kaduk powder diffractionindustrial needs for powder and single crystal diffraction james a. kaduk...
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Industrial Needs for Powder and Single Crystal Diffraction
James A. KadukINEOS TechnologiesNaperville IL 60566
Industrial problem solving is almost by definition
multi-hamlet and multi-village!The synchrotron is an extension
of the home lab.
Single Crystal Diffractionget the model (from a microcrystal)
A microdiffraction set-up for nanoporous metal-organic-framework-type solids, Christophe Volkringer, et al., Nature Materials 6, 760 - 764 (2007).MIL-110 from a 3 × 3 × 10 μm crystal
Powder Diffraction
• Structure solution and refinement• Micro(nano)structure characterization• In situ characterization of real systems
Multiple Partially-Occupied Sites
10 20 30 40 50 60 70 80 90Two-Theta (deg)
x103
5.0
10.0
15.0
20.0
Inte
nsity
(Cou
nts)
[moor242.raw] 22006-106-3 Batch 83 (40,40,0.3,zbc ) JAK
Profile Shapes
In situ Characterization
Every catalyst I have ever characterized at reaction conditions has had a different structure than at ambient conditions!
RT 300°C
Environments
• Vacuum, nitrogen, helium• 3000 psig hydrogen• Butane + air• Propylene + air + ammonia• …
Put the beam there
• Interactions between phases (interfaces) in a polycrystalline catalyst
• A particular spot in a catalyst particle• Defects, inclusions, impurities, failures
(environmental SEM at sample position?)
Dispersed Systems as f(t, …)
10 20 30 40 50 60 70 80 90Two-Theta (deg)
x10 3
5.0
10.0
15.0
20.0
25.0
30.0
35.0
40.0
45.0
Inte
nsity
(Cou
nts)
[nube130.raw] 22126-94DW (40,40,0.3) JAK
10 20 30 40 50 60 70 80 90Two-Theta (deg)
x10 3
2.0
4.0
6.0
8.0
10.0
Inte
nsity
(Cou
nts)
[vido24.raw] 0235-85 (40,40,0.3,Kapton) JAK
Polymers (and Catalysts)
ambient 2X draw
In situ porosity measurements
Quantitative SAXS from > 2 phase systems
What does it cost to patent the wrong thing?