Nogami, Masayuki

English

Lehigh University: Lehigh Preserve

Lehigh University 
Lehigh Preserve 
US-Japan Winter School Semester Length Glass Courses and Glass Schools 
Winter 1-1-2008 
Lecture 4, Part 2: Proton conduction in glass sand its application 
to fuel cell - Proton conduction, continued 
Masayuki Nogami 
Nagoya Institute of Technology, Japan 
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 Part of the Materials Science and Engineering Commons 
Recommended Citation 
Nogami, Masayuki, "Lecture 4, Part 2: Proton conduction in glass sand its application to fuel cell - Proton 
conduction, continued" (2008). US-Japan Winter School. 12. 
https://preserve.lehigh.edu/imi-tll-courses-usjapanwinterschool/12 
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Proton conduction in glass and its application to fuel cell
Masayuki NOGAMI
Email: nogami@nitech.ac.jp
Home Page: http://nitzy.mse.nitech.ac.jp/~nogamilab/index.html
Department of Materials Science and Engineering, 
Graduate School of Engineering, 
Nagoya Institute of Technology
Au Nanochains
Au Nanoparticles
Au
shell
R2,C2
R1,C1
tip
Si substrate
A
V
Metal Nanoparticles
★ New optical glasses
★ Fast proton conducting glasses and their application to fuel cell
★ Self-assembling of nanoparticles
400 500 600 700 800
F
l
u
o
r
e
s
c
e
n
c
e
 
i
n
t
e
n
s
i
t
y
 
(
A
r
b
.
 
u
n
i
t
s
)
Wavelength  (nm)
(a)  x150
(b)  x1
Optics,  Rare-earth
560 600 640 680
λ
ex
= 800 nm
λ
ex
= 267 nm
 
 
I
n
t
e
n
s
i
t
y
 
(
a
.
 
u
.
)
W aveleng th (nm )
0.2
0.3
0.4
0.5
0.6
0.7
0.8
0.9
1
0
5
10
15
20
25
30
35
40
0 20 40 60 80 100 120 140
C
e
l
l
 
V
o
l
t
a
g
e
 
(
V
)
Pow
er D
ensity (m
W
/cm
2)
Current Density (mA/cm2)
-4
-3.5
-3
-2.5
-2
-1.5
-1
-0.5
2 3 4 5
050150 100 -50 -75
Temperature   (oC)
(Temperature, K)-1    x10-3
l
o
g
 
 
C
o
n
d
u
c
t
i
v
i
t
y
 
 
 
 
 
 
 
 
 
 
 
 
(
S
/
c
m
)
Proton Conductor 
Fuel Cell
Glass Electrolyte
Optical memory
Nonlinearity
Fuel cell
Sensors
Laser
560 600 640 680
λex= 800 nm
λex= 267 nm
 
 
I
n
t
e
n
s
i
t
y
 
(
a
.
 
u
.
)
Wavelength (nm)
Fluorescence  
Faraday rotation 
0   0   1   0   1  0    1  0  1  0  1  0   0   0
PSHB spectrum in Eu3+-doped glass
Hole
Spectral Hole-burning 
Rare-earth
in
Glasses
Self-Assembling of  Nano-Particles and Nonlinear Optics
Shape-ControlSpectral Hole-burning 
Nanoparticles 
500 600 700 800
0
40
80
120
-5 0 5 10 15
Pump power: 30 mW
 
Delay time (ps)
N
o
r
m
a
l
i
z
e
d
 
∆
T
/
T
 
(
a
.
u
.
)
 
χ
(
3
)
 
(
1
0
-
1
1
 
e
s
u
.
)
Wavelength (nm)
Self－Assembly
600 800 1000 1200 1400 1600 1800
I
n
t
e
n
s
i
t
y
 
 
(
a
.
 
u
.
)
Wavenumber   (cm-1)
Morphology-Control
Au
shell
R2,C2
R1,C1
tip
Si substrate
A
V
Fuel cell
Sensors
Proton conduction in glass and its application to fuel cell
• Introduction
Possibility of fast proton conduction in the glass  
• Sol-gel method for preparation of proton conducting glasses 
Mechanism of proton conduction in porous glass
Glasses and films exhibiting high proton conductivities at
150oC ~ -100oC
• Applications
Electrolytes for gas sensor and fuel cell
• Conclusions
0.2
0.3
0.4
0.5
0.6
0.7
0.8
0.9
1
0
5
10
15
20
25
30
35
40
0 20 40 60 80 100 120 140
C
e
l
l
 
V
o
l
t
a
g
e
 
(
V
)
Pow
er D
ensity (m
W
/cm
2)
Current Density (mA/cm2)
-4
-3.5
-3
-2.5
-2
-1.5
-1
-0.5
2 3 4 5
050150 100 -50 -75
Temperature   (oC)
(Temperature, K)-1    x10-3
l
o
g
 
 
C
o
n
d
u
c
t
i
v
i
t
y
 
 
 
 
 
 
 
 
 
 
 
 
(
S
/
c
m
)
High proton conducting glasses for the fuel cell electrolyte
+
+
+---
H2 O2
Cells
Stack
Electrode
E
l
e
c
t
r
o
d
e
C
a
t
a
l
y
s
t
Anode
H2 2H+ + 2e-
Cathode
2H+ + 1/2O2 +  2e- H2O
Total
H2 + 1/2O2 H2O 
Electrolyte
Perfluorosulfonate ionomers (Nafion)
High proton conductivity at around 
room temperature
Degradation in thermal and chemical 
attacks
High efficiency, Clean energy
Proton conducting membrane
Inorganic Sol-gel-derived Glass
High proton conductivity at temperatures  
of 150oC to -30oC
High stability against the thermal and  
chemical  attacks
Electrolyte
• Mechanism of proton conduction in the sol-
gel-derived porous glasses.
• Effect of pore structure on the proton 
conduction.
• Preparation of glass films with ordered pore 
structure.
• Application to the gas sensor and fuel cell.
Fast proton conducting-glasses prepared by the sol-gel process 
Sample Preparation
Si(OC2H5)4
H2O,EtOH and HCl
Stirring
Drying at R.T. 
Gel
Porous Glass
Heat Treatment
OO
H
O
HOH
O
H
O
OH
O
H
HO
H
H
O
H
O
H
OH
H
O
H
O
H
O
H
O
H
O
H
O
OH
HO
HOHO HO
OH
OHHO
H
O H
O
OH
O
HO
H
O
H
OOH
O
H
HO
H
O
HO
H
O
OH
H
OH
O H
O
OH
H
O
H
O
H
OH
O
Glass
Pore
HO
O
HO
H
HO
OH
HO
HO
H
O
H
O
H
O
H
O
H
OHO
O H
O
HO
H
O
H
O OH
O
H
HO
HO
HOHO
OH
H
O HO
H
O
OH
H
O
HO
HO
HO
HO
OH
OH
HO
HO
HO
O
HO
H
O
H
O
OH
H
O
H
O
H
O
OH
H
O
H
O
H
O
H
H
O
O
O
H O
H O
H O
H O
OH O H
HO
HO
H
O
H
O
OH
H
O
H
O
H
O
OH
H
O
H
O
H
O
H
O
H
OH
O
O
H
O
HO
H
O
H
O
OH
O
H
HO
HO
H
O
H
O
OH
H
O
H
O
H
O
OH
H
O
H
O
H
O
H
O
Pore
Glass
Glass
SiOH bonds
Porous structure of the sol-gel-derived glasses
Surface Area
up to ~1000m2/g 
Pore volume
0.1 ~ 0.5 cm3/g
Pore size
> 1 nm
0
1
2
3
4
1 10
d
V
/
d
 
l
o
g
r
 
(
c
m
3
 
n
m
-
1
 
g
-
1
)
Pore radius (nm)
Porous properties of the 
glass
Water molecules absorbed in the porous glasses
OO
H
O
HOH
O
H
O
OH
O
H
HO
H
H
O
H
O
H
OH
H
O
H
O
H
O
H
O
H
O
H
O
OH
H
O H
O
OH
O
HO
H
O
H
OOH
O
H
HO
H
O
HO
H
O
OH
H
OH
O H
O
OH
H
OH
O
H Ｈ
O
H
O
H
O
H
O
H
O
H Ｈ
O
H Ｈ
O
H Ｈ
O
H Ｈ
O
H Ｈ
O
H Ｈ
O
H Ｈ
O
H Ｈ
O
H Ｈ
O
H Ｈ
O
H Ｈ
O
H Ｈ
O
Glass
Glass
HＨ
O
HＨ
O
HＨ
O
HＨ
OHＨ
O
HＨ
O
HＨ
O
HＨ
OHＨ
O
HＨ
O
HＨ
OHＨ
OHＨ
O
H ＨO
HＨ
O
HＨ
O
HＨ
O
HＨ
O HＨ
O
H
ＨO
HＨ
O
HＨ
O
H ＨO
HＨ
O
HＨ
O
H
ＨO
H
Ｈ O
H
Ｈ O
H ＨO
HＨ
O
HＨ
O
H
ＨO
H
Ｈ O
H
Ｈ O
H ＨO
HＨ
O
HＨ
O
H ＨO
HＨ
O
HＨ
O
H ＨO
HＨ
O
HＨ
O
OO
H
O
HOH
O
H
O
OH
O
H
HO
H
H
O
H
O
H
OH
H
O
H
O
H
O
H
O
H
O
H
O
OH
H
O H
O
OH
O
HO
H
O
H
OOH
O
H
HO
H
O
HO
H
O
OH
H
OH
O H
O
OH
H
OH
O
H Ｈ
O
H
O
H
O
H
O
H
O
H Ｈ
O
H Ｈ
O
H Ｈ
O
H Ｈ
O
H Ｈ
O
H Ｈ
O
H Ｈ
O
H Ｈ
O
H Ｈ
O
H Ｈ
O
H Ｈ
O
H Ｈ
O
Glass
Glass
HＨ
O
HＨ
O
HＨ
O
HＨ
OHＨ
O
HＨ
O
HＨ
O
HＨ
OHＨ
O
HＨ
O
HＨ
OHＨ
OHＨ
O
H
ＨO
HＨ
O
HＨ
O
H
ＨO
H
Ｈ O
H
Ｈ O
H
ＨO
H
Ｈ O
H
Ｈ O
H
ＨO
H
Ｈ O
H
Ｈ O
Hydrogen bonded 
H2O
Physically 
adsorbed 
H2O
SiOH
bonds
OO
HO
HOHO HO
OH
OHHO
H
HO
HOH
OH
HO HOHO
HO
HO
HO
OH
HO
HOHO HO
OH
OHHO
HO HO
OH
O
HO
HO
HOOH
OH
HO
HO
HO H
O
OH
HOHO HO
OH
HO
HO
HOHO
HO O
HO
H
HO
OH
HO
HO
HO
HO
HO
HO
HOHO
O HO
HOHO
HO OH
OH
HO
HO
HOHO
OH
HO HO
HO
OH
HO
HO
HO
HO
HO
OH
OH
HO
HO
HO
O
HO
HO
HO OH
HO
HO
HO
OH
HO
HO
HO
H H
O
O
O
H OHO H O
H O
OH O H HO
HO
HO
HO
OH
HOHO
HOOH HO
HO HOHO
HOHO
O
HO
HO
HO
HO
OH
OH
HO
HOHOHO
OH
H
O
HO
HO
OH
HO
HO
HO HO
SiOH bonds
Physically adsorbed 
H2O
Physically adsorbed 
H2O molecules are 
removed by heating 
at around 100oC. 
Heatingor 
exposure
Exposure 
to humid 
atmosphere
00.2
0.4
0.6
0.8
1
-5
-4
-3
-2
-1
0
1
0 10 20 30 40 50 60 70 80
N
o
r
m
a
l
i
z
e
d
 
w
e
i
g
h
t
 
g
a
i
n
l
o
g
 
 
 
 
 
 
 
 
 
(
S
/
c
m
)
Time    (min)
σ
 Weight gain
Conductivity
-4
-3
-2
-1
0 0 1 2 3 4
Z
"
 
(
 
x
1
0
3
 
Ω
)
Z' ( x103 Ω)
4nm-glass
2nm-glass
-10
-9
-8
-7
0.6 0.8 1 1.2
l
o
g
 
 
 
 
 
(
S
/
c
m
)
log [H2O]
σ
log  σ =  K log [H2O]
Effect of the physically bonded H2O molecules 
on the conductivity
Controlling the amount of the chemically bonded H2O molecules
OO
H
O
HOH
O
H
O
OH
O
H
HO
H
H
O
H
O
H
OH
H
O
H
O
H
O
H
O
H
O
H
O
OH
HO
HOHO HO
OH
OHHO
H
O H
O
OH
O
HO
H
O
H
OOH
O
H
HO
H
O
HO
H
O
OH
H
OH
O H
O
OH
H
O
H
O
H
OH
O
Glass
Pore
HO
O
HO
H
HO
OH
H
Ｈ O
HO
HO
H
O
H
O
H
O
H
O
H Ｈ
O
H Ｈ
O
H Ｈ
O
H Ｈ
O
H Ｈ
O
H Ｈ
O
H Ｈ
O
H Ｈ
O
H Ｈ
O
H
OHO
O H
O
HO
H
O
H
O OH
O
H
HO
HO
HOHO
OH
H
O HO
H
O
OH
H
O
HO
HO
HO
HO
OH
OH
HO
HO
HO
O
HO
H
O
H
O
OH
H
O
H
O
H
O
OH
H
O
H
O
H
O
H
H
O
O
O
H O
H O
H O
H O
OH O H
HO
HO
H
O
H
O
OH
H
O
H
O
H
O
OH
H
O
H
O
H
O
H
O
H
OH
O
O
H
O
HO
H
O
H
O
OH
O
H
HO
HO
H
O
H
O
OH
H
O
H
O
H
O
OH
H
O
H
O
H
O
H
O
H Ｈ
O
HＨ
O
HＨ
O
HＨ
O
HＨ
OChemically bonded 
H2O molecules are 
removed by heating 
at around 200oC.
Effect of the chemically bonded H2O molecules 
on the conductivity and its activation energy
60
80
100
120
-1 -0.5 0 0.5 1
log [H2O]・[H+]
A
c
t
i
v
a
t
i
o
n
e
n
e
r
g
y
 
 
 
 
(
k
J
/
m
o
l
)
-16
-15
-14
-13
-12
-11
-1 -0.5 0 0.5 1
log [H2O]・[H+]
l
o
g
 
σ
(
S
/
c
m
)
 
 
 
 
a
t
 
1
5
0
o
C
-13
-12.5
-12
-11.5
1.8 2 2.2 2.4 2.6 2.8
l
o
g
1
0
 
 
 
 
 
 
 
(
S
c
m
-
1
)
1/Temperature (K)
160oC
σ
x 10-3
250oC
210oC310
oC
log σ = k  log [H2O]・[H+]
E  = k log [H2O]・[H+]
Proton conduction in the porous 
glass
H H 
O
H H 
O
H H 
O
H H 
O
O
Si
O
H +
H
O
Si
O
O
Si
O
H+
H
O
Si
O
O
Si
O
H H 
O
H +
Conduction process of proton 
through the porous glass
Proton conduction is controlled by 
the proton dissociation from the 
SiOH bond and the proton hopping 
between SiOH and H2O. 
0
20
40
60
80
100
120
0 1 2 3
A
c
t
i
v
a
t
i
o
n
 
e
n
e
r
g
y
 
(
k
J
/
m
o
l
)
log
10
{[H] [H
2
O]}   (mol/l)
Chemically 
bonded H2O
Physically 
bonded H2O
E
• Mechanism of proton conduction in the sol-
gel-derived porous glasses.
• Effect of pore structure on the proton 
conduction.
• Preparation of glass films with ordered pore 
structure. 
• Application to the gas sensor and fuel cell.
Fast proton conducting-glasses prepared by the sol-gel process 
Pore size
5 c m
B u lk  G la s s
Catalysts
Heating
Templates Reacting
H y d r o l y z i n g
Drying
Gels
Si(OC2H5)4
Porous Glasses
Preparation of glasses with different pore size
Pore size distribution and its effect on the conductivity
0
2
4
6
1 10d V
/
d
(
l
o
g
D
)
 
(
c
m
3
.
g
-
1
 
n
m
-
1
)
Pore Diameter (nm)
2 5 20 50
No. 3
No. 1
No. 2 No. 4
-12
-10
-8
-6
-4
-2
40 60 80
l
o
g
 
 
c
o
n
d
u
c
t
i
v
i
t
y
 
 
 
 
 
(
S
/
c
m
)
Relative humidity  (%)
No. 3, 4
No. 2
No. 1
-4
-3
-2
-1
3.2 3.4 3.6 3.8 4 4.2 4.4
30            0                -30
Temperature (oC)
l
o
g
 
σ
 
(
S
/
c
m
)
1000/T (K-1)
No.2
No.3
-60 -40 -20 0 20
E
x
o
t
h
e
r
m
 
Temperature (oC)
Solidification of H
2
O
             = -45oC
DTA curve for No. 2 glass
Quantum dot 
effect
Effect of the pore size on the proton conductivity
0
2
4
6
1 10d V
/
d
(
l
o
g
D
)
 
(
c
m
3
.
g
-
1
 
n
m
-
1
)
Pore Diameter (nm)
2 5 20 50
No. 3
No. 2
P5+ ion
Heating
Reacting
Hydrolyzing
Drying
Gels
Si(OC2H5)4
Porous Glasses
Effect of P2O5 on proton conductivity
PO(OCH3)3
FT-IR 
Si -OH
H
O
H 
P -OH
H
O
H 
20002500300035004000
Wave Number  ( cm-1)
A
b
s
o
r
p
t
i
o
n
 
c
o
e
f
f
i
c
i
e
n
t
 
 
 
 
(
c
m
-
1
)
SiO2 glass
20002500300035004000
Wave Number  ( cm-1)
A
b
s
o
r
p
t
i
o
n
 
c
o
e
f
f
i
c
i
e
n
t
 
 
 
 
(
c
m
-
1
)
P2O5-SiO2 glass
Dissociation energy 
for proton;
SiOH >  POH
High proton conductivity 
can be expected for POH 
bonds.
Glass Composition
Dependence of Conductivity on 
Temperature
-8
-7
-6
-5
-4
-3
-2
-1
0
2 3 4 5
050150 100 -50 -75
Temperature   (oC)
(Temperature, K)-1    x10-3
l
o
g
 
 
C
o
n
d
u
c
t
i
v
i
t
y
 
 
 
 
 
 
 
 
 
 
 
 
(
S
/
c
m
)
Glasses
Nafion
Sol-gel glasses
• Proton conduction 
mechanism 
proton dissociation from the   
SiOH bond and the proton  
hopping between SiOH and   
H2O. 
• High proton conductivity 
in wide temperature 
range
-30oC to 150oC  
(ex. 170 mS/cm at 150oC)
• Mechanism of proton conduction in the sol-
gel-derived porous glasses.
• Effect of pore structure on the proton 
conduction.
• Preparation of glass films with ordered pore 
structure. 
• Application to the gas sensor and fuel cell.
Fast proton conducting-glasses prepared by the sol-gel process 
Sol-Gel Method for Glass 
Preparation
5cm
Bulk Glass
Catalysts
Heating
Templates Reacting
Hydrolyzing
Drying
Gels
Si(OC2H5)4
Porous Glasses
Substrate
200nm
Thin Film
Pore size
Pore 
orientation
Preparation of pore-oriented glass films
Pore-oriented glass films by self-assembling method
Preparation of glass film by self-assembling method using templates
CTAB;
(CH3(CH2)15N+(CH3)3Br
C16EO10;
(C16H33(OCH2CH2)10OH
Solution
Gel Porous glass film
HeatingDipping
Film
Substrate
Film
Substrate
Pore
2 3 4 5 6
I
n
t
e
n
s
i
t
y
 
 
(
A
r
b
.
 
u
n
i
t
s
)
2θ   (degrees)
(a)  C16EO10
2
0
0
2
1
0
2
1
1
1
0
0(b)  CTAB
(b)  hkl   d(nm)     a=2.98 nm
      100    2.98
(a) hkl   d(nm)      a=9.50 nm
    200    4.75
    210    4.44
    211    4.18
Self-assembled pore-oriented glass films
Sub.
Glass film
Hexagonal
Cubic
200 nm
-11
-10
-9
-8
-7
-6
-5
-4
40 50 60 70 80 90
l
o
g
1
0
σ  
 
 
 
(
S
/
c
m
)
Relative Humidity (RH %)
(a)  C16EO10
(b)  CTAB
Conductivities of pore-oriented glass films
I
V
I
V
• Mechanism of proton conduction in the sol-
gel-derived porous glasses.
• Effect of pore structure on the proton 
conduction.
• Preparation of glass films with ordered pore 
structure.
• Application to the gas sensor and fuel cell.
Fast proton conducting-glasses prepared by the sol-gel process 
Application of proton conducting 
glasses
Sensors
Hydrogen,  Humidity
H+
e-
PHIPHII
EMF
H2 = 2H+ +  2e- 2H+ +  2e- =  H2 EMF =         lnnF
RT
PHI
PHII
020
40
60
80
0 20 40 60
E
M
F
 
 
 
(
m
V
)
Time   (min)
25
50
1
100
Responsibility to H2 gas
-20
0
20
40
60
80
0.0 1.0 2.0 3.0 4.0 5.0
E
M
F
 
 
 
(
 
m
V
 
)
ln (P
H
)
EMF  =  (RT/nF) ln(PH)
n = 2
H2 = 2H+ +  2e-
PHII
PHI
=
Alcohol 
vapor 
ITO glass substrate 
Pt
Glass film
Manganese Oxide 
Gas sensors ~ Preparation of thin films ~
P/G stat Air or Ar
25 oC
Reference electrode
Solid electrolyte
Si(OC2H5）4, 2-PrOH, HClaq
Glass film 
H3PO4 
Brij56 
HClaq
Spin coating 
Heat treatment (400oC,4h)
( 組成 : 5P2O5-95SiO2 ) 
20 30 40 50 60 70
I
n
t
e
n
s
i
t
y
 
(
a
.
u
.
)
2θ / deg (Cu-Kα)
ITO substrate
MnO
2
MnO2+4H++2e- ↔Mn2++2H2O 
Gas sennsing
0
0.1
0.2
0.3
0 10 20 30 40 50
E
M
F
 
/
 
V
Time / Sec
25 oC
1%H
2
1%CH
3
OH vapor
0.5%NH
3
 vapor
1%C
2
H
5
OH vapor
1%CH
3
COCH
3
 vapor
0
0.1
0.2
0 500 1000 1500
E
M
F
 
/
 
V
Time / Sec
25 oC
1%CH
3
OH vapor in air
High proton conducting glasses for the fuel cell electrolyte
+
+
+---
H2 O2
Cells
Stack
Electrode
E
l
e
c
t
r
o
d
e
C
a
t
a
l
y
s
t
Anode
H2 2H+ + 2e-
Cathode
2H+ + 1/2O2 +  2e- H2O
Total
H2 + 1/2O2 H2O 
Electrolyte
Perfluorosulfonate ionomers (Nafion)
High proton conductivity at around 
room temperature
Degradation in thermal and chemical 
attacks
High efficiency, Clean energy
Proton conducting membrane
Inorganic Sol-gel-derived Glass
High proton conductivity at temperatures  
of 150oC to -30oC
High stability against the thermal and  
chemical  attacks
Electrolyte
Fuel Cell
0.2
0.3
0.4
0.5
0.6
0.7
0.8
0.9
1
0
10
20
30
40
50
60
0 50 100 150 200 250
C
e
l
l
 
v
o
l
t
a
g
e
 
(
V
)
P
o
w
e
r
 
d
e
n
s
i
t
y
 
(
m
W
/
c
m
2
)
Current density (mA/cm2)
50.7 mW/cm2
Conclusions
• Fast proton-conducting porous glass 
+ Preparation by the sol-gel method
Porous glass with large surface area and small-sized pores
+ Proton conduction process
Dissociation of the protons and their hopping between
water molecules and hydroxyl groups
• High proton conductivities
+In wide temperature range from -30oC to 150oC
ex. 170 mS/cm at 150oC
• Glass films having high-ordered pore structure
• Possible application as the  electrolyte
+ Sensor and Fuel cell 
Thank you


Lecture 4, Part 2: Proton conduction in glass sand its application to fuel cell - Proton conduction, continued

https://preserve.lehigh.edu/cgi/viewcontent.cgi?article=1011&context=imi-tll-courses-usjapanwinterschool

Lecture 4, Part 2: Proton conduction in glass sand its application to fuel cell - Proton conduction, continued

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