0
Research Papers

Polymer Stamp-Based Mechanical Exfoliation of Thin High-Quality Pyrolytic Graphite Sheets

[+] Author and Article Information
David Hahn

The George W. Woodruff School of
Mechanical Engineering,
Georgia Institute of Technology,
Atlanta, GA 30332
e-mail: dhahn7@gatech.edu

Buddhika Jayasena

The George W. Woodruff School
of Mechanical Engineering,
Georgia Institute of Technology,
Atlanta, GA 30332
e-mail: buddhikaphd@gmail.com

Zhigang Jiang

School of Physics,
Georgia Institute of Technology,
Atlanta, GA 30332
e-mail: zhigang.jiang@physics.gatech.edu

Shreyes N. Melkote

The George W. Woodruff School
of Mechanical Engineering,
Georgia Institute of Technology,
Atlanta, GA 30332
e-mail: shreyes.melkote@me.gatech.edu

Contributed by the Manufacturing Engineering Division of ASME for publication in the JOURNAL OF MICRO-AND NANO-MANUFACTURING. Manuscript received February 9, 2019; final manuscript received April 10, 2019; published online May 15, 2019. Assoc. Editor: Michael Cullinan.

J. Micro Nano-Manuf 7(1), 011005 (May 15, 2019) (7 pages) Paper No: JMNM-19-1007; doi: 10.1115/1.4043502 History: Received February 09, 2019; Revised April 10, 2019

This paper reports on a polymer stamp-based mechanical exfoliation method for producing thin (<1 μm) graphite sheets from a highly ordered pyrolytic graphite (HOPG) source by tailoring key exfoliation process parameters, utilizing in-plane shear oscillation during exfoliation, and controlling the thickness of a polydimethylsiloxane (PDMS) stamp. Experiments on the effect of high frequency in-plane shear oscillation and the effect of PDMS stamp thickness are designed to reduce the thickness of exfoliated layers and to minimize surface morphological variations. Results show that the exfoliated sheets consist of a range of layer thicknesses, surface areas, and surface morphological features. The exfoliated HOPG sheets are also found to be thinner, more electrically and thermally conductive, and of higher quality than commercially available pyrolytic graphite sheets.

FIGURES IN THIS ARTICLE
<>
Copyright © 2019 by ASME
Your Session has timed out. Please sign back in to continue.

References

Novoselov, K. S. , Jiang, D. , Schedin, F. , Booth, T. J. , Khotkevich, V. V. , Morozov, S. V. , and Geim, A. K. , 2005, “ Two-Dimensional Atomic Crystals,” Proc. Natl. Acad. Sci. U.S.A., 102(30), pp. 10451–10453. [CrossRef] [PubMed]
Miro, P. , Audiffred, M. , and Heine, T. , 2014, “ An Atlas of Two-Dimensional Materials,” Chem. Soc. Rev., 43(18), pp. 6537–6554. [CrossRef] [PubMed]
Butler, S. Z. , Hollen, S. M. , Cao, L. , Cui, Y. , Gupta, J. A. , Gutiérrez, H. R. , Heinz, T. F. , Hong, S. S. , Huang, J. , Ismach, A. F. , Johnston-Halperin, E. , Kuno, M. , Plashnitsa, V. V. , Robinson, R. D. , Ruoff, R. S. , Salahuddin, S. , Shan, J. , Shi, L. , Spencer, M. G. , Terrones, M. , Windl, W. , and Goldberger, J. E. , 2013, “ Progress, Challenges, and Opportunities in Two-Dimensional Materials Beyond Graphene,” ACS Nano, 7(4), pp. 2898–2926. [CrossRef] [PubMed]
Geim, A. K. , and Grigorieva, I. V. , 2013, “ Van Der Waals Heterostructures,” Nature, 499(7459), pp. 419–425. [CrossRef] [PubMed]
Nah, J. , Kumar, S. B. , Fang, H. , Chen, Y.-Z. , Plis, E. , Chueh, Y.-L. , Krishna, S. , Guo, J. , and Javey, A. , 2012, “ Quantum Size Effects on the Chemical Sensing Performance of Two-Dimensional Semiconductors,” J. Phys. Chem. C, 116(17), pp. 9750–9754. [CrossRef]
Panasonic Corporation of North America, 2016, “ Pyrolytic Graphite Sheet: The Advanced Thermal Solution for Today's Designs,” Panasonic Corporation of North America, accessed Apr. 26, 2019, http://www1.futureelectronics.com/Mailing/etechs/Panasonic/etechALERT_Panasonic_LightControleSolutions/Panasonic_PGS_Brochure_Online.pdf
Panasonic, 2015, “ Pyrolytic Graphite Sheet Evolves to Meet Tough Thermal Demands,” Electronic Design, accessed Apr. 26, 2019, http://electronicdesign.com/circuit-protection/pyrolytic-graphite-sheet-evolves-meet-tough-thermal-demands
Wen, C.-Y. , and Huang, G.-W. , 2008, “ Application of a Thermally Conductive Pyrolytic Graphite Sheet to Thermal Management of a PEM Fuel Cell,” J. Power Sources, 178(1), pp. 132–140. [CrossRef]
Yoichi, T. , Sayuri, K. , and Kuniaki, S. , 2008, “ Performance Improvement of Stacked Graphite Sheets for Cooling Applications,” 58th Electronic Components and Technology Conference (ECTC), Lake Buena Vista, FL, May 27–30, pp. 760–764.
Jayasena, B. , and Melkote, S. N. , 2015, “ An Investigation of PDMS Stamp Assisted Mechanical Exfoliation of Large Area Graphene,” Procedia Manuf., 1, pp. 840–853. [CrossRef]
Carlson, A. , Bowen, A. M. , Huang, Y. , Nuzzo, R. G. , and Rogers, J. A. , 2012, “ Transfer Printing Techniques for Materials Assembly and Micro/Nanodevice Fabrication,” Adv. Mater., 24(39), pp. 5284–5318. [CrossRef] [PubMed]
Meitl, M. A. , Zhu, Z.-T. , Kumar, V. , Lee, K. J. , Feng, X. , Huang, Y. Y. , Adesida, I. , Nuzzo, R. G. , and Rogers, J. A. , 2006, “ Transfer Printing by Kinetic Control of Adhesion to an Elastomeric Stamp,” Nat Mater, 5(1), pp. 33–38. [CrossRef]
Hahn, D. , 2017, “ Viscoelastic Polymer-Assisted Mechanical Exfoliation of Large Area Highly Oriented Pyrolytic Graphite,” M.S. thesis, Georgia Institute of Technology, Atlanta, GA.
Van der Pauw, L. J. , 1958, “ A Method of Measuring the Resistivity and Hall Coefficient on Lamellae of Arbitrary Shape,” Philips Tech. Rev., 20, pp. 220–224.
Park, J. S. , Reina, A. , Saito, R. , Kong, J. , Dresselhaus, G. , and Dresselhaus, M. S. , 2009, “ Band Raman Spectra of Single, Double and Triple Layer Graphene,” Carbon, 47(5), pp. 1303–1310. [CrossRef]
Parobek, D. , Shenoy, G. , Zhou, F. , Peng, Z. , Ward, M. , and Liu, H. , 2016, “ Synthesizing and Characterizing Graphene Via Raman Spectroscopy: An Upper-Level Undergraduate Experiment That Exposes Students to Raman Spectroscopy and a 2D Nanomaterial,” J. Chem. Educ., 93(10), pp. 1798–1803. [CrossRef]
Ferrari, A. C. , 2007, “ Raman Spectroscopy of Graphene and Graphite: Disorder, Electron–Phonon Coupling, Doping and Nonadiabatic Effects,” Solid State Commun., 143(1–2), pp. 47–57. [CrossRef]
Schroder, D. K. , 2006, Semiconductor Material and Device Characterization, Wiley, Hoboken, NJ, pp. 1–11.
Wang, Y. , Alsmeyer, D. C. , and McCreery, R. L. , 1990, “ Raman Spectroscopy of Carbon Materials: Structural Basis of Observed Spectra,” Chem. Mater., 2(5), pp. 557–563. [CrossRef]

Figures

Grahic Jump Location
Fig. 1

Schematic of the experimental test-bed

Grahic Jump Location
Fig. 2

Exfoliation process in the presence of in-plane shear oscillation

Grahic Jump Location
Fig. 3

Average exfoliated sheet thickness as a function of the shear oscillation frequency; oscillation amplitude = ±1 μm

Grahic Jump Location
Fig. 4

Exfoliated layers obtained at different oscillation frequencies: (a) 500 Hz, (b) 1000 Hz, (c) 1500 Hz, (d) 2000 Hz, (e) 2500 Hz, and (f) 3000 Hz

Grahic Jump Location
Fig. 5

Effect of stamp thickness on successfully exfoliating sheets with greater than 95% of the nominal HOPG surface area

Grahic Jump Location
Fig. 6

Representative exfoliated PGS produced by the 236 μm thick PDMS stamp

Grahic Jump Location
Fig. 7

Exfoliated sheet surface morphologies obtained with PDMS stamp thicknesses of (a) 236 μm and (b) 476 μm

Grahic Jump Location
Fig. 8

(a) Exfoliated sheet number 1 and (b) exfoliated sheet number 2; 236 μm PDMS stamp, shear oscillation of 3000 Hz and ±1 μm amplitude

Grahic Jump Location
Fig. 9

Surface morphologies of exfoliated sheets obtained using the 236 μm thick PDMS stamp and shear oscillation (3000 Hz, ±1 μm amplitude): (a) exfoliated sample 1 and (b) exfoliated sample 2, imaged at different locations of the respective samples

Grahic Jump Location
Fig. 10

Comparison of exfoliated sheet thicknesses obtained under different conditions

Grahic Jump Location
Fig. 11

In-plane thermal conductivities of the exfoliated sheet and commercially available PGS sheets of varying thickness

Grahic Jump Location
Fig. 12

Raman spectra of the 1.25 ± 0.42 μm thick exfoliated layer. The excitation wavelength utilized in the measurements is 532 nm.

Tables

Errata

Some tools below are only available to our subscribers or users with an online account.

Related Content

Customize your page view by dragging and repositioning the boxes below.

Related Journal Articles
Related eBook Content
Topic Collections

Sorry! You do not have access to this content. For assistance or to subscribe, please contact us:

  • TELEPHONE: 1-800-843-2763 (Toll-free in the USA)
  • EMAIL: asmedigitalcollection@asme.org
Sign In