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    Experiments

    Synthesis of Nano Particles and

    Encapsulation

    Synthesis of Hexagonal Mesoporous

    Silica & Carbon

    Synthesis of Organic and Carbon

    Xerogels

    Synthesis of Silver NanoWires

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    Demostration Experiments

    Sol-Gel Synthesis via TMOS

    Sol-Gel Synthysis using Sodium silicate

    better known as furnace cement.

    Ultrasonic synthesis of TMOS

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    SOL-GEL SCIENCE

    Gelification

    Aging

    Soaking

    Mix the reactives

    Sol

    Gel

    Gel Aerogel

    Hydrolysis and Condesation

    reactions take place

    Gelification

    Aging Drying

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    Gelification

    Mix reactives

    Sol

    Gel

    Gel

    Gelification

    Aging

    SiOR

    OR

    OR

    OR

    OH2+ ROH+SiOH

    OROR

    OR

    + + ROHSiOR

    OROR

    OR

    SiO

    Si

    OR OR

    OR OR

    OR OR

    SiOH

    OROR

    OR

    + OH2SiOR

    OR

    OH

    OR

    SiOH

    OR

    OR

    OR

    + SiO

    Si

    OR OR

    OR OR

    OR OR

    Hydrolysis and Condesation

    reactions take place

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    Designing Nanomaterials

    First Step

    Silica Solution

    Precursor: Tetraetilortosilicate

    Si(OCH2CH3)4Solvent: Ethanol

    Catalyst: OxalicAcid

    ModificationspH (final product)Temperature (crystal phase)Precursor (Type of material)

    Time (Strength)

    etc

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    (I) SOL-GEL SYNTHESIS OF AEROGELS

    Aerogels are a unique, nanostrutured material derived from gels. Gels are a novel class

    of material exhibiting solid-like behavior although consisting predominantly of a liquid phase.Their solidity derives from a continuous interpenetrating framework that, in essence, acts like a

    molecular scaffold extending throughout the liquid. This perspective of a gel as a molecular

    web in a liquid has found many industrial applications.

    Figure 1: A silicon oxide low density aerogel

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    Synthesis of Nano Particles and

    Encapsulation Synthsis of Tiatnium and silica

    nanoparticles

    Sol-Gel Encapsulation

    Jorge Arias

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    Encapsulated Dendrimer

    The following figure shows mono dispersed

    Starburst PAMAM polyamidoamine dendrimersencapsulated in a sol-gel matrix of silica at 25 wt.

    %. Surface area analysis shows the material

    surface area was 617 m2/g. The dark spheres in

    Figure 1 dispersed throughout the silica matrixshow diameters similar to their hydrodynamic

    values for this dendrimer in solution.

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    PAMMA Dendrimer

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    Sol-Gel Encapsulated Dendrimer

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    Synthesis of Hexagonal

    Mesoporous Silica & Carbon

    This lab couples the hydrolysis andcondensation of TEOS or other silica

    sources with Structure directing agents suchas surfactants or polymers .

    It also uses the final silica mesoporousmaterial as a template to synthesize a high

    surface area, hexagonal pure carbonmaterial.

    Phong Nugyen, instructor

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    The uniqueness of surfactant templated materials allows a variety of metal oxides to be

    formed with uniform honeycomb structure and surface area approaching 1000 m2/g.

    Surfactant templated materials have already been synthesized by the authors Thesematerials were synthesized with Mg, Cr, Ru, Pt, and Co doped in the MCM-41 silica

    oxide.

    MESOPOROUS ZEOLITE-TYPE MATERIALS

    FIGURE 7. TEM of MCM-41 synthesized by the author

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    FIGURE 8: TEM of mesoporous silica with different average poressizes

    Synthesis of large Scale Mesoporous Substrates

    (A) 60, (B) 89 , (C) 200 , (D)260 .

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    Synthesis of Organic and

    Carbon Xerogels Resorcinol is a molecule that much like TEOS can

    undergo hydrolysis and condensation reaction to

    form a gel structure that can be dry as a xerogel oraerogel.

    This gel can be further transformed in to a high

    surface area carbon material. It gives the highest

    capacitance per unit volume .

    Laurent Moch will demonstrate.

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    Synthesis of Silver NanoWires

    Particles are templated into a cylindrical

    shape using a polymer.

    Martina Dreyer.

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    Synthesis of Silver NanoWires

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    Figure 5: Anodized Alunminum

    NANOSTRUCTURED ANODIZED ALUMINUM

    Anodized aluminum is an ideal substrate in that it possesses verticalpores perpendicular to its surface.These nanopores are formed byelectrochemical etching and pore diameter can be precisely controlledfrom 300 nm down to 2nm.

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    Figure 6: Diagram for using anodized aluminum to synthesize carbon nanotubes

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    FIGURE 4: Nanotube Reactor for CVD Synthesis of Carbon Nanobes in Our

    Laboratory

    Reactors CVD Synthesis of SWNTs

    Two parallel thermal reactors capable have already been constructed and tested,

    These carbon nanotube reactors can operate from 100 torr to above atmosphericThe reactors temperature is computer controlled and may be ramped.

    The reactors are set up to run either in parallel or separately

    One of the reactors can handle large substrates such as silicon wafers up to 6

    inches.

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    (II) CARBON NANOTUBES

    Below is pictured a diagram of the unique geometry of a carbon nanotube as well as a transmission electronmicrograph of a single wall nanotube produced in our department.

    FIGURE 2: Open Nanotube (Newman)

    At 100-150 times the strength of steel yet only 1/60th of its weight, nanotubes are being recognized as thepenultimate fiber with a promise for material technology far surpassing all previous fibers yet created. This promise,as noted, is far beyond just the properties obtained with carbon fibers, now used in the highest performancecomposites. Potentially, future airplanes formed from

    CARBON NANOTUBE TEM OF NANOTUBE

    FIGURE 3: Nanostructure and TEM of single wall nanotube as synthisized


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