The University of Nottingham Nanotechnology and Nanoscience Centre (NNNC)
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[4] and analyse the size and morphology of soot The University of Nottingham particles from diesel engines to mention but a few Nanotechnology and examples [5]. Nanoscience Centre (NNNC) The FEGTEM is complemented by the FIBSEM, which is used for the preparation of electron transparent lamellae by site-specific thinning and There are four members of staff, Emily Smith The Nottingham Nanoscience and lift-out using an Omniprobe. The FIBSEM is also (XPS), Dr. Peter Milligan (Business Development), Nanotechnology Centre is located used for the imaging and EDX analysis of a range Dr. Mike Fay (TEM/FIBSEM, EM suite manager) and in the heart of the University of soft and hard materials. In particular, the FIBSEM Dr. Chris Parmenter (FIBSEM/Cryo (SEM/TEM), Park campus and boasts a wide is equipped with a Quorum 2000 PPT cryo-stage, with responsibility for the everyday running of which enables the preservation of delicate hydrated range of microscopes and other the Centre. The NNNC is led by a director and a samples in a near-native state. analytical instruments. The management board of academic advisors. In August Centre’s Dr Chris Parmenter 2013, Prof. Clive Roberts, the Centre’s inaugural Reconstruction of gold nanoparticles in a graphitic nanofibre, by dark field tomography [3]. For example, the CryoFIBSEM has been used for director, became Head of the School of Pharmacy guides us through their catalogue the imaging of diatoms in their native states, being and Prof. Andrei Khlobystov was appointed as the holder for performing electrical measurements; and and highlights some of their of interest to researchers in the Department of a gas-cell reaction holder. The FEGTEM also features applications to date. new NNNC director. a full complement of digital cameras and detectors, The Centre has two electron microscopes, a JEOL for bright and dark field STEM, electron energy loss 2100F field emission gun TEM (FEGTEM) and an FEI spectroscopy (EELS), energy filter (GIF) and energy Quanta 200i 3D FIBSEM with a range of holders and dispersive X-ray (EDX) analysis. stages. The JEOL 2100F is equipped with single and double tilt holders, a rotational holder, and a high JEOL 2100F TEM is utilised for imaging molecules, tilt tomography holder which has been configured nanoparticles and individual atoms entrapped inside for automated image acquisition in conventional carbon nanotubes which play a role of miniature −21 diffraction contrast, high angle angular dark field test tubes with zeptoliter (10 litre) internal HRTEM micrograph of soot extracted from a diesel engine [5]. (HAADF) and scanning transmission electron volume. TEM enables investigation of structures and microscopy (STEM) modes. Additional holders dynamic behaviour of molecules confined in the Geography working on environmental science / include a Gatan cryo-holder for cryo-TEM or the nano test tubes, in real space and time, revealing ecology projects. Typically, diatoms are prepared The Nottingham Nanotechnology and Nanoscience Centre, on the investigation of temperature sensitive samples; a some unique physical and chemical phenomena that University Park campus. from a body of water, from which they can be heating holder (up to 1000 °C) for studying high can only emerge at the nanoscale. For example, concentrated, dried and the organic remnants temperature processes in situ; a scanning transmission chemical reactions can drastically change their The NNNC, opened six years ago by Nobel removed using acid to leave silicate shells. However, electron beam induced conductivity (STEBIC) mechanisms and pathways inside nanotubes leading Laureate Professor Sir Harry Kroto, was established this approach effectively throws away the biological to new unexpected products, such as graphene by the Schools of Chemistry, Pharmacy, Physics & parts of the diatom, including the internal cellular nanoribbons and unusual polymers, inaccessible Astronomy and the Faculty of Engineering, with a material and the external biofilms. Use of the FIBSEM by any other means. Carbon nanotubes hold the £3.2m SRIF3 investment, to serve the University of cryo-stage allows the stabilisation and preservation record for the World’s tiniest test tube since 2005, Nottingham’s diverse engineering, physical and life of organic components, whilst FIB has been used to and our latest work at the NNNC may prove them sciences research portfolio. The NNNC acts as a reveal the internal diatom structures. EDX mapping to be the World’s tiniest chemical reactors [1,2]. hub for nano and micro-scale research, is open to all, allowed the silicon and oxygen of the silicate shell To date the TEM has been used to gain tomographic and works closely with both academic and industrial to be distinguished from carbon representing the data of nanoparticles on carbon nanotubes [3] researchers in areas ranging from nanostructured diatom single-cell content and surface biofilm. , observe the real-time growth of particles of carbons and catalysts to aerospace materials and iron oxide produced by hydrothermal synthesis Snapshot from the observation of Fe O nanorod growth [4]. drug delivery systems. 2 3 34 ISSUE 31 SEPTEMBER 2013 35 investigation of ionic liquids. This opens up a wide Poliakoff and filmmaker Brady Haran (Periodic range of new experimental options for investigation. videos) to engrave the image of the queen onto a The original Al-source XPS has always been heavily layer of diamond. used by researchers across campus. Siting both instruments within the same laboratory in the The NNNC regularly hosts visits from students NNNC provides a useful focal point for all XPS on the ‘seeing the un-seeable’ programme, in users in the future. conjunction by the School of Physics & Astronomy. Dr Mike Fay regularly provides outreach sessions In 2012, the NNNC invested in an Avizo Fire for schools, science fairs and education centres. 3D imaging and analysis package from VSG. This software supports the interpretation of data Future Collaborations from the TEM and FIBSEM, whilst also being The staff at the NNNC are always open to useful for X-ray tomography, positron emission collaboration with researchers in both academia tomography (PET) and magnetic resonance imaging and industry and regularly collaborate on one-off, (MRI) investigations, all of which are available at short and longer term research projects with those who want to make use of the facility. Micrographs of a diatom before and after outer layer removal by using a FIB, followed by EDX analysis, Oxygen (red), Silicon (blue), Carbon (yellow) the University. maps shown. If you would like more information on the centre, Outreach Cryogenic preservation can be achieved in a number situated in the School of Chemistry, was moved are interested in using the facilities or would like The NNNC has been involved in a number of of different ways dependent on the nature of the to a newly refurbished laboratory in the NNNC to propose some exploratory work with them, outreach projects including ‘NanoWhat?’ and sample. For CryoFEGTEM investigations, samples in May 2013. This was joined in August 2013 by a please go to http://www.nottingham.ac.uk/NNNC ‘Let Nano Fly’ (a Nano-aerospace programme). up to ~ 500 nm in thickness may be stabilised by new instrument, a Kratos Axis Ultra with a silver or contact Dr Peter Milligan, peter.milligan@ The NNNC has taken part in the creation of rapid plunging into liquid ethane using the NNNC‘s monochromated X-ray source (~3000 eV) and a nottingham.ac.uk or 0115 84 67729. a number of educational videos for both the Gatan CP3. This approach has facilitated the study bespoke sample stage for the in situ electrochemical Periodic Tables Videos and the Sixty Symbols References of vesicles and polymer-DNA conjugates of interest investigation of ionic liquids. series, including the imaging flakes of snow and [1] W.A. Solomonsz, G.A. Rance, M. Suyetin, A. La to researchers from Engineering and Pharmacy. the writing of ‘Merry Christmas’ on a snowflake Torre, E. Bichoutskaia, A.N. Khlobystov, Controlling Preparation of larger samples may be performed The new silver source XPS provides information (http://www.youtube.com/watch?v=_hcp5NT0AyI). the Regioselectivity of the Hydrosilylation Reaction by vitreous sectioning, using an RMC Powertome to greater sampling depths than the conventional The NNNC now hold two Guinness World in Carbon Nanoreactors, Chem. Eur. J., 2012, 18, and diamond knife, facilitating TEM analysis under aluminium source XPS (because the excited records, for the smallest Periodic Table (http://www. 13180-13187. cryogenic conditions. Samples may also be prepared electrons are moving faster), whilst providing youtube.com/watch?v=cQU2IAsQak8), and the [2] W. Chamberlain, J. Biskupek, G.A. Rance, A. by metal mirror freezing, using a Leica MM80, or by information content from electron orbitals which smallest advertisement (http://www.youtube.com/ Chuvilin, T.J. Alexander, E. Bichoutskaia, U. Kaiser, sucrose infiltration followed by plunging into liquid otherwise would be unexcitable. For example, watch?feature=player_embedded&v=SfAo1saSLJ0), A.N. Khlobystov, Size, Structure, and Helical nitrogen. Metal mirror freezing has also been used the interpretation of complex peak structures to both of which were written onto human hair. Twist of Graphene Nanoribbons Controlled by to stabilise samples for Cryo-SEM or Cryo-FIBSEM determine oxidation states is of great importance Following these records, the NNNC was contacted Confinement in Carbon Nanotubes, ACS Nano, investigations.