| Slide1 : Advancement of TEDDI for studies of materials chemistry processing and environmental systems
Paul Barnes
(Industrial Materials Group) Department of Crystallography,
Birkbeck College, Department of Chemistry,
University College, University of London |
| Slide2 : Daniel Häusermann & Bob Cernik
Andy Jupe, Sally Colston, Jeremy Cockcroft, David Hooper, Mark Betson, Adrian Rennie, Katie Pile, Kevin Roberts, Xiaojun Lai, Richard Williams, Gordon Tiddy, Helen Dutton............ TEDDI
Tomographic Energy-Dispersive Diffraction Imaging Paul Barnes, Christopher Hall, Simon Jacques |
| Slide3 : TEDDI
Tomographic Energy-Dispersive Diffraction Imaging G Harding et al 1990 Phys. Med. Biol. 35 33-41
Energy-dispersive X-ray diffraction tomography
G. Harding, M. Newton and J. Kosanetzky Philips GmbH, Hamburg, West Germany Print publication: Issue 1 (January 1990)
Abstract. A novel tomographic imaging technique is described based on the energy analysis, at fixed angle, of coherent X-ray scatter excited in an object by polychromatic radiation. The authors term their technique 'energy-dispersive X-ray diffraction tomography' (EXDT). It permits the X-ray diffraction properties of small voxels of an extended object to be measured in vivo. Tomographic information is obtained directly without the need to reconstruct from projections. EXDT images of a simple test object comprising water and various plastic materials are presented to illustrate the feasibility of the technique. Potential applications of EXDT in bone imaging are discussed. |
| Slide4 : The basic principle of TEDDI |
| Slide5 : i The problem of the long lozenge dimension
• high X-ray absorption
• long d-spacings
requires working at small 2θ-angles (Edsinθ = hc/2) low
2θ-angle long lozenge |
| Slide6 : Two defining examples of 2D-TEDDI
• PEEK phantom disk (spatial resolution)
• concrete block (size scale) |
| Slide7 : • PEEK phantom disk (spatial resolution)
25 mm (effective lozenge size = 36 μm) |
| Slide8 : • concrete block (size scale) (concrete block is 77 × 78 × 42 mm) |
| Slide9 : • concrete block (size scale)
maps: calcite dolomite portlandite ettringite
aggregates cement hydrates |
| Slide10 : defining characteristics
• PEEK phantom disk (spatial resolution)
• concrete block (size scale)
exploiting the features of an ED-pattern
• fluorescence lines (composition, tracers)
• relative intensities (alignment)
two recent "dynamic" examples
• hydrothermal (autoclave) synthesis (1D)
• chemical engineering processing (2D)
|
| Slide11 :
exploiting the features of an ED-pattern
• fluorescence lines (composition, tracers)
• relative intensities (alignment)
|
| Slide12 : • diffraction + fluorescence lines Characterisation of porosity in English chalk (Betson et al.)
(porosity 20-45%; pore range ~0.01 - 100 μm with mean ~0.5 μm)
|
| Slide13 : Characterisation of porosity in English chalk
Cs-fluorescenc-TEDDI versus solution saturation
(sample 10×10×5 mm; beam 1 mm; 2θ~2.2, 5.0, 7.8°; Δt=270 s)
|
| Slide14 : Characterisation of porosity in English chalk
(2) Comparison of calcite-diffraction-TEDDI
versus
Cs-fluorescence- TEDDI |
| Slide15 :
useful fluorescence peaks (keV) |
| Slide16 :
exploiting the features of an ED-pattern
• fluorescence lines (composition, tracers)
• relative intensities (alignment)
|
| Slide17 : • relative intensities (alignment)
Alignment of kaolinite platelets under flow (Rennie, Barè, Cockcroft et al.)
(Details: flow pipe ×-section = 1mm × 10 mm; EDD beam ×-section = 100m 5 mm;
water/particles flow rate = 1.5 ml s-1; 2θ = 3.9º; pattern collection times = 2-10 min) |
| Slide18 : Two recent "dynamic" examples
• hydrothermal (autoclave) synthesis
(1D-TEDDI; changing system)
• chemical engineering processing
(2D-TEDDI; dynamic equilibrium system)
|
| Slide19 : Two recent "dynamic" examples
• hydrothermal (autoclave) synthesis
(1D-TEDDI; changing system)
• chemical engineering processing
(2D-TEDDI; dynamic equilibrium system)
|
| Slide20 : SR hydrothermal synthesis: birth of a (seeded) zeolite-4A membrane 1D-scan: |
| Slide21 : hydrothermal synthesis: birth of a (seeded) zeolite membrane |
| Slide22 :
point 7/13 after 111 min. points 6-13 throughout synthesis (2 = 4.0046º) hydrothermal synthesis: birth of a (seeded) zeolite membrane |
| Slide23 : Example EDD pattern (2 = 2.5) hydrothermal synthesis: zeolite crystallisation on ceramic support |
| (2): zeolite crystallisation on ceramic support :
(2): zeolite crystallisation on ceramic support 1 2 3 |
| Slide25 : Absorption during these in situ (hydrothermal) studies |
| Slide26 : Two recent "dynamic" examples
• hydrothermal (autoclave) synthesis
(1D-TEDDI; changing system)
• chemical engineering processing
(2D-TEDDI; dynamic equilibrium system)
|
| Slide27 : Two recent "dynamic" examples
• hydrothermal (autoclave) synthesis
(1D-TEDDI; changing system)
• chemical engineering processing
(2D-TEDDI; dynamic equilibrium system)
|
| Slide28 : (1): use of TEDDI in the polymorphism story:
α-/β-glutamic acid as a model polymorphic system
(S.D.M. Jacques, K. Pile, X. Lai, P.Barnes, K.J. Roberts, R.Williams)
|
| Slide29 : (1): use of TEDDI in the polymorphism story:
α-/β-glutamic acid as a model polymorphic system |
| Slide30 : β-glutamic acid v mixer speed, many hkl |
| Slide31 : β-glutamic acid v mixer speed, 004 alignment |
| Slide32 : β-glutamic acid v mixer speed,
"on-edge 004 alignment band" |
| Slide33 : (2): use of TEDDI to examine mixing:
|
| Slide34 : Attributes of TEDDI being EDD, patterns can be collected rapidly
both diffraction and fluorescence peaks are used
useful synchrotron X-ray energy range is 20-125 keV
at these energies, X-rays are highly penetrating
the technique is non-destructive
the site can be re-visited over seconds or months
the sampling shape (lozenge) is awkward
EDD peak resolution is low
2D/3D maps are slow, even at 1 second per pixel |
| Slide35 : overcoming the speed/dimensionality problem real time 1D-TEDDI? R S; R~S |
| Slide36 : overcoming the speed/dimensionality problem real time 2D-TEDDI? |
| Slide37 : Energy resolving detector array: 256 300×300m2 pixels Femtosecond laser-drilled holes in 0.5 mm W-plate realisation of real time 2D-TEDDI? (+ Bob Cernik, Bill O'Neill, Paul Seller) |
| Slide38 : Sponsorship,
Facilities
EPSRC, CCLRC
SRS, ESRF
MEL Chemicals
BNFL
Castle Cement
Schlumberger CR
Acknowledgements Collaborators
Jeremy K. Cockcroft, John Bensted, Mark Betson, Sally Colston, David Hooper, Simon Jacques, Andrew Jupe, Katie Pile, Dmitry Strusevich, Martin Vickers, Paul Stukas
Chris Hall, M. Hanfland & ESRF staff, Adrian Rennie, Scott Owens, S.Barè, Dave Taylor & SRS staff, Bob Cernik, Bill O'Neill, Paul Seller, G. Sankar, Andy Beale, Dick Livingston, Daniel Häusermann, Bob Cernik, Kevin Roberts, Xiaojun Lai, Richard Williams, Tim de V.Naylor, Gordon Tiddy, Helen Dutton …
|
| Slide39 : Miscellanea TEDDI map interpolations: Kriging interpolation between nodes;
Journel, AG. & Huijbregts, CHJ, Mining Geostatistics, Academic Press - N.Y. (1981).
Oliver, MA & Webster,R, Inter. J. Geogr. Inf. Syst. 4, 313 (1990).
Surf/surfc routines in MATLAB package, in which the colour within a surface patch is a bilinear
function of the local coordinates
3-element ED-Ge-detector:
8 mm diam.× 6 mm thickness; ΔE=135-140 eV at 5.9 keV; ΔE=460-466 at 122 keV
Oxford Dictionary definition of tomography:
tomography ►noun [mass noun] a technique for displaying a representation of a cross section through a human body or other solid object using X-rays of ultrasound.
- DERIVATICES tomographic adjective.
- ORIGIN 1930s: from Greek tomos ‘slice, section’ + -GRAPHY. |