Facilities

Our >£1,000,000 laboratory is well equipped for a huge variety of tasks. As well as our main laboratory we have access to two test bays for larger scale projects, a synthesis and preparation laboratory and department characterisation facilities (e.g. XRD, SEM, BET). The main laboratory has eight fume-cupboards paired in four bays, two of which are walk-in. There is ample bench and storage space with each fume-cupboard and additional bench top space running the entire length of the lab. The fume-cupboard bays have ventilated gas cylinder cabinets with a capacity for five L size gas cylinders. The rear of the lab has a well equipped workspace for such tasks as reactor assembly and disassembly and basic metalworking. The laboratory is fully ventilated and has a range of gas alert alarms fitted (e.g. carbon monxide).

Our equipment and facilities include:

  • Chemical Looping Reactor
  • In-Situ Raman Spectroscopy
  • Gas Analysis
  • Characerisation Equipment
  • Controlled Atmosphere & High Temperature Furnaces
  • Materials Synthesis & Fabrication 
  • Thermogravimetric Analysis
  • Membrane Reactor
  • Solid Electrolyte Potentiometry

 
 
We have designed, constructed and now operate a fully portable chemical looping reactor. The reactor has been operated in both Newcastle and Grenoble (at the ESRF Synchrotron facility), the latter facilitated by the unique design feature of having open narrow slots for X-ray penetration into the reaction bed. The system comprises a vertical reactor, with a ~20 cm reaction bed, mass flow regulated gas supplies with automated valves and gas analysis equipment. The system has a state-of-the-art water delivery system, which allows us to feed low concentrations of water vapour at low flow rates. Here you can see Wenting inspecting the equipment during the initial setup in Newcastle. 

 

 

We maintain and operate the department Raman spectroscopy facility. The spectrometer is a top of the range Horiba LabRam Evolution HR instrument operating with a high power (455 mW) 532 nm laser. The system is ideal for the study of ceramic materials and offers unprecedented spectral resolution. Full details of the instrument can be found here. We also have our own in-situ Raman cell (Linkam TS1500) capable of operation up to 1500 °C (inset top left). Full details for the in-situ cell can be found here. Through collaboration we have access to a range of spectroscopic and tomographic facilities, including open bench Raman facilities (inset top right), in-situ FTIR and micro-/nano-CT.

 

The majority of our work involves the analysis of gases. Therefore we are extremely well equipped for highly sensitive and highly resolved gas analysis. We have numerous gas chromatographs around the laboratory, as well as numerous mass spectrometers. We have hygrometers, NOx/SOx analysers, CO/CO2 and H2O FTIR analysers, and a newly ordered suite of NDIR analysers capable of analysing a range of gases. Shown above is our MKS MultiGas FTIR analyser. Overall we have an incredible range of gas analysis apparatus with the ability to measure in the most challenging of conditions.

 

We routinely access the School of Engineering characterisation facilities. Shown above is the ThermoScientific Surfer, a surface area and porosity analyser. We also have access to the Advanced Chemical and Materials Analysis (ACMA) facility, providing us with SEM, XRD and other routine chemical analyses (full details here). Finally, we closely collaborate with the National EPSRC XPS User's Service (NEXUS) facility, located in the building adjacent to us, provding us with access to state-of-the-art facilities such as TOF-SIMS, Helium Ion Microscopy and combined Raman-XPS (full details here). Overall, within our the university we can easily charaterise a range of materials properties using both routine and unique characterisation equipment.

 

 
 
 
Across our laboratories we have a huge range of furnaces in terms of size, geometry (e.g. vertical, horizontal and split-tube) and function. We have a range of controlled atmosphere furnaces, including those with optical access and the possibility to work under reduced pressures. We use these for the preparation and characterisation of materials. Examples include monitoring wetting of molten salts on ceramic supports (image shown above) and the preparation of exsolved materials in controlled gaseous environments (image shown below). Through collaboration we have access to a floating zone furnace which can be used to prepare specifically oriented single crystals of wide-ranging composition.
 

 

 

Our newly acquired synthesis and preparation laboratory is fitted with a fume-hood for wet chemical preparation, a drying oven, a calcination furnace, ultrasonic probe and polishing/cutting equipment (shown above). Overall, this allows us to prepare a range of catalytic, membrane and chemical looping materials. Via industrial and academic collaboration we routinely prepare model systems through microfabrication methods, which we use to better understand mechanism in our materials and processes.

 

 

Our thermogravimetric analyser (TGA) is a Rubotherm DynTHERM system capable of operating under elevated pressure and with flowing steam. The system provides highly sensitive and highly resolved measurements which are particularly useful for our chemical looping materials. Full details of the system can be found here

 
We routinely characterise high temperature membranes in operation. Shown above is an example of one of our membrane reactor rigs. At the right you can see the gases entering through high pressure fittings into mass flow controllers. The membrane reactor is placed inside a high temperature furnace, with gases exiting the reactor analysed by mass spectrometery (bottom left hand side), gas chromatography (bottom right hand side) or FTIR analysis (green box within fume hood).  

We have recently commisioned a solid electrolyte potentiometry cell. The cell will allow us to probe the oxygen content of oxide materials, electrochemically, whilst manipulating the oxygen content of the environment. We are particularly interested to study non-stoichiometric perovskites for applications in chemical looping.