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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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