J. Semicond. > 2022, Volume 43 > Issue 6 > 061101, doi: 10.1088/1674-4926/43/6/061101
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Graphene synthesis, fabrication, characterization based on bottom-up and top-down approaches: An overview

Agbolade Lukman Olatomiwa1, 3, 4, Tijjani Adam1, 3, , Subash C. B. Gopinath2, 3, 5, Sanusi Yekinni Kolawole4, Oyeshola Hakeem Olayinka4 and U. Hashim3

+ Author Affiliations

 Corresponding author: tijjani@unimap.edu.my

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Abstract: This study presents an overview on graphene synthesis, fabrication and different characterization techniques utilized in the production. Since its discovery in 2004 by Andre Geim and Kostya Novoselov several research articles have been published globally to this effect, owing to graphene’s extraordinary, and exclusive characteristics which include optical transparency, excellent thermal, and mechanical properties. The properties and applications of this two-dimensional carbon crystal composed of single-layered material have created new avenues for the development of high-performance future electronics and technologies in energy storage and conversion for the sustainable energy. However, despite its potential and current status globally the difficulty in the production of monolayer graphene sheet still persists. Therefore, this review highlighted two approaches in the synthesis of graphene, which are the top-down and bottom-up approaches and examined the advantages and failings of the methods involved. In addition, the prospects and failings of these methods are investigated, as they are essential in optimizing the production method of graphene vital for expanding the yield, and producing high-quality graphene.

Key words: two-dimensional material, nanomaterial, carbon material, nanostructure



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Fig. 1.  (Color online) Structures of (a) 3D graphite, (b, c) 2D graphene and its edge, (d, e) graphene oxide, (f) reduced graphene oxide[22].

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Fig. 2.  (Color online) Top-down and bottom-up approaches for synthesis of graphene[23].

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Fig. 3.  Schematic diagram of the soluble salt assisted (Na2SO4) wet ball milling approach for synthesis of graphene nanosheet powder[36].

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Fig. 4.  (Color online) (a) Pure graphene. (b) Dry ice. (c) Edge-carboxylated graphite prepared by ball milling for 48 h. (d) Schematic view of physical cracking and edge-carboxylation of graphite by ball milling in the presence of dry ice, and protonation[38].

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Fig. 5.  (Color online) Schematic view: preparation of graphene oxide in laboratory designed ball mill[40].

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Fig. 6.  (Color online) Schematic view of tip sonication processing with parameters that influence graphene nanoplatelets dispersion in a liquid medium with obtained phenomena. (a) Fragmentation. (b) Exfoliation. (c) Defect[46].

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Fig. 7.  (Color online) Separation of graphitic oxide by sonication for 0.5 h.

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Fig. 8.  (Color online) Sonochemical synthesis of graphene oxide into graphene nanosheets in the presence NaOH[48].

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Fig. 9.  (Color online) Image of graphite flakes after electrochemical exfoliation. (b) Dispersed EG in DMF solution (concentration 2.5 mg/mL). (c) EG size on a bulk scale (163 g). (d) Diagrammatic representation of the principle of electrochemical exfoliation[53].

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Fig. 10.  (Color online) (a) Schematic view of the configuration used for face-to-face growth technique setup; (b) magnified view of the sample set up highlighted in panel (c) enlarged view of mounted SiC substrates highlighted by red lines in panel[64].

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Fig. 11.  (Color online) (a) Roll-to-roll process for the transfer of FLG from Ni foil to EVA/PET metal surface[76].

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Fig. 12.  (Color online) The graph of the sheet resistance versus the transmittance of the FLG/EVA/PET samples[76].

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Fig. 13.  (a) Pure VCCD-MWNT revealed the graphene helices released from the walls. (b) Milled for 1 h. (c, c’) Milled for 120 min[83].

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Fig. 14.  (Color online) Image of powder and the aqueous dispersion of graphene oxide (0.5 mg/mL) before (left) and after reduction (right)[104].

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Fig. 15.  SEM image of graphite-oxide[97].

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Fig. 16.  TEM images of graphite oxide[97].

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Fig. 17.  Plot of thermogravimetric analysis of (a) graphite oxide and (b) graphene[97]

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Fig. 18.  (Color online) Schematic view of the oxygen functionalities in GO and RGO [108].

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Table 1.   Indicating the different graphene produced using CVD method.

Metal surfacePressureTemp. (K)Size & shapeH2/CH4
(/Ar)		Methods or annealing pretreatmentMobility (cm2/(V·s))Growth timeReference
Cu foilLPCVD1308.150.5 × 10–3 m, dendrites2/1.3Inside surface of copper-foil enclosures4000 (e)[87] (2011)
Cu foilAPCVD1323.15~15 μm hexagonalH2/Ar, 10/300 CH4 in Ar 8 ppmH2/Ar, 10/ 300 sccm, 1323.15 K, 30 min annealing<103–104~0.167 h[88] (2011)
Cu foilLPCVD1350.15~2.3 × 10–3 m, ~4.5 × 10–6 m70/0.15High pressure annealing (1500 torr, 500 sccm H2, 1350.15 K, electrochemical polishing~110002.083 h[89] (2012)
Ni (111)UHV873.15–1073.15Millimeter sizePropylene ga(C3H6)Ni(111) hetero-epitaxially grown on MgO(111)
–		0.0833 h
[90] (2011)
Cu foilLPCVD1273.15100 μm, six-lobed flower12.5/10.667 h; vapor trapping4200; 20000 (hbn)0.5 h[91] (2012)
Liquid foilAPCVD1433.15>100 μm, hexagonal300/6200 sccm H2, 1373.15 K, 0.5 h1000–25000.5 h, 10–50 μm/min[92] (2012)
Liquid foilAPCVD1363.15>200 μm, hexagonal80/10, CH4:Ar, 1.99100 sccm (1.3 H2/Ar mix) 1090 °C, 0.5 h––[93] (2012)
Cu foilLPCVD1308.15Centimeter size10/0.10.1 torr H2, 1308.15, 0.5 h; 1 × 10–340000-65000 (1.7 K); 15000–30000 (r.t)12 h[94] (2013)
Cu foilAPCVD1273.1525 × 10–3 m diameter quartz10–15 sccm Ar, 600 sccm for H2, and 10–50 sccm for CH410–3700 (1273.15)0.333–0.16 h[95] (2011)
Cu foilLPCVD1308.15~2 × 10–3 m10/0.1Inside surface of Cu tube electroplating52006 h[96] (2013)
Cu foilLPCVD1273.15–
1318.15		0.25-inch-wide, 0.002 inch thick10/3151010 °C and a pressure of 533.289 pascals with flows of 100 sccm H2 in both the inner tube were changed to 300 sccm H2 for the tube gap25 mm/min (1273.15–
1318.15)		24 h[97] (2015)
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Table 2.   Different strategies on green synthesis of graphene.

SourcePreparationMorphologyAdvantagePropertiesApplicationRef.
citrullus colocynthis (leaf extract)RGO was prepared from graphite powder using the modifiedhummers methodStabilized
reduced graphene sheets		Low cost, facile, green method for deoxygenation of GO.Sharp diffraction peak
increase in interlayer spacing of GO		Anticancer drugs[110] (2017)
c. nucifera (cocos nucifera l.)Graphite oxide was prepared by oxidation of graphite with a mixture of sodium nitrate, concentrated ssulfuric acid and potassium chlorateSEM and TEM images showed transparent and stable layers towards electron beam. AFM showed the bi-layer graphene.Environmentally friendly
non-toxic reducing agent		Low surface charge densityBiological materials[111]
(2013)
Plants extracts (cherry, platanus, magnolia, persimmon, maple, pine and ginkgo).Graphene oxide was prepared using the modified hummers method, which was followed by ultrasonication.Reduced graphene oxideEnvironmentally friendlyIncrease in hydrophilicity which was caused by the reduction in polar functionality on the surface of the layersBiomedical applications[110] (2013)
Pomegranate juiceImproved hummers method was used to oxidize graphite for the synthesis of graphite oxide and followed by reduction of as-produced graphene oxide by pomegranate juice to form graphene nanosheetsSingle or few layer graphene sheetsFacile and green methodPresence of several oxygen containing group in the presence of graphene oxideBiological and optoelectronics.[109]
(2014)
Ascorbic acidModified hummers methodSingle layered graphene is 1 nm thick.Low cost, green and efficient method, naturally availableRemoval of oxygen functional groupWater purification[111]
(2017)
Wild carrot rootModified hummers methodFew layers grapheneEnvironmentally friendly reduction method, cost effectiveness, simple approachPartial removal of oxygen functionalityElectronic devices[112]
(2012)
Lime juice (citrus aurantifolia)The oxidization of graphite using hummers method to form GO and then the graphene oxide was reduced where lime was used as the natural reducing agentsReduced graphene oxideLow cost, environmentally benign methodThe high intensity of the main peak in GO shows a sizeable number of oxygen containing groups, which occur after the deposition.Biological materials[113]
(2019)
magnifera indicaMango leaves was cut down into tiny pieces (1–2 cm) and dipped in ethanolFew layers grapheneEnvironmentally friendly, scalable, far and green method.Biocompatible, photostable, excellent cellular uptake, good resolutionBiomedical nanotechnology applications[114]
(2016)
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Table 3.   Different ways of synthesis for graphene.

MethodSizeAdvantageDisadvantageApplicationRef.
Epitaxial growth50 μmHigh quality, suitable for electronicsHighly expensive, low yield, wafer size, introduces voids in the transfer processField effect transistors, photodetectors[115,116]
Chemical vapor deposition0.2–10 μmHigh quality and mass production, easy to transfer to other materials.The use of harmful oxidizer or carboxylic acids, cost of the substrates may be high. The formation of graphene via high temperature on metal surface.Electronics: light emitting diode, biosensors[117,118]
Green synthesis200–800 nmLow cost, facile (simple), Green method for deoxygenation of GO, reduces waste, the use of harmless solvent, suitable for large scale production of graphene nanoparticles, high temperature and pressure are not required, environmentally friendlyDye removal, electrochemical storage, Photocatalysis[119,120]
Mechanical exfoliation5–10 nmCost effective, high quality graphene layers and laborsavingLow yield, defects and in the flakes produce are inconsistent.Space protection, energy[121,122]
Electrochemical exfoliation2–3 nmHigh quality single layerDifficulty in removing the surfactants molecules, inconsistency in the produced graphene layerSupercapacitors, batteries[118,119]
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    Received: 17 November 2021 Revised: 23 December 2021 Online: Accepted Manuscript: 12 February 2022Uncorrected proof: 19 February 2022Published: 06 June 2022

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      Article Navigation >  Journal of Semiconductors  > 2022  >  43(6): 061101
      Agbolade Lukman Olatomiwa, Tijjani Adam, Subash C. B. Gopinath, Sanusi Yekinni Kolawole, Oyeshola Hakeem Olayinka, U. Hashim. Graphene synthesis, fabrication, characterization based on bottom-up and top-down approaches: An overview[J]. Journal of Semiconductors, 2022, 43(6): 061101. doi: 10.1088/1674-4926/43/6/061101 A L Olatomiwa, T Adam, S C B Gopinath, S Y Kolawole, O H Olayinka, U Hashim. Graphene synthesis, fabrication, characterization based on bottom-up and top-down approaches: An overview[J]. J. Semicond, 2022, 43(6): 061101. doi: 10.1088/1674-4926/43/6/061101Export: BibTex EndNote
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      Agbolade Lukman Olatomiwa, Tijjani Adam, Subash C. B. Gopinath, Sanusi Yekinni Kolawole, Oyeshola Hakeem Olayinka, U. Hashim. Graphene synthesis, fabrication, characterization based on bottom-up and top-down approaches: An overview[J]. Journal of Semiconductors, 2022, 43(6): 061101. doi: 10.1088/1674-4926/43/6/061101

      A L Olatomiwa, T Adam, S C B Gopinath, S Y Kolawole, O H Olayinka, U Hashim. Graphene synthesis, fabrication, characterization based on bottom-up and top-down approaches: An overview[J]. J. Semicond, 2022, 43(6): 061101. doi: 10.1088/1674-4926/43/6/061101
      Export: BibTex EndNote
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      Graphene synthesis, fabrication, characterization based on bottom-up and top-down approaches: An overview

      doi: 10.1088/1674-4926/43/6/061101
      • 1.

        Faculty of Electronic Engineering Technology, Universiti Malaysia Perlis, 02600 Arau, Perlis, Malaysia

      • 2.

        Faculty of Chemical Engineering Technology, Universiti Malaysia Perlis, 02600 Arau, Perlis, Malaysia

      • 3.

        Institute of Nano Electronic Engineering, Universiti Malaysia Perlis, Perlis, Malaysia

      • 4.

        Pure and Applied Physics, Ladoke Akintola University of Technology, Nigeria

      • 5.

        Centre of Excellence for Nanobiotechnology and Nanomedicine (CoExNano), Faculty of applied Sciences, AIMST University, Semeling, 08100 Kedah, Malaysia

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      • Author Bio:

        Agbolade Lukman Olatomiwa is a master student at Institute Nano Electronic Engineering, Universiti Malaysia Perlis. He received his BS from Ladoke Akintola University of Technology in 2019. His research focuses on graphene solar cells

        Tijjani Adam is a lecturer at Universiti Malaysia Perlis. He received his PhD from Institute Nano Electronic Engineering, Universiti Malaysia Perlis in 2015. His research focuses on nanomaterials and devices

      • Corresponding author: tijjani@unimap.edu.my
      • Received Date: 2021-11-17
      • Accepted Date: 2022-01-22
      • Revised Date: 2021-12-23
        • Available Online: 2022-04-24

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