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1 Block Copolymer Mimetic Self-Assembly of Inorganic Nanoparticles Yunyong Guo, Saman Harirchian-Saei, Celly M. S. Izumi and Matthew G. Moffitt* Department of Chemistry, University of Victoria, P.O. Box 3065, Victoria, BC V8W 3V6, Canada. Supporting Information Fig. S1. (A) Structure and 1 H NMR peak assignments of constituent PS-b-PAA-b-PMMA triblock copolymer; (B) 1 H NMR spectra of PS/PMMA-CdS XL ; (C) 1 H NMR spectra of SM-NPs, indicating essentially complete hydrolysis of PMMA chains to PMAA. Both spectra were obtained from the corresponding polymer-coated nanoparticles dispersed in DMSO-d. 1

2 Fig. S2. Refractive index (RI) detector response from gel permeation chromatography (GPC) of (A) PS-b-PtBA-b-PAA starting material, (B) PS/PMMA-CdS XL, and (C) SM-NPs. All chromatograms were run with THF as the eluting solvent. The GPC in A shows the single chains of the triblock copolymer starting material at an elution volume ~14 ml; the weak lower molecular weight peak at ~15 ml is attributed to PS or PS-b-PtBA due to killing during anionic polymerization. In B, the main peak is shifted to lower elution volumes (centered at ~13 ml), attributed to micellization of single chains leading to PS/PMMA-CdS XL ; the slight high elution-volume shoulder indicates a small fraction of unmicellized single chains in the SM-NP sample. Following the hydrolysis of PMMA chains, the GPC in C shows no significant increase in the single chain fraction compared to B; this indicates that the core-crosslinked micelles remained intact during conversion to amphiphilic SM-NPs. 2

3 Fig. S3. Dynamic light scattering (DLS) data for individual SM-NPs dispersed in polar organic solvents. (A) Effective hydrodynamic diameters at various concentrations for SM-NPs in DMF determined from cumulant analysis, with single-particle hydrodynamic diameter (51 nm) obtained from extrapolation to infinite dilution. (B) CONTIN distribution for SM-NPs dispersed in THF at 4.5 mg / ml, showing peak hydrodynamic diameter of ~60 nm. The hydrodynamic sizes of SM-NPs in DMF and THF are consistent with those of PS/PMMA-CdS nanoparticles in solvents in which both blocks are soluble. 1 CONTIN results in THF confirm the absence of aggregates, and indicate that SM-NPs are individually dispersed prior to water addition-induced self-assembly. 3

4 Fig. S4. X-ray powder diffraction (XRD) patterns from (A) SM-NPs (shown in Fig. 2A), (B) spherical supermicelles (shown in Fig. 2, B and C), (C) wormlike assemblies (shown in Fig. 3) and (D) bilayer vesicles (shown in Fig. 6A). The red lines correspond to the (111), (200), (220), and (311) reflections for a cubic CdS lattice structure, showing good overlap with diffraction peaks of the SM-NP building blocks and their various assemblies. The peak observed at 2θ = 30 o in all four diffraction patterns corresponds to a d spacing of 0.56 nm, which is attributed to the mean distance between polymer chains at the core surface of SM-NPs. The core surface area per coronal chain for the mixed brush is calculated from light scattering data to be 1.3 nm 2 / chain, 1 which gives a mean distance of ~1 nm between chains, assuming a square lattice arrangement; therefore, the assignment of the 2θ = 30 o to an interchain distance at the core surface is reasonable. 4

5 Fig. S5. UV-vis absorbance and photoluminescence (PL) spectra of SM-NPs dispersed in THF. The absorbance spectrum shows an exciton shoulder (~450 nm) and an absorption threshold (λ thresh = 502 nm) indicative of quantum confinement effects within SM-NP CdS nanoparticles. The broad emission at ~600 nm (λ ex = 400 nm) is from CdS surface trap states. 2 5

6 Fig. S6. Additional transmission electron microscopy (TEM) images of wormlike assemblies produced by adding 75 wt % water to 1.0 wt % SM-NPs in THF followed by immediate kinetic freezing. The small background particles visible in images A-C are simple spherical micelles (~40 nm) formed from a small percentage of triblock copolymer impurity in SM-NP. 6

7 Fig. S7. Additional high-angle annular dark field (HAADF) TEM images of wormlike assemblies produced by adding 75 wt % water to 1.0 wt % SM-NPs in THF followed by immediate kinetic freezing. In the reverse contrast images, the CdS nanoparticles appear as bright dots. 7

8 Fig. S8. (A) HAADF TEM image of a wormlike assembly. (B) Energy-dispersive X-ray (EDX) spectra corresponding to regions 1, 2 and 3 indicated by white spots in A. The EDX spectrum in region 1 shows strong elemental contribution of Cd and S, confirming CdS nanoparticle localization within the periodic electron-dense disks; only extremely weak Cd and S signals are detected in region 2 (between two disks), and no detectable Cd and S signal is found in the background region (outside of the nanoparticle assembly). 8

9 Fig. S9. (A) Atomic force microscopy (AFM) image of a wormlike assembly on glass. (B) Topology profile for white line in A, along with 3D representation of 2D image data. Both 2D and 3D images show the segmental structure of worms; the lower relative height of the thin CdS nanoparticle / PMAA disks is explained by the decrease in volume of swollen PMAA upon water evaporation. The mean height and FWHM of the assemblies from AFM data are very similar (~500 nm), confirming the cylindrical geometry of the worms. (C and D) Laser scanning confocal fluorescence microscopy (LSCFM) images of wormlike assemblies, with contrast from photoluminescence of constituent CdS nanoparticles. The optimal spatial resolution of the LSCFM instrument is ~200 nm in the xy plane, such that localized photoluminescence from discrete disks of CdS nanoparticles with ~100 nm spacing cannot be resolved even in the higher magnification image in D. 9

10 Fig. S10. (A and B) Equilibrium bilayer vesicles produced by adding 75 wt % water to SM-NPs in THF containing HCl (1.0 wt % SM-NPs, R HCl = 0.8). Bilayer vesicle dimensions are very similar to those obtained via self-assembly in a solution containing NaCl (1.0 wt % SM-NPs, R HCl = 3.0) (shown in Fig. 6A). Mean diameters and wall thicknesses from TEM data are 83 nm and 23 nm, respectively, compared to 93 nm and 24 nm for the vesicles shown in Fig. 6 A. 10

11 Fig. S11. (A) Plot of zeta potential vs. ph for SM-NP vesicles (formed with R NaCl = 3.0). (B) Plot of hydrodynamic diameter vs. ph for SM-NP vesicles (formed with R NaCl = 3.0). Both plots were obtained by titrating acid or base to vary the ph following transfer of the vesicles into pure water; due to the glassy nature of the PS walls, the basic morphology of the vesicles will remain constant during the changes in ph, although the solubilized PMAA corona can expand or contract. The plot in A shows that the zeta potential of the vesicles is negative over the investigated ph range, indicating negative surface charge, and increases in magnitude with increasing ph, consistent with an increase in the degree of ionization of the polyacid external chains. Meanwhile, the plot in B shows that the hydrodynamic diameter of the vesicles increases with increasing ph, as the increase in electrostatic repulsion between PMAA chains leads to higher degrees of stretching within the coronal layer. 11

12 References 1. Guo, Y.; Moffitt, M. G. Semiconductor Quantum Dots with Environmentally Responsive Mixed Polystyrene/Poly(methyl methacrylate) Brush Layers. Macromolecules 2007, 40, Wang, C.-W.; Moffitt, M. G. Surface-Tunable Photoluminescence from Block Copolymer- Stabilized Cadmium Sulfide Quantum Dots. Langmuir 2004, 20,

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