Materials Analysis

Identification and Characterisation

We have a wide range of microscopic techniques available which provide imaging, elemental analysis and spatial resolution of molecular information. These include: optical, SEM with EDX and TEM and microscopic Raman.

Spectroscopic analysis

We can identify the chemical nature of a material using FT-IRFourier Transform Infra-Red or Raman spectroscopy in the laboratory. We can also apply our own portable instruments on site if required. These techniques measure the molecular vibrations of the samples either in the laboratory or through fibre optics in-situ. The analysis can be used to calculate concentration, not only for the sample but of individual molecular components. We can also monitor reactions and determine parameters such as degree of cure and reaction kinetics.

Raman Spectra

The image shows the Raman spectra generated during an in-situ measurement of the polymerisation of styrene. The C=C band at 3010cm-1 due to the vinyl group in the styrene decreases as the band at 2900cm-1 due to the CH stretch in polystyrene increases. From this analysis we were able to determine the degree of polymerisation as a function of temperature and time.

Microscopic analysis

We can examine the morphology of materials using optical or electron microscopy (using electrons rather than light to produce a high resolution image. SEM Scanning Electron Microscopy works by detecting backscattered and secondary electrons emitted from the sample after contact with the electron beam. X-rays are also emitted so by using an EDX Energy Dispersive X-ray detector, composition information is produced. We use SEM for surface analysis. For Bulk analysis we use TEM Transmission Electron Microscopy , this works on a similar principal to the SEM but uses different detectors and has a higher magnification capability.

The image is a TEM image of a carbon replica of permanganically etched XLPE cross-linked polyethylene . The individual lamellae are clearly visible. TEM analysis was used to identify voids in XLPE power cable. This was combined with spectroscopic analysis of the cable which showed rate of migration of additives from the semiconducting cable layer into the XLPE and the degradation of peroxide additives in the XLPE itself. This allowed us to predict the lifetime of the cable in service.

TEM Image SEM Image EDX Image

The SEM Image is of worn flame retarded fabric and the accompanying EDX image is of a particle found in the fabric. The SEM shows the fibre structure while the EDX shows elements such as bromine and antimony in the particle. Analysis of flame retarded fabrics allowed us to assess the health risks of using flame retardants in home furnishings.

Properties and Performance

Thermal methods such as DSC Differential Scanning Calorimetry, TGA Thermogravimetric Analysis, DMA Dynamic Mechanical Analysis and Dielectric Spectroscopy are used to determine properties such as glass transition temperature (Tg), melting, curing and degradation behaviour; this is combined with mechanical, electrical and dielectric property measurements, as a function of temperature and frequency, to determine physical properties. We also have special experiment rigs for thermal conductivity, wear rate and dynamic friction measurements.