Name: fabrication of three-dimensional graphene-based polyhedrons via origami-like self-folding
Uploaded: 2018-09-23T14:30:00
Description: Watch this Scientific Journal Video about Fabrication of Three-Dimensional Graphene-Based Polyhedrons via Origami-Like Self-Folding at JoVE.com

This material is based upon work supported by a start-up fund at the University of Minnesota, Twin Cities and an NSF CAREER Award (CMMI-1454293). Parts of this work were carried out in the Characterization Facility at the University of Minnesota, a member of the NSF-funded Materials Research Facilities Network (via the MRSEC program. Portions of this work were conducted in the Minnesota Nano Center, which is supported by the National Science Foundation through the National Nano Coordinated Infrastructure Network (NNCI) under Award Number ECCS-1542202. C. D. acknowledges support from the 3M Science and Technology Fellowship.

CAUTION: Several of the chemicals used in these syntheses are toxic and may cause irritation and severe organ damage when touched or inhaled. Please use appropriate safety equipment and wear personal protective equipment when handling the chemicals.
1. Preparation of Aluminum Oxide and Chromium Protection Layers on a Copper Sacrificial Layer
<ol>
	<li>Using an electron-beam evaporator, deposit 10 nm thick chromium (Cr) and 300 nm thick copper (Cu) layers (sacrificial layer) on the silicon (S...

<ol>
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K., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Graphene+kirigami.">Graphene kirigami.</a> Nature. 524 (7564), 204-207 (2015).</li><li>Michael Cai, W., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Mechanical+instability+driven+self-assembly+and+architecturing+of+2D+materials.">Mechanical instability driven self-assembly and architecturing of 2D materials.</a> 2D Materials. 4 (2), 022002 (2017).</li><li>Shenoy, V. B., Gracias, D. H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Self-folding+thin-film+materials:+From+nanopolyhedra+to+graphene+origami.">Self-folding thin-film materials: From nanopolyhedra to graphene origami.</a> MRS Bulletin. 37 (9), 847-854 (2012).</li><li>Zhu, S., Li, T. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Hydrogenation-Assisted+Graphene+Origami+and+Its+Application+in+Programmable+Molecular+Mass+Uptake,+Storage,+and+Release.">Hydrogenation-Assisted Graphene Origami and Its Application in Programmable Molecular Mass Uptake, Storage, and Release.</a> ACS Nano. 8 (3), 2864-2872 (2014).</li><li>Zhang, L., Zeng, X., Wang, X. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Programmable+hydrogenation+of+graphene+for+novel+nanocages.">Programmable hydrogenation of graphene for novel nanocages.</a> Scientific Reports. 3, 3162 (2013).</li><li>Vickery, J. L., Patil, A. J., Mann, S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Fabrication+of+Graphene-Polymer+Nanocomposites+With+Higher-Order+Three-Dimensional+Architectures.">Fabrication of Graphene-Polymer Nanocomposites With Higher-Order Three-Dimensional Architectures.</a> Advanced Materials. 21 (21), 2180-2184 (2009).</li><li>Yang, X., Zhu, J., Qiu, L., Li, D. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Bioinspired+effective+prevention+of+restacking+in+multilayered+graphene+films:+towards+the+next+generation+of+high-performance+supercapacitors.">Bioinspired effective prevention of restacking in multilayered graphene films: towards the next generation of high-performance supercapacitors.</a> Advanced Materials. 23 (25), 2833-2838 (2011).</li><li>Choi, B. G., Yang, M., Hong, W. H., Choi, J. W., Huh, Y. S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=3D+macroporous+graphene+frameworks+for+supercapacitors+with+high+energy+and+power+densities.">3D macroporous graphene frameworks for supercapacitors with high energy and power densities.</a> ACS Nano. 6 (5), 4020-4028 (2012).</li><li>Niu, Z., Chen, J., Hng, H. H., Ma, J., Chen, X. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+leavening+strategy+to+prepare+reduced+graphene+oxide+foams.">A leavening strategy to prepare reduced graphene oxide foams.</a> Advanced Materials. 24 (30), 4144-4150 (2012).</li><li>Li, Y., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Growth+of+conformal+graphene+cages+on+micrometre-sized+silicon+particles+as+stable+battery+anodes.">Growth of conformal graphene cages on micrometre-sized silicon particles as stable battery anodes.</a> Nature Energy. 1 (2), (2016).</li><li>Cho, J. H., Gracias, D. 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For the cubes fabricated with CVD graphene, because each face of a given cube is designed with an outer frame surrounding a ~160 &#215; 160 &#181;m2 area of free-standing graphene, a single sheet of monolayer graphene does not have the necessary strength to permit parallel processing of the cubes. For this reason, graphene membranes consisting of three layers of CVD graphene monolayer sheets are produced via three separate graphene transfers using multiple PMMA coating/removal steps. On the other hand...

Two-dimensional (2D) graphene sheets possess extraordinary optical, electronic, and mechanical properties, making them model systems for the observation of novel quantum phenomena for next-generation electronic, optoelectronic, electrochemical, electromechanical, and biomedical applications1,2,3,4,5,6. Apart from the as-produced 2D layered structure of graphene, recently, various modification approaches have been investigated to observe new functionalities of graphene and seek new application opportunities. For example, modulating (or tuning) its physical properties (i.e.,&#160;doping level and/or band gap) by tailoring the shapes or patterning of the 2D structure to a one-dimensional (1D) or zero-dimensional (0D) structure (e.g., graphene nanoribbon or graphene quantum dots) has been studied to obtain new physical phenomena including quantum confinement effects, localized plasmonic modes, localized electron distribution, and spin-polarized edge states7,8,9,10,11,12. In addition, varying the texture of 2D graphene by crumpling (often called kirigami), delamination, buckling, twisting, or stacking of multiple layers, or changing the graphene surface shape by transferring 2D graphene on top of a 3D feature (substrate) has been shown to change the graphene&#39;s wettability, mechanical characteristics, and optical properties13,14.
Beyond changing the surface morphology and layered structure of 2D graphene, assembly of 2D graphene into functionalized, well-defined, three-dimensional (3D) polyhedrons has been of great interest recently in the graphene community to obtain new physical and chemical phenomena15. In theory, the elastic, electrostatic, and van der Waals energies of 2D graphene-based structures can be leveraged to transform the 2D graphene into various 3D graphene-origami configurations16,17. Based on this concept, theoretical modeling studies have investigated 3D graphene structure designs, formed from nanoscale 2D graphene membranes, with possible uses in drug delivery and general molecular storage16,17.&#160;Yet, the experimental progress of this approach is still far from realizing these applications. On the other hand, a number of chemical synthetic methods have been developed to achieve 3D structures via template-assisted assembly, flow-directed assembly, leavening assembly, and conformal growth methods18,19,20,21,22. However, these methods are currently limited in that they cannot produce a 3D, hollow, enclosed structure without losing the intrinsic properties of the graphene sheets.
Here, a strategy for building 3D, hollow, graphene-based microcubes (overall dimension of ~200 &#181;m) by using origami-like self-folding is outlined; overcoming the foremost challenges in the construction of free-standing, hollow, 3D, polyhedral, graphene-based materials. In origami-like, hands-free self-folding techniques, 2D lithographically patterned planar features (i.e.,&#160;graphene-based membranes) are connected with hinges (i.e.,&#160;thermal-sensitive polymer, photoresist) at various joints, thereby forming 2D nets which fold up when the hinges are heated to melting temperature23,24,25,26. The graphene-based cubes are realized with window membrane components composed of a few layers of chemical vapor deposition (CVD) grown graphene or graphene oxide (GO) membranes; both with the use of polymer frames and hinges. The fabrication of the 3D graphene-based cubes involves: (i) preparation of protection layers, (ii) graphene-membrane transfer and patterning, (iii) metal surface patterning on graphene-membranes, (iv) frame and hinges patterning and deposition, (v) self-folding, and (vi) removal of the protection layers (Figure 1). This article focuses mostly on the self-folding aspects of the 3D graphene-based cubes fabrication. Details on physical and optical properties of the 3D graphene-based cubes can be found in our other recent publications27,28.

<table border="0" cellpadding="0" cellspacing="0" style="width:1315px;" width="1313">
	<tbody>
		<tr height="21">
			<td height="21" style="height:21px;width:311px;">Acetone</td>
			<td style="width:295px;">Fisher Chemical</td>
			<td style="width:199px;">A18P-4</td>
			<td style="width:511px;">N/A</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:311px;">Aluminium oxide</td>
			<td style="width:295px;">Kurt J. Lesker Company</td>
			<td style="width:199px;">EVMALO-1-2.5</td>
			<td>99.99% Pure</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:311px;">APS Copper Etchant 100</td>
			<td style="width:295px;">Transene Company, Inc.</td>
			<td style="width:199px;">N/A</td>
			<td>N/A</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:311px;">Camera (for 3D image)</td>
			<td style="width:295px;">Nikon</td>
			<td style="width:199px;">D5100</td>
			<td>1080p Full HD, Effective pixels: 16.2 million, Sensorsize: 23.6 mm x 15.6 mm</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:311px;">CE-5 M Chromium Mask Etchant</td>
			<td style="width:295px;">Transene Company, Inc.</td>
			<td style="width:199px;">N/A</td>
			<td>N/A</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:311px;">Chemical deposition growth (CVD) system</td>
			<td style="width:295px;">Customized</td>
			<td style="width:199px;">N/A</td>
			<td>Lindberg/Blue Tube Furnace</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:311px;">Chromium</td>
			<td style="width:295px;">Kurt J. Lesker Company</td>
			<td style="width:199px;">EVMCR35J</td>
			<td>99.95% pure</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:311px;">Chromium Etchant 473</td>
			<td style="width:295px;">Transene Company, Inc.</td>
			<td style="width:199px;">N/A</td>
			<td>N/A</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:311px;">Copper</td>
			<td style="width:295px;">Kurt J. Lesker Company</td>
			<td style="width:199px;">EVMCU40QXQJ</td>
			<td>99.99% pure</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:311px;">Developer-1 (MF319 developer)</td>
			<td style="width:295px;">Microposit</td>
			<td style="width:199px;">10018042</td>
			<td>N/A</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:311px;">Developer-2 (AZ developer)</td>
			<td style="width:295px;">Merck performance Materials Corp.</td>
			<td style="width:199px;">1005422496</td>
			<td>N/A</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:311px;">Developer-3 (SU-8 developer)</td>
			<td>MicroChem</td>
			<td style="width:199px;">NC9901158</td>
			<td>N/A</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:311px;">Digital Hot Plate</td>
			<td style="width:295px;">Thermo Scientific</td>
			<td style="width:199px;">HP131725</td>
			<td>Super-Nuvoa series, maximum temperature: 370 &#176;C</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:311px;">E-Beam Evaporator System</td>
			<td style="width:295px;">Rocky Mountain Vacuum Tech.</td>
			<td style="width:199px;">N/A</td>
			<td>RME-2000</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:311px;">Graphene oxide</td>
			<td style="width:295px;">Goographene</td>
			<td style="width:199px;">N/A</td>
			<td>Purity: ~ 99%; Single layer ratio: ~99%;&#160; 0.7-1.2 nm in thickness.</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:311px;">Isopropyl Alcohol</td>
			<td style="width:295px;">Fisher Chemical</td>
			<td style="width:199px;">A416-4</td>
			<td>N/A</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:311px;">Mask Aligner</td>
			<td style="width:295px;">Midas</td>
			<td style="width:199px;">MDA-400LJ</td>
			<td>N/A</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:311px;">Microscope</td>
			<td style="width:295px;">Omax</td>
			<td style="width:199px;">NJF-120A</td>
			<td>N/A</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:311px;">multiple polymethyl methacrylate (PMMA)</td>
			<td style="width:295px;">MicroChem</td>
			<td style="width:199px;">950 PMMA A9</td>
			<td>N/A</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:311px;">Oxygen plasma&#160;</td>
			<td style="width:295px;">Technics Inc.</td>
			<td style="width:199px;">SERIES 800</td>
			<td>Microscale reactive ion etching (RIE)</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:311px;">Photoresist-1 (S1813 Photoresist)</td>
			<td style="width:295px;">Microposit</td>
			<td style="width:199px;">10018348</td>
			<td>N/A</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:311px;">Photoresist-2 (SPR220 Photoresist)</td>
			<td style="width:295px;">MicroChem</td>
			<td style="width:199px;">SPR00220-7G</td>
			<td>N/A</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:311px;">Photoresist-3 (SU-8 Photoresist)</td>
			<td>MicroChem</td>
			<td style="width:199px;">SU-8-2010</td>
			<td>N/A</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:311px;">Profilometer</td>
			<td style="width:295px;">Tencor Instruments</td>
			<td style="width:199px;">N/A</td>
			<td>Alpha-Step 200</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:311px;">Raman</td>
			<td style="width:295px;">WITec Instruments Corp.</td>
			<td style="width:199px;">Alpha300R</td>
			<td>Confocal Raman Microscope</td>
		</tr>
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			<td height="21" style="height:21px;width:311px;">Silicon Wafer</td>
			<td style="width:295px;">Siltronic AG</td>
			<td style="width:199px;">N/A</td>
			<td>100mm diameter, N-type, one-side polish, resitivity: 560-840 &#937;&#8226;cm</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:311px;">Spinner</td>
			<td style="width:295px;">Best Tools</td>
			<td style="width:199px;">S0114031123</td>
			<td>SMART COATER 100</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:311px;">Titanium</td>
			<td style="width:295px;">Kurt J. Lesker Company</td>
			<td>EVMTI45QXQA</td>
			<td>99.99% Pure</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:311px;">Ultrasonic Cleaner</td>
			<td style="width:295px;">Crest Ultrasonics</td>
			<td style="width:199px;">N/A</td>
			<td>Powersonic series</td>
		</tr>
	</tbody>
</table>

fabrication of three-dimensional graphene-based polyhedrons via origami-like self-folding

The assembly of two-dimensional (2D) graphene into three-dimensional (3D) polyhedral structures while preserving the graphene's excellent inherent properties has been of great interest for the development of novel device applications. Here, fabrication of 3D, microscale, hollow polyhedrons (cubes) consisting of a few layers of 2D graphene or graphene oxide sheets via an origami-like self-folding process is described. This method involves the use of polymer frames and hinges, and aluminum oxide/chromium protection layers that reduce tensile, spatial, and surface tension stresses on the graphene-based membranes when the 2D nets are transformed into 3D cubes. The process offers control of the size and shape of the structures as well as parallel production. In addition, this approach allows the creation of surface modifications by metal patterning on each face of the 3D cubes. Raman spectroscopy studies show the method allows the preservation of the intrinsic properties of the graphene-based membranes, demonstrating the robustness of our method.

Figure 2&#160;displays optical images of the lithographic processes of the 2D graphene and GO net structures and subsequent self-folding process. The self-folding process is monitored in real-time via a high-resolution microscope. Both types of 3D graphene-based cubes are folded at ~80 &#176;C. Figure 3 lays out video captured sequences showing the self-folding of 3D graphene-based cubes in a parallel manner. Under an op...

Watch this Scientific Journal Video about Fabrication of Three-Dimensional Graphene-Based Polyhedrons via Origami-Like Self-Folding at JoVE.com

Fabrication of Three-Dimensional Graphene-Based Polyhedrons via Origami-Like Self-Folding

Here, we present a protocol for fabrication of 3D graphene-based polyhedrons via origami-like self-folding.

Fabrication of Three-Dimensional Graphene-Based Polyhedrons via Origami-Like Self-Folding

The assembly of two-dimensional (2D) graphene into three-dimensional (3D) polyhedral structures while preserving the graphene's excellent inherent ...

Research

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Engineering

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Fabrication of Uniform Nanoscale Cavities via Silicon Direct Wafer Bonding

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Atomically Traceable Nanostructure Fabrication

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Using Synchrotron Radiation Microtomography to Investigate Multi-scale Three-dimensional Microelectronic Packages

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