Transmission Electron Microscopy (TEM)

TEM is employed as a method of cross correlating and cross validating the results of the spectroscopic and scattering methods which will be employed as inline online and at-line process analytical tools. Using the spatial resolving power of a TEM it will be possible to obtain accurate sizes of the particles and estimates of their distributions. Giving highly accurate feedback on the measurements obtained by the PAT tools. These measurements will be made off-line and with post-analysis of the online measurements.

The TEM’s available for these measurements are, on the left, a Thermo Fisher (nee FEI)  Monochromated, double aberration corrected Titan Themis, equipped with a 4 quadrant Energy Dispersive Spectroscopy (EDS) system, and high sensitivity high frame rate detectors of up to 1400 frames per second. On the right we have a JEOL 2100F with EDS.

In addition to the standard comparisons with dried particles on a TEM grid, we will utilise the latest developments in Liquid phase TEM to make like for like comparisons with particles in liquids, mitigating differences in size between the measurement techniques due to drying or solvation shells.

Top shows a drawing of a liquid cell holder tip, with the chips (orange) sandwiched inside the tip to create the liquid cell. Below are the MEMS chips (green) which are sandwiched inside the holder tip to create a microfluidic channel for the liquid to flow through and be observed through the 10nm thick Silicon Nitride windows.

Energy Dispersive Spectroscopy (EDS) is also available to identify and measure the particles composition, enabling the analysis of not only size and distribution of particles, but also their composition if deemed to be a contributing factor to the experimental results from the spectroscopy and scattering technique results.

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