Nanostructured, electroactive and bioapplicable materials

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Preface The overall objective of this dissertation is to develop new advanced materials, more specifically, nanostructured porous materials, nanocomposites and electroactive materials, for potential applications in electrooptical devices, biosensors, drug delivery and tissue engineering. Among others, two main considerations are present throughout this research work. Firstly, it is always desirable to have versatile and controllable synthesis processes and products. Of our special interest is the versatility of the newly developed nonsurfactant templating sol-gel pathway. Aiming at a variety of potential applications, it is desired that a broad selection of templates can be used, materials with different morphologies and compositions can be produced, and the entire process can be fine-tuned. Secondly, due to the special requirement of bio-applications, these materials and/or their synthetic reagents and conditions need to do no harm to biomolecules and cells, and this property is described as “biofriendly” in this dissertation. The organization of the dissertation is as follows. Chapter 1 is an overview of nanostructured porous sol-gel materials. Based on an introduction of fundamental sol-gel chemistry, mesoporous materials (i.e., with pore diameter of 2-50 nm) obtained from both surfactant and nonsurfactant templated sol-gel methods are described in detail. Discussions include the template species, templating mechanisms, reaction conditions and the characteristic microstructures of porous materials. Description of general characterization and testing methods for porous materials is provided with an emphasis on gas sorption measurement. 1
Chapter 2 presents a study focused on the synthesis of mesoporous materials with a new category of nonsurfactant template, i.e., thermal decomposable compounds. With this new class of templates, conventional high temperature (i.e., 500-600 °C) calcination template removal process can be avoided. The materials with typical nonsurfactant templated mesoporous structure are prepared with a template removal process at a relatively low temperature (e.g., 150 °C). The materials synthesis and characterization are described. The template removal process is discussed in detail. Chapter 3 describes the development of a synthetic route to prepare mesoporous nanospheres with uniform size and shape. The study demonstrates the morphological controllability of the nonsurfactant templating method. The experimental method, material characterization and template effect on pore structures are discussed. In this work, fructose was selected as the nonsurfactant template because it has been proven by our group previously a very effective and biofriendly template, among over one hundred other nonsurfactant molecules examined (e.g., glucose, maltose, soluble starch, cyclodextrins, glycerol, oligopeptides, tartaric acid, etc.). With well-defined morphology and nanostructure, the nanospheres are potentially useful for a variety of applications, such as drug delivery, bio-sensor and catalyst. Chapter 4 presents the studies on gold nanoparticle dispersion in mesoporous silica matrices for the perceivable chemical and biological sensing applications. The gold-silica nanocomposites were prepared through a nonsurfactant templated sol-gel pathway with a gold sol as the source of metal particles. The obtained nanocomposites 2
Page 1: Nanostructured, Electroactive and B
Page 4 and 5: Dedications This dissertation is de
Page 6 and 7: School of Biomedical Engineering, S
Page 8 and 9: 2.2. Experimental .................
Page 10 and 11: 5.2.2. Treatment of Substrate Surfa
Page 12 and 13: 8.2. Electroactive, Bioapplicable M
Page 14 and 15: List of Tables Table 2-1. Compositi
Page 16 and 17: Figure 2-9. BJH pore size distribut
Page 18 and 19: xvi pattern of gold nanoparticles i
Page 20 and 21: xviii PANI under culturing conditio
Page 22 and 23: Figure B-8. Cyclic voltammogram (Pt
Page 24: The resultant polyaniline-collagen
Page 29 and 30: Chapter 7 is focused on the synthes
Page 31 and 32: surfactant templated method was ext
Page 33 and 34: The porous structure of the silica
Page 35 and 36: Before early 1990s, with a pore or
Page 37 and 38: − Neutral surfactants: the hydrop
Page 39 and 40: The mechanism of nonsurfactant temp
Page 41 and 42: zero in a pore. Structural informat
Page 43 and 44: 1.5.1. Gas Sorption Measurement As
Page 45 and 46: which is usually associated with ca
Page 47 and 48: 16. Iler, R. K. The Chemistry of Si
Page 49 and 50: 52. Sayari, A.; Danumah, C.; Moudra
Page 51 and 52: Figure 1-1. Three structure types p
Page 53 and 54: Figure 1-3. IUPAC classification of
Page 55 and 56: Chapter 2. Mesoporous Sol-Gel Mater
Page 57 and 58: well formed below the isoelectric p
Page 59 and 60: 2.1.2. Nonsurfactant Templates and
Page 61 and 62: since controllable partial removal
Page 63 and 64: were ground manually into fine powd
Page 65 and 66: volatile sol-gel reaction byproduct
Page 67 and 68: After the thermal treatment at 150
Page 69 and 70: oiling point of benzoin (i.e., 194
Page 71 and 72: interconnected pores or channels wi
Page 73 and 74: 6. Huo, Q.; Magargolese, D. I.; Cie
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Table 2-1. Composition and pore par
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Weight (%) 100 80 60 40 20 0 0 100
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Weight (%) 100 90 80 70 60 0 100 20
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Weight (%) 100 90 80 70 60 50 40 0
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Figure 2-7. Representative IR spect
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dV/dD Pore Volume (cm 3 g -1 Å -1
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dv/dD, Pore Volume (cm 3 g -1 Å -1
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Net Pore Volume (cm 3 g -1 ) 0.6 0.
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Chapter 3. Synthesis of Mesoporous
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preparation conditions. In general,
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cubic, as well as vesicular structu
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3.2 Experimental The synthesis appr
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3.2.3. Synthesis of Mesoporous Sphe
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fructose is incorporated into the s
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mainly attributed to the monolayer-
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with nonsurfactant templates at dif
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3.4. Conclusions and Remarks In the
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11. Matijević, E.; Gheradi, P. Tra
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41. Polarz, S.; Smarsly, B.; Bronst
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(a) (b) Figure 3-1. Typical SEM ima
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Volume Adsorbed (cm 3 g -1 , STP) 3
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Figure 3-5. Representative TEM imag
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(a) (b) Figure 3-7. Typical SEM ima
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Chapter 4. Synthesis of Mesoporous
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nm, and the reaction reaches the hi
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microemulsion. 39 Martino et al. re
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the colloidal gold sol was combined
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holders with adhesive carbon tape.
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trapped in the gold-silica matrix,
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108 The Barrett-Joyner-Halenda (BJH
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indicative of a well-defined crysta
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(i.e., 2-50 nm). Combining both hig
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19. Hayashi, T.; Tanaka, K.; Haruta
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53. Qi, L.; Ma, J.; Cheng, H.; Zhao
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Figure 4-1. Representative X-ray en
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Pore Volume (cm 3 g -1 A -1 ) 0.06
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(a) (b) 122 Figure 4-5. (a) Represe
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Absorbance Wavelength (nm) Figure 4
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5.1.1. Organic-Inorganic Nanocompos
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128 We are also interested in the p
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mica and graphite, the top layer wa
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mode. Scanning electron microscopy
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Waal’s forces), the agglomeration
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136 A single glass transition tempe
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5.5. Acknowledgments 138 I want to
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30. Dimitrov, A. S.; Nagayama, K. L
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(a) (b) 142 Figure 5-2. Representat
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144 Figure 5-4. Representative AFM
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Figure 5-6. Representative IR spect
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(a) (b) Figure 5-8. Representative
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the possibility of utilizing conduc
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iocompatibility and water solubilit
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emeraldine salt, the unique conduct
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acid (HCl, 37.3%, Fisher), hydrogen
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the surface of polymer coated cultu
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acidic acid aqueous solution showed
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oxidant, indicating the formation o
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complex was synthesized by pre-alig
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8. Epstein, A. J. Springer Ser. Mat
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45. Liu, J.-M.; Yang, S. Chem. Comm
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Figure 6-1. Schematics of biologica
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172 Figure 6-3. UV-Vis absorption s
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Figure 6-5. FT-IR spectra of (a) co
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176 Figure 6-7. UV-Vis absorption s
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(a) (b) 178 Figure 6-9. Comparison
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prepared and purified as substitute
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greatest advantages of organic mate
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een explored as a direct and effect
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if we could fine-tune the carrier t
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NMR (250 MHz, DCCl3) δ (ppm): 8.95
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7.2.4. Instrumentation and Characte
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The absence of the proton from the
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194 The absorbance at 600 nm is the
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L3Al dissociated to free ligand (L)
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198 State and Integrated Circuit Te
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34. Stossel, M.; Staudigel, J.; Ste
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Table 7-1. The UV absorbance at 600
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Figure 7-2. Schematic cross-section
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Figure 7-4. NMR Spectra of ligand 1
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Figure 7-6. FT-IR spectra of (a) li
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Figure 7-8. During air oxidation: 1
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[A] 1.2E-04 1.0E-04 8.0E-05 6.0E-05
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Figure 7-12. Mass spectrum of alumi
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Chapter 8. Concluding Remarks 216 T
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218 In contrast to the conventional
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properties of gold nanoparticles ma
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222 In an effort to obtain new elec
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as sensor units, the biodegradable
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polyanhydrides, 4 polyorthoesters,
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substitution reaction, several hund
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polyphosphazenes. Obtained material
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polyphosphazene network. Studies in
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matrix is readily formed due to the
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236 The delivery system can be made
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phosphazene main chains. Further in
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9. Allcock, H. R. Adv. Mater. 1994,
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Figure A-1. Repeating unit in polyp
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Figure A-3. Applications of materia
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Figure A-5. Preparation of poly(N-i
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B.3. Acknowledgments 248 I am grate
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Figure B-2. Cyclic voltammogram (Hg
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Figure B-4. Cyclic voltammogram (Pt
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Figure B-6. Cyclic voltammogram (Hg
Page 281 and 282:
Figure B-8. Cyclic voltammogram (Pt
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