Metal Oxide Combinatorial Synthesis and Characterization

Metal Oxide Combinatorial Synthesis and Characterization

Institute for Nanotechnology & Advanced MaterialsBar Ilan Universtiy, Ramat Gan 52900

yaniv.phd@gmail.com

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

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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

ombinatorial

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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 crystalline

phase

new amorphous

phase

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

ombinatorial

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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

ombinatorial

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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 Profilometerd(x,y) = d0 · cosnx(x-x0) · cosny(y-y0)

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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

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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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Yaniv.phd@gmail.com

Thank you for your attention!