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Grain Boundary Character Distribution of Nanocrystalline Cu Thin Films Using Stereological Analysis of Transmission Electron Microscope Orientation Maps

Published online by Cambridge University Press:  04 February 2013

A.D. Darbal
Affiliation:
Materials Research Science and Engineering Center, Carnegie Mellon University, 5000 Forbes Avenue, Pittsburgh, PA 15213, USA
K.J. Ganesh
Affiliation:
Materials Science and Engineering Program, The University of Texas at Austin, 1 University Station, Austin, TX 78712, USA
X. Liu
Affiliation:
Materials Research Science and Engineering Center, Carnegie Mellon University, 5000 Forbes Avenue, Pittsburgh, PA 15213, USA
S.-B. Lee
Affiliation:
Materials Research Science and Engineering Center, Carnegie Mellon University, 5000 Forbes Avenue, Pittsburgh, PA 15213, USA
J. Ledonne
Affiliation:
Materials Research Science and Engineering Center, Carnegie Mellon University, 5000 Forbes Avenue, Pittsburgh, PA 15213, USA
T. Sun
Affiliation:
Materials Science and Engineering Program, The University of Texas at Austin, 1 University Station, Austin, TX 78712, USA
B. Yao
Affiliation:
Materials Science and Engineering Program, The University of Texas at Austin, 1 University Station, Austin, TX 78712, USA
A.P. Warren
Affiliation:
Advanced Materials Processing and Analysis Center, University of Central Florida, 4000 Central Florida Boulevard, Orlando, FL 32816, USA
G.S. Rohrer
Affiliation:
Materials Research Science and Engineering Center, Carnegie Mellon University, 5000 Forbes Avenue, Pittsburgh, PA 15213, USA
A.D. Rollett
Affiliation:
Materials Research Science and Engineering Center, Carnegie Mellon University, 5000 Forbes Avenue, Pittsburgh, PA 15213, USA
P.J. Ferreira
Affiliation:
Materials Science and Engineering Program, The University of Texas at Austin, 1 University Station, Austin, TX 78712, USA
K.R. Coffey
Affiliation:
Advanced Materials Processing and Analysis Center, University of Central Florida, 4000 Central Florida Boulevard, Orlando, FL 32816, USA
K. Barmak*
Affiliation:
Materials Research Science and Engineering Center, Carnegie Mellon University, 5000 Forbes Avenue, Pittsburgh, PA 15213, USA
*
Corresponding author. E-mail: [email protected]
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Abstract

Stereological analysis has been coupled with transmission electron microscope (TEM) orientation mapping to investigate the grain boundary character distribution in nanocrystalline copper thin films. The use of the nanosized (<5 nm) beam in the TEM for collecting spot diffraction patterns renders an order of magnitude improvement in spatial resolution compared to the analysis of electron backscatter diffraction patterns in the scanning electron microscope. Electron beam precession is used to reduce dynamical effects and increase the reliability of orientation solutions. The misorientation distribution function shows a strong misorientation texture with a peak at 60°/[111], corresponding to the Σ3 misorientation. The grain boundary plane distribution shows {111} as the most frequently occurring plane, indicating a significant population of coherent twin boundaries. This study demonstrates the use of nanoscale orientation mapping in the TEM to quantify the five-parameter grain boundary distribution in nanocrystalline materials.

Type
Materials Applications
Copyright
Copyright © Microscopy Society of America 2013

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Footnotes

A.D. Darbal, formerly at Carnegie Mellon University, is now at NanoMEGAS USA, Tempe, AZ, USA.

K.J. Ganesh, formerly at the University of Texas at Austin, is now at Intel Corporation, Hilsboro, OR, USA.

#

T. Sun, formerly of the University of Central Florida, is now at Integrated System Ltd., Wanchai, Hong Kong.

§

B. Yao, formerly of the University of Central Florida, is now at the Pacific Northwest National Laboratory.

References

Adams, B.L., Wright, S.I. & Kunze, K. (1993). Orientation imaging: The emergence of a new microscopy. Metal Trans A 24, 819831.Google Scholar
Bollmann, W. (1970). Crystal Defects and Crystalline Interfaces. New York: Springer Verlag.Google Scholar
Dingley, D. (2004). Progressive steps in the development of electron backscatter diffraction and orientation imaging microscopy. J Microsc 213, 214224.Google Scholar
Dingley, D.J. (2006). Orientation imaging microscopy for the transmission electron microscope. Microchimica Acta 155, 1929.Google Scholar
Feldman, B., Park, S., Haverty, M., Shankar, S. & Dunham, S.T. (2010). Simulation of grain boundary effects on electronic transport in metals, and detailed causes of scattering. Phys Staus Solidi B 247, 17911796.CrossRefGoogle Scholar
Ganesh, K.J., Darbal, A., Rajasekhara, S., Rohrer, G.S., Barmak, K. & Ferreira, P.J. (2012). Effect of downscaling copper interconnects on the microstructure revealed by high resolution TEM-orientation-mapping. Nanotechnology 23 135702. Google Scholar
Ganesh, K.J., Kawasaki, M., Zhou, J.P. & Ferreira, P.J. (2010). D-STEM: A parallel electron diffraction technique applied to nanomaterials. Microsc Microanal 16, 614621.Google Scholar
Holm, E.A., Rohrer, G.S., Foiles, S.M., Rollett, A.D., Miller, H.M. & Olmsted, D.L. (2011). Validating computed grain boundary energies in fcc metals using the grain boundary character distribution. Acta Mater 59, 52505256.Google Scholar
Li, J., Dillon, S.J. & Rohrer, G.S. (2009). Relative grain boundary area and energy distributions in nickel. Acta Mater 57, 43044311.Google Scholar
Liu, H.H., Schmidt, S., Poulsen, H.F., Godfrey, A., Liu, Z.Q., Sharon, J.A. & Huang, X. (2011). Three-dimensional orientation mapping in the transmission electron microscope. Science 332, 833834.Google Scholar
Lu, K., Lu, L. & Suresh, S. (2009). Strengthening materials by engineering coherent internal boundaries at the nanoscale. Science 324, 349352.Google Scholar
Lu, L., Shen, Y., Chen, X., Qian, L. & Lu, K. (2004). Ultrahigh strength and high electrical conductivity in copper. Science 304, 422426.Google Scholar
Mackenzie, J.K., Moore, A.J.W. & Nichols, J.F. (1962). Bonds broken at atomically flat crystal surfaces—I: Face-centred and body-centred cubic crystals. J Phys Chem Solids 23, 185193.Google Scholar
Oleynikov, P., Hovmuller, S. & Zou, X.D. (2007). Precession electron diffraction: Observed and calculated intensities. Ultramicroscopy 107, 523533.Google Scholar
Olmsted, D.L., Foiles, S.M. & Holm, E.A. (2009). Survey of computed grain boundary properties in face-centered cubic metals: I. Grain boundary energy. Acta Mater 57, 36943703.Google Scholar
Portillo, J., Rauch, E.F., Nicolopoulos, S., Gemmi, M. & Bultreys, D. (2010). Precession electron diffraction assisted orientation mapping in the transmission electron microscope. Mater Sci Forum 644, 17.Google Scholar
Randle, V. (1996). The Role of Coincident Site Lattice in Grain Boundary Engineering. London: Cambridge University Press.Google Scholar
Randle, V., Rohrer, G.S., Miller, H.M., Coleman, M. & Owen, G.T. (2008). Five-parameter grain boundary distribution of commercially grain boundary engineered nickel and copper. Acta Mater 56, 23632373.Google Scholar
Rauch, E.F. & Duft, A. (2005). Orientation maps derived from TEM diffraction patterns collected with an external CCD camera. Mater Sci Forum 495497, 197202.CrossRefGoogle Scholar
Rauch, E.F. & Dupuy, L. (2005). Rapid diffraction patterns identification through template matching. Arch Metall Mater 50, 8789.Google Scholar
Rauch, E.F. & Veron, M. (2005). Coupled microstructural observations and local texture measurements with an automated crystallographic orientation mapping tool attached to a tem. Materialwiss Werkst 36, 552556.Google Scholar
Rohrer, G.S., El Dasher, B.S., Miller, H.M., Rollett, A.D. & Saylor, D.M. (2004a). Distribution of grain boundary planes at coincident site lattice misorientations. Mat Res Soc Symp Proc 819, N7.2. Google Scholar
Rohrer, G.S., Holm, E.A., Rollett, A.D., Foiles, S.M., Li, J. & Olmsted, D.L. (2010a). Comparing calculated and measured grain boundary energies in nickel. Acta Mater 58, 50635069.Google Scholar
Rohrer, G.S., Li, J., Lee, S., Rollett, A.D., Groeber, M. & Uchic, M.D. (2010b). Deriving grain boundary character distributions and relative grain boundary energies from three-dimensional EBSD data. Mater Sci Technol 26, 661669.Google Scholar
Rohrer, G.S., Saylor, D.M., Dasher, B.E., Adams, B.L., Rollett, A.D. & Wynblatt, P. (2004b). The distribution of internal interfaces in polycrystals. Z Metallk 95, 197214.Google Scholar
Rouvimov, S., Moeck, P., Rauch, E.F., Maniette, Y. & Bultreys, D. (2008). Crystallographic characterization of polycrystalline materials: High resolution automated crystallite orientation. Microsc Microanal 14, 768769.Google Scholar
Saylor, D.M., Dasher, B.S., Adams, B.L. & Rohrer, G.S. (2004a). Measuring the five-parameter grain-boundary distribution from observations of planar sections. Metal Mater Trans A 35, 19811989.CrossRefGoogle Scholar
Saylor, D.M., Dasher, B.S.E., Rollett, A.D. & Rohrer, G.S. (2004b). Distribution of grain boundaries in aluminium as a function of five macroscopic parameters. Acta Mater 52, 36493655.Google Scholar
Saylor, D.M., El, D.B., Pang, Y., Miller, H.M., Wynblatt, P., Rollett, A.D. & Rohrer, G.S. (2004c). Habits of grains in dense polycrystalline solids. J Am Ceram Soc 87, 724726.Google Scholar
Sun, T., Yao, B., Warren, A.P., Barmak, K., Toney, M.F., Peale, R.E. & Coffey, K.R. (2010). Surface and grain-boundary scattering in nanometric Cu films. Phys Rev B 81.CrossRefGoogle Scholar
Sun, T., Yao, B., Warren, A.P., Kumar, V., Roberts, S., Barmak, K. & Coffey, K.R. (2008). Classical size effect in oxide-encapsulated Cu thin films: Impact of grain boundaries versus surfaces on resistivity. J Vac Sci Technol A 26, 605609.Google Scholar
Vincent, R. & Midgley, P.A. (1994). Double conical beam-rocking system for measurement of integrated electron diffraction intensities. Ultramicroscopy 53, 271282.Google Scholar
Williams, D.B. & Carter, C.B. (2009). Transmission Electron Microscopy: A Textbook for Materials Science, pp. 167168. New York: Springer.Google Scholar
Wright, S.I. & Larsen, R.J. (2002). Extracting twins from orientation imaging microscopy scan data. J Microsc 205, 245252.Google Scholar
Yao, B., Petrova, R.V., Vanfleet, R.R. & Coffey, K.R. (2006). A modified back-etch method for preparation of plan-view high-resolution transmission electron microscopy samples. J Electron Microsc 57, 4752.Google Scholar
Yao, B., Sun, T., Warren, A., Heinrich, H., Barmak, K. & Coffey, K.R. (2010). High contrast hollow-cone dark field transmission electron microscopy for nanocrystalline grain size quantification. Micron 41, 177182.Google Scholar
Zaefferer, S. (2007). On the formation mechanisms, spatial resolution and intensity of backscatter Kikuchi patterns. Ultramicroscopy 107, 254266.Google Scholar