Wire-shaped supercapacitor by hydrothermal self-assembly of graphene on copper wires

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1 Wire-shaped supercapacitor by hydrothermal self-assembly of graphene on copper wires Andrea Lamberti 22 September 2015

2 Outline Introduction Supercapacitors Wearable SCs Graphene Aerogels Synthesis Characterizations Wire-shaped Supercapacitors Device assembly Characteriztion Electrochemical performance Conclusions

3 Outline Introduction Supercapacitors Wearable SCs Graphene Aerogels Synthesis Characterizations Wire-shaped Supercapacitors Device assembly Characteriztion Electrochemical performance Conclusions

Electrochemical supercapacitors Electrical double layer capacitance (EDLC) electrostatic energy storage by separating charges at the interface between the surface of a conductive electrode and an

4 Electrochemical supercapacitors Electrical double layer capacitance (EDLC) electrostatic energy storage by separating charges at the interface between the surface of a conductive electrode and an electrolyte without faradaic reactions Pseudo-capacitance faradaic electrochemical energy storage by fast reversible surface redox reactions, intercalation or electrosorption at or near the surface of some electrode materials 0,0021 0,0014 0,0007 Current (A) 0,0000-0,0007-0, mv/s 50 mv/s 100 mv/s -0, Voltage (V)

General characteristics Ragone chart EDL SCs high power density excellent cycling stability low energy density due to a limited specific capacitance of carbon materials Pseudocapacitive materials

5 General characteristics Ragone chart EDL SCs high power density excellent cycling stability low energy density due to a limited specific capacitance of carbon materials Pseudocapacitive materials (transition metal oxides or hydroxides) Common approach to improve the SC performance is to use composites of pseudocapacitive materials and carbon as electrodes much higher specific capacitance, as much as ten times that of an EDLC. poor rate capability and low electrical conductivity

Conventional SCs have 2D planar architectures with two metal plates as current collectors, two

SCs configurations Our goals/target applications small-sized flexible energy storage units for

fiber-based supercaps Development of hybrid devices with integrated energy harvesting and

6 Conventional SCs have 2D planar architectures with two metal plates as current collectors, two flat electrodes, one membrane charge separator, and electrolyte sandwiched together. SCs configurations Our goals/target applications small-sized flexible energy storage units for low power electronics and sensors microsupercaps Wearable electronics and smart textile fiber-based supercaps Development of hybrid devices with integrated energy harvesting and storage μbial fuel cell-sc hybrid device solar harvester- SC hybrid device mechanical harvester-sc hybrid device

Wearable electronics or e-textile Wearable

medical biomonitoring devices or implants,

safety and construction gear like illuminated

Adidas MiCoach, Cutecircuit Galaxy Dress and

phone-glove, all are powered with conventional

To date a fully developed textile energy storage

7 Wearable electronics or e-textile Wearable energy storage applications: provide power to medical biomonitoring devices or implants, military equipment for soldiers in combat, safety and construction gear like illuminated vests, Notable examples of wearable technology : Adidas MiCoach, Cutecircuit Galaxy Dress and T-shirtOS, Hi-call Bluetooth enabled phone-glove, all are powered with conventional batteries and capacitors. To date a fully developed textile energy storage device does not exist, nor does a streamlined manufacturing process integrating the various components.

Smart power bodysuit Energy Environ. Sci., 2013, 6, 2698 2705 Design concept for a smart power bodysuit.

8 Smart power bodysuit Energy Environ. Sci., 2013, 6, Design concept for a smart power bodysuit. (a) Piezoelectric patch converts body movements to electrical energy; (b) textile antennas to transmit communications; (c) textile electrochemical energy storage to store energy from harvesting devices; (d) integrated conductive yarns act as leads to transmit energy or information throughout the garment.

Wearable supercapacitors Low costand flexible

all-cotton-derived, arbitrarily foldable,

9 Wearable supercapacitors Low costand flexible mesh-based supercapacitors for promising large-area flexible/wearable energy storage. Nano Energy(2014) 6, An all-cotton-derived, arbitrarily foldable, highrate, electrochemical supercapacitor Phys.Chem. Chem. Phys., 2013, 15, 8042

Wire-shaped supercapacitors Electrolyte:

A coaxial single fibre supercapacitor for

10 Wire-shaped supercapacitors Electrolyte: PVA H 3 PO 4 H 2 O gel solution; this layer serves as both the ion transport layer and separator between two electrodes A coaxial single fibre supercapacitor for energy Storage. Phys.Chem. Chem. Phys., 2013, 15, 12215

11 Wire-shaped supercapacitors All-Graphene Core-Sheath Microfi bers for All-Solid-State, Stretchable Fibriform Supercapacitors and Wearable Electronic Textiles. Adv. Mater. 2013, 25,

12 Outline Introduction Supercapacitors Wearable SCs Graphene Aerogels Synthesis Characterizations Wire-shaped Supercapacitors Device assembly Characteriztion Electrochemical performance Conclusions

Reduced graphene oxide aerogel Process flow R.

13 Carbon based scaffolds Requirements high electrical conductivity controlled porosity high exposed area Reduced graphene oxide aerogel Process flow R. Giardi et al Applied Materials Today In press 200 C 12 h

14 Carbon based scaffolds Typically SSA for ELDCs: > 1000 m²/g Theoretical value for graphene: ~ 2620 m²/g XPS good results in GO reduction R. Giardi et al Applied Materials Today In press

Planar device as test bench Dispersion of active material and 2.

Slurry B: 50% rgo + 50% Graphite + Acetylene black + PVDF 13:1:1 ratio Platinum sputtered on

Current (A) 0,0007 0,0000-0,0007-0,0014-0,0021-1 0 1 Voltage (V) 10 mv/s 50 mv/s 100 mv/s

15 Planar device as test bench Dispersion of active material and 2.8 wt% of PVDF in NMP 13:1 ratio Slurry A: Graphite + Acetylene black + PVDF 13:1:1 ratio Slurry B: 50% rgo + 50% Graphite + Acetylene black + PVDF 13:1:1 ratio Platinum sputtered on top of glass slides Current collectors Graphite/PVDF Graphene/PVDF 0,0021 0,003 0,0014 0,002 Current (A) 0,0007 0,0000-0,0007-0,0014-0, Voltage (V) 10 mv/s 50 mv/s 100 mv/s Current (A) 0,001 0,000-0,001-0,002-0, Voltage (V) 10 mv/s 50 mv/s 100 mv/s R. Giardi Applied Materials Today In press

16 Outline Introduction Supercapacitors Wearable SCs Graphene Aerogels Synthesis Characterizations Wire-shaped Supercapacitors Device assembly Characteriztion Electrochemical performance Conclusions

17 Process flow Graphene aerogel self-assembly 200 C 12 h RGO@Cu wire A.Lamberti et al. Submitted to ADV. ENER. MATER. Cu wire

18 A.Lamberti et al. - Submitted to ADV. ENER. MATER. Material characterizations D G

19 A.Lamberti et al. - Submitted to ADV. ENER. MATER. Device assembly Polyvinylpyrrolidone (PVP) gel was prepared by dissolving 10g PVP in 10 ml H2O at 90 C PVP gel electrolyte was prepared by dissolving 1g NaI in 20g PVP gel water at 90 C.

20 Electrochemical characterizations A.Lamberti et al. - Submitted to ADV. ENER. MATER.

21 Electrochemical characterizations 62 F/g Yu, Dingshan, et al. "Emergence of fiber supercapacitors." Chemical Society Reviews 44.3 (2015):

22 Electrochemical characterizations 13 mf/cm Yu, Dingshan, et al. "Emergence of fiber supercapacitors." Chemical Society Reviews 44.3 (2015):

23 Outline Introduction Supercapacitors Wearable SCs Graphene Aerogels Synthesis Characterizations Wire-shaped Supercapacitors Device assembly Characteriztion Electrochemical performance Conclusions

24 Conclusions Development of a graphene aerogel self-assembly process on copper wires Deep characterization by chemico-phisical point on view Good performance of assembled and integrated devices (bending) Future developments Test different current collectors Test different electrolytes Pseudosupercapacitors exploiting Metal-Oxides or Graphene composites Packaging Self-powered devices (energy harvesting & storage)

25 Photovoltaics: Dyesensitized solar cells Energy harvesting & storage 2 DSCs 1 DSC LOAD

26 S. Stassi et al Submitted to NANOENERGY Mechanical harvester: piezonanogenerator Energy harvesting & storage

27 Acknoledgements FILGREEN national project Prof. E. Tresso Prof. F. Pirri Dr. S. Bianco Dott. A. Gigot Dr. M. Castellino Dr. S.Marasso Dr. M. Fontana Dr. R. Giardi Dr. P. Rivolo Dr. D. Mombello Dr. M. Cocuzza Dr. M. Serrapede

28 Thank you for your kind attention! Questions?

FIB & XPS characterizations Bare crosssection without FIB a) + Cu Cu

un.) Cu 2+ satellite before sputtering after sputtering Intensity

) Cu2p 1/2 Cu2p 3/2 Cu LMM Auger peaks 960 956 952 948 944 940 936

30 FIB & XPS characterizations Bare crosssection without FIB a) + Cu Cu 2+ Cu 2+ Cu + b) before sputtering after sputtering Intensity (arb. un.) Cu 2+ satellite before sputtering after sputtering Intensity (arb. un.) Cu2p 1/2 Cu2p 3/2 Cu LMM Auger peaks Binding energy (ev) Binding energy (ev) A.Lamberti et al. - Submitted to ADV. ENER. MATER.

31 A.Lamberti et al. - Submitted to ADV. ENER. MATER. Other metal wires

32 Optimizations Cover Cu with Graphene monolayer by CVD Reference With G CVD Exploit different current collector carbon fibers

33 Alternative textile electrolyte

Microsupercapacitors Current / A 0,002 0,001

34 Microsupercapacitors Current / A 0,002 0,001 0,000-0,001 Grafene "in-situ" Liquid electrolyte (1M Na 2 SO 4 )+ microfluidic cap -0,002-0,003-0,10-0,05 0,00 0,05 0,10 Voltage / V SU8 lithography (200 μm) Graphene-based (or carbon-based) paste deposited by doctor blade

Planar device as test bench Graphite/PVDF 0,0021 0,0014 0,003 0,002 Graphene/PVDF Current (A) 0,0007 0,0000-0,0007 Current (A) 0,001 0,000-0,001-0,0014 10 mv/s 50 mv/s 100 mv/s -0,002 10 mv/s 50 mv/s

35 Planar device as test bench Graphite/PVDF 0,0021 0,0014 0,003 0,002 Graphene/PVDF Current (A) 0,0007 0,0000-0,0007 Current (A) 0,001 0,000-0,001-0, mv/s 50 mv/s 100 mv/s -0, mv/s 50 mv/s 100 mv/s -0, Voltage (V) -0, Voltage (V) 0,006 0, ,002 Current (A) 0,000-0,002-0,004-0, Voltage (V) 0.5 mv/s 10 mv/s 50 mv/s 100 mv/s Graphene/MoO2/PVDF Specific Capacitance (F/g) ,00 0,05 0,10 Scan Rate (V/s) Graphite/without PVDF_NaCl Graphite/PVDF_15/1_NaCl Graphene/PVDF_15/1_NaCl Graphene+MoO2/PVDF_15/1_NaCl Graphene+MoS2/PVDF_15/1_NaCl

36 Pseudo SCs Cu x O nanostructures Poster n 185 ANM-Posters 20 July ( hrs) A. Lamberti et al. Flexible copper oxide-based supercapacitor by thermal oxidation of copper foils

37 Pseudo SCs TiO 2 Nanotubes

38 In situ synthesis of MoO 2 nanoparticles from a liquid precursor Decoration with MoO 2 NPs

39 Packaging: stereolithography

40 Industrial integration Asymmetric carbon nanotube MnO2 two-ply yarn supercapacitors for wearable Electronics, Nanotechnology 25 (2014) (8pp)

Tailorable and Wearable Textile Devices for Solar Energy Harvesting and Simultaneous Storage

Supporting Information Tailorable and Wearable Textile Devices for Solar Energy Harvesting and Simultaneous Storage Zhisheng Chai,, Nannan Zhang,, Peng Sun, Yi Huang, Chuanxi Zhao, Hong Jin Fan, Xing Fan,*,