XAS Capabilities

Standard Experimental Hutch for Efficient XAS, both ex- and in-situ

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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.

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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).

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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). We use a Newport Kinematic Base (M-BKL-4) as the adapter plate between the stage and in-situ cell.

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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.

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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

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.

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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

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.