Small-angle x-ray scattering...and crystallisation processes
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1 هب انم خدا
2 Small-angle x-ray scattering......and crystallisation processes Rudolf Winter Daniel Le Messurier Andy Lyons Kristin Høydalsvik Chris Martin 1 Graham Clark 1 Armin Hoell 2 Dragomir Tatchev 2 Sylvio Haas 2 Materials Physics Ffiseg Defnyddiau 1 STFC Daresbury Laboratory 2 Hahn-Meitner Institut Berlin
3 Small-angle x-ray scattering Anomalous SAXS Nanoscale refractory analogue - Gelation & Calcination - Sintering
4 A small-angle x-ray scattering camera flight tube e.g.: HMI SAXS beamline at Bessy, Berlin sample position detector x-rays from storage ring
5 Small-angle scattering vs. diffraction k k' q=k'-k q = (4 sin x-rays scatter from electrons neutrons scatter from nuclei and magnetic moments diffraction small-angle scattering - scattering from atomic structures - size of objects ~ - small length scale -> large angle - scattering from interfaces - size of objects >> - large length scale -> small angle
6 SAXS and particle size
7 SAXS and particle size
8 What can we learn from a SAXS pattern? Porod slope at larger q q -n where n represents the surface morphology n=4: smooth 3<n<4: surface fractal 1<n<3: mass fractal Guinier regime Guinier radius is proportional to the particle size (radius of gyration of the particles)
9 Small-angle x-ray scattering Anomalous SAXS Nanoscale refractory analogue - Gelation & Calcination - Sintering
10 Anomalous SAXS Resonant scattering and absorption Side effects not entirely unwanted! experiment at 18keV -> compressed q scale difference patterns reveal which features are due to edge element even if partial scattering functions cannot be computed atomic scattering factor: f(q,e) = f 0 (q) + f '(q,e) + jf (q,e) scattered intensity ~ f 2 = f f 0 f ' + (f ' 2 +f 2 ) normal SAXS correlations btw. edge element & others correlations between labelled phases only
11 Chemical contrast ASAXS: 3 energies below the edge => determine partial structure factors but: chemical edge shift photon energy calibrated to Zr foil at keV 8eV chemical shift of edge in unreacted sample edge shifts by several ev as reaction progresses
12 Chemical contrast Energy-dependent SAXS: compare above/below edge => maximum contrast with little uncertainty w.r.t. chemical shifts but: fluorescence photon energy calibrated to Zr foil at keV 8eV chemical shift of edge in unreacted sample edge shifts by several ev as reaction progresses
13 Finding the resonance 1. Absorption measurement gives f": f"(e) ~ E µ(e) 2. Extend the measured range according to tabulated data 3. Kramers-Kronig transform gives f':
14 Small-angle x-ray scattering Anomalous SAXS Nanoscale refractory analogue - Gelation & Calcination - Sintering
15 Precursors and ceramics under heat load How do particles in a ceramic bond to the matrix? reactive sintering annealing
16 Small-angle x-ray scattering Anomalous SAXS Nanoscale refractory analogue - Gelation & Calcination - Sintering
17 Making a sol-gel ceramic 1. Gelation. Zr(OiPr) H 2 O = Zr(OH) iproh In-situ SAXS experiment at Daresbury q / nm
18 Making a sol-gel ceramic 1. Gelation. Zr(OiPr) H 2 O = Zr(OH) iproh 3. Calcination. ZrO 2 2 H 2 O = ZrO H 2 O and crystallisation beamstop structure factor macro scatterers individual scatterers q / nm Drying. Zr(OH) 4 = ZrO 2 2 H 2 O and polymerisation 10. q / nm Polymerisation precedes crystallisation. Nuclei form at room temperature, crystallisation requires ~800 o C to activate.
19 Small-angle x-ray scattering Anomalous SAXS Nanoscale refractory analogue - Gelation & Calcination - Sintering
20 In-situ sintering experiments at Daresbury-6.2 T/ o C fast tunable monochromator 300 energy up to 18keV (Zr-K edge) Rapid detector family 275 pellet furnace (to 1100 o C) time each temperature step (17min) comprises: Fig. from CC Tang et al., Nucl. Instr. Meth. Phys. Res. B222 (2004) 659 ramp at 12.5K/min (2min) equilibration (3min) 18.02keV experiment (5min) 18.05keV experiment (5min) 17.98eV experiment (90s)
21 In-situ sintering experiments at Daresbury C C
22 What can we learn from a SAXS pattern? Porod slope at larger q q -n where n represents the surface morphology n=4: smooth 3<n<4: surface fractal 1<n<3: mass fractal Guinier regime Guinier radius is proportional to the particle size (radius of gyration of the particles)
23 Guinier radius: matrix softening & agglomeration Littleton softening point agglomeration & densification slow growth
24 Porod slope: matrix softening & agglomeration below edge: zirconia-air contrast below edge high-t: zirconia-glass contrast above edge: glass-air contrast above edge
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29 Small-angle x-ray scattering Anomalous SAXS Nanoscale refractory analogue - Gelation & Calcination - Sintering
30 Summary: Energy-dependent SAXS Standard SAXS - characteristic length scales - interface morphology - but: messy in complex systems Difference SAXS above/below edge - chemical contrast - but: fluorescence Anomalous SAXS - partial structure factors - but: very sensitive to chemical shifts
31 Summary: Refractory ceramics Gelation Calcination Sintering glass grain surfaces becomes smoother near the softening point pores consolidate Initial formation of a polymer network Polymerisation, then crystallisation Corrosion ZrO2 component of the refractory is less prone to corrosion by K + than by Na + ZrO2 particles agglomerate inside the pores
32 Small-angle x-ray scattering......and crystallisation processes Rudolf Winter Daniel Le Messurier Andy Lyons Kristin Høydalsvik Chris Martin 1 Graham Clark 1 Armin Hoell 2 Dragomir Tatchev 2 Sylvio Haas 2 Materials Physics Ffiseg Defnyddiau 1 STFC Daresbury Laboratory 2 Hahn-Meitner Institut Berlin
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