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Influence of Silica Nanoparticles on the Crystallization Behavior of and Proton Relaxation in Cesium Hydrogen Sulfate

Kislitsyn, Mikhail and Haile, Sossina M. (2010) Influence of Silica Nanoparticles on the Crystallization Behavior of and Proton Relaxation in Cesium Hydrogen Sulfate. Chemistry of Materials, 22 (8). pp. 2417-2426. ISSN 0897-4756. https://resolver.caltech.edu/CaltechAUTHORS:20100607-083648823

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Abstract

The influence of nanoparticulate SiO_2 on the crystallization behavior of CsHSO_4 from aqueous solution has been quantitatively evaluated using powder X-ray diffraction (XRD) and ^1H magic angle spinning nuclear magnetic resonance (NMR) spectroscopy. It is shown that SiO_2 induces amorphization of a portion of CsHSO_4 and crystallization of the otherwise metastable phase II form of CsHSO_4. The fraction of amorphized CsHSO_4 (as determined from an evaluation of the XRD peak intensity) was found to increase from 0% in the absence of SiO_2 to fully amorphized in the presence of 90 mol % (~70 wt %) SiO_2. Within the crystalline portion of the composites, the weight fraction of CsHSO_4 phase III was observed to fall almost monotonically from 100% in the absence of SiO_2 to about 40% in the presence of 70 mol % SiO_2 (from both XRD and NMR analysis). These results suggest a crystallization pathway in which SiO_2 particles incorporate an amorphous coating of CsHSO_(4-)like material and are covered by nanoparticulate CsHSO_(4-II), which coexists with independently nucleated particles of CsHSO_(4-III). In composites with small molar fractions of CsHSO_4, the entirety of the acid salt is consumed in the amorphous region. At high CsHSO_4 content, the extent of amorphization becomes negligible, as does the extent of crystallization in metastable phase II. The phase distribution was found to be stable for over 1 year, indicating the strength of the stabilization effect that SiO_2 has on phase II of CsHSO_4.


Item Type:Article
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URLURL TypeDescription
http://dx.doi.org/10.1021/cm9031495DOIArticle
http://pubs.acs.org/doi/abs/10.1021/cm9031495PublisherArticle
ORCID:
AuthorORCID
Haile, Sossina M.0000-0002-5293-6252
Additional Information:© 2010 American Chemical Society. Received March 27, 2009. Revised Manuscript Received February 6, 2010. The authors gratefully acknowledge support from the National Science Foundation (Grant DMR- 0435221) and via the Caltech Center for the Science and Engineering of Materials (Grant DMR-0520565). Dr. Sonjong Hwang of the California Institute of Technology has kindly assisted with the acquisition of NMR data. We also thank Dr. Clare Grey of SUNY Stonybrook for valuable discussions.
Funders:
Funding AgencyGrant Number
NSFDMR-0435221
NSFDMR-0520565
Issue or Number:8
Record Number:CaltechAUTHORS:20100607-083648823
Persistent URL:https://resolver.caltech.edu/CaltechAUTHORS:20100607-083648823
Official Citation:Influence of Silica Nanoparticles on the Crystallization Behavior of and Proton Relaxation in Cesium Hydrogen Sulfate Mikhail Kislitsyn and Sossina M. Haile pp 2417–2426 DOI: 10.1021/cm9031495
Usage Policy:No commercial reproduction, distribution, display or performance rights in this work are provided.
ID Code:18576
Collection:CaltechAUTHORS
Deposited By: Ruth Sustaita
Deposited On:07 Jun 2010 22:26
Last Modified:03 Oct 2019 01:44

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