status of the lvp beamline at petra iii. · r. farla | extreme conditions research | 25 jan 2018 |...

R. Farla | Extreme Conditions Research | 25 Jan 2018 |

Status of the

LVP beamline

at PETRA III.

R. Farla (DESY)

Diffracted

X-rays

Diffracted

X-rays


• 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


Synthesis of transparent cubic silicon nitride

Summary Optically and intrinsically transparent

silicon nitride (c-Si3N4) 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.

Nishiyama N, Ishikawa R, Ohfuji H, et al. Scientific Reports 7:44755 (2017)

Transparent cubic silicon nitride

(c-Si3N4), synthesized under high

pressure.


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)


BC4N and BC2N compounds

- Dr. Bhat showed amorphous BC4N and BC2N 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. B6N4O3 were discovered with yet

unknown properties.


Current users of the Large Volume Press

Scientist Affiliation Supervisor

Dr. Shrikant Bhat Bayerisches

Geoinstitut/DESY

Prof.

Katsura

Nico Gaida Kiel University/DESY

(Materials Science and

Engineering)

Prof. Holzheid, Dr. Beermann,

Prof. Nishiyama (Tokyo)

Eleonora Kulik Bayerisches

Geoinstitut/DESY

Prof.

Katsura, Prof. Nishiyama

New collaborators

Scientist Affiliation Supervisor

Matthias Brensing TU Bergakademie Freiberg Prof. Biermann, Dr.

Schwarz,…

Dr. Maged Bekheet TU Berlin Prof. Gurlo

Prof. Ulrich Haussermann Stockholm University n/a


Current users of the Large Volume Press

Scientist Project

Dr. Shrikant Bhat High pressure synthesis of novel nitrides

(Sn-Ge-N and Si-Ti-N)

Nico Gaida Synthesis and characterisation of polycrystalline ceramics

(oxide-ceramics) which possess improved optical and

mechanical properties (e.g. Al2O3/SiO2/Al2SiO5)

Eleonora Kulik Solid solution in SiO2-GeO2 system and thermal expansion of

coesite (SiO2 high-pressure polymorph)

Scientist Project

Matthias Brensing Phase transitions in high-alloy austenitic TRIP/TWIP steels

under high pressure

Dr. Maged Bekheet Studies on high pressure polymorphs of In2O3

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.

New collaborators


Pressure calibrations for 6-8 compression geometry

Typical OCT/TEL ratios:

(in mm)

6-8 geometry – pressure range

25/15, 25/17 0.3 – 5, – 10 GPa

18/11, 18/10 1 – 12 GPa

14/7, 14/8 9 – 16 GPa

10/5, 10/4 14 – 22 GPa

8/3, 7/3 16 – 25 GPa

6/2 up to 35 GPa

5.7/1.5 up to 65 Gpa

(using 1° tapered anvils)

High Pressure Research, 2017



0.0

5.0

10.0

15.0

20.0

25.0

0 1 2 3 4 5 6 7 8

Sam

ple

Pre

ssu

re (

GP

a)

Load (MN)

6-6 geometry

Assembly

calibrations

15 mm

Current

- 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…



0.0

5.0

10.0

15.0

20.0

25.0

0 1 2 3 4 5 6 7 8

Sam

ple

Pre

ssu

re (

GP

a)

Load (MN)

6-6 geometry

Assembly

calibrations

15 mm

12 mm

9 mm 6 mm

4 mm

3 mm

2.5 mm 2.0 mm

To be

purchased

Purchased

Current

TEL ->

- Higher pressures!

(Large samples)

- Sample deformation

(Harder WC anvils)

Priority once LVP is

back online

TEL


Last experiment:

13 December 2017


08-01-2018


09-01-2018


10-01-2018


12-01-2018


22-01-2018


Schematic overview of the beamline (P61B)

Fig. 1 Wigglers (x10)

The last wiggler is

~133m away from the

LVP

5 m 9 m


Detector table and space for second (smaller) LVP

The 6-rams LVP ~1.7 m for a 2nd LVP Detector table


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°


Energy-dispersive X-ray diffraction (ED-XRD)

Slits for collimation and

volume definition

Gauge volume

Incoming polychromatic beam

Detector

Measurement direction

• Excellent spatial resolution!

• Excellent collimation!

(XRD of sample only)

• Fast collection! (10-100s)

• Purposeful for amorphous,

liquid and low-Z materials

• HP Ge-detector development

has stagnated…

• Low peak resolution

(> 500 FWHM)

• -> will add complementary

AD-XRD in future!

𝑛ℎ𝑐

𝐸ℎ𝑘𝑙= 2𝑑ℎ𝑘𝑙 sin θ

Constant for ED-XRD

where λ = ℎ𝑐/𝐸


𝑛λ = 2𝑑ℎ𝑘𝑙 sin θ

Constant for AD-XRD (e.g. 0.2254 Å at 55 keV)

ESRF (ID06)

423x434 mm2

100 fps FF, 0.95 ms

pixel size: 172 um

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)

Angle-dispersive XRD at ID06, ESRF

Expensive

Cheap


(hkl) reflections in 2-d X-ray diffraction patterns (AD-XRD)

2-theta (degrees)

Azim

uth

(degre

es)

HT-HP annealing

2-theta (degrees)

HT-HP deformation

eclo

gite

garn

etite

clin

opyro

xenite

eclogite

garnetite

clinopyroxenite

Anvil

shadow


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??


Total flux

10 Wigglers,

133m from last

Useful energy

range:

~30-200 keV


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 4th filter in the OH

of P61B?


Photon flux

Comparison with

other existing

high-pressure

beamlines


Power density

Beam power is

significant

(without filters)

Distance (mm)


Total power

(thru 1 x 1 mm2

aperture)

3x filtered beam

will still yield

~10 W/mm2 in EH

Front end

P61B optics hutch


Total power

(thru any

aperture)

3x filtered beam

will still yield

~10 W/mm2 in EH (~53 W in max. for

2.5x2.5 mm2 beam)

4th 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) !!


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)


N. Gaida

High-pressure glass crystallization of transparent nano-

ceramics consisting of birefringent crystals with low chromatic

aberration

E. Kulik

Fabrication of toughened hard polycrystalline

materials and elucidation of the toughening

mechanism


The Earth


New achievements with the large volume press (LVP)


Fig. 3 Experimental conditions and

photographs of recovered samples.

Gaida N et al. “Synthesis of Al2O3

/ SiO2 nano-nano composite

ceramics under high pressure

and its inverse Hall – Petch

behavior.” J. Am. Ceramic Soc.

100: 323-332 (2017)

Synthesis of Al2O3 / SiO2 nano-nano composite ceramics

Summary Synthesis of Al2O3 / SiO2 nano-ceramics at P > 12 GPa and

T > 1300 °C, with improved optical and mechanical properties.

Gaida N et al. J. Am. Ceramic Soc. 100: 323-332 (2017)

status of the lvp beamline at petra iii. · r. farla | extreme conditions research | 25 jan 2018 |...

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