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Woodhead Publishing Series in Composites
Science and Engineering
Layered Double
Hydroxide Polymer
Nanocomposites
Edited by
Sabu Thomas
International and Inter University Centre for
Nanoscience and Nanotechnology,
Mahatma Gandhi University,
Kottayam, Kerala, India
School of Chemical Sciences,
Saju Daniel
International and Inter University Centre for
Nanoscience and Nanotechnology,
St. Xavier’s College Vaikom, Kottayam,
Kerala, India
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Contents
List of contributors xvii

Preface xxi
Acknowledgement xxv
1. Layered double hydroxides: fundamentals to applications 1

Saju Daniel and Sabu Thomas
1.1 Introduction 1
1.2 Layered double hydroxides 2
1.2.1 Structure of layered double hydroxides 2
1.2.2 Differences between Ordinary Clays and Layered Double
Hydroxides 4
1.2.3 Synthesis Routes of Layered Double Hydroxides 4
1.3 Organic Modification of Layered Double Hydroxides 7
1.3.1 One step Co-precipitation 11
1.3.2 Anion exchange reaction 12
1.3.3 Memory Effect or Regeneration Method 12
1.3.4 The delamination/restacking method 13
1.4 Characterization of layered double hydroxides and modified
layered double hydroxides 14
1.5 Potential applications of layered double hydroxides, organically
modified layered double hydroxides and layered double hydroxide
nanocomposites 21
1.5.1 Flame retardant applications 23
1.5.2 Catalysis 25
1.5.3 Water splitting 26
1.5.4 Environmental remediation 27
1.5.5 Electrode for super capacitor 30
1.5.6 Biomedical applications 32
1.6 Introduction to Layered Double Hydroxide Polymer
Nanocomposites 35
1.7 Different Fabrication Techniques of Layered Double Hydroxide
polymer Nanocomposites 35
1.7.1 Melt Compounding 35
1.7.2 Solution Blending 37
1.7.3 In Situ Methods 38
1.7.4 Layer By Layer Assembly 39
1.7.5 Two roll mill mixing 41
vi Contents
1.7.6 Sonication 42
1.7.7 High energy ball milling 42
1.8 Applications of Layered Double Hydroxide Polymer
Nanocomposites 43
1.8.1 Flame Retardant Application 43
1.8.2 Biomedical Application 44
1.8.3 Gas sensing Applications 49
1.8.4 Energy Applications 50
1.8.5 Food Packaging Applications 51
1.8.6 Water Purification 52
1.8.7 Gas Barrier Materials 53
1.8.8 Agricultural Applications 54
1.8.9 Anti Corrosion Materials 55
1.9 LDH based polymer hybrid nanocomposites 56
1.10 Conclusion and perspectives 63
1.11 Abbreviations 66
References 68
2. FTIR characterization of layered double hydroxides and modified

layered double hydroxides 77
Meisam Shabanian, Mohsen Hajibeygi and Ahmad Raeisi
2.1 Introduction 77
2.2 Fourier transform infrared spectra of layered double hydroxides 79
2.2.1 Fourier transform infrared characteristic absorption bands
of layered double hydroxides with different anions 79
2.2.2 Fourier transform infrared characteristic absorption bands
of layered double hydroxides with different metals 83
2.2.3 FTIR spectra of layered double hydroxides containing three
metals 85
2.3 FTIR spectra of organo-modified layered double hydroxides 87
2.4 Conclusion 95
References 96
3. Fabrication technologies of layered double hydroxide polymer

nanocomposites 103
Shadpour Mallakpour and Farbod Tabesh
3.1 Introduction 103
3.1.1 Layered double hydroxides 103
3.1.2 Modification of layered double hydroxides 104
3.2 Preparation of polymer/layered double hydroxide nanocomposites 106
3.2.1 Introduction 106
3.3 Preparation of Natural polymer/layered double hydroxide
nanocomposites 115
3.3.1 Preparation of carboxymethylcellulose/layered double
hydroxide nanocomposites 115
Contents vii
3.3.2 Preparation of pectin/layered double hydroxide

nanocomposites 116
3.3.3 Preparation of chitosan/layered double hydroxide
nanocomposites 117
3.3.4 Preparation of natural rubber/layered double hydroxide
nanocomposites 118
3.3.5 Other natural polymer/layered double hydroxide
nanocomposites 120
3.4 Preparation of synthetic polymer/layered double hydroxide
nanocomposites 120
3.4.1 Preparation of polyimide/layered double hydroxide
nanocomposites 122
3.4.2 Preparation of poly(methyl methacrylate)/layered double
3.4.3 Preparation of polyvinyl acetate/layered double hydroxide
nanocomposites 124
3.4.4 Preparation of P(MMA-co-BA)/layered double hydroxide
nanocomposites 124
3.4.5 Preparation of wood flour/polypropylene/layered double
3.4.6 Preparation of poly(amide-imide)/layered double
3.4.7 Preparation of low-density polyethylene/layered double
3.4.8 Preparation of polyvinyl alcohol/layered double hydroxide
nanocomposites 134
3.4.9 Preparation of polyester/layered double hydroxide
nanocomposites 136
3.4.10 Preparation of polyvinyl chloride/layered double hydroxide
nanocomposites 137
3.4.11 Preparation of polypropylene-ethylene vinyl acetate/layered
double hydroxide nanocomposites 139
3.4.12 Preparation of silicone rubber/layered double hydroxide
nanocomposites 140
3.4.13 Preparation of epoxy resin/MoS2/layered double hydroxide
nanocomposites 141
3.4.14 Preparation of polyurethane/nitrile butadiene rubber
Blend/layered double hydroxide nanocomposites 143
3.4.15 Preparation of polyethyleneimine/poly(sodium 4-styrene
sulfonate) hybrid/layered double hydroxide
nanocomposites 144
3.4.16 Preparation of isotactic polypropylene/layered double
3.5 Conclusions and future perspectives 148
viii Contents
Acknowledgments 152
References 152
4. Microscopic characterization techniques for layered double

hydroxide polymer nanocomposites 157
Shadpour Mallakpour and Shima Rashidimoghadam
4.2 Microscopic characterization techniques for PNCs 158
4.2.1 Optical microscope 159
4.2.2 Scanning electron microscope 159
4.2.3 Transmission electron microscope 160
4.2.4 Field ion microscope 162
4.2.5 Scanning probe microscope 162
4.2.6 Scanning tunneling microscope 163
4.2.7 Atomic force microscope 164
4.2.8 X-Ray diffraction topography 165
4.3 Microscopic characterization of polymer/LDH NCs 165
4.3.1 Microscopic characterization of elastomer/LDH NCs 166
4.3.2 Microscopic characterization of thermoplastic
polymer/LDH NCs 170
4.3.3 Microscopic characterization of thermosetting
polymer/LDH NCs 183
4.3.4 Microscopic characterization of polymer blend/LDH NCs 192
4.4 Conclusions 197
Acknowledgments 197
References 197
Further reading 203
5. X-ray diffraction analysis of layered double hydroxide polymer

nanocomposites 205
Rodrigo Botan and Sabrina de Bona Sartor
5.2 X-ray diffraction analysis 206
5.3 X-ray diffraction analysis of layered double hydroxides and
Modified Layered Double Hydroxides 210
5.4 X-ray diffraction analysis of layered double hydroxide polymer
nanocomposites 216
5.5 Conclusion 225
References 226
6. Spectroscopic characterization techniques for layered double

Shadpour Mallakpour and Faezeh Azimi
Contents ix
6.2 Spectroscopy of polymer nanocomposites 232

6.2.1 Fourier transform infrared spectroscopy 233
6.2.2 Raman spectroscopy 233
6.2.3 Energy-dispersive X-ray spectroscopy 233
6.2.4 Fluorescence spectroscopy 234
6.2.5 Dielectric spectroscopy 234
6.2.6 Nuclear magnetic resonance spectroscopy 234
6.2.7 UVvis spectrophotometry 235
6.2.8 X-ray photoelectron spectroscopy 235
6.3 Spectroscopic characterization of layered double hydroxide
polymer nanocomposites 236
6.3.1 Fourier transform infrared spectroscopy of layered double
6.3.2 Raman spectroscopy of layered double hydroxide polymer
nanocomposites 239
6.3.3 Energy-dispersive X-ray spectroscopy of layered double
6.3.4 Fluorescence spectroscopy of layered double hydroxide
6.3.5 Dielectric spectroscopy of layered double hydroxide
6.3.6 Nuclear magnetic resonance spectroscopy of layered
double hydroxide polymer nanocomposites 258
6.3.7 UVvis spectroscopy of layered double hydroxide
6.3.8 X-ray photoelectron spectroscopy of layered double
6.4 Spectroscopic characterization for the aging process 270
6.5 Conclusions 273
Acknowledgments 274
References 274
Further reading 279
7. Melt rheological properties of layered double hydroxide polymer

nanocomposites 281
Appukuttan Saritha and Kuruvilla Joseph
7.1.1 The importance of rheological studies of polymer
nanocomposites 281
7.1.2 Rheology of polymer layered double hydroxide
nanocomposites 282
7.2 Rheology of thermoplastic polymer layered double hydroxide
nanocomposites 284
7.3 Rheology of thermosetting polymer layered double hydroxide
nanocomposites 297
x Contents
7.4 Modeling of rheological properties 301

7.5 Conclusions and future scope 305
References 305
Further reading 310
8. Thermal properties and flame-retardant characteristics of layered

double hydroxide polymer nanocomposites 311
Yanshan Gao, Lei Qiu, Dermot O’Hare and Qiang Wang
8.2 The techniques for determining thermal stability properties and
flame retardancy performance 313
8.2.1 The techniques for determining thermal stability properties
of polymers 313
8.2.2 The techniques for determining the flame-retardant
performance of polymers 314
8.3 LDH-based thermal stabilizer materials and their applications 317
8.3.1 Thermal stabilizer introduction 317
8.3.2 Thermal stability properties of LDH-based nanocomposites 318
8.3.3 The mechanism of thermostability using LDHs 322
8.4 LDH-based flame-retardant materials and their applications 323
8.4.1 Flame retardant introduction 323
8.4.2 Flame-retardant performance of LDH-based nanocomposites 324
8.4.3 Posttreatment of LDHs as flame retardants 337
8.4.4 The mechanism of flame retardancy using LDH 338
8.5 Conclusions and future development 340
References 340
9. Mechancial and dynamical mechanical properties of layered double

hydroxide-filled elastomer and elastomeric blend nanocomposites 347
Suneel Kumar Srivastava
9.2 Preparative methods of LDH-elastomer and LDH-elastomeric
blend nanocomposites 349
9.3 Different types of layered double hydroxide fillers used in the
fabrication of elastomer and elastomeric blend nanocomposites 350
9.4 Morphology of elastomer-LDH and elastomeric blend-LDH
nanocomposites 350
9.4.1 Morphology of elastomeric-LDH nanocomposites 350
9.4.2 Morphology of elastomeric blend-LDH nanocomposites 367
9.5 Mechanical properties of elastomer-LDH and elastomeric
blend-LDH nanocomposites 372
9.5.1 Mechanical properties of elastomer-LDH nanocomposites 372
9.5.2 Mechanical properties of elastomeric blend-LDH
nanocomposites 383
Contents xi
9.6 Dynamical mechanical properties of LDH-filled elastomer and

elastomeric blend nanocomposites 388
9.6.1 Dynamical mechanical properties of elastomer-LDH
nanocomposites 388
9.6.2 Dynamical mechanical properties of elastomer blend-LDH
nanocomposites 398
9.7 Conclusion 402
References 403
10. Layered double hydroxide nanocomposites based on carbon

nanoforms 411
Gonzalo Abellán, Jose A. Carrasco and Eugenio Coronado
10.1 A general introduction to LDH-carbon nanoform nanocomposites 411
10.2 Graphene and graphene oxide/LDH nanocomposites 415
10.2.1 Synthesis 417
10.3 Carbon nanotubes/LDH nanocomposites 425
10.3.1 Synthesis 427
10.4 Other CNF/LDH nanocomposites 431
10.4.1 Fullerene/LDH nanocomposites 431
10.4.2 Carbon quantum dot/LDH nanocomposites 431
10.4.3 Carbon spheres/LDH nanocomposites 431
10.4.4 Carbon (nano)fibers/LDH nanocomposites 432
10.4.5 Graphene/single-walled CNT/LDH nanocomposites 436
10.5 Applications of CNF/LDH nanocomposites 436
10.5.1 Energy storage and conversion 436
10.5.2 Catalysis 443
10.5.3 Miscellanea 445
10.6 Conclusions 448
10.7 Perspectives 449
Acknowledgments 450
References 450
Further reading 460
11. Recent advances in layered double hydroxide/polymer latex

nanocomposites: from assembly to in situ formation 461
V. Prevot and E. Bourgeat-Lami
11.2 Use of latex technology for the production of LDH-based
composite materials and macroporous structures 464
11.2.1 Assembly of preformed LDH and latex particles 464
11.2.2 LDH-based nanocomposites by in situ emulsion and
suspension polymerizations 468
11.2.3 Latex-templating approaches 475
11.3 Properties of LDH-based nanocomposites and LDH macroporous
structures 481
xii Contents
11.3.1 LDH-based nanocomposites 481

11.3.2 LDH-based macroporous structures 485
11.4 Concluding remarks and general trends 489
References 489
12. Fabrication, assembly, and optoelectric properties of layered double

hydroxide/conjugated polymer nanocomposites 497
Yaping Huang, Harrone Muhammad Sohail and Jun Lu
12.1 Fabrication and assembly of LDHs/conjugated polymer
nanocomposites 497
12.1.1 Introduction 497
12.1.2 Fabrication and assembly of LDH/CP nanocomposites 499
12.2 Optical and optoelectric properties of LDH/CP nanocomposites 515
12.2.1 Optical properties 515
12.2.2 Optoelectric properties 522
12.3 Conclusions and outlook 525
References 526
13. Polymer layered double hydroxide hybrid nanocomposites 531

Shadpour Mallakpour and Elham Khadem
13.2 Modification of LDHs with organic compounds 532
13.3 Layered double hydroxide/Carbonaceous nanofiller hybrids 535
13.4 Synthesis of LDH/Carbonaceous nanofiller hybrids 536
13.5 Applications of LDH/Carbonaceous nanofiller hybrids 538
13.5.1 Removal of pollution 538
13.5.2 Supercapacitor 543
13.5.3 Catalyst 546
13.6 Polymer/LDH/Carbonaceous nanofiller hybrid nanocomposites 548
13.6.1 Polymer/LDH/CNT hybrid nanocomposites 550
13.6.2 Polymer/LDH/graphene hybrid nanocomposites 554
13.6.3 Polymer/LDH/Other nanofiller hybrids 556
Acknowledgments 559
References 559
14. Electrical and electronic applications of layered double-hydroxide

Shadpour Mallakpour and Forough Motirasoul
14.2 Supercapacitors 568
14.2.1 Application of Layered Double Hydroxide
Nanocomposites in Supercapacitors 568
14.2.2 Application of Layered Double Hydroxide/Polymer
Nanocomposites in Supercapacitors 571
Contents xiii
14.3 Batteries 574

14.3.1 Application of Layered Double Hydroxide
Nanocomposites in Batteries 575
Nanocomposites in Batteries 577
14.4 Fuel Cells 579
Nanocomposites in Fuel Cells 580
14.5 Other Electrical and Electronic Applications of Layered Double
Hydroxide/Polymer Nanocomposites 587
Acknowledgments 591
References 592
15. Applications of layered double hydroxide biopolymer

nanocomposites 599
Shadpour Mallakpour and Leila khodadadzadeh
15.2 Biopolymer/layered double hydroxide nanocomposites 604
15.2.1 Polysaccharide/layered double hydroxide nanocomposites 604
15.2.2 Protein/layered double hydroxide nanocomposites 632
15.2.3 PHA/layered double hydroxide nanocomposites 633
15.2.4 PLA/layered double hydroxide nanocomposites 643
15.2.5 PVA/layered double hydroxide nanocomposites 653
Acknowledgments 665
References 665
16. Layered double hydroxide based nanocomposites for biomedical

applications 677
Raji Vijayamma, Nandakumar Kalarikkal and Sabu Thomas
16.1.1 Layered double hydroxide nanocomposites 678
16.1.2 Layered double hydroxide nanocomposites
in the medical field 680
16.2 Biomedical applications of layered double hydroxide
nanocomposites 685
in drug-delivery applications 685
in gene-delivery applications 688
16.2.3 Bioimaging applications 693
16.2.4 Biosensor 694
16.2.5 Layered double hydroxide nanocomposites for tissue
engineering applications 694
xiv Contents
16.3 Layered double hydroxide polymer nanocomposites for

biomedical applications 695
16.3.1 Alginatelayered double hydroxide nanocomposites 695
16.3.2 Chitosanlayered double hydroxide nanocomposites 698
16.3.3 Other polymerlayered double hydroxide nanocomposites 709
16.4 Summary 710
References 710
Further reading 714
17. Layered double hydroxide nanocomposites for agricultural

applications 715
Luı´z Paulo Figueredo Benı´cio, Frederico Garcia Pinto and Jairo Tronto
17.2 The history and evolution of chemical use in agriculture 716
17.3 Principal agricultural problems to resolve with new technologies 718
17.4 Layered double hydroxide applications in agriculture 719
17.4.1 Layered double hydroxide matrices of slow-release
fertilizers 720
17.4.2 Layered double hydroxides for storage and gradual
herbicide release 726
17.4.3 Layered double hydroxides for storage and slow release
of plant growth regulators 727
17.4.4 Use of layered double hydroxides for pesticide removal 730
17.5 Final considerations 733
List of abbreviations 734
References 734
Further reading 741
18. Layered double hydroxide polymer nanocomposites for

food-packaging applications 743
Giuliana Gorrasi and Andrea Sorrentino
18.1.1 Characterization and analytical techniques of polymer
nanocomposites for food-packaging applications 747
18.2 Layered double hydroxides as hosts of active molecules for
potential in food-packaging applications 748
18.3 Polymeric nanocomposites based on layered double
hydroxide-active molecules 754
18.3.1 Nanocomposites from oil-derived polymers 756
18.3.2 Nanocomposites of bioplastics from fossil-based
resources 760
18.3.3 Nanocomposites of bioplastics from renewable sources 764
18.4 Regulation issues 766
18.5 Conclusions and future perspectives 767
Contents xv
Acknowledgment 768
References 768
19. Layered double hydroxide polymer nanocomposites for water

purification 781
Shadpour Mallakpour and Vajiheh Behranvand
19.2 Pollutant elimination from water: why layered double hydroxides? 782
19.2.1 Structural properties of layered double hydroxides 782
19.2.2 Layered double hydroxide modification 782
19.2.3 Water pollutants 783
19.2.4 Mechanisms of adsorption 783
19.3 Pollutant elimination by polymer/layered double hydroxide
nanocomposites 790
19.3.1 Importance of using polymer/layered double hydroxide
nanocomposites in water purification 790
19.3.2 Polymer/layered double hydroxide-based adsorbents 791
Acknowledgments 798
References 799
20. Layered double hydroxide polymer nanocomposites for catalysis 805

Shadpour Mallakpour and Hashem Tabebordbar
20.2 Applications of layered double hydroxides in catalysis 807
20.3 Polymer/layered double hydroxide nanocomposites 811
20.3.1 Preparation of polymer/layered double hydroxide
nanocomposites 812
20.4 Applications of polymer/layered double hydroxide nanocomposites
in catalysis 815
Acknowledgments 829
References 829
Index 835
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List of contributors
Gonzalo Abellán Institute of Molecular Science (ICMol), University of Valencia,

Valencia, Spain; Department of Chemistry and Pharmacy and Joint Institute of
Advanced Materials and Processes (ZMP), University Erlangen-Nürnberg, Fürth,
Germany
Faezeh Azimi Chemistry Group, Pardis College, Isfahan University of

Technology, Isfahan, Islamic Republic of Iran
Vajiheh Behranvand Organic Polymer Chemistry Research Laboratory,

Department of Chemistry, Isfahan University of Technology, Isfahan, Islamic
Republic of Iran
Luı́z Paulo Figueredo Benı́cio Soil Department, Federal University of Viçosa,

Brazil
Rodrigo Botan Unifacvest University, Lages, SC, Brazil
E. Bourgeat-Lami University of Lyon, Université Claude Bernard Lyon 1, CPE

Lyon, CNRS, UMR 5265, Chemistry, Catalysis, Polymers and Processes (C2P2),
Villeurbanne, France
Jose A. Carrasco Institute of Molecular Science (ICMol), University of Valencia,

Valencia, Spain
Eugenio Coronado Institute of Molecular Science (ICMol), University of

Valencia, Valencia, Spain
Saju Daniel International and Inter University Centre for Nanoscience and
Nanotechnology, Mahatma Gandhi University, Kottayam, Kerala, India; St.
Xavier’s College Vaikom, Kottayam, Kerala, India
Sabrina de Bona Sartor Unifacvest University, Lages, SC, Brazil
Yanshan Gao College of Environmental Science and Engineering, Beijing

Forestry University, Beijing, P.R. China
xviii List of contributors
Giuliana Gorrasi Department of Industrial Engineering, University of Salerno-via

Giovanni Paolo II 132, Fisciano, Italy
Mohsen Hajibeygi Faculty of Chemistry, Kharazmi University, Tehran, Iran
Yaping Huang Beijing University of Chemical Technology, Beijing, P.R. China
Kuruvilla Joseph Department of Chemistry, Indian Institute of Space Science and

Technology, Valiamala, Thiruvananthapuram, Kerala, India
Nandakumar Kalarikkal International and Inter University Centre for

Nanoscience and Nanotechnology, Mahatma Gandhi University, Kottayam,
India; School of Pure and Applied Physics, Mahatma Gandhi University,
Kottayam, India
Elham Khadem Organic Polymer Chemistry Research Laboratory, Department of

Chemistry, Isfahan University of Technology, Isfahan, Islamic Republic of Iran
Leila Khodadadzadeh Chemistry Group, Pardis College, Isfahan University of

Jun Lu Beijing University of Chemical Technology, Beijing, P.R. China
Shadpour Mallakpour Organic Polymer Chemistry Research Laboratory,

Republic of Iran; Research Institute for Nanotechnology and Advanced Materials,
Isfahan University of Technology, Isfahan, Islamic Republic of Iran; Chemistry
Group, Pardis College, Isfahan University of Technology, Isfahan, Islamic Republic
of Iran
Forough Motirasoul Organic Polymer Chemistry Research Laboratory,

Republic of Iran
Dermot O’Hare University of Oxford, Oxford, United Kingdom
Frederico Garcia Pinto Institute of Exact and Technological Sciences, Federal

University of Viçosa - Rio Paranaı́ba Campus, Brazil
V. Prevot CNRS, ICCF - Institut de Chimie de Clermont-Ferrand, Université

Clermont Auvergne, Clermont-Ferrand, France
Lei Qiu College of Environmental Science and Engineering, Beijing Forestry

University, Beijing, P.R. China
List of contributors xix
Ahmad Raeisi Organic Polymer Chemistry Research Laboratory, Department of

Chemistry, Faculty of Science, Arak University, Arak, Iran
Shima Rashidimoghadam Department of Chemistry, Organic Polymer Chemistry

Research Laboratory, Isfahan University of Technology, Isfahan, Islamic Republic
of Iran
Appukuttan Saritha Department of Chemistry, School of Arts and Sciences,

Amrita Vishwa Vidyapeetham, Amritapuri, Kollam, Kerala, India
Meisam Shabanian Faculty of Chemistry and Petrochemical Engineering,

Standard Research Institute (SRI), Karaj, Iran
Harrone Muhammad Sohail Beijing University of Chemical Technology,

Beijing, P.R. China
Andrea Sorrentino Institute for Polymers, Composites and Biomaterials (IPCB),

National Research Council (CNR), Lecco, Italy
Suneel Kumar Srivastava Department of Chemistry, Indian Institute of

Technology, Khragpur, India
Hashem Tabebordbar Organic Polymer Chemistry Research Laboratory,

Republic of Iran
Farbod Tabesh Chemistry Group, Pardis College, Isfahan University of

Sabu Thomas International and Inter University Centre for Nanoscience and
Nanotechnology, Mahatma Gandhi University, Kottayam, Kerala, India; School of
Chemical Sciences, Mahatma Gandhi University, Kottayam, Kerala, India
Jairo Tronto Institute of Exact and Technological Sciences, Federal University of

Viçosa - Rio Paranaı́ba Campus, Brazil
Raji Vijayamma International and Inter University Centre for Nanoscience and
Nanotechnology, Mahatma Gandhi University, Kottayam, Kerala, India
Qiang Wang College of Environmental Science and Engineering, Beijing Forestry

University, Beijing, P.R. China
Preface
Recently the researchers have turned their attention toward layered double hydroxide
(LDH) polymer nanocomposites because of the distinctive properties of LDHs such as
wide range of chemical compositions, structural homogeneity, unique and excellent
anion exchanging ability, easy synthesis, high bound water content, memory effect,
nontoxicity and biocompatibility, and their wide range of applications. This book
really showcases the researches of many famous scientists who have been working in
the field of LDHs. The aspire of introducing this compendium is to replenish a solid
understanding of the recent innovative advances in the fabrication, characterization, and
applications of polymer LDH nanocomposites in various fields such as biomedical,
aerospace, electrical and electronics, automotive industry, agricultural, water treatment,
and catalysis.
This book consists of 20 chapters and all the chapters cover various relevant topics
and state of the art, new challenges, and opportunities in each field. Chapter 1 is actu-
ally a voyage from LDHs to LDH polymer nanocomposites so that one can acquire
the knowledge of different strategies required to convert LDHs to exfoliated LDH
polymer nanocomposites. Chapter 2 provides Fourier transform infrared spectroscopic
characterization of various LDHs and organically modified LDHs with the help of
which success of organic modification can be easily identified. Chapter 3 illustrates
recent advances in the fabrication technologies of LDH polymer nanocomposites
with suitable examples and it helps to find the novel and green procedure for the fab-
rication of LDHbased nanocomposites of each type of polymer.
Chapters 46 highlight advanced morphological characterization techniques
such as X-ray diffraction analysis, wide range of spectroscopic and microscopic
characterization techniques for LDH, organically modified LDHs, and LDH poly-
mer nanocomposites. In chapter 4 basal spacing of various organically modified
LDHs are provided so that suitable organic modifiers required for the preparation
of exfoliated polymer nanocomposites can be easily detected and the diffraction
pattern of the polymer nanocomposite helps to predict the morphology of the com-
posite—intercalated or exfoliated. Chapters 5 and 6 focus on spectroscopic charac-
terization techniques such as nuclear magnetic resonance spectroscopy, electron
spin resonance spectroscopy, ultraviolet visible spectroscopy, Fourier transform
infrared spectroscopy, dielectric spectroscopy, fluorescence spectroscopy, Raman
spectroscopy, X-ray photoelectron spectroscopy, and microscopic characterization
techniques such as optical microscopy, scanning electron microscopy, transmission
electron microscopy, and atomic force microscopy to help in characterizing the
xxii Preface
nanoscale dispersions, phase segregation, and interface/interphases of polymer

nanocomposites.
Chapters 79 discuss specific properties of LDH polymer nanocomposites such
as melt rheological properties, thermal and flame retardancy, and mechanical and
dynamic mechanical properties. Chapter 7 reviews the rheology of nanocomposites
of thermoplastics and thermosetting polymers filled with LDH and modified LDH
with special emphasis on the modeling of rheological properties to understand the
LDH particle dispersion and its influence on the melt flow behavior of the nano-
composites. Chapter 8 summarizes the thermal stability and flame retardancy of
LDH polymer nanocomposites, their characterization techniques such as thermogra-
vimetric analysis, cone calorimetry, limiting oxygen index and UL94 investigations,
and the synergistic effect of LDH with other thermal stabilizers and fire retardants.
Chapter 9 reviews recent advances on the mechanical and dynamical mechanical
properties of LDH filled elastomer and elastomeric blend nanocomposites.
Chapters 1013 discuss fabrication and applications of carbon nanoform/LDH
nanocomposites, LDH/polymer latexes nanocomposites, LDH/conjugated polymer
nanocomposites, and LDHbased polymer hybrid nanocomposites. Chapter 10
deals with the fabrication of carbon nanoform/LDH nanocomposites and their appli-
cations in super capacitor, water splitting, catalysis, drug delivery, and environment
protection. In Chapter 11 three main routes for the fabrication of LDH/polymer
latexes nanocomposites such as electrostatic assembly, in situ polymerization, and
latex-templating and their flame retardant applications are reviewed. Chapter 12
introduces various LDH/conjugated polymer nanocomposites fabricated by layer-
by-layer assembly through electrostatic interaction, hydrogen bonds, van der Waals
force of attraction, and miscellaneous interactions for optoelectronic applications.
Chapter 13 focuses on the state of the art in the preparation of polymer/LDH/carbo-
naceous nanomaterial hybrids and the influence of hybrid fillers on the properties
such as thermal, mechanical, permeability, and drug delivery properties of
polymers.
Chapters 1420 discuss wide range applications of LDH polymer nanocompo-
sites, such as electrical and electronic applications such as super capacitors, batter-
ies, and fuel cells, biomedical applications, such as controlled drug delivery, gene
delivery, tissue engineering, and photodynamic therapy, and agricultural applica-
tions, such as controlled fertilizer, herbicide and plant growth regulators release and
pesticide removal, food packaging, water purification, and catalysis. The main focus
of Chapter 15 is on the fabrication of LDHbased polymer nanocomposites con-
taining biopolymer matrix for the environmental protection and their important
applications in the fields of water treatment, drug delivery, tissue engineering, pack-
aging, and catalysis.
This book is really an one stop reference book emphasizing recent advances in
the technologies for the fabrication and characterization of LDHs, organically modi-
fied LDHs, LDH nanocomposites, LDHbased polymer nanocomposites, and
LDH-based polymer hybrid nanocomposites and their wide range of applications
thereby covering almost all the points of LDH chemistry. Therefore this book will
Preface xxiii
lend a hand to academics, researchers, scientists, engineers, industrialists, and stu-

dents in the field of polymer nanocomposites especially polymer LDH nanocompo-
sites to discern solutions to their unreciprocated posers.
Sabu Thomas and Saju Daniel

Acknowledgement
We express our sincere thanks to all the authors who have taken so much effort and
spent their valuable time for contributing chapters to this book. We are very much
grateful to the peer reviewers for the valuable guidance. We would like to appreci-
ate and acknowledge all the Elsevier team members of this project for their continu-
ous and unforgettable support throughout the editing of this book.
Layered double hydroxides:
fundamentals to applications 1
Saju Daniel1,2 and Sabu Thomas1,3
1
International and Inter University Centre for Nanoscience and Nanotechnology,
Mahatma Gandhi University, Kottayam, Kerala, India, 2St. Xavier’s College Vaikom,
Kottayam, Kerala, India, 3School of Chemical Sciences, Mahatma Gandhi University,
1.1 Introduction
In recent years, Layered double hydroxides have achieved a lot of attention both
from academia and industries due to their easy and ecofriendly synthesis, low cost,
non toxicity, structural and compositional tunability, high chemical and thermal
stability, high biocompatibility and broad spectrum applications. By exploiting the
three outstanding properties of layered double hydroxides, compositional flexibility
in cations and anions, excellent anion exchange ability, memory effect, it is very
easy to tailor layered double hydroxides into functional hybrid materials and nano-
composites for vast field applications. LDHs can be synthesized by simple methods
which enable control over structure, composition and shape by properly varying the
conditions. Recent developments in the synthesis methods have offered various
morphologies such as microspheres, fibrous structures, nano sized belt, LDH films
on substrates etc leads to tremendous range of possibilities for the fabrication of
smart high-performance multifunctional materials. So the fabrication of layered dou-
ble hydroxide based functional hybrid materials and nanocomposites have become
one of the most fascinating topics of today’s research. One way of producing the
LDH hybrid is the intercalation of smart inorganic or organic functional materials
into the nanospace in the intergallery space by anion exchange to form inorganic/
inorganic or inorganic/organic hybrid system for controlled drug delivery, pesticide
delivery, gene delivery, biosensor applications, bioimaging etc. Second way is to
mix LDH with smart nanomaterials like graphene, carbon nanotube etc to form
nanocomposites for energy storage and conversion like electrode for super capaci-
tors, batteries, fuel cell, solar cell, photo catalysts and electro catalysts for water
splitting, environmental remediation such as water treatment, removal of toxic gases
from atmosphere. Third way is to introduce organically modified LDH or exfoliated
LDH sheets or LDH/other nanofillers hybrid into the polymer matrix to develop
polymer nanocomposites or LDH based polymer hybrid nanocomposites for energy,
food packaging, agricultural, biomedical, flame retardant, gas barrier, anticorrosion,
waste water treatment etc. Thin films and core-shell hierarchical hybrid nanostruc-
tures formed from LDH sheets and any other nanofillers or polymers attracted much
Layered Double Hydroxide Polymer Nanocomposites. DOI: https://doi.org/10.1016/B978-0-08-101903-0.00001-X
© 2020 Elsevier Ltd. All rights reserved.
2 Layered Double Hydroxide Polymer Nanocomposites
attention because of their high performance in photoluminescence, drug delivery,

electrode for super capacitors etc. The aim of this chapter is to make aware of the
readers the importance of layered double hydroxides, layered double hydroxide
nanocomposites and layered double hydroxide based polymer nanocomposites so as
to motivate them to develop hierarchical hybrid nanostructures for the benefit of the
society. For this purpose, from fundamentals to applications of layered double
hydroxides, LDH hybrids and polymer nanocomposites are reviewed.
1.2 Layered double hydroxides

Layered double hydroxides are versatile and emergent class of two dimensional
inorganic layered nanomaterials, natural or synthetic anionic clay minerals, of
which the general formula is [M211-x Mx31 (OH) 2] x1 (An2) x/n. yH2O where MII
is a divalent ion, MIII is a trivalent ion, An2 is an anion and charge density of LDH
layers, x 5 MIII/MII 1 MIII whose value lies between 0.2 and 0.33 for pure LDH
phase (Taviot-Guého et al., 2018; Basu et al., 2014). This formula gives rise to a
generic layer sequence [AcBZAcB]n for layered double hydroxides in which A and
B represents layers of hydroxide anions, c represents layers of metal cations and
Z represents layers of other anions such as carbonate ion, chloride ion, nitrate ion
etc and neutral molecules like water molecules (https://en.wikipedia.org/wiki/
Layered_double_hydroxides). Hydrotalcite is one of the naturally occurring LDH
clays and the parent member of the family layered double hydroxides with the
chemical formula Mg6 Al2 (OH) 16CO3.4H2O and its name attributable to high
water content (hydro) and talc like appearance (Selvam et al., 2014; Maheskumar
et al., 2014; Mishra et al., 2018). Its existence was first declared by Hochstetter in
1842 and synthesized 100 years later by Feitknecht (Basu et al., 2014; Grosu et al.,
2018). It is most common and its structure and properties were studied extensively
and is considered as the representative of LDHs. So LDHs are also known as
hydrotalcite-like compounds (Evans and Duan, 2006).
1.2.1 Structure of layered double hydroxides

The structure of layered double hydroxides can be easily reviewed by analogizing
its structure with that of brucite which has the formula Mg (OH) 2. Brucite has
hexagonal close packing of hydroxide ions in which alternate octahedral sites are
occupied by Mg21 ions so that hydroxide layers are neutral. The neutral hydrox-
ide layers are stacked one upon the other and are held together by Vanderwaal’s
force of attraction which results in a basal spacing of about 0.48 nm. Schematic
representation of brucite structure is shown in Fig. 1.1 (Arizaga et al., 2007). It
can be imagined that the substitution of some divalent ions in brucite structure by
some trivalent ions isomorphously results in the formation of a positively charged
mixed metal hydroxide layers [M1-x II M x III (OH) 2] x1 and the intercalation of
anions in the inter layer regions counterbalance the residual positive charge on the
Layered double hydroxides: fundamentals to applications 3
Figure 1.1 Schematic representation of the brucite structure. (a) Side and (b) top view of
the layer.
Source: Adapted from Arizaga, G.G.C., Satyanarayana, K.G. and Wypych, F., 2007. Layered
hydroxide salts: synthesis, properties and potential applications. Solid State Ionics, 178
(1518), pp. 11431162. with kind permission of elsevier
Figure 1.2 Schematic representation of the structure of a generic LDH. (a) Side and (b) top
view of the layer.
Source: Adapted from Arizaga, G.G.C., Satyanarayana, K.G. and Wypych, F., 2007. Layered
hydroxide salts: synthesis, properties and potential applications. Solid State Ionics, 178
(1518), pp. 11431162. with kind permission of elsevier
metal hydroxide layers resembles layered double hydroxide structures. Water

molecules in the interlayer region bind to the metal hydroxide layers and anions
via extensive hydrogen bonding and help to stabilize the crystal structure of
layered double hydroxides. Due to the intercalation of water molecules and anions
in the inter lamellar region, the basal spacing has been increased from 0.48 nm
in brucite to about 0.77 nm in hydrotalcite (Basu et al., 2014). Schematic
representation of structure of layered double hydroxide is shown in Fig. 1.2
(Arizaga et al., 2007).
1.2.1.1 Metal cations in the layers

The metal cations both divalent and trivalent ions in the layers of LDHs are mainly
from third and fourth periods of the periodic table. The divalent metal ions that are
found commonly in the layers are Mg21, Ni21, Zn21, Co21, Fe21, Mn21, Cu21,
Ti21, Cd21, Ca21 etc and the common trivalent metal ions that are found in the
layers are Al31, Cr31, Fe31, Mn31, Ga31, V31, In31, Y31, La31, Ru31 etc.
1.2.1.2 Interlamellar anions

The generally found interlamellar anions in LDHs are halides e.g. fluoride, chloride
etc oxoanions such as carbonate, nitrate, sulphate, bromate etc, oxo and polyoxo-
metallates like chromate, dichromate, (Mo7O24) 62, (V10O28) 62etc, anionic complexes
such as ferro and ferricyanide, (PbCl4) 22 etc and organic anions like carboxylates,
phosphonates, alkyl sulphates etc.
1.2.2 Differences between Ordinary Clays and Layered Double

Hydroxides
Even though LDHs have layered crystalline structures with substitutable ions in the
interlamellar region similar to layered silicates such as montmorillonite, their chem-
ical and structural features such as composition, geometries, and layer thickness are
not identical. As already mentioned LDHs are anionic clays because of the presence
of anions in the interlamellar gallery of positively charged layers whereas reversed
structure can be observed in the case of layered silicates so the name cationic clays.
Each crystal layer in LDHs consists of single octahedral metal hydroxide sheet
whereas in layered silicates two or more sheets of metal oxides in the sandwiched
structure are observed. In montmorillonite, single crystal layer is a sandwiched sys-
tem of one octahedral sheet containing Fe, Al, and Mg between two silica tetrahe-
dral sheets. Hence crystal layer thickness and rigidity of LDHs are lower than that
of layered silicates (Basu et al., 2014; Das et al., 2008). Schematic diagram show-
ing structural and chemical difference between LDH and MMT is given in Fig. 1.3
(Das et al., 2008).
1.2.3 Synthesis Routes of Layered Double Hydroxides

A number of techniques can be applied for the synthesis of LDHs and the selection
of the method highly depends on the type of cations in the hydroxide layers, the
intercalated anions and the desired physicochemical properties such as phase purity,
crystallinity, porosity, morphology, and electronic and optical characteristics of the
final materials. The direct methods used for the synthesis of LDHs are co precipita-
tion, urea hydrolysis, salt- oxide method, sol-gel synthesis, electrochemical synthe-
sis, and in-situ film growth and the indirect method used for the synthesis of LDHs
are anion exchange, reconstruction by memory effect, and delamination followed
by restacking (Richetta et al., 2017).
Figure 1.3 Schematic diagram showing structural and chemical difference between LDH
and MMT.
Source: Adapted from Das, A., Costa, F.R., Wagenknecht, U. and Heinrich, G., 2008.
Nanocomposites based on chloroprene rubber: effect of chemical nature and organic
modification of nanoclay on the vulcanizate properties. European Polymer Journal, 44 (11),
pp. 34563465 with kind permission of elsevier
1.2.3.1 Co-Precipitation
It is the most common and useful method for the preparation of large amount of
layered double hydroxides and this method is also known as salt-base method. This
method involves the slow addition of mixed aqueous solution of salts of both diva-
lent and trivalent ions in proper proportion into water taken in a reactor and the
co-precipitation of both the metal ions from the aqueous solution by the simulta-
neous addition of dilute solutions of sodium hydroxide and/or sodium bicarbonate,
sodium carbonate, or ammonium hydroxide solution at controlled temperature and
under vigorous shaking. Generally the pH of the reaction medium is kept constant
in the range of 710, on the basis of nature of metal ions. Finally the suspension
is subjected to hydrothermal treatment to obtain well crystallized sample
(Basu et al., 2014; Richetta et al., 2017; Radulescu et al., 2008; Yan et al., 2016;
Rives et al., 2013).
1.2.3.2 Urea Hydrolysis

In this sophisticated method, an aqueous solution of the selected metal ions that
required to be present in the LDH and urea in the stoichiometric molar ratio is
heated in the temperature range from 100 C to reflux temperature for two to three
days. At the end of the process, urea hydrolyses to ammonium carbonate that leads
to the precipitation of LDH with carbonate ion as interlayer anion. This homoge-
neous precipitation method via urea hydrolysis offers LDH with high crystalline
and narrow particle size distribution (Basu et al., 2014; Radulescu et al., 2008).
1.2.3.3 Hydrothermal Crystallization

In this method, an aqueous suspension of two oxides, one of trivalent metal ion,
M2O3 and another of divalent metal ion, M2O are taken in a pressurized vessel and
subjected to hydrothermal treatment at elevated temperature for a few days. During
this process the precursor amorphous hydrated M2O3 crystallizes in the presence of
reactive basic oxide M2O which acts as the crystallizing agent (Basu et al., 2014;
Radulescu et al., 2008; Xu and Lu, 2005).
1.2.3.4 Sol-Gel Method

In this method the sol- gel transition occurs during the strong acid hydrolysis of
required metal precursors such as metal based alkoxides or acetyl acetonides in ethanol-
water system into metal hydroxides using HCl or HNO3. The heating of the mixture to
reflux with stirring should be continued until gel formation (Richetta et al., 2017).
1.2.3.5 Salt-oxide Method

This is actually a solid-liquid reaction in which aqueous solution of the chloride
salt of trivalent ion in excess is treated with an aqueous suspension of the metal (II)
oxide (Richetta et al., 2017).
1.2.3.6 Electrochemical deposition

In this method nitrate ions are reduced electrically to hydroxide ions on the working
electrode due to which local pH value increases that induces the precipitation of
LDH films. This is a good method for depositing LDH films of any desired
thickness, morphology and film density on metal substrate with good adhesion
(Richetta et al., 2017).
1.2.3.7 In-situ film growth

In this method the substrate is immersed in water solution of other metal salt and a base
is added to control the pH. Here the substrate shows dual role as a source of one of the
reacting metal ions and act as the surface for film deposition (Richetta et al., 2017).
1.2.3.8 Anion exchange

It is an indirect method widely used for preparing LDH with any desired anions in
the inter lamellar region. In actual practice, an aqueous suspension of the LDH pre-
cursors or of the pre-synthesized LDH is stirred in the presence of a large excess of
the salt of the anion to be intercalated. The anionic exchange occurring in the solu-
tion can be expressed as

M21 2 M31 2 A 1 B ! M21 2 M31 2 B 1 A
where A and B represent different anions

The exchange of the anion depends on the electrostatic forces between positively
charged LDH layers and the exchanging anions. The main criterion for anionic
exchange is that the force of attraction between the host ion and the LDH sheet
must be lower than that of guest ion and the sheet. The affinity between various
anions and the positively charged LDH sheets is in the order NO32 , Br2 , Cl2
, F2 , OH2 , MoO422 , SO422 , CrO422 , HPO422 , CO322. This method
can be used for the preparation of layered double hydroxides with any inorganic
anions or organic anions. The entire process of anion-exchange must be carried out
in an inert atmosphere (Basu et al., 2014; Selvam et al., 2014; Mishra et al., 2018;
Richetta et al., 2017; Bullo Saifullah, 2015).
1.2.3.9 Reconstruction / rehydration method

The noticeable property of LDHs is the regaining of original structure back after
subjecting it to calcination between 400500 C followed by rehydration. When
LDH is heated between 400500 C, it changes to mixed metal oxides. It is
immersed in water or any other solution of anions to be intercalated. The overall
process of rehydration must be carried out in an inert nitrogen atmosphere. This
method can also be used for the synthesis of LDH with any inorganic or organic
anions (Basu et al., 2014; Mishra et al., 2018; Richetta et al., 2017; Bullo Saifullah,
2015). Some examples for the synthesis of layered double hydroxides by various
methods are given in Table 1.1.
1.3 Organic Modification of Layered Double Hydroxides

The prime objective of organic modification of layered double hydroxides is to
enhance the interlayer spacing of LDH materials (Fig. 1.4) so as to make it eas-
ily accessible for the intercalation of large hydrophobic polymer chains. Some
important organic modifiers used for the modifications of LDHs are given in
Table 1.2 The fine tuning of the inter lamellar galleries of layered double hydro-
xides with suitable organic anions offer exfoliated layered double hydroxide
polymer nanocomposites with multifaceted applications such as biomedical,
energy, food packaging, flame retardant, gas barrier, agricultural, water purifica-
tion etc. This is also an efficient way to tailor the nano space in the intergallery
region with functional materials like pesticides, drugs, nucleic acids, enzymes
etc for vast applications such as controlled pesticides release, drug delivery,
gene delivery, biosensors etc. Organic modification can be carried out success-
fully by following any one of the important strategies such as anion exchange
reaction, reconstruction, direct synthesis and restacking (Leroux and Taviot-
Guého, 2005).
Sometimes bilayers, instead of mono layers of organic anions are formed in the
inter gallery space as a result of which basal spacing becomes double that is a
boon for producing polymer nanocomposites. This happens when the process is
carried out in the presence of excess of organic anions for a long time with
Table 1.1 Some examples for the synthesis of layered double hydroxides by various methods (Yan et al., 2016; Prince et al., 2009; Wu et al., 2014; Xie
et al., 2008; Baskaran et al., 2014; Yarger et al., 2008; Raynal et al., 2014; Liu et al., 2006a; Liu et al., 2006b).
Method of Precursors Reaction conditions Type of LDH References

Synthesis formed
Urea hydrolysis Ni (NO3) 2 6H2O NO32 /urea molar ratio of 0.25; hydrothermal treatment NiFeCO3LDH Wu et al. (2014)
Fe (NO3) 3 9H2O at 110 Cfor 24 h
Ni (NO3) 2 6H2O NO32/urea molar ratio of 3.0; hydrothermal treatment at NiFeNO3- Wu et al. (2014)
Fe (NO3) 3 9H2O 110 C for 24 h LDH
Co precipitation Co (NO3) 2 6H2O, solution1of Co21, Al31salt; solution 2 of (NH4) 2CO3 CoAlCO3LDH Baskaran et al. (2014)
Al (NO3) 3 9H2O and NH4OH; solution 2 was added dropwise to
solution1 with constant stirring at 40 C for 1 h, with
pH 8.5; washed, filtered, and dried at 80 C overnight
Mg (NO3) 2 6H2O, NaOH solution was continuously dropped into the mixed MgCoAlNO3 Xie et al. (2008)
Co (NO3) 2 6H2O, salt solution until pH 7.8; stirred for 30 min; LDH
Al (NO3) 3 9H2O hydrothermally treated at 110 C for 3 h; filtered,
washed, and then dried at 80 C for 12 h
Mg (NO3) 2 6H2O, Solution 1of NaOH and Na2CO3, and solution2 of mixed MgAlCO3 Zhao et al. (2014)
Al (NO3) 3 9H2O salt were continuously dropped. into a beaker with LDH
constant pH 9.5; aged at 100 C for 13 h; filtered,
washed, and dried at 100 C for 24 h
Sol-Gel method Mg (OEt) 2, Al (OsBu) 3 HNO3 as hydrolysis acid, temperature of 0 C, ethanol as Mg Al LDH Prince et al. (2009)
solvent, dried at 70 C for 24 h
Ni (OAc) 2, Al (Os-Bu) 3 HNO3 as hydrolysis acid, temperature of 0 C, ethanol as Ni Al LDH Prince et al. (2009)
solvent, dried at 70 Cfor 24 h
Co (OAc) 2, Ni (OAc) 2, HNO3 as hydrolysis acid, temperature of 0 C, ethanol as NiCoAl LDHs Prince et al. (2009)
Al (Os-Bu) 3 solvent, dried at 70 C for 24 h
Electro Zn (NO3) 2 6H2O Working electrodes preparation by e-beam evaporation Zn-Al NO3LDH Yarger et al. (2008)
deposition Al (NO3) 3 9H2O of 200 Å titanium and 600 Å of platinum, followed by
2000 Å gold on a cleaned glass substrate. After each
electro deposition wash the film with de ionized water
and dry with gentle stream of N2 gas. Ag/AgCl
electrode-reference electrode Pt wire counter electrode
ZnSO4 7H2O Zn21: Co21 5 2: 1 in molar ratioH2O2: Co21 55 5 1: 2 ZnCo-LDH Li et al. (2014)
CoSO4 7H2O in molar ratio. A cleaned Ni foil (1 cm 3 1 cm in films
square) -working electrode, Ag/Ag Cl electrode-
reference electrode Pt wire counter electrode
In-situ growth Al substrate dipped in Zn21 solution Zn Al LDH Liu, Jinping, et al
(2006a)
Anion CoCl2.6H2O Co-Al-CO3 LDH was synthesized by urea method by Co-Al-Cl LDH Liu, Zhaoping, et al
exchange AlCl3.6H2O mixing and refluxing 10, 5, and 35 mM solutions of Co-Al-NO3LDH (2006b)
CoCl2.6H2O, AlCl3.6H2O, and urea in 1 dm3 of Co-Al-ClO4-
deionized water for 2 days in the presence nitrogen LDH
with magnetic stirring. Treat Co-Al-CO3 LDH with
salt-acid mixed solution (NaCl-HCl) in an inert
atmosphere of nitrogen at ambient temperature.
Disperse NaCl-HCl treated LDH sample into 500 cm3
of an aqueous solution containing 0.1 M sodium
nitrate and sodium per chlorate respectively
Co (NO3) 2.6H2O Solution 1 Co (NO3) 2.6H2O (1 M) and Al (NO3) 3. CoAl-HT-Si Baskaran et al. (2014)
Al (NO3) 3. 9H2O 9H2O (0.33 M) in 2.6 L deionized H2O. Solution 2
(NH4) 2CO3 (0.67 M) and NH4OH (3.27 M) in
2.225 L deionized H2O. Add solution 2 to solution1
with constant stirring at 40 C for 1 h. Silicate
solutions of appropriate concentrations were added
slowly to the HT gel at room temperature and stirred
for 48 h. Exchange of CO322 by silicate anion
Figure 1.4 Schematic representation of ion-exchange technique.

Source: Adapted from Mishra, G., Dash, B. and Pandey, S., 2018. Layered double
hydroxides: A brief review from fundamentals to application as evolving biomaterials.
Applied Clay Science, 153, pp. 172-186 with kind permission of Elsevier
Table 1.2 Some important organic modifiers used for the modifications of LDHs (Basu
et al., 2014).
Organic Modifiers Structure Symbol

Sodium dodecyl SDBS
benzenesulfonate
Sodium dodecyl sulfate SDS
Stearic Acid SA
Oleic Acid OA
OH
Lauric acid LA
Bis (2-ethylhexyl) BEHP

hydrogen phosphoric
acid
Figure 1.5 Schematic showing the arrangement of MAPK anions in the OLDH interlayer
region. (b) TEM images and size distribution of the OLDH.
Source: Adapted from Xie, J., Wang, Z., Zhao, Q., Yang, Y., Xu, J., Waterhouse, G.I., Zhang,
K., Li, S., Jin, P. and Jin, G., 2018. Scale-up fabrication of biodegradable poly (butylene
adipate-co-terephthalate) /organophilicclay nanocomposite films for potential packaging
applications. ACS Omega, 3 (1), pp. 1187-1196 with kind permission of ACS
vigorous shaking. Xie et al. (2018) intercalated mitogen activated protein kinase
(MAPK) into the interlamellar region of Zn Al LDH by solvent free high energy
ball milling and the organically modified ZnAl-MAPK OLDH is incorporated into
PBAT matrix to form nanocomposite for food packaging applications. By carefully
analyzing the basal spacing for OLDH obtained from XRD analysis (4.07 nm), the
alkyl chain length of mitogen activated protein kinase (MAPK) (1.86 nm) and the
thickness of metal hydroxide layer (0.47 nm) in the LDH sheets, it can be obviously
concluded that bilayer of MAPK anions are formed in the interlayer space
(Fig. 1.5).
1.3.1 One step Co-precipitation

In early days, organically modified layered double hydroxides are prepared via two
step procedure. The first step is the preparation of LDH containing CO322, NO32 and
Cl2 and the second step is the exchange of these anions by organic anions. Now- a-
days, in most of the reported works, researchers merge these two steps into one and
called it as one step co- precipitation. One step co precipitation involves the slow addi-
tion of a solution of target anion into a solution containing divalent and trivalent ion.
It is noted that thermal treatment is essential to improve the crystallinity and the addi-
tion of alkali maintains the pH at the required level to achieve the co precipitation of
the two metallic salts (Mishra et al., 2018). Wang et al. (2015) extracted bio-based
modifier (cardanol-BS) from renewable resource cardanol through the ring-opening of
1, 4-butane sultone (BS). Cardanol-BS modified layered double hydroxide (m-LDH)
was prepared by one-step co- precipitation method and fabricated EP/ m-LDH
nanocomposite for flame retardant application (Scheme 1.1).
Scheme 1.1 Diagrammatic Illustration of the Synthetic Route of Cardanol-BS Modified LDH.
Source: Adapted from Wang, X., Kalali, E.N. and Wang, D.Y., 2015. Renewable cardanol-based
surfactant modified layered double hydroxide as a flame retardant for epoxy resin. ACS
Sustainable Chemistry & Engineering, 3 (12), pp. 3281-3290. with kind permission of ACS
1.3.2 Anion exchange reaction

The procedure for the anion exchange reaction implicates the dispersal of pristine
LDH into the aqueous solution of the anionic surfactant that has to be introduced
into the inter lamellar galleries so as to replace the existing anion to produce the
organically modified LDHs, with constant stirring at room temperature for several
hours (Basu et al., 2014). Anion exchange plays a major role in the widespread
applications of layered double hydroxides and their composites as this method is
the principal step for introducing functional anions in the interlamellar region, pil-
laring and delamination.
1.3.3 Memory Effect or Regeneration Method

It is the widely accepted method for the modification of layered double hydroxides
in which heating of LDH in a Muffle furnace at 450 C for 3 hours leads to the for-
mation of amorphous mixed metal oxide. The mixed oxide is dispersed into water
containing anionic surfactant which is to be introduced into the inter lamellar gal-
leries of LDH and kept for 24 hours with constant magnetic stirring. During this
stirring carbonate anions already present in the inter lamellar galleries are replaced
by the organic anions and the material memorize its original structure so the name
3 hours @ 450°C
Calcination in a
Unmodified LDH Mixed oxide
muffle furnace
Centrifuging Stirring for

and drying @ 24 hours at
60°C to a ambient
constant weight temperature
Modified LDH Addition of mixed oxide Dispersion into aq.
as solid residue into a specific volume solution of the
of a surfactant solution desired surfactant
(0.1–0.2 M)
Figure 1.6 A simplified schematic showing the synthesis route to obtain modified LDH
from unmodified LDH.
Source: Adapted from Basu, D., Das, A., Stöckelhuber, K.W., Wagenknecht, U. and Heinrich,
G., 2014. Advances in layered double hydroxide (LDH) -based elastomer composites.
Progress in Polymer Science, 39 (3), pp. 594-626 with kind permission of elsevier
Figure 1.7 Mg/Al LDH loaded with 5-fluorouracil (5-FU) via memory effect.
Source: Adapted from Peng, F., Wang, D., Cao, H. and Liu, X., 2018. Loading
5-Fluorouracil into calcined Mg/Al layered double hydroxide on AZ31 via memory effect.
Materials Letters, 213, pp. 383-386 with kind permission of elsevier
memory effect (Basu et al., 2014) (Fig. 1.6). Peng et al. (2018a) successfully inter-
calated anticancer drug 5-Fluorouracil in the intergallery space of Mg/Al LDH via
memory effect for drug delivery applications. Mg/Al LDH prepared in-situ by a
hydrothermal process and the original layered structure is recovered by adding cal-
cined LDH into a solution containing anticancer drug molecules 5-Fluorouracil
(Fig. 1.7).
1.3.4 The delamination/restacking method

In this method, the complete separation of LDHs into single sheets by using
suitable solvent so that a stable colloidal suspension is obtained. The aqueous
Figure 1.8 Schematic illustration of the preparation process for metalloporphyrin
intercalated LDH nanocomposites via the exfoliation/ restacking route.
solution of organic anion is added to this colloidal solution in an inert atmosphere

of nitrogen. Then the colloidal solution is subjected to drying, well-ordered LDHs
intercalated with desired anions are obtained (Richetta et al., 2017). Ma et al.
(2014) intercalated metalloporphyrin into the intergallery space of Ni-Al LDH and
Mg-Al LDH by delamination /restacking method. The prepared LDH-CO3 is con-
verted into LDH-NO3 by direct salt-acid method. It is delaminated by shaking with
formamide and aqueous solution of metalloporphyrin is added to this
colloidal solution in the presence of an inert atmosphere of nitrogen (Fig. 1.8)
(Ma et al., 2014).
1.4 Characterization of layered double hydroxides and

modified layered double hydroxides
The success of synthesis of LDHs and modification of LDHs can be evaluated by
the characterization techniques such as SEM, TEM, AFM, XRD, FTIR, EDS,
Raman spectroscopy and X-ray photoelectron spectroscopy and thermo gravimetric
analysis. The sharp reflections corresponding to the (00n) planes in the powder
X-ray diffraction patterns confirm the formation of LDH crystals and shifting of
the typical and characteristic Bragg reflections in the diffraction pattern confirm
the successful organic modification of the layered double hydroxides. The basal
spacing of LDH and modified LDH can be calculated from the 2θ value corre-
sponding to the first-order basal plane reflection by using Bragg’s equation. The
shifting of the first-order basal plane reflection towards higher d-values or lower
2θ values indicates the successful intercalation of organic anions into the inter
lamellar gallery of layered double hydroxides. XRD analysis goes into the in-depth
study of the crystal by providing the unit cell parameters, miller indices crystallite
size or particle size (calculated with the help of Scherrer equation) etc. SEM and
TEM give valuable information regarding the size and shape of the LDHs and
modified LDHs. The chemical compositions of the LDHs and modified LDHs are
determined by energy-dispersive X-ray spectra (EDS). The thickness of LDHs and
modified LDHs can be detected from the AFM height images and the correspond-
ing height profiles. The FTIR spectrum confirms the formation of LDH by provid-
ing peaks corresponding to interlayer anion, interlayer water molecules, O-H of
metal hydroxide layer, M-O lattice etc (Nagendra et al., 2017a; Nagendra et al.,
2015; Nagendra et al., 2017b). The increase in basal spacing obtained from XRD
and the characteristic peak corresponding to the organic modifier from the FTIR
spectrum and visualization of increase in basal spacing by taking the image by
high resolution TEM etc indicates the successful modification of layered double
hydroxides with the organic modifiers. Some of the characterization techniques are
illustrated here with suitable examples, which are taken from some previously
reported research work, for the better understanding of this topic.
Nagendra et al (2017b) synthesized Co 2 Al, Zn 2 Al LDH and Co 2 Zn 2 Al
LDH by co precipitation method. The size and shape of these LDHs were character-
ized by SEM and TEM analysis and visualized as circular platelets, hexagonal
platelets with rounded edges, and hexagonal platelets with sharp edges morpholo-
gies respectively for Co 2 Al LDH, Zn 2 Al LDH, and Co 2 Zn 2 Al LDH
(Fig. 1.9). This difference in shape is attributed to the difference in nucleation and
growth mechanism of LDH in the presence of different metal salts. The crystallinity
was confirmed by XRD and the prepared LDH crystals are found to be highly pure
as there were no peaks other than typical LDH (Fig. 1.10a). Because of water mole-
cules in the interlamellar region and hydroxyl groups in the LDH layers, a dominant
oxygen peak was observed in EDS of different LDH. (Fig. 1.9) The FTIR bands at
1356 and1382 cm21 indicated the presence of carbonate and nitrate respectively,
the bands at 3440 cm21 (ν (O-H) ) and 1632 cm21 (δ (H2O) ) indicated the pres-
ence of water molecules in the inter lamellar region (Fig. 1.10b).
Xu et al. (2013b) synthesized LDH-CO3 by urea method and converted it to
LDH-NO3 by an acidsalt direct exchange method. The reason for the conversion
is that it is difficult to substitute interlayer CO322 anions by organic anions directly,
because of high electrostatic attraction between CO322 and LDH platelets. After the
first conversion, LDH NO3 was again converted to LDH-DS and LDH -DBS by
anion exchange reaction. From the XRD data, it is clear that the basal space of
LDH-NO3, LDH-DS, and LDH-DBS are 0.88 nm, 2.78 and 2.96 nm respectively
which are found to be well agreement with the theoretical values (Fig. 1.11 and
Fig. 1.12). The characteristic reflection peak of LDH-CO3 corresponding to
2θ 5 11.8 is absent in XRD graphs of all the other LDHs mentioned above which
indicates complete conversion of CO322. XRD data of unmodified and some organ-
ically modified LDHs are given in Table 1.3. In addition to that, the characteristic
absorption band of the carbonate at around 1352 cm21 was not observed in the
Figure 1.9 SEM, TEM, and EDS analysis of the as-synthesized LDH: (a) Co 2 Al LDH,
(b) Zn 2 Al LDH, and (c) Co 2 Zn 2 Al LDH.
Source: Adapted from Nagendra, B., Rosely, C.S., Leuteritz, A., Reuter, U. and Gowd, E.B.,
2017. Polypropylene/layered double hydroxide nanocomposites: Influence of LDH intralayer
metal constituents on the properties of polypropylene. ACS Omega, 2 (1), pp. 20-31 with
kind permission of ACS
Figure 1.10 (a) Powder XRD patterns and (b) FTIR spectra of as-prepared Co 2 Al LDH,
Zn 2 Al LDH, and Co 2 Zn 2 Al LDH.
Source: Nagendra, B., Rosely, C.S., Leuteritz, A., Reuter, U. and Gowd, E.B., 2017.
Polypropylene/layered double hydroxide nanocomposites: Influence of LDH intralayer metal
constituents on the properties of polypropylene. ACS Omega, 2 (1), pp. 20-31 with kind
permission of ACS
Figure 1.11 Schematic diagrams showing the theoretical calculation results of the anion
alignments in the interlayer of LDH-DS (a) and LDH-DBS (b).
Source: Adapted from Xu, K., Chen, G. and Shen, J., 2013. Exfoliation and dispersion of
micrometer-sized LDH particles in poly (ethylene terephthalate) and their nanocomposite
thermal stability. Applied Clay Science, 75, pp. 114-119 with kind permission of Elsevier
Figure 1.12 XRD patterns of the LDH-NO3, LDH-DS and LDH-DBS samples.
Source: Adapted from Xu, K., Chen, G. and Shen, J., 2013. Exfoliation and dispersion of
micrometer-sized LDH particles in poly (ethylene terephthalate) and their nanocomposite
thermal stability. Applied Clay Science, 75, pp. 114-119. with kind permission of elsevier
Table 1.3 XRD data of unmodified and some organically modified LDHs
(Basu et al., 2014; Xu et al., 2013b; Costa et al., 2008; Liu et al., 2008;
Manzi-Nshuti et al., 2009).
Type of LDH Basal spacing (nm)

LDH NO3 0.89
LDH-DS 2.78
LDH- DBS 2.96
LDH-laurate 2.45
LDH-oleate 3.4
LDH-stearate 3.37
LDH-BEHP (Bis (2-ethylhexyl) hydrogen 1.52
3phosphate-modified LDH)
FTIR spectrum of LDH-NO3, LDH-DS, and LDH-DBS. At the same time, some
new peaks were observed at 1384 cm21, 2957, 2920 and 2845 cm21. The first peak
arises due to the stretching mode of NO32 and the three other peaks arises as a
result of asymmetric and symmetric stretching vibrations of CH3/CH2 group of long
alkyl chains of the DS and DBS anions. Some additional bands were observed at
1220 cm21, 1200 and 1042 cm21, 1133 and 1011 cm21, first band results from the
DS anions, a couple of bands (second and third) characteristic of the DBS absorption
and the next pair of bands (fourth and fifth) characteristic of the C-H aromatic in-plane
bendings of the LDH-DBS. In addition to all these bands, a broad absorption band
appeared between 3700 and 3000 cm21 can be assigned to the O-H group stretching
(Fig. 1.13). FTIR bands of some organically modified LDHs are given in Table 1.4.
The information obtained from thermo gravimetric analysis of various types of
LDHs reported in literature is that thermal stability of layered double hydroxides is
only up to 200 C and above that temperature it decomposes to amorphous mixed
metal oxides. Yang et al. (2002) conducted several in situ techniques such as
DRIFTS, TG/DTA, MS, and HTXRD to detect the thermal evolution of the struc-
ture of an MgAlCO3 layered double hydroxide (LDH) under an inert atmo-
sphere (Fig. 1.14). The diffuse reflectance infrared Fourier transform spectroscopy
(DRIFTS) helped to determine the changes in the functional groups. TG/DTA
investigate the changes in mass and energy changes (Fig. 1.15), MS identifies the
products liberated during each stage of heating and HTXRD monitors the structure
evolution. A model has been proposed on the basis of the study to describe the
structural evolution of the MgAlCO3 LDH. In this model, the conversion of lay-
ered double hydroxides into mixed metal oxides is divided into four stages. In the
first stage, between 70190 C, removal of interlayer water takes place and a
change from Phase I with a basal spacing ranging from 7.5 to 7.3 A to Phase II
with basal spacing of 6.6 A which indicates that no change in the LDH tactoid
structure. In stage 2, between 190280 C, the OH2 group bonded to Al31 disap-
pears, in the third stage, between190280 C, the OH 2 group linked to
Mg21disappears and in the final stage, between 405580 C, loss of CO322 takes
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in their footsteps exactly when returning in the dark. He added:
“There never has been an accident happen to anybody from my
house, and I should feel real mean if one did: but there have been a
power of narrow escapes.”
First of all we descended the precipice, 300 feet in depth, forming
the wall of the old crater, but now thickly covered with vegetation. It
is so steep in many places that flights of zigzag wooden steps have
been inserted in the face of the cliff in some places, in order to
render the descent practicable. At the bottom we stepped straight on
to the surface of cold boiled lava, which we had seen from above last
night. Even here, in every crevice where a few grains of soil had
collected, delicate little ferns might be seen struggling for life, and
thrusting out their green fronds towards the light. It was the most
extraordinary walk imaginable over that vast plain of lava, twisted
and distorted into every conceivable shape and form, according to
the temperature it had originally attained, and the rapidity with which
it had cooled, its surface, like half-molten glass, cracking and
breaking beneath our feet. Sometimes we came to a patch that
looked like the contents of a pot, suddenly petrified in the act of
boiling; sometimes the black iridescent lava had assumed the form
of waves, or more frequently of huge masses of rope, twisted and
coiled together; sometimes it was piled up like a collection of organ-
pipes, or had gathered into mounds and cones of various
dimensions. As we proceeded the lava became hotter and hotter,
and from every crack arose gaseous fumes, affecting our noses and
throats in a painful manner; till at last, when we had to pass to
leeward of the molten stream flowing from the lake, the vapours
almost choked us, and it was with difficulty we continued to advance.
The lava was more glassy and transparent-looking, as if it had been
fused at a higher temperature than usual; and the crystals of sulphur,
alum, and other minerals, with which it abounded, reflected the light
in bright prismatic colours. In places it was quite transparent, and we
could see beneath it the long streaks of a stringy kind of lava, like
brown spun glass, called “Pélé’s hair.”
LAVA CASCADE FLOW.
At last we reached the foot of the present crater, and commenced
the ascent of the outer wall. Many times the thin crust gave way
beneath our guide, and he had to retire quickly from the hot, blinding,
choking fumes that immediately burst forth. But we succeeded in
reaching the top; and then what a sight presented itself to our
astonished eyes! I could neither speak nor move at first, but could
only stand and gaze at the terrible grandeur of the scene.
We were standing on the extreme edge of the precipice,
overhanging a lake of molten fire, a hundred feet below us, and
nearly a mile across. Dashing against the cliffs on the opposite side,
with a noise like the roar of a stormy ocean, waves of blood-red,
fiery, liquid lava hurled their billows upon an iron-bound headland,
and then rushed up the face of the cliffs to toss their gory spray high
in the air. The restless, heaving lake boiled and bubbled, never
remaining the same for two minutes together. Its normal colour
seemed to be a dull, dark red, covered with a thin grey scum, which
every moment and in every part swelled and cracked, and emitted
fountains, cascades, and whirlpools of yellow and red fire, while
sometimes one big golden river, sometimes four or five flowed
across it. There was an island on one side of the lake, which the fiery
waves seemed to attack unceasingly with relentless fury, as if bent
on hurling it from its base. On the other side was a large cavern, into
which the burning mass rushed with a loud roar, breaking down in its
impetuous headlong career the gigantic stalactites that overhung the
mouth of the cave, and flinging up the liquid material for the
formation of fresh ones.
It was all terribly grand, magnificently sublime; but no words could
adequately describe such a scene. The precipice on which we were
standing overhung the crater so much that it was impossible to see
what was going on immediately beneath; but from the columns of
smoke and vapour that arose, the flames and sparks that constantly
drove us back from the edge, it was easy to imagine that there must
have been two or three grand fiery fountains below. As the sun set,
and the darkness enveloped the scene, it became more awful than
ever. We retired a little way from the brink, to breathe some fresh air,
and to try and eat the food we had brought with us; but this was an
impossibility. Every instant a fresh explosion or glare made us jump
up to survey the stupendous scene. The violent struggles of the lava
to escape from its fiery bed, and the loud and awful noises by which
they were at times accompanied, suggested the idea that some
imprisoned monsters were trying to release themselves from their
bondage with shrieks and groans, and cries of agony and despair, at
the futility of their efforts.
Sometimes there were at least seven spots on the borders of the
lake where the molten lava dashed up furiously against the rocks—
seven fire-fountains playing simultaneously. With the increasing
darkness the colours emitted by the glowing mass became more and
more wonderful, varying from the deepest jet-black to the palest
grey, from darkest maroon through cherry and scarlet to the most
delicate pink, violet, and blue; from the richest brown, through
orange and yellow, to the lightest straw-colour. And there was yet
another shade, only describable by the term “molten-lava colour.”
Even the smokes and vapours were rendered beautiful by their
borrowed lights and tints, and the black peaks, pinnacles, and crags,
which surrounded the amphitheatre, formed a splendid and
appropriate background. Sometimes great pieces broke off and
tumbled with a crash into the burning lake, only to be remelted and
thrown up anew. I had for some time been feeling very hot and
uncomfortable, and on looking round the cause was at once
apparent. Not two inches beneath the surface, the grey lava on
which we were standing and sitting was red-hot. A stick thrust
through it caught fire, a piece of paper was immediately destroyed,
and the gentlemen found the heat from the crevices so great that
they could not approach near enough to light their pipes.
One more last look, and then we turned our faces away from the
scene that had enthralled us for so many hours. The whole of the
lava we had crossed, in the extinct crater, was now aglow in many
patches, and in all directions flames were bursting forth, fresh lava
was flowing, and smoke and steam were issuing from the surface. It
was a toilsome journey back again, walking as we did in single file,
and obeying the strict injunctions of our head guide to follow him
closely, and to tread exactly in his footsteps. On the whole it was
easier by night than by day to distinguish the route to be taken, as
we could now see the dangers that before we could only feel; and
many were the fiery crevices we stepped over or jumped across.
Once I slipped, and my foot sank through the thin crust. Sparks
issued from the ground, and the stick on which I leaned caught fire
before I could fairly recover myself.
Monday, December 25th, (Christmas Day).

Turning in last night was the work of a very few minutes, and this
morning I awoke perfectly refreshed and ready to appreciate anew
the wonders of the prospect that met my eyes. The pillar of fire was
still distinctly visible, when I looked out from my window, though it
was not so bright as when I had last seen it: but even as I looked it
began to fade, and gradually disappeared. At the same moment a
river of glowing lava issued from the side of the bank which we had
climbed with so much difficulty yesterday, and slowly but surely
overflowed the ground we had walked over. I woke Tom, and you
may imagine the feelings with which we gazed upon this startling
phenomenon, which, had it occurred a few hours earlier, might have
caused the destruction of the whole party.
A Voyage in the Sunbeam (London, 1878).
TROLLHÄTTA
HANS CHRISTIAN ANDERSEN
Whom did we meet at Trollhätta? It is a strange story. We will relate
it.
We landed at the first sluice and immediately stood in a kind of
English garden; the broad pathways are covered with gravel and rise
in low terraces between the green sunlit greensward. It is charming
and delightful here, but by no means imposing; if one desires to be
excited in this manner, he must go a little higher up to the old sluices,
that have burst, deep and narrow, through the hard rock. Nature is
magnificent here, and the water roars and foams in its deep bed far
below. Up here one looks over valley and river; the bank of the river
on the other side rises in green undulating hills, with clusters of leafy
trees and wooden houses painted red; rocks and pine forests hem in
the landscape. Through the sluices steamboats and sailing vessels
are ascending; the water itself is the attendant spirit that must bear
them up above the rock. And from the forest it issues, buzzing,
roaring, and blustering. The din of the Trollhätta Falls mingles with
the noise of the sawmills and the smithies.
“In three hours we shall be through the sluices,” said the Captain,
“and then you shall visit the Falls. We shall meet again at the inn
above.”
We went along the path that led through the forest and thickets; a
whole flock of bare-headed boys surrounded us, all wishing to be our
guides; each one outscreamed the other, and each gave
contradictory explanations of how high was the water and how high it
did not or could rise; and here was also a great difference of opinion
among the learned. Soon we came to a halt on a large heather-
covered rock, a dizzying eminence. Before us, but deep below, the
foaming, roaring water—the Hell Fall, and over this, cascade after
cascade, the rich, swelling, rushing river, the outlet of the largest lake
in Sweden. What a sight, what a foaming above and below! It is like
the waves of the sea, or like effervescing champagne, or like boiling
milk; the water rushes around two rocky islands above so that the
spray rises like mist from a meadow, while below, it is more
compressed, and, hurrying away, returns in circles; then it rolls down
in a long wave-like fall, the Hell Fall. What a roaring storm in the
deep—what a spectacle! Man is dumb. And so were also the
screaming little guides; they were silent, and when they renewed
their explanations and stories, they did not get far before an old
gentleman, whom none of us had noticed, although he was here
among us, made himself heard above the noise with his peculiarly
shrill voice; he spoke of the place and its former days as if they had
been of yesterday.
“Here on the rocky isles,” said he, “here in olden times the warriors,
as they are called, decided their disputes. The warrior, Stärkodder,
dwelt in this region, and took a fancy to the pretty maid Ogn; but she
fancied Hergrimer the more, and in consequence he was challenged
by Stärkodder to a duel here by the Falls and met his death; but Ogn
sprang towards them, and, seizing her lover’s bloody sword, thrust it
into her heart. Stärkodder did not get her. So a hundred years
passed and another hundred; the forest became heavy and thick,
wolves and bears prowled here summer and winter, and wicked
robbers hid their booty here and no one could find them; yonder, by
the Fall before Top Island, on the Norwegian side, was their cave;
now it has fallen in—the cliff there overhangs it!”
“Yes, the Tailors’ Cliff!” screamed all the boys. “It fell in the year
1755!”
“Fell!” cried the old man as if astonished that any one could know of
it but himself. “Everything will fall: the tailor also fell. The robbers
placed him upon the cliff and told him that if he would be liberated for
his ransom he must sew a suit of clothes there; he tried to do it, but
as he drew out his thread at the first stitch, he became dizzy and fell
into the roaring water, and thus the rock got the name of The Tailors’
Cliff. One day the robbers caught a young girl, and she betrayed
them; she kindled a fire in the cavern, the smoke was seen, the
cavern was discovered, and the robbers imprisoned and executed;
that outside there is called The Thieves’ Fall, and below, under the
water, is another cave; the river rushes in there and issues out
foaming; you can see it well up here and hear it too, but it can be
heard better under the stony roof of the mountain sprite.”
And we went on and on along the waterfall towards Top Island,
always on smooth paths covered with saw-dust to Polhelm’s-Sluice;
a cleft has been made in the rock for the first intended sluice-work,
which was not finished, but on account of which has been shaped
the most imposing of all the Trollhätta Falls; the hurrying water falls
perpendicularly into the dark depth. The side of the rock here is
connected with Top Island by means of a light iron bridge, which
seems to be thrown over the abyss; we venture on this swaying
bridge above the rushing, whirling water, and soon stand on the little
rocky island between firs and pines that dart out of the crevices;
before us rushes a sea of waves, broken as they rebound against
the rock on which we stand, spraying us with their fine eternal mist;
on each side the torrent flows as if shot from a gigantic cannon,
waterfall upon waterfall; we look above them all and are lulled by the
harmonic tone that has existed for thousands of years.
“No one can ever get to that island over there,” said one of our party,
pointing to the large island above the highest fall.
“I know one who got there!” exclaimed the old man, and nodded with
a peculiar smile.
“Yes, my grandfather got there!” said one of the boys, “but for a
hundred years scarcely any one else has reached it. The cross that
stands there was set up by my grandfather. It had been a severe
winter, the whole of Lake Venern was frozen, the ice dammed up the
outlet, and for many hours the bottom was dry. Grandfather has told
us about it: he and two others went over, set up the cross, and
returned. Just then there was a thundering and cracking noise just
like cannon, the ice broke up and the stream overflowed meadows
and forest. It is true, every word I say!”
TROLLHÄTTA.
One of the travellers cited Tegner:
“Vildt Göta stortade fran Fjallen,

Hemsk Trollet fran sat Toppfall röt!
Men Snillet kom och sprängt stod Hallen,
Med Skeppen i sitt sköt!”
“Poor mountain sprite,” he added, “thy power and glory are failing!
Man flies beyond thee—Thou must learn of him!”
The garrulous old man made a grimace, and muttered something to
himself—but we were now by the bridge before the inn, the
steamboat glided through the open way, every one hurried on board
and immediately it shot above the Fall just as if no Fall existed.
It was evening; I stood on the heights of Trollhätta’s old sluices, and
saw the ships with outspread sails glide away over the meadows like
large white spectres. The sluice-gates opened with a heavy, crashing
sound like that related of the copper gates of the Vehmgericht; the
evening was so still; in the deep silence the tone of the Trollhätta Fall
was like a chorus of a hundred water-mills, ever one and the same
tone and sometimes the ringing of a deep and mighty note that
seemed to pass through the very earth—and yet through all this the
eternal silence of Nature was felt;—suddenly a great bird with
heavily flapping wings flew out of the trees in the deep woods
towards the waterfall. Was it the mountain sprite? We must believe
so.
Pictures of Sweden (Leipzig, 1851).
THE GRAND CANYON OF THE
COLORADO
(UNITED STATES)
C. F. GORDON-CUMMING
Probably the greatest chasm in the known world is the grand canyon
of the Colorado river (the Rio Colorado Grande), which is a gorge
upward of two hundred miles in length, and of tremendous depth.
Throughout this distance its vertical crags measure from one to
upwards of six thousand feet in depth! Think of it! The highest
mountain in Scotland measures 4,418 feet. The height of Niagara is
145 feet. And here is a narrow, tortuous pass where the river has
eaten its way to a depth of 6,200 feet between vertical granite crags!
Throughout this canyon there is no cascade; and though the river
descends 16,000 feet within a very short distance, forming rushing
rapids, it is nevertheless possible to descend it by a raft—and this
has actually been done, in defiance of the most appalling dangers
and hardships. It is such a perilous adventure as to be deemed
worthy of note even in this country, where every prospector carries
his life in his hand, and to whom danger is the seasoning of daily life,
which, without it, would appear positively monotonous.
I suppose no river in the world passes through scenery so
extraordinary as does the Colorado river, in its journey of 2,000 miles
from its birthplace in the Rocky mountains, till, traversing the burning
plains of New Mexico, it ends its course in the Gulf of California. Its
early career is uneventful. In its youth it bears a maiden name, and,
as the Green river, wends it way joyously through the upper forests.
Then it reaches that ghastly country known as the mauvaises terres
of Utah and Arizona—a vast region—extending also into Nevada
and Wyoming, which, by the ceaseless action of water, has been
carried into an intricate labyrinth of deep gloomy caverns.
For a distance of one thousand miles the river winds its tortuous
course through these stupendous granite gorges, receiving the
waters of many tributary streams, each rushing along similar deeply
hewn channels.
In all the range of fiction no adventures can be devised more terrible
than those which have actually befallen gold-seekers and hunters
who, from any cause, have strayed into this dreary and awesome
region. It was first discovered by two bold explorers, by name Strobe
and White, who, being attacked by Indians, took refuge in the
canyons. Preferring to face unknown dangers to certain death at the
hands of the enemy, they managed to collect enough timber to
construct a rude raft, and determined to attempt the descent.
Once embarked on that awful journey, there was no returning—they
must endure to the bitter end.
On the fourth day the raft was upset. Strobe was drowned, and the
little store of provisions and ammunition was lost. White contrived to
right the raft, and for ten days the rushing waters bore him down the
frightful chasm, seeing only the perpendicular cliffs on either side,
and the strip of sky far overheard—never knowing, from hour to hour,
but that at the next winding of the canyon the stream might overleap
some mighty precipice, and so end his long anguish. During those
awful ten days of famine, a few leaves and seed-pods, clutched from
the bushes on the rocks, were his only food.
At length he reached a wretched settlement of half-bred Mexicans,
who, deeming his escape miraculous, fed him; and eventually he
reached the homes of white men, who looked on him (as well they
might) as on one returned from the grave. The life thus wonderfully
saved, was, however, sacrificed a few months later, when he fell into
the hands of his old Indian foes.
The story of White’s adventure was confirmed by various trappers
and prospectors, who, from time to time, ventured some little way
into this mysterious rock-labyrinth; and it was determined to attempt
a government survey of the region. Accordingly, in 1869, a party,
commanded by Major J. W. Powell, started on this most interesting
but dangerous expedition. Warned by the fate of a party who
attempted to explore the country in 1855, and who, with the
exception of two men (Ashley and another), all perished miserably,
the government party started with all possible precautions.
THE GRAND CAÑON OF THE COLORADO.
Four light Chicago-built boats were provisioned for six months, and,
with infinite difficulty, were transported 1,500 miles across the desert.
On reaching their starting-point, they were lowered into the awful
ravines, from which it was, to say the least, problematic whether all
would emerge alive. The dangers, great enough in reality, had been
magnified by rumour. It was reported, with every semblance of
probability, that the river formed terrible whirlpools—that it flowed
underground for hundreds of miles, and emerged only to fall in
mighty cataracts and appalling rapids. Even the friendly Indians
entreated the explorers not to attempt so rash an enterprise,
assuring them that none who embarked on that stream would
escape alive.
But in the face of all such counsel, the expedition started, and for
upwards of three months the party travelled, one may almost say in
the bowels of the earth—at least in her deepest furrows—through
canyons where the cliffs rise, sheer from the water, to a height of
three-quarters of a mile!
They found, as was only natural, that imagination had exaggerated
the horrors of the situation, and that it was possible to follow the
rock-girt course of the Colorado through all its wanderings—not
without danger, of course. In many places the boat had to be carried.
One was totally wrecked and its cargo lost, and the others came to
partial grief, entailing the loss of valuable instruments, and almost
more precious lives. Though no subterranean passage was
discovered, nor any actual waterfall, there were, nevertheless, such
dangerous rapids as to necessitate frequent troublesome portage;
and altogether, the expedition had its full share of adventure.
The ground was found to vary considerably. In some places the rock
is so vivid in colour—red and orange—that the canyons were
distinguished as the Red Canyon and the Flaming Gorge. Some are
mere fissures of tremendous depth; while in other places, where the
water has carved its way more freely, they are broad, here and there
expanding into a fertile oasis, where green turf and lovely groves are
enclosed by stupendous crags—miniature Yosemites—which to
these travellers appeared to be indeed visions of Paradise.
Granite Crags (Edinburgh and London, 1884).
THE ROCK OF GIBRALTAR
(SPAIN)
AUGUSTUS J. C. HARE
It was a lovely day, and a calm sea, which was a great subject of
rejoicing, for even as it was the rickety Spanish vessel rolled
disagreeably. Owing to the miserable slowness of everything, we
were eleven hours on board. There was little interest till we reached
the yellow headland of Trafalgar. Then the rugged outlines of the
African coast rose before us, and we entered the straits, between
Tarifa sleeping amid its orange groves on the Spanish coast, and the
fine African peak above Ceuta. Soon, on the left, the great rock of
Gibraltar rose from the sea like an island, though not the most
precipitous side, which turns inwards towards the Mediterranean. But
it was already gun-fire, and too late to join another steamer and land
at the town, so we waited for a shoal of small boats which put out
from Algeciras, and surrounded our steamer to carry us on shore.
Here we found in the Fonda Inglesa (kept by an English landlady),
one of the most primitive but charming little hotels we ever entered.
The view from our rooms alone decided us to stay there some days.
Hence, framed by the balcony, Gibraltar rose before us in all the
glory of its rugged sharp-edged cliffs, grey in the morning, pink in the
evening light, with the town at its foot, whence, at night, thousands of
lights were reflected on the still water. In the foreground were groups
of fishing-boats at anchor, and, here and there, a lateen sail flitted,
like a white albatross, across the bay. On the little pier beneath us
was endless life and movement, knots of fishermen, in their blue
shirts and scarlet caps and sashes, mingling with solemn-looking
Moors in turbans, yellow slippers, and flowing burnouses, who were
watching the arrival or embarcation of their wares; and an endless
variety of travellers from all parts of Europe, waiting for different
steamers, or come over to see the place. Here an invalid might stay,
imbibing health from the fine air and sunshine, and never be weary
of the ever changing diorama. In every direction delightful walks wind
along the cliffs through groves of aloes and prickly-pear, or descend
into little sandy coves full of beautiful shells. Behind the town, a fine
old aqueduct strides across the valley, and beyond it the wild moors
begin at once sweeping backwards to a rugged chain of mountains.
Into the gorges of these mountains we rode one day, and most
delightful they are, clothed in parts with magnificent old cork-trees,
while in the depths of a ravine, overhung with oleander and
rhododendron, is a beautiful waterfall.
THE ROCK OF GIBRALTAR.

It was with real regret that we left Algeciras and made the short
voyage across the bay to Gibraltar, where we instantly found
ourselves in a place as unlike Spain as it is possible to imagine.
Upon the wharf you are assailed by a clamour of English-speaking
porters and boatmen. Passing the gates, you come upon a barrack-
yard swarming with tall British soldiers, looking wonderfully bright
and handsome, after the insignificant figures and soiled, shabby
uniforms of the Spanish army. Hence the Waterport Street opens,
the principal thoroughfare of the town, though from its insignificant
shops, with English names, and its low public-houses, you have to
look up at the strip of bright blue sky above, to be reminded that you
are not in an English seaport.
Just outside the principal town, between it and the suburb of Europe,
is the truly beautiful Alameda, an immense artificial garden, where
endless gravel paths wind through labyrinths of geraniums and
coronella and banks of flame-coloured ixia, which are all in their full
blaze of beauty under the March sun, though the heat causes them
to wither and droop before May. During our stay at Gibraltar, it has
never ceased to surprise us that this Alameda, the shadiest and
pleasantest place open to the public upon the Rock, should be
almost deserted; but so it is. Even when the band playing affords an
additional attraction, there are not a dozen persons to listen to it;
whereas at Rome on such occasions, the Pincio, exceedingly inferior
as a public garden, would be crowded to suffocation, and always
presents a lively and animated scene.
One succession of gardens occupies the western base of the Rock,
and most luxuriant and gigantic are the flowers that bloom in them.
Castor-oil plants, daturas, and daphnes, here attain the dignity of
timber, while geraniums and heliotropes many years old, so large as
to destroy all the sense of floral proportions which has hitherto
existed in your mind. It is a curious characteristic, and typical of
Gibraltar, that the mouth of a cannon is frequently found protruding
from a thicket of flowers.
The eastern side of the Rock, in great part a perpendicular precipice,
is elsewhere left uncultivated, and is wild and striking in the highest
degree. Here, beyond the quaint Jewish cemetery of closely set
gravestones, bearing Hebrew inscriptions on the open hillside, a
rugged path winds through rocks and tangled masses of flowers and
palmists, to a curious stalactitic cavern called Martin’s Cave. On this
side of the cliff a remnant of the famous “apes of Tarshish” is
suffered to remain wild and unmolested, though their numbers,
always very small, have lately been reduced by the very ignorant
folly of a young officer, who shot one and wounded nine others, for
which he has been very properly impounded.
On the northern side of the Rock are the famous galleries tunnelled
in the face of the precipice, with cannon pointing towards Spain from
their embrasures. Through these, or, better, by delightful paths,
fringed with palmettos and asphodel, you may reach El Hacho, the
signal station, whence the view is truly magnificent over the sea, and
the mountain chains of two continents, and down into the blue
abysses beneath the tremendous precipice upon which it is placed.
THE ROCK OF GIBRALTAR.

The greatest drawback to the charms of Gibraltar has seemed to be
the difficulty of leaving it. It is a beautiful prison. We came fully
intending to ride over the mountain passes by Ronda, but on arriving
we heard that the whole of that district was in the hands of the
brigands under the famous chief Don Diego, and the Governor
positively refused to permit us to go that way. Our lamentations at

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Layered double hydroxide polymer

Graphene to Polymer/ Graphene Nanocomposites. Emerging

New Polymer Nanocomposites for Environmental

Silica and Clay Dispersed Polymer Nanocomposites :

Enhanced adsorption of bromate from aqueous solutions

Layered 2D Materials And Their Allied Application

Metal oxide glass nanocomposites Sanjib Bhattacharya

Green Micro and Nanocomposites Thomas S.

Applications of Polymer Nanofibers Anthony L. Andrady

Copyright © 2020 Elsevier Ltd. All rights reserved.

British Library Cataloguing-in-Publication Data

Library of Congress Cataloging-in-Publication Data

ISBN: 978-0-08-102261-0 (print)

ISBN: 978-0-08-101904-7 (online)

For information on all Woodhead Publishing publications

Publisher: Matthew Deans

Typeset by MPS Limited, Chennai, India

List of contributors xvii

1. Layered double hydroxides: fundamentals to applications 1

2. FTIR characterization of layered double hydroxides and modified

3. Fabrication technologies of layered double hydroxide polymer

3.3.2 Preparation of pectin/layered double hydroxide

4. Microscopic characterization techniques for layered double

5. X-ray diffraction analysis of layered double hydroxide polymer

6. Spectroscopic characterization techniques for layered double

6.2 Spectroscopy of polymer nanocomposites 232

7. Melt rheological properties of layered double hydroxide polymer

7.4 Modeling of rheological properties 301

8. Thermal properties and flame-retardant characteristics of layered

9. Mechancial and dynamical mechanical properties of layered double

9.6 Dynamical mechanical properties of LDH-filled elastomer and

10. Layered double hydroxide nanocomposites based on carbon

11. Recent advances in layered double hydroxide/polymer latex

11.3.1 LDH-based nanocomposites 481

12. Fabrication, assembly, and optoelectric properties of layered double

13. Polymer layered double hydroxide hybrid nanocomposites 531

14. Electrical and electronic applications of layered double-hydroxide

14.3 Batteries 574

15. Applications of layered double hydroxide biopolymer

16. Layered double hydroxide based nanocomposites for biomedical

16.3 Layered double hydroxide polymer nanocomposites for

17. Layered double hydroxide nanocomposites for agricultural

18. Layered double hydroxide polymer nanocomposites for

19. Layered double hydroxide polymer nanocomposites for water

20. Layered double hydroxide polymer nanocomposites for catalysis 805

Gonzalo Abellán Institute of Molecular Science (ICMol), University of Valencia,

Faezeh Azimi Chemistry Group, Pardis College, Isfahan University of

Vajiheh Behranvand Organic Polymer Chemistry Research Laboratory,

Luı́z Paulo Figueredo Benı́cio Soil Department, Federal University of Viçosa,

Rodrigo Botan Unifacvest University, Lages, SC, Brazil

E. Bourgeat-Lami University of Lyon, Université Claude Bernard Lyon 1, CPE

Jose A. Carrasco Institute of Molecular Science (ICMol), University of Valencia,

Eugenio Coronado Institute of Molecular Science (ICMol), University of

Sabrina de Bona Sartor Unifacvest University, Lages, SC, Brazil

Yanshan Gao College of Environmental Science and Engineering, Beijing

Giuliana Gorrasi Department of Industrial Engineering, University of Salerno-via

Mohsen Hajibeygi Faculty of Chemistry, Kharazmi University, Tehran, Iran

Yaping Huang Beijing University of Chemical Technology, Beijing, P.R. China

Kuruvilla Joseph Department of Chemistry, Indian Institute of Space Science and

Nandakumar Kalarikkal International and Inter University Centre for

Elham Khadem Organic Polymer Chemistry Research Laboratory, Department of

Leila Khodadadzadeh Chemistry Group, Pardis College, Isfahan University of

Jun Lu Beijing University of Chemical Technology, Beijing, P.R. China