LabAdviser/314/Preparation 314-307/Solid-matter/FIB-lamella: Difference between revisions
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'''FIB lamella preparation''' | '''Feedback to this page''': '''[mailto:labadviser@nanolab.dtu.dk?Subject=Feed%20back%20from%20page%20http://labadviser.nanolab.dtu.dk/index.php/LabAdviser/314/Preparation_314-307/Solid-matter/FIB-lamella click here]''' | ||
(''content by Anton Bay Andersen @DTU Nanolab, March 2020'') | |||
[[Category:314]] | |||
[[Category:314-Preparation]] | |||
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=FIB lamella preparation= | =FIB lamella preparation= | ||
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SEM sample) and attach it to a grid suitable for TEM imaging. The desired sample outcome is a lamella thin enough to be suited for TEM/STEM/EELS/EDX measurements (<100nm is desirable). Throughout this document it is assumed that the operator is an experienced SEM user, always works at eucentric height (the crossover of the ion and electron beam) and has an understanding of the chamber geometry. Furthermore, all settings are material and sample dependent. As a rule of thumb, the harder a material is the more difficult it is to mill with the ion beam. As an example, 20nA is on the low end for milling larger sections of corundum efficiently but 2.8nA is almost too aggressive for gold. | SEM sample) and attach it to a grid suitable for TEM imaging. The desired sample outcome is a lamella thin enough to be suited for TEM/STEM/EELS/EDX measurements (<100nm is desirable). Throughout this document it is assumed that the operator is an experienced SEM user, always works at eucentric height (the crossover of the ion and electron beam) and has an understanding of the chamber geometry. Furthermore, all settings are material and sample dependent. As a rule of thumb, the harder a material is the more difficult it is to mill with the ion beam. As an example, 20nA is on the low end for milling larger sections of corundum efficiently but 2.8nA is almost too aggressive for gold. | ||
== 1,2: Protective Pt deposition == | == Step: 1,2: Protective Pt deposition == | ||
[[File:fig1.PNG|600px]] | [[File:fig1.PNG|600px]] | ||
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Fig 2: Sketch of subsequent platinum deposition. | Fig 2: Sketch of subsequent platinum deposition. | ||
[[File:fig31.png| | [[File:fig31.png|400px]] | ||
[[File:fig32.png| | [[File:fig32.png|400px]] | ||
Fig 3: SE images acquired before and after electron beam deposited platinum. | Fig 3: SE images acquired before and after electron beam deposited platinum. | ||
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== | == Step 3,4: Initial rough cut and rough cleaning == | ||
[[File:fig4.PNG| | [[File:fig4.PNG|500px]] | ||
Fig 4: Sketch of the desired rough cut and rough cleaning. | Fig 4: Sketch of the desired rough cut and rough cleaning. | ||
[[File:fig5_1.png| | [[File:fig5_1.png|400px]][[File:fig5_2.png|400px]] | ||
Fig 5: SE images acquired with the ion beam before and after the rough cut. | Fig 5: SE images acquired with the ion beam before and after the rough cut. | ||
[[File:fig6.png| | [[File:fig6.png|400px]] | ||
Fig 6: SE images acquired with the ion beam after the rough cleaning. | Fig 6: SE images acquired with the ion beam after the rough cleaning. | ||
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==Step 5: Undercut == | ==Step 5: Undercut == | ||
[[File:fig7.PNG| | [[File:fig7.PNG|500px]] | ||
Fig 7: Illustration of step 5-7. | Fig 7: Illustration of step 5-7. | ||
[[File:fig8. | [[File:fig8.png|400px]] | ||
Fig 8: After undercut from both sides. | Fig 8: After undercut from both sides. | ||
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[[File:fig9. | [[File:fig9.png|400px]] | ||
Fig 9: Attachment of the omni probe to a lamellae prior to cutting the lamellae free. | Fig 9: Attachment of the omni probe to a lamellae prior to cutting the lamellae free. | ||
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==Step 7: Attachment TEM grid== | ==Step 7: Attachment TEM grid== | ||
[[File:fig10.PNG| | [[File:fig10.PNG|400px]] | ||
Fig 10: Attachment of the omniprobe to the omniprobe grid. | Fig 10: Attachment of the omniprobe to the omniprobe grid. | ||
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==Step 8: Final thinning with Ga beam== | ==Step 8: Final thinning with Ga beam== | ||
[[File:fig11_1.png| | [[File:fig11_1.png|400px]][[File:fig11_2.png|400px]] | ||
Fig 11: Viewing directions during thinning. Left ion beam, right electron beam. | Fig 11: Viewing directions during thinning. Left ion beam, right electron beam. | ||
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Note: Milling like described above makes a wedge shaped sample. This increases mechanical stability while still making an extremely thin sample at the surface. If a flat sample is desired you can compensate by tilting the sample. The amount of tilt depends on material, acceleration voltage and current, so a bit of experimenting is required. | Note: Milling like described above makes a wedge shaped sample. This increases mechanical stability while still making an extremely thin sample at the surface. If a flat sample is desired you can compensate by tilting the sample. The amount of tilt depends on material, acceleration voltage and current, so a bit of experimenting is required. | ||