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1 Supporting Information Precisely Controllable Core-Shell Dots Nanoparticles: Application to in Situ Super-Sensitive Monitoring of Catalytic Reactions Jing Jin, Shoujun Zhu, Yubin Song, Hongyue Zhao, Zhen Zhang, Yue Guo, Junbo Li, Wei Song,*, Bai Yang, and Bing Zhao State Key Laboratory of Supramolecular Structure and Materials, Jilin University, Changchun , P. R. China. * Alan G. MacDiarmid Institute, College of Chemistry, Jilin University, Changchun, , P. R. China. 1
2 1. EXPERIMENTAL SECTION Materials. p-aminothiophenol (PATP) was obtained from Sigma-Aldrich. AgNO 3 and dimethyl sulfone (DMSO) were bought from Sinopharm Chemical Reagent Co., Ltd. NaOH, NaBH 4 and H 2 O 2 (30%) were obtained from Beijing Chemical Works, 3,3,5,5 - tetramethylbenzidine (TMB) was bought from Aladdin Industrial corporation. p-nitrothiophenol (PNTP) was purchased from Matrix Scientific. NaAc buffer solution (ph=4) was obtained from Beijing Dingguo Changsheng Biotechnology Co., Ltd. Polymer CDs were prepared with the similar procedure based on the previous report. 1 Synthesis of core-shell structured Ag@CDs NPs. The procedure for synthesizing the coreshell structured Ag@CDs NPs with a mean diameter of ca. 40 nm is as follows. A mixed 30 ml of aqueous solution consisting of AgNO 3 (0.2 mmol/l), NaOH (0.01 mol/l), CDs (33 mg/l) was kept at a temperature of 50 in water bath for 5 min until a stable dark brown suspension of Ag@CDs NPs was produced. Then the suspension was centrifuged and washed with deionized for another two times to remove the excess CDs, after that, the sample was redispersed in 6 ml of deionized water. The concentration of optimized Ag@CDs NPs was calculated to be about 0.28 mg/ml by weighing the dried Ag@CDs sample. Ag@CDs NPs with different morphologies and sizes have also been prepared via the same process only by adjusting the feeding mass ratio of CDs to AgNO 3 and the growth mechanism was studied thoroughly by adjusting the reaction time. Preparation of individual Ag NPs by sodium citrate. Ag NPs with an average diameter of ca. 40 nm was prepared by the reduction of an aqueous solution of AgNO 3 with sodium citrate, which has been reported by Lee and Meisel. 2 In a typical experiment, 36 mg of AgNO 3 was dissolved in 200 ml of deionized water in 500 ml three-necked flask and brought to boiling 2
3 rapidly under vigorous stirring and reflux. Then 4 ml of 1% (w/v) sodium citrate aqueous solution was added into the above solution and boiled for further 40 min. After the solution was cooled to room temperature, a green-gray colloid solution was obtained. Then the colloid solution was centrifuged and washed with deionized for another two times, then the Ag NPs were dried under vacuum. Finally, a certain amount of the Ag NPs were redispersed in deionized water to prepare Ag NPs suspension with the same concentration of optimized Ag@CDs NPs. UV-vis and SERS in situ monitoring of peroxidase-like catalytic oxidation of TMB by Ag@CDs NPs in the presence of H 2 O 2. In a typical process, a solution of 250 µl peroxidaselike nanocatalysts, Ag@CDs NPs or Ag NPs prepared by sodium citrate (final concentration of 0.02 mg/ml), TMB solution in DMSO solvent (final concentration of M), and 10 µl 30% of H 2 O 2 (final concentration of M) was added into 3 ml NaAc buffer (ph= 4.0). The reaction progress was monitored at a regular time interval of 2 min by the UV-vis spectra and SERS spectra under continuous 633 nm laser excitation. For H 2 O 2 detection, we examined the concentration-dependent UV-vis and SERS spectra under continuous 633 nm laser excitation for H 2 O 2 concentrations ranging from to M and the blank sample. 250 µl of Ag@CDs NPs (final concentration of 0.02 mg/ml) was used as the catalyst and immersed in a mixed solution of final concentration of M of TMB in NaAc buffer solution with different concentrations of H 2 O 2 for 20 min. SERS in situ monitoring of plasmon-enhanced driven catalytic reaction of PNTP dimerizing into DMAB and catalytic driven reduction of PNTP to PATP in the present of NaBH 4. To study the plasmon-enhanced driven catalytic reaction for conversions of PNTP to DMAB without the addition of the reductant, 4.5 ml of Ag@CDs NPs or individual Ag NPs were immersed into 0.5 ml of PNTP ethanol solution ( M) for 1 h to ensure sufficient 3
4 adsorption, respectively. After that, they were washed thoroughly with deionized water and centrifuged to remove the unbounded molecules. Subsequently, the sample was redispersed in 5 ml of deionized water. And then, time-dependent SERS spectra of the catalytic reaction were acquired directly from the above solution under continuous 633 nm laser excitation, respectively. The spectra were collected with a time interval of 1 s. To study the Ag@CDs NPs catalytic driven reduction of PNTP to PATP in the presence of NaBH 4, 4.5 ml of Ag@CDs NPs or Ag NPs were immersed into 0.5 ml of PNTP ethanol solution ( M) for 1 h to ensure sufficient adsorption respectively. After that, they were washed thoroughly with deionized water and centrifuged to remove the unbounded molecules, the sample was redispersed in 5 ml of deionized water. Then the sample was mixed with 2 ml of 10-4 M NaBH 4 aqueous solution, respectively. The corresponding SERS spectra were recorded at 3 min intervals directly after the addition of the NaBH 4 solution. SERS spectra were recorded under continuous 633 nm laser excitation and data were acquired with one 20 s accumulation. Characterization. The morphologies of CDs, Ag@CDs and Ag NPs were characterized by the JEOL JEM-2100F transmission electron microscope (TEM) operated at 200 kv. UV-vis spectra were obtained from Shimadzu UV-3600 UV-Via-NIR spectrophotometer. The fluorescence spectra were recorded on Shimadzu 5301PC fluorescence spectrometer. X-Ray photoelectron spectroscopy (XPS) data were obtained from a Thermo ESCALAB 250 photoelectron spectrometer with Al Ka X-ray radiation. X-Ray diffraction (XRD) patterns were obtained from a PANalytical B.V. (Empyrean) diffractometer using Cu Kα radiation. The Raman spectra for PATP molecules are measured by Renishaw-1000 spectrometer with a He/Ne laser as excitation line of 532 nm, the laser power at the sample position was typically 1.1 mw. Raman spectra for monitoring the catalytic reactions were measured with by a LabRAM ARAMIS 4
5 Smart Raman Spectrometer with the radiation from an air-cooled HeNe laser (633 nm), the laser power at the sample position was typically 3.6 mw. The spectrometer was calibrated by Raman band at cm -1 of a Si wafer. 2. The enhancement factor (EF) calculation details: EF= (I SERS /N SERS )/(I 0 /N 0 ), where I SERS and I 0 denote the integrated intensity of the quivalent bands ascribed to PATP in SERS and normal Raman spectra, respectively, N SERS and N 0 represent the average number of adsorbed molecules in the detection region for the SERS experiments and normal Raman experiments respectively. N SERS =Ac surf VN A /A 0, N 0 =c 0 AhN A, where A is the area of the laser spot (1 µm), c surf is the concentration of the determined PATP molecules, c 0 is the concentration of PATP for the normal Raman measurement, N A is the Avogadro constant, V is the volume of the adsorbed molecules, A 0 is the area of the modified substrate, h is the effective focused depth which can be calculated based on the confocal feature of the microscope. We suppose that all molecules within the effective focused depth contribute to the whole Raman signal, and neglect the Raman signal from outside of the effective focused depth. The effective focused depth can be calculated to be 200 µm. The SERS spectra and normal Raman were measured under the same laser power, excitation wavenumber, and same acquisition time. In conclusion, a EF value of about was obtained for Ag@CDs NPs substrate. 5
6 Figure S1. (a) HRTEM image of individual CDs, (b) TEM image and size distribution of NPs, (c) EDX spectrum of NPs. 6
7 a) min 1 min 3 min 5 min 7 min min 1 min 3 min 5 min 7 min 250 PL Intensity Absorbance 0.5 b) Wavelength (nm) Wavelength (nm) Figure S2. (a) UV vis spectra, (b) PL spectra of the Ag@CDs NPs that were synthesized by incubating AgNO3 (0.2 mm) with CDs (33 mg/l) in 0.01 M NaOH at 50 C for 0 min, 1 min, 3 7
8 min, 5 min, 7 min. (c-f) TEM images of the Ag@CDs NPs that were synthesized by incubating the above mixed solution at 50 C for 1 min, 3 min, 5 min, 7 min. Figure S3. TEM images of the as-prepared Ag@CDs nanoparticles that were synthesized by using different concentrations of AgNO3 as the precursors. a) [AgNO3]=0.1 mmol/l, b) [AgNO3]=0.2 mmol/l, c) [AgNO3]=0.4 mmol/l. Other conditions: [CDs]=33 mg/l, [NaOH]=0.01 M, temperature: 50oC. 8
9 Figure S4. Excitation-dependent PL of CDs aqueous solution. 9
10 Figure S5. (a) TEM image of individual Ag NPs prepared by sodium citrate. (b) SERS spectra of M PATP on individual Ag NPs prepared by sodium citrate (b1) and in Ag@CDs NPs suspension (b2) with the same nanoparticle concentration. 10
11 Figure S6. Successive UV-vis spectra for the oxidation reaction of TMB with H 2 O 2 catalyzed by prepared Ag@CDs NPs (a); Ag NPs prepared by sodium citrate (b); CDs (c). The time between consecutive curves is 2 min. 11
12 Figure S7. Time-dependent maximum absorbance changes at 650 nm of the oxidation of TMB with H 2 O 2 catalyzed by Ag@CDs NPs (a); Ag NPs prepared by sodium citrate (b); CDs (c). 12
13 Figure S8. The curves of relationship between the concentration of oxidation of TMB and the reaction time according to the band at 1605 cm
14 Figure S9. Concentration-dependent UV-vis spectra for the oxidation reaction of TMB with the change of H 2 O 2 concentration range of ( ~ mol/l) and the blank sample catalyzed by Ag@CDs NPs. 14
15 Figure S10. The time-dependent SERS spectra for the reaction of PNTP dimerizing into DMAB by NPs; SERS spectra were recorded with an integration time of 1 s under continuous 633 nm laser excitation. 15
16 Raman Intensity (a.u.) v(dmab) v(dmab) a) b) 2000 Raman Intensity (a.u.) cm cm cm Wavenumber (cm -1 ) Reaction times (s) Figure S11. (a) Time-dependent SERS spectra of the individual Ag NPs catalyzed plasmonenhanced driven reaction of PNTP dimerizing into DMAB under continuous 633 nm laser excitation, (b) Time-dependent intensities of the characteristic bands of DMAB catalyzed by individual Ag NPs; SERS spectra were recorded with an integration time of 1 s. 16
17 Figure S12. The time-dependent SERS spectra of the NPs catalyzed reduction of PNTP to PATP, the characteristic bands of PNTP (a); the characteristic bands of DMAB (b); the characteristic bands of PATP (c). Spectra were recorded with an integration time of 3 min after the addition of NaBH 4 under 633 laser excitation. 17
18 Raman Intensity (a.u.) PNTP DMAB PATP min 30 min 20 min 13 min 1 min Wavenumber (cm -1 ) Figure S13. SERS spectra of individual Ag NPs catalyzed reduction of PNTP to PATP by NaBH 4 in a suspension solution; spectra were recorded after the addition of NaBH 4 under 633 laser excitation; the data were acquired with one 20 s accumulation. 18
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