Hostname: page-component-586b7cd67f-dlnhk Total loading time: 0 Render date: 2024-11-25T15:40:01.051Z Has data issue: false hasContentIssue false

The Effects of Gas Composition on the Ion Milling of Cross Sectional Tem Samples Containing Carbon Layers

Published online by Cambridge University Press:  10 February 2011

Scott D. Walck
Affiliation:
Materials Directorate, Wright Laboratory, WPAFB, OH 45433-7750
Frank J. Scheltens
Affiliation:
UES, Inc., Dayton, OH 45432
Josekutty J. Nainaparampil
Affiliation:
Systran, Inc., Dayton, OH 45432
Get access

Abstract

During conventional ion milling of carbon thin films on Si or SiC, the carbon has a much slower milling rate than the Si, SiC, and the epoxy resin. As a result, the substrates were thinned much more rapidly than the carbon films. A solution suggested by several subscribers to the Microscopy Society of America's Microscopy Listserver among others was to reactively ion mill the samples with a 20–25% oxygen-argon gas mixture. Is this the best inert gas to use? Neon has a mass that is between Si and C and therefore should impart a higher energy transfer to the C atoms than Ar. To determine whether the mass of the inert gas is important in balancing the milling rates, four gases were used to ion mill samples of a PLD DLC film with a nominal thickness of 0.5 μm. For improved adhesion of the films to the Si substrate, an initial 2 nm of Ti and a nominal 0.5 μm thick layer of TiC was grown using a combined PLD and magnetron sputtering technique prior to the PLD DLC.1,2 The gases were 100%Ar, 100%Ne, 75%Ar-25%O2, and 75%Ne-25%O2. Using the Tripod Polisher, the samples were polished flat using typical conditions and the surfaces examined by atomic force microscopy and compared. TEM samples prepared by single-sided dimpling prior to ion milling were prepared using the gas composition which gave the best results with respect to the AFM. A methodology is established for determining ion milling conditions for samples having layers of different compositions.

Type
Research Article
Copyright
Copyright © Materials Research Society 1997

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

1. Voevodin, A. A., Capano, M. A., Laube, S. J. P., Donley, M. S., Zabinski, J. S., Design of a Ti/TiCiDLC Functionally Gradient Coating Based on Studies of Structural Transitions in Ti-C Thin Films, Thin Solid Films, in press.Google Scholar
2. Voevodin, A. A., Walck, S. D., Zabinski, J. S., Architecture of Multilayer Nanocomposite Coatings with Super-hard Diamond-like Carbon Layers for Wear Protection at High Contact Loads, Wear, in press.Google Scholar
3. Árpád Barna, in Specimen Preparation for Transmission Electron Microscopy of Materials -III, eds. Anderson, Ron, Tracy, Bryan, and Bravman, John, Materials Research Society, Pittsburgh, p. 3, 1992.Google Scholar
4. Bravman, J. C. and Sinclair, R., J. Electron Micros. Tech., 1, p. 53 (1984).Google Scholar
5. EpoTek 353ND, Epoxy Technology, Inc, Billerica, MAGoogle Scholar
6. Tripod PolisherTM and accessories, South Bay Technology, Inc, San Clemente, CA.Google Scholar
7. Benedict, John, Anderson, Ron, and Klepeis, Stanley J., in Specimen Preparation for Transmission Electron Microscopy of Materials -III, ed, Anderson, S. Ron, Tracy, Bryan, and Bravman, John, Materials Research Society, Pittsburgh, p. 121, 1992.Google Scholar
8. Benedict, J. P., Klepeis, S. J., Vandygrift, W. J., and Anderson, Ron, A Method for Precision Specimen Preparation for Both SEM and TEM Analysis, EMSA Bulletin, 19, p. 74, 1989.Google Scholar