A New Industrially Relevant Route to
High Quality Graphene
Paul Ladislaus
Advanced Materials Division
HVM Graphene+ 2014 C...
Thomas	
  Swan	
  &	
  Co.	
  Ltd.	
  
•  Independently	
  owned	
  
•  Medium	
  sized	
  enterprise	
  (SME)	
  
•  168	...
Performance	
  Chemicals	
  
•	
  Proven	
  reliability	
  in	
  tyre	
  &	
  rubber,	
  coaGng	
  addiGves	
  &	
  
	
  h...
Our	
  CapabiliGes	
  
• Established	
  manufacturing	
  
infrastructure	
  
• Capital	
  Engineering	
  
• Quality	
  Con...
Advanced	
  Materials	
  Division	
  
Reliability	
  &	
  Quality	
  in	
  carbon	
  nanomaterials.	
  
	
  
	
  
Advanced	
  Materials	
  –	
  Carbon	
  Nanotubes	
  
Elicarb®	
  Carbon	
  Nanotubes:	
  
Single	
  wall	
  (SW)	
  and	
...
Elicarb®	
  SW	
  products	
  
•  Elicarb®	
  SW	
  and	
  Elicarb®	
  SW	
  Low	
  Residue	
  are	
  market	
  leading	
 ...
Elicarb®	
  MW	
  products	
  
•  Elicarb®	
  MW	
  is	
  a	
  specialist	
  MWNT	
  product	
  which	
  Thomas	
  Swan	
 ...
Advanced	
  Materials	
  –	
  Graphene	
  
	
  
•  Thomas	
  Swan	
  selected	
  liquid	
  phase	
  
exfoliaGon	
  of	
  g...
Graphene	
  -­‐	
  TCD	
  Lab	
  Exfoliated	
  
Graphene	
  platelets	
  produced	
  by	
  
liquid	
  phase	
  exfoliaOon	...
TCD	
  -­‐	
  High	
  Shear	
  Liquid	
  ExfoliaGon	
  
• Liquid	
  phase	
  exfoliaGon	
  by	
  high	
  
shear	
  mixing....
2 4
Re / 10Mixer ND ρ η= =
Turbulence
!γ ≈
π DN
d
=104
s−1
Minimum	
  shear	
  rate	
  more	
  important	
  than	
  turbul...
Scale	
  Up	
  Parameters	
  are	
  Available	
  
GeneraGon	
  of	
  Significant	
  Public	
  Interest	
  
Thomas	
  Swan	
  Elicarb®	
  Graphene	
  	
  
Raman	
  spectra	
  of	
  Elicarb®	
  Graphene	
  Powder	
  
(514	
  nm	
  ...
Thomas	
  Swan	
  Elicarb®	
  Graphene	
  	
  
TEM	
  analysis	
  of	
  	
  typical	
  	
  Elicarb®	
  Graphene	
  Powders...
Thomas	
  Swan	
  Elicarb®	
  Graphene	
  	
  
TEM	
  Image	
  	
  parOcle	
  size	
  analysis	
  of	
  Elicarb®	
  
Graph...
Thomas	
  Swan	
  Elicarb®	
  Graphene	
  	
  
Sheet	
  Resistance:	
  
•  4	
  point	
  probe	
  
•  Filtered	
  solids	
...
Summary:	
  Elicarb®	
  Graphene	
  Products	
  	
  
•  We	
  have	
  developed	
  a	
  scalable	
  route	
  to	
  prisGne...
Follow	
  up	
  QuesGons	
  
Many	
  thanks	
  for	
  your	
  aeenGon.	
  
I	
  am	
  happy	
  to	
  answer	
  quesGons.	
...
Advanced	
  Materials	
  Division	
  
Reliability	
  &	
  Quality	
  in	
  carbon	
  nanomaterials.	
  
	
  
	
  
Appendix	
  
Nanomaterial	
  Safety	
  &	
  Regulatory	
  
ConGnuing	
  safe	
  commercialisaGon	
  of	
  new	
  nanomaterials	
  remai...
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www.hvm-uk.com 2014 Talk at HVM Graphene+ Oxford

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Hvmg14oladislaus

  1. 1. A New Industrially Relevant Route to High Quality Graphene Paul Ladislaus Advanced Materials Division HVM Graphene+ 2014 Conference Oxford, United Kingdom 15 May 2014 www.hvm-uk.com
  2. 2. Thomas  Swan  &  Co.  Ltd.   •  Independently  owned   •  Medium  sized  enterprise  (SME)   •  168  employees   •  ca.  £27M  revenue  (2012/13)   •  UK  manufacturing  base   •  Conse=,  Co.  Durham,UK.   •  Export  performance   •  UK/EU/Outside  EU   •  Commitment  to  highest  standards    
  3. 3. Performance  Chemicals   •  Proven  reliability  in  tyre  &  rubber,  coaGng  addiGves  &    household  care.     Custom  Manufacture   •  Flexible  and  responsive  with  over  100  custom   manufacturing  products.     Advanced  Materials   •  Excited  by  new  opportuniOes  for  high  performance   materials  in  emerging  markets.     Thomas  Swan  Group   •  AppeOte  for  venturing  and  early  investors  in  new    technologies.   Our  Business   Performance Chemicals / Custom Manufacture / Advanced Materials
  4. 4. Our  CapabiliGes   • Established  manufacturing   infrastructure   • Capital  Engineering   • Quality  Control   • Environmental  Control   • Scheduling/LogisGcs   • Regulatory  Affairs   • Process  Engineering     • Process  design  and  piloGng   • Flexible  chemistries   • Proven  scale-­‐up  experience   • Underpinned  by  recognised   accreditaGons   • ISO  9001   • ISO  14001   • OHSAS  18001   • Responsible  Care   …….and  Customer  Care  excellence.  
  5. 5. Advanced  Materials  Division   Reliability  &  Quality  in  carbon  nanomaterials.      
  6. 6. Advanced  Materials  –  Carbon  Nanotubes   Elicarb®  Carbon  Nanotubes:   Single  wall  (SW)  and  mulO-­‐wall  (MW)  products:   From  iniGal  investments  with  the  University  of   Cambridge  in  2004  to  .......   •  World  leading  SW  manufacturing  capability.   •  Scaled  to  support  both  exisGng  and  emerging    opportuniGes.   •  Proven  ability  to  supply  mulG-­‐kg  quanGGes  at    compeGGve  pricing  to  global  customers.    •  high  quality  nanotubes    •  low  catalyst  residues    •  high  surface  area           500kg/yr  washing  facility  for  Elicarb®  SW  Low  Residue   products  at  Thomas  Swan's  Consee  site.    
  7. 7. Elicarb®  SW  products   •  Elicarb®  SW  and  Elicarb®  SW  Low  Residue  are  market  leading  SWNT   products  for  advanced  electronics.   Raman  shows  high  graphiGc  carbon  content   TGA  shows  high  carbon  content   SEM  shows  high  SW  carbon   nanotube  content.   TEM  shows  high  SWNT  &  DWNT   content.  
  8. 8. Elicarb®  MW  products   •  Elicarb®  MW  is  a  specialist  MWNT  product  which  Thomas  Swan  provides  in   development  &  prototyping  quanGGes.   Raman  shows  typical  MW  graphiGc  carbon  content   TGA  shows  high  carbon  content   SEM  shows    high  MW   carbon  nanotube  content.   TEM  shows  mulG-­‐wall   structure.  
  9. 9. Advanced  Materials  –  Graphene     •  Thomas  Swan  selected  liquid  phase   exfoliaGon  of  graphite  as  a  route  to   graphene.   •  Aiming  for  Graphene  Nanoplatelets  which   are  substanGally  non-­‐oxidised  with  no   catalyst  residues.   •  Process  developed  in  collaboraGon  with   Prof.  J.  Coleman  at  CRANN,  Trinity  College   Dublin  (TCD).   •  Exclusively  licensed  to  Thomas  Swan  &  Co.   Ltd.   •  Target  applicaGons  include:   •  ConducGve  inks   •  Super-­‐capacitors  &  baeeries   •  Barrier  &  separaGons   •  Thermal  management   Elicarb®  Graphene:     “Industrially  relevant  route  to  high   quality  graphene”.      
  10. 10. Graphene  -­‐  TCD  Lab  Exfoliated   Graphene  platelets  produced  by   liquid  phase  exfoliaOon  at  TCD  are   non-­‐oxidised,  with  typical  X-­‐Y  size  of   1000nm  and  5-­‐7  carbon  layers  in   depth.     Transmission  electron  micrograph   showing  typical  graphene  platelets.  The   average  platelet  diameter  is  1000nm.   Raman  spectrum  shows  a  strong  graphite   band  (D/G  raOo  =  0.36)  when  compared   with  the  compeOtor  material  prepared  by   ion  intercalaOon  (D/G  raOo  =  0.75).   XPS  analysis  of  solvent   exfoliated  graphene.  The  N,  O,   and  H  signals  are  consistent   with  the  presence  of  solvent   residues.   0 5 10 15 20 25 30 0 4 8 12 16 AFMCount(%) Thickness, N <N>=6.6 AFM  analysis  of  mean  thickness   in  NMP  exfoliated  GNPs  shows   an  average  plate  thickness   between  5  and  7  carbon  layers.        
  11. 11. TCD  -­‐  High  Shear  Liquid  ExfoliaGon   • Liquid  phase  exfoliaGon  by  high   shear  mixing.   • No  ultrasonics   • No  aggressive  chemistry   • Ambient  condiGons.   • Range  of  solvents  –  including  water.   • Stabilised  graphene  dispersions.   • Patented  process.   • Full  scienGfic  details  published  in   April  2014:   Paton  et  al.,  Scalable  producGon  of  large  quanGGes  of   defect-­‐free,  few-­‐layer  graphene  by  shear-­‐exfoliaGon  in   liquids,  Nature  Materials  (2014)     Typical  Rotor/Stator  equipment  used  for  preparing   graphene  dispersions.     •  Liquid  phase  exfoliaGon   process  is  being  scaled  at   Thomas  Swan,  Consee.     •  Current  status  is  g/day  pilot   which  will  reach  kg/day  by  end   2014.  
  12. 12. 2 4 Re / 10Mixer ND ρ η= = Turbulence !γ ≈ π DN d =104 s−1 Minimum  shear  rate  more  important  than  turbulence   What  is  the  ExfoliaGon  Mechanism?  
  13. 13. Scale  Up  Parameters  are  Available  
  14. 14. GeneraGon  of  Significant  Public  Interest  
  15. 15. Thomas  Swan  Elicarb®  Graphene     Raman  spectra  of  Elicarb®  Graphene  Powder   (514  nm  excitaOon  laser  wavelength).   The  Raman  spectrum  shows  high  quality  sp2   network  with  D/G  raOo  of  0.23  and  D/D’  of  4.8    TGA  to  1100oC  in  air    of  Elicarb®  Graphene   Powder  exfoliated  in  water/surfactant  shows    a   small    surfactant  residue  (loss  at  ca.  300oC).    Primary  decomposiOon  of  graphene  at    800oC.  
  16. 16. Thomas  Swan  Elicarb®  Graphene     TEM  analysis  of    typical    Elicarb®  Graphene  Powders.  
  17. 17. Thomas  Swan  Elicarb®  Graphene     TEM  Image    parOcle  size  analysis  of  Elicarb®   Graphene  Powder.  Average  X-­‐Y  dimension  is   ca.  1  micron.     TEM  analysis  of  Elicarb®  Graphene  Powder   shows  very  consistent  flake  size  between   batches.   500nm  scale  bar   100nm  scale  bar  
  18. 18. Thomas  Swan  Elicarb®  Graphene     Sheet  Resistance:   •  4  point  probe   •  Filtered  solids   10  Ω/□  for  25µm  film.     Graphene  platelet  thickness:   •  5-­‐7  carbon  layers.         Elicarb®  Graphene  Products:   Products  are  available  commercially   Elicarb®Graphene   Powder   Elicarb®Graphene   Dispersion  (AQ)  
  19. 19. Summary:  Elicarb®  Graphene  Products     •  We  have  developed  a  scalable  route  to  prisGne  graphene   nanoplatelets.   •  Typical  parGcle  size  is  1000nm  in  X-­‐Y  dimension  and  5-­‐7   carbon  layers  in  Z  dimension.   •  The  products  have  low  defect  levels  and  high  conducGvity  /   low  sheet  resistance.   •  Development  products  are  now  available  for  evaluaGon.  
  20. 20. Follow  up  QuesGons   Many  thanks  for  your  aeenGon.   I  am  happy  to  answer  quesGons.   pladislaus@thomas-­‐swan.co.uk     We  would  be  delighted  to  discuss  the  needs  of  your  applicaGon.    
  21. 21. Advanced  Materials  Division   Reliability  &  Quality  in  carbon  nanomaterials.      
  22. 22. Appendix  
  23. 23. Nanomaterial  Safety  &  Regulatory   ConGnuing  safe  commercialisaGon  of  new  nanomaterials  remains  a   priority  for  the  materials  industry.    This  is  an  evolving  framework  and   Thomas  Swan  takes  a  pro-­‐acGve  role……       •  Compliance   .....with  exisGng  legislaGon…..plus  external  verificaGon.   •  Awareness   …..of  new  scienGfic  publicaGon  and  changing  regulatory  requirements.   •  Support   .....increased  understanding  through  in-­‐house  studies  and  collaboraGons  (eg.   NanoReg).   •  Engagement   …..with  Industry  associaGons    such  as  CIA  Nanomaterials  Issue  Team.   •  CommunicaGon   …..of  new  informaGon  as  we  enhance  our  understanding.    
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