Cross-cutting Analysis Tools: panel members

p. 1

basic research needs workshop forCarbon Capture: Beyond 2020

Plenary Closing SessionMarch 5, 2010

Cross-cutting Analysis Tools: panel members

* Panel co-lead

Murray Gibson*

Martin Zanni*

Yves Chabal

Phil Grandinetti

Alex Harris

Wendy Mao

Taner Yildirim

Argonne National Laboratory

University of Wisconsin

UT Dallas

Ohio State

Brookhaven National Laboratory

Stanford University

U. Pennsylvania/NIST

p. 2



Cross-Cutting Analysis Toolstechnology challenges

Access to integrated state-of-the-art characterization tools is a challenge

New tools should be developed to address specific challenges especially in-situ, fast processes and interfacial/thin films

Guiding atomic-level synthesis

p. 3



Cross-Cutting Analysis Tools: current status

Include examples of state-of-the-art characterization MOF’s neutron and x-ray pdf TEM example of a membrane? NMR Spectroscopy

p. 4



The use of data from multiple techniques, combined with simulation and modeling, to fully characterize materials

Techniques that can separate individual events from the ensemble over which they are often measured Often demands faster, more sensitive measurement and brighter

sources

Cross-Cutting Analysis Tools: basic-science challenges, opportunities, and needs

p. 5



Potential scientific impact Potential impact on Carbon Capture

Summary of research directionScientific challenges

Cross-Cutting Analysis Tools: In-situ chemistry, structure, and dynamics

•Develop in-situ characterization techniques and sample environments•Develop suite of probes which can couple with the relevant temporal and spatial scales to probe dynamics

•Understanding how carbon capture materials behave under ‘real’ operating conditions (e.g. P-T-x of flue gas)

•Understanding the dynamics involved in the molecular capture and regeneration of the potential host for the range of interactions from physisorption to chemisorption

•Enable materials by design for breakthrough improvements in key transport, reaction and thermodynamic properties under actual conditions of operation.

•New analysis tools for studying structural and dynamic properties of materials under wide P-T-x conditions will have impact not only in carbon capture but also in broad areas of energy research such as catalysis, fuel cell energy conversion and complex materials synthesis

p. 6



• Bridging the gap between model and real materials and conditions. Advanced materials characterization methods are difficult to apply under operating conditions (e.g. varying P-T, under fluid contact, in the presence of reactive or corrosive gases, over many cycles (aging)).

• Structural and dynamics properties of gas capture materials including sorbents, membranes and complex fluids change with conditions and affect the key thermodynamic and kinetic properties that determine performance.

• Advanced sample chambers with suitable windows for access to in-situ characterization via penetrating, non-destructive probes

• Nanoprobes immersed in real environments


Develop in-situ characterization techniques and sample environments

p. 7



• Advanced techniques for characterizing chemistry, structure, and dynamics during CO2 capture and release

• exploit capabilities of synchrotron (and FEL) light sources, neutron, and nanoscience user facilities.

• further develop advanced vibrational spectroscopy techniques

• Timescales ranging from seconds down to femtoseconds (diffusion to bond-breaking and formation); development of ultrafast x-ray and light scattering techniques

• Spatial scales ranging from nanoscale to macroscale (individual CO2 interaction with host to movement of CO2 diffusion front); electron microscopy, x-ray and neutron radiography; nanoscale x-ray diffraction imaging

wew


Develop suite of probes which can couple with the relevant temporal and spatial scales to probe dynamics

p. 8





Cross-Cutting Analysis Tools: Interfacial and thin film characterization

• Develop and apply interface-sensitive methods for interfacial and thin film structure and dynamics at the atomic and molecular level in complex molecular systems: advanced techniques, including user facility capabilities• Master the measurement of mechanical, thermodynamics and transport properties in ultrathin films (<100nm). • Understand near surface fluid properties.

Interfacial and thin film structure/dynamics at the atomic and molecular level determine crucial thermodynamic and kinetic properties of multiphase gas capture media.

Characterization of interfacial or very thin film structure or dynamics are extremely challenging in the midst of complex, often non-crystalline, bulk materials.

Interfacial characterization methods for complex materials will impact the ability to elucidate and design improved interfaces that are critical to many fields of energy science, including catalysis, corrosion, electrical energy storage, and fuel cell energy conversion.

Enable design of complex multiphase gas capture materials such as membranes and complex fluids whose interfaces enable breakthrough performance in high transport kinetics combined with low energy penalty for carbon dioxide separations cycles.

p. 9



• Advanced techniques for atomic structure and dynamics of interfaces using x-rays, electron microscopy, and neutron scattering methods, particularly exploiting capabilities of light source, neutron and nanoscience user facilities.

• New methods for complex liquid interface structure, transport and reactivity. Possible approaches include new molecular beam scattering methods for liquid interfaces.

• Master methods and understanding of interface specific spectroscopies (nonlinear optical, photoemission) and existing surface-compatible spectroscopies (IR, Raman, XPS) for complex, poorly ordered interfaces.

Cross-Cutting Analysis Tools: Interfacial and thin film characterization (1)

Advanced methods for interfacial structure & dynamicsChallenge: Develop interface-sensitive methods for interfacial structure and dynamics and apply in complex gas separations materials.

p. 10



Need to characterize structure on real membranes: nanostructuring, profiling, structural evolution in use

Develop advanced methods such as transmission electron microscopy, grazing incidence x-ray scattering, neutron reflectometry

In-situ properties with TEM, X-ray or spectroscopic microscopy Develop existing in-situ methods (Vibrational, optical, NMR)

Characterize physical properties: mechanical, transport Probe microscopy for microscopic property measurements Derive mechanical and transport properties from interaction potential

sensitive techniques (IR, Raman, NMR) New geometries for transport


Characterization of ultra-thin films (<100nm)Challenge: Ultra thin membranes for high permeance yet robust need to be nanostructured and characterized for structure and properties.

p. 11



Structure of near-interface matters: find methods to characterize as a function of distance from interface Depth profiling of solute concentrations over sub-nanometer distances

near interfaces (x-ray reflectivity, etc.) Time resolved measurements of inhomogeneous growth from surface

Dynamics and transport at interface: dynamic methods Novel molecular beam methods for reactivity/transport at liquid surfaces Dynamic spectroscopies, such as neutron/photon scattering and

vibrational spectroscopies


Near-interface properties of fluids and complex materialsChallenge: Near-interface properties govern wetting in ultrasmall capillaries, kinetics of exchange and reaction, yet are difficult to isolate in bulk matter.

p. 12





Cross-Cutting Analysis Tools: Atomic Scale View of Gas-Host Interactions

• develop tools/methods to … - identify and characterize adsorption sites in solid, liquid, membrane, and hybrid structures. - characterize gas organization, kinetics and dynamics around adsorption sites - distinguish gas from host dynamics - measure bulk phase diffusion of absorbed gases • develop methods to deal with gas molecules in confined environments (e.g. loading) • increased involvement of characterization experts in guiding both synthesis and modeling

Obtain greater level of atomic-level details in gas-host interactions for adsorption sites, kinetics (diffusion, reaction) and dynamics (vibrations, rotation, libration, translation) of molecules in complex media (liquids, solids)

• Validate advanced theoretical modeling Guide development of nanoengineeringImportant for fuel cells, capacitors, batteries, catalysis, high surface area materials applications

• Functional materials for gas adsorption and separationGuide for nanosynthesis

10 year impacts

p. 13



• Locating Guest Molecules by…• Elastic and Inelastic Neutron Scattering• X-ray scattering• Magnetic Resonance• Electron Imaging Methods

• Host Response to Gas Loading

• Matrix Structural Deformation

• Chemical Interaction

Cross-Cutting Analysis Tools:Atomic Scale View of Gas-Host Interactions (1)

Structure Determination in Complex Media

p. 14



• Determining Local Interaction Potentials• Vibrational Response• Frustrated Motion• Validating Theoretical Models

• Fundamental Understanding of Transport

• Spatial Mapping of Interaction Potentials

• Cooperative Effects (Gas-Gas, Host-Phonon, …)

• Disordered (solid and liquid) hosts

• Lower dimensional transport

Cross-Cutting Analysis Tools:Atomic Scale View of Gas-Host Interactions (2)

Kinetics and Dynamics in Complex Media

p. 15



• Unexpected Chemistry• With host or other guest molecules at higher loading• With help of incorporated catalyst (low to high catalyst doping)• Through unsaturated metal centers

• Mechanical Catastrophes

• Internal pressure changes upon heterogeneous loading

Cross-Cutting Analysis Tools: Gas Molecules in Confined Environments (3)

p. 16





Cross-Cutting Analysis Tools: Characterization for guided synthesis &processing

• Nanoscale synthesis: patterning and atomic arrangement in 2-d structures (channels, internal and external surfaces)

• Placement of functional groups in 1-d structures (e.g. mouth of channels)

• Guided synthesis of 3-d materials

Membrane formation

New solid adsorbents

Tunable materials of localized dynamics

Materials with controllable textures

Biomimetic and multifunctional membranes and solid materials

Novel concepts for improving materials functionality (gas storage, separation, reactions)

Novel nanoscale synthesis methods

•Efficient membranes for gas separation

•Efficient nanoporous materials for gas sorption and transformation

•10-20 year impact

p. 17



Develop self-assembly or other methods to nanopattern external and internal surfaces, including channels (liquid and vapor approaches, atomic manipulation methods, etc…)

Develop methods to probe nanopatterning and atomic arrangements, including imaging (electron, force, ..), diffraction (x-ray, electron, neutron), and spectroscopy (vibrational, optical, electron, neutron, etc…)

Develop methods to aid imaging nano- and meso-scale two-dim. structures (e.g. quantum dots, nanoparticles)

Cross-Cutting Analysis Tools: Characterization for guided synthesis &processing (1)

Control of nanoscale synthesis in 1- and 2 dimensions

p. 18



Develop self-assembly or other methods to functionalize the openings of 1-dimensional structures (e.g. channels), such as aligned carbon nanotubes (membranes) or external surfaces of nanoporous channels in crystalline and amorphous materials

Develop methods to probe chemical functionalization at spatially restricted areas such as openings of channels

Cross-Cutting Analysis Tools:Characterization for guided synthesis &processing (2)

“One-dimensional” tailored functionalization

p. 19



New 3-D materials by design “inverse engineering” of new materials Relies on intimate cooperation of innovative materials synthesis,

characterization and computation Goes beyond the empirical trail and error to guide synthesis more

efficiently and more innovatively Co-location or close networking of expertise and capabilities Use-inspired collaborations focused on carbon capture Uses routine, high-throughput techniques, e.g. powder x-ray diffraction,

with innovative methods e.g. in-situ observation of phase nucleation and kinetics

Ultimate aim is predictive capability for new functional materials

Cross-Cutting Analysis Tools:Characterization for guided synthesis &processing (3)

Guided 3-d synthesis & processing

In-situ characterization of materials during synthesis and performance

Atomic level control of dynamics for host-gas interactions

Guided synthesis of new materials and structures with close coordination of novel synthesis, characterization and simulation

Better tools to study structure and properties of interfaces and thin films

Technology Maturation & DeploymentApplied Research Grand Challenges Discovery and Use-Inspired Basic Research

How nature works Materials properties and functionalities by design

Controlling materials processes at the level of quantum behavior of electrons

Atom- and energy-efficient syntheses of new forms of matter with tailored properties

Emergent properties from complex correlations of atomic and electronic constituents

Man-made nanoscale objects with capabilities rivaling those of living things

Controlling matter very far away from equilibrium

BESAC & BES Basic Research Needs Workshops

BESAC Grand Challenges Report DOE Technology Office/Industry Roadmaps

How Nature Works … to … Materials and Processes by Design to … Technologies for the 21st Century

Basic Energy SciencesBasic Energy Sciences Goal: new knowledge / understandingMandate: open-endedFocus: phenomenaMetric: knowledge generation

DOE Technology Offices: EERE, NE, FE, EM, RW…DOE Technology Offices: EERE, NE, FE, EM, RW… Goal: practical targetsMandate: restricted to targetFocus: performanceMetric: milestone achievement

Cross-cutting Analysis Tools: panel members

Documents

Transcript of Cross-cutting Analysis Tools: panel members