Sample Environments

Most samples will be run using the robotic sample changer. You will load your sample into beamline supplied capillaries which will then be placed on pucks. The robot can then load your samples to and from the beam position, allowing for a scriptable and automated experiment. Each puck can hold up to 22 samples, with 20 positions on the table, allowing for 440 samples to be measured in one go!

This method is also compatible with the Cobra/Cryostream (low temperature) and Hot Air Blower (high temperature) allowing for an automated collection ranging from 100K to 1000K. 

An Oxford Instruments Cobra is capable of cooling and heating capillary samples in the temperature range 100-450 K with no nitrogen dewar. We also possess a Cryostream Series 700 which has the same capabilities but requires a dewar of liquid nitrogen. Both systems are compatible with our robotic sample changing system by mounting on movable stages that move the devices. Both the cobra/cryostream and hot air blower can be mounted on the beamline at the same time to cover a wide temperature range. 

Used to heat capillary samples from room temperature up to 1100 K. Temperatures of up to 1200 K can be reached with smaller samples. The blower can be used in conjunction with the robotic system to allow for automated collections.

Hexapod and Translation Stages

We have the ability to manipulate the position of your sample via the 6-axis hexapod or the translation X/Y stages. All sample environments on the beamline will be mounted from either of these stages, allowing for full and precise control (to micron accuracy) of your sample in the beam.

Non-Standard Samples

For samples that do not fit inside our standard capillaries, we offer generic mounts that can be secured on the hexapod. These mounts can allow for the mounting of pellets, rods, films etc. allowing for precise PDF measurements of bulk samples.

DRIX is the optimised routine for running battery type experiments on the beamline. Based on Swagelok pieces, these have been optimised to allow for the highest quality PDF data of these energy materials. Up to 6 cells can be mounted on the beamline, allowing for the in-situ battery cycling of multiple samples. During your experiment, we will show you how to automate the script to allow you to collect every n seconds, to see how your samples are changing as a function of cycle.

An 8-channel Ivium-n-Stat is available for in-situ electrochemical measurements and cycling. This can be used to perform in-situ PDF measurements on up to 8 batteries while they are cycling.

Gas flow experiments have become a popular in-situ environment for catalysis experiments and can be flexible to fit the needs of the proposed reaction. Flexibility of the system has been established, using Swagelok connections, allowing for the connection of auxiliary equipment before and after the cell. This cell is also compatible with the hot air blower, allowing for the heating of samples. Typically a 1/8" quartz capillary is used with this environment to allow for adaquette gas flow over the sample, allowing for heating up to ~950K. A 1/16" capillary can also be used to allow for higher temperature, but at the expense of reduced gas flow.

A gas delivery system, made up of many MFCs, can also be provided by the beamline to supply:

• Nitrogen/Argon/Inert Gases
• <4% H₂ in inert
• <10% O₂ in inert
• CO₂

Due to current extract regulations, we cannot safely extract ammonia, higher percentage hydrogen/oxygen as well as corrosives/alkenes etc. We aim to resolve this as soon as possible. If you are working with water vapour, a trap will need to be provided to avoid extraction of water into the ducts. 

Beyond this, we allow for a lot of flexibility around the cell, and can host user equipment, extra analysis equipment (such as mass spectometers) and much more. Please get in contact to discuss your needs.

We offer a liquid flow cell as a common in-situ environment on the beamline. This cell can be used to examine liquid flows, in-situ synthesis, crystallisation and much more. 
Similar to the gas flow, flexibility has been at the forefront of the design of the cell, allowing us to offer a number of different experiments. We can offer both syringe and peristaltic pumps to allow for injection and continuous flow experiments. Both are based on 1/8" and 1/16" tubing, allowing for compatibility with extra equipment that will increase the success of your experiment.

We are also in the process of improving this setup by development of jacketed tubing, to allow for better temperature control of the fluids, as well as controllable freezing at the sample position. If you are interested in either of these capabilities, or want to help develop this environment, please get in touch.

A hydrothermal cell is available which is capable of operating up to 200°C. The cell design is optimised so that the only contribution to the background is that of the fused-quartz capillary holding the sample. You can have two samples in the cell at any one time, allowing one to alternate between the two, allowing for increased sample collection.

Uncommon Beamline Supplied Environments

The above summarises the main sample environments provided by the beamline. Beyond this, we also can use:

• Linkam Furnace
• Acoustic Levitator
• Heated DRIX Cell

These are less used and are in various states of commissioning, so please get in contact if you are interested in using these, please get in contact.

Borrowing Other Beamline Equipment

We understand that you may want to recreate experiments that you have conducted on other beamlines. This means that we are happy to try and use other equipment so long as you have the permission of the other beamline prior to the experiment. Please contact the relevant beamline and cc us in your chain to make sure that the equipment is both available and compatible with I15-1. If it is not, we will try our best to create/adapt to recreate your complementary experiment.

User Supplied Environments

We are also very open to user supplied environments on the beamline, and welcome any users wishing to try something new! These can range from ball mills to extruders to liquid jet cells, showing the versatility of the beamline. However, it is very important that you contact a member of beamline staff before submitting a proposal to make sure that it is a feasible experiment to be conducted.