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1 Supporting Information Wiley-VCH Weinheim, Germany Silver Nanocrystals with Concave Surfaces and Their Optical and Surface-Enhanced Raman Scattering Properties** Xiaohu Xia, Jie Zeng, Brenden McDearmon, Yiqun Zheng, Qingge Li, and Younan Xia* anie_ _sm_miscellaneous_information.pdf
2 Experimental Section Chemicals and materials. All chemicals were obtained from Sigma-Aldrich unless specified, and all of them were used as received. Silver trifluoroacetate (CF 3 COOAg, 99.99%), ethylene glycol (EG), sodium hydrosulfide hydrate (NaHS), copper(ii) nitrate hydrate (Cu(NO 3 ) 2, >99.0%), copper(ii) chloride (CuCl 2, >99.0%), copper sulfate (CuSO 4, 99.0%), 1,4- benzenedithiol (1,4-BDT, 98%), poly(vinyl pyrrolidone) (PVP, M W 55,000), L-ascorbic acid (AA, 99.0%), silver nitrate (AgNO 3, >99%). All aqueous solutions were prepared using deionized (DI) water with a resistivity of 18.2 MΩ cm. Preparation of cubic Ag seeds. Silver cubic seeds were prepared using a recently reported polyol process, with EG serving as a solvent and CF 3 COOAg as a precursor to elemental silver. [1] In a typical synthesis, 20 ml of EG was added into 100 ml round-bottom flask and pre-heated under magnetic stirring in an oil bath set to 150 o C, and then 250 µl of NaHS (3 mm in EG) was quickly injected. After 2 min, 2 ml of HCl (3 mm in EG) was injected into the reaction solution, followed by quick injection of 5 ml of PVP (20 mg/ml in EG). After another 2 min, 1.5 ml of CF 3 COOAg (282 mm in EG) was added into the mixture. During the entire process, the flask was capped with a glass stopper, except for the introductions of reagents. The 23, 40, and 60-nm cubic seeds were obtained by quenching the reaction with an ice-water bath when the major SPR peak of the suspensions had reached 405, 440, and 475 nm, respectively. After centrifugation and washing with acetone and DI water twice, the seeds were stored in 5 ml of DI water for future use. Synthesis of Ag concave octahedrons and trisoctahedrons. In a typical synthesis of Ag concave octahedrons, 10 µl of the as-prepared Ag cubic seeds were added into 10 ml of DI water containing 0.3 mm AA that was hosted in a 50 ml glass beaker under magnetic stirring. Then, an aqueous AgNO 3 solution (0.2 mm) was injected at a rate of 10 ml/h using a syringe pump. Aliquots were taken at different reaction stages of the synthesis and then diluted with DI water in cuvettes, followed by recording of their UV-vis extinction spectra. The products at different reaction stages (as indicated in the text) were collected by centrifugation (14,500 rpm for 15 min) and then washed with water once. The typical synthesis of Ag concave trisoctahedrons was similar to what was used for the Ag concave octahedrons except for the addition of 0.8 mm Cu(NO 3 ) 2 into the final reaction solution and an injection volume of 10 ml for AgNO 3 solution.
3 Surface-enhanced Raman scattering. The Ag nanocrystals were functionalized with a 1 mm ethanol solution of 1,4-BDT over a period of 2 h. Ethanol was used to wash the sample several times before the particles were re-dispersed in water to obtain a concentration of 0.5 nm in terms of particles. The Raman spectra were recorded from the suspension using a Renishaw in Via confocal Raman spectrophotometer coupled to a Leica microscope with a 50 objective (N.A. = 0.90) in backscattering configuration. The SERS data were collected with λ ex = 514 nm, P laser 2 mw, and t = 30 s. The light source at 514 nm was generated from an argon cw laser and used with a holographic notch filter based on a grating of 1,200 lines per mm. The backscattered Raman signals were collected on a thermoelectrically cooled (-60 o C) CCD detector. Sample cells were constructed by attaching the cap of a microcentrifuge tube to a glass slide. The cap served as a vessel for the liquid sample, and a glass cover slip ( mm) was carefully placed on top to prevent solvent evaporation and to serve as a reference point from which the focal volume was lowered to a depth of 200 µm into the sample. All data analyses were done with IGOR Pro software (Portland, OR). The data was baseline-corrected before normalization. For the baseline correction, a fourth order polynomial was fitted to the raw Raman spectrum and subtracted. We employed the peak at 1562 cm -1 (the strongest band in the spectra) to estimate the SERS enhancement factor (EF) using the following equation: [2] EF = (I SERS N bulk )/(I bulk N SERS ) Where I SERS and I bulk are the intensities of the same band for the SERS and ordinary spectra from a bulk sample, N bulk is the number of molecules probed for a bulk sample, and N SERS is the number of molecules probed in SERS. N bulk was determined based on the Raman spectrum of a 0.1 M 1,4-BDT solution in 12 M NaOH (aq) and the focal volume of our Raman system (1.48 pl). When determining N SERS, we assumed that the 4-MBA molecules were adsorbed as a monolayer with a molecular footprint of 0.54 nm 2, [3] and a surface area of , , and nm 2 were used for a concave trisoctahedron, a concave octahedron, and a conventional octahedron, respectively, based on the shape and size of the nanoparticles (Figure S2). The N SERS here represents a theoretical maximum number of molecules. Therefore, the actual EF is supposed to be higher than the value reported here. Since 1,4-BDT does not have any absorption at 514 nm, no resonance Raman effect should be involved. Characterizations. The as-prepared samples were characterized by TEM and SEM. TEM S2
4 imaging was performed using an FEI TEM (Tenai G2 Spirit Twin, Hillsboro, OR) operated at 120 kv. An FEI field-emission SEM (Nova NanoSEM 230, Hillsboro, OR) was used to image the Ag nanocrystals operated at 15 kv. High-resolution TEM analyses were performed using a JEOL 2100F microscope operated at 200 kv accelerating voltage. The concentrations of Ag ions were determined using inductively-coupled plasma mass spectrometry (ICP-MS, Perkin Elmer Elan DRC II), which could be converted to the particle concentrations of Ag nanocrystals once the particle sizes and morphologies had been determined by TEM and SEM imaging. Extinction spectra of all the nanocrystals were recorded using a UV-vis spectrophotometer (Varian, Cary 50). S3
5 Figure S1. TEM images of Ag cubic seeds with different average edge lengths: (a) 40, (b) 23, and (c) 60 nm, respectively. S4
6 Figure S2. Definition of size (L) for (a) a concave octahedron, (b) a concave trisoctahedron, and (c) a traditional octahedron. The estimate of surface area (S) for each type of particle is listed below each model. S5
7 Figure S3. SEM images of (a) Ag concave octahedrons and (b) Ag concave trisoctahedrons at a lower magnification relative to the images shown in Figure 1a and Figure 2a, respectively. Insets shows individual nanocrystals at a higher magnification, with the scale bars being 20 nm. S6
8 Figure S4. (a) A model of the concave trisoctahedron viewed along the <110> direction. The 4 edge-on facets out of the 24 facets of a trisoctahedron are marked with arrows. (b) A table showing the values calculated for angle α when the concave trisoctahedron is bounded by different facets. (c, d) TEM images of two concave trisoctahedrons with α = 130 and 154, respectively, indicating that the edge-on facets of the particles shown in (a) were {331} and {332} planes, respectively. S7
9 Figure S5. (a, c) SEM images of Ag concave octahedrons with average sized of (a) 32 nm and (c) 120 nm that were prepared using the 23- and 60-nm cubic seeds (see Figure S1b, c), respectively. (b, d) SEM images of Ag concave trisoctahedrons with average sized of (b) 45 nm and (d) 150 nm that were prepared using the 23- and 60-nm cubic seeds, respectively. S8
10 Figure S6. SEM images taken from samples of the standard syntheses for Ag concave octahedrons and trisoctahedrons after (a) 7.0 ml and (b) 14 ml of AgNO 3 solution had been added into the reaction, respectively. S9
11 Figure S7. SEM images of Ag nanocrystals that were prepared using the standard procedure for Ag concave octahedrons except for the variation in concentration of AA: (a) 0.05 mm, (b) 0.2 mm, and (c) 2 mm. S10
12 Figure S8. UV-vis spectra of aqueous suspensions of the Ag nanocrystals shown in Figure 3. Dash curves in (a) and (b) represent the UV-vis spectra of an aqueous suspension of the 40-nm Ag cubic seeds (Figure S1a). S11
13 References [1] Q. Zhang, W. Li, L. P. Wen, J. Chen, Y. Xia, Chem. Eur. J. 2010, 16, [2] K. Kim, J. K. Yoon, J. Phys. Chem. B 2005, 109, [3] a) S. W. Joo, S. W. Han, K. Kim, J. Colloid Interface Sci. 2001, 240, 391; b) S. H. Cho, H. S. Han, D. J. Jang, K. Kim, M. S. Kim, J. Phys. Chem. 1995, 99, S12
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