Degradation Analysis of Thin Mg-xAg Wires Using X-ray Near-Field Holotomography

Magnesium–silver alloys are of high interest for the use as temporary bone implants due to their antibacterial properties in addition to biocompatibility and biodegradability. Thin wires in particular can be used for scaffolding, but the determination of their degradation rate and homogeneity using traditional methods is difficult. Therefore, we have employed 3D imaging using X-ray near-field holotomography with sub-micrometer resolution to study the degradation of thin (250 μm diameter) Mg-2Ag and Mg-6Ag wires. The wires were studied in two states, recrystallized and solution annealed to assess the influence of Ag content and precipitates on the degradation. Imaging was employed after degradation in Dulbecco’s modified Eagle’s medium and 10% fetal bovine serum after 1 to 7 days. At 3 days of immersion the degradation rates of both alloys in both states were similar, but at 7 days higher silver content and solution annealing lead to decreased degradation rates. The opposite was observed for the pitting factor. Overall, the standard deviation of the determined parameters was high, owing to the relatively small field of view during imaging and high degradation inhomogeneity of the samples. Nevertheless, Mg-6Ag in the solution annealed state emerges as a potential material for thin wire manufacturing for implants.

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Degradation Analysis of Thin Mg-xAg Wires Using X-Ray Near-Field Holotomography

10.20944/preprints202107.0566.v2 ◽

2021 ◽

Author(s):

Sebastian Meyer ◽

Andreas Wolf ◽

Daniela Sanders ◽

Kamila Iskhakova ◽

Hanna Ćwieka ◽

...

Keyword(s):

3D Imaging ◽

Near Field ◽

Antibacterial Properties ◽

X Ray ◽

Thin Wires ◽

Degradation Rates ◽

Degradation Analysis ◽

Fetal Bovine ◽

Small Field Of View

Magnesium-silver alloys are of high interest for the use as temporary bone implants due to their antibacterial properties in addition to biocompatibility and biodegradability. Thin wires in particular can be used for scaffolding, but the determination of their degradation rate and homogeneity using traditional methods is difficult. Therefore, we have employed 3D imaging using X-ray near-field holotomography with sub-micrometer resolution to study the degradation of thin (250 μm diameter) Mg-2Ag and Mg-6Ag wires. The wires were studied in two states, recrystallized and solution annealed to assess the influence of Ag content and precipitates on the degradation. Imaging was employed after degradation in Dulbecco’s modified Eagle’s medium and 10% fetal bovine serum after 1 to 7 days. At 3 days of immersion the degradation rates of both alloys in both states were similar, but at 7 days higher silver content and solution annealing lead to decreased degradation rates. The opposite was observed for the pitting factor. Overall, the standard deviation of the determined parameters was high, owing to the relatively small field of view during imaging and high degradation inhomogeneity of the samples. Nevertheless, Mg-6Ag in the solution annealed state emerges as a potential material for thin wire manufacturing for implants.

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Lateral resolution of the electron microbeam analysis

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100109859 ◽

1978 ◽

Vol 36 (1) ◽

pp. 542-543

Author(s):

H.J. Dudek

Keyword(s):

Quantitative Analysis ◽

Depth Resolution ◽

Lateral Resolution ◽

Cylindrical Particle ◽

Correction Procedure ◽

X Ray ◽

Element Concentrations ◽

Microbeam Analysis ◽

The Matrix

The chemical inhomogenities in modern materials such as fibers, phases and inclusions, often have diameters in the region of one micrometer. Using electron microbeam analysis for the determination of the element concentrations one has to know the smallest possible diameter of such regions for a given accuracy of the quantitative analysis.In th is paper the correction procedure for the quantitative electron microbeam analysis is extended to a spacial problem to determine the smallest possible measurements of a cylindrical particle P of high D (depth resolution) and diameter L (lateral resolution) embeded in a matrix M and which has to be analysed quantitative with the accuracy q. The mathematical accounts lead to the following form of the characteristic x-ray intens ity of the element i of a particle P embeded in the matrix M in relation to the intensity of a standard S

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Sem and X-Ray Analysis of Renal and Biliary Calculi

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100091512 ◽

1976 ◽

Vol 34 ◽

pp. 306-307

Author(s):

R. J. Narconis ◽

G. L. Johnson

Keyword(s):

Chemical Constituents ◽

Natural State ◽

X Ray Diffraction ◽

Chemical Methods ◽

X Ray ◽

Additional Dimension ◽

Biliary Calculi ◽

Calculus Formation ◽

Scanning Electron

Analysis of the constituents of renal and biliary calculi may be of help in the management of patients with calculous disease. Several methods of analysis are available for identifying these constituents. Most common are chemical methods, optical crystallography, x-ray diffraction, and infrared spectroscopy. The application of a SEM with x-ray analysis capabilities should be considered as an additional alternative.A scanning electron microscope equipped with an x-ray “mapping” attachment offers an additional dimension in its ability to locate elemental constituents geographically, and thus, provide a clue in determination of possible metabolic etiology in calculus formation. The ability of this method to give an undisturbed view of adjacent layers of elements in their natural state is of advantage in determining the sequence of formation of subsequent layers of chemical constituents.

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Preparation And elemental analysis of ancient fibers

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100126846 ◽

1987 ◽

Vol 45 ◽

pp. 410-411

Author(s):

Allen Angel ◽

Kathryn A. Jakes

Keyword(s):

Cross Sections ◽

Physical Structure ◽

Energy Dispersive ◽

Archaeological Sites ◽

X Ray ◽

Long Term Storage ◽

Backscattered Electron ◽

Electron Imaging

Fabrics recovered from archaeological sites often are so badly degraded that fiber identification based on physical morphology is difficult. Although diagenetic changes may be viewed as destructive to factors necessary for the discernment of fiber information, changes occurring during any stage of a fiber's lifetime leave a record within the fiber's chemical and physical structure. These alterations may offer valuable clues to understanding the conditions of the fiber's growth, fiber preparation and fabric processing technology and conditions of burial or long term storage (1).Energy dispersive spectrometry has been reported to be suitable for determination of mordant treatment on historic fibers (2,3) and has been used to characterize metal wrapping of combination yarns (4,5). In this study, a technique is developed which provides fractured cross sections of fibers for x-ray analysis and elemental mapping. In addition, backscattered electron imaging (BSI) and energy dispersive x-ray microanalysis (EDS) are utilized to correlate elements to their distribution in fibers.

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Determination of Stoichiometry of GaAs Component in (Gaas)Ge Epitaxially Grown Thin Films by Electron Microprobe X-Ray Analysis

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100134922 ◽

1990 ◽

Vol 48 (2) ◽

pp. 264-265

Author(s):

D. R. Liu ◽

S. S. Shinozaki ◽

R. J. Baird

Keyword(s):

Thin Film ◽

Thin Films ◽

Monte Carlo Simulation ◽

Monte Carlo ◽

Compound Semiconductors ◽

Energy Dispersive Analysis ◽

X Ray ◽

Metastable Alloys ◽

Lower Voltage

The epitaxially grown (GaAs)Ge thin film has been arousing much interest because it is one of metastable alloys of III-V compound semiconductors with germanium and a possible candidate in optoelectronic applications. It is important to be able to accurately determine the composition of the film, particularly whether or not the GaAs component is in stoichiometry, but x-ray energy dispersive analysis (EDS) cannot meet this need. The thickness of the film is usually about 0.5-1.5 μm. If Kα peaks are used for quantification, the accelerating voltage must be more than 10 kV in order for these peaks to be excited. Under this voltage, the generation depth of x-ray photons approaches 1 μm, as evidenced by a Monte Carlo simulation and actual x-ray intensity measurement as discussed below. If a lower voltage is used to reduce the generation depth, their L peaks have to be used. But these L peaks actually are merged as one big hump simply because the atomic numbers of these three elements are relatively small and close together, and the EDS energy resolution is limited.

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Polarity Determination in Sphalerite and Wurtzite Structures

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100136106 ◽

1990 ◽

Vol 48 (2) ◽

pp. 500-501

Author(s):

Stuart McKernan ◽

C. Barry Carter

Keyword(s):

Opposite Polarity ◽

Single Domain ◽

Polar Material ◽

Electron Microscopic ◽

Dynamical Interaction ◽

X Ray ◽

Polarity Determination ◽

The Absolute ◽

Microscopic Techniques

The determination of the absolute polarity of a polar material is often crucial to the understanding of the defects which occur in such materials. Several methods exist by which this determination may be performed. In bulk, single-domain specimens, macroscopic techniques may be used, such as the different etching behavior, using the appropriate etchant, of surfaces with opposite polarity. X-ray measurements under conditions where Friedel’s law (which means that the intensity of reflections from planes of opposite polarity are indistinguishable) breaks down can also be used to determine the absolute polarity of bulk, single-domain specimens. On the microscopic scale, and particularly where antiphase boundaries (APBs), which separate regions of opposite polarity exist, electron microscopic techniques must be employed. Two techniques are commonly practised; the first [1], involves the dynamical interaction of hoLz lines which interfere constructively or destructively with the zero order reflection, depending on the crystal polarity. The crystal polarity can therefore be directly deduced from the relative intensity of these interactions.

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Problems in Thin-Film X-ray Quantification

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100135897 ◽

1990 ◽

Vol 48 (2) ◽

pp. 458-459

Author(s):

J N Chapman ◽

W A P Nicholson

Keyword(s):

Thin Film ◽

Specimen Thickness ◽

X Rays ◽

Characteristic Peak ◽

Local Composition ◽

X Ray ◽

Measured Ratio ◽

Path Lengths ◽

Composition Changes

Energy dispersive x-ray microanalysis (EDX) is widely used for the quantitative determination of local composition in thin film specimens. Extraction of quantitative data is usually accomplished by relating the ratio of the number of atoms of two species A and B in the volume excited by the electron beam (nA/nB) to the corresponding ratio of detected characteristic photons (NA/NB) through the use of a k-factor. This leads to an expression of the form nA/nB = kAB NA/NB where kAB is a measure of the relative efficiency with which x-rays are generated and detected from the two species.Errors in thin film x-ray quantification can arise from uncertainties in both NA/NB and kAB. In addition to the inevitable statistical errors, particularly severe problems arise in accurately determining the former if (i) mass loss occurs during spectrum acquisition so that the composition changes as irradiation proceeds, (ii) the characteristic peak from one of the minority components of interest is overlapped by the much larger peak from a majority component, (iii) the measured ratio varies significantly with specimen thickness as a result of electron channeling, or (iv) varying absorption corrections are required due to photons generated at different points having to traverse different path lengths through specimens of irregular and unknown topography on their way to the detector.

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Reduction of Potassium in Kidney Proximal Tubules to Aid in Electron Probe X-Ray Microanalysis of Calcium

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100119193 ◽

1985 ◽

Vol 43 ◽

pp. 474-475

Author(s):

A. LeFurgey ◽

P. Ingram ◽

L.J. Mandel

Keyword(s):

Smooth Muscle ◽

Proximal Tubule ◽

Electron Probe ◽

Clinical Applications ◽

Proximal Tubules ◽

Rabbit Kidney ◽

Target Cells ◽

X Ray ◽

Freeze Dried

For quantitative determination of subcellular Ca distribution by electron probe x-ray microanalysis, decreasing (and/or eliminating) the K content of the cell maximizes the ability to accurately separate the overlapping K Kß and Ca Kα peaks in the x-ray spectra. For example, rubidium has been effectively substituted for potassium in smooth muscle cells, thus giving an improvement in calcium measurements. Ouabain, a cardiac glycoside widely used in experimental and clinical applications, inhibits Na-K ATPase at the cell membrane and thus alters the cytoplasmic ion (Na,K) content of target cells. In epithelial cells primarily involved in active transport, such as the proximal tubule of the rabbit kidney, ouabain rapidly (t1/2= 2 mins) causes a decrease2 in intracellular K, but does not change intracellular total or free Ca for up to 30 mins. In the present study we have taken advantage of this effect of ouabain to determine the mitochondrial and cytoplasmic Ca content in freeze-dried cryosections of kidney proximal tubule by electron probe x-ray microanalysis.

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