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Room-temperature synthesis of mesoporous CuO nanostructure and its catalytic activity for cyclohexene oxidation
Xinxin Sang, Jianling Zhang*, Tianbin Wu, Bingxing Zhang, Xue Ma, Li Peng, Buxing
Han, Xinchen Kang, Chengcheng Liu, Guanying Yang
Beijing National Laboratory for Molecular Sciences, CAS Key Laboratory of Colloid
and Interface and Thermodynamics, Institute of Chemistry, Chinese Academy of
Sciences.
4000 3500 3000 1500 1000 500
Wavenumber / cm-1
commercial CuO CuO in this work
Inte
nsity
Fig. S1 FT-IR spectrum of (a) CuO synthesized in TEA and (b) commercial CuO. CuO
obtained in this work presents the same FT-IR spectrum as commercial CuO. The
bands in the infrared spectrum at below 700 cm-1 are due to Cu-O vibrations.
The peak at 3500 cm-1 indicates that there are still traces of hydroxyl groups
due to the surface adsorption. No peaks of TAE were observed.
Electronic Supplementary Material (ESI) for RSC Advances.This journal is © The Royal Society of Chemistry 2015
1200 800 400
Inte
nsity
Binding energy (eV)
a
960 950 940 930
953.5
Inte
nsity
Binding energy (eV)
933.6Cu2pShake-upsatellites
b
534 531 528
c
Inte
nsity
Binding energy (eV)
529.7
531.2
Fig. S2 XPS study of CuO synthesized in TEA: (a) A wide-range of XPS spectra (b) Cu2p
spectra (c) O1s spectra. The survey spectra (Fig. S2a) indicates that there is no
amine left on the surface of CuO nanocrystals because the characteristic N1s
peaks do not appeare in the range of 394-410 eV. In Fig. S2b, the peaks located
at 933.6 eV and 953.5 eV can be assigned to Cu2p3/2 and Cu2p1/2 of CuO,
respectively. The Cu2p spectrum contains a characteristic (for the Cu2+ state)
“shake-up” satellite. In Fig. S2c, the peak at 529.7 eV corresponds to O2− in CuO.
The O1s spectrum contains a small shoulder on the side with binding energy 531.2
eV, which can be attributed to the weakly charged oxygen species from air. The Cu2p
and O1s spectra presented in Fig. S2 are typical for CuO samples and agree well with
the literature data.1
Trimethylamine
(222
)(3
11)
(113
)(3
10)
(113
)(2
02)
(020
)(202
)(1
12)
(111
)(0
02)
Inte
nsity
2-Theta / o
(110
)
20 30 40 50 60 70 80
JCPDS:48-1548
Inte
nsity
Tripropylamine
10 20 30 40 50 60 70 80
JCPDS:48-1548
JCPDS:13-0420
2-Theta / o
Inte
nsity
Tributylamine
10 20 30 40 50 60 70 80
JCPDS:48-1548
JCPDS:13-0420
2-Theta / o
2-Theta / o
JCPDF 13-0420
Inte
nsity
Diethylamine
JCPDF 48-1548
10 20 30 40 50 60 70 80
Inte
nsity
2-Theta / o
Ethylamine
JCPDF 13-0420
10 20 30 40 50 60 70 80
Fig. S3 XRD patterns of the samples synthesized in different amine solution.
Fig. S4 TEM images of the samples synthesized in TMA (a, b), TPA (c, d), TBA (e, f)
solution.
Fig. S5 TEM images of the samples synthesized in DEA (a, b) and EA (c, d).
20 30 40 50 60 70 80
c
b
2-Theta / o
Inte
nsity
a
Fig. S6 XRD patterns of the CuO synthesized from Cu(NO3)2 (a), CuSO4 (b) and CuCl2
(c) in TEA aqueous solution.
Fig. S7 TEM image of commercial CuO.
0.0 0.2 0.4 0.6 0.8 1.00
2
4
6
Relative Pressure (P/Po)
Vol
ume a
dsor
bed /
cm3 g-1
Fig. S8 N2 adsorption-desorption isotherm of commercial CuO.
Fig. S9 TEM image of the CuO reused four times.
References
1. H. Cao, H. F. Jiang, X. S. Zhou, C. R. Qi, Y. G. Lin, J. Y. Wu and Q. M. Liang, Green
Chem., 2012, 14, 2710.
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