Rutherford Appleton Laboratory Campus Martin Owen Jones Energy - PowerPoint PPT Presentation

Rutherford Appleton Laboratory Campus Martin Owen Jones – Energy Materials Coordinator, ISIS facility Chiu Tang - Principal Scientist for Beam line I11, Diamond Light Source

Harwell Science & Innovation Campus Diamond Lasers ISIS Big Facilities for Small Science

ISIS Beam lines Diamond Beam lines

Neutron cross-section - isotopic dependence Li Li Li Li C C C C S S S S Mn Mn Mn Mn Zr Zr Zr Zr Cs Cs Cs Cs H H H H O O O O X-rays X-rays neutrons neutrons

Diamond and ISIS beam lines Chemical Information Physical Information / Diffraction µ m Size: < Å Å and nm nm

100000 High Resolution Powder Diffraction (a) 3000 LaB 6 Data Intensity (counts) Fit 80000 2000 E=15 keV Dif hkl 1000 60000 Intensity (counts) 0 40000 MACs 100 110 120 130 140 2 θ (deg.) 20000 0 Robotic arm 20 40 60 80 100 2 θ (deg.) PSD Large XYZ table Carousel (200 samples)

Infineum cell with multi-sample holders (-30°C) on I11 • Introduction of biofuels brings unintended consequences – especially crystallization problems in engines during winter temperatures. It is important to understand the problem so we can cure it. • Crystal morphologies/unit cells and habit are crucial to crystallisation process. • Work underway on I11 to study crystal structures and crystallisation, particularly from solution data, and the effect of additives Crystallisation data as a function of temperature

I19 Small Molecule Single-Crystal Diffraction Experimental hutch 2 (EH2) – large heavy duty 4- Mono beam size at sample = 50 - 100 µ m 2 circle diffractometer for large, bulky, sample Single crystal size ~ 20 – 100 µ m environment cells (cryostat, pressure or chemical cell, others) Experimental hutch 1 (EH1) – for relatively “conventional” structural chemistry – albeit on extremely challenging systems (small weakly diffracting samples with poor crystallinity). EH 1 4-circle diffractometer EH 2 Robotic sample changer

Crystal structure, active-site Nuclear density maps (a,c) and electron density maps (b, d) and hydrogen position unambiguously identify determination deuterium atoms (white)

I22 - Endstation Beamline I22 - Non-Crystalline Diffraction (NCD) What information? SAX NCD provides information on the WAX structure and dynamics of large molecular assemblies in low ordered environments. These are characteristic of many complex materials such as biofuels, polymers and colloids.… Techniques: Small and Wide Angle Scattering (SAXS & WAXS) Length scale 10Å - 10000Å (1µm)

Total Scattering Instruments GEM 0.04Å -1 < Q < 15Å -1 ~0.4Å to >10Å POLARIS 0.2Å to 21Å WISH 0.7Å to 50Å NIMROD 0.01Å -1 < Q < 50Å -1 <1Å to >300Å

GEM : LOCAL STRUCTURES IN PEROVSKITES Bi Bi(Ti 3/8 Fe 2/8 Mg 3/8 )O 3 possible lead-free replacement for PZT piezoelectric material. RMC modelling of Fe provide insights Ti into several unexplained aspects of earlier crystallographic studies. Locally monoclinic Mg clusters accounts for micro-strain broadening required for Rietveld refinement using the Chong et al , 2012 rhombohedral structural model.

I12 Joint Engineering Environment and Processing (JEEP) High energy X-rays - 50 keV – 150 keV (0.28 Å - 0.08 Å) X-ray tomography , difffraction and scattering EH2: heavy duty (white or monochromatic beam) sample goniometer) EH1 EH2: External large hutch EH2 (external) Four stroke engine

23 elements ED detector Large sample I12 - 1 st Exp. Hutch (EH1) goniometer Furnace Installed (100-1000 o C) Cold Stage Installed Heraeus “Nobleight” IR lamp heating Two thermo-electric elements. coolers, at top and bottom of sample Split furnace fits cup. around load chain and sample. temperature range of Temperature +20 to -20 o C. monitoring with thermocouples

Neutron tomography ENGIN-X : CRACKING OF MAGNESIUM ALLOYS Turski et al (2010).

Beamline B22 - Infrared Microspectrocopy A complex material: organic To study molecular structures and their physical, matter typical chemical and boilogical properties. spectrum Applications: life sciences, solid state physics & chemistry, forensic, polymer, …. A simple gas: water vapor B22 layout

Chemical Spectroscopy at ISIS Timescales [sec] 1x10 -7 to -11 -12 -13 -14 -15 -16 -17 1x10 1x10 1x10 1x10 1x10 1x10 1x10 1x10 -11 Simultaneous high- Photons resolution Brillouin, THz & Raman Infrared & Raman VIS, UV, X-ray Spectroscopy Spectroscopy (not precisely equivalent) diffraction Surface ce Cata talyti tic Quant ntum um Prot oton on condu duction on Adsor orpt ption on Activity Ef Effec ects Inelastic (lattice & intramolecular modes) MA MAPS High en ener ergies es Neutrons Deep Inelastic Single-particle (Compton) Scattering Quasielastic (diffusion / tunnelling) elastic Widest spectral 0 1 2 3 4 5 6 10 10 10 10 10 10 10 line Energy [meV] range in the IRIS OSIRIS world Inter ermed ediate en e ener ergies es Low e energy ( (Brillou illouin in, THz) (infrared, Ra Rama man)

I15: Extreme conditions White and monochromatic E = 20 -80 keV Beam size at sample: 30 – 80 µ m 2 2D detector Diamond anvil (120) FeGe cell (DAC) p=29.4 GP a T=230 K Diamond E=30 keV anvil Intensity (counts) (211) (321) (111) (221) (200) (311) (320) (310) (400) (220) Metallic gasket (+ sample) 5 10 15 20 25 2 Theta (degree)

In-situ d-spacing • (a) high temperature (> 600 K), flow-through, Swagelok™ sealed stainless steel cell • (b) high temperature gold wire sealed Zircaloy™ cell and (c) low volume • (d) high volume O-ring sealed aluminium cells for batch reactions • (f) aluminium cell for off-line prepared samples • (g) low temperature (323 K <) indium wire sealed aluminium cell • (h) flow-through, Conflat™ sealed stainless steel cell for use on MARI at ISIS.

I11 Long Duration Experiments (LDE) • Slow dynamics in natural systems, engineering processes and energy materials • Important information on the development of phases over time cannot be obtained via ex-situ methods • Use LDE to periodically monitor the experiment in-situ over longer timescales (weeks, months, years...) Areas of Scientific Interest Project key milestones • Energy • Start of project (Oct 12) √ • Catalysis • LDE Hutch built (Jul 13) √ • Environmental • Cabin and Service (Sep13) √ • Radiation exposure • Diagnostic & Shutter (Jan 14) √ • Pharmaceuticals • PSS system (Mar 14) √ • Metallurgy and alloys 1 st beam (Apr 14) √ • • Gas storage materials • Test samples with beam (Jul 14) √ • Corrosion 1 st Users and LDE expt (Oct 14) √ •

Joint ISIS –Diamond CDT Training School 9 th – 15 th March 2015 Neutrons X-rays Muons Diffraction, Spectroscopy, Magnetism, Modelling and Theory

Harwell Science & Innovation Campus Single Crystal Spectroscopy Tomography Total Scattering Diffraction In-Operando