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Title: A modular reactor design for in situ synchrotron X-ray investigation of atomic layer deposition processes

Abstract

Synchrotron characterization techniques provide some of the most powerful tools for the study of film structure and chemistry. The brilliance and tunability of the Advanced Photon Source allow access to scattering and spectroscopic techniques unavailable with in-house laboratory setups and provide the opportunity to probe various atomic layer deposition (ALD) processes in situ starting at the very first deposition cycle. Here, we present the design and implementation of a portable ALD instrument which possesses a modular reactor scheme that enables simple experimental switchover between various beamlines and characterization techniques. As first examples, we present \textit{in situ} results for 1.) X-ray surface scattering and reflectivity measurements of epitaxial ZnO ALD on sapphire, 2.) grazing-incidence small angle scattering of MnO nucleation on silicon, and 3.) grazing-incidence X-ray absorption spectroscopy of nucleation-regime Er2O3 ALD on amorphous ALD alumina and single crystalline sapphire.

Authors:
; ; ; ; ; ; ; ; ;
Publication Date:
Research Org.:
Argonne National Lab. (ANL), Argonne, IL (United States)
Sponsoring Org.:
Canadian Light Source, Inc.; University of Washington; USDOE Office of Science - Early Career Award; USDOE Office of Science - Energy Frontier Research Center - Argonne-Northwestern Solar Energy Research (ANSER); USDOE Office of Science (SC), Basic Energy Sciences (BES) (SC-22)
OSTI Identifier:
1237843
DOE Contract Number:
AC02-06CH11357
Resource Type:
Journal Article
Resource Relation:
Journal Name: Review of Scientific Instruments; Journal Volume: 86; Journal Issue: 11
Country of Publication:
United States
Language:
English
Subject:
X-ray scattering; X-ray spectroscopy; atomic layer deposition; thin film growth

Citation Formats

Klug, Jeffrey A., Weimer, Matthew S., Emery, Jonathan D., Yanguas-Gil, Angel, Seifert, Sonke, Schleputz, Christian M., Martinson, Alex B. F., Elam, Jeffrey W., Hock, Adam S., and Proslier, Thomas. A modular reactor design for in situ synchrotron X-ray investigation of atomic layer deposition processes. United States: N. p., 2015. Web. doi:10.1063/1.4934807.
Klug, Jeffrey A., Weimer, Matthew S., Emery, Jonathan D., Yanguas-Gil, Angel, Seifert, Sonke, Schleputz, Christian M., Martinson, Alex B. F., Elam, Jeffrey W., Hock, Adam S., & Proslier, Thomas. A modular reactor design for in situ synchrotron X-ray investigation of atomic layer deposition processes. United States. doi:10.1063/1.4934807.
Klug, Jeffrey A., Weimer, Matthew S., Emery, Jonathan D., Yanguas-Gil, Angel, Seifert, Sonke, Schleputz, Christian M., Martinson, Alex B. F., Elam, Jeffrey W., Hock, Adam S., and Proslier, Thomas. 2015. "A modular reactor design for in situ synchrotron X-ray investigation of atomic layer deposition processes". United States. doi:10.1063/1.4934807.
@article{osti_1237843,
title = {A modular reactor design for in situ synchrotron X-ray investigation of atomic layer deposition processes},
author = {Klug, Jeffrey A. and Weimer, Matthew S. and Emery, Jonathan D. and Yanguas-Gil, Angel and Seifert, Sonke and Schleputz, Christian M. and Martinson, Alex B. F. and Elam, Jeffrey W. and Hock, Adam S. and Proslier, Thomas},
abstractNote = {Synchrotron characterization techniques provide some of the most powerful tools for the study of film structure and chemistry. The brilliance and tunability of the Advanced Photon Source allow access to scattering and spectroscopic techniques unavailable with in-house laboratory setups and provide the opportunity to probe various atomic layer deposition (ALD) processes in situ starting at the very first deposition cycle. Here, we present the design and implementation of a portable ALD instrument which possesses a modular reactor scheme that enables simple experimental switchover between various beamlines and characterization techniques. As first examples, we present \textit{in situ} results for 1.) X-ray surface scattering and reflectivity measurements of epitaxial ZnO ALD on sapphire, 2.) grazing-incidence small angle scattering of MnO nucleation on silicon, and 3.) grazing-incidence X-ray absorption spectroscopy of nucleation-regime Er2O3 ALD on amorphous ALD alumina and single crystalline sapphire.},
doi = {10.1063/1.4934807},
journal = {Review of Scientific Instruments},
number = 11,
volume = 86,
place = {United States},
year = 2015,
month =
}
  • Synchrotron characterization techniques provide some of the most powerful tools for the study of film structure and chemistry. The brilliance and tunability of the Advanced Photon Source allow access to scattering and spectroscopic techniques unavailable with in-house laboratory setups and provide the opportunity to probe various atomic layer deposition (ALD) processes in situ starting at the very first deposition cycle. Here, we present the design and implementation of a portable ALD instrument which possesses a modular reactor scheme that enables simple experimental switchover between various beamlines and characterization techniques. As first examples, we present in situ results for (1) X-raymore » surface scattering and reflectivity measurements of epitaxial ZnO ALD on sapphire, (2) grazing-incidence small angle scattering of MnO nucleation on silicon, and (3) grazing-incidence X-ray absorption spectroscopy of nucleation-regime Er{sub 2}O{sub 3} ALD on amorphous ALD alumina and single crystalline sapphire.« less
  • Cited by 4
  • Spatial atomic layer deposition (ALD) is a new version of ALD based on the separation of reactant gases in space instead of time. In this paper, the authors present results for spatial ALD on flexible substrates using a modular rotating cylinder reactor. The design for this reactor is based on two concentric cylinders. The outer cylinder remains fixed and contains a series of slits. These slits can accept a wide range of modules that attach from the outside. The modules can easily move between the various slit positions and perform precursor dosing, purging, or pumping. The inner cylinder rotates withmore » the flexible substrate and passes underneath the various spatially separated slits in the outer cylinder. Trimethyl aluminum and ozone were used to grow Al{sub 2}O{sub 3} ALD films at 40 °C on metallized polyethylene terephthalate (PET) substrates to characterize this spatial ALD reactor. Spectroscopic ellipsometry measurements revealed a constant Al{sub 2}O{sub 3} ALD growth rate of 1.03 Å/cycle with rotation speeds from 40 to 100 RPM with the outer cylinder configured for one Al{sub 2}O{sub 3} ALD cycle per rotation. The Al{sub 2}O{sub 3} ALD growth rate then decreased at higher rotation rates for reactant residence times < 5 ms. The Al{sub 2}O{sub 3} ALD films were also uniform to within <1% across the central portion of metallized PET substrate. Fixed deposition time experiments revealed that Al{sub 2}O{sub 3} ALD films could be deposited at 2.08 Å/s at higher rotation speeds of 175 RPM. Even faster deposition rates are possible by adding more modules for additional Al{sub 2}O{sub 3} ALD cycles for every one rotation of the inner cylinder.« less