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Microscopia de Iones y Nano-Tecnología

Microscopia de Iones y Nano-Tecnología. Eduardo H. Montoya Rossi. The Focused Ion Beam (FIB) Instrument. The FIB column. How the FIB works. How the FIB works. What is it possible with FIB?. Micromachining. What is it possible with FIB?. FIB tomography. Material deposition.

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Microscopia de Iones y Nano-Tecnología

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  1. Microscopia de Iones y Nano-Tecnología Eduardo H. Montoya Rossi

  2. The Focused Ion Beam (FIB) Instrument.

  3. The FIB column.

  4. How the FIB works.

  5. How the FIB works.

  6. What is it possible with FIB? • Micromachining.

  7. What is it possible with FIB? • FIB tomography.

  8. Material deposition. • What is it possible with FIB?

  9. TEM sample preparation. • What is it possible with FIB?

  10. Sample preparation is a critical step in Transmission Electron Microscopy (TEM) studies.

  11. Conventional techniques have been used for long time.

  12. New, state of the art, transmission electron microscopes require ultra high quality samples, “free from any surface damage and with negligible surface roughness”(Genç et al. Microscopy & Microanalysis, 13:1520-1521, 2007).

  13. Constant thickness is required for quantitative transmission electron microscopy (TEM) methods.

  14. Bulk sample surface FIB preparation of a TEM specimen: • A thick lamella is machined by focused ion beam milling. • Then extracted (lift out) by a needle.

  15. BF - TEM FIB preparation of a TEM specimen: • The specimen is welded to a TEM grid and released from the needle. • Then thinned by low current and low energy FIB milling. • The result is a (high quality?) TEM lamella.

  16. Finished at 10 keV Finished at 5 keV HRTEM HRTEM HAADF-STEM Finished at 5 keV FIB – TEM on mono-crystalline Ge • Difficult case • Top: S. Rubanov & P.R. Munroe. Micron, 35:549 – 556 (2004) • Bottom: present work.

  17. STO LAO Ion milling – HRTEM on LAO / STO multilayer • S. Bals, unpublished

  18. STO LAO LAO / STO multilayer: HRTEM • FIB

  19. Double cross sectional study: Examining the cross section of the cross section. Why is it important? • Provides direct measurement of the thickness of a FIB prepared TEM specimen. • Provides information about the thickness, origin, structure and composition of the damaged / amorphous layers induced by the FIB preparation process.

  20. 1 2 Grid horizontally mounted 2 1 • Cover both sides of the specimen with sputtered Au. • Embed the Au-covered specimen in a Pt brick. • Cut slices from the Pt brick. Double cross section technique 1,2: observation directions

  21. Proposed procedure is clean, easy, fast and reliable

  22. HAADF-STEM Double cross sectional study: LAO / STO • Specimen thickness is fairly constant inside the Region of Interest (ROI). • Bottle like shape of the cross section.

  23. FIB Au Au Double cross sectional study: LAO / STO • ROI: HAADF-STEM image (A) and EFTEM maps of Ti, La and Ga (B, C). • Spreading of La (B) and enrichment of Ga (C) in amorphous layers. • Boxes indicate regions selected for intensity scan plots (next slide). EFTEM HAADF-STEM EFTEM

  24. Double cross sectional study: LAO / STO Intensity scan plots across (A) and along the multilayer (B). • Question marks (A): La and Ti signals not detected by HAADF-STEM. • These signals correspond to redeposited amorphous material. • Peaks of La at borders of original specimen cross-section (B).

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