Hostname: page-component-78c5997874-v9fdk Total loading time: 0 Render date: 2024-11-10T10:52:26.131Z Has data issue: false hasContentIssue false

Quantitative Microanalysis of (1–x)Pb(Mg1/3Nb2/3)O3×xPbTiO3 (PMNT) Ferroelectric Ceramicsa

Published online by Cambridge University Press:  05 March 2015

Zoran Samardžija*
Affiliation:
Jožef Stefan Institute, Department for Nanostructured Materials, Jamova cesta 39, SI-1000 Ljubljana, Slovenia
*
*Corresponding author.zoran.samardzija@ijs.si
Get access

Abstract

Optimized quantitative electron-probe microanalysis was applied for compositional characterization of a ferroelectric ceramic single crystal that was made from the complex perovskite-type solid-solution (1–x)Pb(Mg1/3Nb2/3)O3×xPbTiO3 (PMNT). Cation concentrations were determined with high accuracy and ultimate relative experimental uncertainty of ≤±1%, showing that the average chemical composition of the crystal corresponds to Pb(Mg1/3Nb2/3)0.67Ti0.33O3 (i.e., x=0.33), which is close to the morphotropic phase boundary composition. Over the PMNT single crystal slight compositional heterogeneity was measured for concentrations of the perovskite B-site cations Ti4+, Mg2+, and Nb5+, with variations up to ±2.3%, whereas the Pb concentration remained uniform within a variation below ±0.5%.

Type
EMAS Special Issue
Copyright
© Microscopy Society of America 2015 

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.)

Footnotes

a

This article is intended for the Special Issue from the EMAS 2014 Workshop on Electron Probe Microanalysis of Materials TodayRare and Noble Elements: from Ore Deposits to High-tech Materials.

References

Bastin, G.F., Dijkstra, J.M. & Heijligers, H.J.M. (1998). PROZA 96: an improved matrix correction program for electron probe microanalysis based on double gaussian φ(ρz) approach. X-Ray Spectrom 27, 310.Google Scholar
Drouin, D., Couture, A.R., Joly, D., Tastet, X., Aimez, V. & Gauvin, R. (2007). CASINO V2.42 – a fast and easy-to-use modeling tool for scanning electron microscopy and microanalysis users. Scanning 29, 92101.Google Scholar
Fan, H., Zhao, L. & Tian, C. (2004). Microstructure evolution of the templated grain growth in textured Pb(Mg1/3Nb2/3)0.67Ti0.33O3 by excess PbO addition. Ferroelectrics 302, 307311.CrossRefGoogle Scholar
Goldstein, J.I., Newbury, D.E., Echlin, P., Joy, D.C., Romig, A.D., Lyman, C.E., Fiori, C. & Lifshin, E. (1992). Scanning Electron Microscopy and X-Ray Microanalysis. New York: Plenum Press.Google Scholar
Lifshin, E. & Gauvin, R. (1998). The role of Monte Carlo calculations in quantitative analysis. Microsc Microanal 4, 232233.CrossRefGoogle Scholar
Lifshin, E. & Gauvin, R. (2001). Minimizing errors in electron microprobe analysis. Microsc Microanal 7, 168177.Google Scholar
Luo, H., Xu, G., Xu, H., Wang, P. & Yin, Z. (2000). Compositional homogeneity and electrical properties of lead magnesium niobate titanate single crystals grown by a modified Bridgman technique. Jpn J Appl Phys 39, 55815585.Google Scholar
Marinenko, R. & Leigh, S. (2004). Heterogeneity evaluation of research materials for microanalysis standards certification. Microsc Microanal 10, 491506.Google Scholar
Messing, G.L., Trolier-McKinstry, S.E., Sabolsky, M., Duran, C., Kwon, S., Brahmaroutu, B., Park, P., Yilmaz, H., Rehrig, P.W., Eitel, K.B., Suvaci, E., Seabaugh, M. & Oh, K.S. (2004). Templated grain growth of textured piezoelectric ceramics. Crit Rev Solid State Mater Sci 29, 4596.Google Scholar
Park, S.E. & Shrout, T.R. (1997). Ultrahigh strain and piezoelectric behaviour in relaxor based ferroelectric single crystals. J Appl Phys 82, 18041811.Google Scholar
Scott, V. D. & Love, G. (1983). Quantitative Electron-Probe Microanalysis. New York: Willey & Sons.Google Scholar
Tu, C.S., Chen, L.F., Schmidt, V.H. & Tsai, C.L. (2001). Phases and domain structures in relaxor-based ferroelectric (PbMg1/3Nb2/3O3)0.69(PbTiO3)0.31 single crystal. Jpn J Appl Phys 40, 41184125.Google Scholar
Ye, Z.G. & Dong, M. (2000). Morphotropic domain structures and phase transitions in relaxor-based piezo-/ferroelectric (1–x)Pb(Mg1/3Nb2/3)O3-xPbTiO3 single crystals. J Appl Phys 87, 23122319.Google Scholar
Zawilski, K.T., Custodio, M.C.C., DeMattei, R.C., Lee, S.G., Monteiro, R.G., Odagawa, H. & Feigelson, R.S. (2003). Segregation during the vertical Bridgman growth of lead magnesium niobate-lead titanate single crystals. J Cryst Growth 258, 353367.Google Scholar
Ziebold, T.O. (1967). Precision and sensitivity in electron probe microanalysis. Anal Chem 39, 858861.CrossRefGoogle Scholar