Synthesis of Uniform Hollow Oxide Nanoparticles. through Nanoscale Acid Etching

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1 Supporting Information Synthesis of Uniform Hollow Oxide Nanoparticles through Nanoscale Acid Etching Kwangjin An, Soon Gu Kwon, Mihyun Park, Hyon Bin Na, Sung-Il Baik, Jung Ho Yu, Dokyoon Kim, Jae Sung Son, Young Woon Kim, In Chan Song, Woo Kyung Moon, Hyun Min Park, and Taeghwan Hyeon*, National Creative Research Initiative Center for Oxide Nanocrystalline Materials, and School of Chemical and Biological Engineering, Seoul National University, Seoul , Korea. School of Materials Science and Engineering, Seoul National University, Seoul , Korea. Diagnostic Radiology, Seoul National University Hospital, and the Institute of Radiation Medicine, Medical Research Center, Seoul National University, Seoul , Korea. New Material Evaluation Center, Korea Research Institute of Standards and Science, Taejon , Korea. Experimental Section Chemicals Trioctylphosphine oxide (TOPO, 90% technical grade, Aldrich), trioctylphosphine oxide (TOPO, Aldrich, 99%), 1-octadecene (Aldrich, 90%), methylphosphonic acid (MPA, Aldrich, 98%), n-hexylphosphonic acid (HPA, Alfar aesar), n-tetradecylphosphonic acid (TDPA, Alfar aesar, 98%), and n- octadecylphosphonic acid (ODPA, Alfar aesar) were used as received without further purification. Synthesis of metal oxide nanocrystals Monodisperse MnO, Fe 3 O 4, and MnFe 2 O 4 nanocrystals were synthesized by a thermal decomposition method described in Nat. S1

2 Mater. 2004, 3, Monodisperse α-fe 2 O 3 nanocubes were synthesized by a method reported in J. Phys. Chem. C 2007, 111, Synthesis of hollow oxide nanoparticles 4 ml of a dispersion of 18 nm-sized MnO nanocrystals in n-hexane ([Mn]=0.5 M) was added to 10 g TOPO of the technical grade under vigorous stirring, and the solution was degassed under vacuum for 1 hr to remove n-hexane and air. Then, under argon atmosphere, the MnO nanocrystals solution was heated up to 300 o C and maintained at that temperature for 2 hr. During the reaction, the mixture solution became transparent. Hollow intermediates with inner core in a wall were sampled from the solution at 30 min after the mixture became transparent. After cooling down to room temperature, hollow oxide nanoparticles were precipitated with 30 ml of acetone and 20 ml of methanol and collected by centrifugation. The precipitate was re-dispersed in chloroform or n-hexane. Fe 3 O 4 and MnFe 2 O 4 nanocrystals and α- Fe 2 O 3 nanocubes were also used as the starting metal oxide nanocrystals. Controlled etching experiments using phosphonic acids 0.05 g of MPA or HPA, or 0.1 g of TDPA or ODPA was added to 4 g of highly pure TOPO (99%). To this mixture, 1.6 ml of a dispersion of 18 nm-sized MnO nanocrystals in n-hexane ([Mn]=0.5 M) was added and n-hexane was evaporated under vacuum. The mixture was heated at o C (MPA and HPA) or 250 o C (TDPA and ODPA) for hours. Characterization The resulting nanoparticles were analyzed with transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), energy dispersive X-ray analysis (EDX), electron energy loss spectroscopy (EELS), and superconducting quantum interference device (SQUID). The TEM images were taken with a JEOL JEM-2010 transmission electron microscope operating at 200 kv. Samples were prepared by putting a drop of the particle dispersions onto a carbon-coated copper grid. XRD patterns were obtained using a Rigaku D/Max-3C diffractometer equipped with a rotation anode and a Cu K α radiation source (λ = nm). The phase identification was performed using JCPDS-ICDD 2000 software (The International Centre for Diffraction Data; ICDD). The XPS experiment was performed on Sigma Probe (ThermoVG) model spectrometer equipped with a microfocused monochromator X-ray source running at 15 kv, a spherical sector analyzer, and a multichannel detector. The elemental mapping was performed using a FEI Technai F20 scanning transmission electron microscope equipped with EDX detector and EELS. The magnetic properties were studied using a magnetic property measurement system (MPMS) 5XL Quantum Design SQUID magnetometer. Measurement of spin relaxation enhancement of hollow nanoparticles in magetic resonance imaging Water-dispersible and biocompatible hollow oxide nanoparticles S2

3 were prepared according to a reported method described in Angew. Chem., Int. Ed. 2007, 46, 1-6. Hollow oxide nanoparticles dispersed in chloroform were encapsulated in a polyethyleneglycol(peg)-phospholipid shell to make them biocompatible. Magnetic resonance imaging (MRI) of phantoms was performed under wrist coil and a 1.5T MR scanner (Sigma Horizon; GE Medical Systems, Milwaukee, Wis) using T 2 -axial images. The sequence parameters were; repetition time = 5000 ms, effective echo time = 90 ms, field of view (FOV) = mm, flip angle = 90, matrix = , slice thickness = 2.0 mm, and slice separation = 0 mm, number of excitations (NEX) = 3.0. T 2 were measured by using a conventional spin-echo (repetition time (T R ) / echo time (T E ) = 5000 ms/15, 30, 45, 60, 80, 160, 240, 320, 400, 800, 1200, 1600 ms) and gradient-echo sequences (T R /T E = 1000 ms/4.16, 11.15, 18.14, 25.14, 32.13, ms) with one echo for each sequence, while varying the T E. T 1 and T 2 were calculated by fitting the decreased signal intensities with increasing T Es into a mono-exponential function. S3

4 Figure S1. TEM images of hollow oxide nanoparticles synthesized from (a) 11 and (b) 24 nm-sized MnO nanocrystals and (c) 11 and (d) 24 nm-sized Fe3O4 nanocrystals, respectively. S4

5 Figure S2. TEM images of 20 nm-sized Fe-rich manganese ferrite nanocrystals (a) and hollow oxide nanoparticles synthesized from them (b). The elemental analysis by inductively coupled plasma atomic emission spectrometry (ICP-AES) showed that the molar ratios of Mn to Fe in (a) and (b) are 1:2.70 and 1:2.57, respectively. Figure S3. Particle size distribution histograms of MnO (a) and Fe3O4 (c) nanocrystals and the corresponding hollow oxide nanoparticles (b, d) through the etching process. (<D>: mean size of nanoparticles, σr : relative standard deviation of nanoparticles) S5

6 Figure S4. High resolution TEM images and the corresponding point EDX analysis of core-shell-void intermediate (a), hollow nanobox (b) etched from α-fe 2 O 3 nanocubes and hollow nanoparticles (c) etched from MnO. S6

7 Figure S5. TEM images of MnO nanocrystals etched in a mixture of highly pure TOPO and MPA (a) and TDPA (b). Figure S6. The plots for the relative abundant of each element as functions of position for the hollow nanoparticles synthesized from MnO nanocrystals obtained by EDX linescanning analysis. In the inset, the corresponding High resolution TEM image of hollow nanoparticle is shown. S7

8 Figure S7. TEM images of hollow intermediate structures synthesized with solid MnO (a), and Fe 3 O 4 (b) in the presence of TOPO. Figure S8. XPS spectrum of P 2p peak for hollow nanoparticles synthesized with α- Fe 2 O 3 in the presence of TOPO. S8

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