TetrazoleSubstitutedPolymer Myhanh Modified 1

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PHOSPHORIC ACID DOPED TETRAZOLE SUBSTITUTEDPOLY(ARYL ETHER) FOR PROTON EXCHANGE

MEMBRANE

2014 / 06 / 13

Duong Ngoc My Hanh

Fuel cell research center

KIST

1


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CONTENT

1. Introduction

2. Experimental

3. Result and Conclusion

4. Future plan

2


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3

1. INTRODUCTION

Proton !change Me"#rane Fuel $ell

World energydemand


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%

1. INTRODUCTION

Introduce te tetra!ole "roup to te aromatic pol#mer $ac%$one &or

i" proton conducti'it# and termal sta$ilit#

What is Neee!& "e"#rane '(th a h(gh )roton con*uct(+(ty at T,120o$ an*

,2%- .H

& "e"#rane that o)erates '(thout 'ater at ele+ate* T

The P"#$%e&s 'ith Na#Naon *ehy*rates at T0o$ an* .H 100-

!)ens(+e

PEM Mate"ia% #* Ch#i+e *#" H,-Ai" F.e% Ce%% at /0#C isNa#


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2.E()ERI*ENT+,

S1thesi2e 3CN +#taii4 P#%1(a"1% ethe" )

Tet"a2#%e s.$stit.te P#%1(a"1% ethe") $15C%i+6 Che&ist"17

NaN35n$l2

NMP

NaN35n$l2

NMP

7 7K2$83

5DM&c

10o$

$haracter(9e the atta(ne* )oly"er #y NM.5 I.5T:&


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,8EXPERIMENT

Ph#s9h#"i+ a+i #9i4 9"#+ess

-Cast the membrane in DMAc solvent

-Wash up and dry in vacuum oven for 24 hours to completely remove salt

-Prepare the samples ( size 14 cm!

-Dip samples in Phosphoric acid solution "#$ %t

-Measure the %ei&ht upta'e every 2 hours

-Dry in vacuum oven at 11C to the pristine %ei&ht of membrane

-Measure in)plane conductivity in anhydrous condition at various temperature from 4oC * 1+oC

-,uel cell test- .on& term test


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;

3. RE-U,T- +ND CONC,U-ION-

NMR st.1

. e s p

8.0 7.5 7.0 6.5 6.0 5.5 5.0 4.5 4.0 3.5 3.0 2.5 2.0 1.5 1.0Chemical Shift (ppm)

0

0.01

0.02

0.03

0.04

0.05

0.06

0.07

0.08

0.09

0.10

0.11

0.12

0.13

Norm

alize

!"te"sit#

. e s p

8.0 7.5 7.0 6.5 6.0 5.5 5.0 4.5 4.0 3.5 3.0 2.5 2.0 1.5

Chemical Shift (ppm)

0.005

0.010

0.015

0.020

0.025

0.030

Normalize!"te"sit#

3.3

4

2.96

2.80

2.54

2.53

2.53

2.52

2.52

2.51

2.51

2.3

1

2.2

3


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10


NMR st.1. e s p


0

0.05

0.10

0.15

0.20

0.25

0.30

0.35

0.40

0.45

0.50

0.55

Normalize!"te"sit#

0.0410.630.704.330.720.700.035.121.882.211.290.4221.94. e s p


0

0.05

0.10

0.15

0.20

0.25

0.30

0.35

0.40

0.45

0.50

0.55

0.60

0.65

0.70

0.75

0.80

0.85

0.90

0.95

1.00

Norm

alize

!"te

"sit#


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11


FT3IR st.1

TPN #e


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3. RE-U,T- +ND CONC,U-ION

Ph#s9h#"i+ a+i #9i4

The "a!("u" ac(* u)ta=e o< TPN (s 11% 't- at 120o$

The "a!("u" ac(* u)ta=e o< TSPN (s %2 't- at 120o$


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13


The""a:i&et"i+ aa%1sis

The""a:i&et"i+ aa%1sis (TGA) +.":es #* &e&$"ae $e*#"e a a*te" a+i#9e .e" it"#4e

8l* chart '(th t9)een "e"#rane st(ll ha+esol+ent

I )re)are* another TPN "e"#rane5*r(e* (n

+acuu" unt(l the 'e(ght (s unchange* the

%- 't >oss te")erature o< TPN (s h(gher

than the ol* one

For the ac(* *o)e* "e"#rane5 I use* the

h(ghest ac(* *o)(ng le+el "e"#rane


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14


Me+hai+a% test

Mechan(cal test


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1%


39%ae +#.+ti:it1

&ct(+at(on energyTPN? 2%%4 KC/"olTSPN? 2;6% KC/"ol


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16


F.e% +e%% test

B 103 "g/c"2Pt loa*(ng

-&ct(+at(on t("e? 24 hrs

-$ell te")erature? 160o$

B &ct(+e area? 4 c"2

IV curve after 24 hours activation IV curve after 96 hours activation

u(l(#r(u" t("e


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1


F.e% +e%% test


-&ct(+at(on t("e? 24 hrs

-$ell te")erature? 160o$

B $ell area? 4 c"2

-Do)(ng te")erature? 120 o$

-T("e? 24 h

-Do)(ng le+el ? %6 -

-&


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F.e% +e%% test

C#iti#s!


-&ct(+at(on t("e? 24 hrs-$ell te")erature? 160o$

B &ct(+e area? 4 c"2

-Do)(ng le+el ? 61;4-

-Th(c=ness? %0 u"


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1;

8 FUTURE PLAN

Ese h(gher ac(* *o)(ng le+el "e"#rane

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