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Ultra-versatile Nanoparticle Integration into Organiszed Nanoclusters

Issue 3 - Winter / Spring 2016

This is UNION
UNION Overview
Extending the Formation of Nanoparticle Cluster: From Thermoelectric to Magnetic Building Blocks
Malvern: Monitoring the Assembly Process

This is UNION

UNION is developing nanoparticle assembly techniques to prepare novel hierarchically-ordered nanoparticle clusters as a route to materials with tailored and predictable properties.
Close to the end of the project, the UNION consortium has extended its knowledge and expertise on hierarchically-ordered nanoparticle cluster (NPCs) formation with different functionalities. In addition, and thanks to the excellent control over the syntheses achieved by the partners, UNION research has contributed to the development of a new technology to monitor the colloidal assembly process in situ. 
UNION Overview

Title: UNION - Ultra-versatile Nanoparticle integration into Organized Nanoclusters

Budget: €3,798,053

No. of partners: 8

Start Date: February 2013

End Date: January 2016

Duration: 36 months

UNION main achievements were presented at the E-MRS Fall Meeting from September 16th – 19th 2015 in Warsaw. Our consortium successfully organized the symposium “Hierarchical Assembly of Nano-Scale Building Blocks”, which was very exciting and hugely informative for the PI, PostDocs and PostGrads in the UNION project.

The UNION materials, processes and models featured strongly. Hot topics in assembly that we covered included
  • Mechanisms and strategies for the preparation of nanoparticle clusters and 1D, 2D and 3D nanoparticle assemblies.
  • Modelling of nanoparticle self- and directed-assembly
  • In-situ characterization of nanoparticle assembling
  • Characterization of nanoparticle assemblies
  • Modelling optical and transport properties of nanoparticles assemblies
  • Use and integration of nanoparticle assemblies in biomedical, energy conversion and storage, optoelectronic, photonic, and other relevant applications
  • Scale-up of nanoparticle synthesis and assembly processes

Image courtesy of European Materials Research Society (E-MRS).

The symposium ran over three days and attracted was well attended throughout, we had over 200 registered attendees. Prominent invited speakers included: Prof. Willem K. Kegel, Utrecht University; Prof. Andrey Rogach, City University of Hong Kong; Prof. Massimo Morbidelli, ETH Zurich; Prof. Marco Lattuada, University of Freiburg; Prof. Alesio Zaccone, Technische Universität München; Prof. Alexander Govorov , Ohio University; Prof. Antonios Kanaras, University of Southampton; Prof. Stefano Sacanna , New York University; Prof. Bartosz A. Grzybowski, Ulsan National Institute of Science and Technology; Prof. Maksym Kovalenko, ETH Zurich & EMPA; Prof. Beatriz Hernández-Juárez, IMDEA & Universidad Autónoma de Madrid; Prof. Erik Reimhult, University of Vienna; and Prof. Alexander Bittner, CIC nanoGUNE.
Extending the Formation of Nanoparticle Cluster: From Thermoelectric to Magnetic Building Blocks

Within the scope of the UNION project, IREC, in close collaboration with the other UNION partners, has been investigating “bottom-up” assembly methods for the production of nanoparticle clusters. One area that shows great promise are micelle-assembly methods, in which NPs in non-polar solvents and surfactants in an aqueous solution are mixed to form an emulsion solution comprised of nano-micelles. Solvent evaporation and subsequent micelle collapse lead to the eventual formation of spherical NPCs.

IREC has tested several assembly methods, utilizing quaternary ammonium salts (DTAB & CTAB) in which nanomicelles are destabilized in the presence of ethylene glycol and polyvinylpyrrolidone or water to create densely-packed, spherical NPCs. NPCs comprised of Fe3O4 magnetic nanoparticles were also produced that while somewhat polydisperse, exhibit lattice alignment and spatial arrangement within the individual clusters. The development of binary/multicomponent NPCs is also underway, with the production of PbS:PbSe and PbSe:PbTe NPCs for thermoelectric applications. It is now possible to create spherical NPCs with control over composition and a degree of control over NPC size as well.

Figure 1. (Left) TEM image of PbS-PbSe binary NPCs produced by DTAB-micelle method (Right) SEM image of PbS-PbSe binary NPCs produced by DTAB-micelle method.

IREC have also been working on micelle-assembly methods using amphiphilic polymers (Pluronic F127 & P123) to produce magnetic NPCs. NPCs have been created using iron oxide (Fe3O4) magnetic NPs which are spherical and well-formed. Utilization of a magnetic field during the assembly seems to result in spherical NPCs with greatly narrowed size distribution and lattice alignment of the component NPs within the NPCs. Efforts to decrease the size distribution of the resulting NPCs and incorporation of multiple types of nanoparticles (Fe3O4, CdSe, Au) will result in the creation of multifunctional NPCs for the field of biomedicine. The magnetic, magnetic resonance and hyperthermic properties of these materials will be characterized at DCU over the final month of the project.

Figure 2. TEM images of Fe3O4 hexagonal NPCs 

We have also been able to produce hexagonal NPC clusters by utilizing a novel emulsion/assembly method. The NPCs order well on TEM grids and exhibit lattice alignment of the component NPs as seen previously with spherical NPCs. For the remainder of the UNION project, IREC will be focusing on the development of these hexagonal NPCs, micelle-assembly methods with amphiphilic polymers, and the production of binary NPCs utilizing these methods.    
Malvern: Monitoring the Assembly Process

Within UNION, Malvern’s main focus is monitoring the assembly process associated with the formation of nanoparticle clusters. Malvern aim to develop novel in situ light scattering technologies for monitoring assembly at 10-200 mL scale. The ability to monitor the assembly process will directly feed into the cluster assembly modelling work package which aims to build on knowledge of nanoparticle interactions through controlled aggregation. From the collaboration Malvern hope to develop these technologies for a range of applications and in the future potentially incorporate this into their product range.

Over the past months Malvern have been making good progress on the new technologies and are at a stage of sending instruments out to the partners within UNION. Malvern have developed a probe to monitor the growth of the NPCs utilising a number of the current technologies associated with the current range of Zetasizer products. The patented non-invasive backscatter (NIBs) angle of detection has been maintained which extends the concentration limits of detection and allows for direct comparisons to be made with measurements previously performed on Zetasizer instruments. Having utilised a number of components from the current range of products Malvern were able to design the probe to be interfaced with the current version of software and subsequently allow direct comparisons to be made with current instrumentation and previous results obtained by the partners.


Figure 3. 3D model of probe showing NIBs angle of detection and incorporation of optical temperature sensor into the probe. Probe is mounted on external cell holder allowing for size measurements to be taken using 12 mm cuvettes.

New additions include an optical temperature probe allowing the user to directly measure the sample temperature and the inclusion of two different lasers; a 635 nm laser for alignment purposes and an 830 nm high power laser for measurement. The optical temperature sensor has a separate touchscreen mounted at the front of the instrument to allow for instant temperature monitoring, trend measurements, recording (via on board SD card) and alarm functions to identify significant fluctuations in temperature.

Figure 4.  Image showing the current progress of the UNION instrument and probe.

Two instruments have now been completed, with one staying in Malvern for further development and the second having been recently installed at DCU. Current development opportunities within the UNION project for the probe instrument include investigating a range of vessels and probe heads that may be utilised by the instrument. During the remainder of the project Malvern will work closely with the partners to further develop the probe and subsequently improve our understanding of the assembly processes.  
This project has received funding from the European Union’s Seventh Framework Programme for research, technological development and demonstration under grant agreement no 310250.
For Further Information:

UNION Coordinator

Dr. Dermot Brougham
School of Chemical Sciences
Dublin City University
Dublin 9,

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