Combination of high spatial resolution and low minimum detection limit using thinned specimens in cutting-edge electron probe microanalysis

2015 ◽  
Vol 157 ◽  
pp. 48-56 ◽  
Author(s):  
Yugo Kubo ◽  
Kotaro Hamada
2018 ◽  
Vol 103 (9) ◽  
pp. 1473-1486 ◽  
Author(s):  
Ery C. Hughes ◽  
Ben Buse ◽  
Stuart L. Kearns ◽  
Jon D. Blundy ◽  
Geoff Kilgour ◽  
...  

2021 ◽  
Vol 26 (3) ◽  
pp. 51
Author(s):  
Tamme Claus ◽  
Jonas Bünger ◽  
Manuel Torrilhon

The spatial resolution of electron probe microanalysis (EPMA), a non-destructive method to determine the chemical composition of materials, is currently restricted to a pixel size larger than the volume of interaction between beam electrons and the material, as a result of limitations on the underlying k-ratio model. Using more sophisticated models to predict k-ratios while solving the inverse problem of reconstruction offers a possibility to increase the spatial resolution. Here, a k-ratio model based on the deterministic M1-model in Boltzmann Continuous Slowing-Down approximation (BCSD) will be utilized to present a reconstruction method for EPMA which is implemented as a PDE-constrained optimization problem. Iterative gradient-based optimization techniques are used in combination with the adjoint state method to calculate the gradient in order to solve the optimization problem efficiently. The accuracy of the spatial resolution still depends on the number and quality of the measured data, but in contrast to conventional reconstruction methods, an overlapping of the interaction volumes of different measurements is permissible without ambiguous solutions. The combination of k-ratios measured with various electron beam configurations is necessary for a high resolution. Attempts to reconstruct materials with synthetic data show challenges that occur with small reconstruction pixels, but also indicate the potential to improve the spatial resolution in EPMA using the presented method.


Author(s):  
Claude Lechene

Electron probe microanalysis of frozen hydrated kidneysThe goal of the method is to measure on the same preparation the chemical elemental content of the renal luminal tubular fluid and of the surrounding renal tubular cells. The following method has been developed. Rat kidneys are quenched in solid nitrogen. They are trimmed under liquid nitrogen and mounted in a copper holder using a conductive medium. Under liquid nitrogen, a flat surface is exposed by sawing with a diamond saw blade at constant speed and constant pressure using a custom-built cryosaw. Transfer into the electron probe column (Cameca, MBX) is made using a simple transfer device maintaining the sample under liquid nitrogen in an interlock chamber mounted on the electron probe column. After the liquid nitrogen is evaporated by creating a vacuum, the sample is pushed into the special stage of the instrument. The sample is maintained at close to liquid nitrogen temperature by circulation of liquid nitrogen in the special stage.


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