kaduk powder diffractionindustrial needs for powder and single crystal diffraction james a. kaduk...

Industrial Needs for Powder and Single Crystal Diffraction

James A. KadukINEOS TechnologiesNaperville IL 60566

James.Kaduk@innovene.com

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?