Design of Carbon Materials with Hierarchical Pore Architecture for Electrochemical Energy Storage
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1 Design of Carbon Materials with Hierarchical Pore Architecture for Electrochemical Energy Storage Dr. Martin Oschatz, Prof. Dr. Stefan Kaskel 1 st German-Chinese-Symposium, Germany Development and Technology of Carbon Materials , Harnack House, Berlin
2 Motivation Evolution of and Porosity Outline Carbide-Derived Carbon Aerogels Well-defined carbon nanomaterials with hierarchical pore architecture. CDCs by Nanocasting CDCs from Emulsions Gas Storage/ Gas Purification Catalysis CDC Aerogels CDC Nanoparticles Li-S Batteries Electrical Double-Layer Capacitors Surface Area Pore Structure Materials Transport 2
3 Introduction Carbide-Derived Carbide-derived Carbons Aerogels Nanocarbons Microporous Activated Carbons Fullerenes Carbon Nanotubes Carbide-Derived Carbons (CDCs) Graphene (1 x) C H 2O H CO( g ) 2( g ) ( 2 3 xc 2 x) C 6KOH 2K CO 2K xc SiC (s) + 2 Cl 2(g) SiCl 4(g) + C (s) Starfire Systems V. Presser, M. Heon, Y. Gogotsi, Adv. Funct. Mater. 211, 21, 81 Y. Gogotsi, A. Nikitin, H. Ye, W. Zhou, J. E. Fischer, B. Yi, H. C. Foley and M. W. Barsoum, Nat. Mater. 23, 2,
4 N 2 adsorbed (cm 3 /g) Carbide-Derived Synthesis and Carbon Structure Aerogels Synthesis of CDC-Mesofoams by Nanocasting CDC Mesofoams Transmission Electron Microscopy N 2 Physisorption, -196 C SiO 2 Foam SiC Foam CDC Foam CDC Foam Chlorine Treatment p/p M. Oschatz, L. Borchardt, K. Pinkert, S. Thieme, M. R. Lohe, C. Hoffmann, M. Benusch, F. M. Wisser, C. Ziegler, L. Giebeler, M. H. Rümmeli, J. Eckert, A. Eychmüller, S. Kaskel, Adv. Energy Mater. 214, 4, 13645/1. CDC-Mesofoam SSA BET : 29 m 2 /g V Pore : 2.6 cm 3 /g Mesoporous SiC Foam SSA BET : 65 m 2 /g V Pore :.7 cm 3 /g 4
5 CDC Mesofoams Carbide-Derived Electrochemical Energy Carbon Storage Material Aerogels Electrode Material in EDLCs Electrode Material in Li-S Batteries F. Beguin, V. Presser, A. Balducci, E. Frackowiak, Adv. Mater. 214, 26, ~ 25 F/g in 1 M H 2 SO 4 Electrolyte ~ 115 mah/g Sulfur ~ 7 mah/g Cathode M. Oschatz, L. Borchardt, K. Pinkert, S. Thieme, M. R. Lohe, C. Hoffmann, M. Benusch, F. M. Wisser, C. Ziegler, L. Giebeler, M. H. Rümmeli, J. Eckert, A. Eychmüller, S. Kaskel, Adv. Energy Mater. 214, 4, 13645/1. 5
6 CDC PolyHIPEs Carbide-Derived Synthesis Carbon Aerogels High Internal Phase Emulsions Pulko and P. Krajnc, Macromol. Rapid Commun., 212, 33, R. Frind, M. Oschatz, S. Kaskel, J. Mater. Chem. 211, 21, Synthesis of PolyHIPE-CDCs M. Oschatz, L. Borchardt, M. Thommes, K. A. Cychosz, I.Senkovska, N. Klein, R. Frind, M. Leistner, V. Presser, Y. Gogotsi, S. Kaskel, Angew. Chem. Int. Ed. 212, 51, M. Oschatz, L. Borchardt, I. Senkovska, N. Klein, M. Leistner, S. Kaskel, Carbon 213, 56,
7 CDC PolyHIPEs Carbide-Derived Structure Carbon Aerogels N 2 Physisorption, -196 C Mercury Intrusion Porosimetry PolyHIPE-CDC SSA BET : 29 m 2 /g V Pore,Micro+Meso : 1.1 cm 3 /g V Pore,Macro : 7.5 cm 3 /g M. Oschatz, L. Borchardt, M. Thommes, K. A. Cychosz, I.Senkovska, N. Klein, R. Frind, M. Leistner, V. Presser, Y. Gogotsi, S. Kaskel, Angew. Chem. Int. Ed. 212, 51, M. Oschatz, L. Borchardt, I. Senkovska, N. Klein, M. Leistner, S. Kaskel, Carbon 213, 56,
8 CDC Nanospheres Carbide-Derived Synthesis and Carbon Structure Aerogels Synthesis of CDC Nanospheres by the Miniemulsion Technique Electron Microscopy Ultrasound Cross- Linking+ Solvent Evaporation Pyrolysis (Polycarbosilane Decompositon) Oil Phase (SMP-1 + p-dvb + Hexadecane) Water Surfactant (SDS) Miniemulsion Cross-Linked Polycarbosilane Nanospheres CDC Nanospheres Silicon Carbide Nanospheres High-Temperature Chlorine Treatment (Silicon Removal) N 2 Physisorption, -196 C Volume at STP (cm 3 /g) SiC-NS-5-5 SiC-NS P/P Volume at STP (cm 3 /g) CDC-NS-5-5 CDC-NS P/P M. Oschatz, M. Zeiger, N. Jäckel, P. Strubel, L. Borchardt, R. Reinhold, W. Nickel, J. Eckert, V. Presser, S. Kaskel, J. Mater. Chem. A 215, 3,
9 CDC Nanospheres Carbide-Derived Electrochemical Carbon Properties Aerogels Synthesis of CDC Nanospheres by the Miniemulsion Technique Electron Microscopy Ultrasound Cross- Linking+ Solvent Evaporation Pyrolysis (Polycarbosilane Decompositon) Capacitance (Fg -1 ) Oil Phase (SMP-1 + p-dvb + Hexadecane) Water Surfactant (SDS) CDC-NS-7-3 CDC-NS-5-5 Miniemulsion mv/s Time (s) -2 E A itance (F/g) 1 1. Cell voltage (V) 75 5 C/C.9.8 Cross-Linked Polycarbosilane Nanospheres CDC Nanospheres 2 CDC-NS CDC-NS CDC Nanospheres as Electrode Material in EDLCs 5 5 Capacitance (F/g) C Cell voltage (V) -5-1 Capacitance (Fg -1 ) Cell voltage (V) A/g.1 A/g CDC-NS-5-5 CDC-NS B Capacitance (F/g) Silicon Carbide Nanospheres High-Temperature Chlorine Treatment (Silicon Removal) ~ 13 F/g -5 in 1 M TEABF 4 in ACN Electrolyte D Cell voltage (V) F itance (Fg -1 ) A/g C/C CDC-NS-5-5 CDC-NS-7-3 Cell voltage (V).1 A/g CDC-NS-5-5 CDC-NS Time (s) Current (Ag -1 ) M. Oschatz, M. Zeiger, N. Jäckel, P. Strubel, L. Borchardt, R. Reinhold, W. Nickel, J. Eckert, V. Presser, S. Kaskel, J. Mater. Chem. A 215, 3,
10 CDC Aerogels Carbide-Derived Synthesis and Carbon Structure Aerogels Synthesis of CDC Aerogels by Cross-Linking of Polycarbosilanes Hydrosilylation Reaction H H C H2 Si C H H 2 Si + H 2 Si SiH 19 Pt Catalyst Pt C H2 H H 2 Si Si C H H M. Oschatz, W. Nickel, M. Thommes, K. A. Cychosz, M. Leistner, M. Adam, G. Mondin, P. Strubel, L. Borchardt, S. Kaskel, J. Mater. Chem. A 214, 2,
11 N 2 adsorbed (cm 3 /g) SSA BET (m 2 /g) V Micropore (cm 3 /g) CDC Aerogels Carbide-Derived Synthesis and Carbon Structure Aerogels Synthesis of CDC Aerogels by Cross-Linking of Polycarbosilanes Scanning Electron Microscopy 6 N 2 Physisorption (-196 C) CDC-Aero-1 C CDC-Aero-7 C CDC-Aero-Act (CO 2 Activated) M. Oschatz, W. Nickel, M. Thommes, K. A. Cychosz, M. Leistner, M. Adam, G. Mondin, P. Strubel, L. Borchardt, S. Kaskel, J. Mater. Chem. A 214, 2, p/p 11
12 Specific capacitance (F/g) Specific capacitance (F/g) Voltage (V) CDC Aerogels Carbide-Derived Electrochemistry Carbon Aerogels Synthesis of CDC Aerogels by Cross-Linking of Polycarbosilanes CDC Aerogels as Electrode Material in EDLCs with Organic Electrolytes ~ 12 F/g in 1 M TEABF 4 in ACN Electrolyte CVs at 5 mv/s. CDC-Aero-7 C CDC-Aero-Act Voltage (V) CDC-Aero-1 C CDC-Aero-7 C CDC-Aero-Act Current density (A/g) A/g 6 A/g 2 A/g 1 A/g CDC-Aero-Act Time (s) M. Oschatz, W. Nickel, M. Thommes, K. A. Cychosz, M. Leistner, M. Adam, G. Mondin, P. Strubel, L. Borchardt, S. Kaskel, J. Mater. Chem. A 214, 2, M. Oschatz, S. Boukhalfa, W. Nickel, C. Fischer, G. Yushin, S. Kaskel, Carbon 216, submitted. 12
13 Polymer-based CDC Structures Carbide-Derived Structural Carbon Variety Aerogels 13
14 Polymer-based CDCs Carbide-Derived Carbon Aerogels Model Substances for Adsorption and Structural Investigations MAS NMR (Ion Adsorption) InfraSORP Technology n-nonane Preadsorption L. Borchardt, M. Oschatz, S. Paasch, S. Kaskel, E. Brunner, Phys. Chem. Chem. Phys. 213, 15, In Situ 129 Xe NMR M. Oschatz, M. Leistner, W. Nickel, S. Kaskel, Langmuir 215, 31, 44. M. Oschatz, L. Borchardt, S. Rico-Frances, F. Rodriguez-Reinoso, S. Kaskel, J. Silvestre-Albero, Langmuir 213, 29, TEM Study of Carbon Microstructure M. Oschatz, H. C. Hoffmann, J. Pallmann, J.Schaber, L. Borchardt, W. Nickel, I. Senkovska, S. Rico-France s, J. Silvestre-Albero, S. Kaskel, E. Brunner, Chem. Mater. 214, 26, 328. M. Oschatz, P. Pre, S. Dörfler, W. Nickel, P. Beaunier, J.-N. Rouzaud, C. Fischer, E. Brunner, S. Kaskel, Carbon 216, 15,
15 Evolution Summary of Porosity in Carbide-Derived Carbon Aerogels CDC Mesofoams prepared by Nanocasting as Versatile Electrochemical Energy Storage Materials CDC Nanospheres and CDC PolyHIPEs Overview over Polymer-Based CDC Materials and Adsorption Studies CDC Aerogels Synthesized from Cross-Linked PCS Aerogels as Electrode Materials in EDLCs 15
16 Evolution Acknowledgements of Porosity in Carbide-Derived Carbon Aerogels Prof. Dr. Stefan Kaskel Dr. Lars Borchardt (TU Dresden) W. Nickel (TU Dresden) G. Yushin group (Georgia Tech) E. Brunner group (TU Dresden) M. Thommes (Quantachrome) J. Slivestre-Albero group (Alicante) M. Leistner (IWS Dresden) B. Smarsly group (Giessen) Y. Gogotsi group (Drexel) J. Eckert group (IFW Dresden) M. Biesheuvel (Wetsus) V. Presser (Saarbrücken) 16
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