DOI: 10.1073/pnas.0400066101. Deformation mechanisms in free-standing nanoscale thin films: A quantitative <i>in situ</i> transmission electron microscope study

Deformation mechanisms in free-standing nanoscale thin films: A quantitative in situ transmission electron microscope study

10.1073/pnas.0400066101

Crossref journal-article

Proceedings of the National Academy of Sciences

Proceedings of the National Academy of Sciences (341)

Abstract

We have added force and displacement measurement capabilities in the transmission electron microscope (TEM) for in situ quantitative tensile experimentation on nanoscale specimens. Employing the technique, we measured the stress–strain response of several nanoscale free-standing aluminum and gold films subjected to several loading and unloading cycles. We observed low elastic modulus, nonlinear elasticity, lack of work hardening, and macroscopically brittle nature in these metals when their average grain size is 50 nm or less. Direct in situ TEM observation of the absence of dislocations in these films even at high stresses points to a grain-boundary-based mechanism as a dominant contributing factor in nanoscale metal deformation. When grain size is larger, the same metals regain their macroscopic behavior. Addition of quantitative capability makes the TEM a versatile tool for new fundamental investigations on materials and structures at the nanoscale.

Bibliography

Haque, M. A., & Saif, M. T. A. (2004). Deformation mechanisms in free-standing nanoscale thin films: A quantitative in situ transmission electron microscope study. Proceedings of the National Academy of Sciences, 101(17), 6335â6340.

Authors 2

M. A. Haque (first)
M. T. A. Saif (additional)

References 48 Referenced 222

10.1088/0370-1301/64/9/303
Petch, N. J. (1953) J. Iron Steel Inst. 174, 25-28. / J. Iron Steel Inst. (1953)
10.1016/0956-7151(94)90502-9
10.1557/JMR.1995.0853
10.1016/S1359-6454(98)00153-0
10.1016/S0022-5096(98)00103-3
10.1016/S1359-6454(03)00116-2
10.1016/S1359-6454(98)00231-6
10.1016/S1359-6454(99)00285-2
Gutkin, M. Y., Ovidko, I. A. & Pande, C. S. (2001) Rev. Adv. Mater. Sci. 2, 80-102. / Rev. Adv. Mater. Sci. (2001)
10.1080/01418639708241122
10.1016/S1359-6454(98)00150-5
10.1016/S1359-6454(97)00092-X
10.1016/S1359-6454(00)00128-2
10.1557/JMR.1995.2892
10.1016/S0965-9773(99)00052-5
10.1016/S1359-6454(99)00353-5
10.1557/mrs2002.17
10.1016/0956-716X(91)90256-Z
10.1038/35328
10.1080/01418610108214329
10.1016/S1359-6462(99)00213-4
Koch, C. C. & Naryan, J. (2001) MRS Symp. Proc. 634, B5.1.1-B5.1.11. / MRS Symp. Proc. (2001)
10.1016/S0022-5096(02)00062-5
10.1007/BF02411051
10.1109/84.946774
10.1007/BF02411059
10.1023/A:1026321404286
10.1016/S1359-6454(99)00302-X
Youngdahl, C. J., Hugo, R. C., Kung, H. & Weertman, J. R. (2001) MRS Symp. Proc. 634, B.1.2.1-B.1.2.6. / MRS Symp. Proc. (2001)
10.1016/S1359-6454(02)00599-2
10.1016/0965-9773(95)00281-I
10.1080/01418610008212096
10.1016/S1359-6454(99)00286-4
Honeycombe R. W. K. (1968) The Plastic Deformation of Metals (Arnold London).
10.1063/1.1367896
Sakai, S., Tanimoto, H. & Mizubayashi, H. (1999) Acta Mater. 47, 211-217. / Acta Mater. (1999)
10.1557/mrs2002.16
10.1023/A:1011056927880
10.1016/0304-3991(92)90135-7
10.1103/PhysRevB.62.831
10.1080/09500830031000120891
10.1080/01418618608242870
10.1103/PhysRevLett.60.1170
10.1557/PROC-351-337
10.1016/S1359-6462(01)00678-9
Voter, A. F. & Chen, S. P. (1987) MRS Symp. Proc. 82, 175-180. / MRS Symp. Proc. (1987)
10.1016/S0022-5096(99)00022-8

Dates

Type	When
Created	21 years, 4 months ago (April 14, 2004, 8:13 p.m.)
Deposited	3 years, 4 months ago (April 12, 2022, 9:51 a.m.)
Indexed	1 month ago (July 20, 2025, 12:11 a.m.)
Issued	21 years, 4 months ago (April 14, 2004)
Published	21 years, 4 months ago (April 14, 2004)
Published Online	21 years, 4 months ago (April 14, 2004)
Published Print	21 years, 3 months ago (April 27, 2004)

Funders 0

None

BibTeX

@article{Haque_2004, title={Deformation mechanisms in free-standing nanoscale thin films: A quantitative in situ transmission electron microscope study}, volume={101}, ISSN={1091-6490}, url={http://dx.doi.org/10.1073/pnas.0400066101}, DOI={10.1073/pnas.0400066101}, number={17}, journal={Proceedings of the National Academy of Sciences}, publisher={Proceedings of the National Academy of Sciences}, author={Haque, M. A. and Saif, M. T. A.}, year={2004}, month=apr, pages={6335–6340} }

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