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Calcium Phosphate Phase Identification Using XPS and Time-of-Flight Cluster SIMS.

C C Chusuei1, D W Goodman, M J Van Stipdonk

  • 1Department of Chemistry, Texas A&M University, P.O. Box 30012, College Station, Texas 77842-3012.

Analytical Chemistry
|June 14, 2011
PubMed
Summary
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Time-of-flight cluster static secondary ion mass spectrometry (ToF-SSIMS) effectively identifies calcium phosphate (CP) phases, even at low coverages. This technique, combined with X-ray photoelectron spectroscopy (XPS), offers a promising method for microscopic CP analysis.

Area of Science:

  • Materials Science
  • Surface Chemistry
  • Analytical Chemistry

Background:

  • Calcium phosphates (CPs) are crucial in biomaterials and geology.
  • Distinguishing between various CP phases, especially at low concentrations, is challenging with traditional methods like X-ray diffraction.
  • Microscopic analysis of CP phases is essential for understanding their properties and applications.

Purpose of the Study:

  • To evaluate the efficacy of Time-of-Flight Cluster Static Secondary Ion Mass Spectrometry (ToF-SSIMS) for identifying different calcium phosphate phases.
  • To compare the capabilities of ToF-SSIMS with X-ray diffraction (XRD) for detecting low concentrations of CPs.
  • To explore the combined use of ToF-SSIMS and X-ray Photoelectron Spectroscopy (XPS) for differentiating CP phases on surfaces.

Main Methods:

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  • Acquisition of reproducible ToF-SSIMS spectra for standard calcium phosphate powders.
  • Analysis of X-ray photoelectron spectroscopy (XPS) core levels (P 2p, Ca 2p, O 1s) and O 1s loss intensity.
  • Bombardment of samples with (CsI)Cs(+) projectiles for SIMS analysis.

Main Results:

  • ToF-SSIMS successfully identified various standard calcium phosphate phases, including α-tricalcium phosphate, β-tricalcium phosphate, amorphous calcium phosphate, octacalcium phosphate, brushite, and hydroxyapatite.
  • X-ray diffraction was unable to detect signals from microscopic amounts of CP (∼15 mmol m(-)(2)).
  • The PO(3)(-)/PO(2)(-) ratios from ToF-SSIMS, coupled with XPS data, demonstrated significant potential for differentiating between CP phases on metal oxide surfaces at microscopic levels.

Conclusions:

  • ToF-SSIMS is a powerful technique for the phase identification of calcium phosphates, outperforming XRD for trace amounts.
  • The combination of ToF-SSIMS and XPS provides a robust analytical approach for characterizing microscopic calcium phosphate coverages.
  • This methodology holds promise for applications requiring sensitive and specific analysis of calcium phosphate materials.