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Characterization of an Inorganic Cryptomelane Nanomaterial Synthesized by a Novel Process Using Transmission Electron Microscopy and X-Ray Diffraction

Published online by Cambridge University Press:  04 July 2008

Longzhou Ma ,
Thomas Hartmann ,
Marcos A. Cheney ,
Nancy R. Birkner  and
Pradip K. Bhowmik
Longzhou Ma*
Affiliation:
Harry Reid Center for Environmental Studies, University of Nevada Las Vegas, 4505 Maryland Parkway, Las Vegas, NV 89154, USA
Thomas Hartmann
Affiliation:
Harry Reid Center for Environmental Studies, University of Nevada Las Vegas, 4505 Maryland Parkway, Las Vegas, NV 89154, USA Institute of Nuclear Science and Engineering, Idaho State University, Idaho Falls, ID 83402, USA
Marcos A. Cheney
Affiliation:
Department of Health Physics, University of Nevada Las Vegas, 4505 Maryland Parkway, Las Vegas, NV 89154, USA Department of Chemistry, University of Nevada Las Vegas, 4505 Maryland Parkway, Las Vegas, NV 89154, USA
Nancy R. Birkner
Affiliation:
Department of Chemistry, University of Nevada Las Vegas, 4505 Maryland Parkway, Las Vegas, NV 89154, USA
Pradip K. Bhowmik
Affiliation:
Department of Chemistry, University of Nevada Las Vegas, 4505 Maryland Parkway, Las Vegas, NV 89154, USA
*
Corresponding author. E-mail: lma@unlv.nevada.edu
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Abstract

Layer- and tunnel-structured manganese oxide nanomaterials are important because of their potential applications in industrial catalysis. A novel soft chemistry method was developed for the synthesis of inorganic cryptomelane nanomaterials with high surface area. Bright field transmission electron microscopy (BF-TEM) and high-resolution transmission electron microscopy (HRTEM) techniques were employed to characterize this nanomaterial. A nanosized material with fibrous texture comprised of 140–160 nm striations was identified by BF-TEM imaging. HRTEM images show multiple atomic morphologies such as “helix-type,” “doughnut-like,” and tunnel structures lying on different crystallographic planes. The crystallographic parameters of this material were analyzed and measured by X-ray powder diffraction (XRD) showing that the synthesized nanomaterial is single phased and corresponds to cryptomelane with major diffraction peaks (for 10° < 2θ < 60°) at d-spacing values of 6.99, 4.94, 3.13, 2.40, 2.16, 1.84, 1.65, and 1.54 Å. A “doughnut-like” crystal structure was confirmed based on the crystallographic data. Structure and lattice parameters refinement was performed by XRD/Rietveld analysis. Simple simulation of HRTEM images and selected area diffraction patterns were applied to interpret the HRTEM images as observed.

Keywords

cryptomelaneTEMHRTEMXRD
Type
Materials Applications
Information
Microscopy and Microanalysis , Volume 14 , Issue 4 , August 2008 , pp. 328 - 334
Copyright
Copyright © Microscopy Society of America 2008

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References

REFERENCES

Cheney, M.A., Bhowmik, P.K., Moriuchi, S., Birkner, N.R., Hodge, V.F. & Elkouz, S.E. (2007). Synthesis and characterization of two phases of manganese oxide from decomposition of permanganate in concentrated sulfuric acid at ambient temperature. Colloids and Surfaces A: Physicochem Eng Aspects 307, 62–70.Google Scholar
Cheney, M.A., Birkner, N.R., Ma, L.-Z., Hartmann, T., Bhowmik, P.K., Vernon, V.F. & Steinberg, S.M. (2006). Synthesis and characterization of inorganic double helices of cryptomelane nanomaterials. Colloids and Surfaces A: Physicochem Eng Aspects 289, 185–192.Google Scholar
Ding, Y.S., Shen, Y.F., Gomez, S., Luo, H., Aindow, M. & Suib, S.L. (2006). Hydrothermal growth of manganese dioxide into three-dimensional hierarchical nanoarchitectures. Adv Func Mater 16, 549–555.Google Scholar
Ding, Y.S., Shen, X.F., Sithambaram, S., Gomez, S., Kumar, R., Crisostomo, V.M.B., Suib, S.L. & Aindow, M. (2005). Synthesis and catalytic activity of cryptomelane-type manganese dioxide nanomaterials produced by a novel solvent-free method. Chem Mater 17, 5382–5389.Google Scholar
Feng, Q., Kanoh, H. & Ooi, K. (1999). Manganese oxide porous crystals. J Mater Chem 9, 319–333.Google Scholar
Giraldo, O., Brock, S.L., Marquez, M., Suib, S.L., Hillhouse, H. & Tsapatsis, M. (2000). Spontaneous formation of inorganic helices. Nature 405, 38.Google Scholar
Rosi, N.L., Eckert, J., Eddaoudi, M., Vodak, D.T., Kim, J., O'Keeffe, M. & Yaghi, O.M. (2003). Hydrogen storage in microporous metal-organic frameworks. Science 300, 1127–1129.Google Scholar
Shen, Y.F., Ding, Y.S., Liu, J., Cai, J., Laubernds, K., Zerger, R.P., Vasiliev, A., Aindow, M. & Suib, S.L. (2005). Control of nanometer-scale tunnel sizes of porous manganese oxide octahedral molecular sieve nanomaterials. Adv Mater 17, 805–809.Google Scholar
Shen, Y.F., Zerger, R.P., DeGuzman, R., Zuib, S.L., McCurdy, L., Potter, D.I. & O'Young, G.L. (1993). Octahedral molecular sieves: Synthesis, characterization and application. Science 260, 511–515.Google Scholar
Tian, Z.R., Tong, W., Wang, J.Y., Duan, N.G., Krishnan, V.V. & Suib, S.L. (1997). Manganese oxide mesoporous structures: Mixed-valent semiconducting catalysts. Science 276, 926–930.Google Scholar
Vicat, J., Fanchon, E., Strobel, P. & Qui, D.T. (1986). The structure of potassium manganate (K1.33Mn8O16) and ordering in hollandite-type structures. Acta Crystallographia, Sect B: Struct Sci B42, 162–167.Google Scholar
Villegas, J.C., Garces, L.J, Gomes, S., Durand, J.P. & Suib, S.L. (2005). Particle size control of cryptomelane nanomaterials by use of H2O2 in acidic conditions. Chem Mater 17, 1910–1918.Google Scholar
Walanda, D.K., Geoffrey, A.L. & Donne, S.W. (2005). Hydrothermal MnO2: Synthesis, structure, morphology and discharge performance. J Power Sources 139, 325–341.Google Scholar
Wu, C.G. & Bein, T. (1994). Conducting polyaniline filaments in a mesoporous channel host. Science 264, 1757–1759.Google Scholar
Zuo, J.M. & Mabon, J.C. (2004). WebEMAPS software, University of Illinois at Urbana-Champaign. Available at: http://emaps.mrl.uiuc.edu/.Google Scholar