Sample environments

Room temperature capillaries

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The capillaries are mounted in a motorised goniometer heads (two tilt and two translation axes). The single sample spinner is completely compatible with the Cryostream and hot-air blower ancillaries, and the spinning speed is adjustable.  

Capillary sample information and preparation information can be found here.

Variable temperature capillaries

We have two hot air blowers and a cryostream that can be used with capillaries. Please see the variable temperature sample environment page for details on their temperature range, and heating and cooling ramp rate.

There are special requirements for high pressure capillary experiments. Please see our high pressure capillary measurements page for further information.

The Norby cell is for flow experiments and can be used with a gas manifold for gas mixtures. Maximum pressure allowed through capillary is 20 bar.

A flow through cell for gas flow experiments when flow rate coming out of the capillary needs to be measured. Can be used with a gas manifold.  

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Norby cell

Coin cell batteries

Anton Paar furnaces

Higher temperatures can be achieved using either the Anton Paar HTK2000 furnace or Anton Paar DHS1100 furnace

The beamline is unable to supply Pt and W strips for User experiments. Users intending to use the Anton Paar furnace for their experiments can obtain their own strips in two ways: 1. Purchasing directly from Anton Paar. These strips are supplied with thermocouples attached. 2. Locally by XRF Scientific. If you wish to use a cavity, then you will need to make separate arrangements as XRF Scientific do not machine the cavity.  The cavity in the Pt strip is 0.2 mm deep and is approximately 20 mm (L) x 8 mm (W) located in the centre of the strip.  S-type (0.35 mm diameter) thermocouple wire will need to be purchased separately. Staff at the beamline are able to attach the thermocouples to your strips. The beamline does not supply thermocouple wire. Hints on the preparation of samples for furnace experiments are provided by Anton Paar and are available here. Additional information regarding the reactivity of samples with platinum is available here; this information should be read carefully, well in advance of the proposed experiment.

DHS1100

The Anton Paar domed heating stage (DHS1100) can be used to heat flat plate samples from ambient temperature to 1100 °C in a variety of inert gas atmospheres or under vacuum.  Solid compact, thin film and powder samples can be used in the furnace.  The furnace is able to oscillate, giving markedly improved powder averaging compared to the HTK2000, however sample preparation is important for obtaining high quality results.

Solid compact and thin film samples can be directly placed on the aluminium nitride heating plate and held in place with Inconel spring clips.  Sample dimensions should be no larger than 20 mm in diameter and 1 mm thick (see Figure below).  Sample thickness should be as small as possible due to temperature gradients from the heated bottom of the sample through to the top where the diffraction data is obtained.

Powder samples are mounted in special, circular Inconel sample holders that are 20 mm in diameter and have a well depth of 1 mm.  The powder sample holders are supplied by the beamline and are re-usable.   Although Inconel is resistant to oxidation, and is relatively stable at high-temperatures, it is possible that samples may react with the sample holder.

Due to variable sample thicknesses and thermal properties it is recommended that experimental teams carry out their own calibration during beamtime.  Adequate time (approximately 4 hours) should be allocated in beam time proposals for the calibration.  An adapter for collecting the temperature calibration will be provided.

High Pressure Diamond Anvil Cell

High-pressure (greater than 0.1 GPa) apparatus is available to be used at ambient temperature. For experiments where pressures exceed 10 GPa, users will need to supply their own diamonds and WC seats, or discuss with a Beamline Scientist. 

Capillary furnace

The Stoe capillary furnace is capable of heating quartz capillaries from room temperature to 1370 K. The samples are heated using graphite furnace inserts specifically sized for different capillary diameters: 0.3-1 mm.

Normal thin-walled capillaries (10 μm) can be used and the capillaries are rotated to improve powder averaging during data collection. To ensure that the sample is in the beam, the capillary must be filled to a depth of 4 cm from the sealed end. There is no need to break off the funnel or shorten the capillary as the full length is required to ensure the capillary is properly housed in the furnace.

Cryostat

Information on preparing samples for the cryostat are described below:

A CCR Cryostat capable of achieving temperatures between 10-300 K is available. The samples will be mounted in either reflection or transmission geometry, and the design allows for a single Al capillary sample holder or three samples to be loaded into the holder at once. 

Samples are mounted in the cryostat within the sample holder, which can hold up to three samples at once. The samples will be in flat transmission geometry and sealed in each position with Kapton film. Sample changeover requires venting the sample chamber, dismantling the cryostat and then reassembling and pumping down the system after the samples are changed. It is expected that this will take approximately 90 minutes so time should be set aside for this procedure in your experimental plan.

I'm bringing my own stage...

Users need to be in contact with the owner of the stage before submitting a proposal. the setup must be approved before the proposal has been submitted according to ANSTO safety processes and procedures. Failure to do so on consultation with the beamline team will mean the proposal is marked infeasible at technical review.

Users are also welcome to manufacturer their own stage, providing they fit within the constraints of the omega circle. Refer to Diffractometer mounting space for sample stages. Sample stages requiring centering adjustment may be mounted to a Huber 5102.20 XY stage which is positioned on the omega circle.

Each axis on the X-Y stage is capable of plus or minus 12 mm translation and can be controlled via the beamline control station. Samples not requiring this additional adjustment can be mounted directly to the omega circle, For an engineering drawing of the XY-stage and also information on the hole pattern that may be used for mounting sample stages, see here. The distance from the face of the omega circle to the beam centre is 250 mm. The distance from the face of the XY-stage when mounted on the omega circle to the beam centre line is 188 mm.