Page 7 - Periodic Issue 02

each configuration has required careful planning, but has
certainly been worth it now each system is optimised.

To provide power to the furnace and to allow it to be
controlled safely, a controller box was custom-designed
for use with the furnace at Diamond. This was done with
the help of Nenad Vrangeš and Paul Smith in our very own
Inorganic Chemistry Laboratory Electronics and Design
Facility. The controller, including all circuits and display
panels, was built entirely from scratch. It incorporates an
intelligent temperature controller unit, in addition to a series
of vital “interlocks”. These interlocks are designed to ensure
the safe working of ODISC so that if, for example, the
water or air cooling systems fail the power to the furnace is
disconnected.

The design and construction of ODISC has involved a huge
shape, the distance between the layers in the structure team effort. An important aspect of this project, and one of
changes significantly. This distortion of the structure can my favourites, has been the regular discussion of design
be easily monitored using in situ X-ray diffraction, which ideas with experts from a range of different disciplines:
in turn allows us to probe very precisely the behaviour of from academics to electronics engineers, and beamline
these compounds during a reaction. In 2011, I successfully scientists to workshop technicians. It is entirely down to the
probed the exchange of anions within a novel layered input of a large group of individuals that such an efficient
double hydroxide material as part of the first ever in situ and useful piece of equipment has been created.
processing experiments to be undertaken on Beamline I12.
A SUCCESS STORY
HOTTING UP Since the finishing touches were applied to ODISC,
A very important and challenging aspect of my DPhil was a number of significant accomplishments have been
to construct a piece of equipment that allows chemical achieved. In March 2012, the equipment underwent
reactions to be studied using the X-ray diffraction complete safety testing and commissioning onto Beamline
facilities at the Diamond Light Source. The simple aim I12 at Diamond. At the same time, we collected our
was to build a cell that heats and stirs reacting samples first X-ray diffraction measurements using the cell – the
whilst simultaneously passing an X-ray beam through syntheses of some novel oxide phases were probed with
the reaction. In 2012, I, along with several individuals at great success, at temperatures up to 1000 °C. In June, we
Oxford and Diamond, succeeded in constructing the transported our equipment and chemicals to Hamburg to
Oxford-Diamond In Situ Cell (or “ODISC”). This equipment carry out further experiments on layered double hydroxides
comprises a high-temperature chemical reaction furnace, at the DESY synchrotron. And in August 2012, a paper
as well as an intricate furnace controller box. detailing the design and optimisation of the cell was
published in Review of Scientific Instruments journal.
The furnace is distinctive in that it heats samples using
highly-focussed infrared radiation. Gold-coated ellipsoids One overwhelming triumph, which initially came as a
direct the IR-radiation from four halogen lamps in the sides surprise to me, has been the extremely positive response
of the furnace onto a cylindrical sample vessel in the centre we received from the wider scientific community. To date,
of the furnace chamber. This technique allows samples to researchers from seven different institutions including
be heated and cooled very rapidly, to temperatures as high the University of Warwick, University of Liverpool, and
as 1200 °C. Not all materials absorb infrared radiation and University College London have used ODISC to investigate
so sample tubes made of matt black materials, such as their own chemical reactions. It is my hope that, through
glassy carbon and silicon carbide, are used to transfer heat the continued efforts of scientists at Oxford and Diamond,
to the reagents. ODISC will be helping to make important scientific
discoveries for years to come.
An important consideration when designing the furnace
was to maximise its versatility. To allow it to be used in as
many different areas of chemistry as possible, a series
of “sample configurations” were constructed with the Key references:
help of Charles Evans in the Physical and Theoretical 1. S. J. Moorhouse, N. Vranjes, A. Jupe, M.
Chemistry Laboratory Workshop. Each separate Drakopoulos and D. O’Hare, Review of Scientific
configuration accommodates a different sample vessel Instruments 83 (8), 084101-084108 (2012).
– from tubes used in high/low temperature studies, to 2. G. R. Williams, S. J. Moorhouse, T. J. Prior, A. M.
thin glass capillaries and bulky sealed steel containers. Fogg, N. H. Rees and D. O’Hare, Dalton T. 40 (22),
Perfecting the uniform heating and correct positioning of
6012 (2011).

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Periodic
The Magazine of the Department of Chemistry