To evaluate the performance of the three novel PATs in monitoring the synthesis in the different case studies, the industrial manufacturing processes were successfully replicated at lab-scale by the RTOs of the NANOPAT consortium (UPV: polymeric nanoparticles, UP: silica nanoparticles, MUG: nano-hydroxyapatite, ZHAW: zeolites, MUG: ceramic NPs electrolyte suspensions). Each RTO was equipped with their according PAT instruments (PDW: polymer dispersions, nano-silica and zeolite NPs; OF2i: hydroxyapatite and ceramic NPs; TUS: silica, ceramic NPs, polymer dispersions). Importantly, critical phases of different industrial processes have been distinguished. The monitoring of the evolution of particle size in the nano scale has for some cases been demonstrated and for others measures to achieve this have been identified and are currently being implemented. These achievements are supported by the effective utilisation of appropriate reference technologies. The traceability of the OF2i system has been greatly strengthened. The PDW and TUS probes, in the absence of specific national or European guidelines dedicated to inline nano characterisation, have been referenced by methods according to the requirements of the industrial processes and in accordance with guidelines for offline methods such as the OECD Test Guideline no. 125. Additionally, the specifications for upscaling the use cases have been defined.
The instrument hardware and measurement capabilities along with their software and documentation have been better adapted to the needs of the industrial partners on the basis of intensive pilot scale testing. The selected wavelengths and the dimensions of the PDW probe have been optimised. The OF2i technology has taken a major step towards sample-independent equipment validation routines and the stability of the measuring cell has been increased to deal with air bubbles. Also, the software has been expanded for nanoparticles with higher refractive indices. The hardware and software of the TUS system has been successfully modified to enable automatic dilution and demonstrated the potential for feedback control during the electroplating process. (WP2, WP3, WP4).
ADSC and IRIS have continued the development of a digital platform that stores, combines, and processes the monitoring data of the respective PATs for each case study to achieve maximum data exploitation. The viability for integrating at least two the PAT instruments has been shown. They have also implemented Computational Fluid Dynamics (CFD) studies for the correct location of each of the measuring devices within the case studies and for scale-up procedures later in the project. In two of the cases, the CFD studies have provided recommendations to increase process efficiency. For production of zeolites, the potential for reduction in agitation speed, including a modification of the mixing technology, was demonstrated. For the case of electroplating, the CFD pointed towards an increase in mixing efficiency via changing the inlet position. Many of the studies have yielded valuable information on sensor placement.
A summary of the deployment of the PAT instruments involved in the project (PDW, TUS, OF2i) in the five case studies has been generated. This includes a statement of each end user commenting on the suitability of each PAT for their case study. This deliverable aims to inform the public about the current state of the project, emphasising the potential impact the knowledge and technology transfer of NanoPAT may have on large industrial companies and, therefore, the European economy (WP6).
