Supporting Information Facile Microwave-assisted Hydrothermal Synthesis of CuO Nanomaterials and Their Catalytic and Electrochemical Properties Guohong Qiu,†,‡ Saminda Dharmarathna,‡ Yashan Zhang,‡ Naftali Opembe,‡ Hui Huang,‡ and Steven L. Suib*,‡ †
Key Laboratory of Subtropical Agricultural Resources and Environment, Ministry of Agriculture,
College of Resources and Environment, Huazhong Agricultural University, Wuhan, 430070, P. R. China ‡
Department of Chemistry, University of Connecticut, 55 North Eagleville Road, Storrs,
Connecticut, 06269-3060, USA * Corresponding author:
[email protected], Tel: 1 860 486 2797, Fax: 1 860 486 2981
Figure S1 shows the representative profiles of temperature, pressure, and power when the reaction was performed at 150 o C for 30 min in Cu(CH3 COO)2 (0.1 M)/urea(0.5 M) and Cu(NO 3 )2 (0.1 M)/urea(0.5 M) aqueous systems. For the solutions of Cu(CH3 COO)2 /urea and Cu(NO 3 )2 /urea, temperature in the reactor vial was well maintained at 150 o C, and the pressure was kept at about 8.0 bar, and the power ranged from 26 to 36 W as the reaction proceeded, which suggested that the energy consumption was very low during this process. The prepared copper oxides were designated as CuO-1 and CuO-2 when Cu(CH3 COO)2 and Cu(NO 3 )2 were used as divalent copper sources in the above reaction systems at 150 o C for 30 min, respectively. Figure S2 presents FTIR spectra of CuO-1 and CuO-2 synthesized at 150 o C for 30 min in Cu(CH3 COO)2 (0.1 M)/urea(0.5 M) and Cu(NO 3 )2 (0.1 M)/urea(0.5 M) aqueous solutions, respectively. Figure S3 shows the typical TEM and HRTEM images of CuO-1 (a) and CuO-2 (b). Figure S4 exhibits nitrogen adsorption-desorption isothermal curves of CuO-1 (a) and CuO-2 (b). Figure S5 presents the XRD patterns of the products synthesized in the solution of 0.1 M Cu(NO 3 )2 and 0.5 M urea at 150 o C for 5 min and 10 min. Figure S6 shows the SEM images of CuO-1 (a) and CuO-2 (b) after a series of catalytic oxidation reactions of CO to CO 2 . S1
1. The representative profiles of temperature, pressure, and power in synthesis process o
Temperature ( C)
Pressure (bar)
Power (W)
(a)
(b)
Time (min)
Time (min)
Time (min)
Figure S1. Representative profiles of temperature, pressure, and power when the o
reaction was performed at 150 C for 30 min in different solutions: (a) 0.1 M Cu(CH3 COO)2 + 0.5 M urea, (b) 0.1 M Cu(NO3 )2 + 0.5 M urea.
2. FTIR of CuO-1 and CuO-2
(b)
(a)
Figure S2. FTIR spectra of the products synthesized at 150 o
C for 30 min in different solutions : (a) 0.1 M Cu(CH3 COO)2
+ 0.5 M urea, (b) 0.1 M Cu(NO3 )2 + 0.5 M urea. S2
3. TEM and HRTEM images of CuO-1 and CuO-2 0.25 nm
(a)
0.25 nm
(b)
0.25 nm
100 nm
200 nm
Figure S3. Typical TEM and HRTEM images of the synthesized products: (a) CuO-1, (b) CuO-2.
4. BET adsorption-desorption curves of CuO-1 and CuO-2
(a)
(b)
Figure S4. Nitrogen adsorption-desorption isothermal curves of the synthesized products: (a) CuO-1, (b) CuO-2.
S3
5. XRD patterns of the products synthesized in the solution of 0.1 M Cu(NO3 )2 and 0.5 M urea
(b)
(a)
Figure S5. XRD patterns of the products synthesized in the solution of 0.1 M Cu(NO3 )2 and 0.5 M urea at 150 o C for 5 min (a) and 10 min (b).
6. SEM images of CuO-1 and CuO-2 after catalytic reactions (a)
(b)
200 nm
200 nm
Figure S6. SEM images of copper oxides after a series of catalytic oxidation reactions of CO to CO2 : (a) CuO-1, (b) CuO-2.
S4