# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2004
Mesoporous Silica with Ia3d Cubic Structure and Good Thermal Stability
Jiebin Pang, J. Eric Hampsey, Qingyuan Hu, Zhiwang Wu, Vijay T. John, and Yunfeng Lu*
Figure 1. XRD (a, c) and nitrogen sorption isotherms (b, d) of the as-synthesized
powders after calcinations in air at 900 oC for 4 h (a, b) and the as-synthesized powders
after calcinations in air at 500 oC for 6 h and then at 900 oC for 4 h in nitrogen or air (c,
d). For comparison, the results of the powders calcined in nitrogen at 900 oC for 4 h or
calcined in air at 500 oC for 6 h are also included.
80000
3 -1
carbonized in nitrogen
o
at 900 C for 4 h
60000
Intensity (CPS)
Volume Adsorbed (cm g , STP)
500
70000
50000
40000
30000
calcined in air
o
at 900 C for 4 h
20000
10000
0
450
400
300
250
200
(a)
2
3
4
5
6
7
8
9
10
100
50
0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0
(b)
2Theta (degrees)
Calcined in air
o
at 900 C for 4 h
150
-10000
1
Carbonized in nitrogen
o
at 900 C for 4 h
350
Relative Pressure (P/P0)
70000
Volume Adsorbed (cm g , STP)
calcined in air
o
at 500 C for 6 h
60000
3 -1
Intensity (CPS)
50000
40000
o
calcined in air at 500 C for 6 h
o
and then 900 C for 4 h in N2 or air
30000
20000
N2
air
10000
0
-10000
1
(c)
2
3
4
5
6
7
8
9
10
600
400
300
200
100
(d)
2Theta (degrees)
calcined in air
o
at 500 C for 6 h
500
o
calcined in air at 500 C for 6 h
o
and then 900 C for 4 h in N2 or air
N2
air
0
0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0
Relative Pressure (P/P0)
Figure 2. XRD pattern of the sample prepared with the molar ratio of DM/CTAB is 1/2,
showing a hexagonal mesostructure.
50000
100, d=4.03 nm
Intensity (CPS)
40000
30000
as synthesized
20000
110
10000
200
0
1
2
3
4
5
6
7
8
9
10
2Theta (degrees)
1
# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2004
Figure 3. EDS spectrum of the powders carbonized in nitrogen at 900 oC for 4 h. (Note:
The samples were prepared by directly dispersing the fine powders onto a Cu grid coated
with a porous C film. For the EDS analysis, the electron beam was focused on the sample
to decrease the disturbance from the C film coated on Cu grid. EDS is mainly used for
qualitative analysis rather than quantitative analysis, therefore the quantitative values are
just for reference.)
Figure 4. TGA curve of the powders carbonized in nitrogen at 900 oC for 4 h. (Note:
TGA of the samples was performed on a Thermal Analysis Hi-Res TGA 2950 instrument
with a heating rate of 5 oC/min, a heating range from 30 to 700 oC, and an oxygen flow
rate of 80 cm3/min.)
105
Weight (%)
100
6.5 wt%
95
90
85
80
100
200
300
400
500
600
700
O
Temperature ( C)
Scheme 1. Proposed formation mechanism of the the Ia3d cubic mesostructure in
nitrogen at high temperatures such as 900 oC.
2