Abstract
It is well known that the crystallographic phase and morphology of many materials changes with the crystal size in the tens of nanometer range and that many nanocrystals possess structural defects in excess of their equilibrium levels. A need to determine the ideal and real structure of individual nanoparticles, therefore, arises. High-resolution phase-contrast transmission electron microscopy (TEM) and atomic resolution Z-contrast scanning TEM (STEM) when combined with transmission electron goniometry offer the opportunity of develop dedicated methods for the crystallographic characterization of nanoparticles in three dimensions. This paper describes tilt strategies for taking data from individual nanocrystals “as found”, so as to provide information on their lattice structure and orientation, as well as on the structure and orientation of their surfaces and structural defects. Internet based java applets that facilitate the application of this technique for cubic crystals with calibrated tilt-rotation and double-tilt holders are mentioned briefly. The enhanced viability of image-based nanocrystallography in future aberration-corrected TEMs and STEMs is illustrated on a nanocrystal model system.
Similar content being viewed by others
References
P. Fraundorf, Determining the 3D Lattice Parameters of Nanometer-sized Single Crystals from Images, Ultramicroscopy 22, 225–230 (1987)
P. Möck, Verfahren zur Durchführung und Auswertung von elektronenmikroskopischen Untersuchungen, German patents DE 4037346 A1 and DD 301839 A7, priority date: 21 November, 1989
P. Fraundorf, Stereo Analysis of Single Crystal Electron Diffraction Data, Ultramicroscopy 6, 227–236 (1981)
P. Fraundorf, Stereo Analysis of Electron Diffraction Pattern from Known Crystals, Ultramicroscopy 7, 203–206 (1981)
P. Möck, A Direct Method for Orientation Determination Using TEM (I), Description of the Method, Cryst. Res. Technol. 26, 653–658 (1991); A Direct Method for Orientation Determination Using TEM (II), Experimental Example, Cryst. Res. Technol. 26, 797–801 (1991)
P. Möck, A Direct Method for the Determination of Orientation Relationships Using TEM, Cryst. Res. Technol. 26, 975–962 (1991)
P. Möck and W. Hoppe, ELCRYSAN - A program for direct crystallographic analyses, Proc. 10th European Conference on Electron Microscopy Vol. 1, 193–194 (1992)
P. Möck, Estimation of Crystal Textures using Electron Microscopy, Beitr. Elektronenmikroskop. Direktabb. Oberfl. 28, 31–36 (1995).
W. Prantl, A computer program for the evaluation of orientation relationships from simple electron-diffraction spot patterns, J. Appl. Cryst. 20, 439–440 (1987)
W. Prantl, A computer program for trace analyses in transmission electron microscopy, J. Appl. Cryst. 20, 440441 (1987)
C.T. Chou, Computer Software for Specimen Orientation Adjustment Using Double-Tilt or Rotation Holders, J. Electron. Microsc. Technique 7, 263–268 (1987).
W. Qin and P. Fraundorf, Lattice parameters from direct-space images at two tilts, Ultramicroscopy 94, 245–262 (2003)
W. Qin, Direct space nano(crystallography) via high-resolution Transmission Electron Microscopy, PhD thesis, University of Missouri-Rolla, 2000
R.C. Pond. Line Defects in Interfaces; in Dislocations in Solids 8, 1 (1989), ed. F.R.N. Nabarro (Elsevier)
T.V. Barker, Systematic Crystallography: An Essay on Crystal Description, Classification and identification, (Thomas Murby & Co, London, 1930)
M.W. Porter and R.C. Spiller, The Barker Index of Crystals, (W. Heffer and Sons, Cambridge, 1951)
A.K. Boldyrew, Bestimmungstabellen für Kristalle, Band I, (Leningrad, 1936)
O. Johari and Thomas G., The stereographic projection and its application (Wiley, 1969)
J.F.C. Hessel, Krystallometrie, oder Krystallonomie und Krystallographie auf eigenthümliche Weise und mit Zugrundelegung neuerer allgemeiner Lehren der reinen Gestaltenkunde, sowie mit vollständiger Berücksichtigung der wichtigsten Arbeitern und Methoden anderer Krystallographen, 1830, (Ostwald’s Klassiker der exakten Wissenschaften Nr. 88, Wilhelm Englemann, Leipzig, 1897)
V. Goldschmidt, Krystallographische Winkeltabellen, (Berlin, 1897)
E.S. Fedorow, Das Kristallreich: Tabellen zur Kristallochemischen Analyse, mit Atlas (1920)
P. Terpstra and L.W. Godd, Crystallometry, (Academic Press, New York, 1961)
X.Z. Li, JECP/SP: a computer program for generating stereographic projections, applicable to specimen orientation adjustment in TEM experiments, J. Appl. Cryst. 37 (2004) 506–507
http://www.physics.pdx.edu/~pmoeck/tilt-rotationgoniometersimulation.htm
http://www.physics.pdx.edu/~pmoeck/double/double-tiltgoniometersimulation.htm
K.J. Batenburg, Electronic notes in discrete mathematics 12 (2003), Elsevier online
C. Kisielowski, private communications
P. Moeck, M. Kapilashrami, A. Rao, K. Aldushin, J. Lee, J.E. Morris, N.D. Browning, and P.J. McCann, Nominal PbSe nano-islands on PbTe: grown by MBE, analyzed by AFM and TEM, Mat. Res. Soc. Symp. Proc. Vol. 839 (2005) P.4.3.1–P.4.3.6
P. Moeck, W. Qin, and P.B. Fraundorf, Image-based nanocrystallography in future aberration corrected transmission electron microscopes, Mat. Res. Soc. Symp. Proc. Vol. 818 (2004) M11.3.1–M11.3.6
Acknowledgments
This research was supported by an award from Research Corporation. Additional support was provided by faculty enhancement and development awards from Portland State University.
Author information
Authors and Affiliations
Corresponding author
Rights and permissions
About this article
Cite this article
Moeck, P., Qin, W. & Fraundorf, P.B. Towards 3D image-based nanocrystallography by means of transmission electron goniometry. MRS Online Proceedings Library 839, 89–94 (2004). https://doi.org/10.1557/PROC-839-P4.3
Published:
Issue Date:
DOI: https://doi.org/10.1557/PROC-839-P4.3