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Metal Oxide Combinatorial Synthesis and Characterization. Yaniv Bouhadana Assaf Anderson Eli Rosh- Hodesh Hannah- Noa Barad Simcha Meir Sven Rühle Arie Zaban. Institute for Nanotechnology & Advanced Materials Bar Ilan Universtiy , Ramat Gan 52900 [email protected]. - PowerPoint PPT Presentation
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Metal Oxide Combinatorial Synthesis and Characterization
Institute for Nanotechnology & Advanced MaterialsBar Ilan Universtiy, Ramat Gan 52900
Yaniv Bouhadana Assaf Anderson Eli Rosh-Hodesh
Hannah-Noa Barad
Simcha MeirSven RühleArie Zaban
What is Our Main Goal?
Cheng, F., & Chen, J. (2012).. Chemical Society reviews, 41(6), 2172–92.
We want to find an efficient, durable, low cost electro-catalyst
for metal air batteries
Methodology
Combinatorial Material Science
Metal Oxides
Outlines
• Combinatorial Research ConceptsCombinatorial
• High Throughput Synthesis MethodsSynthesis
• High Throughput Analysis MethodsAnalysis
• Data Mining, DOE, Computational ChemistryData Analysis
Com
binatorialSynthesis
Analysis
Data M
ining
Based on our parallel research in All-Oxide PV.
Why Oxides?
long term stability
Low Cost synthesis/fabrication
Non-hazardous materials
Abandon materials
Com
binatorialSynthesis
Analysis
Data M
ining
Combinatorial Material Science - Concept Abundance of Elements
Com
binatorialSynthesis
Analysis
Data M
ining
Combinatorial Material ScienceC
ombinatorial
SynthesisA
nalysisD
ata Mining
Combinatorial Material Science 60 “useful” elements which are the constituents of ~30.000 inorganic compounds 60 x 60 = 3600 binary compounds (A-B, still not includes AxB,
ABx etc..) most known 60 x 60 x 60 = 216,000 ternary compounds (A-B-C…)
~3% known
Com
binatorialSynthesis
Analysis
Data M
ining
Proof of Concept: High TC Superconductors
Com
binatorialSynthesis
Analysis
Data M
ining
New Composite Oxides
low impurity concentration
(doping)
new crystalline
phase
new amorphous
phase
polycrystalline composite material – bi-
functional catalysts.
Com
binatorialSynthesis
Analysis
Data M
ining
Combinatorial Material Science
The Ultimate Oxide Electro Catalist
Materials
Com
binatorialSynthesis
Analysis
Data M
ining
Combinatorial Synthesis Methods
Spray Pyrolysis
Pulse Laser Deposition
(+Multi-Source Sputtering)
Com
binatorialSynthesis
Analysis
Data M
ining
Fully Computerized
Combinatorial Synthesis Methods
Pulsed Laser DepositionContinuous Compositional Spread (CCS)
Com
binatorialSynthesis
Analysis
Data M
ining
Composite OxideSrTiO3 + Co3O4
Co3O4
Co3O4
SrTiO3
Jsc
Jsc
Com
binatorialSynthesis
Analysis
Data M
ining
Large Throughput Analysis
Scanning Electrochemical Characterization Scanning Optical Characterization Scanning Profilometer Scanning Electric Conductivity Scanning X-Ray Diffraction (soon) Scanning Seebeck Effect (planned)
Com
binatorialSynthesis
Analysis
Data M
ining
Electronics: BioLogic Potentiostat (includes FRA Module) Tango XYZ table. Perestaltic Punp (RS485/232 controled). Silent vacume pump + solution trup.
Mechanics: Special smaple holder (secured). Spacial surface Portable electrocemical cell. Tubing.
Softwere: Operating softwere. Analisys softwere.
Scanning Electrochemical Meas.C
ombinatorial
SynthesisA
nalysisD
ata Mining
Electrochemical Scan ProcedureC
ombinatorial
SynthesisA
nalysisD
ata Mining
At the initial stage the measurement that is preformed in the electrochemical scanner is cyclic voltammetry and the percentage of oxygen is constant.
Portable electrochemical cell• 3 Electrodes Cell:
– Counter : any metallic foil : preferred – platina foil, current – stainless steel.
– Working : the combinatorial samples bases on FTO.
– Reference : Ag/AgCl (Kalomel) , PdS
Electrolyte : Polysulfide, K3Fe(CN)6/K4Fe(CN)6/KCl
Ref
Counter
Solution In
Solution Out
Scanning Electrochemical Meas.C
ombinatorial
SynthesisA
nalysisD
ata Mining
Scanning Optical Characterizationdesigned by Dr. Assaf Anderson
What do we measure? Total Transmission Total Reflection Specular Reflection 350 – 1100 nm
What can we extract? absorption coefficient thickness band gap
Com
binatorialSynthesis
Analysis
Data M
ining
Scanning Profilometerd(x,y) = d0 · cosnx(x-x0) · cosny(y-y0)
Com
binatorialSynthesis
Analysis
Data M
ining
Scanning ConductivityWhat do we measure? I-V curve (2 point or 4 point
contact) temperature dependent (planned)
What can we extract? conductivity σ / resistivity ρ thickness activation energies
(planned)
Example: Resistance of ZnO with linear thickness gradient
Com
binatorialSynthesis
Analysis
Data M
ining
Scanning Seebeck Effect Meas.(planned)
SA, SB = Thermopower or
Seebeck Coefficient
What do we measure? Voltage
What can we extract? Seebeck coefficient type of doping (n or p)
Heater
Com
binatorialSynthesis
Analysis
Data M
ining
Scanning X-Ray Diffraction
What can we extract? phase analysis, structural data
Com
binatorialSynthesis
Analysis
Data M
ining
Presentation of ResultsFe
O2
SnO2
Com
binatorialSynthesis
Analysis
Data M
ining
Database and Data MiningC
ombinatorial
SynthesisA
nalysisD
ata Mining
Database and Data Mining
The Ultimate Oxide Electro Catalist
Materials
Com
binatorialSynthesis
Analysis
Data M
ining
Summary Combinatorial Material Science – Concept
Let’s look into the unknown
Combinatorial Synthesis Methods Spray Pyrolysis/ PLD High Throughput Analysis
optical, conductivity, profilometer,
electrochemical , etc. Data Mining and Theoretical Chemistry
Proof of Concept, lookout for trendlines and
predict our next research items.
Com
binatorialSynthesis
Analysis
Data M
ining
Thank you for your attention!