MANIFEST Researcher Workshop

3D imaging studies on

electrochemical systems at

Imperial College London

Dami Taiwo, Vladimir Yufit, Farid Tariq, Enrique Ruiz-Trejo, Antonio Bertei,

Kristina Maria Kareh, Ann Huang, Barun Chakrabarti, Moshiel Biton,

Sam Cooper, Nigel P. Brandon

10 November 2017

Batteries and fuel cells

Electrode microstructurefor

Performance optimisation

↓Bulk properties• volume fractions• connectivity• area per unit

volume

Degradation

↓Local hot spots

Structural evolution

3D Imaging Facilities

• Lab X-ray CT* unit with high-efficiency flat panel

detector.

• Up to 1 µm spatial resolution.

• Capability to incorporate in-situ rigs for dynamic

experiments.

• Access to FIB-SEM tomography equipment.

• High spatial resolution (<10 nm for FIB imaging).

• Better suited for nanostructured material analysis.

*From energy storage capital grant : EPSRC Capital for Great Technologies call - Grid-Scale Energy Storage

Zn dendrite formation during the first charge

Zn(OH)42-

KOH

additives

Pump

Zn + 4OH- ↔Zn(OH)42- + 2e-

Load / Power generator

1/2O2 + H2O + 2e- ↔ 2OH-

OH-OH-

ZnZn

Air

Air

Zinc-based flow batteries – Morphological degradation of Zn

5

M. Biton,F. Tariq,V. Yufit, Z. Chen,N. Brandon, Acta Materialia 2017, 141, 39-46

Zn(OH)42-

KOH

additives

Pump

Zn + 4OH- ↔Zn(OH)42- + 2e-

Load / Power generator

1/2O2 + H2O + 2e- ↔ 2OH-

OH-OH-

ZnZn

Air

Air

Zinc-based flow batteries – Morphological degradation of Zn

In-situ observation of Zn dendritic growth

M. Biton,F. Tariq,V. Yufit, Z. Chen,N. Brandon, Acta Materialia 2017, 141, 39-46

6

No rGO Single side rGO Double side rGO

Vanadium redox flow batteries – Carbon paper modification

Total specific

surface area with

XCT [μm2 μm−3]

BET specific

surface area

[μm2 μm−3]

Untreated CP 0.81 2.8

One-sided 1.01 5.1

Double sided 1.11 11.1

B. Chakrabarti, D. Nir, V. Yufit, F. Tariq, J. Rubio-Garcia, R. Maher, A. Kucernak, P. Aravind, N. Brandon, ChemElectroChem 2017, 4, 194.

Lithium-ion batteries – Thick electrodes with controlled porosity

Image ref: Deville, S., Ice templating of

porous materials

Cross section

SEM

X-ray µCT

• In collaboration with Prof. P. Grant and Dr. A. Huang (Oxford)

• Manufacture of thick high energy density electrodes

• Improve battery power through microstructure control

Si/SiOX

Solid Oxide Fuel Cells – Microstructural degradation in NiScSZ

1 μm

1 μm

(xy) slice

Deg

rad

ed

an

od

e

Init

ial

an

od

e

Ni + ScSZ

1 µm

1 µm

TPBsFIB-SEM

0

5

10

15

20

0 5 10 15 20 25 30 35 40

-ZIm

/ W

cm

-2

ZRe / W cm-2

200 h80 h24 h2 h0.5 h

x19550 C @ OCV5% H2/3% H2O

oxygentransfer

ScSZ-YSZ

distributedcharge transfer

at TPB

gasdiffusiontest rig

ohmic

A.Bertei, E.Ruiz-Trejo, K.Kareh, V.Yufit, X.Wang, F.Tariq, N.P.Brandon, Nano Energy 2017, 36, 526-536

Solid Oxide Fuel Cells – Microstructural degradation in NiScSZ

0.0

0.5

1.0

1.5

2.0

2.5

3.0

NiS

cS

z a

rea (

m2

m-3) Initial

Degraded

2.39 1.85

0

5

10

15

20

25

TP

B d

en

sit

y (

m

m-3) Initial

Degraded

19.77 11.67

1 μm

1 μm

(xy) slice

De

gra

de

d a

no

de

In

itia

l a

no

de

Ni + ScSZ

1 µm

1 µm

TPBsNi + ScSZ

1 μm

1 μm

(xy) slice

De

gra

de

d a

no

de

In

itia

l a

no

de

Ni + ScSZ

1 µm

1 µm

TPBs

A.Bertei, E.Ruiz-Trejo, K.Kareh, V.Yufit, X.Wang, F.Tariq, N.P.Brandon, Nano Energy 2017, 36, 526-536

Thanks to..

Vladimir

Yufit

Farid Tariq Sam Cooper Enrique

Ruiz-Trejo

Antonio

Bertei

Kristina

Maria KarehBarun

Chakrabarti

Ann HuangMoshiel

Biton