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@INPROCEEDINGS{Park:911525,
author = {Park, Junbeom and Jo, Janghyun and Xu, Qi and Camara,
Osmane and Tempel, Hermann and Kungl, Hans and Basak,
Shibabrata and Bauer, Alexander and Eichel, Rüdiger-A.},
title = {{FIB}-based lamella preparation on {MEMS} chip for in-situ
{TEM}},
reportid = {FZJ-2022-04785},
year = {2022},
abstract = {The in-situ transmission electron microscope (in-situ TEM)
method enables observing the morphological, structural, and
chemical transition of the sample with stimuli such as
heating or biasing via up to atomic resolution. For a
successful in-situ TEM experiment, the sample should be
prepared to fit the experimental requirements to stimulate
correctly. In the sintering process, heating and gas
environments are required as stimuli. Compared to heating,
the gas environment is a challenging stimulus because the
inside of TEM is ultra-high vacuum $(10^-4$ ~ $10^-9$ Pa)
condition. Environmental TEM (ETEM) can form the gas
environment up to 10 Pa, but many sintering processes are
conducted at atmospheric pressure $(10^6$ Pa). Therefore, a
nano-sized closed chamber is mandatory to replicate the real
sintering process in TEM. Electron transmittable thin SiN
film-coated micro-electromechanical system (MEMS) chips
enable the formation of atmospheric conditions in the TEM.
If the sample is a nanoparticle, drop-casting on a MEMS chip
is the simplest way to prepare. However, nanoparticle shape
is not available to investigate the phenomena such as
interaction on composite materials. The focused ion-beam
(FIB) method is a useful preparation method for the TEM
sample (lamella) from the bulk to analyze the sample beyond
nanoparticles. The FIB-based preparation for the in-situ TEM
method contains two processes; lamella preparation and
lamella attachment on MEMS chip. Lamella preparation for
MEMS chip is almost similar to regular TEM analysis, except
if the stimulus is biasing. In the case of biasing
experiment, the lamella should be prepared without the Pt
layer, which is typically used as a protective layer during
the FIB process. To obtain the lamella properly without Pt
protection layer, the ion beam should be adjusted to lower
electron voltage and lower current conditions.Lamella
attachment on the MEMS chip is the most challenging point.
Electron beam imaging and ion beam imaging are generally
used to recognize 3-dimensional movement during the
attachment. In MEMS chips case, especially for gas
experiments, ion beam imaging can break the thin SiN film.
To avoid breaking the SiN film, lamella should be controlled
mostly on electron beam and carefully checked with minimum
ion beam dose as much as possible. We will introduce the
FIB-based sample preparation and in-situ TEM gas experiment
result to investigate the solid-state electrolyte sintering
process.},
month = {Sep},
date = {2022-09-04},
organization = {16th Multinational Congress on
Microscopy, Brno (Czech Republic), 4
Sep 2022 - 9 Sep 2022},
subtyp = {After Call},
cin = {IEK-9 / ER-C-1},
cid = {I:(DE-Juel1)IEK-9-20110218 / I:(DE-Juel1)ER-C-1-20170209},
pnm = {1232 - Power-based Fuels and Chemicals (POF4-123) / iNEW2.0
(BMBF-03SF0627A) / Electroscopy - Electrochemistry of
All-solid-state-battery Processes using Operando Electron
Microscopy (892916) / HITEC - Helmholtz Interdisciplinary
Doctoral Training in Energy and Climate Research (HITEC)
(HITEC-20170406)},
pid = {G:(DE-HGF)POF4-1232 / G:(DE-Juel1)BMBF-03SF0627A /
G:(EU-Grant)892916 / G:(DE-Juel1)HITEC-20170406},
typ = {PUB:(DE-HGF)6},
url = {https://juser.fz-juelich.de/record/911525},
}