Nanomaterials for Electrocatalysis

Thandavarayan Maiyalagan
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Nanomaterials for
Electrocatalysis
 Micro and Nano Technologies Series

Nanomaterials for
Electrocatalysis
Edited by

Thandavarayan Maiyalagan
Department of Chemistry, SRM Institute of Science
and Technology, Kattankulathur, India

Mahima Khandelwal
Department of Materials Science and Engineering,
Korea University, Seoul, South Korea

Ashok Kumar Nadda

Department of Biotechnology and Bionformatics,
Jaypee University of Information Technology,
Waknaghat, India

Tuan Anh Nguyen

Microanalysis Department, Institute for Tropical
Technology, Vietnam Academy of Science and
Technology, Hanoi, Vietnam

Ghulam Yasin
Institute for Advanced Study, College of Physics and
Optoelectronic Engineering, Shenzhen University,
Shenzhen, Guangdong, China
Elsevier
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Contents

Contributors . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . xv
Preface ... . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . xix

PART 1 Introduction
CHAPTER 1 Nanoelectrocatalysis: An introduction ..................... 3
Ghulam Yasin, Shumaila Ibraheem, Rashid Iqbal,
Anuj Kumar and Tuan Anh Nguyen
1.1 Introduction .. .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. 3
1.2 Construction and characterization of nanostructures . ... .. .. .. ... .. 4
1.3 Efficient electrocatalysis enabled by nanostructures . ... .. .. .. ... .. . 4
1.3.1 Low-dimensional nanostructures . .. ... .. .. .. ... .. .. ... .. .. .. .. 4
1.3.2 2D nanostructures .. .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. .. 5
1.3.3 3D nanostructures .. .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. .. 6
1.4 Conclusion ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. ... .. .. .. ... .. .. .. 6
References .. .. ... .. .. .. ... .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .6
CHAPTER 2 2D hybrid electrocatalysts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11
Rashid Iqbal, Shumaila Ibraheem, Mohammad Tabish,
Adil Saleem, Anuj Kumar, Tuan Anh Nguyen and
Ghulam Yasin
2.1 Introduction .. .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. ... .. .. .. ... .. .. . 11
2.2 Graphene-based electrocatalysts .. .. ... .. .. ... .. .. .. ... .. .. .. ... .. .. 12
2.3 Graphene nonmetallic composites .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. . 13
2.4 Graphene-metallic composites .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. 15
2.5 Conclusion ... .. .. .. ... .. .. .. ... .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. . 16
References . .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. ... .. .. .. ... .. .. .. . 17
CHAPTER 3 MXene-based nanomaterials for electrocatalysis .... 23
Anuj Kumar, Charu Goyal, Sonali Gautam,
Shumaila Ibraheem, Tuan Anh Nguyen and Ghulam Yasin
3.1 Introduction .. .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. ... .. .. .. ... .. .. . 23
3.2 Structural and electronic properties . .. .. ... .. .. .. ... .. .. .. ... .. .. .. .24
3.2.1 Structural properties . .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... 24
3.2.2 Electronic properties . ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. ... .. .. 25
3.3 Engineering of MXene-based nanomaterial .. ... .. .. ... .. .. .. ... .. .27
3.3.1 HF etching . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27
3.3.2 Lewis acidic etching . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28

v
vi Contents

3.3.3 Water-free etching . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .30

3.3.4 Treatment with alkali . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 30
3.3.5 Electrochemical etching .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. 31
3.3.6 Chemical vapor deposition method .. .. .. ... .. .. .. ... .. .. .. .. 31
3.4 Applications in electrocatalysis .. .. .. ... .. .. .. ... .. .. ... .. .. .. ... .. . 31
3.4.1 Oxygen reduction reaction .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. .. 35
3.4.2 Oxygen evolution reaction .. .. .. ... .. .. .. ... .. .. ... .. .. .. ... ..35
3.4.3 Hydrogen evolution reaction . ... .. .. ... .. .. .. ... .. .. .. ... .. .. 39
3.4.4 CO2 reduction reaction .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. . 40
3.5 Summary and outlook . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .42
References . .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. ... .. .. .. ... .. .. .. . 42

PART 2 Nanomaterials for Electrocatalytic reactions

such as ORR, OER and HER
CHAPTER 4 Transition metal nanoparticles as
electrocatalysts for ORR, OER, and HER . . . . . . . . . . . . . . . . . 49
Dinh Chuong Nguyen, Thi Luu Luyen Doan,
Duy Thanh Tran, Nam Hoon Kim and Joong Hee Lee
4.1 Introduction .. .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. ... .. .. .. ... .. .. . 49
4.2 Synthesis methods of the TM nanoparticle-based catalysts . .. .. ..50
4.2.1 Hydrothermal method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .50
4.2.2 Solvothermal method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 52
4.2.3 Chemical reduction method ... .. .. ... .. .. .. ... .. .. .. ... .. .. .. 53
4.2.4 Electrochemical deposition method .. .. .. ... .. .. .. ... .. .. .. . 55
4.2.5 Other synthetic methods .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. 56
4.3 Structure and properties of TM nanoparticle-based catalysts . .. ..57
4.3.1 Substrate-free TM nanoparticle-based catalysts .. ... .. .. .. . 57
4.3.2 Carbon substrate-assisted TM nanoparticle-based
catalysts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 61
4.3.3 Metallic substrate-assisted TM nanoparticle-based
catalysts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 64
4.4 Applications of TM nanoparticle-based catalysts toward
the ORR, HER, and OER . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 66
4.4.1 ORR applications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 66
4.4.2 HER applications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .68
4.4.3 OER applications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .69
4.5 Summary . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 70
References . .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. ... .. .. .. ... .. .. .. . 72
 Contents vii

CHAPTER 5 Transition metal chalcogenides-based

electrocatalysts for ORR, OER, and HER . . . . . . . . . . . . . . . . . 83
Tenzin Ingsel and Ram K. Gupta
5.1 Introduction .. .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. ... .. .. .. ... .. .. . 83
5.1.1 Overpotential (η) .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 86
5.1.2 Tafel plot . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 86
5.1.3 Faradaic efficiency . ... .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. 86
5.1.4 Stability .. .. ... .. .. .. ... .. .. .. ... .. .. ... .. .. .. ... .. .. .. ... .. .. .. 86
5.2 Synthesis of metal chalcogenides . .. .. .. ... .. .. .. ... .. .. ... .. .. .. ... 87
5.2.1 Solvothermal .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .87
5.2.2 Chemical vapor deposition .. ... .. .. .. ... .. .. ... .. .. .. ... .. .. . 88
5.2.3 Other methods .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. 88
5.3 Transition metal chalcogenides-based electrocatalysts
for OER . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 89
5.4 Transition metal chalcogenides-based electrocatalysts
for ORR . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 92
5.5 Transition metal chalcogenides-based electrocatalysts
for HER . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 98
5.6 Transition metal chalcogenides-based multifunctional
electrocatalysts .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. ... .. .. .. 103
5.7 Conclusion and outlook .. .. ... .. .. .. ... .. .. ... .. .. .. ... .. .. .. ... .. . 105
Acknowledgment .. .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. 106
References . .. .. .. ... .. .. .. ... .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. 106
CHAPTER 6 Metal-organic framework-based electrocatalysts
for ORR, OER, and HER . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 111
Muhammad Rizwan Sulaiman and Ram K. Gupta
6.1 Introduction .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. . 111
6.2 MOF-based electrocatalysts for ORR . ... .. .. .. ... .. .. .. ... .. .. .. . 116
6.2.1 MOF-derived nitrogen-doped carbon-based
electrocatalysts for ORR . .. .. .. ... .. .. .. ... .. .. ... .. .. .. ... . 117
6.2.2 MOF-derived nonprecious metal-based
electrocatalysts for ORR . .. .. .. ... .. .. .. ... .. .. ... .. .. .. ... . 120
6.3 MOF-based electrocatalysts for OER . ... .. .. .. ... .. .. .. ... .. .. .. . 124
6.3.1 MOF-derived metal-free materials for OER
electrocatalyst . .. .. .. ... .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. 124
6.3.2 MOF-derived nonprecious metal-based OER
electrocatalyst . .. .. .. ... .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. 126
6.4 MOF-based electrocatalysts for HER . ... .. .. .. ... .. .. .. ... .. .. .. . 130
viii Contents

6.4.1 MOF-derived metal-free carbon-based material

for HER . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .131
6.4.2 MOF-derived NPM-based electrocatalyst for HER . .. ... .132
6.4.3 Metal carbide, phosphides, and chalcogenides . .. ... .. .. .. 133
6.5 MOF-based multifunctional electrocatalysts ... .. .. ... .. .. .. ... .. 136
6.5.1 MOF-derived OER/ORR bifunctional electrocatalysts . .. 136
6.5.2 MOF-derived HER/OER bifunctional electrocatalysts . .. 137
6.5.3 MOF-derived HER/ORR bifunctional electrocatalysts . .. 137
6.5.4 MOF-derived HER/OER/ORR trifunctional
electrocatalysts . .. .. .. ... .. .. .. ... .. .. .. ... .. .. ... .. .. .. ... .. . 138
6.6 Summary . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 138
References . .. .. .. ... .. .. .. ... .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. 139
CHAPTER 7 Heteroatom-doped graphene-based
electrocatalysts for ORR, OER, and HER . . . . . . . . . . . . . . . 145
Xun Cui, Likun Gao, Yingkui Yang and Zhiqun Lin
7.1 Introduction .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. . 145
7.2 Overview of graphene and heteroatom-doped
graphene-based materials .. ... .. .. .. ... .. .. .. ... .. .. ... .. .. .. ... .. . 147
7.2.1 Graphene . .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. 147
7.2.2 Heteroatom-doped graphene-based materials .. ... .. .. .. .. 149
7.2.3 Synthesis of heteroatom-doped graphene-based
materials . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 151
7.3 Heteroatom-doped graphene-based materials
as electrocatalysts for ORR, OER, and HER .. .. .. ... .. .. .. ... .. . 152
7.3.1 Heteroatom-doped graphene-based materials
for ORR . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .152
7.3.2 Heteroatom-doped graphene-based materials
for OER . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .156
7.3.3 Heteroatom-doped graphene-based materials
for HER . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .158
7.4 Summary and perspective .. .. .. .. ... .. .. .. ... .. .. .. ... .. .. ... .. .. .. 160
Acknowledgments . ... .. .. .. ... .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. . 161
References . .. .. .. ... .. .. .. ... .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. 161
CHAPTER 8 Metal-containing heteroatom doped carbon
nanomaterials for ORR, OER, and HER . . . . . . . . . . . . . . . . . . 169
Álvaro García, Jorge Torrero, María Retuerto
and Sergio Rojas
8.1 Introduction .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. . 169
8.2 M/N/C catalysts for the ORR .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 170
 Contents ix

8.3 Synthesis of highly active M/N/C catalyst for the ORR . .. .. ... . 177
8.3.1 Fe/N/M catalysts derived from metal-organic
frameworks . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 177
8.3.2 Fe/M/N catalysts from sacrificial templates . .. ... .. .. .. ... 178
8.3.3 Fe/N/C catalysts derived from PANI . .. ... .. .. .. ... .. .. .. .. 180
8.3.4 Fe/N/C catalyst from porous organic polymers as
precursors . ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. ..181
8.3.5 Other strategies for obtaining highly active M/N/C
catalysts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .181
8.4 Assessment of ORR performance of M/N/C catalysts .. .. ... .. .. 181
8.5 Physicochemical characterization of pyrolyzed M/N/C
catalysts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .185
8.5.1 Mössbauer spectroscopy . .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... . 186
8.5.2 X-ray photoelectron spectroscopy ... .. .. .. ... .. .. .. ... .. .. .189
8.5.3 X-ray absorption spectroscopy .. ... .. .. .. ... .. .. .. ... .. .. .. 191
8.5.4 Transmission electron microscopy .. .. .. ... .. .. .. ... .. .. .. . 194
8.6 Metal-containing heteroatom-doped carbon
nanomaterials for OER and HER reactions . .. ... .. .. .. ... .. .. .. ..195
References . .. .. .. ... .. .. .. ... .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. 200
CHAPTER 9 Metal-organic frameworks for the electrocatalytic
ORR and HER . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 211
Anuj Kumar, Shashank Sundriyal, Charu Goyal,
Tribani Boruah, Dipak Kumar Das, Ghulam Yasin,
Tuan Anh Nguyen and Sonali Gautam
9.1 Introduction .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. . 211
9.2 Engineering and effective strategies for modification of MOFs 212
9.2.1 Modification of MOFs by doping . .. .. .. ... .. .. .. ... .. .. .. . 212
9.2.2 MOF-derived materials . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .214
9.2.3 MOF-based composites . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 217
9.3 Applications of MOFs-based materials in fuel cells . .. .. ... .. .. . 220
9.3.1 MOFs for electrocatalytic ORR . .. ... .. .. .. ... .. .. .. ... .. .. 221
9.3.2 MOFs for hydrogen production .. .. .. .. ... .. .. .. ... .. .. .. .. 223
9.4 Conclusion and future prospects . .. .. ... .. .. .. ... .. .. .. ... .. .. .. ...229
References . .. .. .. ... .. .. .. ... .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. 229
CHAPTER 10 LDH-based nanostructured electrocatalysts
for hydrogen production . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 237
Mohammad Tabish, Shumaila Ibraheem,
Muhammad Asim Mushtaq, Rashid Iqbal,
Tuan Anh Nguyen and Ghulam Yasin
x Contents

10.1 Introduction .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. . 237

10.2 Construction of TM-LDH nanostructures . .. ... .. .. .. ... .. .. .. ... .238
10.2.1 Bottom-up approaches .. .. .. ... .. .. .. ... .. .. .. ... .. .. ... .. . 238
10.2.2 Top-down approaches . ... .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... 240
10.3 Carbon nanomaterial-based TM-LDH nanohybrids . .. .. .. ... .. . 240
10.4 Electrocatalytic application for hydrogen production .. .. .. ... .. .241
10.5 Conclusion ... .. .. .. ... .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. ..245
References . .. .. .. ... .. .. .. ... .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. 246
CHAPTER 11 MOFs-derived hollow structure as a versatile
platform for highly-efficient multifunctional
electrocatalyst toward overall water-splitting
and Zn-air battery . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 251
Lei Zhang, Yuan-Xin Zhu and Guang-Zhi Hu
11.1 Introduction .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. . 251
11.2 Brief classification of hollow structures based on
their geometrical configuration . .. .. .. ... .. .. .. ... .. .. ... .. .. .. ... . 252
11.2.1 Single-shelled hollow structures . . . . . . . . . . . . . . . . . . . . . . . . . . 252
11.2.2 Multishelled hollow structures . .. .. .. ... .. .. .. ... .. .. .. ... 253
11.2.3 Other complex hollow structures . . . . . . . . . . . . . . . . . . . . . . . . . .254
11.3 Active regulation strategy . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 257
11.3.1 Active site assembly . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 257
11.3.2 Electronic structure effect . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 259
11.3.3 Single-atom catalyst . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .260
11.3.4 Defect chemistry . .. ... .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. . 262
11.3.5 Synergistic catalysis . .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. .262
11.4 Conclusions and perspectives .. ... .. .. .. ... .. .. .. ... .. .. ... .. .. .. .. 265
Acknowledgments . ... .. .. .. ... .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. . 265
References . .. .. .. ... .. .. .. ... .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. 265

PART 3 Nanomaterials for Electrochemical Nitrogen

reduction reaction (NRR)
CHAPTER 12 Noble-metals-free catalysts for
electrochemical NRR . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 273
Xue Zhao and Guangzhi Hu
12.1 Introduction .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. . 273
12.2 Non-noble metal-based metal catalysts .. .. ... .. .. ... .. .. .. ... .. .. 274
12.2.1 Mo-based catalysts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 274
12.2.2 Fe-based catalysts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 277
 Contents xi

12.2.3 Ti-based catalysts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .279

12.2.4 Bi-based catalysts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 282
12.2.5 Co, Ni-based catalysts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 283
12.2.6 Other non-noble metal metal-based catalysts .. .. ... .. .. . 284
12.3 Non-metal-based catalysts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 285
12.3.1 B-based NRR catalysts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 286
12.3.2 N-based catalysts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 288
12.3.3 O- and S-based catalysts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 290
12.3.4 P-based catalysts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 291
Competing interests . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .291
Acknowledgments . ... .. .. .. ... .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. . 291
References . .. .. .. ... .. .. .. ... .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. 291
CHAPTER 13 Noble metals-based nanocatalysts for
electrochemical NNR . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 299
Jing Li, Zihao Ye and Weiwei Cai
13.1 Introduction .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. . 299
13.2 Ru-based NRR catalysts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .300
13.2.1 Single-atom Ru-based NRR catalysts . ... .. .. .. ... .. .. .. . 300
13.2.2 Supported Ru-based NRR catalysts . .. .. ... .. .. .. ... .. .. ..301
13.2.3 Ru-based alloy catalysts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 303
13.3 Au-based NRR catalysts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 304
13.3.1 Au catalyst nanostructure adjusting .. .. ... .. .. .. ... .. .. .. .306
13.3.2 Supported Au-based NRR catalysts ... .. .. .. ... .. .. .. ... . 307
13.3.3 Au-based alloy NRR catalyst . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .308
13.4 Other noble metal-based NRR catalysts .. .. ... .. .. .. ... .. .. .. ... . 310
13.4.1 Pd-based NRR catalysts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 310
13.4.2 Pt-based NRR catalysts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 311
13.5 Conclusions and prospects . .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. .. 312
References . .. .. .. ... .. .. .. ... .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. 313
CHAPTER 14 Electrochemical NRR with noble metals-based
nanocatalysts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 317
Mohd Khalid, Mohammad Rafe Hatshan,
Ana Maria Borges Honorato, Bijandra Kumar
and Hamilton Varela
14.1 Introduction .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. . 317
14.2 NRR mechanism . .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. ... . 318
14.3 Types of the electrochemical cell for NRR ... .. .. ... .. .. .. ... .. .. 320
14.4 Electrolytes for NRR . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 322
14.5 NRR based on noble metals .. .. ... .. .. ... .. .. .. ... .. .. .. ... .. .. .. ..323
xii Contents

14.6 NRR based on Au nanocatalysts .. .. .. ... .. .. .. ... .. .. .. ... .. .. ... .324

14.7 NRR based on Ru nanocatalysts . .. .. .. ... .. .. .. ... .. .. .. ... .. .. ...326
14.8 NRR based on Pd nanocatalysts .. .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. 327
14.9 Conclusions and outlook .. .. ... .. .. .. ... .. .. .. ... .. .. ... .. .. .. ... .. 328
Acknowledgments . ... .. .. .. ... .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. . 329
References . .. .. .. ... .. .. .. ... .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. 330
CHAPTER 15 Electrochemical NRR with noble metals-free
catalysts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 335
Zehui Yang, Quan Zhang and Shenglin Xiao
15.1 Introduction .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. . 335
15.2 Transition metal oxides-based electrocatalysts ... .. .. .. ... .. .. .. . 336
15.2.1 Titanium oxides . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 336
15.2.2 Chromium oxides . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 338
15.2.3 Manganese oxides .. .. .. ... .. .. .. ... .. .. ... .. .. .. ... .. .. .. .. 338
15.2.4 Iron oxides . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 340
15.2.5 Nickel-based oxides . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 341
15.2.6 Niobium oxides . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .342
15.2.7 Other transition metal oxides .. ... .. .. .. ... .. .. ... .. .. .. ...342
15.3 Transition metal sulfides-based electrocatalysts ... .. .. .. ... .. .. ..346
15.3.1 Molybdenum sulfides .. .. .. .. ... .. .. ... .. .. .. ... .. .. .. ... .. 346
15.3.2 Iron sulfides . .. .. .. ... .. .. .. ... .. .. ... .. .. .. ... .. .. .. ... .. .. . 348
15.3.3 Other transition metal sulfides . .. .. ... .. .. .. ... .. .. .. ... .. 350
15.4 Transition metal nitride-based electrocatalysts ... .. .. .. ... .. .. .. . 351
15.5 Transition metal phosphides-based electrocatalysts .. ... .. .. .. ...353
15.5.1 Cobalt phosphides .. .. ... .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... . 353
15.5.2 Nickel phosphides .. ... .. .. .. ... .. .. .. ... .. .. ... .. .. .. ... .. . 355
15.5.3 Iron phosphides ... .. .. .. ... .. .. .. ... .. .. ... .. .. .. ... .. .. .. ..355
15.6 Transition metal carbides-based electrocatalysts . ... .. .. .. ... .. .. 357
15.6.1 Mxene-based electrocatalysts .. .. ... .. .. .. ... .. .. .. ... .. .. 357
15.6.2 Molybdenum carbides-based electrocatalysts .. ... .. .. .. .357
15.7 Metal-free electrocatalysts . ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. ... .. . 358
15.7.1 Boron-doped carbon .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. . 358
15.7.2 Nitrogen-doped carbon .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... 360
15.7.3 Fluorine-doped carbon . .. .. ... .. .. .. ... .. .. .. ... .. .. ... .. .. 360
15.7.4 Sulfur-doped carbon .. .. ... .. .. .. ... .. .. .. ... .. .. ... .. .. .. . 362
15.7.5 Black phosphorus . .. .. ... .. .. .. ... .. .. ... .. .. .. ... .. .. .. ... 363
15.8 Conclusion ... .. .. .. ... .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. ..363
References . .. .. .. ... .. .. .. ... .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. 364
 Contents xiii

PART 4 Nanomaterials for Electrochemical CO2

reduction reaction
CHAPTER 16 Nanomaterials for electrochemical reduction
of CO2 : An introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 373
Anuj Kumar, Ghulam Yasin and Tuan Anh Nguyen
References . .. .. .. ... .. .. .. ... .. .. ... .. .. .. ... .. .. .. ... .. .. .. ... .. .. .. 375
Index ...... . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 377
Contributors

Tribani Boruah
Northeast Hill University (NEHU), Umshing Mawkynroh, Shillong, Meghalaya,
India
Weiwei Cai
Sustainable Energy Laboratory, Faculty of Materials Science and Chemistry,
China University of Geosciences, Wuhan, China
Xun Cui
School of Materials Science and Engineering, Georgia Institute of Technology,
Atlanta, GA, United States; Key Laboratory of Catalysis and Energy Materials
Chemistry of Ministry of Education and Hubei Key Laboratory of Catalysis
and Materials Science, South-Central University for Nationalities, Wuhan,
China
Dipak Kumar Das
Department of Chemistry, GLA University, Mathura, Uttar Pradesh, India
Thi Luu Luyen Doan
Department of Nano Convergence Engineering, Jeonbuk National University,
Jeonju, Jeonbuk, Republic of Korea
Likun Gao
School of Materials Science and Engineering, Georgia Institute of Technology,
Atlanta, GA, United States; Key Laboratory of Bio-based Material Science and
Technology of Ministry of Education, Northeast Forestry University, Harbin,
China
Álvaro García
Grupo de Energía y Química Sostenibles Instituto de Catálisis y Petroleoquímica,
CSIC, Madrid, Spain
Sonali Gautam
Department of Chemistry, GLA University, Mathura, Uttar Pradesh, India
Charu Goyal
Department of Chemistry, GLA University, Mathura, Uttar Pradesh, India
Ram K. Gupta
Department of Chemistry, Kansas Polymer Research Center, Pittsburg State
University, Pittsburg, KS, United States
Mohammad Rafe Hatshan
Department of Chemistry, College of Science, King Saud University, Riyadh,
Saudi Arabia
Ana Maria Borges Honorato
Department of Materials Engineering, Federal University of São Carlos, São
Carlos, SP, Brazil

xv
xvi Contributors

Guangzhi Hu
Institute for Ecological Research and Pollution Control of Plateau Lakes, School
of Ecology and Environmental Science, School of Chemical Science and
Technology, Yunnan University, Kunming, China
Shumaila Ibraheem
Institute for Advanced Study, College of Physics and Optoelectronic Engineering,
Shenzhen University, Shenzhen, Guangdong, China
Tenzin Ingsel
Department of Chemistry, Kansas Polymer Research Center, Pittsburg State
University, Pittsburg, KS, United States
Rashid Iqbal
Institute for Advanced Study, College of Physics and Optoelectronic Engineering,
Shenzhen University, Shenzhen, Guangdong, China
Mohd Khalid
Institute of Chemistry of São Carlos, University of São Paulo, São Carlos, SP,
Brazil
Nam Hoon Kim
Department of Nano Convergence Engineering, Jeonbuk National University,
Jeonju, Jeonbuk, Republic of Korea
Anuj Kumar
Nano-Technology Research Laboratory, Department of Chemistry, GLA
University, Mathura, Uttar Pradesh India; College of Materials Science and
Engineering, Beijing University of Chemical Technology, Beijing, China
Bijandra Kumar
Department of Math., Comp. Sci. and Eng. Technology, Elizabeth City State
University , Elizabeth City, NC, United States
Joong Hee Lee
Department of Nano Convergence Engineering, Jeonbuk National University,
Jeonju, Jeonbuk, Republic of Korea; Carbon Composite Research Center,
Department of Polymer-Nano Science and Technology, Jeonbuk National
University, Jeonju, Jeonbuk, Republic of Korea
Jing Li
Sustainable Energy Laboratory, Faculty of Materials Science and Chemistry,
China University of Geosciences, Wuhan, China
Zhiqun Lin
School of Materials Science and Engineering, Georgia Institute of Technology,
Atlanta, GA, United States

Muhammad Asim Mushtaq

State Key Laboratory of Chemical Resource Engineering, Beijing University of
Chemical Technology, Beijing, China
 Contributors xvii

Dinh Chuong Nguyen

Department of Nano Convergence Engineering, Jeonbuk National University,
Jeonju, Jeonbuk, Republic of Korea
Tuan Anh Nguyen
Institute for Tropical Technology, Vietnam Academy of Science and Technology,
Hanoi, Viet Nam
María Retuerto
Grupo de Energía y Química Sostenibles Instituto de Catálisis y Petroleoquímica,
CSIC, Madrid, Spain
Sergio Rojas
Grupo de Energía y Química Sostenibles Instituto de Catálisis y Petroleoquímica,
CSIC, Madrid, Spain
Adil Saleem
Institute for Advanced Study, Shenzhen University, Shenzhen, Guangdong,
China; College of Physics and Optoelectronic Engineering, Shenzhen University,
Shenzhen, Guangdong, China
Muhammad Rizwan Sulaiman
Department of Chemistry, Kansas Polymer Research Center, Pittsburg State
University, Pittsburg, KS, United States
Shashank Sundriyal
Advanced Carbon Products Department, CSIR-National Physical Laboratory,
New Delhi, India
Mohammad Tabish
State Key Laboratory of Electrochemical Process and Technology for Materials,
College of Materials Science and Engineering, Beijing University of Chemical
Technology, Beijing, China
Jorge Torrero
Grupo de Energía y Química Sostenibles Instituto de Catálisis y Petroleoquímica,
CSIC, Madrid, Spain
Duy Thanh Tran
Department of Nano Convergence Engineering, Jeonbuk National University,
Jeonju, Jeonbuk, Republic of Korea
Hamilton Varela
Institute of Chemistry of São Carlos, University of São Paulo, São Carlos, SP,
Brazil
Shenglin Xiao
Sustainable Energy Laboratory, Faculty of Materials Science and Chemistry,
China University of Geosciences Wuhan, Wuhan, PR China
Yingkui Yang
Key Laboratory of Catalysis and Energy Materials Chemistry of Ministry of
Education and Hubei Key Laboratory of Catalysis and Materials Science,
South-Central University for Nationalities, Wuhan, China
xviii Contributors

Zehui Yang
Sustainable Energy Laboratory, Faculty of Materials Science and Chemistry,
China University of Geosciences Wuhan, Wuhan, PR China
Ghulam Yasin
Institute for Advanced Study, College of Physics and Optoelectronic Engineering,
Shenzhen University, Shenzhen, Guangdong, China
Zihao Ye
Sustainable Energy Laboratory, Faculty of Materials Science and Chemistry,
China University of Geosciences, Wuhan, China
Lei Zhang
School of Materials Science and Engineering, Anhui University of Science and
Technology, Huainan, Anhui, PR China
Quan Zhang
Sustainable Energy Laboratory, Faculty of Materials Science and Chemistry,
China University of Geosciences Wuhan, Wuhan, PR China
Xue Zhao
Institute for Ecological Research and Pollution Control of Plateau Lakes, School
of Ecology and Environmental Science, School of Chemical Science and
Technology, Yunnan University, Kunming, China
Yuan-Xin Zhu
School of Materials Science and Engineering, Anhui University of Science and
Technology, Huainan, Anhui, PR China
Preface

The distinct depletion of fossil fuels and ever-growing human dependence on the
energy-based usages has triggered a stern decline in ordinary energy reservoirs and
also worsened our environment. It is expected that the world will requisite to duple its
energy sources to endure the universal economy progression by 2050. Subsequently,
there is an imperative need than ever to discover the use of renewable, clean, and
bounteous energy sources. In this trend, an encouraging progress is the usage of
sustainable energy fonts to transform molecules (i.e., nitrogen, carbon dioxide, and
water) in the atmosphere into valued products (i.e., ammonia, hydrocarbons, and
hydrogen) through electrocatalysis technologies. Indeed, a number of innovative
energy conversion and storage systems, for instance, rechargeable metal-air batter-
ies, water electrolysis, and fuel cells have broadly been considered. Remarkably,
these techniques vastly reliant on the chain of electrochemical reactions, comprising
the oxygen reduction reaction (ORR), oxygen evolution reaction (OER), hydrogen
evolution reaction (HER), CO2 reduction reaction (CO2 RR), and nitrogen reduction
reaction (NRR), etc. Nonetheless, the efficacy of these reactions intensely depends on
the synthetic structure and properties of the catalysts used. The modern advancement
in nanomaterials has opened up the innovative avenue by building nanostructures for
proficient energy storage and conversion. This book credibly focuses on the enduring
and advances in the nanotechnology and development of nanomaterials for advanced
electrocatalysis.
Of particular attention, metal-based and metal-free nanomaterials have been
cost-efficiently designed into various electrocatalysts with efficient energy stor-
age/conversion capabilities. The consequent innovations in building the compe-
tent nanostructures unlocked a novel era in electrochemistry and material science.
Ever since then, transition-metal-, and carbon-based nanomaterials with distinctive
surface/size-reliant electrochemical possessions have been revealed to be beneficial
in electrocatalysis, and marvelous development has been accomplished in emerging
nanomaterials for proficient energy storage and conversion technologies. This is a
blistering field wherein a substantial extent of literature has been promptly engendered
with several publications ongoing to upturn annually. So, it is very significant to cover
the utmost latest advances in this field in a well-timed mode.
This book compacts with the fundamentals, synthesis methods, and wide range
applications of these metal-based and metal-free nanostructures. So as to cover the
multistructured meadow of such variety, transition-metal, noble-metal and carbon-
based nanomaterials for energy technologies deliver a pool of chapters transcribed
by top scholars who have been keenly employed in associated fields, and the script
has been distributed into different parts. This book is anticipated to cover all the
different types of transition-metal based (e.g., transition metal oxides, hydroxides,
and chalcogenides), noble-metal based, metal-free (e.g., carbon- and graphene-
based, heteroatom-doped carbon), and hybrid nanomaterials for electrocatalysis. The

xix
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