The crystallization of hectorite clays as monitored by small angle X-ray scattering and NMR

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The authors have probed the 48-hr crystallization of a magnesium silicate clay called hectorite. Small angle X-ray scattering (SAXS) at the Advanced Photon Source using aliquots ex situ has revealed that data is consistent with ex situ XRD, TGA, AFM, and IR data in that all these techniques see clay crystallite beginning to form in the first few hours of reaction. Tetraethylammonium (TEA) ions are used to aid crystallization and become incorporated as the exchange cations within the interlayers. {sup 13}C NMR shows that 80% of the final TEA loading is accomplished in the first 10 hrs. {sup 29}Si NMR ... continued below

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8 p.

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Carrado, K. A.; Xu, L.; Seifert, S.; Gregory, D.; Song, K. & Botto, R. E. December 13, 1999.

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The authors have probed the 48-hr crystallization of a magnesium silicate clay called hectorite. Small angle X-ray scattering (SAXS) at the Advanced Photon Source using aliquots ex situ has revealed that data is consistent with ex situ XRD, TGA, AFM, and IR data in that all these techniques see clay crystallite beginning to form in the first few hours of reaction. Tetraethylammonium (TEA) ions are used to aid crystallization and become incorporated as the exchange cations within the interlayers. {sup 13}C NMR shows that 80% of the final TEA loading is accomplished in the first 10 hrs. {sup 29}Si NMR displays a visible clay silicate peak after just 1 hr. In addition, the first in situ study of clay crystallization of any kind was performed by in situ SAXS. Results are consistent with the ex situ data as well as showing the sensitivity of SAXS to sol gel reactions occurring on the order of minutes.

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8 p.

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OSTI as DE00750554

Medium: P; Size: 8 pages

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  • 219th American Chemical Society National Meeting, San Francisco, CA (US), 03/26/2000--03/30/2000

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  • Report No.: ANL/CHM/CP-100278A
  • Grant Number: W-31109-ENG-38
  • Office of Scientific & Technical Information Report Number: 750554
  • Archival Resource Key: ark:/67531/metadc706881

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  • December 13, 1999

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  • Sept. 12, 2015, 6:31 a.m.

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  • April 11, 2017, 3:55 p.m.

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Carrado, K. A.; Xu, L.; Seifert, S.; Gregory, D.; Song, K. & Botto, R. E. The crystallization of hectorite clays as monitored by small angle X-ray scattering and NMR, article, December 13, 1999; Illinois. (digital.library.unt.edu/ark:/67531/metadc706881/: accessed December 18, 2018), University of North Texas Libraries, Digital Library, digital.library.unt.edu; crediting UNT Libraries Government Documents Department.