لایب سان

1 Chapter I Introduction..................................................................................................... 1 2 Chapter II Literature Review .......................................................................................... 2 2.1 Cooperativity ........................................................................................................................................ 2 2.2 Thin Films ............................................................................................................................................ 5 2.3 Spin Coating ......................................................................................................................................... 8 2.4 Ellipsometry ....................................................................................................................................... 10 2.5 Dielectric Analysis ............................................................................................................................. 11 2.6 Thermal Mechanical Analysis ............................................................................................................ 12 2.7 Polymer Brushes................................................................................................................................. 12 2.8 Contact Angles ................................................................................................................................... 16 2.9 Atomic Force Microscopy.................................................................................................................. 17 3 Chapter III Experimental .............................................................................................. 19 3.1 Cooperativity Studies ......................................................................................................................... 19 3.2 Polymer Brush Studies ....................................................................................................................... 22 4 Chapter IV Results and Discussion: Cooperativity Studies.......................................... 27 4.1 Differential Scanning Calorimetry ..................................................................................................... 27 4.2 Gel Permeation Chromatography ....................................................................................................... 28 4.3 Ellipsometry ....................................................................................................................................... 29 4.4 Dielectric Analysis ............................................................................................................................. 32 4.5 Thermal Mechanical Analysis ............................................................................................................ 36 4.6 Summary of Cooperativity Studies..................................................................................................... 39 5 Chapter V Results and Discussion: Polymer Brush Studies......................................... 40 5.1 Contact Angles ................................................................................................................................... 40 5.2 X-ray Photoelectron Spectroscopy ..................................................................................................... 42 5.3 Ellipsometry ....................................................................................................................................... 47 5.4 Atomic Force Microscopy.................................................................................................................. 48 5.5 Summary of Polymer Brush Studies................................................................................................... 70 ii List of Figures Figure 2.1-1: Temperature dependence of the shift factor for several polymers................ 4 Figure 2.2-1: Substrate-polymer interactions of PMMA on silicon. .................................. 7 Figure 2.2-2: Change of Tg with film thickness.................................................................. 8 Figure 2.3-1: Stages of spin coating .................................................................................. 9 Figure 2.7-1: Polymer brush chain conformations. .......................................................... 13 Figure 2.7-2: Brush height versus grafting amount for homopolymers (Rg = radius of gyration). .................................................................................................................... 14 Figure 2.7-3: Brush height versus grafting density for di-block copolymers. .................. 14 Figure 2.7-4: Polymer brush self-assembly of a di-block copolymer............................... 15 Figure 2.8-1: Contact Angle Analysis ............................................................................. 16 Figure 3.1-1: Schematic of Dielectric Instrument............................................................. 21 Figure 3.2-1: Chemical structure of di-block copolymer.................................................. 22 Figure 4.1-1: DSC scan of PMMA (Endotherm Up)........................................................ 27 Figure 4.2-1: GPC results for PMMA............................................................................... 28 Figure 4.3-1: Film Thickness versus Spin Speed for each sample ................................... 30 Figure 4.3-2: Film thickness vs. solution concentration for the 3000 rpm samples ......... 31 Figure 4.4-1: DEA results for clean silicon wafer, permittivity as temperature increased32 Figure 4.4-2: DEA of clean silicon wafer......................................................................... 33 Figure 4.4-3: DEA results of 50 nm PMMA film on silicon............................................ 34 Figure 4.4-4: DEA results of a second 50 nm film sample on silicon.............................. 35 Figure 4.4-5: DEA results of a second clean silicon wafer sample .................................. 36 Figure 4.5-1: 900 nm DMA .............................................................................................. 37 Figure 4.5-2: TMA results of 50 nm film of PMMA, no apparent transition................... 38 Figure 4.5-3: TMA results of 660 nm film superimposed on blank silicon wafer ........... 39 Figure 5.1-1: Contact angles of water on copolymer brush samples................................ 41 Figure 5.2-1: XPS elemental analysis of oxygen on 20t sample ...................................... 45 Figure 5.2-2: XPS elemental analysis of oxygen on 20ht sample .................................... 45 Figure 5.2-3: XPS elemental analysis of carbon on 20t sample ....................................... 46 Figure 5.2-4: XPS elemental analysis of carbon on 20ht sample ..................................... 46 Figure 5.4-1: AFM image of a clean silicon wafer........................................................... 49 iii Figure 5.4-2: 3-D AFM image of a clean silicon wafer.................................................... 49 Figure 5.4-3: AFM image of 40t sample after 10 hours of toluene wash......................... 50 Figure 5.4-4: AFM image of 100t sample after 10 hours of toluene wash....................... 51 Figure 5.4-5: AFM images of 10t sample......................................................................... 52 Figure 5.4-6: 3-D AFM image of 10t sample. .................................................................. 52 Figure 5.4-7: AFM images of 20t sample......................................................................... 53 Figure 5.4-8: 3-D AFM image of 20t sample. .................................................................. 53 Figure 5.4-9: AFM images of 40t sample......................................................................... 54 Figure 5.4-10: 3-D AFM image of 40t sample. ................................................................ 54 Figure 5.4-11: AFM images of 100t sample..................................................................... 55 Figure 5.4-12: 3-D AFM image of 100t sample. .............................................................. 55 Figure 5.4-13: AFM images of 40ht sample..................................................................... 57 Figure 5.4-14: 3-D AFM image of 40ht sample. .............................................................. 57 Figure 5.4-15: AFM images of 100ht sample................................................................... 58 Figure 5.4-16: 3-D AFM image of 100ht sample. ............................................................ 58 Figure 5.4-17: AFM images of 100c sample. ................................................................... 59 Figure 5.4-18: 3-D AFM image of 100c sample............................................................... 59 Figure 5.4-19: AFM images of 100hc sample. ................................................................. 60 Figure 5.4-20: 3-D AFM image of 100hc sample............................................................. 60 Figure 5.4-21: Summary chart of the average height difference for each polymer brush sample. ....................................................................................................................... 62 Figure 5.4-22: Height analysis of AFM image for 10t sample. ........................................ 63 Figure 5.4-23: Height analysis of AFM image for 20t sample. ........................................ 64 Figure 5.4-24: Height analysis of AFM image for 40t sample. ........................................ 65 Figure 5.4-25: Height analysis of AFM image for 100t sample. ...................................... 66 Figure 5.4-26: Height analysis of AFM image for 40ht sample. ...................................... 67 Figure 5.4-27: Height analysis of AFM image for 100ht sample. .................................... 68 Figure 5.4-28: Height analysis of AFM image for 100c sample. ..................................... 69 Figure 5.4-29: Height analysis of AFM image for 100hc sample. ................................... 70 iv List of Tables Table 2.1-1: Coupling parameters of several polymers. ..................................................... 3 Table 2.8-1: Contact angle results for polymethacrylates. ............................................... 17 Table 4.3-1: Film Thickness and error for 2% PMMA solution....................................... 29 Table 4.3-2: Film Thickness and error for 5% PMMA solution....................................... 29 Table 4.3-3: Film Thickness and error for 10% PMMA solution..................................... 29 Table 5.1-1: Contact angles for methylene iodide. ........................................................... 42 Table 5.1-2: Surface energy with dispersive and polar components. ............................... 42 Table 5.2-1: XPS results (15°), atomic concentration table for one measurement of 20ht sample. ....................................................................................................................... 43 Table 5.2-2: XPS results (90°), atomic concentration table for one measurement of 20ht sample. ....................................................................................................................... 43 Table 5.2-3: XPS results (15°), atomic concentration table for one measurement of 20t sample. ....................................................................................................................... 44 Table 5.2-4: XPS results (90°), atomic concentration table for one measurement of 20t sample. ....................................................................................................................... 44 Table 5.3-1: Di-block sample film thickness from ellipsometry after 10 hours of washing .................................................................................................................................... 47 Table 5.3-2: Di-block sample film thickness from ellipsometry after 34 hours of washing .................................................................................................................................... 4

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