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Internship Master 2 IC July 5th 2012 Nanopowder Synthesis Nanopowder Synthesis for Solid Oxide Fuel for Solid Oxide Fuel Cells Anodes Cells Anodes CREPE – Faculté de génie- Université de Sherbrooke Supervisors: Prof. François Gitzhofer Yan Shen (PhD) Anh Mai DO QUANG
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Page 1: Oral presentation

Internship Master 2 ICJuly 5th 2012

Nanopowder Synthesis Nanopowder Synthesis for Solid Oxide Fuel for Solid Oxide Fuel Cells AnodesCells Anodes

CREPE – Faculté de génie- Université de Sherbrooke

Supervisors: Prof. François GitzhoferYan Shen (PhD)

Anh Mai DO QUANG

Page 2: Oral presentation

I. Laboratory Overview

II. Project & Objectives

III. SOFC Fundamentals

IV. Methodology

V. Results & Discussions

VI. Conclusion & Future work

CONTENTSCONTENTS

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I.I. LABORATORY OVERVIEWLABORATORY OVERVIEW

Anh Mai DO QUANG

Centre de Recherche en Energie, Plasma et Electrochimie (CREPE)

Mission : Develop new materials by using plasma processDirector : François Gitzhofer , ing. PhDResearch themes :• Development of materials for solid oxide fuel cell (SOFC);• Synthesis of nanopowder;• Synthesis of new catalysts based on nanoscale materials by using plasma

technology;• Application in nano-structured and new compositions of coating deposition

to improve the performances of aircraft turbines and diesel engines;• Biomedical application (synthesis of bio-materials for prosthetic bones).

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II.II. PROJECT & OBJECTIVESPROJECT & OBJECTIVES

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PROJECT

Solid Oxide Fuel Cells (SOFC) :• Applications : auxiliary power units in vehicles to stationary power

generation with outputs from 100 W to 2 MW

• Advantages : clean device, high efficiency, flexibility in the choice of fuel, internal gas reforming, no moving part…

• Project :

- Work on SOFC anode materials within the NSERC Solid Oxide Fuel Cells Canada Strategic Research Network

- Synthesis of nanoscale material by using plasma technology

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II.II. PROJECT & OBJECTIVESPROJECT & OBJECTIVES

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OBJECTIVES• SOFC anode material : Lanthane Doped Ceria – Lanthane Doped with

Strontium titanate – Yttria Stabilized Zirconia

• Nanopowder synthesis with a pure nanostructured phase of La0.4Ce0.6O2

• Contribution to the anode coating deposition of a suspension of :– La0.4Sr0.6TiO3 and Yttria Stabilized Zirconia on a thin disk

– La0.4Ce0.6O2 - La0.4Sr0.6TiO3 – Yttria Stabilized Zirconia on a thin disk

The coating must be porous, homogeneous and provide a good boundary at the anode/electrolyte interface

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III.III. SOFC FUNDAMENTALSSOFC FUNDAMENTALS

Anh Mai DO QUANG

HOW DOES A SOLID OXIDE FUEL CELL WORK?

– 3 main components : Anode – Electrolyte – Cathode

– Cathode reaction : O2 + 4e- → 2O2-

– Anode reactions : H2 + O2- → H2O + 2e- CO + O2- → CO2 + 2e-

– Reformer reaction : CxH2x+2 + xH2O → xCO + (X+2)H2

– Operating temperature : 600°C-1000 °C6

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Green – Bio – Regular Diesel+ Water

Oxygen

Water + CO2

Electrolyte

CathodeAnode

600-700˚C

e

e e

e e

e

Oe

e

HH

H

HO

2 H2 + O2 = 2 H2O

CO + ½ O2 = CO2O

e

e

Reformer

C

O

OO C

Internal Reformer Supported SOFC Operation Principle

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ANODE REQUIREMENTS

– Stable in a reducing environment– Suitable porosity– Thermal expansion coefficient (TEC) similar to the other

components– Tolerance to sulfur (5000 ppm)– Catalytic activity towards electro-oxidation of fuels– High electronic conductivity – Sufficient ionic conductivity

III.III. SOFC FUNDAMENTALSSOFC FUNDAMENTALS

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IV.IV. METHODOLOGYMETHODOLOGY

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• Synthesis of LDC powder by solution plasma spraying

Solution of La0.4Ce0.6O2 is made of La(NO3)3•6H2O and Ce(NO3)3•6H2O

Plasma torch Tekna PL - 50

Torch nozzle diameter 45 mm

Central plasma gas (Ar) 27 slpm

Sheath plasma gases (O2) 80 slpm

Atomization gas (Ar) 11.4 slpm

Plasma power 35-40 kW

Chamber pressure 150 Torrs

Solution injection flow rate 5-4 ml/min

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Reactor

Filter Unit

Vacuum

Torch

Solution

Porous metal filter

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• Deposition of La0.4Sr0.6TiO3 – Yttria Stabilized Zirconia on a thin Yttria Stabilized Zirconia disk (~380 µm) by suspension plasma spraying

– Solution of La0.4Sr0.6TiO3 + suspension of Yttria Stabilized Zirconia nanopowder.• The solution of La0.4Sr0.6TiO3 was made of a nitrate solution of

lanthanum and strontium which was stirred with titanium propoxide and triethanolamine

– Several tests of the disks in the plasma with varied parameters (spraying distance, power…)

IV.IV. METHODOLOGYMETHODOLOGY

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• Lanthanum Doped Ceria XRD : First Synthesis

V.V. RESULTS & DISCUSSIONSRESULTS & DISCUSSIONS

Plasma power 35 kW

Solution concentration 1 mol/L

Solution injection flow rate 5 ml/min

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• Lanthanum Doped Ceria XRD : Second Synthesis

V.V. RESULTS & DISCUSSIONSRESULTS & DISCUSSIONS

Plasma power 40 kW

Solution concentration 0,8 mol/L

Solution injection flow rate 4 ml/min

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• Lanthanum Doped Ceria TEM : Second Synthesis

V.V. RESULTS & DISCUSSIONSRESULTS & DISCUSSIONS

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• Coating deposition of LST-YSZ on the thin substrate

Proper deposition way and suitable plasma parameters of preventing the YSZ disks from cracking have been finished

The quality of the coating still needs to be improved

V.V. RESULTS & DISCUSSIONSRESULTS & DISCUSSIONS

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CONCLUSION AND FUTURE WORK CONCLUSION AND FUTURE WORK

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CONCLUSION Lanthanum Doped Ceria powder synthesis : suitable parameters have

been found to obtain a pure phase Lanthanum doped Strontium Titanate – Yttria Stabilized Zirconia

deposition : suitable parameters for the survival of disk have been found but not for the quality of the coating

FUTURE WORK:– Lanthanum Doped Ceria powder : Do the synthesis again– Coating deposition of Lanthanum doped Strontium Titanate – Yttria

Stabilized Zirconia : overcome the thermal shock problem (micro-heater), new substrate

– Do experiments for Lanthanum Doped Ceria – Lanthanum Doped with Strontium titanate – Yttria Stabilized Zirconia

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ACKNOWLEDGEMENTACKNOWLEDGEMENT

Anh Mai DO QUANG

SPECIAL THANKS TO :

o Prof. François Gitzhofer, for his general supervision and his advice during the internship;

o Yan Shen, a PhD candidate, for following me up during this internship;

o Kossi Béré, the lab technician, for his precious help during the experiments;

o Mingwen Guo, a Master candidate, for his assistance ;o Stéphane Gutierrez and Charles Bertrand for their work to the

sample characterization ;o SOFC Canada for their funding support and for their invitation to

the SOFC annual general meeting at Calgary.

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