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.

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Fig. 1

Schematic of the experimental test-bed

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Fig. 2

Exfoliation process in the presence of in-plane shear oscillation

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Fig. 3

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

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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

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Fig. 5

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

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Fig. 6

Representative exfoliated PGS produced by the 236 μm thick PDMS stamp

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Fig. 7

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

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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

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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

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Fig. 10

Comparison of exfoliated sheet thicknesses obtained under different conditions

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Fig. 11

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

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Fig. 12

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



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