APPLIED CHEMICALS AND MATERIALS DIVISION Lauren F. Greenlee Hope A. Weinstein, Michael Voecks, Katie Estoque, Nikki S. Rentz, Nicholas M. Bedford Iron Nanoparticle Synthesis and Immobilization 200 nm Advances in Materials and Processes for Polymeric Membrane Mediated Water Purification Pacific Grove, CA February 18, 2015
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APPLIED CHEMICALS AND MATERIALS DIVISION
Lauren F. Greenlee
Hope A. Weinstein, Michael Voecks, Katie Estoque, Nikki S. Rentz,
NIST mission:To promote U.S. innovation and industrial competitiveness by advancing measurement science, standards, and technology in ways that enhance economic security and improve our quality of life.
DMAC: slow outflux of solvent = fast influx of non-solvent = delayed demixing, macrovoid formation & larger polymer precipitates/aggregates form
DMSO: fast outflux of solvent = slow influx of non-solvent = reduction in macrovoid formation, smaller polymer precipitates, cellular or nodular structures form
Flux decreases with increasing PES-solvent solubility
AcknowledgementsProf. Andrew Herring & lab members, Colorado School of MinesProf. Matthew Liberatore & lab members, Colorado School of MinesNIST TEM – Roy Geiss, Alex Curtin, Ann Debay, Taylor WoehlNIST XRD – Justin ShawCU TEM – Tom GiddingsNIST/Argonne HE-XRD: Nicholas Bedford
Effect of stabilizer properties on Fe NP oxidation in water
200 nm
DTPMP prevents Fe NP oxidation in flowing water.
Stabilizer size and chelator strength appear to affect NP oxidation in water.
APPLIED CHEMICALS AND MATERIALS DIVISION
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ENGINEERED NANOPARTICLE SYSTEMS
Size Control of Bimetallic FeNi Nanoparticles
200 nm
100 nm
0.05 mol ATMP:mol Fe
0.8 mol ATMP:mol Fe
APPLIED CHEMICALS AND MATERIALS DIVISION
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ENGINEERED NANOPARTICLE SYSTEMS
0
0.04
0.08
0.12
0.16
0.2
Vis
cosi
ty (
Pa*
s)Membranes: How do nanoparticles change casting solution properties?
Viscosity: Higher viscosity tends to slow kinetics of phase inversion due to slower diffusion of solvent and non-solvent; slower demixing = reduction in macrovoids
No Nanoparticles
1% 5% 15% 25%
15% PES in DMAC
1% Nanoparticles
1% 5% 15% 25%
EtOH Vol. %EtOH Vol. %
APPLIED CHEMICALS AND MATERIALS DIVISION
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ENGINEERED NANOPARTICLE SYSTEMS
Cloud point measurement: Thermodynamic stability & polymer solubility
0
5
10
15
20
25
30
35
No
n-S
olv
en
t A
dd
ed
(m
l)
No Nanoparticles
1% 5% 15% 25%
15% PES in DMAC
1% Nanoparticles
EtOH Vol. %
1% 5% 15% 25%
EtOH Vol. %
Cloud point: Thermodynamic stability of solution – lower stability of polymer-solvent solution = lower polymer solubility, increased outflux of solvent and decreased influx of non-solvent = reduction in macrovoid formation
APPLIED CHEMICALS AND MATERIALS DIVISION
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ENGINEERED NANOPARTICLE SYSTEMS
Membrane lifetime: PES with iron nanoparticles
PES
1 µm2 µm
400 nm
Before filtration After filtration
After filtration
Significant flux decline & surface
degradation
100 nm
Before filtration
APPLIED CHEMICALS AND MATERIALS DIVISION
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ENGINEERED NANOPARTICLE SYSTEMS
Advanced Photon Source, Argonne Nat’l Lab: A Synchrotron Facility
Stats:
• Circumference: 3,622 ft. (0.69 miles)
• 35 experimental sectors• >1000 bending magnets• Electron energy:
• Linear accelerator: 450 MeV
• Booster synchrotron: 7 GeV
• X-rays: 3 keV – 100 keV
e-
X-rays
APPLIED CHEMICALS AND MATERIALS DIVISION
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ENGINEERED NANOPARTICLE SYSTEMS
X-Ray Absorption Spectroscopy (XAS)
Information Obtained:Element-specific chemical state: Coordination #, oxidation state
X-Ray Absorption Near Edge Structure (XANES)
Extended X-Ray Absorption Fine Structure (EXAFS)
X-Ray Absorption Spectroscopy (XAS)
Single Scattering:Who is my neighbor?-Atomic pair distribution-Modeling of interatomic distances
Multiple Scattering:Who is my neighbor?-First coordination sphere
ENGINEERED NANOPARTICLE SYSTEMSPDF Results for Peptide-Enabled Pd Nanoparticles
1 nm
Pd4 A6 A11
A6,11 C6 C11
C6,11 C6A11 A6C11
Clear sequence-dependence structural differences
APPLIED CHEMICALS AND MATERIALS DIVISION
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ENGINEERED NANOPARTICLE SYSTEMS
Viscosity: Effect of nanoparticles, pore former, and non-solvent
0
0.04
0.08
0.12
0.16
0.2
Vis
cosi
ty (
Pa*s
)
CMC
ATMP
No NPs
Higher viscosity tends to slow kinetics of phase inversion due to slower diffusion of solvent and non-solvent; slower demixing = reduction in macrovoids
15% PES 15% PES2% PVP
15% PES2% PVP5% EtOH
15% PES2% PVP25% EtOH
15% PES5% EtOH
15% PES25% EtOH
APPLIED CHEMICALS AND MATERIALS DIVISION
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ENGINEERED NANOPARTICLE SYSTEMS
Nanoparticle Catalysis
Lee and Sedlak. (2008) ES&T 42, 8528-8533.Chun et al. (2010) ES&T 44, 5079-5085.Alayoglu and Eichhorn (2008) JACS 130, 17479–17486.Sasaki et al. (2012) Nature Communications, 3, 1115.