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Applications
of Nanomaterials
Advances and Key Technologies

Edited by

Sneha Mohan Bhagyaraj

Oluwatobi Samuel Oluwafemi
Nandakumar Kalarikkal
Sabu Thomas

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Contents

Contributors xv

1. Nanocomposites and Its Applications 1

Gunvant H. Sonawane, Sandip P. Patil and Shirish H. Sonawane
1.1 Introduction 1
1.1.1 Advanced Oxidation Processes 2
1.2 Nanocomposite Preparation 4
1.2.1 Precipitation 4
1.2.2 Intercalation 4
1.2.3 Ion Exchange Method 5
1.2.4 Hydrothermal Synthesis 6
1.2.5 Sol-Gel Method 7
1.2.6 Sonochemical Synthesis 8
1.3 Characterization of Nanocomposites 8
1.4 Degrading Pollutants With Nanocomposites 9
1.4.1 Clay Supported Nanocomposites 10
1.4.2 Graphene and Graphene Oxide Supported
Nanocomposites 11
1.4.3 Binary and Ternary Metal Oxides and Heterostructures 12
1.5 Mechanism of Degradation 14
1.6 Various Applications 16
1.7 Case Study 17
1.8 Conclusion and Future Prospects 18
References 18

2. Semiconductor/Graphene Nanocomposites: Synthesis,

Characterization, and Applications 23
Ramin Yousefi and Mohsen Cheraghizade
2.1 Introduction 23
2.2 Graphene and Graphene Oxide 24
2.2.1 Different Methods to Change GO to rGO 27
2.3 Different Semiconductor Family/Graphene Nanocomposites 29
2.3.1 Metal-Oxide/Graphene Nanocomposites 29
2.3.2 Metal-Chalcogenide/Graphene Nanocomposites 36
2.4 Summary and Future Outlook 39
Acknowledgment 40
References 40
Further Reading 43

v
vi Contents

3. Nanomaterials as Catalysts 45
U.P.M. Ashik, Anchu Viswan, Shinji Kudo and Jun-ichiro Hayashi
3.1 Introduction 45
3.2 Nanocatalysts 47
3.2.1 Metal Based Nanocatalysts 47
3.2.2 Nanocarbon Catalysts 52
3.2.3 Nanocarbon as Catalyst Support 55
3.2.4 Quantum Dots 57
3.3 Governance of Catalytic Performance 59
3.4 Catalytic Applications 60
3.4.1 Hydrogen Production From Methane 60
3.4.2 Ammonia Cracking 62
3.4.3 Dry Reforming of Methane to Produce syn-Gas 63
3.4.4 Fischer-Tropsch Synthesis 65
3.4.5 Fuel Cell Applications 66
3.4.6 Bio-Application 68
3.4.7 Photocatalytic Applications 71
3.4.8 Electrocatalytic Applications 72
References 74
Further Reading 82

4. The Electrochemical Conversion of Carbon Dioxide to

Carbon Monoxide Over Nanomaterial Based Cathodic
Systems: Measures to Take to Apply This Laboratory
Process Industrially 83
Ibram Ganesh
4.1 Introduction 83
4.1.1 The Current Status of CO2 Sequestration Technology
and Nature’s Response to Anthropogenic CO2 Increase
in the Atmosphere 83
4.1.2 The Present Capacity of Fossil Fuel Deposits
and Global Energy Inventories and Their Relevance to
Converting CO2 Into Useful Chemicals and Fuel 86
4.1.3 The Amount of Energy Drawn Today From Various
Sources of Renewable Energy 88
4.1.4 The Energy Density of Various Fuels Used in
Transportation and Other Sectors 89
4.2 The Capacity of Today’s Industrial CO2 Conversion
Plants Relative to the Social Cost of Carbon 90
4.3 General Methods of Converting CO2 Into Useful
Value-Added Chemicals 97
4.4 The Cost Economics Involved in the Electrochemical
CO2 Reduction to CO 98
 Contents vii

4.5 State-of-the-Art Developments in the Electrochemical

Reduction of CO2 (ERC) to CO 99
4.6 The Effects of CO2 Pressure on ERC Process Efficiency 103
4.7 Requirements and Effects of Separators for Anodic and
Cathodic-Compartments 104
4.8 The Energy and Kinetics Involved in the ERC to CO 104
4.9 The Necessity of RTIL Helper Catalysts for ERC to CO 109
4.10 The Stability of RTIL Helper Catalysts in ERC to
CO Process 114
4.11 Methods to Reduce the Cost of the RTILs Employed as
Helper Catalysts in ERC to CO 116
4.12 The Desired Features, Cost, and Stability of Electrodes
and Electrolyte for ERC to CO 117
4.13 Electrolyzer Designs for ERC to CO 118
4.14 Concluding Remarks and Future Perspectives 118
Acknowledgments 124
References 125
Further Reading 131

5. Green Nanotechnology—A Road Map to Safer

Nanomaterials 133
Renu Geetha Bai, Rana Sabouni and Ghaleb Husseini
5.1 Introduction 133
5.1.1 Nanotechnology 133
5.1.2 Nanotoxicity 134
5.1.3 Green Chemistry 135
5.1.4 Green Chemistry—History & Principles 135
5.1.5 Green Chemistry—Scope & Applications 138
5.2 Green Nanotechnology 138
5.2.1 Designing Green Nanomaterials 140
5.3 Green Nanomaterial Preparations 140
5.4 Green Nanomaterial Synthesis Utilizing Biomolecules 141
5.5 Biosynthesis Approaches for Green Nanomaterials 142
5.6 Applications of Green Nanomaterials 142
5.7 Biomedical Applications of Green Nanomaterials 145
5.7.1 Diagnosis Applications of Green
Nanomaterials 146
5.7.2 Therapeutic Applications of Green
Nanomaterials 146
5.8 Limitations of Green Nanotechnology 147
5.9 Future Perspectives 150
5.10 Conclusion 151
Acknowledgment 151
References 151
viii Contents

6. Nanobiosensors Based on Graphene Electrodes:

Recent Trends and Future Applications 161
Georgia-Paraskevi Nikoleli, Dimitrios P. Nikolelis,
Christina Siontorou, Stephanos Karapetis,
Spyridoula Bratakou and Nikolaos Tzamtzis
6.1 Introduction 161
6.2 Scope of This Chapter 162
6.3 Graphene and Biosensors 162
6.4 Graphene-Based Enzymatic Electrodes 164
6.4.1 Graphene-Based Electrochemical Enzymatic
Biosensors for Glucose Detection 164
6.4.2 Graphene-Based Electrochemical Enzymatic
Biosensors for Hydrogen Peroxide Detection 165
6.4.3 Graphene-Based Electrochemical Enzymatic
Biosensors for NADH Detection 166
6.4.4 Graphene-Based Electrochemical Enzymatic
Biosensors for Cholesterol Detection 166
6.4.5 Graphene-Based Electrochemical Enzymatic
Biosensors for Urea Detection 167
6.5 Graphene-Based Electrochemical DNA Sensors 168
6.6 Graphene-Based Electrochemical Immunosensors 169
6.6.1 Graphene-Based Electrochemical Immunosensors
for Biomarker Detection 170
6.6.2 Graphene-Based Electrochemical Immunosensors
for Pathogen Detection 171
6.7 Commercial Activities in the Field of Graphene Sensors 172
6.8 Recent Developments in the Field of Graphene Sensors 172
6.9 Conclusions and Future Prospects 173
References 174

7. Applications of Nanofibers in Tissue Engineering 179

Vinay Kumar, Saba Naqvi and P. Gopinath
7.1 Introduction 179
7.2 Historical Perspective 180
7.3 Current State 180
7.4 Tissue Engineering Triad 181
7.5 Scaffold or 3D Biomaterial Requirements 182
7.5.1 Biocompatibility 182
7.5.2 Biodegradability 182
7.5.3 Mechanical Properties 182
7.5.4 Scaffold Architecture 183
7.6 Biomaterials 183
7.7 Fabrication of 3D Scaffolds for Tissue Engineering 184
7.8 Nanofibers 185
7.8.1 Methods for Nanofibers Synthesis 185
 Contents ix

7.8.2 Electrospinning: A Technique for Synthesizing

Nanofibers 185
7.8.3 Parameters Affecting the Electrospinning Process 186
7.9 Polymeric Materials for Nanofiber Synthesis Using
Electrospinning Process 186
7.9.1 Natural Polymeric Materials for Nanofibers 186
7.9.2 Synthetic Polymeric Materials for Nanofibers 188
7.10 Applications: Electrospun Nanofibers in Tissue Engineering 188
7.10.1 Nanofibers for Bone Tissue Engineering 188
7.10.2 Nanofibers for Cartilage Tissue Engineering 189
7.10.3 Nanofibers for Ligament Tissue Engineering 190
7.10.4 Nanofibers for Skeletal Muscle Tissue Engineering 191
7.10.5 Nanofibers for Skin Tissue Engineering 193
7.10.6 Nanofibers for Vascular Tissue Engineering 194
7.10.7 Nanofibers for Neural Tissue Engineering 195
7.10.8 Nanofibers for Controlled Drug Delivery 197
7.10.9 Nanofibers for DNA, Protein and Enzyme Delivery 198
7.11 Conclusion 198
Acknowledgments 200
References 200

8. Nano-Enabled Immunosensors for Point-of-Care

Cancer Diagnosis 205
Dhesingh Ravi Shankaran
8.1 Introduction 205
8.2 Cancer 206
8.2.1 Cancer Biomarkers 206
8.3 Detection of Cancer 207
8.3.1 Currents Methods of Cancer Diagnosis 207
8.4 Immunosensors 208
8.4.1 Immunosensor Detection Principles 210
8.5 Functionalization (Preparation) of the Immunosensor
Surface 211
8.5.1 Self-Assembled Monolayers 213
8.6 Nanomaterials in Clinical Diagnosis 213
8.7 Optical Immunosensors 215
8.7.1 Surface Plasmon Resonance 215
8.7.2 Localized Surface Plasmon Resonance 224
8.7.3 Surface Enhanced Raman Spectroscopy 224
8.7.4 Fluorescence Spectroscopy 225
8.7.5 Colorimetric Sensing 226
8.8 Electrochemical Immunosensor 227
8.8.1 Voltammetric/Amperometric 227
8.8.2 Field-Effect Transistor-Based 234
8.8.3 Impedimetric 235
x Contents

8.9 Point-of-Care Immunodiagnostics 236

8.9.1 Microfluidic Immunoassays and Arrays 240
8.9.2 Paper-Based Microfluidic Sensors 241
8.9.3 Hand-Held Devices and Smartphone POC Diagnostics 242
8.10 Summary and Future Perspective 243
Acknowledgment 245
References 245
Further Reading 250

9. The Role of Nanomaterials in Analytical Chemistry:

Trace Metal Analysis 251
Inmaculada de la Calle and Vanesa Romero-Rivas
9.1 Introduction 253
9.2 Types of Nanomaterials 255
9.2.1 Carbon-Based Nanomaterials 258
9.2.2 Metallic Nanomaterials 261
9.3 Applications of Nanomaterials in Analytical Chemistry
(Trace Metal Analysis) 266
9.3.1 Sample Preparation 266
9.3.2 Chromatographic and Electrophoretic Separation 286
9.3.3 Detection Systems 287
9.4 Concluding Remarks 292
Acknowledgments 293
References 293

10. Comparative Study on Doxorubicin Loaded

Metallic Nanoparticles in Drug Delivery Against
MCF-7 Cell Line 303
Alagu Thirumurugan, Vijayakumar Blessy and Muthu Karthikeyan
10.1 Introduction 303
10.2 Materials and Methods 304
10.2.1 Synthesis of Metallic Nanoparticles 304
10.2.2 Characterization of Metallic Nanoparticles 305
10.2.3 Drug Entrapment Efficiency 305
10.2.4 Cell Culture 305
10.2.5 Cell Treatment and Anticancer Activity by MTT Assay 305
10.3 Results and Discussion 306
10.4 Conclusion 311
References 311

11. Nanomaterial Toxicity: A Challenge to End Users 315

Saba Naqvi, Vinay Kumar and P. Gopinath
11.1 Introduction 315
11.2 Environmental Fate and Behavior of Nanomaterials Based on
Intrinsic Properties 318
11.2.1 Chemical and Photo-Chemical Transformations in the
Environment 319
 Contents xi

11.2.2 Physical Transformation of Nanomaterials 325

11.2.3 Biological Transformation 327
11.3 Metal Oxide Nanoparticles 328
11.3.1 Copper Oxides Nanomaterials 328
11.3.2 Zinc Oxide (ZnO) Nanoparticles 330
11.4 Carbon-Based Nanomaterials/Carbonaceous
Nanomaterials 330
11.4.1 Single- and Multi-Wall Carbon Nanotubes
(SWCNT and MWCNT) Toxicity 330
11.4.2 Fullerenes/nC60 Toxicity 332
11.5 Nanomaterials Risk Assessment: Strategies 333
11.6 Conclusion 335
Acknowledgments 336
References 336

12. Biomedical Applications of Magnetic Nanomaterials 345

Anupam Guleria, Kalpana Priyatharchini and Dinesh Kumar
12.1 Introduction 345
12.2 Magnetic Nanoparticles as MRI Contrast Agents 348
12.2.1 Introduction to MRI Contrast Agents 348
12.2.2 Magnetic Nanoparticle Based T1 MRI Contrast
Agents 350
12.2.3 Magnetic Nanoparticle Based T2 MRI Contrast
Agents 353
12.2.4 Magnetic Nanoparticle Based T1-T2 Dual-Mode
MRI Contrast Agents 357
12.3 Surface Coating and Functionalization of Magnetic
Nanoparticles 358
12.3.1 Monomeric Organic Stabilizers 359
12.3.2 Polymeric Stabilizers 360
12.3.3 Inorganic Coatings 362
12.3.4 Functionalization of Coated MNPs With Targeting
Ligands 364
12.4 Disease Therapy Using Magnetic Nanoparticle-Based
Theranostics 367
12.4.1 Targeted Drug Delivery 367
12.4.2 Magnetic Hyperthermia 370
12.4.3 Hyperthermia-Based Controlled Drug Delivery 371
12.4.4 Magnetic Nanoparticle Mediated Transfection
for Gene Therapy 372
12.5 Multimodal Bioimaging 375
12.5.1 MRI-Optical Imaging 376
12.5.2 MRI-PET/SPECT Imaging 377
12.5.3 MRI-CT Imaging 378
12.6 Conclusions and Future Prospective 380
Acknowledgments 381
References 381
xii Contents

13. Carbon Nanotube Tube Filled Polymer

Nanocomposites and Their Applications in Tissue
Engineering 391
Deepalekshmi Ponnamma, Neethu Ninan and Sabu Thomas
13.1 Introduction 391
13.1.1 Methods of Preparation 393
13.1.2 Properties of CNTs 394
13.1.3 Dispersion and Functionalization of CNTs 395
13.2 CNT/Polymer Composites 396
13.3 Characteristic Properties of the Composites 397
13.3.1 Mechanical Properties 397
13.3.2 Rheological Properties 398
13.3.3 Thermal Properties 400
13.3.4 Electrical Properties 401
13.4 Polymer/CNT Composites in Tissue Engineering 402
13.4.1 Cell Compatibility of CNT 403
13.4.2 CNT Scaffolds Prepared by Electrospinning 404
13.4.3 CNT Scaffolds Prepared by Lyophilization 407
13.4.4 CNT Scaffolds Prepared by Rapid Prototyping 408
13.4.5 CNT Scaffolds Prepared by Solvent Casting 409
13.5 Conclusions and Future Outlook 410
References 411

14. Cellulose Nanocrystals for Health Care Applications 415

Dhesingh Ravi Shankaran
14.1 Introduction 415
14.2 Structural Organization of Cellulose 416
14.3 Hierarchical Structure of Lignocellulosic Fibers and
Mechanical Potential 418
14.4 Cellulose Nanocrystals 419
14.5 Sources of Cellulose Nanocrystals 419
14.5.1 Wood 420
14.5.2 Plant 420
14.5.3 Tunicates 420
14.5.4 Algae 420
14.5.5 Bacterial 421
14.5.6 Lignocellulosic Sources 421
14.6 Preparation of Cellulose Nanocrystals 422
14.6.1 Isolation of Cellulose Particles 422
14.6.2 Acid Hydrolysis 428
14.6.3 Mechanical Processes 428
14.7 Surface Chemistry and Functionalization of Cellulose
Nanocrystals 430
14.7.1 Functionalization Via CNCs Synthesis 431
14.7.2 Functionalization Via Adsorption 432
14.7.3 Functionalization Via Chemical Modification 432
 Contents xiii

14.8 Properties of Cellulose Nanocrystals 432

14.8.1 Mechanical Properties 433
14.8.2 Thermal Properties 433
14.8.3 Liquid Crystallinity 434
14.8.4 Rheological Properties 435
14.8.5 Optical Properties 435
14.9 Application of Cellulose Nanocrystals 435
14.9.1 Drug Delivery Applications 436
14.9.2 Biosensors Application 438
14.9.3 Water Purification 446
14.9.4 Food Packaging Application 447
14.10 Conclusion and Future Prospects 452
References 454

Index 461
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Contributors

Numbers in Parentheses indicate the pages on which the authors’ contributions begin.
U.P.M. Ashik (45), Institute for Materials Chemistry and Engineering, Kyushu
University, Kasuga, Japan
Renu Geetha Bai (133), American University of Sharjah, University City, Sharjah,
United Arab Emirates
Vijayakumar Blessy (303), Department of Biotechnology, Kumaraguru College of
Technology, Coimbatore, Tamil Nadu, India
Spyridoula Bratakou (161), Laboratory of Inorganic & Analytical Chemistry, School
of Chemical Engineering, Dept 1, Chemical Sciences, National Technical University
of Athens, Athens, Greece
Mohsen Cheraghizade (23), Young Researchers and Elite Club, Ahvaz Branch, Islamic
Azad University, Ahvaz, Iran
Inmaculada de la Calle (251), University of Vigo, Vigo, Spain
Ibram Ganesh (83), Centre of Excellence for Artificial Photosynthesis, International
Advanced Research Centre for Powder Metallurgy and New Materials (ARCI),
Hyderabad, Telangana, India
P. Gopinath (179, 315), Department of Biotechnology; Nanobiotechnology Laboratory,
Centre for Nanotechnology, Indian Institute of Technology Roorkee, Roorkee, India
Anupam Guleria (345), Centre of Biomedical Research, SGPGIMS Campus, Lucknow,
India
Jun-ichiro Hayashi (45), Institute for Materials Chemistry and Engineering, Kyushu
University, Kasuga, Japan
Ghaleb Husseini (133), American University of Sharjah, University City, Sharjah,
United Arab Emirates
Stephanos Karapetis (161), Laboratory of Inorganic & Analytical Chemistry, School of
Chemical Engineering, Dept 1, Chemical Sciences, National Technical University of
Athens, Athens, Greece
Muthu Karthikeyan (303), Department of Biotechnology, Kumaraguru College of
Technology, Coimbatore, Tamil Nadu, India
Shinji Kudo (45), Institute for Materials Chemistry and Engineering, Kyushu
University, Kasuga, Japan
Vinay Kumar (179, 315), Department of Biotechnology, Indian Institute of Technology
Roorkee, Roorkee, India

xv
xvi Contributors

Dinesh Kumar (345), Centre of Biomedical Research, SGPGIMS Campus, Lucknow,

India
Saba Naqvi (179, 315), Nanobiotechnology Laboratory, Centre for Nanotechnology,
Indian Institute of Technology Roorkee, Roorkee, India
Georgia-Paraskevi Nikoleli (161), Laboratory of Inorganic & Analytical Chemistry,
School of Chemical Engineering, Dept 1, Chemical Sciences, National Technical
University of Athens, Athens, Greece
Dimitrios P. Nikolelis (161), Laboratory of Environmental Chemistry, Department of
Chemistry, University of Athens, Athens, Greece
Neethu Ninan (391), Mahatma Gandhi University, Kottayam, India
Sandip P. Patil (1), Nano-Chemistry Research Laboratory, G.T. Patil College,
Nandurbar, India
Deepalekshmi Ponnamma (391), Mahatma Gandhi University, Kottayam, India
Kalpana Priyatharchini (345), Centre of Biomedical Research, SGPGIMS Campus,
Lucknow, India
Vanesa Romero-Rivas (251), University of Vigo, Vigo, Spain
Rana Sabouni (133), American University of Sharjah, University City, Sharjah,
United Arab Emirates
Dhesingh Ravi Shankaran (205, 415), Nano-Bio Materials and Sensors Laboratory,
National Centre for Nanoscience and Nanotechnology, University of Madras,
Guindy Campus, Chennai, India
Christina Siontorou (161), Laboratory of Simulation of Industrial Processes,
Department of Industrial Management and Technology, School of Maritime and
Industry, University of Piraeus, Piraeus, Greece
Gunvant H. Sonawane (1), Department of Chemistry, Kisan Arts, Commerce and
Science College, Parola, India
Shirish H. Sonawane (1), National Institute of Technology, Warangal, India
Alagu Thirumurugan (303), Department of Biotechnology, Kumaraguru College of
Technology, Coimbatore, Tamil Nadu, India
Sabu Thomas (391), Mahatma Gandhi University, Kottayam, India
Nikolaos Tzamtzis (161), Laboratory of Inorganic & Analytical Chemistry, School of
Chemical Engineering, Dept 1, Chemical Sciences, National Technical University of
Athens, Athens, Greece
Anchu Viswan (45), Nanovision Technology/RIE, GSST, Shizuoka University,
Hamamatsu, Japan
Ramin Yousefi (23), Department of Physics, Masjed-Soleiman Branch, Islamic Azad
University (I.A.U), Masjed-Soleiman, Iran
Chapter 1

Nanocomposites and Its

Applications
Gunvant H. Sonawane*, Sandip P. Patil† and Shirish H. Sonawane‡
*
Department of Chemistry, Kisan Arts, Commerce and Science College, Parola, India, †Nano-
Chemistry Research Laboratory, G.T. Patil College, Nandurbar, India, ‡Chemical Engineering
Department, National Institute of Technology, Warangal, India

1.1 INTRODUCTION
Today, environmental pollution is a major area of concern due to its impact on
living organisms, both directly and indirectly. Various industries pollute
through the discharge of organic and inorganic materials into local water
streams. But rapid advances in the fields of science, engineering and technology
have yielded specific materials and methods to tackle this problem. Wastewater
treatment involves adsorption, destruction by photocatalysis and/or oxidation
processes, and enzymatic and microbial decomposition. Among the various
wastewater treatment methods, adsorption is considered more effective due
to its convenience, ease of operation, and simplicity of design. Activated carbon
is one of the adsorbent used efficiently. However it‘s high cost is a drawback.
Cost is the decisive parameter for the choice of adsorbent. According to Crini
[1], a sorbent can be considered low cost if it requires little processing, is abun-
dant in nature, or is an industrial by-product [2]. Sometimes these methods are
ineffective and partial oxidation of organic contaminants produces secondary
pollutants more toxic than parent compounds [3].
The adsorption method suffers from difficulties in the treatment of insoluble
dyestuff effluent as well as in finding the desorption process [4]. The main
drawbacks of these techniques are the disposal of the spent contaminated acti-
vated sludge and difficulties in controlling the appropriate reaction conditions
and amount of by-products [5,6].
Various developments in nanoscience/nanotechnology wherein nanoscale
materials are synthesized with the ability to change harmful pollutants into
less/non harmful ones have shown a major impact.
Being a green, highly efficient, and effective technology, heterogeneous
photocatalysis is regarded as a promising technology to address environmental

Applications of Nanomaterials. https://doi.org/10.1016/B978-0-08-101971-9.00001-6

Copyright © 2018 Elsevier Ltd. All rights reserved. 1
2 Applications of Nanomaterials

challenges in the near future [7,8]. It is an excellent method over the others due
to its use of oxygen as an oxidant and oxidation of organics at low temperature
and low concentrations with complete mineralization. Thus some of the semi-
conductor metal oxides like TiO2 and ZnO have a higher band gap for the exci-
tation of electrons from valence band to conduction band and require high
energy UV radiations. Therefore, many studies have been devoted either to
modify the energy band gap of these semiconductor metal oxides or to find
alternatives to them in order to utilize solar energy. These methods involve
(a) doping with other elements, (b) the fabrication of heterojunction structure
by combining a semiconductor with metals or other semiconductors, (c) the
use of clay or graphene/graphene oxide as a support to enhance solar light
sensitivity [9].
Clay or graphene/graphene-oxide supported nanocomposites are found
to exhibit versatile degradation properties as clay minerals possess good
adsorption-desorption properties. They change the photocatalysis from UV to
the visible region. They also are responsible for the separation of electron-hole
pairs to enhance the photocatalytic power of nanomaterials.

1.1.1 Advanced Oxidation Processes

Advanced oxidation processes (AOPs) are one of the most useful techniques for
the degradation of organic compounds in wastewater treatment. The mechanism
of AOPs relies on the formation of highly reactive oxidant species, mainly
hydroxyl radicals, which can react with harmful compounds until their degra-
dation [10]. However, the application of AOPs to degrade all pollutants from
wastewaters can be not sustainable. Their combination with heterogeneous
photocatalysis can be considered as an equally valid option. It has been exten-
sively proven that AOPs can improve the degradation efficiency of waste-
waters, thus enhancing the degradation of both organic and recalcitrant
compounds. Advanced oxidation processes that involve the in situ generation
l
of highly potent chemical oxidants such as the hydroxyl radical (OH ) have
recently emerged as an important class of technologies for accelerating the oxi-
dation and destruction of a wide range of organic contaminants in wastewater
[11]. AOPs, when applied in the right place, give a good opportunity to reduce
the contaminant concentration from several hundred ppm to less than five ppb.
That is why they are called “the treatment processes of the 21st century”. The
improving degradation ability of AOPs in recalcitrant compounds in wastewater
depends on both chemical and physical properties of contaminants as well as on
the generation of reactive free radicals, in most cases hydroxyl radicals [12].
The oxidation reaction between these radicals and the contaminants is the
mechanism behind the degradation of the contaminant itself. The generation
of these reactive agents can be achieved by means of several processes, includ-
ing sonolysis [13], ozone-based processes [14], Fenton-based reactions [15],
heterogeneous photocatalysis [16] and various combinations of these technol-
ogies [17,18]. Each one can be characterized according to its specific method
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ALAMEEN-BEN MOHAMMED EL KANEMY.

SHEIKH OF BORNOU.
Published by John Murray, London. Feb. 1826.
 N A R R AT I V E
OF

T R AV E L S A N D D I S C O V E R I E S
IN

NORTHERN AND CENTRAL AFRICA,

IN THE YEARS 1822, 1823, AND 1824,

BY MAJOR DENHAM, CAPTAIN CLAPPERTON, AND THE

LATE DOCTOR OUDNEY,
EXTENDING ACROSS THE
GREAT DESERT TO THE TENTH DEGREE OF NORTHERN LATITUDE, AND FROM
KOUKA IN BORNOU, TO SACKATOO, THE CAPITAL OF THE FELLATAH EMPIRE.
WITH

AN APPENDIX,
PUBLISHED BY AUTHORITY OF THE RIGHT HONOURABLE EARL BATHURST, ONE OF
HIS
MAJESTY’S PRINCIPAL SECRETARIES OF STATE, AND DEDICATED BY
PERMISSION TO HIS LORDSHIP,

B Y M A J O R D I X O N D E N H A M,
OF HIS MAJESTY’S 17TH REGIMENT OF FOOT,

AND

C A P TA I N H U G H C L A P P E RTON,
OF THE ROYAL NAVY,

THE SURVIVORS OF THE EXPEDITION.

LONDON:
JOHN MURRAY, ALBEMARLE-STREET.

MDCCCXXVI.
 LONDON:
PRINTED BY THOMAS DAVISON, WHITEFRIARS.
 TO

THE RIGHT HONOURABLE

THE EARL BATHURST, K.G.

HIS MAJESTY’S PRINCIPAL SECRETARY OF STATE FOR THE COLONIES,

THIS VOLUME,
CONTAINING

AN ACCOUNT OF THEIR DISCOVERIES

MADE UNDER THE AUSPICES OF HIS LORDSHIP,

IS INSCRIBED,

WITH THE GREATEST RESPECT AND GRATITUDE,

BY HIS OBLIGED AND FAITHFUL SERVANTS,

THE AUTHORS.
 P R E FA C E .

By the death of Dr. Oudney, it has fallen to the lot of Captain

Clapperton and myself to render an account to the public of our
expedition into the interior and central parts of Northern Africa. The
sudden departure of my surviving companion, on a second mission,
has necessarily thrown the greater part of the burden on myself. I
believe, however—for I have not seen any of his papers—that
Captain Clapperton, during the lifetime of Dr. Oudney, made but few
remarks himself beyond the construction of the chart of our route,
from daily observations of the latitude, and of lunars for the
longitude, whenever favourable opportunities occurred; but,
subsequently to the death of his travelling companion, which
happened at an early stage of their journey into Soudan, a journal of
his proceedings and remarks appears to have been regularly kept;
and this, together with other documents connected with that journey,
were left at his departure in the hands of Mr. Barrow, with a request
that he would see them through the press.
It may naturally enough be asked, Why something more than a
short excursion to the westward of Mourzuk, and a few notes, do not
appear from the pen of Dr. Oudney in the present volume? I can only
answer the question by the fact, that the only papers placed in my
hands consist of “An Itinerary from Mourzuk to Bornou;” and “An
Excursion to the Westward of Mourzuk;” neither of which have been
deemed fit for publication in extenso, from their imperfect state, and
containing very little beyond what will be found in my own journals. I
have, however, printed in foot notes such parts of them as have
been pointed out to me. Not a paper of his, to my knowledge, has
been lost or destroyed; and I can only account for the unsatisfactory
state in which they have been found, from the circumstance of his ill
health, which became extremely precarious from the moment of our
departure from Mourzuk, where he had caught a cold, which settled
on his lungs, and never left him. On our arrival at Kouka, and
frequently afterwards, he experienced so many attacks of fever, that
there appeared little hope of his surviving to return to England, which
was indeed his own opinion; and when he set out on his last journey
towards Soudan, he was so exhausted, and in a state so unfit for
such an undertaking, that he fell a martyr to his zeal very soon after
his departure, though, had he remained at Kouka, the melancholy
event would not, in all probability, have been prolonged many days.
My own expeditions in various parts of Bornou, in Mandara, and
Loggun, and the two fruitless attempts I made to complete the tour of
the great lake Tchad, will be found to occupy a considerable portion
of the volume; and being made in countries, and among a people
unknown to Europeans,—many of them even by name or report,—it
is hoped that observations, faithfully and circumstantially minuted
down at the time and spot, will not be found tedious or uninteresting
to the reader.
It will, perhaps, be thought by some, that I have been more minute
than necessary in the account of our journey across that tremendous
desert which lies between Mourzuk and Bornou, and which,
generally speaking, is made up of dark frowning hills of naked rock,
or interminable plains, strewed in some places with fragments of
stone and pebbles, in others of one vast level surface of sand, and,
in others again, the same material rising into immense mounds,
altering their form and position according to the strength and
direction of the winds. But, even in the midst of this dreary waste,
towns, villages, wandering tribes, and kafilas, or caravans,
sometimes occur to break the solitude of this dismal belt, which
seems to stretch across Northern Africa, and, on many parts of
which, not a living creature, even an insect, enlivens the scene. Still,
however, the halting places at the wells, and the wadeys or valleys,
afford an endless source of amusement to the traveller, in witnessing
the manners, and listening to the conversation, of the various tribes
of natives, who, by their singing and dancing, their story telling, their
quarrelling and fighting, make him forget, for a time, the ennui and
fatigue of the day’s journey.
 As for the rest, I have to trust to its novelty, for its
recommendation to the public, rather than to any powers of writing,
which I pretend not to possess; and it is now a source of great
satisfaction to me that, under all my difficulties, and they were not
few, I was able to adhere to the resolution I set out with, of recording,
at the end of each day, the occurrences, however trifling, that had
taken place.
To Sir Robert Ker Porter, my friend since the days of boyhood, I
am indebted for having perfected several drawings, with his
experienced pencil, from my hasty, but yet faithful sketches, of the
people and scenery of Central Africa. His eye was nearly as familiar
as my own with the picturesque objects they display; and, indeed, all
who are acquainted with the published narrative of his Researches
amongst the Remains of Ancient Persia and Babylonia, might readily
recognise the same hand, in these his spirited delineations of African
costume and character.
DIXON DENHAM.
Albany, London,
Jan. 1st. 1826.
 Map of the Travels and
Discoveries made in Northern
& Central Africa, by Dr.
Oudney, Major Denham, &
Captn. Clapperton, R.N. in the
Years 1822, 3, & 4.

J. & C. Walker Sculpt.

(Large-size)

Published as the Act directs Feby. 1826,

by John Murray Albemarle Street London.
 CONTENTS.

Page
Introductory Chapter.—From Tripoli to Mourzuk xi
Excursion to the Westward of Mourzuk xliii

MAJOR DENHAM’S NARRATIVE.

Chap. I.—From Mourzuk to Kouka in Bornou 1
Chap. II.—Kouka 67
Chap. III.—Expedition to Mandara 99
Chap. IV.—Excursion to Munga and the Gambarou 149
Chap. V.—Rainy Season at Kouka 181
Chap. VI.—Excursion to Loggun, and Death of Mr. Toole 226
Chap. VII.—Journey to the Eastern Shores of the Lake Tchad 248
Supplemental Chapter on Bornou 314

CAPTAIN CLAPPERTON’S NARRATIVE.

Prefatory notice to the Narrative, by John Barrow
Sect. I.—From Kouka to Murmur, where Dr. Oudney died 1
Sect. II.—From Murmur to Kano 34
Sect. III.—From Kano to Sackatoo, and Residence there 67

APPENDIX.
No. I.—Translation of a Letter from the Sheikh Mohammed El Kanemy 139
No. II.—Translation of a Letter from an African Chieftain 140
No. III.—A Letter from Yousuf, Pasha of Tripoli, to the Sheikh of Bornou 141
No. IV.—A Letter from the Pasha of Tripoli 143
No. V.—A Letter from the Sheikh of Bornou to the Sultan of Kanou 144
No. VI.—A Letter from the Sheikh of Bornou to the Sultan of Hoossa 145
No. VII.—A Letter from the Chieftain Mohammed Gamsoo 146
No. VIII.—A Document relating to the Death of Mungo Park 147
No. IX.—A Letter from the Sheikh of Bornou to Captain Clapperton 148
No. X.—A Document made at the Court of Justice of Bornou 149
No. XI.—Translation of Letters and Documents received from the Sheikh
of Bornou concerning Mr. Tyrwhit’s Death 151
No. XII.—Translation of an Arabic MS. 158
No. XIII.—A Narrative of the first Battle of Kadawee 167
No. XIV.—The Song of Mohammed-Alameen ben Mohammed El Kanemy 171
No. XV.—Translation of an extempore Arab Song 173
No. XVI.—Translation of the Song of the Fezzanneers, on Boo
Khaloom’s Death 174
No. XVII.—Bornou Vocabulary 175
No. XVIII.—Begharmi Vocabulary 179
No. XIX.—Mandara Vocabulary 180
No. XX.—Timbuctoo Vocabulary 181
No. XXI.—Zoology 183
No. XXII.—Botany 208
No. XXIII.—Letter to Major Denham on the Rock Specimens 247
No. XXIV.—Thermometrical Journals 262
 L I S T O F P L AT E S .

No. Page
1. Alameen ben Mohammed El Kanemy, Sheikh of
Bornou, Frontispiece

2. Part of the Stony Desert, to face page xvi

3. Castle at Mourzuk, from Mr. Ritchie’s Grave xxi
4. Woman of Sockna xxvii
5. Vignette, Arabs Meeting xlii
6. View of the Bahr Mandia lviii
7. Castle, and Salt Lake at Tegerhy 5
8. Anay Tibboo Country 17
9. Kanemboo Marketwoman,—Unmarried Woman of Soudan 46
10. Body Guard of the Sheikh of Bornou 64
11. Reception of the Mission by the Sultan of Bornou 79
12. Shouaa Women, kingdom of Bornou 94
13. Arrival at Mora, the capital of Mandara 111
14. Mandara Musicians 123
15. Plan of the Pass of Hairy, Mandara mountains 127
16. Attack on Musfeia 133
17. Vignette, Manner of Roasting Fish 148
18. The River Gambarou, or Yeou, near Lada 152
19. Favourite of the Seraglio, accompanying a Military Expedition 163
20. Kanemboo Spearman,—Munga Bowman, in the service of the Sheikh
of Bornou 166
21. Abdel Gassam, a Felatah from Timbuctoo—A Bornouese on a
Journey 177
22. Vignette, Kanemboo Night Watch 180
23. Hut, and Carpenter’s Shop 201
24. Vignette, Plan of Kouka 225
25. Fishing Boats on the River Shary 229
26. River Shary, from the Walls of Kussery 235
27. Vignette, Negresses Pounding Corn 247
28. A Loggun Lady—Funha of Maffatai—Abdelahi of Mandara 259
29. Hager Teous, or the Footstool of Noah 261
30. Sketch of the Lake Tchad 266
31. Lancers of the Sultan of Begharmi 279
32. Manner of Fishing on the River Yeou 284
33. Encampment near Woodie 289
34. Ghirza, south face of Building 305
35. Frieze on do. ib.
36. Town of Sangeia, in Houssa 36
37. Natives of Soudan 54
38. Vignette, Plan of the Town of Kano 56
39. A Reduction of Bello’s Map of Central Africa 109
40. Appendix—Fennecus Cerdo 183
41.
Arms and Armour of Central Africa, brought home by Major Denham,
42.
—Three Plates.
43.
44. General Map of the Routes of the Travellers.
 INTRODUCTORY CHAPTER.

BY MAJOR DENHAM.

FROM TRIPOLI TO MOURZUK.

Previous to any knowledge I had received of the intentions of

His Majesty’s government to follow up the mission of Mr. Ritchie and
Captain Lyon, I had volunteered my services to Lord Bathurst to
proceed to Timbuctoo, by nearly the same route which Major Laing is
now pursuing. I learnt, in reply, that an expedition had been planned,
and that Doctor Oudney and Lieutenant Clapperton, both of the
navy, were appointed; and with these gentlemen, by the kindness of
Lord Bathurst, I was, at my request, associated. My companions left
London before me; but, as soon as ready, I lost no time in
proceeding in the packet to Malta, where I found that they had left
the island for Tripoli nearly a month before. By the kindness of
Admiral Sir Graham Moore, Sir Manley Power, Sir Richard Plasket,
and Captain Woolley, commissioner of the dock-yard, all my wants
were amply supplied; and judging that the assistance of a shipwright
or carpenter might prove of essential use, and being allowed by my
instructions to engage any one, at a reasonable salary, who might
choose to volunteer to accompany the mission, William Hillman,
shipwright, a man of excellent character, immediately offered his
services, on an agreement that he should receive 120l. a year so
long as he should continue to be employed.
I embarked in the Express schooner, which the admiral lent me for
the purpose, and, on the 18th November, after three days’ sail,
arrived at Tripoli, and found my two companions at the house of Mr.
Consul Warrington, anxiously expecting my arrival. Of this gentleman
it is not too much to say, that by his cheerful and good humoured
disposition, his zeal, perseverance, and extraordinary good
management, we owe, in a great degree, that influence which
England possesses with this government far beyond that of any
other of the Barbary powers. The English name, in fact, is of such
importance in Tripoli, that there is scarcely a point to carry, or a
dispute to settle, in which the bashaw does not request the
interference of the British consul: and to him, indeed, is, in a great
degree, owing the origin and success of the late mission. He stated
broadly to the government at home, that the road from Tripoli to
Bornou was as open as that from London to Edinburgh; which, with a
small allowance for Oriental hyperbole, was found to be true—
witness the journey of my lamented friend Lieutenant Toole, and also
of Mr. Tyrwhitt, the latter laden with valuable presents.
But this is not all: the British flag has a peculiar power of
protection, and the roof of the English consul always affords a
sanctuary to the perpetrator of any crime, not even excepting
murder; and scarcely a day passes that some persecuted Jew or
unhappy slave, to escape the bastinado, does not rush into the
court-yard of the British consulate for protection. A circumstance
occurred in returning from one of our excursions, which shows in
what high estimation the English character is held in Tripoli. A poor
wretch, who, for some trifling offence, was sentenced to five hundred
bastinadoes, having, while on his way to receive the sentence of the
law, contrived to slip from the custody of his guards, fortunately met
with the child and servant of Doctor Dickson, a most respectable and
intelligent English physician practising in Tripoli: the condemned
wretch, with wonderful presence of mind, snatched up the child in his
arms, and halted boldly before his pursuers. The talisman was
sufficiently powerful: the emblem of innocence befriended the guilty,
and the culprit walked on uninterrupted, triumphantly claiming the
protection of the British flag.
But the following proves still more strongly to what extent the
influence of the British flag might be carried.—Since the reduction of
the refractory Arabs to submission, no chief had received such
repeated marks of kindness and attention from the bashaw, as
sheikh Belgassam ben Khalifa, head of the powerful tribe of El Gibel.
At the particular request of the former, sheikh Khalifa had quitted his
tents and flocks, resided in the city, and was high in his prince’s
confidence—fatal pre-eminence in Barbary states!—and had been
presented, but a few months before, with one of the most beautiful
gardens in the Minshea. Returning from the castle after an evening
of music and dancing in the bashaw’s private apartments,
Belgassam kissed the hand that had signed his death-warrant, and
took his leave. At his own door a pistol-shot wounded him in the arm,
and on entering the skiffa, or passage, a second entered his body.
The old sheikh, after his slave had fastened the door, staggered to
his carpet, and then, in the arms of his wife, proclaimed his assassin
to be his own nephew, sheikh Mahmoud Belgassam Wildé
Sowdoweah. The work being, however, but half done, others rushed
in, and seven stabs put an end to his sufferings, notwithstanding the
screams of his wife, who received two wounds herself, in
endeavouring to save her husband. The poor old man was almost
instantly buried, and the three persons who had undertaken the
murder fled to the British consulate for protection. Early the next
morning, however, the consul despatched his dragoman to give the
bashaw notice, “that the murderers of Khalifa would find no
protection under the flag of England.” The bashaw said, “he was
shocked at the murder, and regretted the assassins having taken
refuge in the consulate, as it was a sanctuary he could not violate,
particularly as he understood they meant to resist, and were well
armed.” Our consul replied, “that the bashaw was at liberty to send
any force he pleased, and use any means he thought best, to drag
them from beneath a banner that never was disgraced by giving
protection to assassins.” The minister also came and expressed the
bashaw’s delicacy; and it was evident he did not expect such would
be the conduct of the consul: he was, however, peremptory, and the
bashaw dared not seem to favour such an act of villany. It was
sunset before he decided on taking them away, when about sixteen
of the chosen people of the castle entered the consulate, and the
wretches, although provided with arms, which they had loaded,
tremblingly resigned themselves, and were, in less than an hour,
hanging over the walls of the castle.
On a day appointed we waited on the bashaw. After passing the
court-yard, crowded with guards, and several groups of Arabs in the
passages and ante-rooms playing at cards or dice, we were
introduced to the audience chamber, where the bashaw, sitting
cross-legged on a carpet, supported by his two sons, and attended
by armed negroes, received us kindly, ordered us to be served with
sherbet and coffee, and expressed himself in the most favourable
manner on the subject of our mission, which he promised to forward
in safety into the interior of Africa. He invited us to join him in a
hawking party. The cavalcade, consisting of about three hundred,
altogether presented so novel an appearance, that I shall endeavour
to give some description of our morning’s amusement. The bashaw
was mounted on a milk-white Arabian, superbly caparisoned, with
saddle of crimson velvet richly studded with gold nails, heavy stirrups
of the same, and trappings of embroidered cloth hanging down on
each side nearly to the horse’s fetlock joint; he was preceded by six
chaoushes, or officers, also mounted and richly caparisoned, armed
with long guns, swords, and pistols, and a white silk barracan thrown
loosely and gracefully round their bodies. His highness was
supported on each side by a favourite black slave, whose glittering
vest, light bornouse, and white turban, formed a pleasing contrast to
the costume of the Arabs. We proceeded in a westerly direction; and
on arriving at the desert, parties of six and eight dashed forward,
with the rapidity of lightning, several hundred paces, fired,
immediately halted in a most surprising manner, and with loud cries
rushed back again to the main body, when instantly the same
ceremony was repeated by another party. Their superior skill in the
management of their horses is really beautiful; and the way they
manœuvre their long musket, by repeatedly spinning it over their
heads at full speed, has a most picturesque effect. Near the
bashaw’s person rode Sidy Ali, his third son, although second in
succession, in consequence of the banishment of the eldest; he also
was attended by his particular guard of Arabs, distinguished not only
by their superior and determined appearance, but by their figured
muslin bornouses. Sidy Ali is the bashaw’s favourite son, and is
particularly handsome, although what we should call too fat, and is
said to resemble very much what the bashaw was at his age: he is
allowed great privilege and liberty, which is indeed proved by his
saying, the other day, to his father, “I shall succeed you as bashaw.”