Versatile technique for assessing thickness of 2D layered materials by XPS

Zemlyanov, Dmitry Y.; Jespersen, Michael; Zakharov, Dmitry N.; Hu, Jianjun; Paul, Rajib; Kumar, Anurag; Pacley, Shanee; Glavin, Nicholas; Saenz, David; Smith, Kyle C.; Fisher, Timothy S.; Voevodin, Andrey A.

doi:10.1088/1361-6528/aaa6ef

Versatile technique for assessing thickness of 2D layered materials by XPS

Journal Article · Wed Feb 07 00:00:00 EST 2018 · Nanotechnology

DOI:https://doi.org/10.1088/1361-6528/aaa6ef· OSTI ID:1434775

Zemlyanov, Dmitry Y. ^[1]; Jespersen, Michael ^[2]; ^[3]; Hu, Jianjun ^[2]; ^[4]; Kumar, Anurag ^[1]; Pacley, Shanee ^[2]; Glavin, Nicholas ^[5]; Saenz, David ^[1]; ^[6]; Fisher, Timothy S. ^[7]; Voevodin, Andrey A. ^[8]

Purdue Univ., West Lafayette, IN (United States)
Air Force Research Lab., WPAFB, OH (United States)
Purdue Univ., West Lafayette, IN (United States); Brookhaven National Lab. (BNL), Upton, NY (United States)
Purdue Univ., West Lafayette, IN (United States); Case Western Reserve Univ., Cleveland, OH (United States)
Purdue Univ., West Lafayette, IN (United States); Air Force Research Lab., WPAFB, OH (United States)
Purdue Univ., West Lafayette, IN (United States); Univ. of Illinois at Urbana-Champaign, Urbana, IL (United States)
Purdue Univ., West Lafayette, IN (United States); Air Force Research Lab., WPAFB, OH (United States); Univ. of California, Los Angeles, CA (United States)
Purdue Univ., West Lafayette, IN (United States); Air Force Research Lab., WPAFB, OH (United States); Univ. of North Texas, Denton, TX (United States)

X-ray photoelectron spectroscopy (XPS) has been utilized as a versatile method for thickness characterization of various two-dimensional (2D) films. Accurate thickness can be measured simultaneously while acquiring XPS data for chemical characterization of 2D films having thickness up to approximately 10 nm. For validating the developed technique, thicknesses of few-layer graphene (FLG), MoS₂ and amorphous boron nitride (a-BN) layer, produced by microwave plasma chemical vapor deposition (MPCVD), plasma enhanced chemical vapor deposition (PECVD), and pulsed laser deposition (PLD) respectively, were accurately measured. The intensity ratio between photoemission peaks recorded for the films (C 1s, Mo 3d, B 1s) and the substrates (Cu 2p, Al 2p, Si 2p) is the primary input parameter for thickness calculation, in addition to the atomic densities of the substrate and the film, and the corresponding electron attenuation length (EAL). The XPS data was used with a proposed model for thickness calculations, which was verified by cross-sectional transmission electron microscope (TEM) measurement of thickness for all the films. The XPS method determines thickness values averaged over an analysis area which is orders of magnitude larger than the typical area in cross-sectional TEM imaging, hence provides an advanced approach for thickness measurement over large areas of 2D materials. The study confirms that the versatile XPS method allows rapid and reliable assessment of the 2D material thickness and this method can facilitate in tailoring growth conditions for producing very thin 2D materials effectively over a large area. Furthermore, the XPS measurement for a typical 2D material is non-destructive and does not require special sample preparation. Furthermore, after XPS analysis, exactly the same sample can undergo further processing or utilization.

View Accepted Manuscript (DOE)

Research Organization:: Brookhaven National Laboratory (BNL), Upton, NY (United States)

Sponsoring Organization:: USDOE Office of Science (SC), Basic Energy Sciences (BES) (SC-22)

Grant/Contract Number:: SC0012704

OSTI ID:: 1434775

Alternate ID(s):: OSTI ID: 23113994

Report Number(s):: BNL--203564-2018-JAAM

Journal Information:: Nanotechnology, Journal Name: Nanotechnology Journal Issue: 11 Vol. 29; ISSN 0957-4484

Publisher:: IOP PublishingCopyright Statement

Country of Publication:: United States

Language:: English

References (42)

The Thickogram: a method for easy film thickness measurement in XPS Cumpson, Peter J. Surface and Interface Analysis, Vol. 29, Issue 6 https://doi.org/10.1002/1096-9918(200006)29:6<403::aid-sia884>3.0.co;2-8	journal	January 2000
Amorphous Boron Nitride: A Universal, Ultrathin Dielectric For 2D Nanoelectronics Glavin, Nicholas R.; Muratore, Christopher; Jespersen, Michael L. Advanced Functional Materials, Vol. 26, Issue 16 https://doi.org/10.1002/adfm.201505455	journal	March 2016
Synthesis of Large-Area MoS₂ Atomic Layers with Chemical Vapor Deposition Lee, Yi-Hsien; Zhang, Xin-Quan; Zhang, Wenjing Advanced Materials, Vol. 24, Issue 17, p. 2320-2325 https://doi.org/10.1002/adma.201104798	journal	March 2012
XPS: Energy calibration of electron spectrometers. 1—An absolute, traceable energy calibration and the provision of atomic reference line energies Anthony, M. T.; Seah, M. P. Surface and Interface Analysis, Vol. 6, Issue 3 https://doi.org/10.1002/sia.740060302	journal	June 1984
Prevention of Water Permeation by Strong Adhesion Between Graphene and SiO ₂ Substrate Jung, Wonsuk; Park, Joonkyu; Yoon, Taeshik Small, Vol. 10, Issue 9 https://doi.org/10.1002/smll.201302729	journal	December 2013
Properties of oxidized silicon as determined by angular-dependent X-ray photoelectron spectroscopy Hill, J. M.; Royce, D. G.; Fadley, C. S. Chemical Physics Letters, Vol. 44, Issue 2 https://doi.org/10.1016/0009-2614(76)80496-4	journal	December 1976
Energy calibration in electron spectroscopy and the re-determination of some reference electron binding energies Bird, R. J.; Swift, P. Journal of Electron Spectroscopy and Related Phenomena, Vol. 21, Issue 3 https://doi.org/10.1016/0368-2048(80)85050-X	journal	January 1980
Energy calibration in electron spectroscopy and the re-determination of some reference electron binding energies Bird, R. J.; Swift, P. Journal of Electron Spectroscopy and Related Phenomena, Vol. 21, Issue 3 https://doi.org/10.1016/0368-2048(80)85050-x	journal	January 1980
Anomalies in thickness measurements of graphene and few layer graphite crystals by tapping mode atomic force microscopy Nemes-Incze, P.; Osváth, Z.; Kamarás, K. Carbon, Vol. 46, Issue 11 https://doi.org/10.1016/j.carbon.2008.06.022	journal	September 2008
AFM study of ridges in few-layer epitaxial graphene grown on the carbon-face of 4H–SiC Prakash, Gyan; Capano, Michael A.; Bolen, Michael L. Carbon, Vol. 48, Issue 9 https://doi.org/10.1016/j.carbon.2010.02.026	journal	August 2010
Determining the thickness of chemically modified graphenes by scanning probe microscopy Solís-Fernández, P.; Paredes, J. I.; Villar-Rodil, S. Carbon, Vol. 48, Issue 9 https://doi.org/10.1016/j.carbon.2010.03.033	journal	August 2010
Rapid synthesis of few-layer graphene over Cu foil Kumar, A.; Voevodin, A. A.; Zemlyanov, D. Carbon, Vol. 50, Issue 4 https://doi.org/10.1016/j.carbon.2011.11.033	journal	April 2012
Histogram method for reliable thickness measurements of graphene films using atomic force microscopy (AFM) Yao, Yaxuan; Ren, Lingling; Gao, Sitian Journal of Materials Science & Technology, Vol. 33, Issue 8 https://doi.org/10.1016/j.jmst.2016.07.020	journal	August 2017
Raman spectroscopy of graphene and graphite: Disorder, electron–phonon coupling, doping and nonadiabatic effects Ferrari, Andrea C. Solid State Communications, Vol. 143, Issue 1-2, p. 47-57 https://doi.org/10.1016/j.ssc.2007.03.052	journal	July 2007
Synthesis of few-layer, large area hexagonal-boron nitride by pulsed laser deposition Glavin, Nicholas R.; Jespersen, Michael L.; Check, Michael H. Thin Solid Films, Vol. 572 https://doi.org/10.1016/j.tsf.2014.07.059	journal	December 2014
Methanol wetting enthalpy on few-layer graphene decorated hierarchical carbon foam for cooling applications Paul, R.; Zemlyanov, D.; Voevodin, A. A. Thin Solid Films, Vol. 572 https://doi.org/10.1016/j.tsf.2014.08.020	journal	December 2014
A Confocal Raman-AFM Study of Graphene Schmidt, U.; Dieing, T.; Ibach, W. Microscopy Today, Vol. 19, Issue 6 https://doi.org/10.1017/S1551929511001192	journal	October 2011
A Confocal Raman-AFM Study of Graphene Schmidt, U.; Dieing, T.; Ibach, W. Microscopy Today, Vol. 19, Issue 6 https://doi.org/10.1017/s1551929511001192	journal	October 2011
Atomic Layer Deposition of FeO on Pt(111) by Ferrocene Adsorption and Oxidation Paul, Rajib; Reifenberger, Ronald G.; Fisher, Timothy S. Chemistry of Materials, Vol. 27, Issue 17 https://doi.org/10.1021/acs.chemmater.5b01778	journal	August 2015
New Approach for Thickness Determination of Solution-Deposited Graphene Thin Films Jussila, Henri; Albrow-Owen, Tom; Yang, He ACS Omega, Vol. 2, Issue 6 https://doi.org/10.1021/acsomega.7b00336	journal	June 2017
Statistical Raman Microscopy and Atomic Force Microscopy on Heterogeneous Graphene Obtained after Reduction of Graphene Oxide Eigler, Siegfried; Hof, Ferdinand; Enzelberger-Heim, Michael The Journal of Physical Chemistry C, Vol. 118, Issue 14 https://doi.org/10.1021/jp500580g	journal	March 2014
Atomic Force and Scanning Tunneling Microscopy Imaging of Graphene Nanosheets Derived from Graphite Oxide Paredes, J. I.; Villar-Rodil, S.; Solís-Fernández, P. Langmuir, Vol. 25, Issue 10 https://doi.org/10.1021/la804216z	journal	May 2009
Atomic Structure of Graphene on SiO₂ Ishigami, Masa; Chen, J. H.; Cullen, W. G. Nano Letters, Vol. 7, Issue 6, p. 1643-1648 https://doi.org/10.1021/nl070613a	journal	June 2007
Superior Thermal Conductivity of Single-Layer Graphene Balandin, Alexander A.; Ghosh, Suchismita; Bao, Wenzhong Nano Letters, Vol. 8, Issue 3, p. 902-907 https://doi.org/10.1021/nl0731872	journal	March 2008
Strong Suppression of Electrical Noise in Bilayer Graphene Nanodevices Lin, Yu-Ming; Avouris, Phaedon Nano Letters, Vol. 8, Issue 8 https://doi.org/10.1021/nl080241l	journal	August 2008
Anomalous Lattice Vibrations of Single- and Few-Layer MoS ₂ Lee, Changgu; Yan, Hugen; Brus, Louis E. ACS Nano, Vol. 4, Issue 5 https://doi.org/10.1021/nn1003937	journal	March 2010
Vapour phase growth and grain boundary structure of molybdenum disulphide atomic layers Najmaei, Sina; Liu, Zheng; Zhou, Wu Nature Materials, Vol. 12, Issue 8, p. 754-759 https://doi.org/10.1038/nmat3673	journal	June 2013
Domain engineering of physical vapor deposited two-dimensional materials Alam, Tarek; Wang, Baoming; Pulavarthy, Raghu Applied Physics Letters, Vol. 105, Issue 21 https://doi.org/10.1063/1.4902937	journal	November 2014
Insights into few-layer epitaxial graphene growth on 4 H -SiC ( 000 1 ¯ ) substrates from STM studies Biedermann, Laura B.; Bolen, Michael L.; Capano, Michael A. Physical Review B, Vol. 79, Issue 12 https://doi.org/10.1103/PhysRevB.79.125411	journal	March 2009
Atomically Thin MoS2 A New Direct-Gap Semiconductor Mak, Kin Fai; Lee, Changgu; Hone, James Physical Review Letters, Vol. 105, Issue 13, Article No.136805 https://doi.org/10.1103/PhysRevLett.105.136805	journal	September 2010
Insights into few-layer epitaxial graphene growth on 4 H -SiC ( 000 1 ¯ ) substrates from STM studies Biedermann, Laura B.; Bolen, Michael L.; Capano, Michael A. Physical Review B, Vol. 79, Issue 12 https://doi.org/10.1103/physrevb.79.125411	journal	March 2009
Atomically Thin MoS2 A New Direct-Gap Semiconductor Mak, Kin Fai; Lee, Changgu; Hone, James Physical Review Letters, Vol. 105, Issue 13, Article No.136805 https://doi.org/10.1103/physrevlett.105.136805	journal	September 2010
Impact of reduced graphene oxide on MoS ₂ grown by sulfurization of sputtered MoO ₃ and Mo precursor films Pacley, Shanee; Hu, Jianjun; Jespersen, Michael Journal of Vacuum Science & Technology A: Vacuum, Surfaces, and Films, Vol. 34, Issue 4 https://doi.org/10.1116/1.4952399	journal	July 2016
Summary Abstract: Accurate determination of the energies of Auger electrons and photoelectrons from nickel, copper, and gold Powell, C. J.; Erickson, N. E.; Jach, T. Journal of Vacuum Science and Technology, Vol. 20, Issue 3 https://doi.org/10.1116/1.571409	journal	March 1982
Electric Field Effect in Atomically Thin Carbon Films Novoselov, K. S. Science, Vol. 306, Issue 5696, p. 666-669 https://doi.org/10.1126/science.1102896	journal	October 2004
Graphene Visualizes the First Water Adlayers on Mica at Ambient Conditions Xu, K.; Cao, P.; Heath, J. R. Science, Vol. 329, Issue 5996 https://doi.org/10.1126/science.1192907	journal	September 2010
New Approach for Thickness Determination of Solution-Deposited Graphene Thin Films Jussila, H.; Albrow-Owen, Thomas; Yang, H. Apollo - University of Cambridge Repository https://doi.org/10.17863/cam.12740	text	January 2017
Atomic Structure of Graphene on SiO2 Ishigami, Masa; Chen, J. H.; Cullen, W. G. arXiv https://doi.org/10.48550/arxiv.0811.0587	text	January 2008
Anomalies in thickness measurements of graphene and few layer graphite crystals by tapping mode atomic force microscopy Nemes-Incze, P.; Osvath, Z.; Kamaras, K. arXiv https://doi.org/10.48550/arxiv.0812.0690	text	January 2008
Anomalous Lattice Vibrations of Single and Few-Layer MoS2 Lee, Changgu; Yan, Hugen; Brus, Louis E. arXiv https://doi.org/10.48550/arxiv.1005.2509	text	January 2010
Vapor Phase Growth and Grain Boundary Structure of Molybdenum Disulfide Atomic Layers Najmaei, Sina; Liu, Zheng; Zhou, Wu arXiv https://doi.org/10.48550/arxiv.1301.2812	text	January 2013
Electric Field Effect in Atomically Thin Carbon Films Novoselov, K. S.; Geim, A. K.; Morozov, S. V. arXiv https://doi.org/10.48550/arxiv.cond-mat/0410550	text	January 2004

Cited By (2)

Enhancing Interconnect Reliability and Performance by Converting Tantalum to 2D Layered Tantalum Sulfide at Low Temperature Lo, Chun‐Li; Catalano, Massimo; Khosravi, Ava Advanced Materials https://doi.org/10.1002/adma.201902397	journal	June 2019
Single process CVD growth of hBN/Graphene heterostructures on copper thin films Siegel, Gene; Grzybowski, Gordon; Prusnick, Timothy Journal of Materials Research, Vol. 33, Issue 24 https://doi.org/10.1557/jmr.2018.392	journal	November 2018

Similar Records

Thermally Evaporated Iron (Oxide) on an Alumina Barrier Layer, by XPS

Journal Article · Fri Sep 06 00:00:00 EDT 2013 · Surface Science Spectra, 20(1):Article No. 49 · OSTI ID:1094926

XPS Investigation of Surface Secondary Phase Segregation in CIGS Thin Film

Conference · Fri Dec 31 23:00:00 EST 2010 · OSTI ID:1049003

Pulsed Laser Deposition of Photoresponsive Two-Dimensional GaSe Nanosheet Networks

Journal Article · Tue Dec 31 23:00:00 EST 2013 · Advanced Functional Materials · OSTI ID:1156737

Related Subjects

2D film thickness
77 NANOSCIENCE AND NANOTECHNOLOGY
MoS2 film
XPS thickness measurement
amorphous BN film
few-layer graphene
non-destructive measurement

Versatile technique for assessing thickness of 2D layered materials by XPS

Citation Formats

References (42)

Cited By (2)

Similar Records

Related Subjects