Mitigating e-beam-induced hydrocarbon deposition on graphene for atomic-scale scanning transmission electron microscopy studies

Dyck, Ondrej; Kim, Songkil; Kalinin, Sergei V.; Jesse, Stephen

doi:10.1116/1.5003034

Title: Mitigating e-beam-induced hydrocarbon deposition on graphene for atomic-scale scanning transmission electron microscopy studies

Journal Article · Mon Dec 04 00:00:00 EST 2017 · Journal of Vacuum Science and Technology B

DOI:https://doi.org/10.1116/1.5003034· OSTI ID:1771916

^[1];

^[1]

Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Center for Nanophase Materials Sciences (CNMS); Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Inst. for Functioanl Imaging of Materials

Chemical vapor deposition (CVD) grown graphene used in (scanning) transmission electron microscopy [(S)TEM] studies must undergo a careful transfer of the one-atom-thick membrane from the growth surface (typically a Cu foil) to the TEM grid. During this transfer process, the graphene invariably becomes contaminated with foreign materials. This contamination proves to be very problematic in the (S)TEM because often >95% of the graphene is obscured, and imaging of the pristine areas results in e-beam-induced hydrocarbon deposition which further acts to obscure the desired imaging area. In this article, the authors examine two cleaning techniques for CVD grown graphene that mitigate both aspects of the contamination problem: visible contamination covering the graphene, and “invisible” contamination that deposits onto the graphene under e-beam irradiation. Furthermore, the visible contamination may be removed quickly by a rapid thermal annealing to 1200 °C in situ and the invisible e-beam-deposited contamination may be removed through an Ar/O₂ annealing procedure prior to imaging in the (S)TEM.

View Accepted Manuscript (DOE)

Cite

Export

Save

Research Organization:: Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States)

Sponsoring Organization:: USDOE Office of Science (SC)

Grant/Contract Number:: AC05-00OR22725

OSTI ID:: 1771916

Alternate ID(s):: OSTI ID: 1411101

Journal Information:: Journal of Vacuum Science and Technology B, Vol. 36, Issue 1; ISSN 2166-2746

Publisher:: American Vacuum Society / AIPCopyright Statement

Country of Publication:: United States

Language:: English

Citation Metrics:

Cited by: 37 works

Citation information provided by
Web of Science

References (33)

How the doors to the nanoworld were opened Gerber, Christoph; Lang, Hans Peter Nature Nanotechnology, Vol. 1, Issue 1 https://doi.org/10.1038/nnano.2006.70	journal	October 2006
Atomic-scale study of electric dipoles near charged and uncharged domain walls in ferroelectric films Jia, Chun-Lin; Mi, Shao-Bo; Urban, Knut Nature Materials, Vol. 7, Issue 1 https://doi.org/10.1038/nmat2080	journal	December 2007
Unit-cell scale mapping of ferroelectricity and tetragonality in epitaxial ultrathin ferroelectric films Jia, Chun-Lin; Nagarajan, Valanoor; He, Jia-Qing Nature Materials, Vol. 6, Issue 1 https://doi.org/10.1038/nmat1808	journal	December 2006
Suppression of Octahedral Tilts and Associated Changes in Electronic Properties at Epitaxial Oxide Heterostructure Interfaces Borisevich, A. Y.; Chang, H. J.; Huijben, M. Physical Review Letters, Vol. 105, Issue 8 https://doi.org/10.1103/PhysRevLett.105.087204	journal	August 2010
Control of Octahedral Tilts and Magnetic Properties of Perovskite Oxide Heterostructures by Substrate Symmetry He, Jun; Borisevich, Albina; Kalinin, Sergei V. Physical Review Letters, Vol. 105, Issue 22 https://doi.org/10.1103/PhysRevLett.105.227203	journal	November 2010
Mapping Octahedral Tilts and Polarization Across a Domain Wall in BiFeO ₃ from Z-Contrast Scanning Transmission Electron Microscopy Image Atomic Column Shape Analysis Borisevich, AlbinaY.; Ovchinnikov, Oleg S.; Chang, Hye Jung ACS Nano, Vol. 4, Issue 10 https://doi.org/10.1021/nn1011539	journal	October 2010
Towards 3D Mapping of BO ₆ Octahedron Rotations at Perovskite Heterointerfaces, Unit Cell by Unit Cell He, Qian; Ishikawa, Ryo; Lupini, Andrew R. ACS Nano, Vol. 9, Issue 8 https://doi.org/10.1021/acsnano.5b03232	journal	July 2015
Probing oxygen vacancy concentration and homogeneity in solid-oxide fuel-cell cathode materials on the subunit-cell level Kim, Young-Min; He, Jun; Biegalski, Michael D. Nature Materials, Vol. 11, Issue 10 https://doi.org/10.1038/nmat3393	journal	August 2012
Atomic-resolution imaging of oxidation states in manganites Varela, M.; Oxley, M. P.; Luo, W. Physical Review B, Vol. 79, Issue 8 https://doi.org/10.1103/PhysRevB.79.085117	journal	February 2009
An Environmental Transmission Electron Microscope for in situ Synthesis and Characterization of Nanomaterials Sharma, Renu Journal of Materials Research, Vol. 20, Issue 7 https://doi.org/10.1557/JMR.2005.0241	journal	July 2005
Engineering of nanostructured carbon materials with electron or ion beams Krasheninnikov, A. V.; Banhart, F. Nature Materials, Vol. 6, Issue 10 https://doi.org/10.1038/nmat1996	journal	October 2007
Imaging and dynamics of light atoms and molecules on graphene Meyer, Jannik C.; Girit, C. O.; Crommie, M. F. Nature, Vol. 454, Issue 7202 https://doi.org/10.1038/nature07094	journal	July 2008
Manipulating low-dimensional materials down to the level of single atoms with electron irradiation Susi, Toma; Meyer, Jannik C.; Kotakoski, Jani Ultramicroscopy, Vol. 180 https://doi.org/10.1016/j.ultramic.2017.03.005	journal	September 2017
Atomic Structure and Dynamics of Metal Dopant Pairs in Graphene He, Zhengyu; He, Kuang; Robertson, Alex W. Nano Letters, Vol. 14, Issue 7 https://doi.org/10.1021/nl500682j	journal	June 2014
Probing the Bonding and Electronic Structure of Single Atom Dopants in Graphene with Electron Energy Loss Spectroscopy Ramasse, Quentin M.; Seabourne, Che R.; Kepaptsoglou, Despoina-Maria Nano Letters, Vol. 13, Issue 10 https://doi.org/10.1021/nl304187e	journal	January 2013
Direct writing on graphene ‘paper’ by manipulating electrons as ‘invisible ink’ Zhang, Wei; Zhang, Qiang; Zhao, Meng-Qiang Nanotechnology, Vol. 24, Issue 27 https://doi.org/10.1088/0957-4484/24/27/275301	journal	June 2013
Electron-beam-assisted superplastic shaping of nanoscale amorphous silica Zheng, Kun; Wang, Chengcai; Cheng, Yong-Qiang Nature Communications, Vol. 1, Issue 1 https://doi.org/10.1038/ncomms1021	journal	June 2010
Partial Dislocations in Graphene and Their Atomic Level Migration Dynamics Robertson, Alex W.; Lee, Gun-Do; He, Kuang Nano Letters, Vol. 15, Issue 9 https://doi.org/10.1021/acs.nanolett.5b02080	journal	August 2015
Atomic-Level Sculpting of Crystalline Oxides: Toward Bulk Nanofabrication with Single Atomic Plane Precision Jesse, Stephen; He, Qian; Lupini, Andrew R. Small, Vol. 11, Issue 44 https://doi.org/10.1002/smll.201502048	journal	October 2015
Ion and electron irradiation-induced effects in nanostructured materials Krasheninnikov, A. V.; Nordlund, K. Journal of Applied Physics, Vol. 107, Issue 7 https://doi.org/10.1063/1.3318261	journal	April 2010
Electron beam damage in oxides: a review Jiang, Nan Reports on Progress in Physics, Vol. 79, Issue 1 https://doi.org/10.1088/0034-4885/79/1/016501	journal	December 2015
Transferring and Identification of Single- and Few-Layer Graphene on Arbitrary Substrates Reina, Alfonso; Son, Hyungbin; Jiao, Liying The Journal of Physical Chemistry C, Vol. 112, Issue 46 https://doi.org/10.1021/jp807380s	journal	October 2008
Transfer of Large-Area Graphene Films for High-Performance Transparent Conductive Electrodes Li, Xuesong; Zhu, Yanwu; Cai, Weiwei Nano Letters, Vol. 9, Issue 12 https://doi.org/10.1021/nl902623y	journal	December 2009
Creation of Nanostructures with Poly(methyl methacrylate)-Mediated Nanotransfer Printing Jiao, Liying; Fan, Ben; Xian, Xiaojun Journal of the American Chemical Society, Vol. 130, Issue 38 https://doi.org/10.1021/ja805070b	journal	September 2008
Nanometer-scale lithography on microscopically clean graphene van Dorp, W. F.; Zhang, X.; Feringa, B. L. Nanotechnology, Vol. 22, Issue 50 https://doi.org/10.1088/0957-4484/22/50/505303	journal	November 2011
Clean graphene surface through high temperature annealing Xie, Wenjing; Weng, Lu-Tao; Ng, Kai Mo Carbon, Vol. 94 https://doi.org/10.1016/j.carbon.2015.07.046	journal	November 2015
Graphene Annealing: How Clean Can It Be? Lin, Yung-Chang; Lu, Chun-Chieh; Yeh, Chao-Huei Nano Letters, Vol. 12, Issue 1, p. 414-419 https://doi.org/10.1021/nl203733r	journal	December 2011
Clean Transfer of Graphene for Isolation and Suspension Lin, Yung-Chang; Jin, Chuanhong; Lee, Jung-Chi ACS Nano, Vol. 5, Issue 3 https://doi.org/10.1021/nn200105j	journal	February 2011
Toward Clean and Crackless Transfer of Graphene Liang, Xuelei; Sperling, Brent A.; Calizo, Irene ACS Nano, Vol. 5, Issue 11 https://doi.org/10.1021/nn203377t	journal	October 2011
Effect of airborne contaminants on the wettability of supported graphene and graphite Li, Zhiting; Wang, Yongjin; Kozbial, Andrew Nature Materials, Vol. 12, Issue 10 https://doi.org/10.1038/nmat3709	journal	July 2013
Cleaning graphene: Comparing heat treatments in air and in vacuum: Cleaning graphene Tripathi, Mukesh; Mittelberger, Andreas; Mustonen, Kimmo physica status solidi (RRL) - Rapid Research Letters, Vol. 11, Issue 8 https://doi.org/10.1002/pssr.201700124	journal	July 2017
Effective Cleaning of Hexagonal Boron Nitride for Graphene Devices Garcia, Andrei G. F.; Neumann, Michael; Amet, François Nano Letters, Vol. 12, Issue 9 https://doi.org/10.1021/nl3011726	journal	January 2012
Placing single atoms in graphene with a scanning transmission electron microscope Dyck, Ondrej; Kim, Songkil; Kalinin, Sergei V. Applied Physics Letters, Vol. 111, Issue 11 https://doi.org/10.1063/1.4998599	journal	September 2017

Cited By (5)

Atom-by-atom fabrication with electron beams Dyck, Ondrej; Ziatdinov, Maxim; Lingerfelt, David B. Nature Reviews Materials, Vol. 4, Issue 7 https://doi.org/10.1038/s41578-019-0118-z	journal	June 2019
Building and exploring libraries of atomic defects in graphene: Scanning transmission electron and scanning tunneling microscopy study Ziatdinov, Maxim; Dyck, Ondrej; Li, Xin Science Advances, Vol. 5, Issue 9 https://doi.org/10.1126/sciadv.aaw8989	journal	September 2019
Pulsed Laser-Assisted Helium Ion Nanomachining of Monolayer Graphene—Direct-Write Kirigami Patterns Zhang, Cheng; Dyck, Ondrej; Garfinkel, David A. Nanomaterials, Vol. 9, Issue 10 https://doi.org/10.3390/nano9101394	journal	September 2019
Manifold learning of four-dimensional scanning transmission electron microscopy Li, Xin; Dyck, Ondrej E.; Oxley, Mark P. npj Computational Materials, Vol. 5, Issue 1 https://doi.org/10.1038/s41524-018-0139-y	journal	January 2019
Insights into radiation damage from atomic resolution scanning transmission electron microscopy imaging of mono-layer CuPcCl16 films on graphene Mittelberger, Andreas; Kramberger, Christian; Meyer, Jannik C. Scientific Reports, Vol. 8, Issue 1 https://doi.org/10.1038/s41598-018-23077-z	journal	March 2018

Similar Records

Effect of e-beam irradiation on graphene layer grown by chemical vapor deposition

Journal Article · Sun Apr 15 00:00:00 EDT 2012 · Journal of Applied Physics · OSTI ID:1771916

Iqbal, M Z; Kumar Singh, Arun; Iqbal, M W; +2 more

Assessing the quality of large-area monolayer graphene grown on liquid copper for size-selective ionic/molecular membrane separations

Journal Article · Thu Oct 12 00:00:00 EDT 2023 · Materials Research Express (Online) · OSTI ID:1771916

Romaniak, Grzegorz; Cheng, Peifu; Dybowski, Konrad; +2 more

Imaging coherent transport in chemical vapor deposition graphene wide constriction by scanning gate microscopy

Journal Article · Mon Mar 21 00:00:00 EDT 2016 · Applied Physics Letters · OSTI ID:1771916

Chuang, Chiashain; Matsunaga, Masahiro; Ochiai, Yuichi; +6 more

Related Subjects

36 MATERIALS SCIENCE
Organic compounds
scanning electron microscopy
graphene
thin film deposition
sample handling
semiconductor device fabrication
chemical elements
carbon based materials
secondary ion mass spectrometry
electron beams

Title: Mitigating e-beam-induced hydrocarbon deposition on graphene for atomic-scale scanning transmission electron microscopy studies

Citation Formats

References (33)

Cited By (5)

Similar Records

Related Subjects