Hostname: page-component-586b7cd67f-dlnhk Total loading time: 0 Render date: 2024-11-23T05:57:50.042Z Has data issue: false hasContentIssue false
  • English
  • Français

Preparation of a nanostructured organoceramic and its reversible interlayer expansion

Published online by Cambridge University Press:  31 January 2011

Phillip B. Messersmith ,
Paul Osenar  and
Samuel I. Stupp
Phillip B. Messersmith
Affiliation:
Division of Biological Materials and Department of Biomedical Engineering, Northwestern University, Chicago, Illinois 60611
Paul Osenar
Affiliation:
Department of Materials Science and Engineering and The Beckman Institute for Advanced Science and Technology, University of Illinois at Urbana-Champaign, Urbana, Illinois 61801
Samuel I. Stupp*
Affiliation:
Departments of Materials Science and Engineering and Chemistry, Materials Research Laboratory, and The Beckman Institute for Advanced Science and Technology, University of Illinois at Urbana-Champaign, Urbana, Illinois 61801
*
a)Address all correspondence to this author.
Get access

Abstract

We described previously the liquid phase synthesis and characterization of a nanostructured composite from an aqueous solution containing organic polymer and inorganic ions [J. Mater. Res. 7, 2599 (1992)]. The nanocomposite, termed an organoceramic, consisted of poly(vinyl alcohol) chains intercalated between the principal layers of a hydrated calcium aluminate ceramic. A key structural feature of the organoceramic is the polymer-induced expansion of the interlayer spacing by approximately 10 Å compared to the unmodified ceramic. In this paper, we describe the synthetic scheme that favors organoceramic formation and prove the existence of intercalated polymer by observation of reversible interlayer expansion and contraction in response to changes in ambient humidity. This property is unique to the organoceramic and is not observed in the unmodified calcium aluminate ceramic.

Type
Articles
Information
Journal of Materials Research , Volume 14 , Issue 2 , February 1999 , pp. 315 - 318
Copyright
Copyright © Materials Research Society 1999

Access options

Get access to the full version of this content by using one of the access options below. (Log in options will check for institutional or personal access. Content may require purchase if you do not have access.)

References

REFERENCES

1. For a recent review, see Giannelis, E. P., Adv. Mater. 8, 29 (1996).CrossRefGoogle Scholar
2.Blumstein, A., J. Polym. Sci., Part A 3, 2653 (1965).Google Scholar
3.Kato, C., Kuroda, K., and Misawa, M., Clays Clay Miner. 27, 129 (1979).CrossRefGoogle Scholar
4.Mehrotra, V. and Giannelis, E. P., Solid State Commun. 77, 155 (1991).CrossRefGoogle Scholar
5.Messersmith, P. B. and Giannelis, E. P., Chem. Mater. 5, 1064 (1993).CrossRefGoogle Scholar
6.Usuki, A., Kojima, Y., Kawasumi, M., Okada, A., Fukushima, Y., Kurauchi, T., and Kamigaito, O., J. Mater. Res. 8, 1179 (1993).CrossRefGoogle Scholar
7.Messersmith, P. B. and Giannelis, E. P., Chem. Mater. 6, 1719 (1994).CrossRefGoogle Scholar
8.Wang, M. S. and Pinnavaia, T.J., Chem. Mater. 6, 468 (1994).CrossRefGoogle Scholar
9.Wang, Z., Lan, T., and Pinnavaia, T. J., Chem. Mater. 8, 2200 (1996).CrossRefGoogle Scholar
10.Vaia, R. A., Ishii, H., and Giannelis, E. P., Chem. Mater. 5, 1694 (1993).CrossRefGoogle Scholar
11.Stupp, S. I. and Ciegler, G. W., J. Biomed. Mater. Res. 26, 169–183 (1992).CrossRefGoogle Scholar
12.Messersmith, P. B. and Stupp, S. I., J. Mater. Res. 7, 2599 (1992).CrossRefGoogle Scholar
13.Messersmith, P. B. and Stupp, S. I., Chem. Mater. 7, 454 (1995).CrossRefGoogle Scholar
14.Messersmith, P. B. and Stupp, S. I., Polym. Prepr. 32, 536 (1991).Google Scholar
15.Messersmith, P. B. and Stupp, S. I., in Advanced Cementitious Systems: Mechanisms and Properties, edited by Glasser, F.P., McCarthy, G. J., Young, J. F., Mason, T. O., and Pratt, P. L. (Mater. Res. Soc. Symp. Proc. 245, Pittsburgh, PA, 1992), p. 191.Google Scholar
16.Messersmith, P. B., Ph.D. Thesis, University of Illinois (1993).Google Scholar
17.Becze, C. E. and Xu, G., J. Mater. Res. 12, 566 (1997).CrossRefGoogle Scholar
18. A saturated calcium hydroxide solution was prepared by stirring excess CaO (99.9%, Aldrich) in de-ionized water at 5 °C for 1 h and then filtering to remove undissolved material. PVA (99.7% hydrolyzed, Mn= 61,000, PolySciences) was dissolved in a small amount of de-ionized water and added to the filtered Ca(OH)2 solution. A second solution containing Ca and Al ions was prepared by stirring 5 g of monocalcium aluminate (CaAl2O4, 99.99%, Alfa Chemicals) in 500 ml de-ionized water for 90 min at room temperature and then removing undissolved solids by filtration. The PVA concentration was 100 mM with respect to the total precipitation volume. After cooling both solutions to 5 °C and purging with N2, 1 part of the Ca/Al solution was transferred via cannula into 5 parts of stirred Ca(OH)2/PVA solution. Precipitation began to occur within minutes after the start of transfer and was allowed to continue to completion (—24 h). Organoceramic was isolated from the reaction mixture by centrifuging and decanting the supernatant, followed by washing and deionized water and acetone prior to drying in vacuo. Dry powders were stored over CaSO4 at 5 °C.Google Scholar
19.Turriziani, R., in The Chemistry of Cements, edited by Taylor, H.F.W (Academic Press, New York, 1964), pp. 233–286.Google Scholar
20. Becze and Xu17 used both a different solids/water ratio as well as an extended mixing time (3–5 h) compared to our preparation of the supersaturated calcium aluminate solution.Google Scholar
21. Powders were stored in sealed containers above saturated aqueous salt solutions as follows: BaCl2 (90.0% RH); NaCl (75.3% RH); NaBr (57.6% RH); NaOH (8.2% RH); P2O5 (0% RH).Google Scholar
22.Taylor, H.F.W., Miner. Mag. 39, 377 (1973).CrossRefGoogle Scholar