SUPPORTING INFORMATION
Preparation and characterization of activated CMK-1 with Zn and Ni species
applied in hydrogen storage
Juliana M. Juárez, Marcos B. Gómez, Oscar A. Anunziata*
SEM Supporting images
In Fig. 7 we can see a clean CMK-1 without the inorganic template. Fig. S1 exhibits
CMK-1 sample and a crystal of MCM-48, showing that MCM-48 still remains in the
CMK-1 structure after the first hydrofluoric acid extraction; this fact is also proved by
SEM-EDS (Fig. S2)
B
Fig. S1: SEM of CMK-1 sample after first hydrofluoric acid extraction (inorganic
MCM-48 template remaining).
Fig. S2: EDS of MCM-48 crystal in image sowed in Fig. S2.
1
FTIR spectra show characteristic bands of MCM-48 that indicate great crystallinity
of material (see Fig. S3 in Supporting information). The peak at around 1638 cm-1
corresponds to the bending mode of O–H of water. The peaks around 1288 and 1180
cm-1 are attributed to the asymmetric stretching of Si–O–Si groups. The band at 806 cm
-1
and a broad signal appears at 580 cm-1 is assigned to the symmetric stretching modes
of Si–O–Si groups. The peak at 963-967 cm-1 is attributed to the presence of defective
Si–OH groups while the adsorption band at 458 cm-1 is due to Si–O–Si bending
vibration. In carbon CMK-1 and metal/CMK-1, these bands disappeared because the
siliceous material was eliminated in the process of carbon synthesis.
MCM-48
CMK-1
1180
Zn-CMK-1
1228
Ni-CMK-1
458
Absorbance (a.u.)
1638
806
965
2000
1500
1000
500
Wavenumber (cm-1)
Fig. S3. FTIR spectra from 2000 to 400 cm-1 of MCM-48, CMK-1 and metal-containing
CMK-1.
The experimental data obtained of hydrogen storage on non-activated and
activated (before and after hydrogen treatment) for Zn-CMK-1 and Ni-CMK-1
materials (see Fig. S4), indicate that the hydrogen storage of non-activated are
lower than activated materials.
2
2.0
3.5
1.0
0.8
0.6
0.4
0.2
0.0
0.0
0.2
0.4
0.6
Presure (bar)
0.8
1.0
1.5
Adsorption CMK-1
Adsorption ZnO-CMK-1
1.0
Desorption CMK-1
Desorption ZnO-CMK-1
0.5
0.0
H adsorption capacity (wt. %)
2
2.5
1.2
0
2
4
6
8
10
0
2
4
6
8
10
Pressure (bar)
H adsorption capacity (wt%)
2
H adsorption capacity (wt. %)
2
H adsorption capacity (wt%)
2
3.0
3.0
2.5
Adsorption CMK-1
Adsorption NiO-CMK-1
Desorption CMK-1
Desorption NiO-CMK-1
1.4
1.2
1.0
0.8
0.6
0.4
0.2
0.0
0.0
0.2
0.4
0.6
Presure (bar)
0.8
1.0
2.0
1.5
1.0
0.5
0.0
0
2
4
6
8
10
0
2
4
6
8
10
Pressure (bar)
Fig S4: Hydrogen isotherm sorption curves of a: CMK-1, ZnO-CMK-1 and b): NiOCMK-1 at 77 K
3