The Swiss-Norwegian Beamline – BM01A
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The Swiss-Norwegian Beamline – BM01A The Swiss-Norwegian Beamline – BM01A D Chernyshov § , V Dmitriev § , Y Filinchuk § and P Pattison §* § Swiss-Norwegian Beamline, ESRF, Grenoble, FRANCE * Laboratory of Crystallography, EPFL, CH- 1015, Lausanne The Swiss-Norwegian beamlines at the European Synchrotron Radiation Facility have now been in user operation for over a decade. Over the last few years, the scientific activities on the beamline have become more and more focused on solving problems in materials science and crystal chemistry. We present here an overview of the operational characteristics of the beamline and the equipment available on BM01A. Although originally conceived as a station for single crystal diffraction and macromolecular crystallography, the combination of point detector, CCD area detectors and image plate provides a very versatile tool for many types of X-ray diffraction and scattering experiments. Some examples are given of recent results which demonstrate the capabilities of the beamline. KUMA6 DIFFRACTOMETER KUMA6 DIFFRACTOMETER •fast read-out CCD for both single crystal and powder diffraction •flexible geometry + combined use of area and point detectors Diffraction experiment with laser-exited crystal at 13.5 K MAR345 Image Plate MAR345 Image Plate • low background - diffuse scattering experiments • fixed geometry (- rotation) – easy to install auxiliary equipment • MARCCD detector is available for fast data collection Examples of In-Situ Experiments Heatable high-pressure cell (left) Gas flow system (right) Future Future Combined diffraction and Raman scattering experiments, for both single crystals and powders. CryoStream 700+ ( 90-500 K), HeliJet ~13.5 – 70 K, He Cryostat ~4.5 – 300K, Heat Blowers ~ 300- 1000 K, DAC Pressure cells, gas flow systems… Single Crystals Powders 2 5 5 0 7 5 1 00 m a g ne tic d ata a) HS /% diffra ctio n d ata 0 50 100 150 200 250 300 2.00 2.05 2.10 2.15 2.20 T/K b) <Fe 1 -N> <Fe 2 -N> <Fe av -N> d /Å Structure Solution Evolution of Structure Mapping of Reciprocal Space Fast temperature scanning of weak superstructure reflections In-situ studies Refinement of Structure Phase Transitions More information at www.snbl.org RESEARCH RESEARCH INSTRUMENTS INSTRUMENTS Since it began operation in 1995, the scientific productivity of the Swiss-Norwegian beamlines has increased dramatically. The number of publications appearing from both beamlines together has now reached a level of about 70 per year. Improvements in area detector performance using both image plate and CCD technology has now reached a level where a high quality structure solution can be obtained in less than one hour. The use of area detectors for the collection of time-resolved, in-situ powder studies looks very promising, and we expect to see intensive use of these techniques in materials research at SNBL. 0 20 40 60 80 100 120 140 160 180 0,0 0,1 0,2 0,3 0,4 0,5 0,6 0,7 0,8 0,9 1,0 C o nte nto fthe crysta llin e p ha se T im e,m inutes K olm ogorov-A vram ifit A (1 -e xp (-k(t-t o ) n )) t 0 = -1 m in. n = 1.717(5) R 2 = 0.998
description
Future Combined diffraction and Raman scattering experiments, for both single crystals and powders. KUMA6 DIFFRACTOMETER fast read-out CCD for both single crystal and powder diffraction flexible geometry + combined use of area and point detectors - PowerPoint PPT Presentation
Transcript of The Swiss-Norwegian Beamline – BM01A
The Swiss-Norwegian Beamline – BM01AThe Swiss-Norwegian Beamline – BM01AD Chernyshov§, V Dmitriev§, Y Filinchuk§ and P Pattison§*
§Swiss-Norwegian Beamline, ESRF, Grenoble, FRANCE
*Laboratory of Crystallography, EPFL, CH-1015, Lausanne
The Swiss-Norwegian beamlines at the European Synchrotron Radiation Facility have now been in user operation for over a decade. Over the last few years, the scientific activities on the beamline have become more and more focused on solving problems in materials science and crystal chemistry. We present here an overview of the operational characteristics of the beamline and the equipment available on BM01A. Although originally conceived as a station for single crystal diffraction and macromolecular crystallography, the combination of point detector, CCD area detectors and image plate provides a very versatile tool for many types of X-ray diffraction and scattering experiments. Some examples are given of recent results which demonstrate the capabilities of the beamline.
KUMA6 DIFFRACTOMETERKUMA6 DIFFRACTOMETER•fast read-out CCD for both single crystal and powder diffraction
•flexible geometry + combined use of area and point detectors
Diffraction experiment with laser-exited crystal at 13.5 K
MAR345 Image PlateMAR345 Image Plate• low background - diffuse scattering experiments
• fixed geometry (- rotation) – easy to install auxiliary equipment
• MARCCD detector is available for fast data collection
Examples of In-Situ Experiments
Heatable high-pressure cell (left)
Gas flow system (right)
FutureFuture
Combined diffraction and Raman scattering experiments, for both single crystals and powders.
CryoStream 700+ ( 90-500 K), HeliJet ~13.5 – 70 K, He Cryostat ~4.5 – 300K, Heat Blowers ~ 300- 1000 K, DAC Pressure cells, gas flow systems…
Single Crystals Powders
2 5
5 0
7 5
1 0 0
m agnetic data
a)
HS /%
diffraction data
0 50 100 150 200 250 3002.00
2.05
2.10
2.15
2.20
T /K
b) <Fe1-N > <Fe2-N > <Feav-N >
d /Å
Structure Solution
Evolution of Structure Mapping of Reciprocal Space
Fast temperature scanning of weak superstructure reflections
In-situ studies
Refinement of Structure
Phase Transitions
More information at www.snbl.org
RESEARCHRESEARCH
INSTRUMENTSINSTRUMENTS
Since it began operation in 1995, the scientific productivity of the Swiss-Norwegian beamlines has increased dramatically. The number of publications appearing from both beamlines together has now reached a level of about 70 per year. Improvements in area detector performance using both image plate and CCD technology has now reached a level where a high quality structure solution can be obtained in less than one hour. The use of area detectors for the collection of time-resolved, in-situ powder studies looks very promising, and we expect to see intensive use of these techniques in materials research at SNBL.
0 20 40 60 80 100 120 140 160 1800,0
0,1
0,2
0,3
0,4
0,5
0,6
0,7
0,8
0,9
1,0
Co
nte
nt o
f th
e c
ryst
alli
ne
ph
ase
Time, minutes
Kolmogorov-Avrami fit
A(1-exp(-k(t-to)n))
t0 = -1 min.
n = 1.717(5)
R2 = 0.998
