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Preparation of Polymer/Silica Particle Nanocomposites and Their Applications

Preparation of Polymer/Silica Particle Nanocomposites and Their Applications ( 고분자 / 실리카 나노복합체 제조와 응용 ) Nov. 5, 2009 KiRyong Ha ( 계명대학교 화학공학과 ). Colorado 주 및 Colorado 대학 소개. University of Colorado. Three campuses: Boulder, Colorado Springs and Denver.

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Preparation of Polymer/Silica Particle Nanocomposites and Their Applications

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  1. Preparation of Polymer/Silica Particle Nanocomposites and Their Applications (고분자/실리카 나노복합체 제조와 응용) Nov. 5, 2009 KiRyong Ha (계명대학교 화학공학과)

  2. Colorado 주및 Colorado 대학 소개

  3. University of Colorado Three campuses: Boulder, Colorado Springs and Denver.

  4. National Parks in Colorado Mesa Verde National Park Rocky Mountain National Park

  5. National Parks in Colorado Great Sand Dunes National Park Black Canyon of the Gunnison National Park

  6. Tourist Attractions Aspen mountains comprises of 4993 acres, forty lifts and 335 trails along with sharp vertical slopes in the entire Colorado, which makes it more thrilling and stimulating. Aspen Colorado Ski Resort

  7. Tourist Attractions Maroon Bells One Colorado Fall day

  8. Tourist Attractions United States Air Force Academy Garden of the gods

  9. University of Colorado at Boulder

  10. Department of Chemical and Biological Engineering Our department has been ranked 19th overall and 10th among public graduate programs by U.S. News & World Report, and ranked 4th in average citations per publication by University Science Indicators. Dr. Christopher N. Bowman Associate Dean for Research, Patten Professor of Chemical and Biological Engineering, Clinical Professor of Restorative Dentistry and Co-Director of the NSF I/UCRC for Fundamentals and Applications and Photopolyme-rizations

  11. Outlines • Introduction • Composites and Nanocomposites • Silica & Silane Coupling Agent • 2. Experimental • - Silanization of Silica Particles • - Characterization • (a) FTIR • (b) TGA • (c) Solid State NMR • - Fabrication of Nanocomposites • (a) Curing Kinetics using Real Time NIR • (b) DMA results • 3. Conclusions

  12. Introduction

  13. 120,000 20,000 Composite Definition: Materials containing at least two constituents that can be physically or visibly distinguished. Any two-phase material can be considered a composite. Composite theory is based the rule-of-mixtures (simple version or modified rule). In almost all cases, the solid dispersed phase is one with the better properties.

  14. Composite

  15. Effect of Fillers Functional fillers transfer applied stress from the polymer matrix to the strong and stiff mineral.

  16. Polymer Nanocomposites

  17. Polymer Matrices

  18. Dimensions of Nanoparticles

  19. Preparation of Nanocomposites

  20. Interaction Zone Particle Why Nanocomposites?  Multi-functionality • Small filler size: • High surface to volume ratio • Small distance between fillers  bulk interfacial material • Mechanical Properties • Increased ductility with no decrease of strength, • Scratching resistance • Optical properties • Light transmission characteristics particle size dependent

  21. Production of Precipitated Silica • Precipitated silica: reaction of an alkaline silicate solution • with a mineral acid Na2(SiO2)3.3(aq) + H2SO4(aq) → 3.3 SiO2(s) + Na2SO4(aq)

  22. Production process of fumed silica 2) Fumed silica Flame pyrolysis of silicon tetrachloride

  23. Fumed Silica

  24. TEM of SiIica (OX-50 & AS380) Formation of aggregates due to high temperature manufacturing process. TEM of Aerosil 380 TEM of Aerosil OX-50 Evonik technical bulletin No. 11

  25. Fumed Silica for Insulating Materials Reliable and most cost-effective way to reduce both energy use and CO2 emissions. Thermal Conductivity vs Total Pressure & Pore Size

  26. Hydrophobic Treatment of Fumed Silica Silica is hydrophilic in due to silanol (Si-OH) groups on the surface. These silanol groups may be chemically reacted with various reagents to render the silica hydrophobic

  27. Properties of Hydrophobic Fumed Silica

  28. Production of Monodisperse Nanoparticles 3) Stöber-Process Hydrolysis Si(OC2H5)4+ 4H2O →Si(OH)4+4C2H5OH Condensation Si(OH)4 →SiO2+ 2H2O both in a NH3 alcohol solution • monodisperse, spherical silica • nanoparticles that range in size • from 5–2000 nm.

  29. Particle-Matrix Compatibility Regardless of filler size and shape, intimate contact between the matrix and mineral particles is essential, since air gaps represent points of permeability and zero strength.

  30. SiIane Coupling Agent General Formula: R: Amino, vinyl, epoxy, chloro, mercapto, methacryloxy, acryloxy, etc.) X: Hydrolyzable group typically alkoxy, acyloxy, halogen or amine. Gelest Catalog 3000-A, Silicon compounds: Silanes & Silicones, p. 166, Gelest Inc.

  31. SiIane Coupling Agent Silane coupling agents have the ability to form a durable bond between organic and inorganic materials. Enhance interfacial adhesion via chemical bonding. Gelest Catalog 3000-A, Silicon compounds: Silanes & Silicones, p. 166, Gelest Inc.

  32. Silane Coupling agent Treatment Modification with organosilane depends on the ability to form a bond with silanol groups, -Si-OH, and/or aluminol groups (-Al-OH) on the filler surface.

  33. Typical Silane Coupling Agents Generally the reactivity differences between methoxy and ethoxy silanes are not a problem. At typical hydrolysis pH (acidic ~5, basic ~ 9), both versions hydrolyze in under 15 minutes at 2% silane concentrations.

  34. Applying a Silane Coupling Agent

  35. Silane Effectiveness on Inorganics Hydroxyl-containing substrates vary widely in concentration and type of hydroxyl groups present.

  36. Silane Coupling agent Treatment SEM photomicrographs of fractured silica-filled epoxy composite a) silica without silane treatment, b) silica with silane treatment.

  37. CO2 Reduction

  38. Established Nanotechnologies

  39. Green Tires – Lower rolling resistance – Fuel economy  lower carbon dioxide emissions  lower global warming impact

  40. Green Tires

  41. Green Tires How can the Silane coupling agent meet the needs? Si-69; Bis-[-3-(triethoxysilyl)-propyl]-tetrasulfide

  42. Green Tires Silica ––Silane: How it Works

  43. Green Tires Silica ––Silane: How it Works

  44. Green Tires – How it works

  45. Silanes to Meet the Need

  46. New Silanes for Silica Tire 1

  47. Green Tires

  48. Experimental

  49. Properties of SiIica (OX-50 & Aerosil 380) • Noncrystalline form of silicon dioxide (SiO2) – Fumed silica • - OX-50: Low specific surface and only slight tendency to agglomerate. ( 2.2 Si-OH/nm2) • - Aerosil 380: Highest specific surface area (2.5 Si-OH/nm2) • Hydrophilic grades. • 2) BET Surface Area [m2/g]: 50 (+-) 15, 380 (+-) 30 • 3) Average primary particle size: 40 nm, 7 nm • 4) Tapped density: 130 g/L, 50g/L • 5 Density: 2.2g/cm3 • 6)Hardness: 5.3–6.5 (Mohs Scale)Fillers for transparent • scratch-resistant coating • 7) Refractive index: 1.46 – Very close to the most organic monomers • 8) Tensile strength: 48.3 MPa • 9) Bulk modulus: ~37 Gpa • 10) Young’s modulus: 71.7 GPa  Fillers for reinforcing

  50. Experimental • Three parameters which will be dealt here: • Filler surface modification • 2) Filler concentration • 3) Particle size and the particle dispersion state. E. Chabert, M. Bornert, E. Bourgeat-Lami, J.-Y. Cavaille, R. Dendievel, C. Gauthier, J. L. Putaux, and A. Zaoui, Materials Science and Engineering A 381, 302-330 (2004)

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