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 Hierarchical Micro/
Nanostructured Materials
Fabrication, Properties, and Applications

Edited by
Weiping Cai • Guotao Duan • Yue Li
 Hierarchical Micro/
Nanostructured Materials
Fabrication, Properties, and Applications
 Advances in Materials Science and Engineering

Series Editor
Sam Zhang

Aerospace Materials Handbook, edited by Sam Zhang and Dongliang Zhao

Biological and Biomedical Coatings Handbook: Applications, edited by Sam Zhang
Biological and Biomedical Coatings Handbook: Processing and Characterization,
edited by Sam Zhang
Hierarchical Micro/Nanostructured Materials: Fabrication, Properties, and
Applications, Weiping Cai, Guotao Duan, Yue Li
Hydroxyapatite Coatings for Biomedical Applications, edited by Sam Zhang
Nanobiomaterials: Development and Applications, edited by Dong Kee Yi and
Georgia C. Papaefthymiou
Nanostructured and Advanced Materials for Fuel Cells, edited by San Ping Jiang
and Pei Kang Shen
Micro- and Macromechanical Properties of Materials, Yichun Zhou, Li Yang,
and Yongli Huang
 Hierarchical Micro/
Nanostructured Materials

Fabrication, Properties, and Applications

Edited by
Weiping Cai • Guotao Duan • Yue Li
CRC Press
Taylor & Francis Group
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© 2014 by Taylor & Francis Group, LLC

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Contents
Series Statement........................................................................................................ xv
Preface....................................................................................................................xvii
Acknowledgments....................................................................................................xix
Authors.....................................................................................................................xxi

Chapter 1 General Introduction.............................................................................1

1.1 Hierarchical Micro/Nanostructured Powders............................ 1
1.2 Hierarchical Micro/Nanostructured Arrays............................... 2
References............................................................................................. 4

Section I Hierarchical Micro/Nanostructured

Powders

Chapter 2 Solvothermal Routes.............................................................................9

2.1 Introduction................................................................................ 9
2.2 Novel Micro/Nanostructured ZnO............................................. 9
2.2.1 Micro/Nanostructured Porous ZnO Plates.................... 9
2.2.1.1 Morphology and Structure........................... 10
2.2.1.2 Influence of Veg/Vdiw on Products................ 11
2.2.1.3 Formation of Nanoplates............................. 12
2.2.2 Standing Porous Nanoplate-Built Hollow Spheres..... 14
2.2.2.1 Morphology and Structure........................... 15
2.2.2.2 Morphological Evolution............................. 16
2.2.2.3 Influence of Trisodium Citrate
Dihydrate on Morphology........................... 18
2.2.2.4 Formation of Porous
Nanoplate-Built Honeycomb-Like ZnO
Hollow Spheres............................................ 18
2.2.3 Nanoplate-Built Core/Shell-Structured ZnO Objects.21
2.2.3.1 Morphology and Structure........................... 22
2.2.3.2 Morphology Evolution with Reaction
Time............................................................23
2.2.3.3 Influence Factors..........................................26
2.2.3.4 Two-Step Sequential Growth Model........... 27
2.3 Micro/Nanostructured Porous Fe3O4 Nanofibers..................... 30
2.3.1 Morphology and Structure.......................................... 30

v
vi Contents

2.3.2 Influencing Factors...................................................... 32

2.3.2.1 pH Value...................................................... 32
2.3.2.2 Reaction Temperature.................................. 32
2.3.2.3 Content of PR in the Precursor Solution...... 33
2.3.2.4 Effect of C6 H 5O37−........................................ 35
2.3.3 Formation of Porous Oriented Magnetite Fibers........ 35
2.3.3.1 Formation of Ultrafine Fe3O4
Nanoparticles............................................... 35
2.3.3.2 PR-Directed/Magnetic Dipole–Induced
Orientation Assembling............................... 35
2.3.3.3 Existence and Removal of PR in
the Fibers..................................................... 36
2.3.4 Effects of Reaction Parameters................................... 38
2.4 Tremella-Like Micro/Nanostructured Fe3S4/C Composites..... 39
2.4.1 Structure and Morphology..........................................40
2.4.2 Influence of Glucose.................................................... 42
2.4.3 Formation of Tremella-Like Fe3S4/C Composites.......44
2.5 Brief Summary.........................................................................46
References...........................................................................................46

Chapter 3 Template-Etching Strategies............................................................... 53

3.1 Introduction.............................................................................. 53
3.2 Micro/Nanostructured Porous Silicate Hollow Spheres........... 53
3.2.1 Copper Silicate Micro/Nanostructured Hollow
Spheres........................................................................ 54
3.2.1.1 Structure and Morphology........................... 55
3.2.1.2 Formation Mechanism................................. 55
3.2.2 Magnesium Silicate Micro/Nanostructured
Hollow Spheres........................................................... 58
3.2.2.1 Structure and Morphology........................... 58
3.2.2.2 Formation of Magnesium Silicate
Hollow Spheres............................................ 59
3.2.3 Nickel Silicate and Silica–Nickel Composite
Hollow Spheres........................................................... 61
3.2.3.1 Nickel Silicate Hollow Spheres................... 62
3.2.3.2 Silica Hollow Spheres.................................. 63
3.2.3.3 Silica–Nickel Composite Hollow Spheres... 65
3.3 Hierarchical SiO2@γ-AlOOH Microspheres............................ 67
3.3.1 Morphology and Structure.......................................... 67
3.3.2 Formation of Hierarchical SiO2@γ-AlOOH
Microspheres............................................................... 69
3.3.2.1 Morphological Evolution with Reaction...... 69
3.3.2.2 Template-Induced Deposition
Mechanism................................................... 70
3.3.2.3 Effect of Urea............................................... 71
Contents vii

3.4 Structure and Component Controllable Hollow

Nanospheres: The Case of ZnO and Noble Metal
Cluster–Embedded ZnO........................................................... 71
3.4.1 Selective Etching Strategy for Hollow Nanospheres.. 72
3.4.2 Etching by Tartaric Acid............................................. 73
3.4.3 Etching by Weak Acids with Noble Metal Ions.......... 78
3.4.4 Formation of ZnO Hollow Nanospheres.....................80
3.4.5 Noble Metal Doping in ZnO Nanoshells..................... 82
3.4.6 Some Remarks on the Strategy................................... 82
3.5 Brief Summary......................................................................... 83
References........................................................................................... 83

Chapter 4 Electrospinning and In Situ Conversion.............................................. 89

4.1 Introduction.............................................................................. 89
4.2 Polyacrylonitrile/Ferrous Chloride Composite Porous
Nanofibers.................................................................................90
4.2.1 Morphology and Structure.......................................... 91
4.2.2 Existence of FeCl2 within Fibers................................. 93
4.2.3 Extension of the Electrospinning Strategy:
In Situ Conversion.......................................................94
4.2.3.1 Polyacrylonitrile/FeOOH Composite
Nanofibers....................................................94
4.2.3.2 Polyacrylonitrile/Mg(OH)2 Composite
Nanofibers.................................................... 95
4.3 Hierarchically Micro/Nanostructured PAN@γ-AlOOH Fibers... 97
4.3.1 Electrospun Nanofiber–Templated Hydrothermal
Route........................................................................... 98
4.3.2 Morphology and Structure..........................................99
4.3.3 Influence Factors....................................................... 100
4.3.3.1 Annealing Treatment................................. 100
4.3.3.2 Effect of Reaction Duration....................... 101
4.3.3.3 Effect of Hexamethylenetetramine
Addition..................................................... 102
4.3.3.4 Effect of Reaction Temperature................. 102
4.3.4 Formation of Micro/Nanostructured
PAN@γ-AlOOH Fibers............................................. 103
4.4 Electrospun Nanofiber-Based Ag Porous Nanotube Films.... 104
4.4.1 Ag-Coated Nanofiber Template–Plasma Etching
Strategy..................................................................... 105
4.4.2 Morphology and Structure of Ag Porous
Nanotube Films......................................................... 106
4.4.3 Structural Tunability of Ag Porous Nanotube Films.... 107
4.4.4 Formation of Nanopores on Tube Walls................... 109
4.5 Brief Summary....................................................................... 109
References......................................................................................... 110
viii Contents

Chapter 5 Structurally Enhanced Photocatalysis Properties............................. 115

5.1 Introduction............................................................................ 115
5.2 ZnO-Based Micro/Nanoarchitectures.................................... 115
5.2.1 Nanoplate-Built Core–Shell-Structured ZnO
Objects....................................................................... 116
5.2.1.1 Structural Dependence of
Photocatalytic Activity.............................. 116
5.2.1.2 Durability of Photocatalytic Activity........ 118
5.2.1.3 Structure-Induced Enhancement of
Photocatalytic Activity and Durability...... 118
5.2.2 Noble Metal Cluster–Embedded ZnO Composite
Hollow Spheres......................................................... 119
5.2.2.1 Photocatalytic Activity.............................. 120
5.2.2.2 Photostability............................................. 120
5.2.2.3 Pt/ZnO Porous Shells................................ 121
5.2.3 Ag Nanoparticle–Decorated Nanoporous ZnO
Microrods.................................................................. 123
5.2.3.1 Photocatalytic Activity.............................. 125
5.2.3.2 Photostability............................................. 126
5.2.3.3 Interface-Induced Enhancement of
Photocatalytic Activity.............................. 127
5.3 Micro/Nanostructured α-Fe2O3 Porous Spheres.................... 129
5.3.1 Photocatalytic Activity.............................................. 129
5.3.2 Photostability............................................................. 131
5.3.3 Structurally Induced Photocatalytic Enhancement... 131
5.4 Micro/Nanostructured Bi0.5Na0.5TiO3..................................... 132
5.4.1 Morphology and Structure........................................ 132
5.4.2 Photocatalytic Activity.............................................. 133
5.5 Brief Summary....................................................................... 135
References......................................................................................... 135

Chapter 6 Structurally Enhanced Adsorption Performances for Environment..... 141

6.1 Introduction............................................................................ 141
6.2 Micro/Nanostructured ZnO as Adsorbents............................ 142
6.2.1 Adsorption of Cu(II) on Porous ZnO Nanoplates..... 142
6.2.1.1 Adsorption Measurements of Cu(II)......... 142
6.2.1.2 Structurally Enhanced Adsorption............ 143
6.2.1.3 Extension to Anion Adsorption................. 146
6.2.2 Standing Porous Nanoplate–Built ZnO Hollow
Microspheres............................................................. 147
6.2.2.1 Adsorptive Performance of Heavy
Metal Ions.................................................. 147
6.2.2.2 Structurally Enhanced Adsorption and
Its Electronegativity Dependence.............. 150
6.2.3 Brief Remarks........................................................... 153
Contents ix

6.3 Composite Porous Nanofibers for Removal of Cr(VI)........... 154

6.3.1 Cr-Removal Performance.......................................... 154
6.3.1.1 High Cr-Removal Capacity........................ 155
6.3.1.2 Influences of the pH Value and Fe(II)
Content....................................................... 156
6.3.2 PAN···Fe(II) Complexes–Induced Cr Adsorption..... 158
6.3.2.1 Hydrolyzation and Cr Adsorption.............. 158
6.3.2.2 Initial pH Value and Fe Content
Dependence............................................... 159
6.3.3 Micro/Nanostructured PAN@γ-AlOOH Fibers........ 160
6.3.3.1 Adsorption Isotherms of Cr(VI) Ions........ 161
6.3.3.2 Regeneration and Reusability of the
PAN@γ-AlOOH Fibers............................. 161
6.3.3.3 Structurally Enhanced and Protonation-
Dependent Adsorption............................... 162
6.4 Magnetic Micro/Nanostructured Materials as Adsorbents.... 163
6.4.1 Tremella-Like Fe3S4/C Magnetic Adsorbent............. 163
6.4.1.1 Adsorption Kinetics................................... 164
6.4.1.2 Adsorption Isotherms................................ 165
6.4.1.3 Regenerative Adsorption Performance...... 166
6.4.1.4 Enhanced Surface Carbon-Induced
Adsorption and Desorption........................ 168
6.4.2 Micro/Nanostructured Porous Fe3O4 Nanofibers
as an Effective and Broad-Spectral Adsorbent......... 169
6.4.2.1 Highly Effective Removal of PCBs........... 170
6.4.2.2 Strong Adsorption of Heavy Metal
Cations and Anions.................................... 171
6.4.2.3 Recycling Performance.............................. 172
6.5 Micro/Nanostructured Porous Metal Silicate Hollow
Spheres as Efficient Adsorbents............................................. 173
6.5.1 Magnesium Silicate Micro/Nanostructured
Hollow Spheres......................................................... 173
6.5.2 Copper Silicate Micro/Nanostructured Hollow
Spheres...................................................................... 176
6.5.3 Nickel Silicate Micro/Nanostructured Hollow
Spheres...................................................................... 177
6.6 Brief Summary....................................................................... 178
References......................................................................................... 178

Section II Hierarchical Micro/Nanostructured Arrays

Chapter 7 Micro/Nanostructured Block-Built Arrays....................................... 187

7.1 Introduction............................................................................ 187
x Contents

7.2 Zero-Dimensional Object-Built Arrays.................................. 188

7.2.1 Nanoparticle Array and Laser Morphological
Manipulation............................................................. 188
7.2.1.1 Morphology and Evolution........................ 188
7.2.1.2 Laser-Induced Spheroidization.................. 191
7.2.2 Nanoparticles on Microsized PS Sphere Arrays....... 192
7.2.3 Two-Step Replication to Prepare
Zero-Dimensional Nanostructured Materials........... 198
7.3 One-Dimensional Nanoobject-Built Arrays........................... 201
7.3.1 Self-Assembling 1D Nanostructures......................... 201
7.3.2 1D Nanostructure by Pulsed Laser Deposition.........202
7.3.3 1D Nanostructure by Magnetron Sputtering............. 212
7.4 Brief Summary....................................................................... 217
References......................................................................................... 217

Chapter 8 Micro/Nanostructured Ordered Porous Arrays................................ 223

8.1 Introduction............................................................................ 223
8.2 Micro/Nanostructured Ordered Pore Arrays Based on
Solution-Dipping Strategy......................................................224
8.2.1 Monolayer Ordered Pore Arrays............................... 225
8.2.1.1 In Situ Solution Dipping............................ 225
8.2.1.2 Morphology and Structure......................... 226
8.2.1.3 A Solvent Evaporation–Colloidal
Sphere Deformation Model....................... 227
8.2.1.4 Extensions of Solution-Dipping Strategy..... 229
8.2.2 Multilayer Ordered Pore Arrays................................ 236
8.2.2.1 Direct Synthesis of Homopore Sized
Porous Films on Any Surface.................... 236
8.2.2.2 Multilayer Heteropore Sized Porous Films.... 239
8.3 Micro/Nanostructured Ordered Pore Arrays Based on
Electrodeposition Strategy..................................................... 243
8.3.1 Metal Micro/Nanostructured Ordered Through-
Pore Arrays................................................................ 243
8.3.1.1 Electrodeposition Strategy Based on
PS Monolayer............................................. 243
8.3.1.2 Ordered Through-Pore Arrays..................244
8.3.1.3 Molecule Adsorption and Interface-
Weakening Model...................................... 247
8.3.1.4 Universality of the Strategy....................... 249
8.3.2 Semiconductor Micro/Nanostructured Ordered
Pore Arrays................................................................ 249
8.3.2.1 Morphology and Structure......................... 250
8.3.2.2 Oriented Substrate-Induced Oriented
Growth....................................................... 251
8.3.2.3 Other Materials.......................................... 252
Contents xi

8.3.3 Hollow Sphere Array Films Based on

Electrodeposition....................................................... 254
8.3.3.1 Ni Hollow Sphere Arrays.......................... 254
8.3.3.2 Hierarchically Micro/Nanostructured
Monolayer Hollow Sphere Arrays............. 256
8.3.3.3 Standing Ag Nanoplate–Built Hollow
Microsphere Arrays................................... 261
8.4 Micro/Nanostructured Ordered Pore Arrays Based on
Other Routes........................................................................... 269
8.4.1 Micro/Nanostructured Porous Array Based on
Electrophoretic Deposition........................................ 269
8.4.1.1 Strategy...................................................... 269
8.4.1.2 Fabrication of Colloidal Solutions by
Laser Ablation in Liquids.......................... 269
8.4.1.3 Morphology and Structure......................... 271
8.4.1.4 Influence of Current and Substrate............ 272
8.4.1.5 Formation of Hollow Spheres.................... 272
8.4.1.6 Universality of Strategy............................. 273
8.4.2 Noble Metal 3D Micro/Nanostructured Films
Based on Electrophoretic Deposition........................ 276
8.4.2.1 Au/ZnO Micro/Nanorod Arrays by
Electrophoresis in the Au Colloidal
Solution...................................................... 277
8.4.2.2 Au Nanochain–Built 3D Netlike
Porous Films by Electrophoretic
Deposition.................................................. 281
8.4.3 Micro/Nanostructured Hollow Sphere Arrays
Based on Gas-Phase Surface Sol-Gel Process.......... 285
8.5 Brief Summary....................................................................... 286
References......................................................................................... 286

Chapter 9 Surface Wettability and Self-Cleaning Properties............................ 293

9.1 Introduction............................................................................ 293
9.2 Tunable Wettability of Periodic ZnO Pore
Array Films............................................................................ 294
9.3 Controllable Superhydrophobicity of In2O3 Ordered Pore
Array Films............................................................................ 297
9.4 Irradiation-Induced Reversible Wettability of ZnO Pore
Array Films............................................................................300
9.5 Superhydrophobicity of Silver Hierarchical Bowl-Like
Arrays..................................................................................... 301
9.6 Wettability of Silica Ordered Micro/Nanostructured
Arrays..................................................................................... 303
9.6.1 Micro/Nanostructured Ordered Pore Array.............. 303
9.6.2 Ordered Nanopillar Arrays.......................................306
xii Contents

9.7 Wettability of Hierarchical Micro/Nanocomposite Arrays......307

9.7.1 Zero-Dimensional Nanostructures on Microsized
Polystyrene Spheres...................................................307
9.7.2 One-Dimensional Nanostructures on Microsized
Polystyrene Spheres...................................................309
9.8 Superhydrophobic Surfaces on Curved Substrates................. 314
9.9 Superamphiphilicity of TiO2 Hierarchical Micro/
Nanorod Arrays without Ultraviolet Irradiation.................... 316
9.10 Brief Summary and Remarks................................................. 319
References......................................................................................... 320

Chapter 10 Optical Properties and Devices......................................................... 323

10.1 Introduction............................................................................ 323
10.2 Controlled Optical Property of Gold Nanoparticle Arrays...... 323
10.3 Terahertz Absorption Bands in Au/Polystyrene Sphere
Arrays..................................................................................... 324
10.4 Tunable Surface Plasmon Resonance of Au
Opening-Nanoshell Ordered Arrays...................................... 329
10.4.1 Arrays’ Structure and Tunable SPR.......................... 330
10.4.2 Dependence of SERS Effect on SPR........................ 332
10.5 Photoluminescence Properties of Semiconductor
Periodic Arrays....................................................................... 334
10.5.1 PL of Oriented ZnO Ordered Pore Arrays................ 334
10.5.2 PL of In2O3 Ordered Pore Arrays.............................. 335
10.6 Quasi-Photonic Crystal Properties of Monolayer Hollow
Microsphere Array................................................................. 336
10.6.1 Tunable Optical Transmission Stop Band................. 336
10.6.2 Equivalent Double-Layer Photonic Crystal
Approximation.......................................................... 338
10.6.3 Optical Gas-Sensing Devices.................................... 339
10.7 Transmission Mode Wavemeter Devices Based on the
Ordered Pore Arrays...............................................................340
10.7.1 Basic Equations......................................................... 341
10.7.2 Optical Diffraction of the Ordered Pore Arrays....... 342
10.7.3 Resolution and Precision of Wavelength
Measurement.............................................................344
10.8 Brief Summary.......................................................................346
References.........................................................................................346

Chapter 11 Gas-Sensing Devices and Structurally Enhanced Gas-Sensing

Performances..................................................................................... 349
11.1 Introduction............................................................................ 349
11.2 Gas Sensors Based on Homopore-Sized Porous Films.......... 350
11.2.1 Construction of Sensing Device................................ 350
11.2.2 Structure-Dependent Gas-Sensing Performance...... 351
Contents xiii

11.3 Gas-Sensing Devices Based on Heteropore-Sized Porous

Films....................................................................................... 353
11.3.1 Gas-Sensing Devices................................................. 353
11.3.2 Gas-Sensing Performance with Both High
Sensitivity and Fast Response................................... 354
11.3.3 Pore Size–Dependent Gas-Sensing Performance
and Diagram of t R versus S........................................ 355
11.3.4 Structurally Induced Controllability of
Gas-Sensing Performances....................................... 357
11.3.5 Extension of the Strategy.......................................... 358
11.3.6 Doping-Induced Selectivity of Porous Films............ 361
11.4 High-Performance Gas-Sensing Devices Based on the
Porous Films/Mems Chip....................................................... 362
11.4.1 Construction Strategy of the High-Performance
Sensing Devices........................................................ 363
11.4.2 Integrated Gas Sensors.............................................. 365
11.4.3 Morphology and Microstructure............................... 365
11.4.4 Power Consumption and Heating Homogeneity....... 367
11.4.5 High Gas-Sensing Performances.............................. 368
11.4.5.1 Response Time and Sensitivity.................. 368
11.4.5.2 Lower Limit of Detection.......................... 370
11.4.5.3 Dependence of Sensitivity on Working
Temperature............................................... 371
11.4.5.4 Durability and Stability of the
MEMS-Based Sensing Devices................. 371
11.5 Brief Summary and Remarks................................................. 373
References......................................................................................... 374

Chapter 12 Surface-Enhanced Raman Scattering Performances and

Detection Applications...................................................................... 377
12.1 Introduction............................................................................ 377
12.2 Au Hierarchically Micro/Nanostructured Particle Arrays....... 377
12.3 Ag Nanoparticle–Built Hollow Microsphere (Nanoshell)
Arrays..................................................................................... 379
12.3.1 Tunability of the LSPR and SERS Properties........... 380
12.3.2 Structural Parameter-Dependent Coupling Effects...... 382
12.4 Standing Ag Nanoplate–Built Hollow Microsphere
Arrays..................................................................................... 384
12.4.1 SERS Activity of Ag Nanoplate–Built Hollow
Microsphere Arrays................................................... 385
12.4.2 Estimation of Enhancement Factor........................... 385
12.4.3 Structurally Enhanced Effect.................................... 387
12.4.4 Practicability of the Array......................................... 388
12.4.4.1 Reproducibility of Measurements.............. 388
12.4.4.2 Reusability as an SERS Substrate............. 388
xiv Contents

12.4.5 Application in Trace Detection of Cyanide............... 390

12.4.5.1 Surface Cleaning of Substrate................... 391
12.4.5.2 Effect of Excited Power............................. 391
12.4.5.3 Measurement Consistency of Parallel
Substrates................................................... 392
12.4.5.4 Effect of Immersion Time......................... 392
12.4.5.5 Trace Detection of Kalium Cyanide.......... 394
12.5 Brief Summary....................................................................... 397
References......................................................................................... 397
Series Statement
Materials form the foundation of technologies that govern our everyday life, from
housing and household appliances to handheld phones, drug delivery systems, air-
planes, and satellites. Development of new and increasingly tailored materials is the
key to further advancing important applications with the potential to dramatically
enhance and enrich our experiences.
The Advances in Materials Science and Engineering series by CRC Press/Taylor
& Francis is designed to help meet new and exciting challenges in materials science
and engineering disciplines. The books and monographs in the series are based on
cutting-edge research and development, and thus are up to date with new discover-
ies, new understanding, and new insights in all aspects of materials development,
including processing, characterization, and applications in metallurgy; bulk or sur-
face engineering; interfaces; thin films; coatings; and composites, just to name a few.
The series aims at delivering an authoritative information source to readers in
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materials world and the associated fields.
As series editor, I would like to thank all authors and editors of the books in this
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neering and to the advancement of humankind.

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xv
Preface
Nanomaterials and nanotechnology have attracted much attention and been exten-
sively studied for three decades because of their promising applications and scien-
tific significance. Great progress has been achieved in this field. The researchers in
this area have experienced the creation of new structures in early stages to controlled
growth, property and performance studies, and device fabrication and applications
in the past decade. Nanomaterial synthesis experienced changes from simple and
unitary nanostructures to the complicated nanostructures and superstructures, from
nanopowders to assemblies, from nanoparticles to hollow structures, from inorganic
to organic materials, from zero to multidimension, from random to regular growth,
from disordered arrangement to the periodic arrays, and so forth.
Hierarchical micro/nanostructured materials, which are composed of microsized
objects with nanostructures, have been considered in the recent decade. Such struc-
tured materials show the surface activity and specific surface area of nanomaterials,
and the structural stability and robustness of the bulk materials. They combine the
advantages of both nanostructured and bulk materials. Hierarchical micro/nano-
structured materials can exist in the forms of powders and regularly ranged arrays.
Micro/nanostructured object powders have large surface-to-volume ratios, high
stability against aggregation, and are very easily separated from solution. These
materials exhibit strong structurally enhanced properties, such as enhanced adsorp-
tion and catalysis performances compared with nanopowders or bulk ones, and hence
could be good candidates for new environmental materials for high-efficient removal
of contaminants in the environment. Further, if micro/nanostructured objects are
arranged into a pattern on a substrate in some way, hierarchical micro/nanostruc-
tured arrays will be formed. Such arrays could be the important bases of the next
generation of devices. There exist great potential applications in many fields, such
as catalysis, integrated nanophotonics, optical devices, super-high-density storage
media, sensors, nanobiotechnology, surface-enhanced Raman scattering (SERS)
substrates, and so forth.
Although morphology- and structure-controlled growth and synthesis of these
materials remain a promising challenge, a great deal of work in establishing parallel
micro/nanofabrication techniques, performance exploration, and related applications
has been done. Our group has also been in this field for nearly 10 years and focused
on the development of new fabrication methods, exploration of structurally enhanced
performance, surface properties, device applications, and so forth.
In this book, we will mainly present recent research progress of our group in the
hierarchical micro/nanostructured materials, including two sections: Hierarchical
Micro/Nanostructured Powders and Hierarchical Micro/Nanostructured Arrays in
fabrication, properties, and applications, and hope to reflect and show the perspec-
tives of the hierarchical micro/nanostructured materials in fundamental research
and applications.

xvii
xviii Preface

This book consists of 12 chapters. In addition to the general introduction of

hierarchical micro/nanostructured materials in Chapter 1, we introduce, in detail,
the mass production methods for hierarchical micro/nanostructured powders in
Chapters 2 through 4, including solvothermal routes, template-etching strategies,
and electrospinning technology, followed by structurally enhanced photocatalytic
and adsorption performance in Chapters 5 and 6, respectively. Further, we introduce
the modified colloidal lithography-based solution, electrodeposition strategies, and
so forth, for fabrication of hierarchical micro/nanostructured object arrays and their
devices in Chapters 7 and 8. In Chapters 9 through 12, we introduce and discuss
the structure-dependent properties and performance of the micro/nanostructured
arrays, including surface wettability, optical properties, gas-sensing performance,
SERS performance, and detection applications. This book also introduces applica-
tions of hierarchical micro/nanostructured materials in environmental remediation
and detection devices, and reviews the future trend of these materials in research and
applications.
Acknowledgments
This book is financially supported by the National Key Basic Research Program of
China (Grant No. 2013CB934303), the National Basic Research Program of China
(973 Program, Grant No. 2011CB302103), Recruitment Program of Global Experts
(C), the National Natural Science Foundation of China (Grant Nos. 11374303,
11174286, 51371165), and Anhui Provincial Natural Science Foundation for
Distinguished Young Scholar (Grant Nos. 1108085J20, 1408085J10).

xix
Authors
Weiping Cai earned a BS and MS in materials s­ ciences from
Northeast University in 1982 and 1984, respectively. In 1997,
he earned a PhD from Huazhong University of Science and
Technology in materials sciences. Since 1997, he has been
a professor at the Institute of Solid State Physics, Chinese
Academy of Sciences (CAS). His research interests include
micro/nanostructured patterns and detection devices, and
micro/nanomaterials for environmental applications.

Guotao Duan earned his PhD in 2007 from the Institute

of Solid State Physics, CAS, and continued to work there.
From April 2009 to March 2010, he did postdoctoral
work in the National Institute for Materials Science in
Japan. His current research interests focus on micro/
nanofabrication, ordered micro/nanostructured arrays, and
micro/nanodevices.

Yue Li earned his PhD in condensed matter physics at

the Institute of Solid State Physics, CAS, in 2005. Later
he worked as a postdoctoral fellow or visiting scientist in
the Korea Advanced Institute of Science and Technology,
National Institute of Advanced Industrial Science and
Technology, and Max Planck Institute of Colloids and
Interfaces. Since 2011, he has been working as a professor
in the Institute of Solid State Physics, CAS. His research
interests mainly focus on the fabrications, applications, and devices of micro/
nanostructured arrays based on the colloidal monolayer template techniques.

xxi
 1 General Introduction

Hierarchical micro/nanostructured materials are composed of microsized objects

with nanostructures. Such structured materials possess not only the high surface
activity and specific surface area of nanomaterials but also the structural stability
and robustness of the bulk. Micro/nanostructured powders are of large surface to
volume ratios, have high stability against aggregation, are very easily separated
from solution, and also exhibit strong structurally enhanced adsorption and catalysis
performances and, hence, can be used for the highly efficient removal of contami-
nants in the environment. Further, if the micro/nano-sized objects are arranged into
a pattern on a substrate, hierarchical micro/nanostructured arrays are formed. These
arrays have great potential applications in many fields, such as catalysis, integrated
nanophotonics, optical devices, super-high-density storage media, sensors, nano-
biotechnology, and surface-enhanced Raman scattering (SERS) substrates.

1.1 HIERARCHICAL MICRO/NANOSTRUCTURED POWDERS

The hazardous materials, such as organic pollutants and heavy metals from
­industrial production, released by human activities result in decreasing environ-
mental quality or in environmental pollution [1–4]. Such environmental pollution
has attracted more and more attention in recent years, especially in developing
countries. The harmful materials, including heavy metal ions, organic pollutants
have been released to air, water and soil which directly threaten the human health.
Till now, many useful methods and techniques have been developed for pollution
­remediation [5–9]. Among them, removal of pollutants by the method of adsorption
and/or catalysis using adsorptive and/or catalytic materials is important and effective
[10]. In this case, the key issue is the efficiency of absorptive and/or catalytic mate-
rials. Materials with high surface activity, high specific surface area, good selec-
tive adsorption, strong structural stability, and excellent reusable performance are
expected. Although nanosized particle powders can be candidates for such m ­ aterials
due to their high surface area and surface activity [5,6,11–16], they have no struc-
tural stability and are thus very easily aggregated, leading to unwanted reductions in
active surface area and surface activity and, hence, bad reusable p­ roperty. In addi-
tion, the used nanosized adsorbents or photocatalysts are suspended in solution and
difficult to separate from the bulk solution. On the other hand, the microsized par-
ticle powders are of good structural stability and have antiaggregation property, in
addition to being easily separated, but they are lacking in terms of surface area and
activity.
If the microscaled building blocks and the nanostructure are combined together,
hierarchical micro/nanostructured materials are formed [10,17]. Figure 1.1 shows
the typical morphology of TiO2 micro/nanostructured powders by the solvothermal

1
2 Hierarchical Micro/Nanostructured Materials

(a) (b) TiO2

5 µm 1 µm

FIGURE 1.1 A typical morphology of TiO2 microscaled particles with nanostructure by

solvothermal route. (a) and (b) Field-emission scanning electron microscopic images with
different magnifications.

route. The microsized objects resist aggregation, and the nanostructure supplies
high surface area and surface activity during usage. Therefore, such materials with
micro/nanoarchitectures not only possess large surface to volume ratios, have high
structural stability against aggregation, and are very easily separated from solu-
tion during application in pollution remediation but also exhibit strong structur-
ally enhanced adsorption and catalysis performances. They could overcome the
aforementioned shortcomings of the nanoparticles and microscaled objects, and
be good candidates of the environmental materials for high efficient removal of
contaminants.
In recent years, many methods have been developed for controlled and mass pro-
duction of such micro/nanostructured materials. Also, many progresses have been
made in removal of pollutants by using these materials as adsorbents or catalysts.

1.2 HIERARCHICAL MICRO/NANOSTRUCTURED ARRAYS

If the randomly distributed nano-objects [such as zero-dimensional nanoparticles
or nanodots, one-dimensional (1D) nano-objects, and two-dimensional (2D) nano-
plates] or the microscaled objects with nanostructures are regularly arranged, in a
certain way, on a substrate, a micro/nanostructured array is formed. Figure 1.2 shows
some typical micro/nanostructured arrays, including the nanodot array, 1D nano-
object array, and nano–hollow sphere array [18–20]. Such arrays are the important
basis of next generation of devices and have important potential applications in areas
such as catalysis, sensors, cells, SERS substrates, data storage, superhydrophobic
or superhydrophilic films, photonic crystals, optoelectronics, microelectronics, and
optical devices [21].
The properties of micro/nanostructured arrays are strongly correlated with their
structural parameters, such as the size, shape, and interspacing of the building blocks
in the array, and the supporting substrate, in addition to the intrinsic characters. Such
arrays possess not only the properties of the individual building block but also some
new performances due to the coupling effects between the building blocks. Usually,
the supporting substrate is selected according to device realization and compatibility
with desired materials. Building blocks should be controlled in both morphology and
size for a favorable functionality. Arrangement or packing of the building blocks is
General Introduction 3

(a) (b) (c)

100 nm

(a’) (b’) (c’)

1 µm

FIGURE 1.2 Morphologies of some typical nanoparticles and micro/nanostructured

arrays: (a) nanoparticles, (b) one-dimensional (1D) nano-objects, (c) nano–hollow spheres,
(a’) nanodot array, (b’) 1D nano-object array, and (c’) nano–hollow sphere array. (With
kind permission from Springer Science+Business Media: Appl. Phys. B, Laser morphologi-
cal manipulation of gold nanoparticles periodically arranged on solid supports, 81, 2005,
765–8, Sun et al.; Reprinted with permission from Liu et al., 2006, 2375–8. Copyright 2006
American Chemical Society.)

designed according to practical applications. In many cases, an ordered arrangement

of the building blocks is of high importance and allows a homogeneous surface char-
acteristic in a large dimension on the array film, which is obviously advantageous to
the designed devices and, thus, the subsequent stability of output functions.
It is well known that nanoparticles have many unique properties, which depend on
the size, shape, and structure of the particles. Development of new synthesis methods
for nanoparticles with controllable sizes, shapes, and structures and revealing the
new functional performances of nanoparticles have been the hot spot of research
activity in this field. For micro/nanostructured arrays, key issues include construc-
tion with low cost and according to need, reproducible fabrication and structural
consistency, and finding new performances and their structural dependence as well
as tunability. Aiming at the aforementioned key problems, extensive studies have
been performed and big advances been made.
In general, micro/nanostructured arrays can be fabricated by photolithography
[22–24], electron-beam lithography [25–28], microcontact printing [29,30], self-
assembly techniques [31,32], and so on. In the past decade, using 2D colloidal crys-
tals (i.e., the colloidal crystal with only few layers) as a template has shown great
promise for the fabrication of micro/nanostructured arrays. It has been found that
the monodispersed organic colloidal spheres can self-assemble into an ordered,
­hexagonally close-packed arrangement on a cleaned substrate driven by surface ten-
sion. Based on such ordered, arranged colloidal spheres and other assistant tech-
niques, such as physical vapor deposition [33], sol gel [34], solution dipping [35], and
electrodeposition [36,37], one can obtain various micro/nanostructured arrays after
4 Hierarchical Micro/Nanostructured Materials

removal of the colloidal spheres. This strategy, what we call colloidal lithography, is
of great advantages due to the material and substrate general, inexpensive, flexible in
controlling surface morphology and size.
The aforementioned hierarchical micro/nanostructured materials have attracted
much attention in recent years. Their properties depend on morphology and struc-
ture. Although the morphology and structure-controlled growth and ­synthesis of
these materials remain a promising challenge, a great deal of work in establishing
parallel micro/nanofabrication techniques and related applications has been done.
In this book, we present recent advances in the field of hierarchical micro/nano-
structured materials, in two parts, “Hierarchical Micro/Nanostructured Powders”
and “Hierarchical Micro/Nanostructured Arrays,” in terms of fabrication, proper-
ties, and applications.
This book introduces the new routes and technologies in the micro/nanostruc-
tured material field in detail, including structure-directed solvothermal routes,
template-etching strategies, electrospinning and in situ conversion, and modified
colloidal lithography–based solution and electrodeposition strategies. We introduce
and discuss the correlative novel performances and property control arising from
the micro/nanostructures. This book also introduces the applications of hierarchical
micro/nanostructured materials in environmental remediation and detection devices
and reviews the future trend of these materials in research and applications.

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