Atomic Force Microscopic Imaging of Biomineral Powder Samples Formed by Deposits from Ethanolic Suspensions

  • Lorraine M. Siperko
  • William J. Landis


A sample preparation method was developed that facilitates imaging of powders by force microscopy. The feasibility of the method was tested by imaging a NaC1 sample prepared in a like manner. The characteristic face-centered cubic (fcc) structure common to the sodium halide salts was apparent in NaC1 atomic scale images. A periodicity of 0.60 nm, which is within 6% of the value of the NaC1 lattice constant, was measured.

By suspending biomineral powders in ethanol and depositing an aliquot onto a suitable substrate, the images of hydroxyapatite ([Ca10(PO4)6(OH)2]) and brushite ([CaHPO4. 2H2O]) were obtained. On glass substrates, brushite formed flat platelets. Atomic spacings were found to be 0.45 nm and 0.60 nm, which agree well with published values for its <110> crystal plane. In contrast, hydroxyapatite primarily formed well-isolated clusters with atomic spacings of 0.43 nm and 0.68 nm, in agreement with published values for its <110> and <001> crystal planes, respectively.

Preliminary results indicate that substrates affect the structure of the deposits. Structural differences of the two mineral deposits on glass and mica were observed.


Atomic Force Microscopy Crystal Plane Dicalcium Phosphate Atomic Spacing Phosphate Dihydrate 
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  1. 1.
    H. Ji, P.M. Marquis, Modification of hydroxyapatite during transmission electron microscopy, J. Mat. Sei. Lett. 10: 132–134 (1991).CrossRefGoogle Scholar
  2. 2.
    W.J. Landis, J. Moradian-Oldak, S. Weiner, Topographic imaging of mineral and collagen in the calcifying turkey tendon, Connect. Tiss. Res. 25: 181–196 (1991).CrossRefGoogle Scholar
  3. 3.
    W.J. Landis, M.J. Glimcher, Electron diffraction and electron probe microanalysis of the mineral phase of bone tissue prepared by anhydrous techniques, J. Ultrastruct. Res. 63: 188–223 (1978).CrossRefGoogle Scholar
  4. 4.
    M.I. Kay, R.A. Young, A.S. Posner, Crystal structure of hydroxyapatite, Nature 204: 10501052 (1964).Google Scholar
  5. 5.
    H.C.W. Skinner, H.T. Hunt, J. Griswold, Automatic scanning and analysis of multiple-sample Guinier X-ray powder diffraction films, J. Phys. E: Sci. Instrum. 13: 74–79 (1980).CrossRefGoogle Scholar
  6. 6.
    N.A. Curry, D.W. Jones, The application of an empirical correction for absorption and secondary extinction to neutron data for crystals of brushite, CaHPO4.2H2O.Google Scholar
  7. Z. Kristallogr. 181: 205–214 (1987).CrossRefGoogle Scholar
  8. 7.
    R.H. Plovnick, Crystallization of brushite from EDTA-chelated calcium in agar gels, J. Cryst. Growth 114: 22–26 (1991).CrossRefGoogle Scholar
  9. 8.
    M. Ohta, M. Tsutsumi, The relationship between the morphology of brushite crystals grown rapidly in silica gel and its structure, J. Cryst. Growth 56: 652–658 (1981).CrossRefGoogle Scholar
  10. 9.
    M.D. Francis, N.C. Webb, Hydroxyapatite formation from a hydrated calcium monohydrogen phosphate precursor, Calc. Tiss. Res. 6: 335–342 (1971).CrossRefGoogle Scholar
  11. 10.
    L.M. Siperko, W.J. Landis, Atomic scale imaging of hydroxyapatite and brushite in air by force microscopy, Appl. Phys. Lett. 61: 2610–2612 (1992).CrossRefGoogle Scholar
  12. 11.
    Marti, B. Drake, P.K. Hansma, Atomic force microscopy of liquid-covered surfaces: Atomic resolution images, Appl. Phys. Lett. 51: 484–486 (1987).CrossRefGoogle Scholar
  13. 12.
    G. Meyer, N.M. Amer, Optical-beam-deflection atomic force microscopy: The NaC1 (001) surface. Appl. Phys. Lett. 56: 2100–2101 (1990).CrossRefGoogle Scholar
  14. 13.
    L.M. Siperko, W.J. Landis, Atomic force microscopic imaging of biologically important materials. Materials Research Society Fall Meeting, Boston, MA, November 1992 (proceedings at press).Google Scholar
  15. 14.
    C.A. Beevers, The crystal structure of dicalcium phosphate dihydrate, CaHPO4.21–120, Acta Cryst. 11: 273–277 (1958).CrossRefGoogle Scholar

Copyright information

© Springer Science+Business Media New York 1994

Authors and Affiliations

  • Lorraine M. Siperko
    • 1
  • William J. Landis
    • 2
  1. 1.IBM Microelectronics Division D675/14-3EndicottUSA
  2. 2.Harvard Medical School and Children’s Hospital Enders Bldg. Rm. 284BostonUSA

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