Objectives

Nano-scaled materials are abundant in different stages of industrial manufacturing and increasingly used in a number of applications from biomedical to packaging, automotive or energy. Physical and chemical properties of these materials are strongly dependent on their size, making the characterisation of mean size, size distribution, and shape of nano-scaled particles a major critical aspect for the quality and efficiency of manufacturing processes. Yet, conventional characterisation technologies still display manifold shortcomings which represents a major innovation obstacle for manufacturers of nanoparticles. In particular, in most cases, they have to be performed via offline testing of sampled materials, which results in very high characterisation times, impossibility of controlling product quality and reliability during the process, as well as higher costs derived from resource-consuming laboratory procedures. The increasingly demanding market for nano-scaled materials and nanoparticles (NPs) due to the need of guaranteeing product quality and regulatory compliance is considered mandatory to stay competitive in the European market and beyond. Consequently, the development of new technologies capable of improving the speed and reliability of nanoparticle characterisation in real-time industrial applications is a major demand of nano-scaled materials producers. The estimated market size for nano-characterisation has been estimated in 573.7 million Euros for 2016, expecting to grow at an expected CAGR of 7.3 % due to the rise of international quality standards for materials.

Tech-Process

While focusing on the most representative chemical production of nano-scaled particles in suspensions, the NanoPAT project will bridge this gap using three novel, complementary real-time in situ particle size characterisation technologies – Photon Density Wave spectroscopy (PDW), OptoFluidic force induction (OF2i) and Turbidity spectrometry (TUS). These technologies will be advanced from the “lab-status” (TRL 4) to a technology demonstration level for inline/online process monitoring at pilot scale in the industrial environment (TRL 6) of the NanoPAT industrial partners. This is accompanied by a simultaneous development of a PAT (Process Analytical Technology) Software Platform for holistic digital process data storage and analysis, in conjunction with process modelling and the development of a Decision Support System (DSS) to fuse the data-rich multi-modal results of the nano-characterisation technologies with the industrial production reality, allowing for a digitalized real-time process and quality control. Having an even broader potential, the validation of the NanoPAT solution will be performed in 5 different complementary application cases in large and small companies for the production of mineral, polymer and conversion of ceramic NPs electrolyte suspensions with different shape and aggregation behaviours.

Importantly, our project will deliver a set of recommendations for standards as well as nanosafety activities to demonstrate the advantage of the inline monitoring approach. To support the roll out of the project results in the NPs processing industries, the project will also cover technical and transversal training activities also used as a vector for cross-fertilization with other related projects encapsulated in a clustering strategy supported by the partners’ involvement in numerous EU networks, like SPIRE, ETPN or NanoSafety Cluster, as well as in synergistic ongoing H2020 projects. In parallel, NanoPAT will develop a number of outreach activities to improve the understanding and acceptance of NP production in Europe among the public.

The project includes a suite of relevant stakeholders along the supply and value chain to prepare the successful deployment of NanoPAT. The NanoPAT consortium consists of 15 partners, representing instrument developers, process data and modelling experts, academic process researchers, industrial processing specialists, as well as innovation and dissemination experts. NanoPAT will intensively contribute to enhancing the innovation capacity of the European nanotechnology sector. It aims at empowering small to large-scale European industrial manufacturers of nano-scaled particles to gain understanding and thus control on the underlying particle formation processes during production. This will enable them to reduce cost (increased space-time-yield, reduced feedstock and energy demand) and to save on time-to-market for product development as well as to increase product quality and consistency.

All in all, the overriding goal of NanoPAT is to deliver three novel, real-time nano-characterisation Process Analytical Technologies (PAT) validated in five different industrial manufacturing environments, including real-time data handling for digital production process monitoring and quality control. This implies that innovating PATs integrated inline (PDW, TUS) or online (OF2i) will be paired with new data-analytical methodologies in order to provide, for the first time, a real-time analysis for manufacturing processes of particles in the nanometre scale with sub minute temporal resolution. By overcoming the current challenges linked to NPs characterisation, and validating new versatile technologies for real-time process monitoring in a variety of sectors, as well as, thanks to complementary transversal activities, NanoPAT will have enduring impacts for significantly improving the manufacturing of nanoparticles.

 

To achieve our goals, a 48-month work plan with the following specific objectives, linked to their specific work packages (WPs) and related key performance indicators (KPIs), which will be used as milestones (MS) for project implementation, have been defined.

Objective 1: To define the specifications of the processes to be monitored via the tailored NanoPAT technologies (WP1)

After an updated state of the art patent and market review, the industrial requirements for each of the five nanoparticles production and conversion processes involved in NanoPAT will be outlined with the support of the reference RTOs. Detailed specifications for each of the innovative in situ nano-monitoring technologies to be coupled with the industrial applications will be confirmed.

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Objective 2: To develop an inline monitoring tool based on PDW Spectroscopy for the real time characterization of polymer dispersions, nano-silica and zeolite NPs (WP2)

Photon Density Wave (PDW) Spectroscopy will be applied to the selected relevant nanoparticles for the inline, real-time monitoring of the concentration and the dimension of the nanosized structures with an expected error of less than 1% of the measured value and a measurement range from 25 nm to 250 μm at concentrations from 0.1% to 50% in less than a minute.

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Objective 3: To develop an online monitoring tool based on OptoFluidic Force Induction (OF2i) for the characterization of hydroxyapatite and ceramic NPs (WP3)

During NanoPAT project, using the combination and usage of microfluidic environments together with highly defined and accurate optical induced forces, the Optofluidic Force Induction (OF2i) based monitoring system will be validated for the characterization of at least two selected case studies (i.e. hydroxyapatite, ceramic nanoparticles suspension in electrolytic solutions/baths), providing information about nanoparticles shape and size. The feasibility of OF2i for the monitoring of nanostructured hydroxyapatite and ceramic nanoparticles within the electrolyte will be confirmed at pilot scale, providing the relevant particle parameters such as size (20-1000nm, depending on particle-system properties) and size distributions (accuracy to be defined within the project WP3), concentration and basic shape information (aspect ratio, under investigation) in real time (characterisation <10sec latency, and <1min including sample dilution latency, depending on sample volume fraction).

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Objective 4: To develop monitoring tool based on Turbidity Spectrometry (TUS) for the nano-characterization of silica, ceramic NPs suspensions in electrolytes and polymer dispersions (WP4).

NanoPAT will validate a turbidity spectrometry (TUS) based technology for the nano-characterization of ceramic NPs suspensions in electrolytes and silica nanoparticles and polymers dispersion. Following the nature of the materials and their refraction index behaviour, simultaneous characterization of the size, size distribution and concentration of the selected nanoparticles will be determined. Its suitability to measure individual diluted particles above 100 nm, as well as the size distribution of agglomerates up to several hundred nm, within less than 5 seconds (including data treatment time) will be demonstrated.

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Objective 5: To deliver a PAT Platform for holistic digital process data storage and analysis (WP5)

NanoPAT will develop a robust data analysis toolkit for gathering, pre-processing, mining and visualising real-time NP synthesis and conversion processes data. The combination of nano-monitoring solutions with a software platform capable of modelling the data obtained will enable operators to optimise production processes. The conditioning of sensors to make them compatible with production line specificities and realisation of the required minor adaptations in the production line are critical steps. Electronics hardware and communication network will be designed and developed for ad hoc data collection and exchange. To this end, over the course of the project, a PAT Platform will centralise the data coming from the nano-characterization technologies improving the monitoring strategies of the NP production industries and providing data-driven tools to boost process efficiency.

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Objective 6: To design innovative data elaboration techniques for PAT applications (WP5)

Using the PAT platform as a hosting system, several data elaboration techniques specifically oriented at enhancing PAT applications will be developed. Advanced data analysis techniques will be provided to allow users to perform accurate and fast evaluation of the data obtained from the monitoring technologies. Data fusion techniques will allow to complement different signals coming from the nano-monitoring technologies as well as other instrumentation and monitoring devices to maximise its use and increase its accuracy while maintaining an adequate cost-efficiency ratio. A decision support system (DSS) based on Expert System will be implemented which embodies data, information and knowledge that can be defined and input by material experts or induced automatically on raw data from empirical testing. Computational Fluid Dynamics (CFD) simulations for each industrial application will be developed to optimise the integration of nano-monitoring systems and other instrumentation in production processes, guaranteeing representativeness of the measurements.

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Objective 7: To set up the most suitable nano-characterization integrated solution for the production of polymer dispersions in DSM (WP6 – Case study 1)

A feasible system not prone to signal saturation for the characterization of highly concentrated polymer dispersions (up to 60 wt%) will be delivered. DSM will perform the pilot-scale monitoring tool demonstration for the monitoring of the particle size and size distributions of relevant polymer dispersions.

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Objective 8: To set up the tailored nano-characterization integrated solution for the production of silica nanoparticles in EVONIK (WP6 – Case study 2)

The most robust and durable monitoring technique designed to resist the extreme pH conditions needed for the silica nanoparticle synthesis will be implemented in EVONIK at a pilot scale unit in a 2 m³ batch size.

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Objective 9: To set up the tailored nano-characterization integrated solution for zeolites production in ARK (WP6 – Case Study 3)

ARKEMA will validate the potential of the continuous, inline nano-characterization tools developed in NanoPAT for the continuous manufacturing of zeolites.

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Objective 10: To set up the tailored nano-characterization integrated solution for the production of nano-hydroxyapatite in FLU (WP6 – Case Study 4)

NanoPAT will demonstrate the feasibility of a high temporal resolution, continuous nano-monitoring tool for the continuous manufacturing of hydroxyapatite (approx.18 tons/year in FLU facilities).

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Objective 11: To set up the combined nano-monitoring technology to the semi-industrial electroplating pilot line in Cnano (WP6 – Case Study 5)

current technology such as sampling, low sensitivity, low specificity, lack of accuracy will be selected for the specific detection of the selected ceramic nanoparticles employed at electroplating pilot industrial scale. Cnano will provide the semi-industrial pilot line that is established in its premises in Athens for the demonstration activities in the framework of NanoPAT reaching TRL6. Two different types of NPs suspensions in electrolytes will be investigated: (SiC, 100nm) and TiO2 (50 nm).

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Objective 12: To maximize the dissemination and innovation of NanoPAT outcomes through Open Innovation to benefit the NanoPAT consortium and the wider European process industry and Academia (WP7, WP8)

A set of measures will be undertaken to establish a positive framework to stimulate the uptake of the NanoPAT innovation. The outcomes in the form of metadata will be shared with other projects and stakeholders. An aim is for active information exchange amongst the key-players in the emerging nano-characterisation technologies with the final goal of promoting a wide diffusion of the know-how acquired during the project that could be applied to many others industrial nano-production.

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Objective 13: To maximize the impacts of NanoPAT, including growth and job creation, via post project industrial commercialisation of the project outcomes (WP8)

The business models for the three nano-monitoring technologies developed in the project, together with the PAT platform will be defined and the value proposition of our NanoPAT innovation will be formulated. The logistics and investments for the industrial implementation of the monitoring processes will be studied. The project knowledge and results will be managed and protected. Business plans and exploitation paths will be elaborated for all Key Exploitable Results (KERs) to map the post-project phase. Business and marketing strategies will be established.

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