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Inorganic Micro- and
Nanostructures
This page intentionally left blank
 Materials for Biomedical Engineering

Inorganic Micro- and

Nanostructures

Edited by
Valentina Grumezescu
Lasers Department, National Institute for Laser Plasma &
Radiation Physics, Romania

Alexandru Mihai Grumezescu

Faculty of Applied Chemistry and Materials Science, University
Politehnica of Bucharest, Bucharest, Romania
Elsevier
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Contents
List of Contributors .................................................................................................xv
Series Preface .........................................................................................................xix
Preface ....................................................................................................................xxi

CHAPTER 1 Biomedical inorganic nanoparticles: preparation,

properties, and perspectives........................................ 1
Magdalena Stevanović, Miodrag J. Lukić, Ana Stanković,
Nenad Filipović, Maja Kuzmanović and Zeljko ˇ Janićijević
1.1 Introduction ....................................................................................1
1.2 Gold Nanoparticles.........................................................................2
1.3 Silver Nanoparticles .......................................................................5
1.4 Selenium Nanoparticles................................................................10
1.5 Copper Nanoparticles...................................................................11
1.6 Iron Nanoparticles ........................................................................17
1.7 Zinc Oxide Nanoparticles ............................................................19
1.8 Hydroxyapatite Nanoparticles......................................................24
1.9 Conclusions ..................................................................................29
Acknowledgments ....................................................................... 29
References.................................................................................... 29
Further Reading ........................................................................... 45
CHAPTER 2 Inorganic composites in biomedical engineering..... 47
Murthy Chavali, Periasamy Palanisamy,
Maria P. Nikolova, Ren-Jang Wu,
Ravisankar Tadiboyina and P.T.S.R.K. Prasada Rao
2.1 Introduction and Background.......................................................47
2.2 Categorization ..............................................................................52
2.3 Components ..................................................................................53
2.3.1 Matrices............................................................................. 53
2.3.2 Fibers................................................................................. 54
2.3.3 Particles ............................................................................. 56
2.3.4 Interface............................................................................. 57
2.4 Preparation of Composites ...........................................................57
2.4.1 Composites Based on Polymer Matrix ............................. 57
2.4.2 Composites Based on Ceramic Matrix............................. 58
2.5 Properties of Composites .............................................................59
2.6 Anomalies.....................................................................................62
2.6.1 Fracture and Fatigue Failure............................................. 62

v
vi Contents

2.7 Biological Response.....................................................................65

2.8 Applications in Biomedical Engineering.....................................66
2.8.1 Dentistry ............................................................................ 66
2.8.2 Prosthetics and Orthotics .................................................. 68
2.8.3 Tissue Engineering............................................................ 69
2.8.4 Orthopedic......................................................................... 70
2.9 Conclusions ..................................................................................71
References.................................................................................... 72
Further Reading ........................................................................... 78

CHAPTER 3 Structural interpretation, microstructure

characterization, mechanical properties,
and cytocompatibility study of pure and doped
carbonated nanocrystalline hydroxyapatites
synthesized by mechanical alloying.......................... 81
Sushovan Lala and Swapan Kumar Pradhan
3.1 Introduction ..................................................................................81
3.1.1 Carbonation in Biological Apatites .................................. 83
3.1.2 Importance of Zn, Mn, and Mg as Trace
Elements Present in Bone ................................................. 83
3.2 Materials and Methods.................................................................84
3.2.1 Mechanical Alloying......................................................... 84
3.2.2 Sample Preparation by MA .............................................. 84
3.2.3 Spark Plasma Sintering ..................................................... 85
3.2.4 Sample Characterization ................................................... 86
3.2.5 Biological Studies ............................................................. 86
3.2.6 Method of Analysis........................................................... 87
3.3 Results and Discussions ...............................................................90
3.3.1 Phase Confirmation of Unsintered HAp Samples
From XRD Patterns........................................................... 90
3.3.2 Confirmation of Carbonation in HAp by FTIR
Analysis ............................................................................. 90
3.3.3 Quantitative Phase Estimation of Unsintered
Samples Using Rietveld’s Method ................................... 92
3.3.4 Modification in HAp Structure due to Mn/Mg/Zn
Substitution........................................................................ 94
3.3.5 HRTEM Analysis............................................................ 100
3.3.6 Microstructure Characterizations of the Spark
Plasma Sintered Samples ................................................ 103
3.3.7 Mechanical Properties of the Sintered HAp
Samples ........................................................................... 107
 Contents vii

3.3.8 Cytocompatibility Test.................................................... 111

3.4 Conclusions ................................................................................113
References.................................................................................. 113
CHAPTER 4 Multiparticle composites based on
nanostructurized arsenic sulfides As4S4 in
biomedical engineering............................................ 119
Oleh Shpotyuk, Zdenka Bujňáková, Peter Baláž,
Yaroslav Shpotyuk and Adam Ingram
4.1 Introduction ................................................................................119
4.2 As4S4/ZnS NC Preparation Procedure.......................................120
4.2.1 Mechanochemical Synthesis of As4S4/ZnS
NCs in a Dry-Milling Mode ........................................... 121
4.2.2 Mechanochemical Synthesis of As4S4/ZnS-PX407
NSs in a Wet-Milling Mode ........................................... 121
4.3 As4S4/ZnS NC Characterization Methodology .........................121
4.3.1 Atomic-Relevant Structure ............................................. 121
4.3.2 Atomic-Deficient Structure............................................. 123
4.3.3 Biological Activity.......................................................... 126
4.4 NP-Guided Functionality in As4S4/ZnS NCs ............................127
4.4.1 Characterization of As4S4/ZnS NCs Prepared
in a Dry-Milling Mode ................................................... 127
4.4.2 Atomic-Deficient Structure of As4S4/ZnS NCs ............. 130
4.4.3 Characterization of As4S4/ZnS-PX407 NSs
Prepared in a Wet-Milling Mode.................................... 140
4.4.4 Biological Activity of As4S4/ZnS NPs........................... 142
4.5 Conclusions ................................................................................147
References.................................................................................. 148
CHAPTER 5 Quaternary ammonium compound derivatives
for biomedical applications ..................................... 153
Mari Miura Sugii, Fábio Augusto de Souza Ferreira,
Karina Cogo Müller, Ubirajara Pereira Rodrigues Filho
and Flávio Henrique Baggio Aguiar
5.1 Background.................................................................................153
5.2 Biofilm Treatment and Prevention ............................................154
5.3 Quaternary Ammonium Compounds and Their Chemistry ......155
5.3.1 Cationic Acrylates and Cationic Silanes ........................ 156
5.3.2 Quaternary Ammonium Compound Disinfectants
and Preservatives............................................................. 161
viii Contents

5.3.3 In Situ Quaternization of Tertiary Amines to

Form Quaternary Ammonium Compounds and
Nanoparticle Functionalization....................................... 162
5.4 Variables Influencing the Antimicrobial Properties
of Quaternary Ammonium Compound ......................................164
5.5 Cytotoxicity ................................................................................167
5.6 Antimicrobial Resistance ...........................................................168
5.7 Remarks ......................................................................................168
References.................................................................................. 169
CHAPTER 6 Block copolymer micelles as nanoreactors
for the synthesis of gold nanoparticles ................... 177
Rajpreet Kaur and Poonam Khullar
6.1 Introduction ................................................................................177
6.1.1 Poloxamers and Poloxamines ......................................... 178
6.1.2 Micelle Architecture and Mixed Micelles...................... 181
6.1.3 Synthesis of Various Morphologies of Gold
Nanoparticles................................................................... 183
6.1.4 Bimetallic Nanoparticles................................................. 189
6.1.5 Comparison of Poloxamers and Poloxamines................ 190
6.2 Biomedical Applications ............................................................195
6.3 Study Results..............................................................................199
6.4 Future Perspectives ....................................................................202
References.................................................................................. 203
Further Reading ......................................................................... 209

CHAPTER 7 Nanoparticles: synthesis and applications ............. 211

Nguyen Hoang Nam and Nguyen Hoang Luong
7.1 Introduction ................................................................................211
7.2 Synthesis of Nanoparticles.........................................................212
7.2.1 Chemical Reduction........................................................ 212
7.2.2 Coprecipitation ................................................................ 212
7.2.3 Seeding ............................................................................ 213
7.2.4 Microemulsion and Inverse Microemulsion................... 213
7.2.5 Hydrothermal Method..................................................... 213
7.2.6 Sonoelectrodeposition ..................................................... 214
7.3 Functionalization/Coating of Nanoparticles ..............................214
7.3.1 Functionalization of Nanoparticles................................. 214
7.3.2 Silica Coating of Magnetic Nanoparticles ..................... 215
7.3.3 Multifunctional Nanoparticles ........................................ 215
7.4 Applications................................................................................218
 Contents ix

7.4.1 Application of Gold Nanoparticles for Breast

Cancer Cell Detection..................................................... 218
7.4.2 Basal Cell Carcinoma Fingerprinted Detection ............. 219
7.4.3 Antibacterial Test Using Silver Nanoparticles............... 222
7.4.4 Magnetic Nanoparticles .................................................. 223
7.4.5 Applications of Multifunctional Nanoparticles .............. 230
7.5 Conclusion and Perspectives......................................................232
Acknowledgment ....................................................................... 233
References.................................................................................. 233
CHAPTER 8 Multimodal magnetic nanoparticles for
biomedical applications: importance of
characterization on biomimetic in vitro models ..... 241
Mojca Pavlin, Daša Zupančič, Jasna Lojk,
Klemen Strojan and Mateja Erdani Kreft
8.1 Introduction ................................................................................241
8.2 Characterization of Multimodal Magnetic Nanoparticles .........242
8.2.1 Properties of Magnetic Nanoparticles ............................ 242
8.2.2 Magnetic Nanoparticle Properties Change
in Physiological Fluids.................................................... 244
8.2.3 Methods for Characterization of Physicochemical
Properties of Magnetic Nanoparticles ............................ 245
8.2.4 Characterization of Magnetic Nanoparticle
Mobility in 3D Gels and in the Artificial
Extracellular Matrix ........................................................ 246
8.3 Current Biomedical Applications of Multimodal
Magnetic Nanoparticles..............................................................247
8.3.1 Molecular Isolation and Magnetic Separation ............... 248
8.3.2 Magnetic Nanoparticles as Delivery Vectors................. 248
8.3.3 Cell Labeling................................................................... 249
8.3.4 Magnetic Nanoparticles as Contrast Agents
for Magnetic Resonance ................................................. 249
8.3.5 Magnetofection ............................................................... 250
8.3.6 Magnetic Fluid Hyperthermia......................................... 251
8.3.7 Perspectives of Magnetic Nanoparticle
Biomedical Applications................................................. 251
8.4 Endocytosis and Intracellular Fate of Multimodal
Magnetic Nanoparticles..............................................................251
8.4.1 Different Endocytic Pathways ........................................ 252
8.4.2 Uptake Pathway Depends Mainly on the
Properties of Nanoparticles and the Cell Type .............. 253
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x Contents

8.4.3 The Intracellular Trafficking and Fate of

Internalized Nanoparticles .............................................. 255
8.4.4 Endocytosis of Magnetic Nanoparticles Is an
Essential Step for Most Biomedical Applications ......... 257
8.5 In Vivo and In Vitro Models (Classical Cell Cultures,
Biomimetic) for Testing Nanoparticle Toxicity and Their
Penetration Through Cell Plasma Membranes and Tissue
Barriers .......................................................................................258
8.5.1 The Comparison of In Vivo and In Vitro Models
for the Research Into Magnetic Nanoparticle Effects.... 258
8.5.2 The Routes and Model Organisms of Magnetic
Nanoparticle Administration........................................... 260
8.5.3 Biomimetic In Vitro Models Represent the Bridge
Between In Vitro and In Vivo Research ........................ 262
8.6 Advantages, Perspectives, and Limitations of Biomimetic
In Vitro Models Versus Classical Cell Cultures .......................263
8.6.1 Skin Models .................................................................... 263
8.6.2 Lung Models ................................................................... 264
8.6.3 Gastrointestinal Tract Models......................................... 265
8.6.4 Placenta Models .............................................................. 266
8.6.5 Urothelium/Urinary Bladder Models.............................. 266
8.6.6 Perspectives of Biomimetic In Vitro Models................. 267
8.7 Conclusions ................................................................................269
Acknowledgments ..................................................................... 269
References.................................................................................. 269

CHAPTER 9 Aluminosilicate-based composites

functionalized with cationic materials:
possibilities for drug-delivery applications............. 285
Danina Krajišnik, Bojan Čalija and Jela Milić
9.1 Introduction ................................................................................285
9.2 Aluminosilicates as Drug Carriers—Properties,
Advantages, and Limitations......................................................286
9.3 Aluminosilicate-Based Drug Carriers Functionalized
With Cationic Surfactants ..........................................................288
9.3.1 Cationic Surfactants—Properties and
Pharmaceutical Applications .......................................... 288
9.3.2 Preparation and Characterization of
Surfactant-Modified Aluminosilicates............................ 294
9.3.3 Functionality of Surfactant-Modified
Aluminosilicates as Drug Carriers.................................. 298
9.4 Chitosan-Functionalized Aluminosilicates as
Drug Carriers..............................................................................303
 Contents xi

9.4.1 Chitosan—A Versatile Biopolymer................................ 303

9.4.2 Preparation and Characterization of
Chitosan-Modified Aluminosilicates .............................. 307
9.4.3 Functionality of Chitosan
Aluminosilicate
Composites as Drug Carriers .......................................... 310
9.5 Conclusions ................................................................................316
Acknowledgment ....................................................................... 316
References.................................................................................. 316
CHAPTER 10 Bioactive glass nanofibers for tissue
engineering ............................................................... 329
Joaquı´n Penide, Félix Quintero, Jesús del Val,
Rafael Comesaña, Fernando Lusquiños,
Antonio Riveiro and Juan Pou
10.1 Introduction ................................................................................329
10.1.1 Definition of Nanofiber ................................................ 329
10.1.2 Interest in Bioactive Glass Nanofibers in Tissue
Engineering (Scaffolds and Composites) ..................... 330
10.2 Conventional Methods to Produce Glass Microfibers...............332
10.3 Methods to Produce Glass Nanofibers ......................................335
10.3.1 Bottom-Up Methods ..................................................... 335
10.3.2 Top-Down Methods ...................................................... 336
10.4 Bioactive Glass Fibers for Tissue Engineering and
Composites .................................................................................338
10.5 Production of Glass Nanofibers by Laser Spinning
Technique ...................................................................................342
10.5.1 Bioactive Glass Nanofibers for Tissue
Engineering and Composites ........................................ 348
10.6 Summary and Outlook ...............................................................351
Acknowledgment ....................................................................... 351
References.................................................................................. 351
CHAPTER 11 Application of (mixed) metal oxides-based
nanocomposites for biosensors ............................... 357
Ali Salehabadi and Morteza Enhessari
11.1 Introduction ................................................................................357
11.1.1 Semiconducting (Nano)Materials ................................. 358
11.1.2 Polymers........................................................................ 365
11.1.3 Nanocomposites/Particles ............................................. 365
11.2 Sensors and Biosensors ..............................................................367
11.2.1 Sensing Measurement ................................................... 367
11.3 Application of Sensors ...............................................................368
xii Contents

11.3.1 Gas (Bio)Sensors........................................................... 368

11.3.2 Chemical (Bio)Sensors ................................................. 374
11.3.3 Environment Biosensors ............................................... 376
11.3.4 Biological Sensors......................................................... 379
11.3.5 Clinical Biosensors ....................................................... 382
11.4 Fabrication..................................................................................387
11.5 Selectivity, Sensitivity, and Time Factors .................................389
11.6 Summary and Recommendations for Future Work...................390
References.................................................................................. 390
Further Reading ......................................................................... 396
CHAPTER 12 Metal nanoparticles and their composites: a
promising multifunctional nanomaterial for
biomedical and related applications ....................... 397
Vesna V. Vodnik and Una Bogdanović
12.1 Introduction ................................................................................397
12.2 Some Interesting Properties of the Metals
on the Nanometer Length Scale.................................................399
12.3 Nanoparticle Synthesis and Functionalization...........................402
12.3.1 Synthesis Approaches to Metal Nanoparticles............. 402
12.3.2 Functionalization of Metal Nanoparticles:
Manipulation of Nanoparticles Properties.................... 403
12.4 Applications of Metal Nanoparticles and Their
Polymer-Based Nanocomposites................................................406
12.4.1 Medical Applications .................................................... 407
12.4.2 Applications in Biology ................................................ 410
12.5 Conclusions and Outlook ...........................................................416
Acknowledgments ..................................................................... 418
References.................................................................................. 418

CHAPTER 13 Hybrid metal complex nanocomposites

for targeted cancer diagnosis and
therapeutics .............................................................. 427
Jeong-Hwan Kim, Haruki Eguchi,
Masanari Umemura and Yoshihiro Ishikawa
13.1 Introduction ................................................................................427
13.2 Conventional Chemotherapy......................................................429
13.3 Striving Toward Targeted Chemotherapy .................................431
13.4 Metal
Ligand Complexes as a Composite
Anticancer Drug .........................................................................431
13.4.1 Iron Complexes ............................................................. 432
 Contents xiii

13.4.2 Quantitative Structure
Function Relationship

of Iron-Salen Complexes .............................................. 432
13.4.3 Magnetic Nanoparticles (MNPs) as an
Essential Carrier for Magnetic DDS ............................ 433
13.4.4 Molecular Magnetic Iron Complex
for Magneto-DDS ......................................................... 438
13.5 Hybrid Metal Salen
Polymer Nanocomposites as
Nano-DDS ..................................................................................452
13.6 Conclusion ..................................................................................454
References.................................................................................. 455

CHAPTER 14 Nanocoatings and thin films .................................... 463

Valentina Grumezescu and Irina Negut
14.1 Introduction ................................................................................463
14.2 Nanocoating Fabrication Methods .............................................464
14.2.1 Dip-Coating Method ..................................................... 464
14.2.2 Matrix-Assisted Pulsed Laser
Evaporation Method...................................................... 468
14.3 Conclusion ..................................................................................473
References.................................................................................. 473

Index ......................................................................................................................479
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