nickel based superalloy, namely Alloy X, in water at elevated temperatures: subcritical water at 261°C and 27 MPa, the transition between subcritical and supercritical water at 374°C and 27 MPa, and supercritical water at 380°C and 27 MPa for 100 hours. The morphology of the sample surfaces were studied using scanning electron microscopy coupled with focused ion beam milling, and the surface chemistry was investigated using X-ray diffraction, Raman spectroscopy, energy dispersive X-ray spectroscopy, and X-ray photoelectron spectroscopy before and after exposure studies. Surfaces of all samples were identified to comprise of a ferrite spinel containing aluminum.

Fine structure in the red algae - II. The structure of the cell wall of Rhodymenia Palmata

1959 ◽  
Vol 150 (941) ◽  
pp. 447-455 ◽  
Keyword(s):  
Cell Wall ◽  
Chemical Treatment ◽  
Amorphous Matrix ◽  
Dry Weight ◽  
Wall Structure ◽  
X Ray Diffraction ◽  
X Ray ◽  
Floridean Starch ◽  
Thin Sectioning ◽  
Paper Chromatographic Separation

The cell-wall structure of the red alga Rhodymenia palmata has been examined by the methods of X -ray diffraction analysis and electron microscopy, including ultra-thin sectioning. The cell wall is shown to consist of numerous lamellae each of which is made up of unoriented, crystalline microfibrils embedded in an amorphous matrix of other cell-wall constituents. The material can be stretched reversibly up to 100% when wet, and the stretching induces orientation of the microfibrils. The ‘∝ cellulose' fraction, which accounts for only 2 to 7 % of the original dry weight, was isolated chemically and was analyzed by means of hydrolysis and paper chromatographic separation of the resulting sugars, and it was found to be composed of approximately equal quantities of glucose and xylose residues. Chemical treatment of the cell wall was found to cause considerable variations in the X -ray diagrams, which are discussed. It is concluded that the microfibrils contain both glucose and xylose residues in approximately equal proportions and that chemical treatment in this case causes changes in crystallinity of the structural component of the wall. The importance of these findings for the meaning of the term cellulose is discussed. The X -ray diagram of older fronds was found to be complicated by the occurrence of extra rings due to the presence of floridean starch, and the highly elastic properties of the thallus enabled the diagrams of the starch and the cell wall to be separated.

Fine structure in the red algae III. A general survey of cell-wall structure in the red algae

1959 ◽  
Vol 150 (941) ◽  
pp. 456-459 ◽  
Keyword(s):  
Cell Wall ◽  
Red Algae ◽  
Amorphous Matrix ◽  
Cell Wall Structure ◽  
Wall Structure ◽  
X Ray Diffraction ◽  
Cellulose I ◽  
General Survey ◽  
X Ray ◽  
Floridean Starch

A general survey of cell-wall structure in the red algae has been carried out using the methods of X -ray diffraction analysis and electron microscopy. The fifteen species all show a similar wall structure consisting of numerous lamellae each of which is made up of random micro-fibrils embedded in an amorphous matrix. The X -ray diagrams obtained from several species are complicated by the existence of crystalline floridean starch, but nevertheless reveal the absence of cellulose I.

scholarly journals Annealing of focused ion beam damage in gold microcrystals: an in situ Bragg coherent X-ray diffraction imaging study

2021 ◽  
Vol 28 (2) ◽  
pp. 550-565 ◽  
Author(s):  
David Yang ◽  
Nicholas W. Phillips ◽  
Kay Song ◽  
Ross J. Harder ◽  
Wonsuk Cha ◽  
...  
Keyword(s):  
Focused Ion Beam ◽  
Ion Beam ◽  
Imaging Study ◽  
X Ray Diffraction ◽  
Multiple Reflections ◽  
X Ray ◽  
Self Diffusion ◽  
Diffraction Imaging ◽  
Gold Microcrystals

Focused ion beam (FIB) techniques are commonly used to machine, analyse and image materials at the micro- and nanoscale. However, FIB modifies the integrity of the sample by creating defects that cause lattice distortions. Methods have been developed to reduce FIB-induced strain; however, these protocols need to be evaluated for their effectiveness. Here, non-destructive Bragg coherent X-ray diffraction imaging is used to study the in situ annealing of FIB-milled gold microcrystals. Two non-collinear reflections are simultaneously measured for two different crystals during a single annealing cycle, demonstrating the ability to reliably track the location of multiple Bragg peaks during thermal annealing. The thermal lattice expansion of each crystal is used to calculate the local temperature. This is compared with thermocouple readings, which are shown to be substantially affected by thermal resistance. To evaluate the annealing process, each reflection is analysed by considering facet area evolution, cross-correlation maps of the displacement field and binarized morphology, and average strain plots. The crystal's strain and morphology evolve with increasing temperature, which is likely to be caused by the diffusion of gallium in gold below ∼280°C and the self-diffusion of gold above ∼280°C. The majority of FIB-induced strains are removed by 380–410°C, depending on which reflection is being considered. These observations highlight the importance of measuring multiple reflections to unambiguously interpret material behaviour.

scholarly journals Initial Interaction of Crystalline Al/Amorphous Si Bilayer during Annealing

2004 ◽  
Vol 808 ◽  
Author(s):  
Yonghao Zhao ◽  
Jiangyong Wang ◽  
Eric J. Mittemeijer
Keyword(s):  
Auger Electron ◽  
Focused Ion Beam ◽  
Imaging Techniques ◽  
Ion Beam ◽  
X Ray Diffraction ◽  
X Ray ◽  
Initial Interaction ◽  
Magnetron Sputter ◽  
Amorphous Si ◽  
Sputter Deposited

ABSTRACTInitial interaction of a magnetron sputter deposited Al(100 nm, {111} fibre textured)/Si(150 nm, amorphous) bilayer, induced by isothermally annealing at 523 K for 60 min in a vacuum of 2.0×10−4 Pa, was studied by X-ray diffraction, Auger electron microscopy and focused-ion beam imaging techniques. Upon annealing, the crystalline Si had grown into the grain boundaries of the Al layer with a {111} texture, a crystallite size of approximate 12 nm and a tensile stress of +138 MPa. Simultaneously, the Al grains had grown into the Si layer from the original interface of the a-Si and Al sublayers with the lateral grain growth. The stress parallel to the surface of the Al layer had changed from +27 MPa to +232 MPa after annealing.

Effect of Current Density on Anodised Titanium in Mixture of β-Glycerophosphate (β-GP) and Calcium Acetate (CA)

2015 ◽  
Vol 1087 ◽  
pp. 212-217 ◽  
Author(s):  
Hasan Zuhudi Abdullah ◽  
Te Chuan Lee ◽  
Maizlinda Izwana Idris ◽  
Charles Christopher Sorrell
Keyword(s):  
Current Density ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Ceramic Coatings ◽  
Disodium Salt ◽  
Calcium Acetate ◽  
X Ray Diffraction ◽  
X Ray ◽  
Ceramic Films ◽  
Glancing Angle

Anodic oxidation is an electrochemical method for the production of ceramic films on a metallic substrate. It had been widely used to deposit the ceramic coatings on the metals surface. In this study, the surface morphology and crystallinity of titanium foil was modified by anodising in mixture of β-glycerophosphate disodium salt pentahydrate (β-GP) and calcium acetate monohydrate (CA). The experiments were carried out at high voltage (350 V), different anodising time (1, 3, 5 and 10 min) and current density (10 and 20 mA.cm-2) at room temperature. Anodised titanium was characterised by using glancing angle X-ray diffraction (GAXRD), field emission scanning electron microscope (FESEM) and focused ion beam (FIB) milling. The result of the experiment show that colour, porosity, crystallinity and thickness of the titanium films depended strongly on the current density. More porous surface and large amount of anatase was produced at higher current density. FIB results indicated that the thickness of oxide layer increased as increasing of current density.

scholarly journals The Use of Focused Ion Beam (FIB) Technology for Cell Wall Structure Elucidation

2013 ◽  
Vol 19 (S2) ◽  
pp. 882-883
Author(s):  
M. Blumentritt ◽  
S.D. Collins ◽  
S.M. Shaler
Keyword(s):  
Cell Wall ◽  
Structure Elucidation ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Cell Wall Structure ◽  
Wall Structure

Extended abstract of a paper presented at Microscopy and Microanalysis 2013 in Indianapolis, Indiana, USA, August 4 – August 8, 2013.

scholarly journals Micro-beam Laue alignment of multi-reflection Bragg coherent diffraction imaging measurements

2017 ◽  
Vol 24 (5) ◽  
pp. 1048-1055 ◽  
Author(s):  
Felix Hofmann ◽  
Nicholas W. Phillips ◽  
Ross J. Harder ◽  
Wenjun Liu ◽  
Jesse N. Clark ◽  
...  
Keyword(s):  
Focused Ion Beam ◽  
Lattice Strain ◽  
Ion Beam ◽  
Strain Tensor ◽  
Three Dimensional ◽  
Stress Fields ◽  
X Ray Diffraction ◽  
X Ray ◽  
Coherent Diffraction Imaging ◽  
Diffraction Imaging

Multi-reflection Bragg coherent diffraction imaging has the potential to allow three-dimensional (3D) resolved measurements of the full lattice strain tensor in specific micro-crystals. Until now such measurements were hampered by the need for laborious, time-intensive alignment procedures. Here a different approach is demonstrated, using micro-beam Laue X-ray diffraction to first determine the lattice orientation of the micro-crystal. This information is then used to rapidly align coherent diffraction measurements of three or more reflections from the crystal. Based on these, 3D strain and stress fields in the crystal are successfully determined. This approach is demonstrated on a focused ion beam milled micro-crystal from which six reflections could be measured. Since information from more than three independent reflections is available, the reliability of the phases retrieved from the coherent diffraction data can be assessed. Our results show that rapid, reliable 3D coherent diffraction measurements of the full lattice strain tensor in specific micro-crystals are now feasible and can be successfully carried out even in heavily distorted samples.

Stress evaluation in thin films: Micro-focus synchrotron X-ray diffraction combined with focused ion beam patterning for do evaluation

2013 ◽  
Vol 549 ◽  
pp. 245-250 ◽  
Author(s):  
Nikolaos Baimpas ◽  
Eric Le Bourhis ◽  
Sophie Eve ◽  
Dominique Thiaudière ◽  
Christopher Hardie ◽  
...  
Keyword(s):  
Thin Films ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
X Ray Diffraction ◽  
Stress Evaluation ◽  
X Ray ◽  
Ion Beam Patterning
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