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Chapter 3. Abstract...................................................................................................................................43 3.1. Introduction......................................................................................................................44 3.2. Experimental Section 3.2.1. Materials.........................................................................................................................46 3.2.2. Synthesis of PNIPA-N3..................................................................................................................................................47 3.2.3. Synthesis of PNIPA-COOH..........................................................................................50 3.3. Results and discussion.......................................................................................................53 3.3.1. pH responsive contact angle............................................................................................56 3.4. Conclusion...........................................................................................................................60 References and Notes..................................................................................................................61 Chapter 4 Abstract......................................................................................................................................64 4.1. Introduction..........................................................................................................................65 4.2. Experimental Section 4.2.1. Materials............................................................................................................................67 4.2.2. Sample Synthesis. 4.2.2.1.Preparation of [11-(2-chloro)propionyloxy]undecyl-dimethylchlorosilane (CPU-dMCS) as Surface-Attachable ATRP Initiator..................................................................68 4.2.2.2. Preparation of [11-(2-methyl)propionyloxy]undecyl-dimethylchlorosilane (MPU-dMCS) as an ATRP-Inactive Alkyldimethylsilane Derivative...............................................................69 4.2.2.3. Preparation of ATRP Initiator-Deposited Silicon Wafer..............................................71 6
4.2.2.4.General Procedure for Synthesis of Grafted PNIPA from ATRP Initiator-Modified Silicon Wafers...........................................................................................73 4.2.3. Characterization 4.2.3.1. XPS Analysis of monolayer......................................................................................73 4.2.3.3. Equilibrium Contact Angle Measurements.................................................................74 4.2.3.4.Gel Permeation Chromatography (GPC).....................................................................76 4.2.3.5. 1 H NMR spectroscopy...............................................................................................76 4.2.3.6. Fourier Transform Infrared Spectroscopy (FT-IR).....................................................76 4.3. Results and Discussion......................................................................................................78 4.3.1. Preparation of Silicon Surface Modified with ATRP Initiator.......................................78 4.3.2. ATRP of NIPA for Preparation of Grafted Membrane...................................................85 4.3.3. Change in Thickness of High-Density Grafted Membrane of PNIPA in Water with Changing Temperature..........................................................................94 4.3.4. FT-IR to Observe Molecular Behavior of PNIPA in Grafted Membrane under Water................................................................................................96 4.3.5. Contact Angle of Air Bubble underneath PNIPA Grafted Membranes under Water..........................................................................................................102 4.4 Conclusions.........................................................................................................................108 References and Notes...............................................................................................................110 Chapter 5 Abstract.....................................................................................................................................117 5.1. Introduction........................................................................................................................117 7
Page 1 and 2: Facile Approach to Synthesize Stimu
Page 3 and 4: Acknowlwdgement This dissertation w
Page 5: Chapter 1. Table of Contents 1-1. I
Page 9 and 10: Chapter 1 General Introduction 9
Page 11 and 12: The growth in industrial applicatio
Page 13 and 14: 1.3. Grafting methods. Most of thes
Page 15 and 16: 1.5. Components of ATRP. There are
Page 17 and 18: Figure 1-4:Mechanism of the Atomic
Page 19 and 20: near that of the human body, PNIPAm
Page 21 and 22: References and notes. 1. Plastiquar
Page 23 and 24: Chapter 2 Characteristics of High-D
Page 25 and 26: 2.1. INTRODUCTION. Atom transfer ra
Page 27 and 28: . Cl Si H + OH 9 + 10-undecen-1-ol
Page 29 and 30: Figure 2-3 (b): NMR spectrum of Pro
Page 31 and 32: Figure 2-4: Schematic procedure for
Page 33 and 34: 3000 2000 Wavenumber/cm -1 1000 Fig
Page 35 and 36: Figure 2-7: (a) First order kinetic
Page 37 and 38: free polymers. We performed polymer
Page 39 and 40: Figure 2-9: Contact angles of air b
Page 41 and 42: 2.4. CONCLUSION. A detailed explana
Page 43 and 44: Chapter 3 Dominant influence of the
Page 45 and 46: 3.1. Introduction. Temperature resp
Page 47 and 48: and FT-IR analyses, were used as re
Page 49 and 50: azide Figure 3-2: FT-IR spectra of
Page 51 and 52: Figure 3-3: 1 H NMR spectrum of aci
Page 53 and 54: 3.3. Results and discussion. ATRP t
Page 55 and 56: temperature. 28 Electro-negativity
Page 57 and 58:
Contact Angle (degree) 141 138 135
Page 59 and 60:
Figure 3-7 shows equilibrium contac
Page 61 and 62:
References and Notes. (1) S.A. Prok
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Chapter 4 Precise Synthesis and Phy
Page 65 and 66:
4.1. Introduction. Stimuli-sensitiv
Page 67 and 68:
4.2. Experimental Section. 4.2.1. M
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hr and at room temperature for 12 h
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chromatography with hexane/ethyl ac
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4.2.2.4.General Procedure for Synth
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Figure 4-4. Schematic illustration
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Figure 4-5. FT-IR spectra of dried
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are necessary to achieve maximum bo
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Figure 4-1-1: XPS data of (a) C 1S
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The successful deposition of CPU-dM
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where f i is the area fraction of c
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The ATRP in this condition provides
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Figure 4-1-5: AFM image of densely
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Figure 4-1-8. Graft density of PNIP
Page 93 and 94:
Figure 4-1-7. Plots of Ld/Lc,w vers
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Figure 4-1-9. Thickness of high den
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Figure 4-7. a) FT-IR spectra and b)
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Figure 4-1-10 (c): Area ratio for t
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Area ratio 0.4 0.35 0.3 0.25 0.2 0.
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(a) Figure 4-1-11 . Contact angle o
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(c) Figure 4-1-11. Contact angle of
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The temperature dependence for the
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4.4 Conclusions. High-density therm
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(16) Osada, Y.; Gong, J. P. Prog. P
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2006, 22 (9), 4259-4266. L Macromol
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(76) The Young equation, cos θ = (
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Abstract. High-density polymer brus
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previously grafted chain prevents l
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5.3.1. Synthesis procedure of the A
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5.4.1. Fourier Transform Infrared S
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5.5. Result and discussion. Scheme
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graft density (chain/nm 2 ) 0.8 0.6
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Thickness (nm) 50 40 30 20 10 0 0 1
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a nm 1μm b nm 1μm Figure 5-5. The
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5.6. Conclusion. ATRP of PNIPA in D
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(17) Huang, E.; Rockford, L.; Russe
Page 137:
Publications. 1. Suzuki H., Huda M.
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