SAXS continued. 1 Methoden Moderner Röntgenphysik II - Vorlesung im Haupt-/Masterstudiengang, Universität Hamburg, SoSe 2016, S.
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1 SAXS continued 1 Methoden Moderner Röntgenphysik II - Vorlesung im Haupt-/Masterstudiengang, Universität Hamburg,
2 Illustration > USAXS at photonic crystals > USAXS in highly concentrated colloidal suspensions Beamstop 270 nm photonic_table.html Courtesy: V. Boyko (BASF) 2 Methoden Moderner Röntgenphysik II - Vorlesung im Haupt-/Masterstudiengang, Universität Hamburg,
3 Outline > SAXS Introduction > Instrumentation PETRA III > Bulk materials Transmission U/SAXS: Porous materials Ni-base superalloys Droplet drying Chocolate 3 Methoden Moderner Röntgenphysik II - Vorlesung im Haupt-/Masterstudiengang, Universität Hamburg,
4 SAXS collimation and scattering geometry Detector Collimating Slit 2 Collimating Slit 1 bs q min L SD Sample L SD determines resolution q min =bs / (2 L SD ) Use Bragg s law: d max = l q mi 4 Methoden Moderner Röntgenphysik II - Vorlesung im Haupt-/Masterstudiengang, Universität Hamburg, n
5 Layout Different focussing schemes > Flexible choice of beam size and divergence > Fixed focal spot position and size E=13keV 22x12µm 2 E=15keV 24x17µm 2 > Full user operation within design values! CRL System 1 CRL System 2 ~5x10 11 Ph/sec 76.7m Det > Nanofocus end station: <1.5x1.5µm 2 500x500nm 2 To be finished 5 Methoden Moderner Röntgenphysik II - Vorlesung im Haupt-/Masterstudiengang, Universität Hamburg,
6 Rapid change (GI)SAXS / (GI) WAXS > Adjust scattering angles dω q-ranges > 5cm<D SD <8.6m > Highly flexible > Separate WAXS device 6 Methoden Moderner Röntgenphysik II - Vorlesung im Haupt-/Masterstudiengang, Universität Hamburg,
7 USAXS focus > Beam size: 32x23µm 2 > SDD=8470mm > N 2 =12 > PS particles: 400nm Dried on glass slide t acq =1s background corrected 7 Methoden Moderner Röntgenphysik II - Vorlesung im Haupt-/Masterstudiengang, Universität Hamburg,
8 Outline > SAXS Introduction > Instrumentation PETRA III > Bulk materials Transmission U/SAXS: Porous materials Ni-base superalloys Droplet drying Chocolate 8 Methoden Moderner Röntgenphysik II - Vorlesung im Haupt-/Masterstudiengang, Universität Hamburg,
9 Aerogels > Highly porous materials: OLED: matching of refractive indices molecular sieves sensors > Challenges Generation of pores with dimensions greater than 100 nm, yet submicron Characterization of size 9 Methoden Moderner Röntgenphysik II - Vorlesung im Haupt-/Masterstudiengang, Universität Hamburg,
10 Quantitative analysis > Bimodal distribution particles > I Q = Δρ 2 2 N V P 0 > Porod law: R P R D R dr Particle size ~ 30nm Pore size estimate >1300nm Eggers, SVR et al., Langmuir 24, 5887 (2008) 10 Methoden Moderner Röntgenphysik II - Vorlesung im Haupt-/Masterstudiengang, Universität Hamburg,
11 Outline > SAXS Introduction > Instrumentation PETRA III > Bulk materials Transmission U/SAXS: Porous materials Ni-base superalloys Droplet drying Chocolate 11 Methoden Moderner Röntgenphysik II - Vorlesung im Haupt-/Masterstudiengang, Universität Hamburg,
12 Ni-base superalloys > Ni-base W-rich experimental single crystal superalloy (Ni-4.6Al-6.4Ta-5.7Cr-10.8W-2.1Mo) > Ni-Al solid solution Matrix (g), fcc > Precipitates (g Al, ), Ni 3 (Al,Ti) > TEM: g -precipitates R > 50 nm > D > 100 nm g g 12 Methoden Moderner Röntgenphysik II - Vorlesung im Haupt-/Masterstudiengang, Universität Hamburg,
13 ID nm -1 Fit noc_4: P. Strunz et al., J. Appl. Cryst. 36, 854 (2003) Beam: 100 m Courtesy: Gilles Strunz 13 Methoden Moderner Röntgenphysik II - Vorlesung im Haupt-/Masterstudiengang, Universität Hamburg,
![Dz = 5 m Local precipate morphology - SAXS [320] [100] R. Gilles et al. > s phase precipitate: Scripta Mat.](/docs-images/80/80988587/images/14-0.jpg "39, 715 (1998) embrittlement of alloy crack formation and propagation - streaking: correct orientation - s phase: stack - distance 5-15 m diameter 2R < 10 m thickness t > O(100 nm) Dy = 5 m k 0 [001]")
14 Dz = 5 m Local precipate morphology - SAXS [320] [100] R. Gilles et al. > s phase precipitate: Scripta Mat. 39, 715 (1998) embrittlement of alloy crack formation and propagation - streaking: correct orientation - s phase: stack - distance 5-15 m diameter 2R < 10 m thickness t > O(100 nm) Dy = 5 m k 0 [001] Q=1.5 nm Methoden Moderner Röntgenphysik II - Vorlesung im Haupt-/Masterstudiengang, Universität Hamburg,
15 Microfocus: local g - particle size distribution Roth et al., Nucl. Instr. Meth. B 200, 255 (2003) Porod-law Q -4 SAXS: TEM: USAXS: R > 55 nm R 50 nm R = 52 nm Q [nm -1 ] Lower minimum of particle size distribution 15 Methoden Moderner Röntgenphysik II - Vorlesung im Haupt-/Masterstudiengang, Universität Hamburg,
16 Outline > SAXS Introduction > Instrumentation PETRA III > Bulk materials Transmission U/SAXS: Porous materials Ni-base superalloys Droplet drying Chocolate 16 Methoden Moderner Röntgenphysik II - Vorlesung im Haupt-/Masterstudiengang, Universität Hamburg,
17 The drying droplet > Self-organisation: attractive capillary forces > correlated nano-structures > industrial processes spray drying (see also GISAXS part) food processing, pharmaceuticals Paintings/coatings 17 Methoden Moderner Röntgenphysik II - Vorlesung im Haupt-/Masterstudiengang, Universität Hamburg,
18 Wir machen ein Experiment > Der trocknende Tropfen > Wandfarbe! > Haftung! > pps Glassubtrate 18 Methoden Moderner Röntgenphysik II - Vorlesung im Haupt-/Masterstudiengang, Universität Hamburg,
19 Porod invariant practical application > Colloidal solution: drying thick droplet > Evaporation of water: Irradiated volume becomes smaller: shrinking Distance of colloidal partices decreases, F 1 Dr increases (air!), as water removed from interstitial sites Chen et al., Soft Matter 8, (2012) 19 Methoden Moderner Röntgenphysik II - Vorlesung im Haupt-/Masterstudiengang, Universität Hamburg,
20 The drying droplet > Microbeam: local concentration > Q~ f (1 f)( R x ) > Dried droplet: different gradient in f > Homogenous distribution > Agglomeration in shell > Continuous gradient Sen, SVR et al., Soft Matter 10, 1621 (2014) 20 Methoden Moderner Röntgenphysik II - Vorlesung im Haupt-/Masterstudiengang, Universität Hamburg,
21 Porod invariant (arb. unit) The drying droplet part 2 > Slow / fast drying > Concentration of colloids: Arresting of colloids Homogenous Core shell effect ( coffee ring ) > Follow concentration profile in-situ 100 Experimental Model b X (mm) 21 Methoden Moderner Röntgenphysik II - Vorlesung im Haupt-/Masterstudiengang, Universität Hamburg,
22 Outline > SAXS Introduction > Instrumentation PETRA III > Bulk materials Transmission U/SAXS: Porous materials Ni-base superalloys Droplet drying Chocolate 22 Methoden Moderner Röntgenphysik II - Vorlesung im Haupt-/Masterstudiengang, Universität Hamburg,
23 Chocolate > A real multicomponent system > Nestlé, TU HH, DESY > Fat Blooming - pathways Reinke, SVR et al., ACS Appl. Mater. Interfaces, DOI: /acsami.5b02092 (2015) 23 Methoden Moderner Röntgenphysik II - Vorlesung im Haupt-/Masterstudiengang, Universität Hamburg,
24 Chocolate Continuous fat phase: Reinke, SVR et al., ACS Appl. Mater. Interfaces, DOI: /acsami.5b02092 (2015) 24 Methoden Moderner Röntgenphysik II - Vorlesung im Haupt-/Masterstudiengang, Universität Hamburg,
25 Chocolate > A real multicomponent systems Reinke, SVR et al., ACS Appl. Mater. Interfaces, DOI: /acsami.5b02092 (2015) 25 Methoden Moderner Röntgenphysik II - Vorlesung im Haupt-/Masterstudiengang, Universität Hamburg,
26 Chocolate > A real multicomponent system > Superposition of SAXS contributions > Different density difference > Migration: filling of voids by oil: Q decreases Reinke, SVR et al., ACS Appl. Mater. Interfaces, DOI: /acsami.5b02092 (2015) 26 Methoden Moderner Röntgenphysik II - Vorlesung im Haupt-/Masterstudiengang, Universität Hamburg,
27 Chocolate > Peak intensities > Pores, cracks: capillary effect > Then: chemical migration through the fat phase by softening and partial dissolution of the crystalline cocoa butter. > reduction of porosity and a minimization of defects > a reduced content of noncrystallized liquid cocoa butter > b or c Reinke, SVR et al., ACS Appl. Mater. Interfaces, DOI: /acsami.5b02092 (2015) 27 Methoden Moderner Röntgenphysik II - Vorlesung im Haupt-/Masterstudiengang, Universität Hamburg,
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