Transmission Kikuchi diffraction

Transmission Kikuchi diffraction (TKD or t-EBSD{{Cite journal |last1=van Bremen |first1=R. |last2=Ribas Gomes |first2=D. |last3=de Jeer |first3=L.T.H. |last4=Ocelík |first4=V. |last5=De Hosson |first5=J.Th.M. |date=2016 |title=On the optimum resolution of transmission-electron backscattered diffraction (t-EBSD) |url=https://research.rug.nl/en/publications/7729a4b9-d8a6-49d9-b74c-312e4de6e7c9 |url-status=live |journal=Ultramicroscopy |volume=160 |pages=256–264 |doi=10.1016/j.ultramic.2015.10.025 |pmid=26579885 |archive-url=https://web.archive.org/web/20230325200603/https://research.rug.nl/en/publications/on-the-optimum-resolution-of-transmission-electron-backscattered- |archive-date=25 March 2023 |access-date=20 March 2023}}) is an Electron backscatter diffraction (EBSD) technique that is used to analyse the crystallographic orientation and microstructure of materials at a high spatial resolution.{{Cite journal |last1=Keller |first1=R.R. |last2=Geiss |first2=R.H. |date=2012 |title=Transmission EBSD from 10 nm domains in a scanning electron microscope: Transmission EBSD in the SEM |journal=Journal of Microscopy |volume=245 |issue=3 |pages=245–251 |doi=10.1111/j.1365-2818.2011.03566.x |s2cid=39521418}} It is a variation of convergent-beam electron diffraction, which has been introduced around the 1970s, and has since become increasingly popular in materials science research, especially for studying materials at the nanoscale.{{Cite journal |last1=Sneddon |first1=Glenn C. |last2=Trimby |first2=Patrick W. |last3=Cairney |first3=Julie M. |date=2016 |title=Transmission Kikuchi diffraction in a scanning electron microscope: A review |journal=Materials Science and Engineering: R: Reports |volume=110 |pages=1–12 |doi=10.1016/j.mser.2016.10.001}}

In TKD, a thin foil sample is prepared and placed perpendicular to the electron beam of a scanning electron microscope. The electron beam is then focused on a small spot on the sample, and the crystal lattice of the sample diffracts the transmitted electrons. The diffraction pattern is then collected by a detector and analysed to determine the crystallographic orientation and microstructure of the sample.{{Cite journal |last1=Niessen |first1=F. |last2=Burrows |first2=A. |last3=Fanta |first3=A. Bastos da Silva |date=2018 |title=A systematic comparison of on-axis and off-axis transmission Kikuchi diffraction |url=https://backend.orbit.dtu.dk/ws/files/142186738/PostPrint_A_systematic_comparison.pdf |journal=Ultramicroscopy |volume=186 |pages=158–170 |doi=10.1016/j.ultramic.2017.12.017 |pmid=29335225}}

One of the key advantages of TKD is its high spatial resolution that can reach a few nanometres. This is achieved by using a small electron beam spot size, typically less than 10 nanometres in diameter, and by collecting the transmitted electrons with a small-angle annular dark-field detector (STEM-ADF) in a scanning transmission electron microscope (STEM). Another advantage of TKD is its high sensitivity to local variations in crystallographic orientation. This is because the transmitted electrons in TKD are diffracted at very small angles, which makes the diffraction pattern highly sensitive to local variations in the crystal lattice.

TKD can also be used to study nano-sized materials, such as nanoparticles and thin films.{{Cite journal |last=Trimby |first=Patrick W. |date=2012 |title=Orientation mapping of nanostructured materials using transmission Kikuchi diffraction in the scanning electron microscope |journal=Ultramicroscopy |volume=120 |pages=16–24 |doi=10.1016/j.ultramic.2012.06.004 |pmid=22796555}} Thin foil samples can be prepared for TKD using a Focused ion beam (FIB) or ion milling machine. However, such machines are expensive and their operation requires particular skills and training. Additionally, the diffraction patterns obtained from TKD can be more complex to interpret than those obtained from conventional EBSD techniques due to the complex geometry of the diffracted electrons.{{Cite journal |last1=Liu |first1=Junliang |last2=Lozano-Perez |first2=Sergio |last3=Wilkinson |first3=Angus J. |last4=Grovenor |first4=Chris R. M. |date=2019 |title=On the depth resolution of transmission Kikuchi diffraction (TKD) analysis 9300920 |journal=Ultramicroscopy |volume=205 |pages=5–12 |arxiv=1904.04140 |doi=10.1016/j.ultramic.2019.06.003 |pmid=31234103 |s2cid=102350683}}

File:TKD map.png image collect using the diodes in on-axis TKD setup (up) and a TKD map collected around the crack in the ferrite phase of an age hardened duplex stainless steel collected at 30 kV. The map step size is 5 nm.{{Cite journal |last=Koko |first=Abdalrhaman |last2=Marrow |first2=T. James |date=2024-10-01 |title=Transmission-scanning electron microscopy of interface fracture of ferrite deformation twins |url=https://link.springer.com/article/10.1557/s43579-024-00595-8 |journal=MRS Communications |language=en |volume=14 |issue=5 |pages=964–969 |doi=10.1557/s43579-024-00595-8 |issn=2159-6867|doi-access=free }}]]

On-axis and off-axis TKD methods differ in the sample's orientation with respect to the electron beam. In on-axis TKD, the sample is oriented so that the incident electron beam is nearly perpendicular to the sample surface. This results in a diffraction pattern that is nearly centred around the transmitted beam direction.{{Cite journal |last1=Brosusch |first1=N. |last2=Demers |first2=H. |last3=Gauvin |first3=R. |date=2013 |title=Nanometres-resolution Kikuchi patterns from materials science specimens with transmission electron forward scatter diffraction in the scanning electron microscope |journal=Journal of Microscopy |volume=250 |issue=1 |pages=1–14 |doi=10.1111/jmi.12007 |pmid=23346885 |s2cid=20435127}} On-axis TKD is typically used for analysing samples with low lattice strain and high crystallographic symmetry, such as single crystals or large grains.

In off-axis TKD, the sample is tilted with respect to the incident electron beam, typically at an angle of several degrees. This results in a diffraction pattern that is shifted away from the transmitted beam direction. Off-axis TKD is typically used for analysing samples with high lattice strain and/or low crystallographic symmetry, such as nano-crystalline materials or materials with defects. Off-axis TKD is often preferred for materials science research because it provides more information about the crystallographic orientation and microstructure of the sample, especially in samples with a high density of defects{{Cite journal |last1=Liang |first1=X. Z. |last2=Dodge |first2=M. F. |last3=Jiang |first3=J. |last4=Dong |first4=H. B. |date=2019 |title=Using transmission Kikuchi diffraction in a scanning electron microscope to quantify geometrically necessary dislocation density at the nanoscale |journal=Ultramicroscopy |volume=197 |pages=39–45 |doi=10.1016/j.ultramic.2018.11.011 |pmid=30496887 |s2cid=205526130}} or a high degree of lattice strain.{{Cite journal |last1=Meisnar |first1=Martina |last2=Vilalta-Clemente |first2=Arantxa |last3=Gholinia |first3=Ali |last4=Moody |first4=Michael |last5=Wilkinson |first5=Angus J. |last6=Huin |first6=Nicolas |last7=Lozano-Perez |first7=Sergio |date=2015 |title=Using transmission Kikuchi diffraction to study intergranular stress corrosion cracking in type 316 stainless steels 5000700 |journal=Micron |volume=75 |pages=1–10 |doi=10.1016/j.micron.2015.04.011 |pmid=25974882}}{{Cite journal |last1=Yu |first1=Hongbing |last2=Liu |first2=Junliang |last3=Karamched |first3=Phani |last4=Wilkinson |first4=Angus J. |last5=Hofmann |first5=Felix |date=2019 |title=Mapping the full lattice strain tensor of a single dislocation by high angular resolution transmission Kikuchi diffraction (HR-TKD) |journal=Scripta Materialia |volume=164 |pages=36–41 |doi=10.1016/j.scriptamat.2018.12.039 |s2cid=119075799|doi-access=free |arxiv=1808.10055 }} However, on-axis TKD can still be useful for studying samples with high crystallographic symmetry or for verifying the crystallographic orientation of a sample before performing off-axis TKD. The on-axis technique can speed up acquisition by more than 20 times, and a low scattering angle setup also gives rise to higher quality patterns.{{Cite journal |last1=Yuan |first1=H. |last2=Brodu |first2=E. |last3=Chen |first3=C. |last4=Bouzy |first4=E. |last5=Fundenberger |first5=J-J. |last6=Toth |first6=L.S. |date=2017 |title=On-axis versus off-axis Transmission Kikuchi Diffraction technique: application to the characterisation of severe plastic deformation-induced ultrafine-grained microstructures |journal=Journal of Microscopy |volume=267 |issue=1 |pages=70–80 |doi=10.1111/jmi.12548 |pmid=28328010 |s2cid=7988685}}

EBSD resolution is influenced by multiple factors including the beam size, electron accelerating voltage, the material's atomic mass and the specimen's thickness. Out of these variables, sample thickness has the greatest effect on the pattern quality and resolution of the image. An increase in the sample thickness broadens the beam, thus reducing the lateral spatial resolution.{{Cite journal |last1=Rice |first1=K.P. |last2=Keller |first2=R.R. |last3=Stoykovich |first3=M.P. |date=2014 |title=Specimen-thickness effects on transmission Kikuchi patterns in the scanning electron microscope |journal=Journal of Microscopy |volume=254 |issue=3 |pages=129–136 |doi=10.1111/jmi.12124 |pmid=24660836 |s2cid=25006562}}

• {{Cite journal |last=Sneddon |first=Glenn C. |last2=Trimby |first2=Patrick W. |last3=Cairney |first3=Julie M. |date=2016-12-01 |title=Transmission Kikuchi diffraction in a scanning electron microscope: A review |url=https://www.sciencedirect.com/science/article/pii/S0927796X16300493 |journal=Materials Science and Engineering: R: Reports |volume=110 |pages=1–12 |doi=10.1016/j.mser.2016.10.001 |issn=0927-796X}}
• {{Cite journal |last=Fundenberger |first=J. J. |last2=Bouzy |first2=E. |last3=Goran |first3=D. |last4=Guyon |first4=J. |last5=Yuan |first5=H. |last6=Morawiec |first6=A. |date=2016-02-01 |title=Orientation mapping by transmission-SEM with an on-axis detector |url=https://www.sciencedirect.com/science/article/pii/S0304399115300656 |journal=Ultramicroscopy |volume=161 |pages=17–22 |doi=10.1016/j.ultramic.2015.11.002 |issn=0304-3991}}
• {{Cite journal |last=Niessen |first=F. |last2=Burrows |first2=A. |last3=Fanta |first3=A. Bastos da Silva |date=2018-03-01 |title=A systematic comparison of on-axis and off-axis transmission Kikuchi diffraction |url=https://www.sciencedirect.com/science/article/pii/S0304399117303777 |journal=Ultramicroscopy |volume=186 |pages=158–170 |doi=10.1016/j.ultramic.2017.12.017 |issn=0304-3991}}

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