supporting information: glucose-assisted synthesis of copper

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- S1 - Supporting Information: Glucose-Assisted Synthesis of Copper Micropuzzles and Their Application as Nonenzymatic Glucose Sensors Huan Pang, Qingyi Lu, Jianjun Wang, Yecheng Li, Feng Gao Experimental: Synthesis of the copper micropuzzles: In the experiments, various puzzle Cu structures were prepared by the reduction of CuSO 4 ·5H 2 O with glucose through a mild hydrothermal process. In a typical procedure, the starting solution was prepared by mixing 0.10 g of glucose and 0.16 g of CuSO 4 ·5H 2 O in 10 mL of H 2 O, and the resulting solution was transferred into 50 mL stainless-steel autoclaves lined with poly(tetrafluoroethylene) (PTFE, Telfon). The autoclave was sealed and maintained at 160 °C for 8 h and then cooled to room temperature. The red products obtained at the bottom of the autoclave were collected, washed three times with deionized water, and dried in air. Electrochemical Measurements: All measurements were conducted at room temperature (25± 2 °C). The modified electrode was prepared as follows: 0.001 g of Cu nanostructures or commercial Cu powders was mixed well with 100 μL of 0.5 % nafion solution. Then, the 10 μL of the solution was dropped onto the surface of glassy carbon electrode (r = 3 mm), left for dry for 1h. Various concentrations of D-(+) glucose or other agents were injected into 0.1 M phosphate buffer at pH= 7.40. Currents at different glucose concentrations were recorded after the transient steady states reached with constant stirring. CHI660c electrochemical workstation (CHI Co., Shanghai, China) is used for all electrochemical analysis. A three electrode configuration is utilized with Ag/AgCl (saturate KCl) as reference electrode, Pt as auxiliary electrode and glassy carbon electrode as working electrode. Antibacterial test: The antibacterial activity of the synthesized microstructures was tested against Staphylococcus aureus. The micropuzzles were mixed with molten LB-agar at 20 μg/mL. Serial dilution (1/10 4 ) of late log phase bacteria (OD 600 2.0) were then plated onto solidified copper microcrystals agar plates and incubated at 37 °C for 24 h. Characterizations: The morphology of the as-prepared samples was observed by a Hitachi S-4800 Supplementary Material (ESI) for Chemical Communications This journal is (c) The Royal Society of Chemistry 2010

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Page 1: Supporting Information: Glucose-Assisted Synthesis of Copper

- S1 -

Supporting Information:

Glucose-Assisted Synthesis of Copper Micropuzzles and

Their Application as Nonenzymatic Glucose Sensors Huan Pang, Qingyi Lu, Jianjun Wang, Yecheng Li, Feng Gao

Experimental:

Synthesis of the copper micropuzzles: In the experiments, various puzzle Cu structures were

prepared by the reduction of CuSO4·5H2O with glucose through a mild hydrothermal process. In a

typical procedure, the starting solution was prepared by mixing 0.10 g of glucose and 0.16 g of

CuSO4·5H2O in 10 mL of H2O, and the resulting solution was transferred into 50 mL

stainless-steel autoclaves lined with poly(tetrafluoroethylene) (PTFE, Telfon). The autoclave was

sealed and maintained at 160 °C for 8 h and then cooled to room temperature. The red products

obtained at the bottom of the autoclave were collected, washed three times with deionized water,

and dried in air.

Electrochemical Measurements: All measurements were conducted at room temperature (25± 2

°C). The modified electrode was prepared as follows: 0.001 g of Cu nanostructures or commercial

Cu powders was mixed well with 100 μL of 0.5 % nafion solution. Then, the 10 μL of the solution

was dropped onto the surface of glassy carbon electrode (r = 3 mm), left for dry for 1h. Various

concentrations of D-(+) glucose or other agents were injected into 0.1 M phosphate buffer at pH=

7.40. Currents at different glucose concentrations were recorded after the transient steady states

reached with constant stirring. CHI660c electrochemical workstation (CHI Co., Shanghai, China)

is used for all electrochemical analysis. A three electrode configuration is utilized with Ag/AgCl

(saturate KCl) as reference electrode, Pt as auxiliary electrode and glassy carbon electrode as

working electrode.

Antibacterial test: The antibacterial activity of the synthesized microstructures was tested against

Staphylococcus aureus. The micropuzzles were mixed with molten LB-agar at 20 μg/mL. Serial

dilution (1/104) of late log phase bacteria (OD600= 2.0) were then plated onto solidified copper

microcrystals agar plates and incubated at 37 °C for 24 h.

Characterizations: The morphology of the as-prepared samples was observed by a Hitachi S-4800

Supplementary Material (ESI) for Chemical CommunicationsThis journal is (c) The Royal Society of Chemistry 2010

Page 2: Supporting Information: Glucose-Assisted Synthesis of Copper

- S2 -

field-emission scanning electron microscope (FE-SEM) at an acceleration voltage of 10.0 kV. The

phase analyses of the samples were performed by X-ray diffraction (XRD) on a SHIMADZU,

XRD-6000 with Cu Kα radiation (λ = 1.5418 Å).

Supplementary Material (ESI) for Chemical CommunicationsThis journal is (c) The Royal Society of Chemistry 2010

Page 3: Supporting Information: Glucose-Assisted Synthesis of Copper

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30 40 50 60 70 80

(a) (220

)

(200

)

(111

)

Inte

nsity

(a.u

.)

2θ/ degree

(b)

(111

)

Figure SI1 XRD patterns of the as-prepared puzzle-like Cu structures: (a) powder XRD pattern; (b)

XRD pattern of a single puzzle-like Cu plate.

Supplementary Material (ESI) for Chemical CommunicationsThis journal is (c) The Royal Society of Chemistry 2010

Page 4: Supporting Information: Glucose-Assisted Synthesis of Copper

- S4 -

aa bb

cc dd

Figure SI2: SEM images of the sample prepared with CuSO4·5H2O (0.08 g) and glucose (0.1 g)

and distilled water (10 mL) as reactant under 160 °C hydrothermal conditions for 12 h.

Supplementary Material (ESI) for Chemical CommunicationsThis journal is (c) The Royal Society of Chemistry 2010

Page 5: Supporting Information: Glucose-Assisted Synthesis of Copper

- S5 -

Figure SI3 SEM images of the products that were prepared under different conditions: (a~c) SEM

images with different magnification of the sample prepared with CuSO4·5H2O (0.06 g) and

glucose (0.05 g) and distilled water (10 ml) as reactant under 160 °C hydrothermal conditions for

16 h; (d) An SEM image of the sample prepared with CuSO4·5H2O (0.16 g) and glucose (0.05 g)

and distilled water (10 ml) as reactant under 160 °C hydrothermal conditions for 16 h. All these

figures confirm that under these conditions puzzle-like structured Cu could be synthesized.

Supplementary Material (ESI) for Chemical CommunicationsThis journal is (c) The Royal Society of Chemistry 2010

Page 6: Supporting Information: Glucose-Assisted Synthesis of Copper

- S6 -

Figure SI4 An SEM image of commercial copper particles

Supplementary Material (ESI) for Chemical CommunicationsThis journal is (c) The Royal Society of Chemistry 2010

Page 7: Supporting Information: Glucose-Assisted Synthesis of Copper

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a baa bb

Figure SI5. Photos of the LB-agar plate: (a) before the incubation of the bacterial; (b) after the

incubation with the addition of commercial copper powders.

Supplementary Material (ESI) for Chemical CommunicationsThis journal is (c) The Royal Society of Chemistry 2010