NMR at the Nanocomposite Interface
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1 NMR at the Nanocomposite Interface Peter A. Mirau Nanostructured and Biological Materials Branch Materials and Manufacturing Directorate, WPAFB
2 2 Overview Applications Polymer/C60 Interaction Nanoparticle Liquids Peptide/Inorganic Interface Conclusion
3 3 NP at AFRL Power & Energy Photovoltaic Dielectric Energy storage Optical Metamaterials Biomimetric NP synthesis Recognition
4 4 Nanostructured Materials NanoStructured Hybrids Responsive & Self-OscillatingSurfaces In-Situ Structure- Property NP Fabrication Structure and Dynamics of Corona Ag Au
5 Optical density 5 NP Synthesis & Assembly Nanoparticle Growth and Interface Development multi-component, multi-valent organic & biomacromolecular coronas inorganic hybrid synthesis, theory, and characterization Ag +1 AA Ag +1 AA Ag +1 Ag +1 AA AA Au-Ag core-shell Mother Increasing thickness of Ag shell Wavelength(nm)
6 Biological Materials 6
7 Bifunctional NP 7
8 Peptide Recognition 8
9 NC for Energy Harvesting 9
10 Nanostructures for Devices 10
11 CNT Spectra 11 CNT Introduction H H H Polymer Spectra
12 12 C 60 Blends Poly(ethylene oxide) Methanol ppt Poly(9-vinyl carbazole) Polystyrene
13 Intensity (AU) 13 C60 Polymer Blends X-ray PS/C 60 C PS
14 14 Intermolecular CP H TPPM X CP H C
15 15 C 60 Blends 5 ms CH 2 CH 0.1 ms Chemical Shift (ppm) 50 0
16 16 C 60 Dynamics fcc Tycko et al. Phys.Rev. Lett
17 17 CSA Filter H TPPM X CP CSA CSA r r 18 khz 20 khz 3.8 khz Chemical Shift (ppm) 0-50 Mao & Schmidt-Rohr SSNMR 2004, 26, 36
18 18 C 60 Dynamics PS Blends CH 2 CH (b) CSA Filter (a) CPMAS Chemical Shift (ppm) 50 0
19 19 C 60 Dynamics PS Blends N [ CH 2 CH ] Chemical Shift (ppm) 80
20 20 NP Interfaces Synthesis and Characterization of Janus Nanostructures Adsorption and Phase Behavior of Immiscible Ligands Characterization of NP Interfaces Kyoungwoen Park, Folusho Oyerokun, Rich Vaia - RXBN; Igor Altfeder - RXBT Bridging Analysis Capabilities (RXBT-RXBN) Folusho Oyerokun, Kyoungwoen Park, Rich Vaia, P. Mirau - RXBN NP Liquids as MEMS Lubricants A.Voevodin, S. Patton RXBT; R.Vaia, P. Mirau, A. Elsen, J. Kelley -RXBN
21 21 Nanoparticle Liquids Liquid Properties Warren, S. C. et al. J. Am. Chem. Soc. 2006, 128, Core material, corona, and canopy can all be varied to access a range of NPLs tailored to specific applications.
22 22 Au NPL for MEMS + 50 nm Low vapor pressure: little volatile organic content Thermal stability: noble metal core structures Liquid properties: processability
23 Au NPL s for MEMS Improved switch lifetime by a factor of S. T. Patton, et al. Tribology International 2001, 34, Failure was not observed over the course of the experiment. A. Voevodin, et al. Small 2007, 3,
24 24 SiO 2 Nanoparticle Liquids Corona core + Corona corona + Canopy + canopy Ethomee n 100 nm -Canopy +Canopy (Jespersen, Rodriguez, Giannelis)
25 25 Preparation of Silica NPLs Commercially-Available Jeffamines XTJ ph vs. Weight Percent SiO 2 HS30-SIT M-2070 HS30-SIT XTJ-506 HS30-SIT XTJ wt. % ph 6 4 HS30-SIT M wt. % 2 M SiO 2 (wt. %) R. Rodriquez E. Giannellis (Cornell U)
26 26 NPL NMR (a) (b)
27 C(t) 27 T 1 Relaxation C H S Correlation Time (s)
28 28 T1 vs. Temperature T 1 vs. Temperature Methylene Carbons SiO 2 NPL A M-2070 Similar T 1 vs. temperature curves S 2 r Methylene dynamics are insensitive to SiO 2 NP
29 M(G) 29 PFG Diffusion M=M e G D 0 ( /3) 10 0 zg z zg z x y x y ( G) 2 ( - /3) x 10 9
30 30 PFG-NMR Diffusion Results SiO 2 NPL A Sample (Solvent) D M (D 2 O) NPL A (D 2 O) M-2070 (Neat) NPL A (Neat) kt B r H Viscosity (Pa-s) D (m 2 /s) r H (nm) x x x x In both D 2 O and in neat form, the diffusion coefficients are very similar. M-2070 Calculated hydrodynamic radii are the same.
31 31 Canopy Exchange in NPL s Canopy diffusion is 20x faster than NP diffusion
32 32 Biopolymers at the Interface Biomimetics Encapsulated Enzymes DNA Optics/Electronics NPSSLFRYLPSD Sequence/Structure Templating Recognition Structure/Function Transport Organization DNA Conformation Morphology Thin Film Structure
33 33 TiO 2 Binding Peptide Identified by phage display RKLPDAPGMHTW binding controlled by 6 N-terminal residues binds TiO 2, SiO 2, Ag NP (+) (+) (-) (+) Arg-Lys-Leu-Pro-Asp-Ala (-) Sano, K. I.; Sasaki, H.; Shiba, K. Langmuir 2005, 21,
34 34 Peptide Binding to NP H H Possible Results No binding Binding/Fast exchange Binding/Slow exchange H H
35 35 RKLPDA NP Binding A L + 25 nm TiO nm SiO Chemical Shift (ppm) 1 0.5
36 36 RKLPDA NP Binding LNH D NH A NH + 25 nm TiO nm SiO Chemical Shift (ppm) 7.5 7
37 Intensity 37 Binding Mode t t 1 m H H Fast Motion Limit Slow Motion Limit Correlation Time (s)
38 Chemical Shift (ppm) Chemical Shift (ppm) 38 RKLPDA NOESY 0 RKLPDA RKLPDA/TO Chemical Shift (ppm) Chemical Shift (ppm) Binding with fast exchange
39 Chemical Shift (ppm) 39 RKLPDA/TiO 2 Structure 0 1 NH 2 H 3 4 H Chemical Shift (ppm) 7
40 40 Summary & Conclusion Solution and solid-state NMR can be used for the characterization of a wide variety of materials Polymer Nanocomposite Interfaces Nanoparticles Biomimetic Composites and provides molecular-level information about the Structure Conformation Dynamics Transport
41 41 Acknowledgments Silica Nanoparticle Liquids Mike Jespersen, Prof. Emmanuel Giannelis (Cornell), Robert Rodriguez (Cornell), Rich Vaia (RXBN) Gold Nanoparticle Liquids Mike Jespersen, Andrey A. Voevodin (RXBT), Rich Vaia (RXBN), Steven T. Patton (UDRI/RXBT), Robert I. MacCuspie (NIST), Andrea Elsen (SOCHE), John Kelley (SOCHE) Peptide/Inorganic Binding Larry Drummy (RXBN), Melanie Tomczak (RXBN), Rajesh Naik (RXBN), Rich Vaia (RXBN),Henrik Heinz (U Akron) and Rajiv Berry(RXBN)
42 42 Clay-Binding S2 Peptide (+) (+) (+) His-Gly-Ile-Asn-Thr-Thr-Lys-Pro-Phe-Lys-Ser-Val (-) 1 nm 80 nm 20 nm nm Laponite Montmorillonite
43 43 S2/Clay Binding MMT LRD Chemical Shift (ppm) 7 6.5
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