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SYNTHESIS OF SUPER SYNTHESIS OF SUPER NANOPOROUS SYNTHESIS OF SUPER SYNTHESIS OF SUPER-NANOPOROUS NANOPOROUS NANOPOROUS CARBON ALLOY BY CARBON ALLOY BY ELECTROOXIDATION OF A ZEOLITE ELECTROOXIDATION OF A ZEOLITE ELECTROOXIDATION OF A

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SLIDE 1

SYNTHESIS OF SUPER SYNTHESIS OF SUPER NANOPOROUS NANOPOROUS SYNTHESIS OF SUPER SYNTHESIS OF SUPER-NANOPOROUS NANOPOROUS CARBON ALLOY BY CARBON ALLOY BY ELECTROOXIDATION OF A ZEOLITE ELECTROOXIDATION OF A ZEOLITE ELECTROOXIDATION OF A ZEOLITE ELECTROOXIDATION OF A ZEOLITE TEMPLATED CARBON TEMPLATED CARBON

  • E. Morallón, D. Cazorla
  • E. Morallón, D. Cazorla-
  • Amorós,

Amorós,

Universidad de Alicante

  • R. Berenguer
  • R. Berenguer
  • R. Berenguer
  • R. Berenguer

Universidad de Málaga

  • H. Nishihara, H.
  • H. Nishihara, H. Itoi

Itoi, T. Kyotani , T. Kyotani

Tohoku University Tohoku University

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SLIDE 2

Strategic Japanese Strategic Japanese-

  • Spanish

Spanish Cooperative Program (FY2011) Cooperative Program (FY2011) Cooperative Program (FY2011) Cooperative Program (FY2011) “UNIQUE SUPER

UNIQUE SUPER-

  • POROUS CARBON

POROUS CARBON ALLOYS FOR ASYMMETRIC HYBRID ALLOYS FOR ASYMMETRIC HYBRID SUPERCAPACITORS” SUPERCAPACITORS”

Diego Diego Cazorla Cazorla-

  • Amorós, Emilia Morallón

Amorós, Emilia Morallón

Universidad de Alicante

Tomás Cordero, Tomás Cordero, José Rodríguez José Rodríguez Tomás Cordero, Tomás Cordero, José Rodríguez José Rodríguez

Universidad de Málaga

Takashi Takashi Kyotani Kyotani

Tohoku University Tohoku University

PRI-PIBJP-2011-0766

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SLIDE 3

Alicante Málaga Málaga Sendai

Alicante Alicante University University 2

SJ-NANO 2013 Workshop (2013)

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SLIDE 4

Japan Japan-

  • Spain

Spain Cooperation Cooperation Project (2012 Project (2012-

  • 2014)

2014)

Project Title: “Unique super-porous carbon alloys for Unique super porous carbon alloys for asymmetric hybrid supercapacitors” Objective: The aim of this project is to synthesize unique The aim of this project is to synthesize unique porous carbon alloy and to develop a carbon- based asymmetric hybrid supercapacitor using based asymmetric hybrid supercapacitor using the carbon alloy as a positive electrode.

Alicante Alicante University University 2

SJ-NANO 2013 Workshop (2013)

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SLIDE 5
  • High surface

area DLC area DLC

  • High pseudo-

capacitance capacitance (redox rxn.)

Alicante Alicante University University 2

SJ-NANO 2013 Workshop (2013)

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SLIDE 6

Concept of Carbon Alloy:

Carbon materials can be developed with a wide range p g

  • f structures, textures and properties. This led to the

Japanese Carbon Group to propose in 1992:

“Carbon alloys are materials mainly composed f b t i lti t t i

  • f carbon atoms in multi-component systems, in

which each component has physical and/or h i l i t ti ith h th H chemical interactions with each other. Here carbons with different hybrid orbitals account as diff t t ” different components”

Alicante Alicante University University 2

SJ-NANO 2013 Workshop (2013)

(Carbon alloys, E Yasuda et al Editors, Elsevier, 2003, p.9).

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SLIDE 7

Concept of Carbon Alloy:

Carbon materials can be developed with a wide range p g

  • f structures, textures and properties. This lead to the

Japanese Carbon Group to propose in 1992:

“Carbon alloys are materials mainly composed f b t i lti t t i

TO SYNTHESIZE A SUPER- NANOPOROUS CARBON

  • f carbon atoms in multi-component systems, in

which each component has physical and/or h i l i t ti ith h th H

NANOPOROUS CARBON ALLOY BASED ON ZEOLITE TEMPLATED CARBON (ZTC)

chemical interactions with each other. Here carbons with different hybrid orbitals account as diff t t ”

TEMPLATED CARBON (ZTC)

different components”

Alicante Alicante University University 2

SJ-NANO 2013 Workshop (2013)

(Carbon alloys, E Yasuda et al Editors, Elsevier, 2003, p.9).

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SLIDE 8

What is ZTC? Nano-sized carbon material with taylored and ordered pore network prepared taylored and ordered pore network prepared using zeolite as template

carbon filling carbon/zeolite composite nanopore: 1.2 nm zeolite filling

zeolite Y (template)

removal

Kyotani et al. Chem. Mater. 9 (1997), 609. K t i t l Ch C (2000) 2365 Kyotani et al. Chem. Commun. (2000) 2365. Nishihara et al. Carbon, 47 (2009) 1220.

Alicante Alicante University University 2

SJ-NANO 2013 Workshop (2013)

( )

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SLIDE 9

What is ZTC? Nano-sized carbon material with taylored and ordered pore network prepared taylored and ordered pore network prepared using zeolite as template

carbon filling carbon/zeolite composite nanopore: 1.2 nm zeolite filling

zeolite Y (template)

removal

Kyotani et al. Chem. Mater. 9 (1997), 609. K t i t l Ch C (2000) 2365 Kyotani et al. Chem. Commun. (2000) 2365. Nishihara et al. Carbon, 47 (2009) 1220.

Alicante Alicante University University 2

SJ-NANO 2013 Workshop (2013)

( )

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SLIDE 10

U i f t ZTC

1 2

Unique features ZTC

nanopore: 1.2 nm

  • 3D-nanographene network
  • uniform nanopore size (1.2 nm)

high surface area (up to 4000 m2/g) g p

  • high surface area (up to 4000 m2/g)
  • large amount of carbon edge sites!
  • all edge sites and graphene

surface are fully exposed! These features are beneficial to use ZTC as an electrode for electrochemical capacitors

Alicante Alicante University University 2

SJ-NANO 2013 Workshop (2013)

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SLIDE 11

U i f t ZTC Unique features ZTC

These features are beneficial to the use ZTC as an electrode for electrochemical capacitors Adequate electrolyte accessibility

  • Adequate electrolyte accessibility
  • High mass transfer rate
  • High surface area (high double layer capacitance)

High surface area (high double layer capacitance)

  • Formation of large amount of functional groups (redox

properties, pseudocapacitance) p p p p )

Alicante Alicante University University 2

SJ-NANO 2013 Workshop (2013)

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SLIDE 12

U i f t ZTC Unique features ZTC

These features are beneficial to the use ZTC as an electrode for electrochemical capacitors Adequate electrolyte accessibility

  • Adequate electrolyte accessibility
  • High mass transfer rate
  • High surface area (high double layer capacitance)

High surface area (high double layer capacitance)

  • Formation of large amount of functional groups (redox

properties, pseudocapacitance) p p p p )

Alicante Alicante University University 2

SJ-NANO 2013 Workshop (2013)

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U i f t ZTC Unique features ZTC

Hypothetical

  • xidation

process

  • f

ZTC and the modelled

Alicante Alicante University University 2

SJ-NANO 2013 Workshop (2013) molecular structure of fully-oxidized ZTC.

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SLIDE 14

U i f t ZTC Unique features ZTC SUPER SUPER- NANOPOROUS CARBON CARBON ALLOY!

Hypothetical

  • xidation

process

  • f

ZTC and the modelled

Alicante Alicante University University 2

SJ-NANO 2013 Workshop (2013) molecular structure of fully-oxidized ZTC.

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SLIDE 15

Main problems to achieve the objective

  • ZTC has a quite fragile structure

q g

  • ZTC is very reactive
  • Easy structure degradation

y g

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SJ-NANO 2013 Workshop (2013)

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SLIDE 16

Main problems to achieve the objective

  • ZTC has a quite fragile structure

q g

  • ZTC is very reactive
  • Easy structure degradation

y g

Alicante Alicante University University 2

SJ-NANO 2013 Workshop (2013)

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SLIDE 17

Main problems to achieve the objective

  • ZTC has a quite fragile structure

q g

  • ZTC is very reactive
  • Easy structure degradation

y g

Alicante Alicante University University 2

SJ-NANO 2013 Workshop (2013)

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SLIDE 18

Objective of this work: To make a detailed study of the ZTC To make a detailed study of the ZTC electrooxidation to get large concentration of surface oxygen groups and high surface area surface oxygen groups and high surface area

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SJ-NANO 2013 Workshop (2013)

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SLIDE 19

Experimental ti section

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SJ-NANO 2013 Workshop (2013)

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Electrochemical oxidation:

  • Galvanostatic oxidation: I= 2-50 mA, t= 1-15h,

, , T= 25ºC; Electrolytes: 1.0M NaOH, 1.0M H2SO4, 2wt% NaCl

  • Cyclic voltammetry: ∆E= -0.1-1.2 V, v= 1 mV/s,

1 0M H SO 1.0M H2SO4

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SJ-NANO 2013 Workshop (2013)

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SLIDE 21

Electrochemical oxidation:

  • Galvanostatic oxidation: I= 2-50 mA, t= 1-15h,

, , T= 25ºC; Electrolytes: 1.0M NaOH, 1.0M H2SO4, 2wt% NaCl

3-electrode cell

filter

CE: Pt

filter Ti/RuO2 anode filter paste WE: (Ti/RuO2 + ZTC paste) mass = 100 mg area = 2.25 cm2 thickness = 2 mm

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thickness = 2 mm

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SLIDE 22

T = 25 ºC

3-electrode cell

T = 25 C

Ag/AgCl/Cl- sat. REF: Ti or Pt

Electrochemical

  • xidation:
  • xidation:
  • Cyclic voltammetry:

∆E= -0.1-1.2 V, v= 1

1M H2SO4 aq. Electrolyte:

, mV/s, 1.0M H2SO4

WE: 90 wt% active material

5 wt% acetilene black 5 wt% PFTE

CE: Pt wire

5 wt% PFTE mass = 5-10 mg area = 1 cm2 thickness = 0 18 mm

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thickness = 0.18 mm

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SLIDE 23

Chemical oxidation:

  • Oxidation by HNO3 at different temperatures

(45ºC, 80 ºC) and times (from 15 min to 15h). (45 C, 80 C) and times (from 15 min to 15h). Oxidation by H2O2 was also done.

Alicante Alicante University University 2

SJ-NANO 2013 Workshop (2013)

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SLIDE 24

Characterization

Structural-Textural Structural-Textural

  • N2 adsorption (-196 ºC)

CO adsorption (0 ºC)

  • CO2 adsorption (0 C)
  • X-ray diffraction (XRD)

Surface Chemistry

  • Temperature-programmed desorption (TPD)
  • X-ray photoelectron spectroscopy (XPS)

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SJ-NANO 2013 Workshop (2013)

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SLIDE 25

Results and di i discussion.

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SLIDE 26

Results and di i discussion. Chemical oxidation

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SLIDE 27

25 30 40

Chemical Oxidation n

  • 1 g
  • 1)

15 20 25

Chemical Oxidation in

  • 1 g
  • 1)

N30 80 15min N30-80-1h

10 20

O (mol min

5 10 15

O2 (mol mi

N30-45-15min N30-80-15min

1200 200 400 600 800 1000

CO

Temperature (ºC)

200 400 600 800 1000 5

Temperature (ºC)

CO ZTC

3000 4000

nm

  • 1g
  • 1)

ZTC

400 800

V [ml (STP)/g]

ZTC N30-45-15min N30-80-15min N30-80-1h

5 6 7

2

1000 2000

s(w) (m

2n

N30-45-15min N30 80 15 i

0.0 0.2 0.4 0.6 0.8 1.0

V [ml (STP)/g]

P/P0 stacking/flat graphene

0.5 1.0 1.5 2.0 2.5 3.0

Pore width (nm ds

N30-80-15min N30-80-1h

10 20 30 40 50

2

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SJ-NANO 2013 Workshop (2013)

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SLIDE 28

TPD N2 adsorption Sample CO μmol/g CO2 μmol/g O μmol/g ∆O* μmol/g CO CO2 SBET (m2/g) VT(N2) (cm3/g) %SBET ZTC 2644 286 3216 9.24 3650 1.63 100 ZTC N30-45-15min 4181 1506 7193 3977 2.78 2230 1.07 61 ZTC N30-80-15min 4327 1923 8173 4957 2.25 1870 0.88 51 ZTC N30-80-1h 4676 2555 9786 6570 1.83 1420 0.66 39 ZTC N30 80 2h 4708 2864 10436 7220 1 64 1140 0 52 31 ZTC N30-80-2h 4708 2864 10436 7220 1.64 1140 0.52 31

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SJ-NANO 2013 Workshop (2013)

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SLIDE 29

SUMMARY ABOUT CHEMICAL OXIDATION:

  • Chemical oxidation is a fast process that

easily destroys the unique structure of ZTC.

  • It produces a very important decrease in

porosity and structural order. p y

  • High selectivity to CO2-type groups, since it

favours the oxidation of surface-oxidized sites. favours the oxidation of surface oxidized sites.

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SJ-NANO 2013 Workshop (2013)

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SLIDE 30

Results and di i discussion. Electrochemical

  • xidation
  • xidation

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SJ-NANO 2013 Workshop (2013)

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SLIDE 31

Electrochemical oxidation: Galvanostatic oxidation

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SJ-NANO 2013 Workshop (2013)

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SLIDE 32

Electrochemical oxidation: Galvanostatic oxidation

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SJ-NANO 2013 Workshop (2013)

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SLIDE 33

Electrochemical oxidation: Galvanostatic oxidation

TPD N d ti TPD N2 adsorption Sample CO μmol/g CO2 μmol/g O μmol/g ∆O* μmol/g CO CO2 SBET (m2/g) VDR(N2) (cm3/g) %SBET μ g μ g μ g μ g

2

( g) ( g) ZTC 2644 286 3216 9.24 3650 1.54 100 ZTC 20Cl– 1h 4398 529 5456 2240 8.31 2780 1.21 76 ZTC 50Cl– 1h 5083 709 6501 3285 7.17 2680 1.16 73 ZTC 5Cl– 15h 4669 1146 6961 3745 4.07 2430 1.01 67 ZTC 50Cl 3h 5880 1760 9400 6184 3 34 1210 0 50 33 ZTC 50Cl– 3h 5880 1760 9400 6184 3.34 1210 0.50 33 ZTC 50Cl– 10h 4849 4002 12853 9637 1.21 150 0.06 4 ZTC 50H+ 1h 3442 435 4312 1096 7.91 3100 1.31 85 ZTC 50H 1h 3442 435 4312 1096 7.91 3100 1.31 85 ZTC 5H+ 15h 6095 1090 8275 5059 5.59 2290 0.89 63 ZTC 2H+ 36 h (1.2V) 7159 1966 11091 7875 3.64 1863 0.77 51

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SLIDE 34

Electrochemical oxidation: Galvanostatic oxidation

TPD N d ti TPD N2 adsorption Sample CO μmol/g CO2 μmol/g O μmol/g ∆O* μmol/g CO CO2 SBET (m2/g) VDR(N2) (cm3/g) %SBET μ g μ g μ g μ g

2

( g) ( g) ZTC 2644 286 3216 9.24 3650 1.54 100 ZTC 20Cl– 1h 4398 529 5456 2240 8.31 2780 1.21 76 ZTC 50Cl– 1h 5083 709 6501 3285 7.17 2680 1.16 73 ZTC 5Cl– 15h 4669 1146 6961 3745 4.07 2430 1.01 67 ZTC 50Cl 3h 5880 1760 9400 6184 3 34 1210 0 50 33 ZTC 50Cl– 3h 5880 1760 9400 6184 3.34 1210 0.50 33 ZTC 50Cl– 10h 4849 4002 12853 9637 1.21 150 0.06 4 ZTC 50H+ 1h 3442 435 4312 1096 7.91 3100 1.31 85 ZTC 50H 1h 3442 435 4312 1096 7.91 3100 1.31 85 ZTC 5H+ 15h 6095 1090 8275 5059 5.59 2290 0.89 63 ZTC 2H+ 36 h (1.2V) 7159 1966 11091 7875 3.64 1863 0.77 51

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SJ-NANO 2013 Workshop (2013)

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SLIDE 35

Electrochemical oxidation: Galvanostatic oxidation

TPD N d ti TPD N2 adsorption Sample CO μmol/g CO2 μmol/g O μmol/g ∆O* μmol/g CO CO2 SBET (m2/g) VDR(N2) (cm3/g) %SBET μ g μ g μ g μ g

2

( g) ( g) ZTC 2644 286 3216 9.24 3650 1.54 100 ZTC 20Cl– 1h 4398 529 5456 2240 8.31 2780 1.21 76 ZTC 50Cl– 1h 5083 709 6501 3285 7.17 2680 1.16 73 ZTC 5Cl– 15h 4669 1146 6961 3745 4.07 2430 1.01 67 ZTC 50Cl 3h 5880 1760 9400 6184 3 34 1210 0 50 33 ZTC 50Cl– 3h 5880 1760 9400 6184 3.34 1210 0.50 33 ZTC 50Cl– 10h 4849 4002 12853 9637 1.21 150 0.06 4 ZTC 50H+ 1h 3442 435 4312 1096 7.91 3100 1.31 85 ZTC 50H 1h 3442 435 4312 1096 7.91 3100 1.31 85 ZTC 5H+ 15h 6095 1090 8275 5059 5.59 2290 0.89 63 ZTC 2H+ 36 h (1.2V) 7159 1966 11091 7875 3.64 1863 0.77 51

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SJ-NANO 2013 Workshop (2013)

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SLIDE 36

Electrochemical oxidation: Galvanostatic oxidation

TPD N d ti TPD N2 adsorption Sample CO μmol/g CO2 μmol/g O μmol/g ∆O* μmol/g CO CO2 SBET (m2/g) VDR(N2) (cm3/g) %SBET μ g μ g μ g μ g

2

( g) ( g) ZTC 2644 286 3216 9.24 3650 1.54 100 ZTC 20Cl– 1h 4398 529 5456 2240 8.31 2780 1.21 76 ZTC 50Cl– 1h 5083 709 6501 3285 7.17 2680 1.16 73 ZTC 5Cl– 15h 4669 1146 6961 3745 4.07 2430 1.01 67 ZTC 50Cl 3h 5880 1760 9400 6184 3 34 1210 0 50 33

Total oxygen

ZTC 50Cl– 3h 5880 1760 9400 6184 3.34 1210 0.50 33 ZTC 50Cl– 10h 4849 4002 12853 9637 1.21 150 0.06 4 ZTC 50H+ 1h 3442 435 4312 1096 7.91 3100 1.31 85

content 18 wt%!

ZTC 50H 1h 3442 435 4312 1096 7.91 3100 1.31 85 ZTC 5H+ 15h 6095 1090 8275 5059 5.59 2290 0.89 63 ZTC 2H+ 36 h (1.2V) 7159 1966 11091 7875 3.64 1863 0.77 51

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SJ-NANO 2013 Workshop (2013)

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SLIDE 37

Electroxidation Mechanism

ANODE

POLARIZED

Electroxidation Mechanism

LYST

ANODE

CARBON

+H O

DIRECT OXIDATION

CATAL +H2O

  • e–

CTROC ELEC

  • OH

Cl H2O Cl— Cl2

INDIRECT OXIDATION

Electrolyte Oxidants

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SJ-NANO 2013 Workshop (2013)

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SLIDE 38

Electrochemical oxidation: Cyclic voltammetry

1000

)

500

ce (F/g) acitanc

  • 500

Capa

v = 1 mV/s H2SO4 1 M

  • 0,3

0,0 0,3 0,6 0,9

  • 1000

E vs Ag/AgCl/Cl

  • sat (V)

v 1 mV/s

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SJ-NANO 2013 Workshop (2013)

E vs. Ag/AgCl/Cl sat (V)

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SLIDE 39

Electrochemical oxidation: Cyclic voltammetry

3.5 4.0

CO CO2 After CV + GC CO CO2 Pristine

3.5 4.0 3.5 4.0

CO CO2 After CV + GC CO CO2 Pristine CO CO2 After CV + GC CO CO2 After CV + GC CO CO2 Pristine CO CO2 Pristine

at 0.8V

TPD

2 0 2.5 3.0

CO CO2 te C GC

2 0 2.5 3.0 2 0 2.5 3.0

CO CO2 te C GC CO CO2 te C GC CO CO2 te C GC ion rate min–1 g–1)

ZTC

Sample CO/CO2 ZTC 9.24

1.5 1.0 2.0 1.5 1.0 2.0 1.5 1.0 2.0

Desorpti (mol m

ZTC

0.8 V 7.88 0.9 V 5.21

200 1000 400 1400 1600 600 800 1200 1800 0.5 200 1000 400 1400 1600 600 800 1200 1800 200 1000 400 1400 1600 600 800 1200 1800 0.5 0.5

1.0 V 4.68 1.1 V 3.29

Temperature (ºC) Temperature (ºC)

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SLIDE 40

Electrochemical oxidation: Cyclic voltammetry

3.5 4.0

CO CO2 After CV + GC CO CO2 Pristine

3.5 4.0 3.5 4.0

CO CO2 After CV + GC CO CO2 Pristine CO CO2 After CV + GC CO CO2 After CV + GC CO CO2 Pristine CO CO2 Pristine

at 0.8V

TPD

2 0 2.5 3.0

CO CO2 te C GC

2 0 2.5 3.0 2 0 2.5 3.0

CO CO2 te C GC CO CO2 te C GC CO CO2 te C GC ion rate min–1 g–1)

ZTC

Sample CO/CO2 ZTC 9.24

1.5 1.0 2.0 1.5 1.0 2.0 1.5 1.0 2.0

Desorpti (mol m

ZTC

0.8 V 7.88 0.9 V 5.21

Oxygen content 15 wt%

200 1000 400 1400 1600 600 800 1200 1800 0.5 200 1000 400 1400 1600 600 800 1200 1800 200 1000 400 1400 1600 600 800 1200 1800 0.5 0.5

1.0 V 4.68 1.1 V 3.29

Temperature (ºC) Temperature (ºC)

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SLIDE 41

Electrochemical oxidation: Cyclic voltammetry

Total capacitance (from charge-discharge at 50 mA/g in H2SO4):

2 4

  • After CV oxidation up to 0.8 V, C = 500 F/g
  • After CV oxidation up to 1.1 V, C = 700 F/g

Very close to conducting polymers (Pani nanobelts 873 F/g) or ruthenium oxide (720 F/g)*

Alicante Alicante University University 2

SJ-NANO 2013 Workshop (2013) (*)JN Tiwari, RN Tiwari, KS Kim, Progress in Materials Sci, 57 (2012) 724

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SLIDE 42

Conclusions

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SLIDE 43

CONCLUSIONS CONCLUSIONS

  • Synthesis of ZTC alloy has been studied by chemical

and electrochemical oxidations.

  • Chemical oxidation easily destroys the ZTC. Reaction

rate is high at the beginning of the oxidation.

  • Electrochemical oxidation permits a better control of

the kinetics of the process.

  • ZTC alloy with BET surface area close to 1900 m2/g

and oxygen content of 18 wt% has been successfully synthesised.

  • ZTC alloy by cyclic voltammetry has a capacitance as

high as 700 F/g.

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SJ-NANO 2013 Workshop (2013)

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SLIDE 44

Thank you very much f tt ti for your attention

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SJ-NANO 2013 Workshop (2013)