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X-Ray Photoelectron Investigation of Phosphotungstic Acid as a Proton-Conducting Medium in Solid Polymer Electrolytes Clovis A. Linkous Stephen L. Rhoden.

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Presentation on theme: "X-Ray Photoelectron Investigation of Phosphotungstic Acid as a Proton-Conducting Medium in Solid Polymer Electrolytes Clovis A. Linkous Stephen L. Rhoden."— Presentation transcript:

1 X-Ray Photoelectron Investigation of Phosphotungstic Acid as a Proton-Conducting Medium in Solid Polymer Electrolytes Clovis A. Linkous Stephen L. Rhoden Florida Solar Energy Center University of Central Florida Cocoa, Florida, USA E-mail: calink@fsec.ucf.edu Kirk Scammon Advanced Materials Processing and Analysis Center

2 Tungsten trioxide, WO 3 Melting point: 1473 K Insoluble in mineral acids Soluble in alkali WO 3 + 2NaOH  Na 2 WO 4 + H 2 O Formation of phosphotungstic acid, PTA: H 3 PO 4 + 12WO 3  H 3 PW 12 O 40 -xH 2 O

3 Outline PEM fuel cell function Conductivity in polymer electrolytes Effect of PTA on sulfonic acid polymer membrane conductivity XPS observation of W chemical shifts Relating chemical shift data to hydration environment Thermogravimetry Conclusion Future work

4 Polymer Electrolyte Membrane H+H+ H+H+ H+H+ H+H+ Membrane Electrode Assembly (MEA)/ Catalyst Coated Membrane (CCM) e - e - e - e - e - e - e - Gas Diffusion Layer ANODE H 2  2H + + 2e - Catalyst Layer Polymer Electrolyte Membrane Fuel Cell CATHODE O 2 + 4H + + 4e -  2H 2 O Flow Field

5 Typical Current-Voltage curve for a PEM fuel cell

6 Membrane Electrode Assembly- the heart of a PEM fuel cell sprayed catalyst ink layer Polymer membranes with catalyst ink

7 Base Polymer of interest: PEEK and PEKK poly(aryletherketone)

8 Previous work on Nafion  112 and PTA composite

9 Solid Acid Additives for Membrane Modification 10 Å Keggin structure Phosphotungstic acid (PTA) 12WO 3 *H 3 PO 4 *24H 2 O

10 Conductivity vs RH for SPEEK/PTA composite membrane

11 Effect of Cs+ treatment on PTA/SPEEK composites

12 Representative W4f spectra

13 Summary of W4f 7/2 data SampleBinding Energy (eV) WO 3 35.1 PTA + Cs 2 CO 3 35.4 PTA/Cs + /H 2 SO 4 35.6 SPEEK/PTA35.7 PTA + CsCl35.8 Na 3 PTA35.9 PTA-6H 2 O36.0 PTA-EtOH/DMF36.2 PTA (anhydrous)36.2 PTA – 24H 2 O (recrystallized)37.8, 36.0 Na 2 WO 4 -2H 2 O36.7 Cs 2 WO 4 (anhydrous)37.3, 35.3 PTA--24H 2 O (commercial A)37.5 PTA--24H 2 O (commercial B)37.6 Cs 2 WO 4 -2H 2 O37.7

14 Weight loss thermogram for PTA-24H 2 O

15 Weight loss thermogram for PTA-6H 2 O

16 Weight loss thermogram for PTA treated with Cs 2 CO 3

17 Summary of W4f 7/2 data SampleBinding Energy (eV) WO 3 35.1 PTA + Cs 2 CO 3 35.4 PTA/Cs + /H 2 SO 4 35.6 SPEEK/PTA35.7 PTA + CsCl35.8 Na 3 PTA35.9 PTA-6H 2 O36.0 PTA-EtOH/DMF36.2 PTA (anhydrous)36.2 PTA – 24H 2 O (recrystallized)37.8, 36.0 Na 2 WO 4 -2H 2 O36.7 Cs 2 WO 4 (anhydrous)37.3, 35.3 PTA-24H 2 O (commercial A)37.5 PTA-24H 2 O (commercial B)37.6 Cs 2 WO 4 -2H 2 O37.7

18 Conclusion Cs + exchange improves conductivity of SPEEK/PTA composite membranes. W chemical shift related to O-bonding geometry (octahedral vs tetrahedral) and waters of hydration. Cs + treatment lowers PTA water content and its enthalpy of hydration. Cs + functions by destabilizing waters of hydration, rendering them more mobile and better able to conduct protons.

19 Future Work XRD of PTA vs water content IR analysis of retained hydrogen stretching frequencies Obtaining conductivity vs RH curves at temperatures on either side of the TGA water transition. Fabricating Pt//SPEEK/PTA//Pt membrane electrode assemblies and deriving fuel cell current voltage curve

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