VIVALDI

VIVALDI (Very Intense Vertical Axis Laue DIffractometer) surveys large volumes of reciprocal space rapidly using the Laue technique with a cylindrical image-plate detector on a white neutron beam.

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Instrument Description

guide hall n 1, thermal guide H22

 

guide

divergence

7 mrad Å

monochromators

Laue

white thermal beam, 0.8 < λ <5.2 Å

filtered, position 1

0.8 < λ < 3.0 Å

filtered, position 2

3.0 < λ < 4.5 Å

collimation

pinholes

0.5 to 10 mm in diameter

sample

beam size

up to 10 mm in diameter

flux (unfiltered)

∼1.2 108 cm-2s-1

sample space

120 mm in diameter

detector

neutron image plate

Gd2O3 doped BaFBr:Eu2+

configuration

. radius

. length

. active area

. angle subtended

vertical cylinder

159.7 mm

400 mm

800 x 400 mm2

+/-144° in 2θ, +/-52° in ν

pixel size

100 x 100, 200 x 200, or 400 x 400 µm2

readout time

~3.5 min

time-of-flight spectrum analyser

chopper & 3He detector

chopper frequency

6000 rpm

path length

2.0 m

resolution

Δλ = 0.04 Å

Background

The instrument LADI had demonstrated that good-quality macromolecular diffraction data could be rapidly obtained using Laue diffraction on a quasi-white cold-neutron beam with a large-angle cylindrical detector based on neutron image plates . The same technique has been shown in trials on a thermal-neutron beam to be very well suited to fast data collection from the smaller unit cells of interest to physicists, chemists and materials scientists. These trials inspired the design and construction of a new image-plate Laue diffractometer specially adapted to bulky sample environments as part of the ILL Millennium Programme. (Click here for the full scientific case for VIVALDI.)

VIVALDI received its first neutron beam on Friday, November 23, 2001. A few hours later a strong diffraction pattern was observed from a crystal of La1.7Co2, qualitatively similar to those observed on LADI in earlier tests on H22. The first scheduled experiments were performed just two weeks into the first cycle of 2002. Since then VIVALDI has gone from strength to strength...

VIVALDI (Very-Intense, Vertical-Axis Laue DIffractometer) provides a tool for development of new diffraction experiments, and is complementary to other ILL single-crystal diffractometers. Fields of interest for experiments on VIVALDI include magnetism, charge density waves, high-pressure studies and structural phase transitions. VIVALDI allows rapid preliminary investigation of new materials, even when only small single crystals are available. The detector is also suitable for some types of diffuse scattering experiments on a monochromatic beam.

The Instrument

The VIVALDI image-plate detector was constructed by SICN Veurey, in consultation with the EMBL Grenoble Outstation. The key differences compared to the LADI detector are that the detector cylinder axis is vertical to accept an 'Orange' cryostat, and the image plates are mounted and read on the inside of the cylinder to improve the detection efficiency. As on LADI the neutron-sensitive plates are based on the same storage-phosphor (BaFBr doped with Eu2+ ions) which is used for X-ray image plates, but with Gd2O3 added. The Gd nuclei act as neutron scintillators by creating a cascade of rays and conversion electrons.

 
VIVALDI is usually located at the end of the thermal guide H22. The full thermal spectrum can be accepted without detrimental overlap of reflections for primitive unit cells up to 25 Å on edge. A filter based on multilayer supermirrors can be placed upstream to deflect wavelengths longer than 3 Å which would otherwise contribute primarily to the background. A time-of-flight spectrum analyzer lies downstream to monitor coarse changes in the wavelength spectrum due to other instruments on the H22 guide. The entire instrument pivots on air cushions around the filter to allow selection of just wavelengths shorter than 3 Å, just wavelengths longer than 3 Å, or the unfiltered beam. Beam heights between 1100 mm and 1600 mm are acceptable to allow the detector to be used on other guides or monochromatic beams.

Sample Environment

Sample environment possibilities include a dedicated 'Orange' cryostat for 1.5 K to 315 K. This cryostat can also accept standard dilution inserts (down to 50 mK) and high-pressure cells up to 49 mm in diameter. For maximum ease and autonomy a top-loading cryo-refrigerator (1.5 K to 600 K) is under construction. The standard sample supports of LADI (small cryo-refrigerator, He-flow cryostat) and the radiative furnace of D9 (300 K to 1300 K) may also be used.

If you are considering a special sample environment for your sample, please note that the available volume within the detector is a cylinder of diameter 120 mm and length 400 mm, and that any material in the neutron beam gives rise to scattering which will contribute to the observed patterns.

Data Treatment

The user-friendly data-analysis software developed on LADI from the CCP4 Laue suite is used to reduce the data from most experiments, and is accessible on all SGI Unix workstations of the Diffraction Group. Versions for Linux and Macintosh OS X are also available. Software for incommensurate structures and quasi-crystals is under development. John Cowan's web guide to the data-analysis software is available here.