Synchrotron Methods in Nanomaterials Research Marcel MiGLiERiNi Slovak University of Technology in Bratislava and Centre for Nanomaterials Research, Olomouc marcel.miglierini@stuba.sk www.nuc.elf.stuba.sk/bruno
Outline Synchrotron Synchrotron Radiation Applications of SR in Nanomaterials Diffraction of SR Nuclear Resonance with SR 2
Synchrotrons in the World America: Canada 1 USA 8 South America 1 Asia: 15 7 in Japan Europe: Germany 5 France 3 UK 3 Italy 2 Denmark, Spain, Switzerland, Sweden total 16 3
Basic Layout 1. electron gun 3. booster ring 5. beamline 2. linac 4. storage ring 6. experimental station 4
End Station Optics cabin Experiments cabin Control room 5
Outline Synchrotron Synchrotron Radiation Applications of SR in Nanomaterials Diffraction of SR Nuclear Resonance with SR 6
Energy of Synchrotron Radiation Electrons Synchrotron light Colliders X-rays Neutrons House Cell Molecule/Atom Nucleus/Quarks Electromagnetic waves radio waves IR visible light UV soft- hard-x-rays gamma rays synchrotron radiation 7
Brilliance: - combination of flux, source size, and beam divergence - number of photons per second in a certain energy bandwidth, divided by source area and by the solid angle of the radiation cone 1. Brilliance 2. Coherence 3. Pulsed Emission 4. Polarisation 5. Beam stability 6. Tunable energy Properties of Synchrotron Radiation 8
Brilliance (photon/s/0.1%bw/mm 2 /mrad 2 ) 10 14 Emission spectrum 10000 1000 100 10 1 0.1 Brilliance number of photons 1013 10 12 10 11 10 10 10 9 10 8 Sun bending magnet X-ray tubes 10 7 1 ev 10 ev 100 ev 1 kev 10 kev 100 kev energy 9
Outline Synchrotron Synchrotron Radiation Applications of SR in Nanomaterials Diffraction of SR Nuclear Resonance with SR 10
Protein Crystallography Diffraction pattern 3D structure Electron density cloud Protein crystallisation 11
Filming a protein in action with unprecedented precision. Biology Myoglobin is a molecule that stores oxygen in muscles. 12
Scientific research in Materials science Biology Environment science Physics Medicine Chemistry 13
and industrial research In collaboration with the public sector As proprietary research 14
Outline Synchrotron Synchrotron Radiation Applications of SR in Nanomaterials Diffraction of SR Nuclear Resonance with SR 15
BESSY KMC-2: In-situ Heat Treatment energy 7 kev (0.178 nm), scattering geometry linear heating 10K/min, temperature range 300 1080 K 10 s acquisition time, 2D detection 16
Surface Crystallization 60 50 air-side wheel-side wheel side air side relative area (%) 40 30 20 10 0.64 vol.%/deg 1.1 vol.%/deg 0 a.q. 300 400 500 600 annealing temperature ( o C) Fe 79 Mo 8 Cu 1 B 12 17
Transmission Experiment Linkam hot-stage 2D camera Frelon ESRF ID11: energy 88 kev, transmission geometry linear heating 10K/min, temperature range 300 875 K 15 s acquisition time, fast CCD detector beam size 0.7 x 0.3 mm2 18
In-situ XRD 19
Onset of Crystallization (Fe 0.5 Co 0.5 ) 79 Mo 8 Cu 1 B 12 20
Thermal expansion q max scales with the coefficient of volume thermal expansion α th of amorphous solid q q max max 3 ( T ) 0 ( T ) V ( T ) = V ( T0) = { 1+ α ( T T )} th 0 (Fe 1-x Co x ) 79 Mo 8 Cu 1 B 12 (Fe 1-x Co x ) 76 Mo 8 Cu 1 B 15 (3.1±0.1) 10-5 K -1 Bednarcik J., Miglierini M., Curfs C. and Franz H.: AIP Vol. 1258 (2010) 1 21
Outline Synchrotron Synchrotron Radiation Applications of SR in Nanomaterials Diffraction of SR Nuclear Resonance with SR 22
ESRF, Grenoble 23
storage ring Nuclear Resonant Scattering undulator beam t HRM IC sample NIS NFS bunch clock fast electronics nuclear forward scattering measured data nuclear inelastic scattering NFS NIS E = 0 t t t t E = 0 time time E < 0 E > 0 relative energy
Mössbauer Spectrometry with SR 57 Fe 14.4 kev energy domain time domain 25
ESRF ID22N: Nuclear Forward Scattering energy 14.41 kev (3 mev) linear heating 10K/min, temperature range 300 1000 K 60 s acquisition time 26
In-situ Temperature Experiments 600 (Fe 0.75 Co 0.25 ) 79 Mo 8 Cu 1 B 12 log intensity 100 10 50 time (ns) 100 150 200 300 600 500 400 temperature ( o C) temperature ( o C) 500 400 300 200 T x1 T C 20 40 60 80 100 120 140 160 time (ns) 27
NIS: Density of Vibrational States crystalline amorphous (intercrystalline) Stankov S., Yue Y. Z., Miglierini M. et al: Phys. Rev. Let. 100 (2008) 235503 g(e) (mev -1 ) 0.06 0.05 0.04 0.03 0.02 bulk α-fe D C B A as quenched α -Fe foil D -893K / 80 min C -783K / 30 min B -783K / 10 min A -753K / 10 min 0.01 as-quenched 0.00 10 20 30 40 50 Fe 90 Zr 7 B 3 Energy (mev) 28
Scaling of Elastic Properties with the interface fraction: does not matter does not matter sample d, nm X IF d, nm D 14.9(5) 0.11(2) 0.6(5) C 13.4(5) 0.21(2) 1.0(5) B 12.5(5) 0.32(2) 1.5(5) A 10.9(5) 0.51(2) 2.3(5) as-quenched 2.2(5) 0.84(2) 1.0(5) This is the reason Stankov S., Miglierini M., Chumakov A. I. et al. :Phys. Rev. B 82 (2010) 144301 29
To Learn More www.nuc.elf.stuba.sk/wssr2011 WINTER SCHOOL OF SYNCHROTRON RADIATION 31.1. - 4.2.2011 Liptovský Ján, Slovakia 30