Institute for Materials Research

FACULTY OF ENGINEERING

 

Facilities

Facilities by methodology:

Microscopy

Electron microscopy is located in a dedicated suite of rooms (Leeds Electron Microscopy and Spectroscopy - LEMAS Centre), and is a joint facility between Earth Sciences and Materials. There are 3 full time experimental officers in the unit and a number of dedicated microscopy based academic staff, research assistants and students. Optical microscopy facilities, including technical support, are found in Materials with additional facilities dedicated to cement located in Civil Engineering. Materials houses a comprehensive surface analysis facility with additional equipment available in Physics.

Image Processing

  • Kontron KS400 image processing and analysis system

Optical Microscopy

  • Extensive preparation facility for metallic, ceramic and composite materials (freeze drying, resin impregnation, polishing etc.)
  • Wide range of reflected and transmitted light microscopes
  • Polarised light, differential interference contrast, etc.

Scanning Electron Microscopy - Specialised techniques include:

  • High resolution backscattered electron imaging
  • Electron Backscattered diffraction and cathodoluminescence
  • Digital image storage and processing
  • Extensive specimen preparation facilities
  • 2 Camscan Series 4 SEMs with Link Systems EDX facilities
  • Camscan CS-44-EX with Link Systems EDX facility, cathodoluminescence and image analysis
  • LEO Gemini 1530 field-emission SEM for high resolution (c. 1-2 nm) low accelerating voltage work
  • Philips XL30 Environmental SEM including EDX and heating stage
  • FEI Nova 200 Nanolab Dual beam FEGSEM/ Focused Ion Beam (FIB) with nanomanipulation facilities
  • Cameca SX-50 electron microprobe analyser
  • 3 WDX spectrometers + Link Systems 10/55 S EDX system
  • Quantitative analysis and mapping of most elements with atomic numbers > 3
  • Transmission Electron Microscopy
  • Extensive specimen preparation facilities:
  • dual beam FIB with in-situ liftout
  • chemical/electrochemical polishing
  • ion-milling including cryofacility
  • Gatan Precision Ion Polishing System (PIPS)
  • Philips CM200 Field emission TEM/STEM equipped with light element EDX detector and Gatan Imaging Filter (GIF) for PEELS and Energy Filtered TEM
  • Philips CM20 (200 keV) TEM/ STEM with light element EDX detector.
  • Heating/ Cooling holders and ex-situ reaction cell facility for gas/heat treatment (1473K)
  • TEM/STM holder for combined microscopic analysis of nanostructures.
  • Leeds Materials is a major stakeholder in £4.2. million UK SuperSTEM project for a suite of aberration corrected, sub-Angstrom analytical scanning transmission electron microscopes which are to be sited at nearby Daresbury Laboratories.
  • Tomography (IPSE)
  • X-ray tomography
  • Electrical tomography

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Surface characterisation

  • VG Escalab Mk 1 offering complete range of surface spectroscopy techniques
  • XPS for chemical state characterisation
  • UPS for valence band characterisation
  • AES and scanning AES
  • Static, dynamic (depth profiling) and imaging SIMS
  • In-situ reaction cell facilities for gas/ heat treatments (773K)
  • Topometrix Atomic Force Microscope
  • AFM with Micro Thermal Analysis Attachment
  • Access to extensive range of AFM/STM facilities in IPSE and Physics
  • Quantachrome Aotosorb-1, automatioc gas and vapour adsorption apparatus with chemisorption facility. Micropore model with DFT software
  • Additional Surface Analysis Equipment in Physics
  • VG Sigmaprobe with small area XPS and field emission AES
  • UHV-STM
  • Atomic force Microscopy (AFM)
  • Scanning Tunnelling Microscopy (STM)
  • Low temperature STM
  • Contact Angle Apparatus
  • Surface Analysis Facilities (optical) (In Physics)
  • Ellipsometry (including spectroscopic capability)
  • Surface Plasmon Resonance (Spectroscopy and Imaging)
  • Confocal Microscopy

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Spectroscopy

X-ray Fluorescence

  • XRFs located in both Earth Sciences and Mining and Mineral Eng.

The IMR XRD Facility uses Philips/PanAlytical and Siemens Diffractometers and software along with the latest ICDD database. Typical Applications are:

  • Qualitative and quantitative phase analysis
  • High-resolution studies
  • Crystal structure analysis
  • Stress and texture analysis
  • Reflectometry
  • Temperature and atmosphere controlled studies

Solid State NMR

  • Structure determination of amorphous / glassy non-metallic materials.
  • Bruker MSL300 Spectrometer
  • Static Spectra for 2H and 13C giving dynamics information
  • Multinuclear MAS and CPMAS giving structural information
  • Variable Temperature Operation

Spectroscopic Facilities in IMR

  • Ar+-ion pumped laser spectroscopy
  • Tunable Ti-sapphire pumped laser spectroscopy (Emission Spectroscopy of RE/TM ions)
  • Edinburgh Instrument (300-5500 nm) time-resolved fluorimeter
  • Fibre laser and gain characterisation (800-1700 nm)
  • Renishaw inVia Raman Microscope Spectrometer with Low-frequency (up to 10 cm-1) characterisation capability
  • Abbe refractometer and Multiwavelength Prism-coupler for refractive index and waveguide loss characterisation
  • Perkin Elmer FTIR with fibre loss characterisation facility
  • Perkin Elmer Lamda 19 UV-visible-NIR spectrometer from 190-3300 nm

IR and Raman Spectroscopy Facilities (In Physics)

  • Renishaw 2000 Raman Microscope
  • Perkin Elmer 580B double beam dispersive IR spectrometer
  • Nicolet 740 G FTIR spectrometer with photoacoustic attachment
  • Bomem MB 151 FTIR spectrometer

UV-vis Spectroscopy (In Physics)

  • Time Resolved Fluorescence Spectroscopy
  • SNOM (Optical, Fluorescence, Raman)
  • Leachate and Pore Solution Analysis
  • Pore press
  • Ion Chromatograph for determining anions in solution
  • Facilities including clean rooms for isotope tracer studies in Earth Sciences Including K-Ar, 40Ar-39Ar, Rb-Sr and U-Pb system (Earth Sciences)
  • Thermo FI Maxim ICP-AES (Earth Sciences)
  • ICP-MS (Earth Sciences)

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Materials Modelling Software

  • Ab-initio Electronic Structure Software
  • CaSTEP Pseudopotential code
  • WIEN2k FLAPW code
  • Materials Studio and Cerius2 for Crystallographic Visualization
  • Molecular Dynamics (in IPSE)
  • Thermodynamic Software
  • FactSage
  • MTDATA
  • Thermo-Calc

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Thermal Methods

The following thermal analysis equipment is located in the IMR and sister institutes. A wide range of additional equipment is available in other Departments.

  • Perkin-Elmer DSC-7 power-compensated DSC with DDSC attachment (-150 to 723 C)
  • Perkin-Elmer DTA-7 heat-flux DSC/DTA (to 1500 C)
  • Perkin-Elmer DMA (bending and tensile modes to 500C, dilatometry. softening points)
  • Perkin-Elmer DMA-7 for high-temperature rheology
  • Stanton-Redcroft DTA-673-4 DTA (to 1500 C)
  • Stanton-Redcroft STA- combined DTA/TG (to 1500 C)
  • Stanton Redcroft DSC 1500
  • Stanton Redcroft STA-780 (to 1000 degrees)
  • Stanton Redcroft TG 760 (to 1000 degrees)
  • Various controlled atmosphere thermogravimetry facilities for large and small samples
  • Malkin dilatometer (to 1500 C)
  • Netzsch dilatometer (to 1500 C)
  • Theta Instruments dilatometer (high speed)
  • Stanton-Redcroft TMA-790 thermomechanical analysis (to 1000 C)
  • Polymer Laboratories DMTA (bending mode to 500 C)
  • SETARAM HT1000 calvet micro-calorimeter
  • SETARAM HT1500 calorimeter.

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Mechanical Testing

  • NanoTest Nano indenter
  • 50 kN Mayes servoscrew testing machine
  • 20 kN RDP Howden machine
  • 50 kN RDP Howden machine
  • 100 kN RDP Howden servohydraulic machine
  • 50 kN Instron machine with high temperature (1600 C) capability
  • 20 kN Vibraphone fatigue testing machine
  • Rock mechanics testing equipment and instrumentation (In Mining and Mineral Eng.)
  • 50 tons capacity instrumented rock planing machine (In Mining and Mineral Eng.)

Large scale mechanical testing

  • Large test floor with selection of rigs
  • Instron 8500+

Creep and Shrinkage

  • Environmentally controlled laboratories to determine creep and shrinkage.
  • Loading apparatus consists of creep frames for testing small concrete specimens and larger masonry walls/piers.
  • Apparatus for measuring autogenous shrinkage from initial set.

Rheology

  • A range of small scale viscometers are available
  • Haake Rotovisco 2
  • Carri-Med CSL 5000 rheometer
  • Viscoelastic measurements over the temperature range -195 C to 400 C.
  • Ferranti-Shirley

In addition large scale tests are possible using Tattersal vane viscometer for concretes

Fluid Dynamics

  • Sedimentary fluid dynamics laboratory (Earth Sciences)
  • With facilities to handle slurries
  • Fluid dynamics laboratories in Mechanical Engineering and Civil Engineering

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Particle Characterisation

  • Total surface area and pore structure by gas-adsorption
  • Particle size distributions
  • X-ray sedimentometry
  • Laser diffraction (Malvern Mastersizer E, Malvern Zetasizer)
  • Light scattering (Malvern Zetasizer 4, Malvern Nanosizer (IPSE))

Pore Structure and Permeability

  • Quantachrome Aotosorb-1, automatioc gas and vapour adsorption apparatus with chemisorption facility. Micropore model with DFT software
  • Mercury Intrusion Porosimetry (Micromeritics Auotpore 3)
  • Nitrogen Adsorption Porosimetry (Micromeritics ASAP 200 BET)
  • Helium Pyncnometry (Quantachrome Ultrapycnometer 1000)
  • Water Porosity by Vacuum Saturation
  • Water Permeability (with ability to go to 40 bar)
  • Gas Permeability
  • Oxygen Diffusion
  • Chloride Diffusion
  • Steady State
  • Non Steady State
  • Applied Voltage
  • AASHTO T227

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Electrical property characterisation

Complete property characterisation of a wide range of electroceramic materials - measurement ranges of 100 Hz to 10 GHz and -190 C to 1500 C

  • dielectrics
  • piezoelectrics
  • electrostrictives
  • pyroelectrics
  • impedance spectroscopy

Electrochemical and Solid State Science

  • AC and DC electrical measurements from RT to 1200 C
  • In-line gas analysis using EMFC and 300 amu Mass Spectrometry
  • Sensor testing facility for Gases and Molten Metals
  • Multi channel high impedance electrometer
  • Multi channel electrochemical cell tester
  • Automated CIP (400 Mpa)

Corrosion

  • Programmable Gill AC potentiostat
  • Various ionic diffusion testing methods

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Processing of Nanostructures

  • Two floor 150m2 Class 1000 (or ISOClass-6) Cleanroom
  • Electron Beam Lithography System (Raith 50L); Direct writing down to 50nm
  • Focussed Ion Beam Etching and Pt Deposition; down to 20nm
  • Pulsed Laser Deposition
  • Front-to-Back DUV Contact Mask Aligner (KS-MJB-3) & 2 UV-400 Aligners
  • RTP (x) & Tube Furnaces, for contact and implant annealing
  • Surface Profilers (Tencor Alpha Step IQ, Burleigh SPM & STM)
  • RIE Etching (H2CH4, CF4, CHF3, Ar, O2 )
  • PECV Deposition (SiO2, & Si3N4 )
  • RF Sputtering (SiO2, Alumina, Cr, AuGe, Ni, Pd, Au, etc )
  • Vacuum Evaporation (Inc. E-Beam)
  • Wire-bonding & Gold and Copper Plating
  • Scribing, Sawing Polishing, Lapping & Polishing
  • Semiconductor Parameter Probing (down to 5um)

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Processing of Metals

  • Argon Arc-melter
  • Rolling mill
  • Silica encapsulation rig
  • Horizontal tube furnace (max temp. 1200°C) for processing in controlled atmosphere.
  • Range of furnaces

Non-Equilibrium Processing

  • Rapid solidification - chill block melt spinning
  • Containerless melting furnace (electromagnetic levitation/glass fluxing) with growth front velocity measurement option
  • 6m drop tube
  • Inert gas condensation facility for production of nanocrystalline materials and nanocomposites (unique in UK)
  • Mechanical alloying - Retzsch PM4 planetary mill, SPEX 8000 mixer mill

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Processing of Ceramics and Other Powders

  • Comminution of ceramic powders by a variety of routes
  • Small-scale spray drying and freeze-drying
  • Die- and iso-pressing
  • Injection moulding
  • Tape casting
  • Fully-instrumented hot press (to 1900°C)
  • Rate-controlled sintering dilatometer
  • Fast-firing equipment
  • Range of controlled furnaces up to 3000°C
  • Class 1000 clean room (class 100 work stations) for preparation of high grade ceramics, mainly via novel chemical routes
  • Micromeritics Sedigraph 5100 (Civ)
  • Sol-gel synthesis and thin film deposition
  • Hydrothermal synthesis of nanopowders
  • Solution-based oxide powder synthesis, including nanoparticle synthesis
  • Semi Automatic Screen Printing facility

Carbon Materials processing:

  • Range of carbonisation furnaces to 2573 K
  • Instrumented fibre spinning rig and special winding drums for laminate lay-up

Cements Processing:

  • Well equipped and staffed concrete laboratory
  • Dedicated aggregate storage facility
  • Aggregate drying equipment
  • Trefoil kilns for firing wastes to form aggregate (Capable of 1100°C+)
  • Fog curing room
  • Large scale temperature matched curing tanks
  • Cut off saws, grinding and coring equipment
  • Walk in environmental cabinets
  • Supercritical carbonation facilities

Glass Processing:

  • Controlled atmosphere melting furnace for Oxide Glasses (1550 C)
  • Air melting Furnace (1600 C)
  • Radio-frequency furnace capable reaching (1900 C)
  • Field assisted and thermal diffusion Ions in Glass
  • Carbolite controlled gas flow furnace for atmosphere control (1700 C)

Pyrolysis facilities

  • Fixed Bed (In Fuel and Energy)
  • Fluidised Bed (In Fuel and Energy)
  • Pilot scale trefoil kilns (In Civil Eng.)

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Safety Related Facilities

  • Airborne dust sampling and monitoring units (In Mining and Mineral Eng.)
  • Explosion Testing Facilities (In the Centre for Combustion and Energy)
  • Laboratory Fan Stirred high pressure/high temperature turbulent explosion vessel
  • Twin room fire test rig
  • Pool fire test rig
  • Large scale explosion Test Facility

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