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Nafion
H+
S-PEEK
Non-fluorinated
structure.
with
an
aromatic
to
ZrO2
Hydrophilic nature
Thermal stability.
Experimental
Synthesis of the modified S-PEEK
membranes
Casting method
S-PEEK
DMF
Stirring at 80 oC
(Huang, Shao, Burns, & Feng, 2001; Li, 2003; Roelofs, 2010)
T = 35 oC
Time: 3 24 h
ZrO2 (prepared by sol-gel
method)
PWA
ZrO2/PWA-imp
ZrO2/PWA-in-situ (in situ
impregnation)
Characterization of S-PEEK
membranes
Sulfonation degree (SG) and ionic exchange
capacity
(IEC)titration
Acid-base
Water uptake and swelling
Drying at 80 oC
Dry weight
Area
Thickness
S-PEEK in H2O
T=30 oC y T=70 oC
(Yang, 2008)
Wet weight
Area
Thickness
Proton conductivity
Potenciostate
PGSTAT
302
AUTOLAB
Fuel Cell Station PSCompuCell
by Electrochem
PEM
Fuel
Cell
by
Electrochem
Name
Polymer
content (%
peso)
Filler
Specifications
Filler content (%
peso)
S-PEEK
100
S-PEEK+ZrO2
90
ZrO2
Sol-gel
10
S-PEEK+PWA
70
PWA
30
S-PEEK+ZrO2-PWA-imp
90
Conjunto
ZrO2/PWA
Estndar
impregnation
10
S-PEEK+ZrO2-PWA-in-situ
90
Conjunto
ZrO2/PWA
In situ impregnation
10
S.D. (%)
56.12
64.28
65.08
67.62
82.31
83.86
89.21
101.55
2.4
Datos: GS(tsulfonacion)
2.2
Ajuste lineal
2.0
- ln (1 - G S ) (-)
Time (h)
3
4
5
6
17
18
22
24
1.8
1.6
1.4
1.2
1.0
0.8
0
10
15
t sulfonacion (h)
20
25
Feature
S-PEEK
S-PEEK+ZrO2
S-PEEK+PWA
S-PEEK+ZrO2PWA-imp
Wup (%) a 30 oC
Wup (%) a 70 oC
Swelling a 30 oC
Swelling a 70 oC
(mol H2O/mol
SO3H)
18.45
28.13
1.041
1.088
53.22
97.56
0.978
1.069
12.33
21.94
0.985
1.065
36.08
29.85
1.012
1.025
5.43
15.66
3.63
10.62
SPEEK+ZrO2PWA-in-situ
106
32.05
1.0002
1.333
31.19
Proton conductivity
0.45
S-P EEK
S-P EEK+ZrO2
S-P EEK+PWA
S-P EEK+ZrO2/PWA-imp
S-P EEK+ZrO2/PWA-in-situ
0.40
-1
Conductivity (S cm )
0.35
H.R. = 100 %
0.30
0.25
0.20
0.15
0.10
0.05
30
40
50
60
70
80
Temperature ( C)
0.12
0.10
Voltaje (V)
1.0
S-PEEK
S-PEEK+PWA
S-PEEK+ZrO2-PWA-in-situ
1.2
0.08
0.8
0.06
0.6
0.04
0.02
0.4
0.00
0.2
0.00 0.05 0.10 0.15 0.20 0.25 0.30 0.35 0.40
2
S-PEEK+PWA
and
SPEEK+ZrO2-PWA-in-situ
presented a higher current
density
than
S-PEEK.
However, S-PEEK+ZrO2PWA-in-situ performance
was reduced at higher
temperatures
and
at
higher pressures due to
flooding problems in the
fuel cell
1.2
Voltage (V)
conductivity,
fuel
cell
0.090
0.060
0.8
0.045
0.6
0.030
0.015
0.4
0.000
0.2
0.00
0.05
0.10
0.15
0.20
0.25
2
0.30
0.05
0.10
0.15
0.20
0.25
2
0.30
0.075
performance,
b)
1.0
tested.
S-PEEK
S-PEEK+PWA
a)
0.08
1.0
Voltage (V)
0.06
S-P EEK+P WA
0.8
0.04
0.6
0.02
0.4
0.00
0.2
0.00
0.05
0.10
0.15
0.20
2
0.25
Conclusions
S-PEEK+PWA
and
SPEEK+ZrO2-PWA-imp showed
a stable proton conductivity,
despite the high temperatures,
which suggests the addition of
these compounds improves
thermal
and
mechanical
stability.
Conclusions
Finally, among all the inorganic fillers that were tested, PWA
and its addition to the S-PEEK polymeric matrix presented the
best results:
Proper water uptake
Stable proton conductivity (0.114 S cm -1 0.12 S cm-1)
Better performance in PEM fuel cells (0.2 0.3 A cm -2), in
all the conditions tested (temperature, pressure, and
relative humidity).
This makes the PWA a promising material for its application a
membrane modifier, especially in the S-PEEK, and the
application in PEM fuel cells.
References
Carrette, B. L., Friedrich, K. A., & Stimming, U. (2001). Fuel Cells Fundamentals and Applications, (1), 539.
Huang, R. Y. M., Shao, P., Burns, C. M., & Feng, X. (2001). Sulfonation of poly(ether ether ketone)(PEEK):
Kinetic study and characterization. Journal of Applied Polymer Science, 82(11), 26512660.
http://doi.org/10.1002/app.2118
Li, L. (2003a). Sulfonated poly(ether ether ketone) membranes for direct methanol fuel cell. Journal of Membrane
Science, 226(1-2), 159167. http://doi.org/10.1016/j.memsci.2003.08.018
Li, L. (2003b). Sulfonated poly(ether ether ketone) membranes for direct methanol fuel cell. Journal of
Membrane Science, 226(1-2), 159167. http://doi.org/10.1016/j.memsci.2003.08.018
Roelofs, K. S. (2010). Sulfonated Poly ( Ether Ether Ketone ) Based Membranes For Direct Ethanol Fuel Cells
(Vol. 5).
References
Wang, Y., Chen, K. S., Mishler, J., Chan, S., & Cordobes, X. (2011). A review of polymer electrolyte
membrane fuel cells: Technology , applications , and needs on fundamental research. Applied
Energy, 88(4), 9811007. http://doi.org/10.1016/j.apenergy.2010.09.030
Yang, T. (2008). Preliminary study of SPEEK/PVA blend membranes for DMFC applications.
International
Journal
of
Hydrogen
Energy,
33(22),
67726779.
http://doi.org/10.1016/j.ijhydene.2008.08.022