Sample environments
PD has been designed for time resolved and in situ experiments, as such we have a wide range of experimental sample environments. Temperature ranges, ramp rates etc. can be found in the Variable Temperature Sample Environment Summary
Room temperature capillaries
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.
The Norby cell is for flow experiments and can be used with a gas manifold/Hiden XCS gas flow system for gas mixtures. Maximum pressure allowed through a 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/Hiden XCS gas flow system.
There are special requirements for high pressure capillary experiments. Please see our high pressure capillary measurements page for further information.
Coin cell batteries
Up to 4 batteries (type 2032) can be cycled at a time using a Neware battery tester.
Gas flow system and mass spectrometer
The XCS gas system has 4 gas input lines that delivers flow rates as follows: Inlet 1 – 100 ml/min (controllable range 2 – 100 ml/min), inlet 2 – 20 ml/min (controllable range 0.4 – 20 ml/min), inlet 3 - 3 ml/min (controllable range 0.06 – 3 ml/min), and inlet 4 - 3 ml/min (controllable range 0.06 – 3 ml/min). Gas mixtures can be made and gases delivered at a specific flow rate if more than one gas is flowed to the capillary using this system. Typical flow rates used for filled capillaries are 2 – 3 mL min of the gas mixture.
The Hiden QGA mass spectrometer has a gas intake rate of 1 mL min and has a 1‒200 atomic mass units (amu) range.
Anton Paar HTK2000
The beamline is unable to supply Pt and W strips for User experiments. Users intending to use the Anton Paar HTK2000 furnace for their experiments can obtain their own strips in two ways:
Purchasing directly from Anton Paar. These strips are supplied with thermocouples attached.
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.
Anton Paar DHS1100 furnace
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, air 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 can be achieved using a diamond anvil cell. Users will need to supply their own diamonds and WC seats, and must discuss with the Beamline staff before the proposal submission and experiment.
Capillary furnace
The Stoe capillary furnace is capable of heating quartz capillaries from room temperature to 1370 K, above which sapphire capillaries must be used. Users must supply their own capillaries. 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
A CCR Cryostat capable of achieving temperatures between 10-300 K is available. The design allows for a single Al capillary sample holder or three samples to be loaded into the holder at once. The 3 samples will be sealed in each position with Kapton film. Note: greater temperature transfer to the sample is achieved with the aluminium capillary and is recommended for measurements. Users need to provide their own aluminium capillaries.
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.
Electric field cell
Samples are loaded in capillaries so the beamline capillary spinner can be used. The field is applied ~5 mm above and below the sample. The high voltage power supply is an iseg Spezialelektronik THQ 60W compact with 2 high voltage channels and an output voltage of 0.5 - 32kV. The voltage needs to be changed manually on the high voltage power supply controller that is in the experimental hutch. The whole cell is enclosed with Perspex to improve safety so the electrodes cannot be touched while the cell is in operation. An electric field can also be applied while the sample is cooled as it can be used with additional sample environments such as the beamlines cryostream.
User sample environments
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.