1. How do I achieve LOW temperature with capillary-mounted samples?
An Oxford Cryosystems Cryostream Plus can be used in conjunction with capillary-mounted samples to achieve temperatures between 80 - 480 K.

2. Can I cool samples to 10K?
A He-flow cryostat capable of achieving temperatures between 10 - 300 K is available.  The samples will be mounted in flat transmission geometry and the design will allow three samples to be loaded into the holder at once.  Information on sample preparation can be found here.
 

Figure 1.  Cryostat with samples mounted in flat transmission geometry.

   

3. How do I achieve HIGH temperature?

A Cyberstar hot-air blower can be used in conjunction with capillary-mounted samples to achieve temperatures between 350 - 1270 K.

An Anton Paar furnace (Figure 2a) can be used to heat flat plate samples to 1870 K, using a Pt filament (Figure 2b).

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 and requesting a quotation through their website. A link to the website can be found here.  These strips are supplied with thermocouples attached and please use the part numbers shown below.
  2. Locally by XRF Scientific using the dimensions as shown below.  XRF Scientific is a diverse company, so please put 'Attention Mr. Gino Manfredi" in your query on their web page.  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 (Figure 2b).  S-type (0.35 mm diameter) thermocouple wire will need to be purchased separately.  These can be also purchased through XRF Scientific.  Please contact beamline staff if you have any further questions.

 

Part numbers Description
71599
Heating filament Platinum 102 mm x 10 mm x 1 mm
71601 Heating filament Platinum 102 mm x 10 mm x 1 mm with cavity
75727 Heating filament Tungsten with thermocouple 102 mm x 9 mm x 0.5 mm

 

It is possible to recycle used Pt strips through XRF Scientific with additional charges for refining, metal replacement and fabrication.  XRF Scientific do not have the capability to put in a cavity, so this should be machined elsewhere.  S-type (0.35 mm diameter) thermocouple wire will need to be purchased for recycled strips which also can be purchased through XRF Scientific.    Staff at the beamline are able to attach the thermocouples to your strips.  The beamline does not supply thermocouple wire.

 

(NEW) A Stoe capillary furnace (Figure 3) can heat quartz capillaries up to 1370K.

 

   Figure 2a. Anton Paar furnace
Figure 2b. Anton Paar platinum filament, with cavity
Figure 3. Stoe capillary furnace

 

4. Is it possible to do high-pressure experiments?

High-pressure (greater than 1 GPa) apparatus is available.  Our diamond anvil cells (Figure 4) can currently only be used at ambient temperature.  For experiments where pressures exceed 10 GPa, Users will need to supply their own diamonds and WC seats. They can be purchased from: https://www.diamondanvils.com/ or    http://www.almax-industries.com/. Users must consult beamline staff for more information before purchasing, as a number of parameters need to be determined to enable the appropriate diamonds to be acquired.  As Users are required to supply their own diamonds for experiments that exceed 10 GPa, the maximum pressure available is at Users own risk.

The beamline set-up, sample preparation, alignment and data collection is not trivial and is quite time-consuming.  It is recommended that Users without high-pressure sample environment experience contact beamline staff  if interested in submitting a high-pressure proposal.

 

Figure 4.   Diamond anvil cell

 

5. Can I do high pressure / gas flow experiments using capillaries?

Yes, there is a flow cell available; it may be used to either evacuate a capillary, maintain a constant pressure or flow gas(es) during data acquisition. The flow cell is shown in Figure 5 and the gas manifold is shown in Figure 6. For all high pressure capillary experiments using either the Norby or flow cell, the maximum pressure allowed is 2 MPa (20 bar). Higher pressures are possible by prior agreement with beamline staff, however sapphire capillaries will be required.

It is mandatory that thick walled quartz capillaries are used for all high pressure capillary experiments, especially for those that require heating. Pressures of 5 – 10 bar require capillaries with a wall thickness of at least 0.02 mm. 10 – 20 bar experiments require capillaries with a wall thickness of at least 0.05 mm. These can be specially ordered from Hilgenberg.    

Please note that for any high pressure gas experiments above 5 bar with inert gases (at any pressure with flammable gases), 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.

 

Figure 5. Flow cell for powder diffraction measurements

Figure 6. Gas mixing and evacuation manifold

 

 

6. What are the maximum temperatures and pressures that hydrogen gas and hydrogen gas mixtures can be used in capillary and flow cell experiments?

For all Norby and flow cell experiments the maximum pressure allowed is 20 bar.

For pure H2 gas or hydrogen gas mixtures >5% H2, the maximum heating temperature permitted is 500°C. For all other non-combustible gases, the maximum temperature is 1000°C.

Please note that for any flammable gas, at any pressure, flowing or static, 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.

7. Can I use pure CARBON MONOXIDE (CO) gas or gas mixtures containing CO?

Carbon monoxide (CO) is a highly toxic gas (see the safety information below). For this reason we will not permit pure CO gas, gas mixtures containing CO or experiments that generate CO gas at the beamline. Although monitoring is possible, the main issue is that the beamline gas handling and extraction systems are not at a sufficient standard to handle an emergency release.

Safety information as stated in Wikipedia:

"Carbon monoxide is colourless, odorless, and tasteless, but highly toxic. It combines with hemoglobin to produce carboxyhemoglobin, which usurps the space in hemoglobin that normally carries oxygen, but is ineffective for delivering oxygen to bodily tissues. Concentrations as low as 667 ppm may cause up to 50% of the body's hemoglobin to convert to carboxyhemoglobin."

"...levels of 50% carboxyhemoglobin may result in seizure, coma, and fatality."

"Within short time scales, carbon monoxide absorption is cumulative, since the half-life is about 5 hours in fresh air."