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Title: Sub-Monolayer Accuracy in Determining the Number of Atoms per Unit Area in Ultrathin Films Using X-ray Fluorescence

Journal Article · · Chemistry of Materials

We present that the composition and thickness of thin films determine their physical properties, making the ability to measure the number of atoms of different elements in films both technologically and scientifically important. For thin films, below a certain thickness, the X-ray fluorescence intensity of an element is proportional to the number of atoms. Converting this intensity to the number of atoms per unit area is challenging due to experimental geometries and other correction factors. Hence, the ratio of intensities is more commonly used to determine the composition in terms of element ratios using standards or a model. Here, the number of atoms per unit area was determined using X-ray structure information for over 20 different crystallographically aligned samples with integral unit cell thicknesses. The proportionality constant between intensity and the number of atoms per unit area was determined from linear fits of the background subtracted X-ray fluorescence intensity plotted versus the calculated number of atoms per unit area for each element. The results demonstrate that X-ray fluorescence is very sensitive, capable of measuring changes in the number of atoms of less than 1% of a monolayer for some elements in a variety of sample matrices. Finally, using the calibrated values, an 8 unit cell thick MoSe2 was grown and characterized, demonstrating the usefulness of the ablity to quantify the number of atoms per unit area in a film.

Research Organization:
Los Alamos National Lab. (LANL), Los Alamos, NM (United States)
Sponsoring Organization:
USDOE; National Science Foundation (NSF)
Grant/Contract Number:
AC52-06NA25396
OSTI ID:
1469555
Report Number(s):
LA-UR-18-23252
Journal Information:
Chemistry of Materials, Vol. 30, Issue 18; ISSN 0897-4756
Publisher:
American Chemical Society (ACS)Copyright Statement
Country of Publication:
United States
Language:
English
Citation Metrics:
Cited by: 32 works
Citation information provided by
Web of Science

References (39)

Electric Field Effect in Atomically Thin Carbon Films journal October 2004
Nobel Lecture: Graphene: Materials in the Flatland journal August 2011
Observation of Ultrafast Free Carrier Dynamics in Single Layer MoS 2 journal August 2015
Single-layer MoS 2 on Au(111): Band gap renormalization and substrate interaction journal April 2016
Nobel Lecture: Random walk to graphene journal August 2011
Heterostructures containing dichalcogenides-new materials with predictable nanoarchitectures and novel emergent properties journal August 2017
Mixed-dimensional van der Waals heterostructures journal August 2016
Atomically Thin MoS2 A New Direct-Gap Semiconductor journal September 2010
Evolution of Electronic Structure in Atomically Thin Sheets of WS 2 and WSe 2 journal December 2012
Electronic structures and optical properties of realistic transition metal dichalcogenide heterostructures from first principles journal August 2013
Ultrafast Band Structure Control of a Two-Dimensional Heterostructure journal May 2016
Giant bandgap renormalization and excitonic effects in a monolayer transition metal dichalcogenide semiconductor journal August 2014
Controllable growth of monolayer MoS 2 by chemical vapor deposition via close MoO 2 precursor for electrical and optical applications journal January 2017
Chemical vapor deposition growth of monolayer MoSe2 nanosheets journal April 2014
Transport Properties of Monolayer MoS 2 Grown by Chemical Vapor Deposition journal March 2014
Lateral Versus Vertical Growth of Two-Dimensional Layered Transition-Metal Dichalcogenides: Thermodynamic Insight into MoS 2 journal August 2016
Role of the Seeding Promoter in MoS 2 Growth by Chemical Vapor Deposition journal January 2014
Monolayer MoS2 Heterojunction Solar Cells journal July 2014
Growth Mechanism of Transition Metal Dichalcogenide Monolayers: The Role of Self-Seeding Fullerene Nuclei journal May 2016
High-mobility three-atom-thick semiconducting films with wafer-scale homogeneity journal April 2015
Epitaxial Monolayer MoS 2 on Mica with Novel Photoluminescence journal July 2013
Synthesis of Large-Area MoS2 Atomic Layers with Chemical Vapor Deposition journal March 2012
Vapour phase growth and grain boundary structure of molybdenum disulphide atomic layers journal June 2013
Generalized Mechanistic Model for the Chemical Vapor Deposition of 2D Transition Metal Dichalcogenide Monolayers journal March 2016
Shape Evolution of Monolayer MoS 2 Crystals Grown by Chemical Vapor Deposition journal November 2014
Chemical Vapor Deposition Growth of Monolayer WSe 2 with Tunable Device Characteristics and Growth Mechanism Study journal May 2015
Visualization and quantification of transition metal atomic mixing in Mo1−xWxS2 single layers journal January 2013
Direct observation of a gap opening in topological interface states of MnSe/Bi 2 Se 3 heterostructure journal August 2015
Large-Gap Magnetic Topological Heterostructure Formed by Subsurface Incorporation of a Ferromagnetic Layer journal May 2017
Time-of-flight secondary ion mass spectrometry measurements of a fluorocarbon-based self-assembled monolayer on Si journal July 2006
Simultaneous determination of composition and mass thickness of thin films by quantitative x-ray fluorescence analysis journal July 1977
Applicability of X-ray fluorescence spectroscopy as method to determine thickness and composition of stacks of metal thin films: A comparison with imaging and profilometry journal January 2012
X-ray fluorescence measurements of thin film chalcopyrite solar cells journal July 1999
Deposition system for the synthesis of modulated, ultrathin‐film composites
  • Fister, Loreli; Li, Xiao‐Mei; McConnell, John
  • Journal of Vacuum Science & Technology A: Vacuum, Surfaces, and Films, Vol. 11, Issue 6 https://doi.org/10.1116/1.578290
journal November 1993
The theoretical derivation of fluorescent X-ray intensities from mixtures journal January 1955
Über den atomaren Photoeffekt bei großer Härte der anregenden Strahlung journal January 1931
Über den atomaren Photoeffekt in der K-Schale nach der relativistischen Wellenmechanik Diracs journal January 1931
Charge Transfer between PbSe and NbSe 2 in [(PbSe) 1.14 ] m (NbSe 2 ) 1 Ferecrystalline Compounds journal February 2014
On the structure of molybdenum diselenide and disulfide journal September 1986

Cited By (3)

Electronic structure of designed [(SnSe)1+δ]m[TiSe2]2 heterostructure thin films with tunable layering sequence journal April 2019
Ultralow thermal conductivity of turbostratically disordered MoSe 2 ultra-thin films and implications for heterostructures journal April 2019
Strong Non‐Epitaxial Interactions: Crystallographically Aligned PbSe on VSe 2 journal January 2019

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