STATION 11.1
Infrared Microspectroscopy
Description
This station is dedicated to mid infrared microspectroscopy. The advantages of using synchrotron radiation for high spatial resolution spectroscopy have led to developments of similar facilities at many synchrotrons worldwide. The Daresbury beamline can undertake measurements in transmission or reflection mode, and is also equipped with a mapping stage for collecting 2D "maps". In addition a Side Port Accessory is available for the study of large objects.
News
Ancient Helmet Studied Using Synchrotron IR
Beamline
11 has recently been used to perform microanalysis of corrosion products
on the surface of a 6th Century B.C. Corinthian helmet. The helmet showed
evidence of ancient damage and more recent attempts at repair. The use of
a side port reflection accessory allowed infrared reflection measurements
to be made, adding to the data obtained by Surface XRD and Neutron Scattering.
« click image for larger picture
Daresbury IR Group Awarded Detector Development
Funding
The
IR group at Daresbury Laboratory, in conjunction with the Instrumentation
Department Detector Group, have been awarded £247k
to
develop the latest generation of high speed IR array detectors specifically
for use on the synchrotron beamline at Daresbury. It is expected that
the resulting instrumentation will be of great use at other synchrotrons,
including Diamond.
Functional Description
The performance of beamline 11.1 is achieved by focusing the bright
synchrotron beam to an 8 x 8 micron point. A small area, high detectivity
MCT detector allows spectra to be collected the region of 750 cm-1 to 4000
cm-1.
The station is suitable for the study of a wide range of materials
including:
- biological tissue
- mineral surfaces
- single crystals
- paint fragments
- archaeological remains
- polymer multilayers
Samples can be mounted in several differnt ways, including:
- Thin-sectioned and mounted on IR transmitting or reflecting materials.
- Polished for surface reflectance measurements.
- Compressed in a diamond cell for improved transmission
- Large objects are studied in reflectance mode using a side port reflectance accessory
Technical Description
Beamline 11.1 accepts 30 x 30 milliradians of bending magnet radiation from the SRS. A cooled focusing mirror refocuses the beam 1:1, and the beam is reflected upwards through the synchrotron shield roof. The beam passes through a KRS5 vacuum exit window and into the secondary optics system. This system employs a choice of three different focal length mirrors to provide a highly collimated IR beam matched to the beamline experiment. The collimated beam is directed into a Nicolet Nexus FTIR spectrometer coupled to a Nicolet Continuum IR microscope fitted with 32x objective, mapping stage, and 50 micron high D* detector.
Development
The recently installed 50 micron detector from Thermo Nicolet has significantly improved performance of the beamline. The detector element is now more closely matched to the dimensions of the focused SR beam.
A high quality video microscope is now available for users to collect visible light micrographs of their samples.
Registered users will now have access to multivariate data analysis software. Two packages, Pirouette (Infometrics Inc) and Cytospec (specifically for IR imaging) are now available on site in the IR data analysis room.
Proposed Development
A second IR microscope will soon be brought to Daresbury for testing with SR light. The Perkin Elmer "Spotlight" uses a 16 element linear array detector with high-speed direct readout to achieve fast data collection of large area maps. This system will initially be tested on beamline 13.3
A high pressure diamond anvil cell will be commissioned on the beamline within the next year. This will allow users to study minerals at geological pressures, and to understand the behaviour of biological molecules under pressure.
Benchmarks
The performance of 11.1 is routinely assessed prior to user beamtime. Typical performance, based on noise present in a 100% transmission spectrum, generated from two sequential single beam spectra, is given below:
- Detector: 50x50 micron MCT
- Beamsplitter: KBr
- Test target: Gold mirror
- Collection mode: Reflectance
- Aperture dimension: 10x10 microns
- Mirror velocity: 1.898 cm/s
- Spectral resolution: 4cm-1
- Number of scans: 128
- Spectral smoothing: None
- Zero filling: 2 levels
- Spectral region analysed: 2450-2550 cm-1
- Noise expected: 0.04 to 0.06% RMS
