% IMPORTANT: The following is UTF-8 encoded. This means that in the presence % of non-ASCII characters, it will not work with BibTeX 0.99 or older. % Instead, you should use an up-to-date BibTeX implementation like “bibtex8” or % “biber”. @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}, }