Endstation
Last reviewed: December 2012
In AP13, April – September 2013, we intend to user commission a new zone plate XRF facility on I18. Using an incident energy of 8 -12 keV, we intend to offer a beam of around 250 nm V x 700 nm H . We are interested in establishing whether there is sufficient demand for this to become a regular part of I18 operations. Hence in AP13, applications to use I18 with zone plates will be considered separately to the “normal” I18 applications. Please make it obvious you are applying for this set-up by putting zone plate set up in the beamline questions section of the application form.
The main emphasis will be on XRF measurements as XAS scanning will not be available, but within that limited energy range some different energy mapping may be possible, so for Cu and Pt and Au and maybe As (this might be too beam sensitive) some oxidation state mapping is in principle possible.
The flux will be 1-2 orders of magnitude less than normal on i18 so that very dilute element mapping is unlikely to be successful.
| Equipment or detector | Availability | Comments |
| Si(111) monochromator and 27 mm period undulator giving energy range 2- 20.7 keV (core range 5 -15 keV) | Available | |
| Mechanical KB mirrors with Si and Rh stripes. Mirrors can be moved from beam path for bulk EXAFS. | Available | Typically 1.5-3 (V) x 2 -5 (H) micron spot size. Can be defocused up to 100 μm |
| 9 element Ge detector (4 – 20 keV) XANES can be achieved on sub ppm samples given enough time (6-8 hrs) | Available | |
| Sample stage (25 mm X movement, 30 mm Y movement, 4 kg load) now allows XRF map collection while rastering | Available | XRF maps using continuous scanning of the x-stage removes the deadtime associated with step scans allowing for larger and faster XRF maps. A 200 x 200 point map may now be done in about 3.5 hrs if the sample is contrated enough. |
| 4000 x 2500 pixel CCD for transmission diffraction | Available | Max angular range ca 45 degrees two-theta |
| 4 element Si Drifts detector (2 -10 keV) | Available | Primarily used below 5 keV |
| Triax Optical Spectrometer and MCP-PMT for XEOL and OD-XAS | Available | Can be used with Hybrid mode for Time resolved measurements |
| Fluorescence Tomography | Available | Reconstruction algorithm development ongoing |
| ReflEXAFS | Available | 4 element Si detector mounted vertically. |
| Capillary infront of Fluorescence detector for 3d XAS/XRF | Available | A focussing optic on the detector is used to define a narrow sampling volume from the incident x-rays and outgoing fluorescence signal. This confocal arrangement enables slice, volume and depth dependant XRF/XANES studies of thick samples and solid particles. Spatial resolution ranges from 5-15microns depending on energy. |
Sample environments and stages
| Linkam TMS stage: 25 – 600 C | Available | Sample in gas environment |
| Linkam 1500 furnace 0 -1400 C | Available | Sample in gas environment |
| He enclosure for low energy | Available | At room temperature |
| In situ Raman | Available | 785 nm |
| Electron yield cell | Available | TEY or CEY operation |
| Oxford Instruments MicroRes | Available | Vacuum cryostat. The cooling systems have been upgraded. Sample cooling to 4K is now possible with excellent positional stability. |
| LHe and LN2 Cryostreams for VT down to 10K | Available | About 3 mm of sample remains ice free for XRF/XAS. Advantage over Cryostat is no sample dimension constraints and faster sample changeover. The rest of the sample will be iced over. |
| 2 Attocube 6-axis stages | Available | Provided for additional control of small components |
Support Labs
| Three labs: wet, dry and characterisation | Available | With basic equipment such as hot plate, balances, selection of glassware, pestle and mortar, tweezers, spatulas etc. |
| Thermo FT-IR Microscope | Available | FT-IR with mapping capabilites |
| Fischer XDAL-FD XRF | Available | 50keV - 100μm spot size |
| Perkin Elmer UV spectrometer | Available | |
| Renishaw Raman Microscope | Available | Micro-raman system with mapping capabilities. Red and blue lasers. |
| Zeiss AxioVision Optical Microscope | Available | |
| Nikon Polarised Microscope | Available | |
| Fume cupboard | Available | |
| Solvent tolerant dry, O2 free glove box | Available | |
| Incubator | Available | |
| Microbiological safety cabinet (class 2) | Available | |
| Grinding/Polishing machine | Available | Range of polishing grades available |
| Cutting machine | Available | Water cooled |
| Microtome | Available | WC and Stainless blades |
| Pellet Press | Available | 8 and 13mm dies |
| Tube Furnaces | Available on request | Advance notice required. |
| Upright Furnace in Air | Available | Up to 1500C |
| Clean Room | Available | Balance and Microscope installed |
| Fridge/ Freezer (-20 C) | Available | Access to a -80 freezer available on request |
| Low level Radionuclide Handling Lab With Glove Bag, mini centrifuge | Available | Please contact Fred Mosselmans for more info. |
Timing information: A typical EXAFS scan takes 25 minutes with a 3 micron or so sized beam.Mapping at higher energies (using Ge or Si detector) can now be done at around 5 points per second using rastering, 1 pt per second in step by step mode. Tests on rapid scanning with 50pts/second are planned for summer 2012.
Oxford Instruments MicroRes He/LN2 Cryostat
This low-vibration cryostat can be used either with liquid helium or liquid nitrogen. The clip-on stage can support thin samples of a diameter >14 mm (inner diameter of clip is ~10mm so a few extra mm are needed for support). The x-ray visible part of the sample is approx 10mm across; samples with a diameter larger then 20mm can be mounted but may not get to a uniform temperature throughout the sample. The sample chamber is in vacuum.