Sustainable Carbon: Graphene Water and eco-friendly conducting rubbers, electrocatalysts and supercapacitors
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1 Sustainable Carbon: Graphene Water and ecofriendly conducting rubbers, electrocatalysts and supercapacitors Alain Pénicaud Centre de Recherche Paul Pascal, CNRS, Université BordeauxI
2 Outline Ø Eau de Graphène (graphene water): Additive free Single layer graphene in water Ø Carbon Waters : the Company Ø Multi layer Graphene from food waste? conducting rubbers electrocatalysts supercapacitors Alain Pénicaud, CNRSUniversité de Bordeaux penicaud@crppbordeaux.cnrs.fr NanoSpain Bilbao, March
3 Graphene : a single layer of hexagonally arranged carbon atoms The ultimate membrane: painting by Bleue Roy, All surface material thinnest strongest flexible yet tough electrical conductor Thermal conductor Alain Pénicaud, CNRSUniversité de Bordeaux penicaud@crppbordeaux.cnrs.fr NanoSpain Bilbao, March
4 Alain Pénicaud, CNRSUniversité de Bordeaux NanoSpain Bilbao, March Q: How to transfer the property of the individual object to a macroscopic material? A: By properly exfoliating graphite
5 Liquid formulations of graphene Reduced graphene oxide(rgo): Graphite Sulfurique acid / KMnO4 GO full exfoliation water Soluble Defects Reduction RGO Mechanical exfoliation in liquids: Graphite Surfactant Mechanical energy Low cost Distribution of thickness (1 to 20 layers) Concentration < 0.07 g/l Surfactants or toxic solvants (NMP) Reductive Dissolution:. Alain Pénicaud, CNRSUniversité de Bordeaux penicaud@crppbordeaux.cnrs.fr NanoSpain Bilbao, March
6 can You cannot get 100 % single layer graphene in water Alain Pénicaud, CNRSUniversité de Bordeaux penicaud@crppbordeaux.cnrs.fr NanoSpain Bilbao, March
7 Oil Water Alain Pénicaud, CNRSUniversité de Bordeaux NanoSpain Bilbao, March
8 George Bepete Alain Pénicaud Eau de Graphène! Alain Pénicaud, CNRSUniversité de Bordeaux NanoSpain Bilbao, March
9 Full exfoliation to SLG Dissolution of GICs in aprotic solvents Drummond & Penicaud., Acc. Chem. Res. (2013) Valles et al., JACS. (2008) Englert et al., Nat. Chem. (2011) Catheline et al., Soft Matter. (2012) Milner et al., JACS. (2012) Alain Pénicaud, CNRSUniversité de Bordeaux NanoSpain Bilbao, March
10 GIC THF Stable water Unstable degassed water Metastable Bepete et al., Nature Chem, 2017, J. Phys. Chem C, 2016, Phys. Status Solidi RRL 2016 Alain Pénicaud, CNRSUniversité de Bordeaux NanoSpain Bilbao, March
11 Oxidation Addition of water O 2 K O 2 KOH Normal water Degassed water ph = 11 ph = 8 Alain Pénicaud, CNRSUniversité de Bordeaux penicaud@crppbordeaux.cnrs.fr NanoSpain Bilbao, March
12 Raman signatures of graphene in water In liquid! Intensity (a.u.) (i) (ii) (iii) D G * D' 2.33 ev 2D Graphene in water Water Graphene in water after water substraction (iv) NaC stabilized graphene After water substraction Raman shift (cm 1 ) Alain Pénicaud, CNRSUniversité de Bordeaux penicaud@crppbordeaux.cnrs.fr NanoSpain Bilbao, March
13 Raman signatures of SLG in water Intensity (a.u.) D Intensity (a.u.) G & D' Intensity (a.u.) FWHM = 28 cm ev 2D Raman shift (cm 1 ) Raman shift (cm 1 ) Raman shift (cm 1 ) ExcitationEn ergy (ev) D G D 2D Δ Δ Δ Δ Symmetric, narrow and intense 2D band àsignature of SLG Bepete et al., J. Phys. Chem C, 2016 Alain Pénicaud, CNRSUniversité de Bordeaux penicaud@crppbordeaux.cnrs.fr NanoSpain Bilbao, March
14 D band : concentration of defects? EL/ ev ID/IG 2.33 XPS : 1.0 Intensity (a.u.) Lucchese Carbon (2010) ID/ID 600 ppm defects 9.0 Cançado et al.. Nano Lett. (2011) 7 nm (about 0.06 %) Graphite Graphenide film Aqueous graphene dispersion Annealed at 500 C Adapted from:eigler & Hirsch Angew. Chemie (2014) Binding energy (ev)
15 Films from EdG at 2.33 ev a) 2.33 ev Film Treatment 2D A D /A G I D /I D Intensity (a.u.) Dried at RT Dried at 100 C Annealed at 500 C Annealed at 800 C 2G Aqueous dispersion As made film C film C film C film Raman shift (cm 1 ) Defect analysis : Casiraghi et al. Nanolett. 2012, PRB 2013 After annealing, all sp3 defects removed: only edges left σ = 32 ks/m > ρ= Ω.cm (carbon inks ρ= 10 Ω.cm, Ag inks 10 6 Ω.cm) Light, flexible, inert, conductive coatings Alain Pénicaud, CNRSUniversité de Bordeaux penicaud@crppbordeaux.cnrs.fr NanoSpain Bilbao, March
16 Other evidences of SLG in eau de graphene Absorbance (a.u.) λ max 269 nm (4.61 ev) Wavelength (nm) SLG in degassed water (no surfactant/organic additives) c=0.16 g/l 200 m 2 /L, ph=8 Typical flake size 100 nm1 µm Bepete et al., Nature Chemistry, 2016
17 Stability of SLG dispersions Raman spectroscopy Intensity (a.u.) Week 1 Week 2 Week 3 Week 4 Week 5 Week 10 Week Raman shift (cm 1 ) Intensity (a.u.) Week 1 Week 2 Week 3 Week 4 Week 5 Week 10 Week Raman shift (cm 1 ) Same 2D linewidth after 12 weeks Alain Pénicaud, CNRSUniversité de Bordeaux penicaud@crppbordeaux.cnrs.fr NanoSpain Bilbao, March
18 The ingredients behind (meta)stability. I Alain Pénicaud, CNRSUniversité de Bordeaux penicaud@crppbordeaux.cnrs.fr NanoSpain Bilbao, March
19 Eau de Nanotube (Nanotube Water) See Eric Anglaret s talk Alain Pénicaud, CNRSUniversité de Bordeaux penicaud@crppbordeaux.cnrs.fr NanoSpain Bilbao, March
20
21 Carbon Waters : Graphene processing for industry Exclusive licensing of 3 patents, No free nanoparticles No chemical agents Extremely stable Very high quality and no defect materials Can be printed on several surfaces Easy to scaleup Liquid organic nanomaterial solution Surface printing Surfaces with enhanced and reinforced properties Carbon Waters : production and sales of nanocarbons and nanocarbon printed surfaces Alain Pénicaud, CNRSUniversité de Bordeaux penicaud@crppbordeaux.cnrs.fr NanoSpain Bilbao, March
22 Multilayer graphene from food waste Food Waste Anaerobic Digestion: BIOGAS: CH 4 & CO 2 microwave plasma process: biogas to C & H 2 Conducting rubbers Conducting inks Supercapacitors Nanocarbon dispersion Alain Pénicaud, CNRSUniversité de Bordeaux penicaud@crppbordeaux.cnrs.fr NanoSpain Bilbao, March
23 European project (FP7) Graphitic nanocarbon : Graphitic nature (turbostratic) High conductivity (σ~100 S/m) Nanopucks of ca 2030 graphene layers Size distribution: Average thickness = 10 nm lateral size = nm 3070 nm Carbon Nanopucks 10 nm Conductive inks of graphitic nanoparticles from a sustainable carbon feedstock,hof, Kampioti, Huang et al., Carbon 111 (2017) 142. Alain Pénicaud, CNRSUniversité de Bordeaux penicaud@crppbordeaux.cnrs.fr NanoSpain Bilbao, March
24 Applications : Rubber Composites Katerina Kampioti NR/NC nanocomposites NC NR 2 σ (S/m) σ (S/m) NR 2 wt% NC/NR 5 wt% NC/NR 7.5 wt% NC/NR 10 wt% NC/NR f (Hz) Filler (%) wt% NC/NR: 10 orders of magnitude better electrical conductivity!!! Kampioti et al., ACS Omega 2018 Collab. Aldo Zarbin s group, Curitiba, Brazil YouTube : From compost to composites: An ecofriendly way to improve rubber Alain Pénicaud, CNRSUniversité de Bordeaux penicaud@crppbordeaux.cnrs.fr NanoSpain Bilbao, March
25 Filtration Applications : Inks filtration on membrane ρ= 2 Ω.cm (carbon black inks ρ= 1 Ω.cm) Inkjet printing 20 prints on PET Hof, Kampioti, Huang et al., Carbon 2017 Alain Pénicaud, CNRSUniversité de Bordeaux penicaud@crppbordeaux.cnrs.fr NanoSpain Bilbao, March
26 Flexible micro supercapacitor by inkjet printing Kai Huang Canon printer Cyclic voltrammetry testing setup Catridges filled with nanocarbon ink RECE WE Electrolyte: PVAH2SO4 Inplane MSC Sandwich MSC electrolyte Alain Pénicaud, CNRSUniversité de Bordeaux Printed micro supercapacitors on A4 paper NanoSpain Bilbao, March
27 From Food Waste to Efficient Bifunctional Nonprecious Electrocatalyst Ferdinand Hof Hof, F. et al. Chem. Eur. J Alain Pénicaud, CNRSUniversité de Bordeaux NanoSpain Bilbao, March
28 Oxygen reduction reaction (ORR) Oxygen evolution reaction (OER) O 2 4H 4e 2 H 2 O 2 H 2 O O 2 4H 4e GC bare glassy carbon nc graphitic nano carbon Commercial Pt catalysts for fuel cells exhibit an overpotential of V vs RHE theoretical value: E = 1.22 V vs RHE Hof, F. et al. Chem. Eur. J Alain Pénicaud, CNRSUniversité de Bordeaux penicaud@crppbordeaux.cnrs.fr NanoSpain Bilbao, March
29 Conclusion Single layer Graphene can be stabilized in water with no additives. Raman signature of graphene in a liquid Carbon Waters company Few layer graphene from food waste Eco friendly Conducting inks, rubbers, supercapacitors, Alain Pénicaud, CNRSUniversité de Bordeaux penicaud@crppbordeaux.cnrs.fr NanoSpain Bilbao, March
30 Plascarb project : Katerina Kampioti Dr Ferdinand Hof Dr Kai Huang Rubber composites Prof. A. Zarbin (Curitiba) Dr Carolina Matos ( ) Eau de Graphène: Dr George Bepete Dr Carlos Drummond Prof. Eric Anglaret (Montpellier University) Dr Luca Ortolani (CNR Bologna) Dr Vittorio Morandi (CNR Bologna) Carbon Waters project: Dr A. Chesneau, Dr. F. Dragin, Dr. J. Messner Alain Pénicaud, CNRSUniversité de Bordeaux penicaud@crppbordeaux.cnrs.fr NanoSpain Bilbao, March
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