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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 Meir
Sven Rühle
Arie 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
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Based on our parallel research in All-Oxide PV.
Why Oxides?
long term stability
Low Cost synthesis/fabrication
Non-hazardous materials
Abandon materials
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Combinatorial Material Science - Concept Abundance of Elements
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Combinatorial Material ScienceC
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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
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Proof of Concept:
High TC Superconductors
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New Composite Oxides
low impurity concentration
(doping)
new
crystallinephase
new
amorphousphase
polycrystalline composite material – bi-
functional catalysts.
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Combinatorial Material Science
The Ultimate Oxide Electro Catalist
Materials
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Combinatorial Synthesis Methods
Spray Pyrolysis
Pulse Laser Deposition
(+Multi-Source Sputtering)
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Fully Computerized
Combinatorial Synthesis Methods
Pulsed Laser DepositionContinuous Compositional Spread (CCS)
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Composite OxideSrTiO3 + Co3O4
Co3O4
Co3O4
SrTiO3
Jsc
Jsc
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Large Throughput Analysis
Scanning Electrochemical Characterization
Scanning Optical Characterization
Scanning Profilometer
Scanning Electric Conductivity
Scanning X-Ray Diffraction (soon)
Scanning Seebeck Effect (planned)
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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
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Electrochemical Scan ProcedureC
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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
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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
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Scanning Profilometer
d(x,y) = d0 · cosnx(x-x0) · cosny(y-y0)
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Scanning Conductivity
What 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
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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
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Scanning X-Ray Diffraction
What can we extract? phase analysis, structural data
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Presentation of ResultsFe
O2
SnO2
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Database and Data MiningC
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Database and Data Mining
The Ultimate Oxide Electro Catalist
Materials
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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.
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