Graphene Syntheis and Characterization for Raman Spetroscopy At High Pressure
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Graphene Syntheis and Characterization for Raman Spetroscopy At High Pressure

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Master Thesis Presentation, made 2009-09-04 in Luleå.

Master Thesis Presentation, made 2009-09-04 in Luleå.

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  • Young’s Modulus ~1TPa / High toughness-to-weight ratio / High e - and heat conductance (ballistic) All these come from GRAPHENE !!
  • 2D does not exist : Start with the bonds, get from graphite to graphene, why it is excellent
  • Young 1GPA; Thermal 50times diamond;
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Graphene Syntheis and Characterization for Raman Spetroscopy At High Pressure Presentation Transcript

  • 1. Single- and Double-Layer Graphene for in-situ High-Pressure Raman scattering Synthesis and Characterization of Carbon-based Nanomaterials Nicolas MORAL Supervisor: Pr. Alexander SOLDATOV High-Pressure Spectroscopy Laboratory Division of Physics, Luleå Tekniska Universitet, 971 87 Luleå, SWEDEN Department of Applied Physics and Mechanical Engineering
  • 2. Table of contents
    • Introduction
      • Carbon-based Nanomaterials
      • Resonance Raman Scattering
      • High-Pressure experiments
    • Review & Motivation
    • Methods and Materials
      • 2 routes to graphene at High-Pressure
    • Results & Discussions
    • Conclusion
  • 3. Introduction Carbon-based Nanomaterials Raman scattering High-Pressure
  • 4. Carbon-based Nanomaterials
    • Carbon NanoTubes (CNTs)
      • ~1D objects (1*1000 nm)
        • High property-to-weight ratios
      • Applications
        • Composites, Nanoelectronics, Heat transfer
        • Fuel cells and drug delivery
    • Fullerenes
      • ~0D objects ( ø 0.7nm)
      • Applications
        • Nanoelectronics, Transistors
        • Catalyst for diamond production
  • 5. Graphene
    • Graphite, Graphene
      • Single-Layer graphene
        • 2D object
        • One-atom-thick
        • Sp² bonds
        • Honeycomb lattice
      • Origin of other Carbon allotropes
        • Cylinder = CNT
        • Sphere = Fullerenes
        • Stacks = Graphite
  • 6. Graphene
    • Graphene
      • Properties
        • Young’s modulus 0.5 TPa
        • “ high” optical opacity (2.3%)
        • High thermal conductivity (10 3 W.m -1 .K -1 )
        • Ballistic thermal/electronic behavior
        • Quantum Hall effect
  • 7. Graphene
    • Graphene
      • Applications
        • Nanoribbons and spintronics
        • Ultracapacitors
        • Single-molecule detection
        • Bio-devices
  • 8. Introduction Carbon-based Nanomaterials Raman scattering High-Pressure
  • 9. Raman scattering
    • Principle
      • Laser excitation ν 0
      • Phonons scattering Rayleigh ν 0 + Raman ν 0 ± ν m
      • Resonance Raman
  • 10. Raman Scattering
  • 11. High-Pressure
    • Principle
      • Diamond Anvil Cell
        • Simple equipment
        • High pressures (up to 50GPa)
    • Objective
      • SLG: probe the hardest bond in the world, sp² in 2D
      • DLG: experiment the isolated interplane interaction
  • 12. Motivation of the thesis Preparation of in-situ HP Resonance Raman Spectroscopy
  • 13. Motivation of the thesis
    • Synthesis of Graphene
      • SLG, DLG, FLG; reliable and reproducible
    • Characterization of Graphene
      • Optical Microscope
      • Atomic Force Microscope
      • Electronic Microscope
      • Raman
  • 14. Methods and materials Source Materials, Equipment, Protocols
  • 15. Methods and Materials
    • References samples (courtesy of Dr K. Novoselov, Manchester)
      • Graphene on SiO 2 (tape method)
    • Source Material
      • Supported Graphene
        • Si/SiO 2 substrates
        • Mechanical exfoliation = “Tape Method”
      • Free-Standing Graphene
        • Cu grid
        • Epitaxially grown
  • 16. Methods and Materials
    • Equipment: Optical Microscope
      • Olympus BX51
      • 10X, 20X, 100X magnifications
    • Equipment: Atomic Force Microscope
      • AFM/STM NT-MDT Ntegra
    • Equipment: Scanning Electron Microscope
      • Materialteknik Jeol JSM 6460LV
  • 17. Methods and Materials
    • Equipment: Raman stage
      • WiTec confocal Raman imaging system CRM200
        • High signal-to-noise ratio
        • 1cm -1 resolution
      • Lasers
        • Green 532nm (2.33eV) _ SpectraPhysics Millenium IV
          • Powers 200mW up to 5W – 15mW on stage
          • Power densities up to 300 kW/cm²
        • Red 632.8nm (1.96eV) _ Coherent
          • Powers up to 50mW – 8mW on stage
          • Power densities up to 150 kW/cm²
  • 18. Methods and Materials
  • 19. Methods and Materials
    • First route: Supported Graphene
      • Deposition cycle: Substrates cleaning / exfoliation / deposition
      • Optical observation / substrate mapping
      • Spectral confirmation
      • Transfer into the DAC of SPECIFIC flakes (SLG/DLG)
    • Second route: Free-Standing Graphene
      • Provided by Manchester University’s collaborator
        • Macroscopic sample ( ø3 mm)
      • Transfer into the DAC
  • 20. Methods and Materials Route 1: Supported Graphene Route 2: Free-Standing Graphene
  • 21. Methods and Materials
  • 22. Methods and Materials
    • Optical observation
      • Specific optical interference thanks to Si/SiO2 substrate
    • Spectral confirmation
      • Using Raman spectra and comparison to reference samples
    • Transfer
      • Protocol involving HoleyCarbonFilms (Quantifoil ™)
  • 23. Methods and Materials
  • 24. Methods and Materials
  • 25. Methods and Materials
    • Loading into the DAC
      • “ Sandwiching” the flake
      • Cutting the sandwich (sample chamber <200µm)
      • Loading into the DAC
        • Pressure-transmitting medium: ethanol-methanol
  • 26. Methods and Materials Route 1: Supported Graphene Route 2: Free-Standing Graphene
  • 27. Methods and Materials
    • Source Material: Free-Standing Single-Layer Graphene
      • Epitaxial growth on Ni substrate
      • Covered by PMMA
      • Ni etching in acid
      • PMMA-SLG fishing with Copper grid
      • PMMA etching in acetone
    • Loading into the DAC
      • Sandwich method
  • 28. Methods and Materials 100 µm
  • 29. Results and discussions
      • Route 1: Supported Graphene
      • Deposition Cycle
      • Optical Observation
      • Spectral Confirmation
      • Transfer
      • Route 2
  • 30. Supported Graphene
    • Substrates cleanliness
      • Crucial step for successful deposition
    • Deposition optimization
      • Tape selection
      • Exfoliation method
        • Optimal = small crumbs
      • Deposition method
        • Pressing/rubbing/etching
        • Optimal = rubbing
  • 31. Conclusion
    • Step 1: COMPLETE
      • Fast deposition cycle (10-20 samples a day)
      • Reproducible results
      • To be optimized ?
        • Increased average flakes’ size might be possible
  • 32. Results and discussions
      • Route 1: Supported Graphene
      • Deposition Cycle
      • Optical Observation
      • Spectral Confirmation
      • Transfer
      • Route 2
  • 33. Optical observation
    • Finding the flake(s)
    • Identification (contrast)
      • SLG
      • DLG
      • FLG
      • MLG
      • Graphite
    • Substrate mapping
  • 34. Optical observation Graphite Glue DLG ? FLG MLG SLG ?
  • 35. Results and discussions
      • Route 1: Supported Graphene
      • Deposition Cycle
      • Optical Observation
      • Spectral Confirmation (reference spectra)
      • Transfer
      • Route 2
  • 36. Reference spectra
    • Manchester’s graphene on SiO 2
      • SLG
      • DLG
      • FLG
      • Comparison to Graphite reference (NG)
  • 37. Reference spectra
  • 38. Reference spectra
  • 39. Reference spectra
  • 40. Conclusion
    • Reference samples characterization
      • Clear identification of the main 3 target samples is possible
        • SLG
        • DLG
        • FLG
        • Gprime is a fingerprint (shape and peak-fitting)
        • G’/G ratio is also used
      • Transpose to our graphene samples
  • 41. Results and discussions
      • Route 1: Supported Graphene
      • Deposition Cycle
      • Optical Observation
      • Spectral Confirmation (deposited samples)
      • Transfer
      • Route 2
  • 42. Spectral confirmation
    • Raman spectrum
      • Red laser
        • SLG
  • 43. Spectral confirmation
    • Raman spectrum
      • Red laser
        • DLG
  • 44. Spectral confirmation
    • Raman spectrum
      • Red laser
        • 3LG
  • 45. Spectral confirmation
    • Raman spectrum
      • Green laser
        • SLG
  • 46. Spectral confirmation
  • 47. Spectral confirmation
    • Raman spectrum
      • Green laser
        • DLG
  • 48. Spectral confirmation
  • 49. Spectral confirmation
  • 50. Spectral confirmation
    • SLG samples
      • Red laser
        • single peak G’ = 2630 cm -1
        • FWHM = 24 cm -1
        • G’/G ratio >> 1
      • Green laser
        • Single peak G’ = 2670 cm -1
        • FWHM = 26 cm -1
        • G’/G ratio >> 1
      • SLG identification complete and identical to literature reviews
  • 51. Spectral confirmation
  • 52. Spectral confirmation
    • DLG samples
      • Red laser
        • G’ peak = 4peaks
        • FWHM ≈ 24 cm -1
        • G’/G ratio ≈ 1
      • Green laser
        • G’ peak = 4peaks
        • FWHM ≈ 24 cm -1
        • G’/G ratio ≈ 1
      • DLG identification complete and identical to literature reviews
  • 53. Conclusion
    • Step 2: COMPLETE
      • Characterization of produced samples
        • Non-destructive
        • Fast spectra
        • Peak-fitting software = reliable results
        • SLG / DLG / FLG
  • 54. Results and discussions
      • Route 1: Supported Graphene
      • Deposition Cycle
      • Optical Observation
      • Spectral Confirmation (deposited samples)
      • Transfer
      • Route 2
  • 55. Transfer
    • Method 1: IPA
      • Lifting the “grid/film & flake” off the substrate with IPA
      • Unsuccessful so far:
        • Grids’ stiffness
    • Method 2: KOH
      • Etching the SiO 2 layer off
      • Unsuccessful so far:
        • Flakes swim away
  • 56. Conclusion
    • Route 1: Supported Graphene
      • Step 1: DEPOSITION COMPLETE
      • Step 2: CHARACTERIZATION COMPLETE
      • Step 3: Transfer incomplete
  • 57. Results and discussions
      • Route 1
      • Route 2: Free-Standing Graphene
      • Characterization
      • Transfer
  • 58. Free-Standing Graphene
  • 59. Free-Standing Graphene
  • 60. Free-Standing Graphene
  • 61. Conclusion
    • FSG characterization COMPLETE
      • With both lasers
      • Similar results to supported graphene
        • Dirtier (Dband, lots of graphitic dirt)
      • With 20X objective = ready-to-load at High Pressure
  • 62. Results and discussions
      • Route 1
      • Route 2: Free-Standing Graphene
      • Characterization
      • Transfer
  • 63. Transfer
    • Samples size reduction: IN PROGRESS
      • First cuts successful, without damage/alteration
      • Down to 100 µm so far
      • FS SLG damaged
  • 64. Transfer
  • 65. Conclusion
    • Route 2: Free-Standing Graphene
      • Step 1: CHARACTERIZATION COMPLETE
        • SLG available for transfer
        • DLG is missing as a free-standing sample
      • Step 2: Transfer incomplete
  • 66. Summary of Conclusions Route 1: Supported Graphene Route 2: Free-Standing Graphene
  • 67. Summary of Conclusions
    • Synthesis of target samples COMPLETE
      • Supported SLG / DLG
        • “ tape” method
        • Fast, reproducible, reliable
      • Free-Standing SLG available
    • Characterization of available samples COMPLETE
      • Supported SLD / DLG / 3LG
      • Free-Standing SLG
  • 68. Future Work
    • Synthesis
      • Get Free-Standing DLG
      • Optimizing the deposition cycle
    • Characterization
      • Correlate spectra with AFM measurements
    • Transfer
      • Complete loading for both routes
  • 69. Future Work Gband 1580cm -1 (intensity a.u.) G’band 2670cm -1 (intensity a.u.) Gband G’band
  • 70. Acknowledgements
    • Pr Alexander SOLDATOV
      • Supervisor, LTU
    • Dr Kostya NOVOSELOV
      • University of Manchester (UK)
    • My saviors
      • Zoubir Ayadi, EEIGM (France)
      • Lennart Wallström, LTU
    • My colleagues
      • Dr Shujie You
      • Illya Dobryden, PhD
      • Murat Özturk, project student
      • Johnny Grahn, Johanne Mouzon Nils Almqvist
      • David Olevik & Mattias Mases
  • 71. Thank you for your attention Please address your questions NOW !
  • 72.