Exploring pore formation of atomic layer-deposited overlayers by in situ small- and wide-angle X-ray scattering

Tao Li; Saurabh Karwal; Bachir Aoun; Haiyan Zhao; Yang Ren; Christian P. Canlas; Jeffrey W. Elam; Randall E. Winans

doi:10.1021/acs.chemmater.6b03222

Exploring pore formation of atomic layer-deposited overlayers by in situ small- and wide-angle X-ray scattering

Tao Li
, Saurabh Karwal
, Bachir Aoun
, Haiyan Zhao
, Yang Ren
, Christian P. Canlas
, Jeffrey W. Elam
, Randall E. Winans^*

^*Corresponding author for this work

Research output: Journal Publications and Reviews › RGC 21 - Publication in refereed journal › peer-review

24 Citations (Scopus)

Abstract

In this work, we explore the pore structure of overcoated materials by in situ synchrotron small-angle (SAXS) and wide-angle X-ray scattering (WAXS). Thin films of aluminum oxide (Al₂O₃) and titanium dioxide (TiO₂) with thicknesses of 4.9 and 2.5 nm, respectively, are prepared by atomic layer deposition (ALD) on nonporous nanoparticles. In situ X-ray measurements reveal that porosity is induced in the ALD films by annealing the samples at high temperatures. Moreover, this pore formation can be attributed to densification resulting from an amorphous to crystalline phase transition of the ALD films as confirmed by high-resolution X-ray diffraction and the pair distribution function. Simultaneous SAXS and WAXS results show not only that the porosity is formed by the phase transition but also that the pore size increases with temperature.

Original language	English
Pages (from-to)	7082-7087
Journal	Chemistry of Materials
Volume	28
Issue number	19
DOIs	https://doi.org/10.1021/acs.chemmater.6b03222
Publication status	Published - 11 Oct 2016
Externally published	Yes

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Publication details (e.g. title, author(s), publication statuses and dates) are captured on an “AS IS” and “AS AVAILABLE” basis at the time of record harvesting from the data source. Suggestions for further amendments or supplementary information can be sent to [email protected].

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title = "Exploring pore formation of atomic layer-deposited overlayers by in situ small- and wide-angle X-ray scattering",

abstract = "In this work, we explore the pore structure of overcoated materials by in situ synchrotron small-angle (SAXS) and wide-angle X-ray scattering (WAXS). Thin films of aluminum oxide (Al2O3) and titanium dioxide (TiO2) with thicknesses of 4.9 and 2.5 nm, respectively, are prepared by atomic layer deposition (ALD) on nonporous nanoparticles. In situ X-ray measurements reveal that porosity is induced in the ALD films by annealing the samples at high temperatures. Moreover, this pore formation can be attributed to densification resulting from an amorphous to crystalline phase transition of the ALD films as confirmed by high-resolution X-ray diffraction and the pair distribution function. Simultaneous SAXS and WAXS results show not only that the porosity is formed by the phase transition but also that the pore size increases with temperature.",

author = "Tao Li and Saurabh Karwal and Bachir Aoun and Haiyan Zhao and Yang Ren and Canlas, \{Christian P.\} and Elam, \{Jeffrey W.\} and Winans, \{Randall E.\}",

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doi = "10.1021/acs.chemmater.6b03222",

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T1 - Exploring pore formation of atomic layer-deposited overlayers by in situ small- and wide-angle X-ray scattering

AU - Li, Tao

AU - Karwal, Saurabh

AU - Aoun, Bachir

AU - Zhao, Haiyan

AU - Ren, Yang

AU - Canlas, Christian P.

AU - Elam, Jeffrey W.

AU - Winans, Randall E.

N1 - Publication details (e.g. title, author(s), publication statuses and dates) are captured on an “AS IS” and “AS AVAILABLE” basis at the time of record harvesting from the data source. Suggestions for further amendments or supplementary information can be sent to [email protected].

PY - 2016/10/11

Y1 - 2016/10/11

N2 - In this work, we explore the pore structure of overcoated materials by in situ synchrotron small-angle (SAXS) and wide-angle X-ray scattering (WAXS). Thin films of aluminum oxide (Al2O3) and titanium dioxide (TiO2) with thicknesses of 4.9 and 2.5 nm, respectively, are prepared by atomic layer deposition (ALD) on nonporous nanoparticles. In situ X-ray measurements reveal that porosity is induced in the ALD films by annealing the samples at high temperatures. Moreover, this pore formation can be attributed to densification resulting from an amorphous to crystalline phase transition of the ALD films as confirmed by high-resolution X-ray diffraction and the pair distribution function. Simultaneous SAXS and WAXS results show not only that the porosity is formed by the phase transition but also that the pore size increases with temperature.

AB - In this work, we explore the pore structure of overcoated materials by in situ synchrotron small-angle (SAXS) and wide-angle X-ray scattering (WAXS). Thin films of aluminum oxide (Al2O3) and titanium dioxide (TiO2) with thicknesses of 4.9 and 2.5 nm, respectively, are prepared by atomic layer deposition (ALD) on nonporous nanoparticles. In situ X-ray measurements reveal that porosity is induced in the ALD films by annealing the samples at high temperatures. Moreover, this pore formation can be attributed to densification resulting from an amorphous to crystalline phase transition of the ALD films as confirmed by high-resolution X-ray diffraction and the pair distribution function. Simultaneous SAXS and WAXS results show not only that the porosity is formed by the phase transition but also that the pore size increases with temperature.

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U2 - 10.1021/acs.chemmater.6b03222

DO - 10.1021/acs.chemmater.6b03222

M3 - RGC 21 - Publication in refereed journal

SN - 0897-4756

VL - 28

SP - 7082

EP - 7087

JO - Chemistry of Materials

JF - Chemistry of Materials

IS - 19

ER -

Exploring pore formation of atomic layer-deposited overlayers by in situ small- and wide-angle X-ray scattering

Abstract

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