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Combinatorial Synthesis and High Throughput Screening of Effective Catalysts for Chemical Hydrides
Xiao-Dong Xiang Intematix Corporation
Moraga, CA
– A participant in the DOE Center of Excellence for Chemical Hydrogen Storage –
May 23, 2005
DOE 2005 Hydrogen Program Annual Review Washington, D.C., May 23-26, 2005
This presentation does not contain any proprietary or confidential information Project ID #
STP12
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Overview
Timeline • Project start date:FY2005 • Project end date: FY2009 • Percent complete: New Start
Budget • Expected total project funding
– DOE: $1,100K – Intematix: $277K
• Funding for FY2005: $200K
Chemical Hydrogen Storage Center 2 Intematix
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Overview
Barriers • Cost • Weight and volume • Energy efficiency • System life-cycle assessment • Spent material removal • Regeneration processes
Partners • Collaboration with LANL, PNNL, and UCLA on novel
polyhedral boranes • Future collaboration with Penn, NAU, LANL, PNNL
on amine-boranes • Other collaborations with Center partners based on
future discoveries Chemical Hydrogen Storage Center 3 Intematix
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To assist DOE in achieving the DOE/ FreedomCARtarget of a hydrogen storage system of 6.0 wt.% by 2010
Objectives
target of a hydrogen storage system of 6.0 wt.% by 2010
To assist DOE in achieving the DOE/ FreedomCAR
• Develop and validate high-throughput synthesis and screening methods for new low-cost and effectivecompound catalysts for chemical hydrogen storage(current FY)
• Explore catalysts which could improve the kinetics of hydrogen release from candidate hydrogenstorage materials (next FY and beyond)
• Explore new catalysts and catalytic processes which could significantly enhance regeneration processes(next FY and beyond)
Chemical Hydrogen Storage Center 4 Intematix
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Approach
Hydride Catalyst Design:
LANL, UCLA
Combinatorial Synthesis: Intematix
Combinatorial Catalyst
Development Cycle
High throughput
Intematix
Validation of Leads:
LANL, PNNL, UCLA
Intematix Screening:
Chemical Hydrogen Storage Center 5 Intematix
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Concept of Approach
• Combinatorial Synthesis– Intematix proprietary combinatorial synthesis technology
can generate hundreds of different hydrides/catalysts combinations (thin film or nano-particles) in one experiment under oxygen free environment
• High-throughput Screening– Intematix proprietary combinatorial high-throughput
screening technology can test promising catalysts under realistic reaction conditions (high pressure/temperature, oxygen free)
Chemical Hydrogen Storage Center 6 Intematix
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Challenging Issues
• Reactant stability and catalyst surface contamination – in situ transfer between synthesis and screening
• High-throughput screening of arrayed catalysts (thin film or nano-particles)
• Defining initial screening parameters (hydrogen concentration, end products, temperature, reaction time, reaction rate, etc.) for the arrayed catalysts
Chemical Hydrogen Storage Center 7 Intematix
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Validated a combinatorial molecular beam epitaxy (MBE) system for thin film deposition of compound catalysts
Technical Accomplishments
Validated a combinatorial molecular beam
of compound catalysts
A high temperatureeffusion cell (up to1900ºC) has beeninstalled for catalystelements (such asTi) incorporation
epitaxy (MBE) system for thin film deposition
Chemical Hydrogen Storage Center 8 Intematix
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Validated combinatorial ion-beam sputtering (IBS) system for synthesizing catalysts and materials including air-sensitive compounds
Technical Accomplishments
Validated combinatorial ion-beam sputtering(IBS) system for synthesizing catalysts andmaterials including air-sensitive compounds
A getter pump on the combi-IBS system has been installed to reduce the residual O2
Chemical Hydrogen Storage Center 9 Intematix
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Set up an air-tight oxygen-free glove box for in situ sample transfer and characterization
Technical Accomplishments
Set up an air-tight oxygen-free glove box for in situ sample transfer and characterization
Glove-box
The glove box and the MBE growth chamber are directly connected to allow sample transfer in oxygen-free environment.
MBE
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Validating combinatorial nano-particle (CNP) synthesis system – the third proprietary combinatorial materials synthesis technique Intematix has recently developed
Technical Accomplishments
Validating combinatorial nano-particle (CNP) synthesis
synthesis technique Intematix has recently developed system – the third proprietary combinatorial materials
The advantages:• Small particle size~10-
50nm • Narrow particle-size
distribution • Accessible to most
elements • Can optimize size and
composition rapidly
Chemical Hydrogen Storage Center 11 Intematix
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The CNP system is very unique and powerful in high-throughput synthesis of nano-particles
Technical Results
YIG nano-particle prepared by CNP under preliminary condition. Particle has well-
TEM images of TiO2 nano-particles prepared defined circular shape. The left image showsby CNP under optimized conditions. the crystal structure is not well-ordered.
Chemical Hydrogen Storage Center 12 Intematix
The CNP system is very unique and powerful in high-throughput synthesis of nano-particles
25nm
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Designed and constructed micro-reactor arrays to screen combinatorial catalyst libraries for hydrogen release
Technical Progress
Designed and constructed micro-reactor arrays to screen combinatorial catalyst libraries for hydrogen release
Image of a 3x3 micro-reactor arrays
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Addressing Barriers
• Cost – new non-precious metal alloy or compound catalysts will reduce the total system cost
• Weight and volume – new catalysts for high weight efficiency reactions will reduce the system weight and volume
• Energy efficiency – new catalysts enable high efficiency chemical hydrogen storage
• Regeneration processes – new catalysts may enable low cost regeneration process
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Future Plans
• Remainder of FY2005– High-throughput in-situ catalysts screening � Identify key parameters for high throughput in
situ screening � Demonstrate effectiveness of catalyst
screening methodology for model reaction: catalyst
NaBH4 + 2H2O ⎯⎯⎯→ 4H2 + NaBO2
– Validate the capability of CNP for synthesizing catalyst nanoparticles
Chemical Hydrogen Storage Center 15 Intematix
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Future Plans
• FY2006
– Synthesis and screening of catalyst libraries for hydrogen-release in polyhedral boranes, e.g.
catalysts Na2B10H10•16H2O ⎯⎯→ 2 NaBO2 + 4 B2O3 + 21H2
– Characterization of material properties of lead catalysts � Crystal structure, grain size, and alloy composition of
catalyst materials
Chemical Hydrogen Storage Center 16 Intematix
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Summary of Future Plans
quality thin films
release catalyst libraries
FY2005TASK
candidatesregeneration catalyst libraries
material properties of candidate catalysts
candidates
candidates
Task 1: In-situ high throughput screening of hydrogen release catalysts
Task 2: Synthesis of nanoparticle and high-
Task 3: Synthesis and screening of hydrogen-
FY2006 FY2007 FY2008 FY2009
Down-select best synthesis method
Down-select best
Task 4: Synthesis and screening of hydrogen-
Task 5: Characterization of
Down-select best
Down-select lead
Chemical Hydrogen Storage Center 17 Intematix