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A method for obtaining flat n-graphene sheets using reverse exfoliation process V. Huc, IPCMO, Orsay N. Bendiab, LSP-UJF, Grenoble T. Ebbesen, U .Pasteur, Strasbourg C. Delacour, V. Bouchiat, Institut Néel, CNRS- Grenoble
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A method for obtaining flat n-graphene sheets using reverse exfoliation process V. Huc, IPCMO, Orsay N. Bendiab, LSP-UJF, Grenoble T. Ebbesen, U.Pasteur,

Dec 20, 2015

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Page 1: A method for obtaining flat n-graphene sheets using reverse exfoliation process V. Huc, IPCMO, Orsay N. Bendiab, LSP-UJF, Grenoble T. Ebbesen, U.Pasteur,

A method for obtaining flat n-graphene sheets

using reverse exfoliation process

V. Huc, IPCMO, OrsayN. Bendiab, LSP-UJF, Grenoble

T. Ebbesen, U .Pasteur, StrasbourgC. Delacour, V. Bouchiat, Institut Néel, CNRS- Grenoble

Page 2: A method for obtaining flat n-graphene sheets using reverse exfoliation process V. Huc, IPCMO, Orsay N. Bendiab, LSP-UJF, Grenoble T. Ebbesen, U.Pasteur,

Deposited Graphene layers exhibits defects : pleats and folds

Novoselov, Geim group

lowered carrier mobility and suppression ofweak localization in graphene-based devices have beenattributed to corrugation of the graphene.

Page 3: A method for obtaining flat n-graphene sheets using reverse exfoliation process V. Huc, IPCMO, Orsay N. Bendiab, LSP-UJF, Grenoble T. Ebbesen, U.Pasteur,

Masa Ishigami, et al. Nano Lett. ASAP paper 11-May-2007

Novoselov, Geim group

Meyer, J. C.; et al. On the roughness of single- and bi-layer graphenemembranes. Preprint archive, xxx.lanl.gov, cond-mat/0703033, 2007.

Page 4: A method for obtaining flat n-graphene sheets using reverse exfoliation process V. Huc, IPCMO, Orsay N. Bendiab, LSP-UJF, Grenoble T. Ebbesen, U.Pasteur,

Step 1 : Bulk HOPG Bonding (upside down)

Oxidized Silicon chipFreshsly cleaved

Bulk HOPG

Epoxy glue

Epoxy glue

Reverse Exfoliation Process

Page 5: A method for obtaining flat n-graphene sheets using reverse exfoliation process V. Huc, IPCMO, Orsay N. Bendiab, LSP-UJF, Grenoble T. Ebbesen, U.Pasteur,

Reverse Exfoliation Process

Epoxy glue

Epoxy glue

Step 1 : Bulk HOPG Bonding (upside down)

Adhesive wafer bondingF. Niklaus et al. Appl. Phys. 99, 031101 , 2006

Page 6: A method for obtaining flat n-graphene sheets using reverse exfoliation process V. Huc, IPCMO, Orsay N. Bendiab, LSP-UJF, Grenoble T. Ebbesen, U.Pasteur,

Molding of the top Graphite surface into the epoxy

Page 7: A method for obtaining flat n-graphene sheets using reverse exfoliation process V. Huc, IPCMO, Orsay N. Bendiab, LSP-UJF, Grenoble T. Ebbesen, U.Pasteur,

Step 2 : epoxy curing under screw press

Reverse Exfoliation Process

Page 8: A method for obtaining flat n-graphene sheets using reverse exfoliation process V. Huc, IPCMO, Orsay N. Bendiab, LSP-UJF, Grenoble T. Ebbesen, U.Pasteur,

Oxidized Silicon chip

Epoxy glue

Epoxy glue

Reverse Exfoliation Process

Bulk HOPG

Step 3 : Bulk HOPG Scalpel Cleaving

Page 9: A method for obtaining flat n-graphene sheets using reverse exfoliation process V. Huc, IPCMO, Orsay N. Bendiab, LSP-UJF, Grenoble T. Ebbesen, U.Pasteur,

Oxidized Silicon chip

Epoxy glue

Epoxy glue

Bulk HOPG

Step 4 : Scotch™ tape exfoliation

K.S. Novoselov et al;, Science 306, 666 , (2004).

Page 10: A method for obtaining flat n-graphene sheets using reverse exfoliation process V. Huc, IPCMO, Orsay N. Bendiab, LSP-UJF, Grenoble T. Ebbesen, U.Pasteur,

Coupe au niveau d’une bulle

Si

EpoxyGlue

grapheneÉpaisseurÉpaisseurColle = 3µmColle = 3µm

Page 11: A method for obtaining flat n-graphene sheets using reverse exfoliation process V. Huc, IPCMO, Orsay N. Bendiab, LSP-UJF, Grenoble T. Ebbesen, U.Pasteur,

A process reminiscent from the Smart-cut ® process

Atomic scalpel

US Patent 5,882,987, published 1999

Page 12: A method for obtaining flat n-graphene sheets using reverse exfoliation process V. Huc, IPCMO, Orsay N. Bendiab, LSP-UJF, Grenoble T. Ebbesen, U.Pasteur,

A process reminiscent from the Smart-cut ® process

Atomic scalpel

US Patent 5,882,987, published 1999

Bernin

Page 13: A method for obtaining flat n-graphene sheets using reverse exfoliation process V. Huc, IPCMO, Orsay N. Bendiab, LSP-UJF, Grenoble T. Ebbesen, U.Pasteur,

Image d’une fissure de contrainte (colle dans la fissure)

Page 14: A method for obtaining flat n-graphene sheets using reverse exfoliation process V. Huc, IPCMO, Orsay N. Bendiab, LSP-UJF, Grenoble T. Ebbesen, U.Pasteur,

pleats defects

Page 15: A method for obtaining flat n-graphene sheets using reverse exfoliation process V. Huc, IPCMO, Orsay N. Bendiab, LSP-UJF, Grenoble T. Ebbesen, U.Pasteur,

SEM zoom on Pleats defects

Page 16: A method for obtaining flat n-graphene sheets using reverse exfoliation process V. Huc, IPCMO, Orsay N. Bendiab, LSP-UJF, Grenoble T. Ebbesen, U.Pasteur,

Graphene on epi SiC (GaTech U.) :

same kind of pleats

1µm

Page 17: A method for obtaining flat n-graphene sheets using reverse exfoliation process V. Huc, IPCMO, Orsay N. Bendiab, LSP-UJF, Grenoble T. Ebbesen, U.Pasteur,
Page 18: A method for obtaining flat n-graphene sheets using reverse exfoliation process V. Huc, IPCMO, Orsay N. Bendiab, LSP-UJF, Grenoble T. Ebbesen, U.Pasteur,

Effective surface potentialSonde de Kelvin

Scanning Potential Microscopy

Page 19: A method for obtaining flat n-graphene sheets using reverse exfoliation process V. Huc, IPCMO, Orsay N. Bendiab, LSP-UJF, Grenoble T. Ebbesen, U.Pasteur,

Lift height = 5 nm Tip bias = 2V 6 µm Scan

Page 20: A method for obtaining flat n-graphene sheets using reverse exfoliation process V. Huc, IPCMO, Orsay N. Bendiab, LSP-UJF, Grenoble T. Ebbesen, U.Pasteur,

Raman Probing The Raman spectrum of graphite is composed of a strong band at 1582 cm-1, which has been assigned to the in-plane E2g zone centre mode (G band).

Gupta et al. Nano Lett., Vol. 6, No. 12, 2006 p.2668

Page 21: A method for obtaining flat n-graphene sheets using reverse exfoliation process V. Huc, IPCMO, Orsay N. Bendiab, LSP-UJF, Grenoble T. Ebbesen, U.Pasteur,

Raman Probing The Raman spectrum of graphite is composed of a strong band at 1582 cm-1, which has been assigned to the in-plane E2g zone centre mode (G band).

G-band clearly downshifts with increasing n

Gupta et al. Nano Lett., Vol. 6, No. 12, 2006 p.2668

Page 22: A method for obtaining flat n-graphene sheets using reverse exfoliation process V. Huc, IPCMO, Orsay N. Bendiab, LSP-UJF, Grenoble T. Ebbesen, U.Pasteur,

Raman Probing The Raman spectrum of graphite is composed of a strong band at 1582 cm-1, which has been assigned to the in-plane E2g zone centre mode (G band).

G-band clearly downshifts with increasing n

Gupta et al. Nano Lett., Vol. 6, No. 12, p.2668 2006A. C. Ferrari, et al. Phys. Rev. Lett. 97, 187401 (2006).

Page 23: A method for obtaining flat n-graphene sheets using reverse exfoliation process V. Huc, IPCMO, Orsay N. Bendiab, LSP-UJF, Grenoble T. Ebbesen, U.Pasteur,

Raman as a way to assess single graphene layers

Gupta et al. Nano Lett., Vol. 6, No. 12, 2006 p.2668

Page 24: A method for obtaining flat n-graphene sheets using reverse exfoliation process V. Huc, IPCMO, Orsay N. Bendiab, LSP-UJF, Grenoble T. Ebbesen, U.Pasteur,

Raman micro-spectroscopy

MicroRaman spectra are collected using a X100 objective with a spot size of 1m using 514.5 nm excitation under ambient conditions at low laser power (<1mW).

Page 25: A method for obtaining flat n-graphene sheets using reverse exfoliation process V. Huc, IPCMO, Orsay N. Bendiab, LSP-UJF, Grenoble T. Ebbesen, U.Pasteur,

• Marche monocouche

• Colle ? Bulle

AFM sur Zone Raman Monocouche (2)

Page 26: A method for obtaining flat n-graphene sheets using reverse exfoliation process V. Huc, IPCMO, Orsay N. Bendiab, LSP-UJF, Grenoble T. Ebbesen, U.Pasteur,

AFM sur Zone Raman Monocouche (2)

1 µm

Page 27: A method for obtaining flat n-graphene sheets using reverse exfoliation process V. Huc, IPCMO, Orsay N. Bendiab, LSP-UJF, Grenoble T. Ebbesen, U.Pasteur,

Fissure de contrainte ?

2 µm

Page 28: A method for obtaining flat n-graphene sheets using reverse exfoliation process V. Huc, IPCMO, Orsay N. Bendiab, LSP-UJF, Grenoble T. Ebbesen, U.Pasteur,

Reconnection using Pd

100 µm

Page 29: A method for obtaining flat n-graphene sheets using reverse exfoliation process V. Huc, IPCMO, Orsay N. Bendiab, LSP-UJF, Grenoble T. Ebbesen, U.Pasteur,

Contacts Pd/Graphene

5 µm

Page 30: A method for obtaining flat n-graphene sheets using reverse exfoliation process V. Huc, IPCMO, Orsay N. Bendiab, LSP-UJF, Grenoble T. Ebbesen, U.Pasteur,

Conclusion :

Reverse exfoliation make possible the realization of flat graphene sheets

Page 31: A method for obtaining flat n-graphene sheets using reverse exfoliation process V. Huc, IPCMO, Orsay N. Bendiab, LSP-UJF, Grenoble T. Ebbesen, U.Pasteur,

PRL98,166802(2007)