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CNT-Nanostickers Report Summary

Project ID: 659001
Funded under: H2020-EU.1.3.2.

Periodic Reporting for period 1 - CNT-Nanostickers (Anisotropic High-Density Carbon Nanotube Coatings for Thin-Film Electronics)

Reporting period: 2015-07-01 to 2017-06-30

Summary of the context and overall objectives of the project

This project lays the foundation of a technology to produce thin-films made of molecules called Carbon Nanotubes (CNTs). As the name suggests, Nanotubes have a tubular shape; they are flexible, light and excellent electronic conductors. These features make them ideal candidates for engineering new materials for electronic applications where weight and flexibility are crucial, for instance: portable devices or aeroplanes, where a longer travel range could be achieved if using CNT-cables. To be a winner though, CNTs must be arranged into densely-packed and aligned configuration, like bundles or films, so to maximize the number of channels for the flow of electric current.
The first objective of the project is to make a liquid CNTs solution (CNT-ink) which eventually allows aligning CNTs by extrusion. Secondly, the project is a study of the feasibility of a microfluidic nozzle enabling the deposition of aligned CNTs as a film, which is indeed the best mean to convey their properties to a support that can be easily integrated into the production of electronic devices.

Work performed from the beginning of the project to the end of the period covered by the report and main results achieved so far

Months 0 - 6
The project started on two parallel research lines: experiments aiming at making CNT-inks for coating, and the prototyping of coating heads and of a small homemade coater.
A screening of scientific literature allowed selecting the most suitable surfactants for the inks, based on their ability to stick to CNTs and a low toxicity: Sodium dodecyl sulfate (SDS) and Sodium dodecyl benzene sulfonate (SDBS). The ink’s fabrication protocol relied on the exfoliation of CNTs/surfactant solutions in a bath sonicator, followed by a centrifugation step to remove largest CNT clusters.
All coating heads were designed via CAD software and then printed on a chromium mask. The first devices were prototyped by soft-lithography, namely by moulding a polymer (PDMS) on patterned photoresist. The homemade coater was designed on CAD to get a 3D model, then its parts were manufactured in acrylic by laser-cutting and assembled into a frame to fix the PDMS heads for initial evaluation of the coating process.

Months 7 – 12
At concentrations above 1wt.%, CNTs form a nematic liquid crystal, which would be ideal for coating aligned CNTs as it provides high-density and preferential direction. By combining Thermogravimetric and UV-Vis spectroscopy, the applicant measured the concentration of the inks and found a CNT content of 0.05 wt.% after centrifugation, namely too low to expect any CNT alignment. To boost this value, he thus looked at ways to improve the exfoliation yield; first, by processing finer CNTs solutions obtained by ball-milling the feedstock. Yet this route became unpractical due to contamination of the CNTs-solutions by the wear of the system. Secondly, the applicant optimized the ink’s formula and the parameters of the bath-sonicator. The results evidenced a strong increase in yield for inks that have a surfactant’s concentration higher than the Critical Micelle Concentration. A concentration of ~0.1 wt.% could be achieved this time.
Attempts to use the homemade coater showed that the tool was not reliable enough to yield coatings better than those obtained by drop-casting. Also, when the inks were concentrated in a rotary evaporator, they became so viscous that their extrusion causes the catastrophic failure of the PDMS head due to excessive pressure. Still, the efforts provided enough understanding to reconsider some of the project priorities. The host-group hired a post-doc researcher to build an improved version of the coater using a metal frame on a motorized stage. The group also purchased an industrial coater from the company Coatema (Germany).
The viscosity of the ink is due to the larger amount of surfactant compared to that of CNTs in it. The applicant thus implemented a new technique to filter out this excess of surfactant, specifically by centrifuging the ink at a temperature below the surfactant’s Krafft’s point, where micelle’s formation is inhibited. Such solution is original and versatile as it can be extended to other surfactants. At present, these findings are considered for publication.

Months 13 - 18
After year-1, it became clear that making CNT-inks is a complex process often giving inconsistent results, and that the protocols in literature are insufficient. To overcome this challenge, still achieving high-throughput, the applicant assembled a modular setup based on a powerful tip-sonicator (courtesy of Prof. Ian Hutchins at the host-institution) coupled to a flow-thought cell (see figure). A pump recirculates the CNT solution from a reservoir to the cell, in closed loop. The cell’s temperature is stabilized by a chiller. A homogeniser was added in series, so to break CNTs clusters similarly to ball-milling. The setup complies also to tight safety margins, as the applicant built a sound-box around the sonicator and fit it into a fume-hood to avoid the risks of exposure to nanoparticles and of noise induced hearing loss.
Overall, this continuous-flow system greatly increases the through

Progress beyond the state of the art and expected potential impact (including the socio-economic impact and the wider societal implications of the project so far)

This project delivered the following.
- A protocol to make CNT-inks with very reproducible results.
- CNT-inks with a CNT concentration of ~0.1 wt.%, i.e. higher than reported in many scientific works.
- A continuous-flow setup (see picture) to produce inks at high-throughput: 1 litre/day.
- A set of scaling rules for the deterministic production of CNT-ink at high-volume, which is key for manufacturing advanced CNT devices at industrial scale.
- Insights on the challenges to build a coating head for aligning CNTs, which will ground future developments of a coating technology to align CNTs.

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