Synchrotron Methods in Nanomaterials Research

Transcription

1 Synchrotron Methods in Nanomaterials Research Marcel MiGLiERiNi Slovak University of Technology in Bratislava and Centre for Nanomaterials Research, Olomouc

2 Outline Synchrotron Synchrotron Radiation Applications of SR in Nanomaterials Diffraction of SR Nuclear Resonance with SR 2

3 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

4 Basic Layout 1. electron gun 3. booster ring 5. beamline 2. linac 4. storage ring 6. experimental station 4

5 End Station Optics cabin Experiments cabin Control room 5

6 Outline Synchrotron Synchrotron Radiation Applications of SR in Nanomaterials Diffraction of SR Nuclear Resonance with SR 6

7 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

8 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

9 Brilliance (photon/s/0.1%bw/mm 2 /mrad 2 ) Emission spectrum Brilliance number of photons Sun bending magnet X-ray tubes ev 10 ev 100 ev 1 kev 10 kev 100 kev energy 9

10 Outline Synchrotron Synchrotron Radiation Applications of SR in Nanomaterials Diffraction of SR Nuclear Resonance with SR 10

11 Protein Crystallography Diffraction pattern 3D structure Electron density cloud Protein crystallisation 11

12 Filming a protein in action with unprecedented precision. Biology Myoglobin is a molecule that stores oxygen in muscles. 12

13 Scientific research in Materials science Biology Environment science Physics Medicine Chemistry 13

14 and industrial research In collaboration with the public sector As proprietary research 14

15 Outline Synchrotron Synchrotron Radiation Applications of SR in Nanomaterials Diffraction of SR Nuclear Resonance with SR 15

16 BESSY KMC-2: In-situ Heat Treatment energy 7 kev (0.178 nm), scattering geometry linear heating 10K/min, temperature range K 10 s acquisition time, 2D detection 16

17 Surface Crystallization air-side wheel-side wheel side air side relative area (%) vol.%/deg 1.1 vol.%/deg 0 a.q annealing temperature ( o C) Fe 79 Mo 8 Cu 1 B 12 17

18 Transmission Experiment Linkam hot-stage 2D camera Frelon ESRF ID11: energy 88 kev, transmission geometry linear heating 10K/min, temperature range K 15 s acquisition time, fast CCD detector beam size 0.7 x 0.3 mm2 18

19 In-situ XRD 19

20 Onset of Crystallization (Fe 0.5 Co 0.5 ) 79 Mo 8 Cu 1 B 12 20

21 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 (2010) 1 21

22 Outline Synchrotron Synchrotron Radiation Applications of SR in Nanomaterials Diffraction of SR Nuclear Resonance with SR 22

23 ESRF, Grenoble 23

24 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

25 Mössbauer Spectrometry with SR 57 Fe 14.4 kev energy domain time domain 25

26 ESRF ID22N: Nuclear Forward Scattering energy kev (3 mev) linear heating 10K/min, temperature range K 60 s acquisition time 26

27 In-situ Temperature Experiments 600 (Fe 0.75 Co 0.25 ) 79 Mo 8 Cu 1 B 12 log intensity time (ns) temperature ( o C) temperature ( o C) T x1 T C time (ns) 27

28 NIS: Density of Vibrational States crystalline amorphous (intercrystalline) Stankov S., Yue Y. Z., Miglierini M. et al: Phys. Rev. Let. 100 (2008) g(e) (mev -1 ) 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 Fe 90 Zr 7 B 3 Energy (mev) 28

29 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)

30 To Learn More WINTER SCHOOL OF SYNCHROTRON RADIATION Liptovský Ján, Slovakia 30