Standard Experimental Hutch for Efficient XAS, both ex- and in-situ
Our experimental Hutch B is designed for efficient XAS on samples mounted in standard sample holders, but also a large array of in-situ cells. To minimise beamline downtime, the hutch features a non-customisable optical table equipped with a comprehensive set of tools. It supports both transmission and fluorescence on samples at room temperature or within a cryostat at 10K.
The room temperature X-Y stages can accommodate small user-supplied cells for in-situ catalysis, provided they fit within the available space (approximately 10 x 10 x 10 cm). Additionally, Hutch B supports in-situ battery research and capillary heating up to 700°C using the X-Y stage. For more details about our sample environments see below or contact the beamline team to discuss your specific requirements.
Scroll down to see more information on the following:
Room temperature samples
Coin cell batteries
In situ cells
Potentiostat
Capillaries and hot air blower (High Temperature or High Pressure experiments)
Cryostat
Gases
Crystal spectrometer / HERFD (Hutch C)
Room temperature samples
Samples holders are mounted onto a sample “carousel” (below left), which is mounted magnetically to the inside top lid of the room temperature chamber (below right).
The sample carousel has three paddles at 120° separation - ideal for fluorescence samples. A four paddle carousel (90° separation) can be used for transmission mode only, specifically note that the four paddle carousel will clip the incoming beam if used in fluorescence mode. Each paddle can fit up to three of our standard sample holders.
Hint
Tape down a small piece of fluoro card (white) - very useful for finding the beam by visual inspection during alignment!
Coin cell batteries
We have another room temperature sample chamber lid that is optimised for in-situ coin cell batteries. The sample holder lid is shown on the left, and the sample chamber on the right. Electrical connection to user supplied battery testers can be made through the lid (preserving a Helium atmosphere on the inside of the chamber).
Note
Check our review paper on this topic:
https://doi.org/10.1002/batt.202100006
In-situ battery measurements will only work in transmission mode.
 |  |
|---|
In situ cells
The room temperature chamber can be removed and in its place we can accommodate for user supplied in-situ cells, eg for catalysis, provided the cell fits a space envelope of approx 10 x 10 x 10 cm. An example is shown below (see doi.org/10.1021/acs.energyfuels.1c04072)
Note
The beamline does not have an in-situ cell, users supply this themselves. We can however put new groups in touch with those more experienced with the set-up and groups often cross-pollinate ideas and designs.
 |
Potentiostat
The beamline keeps a small potentiostat/galvanostat as a backup in case user supplied equipment fails. Details regarding the PalmSens4 can be found online.
Note
The PalmSens4 is available as a backup only, please bring your own as Plan A.
 |
Capillaries and hot air blower (High Temperature or High Pressure experiments)
A capillary set up and hot air blower from the Powder Diffraction Beamline is pictured below. Please note that because this resource is shared between beamlines, availability is not guaranteed. This is used for variable temperature experiments up to 700°C (this upper limit may be lower for certain flammable gases such as H2), and/or where samples are maintained under a specific gas atmosphere either as flow-through or under pressure up to a maximum of 20 bar. The beamline delivers gas through 6 mm nylon tubes. Please note that these are rated to 10 bar only. If working at pressures above 10 bar, bring your own steel lines.
🧐 Where can I purchase suitable capillaries?
Capillaries can be ordered from e.g. Hilgenberg or Charles Supper, and standard stock items will take at least two weeks to be delivered. For non-standard thicker-walled quartz capillaries, users will need to contact Hilgenberg directly for pricing and availability. Delivery time might be longer.
Requirements
Note that only quartz capillaries with 1 mm outer diameter are allowed, and:
wall thickness of at least 0.05 mm if under pressure (1 to 20 bar maximum)
if under pressure, the choice of gases is also limited, eg inert gases and Nitrogen
wall thickness of at least 0.01 mm if no gas pressure (flow-through)
Note that for any capillary heater experiments there must always be 2 persons present at the beamline to monitor the capillary and ensure that breakages are detected as soon as they occur
Cryostat
We have a 10 Kelvin cryostat in Hutch B that can be used for solid and liquid samples. The cryostat and sample holder are pictured below.
Only one of these sample holders can fit in the cryostat at a time (holding two or three sample depending on the hole configuration, two pellet samples are shown in the photo below).
Allow 30 minutes overhead per sample change, such that the sample will have time to cool down to cryogenic temperatures before scanning.
Note
Variable temperature measurements are not possible using the cryostat.
 |  |
|---|
Gases
The Australian Synchrotron can supply compressed, pure Nitrogen, Helium, Argon, and Air, whilst pure Carbon Dioxide and Oxygen may be supplied only after special permission.
Contact the beamline scientists well ahead of time.
Other specialty gases may need to be purchased by the user group and delivered directly to the Synchrotron (after agreement with the Synchrotron Safety Team).
Ammonia and Methane are not allowed as a supplied/inlet gas. A small amount of production of these gases from sample reactions/cells is fine, provided this has been calculated beforehand and supplied as info in both the EA form and beamtime proposal according to our proposal guide).
Specific to hydrogen gas mixtures our rules are as follows (see: https://doi.org/10.1016/j.energy.2016.12.036):
max 4% H2 (in N2 balance) for room temperature measurements ONLY, and
max 3% H2 (in N2 balance) for temperature dependent measurements up to max 400°C
There is no dedicated gas extraction system in the hutches, consider bringing a gas collection bag that can be emptied in our fume hood post experiment.
We have gas detection monitors in both Hutches B and C for the following gases: CO, CO2, O2, and flammable.
Crystal Spectrometer / HERFD (in Hutch C)
We are currently commissioning a crystal spectrometer (eg for HERFD) in the second experimental hutch and are accepting limited merit beamtime proposals to use the spectrometer. Capability will expand over time, so please make sure to follow our beamline updates pages for the latest news. This experimental hutch is dedicated to, and will only accommodate for, experiments using the spectrometer.