ars.els-cdn.com · Web viewLSV curves of E-CoMo900/CP before and after long-term stability test in H-type cell containing N 2-purged 0.5 M H 2 SO 4 electrolyte. Fig. S 2 3 . Photographs

Supplementary Material

Micro-Nanoporous MoO2@CoMo Heterostructure Catalyst

for Hydrogen Evolution Reaction

Gyeong Ho Han1, Hyunki Kim1, Jooyoung Kim1, Junhyeong Kim1, Soo Young Kim2,**,

Sang Hyun Ahn1,*

1School of Chemical Engineering and Material Science, Chung-Ang University,

84 Heukseok-ro, Dongjak-gu, Seoul 06974, Republic of Korea

2Department of Materials Science and Engineering, Korea University,

145 Anam-ro, Seongbuk-gu, Seoul 02841, Republic of Korea

*Corresponding author. Tel.: +82-2-820-5287; fax: +82-2-824-3495; e-mail: [email protected]

**Corresponding author. Tel.: +82-2-3290-3273; fax: +82-2-928-3584; e-mail: [email protected]

1

Table S1. Peak area ratios of deconvoluted Co 2p and Mo 3d XPS spectra for E-CoMo#/CP.

CatalystCo 2p Mo 3d

Co0 Co2+ Co3+ Co2+ sat. Mo0 Mo2+ Mo4+ Mo6+

E-CoMo300/CP 0.374 0.165 0.386 0.075 0.176 0.237 0.308 0.279

E-CoMo600/CP 0.359 0.236 0.266 0.139 0.161 0.207 0.316 0.316

E-CoMo900/CP 0.262 0.116 0.547 0.025 0.199 0.216 0.328 0.257

E-CoMo1200/CP 0.205 0.154 0.415 0.226 0.142 0.247 0.315 0.296

E-CoMo1800/CP 0.179 0.040 0.4758 0.306 0.071 0.278 0.336 0.315

Table S2. Comparison of electrochemical properties with the Mo-based heterostructure catalysts

reported in recent literature.

CatalystOverpotential

at −50 mA/cm2geo

(mV)

Tafel slope(mV/dec)

Double layercapacitance(mF/cm2

geo)Electrolyte Reference

MoO2-Ni NWs 150 36.6 29.6 1 M KOH 42

MoNi4 30 30 2220 1 M KOH 43

MoS2/MoO2 262 35.6 0.038 0.5 M H2SO4 44

Co/Ni-MoO2 160 80 7.7 1 M KOH 45

MoSe2/MoO2/Mo 185 48.9 88.09 0.5 M H2SO4 46

MoSe2/MoO2 200 (η20) 49.1 0.019 0.5 M H2SO4 47

MoO2/α-Mo2C120190

5065 70.49 1 M KOH

0.5 M H2SO448

Pt Cs/MoO2 NSs-L 120 32.6 26.7 0.5 M H2SO4 49

E-CoMo900/CP 76 50.88 287.8 0.5 M H2SO4 This study

2

Table S3. Comparison of HER overpotential for state-of-the-art catalysts reported in recent literature.

CatalystOverpotential

at −50 mA/cm2geo

(mV)Electrolyte Reference

Rh2-P 55 0.5 M H2SO4 S1

porous NiMo 70 0.5 M H2SO4 S2

Ru@Co-SAs/N-C 103 0.5 M H2SO4 S3

Ni5P4 MP 80 0.5 M H2SO4 S4

NFP/C-3 118 0.5 M H2SO4 S5

MoP/CNT-700 124 0.5 M H2SO4 S6

o-CoSe2IP 156 0.5 M H2SO4 S7

porous NiMo 75 0.5 M H2SO4 S8

Co2P@NPC-800 155 0.5 M H2SO4 S9

3.4 at% S-MoP 130 0.5 M H2SO4 S10

E-CoMo900/CP 76 0.5 M H2SO4 This study

Table S4. Peak area ratios of deconvoluted Co 2p and Mo 3d XPS spectra for E-CoMo#/CP after the

chronoamperometry at ‒0.11 VNHE for 1800 s.

3

CatalystCo 2p Mo 3d


E-CoMo300/CP 0.248 0.234 0.502 0.016 0.196 0.248 0.310 0.246

E-CoMo600/CP 0.392 0.176 0.279 0.153 0.279 0.285 0.293 0.143

E-CoMo900/CP 0.268 0.060 0.619 0.052 0.171 0.197 0.273 0.359

E-CoMo1200/CP 0.342 0.114 0.504 0.040 0.200 0.315 0.256 0.229

E-CoMo1800/CP 0.233 0.06 0.495 0.212 0.103 0.306 0.235 0.356

Table S5. Peak area ratios of deconvoluted Co 2p and Mo 3d XPS spectra for E-CoMo900/CP after

the chronoamperometry at ‒0.11 VNHE for 10, 100, 300, 600, 1200, and 1800 s.

TimeCo 2p Mo 3d


10 s 0.429 0.147 0.289 0.135 0.186 0.232 0.335 0.247

100 s 0.428 0.234 0.212 0.126 0.186 0.249 0.305 0.260

300 s 0.373 0.285 0.245 0.097 0.215 0.251 0.279 0.255

600 s 0.385 0.264 0.242 0.109 0.204 0.239 0.280 0.277

1200 s 0.365 0.271 0.226 0.138 0.163 0.259 0.276 0.302

1800 s 0.280 0.170 0.318 0.232 0.171 0.197 0.273 0.359

Table S6. Peak area ratios of deconvoluted Co 2p and Mo 3d XPS spectra for E-CoMo900/CP after

the chronoamperometry at ‒0.31 VNHE for 10, 100, 300, 600, 1200, and 1800 s.

TimeCo 2p Mo 3d


10 s 0.318 0.111 0.489 0.082 0.175 0.202 0.328 0.295

100 s 0.312 0.164 0.379 0.145 0.178 0.229 0.314 0.279

300 s 0.266 0.185 0.397 0.152 0.162 0.253 0.283 0.302

600 s 0.281 0.235 0.315 0.169 0.148 0.264 0.277 0.311

1200 s 0.256 0.203 0.344 0.197 0.143 0.266 0.275 0.316

1800 s 0.284 0.247 0.371 0.098 0.205 0.214 0.273 0.308

4

-0.32 -0.30 -0.28 -0.26 -0.24 -0.22

-0.4

-0.3

-0.2

-0.1

0.0

0.1

Cur

rent

/ m

A

Potential / V vs. SCE

-0.270 V

Fig. S1. Calibration of the reference electrode. CV curve of Pt wire in the H2-purged 0.5 M H2SO4

electrolyte at a scan rate of 1 mV/s.

Fig. S2. LSV curve of CP substrate in the N2-purged deposition electrolyte at a scan rate of 5 mV/s.

5

50 µm 5 µm

50 µm 5 µm

50 µm 5 µm

50 µm 5 µm

50 µm 5 µm

50 µm 5 µm

(a)

(b)

(c)

(d)

(e)

(f)

Co:Mo = 0.80:0.20

Co:Mo = 0.80:0.20

Co:Mo = 0.82:0.18

Co:Mo = 0.83:0.17

Co:Mo = 0.83:0.17

Fig. S3. FESEM images and EDS spectra of (a) bare CP and CoMo electrodeposited at a potential of

(b) ‒1.2 VSCE, (c) ‒1.4 VSCE, (d) ‒1.6 VSCE, (e) ‒1.8 VSCE, and (f) ‒2.0 VSCE. The deposition time was

fixed at 600 s. Insets: FESEM images at a higher magnification.

6

-0.20 -0.15 -0.10 -0.05 0.00 0.05-50

-40

-30

-20

-10

0

10

20

30 -1.6 VSCE, 600 s -1.8 VSCE, 600 s -2.0 VSCE, 600 s

Bare CP -1.2 VSCE, 600 s -1.4 VSCE, 600 s

Cur

rent

den

sity

/ m

A c

m-2 ge

o

Potential (iR-corrected) / V vs. RHE

-1.2 -1.4 -1.6 -1.8 -2.00

1

2

3

4

5

6

Bul

k C

o/M

o at

omic

rat

io

Deposition potential / V vs. SCE

(a)

(b)

Fig. S4. (a) Bulk Co/Mo atomic ratio of CoMo deposits as a function of deposition potential. (b) LSV

curves of bare CP and CoMo deposits in N2-purged 0.5 M H2SO4 electrolyte at a scan rate of 5 mV/s.

7

(a)

(b)

(c)

(d)

(e)

(f)

(g)

(h)

(i)

(j)

Fig. S5. EDS spectra of (a) CoMo300/CP, (b) CoMo600/CP, (c) CoMo900/CP, (d) CoMo1200/CP, (e)

CoMo1800/CP, (f) E-CoMo300/CP, (g) E-CoMo600/CP, (h) E-CoMo900/CP, (i) E-CoMo1200/CP,

and (j) E-CoMo1800/CP.

8

0.08 VNHE, MoO3 + 6H+ + 6e- ↔ Mo + 3H2O

-0.15 VNHE, MoO2 + 4H+ + 4e- ↔ Mo + 4H2O

-0.20 VNHE, Mo3+ + 3e- ↔ Mo

-1.05 VNHE, MoO42- + 4H2O + 6e- ↔ Mo + 8OH-

-1.76 VNHE (deposition potential, -2.00 VSCE)

0.04 VNHE (etching potential, -0.20 VSCE)

0 VNHE, 2H+ + 2e- ↔ H2

-0.11 VNHE (HER low overpotential, -0.35 VSCE)

-0.28 VNHE, Co2+ + 2e- ↔ Co

-0.31 VNHE (HER high overpotential, -0.55 VSCE)

Potential / V vs. NHE

Fig. S6. Scale of various applied potentials and potentials of electrochemical reactions.

9

0.213 nmCoO(200)

0.205 nmCo0(111)

0.213 nmCoO(200)

0.205 nmCo0(111)

I

0.205 nmCo0(111)

0.158 nmMo0(200)

0.158 nmMo0(200)

0.158 nmMo0(200)

II III0.205 nmCo0(111)

I II III0.213 nmCoO(200)

0.158 nmMo0(200)

Fig. S7. HRTEM images and FFT patterns of CoMo900/CP.

Co0.86Mo0.10O0.04

Co0.72Mo0.13O0.15

Co0.84Mo0.11O0.05

(c)

(a)

(b)

100 nm

100 nm

100 nm

Fig. S8. EDS spectra of CoMo900/CP at the (a) surface, (b) interior, and (c) projected area.

10

0.192 nmMoO2(201)

0.205 nmCo0(111)

0.205 nmCo0(111)

0.192 nmMoO2(201)

0.223 nmMo0(110)

I 0.168 nmMoO2(220)

I

II

II

III

0.223 nmMo0(110)

0.192 nmMoO2(201)

III

0.233 nmMoO2(111)

0.233 nmMoO2(111)

0.233 nmMoO2(111)

0.336 nmMoO2(110)

0.168 nmMoO2(220)

0.233 nmMoO2(111) 0.192 nm

MoO2(201)

0.238 nmMoO2(200)

Fig. S9. HRTEM images and FFT patterns of E-CoMo900/CP.

Co0.66Mo0.16O0.18

Co0.41Mo0.20O0.39

Co0.69Mo0.19O0.12

100 nm

100 nm

(c)

(a)

(b)

100 nm

Fig. S10. EDS spectra of E-CoMo900/CP at the (a) surface, (b) interior, and (c) projected area.

11

240 238 236 234 232 230 228 226 224

Inte

nsity

/ a.

u.

Binding energy / eV800 795 790 785 780 775

Inte

nsity

/ a.

u.

Binding energy / eV

5000 cps

5000 cps

5000 cps

5000 cps

5000 cps

E-CoMo300/CP

E-CoMo600/CP

E-CoMo900/CP

E-CoMo1200/CP

E-CoMo1800/CP

5000 cps

5000 cps

5000 cps

5000 cps

5000 cps

E-CoMo300/CP

E-CoMo600/CP

E-CoMo900/CP

E-CoMo1200/CP

E-CoMo1800/CP

(b)(a)

Fig. S11. (a) Co 2p and (b) Mo 3d XPS spectra of E-CoMo#/CP.

1.3 1.4 1.5 1.6 1.7 1.8

0.05

0.06

0.07

0.08

0.09

0.10

0.11

0.12

0.13

0.14

E-CoMo300/CP E-CoMo600/CP E-CoMo900/CP E-CoMo1200/CP E-CoMo1800/CP

Pote

ntia

l (iR

-cor

rect

ed) /

V v

s. R

HE

log (-j / mA cm-2geo)

(a) (b)

0 2 4 6 8 10 12 14 16 18 20 22

0

2

4

6

8

10

12


Z''

/

Z' /

11.7 Ω

6.8 Ω

20.3 Ω

6.0 Ω4.6 Ω

Fig. S12. (a) Tafel plots of the data in Fig. 6a. (b) Nyquist plots for E-CoMo#/CP measured at a

potential of –0.13 VRHE in N2-purged 0.5 M H2SO4 electrolyte.

12

-0.11 -0.10 -0.09 -0.08 -0.07 -0.06 -0.05-1.5

-1.0

-0.5

0.0

0.5

1.0

1.5

Cur

rent

den

sity

/ m

A c

m-2 ge

o


-0.15 -0.14 -0.13 -0.12 -0.11 -0.10

-2.0

-1.5

-1.0

-0.5

0.0

0.5

1.0

1.5

2.0

Cur

rent

den

sity

/ m

A c

m-2 ge

o

Potential / V vs. SCE-0.21 -0.20 -0.19 -0.18 -0.17 -0.16

-3

-2

-1

0

1

2

3

Cur

rent

den

sity

/ m

A c

m-2 ge

o


-0.28 -0.27 -0.26 -0.25 -0.24 -0.23 -0.22-6

-4

-2

0

2

4

6

Cur

rent

den

sity

/ m

A c

m-2 ge

o

Potential / V vs. SCE-0.29 -0.28 -0.27 -0.26 -0.25 -0.24

-8

-6

-4

-2

0

2

4

6

8

Cur

rent

den

sity

/ m

A c

m-2 ge

o


0.48 0.49 0.50 0.51 0.52 0.53 0.54

-0.00008

-0.00004

0.00000

0.00004

0.00008

0.00012 5 mV/s 6 mV/s 7 mV/s

C

urre

nt d

ensi

ty /

mA

cm

-2 geo


1 mV/s 2 mV/s 3 mV/s 4 mV/s

(a) (b)

(e) (f)

(d)(c)

Fig. S13. Repeated CV curves of (a) bare CP, (b) E-CoMo300/CP, (c) E-CoMo600/CP, (d) E-

CoMo900/CP, (e) E-CoMo1200/CP, and (f) E-CoMo1800/CP at various scan rates in N2-purged 0.5 M

H2SO4 electrolyte.

13

240 238 236 234 232 230 228 226 224

Inte

nsity

/ a.

u.

Binding energy / eV800 795 790 785 780 775

Inte

nsity

/ a.

u.

Binding energy / eV

E-CoMo300/CP

E-CoMo600/CP

E-CoMo900/CP

E-CoMo1200/CP

E-CoMo1800/CP

5000 cps

5000 cps

5000 cps

5000 cps

5000 cps

5000 cps

5000 cps

5000 cps

5000 cps

5000 cps

E-CoMo300/CP

E-CoMo600/CP

E-CoMo900/CP

E-CoMo1200/CP

E-CoMo1800/CP

(b)(a)

Fig. S14. (a) Co 2p and (b) Mo 3d XPS spectra of E-CoMo#/CP after chronoamperometry at –0.11

VNHE for 1800 s.

0 200 400 600 800 1000 1200 1400 1600 1800 2000-30-28-26-24-22-20-18-16-14-12-10-8-6-4-20

Cur

rent

den

sity

/ m

A c

m-2 ge

o

Time / s


0 200 400 600 800 1000 1200 1400 1600 1800 2000-30-28-26-24-22-20-18-16-14-12-10-8-6-4-20

Cur

rent

den

sity

/ m

A c

m-2 ge

o

Time / s


0 200 400 600 800 1000 1200 1400 1600 1800 2000-30-28-26-24-22-20-18-16-14-12-10-8-6-4-20

Cur

rent

den

sity

/ m

A c

m-2 ge

o

Time / s


(a) (b) (c)

Fig. S15. Chronoamperometry of E-CoMo#/CP at –0.11 VNHE for 1800 s in the (a) 1st, (b) 2nd, and (c)

3rd test.

14

0

2

4

6

8

10

12

14

16

Loa

ding

mas

s / m

g cat c

m-2

0

-2

-4

-6

-8

-10

Mas

s act

ivity

/ m

A m

g-1 cat

(a) (b)

Fig. S16. (a) Catalyst loading mass of E-CoMo#/CP. (b) Mass activity calculated from the

chronoamperometry at -0.11 VNHE (Fig. 6d).

-0.15 -0.12 -0.09 -0.06 -0.03 0.00 0.03-50

-40

-30

-20

-10

0

10

Cur

rent

den

sity

/ m

A c

m-2 ge

o



-0.15 -0.12 -0.09 -0.06 -0.03 0.00 0.03-7.5

-5.0

-2.5

0.0

2.5


Mas

s act

ivity

/ m

A m

g cat-1


-0.15 -0.12 -0.09 -0.06 -0.03 0.00 0.03-0.10

-0.08

-0.06

-0.04

-0.02

0.00

0.02


Scal

ed c

urre

nt /

mA

mF-1


(a) (b)

(c)

0

20

40

60

80

100

120

140

Ove

rpot

entia

l (iR

-cor

rect

ed) /

mV At -50 mA/cm2

geo

At -0.10 mA/mF1

At -7.5 mA/mgcat

(d)

Fig. S17. Potentiodynamic curves based on the (a) geometric current density, (b) scaled current, and

(c) mass activity. (d) Summary on the HER overpotential of E-CoMo#/CP.

15

-0.06 VNHE, 270 ~ 300 s -0.06 VNHE, 1770 ~ 1800 s

-0.11 VNHE, 270 ~ 300 s -0.11 VNHE, 1770 ~ 1800 s

-0.16 VNHE, 270 ~ 300 s -0.16 VNHE, 1770 ~ 1800 s

-0.21 VNHE, 270 ~ 300 s -0.21 VNHE, 1770 ~ 1800 s

-0.26 VNHE, 270 ~ 300 s -0.26 VNHE, 1770 ~ 1800 s

-0.31 VNHE, 270 ~ 300 s -0.31 VNHE, 1770 ~ 1800 s

H2 FE : 35.0 ±1.2% H2 FE : 98.2 ±0.8%

H2 FE : 33.7 ±1.5% H2 FE : 102.5 ±1.7%

H2 FE : 37.8 ±0.5% H2 FE : 102.8 ±0.3%

H2 FE : 41.1 ±2.3% H2 FE : 104.3 ±0.1%

H2 FE : 43.5 ±3.7% H2 FE : 104.2 ±0.7%

H2 FE : 42.2 ±0.7% H2 FE : 103.3 ±1.6%

(a)

(c)

(e)

(g)

(i)

(k)

(b)

(d)

(f)

(h)

(j)

(l)

Fig. S18. Gas chromatography analysis of E-CoMo900/CP depending on the applied potential and

measuring time.

16

800 795 790 785 780 775

Inte

nsity

/ a.

u.

Binding energy / eV

10 s

100 s

300 s

600 s

1200 s

1800 s

5000 cps

5000 cps

5000 cps

5000 cps

5000 cps

5000 cps

240 238 236 234 232 230 228 226 224

Inte

nsity

/ a.

u.

Binding energy / eV

5000 cps

5000 cps

5000 cps

5000 cps

5000 cps

5000 cps

(b)(a)10 s

100 s

300 s

600 s

1200 s

1800 s

Fig. S19. (a) Co 2p and (b) Mo 3d XPS spectra of E-CoMo900/CP after chronoamperometry at –0.11

VNHE for 10, 100, 300, 600, 1200, and 1800 s.

17

800 795 790 785 780 775

Inte

nsity

/ a.u

.

Binding energy / eV

5000 cps

5000 cps

5000 cps

5000 cps

5000 cps

5000 cps

5000 cps

5000 cps

5000 cps

5000 cps

5000 cps

5000 cps

240 238 236 234 232 230 228 226 224

Inte

ntis

y / a

.u.

Binding energy / eV

(b)(a)10 s

100 s

300 s

600 s

1200 s

1800 s

10 s

100 s

300 s

600 s

1200 s

1800 s

Fig. S20. (a) Co 2p and (b) Mo 3d XPS spectra of E-CoMo900/CP after chronoamperometry at –0.31

VNHE for 10, 100, 300, 600, 1200, and 1800 s.

18

2.0 2.5 3.0 3.5 4.0 4.50.0

0.1

0.2

0.3

0.4

0.5

0.6

0.7

Z

'' /

Z' /

Rsol = 2.29 Ω

Fig. S21. Nyquist plots for E-CoMo900/CP measured at H-type cell at a potential of –0.13 VRHE in N2-purged 0.5 M H2SO4 electrolyte.

-0.20 -0.16 -0.12 -0.08 -0.04 0.00-100

-80

-60

-40

-20

0

20

Cur

rent

den

sity

/ m

A c

m-2 ge

o


Before stability test After stability test

9.8 mV

Fig. S22. LSV curves of E-CoMo900/CP before and after long-term stability test in H-type cell containing N2-purged 0.5 M H2SO4 electrolyte.

19

(a)

(b)

End plate

Bipolar plate

Membrane

Catalyst

Gasket

0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7

1.5

1.6

1.7

1.8

1.9

2.0

E-CoMo900/CP IrO2/CP

Cel

l vol

tage

/ V

cell

Current density / A cm-2geo

(c)

Fig. S23. Photographs of (a) parts in the PEMWE single cell configuration and (b) the assembled

single cell. (c) Polarization curve of PEMWE single cell employing E-CoMo900/CP cathode and

IrO2/CP anode.

References

20

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ars.els-cdn.com · Web viewLSV curves of E-CoMo900/CP before and after long-term stability test in H-type cell containing N 2-purged 0.5 M H 2 SO 4 electrolyte. Fig. S 2 3 . Photographs