Hostname: page-component-cd9895bd7-mkpzs Total loading time: 0 Render date: 2024-12-28T00:34:45.116Z Has data issue: false hasContentIssue false
  • English
  • Français

Characterization of grain structure in nanocrystalline gadolinium by high-resolution transmission electron microscopy

Published online by Cambridge University Press:  31 January 2011

Martin Seyring ,
Xiaoyan Song ,
Andrey Chuvilin ,
Ute Kaiser  and
Markus Rettenmayr
Martin Seyring*
Affiliation:
Institute of Materials Science and Technology, Friedrich Schiller University, D-07747 Jena, Germany
Xiaoyan Song
Affiliation:
College of Materials Science and Engineering, Beijing University of Technology, Beijing 100022, People's Republic of China
Ute Kaiser
Affiliation:
Electron Microscopy Group of Materials Science, University of Ulm, D-89081 Ulm, Germany
Markus Rettenmayr
Affiliation:
Institute of Materials Science and Technology, Friedrich Schiller University, D-07747 Jena, Germany
*
a) Address all correspondence to this author. e-mail: martin.seyring@uni-jena.de
Get access

Abstract

A method is presented for recognition of nanograins in high-resolution transmission electron microscope (HRTEM) images of nanocrystalline materials. We suggest a numerical procedure, which is similar to the experimental dynamic hollow cone dark-field method in transmission electron microscopy and the annular dark-field method in scanning transmission electron microscopy. The numerical routine is based on moving a small mask along a circular path in the Fourier spectrum of a HRTEM image and performing at each angular step an inverse Fourier transform. The procedure extracts the amplitude from the Fourier reconstructions and generates a sum picture that is a real space map of the local amplitude. From this map, it is possible to determine both the size and shape of the nanograins that satisfy the selected Bragg conditions. The possibilities of the method are demonstrated by determining the grain size distribution in gadolinium with ultrafine nanocrystalline grains generated by spark plasma sintering.

Keywords

Grain sizeNanostructureTransmission electron microscopy (TEM)
Type
Articles
Information
Journal of Materials Research , Volume 24 , Issue 2 , February 2009 , pp. 342 - 346
Copyright
Copyright © Materials Research Society 2009

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.)

References

REFERENCES

1.Song, X.Y., Zhang, J.X., Yue, M., Li, E.D., Zeng, H., Lu, N.D., Zhou, M.L., Zuo, T.Y.: Technique for preparing ultrafine nanocrystalline bulk material of pure rare-earth metals. Adv. Mater. 18, 1210 (2006)Google Scholar
2.Li, E.D., Song, X.Y., Zhang, J.X., Lu, N.D.: Preparation and mechanism study of bulk pure rare-earth metals with amorphous and nanocrystalline structures. Chin. Sci. Bull. 52, 418 (2007)CrossRefGoogle Scholar
3.Song, X.Y., Zhang, J.X., Li, E.D., Lu, N.D., Yin, F.X.: Preparation and characterization of rare-earth bulks with controllable nanostructures. Nanotechnology 17, 5584 (2006)Google Scholar
4.Yue, M., Zhang, J.X., Zeng, H., Wang, K.J.: Preparation, microstructure, and magnetic properties of bulk nanocrystalline Gd metal. Appl. Phys. Lett. 89, 232504 (2006)Google Scholar
5.Lu, N.D., Song, X.Y., Zhang, A.X., Li, E.D.: Preparation of Nd bulk with ultrafine nanocrystalline structure and its physical property. Acta Metall. Sin. 43, 739 (2007)Google Scholar
6.Mitra, R., Ungar, T., Weertman, J.R.: Comparison of grain size measurements by x-ray diffraction and transmission electron microscopy methods. T. Indian Inst. Metals 58, 1125 (2005)Google Scholar
7.Ungar, T.: Characterization of nanocrystalline materials by x-ray line profile analysis. J. Mater. Sci. 42, 1584 (2007)Google Scholar
8.Liu, Z., Shindo, D., Ohnuma, S., Fujimori, H.: Nano-granular Co–Zr–O magnetic films studied by HRTEM and electron holography. J. Magn. Magn. Mater. 262, 308 (2003)Google Scholar
9.Karlsson, L.S., Deppert, K., Malm, J.O.: Size determination of Au aerosol nanoparticles by off-line TEM/STEM observations. J. Nanopart. Res. 8, 971 (2006)Google Scholar
10.Hytch, M.J., Gandais, M.: Quantitative criteria for the detection and characterization of nanocrystals from high-resolution electron-microscopy images. Philos. Mag. A 72, 619 (1995)Google Scholar
11.Williams, D.B., Carter, C.B.: Transmission Electron Microscopy: A Textbook for Materials Science(Plenum Press New York 1996)Google Scholar
12.Ricolleau, C., Audinet, L., Gandais, M., Gacoin, T., Boilot, J.P.: 3D morphology of II-VI semiconductor nanocrystals grown in inverted micelles. J. Cryst. Growth 203, 486 (1999)Google Scholar
13.Zghal, S., Hytch, M.J., Chevalier, J.P., Twesten, R., Wu, F., Bellon, P.: Electron microscopy nanoscale characterization of ball-milled Cu–Ag powders. Part I: Solid solution synthesized by cryo-milling. Acta Mater. 50, 4695 (2002)Google Scholar
14.Guigue-Millot, N., Begin-Colin, S., Champion, Y., Hytch, M.J., Le Caer, G., Perriat, P.: Control of grain size and morphologies of nanograined ferrites by adaptation of the synthesis route: Mechanosynthesis and soft chemistry. J. Solid State Chem. 170, 30 (2003)Google Scholar
15.Hytch, M.J.: Analysis of variations in structure from high resolution electron-microscope images by combining real space and Fourier space information. Microsc. Microanal. M. 8, 41 (1997)Google Scholar
16.Hytch, M.J., Snoeck, E., Kilaas, R.: Quantitative measurement of displacement and strain fields from HREM micrographs. Ultramicroscopy 74, 131 (1998)Google Scholar
17.Gutakovskii, A., Chuvilin, A., Song, S.: Application of high-resolution electron microscopy for visualization and quantitative analysis of strain fields in heterostructures. Bull. Russ. Acad. Sci. Phys. 71, 1426 (2007)Google Scholar
18.Hytch, M.J., Potez, L.: Geometric phase analysis of high-resolution electron microscopy images of antiphase domains: Example Cu3Au. Philos. Mag. A 76, 1119 (1997)Google Scholar
19.Exner, H.E.: Analysis of grain- and particle-size distrbutions in metallic materials. Int. Mater. Rev. 17, 25 (1972)Google Scholar
20.Malm, J.O., Keefe, M.A.O.: Deceptive “lattice spacings” in high-resolution micrographs of metal nanoparticles. Ultramicroscopy 68, 13 (1997)Google Scholar