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Title: Utilizing TiO2 amorphous precursors for polymorph selection: An in situ TEM study of phase formation and kinetics

Abstract

Selective synthesis of metastable polymorphs requires a fundamental understanding of the complex energy landscapes in which these phases form. Recently, the development of in situ high temperature and controlled atmosphere transmission electron microscopy has enabled the direct observation of nucleation, growth, and phase transformations with near atomic resolution. In this work, we directly observe the crystallization behavior of amorphous TiO2 thin films grown under different pulsed laser deposition conditions and quantify the mechanisms behind metastable crystalline polymorph stabilization. Films deposited at 10 mTorr chamber oxygen pressure crystallize into nanocrystalline Anatase at 325 degrees C, whereas films deposited at 2 mTorr crystallize into significantly larger needle-like grains of Brookite and Anatase at 270 degrees C. Increasing film deposition rate by a factor of 4 results in a 10x increase in the crystalline growth front velocity as well as a decrease in crystallization temperature from 270 degrees C to 225 degrees C. Engineering the amorphous precursor state through deposition conditions therefore provides routes to microstructure control and the accessibility of higher energy metastable phases.

Authors:
ORCiD logo [1];  [2]; ORCiD logo [2]; ORCiD logo [1]
+ Show Author Affiliations
  1. Colorado School of Mines, Golden, CO (United States)
  2. National Renewable Energy Lab. (NREL), Golden, CO (United States)
Publication Date:
Research Org.:
Energy Frontier Research Centers (EFRC) (United States). Center for Next Generation of Materials by Design: Incorporating Metastability (CNGMD); National Renewable Energy Lab. (NREL), Golden, CO (United States)
Sponsoring Org.:
USDOE Office of Science (SC), Basic Energy Sciences (BES)
OSTI Identifier:
1598127
Alternate Identifier(s):
OSTI ID: 1580635
Report Number(s):
NREL/JA-5F00-75989
Journal ID: ISSN 0002-7820
Grant/Contract Number:  
AC36-08GO28308; AC3608GO28308
Resource Type:
Accepted Manuscript
Journal Name:
Journal of the American Ceramic Society
Additional Journal Information:
Journal Volume: 103; Journal Issue: 4; Journal ID: ISSN 0002-7820
Publisher:
American Ceramic Society
Country of Publication:
United States
Language:
English
Subject:
36 MATERIALS SCIENCE; amorphous; crystals/crystallization; thin films; titanium dioxide

Citation Formats

Mangum, John S., Garten, Lauren M., Ginley, David S., and Gorman, Brian P. Utilizing TiO2 amorphous precursors for polymorph selection: An in situ TEM study of phase formation and kinetics. United States: N. p., 2019. Web. doi:10.1111/jace.16965.
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Mangum, John S., Garten, Lauren M., Ginley, David S., & Gorman, Brian P. Utilizing TiO2 amorphous precursors for polymorph selection: An in situ TEM study of phase formation and kinetics. United States. doi:https://doi.org/10.1111/jace.16965
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Mangum, John S., Garten, Lauren M., Ginley, David S., and Gorman, Brian P. Fri . "Utilizing TiO2 amorphous precursors for polymorph selection: An in situ TEM study of phase formation and kinetics". United States. doi:https://doi.org/10.1111/jace.16965. https://www.osti.gov/servlets/purl/1598127.
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@article{osti_1598127,
title = {Utilizing TiO2 amorphous precursors for polymorph selection: An in situ TEM study of phase formation and kinetics},
author = {Mangum, John S. and Garten, Lauren M. and Ginley, David S. and Gorman, Brian P.},
abstractNote = {Selective synthesis of metastable polymorphs requires a fundamental understanding of the complex energy landscapes in which these phases form. Recently, the development of in situ high temperature and controlled atmosphere transmission electron microscopy has enabled the direct observation of nucleation, growth, and phase transformations with near atomic resolution. In this work, we directly observe the crystallization behavior of amorphous TiO2 thin films grown under different pulsed laser deposition conditions and quantify the mechanisms behind metastable crystalline polymorph stabilization. Films deposited at 10 mTorr chamber oxygen pressure crystallize into nanocrystalline Anatase at 325 degrees C, whereas films deposited at 2 mTorr crystallize into significantly larger needle-like grains of Brookite and Anatase at 270 degrees C. Increasing film deposition rate by a factor of 4 results in a 10x increase in the crystalline growth front velocity as well as a decrease in crystallization temperature from 270 degrees C to 225 degrees C. Engineering the amorphous precursor state through deposition conditions therefore provides routes to microstructure control and the accessibility of higher energy metastable phases.},
doi = {10.1111/jace.16965},
journal = {Journal of the American Ceramic Society},
number = 4,
volume = 103,
place = {United States},
year = {2019},
month = {12}
}
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DOI:  https://doi.org/10.1111/jace.16965
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I General Theory<span class="fa fa-external-link" aria-hidden="true"></span></a> <small class="text-muted" style="text-transform:uppercase; font-size:0.75rem;"><br/> <span class="type">journal</span>, <span class="date" data-date="1939-12-01">December 1939</span></small> </h2> <ul class="small references-list" style="list-style-type:none; margin-top: 0.5em; padding-left: 0; line-height:1.8em;"> <li> <span style="color:#5C7B2D;"> Avrami, Melvin</span> </li> <li> The Journal of Chemical Physics, Vol. 7, Issue 12, p. 1103-1112</li> <li> <span class="text-muted related-url">DOI: <a href="https://doi.org/10.1063/1.1750380" class="text-muted" target="_blank" rel="noopener noreferrer">10.1063/1.1750380<span class="fa fa-external-link" aria-hidden="true"></span></a></span> </li> </ul> <hr/> </div> <div> <h2 class="title" style="margin-bottom:0;" data-apporder=""> <a href="https://doi.org/10.1016/j.scriptamat.2016.07.010" target="_blank" rel="noopener noreferrer" class="name">Thin film phase transformation kinetics: From theory to experiment<span class="fa fa-external-link" aria-hidden="true"></span></a> <small class="text-muted" style="text-transform:uppercase; font-size:0.75rem;"><br/> <span class="type">journal</span>, <span class="date" data-date="2016-11-01">November 2016</span></small> </h2> <ul class="small references-list" style="list-style-type:none; margin-top: 0.5em; padding-left: 0; line-height:1.8em;"> <li> <span style="color:#5C7B2D;"> Moghadam, M. M.; Voorhees, P. W.</span> </li> <li> Scripta Materialia, Vol. 124</li> <li> <span class="text-muted related-url">DOI: <a href="https://doi.org/10.1016/j.scriptamat.2016.07.010" class="text-muted" target="_blank" rel="noopener noreferrer">10.1016/j.scriptamat.2016.07.010<span class="fa fa-external-link" aria-hidden="true"></span></a></span> </li> </ul> <hr/> </div> <div> <h2 class="title" style="margin-bottom:0;" data-apporder=""> <a href="https://doi.org/10.1007/s10853-012-6465-4" target="_blank" rel="noopener noreferrer" class="name">Tartaric acid-assisted preparation and photocatalytic performance of titania nanoparticles with controllable phases of anatase and brookite<span class="fa fa-external-link" aria-hidden="true"></span></a> <small class="text-muted" style="text-transform:uppercase; font-size:0.75rem;"><br/> <span class="type">journal</span>, <span class="date" data-date="2012-04-17">April 2012</span></small> </h2> <ul class="small references-list" style="list-style-type:none; margin-top: 0.5em; padding-left: 0; line-height:1.8em;"> <li> <span style="color:#5C7B2D;"> Shen, Xiaojun; Zhang, Jinlong; Tian, Baozhu</span> </li> <li> Journal of Materials Science, Vol. 47, Issue 15</li> <li> <span class="text-muted related-url">DOI: <a href="https://doi.org/10.1007/s10853-012-6465-4" class="text-muted" target="_blank" rel="noopener noreferrer">10.1007/s10853-012-6465-4<span class="fa fa-external-link" aria-hidden="true"></span></a></span> </li> </ul> <hr/> </div> <div> <h2 class="title" style="margin-bottom:0;" data-apporder=""> <a href="https://doi.org/10.1107/S0021889809013727" target="_blank" rel="noopener noreferrer" class="name">Determination of the degree of preferred orientation within the March–Dollase approach<span class="fa fa-external-link" aria-hidden="true"></span></a> <small class="text-muted" style="text-transform:uppercase; font-size:0.75rem;"><br/> <span class="type">journal</span>, <span class="date" data-date="2009-05-15">May 2009</span></small> </h2> <ul class="small references-list" style="list-style-type:none; margin-top: 0.5em; padding-left: 0; line-height:1.8em;"> <li> <span style="color:#5C7B2D;"> Zolotoyabko, Emil</span> </li> <li> Journal of Applied Crystallography, Vol. 42, Issue 3</li> <li> <span class="text-muted related-url">DOI: <a href="https://doi.org/10.1107/S0021889809013727" class="text-muted" target="_blank" rel="noopener noreferrer">10.1107/S0021889809013727<span class="fa fa-external-link" aria-hidden="true"></span></a></span> </li> </ul> <hr/> </div> <div> <h2 class="title" style="margin-bottom:0;" data-apporder=""> <a href="https://doi.org/10.1002/(SICI)1521-4095(200001)12:1<38::AID-ADMA38>3.0.CO;2-I" target="_blank" rel="noopener noreferrer" class="name">Formation of High-Magnesian Calcites via an Amorphous Precursor Phase: Possible Biological Implications<span class="fa fa-external-link" aria-hidden="true"></span></a> <small class="text-muted" style="text-transform:uppercase; font-size:0.75rem;"><br/> <span class="type">journal</span>, <span class="date" data-date="2000-01-01">January 2000</span></small> </h2> <ul class="small references-list" style="list-style-type:none; margin-top: 0.5em; padding-left: 0; line-height:1.8em;"> <li> <span style="color:#5C7B2D;"> Raz, S.; Weiner, S.; Addadi, L.</span> </li> <li> Advanced Materials, Vol. 12, Issue 1, p. 38-42</li> <li> <span class="text-muted related-url">DOI: <a href="https://doi.org/10.1002/(SICI)1521-4095(200001)12:1<38::AID-ADMA38>3.0.CO;2-I" class="text-muted" target="_blank" rel="noopener noreferrer">10.1002/(SICI)1521-4095(200001)12:1<38::AID-ADMA38>3.0.CO;2-I<span class="fa fa-external-link" aria-hidden="true"></span></a></span> </li> </ul> <hr/> </div> <div> <h2 class="title" style="margin-bottom:0;" data-apporder=""> <a href="https://doi.org/10.1063/1.1415544" target="_blank" rel="noopener noreferrer" class="name">Highly conductive and transparent aluminum-doped zinc oxide thin films prepared by pulsed laser deposition in oxygen ambient<span class="fa fa-external-link" aria-hidden="true"></span></a> <small class="text-muted" style="text-transform:uppercase; font-size:0.75rem;"><br/> <span class="type">journal</span>, <span class="date" data-date="2001-12-01">December 2001</span></small> </h2> <ul class="small references-list" style="list-style-type:none; margin-top: 0.5em; padding-left: 0; line-height:1.8em;"> <li> <span style="color:#5C7B2D;"> Singh, A. 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M.; Buthrath, Nuttawuth</span> </li> <li> Journal of Applied Physics, Vol. 90, Issue 11</li> <li> <span class="text-muted related-url">DOI: <a href="https://doi.org/10.1063/1.1415544" class="text-muted" target="_blank" rel="noopener noreferrer">10.1063/1.1415544<span class="fa fa-external-link" aria-hidden="true"></span></a></span> </li> </ul> <hr/> </div> <div> <h2 class="title" style="margin-bottom:0;" data-apporder=""> <a href="https://doi.org/10.1021/cm9023887" target="_blank" rel="noopener noreferrer" class="name">Novel Metastable Hexagonal MoO <sub>3</sub> Nanobelts: Synthesis, Photochromic, and Electrochromic Properties<span class="fa fa-external-link" aria-hidden="true"></span></a> <small class="text-muted" style="text-transform:uppercase; font-size:0.75rem;"><br/> <span class="type">journal</span>, <span class="date" data-date="2009-12-08">December 2009</span></small> </h2> <ul class="small references-list" style="list-style-type:none; margin-top: 0.5em; padding-left: 0; line-height:1.8em;"> <li> <span style="color:#5C7B2D;"> Zheng, Lei; Xu, Yang; Jin, Dong</span> </li> <li> Chemistry of Materials, Vol. 21, Issue 23</li> <li> <span class="text-muted related-url">DOI: <a href="https://doi.org/10.1021/cm9023887" class="text-muted" target="_blank" rel="noopener noreferrer">10.1021/cm9023887<span class="fa fa-external-link" aria-hidden="true"></span></a></span> </li> </ul> <hr/> </div> <div> <h2 class="title" style="margin-bottom:0;" data-apporder=""> <a href="https://doi.org/10.1557/JMR.2002.0077" target="_blank" rel="noopener noreferrer" class="name">Nitrogen Effects on Crystallization Kinetics of Amorphous TiO <sub> <em>x</em> </sub> N <sub> <em>y</em> </sub> Thin Films<span class="fa fa-external-link" aria-hidden="true"></span></a> <small class="text-muted" style="text-transform:uppercase; font-size:0.75rem;"><br/> <span class="type">journal</span>, <span class="date" data-date="2002-03-01">March 2002</span></small> </h2> <ul class="small references-list" style="list-style-type:none; margin-top: 0.5em; padding-left: 0; line-height:1.8em;"> <li> <span style="color:#5C7B2D;"> Hukari, Kyle; Dannenberg, Rand; Stach, E. A.</span> </li> <li> Journal of Materials Research, Vol. 17, Issue 3</li> <li> <span class="text-muted related-url">DOI: <a href="https://doi.org/10.1557/JMR.2002.0077" class="text-muted" target="_blank" rel="noopener noreferrer">10.1557/JMR.2002.0077<span class="fa fa-external-link" aria-hidden="true"></span></a></span> </li> </ul> <hr/> </div> <div> <h2 class="title" style="margin-bottom:0;" data-apporder=""> <a href="https://doi.org/10.1111/j.1151-2916.2000.tb01150.x" target="_blank" rel="noopener noreferrer" class="name">Crystallization of Amorphous Precursors in the CalciaAlumina System: A Differential Scanning Calorimetry Study<span class="fa fa-external-link" aria-hidden="true"></span></a> <small class="text-muted" style="text-transform:uppercase; font-size:0.75rem;"><br/> <span class="type">journal</span>, <span class="date" data-date="2000-01-01">January 2000</span></small> </h2> <ul class="small references-list" style="list-style-type:none; margin-top: 0.5em; padding-left: 0; line-height:1.8em;"> <li> <span style="color:#5C7B2D;"> Douy, Andr; Gervais, Monique</span> </li> <li> Journal of the American Ceramic Society, Vol. 83, Issue 1</li> <li> <span class="text-muted related-url">DOI: <a href="https://doi.org/10.1111/j.1151-2916.2000.tb01150.x" class="text-muted" target="_blank" rel="noopener noreferrer">10.1111/j.1151-2916.2000.tb01150.x<span class="fa fa-external-link" aria-hidden="true"></span></a></span> </li> </ul> <hr/> </div> </div> <div class="pagination-container small"> <a class="pure-button prev page" href="#" rel="prev"><span class="fa fa-angle-left"></span></a><ul class="pagination d-inline-block" style="padding-left:.2em;"></ul><a class="pure-button next page" href="#" rel="next"><span class="fa fa-angle-right"></span></a> </div> </div> </div> <div class="col-sm-3 order-sm-3"> <ul class="nav nav-stacked"> <li class="active"><a href="" class="reference-type-filter tab-nav" data-tab="biblio-references" data-filter="type" data-pattern="*"><span class="fa fa-angle-right"></span> All References</a></li> <li class="small" style="margin-left:.75em; text-transform:capitalize;"><a href="" class="reference-type-filter tab-nav" data-tab="biblio-references" data-filter="type" data-pattern="journal"><span class="fa fa-angle-right"></span> journal<small class="text-muted"> (38)</small></a></li> </ul> <div style="margin-top:2em;"> <form class="pure-form small text-muted reference-search"> <label for="reference-search-text" class="sr-only">Search</label> <input class="search form-control pure-input-1" id="reference-search-text" placeholder="Search" style="margin-bottom:10px;" /> <fieldset> <div style="margin-left:1em; font-weight:normal; line-height: 1.6em;"><input type="radio" class="sort" name="references-sort" data-sort="name" style="position:relative;top:2px;" id="reference-search-sort-name"><label for="reference-search-sort-name" style="margin-left: .3em;">Sort by title</label></div> <div style="margin-left:1em; font-weight:normal; line-height: 1.6em;"><input type="radio" class="sort" name="references-sort" data-sort="date" data-order="desc" style="position:relative;top:2px;" id="reference-search-sort-date"><label for="reference-search-sort-date" style="margin-left: .3em;">Sort by date</label></div> </fieldset> <div class="text-left" style="margin-left:1em;"> <a href="" class="filter-clear clearfix" title="Clear filter / sort" style="font-weight:normal; float:none;">[ × clear filter / sort ]</a> </div> </form> </div> </div> </div> </section> <section id="biblio-citations" class="tab-content tab-content-sec osti-curated" data-tab="biblio"> <div class="row"> <div class="col-sm-9 order-sm-9"> <div class="padding"> <p class="lead text-muted" style="font-size: 18px; margin-top:0px;">Works referencing / citing this record:</p> <div class="list"> <div> <h2 class="title" style="margin-bottom:0;" data-apporder=""> <a href="https://doi.org/10.1063/1.5140368" target="_blank" rel="noopener noreferrer" class="name">Crystallization of TiO <sub>2</sub> polymorphs from RF-sputtered, amorphous thin-film precursors<span class="fa fa-external-link" aria-hidden="true"></span></a> <small class="text-muted" style="text-transform:uppercase; font-size:0.75rem;"><br/> <span class="type">journal</span>, <span class="date" data-date="2020-02-01">February 2020</span></small> </h2> <ul class="small references-list" style="list-style-type:none; margin-top: 0.5em; padding-left: 0; line-height:1.8em;"> <li> <span style="color:#5C7B2D;"> Agirseven, O.; Rivella, D. T.; Haggerty, J. E. S.</span> </li> <li> AIP Advances, Vol. 10, Issue 2</li> <li> <span class="text-muted related-url">DOI: <a href="https://doi.org/10.1063/1.5140368" class="text-muted" target="_blank" rel="noopener noreferrer">10.1063/1.5140368<span class="fa fa-external-link" aria-hidden="true"></span></a></span> </li> </ul> <hr/> </div> </div> <div class="pagination-container small"> <a class="pure-button prev page" href="#" rel="prev"><span class="fa fa-angle-left"></span></a><ul class="pagination d-inline-block" style="padding-left:.2em;"></ul><a class="pure-button next page" href="#" rel="next"><span class="fa fa-angle-right"></span></a> </div> </div> </div> <div class="col-sm-3 order-sm-3"> <ul class="nav nav-stacked"> <li class="active"><a href="" class="reference-type-filter tab-nav" data-filter="type" data-pattern="*"><span class="fa fa-angle-right"></span> All Cited By</a></li> <li class="small" style="margin-left:.75em; text-transform:capitalize;"><a href="" class="reference-type-filter tab-nav" data-filter="type" data-pattern="journal"><span class="fa fa-angle-right"></span> journal<small class="text-muted"> (1)</small></a></li> </ul> <div style="margin-top:2em;"> <form class="pure-form small text-muted citation-search"> <label for="citation-search-text" class="sr-only">Search</label> <input class="search form-control pure-input-1" id="citation-search-text" placeholder="Search" style="margin-bottom:10px;" /> <fieldset> <div style="margin-left:1em; font-weight:normal; line-height: 1.6em;"><input type="radio" class="sort" name="references-sort" data-sort="name" style="position:relative;top:2px;" id="citation-search-sort-name"><label for="citation-search-sort-name" style="margin-left: .3em;">Sort by title</label></div> <div style="margin-left:1em; font-weight:normal; line-height: 1.6em;"><input type="radio" class="sort" name="references-sort" data-sort="date" data-order="desc" style="position:relative;top:2px;" id="citation-search-sort-date"><label for="citation-search-sort-date" style="margin-left: .3em;">Sort by date</label></div> </fieldset> <div class="text-left" style="margin-left:1em;"> <a href="" class="filter-clear clearfix" title="Clear filter / sort" style="font-weight:normal; float:none;">[ × clear filter / sort ]</a> </div> </form> </div> </div> </div> </section> <section id="biblio-related" class="tab-content tab-content-sec " data-tab="biblio"> <div class="row"> <div class="col-sm-9 order-sm-9"> <section id="biblio-similar" class="tab-content tab-content-sec active" data-tab="related"> <div class="padding"> <p class="lead text-muted" style="font-size: 18px; margin-top:0px;">Similar Records in DOE PAGES and OSTI.GOV collections:</p> <aside> <ul class="item-list" itemscope itemtype="http://schema.org/ItemList" style="padding-left:0; list-style-type: none;"> <li> <div class="article item document" itemprop="itemListElement" itemscope itemtype="http://schema.org/WebPage"><meta itemprop="position" content="0" /><div class="item-info"> <h2 class="title" itemprop="name headline"><a href="/pages/biblio/1485571-selective-brookite-polymorph-formation-related-amorphous-precursor-state-tio2-thin-films" itemprop="url">Selective Brookite Polymorph Formation Related to the Amorphous Precursor State in TiO<sub>2</sub> Thin Films</a></h2> <div class="metadata"> <small class="text-muted" style="text-transform:uppercase;display:block;line-height:2.5em;">Journal Article</small><span class="authors"> <span class="author">Mangum, John S.</span> ; <span class="author">Agirseven, Okan</span> ; <span class="author">Haggerty, James E. S.</span> ; <span class="author">...</span> <span class="text-muted pubdata"> - Journal of Non-Crystalline Solids</span> </span> </div> <div class="abstract">A wide variety of brookite TiO<sub>2</sub> synthesis methods have been published over the past several decades, but few studies discuss the underlying mechanism that stabilizes brookite over its stable counterparts, rutile and anatase. Here in this study, we investigate of the effect of pulsed laser deposition parameters on the as-deposited amorphous precursor titania thin films, which subsequently crystallize into stable and metastable TiO<sub>2</sub> polymorphs upon annealing. We find that oxygen pressure in the deposition chamber strongly influences the non-equilibrium state of the amorphous precursor, which ultimately allows for selective polymorph formation. Rutile forms as the dominant phase at low pO<sub>2</sub><a href='#' onclick='$(this).hide().next().show().next().show();return false;' style='margin-left:10px;'>more »</a><span style='display:none;'> < 0.1 mTorr, while anatase is favored at high pO<sub>2</sub> > 5 mTorr. Brookite forms primarily at intermediate pO<sub>2</sub> (0.5-1.0 mTorr). Controlling the amorphous structure (i.e. Ti - O bonding and polyhedral arrangement) of the precursors via oxygen deficiency is therefore likely for the selective formation of crystalline TiO<sub>2</sub> polymorphs from sub-stoichiometric amorphous precursors. Lastly, directing phase selectivity by manipulating the structure and internal energy of the precursor amorphous state may have tremendous potential for synthesis of metastable crystalline phases that exhibit more desirable properties in comparison to their stable counterparts.</span><a href='#' onclick='$(this).hide().prev().hide().prev().show();return false;' style='margin-left:10px;display:none;'>« less</a></div><div class="metadata-links small clearfix text-muted" style="margin-top:15px;"> <span class="fa fa-book text-muted" aria-hidden="true"></span> Cited by 2<div class="pure-menu pure-menu-horizontal pull-right" style="width:unset;"> <ul class="pure-menu-list"> <li class="pure-menu-item"><span class="item-info-ftlink">DOI: <a class="misc doi-link " href="https://doi.org/10.1016/j.jnoncrysol.2018.10.049" target="_blank" rel="noopener" title="Link to document DOI" data-ostiid="1485571" data-product-type="Journal Article" data-product-subtype="AM" >https://doi.org/10.1016/j.jnoncrysol.2018.10.049</a></span></li> <li class="pure-menu-item"><span class="item-info-ftlink"><a class="misc fulltext-link " href="/pages/servlets/purl/1485571" title="Link to document media" target="_blank" rel="noopener" data-ostiid="1485571" data-product-type="Journal Article" data-product-subtype="AM" >Full Text Available</a></span></li> </ul> </div> </div> </div> <div class="clearfix"></div> </div> </li> <li> <div class="article item document" itemprop="itemListElement" itemscope itemtype="http://schema.org/WebPage"><meta itemprop="position" content="1" /><div class="item-info"> <h2 class="title" itemprop="name headline"><a href="/pages/biblio/1602697-crystallization-tio2-polymorphs-from-rf-sputtered-amorphous-thin-film-precursors" itemprop="url">Crystallization of TiO<sub>2</sub> polymorphs from RF-sputtered, amorphous thin-film precursors</a></h2> <div class="metadata"> <small class="text-muted" style="text-transform:uppercase;display:block;line-height:2.5em;">Journal Article</small><span class="authors"> <span class="author">Agirseven, O.</span> ; <span class="author">Rivella, D. T.</span> ; <span class="author">Haggerty, J. E. S.</span> ; <span class="author">...</span> <span class="text-muted pubdata"> - AIP Advances</span> </span> </div> <div class="abstract">Crystalline TiO<sub>2</sub> films of anatase, brookite, and rutile are reproducibly made from amorphous precursors deposited by RF magnetron sputtering, producing large-area, single phase films of uniform thickness. Sputtered amorphous TiO<sub>2</sub> precursor thin films follow the general behavior observed for amorphous precursor thin films generated by pulsed laser deposition, namely, that oxygen deficiency is necessary for the formation of brookite and rutile. We quantify the oxygen deficiency and correlate it with the long wavelength optical absorption. We find that the precursor deposition rate is also a contributing factor to phase selection and that brookite and rutile form from films deposited more<a href='#' onclick='$(this).hide().next().show().next().show();return false;' style='margin-left:10px;'>more »</a><span style='display:none;'> rapidly and anatase from films deposited more slowly. Sputtered and pulsed laser deposited amorphous precursor films prepared with similar oxygen deficiency and similar thickness result in the same final state after annealing, but the rate for sputtered precursors is slower.</span><a href='#' onclick='$(this).hide().prev().hide().prev().show();return false;' style='margin-left:10px;display:none;'>« less</a></div><div class="metadata-links small clearfix text-muted" style="margin-top:15px;"> <span class="fa fa-book text-muted" aria-hidden="true"></span> Cited by 1<div class="pure-menu pure-menu-horizontal pull-right" style="width:unset;"> <ul class="pure-menu-list"> <li class="pure-menu-item"><span class="item-info-ftlink">DOI: <a class="misc doi-link " href="https://doi.org/10.1063/1.5140368" target="_blank" rel="noopener" title="Link to document DOI" data-ostiid="1602697" data-product-type="Journal Article" data-product-subtype="AM" >https://doi.org/10.1063/1.5140368</a></span></li> <li class="pure-menu-item"><span class="item-info-ftlink"><a class="misc fulltext-link " href="/pages/servlets/purl/1602697" title="Link to document media" target="_blank" rel="noopener" data-ostiid="1602697" data-product-type="Journal Article" data-product-subtype="AM" >Full Text Available</a></span></li> </ul> </div> </div> </div> <div class="clearfix"></div> </div> </li> <li> <div class="article item document" itemprop="itemListElement" itemscope itemtype="http://schema.org/WebPage"><meta itemprop="position" content="2" /><div class="item-info"> <h2 class="title" itemprop="name headline"><a href="/biblio/282223-solid-state-diffusive-amorphization-tio-sub-zro-sub-bilayers" itemprop="url">Solid-state diffusive amorphization in TiO{sub 2}/ZrO{sub 2} bilayers</a></h2> <div class="metadata"> <small class="text-muted" style="text-transform:uppercase;display:block;line-height:2.5em;">Journal Article</small><span class="authors"> <span class="author">Shin, H</span> ; <span class="author">Agarwal, M</span> ; <span class="author">De Guire, M R</span> ; <span class="author">...</span> <span class="text-muted pubdata"> - Journal of the American Ceramic Society</span> </span> </div> <div class="abstract">Thin films of crystalline TiO{sub 2} were deposited on self-assembled organic monolayers from aqueous TiCl{sub 4} solutions at 80 C; partially crystalline ZrO{sub 2} films were deposited on top of the TiO{sub 2} layers from Zr(SO{sub 4}){sub 2} solutions at 70 C. In the absence of a ZrO{sub 2} film, the TiO{sub 2} films had the anatase structure and underwent grain coarsening on annealing at temperatures up to 800 C; in the absence of a TiO{sub 2} film, the ZrO{sub 2} films crystallized to the tetragonal polymorph at 500 C. However, the TiO{sub 2} and ZrO{sub 2} bilayers underwent solid-state<a href='#' onclick='$(this).hide().next().show().next().show();return false;' style='margin-left:10px;'>more »</a><span style='display:none;'> diffusive amorphization at 500 C, and ZrTiO{sub 4} crystallization could be observed only at temperatures of 550 C or higher. This result implies that metastable amorphous ZrTiO{sub 4} is energetically favorable compared to two-phase mixtures of crystalline TiO{sub 2} and ZrO{sub 2}, but that crystallization of ZrTiO{sub 4} involves a high activation barrier.</span><a href='#' onclick='$(this).hide().prev().hide().prev().show();return false;' style='margin-left:10px;display:none;'>« less</a></div><div class="metadata-links small clearfix text-muted" style="margin-top:15px;"> <div class="pure-menu pure-menu-horizontal pull-right" style="width:unset;"> <ul class="pure-menu-list"> <li class="pure-menu-item"><span class="item-info-ftlink">DOI: <a class="misc doi-link " href="https://doi.org/10.1111/j.1151-2916.1996.tb08023.x" target="_blank" rel="noopener" title="Link to document DOI" data-ostiid="282223" data-product-type="Journal Article" data-product-subtype="AC" >https://doi.org/10.1111/j.1151-2916.1996.tb08023.x</a></span></li> </ul> </div> </div> </div> <div class="clearfix"></div> </div> </li> <li> <div class="article item document" itemprop="itemListElement" itemscope itemtype="http://schema.org/WebPage"><meta itemprop="position" content="3" /><div class="item-info"> <h2 class="title" itemprop="name headline"><a href="/biblio/22215486-synthesis-tio-sub-thin-films-using-single-molecular-precursors-mocvd-method-dye-sensitized-solar-cells-application-study-film-growth-mechanism" itemprop="url">Synthesis of TiO{sub 2} thin films using single molecular precursors by MOCVD method for dye-sensitized solar cells application and study on film growth mechanism</a></h2> <div class="metadata"> <small class="text-muted" style="text-transform:uppercase;display:block;line-height:2.5em;">Journal Article</small><span class="authors"> <span class="author">Nam, Sang Hun</span> ; <span class="author">Hyun, Jae-Sung</span> ; <span class="author">Boo, Jin-Hyo</span> <span class="text-muted pubdata"> - Materials Research Bulletin</span> </span> </div> <div class="abstract">For dye-sensitized solar cells application, in this study, we have synthesized TiO{sub 2} thin films at deposition temperature in the range of 300–750 °C by metalorganic chemical vapor deposition (MOCVD) method. Titanium(IV) isopropoxide, (TIP, Ti(O{sup i}Pr){sub 4}) and Bis(dimethylamido)titanium diisopropoxide, (BTDIP, (Me{sub 2}N){sub 2}Ti(O{sup i}Pr){sub 2}) were used as single source precursors that contain Ti and O atoms in the same molecule, respectively. Crack-free, highly oriented TiO{sub 2} polycrystalline thin films with anatase phase were deposited on Si(1 0 0) with TIP at temperature as low as 450 °C. XRD and TED data showed that below 500 °C, the TiO{sub<a href='#' onclick='$(this).hide().next().show().next().show();return false;' style='margin-left:10px;'>more »</a><span style='display:none;'> 2} thin films were dominantly grown in the [2 1 1] direction on Si(1 0 0), whereas with increasing the deposition temperature to 700 °C, the main film growth direction was changed to [2 0 0]. Above 700 °C, however, rutile phase TiO{sub 2} thin films have only been obtained. In the case of BTDIP, on the other hand, only amorphous film was grown on Si(1 0 0) below 450 °C while a highly oriented anatase TiO{sub 2} film in the [2 0 0] direction was obtained at 500 °C. With further increasing deposition temperatures over 600 °C, the main film growth direction shows a sequential change from rutile [1 0 1] to rutile [4 0 0], indicating a possibility of getting single crystalline TiO{sub 2} film with rutile phase. This means that the precursor together with deposition temperature can be one of important parameters to influence film growth direction, crystallinity as well as crystal structure. To investigate the CVD mechanism of both precursors in detail, temperature dependence of growth rate was also carried out, and we then obtained different activation energy of deposition to be 77.9 and 55.4 kJ/mol for TIP and BTDIP, respectively. Also, we are tested some TiO{sub 2} film synthesized with BTDIP precursor to apply dye-sensitized solar cell.</span><a href='#' onclick='$(this).hide().prev().hide().prev().show();return false;' style='margin-left:10px;display:none;'>« less</a></div><div class="metadata-links small clearfix text-muted" style="margin-top:15px;"> <div class="pure-menu pure-menu-horizontal pull-right" style="width:unset;"> <ul class="pure-menu-list"> <li class="pure-menu-item"><span class="item-info-ftlink">DOI: <a class="misc doi-link " href="https://doi.org/10.1016/J.MATERRESBULL.2012.04.039" target="_blank" rel="noopener" title="Link to document DOI" data-ostiid="22215486" data-product-type="Journal Article" data-product-subtype="AC" >https://doi.org/10.1016/J.MATERRESBULL.2012.04.039</a></span></li> </ul> </div> </div> </div> <div class="clearfix"></div> </div> </li> <li> <div class="article item document" itemprop="itemListElement" itemscope itemtype="http://schema.org/WebPage"><meta itemprop="position" content="4" /><div class="item-info"> <h2 class="title" itemprop="name headline"><a href="/pages/biblio/1388336-interfacial-stabilization-metastable-tio2-films" itemprop="url">Interfacial Stabilization of Metastable TiO<sub>2</sub> Films</a></h2> <div class="metadata"> <small class="text-muted" style="text-transform:uppercase;display:block;line-height:2.5em;">Journal Article</small><span class="authors"> <span class="author">Gregory, Daniel G.</span> ; <span class="author">Lu, Li</span> ; <span class="author">Kiely, Christopher J.</span> ; <span class="author">...</span> <span class="text-muted pubdata"> - Journal of Physical Chemistry. C</span> </span> </div> <div class="abstract">This work demonstrates a phenomenon that preserves the traditionally metastable anatase crystal structure of thin titania (TiO<sub>2</sub>) films along a two-dimensional oxide interface at temperatures well in excess of those that normally trigger a full polymorphic transformation to rutile in higher dimensionality crystalline powders. Whereas atomic surface mobility appears to dominate polymorph transformation processes within bulk TiO<sub>2</sub> powders, a simple reduction in dimensionality to a two-dimensional TiO<sub>2</sub> film (ca. 50–200 nm thick), supported upon a substrate, leads to a remarkable resistance to the calcination-induced anatase-to-rutile transformation. This stabilization does not appear to be specifically reliant on substrate character given its<a href='#' onclick='$(this).hide().next().show().next().show();return false;' style='margin-left:10px;'>more »</a><span style='display:none;'> persistence for TiO<sub>2</sub> films prepared on amorphous silica (SiO<sub>2</sub>) as well as crystalline TiO<sub>2</sub> substrates. Instead, interface-mediated coordination of the TiO<sub>2</sub> film with the substrate, and the inherent confinement of crystallites in two dimensions, is believed to resist polymorph transformation by mitigation of the atomic surface mobility. Furthermore, only when temperatures (i.e., >800 °C) that are conducive to bulk atomic mobilization are reached does reconstructive grain growth convert the film into the thermodynamically stable rutile crystal structure.</span><a href='#' onclick='$(this).hide().prev().hide().prev().show();return false;' style='margin-left:10px;display:none;'>« less</a></div><div class="metadata-links small clearfix text-muted" style="margin-top:15px;"> <span class="fa fa-book text-muted" aria-hidden="true"></span> Cited by 3<div class="pure-menu pure-menu-horizontal pull-right" style="width:unset;"> <ul class="pure-menu-list"> <li class="pure-menu-item"><span class="item-info-ftlink">DOI: <a class="misc doi-link " href="https://doi.org/10.1021/acs.jpcc.6b12943" target="_blank" rel="noopener" title="Link to document DOI" data-ostiid="1388336" data-product-type="Journal Article" data-product-subtype="AM" >https://doi.org/10.1021/acs.jpcc.6b12943</a></span></li> <li class="pure-menu-item"><span class="item-info-ftlink"><a class="misc fulltext-link " href="/pages/servlets/purl/1388336" title="Link to document media" target="_blank" rel="noopener" data-ostiid="1388336" data-product-type="Journal Article" data-product-subtype="AM" >Full Text Available</a></span></li> </ul> </div> </div> </div> <div class="clearfix"></div> </div> </li> </ul> </aside> </div> </section> </div> <div class="col-sm-3 order-sm-3"> <ul class="nav nav-stacked"> <li class="active"><a class="tab-nav disabled" data-tab="related" style="color: #636c72 !important; opacity: 1;"><span class="fa fa-angle-right"></span> Similar Records</a></li> </ul> </div> </div> </section> </div></div> </div> </div> </section> <footer class="" style="background-color:#f9f9f9; /* padding-top: 0.5rem; */"> <div class="footer-minor"> <div class="container"> <hr class="footer-separator" /> <div class="text-center" style="margin-top:1.25rem;"> <div class="pure-menu pure-menu-horizontal"> <ul class="pure-menu-list" id="footer-org-menu"> <li class="pure-menu-item"> <a href="https://energy.gov" target="_blank" rel="noopener noreferrer"> <img src="data:image/gif;base64,R0lGODlhAQABAIAAAP///wAAACH5BAEAAAAALAAAAAABAAEAAAICRAEAOw==" class="sprite sprite-footer-us-doe-min" alt="U.S. Department of Energy" /> </a> </li> <li class="pure-menu-item"> <a href="https://www.energy.gov/science/office-science" target="_blank" rel="noopener noreferrer"> <img src="data:image/gif;base64,R0lGODlhAQABAIAAAP///wAAACH5BAEAAAAALAAAAAABAAEAAAICRAEAOw==" class="sprite sprite-footer-office-of-science-min" alt="Office of Science" /> </a> </li> <li class="pure-menu-item"> <a href="/"> <img src="data:image/gif;base64,R0lGODlhAQABAIAAAP///wAAACH5BAEAAAAALAAAAAABAAEAAAICRAEAOw==" class="sprite sprite-footer-osti-min" alt="Office of Scientific and Technical Information" /> </a> </li> </ul> </div> </div> <div class="text-center small" style="margin-top:0.5em;margin-bottom:2.0rem;"> <div class="pure-menu pure-menu-horizontal"> <ul class="pure-menu-list"> <li class="pure-menu-item"><a href="/disclaim" class="pure-menu-link"><span class="fa fa-institution"></span> Website Policies <span class="hidden-xs">/ Important Links</span></a></li> <li class="pure-menu-item"><a href="/pages/contact" class="pure-menu-link"><span class="fa fa-comments-o"></span> Contact Us</a></li> <li class="d-block d-md-none"></li> <li class="pure-menu-item"><a href="https://www.facebook.com/ostigov" target="_blank" rel="noopener noreferrer" class="pure-menu-link social"><span class="fa fa-facebook" style=""></span></a></li> <li class="pure-menu-item"><a href="https://twitter.com/OSTIgov" target="_blank" rel="noopener noreferrer" class="pure-menu-link social"><span class="fa fa-twitter" style=""></span></a></li> <li class="pure-menu-item"><a href="https://www.youtube.com/user/ostigov" target="_blank" rel="noopener noreferrer" class="pure-menu-link social"><span class="fa fa-youtube-play" style=""></span></a></li> </ul> </div> </div> </div> </div> </footer> <link href="/pages/css/pages.fonts.210415.0019.css" rel="stylesheet"> <script src="/pages/js/pages.210415.0019.js"></script><noscript></noscript> <script defer src="/pages/js/pages.biblio.210415.0019.js"></script><noscript></noscript> <script defer src="/pages/js/lity.js"></script><noscript></noscript> <script async type="text/javascript" src="/pages/js/Universal-Federated-Analytics-Min.js?agency=DOE" id="_fed_an_ua_tag"></script><noscript></noscript> </body> <!-- DOE PAGES v.210415.0019 --> </html>