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Chemical Science
Supplementary information for
Ultra-fast Framework Stabilization of Ge-Rich Zeolites by
Low-
Temperature Plasma Treatment
Mohamad El-Roz,† Louwanda Lakiss,† Aurelie Vicente,† Krassimir
Bozhilov‡ Frederic Thibault-Starzyk† and Valentin Valtchev†*;
E-mail: [email protected]
†Laboratoire Catalyse et Spectrochimie, ENSICAEN - Université de
Caen - CNRS, 6 bd du Maréchal Juin, 14050 Caen, France.
‡ Central Facility for Advanced Microscopy and Microanalysis,
University of California, Riverside, CA 92521, USA
Figure S1. Plasma reactor coupled to IR in situ cell.
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Figure S2. The “sandwich” reactor-IR cell modified for studying
UV photocatalysis: (1)
Adjusting nut for air tightness (modified for UV-guid position),
(2) IR beam, (3) UV-light
guide, (4) Kalrez O-ring, (5) KBr windows, (6) Spectrometer
base-plate, (7) IR cell support,
(8) Oven location, (9) Sample (wafer), (10) Gas inlet, (11)
External shell, (12) Wafer holder,
(13) Thermocouple location, (14) Air cooling outlet, (15) Gas
outlet, (16) Air cooling inlet.
UV source
11
13
16
10
15
3
141
3
7
45
13
12
11
9
8
6
10
14
1
2
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journal is © The Royal Society of Chemistry 2013
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100 nm500 nm
Figure S3. SEM images of Si-BEC (left) and Ti-BEC (right).
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journal is © The Royal Society of Chemistry 2013
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δ 29Si (ppm)
-40 -60 -80 -100 -120 -140 -160 -180
b
e
d
a
-115.0
-109.0
-103.0
c
f
Figure S4. 29Si MAS NMR spectra of (a) calcined and exposed to
inert atmosphere BEC-type
Ge-silicate, (b) calcined BEC-type Ge-silicate exposed to H2O
vapors, (c) Ti-BEC, (d) Ti,Si-
BEC, (e) calcined Ti,Si-BEC and (f) calcined Si-BEC.
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4000 3600 3200 2800 2400 2000 1600 1200
dcb
Wavenumber (cm-1)
0.3
a
A
B
Figure S5. Post-synthesis modification of BEC-type material by
method II: (A) Evolution of
BEC-type material IR spectra vs. plasma treatment time during:
O2-plasma (a), SiCl4-plasma
(b) followed by O2-plasma (c) treatment. (B) IR spectra of
BEC-type material before
treatment (a), after O2-plasma (b), after O2-plasma+SiCl4-plasma
(c) and after O2-
plasma+SiCl4-plasma+O2-plasma (d) treatments.
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5 10 15 20 25 30 35 40 45 50
dc
2 θ (°)
a
b
Figure S6. XRD patterns of: as-synthesized BEC-type Ge-silicate
(a); calcined forms of Si-
BEC (b) and Ti-BEC (c) obtained by method II; and calcined
initial material exposed to water
vapors (d).
Electronic Supplementary Material (ESI) for Chemical ScienceThis
journal is © The Royal Society of Chemistry 2013
