Motivation: Biofunctional Composite Nanoparticles
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2 Motivation: Biofunctional Composite Nanoparticles Iron Oxide Core Magnetic core Alternating magnetic field Brownian and Neél relaxation Bi-Material Composites MRI contrast enhancement and RF thermal tumor treatment Tri-Material Composites Gold Silica Iron Oxide Silica and Gold Coating Gold conductive nanolayer on silica insulating layer Surface plasmon resonance Tuned infrared resonance for laser ablation of tumors Review Paper: Melancon, M. P., W. Lu, et al. (2009). "Gold-Based magneto/optical Nanostructures: Challenges for In Vivo Applications in Cancer Diagnostics and Therapy." MRS Bulletin 34(June). 2
3 Nanotechnology Applications in Energy Catalytic Treatment of Exhaust Reduction of CO in exhaust Production of H 2 for NO x Treatment Fuel Cells Catalysts for proton exchange membranes Catalysts for direct methanol fuel cells Fuel Production Hydrogen from biomass Hydrogen from water Liquid fuels from biomass Astruc, 2008 Zhong et. al, 2010 Nanotechnology Current synthesis techniques rely heavily on wet-chemistry methods. Mor et. al, 2004 Nanoletters
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5 Silica Coated Silver Synthesis Schematic Photoinduced Chemical Vapor Deposition (Photo-CVD) Gold or Silver Dilution N 2 Bipolar Charger N 2 Evaporation Furnace Sintering Furnace Chamber Furnace Polydisperse Aerosol DMA1 Monodisperse Aerosol CaF 2 Window N 2 lamp cooling U.V. Excimer Lamp λ=172nm Coating Chamber Filter Bipolar Charger + - Electrostatic Precipitator DMA2 N 2 Purge N 2 Carrier Gas Xe 2 * CPC TEOS Bubbler DMA Differential Mobility Analyzer TDMA Tandem Differential Mobility Analyzer CPC Condensation Particle Counter
6 Silica Coating of Silver Nanoparticles N 2 Metal Evaporation Coating Chamber Charger DMA U.V. Excimer Lamp λ =172nm Xe 2 * Charger DMA N 2 Carrier Gas Repeatable 1 hour 5 nm CPC Silica Precursor Bubbler 40 nm (2.5 nm coating) 6 Boies et al. (2009) Nanotechnology
7 Silica Coating Thickness on Silver Nanoparticles Purge Flow Residence Time Concentration Coating Thickness 7 Boies et al. (2009) Nanotechnology
8 Coating Chemistry Infrared (IR) Spectroscopy Increased Oxygen Si-O-Si 300 C OH C-H C-H Si-O-Si Si-O Si-O(H) C-H Peak CH 3 Other hydrocarbons OH Note: Oxygen in excess of 5.1 sccm causes nucleation O sccm O sccm O sccm O sccm 8 Boies et al. (2009) Nanotechnology
9 Energy-Dispersive X-Ray (EDX) Verification of Coating Dark- (a) and bright- (b) field images EDX Line Scan of Core-Shell Particle Particles coated at 300 C 9 Boies et al. (2009) Nanotechnology
10 Polydisperse Ag particles produced at 10 7 #/cm 3 Uncoated Coated Sintered Particles Unsintered Particle Cores Particles processed at 400 C 10 Boies et al. (2009) Nanotechnology
11 Coating Thickness (nm) Coating Thickness (nm) Ag Particles Silica Coating 30 nm 40 nm D p,i = 20 nm Photo-CVD Coating NaCl particles Indicative of Diffusion Limited Growth MMA Coating D p,i = 20 nm 30 nm 40 nm 2 1 Indicative of Reaction Limited Growth nm 50 nm TEOS Flow Rate (sccm) MMA Flow Rate (sccm) Adapted from Bin Zhang s Dissertation Diffusion Limited Growth Theory Continuum Regime (Kn<0.1) 1/D p Growth Free Molecule Regime (Kn>10) No Dependence At Atmospheric Pressure, 20 nm Kn=6.5, 30 nm Kn=4.3, 40 nm Kn=3.3 Kn 2λ/D p Kn - Knudsen number λ - Mean free path 11
12 Hot-Wire Gold Particle Production Schematic N 2 98 mm 20 mm 3 mm + - Po Charger Condensation Particle Counter Electrostatic Precipitator - + Differential Mobility Analyzer Au Shell 3 μm mm Pt Core R - Resistance 12
13 Gold Decoration of Silica N 2 TEOS Bubbler N 2 +O 2 Dilution N 2 Decomposition Furnace Sintering Furnace Silicon Dioxide Nanoparticle Production Path A Path B Tube-Furnace Evaporation + - Gold Production Hot-Wire Evaporation Agglomeration Chamber Collection & Characterization a) b) c) Particle size distribution of gold-decorated silica nanoparticles at different residence times 13 Boies et. al, 2010 J Aero Sci
14 Hot-Wire Evaporation Decoration: Densification of Coating Densified Gold Decoration Collected after TDMA High Density Gold Islands Remain 14
15 UV-Vis Spectra of Gold Decorated Silica 15
16 Gold Mobility on Particle Surface at Elevated Temperature 20 C 274 C 438 C 609 C 811 C 906 C 957 C 1040 C 16
17 Gold Mobility on Particle Surface at Elevated Temperature At Low Temp At 957 C 17
18 Tri-Layer Nanoparticle Synthesis Ejector U.V. excimer lamp Fe precursor TEOS bubbler + - Plasma torch Iron oxide production Silicon dioxide coating Gold coating Collection/ Characterization 18
19 Core: Iron Oxide Production Particles 3-5 nm Magnetization Production rate ~mg/min 19
20 Shell 1: Silica Coating TEOS Flow Particle Size 0.28 sccm TEOS 0.62 sccm TEOS 0.05 sccm TEOS 0.94 sccm TEOS No TEOS 1.23 sccm TEOS Similar to Coating of Silver Nanoparticles 7 slm N 2 Purge Flow 20
21 Shell 3: Gold Decoration Silica Shell Au Particles Silica Shell Iron Oxide Core Iron Oxide Core 21
22 Synthesized Composite Nanoparticles Silica Coated Iron Oxide Tri-Layer Gold, Silica, Iron Oxide Organic Coated Aluminum Au Particles Silica Shell Iron Oxide Core Silica Shell Iron Oxide Core Organic Shell Boies et. al, In Prep Nanotech Platinum Decorated Silica Boies et. al, In Prep Nano Let Organic Coated Sodium Chloride He et. al, In Prep J Nanopart Res Silver Decorated Silica Silica Core Organic Shell NaCl Core Silver Decoration Platinum Decoration Boies et al., Not Published Zhang et. al, 2006 J Nanopart Res Silica Core 10 nm 22
23 Future Directions 23
24 Gas Flow Homogenous Mixed Metals Spark Discharge Different Anode and Cathode Materials Evaporation, Dissociation N. Tabrizi, Q. Xu, N. van der Pers, U. Lafont, A. Schmidt-Ott, Synthesis of mixed metallic nanoparticles by spark discharge. Journal of Nanoparticle Research 2010, 11, Mixed Metal Core-Shell Nanoparticles Metal Precursor Thermal or Plasma Dissociation Nucleation Organometallic Precursor Ultraviolet Radiation Collection 24
25 Possible Morphologies Bi-Material Composites Tri-Material Composites Materials of Interest Gold Platinum Rubidium Iron Nickel Iron Oxide Titanium Oxide Carbon On-Line Testing of Catalytic Properties Polydisperse particles Differential Mobility Analyzer Size selected particles CO CO Detection jmwlimited.co.uk 25
26 Gas Flow Gas Flow Catalyst Decorated Nanoparticle Substrates Carbon Nanoparticles or Nanotubes Decorated with Gold and Platinum Thermal Methane Nucleation Evaporation Condensation Impaction Dissociation Heat/Photo Methane or CO Evaporation Condensation Impaction Dissociation Fuel Cell MetOH or H 2 in MetOH or H 2 out Catalyst electrode layer Gas diffusion layer Polymer Electrolyte Membrane Gas diffusion layer O 2 or air in O 2 or air out Critical Parameters to Study Control of particle size and morphology of decoration Catalytic effect of varying platinum and gold and other metal compositions Film formation of particles by impaction Production rate and quality of core 26 particles and nanotubes
27 Acknowledgements Funding Sources National Science Foundation Grant Nitto Denko Technical Corporations 3M Science and Technology Fellowship University of Minnesota Doctoral Dissertation Fellowship Institute of Technology Characterization Facility, a NSF-funded Materials Research 27
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