Status of the LVP beamline at PETRA III. R. Farla (DESY)

Transcription

1 Status of the LVP beamline at PETRA III. R. Farla (DESY) Diffracted X-rays Diffracted X-rays R. Farla Extreme Conditions Research 25 Jan 2018 Page 1

2 Introduction Recent highlights Overview of P61B activity (mid-2017 until now) Development work Further development on the LVP Beamline construction photo gallery Beamline layout Techniques XRD scmos cameras for X-ray imaging Flux and power calculations Summary and outlook R. Farla Extreme Conditions Research 25 Jan 2018 Page 2

3 Synthesis of transparent cubic silicon nitride Nishiyama N, Ishikawa R, Ohfuji H, et al. Scientific Reports 7:44755 (2017) Summary Optically and intrinsically transparent silicon nitride (c-si 3 N 4 ) synthesised at P = 15.6 GPa, T > 1500 C Nano-crystalline silicon nitride (150 nm) Incredible hardness (third hardest material) High-temperature resistance in air (up to 1400 C) Attractive choice for creating optical windows with supreme durability. Transparent cubic silicon nitride (c-si3n4), synthesized under high pressure. R. Farla Extreme Conditions Research 25 Jan 2018 Page 3

4 Crystalline ternary B-C-N, a superhard phase? Predicted by theory Good chemical stability and oxidation resistance High-T stability Commercially hugely attractive ($20 billion market) Yeung et al. Annual Review of Materials Research (2016) R. Farla Extreme Conditions Research 25 Jan 2018 Page 4

5 BC 4 N and BC 2 N compounds - Dr. Bhat showed amorphous BC 4 N and BC 2 N compounds tend to decompose into c-bn and diamond under extreme conditions. Thus, B-C-N materials remain elusive. - New boron oxynitrides (BON) compounds, e.g. B 6 N 4 O 3 were discovered with yet unknown properties. R. Farla Extreme Conditions Research 25 Jan 2018 Page 5

6 Current users of the Large Volume Press Scientist Affiliation Supervisor Dr. Shrikant Bhat Nico Gaida Eleonora Kulik New collaborators Bayerisches Geoinstitut/DESY Kiel University/DESY (Materials Science and Engineering) Bayerisches Geoinstitut/DESY Prof. Katsura Scientist Affiliation Supervisor Prof. Holzheid, Dr. Beermann, Prof. Nishiyama (Tokyo) Prof. Katsura, Prof. Nishiyama Matthias Brensing TU Bergakademie Freiberg Prof. Biermann, Dr. Schwarz, Dr. Maged Bekheet TU Berlin Prof. Gurlo Prof. Ulrich Haussermann Stockholm University n/a R. Farla Extreme Conditions Research 25 Jan 2018 Page 6

7 Current users of the Large Volume Press Scientist Dr. Shrikant Bhat Nico Gaida Eleonora Kulik Project High pressure synthesis of novel nitrides (Sn-Ge-N and Si-Ti-N) Synthesis and characterisation of polycrystalline ceramics (oxide-ceramics) which possess improved optical and mechanical properties (e.g. Al 2 O 3 /SiO 2 /Al 2 SiO 5 ) Solid solution in SiO 2 -GeO 2 system and thermal expansion of coesite (SiO 2 high-pressure polymorph) New collaborators Scientist Matthias Brensing Project Phase transitions in high-alloy austenitic TRIP/TWIP steels under high pressure Dr. Maged Bekheet Studies on high pressure polymorphs of In 2 O 3 Prof. Ulrich Haussermann New ternary and quaternary metal hydride materials (potential superconductors). Investigation of the HPHT phase diagram of complex hydrides by in-situ diffraction at up to 15 GPa. R. Farla Extreme Conditions Research 25 Jan 2018 Page 7

8 Pressure calibrations for 6-8 compression geometry Typical OCT/TEL ratios: (in mm) 6-8 geometry pressure range 25/15, 25/ , 10 GPa 18/11, 18/ GPa 14/7, 14/ GPa 10/5, 10/ GPa 8/3, 7/ GPa 6/2 up to 35 GPa 5.7/1.5 up to 65 Gpa (using 1 tapered anvils) High Pressure Research, 2017 R. Farla Extreme Conditions Research 25 Jan 2018 Page 8

9 Sample Pressure (GPa) Pressure calibrations for 6-6 compression geometry geometry Assembly calibrations mm Current Load (MN) - Large volume 6-6 assembly designed by Dr. Nishiyama in 2015 at DESY - Even larger cells were considered (for up to 4 GPa), but not built so far R. Farla Extreme Conditions Research 25 Jan 2018 Page 9

10 Sample Pressure (GPa) Pressure calibrations for 6-6 compression geometry mm 2.5 mm 3 mm 4 mm TEL To be purchased 6-6 geometry Assembly calibrations Purchased TEL -> mm 9 mm 12 mm 15 mm Current Load (MN) - Higher pressures! (Large samples) - Sample deformation (Harder WC anvils) Priority once LVP is back online R. Farla Extreme Conditions Research 25 Jan 2018 Page 10

11 Last experiment: 13 December 2017 R. Farla Extreme Conditions Research 25 Jan 2018 Page 11

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18 Schematic overview of the beamline (P61B) 5 m 9 m Fig. 1 Wigglers (x10) The last wiggler is ~133m away from the LVP R. Farla Extreme Conditions Research 25 Jan 2018 Page 18

19 Detector table and space for second (smaller) LVP The 6-rams LVP ~1.7 m for a 2 nd LVP Detector table R. Farla Extreme Conditions Research 25 Jan 2018 Page 19

20 Two HPGe-detectors and their configurations Both at θ = ± 6.5 in horizontal plane or two different angles At θ = 6.5 in horizontal and vertical planes for stress measurement Minimum range for horizontal detectors = -5 to 5 Maximum range for horizontal detectors = -10 to +10 Full range for 1 vertical detector = 0 to 27 Minimum range for 1 horizontal and 1 vertical detector = 5 and 5 R. Farla Extreme Conditions Research 25 Jan 2018 Page 20

21 Energy-dispersive X-ray diffraction (ED-XRD) Measurement direction Detector n hc E hkl = 2d hkl sin θ Constant for ED-XRD where λ = hc/e Excellent spatial resolution! Excellent collimation! (XRD of sample only) Fast collection! (10-100s) Purposeful for amorphous, liquid and low-z materials Gauge volume Incoming polychromatic beam Slits for collimation and volume definition HP Ge-detector development has stagnated Low peak resolution (> 500 FWHM) -> will add complementary AD-XRD in future! R. Farla Extreme Conditions Research 25 Jan 2018 Page 21

22 Angle-dispersive XRD at ID06, ESRF nλ = 2d hkl sin θ Constant for AD-XRD (e.g Å at 55 kev) Linear array detector on rotating arm: - 50 seconds for full 360 rotation 2m, 2θ range 8 - pixel size: > 200 µm - ~0.7 m radial coverage (movable to greater radius) Expensive ESRF (ID06) Cheap 423x434 mm fps FF, 0.95 ms pixel size: 172 um R. Farla Extreme Conditions Research 25 Jan 2018 Page 22

23 Azimuth (degrees) (hkl) reflections in 2-d X-ray diffraction patterns (AD-XRD) HT-HP annealing Anvil shadow eclogite eclogite garnetite clinopyroxenite HT-HP deformation garnetite clinopyroxenite 2-theta (degrees) 2-theta (degrees) R. Farla Extreme Conditions Research 25 Jan 2018 Page 23

24 scmos cameras for X-ray radiography 4.2 MP vs 5.5 MP Cameras PCO Edge Andor Zyla Hamamatsu Orca Flash V3 QE! Rolling vs Global shutter?? R. Farla Extreme Conditions Research 25 Jan 2018 Page 24

25 Total flux 10 Wigglers, 133m from last Useful energy range: ~ kev R. Farla Extreme Conditions Research 25 Jan 2018 Page 25

26 Filtered flux Purpose of filters is to manage heat load of white beam The front end will have 3 sets of filters: CVD-Dia & Cu A 4 th filter in the OH of P61B? R. Farla Extreme Conditions Research 25 Jan 2018 Page 26

27 Photon flux Comparison with other existing high-pressure beamlines R. Farla Extreme Conditions Research 25 Jan 2018 Page 27

28 Power density Beam power is significant (without filters) Distance (mm) R. Farla Extreme Conditions Research 25 Jan 2018 Page 28

29 Total power (thru 1 x 1 mm 2 aperture) 3x filtered beam will still yield ~10 W/mm 2 in EH Front end P61B optics hutch R. Farla Extreme Conditions Research 25 Jan 2018 Page 29

30 Total power (thru any aperture) 3x filtered beam will still yield ~10 W/mm 2 in EH (~53 W in max. for 2.5x2.5 mm 2 beam) 4 th filter needed If 4 mm Cu, then power < 7 W, safe for indirect imaging on scmos camera Beam stopper must be water-cooled to dissipate up to 100 W in full beam (& no filters)!! R. Farla Extreme Conditions Research 25 Jan 2018 Page 30

31 Immediate decisions Design of detector table to be finalised Purchase of HP Ge-detectors (2x) Purchase of scmos camera, mirror and scintillator (YAG:Ce) (to convert from X-rays to visible light) Hutch infrastructure (ethernet, cooling water, gas, power, etc.) Front end completion in summer shutdown 2018 Installation of all components until late 2018 Safety inspections First beam at end of 2018? We will see! (LVP should be operational again this March) R. Farla Extreme Conditions Research 25 Jan 2018 Page 31

32 N. Gaida High-pressure glass crystallization of transparent nanoceramics consisting of birefringent crystals with low chromatic aberration E. Kulik Fabrication of toughened hard polycrystalline materials and elucidation of the toughening mechanism R. Farla Extreme Conditions Research 25 Jan 2018 Page 32

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34 The Earth R. Farla Extreme Conditions Research 25 Jan 2018 Page 34

35 New achievements with the large volume press (LVP) R. Farla Extreme Conditions Research 25 Jan 2018 Page 35

36 New achievements with the large volume press (LVP) R. Farla Extreme Conditions Research 25 Jan 2018 Page 36

37 Synthesis of Al 2 O 3 / SiO 2 nano-nano composite ceramics Gaida N et al. J. Am. Ceramic Soc. 100: (2017) Summary Synthesis of Al 2 O 3 / SiO 2 nano-ceramics at P > 12 GPa and T > 1300 C, with improved optical and mechanical properties. R. Farla Extreme Conditions Research 25 Jan 2018 Page 37