# Presentation: 665451

## Next generation powder diffraction

- Bill David
- ISIS Facility, Rutherford Appleton Laboratory

## 2015 challenges

- Bill David
- ISIS Facility, Rutherford Appleton Laboratory

## Opportunities

**Total **
**crystallography**

**Total scattering**

**Microbeam **
**imaging**

## Functional materials

- H-bonding from model systems to supramolecular chemistry
- Novel highly complex molecules or structures;
- Ceramics, dielectrics and ferroelectric materials
**Nanotechnologies**
- Molecular and mesoscopic scale phenomena
- Nano-structured alloys and composites ; Nanotubes
- Self-assembling structures; Surfactant mesophases
- Microemulsions and diffusion at the molecular level
**Cultural Heritage & Archeology**
- Heterogeneous characterisation of archaeological artefacts
**Sustainable development**
- Fuel cells; Structure and dynamics in hydrogen storage materials. Characterisation of lifetime performance of rechargeable batteries. Energy conversion. Concrete ageing. Lightweight batteries for electric vehicles. Lightweight, superhard alloys and polymers
**Information technology**
- Behaviour of oxygen in device materials; Photonic materials
**Catalysis and clean technologies**
- Production of hydrogen for fuel cells; In-situ catalytic reactions
- Processes involving non-hydrogenous compounds,
- e.g. CO, SO2, NOx; Improving clean processes

**Measuring complexity with precision**
- e.g. novel highly complex molecular and macromolecular structures, heterogeneous catalysts
**Measuring order and disorder**
- Beyond the average structure – high Tc / GMR / molecular - (elastically-resolved) diffuse scattering
- Blurring the distinction between crystalline and non-crystalline systems.
- e.g. parametric studies of ordered and disordered        systems - nanomaterials
**Measuring under real conditions**
- Characterisation of lifetime performance of rechargeable batteries, hydrogen storage materials, catalysts
**Measuring rapid kinetics**
- In-situ catalytic reactions, structural transformations
**Measuring multi-parameter space**
- Diffraction measurements as a function of p, T, ...
**Measuring real-space inhomogeneity**
- Raster scanning heterogeneous systems

## Functional materials

- H-bonding from model systems to supramolecular chemistry
- Novel highly complex molecules or structures;
- Ceramics, dielectrics and ferroelectric materials
**Nanotechnologies**
- Molecular and mesoscopic scale phenomena
- Nano-structured alloys and composites ; Nanotubes
- Self-assembling structures; Surfactant mesophases
- Microemulsions and diffusion at the molecular level
**Cultural Heritage & Archeology**
- Heterogeneous characterisation of archaeological artefacts
**Sustainable development**
- Fuel cells; Structure and dynamics in hydrogen storage materials. Characterisation of lifetime performance of rechargeable batteries. Energy conversion. Concrete ageing. Lightweight batteries for electric vehicles. Lightweight, superhard alloys and polymers
**Information technology**
- Behaviour of oxygen in device materials; Photonic materials
**Catalysis and clean technologies**
- Production of hydrogen for fuel cells; In-situ catalytic reactions
- Processes involving non-hydrogenous compounds,
- e.g. CO, SO2, NOx; Improving clean processes

- crystalline

**3nm**

- single crystal

- powders

- amorphous

- From the micron to the angstrom

## Micron diffraction:	Powder or single crystal?

## Slide 7

## Structure solution of polycrystals

- 70 grains of size < 1m
- 1400Ă3 C2/c

## Structural crystallography @ synchrotrons 10 years from now 

- Structural crystallography @ synchrotrons 10 years from now
- 4D movies with time resolution of < 1 minute
- 1 mm3 specimens with a resolution of 1 μm3
- 100 μm3 specimens with a resolution of 100 nm3
- Combination: tomography diffraction (3DXRD) crystallography

## Wish list ...

- Ultra-high resolution powder diffraction
- ID31 resolution or better
- Ensuring high counts @ high Q
- detector solid angle increases with 2
- Mitigating against radiation damage
- ability to lower flux on sample while increasing detected flux
- High spatial resolution powder diffraction
- 4D crystallography; combinatorial thin films
- Rapid kinetic measurements
- area detectors; combinatorial thin films
- Powder diffraction +
- enhanced sample environment
- Another name for powder diffraction ...

## Wish list – more detector coverage at high angles

## Wish list – more detector coverage at high angles

- More precise refinements
- high resolution information obtained from high angle data
- Higher count-rates
- rate limiting step is obtaining good data at high angles

## Wish list – more detector coverage at high angles

- More precise refinements
- high resolution information obtained from high angle data
- Higher count-rates
- rate limiting step is obtaining good data at high angles
- PDF analysis becomes more accessible
- accurate high Q data necessary for good PDF analysis
- beyond the average structure – crystalline disorder
- High quality line-shapes at high as well as low angles
- “small angle scattering” around hkl rather than 000 reflections
- beyond the average structure – particle size and strain

## Wish list – more detector coverage at high angles

- CeO2 round robin sample

## Wish list – more detector coverage at high angles

- CeO2 round robin sample
- 	– accurate line-shape analysis gives size distribution information

## Paracetamol

- _Objectives_
- to study the formation of various hydrates
- to determine crystal structures of new phases
- to understand the nature of the phase transformations

- C8H9NO2.nH20
- pain-killer, analgesic, antipyretic
- 4'-hydroxyacetanilide,
- acetaminophen, tylenol

## Paracetamol – dehydration studies

## Paracetamol – dehydration studies

- water+dissolved
- paracetamol

- crystallisation
- + ice formation

- ice melting

- trihydrate

- step-function in
- water background

- trihydrate – monohydrate
- transformation

- novel phase
- formation

- new intermediate phase

- monohydrate

- 2 mins

## Comparing paracetamol trihydrate structures

## Paracetamol trihydrates (postscript)

## Slide 22

## “High Throughput Synthesis and Screening of Novel Hydrogen Storage Materials” 	DTI/EPSRC funded project

- “High Throughput Synthesis and Screening of Novel Hydrogen Storage Materials” 	DTI/EPSRC funded project

## The Periodic Table of the Elements

- The mass of each element is indicated by the height of each histogram.

## Si

- A tractable combinatorial challenge

- ... playing the odds

- elements 1,3,5,7,11

## Slide 26

## Primary screen

- How: Physical Vapour Deposition
- Where: Ilika (www.ilika.com)
- Throughput: 104 material pixels / day
- Quantity/sample: ~10-12 g
- Absorption characterisation: imaging
- Structural fingerprinting: ESRF/diamond

- Ilika combinatorial PVD plate

- diamond

- ESRF: ID11
- 1 pixel / 5 secs (now)
- 20 frames/sec
- 1 pixel / 0.5 secs
- 30×30 grid – 7.5min

## Secondary  screen

- Tertiary  screen

- How: Robotic synthesis
- Where: RAL
- Throughput: 102 samples / day
- Quantity/sample: ~10-3 g
- Absorption characterisation:  Volumetric
- Structure refinement: ESRF/diamond

- How: Chemical synthesis
- Where: Oxford
- Throughput: 1 sample / day
- Quantity/sample: ~1g
- Absorption characterisation: IGA
- Full structural characterisation: ISIS

- Robotic screening

- X-ray robot

- IGA apparatus

- ISIS

## Secondary  screen

## Slide 30

## Li3N + H2  	Li2NH + LiH + H2  LiNH2 + 2LiH 		

- 2 theta

## Li3N + H2  	Li2NH + LiH + H2  LiNH2 + 2LiH 		

- Li3N + H2  	Li2NH + LiH + H2  LiNH2 + 2LiH

- 2 theta

- Li2-xNHx

- 

- Li1.15(10)NH1.85(10)

## Li3N + H2  	Li2NH + LiH + H2  LiNH2 + 2LiH 		

- 2 theta

## Li3N + H2  	Li2NH + LiH + H2  LiNH2 + 2LiH 		

- 2 theta

## Li3N + H2  	Li2NH + LiH + H2  LiNH2 + 2LiH 		

- 2 theta

*a**n **= a**lo** + n*(a**hi** - a**lo** )/*10
*x**n **= x**lo** + n*(x**hi** - x**lo** )/*10

## Li3N + H2  	Li2NH + LiH + H2  LiNH2 + 2LiH 		

- Li3N + H2  	Li2NH + LiH + H2  LiNH2 + 2LiH

- 2 theta

## Li3N + H2  	Li2NH + LiH + H2  LiNH2 + 2LiH 		

## LiNH2

- LiNH2

- NaNH2

- Mg(NH2)2

- LiBH4

- NaBH4

- LiAlH4

## LiNH2 : NaNH2  phase diagram 		

- LiNH2 : NaNH2  phase diagram

- LiNH2

## LiNH2 : NaNH2  phase diagram 		

- LiNH2

- Li1-xNaxNH2

## Wish list ...

- Ultra-high resolution powder diffraction
- ID31 resolution or better
- Ensuring high counts @ high Q
- detector solid angle increases with 2
- Mitigating against radiation damage
- ability to lower flux on sample while increasing detected flux
- High spatial resolution powder diffraction
- 4D crystallography; combinatorial thin films
- Rapid kinetic measurements
- area detectors; combinatorial thin films
- Powder diffraction +
- enhanced sample environment
- Another name for powder diffraction ...
- real materials diffraction from the angstrom to the micron