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Surface Modification and Analysis Wednesday 15 th October 2014, Ricoh Arena Coventry Lounge One South 09:15 Welcome & Introduction : Prof John Colligon, The University of Huddersfield SESSION 1 Chair: Dr Alison Crossley 09:30 Structure-property relationships in submicron thin films Steve Bull, School of Chemical Engineering and Advanced Materials, Newcastle University 10:00 A study of nanoparticle biomolecular coatings by XPS and particle sizing techniques Caterina Minelli, National Physical Laboratory 10:30 - Coffee break – SESSION 2 Chair: Dr Andrew Thomas 10:50 Every atom counts: Manipulation of single functional molecules on surfaces Leonard Grill, Chemistry Department, University of Graz, Graz, Austria 11:20 Atomic Layer Deposition: a process technology for functional ultra-thin films Paul Chalker, School of Engineering, University of Liverpool SESSION 3 Chair: Dr Alan Webb 11:50 2 Minute Poster Presentations 12:10 Lunch / Exhibition / Posters 13:45 IOP Vacuum Group members AGM (Annual General Meeting) SESSION 4 Chair: Steven Schofield 14:00 Interpretation of scanning tunnelling spectroscopy of semiconductor nanostructures 1
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Page 1: Surface Modification and Analysis - VACUUM SYMPOSIUMAtomic Layer Deposition: a Process Technology for Functional Ultra-Thin Films Paul Chalker School of Engineering, University of

Surface Modification and Analysis

Wednesday 15th October 2014, Ricoh Arena Coventry Lounge One South

09:15 Welcome & Introduction : Prof John Colligon, The University of Huddersfield

SESSION 1 Chair: Dr Alison Crossley 09:30 Structure-property relationships in submicron thin films

Steve Bull, School of Chemical Engineering and Advanced Materials, Newcastle University

10:00 A study of nanoparticle biomolecular coatings by XPS and particle sizing techniques Caterina Minelli, National Physical Laboratory

10:30 - Coffee break –

SESSION 2 Chair: Dr Andrew Thomas 10:50 Every atom counts: Manipulation of single functional

molecules on surfaces Leonard Grill, Chemistry Department, University of Graz, Graz, Austria

11:20 Atomic Layer Deposition: a process technology for functional ultra-thin films Paul Chalker, School of Engineering, University of Liverpool

SESSION 3 Chair: Dr Alan Webb 11:50 2 Minute Poster Presentations 12:10 Lunch / Exhibition / Posters 13:45 IOP Vacuum Group members AGM (Annual General

Meeting)

SESSION 4 Chair: Steven Schofield 14:00 Interpretation of scanning tunnelling spectroscopy of

semiconductor nanostructures

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Page 2: Surface Modification and Analysis - VACUUM SYMPOSIUMAtomic Layer Deposition: a Process Technology for Functional Ultra-Thin Films Paul Chalker School of Engineering, University of

Philipp Ebert* and Holger Eisele+, *Peter Gruenberg Institut, Juelich, Germany, +Technical University, Berlin, Germany

14:30 Atomic force microscopy at the picometer length scale Alfred J. Weymouth and Franz Giessibl, Institute of Experimental and Applied Physics, University of Regensberg, Germany

15:00 Production of superconducting coatings Reza Valizadeh, STFC Daresbury Laboratory, Daresbury, UK

15:30 Tea break / Exhibition / Poster Prize Presentation in Exhibition Hall

SESSION 5 Chair: Professor John Colligon 16:00 A layman’s view of ion-surface modelling

Roger Smith, Computing Science, Loughborough University, UK

16:30 Lost image recovery for stained glass panels from the Rosslyn Chapel C. Jeynes, A. Hamilton1, G.W. Grime, V.V. Palitsin, L. Antwis, R.P.Webb, M. Bambrough2 University of Surrey Ion Beam Centre, Guildford, UK. 1Department of Civil and Environmental Engineering, University of Strathclyde, Scotland 2Scottish Glass Studios, Glasgow, Scotland

SESSION 6 17:00 10 minute short Contributed papers. (titles

to [email protected]) 18:00 - End of meeting -

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Page 3: Surface Modification and Analysis - VACUUM SYMPOSIUMAtomic Layer Deposition: a Process Technology for Functional Ultra-Thin Films Paul Chalker School of Engineering, University of

Functional Thin Films

Thursday 16th October 2014, Ricoh Arena, Coventry Lounge One South

09:45 - Registration in foyer and refreshments in meeting room - 10:15 Welcome and introduction

Dr Andrew Clayton, Glyndwr University

SESSION 1 Chair: Dr James McGettick INVITED SPEAKER 10:20 Rapid optimisation techniques for thin-film materials and

devices Dr Robert Treharne, Stephenson Institute for Renewable Energy (SIRE), University of Liverpool, UK

10:50 In-line metal organic chemical vapour deposition process for solar cell production Dr Vincent Barrioz, Centre for Solar Energy Research, Glyndwr University, UK

11:10 Advanced functional coatings using HIPIMS Holger Gerdes, Fraunhofer Institute for Surface Engineering and Thin Films IST

11:30 - Refreshment break –

SESSION 2 Chair: Dr Russell Binions INVITED SPEAKER 11:50 Solution processed Perovskite solar cells via scalable

methods Dr James McGettick, Sustainable Product Engineering Centre for Innovative Functional Industrial Coatings, University of Swansea, UK

12:20 Smart thin films for micro actuation, microfluidics and lab-on-chip applications Dr Richard Fu, Thin Film Centre, University of West Scotland, UK

12:40 Ionized Jet Deposition – a new class of thin film deposition Dr Petr Nozar, Noivion srl, Italy 13:00 POSTER SESSION and – Lunch break -

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Page 4: Surface Modification and Analysis - VACUUM SYMPOSIUMAtomic Layer Deposition: a Process Technology for Functional Ultra-Thin Films Paul Chalker School of Engineering, University of

Delegates are encouraged to visit the exhibition during lunch, the poster session will be held in the exhibition area. SESSION 3 Chair: Dr Robert Treharne INVITED SPEAKER

14:30 Advances in Thermochromic Vanadium Dioxide thin films Dr Russell Binions, School of Engineering and Materials Science, Queen Mary University of London, UK

15:00 New Agilient Cary 7000 Universal Measurement Spectrophotometer for Analysis of Thin Film Coatings Rob Wills, Agilent, UK

15:20 Abnormal photovoltaic effects in ferroelectric materials and multiferroic tunnel junctions Prof Marin Alexe, Department of Physics, Warwick University, UK

15:40 16:00

Laser printing of organic light-emitting diode pixels by LIFT Dr James Shaw-Stewart, Faculty of Business, Environment and Society, Coventry University, UK Closing Remarks

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Page 5: Surface Modification and Analysis - VACUUM SYMPOSIUMAtomic Layer Deposition: a Process Technology for Functional Ultra-Thin Films Paul Chalker School of Engineering, University of

Contamination Control, Cleaning and Surface Preparation for Vacuum Applications

Thursday 16th October 2014, Ricoh Arena, Coventry, Jaguar Suite

10:00

SESSION 1 Chair: Joe Herbert An Introduction to 'Contamination Control, Cleaning and Surface Preparation for Vacuum Applications' Joe Herbert, ASTeC Vacuum Group, STFC Daresbury Laboratory

10:15 Concerned about the upcoming sunset date for Trichloroethylene Mark Duggan, Acota Ltd, Shrewsbury

10:35 Surface Cleaning with Gas Cluster Ion Sources Tim Nunney, Thermo Fisher Scientific

10:55 Developing cleaning for XHV at Daresbury Keith Middleman, ASTeC Vacuum Group, STFC Daresbury Laboratory

11:15 - Coffee break in the Exhibition Hall - (15 minutes) SESSION 2 Chair: Joe Herbert

11:30 RGA's for Vacuum Diagnostics and Outgassing Measurements Dr. Guenter J Peter, Inficon Ltd., Balzers, Liechtenstein

11:50 Case Study Stephen Fletcher, X-Tek Systems Ltd., Nikon

12:10 Vacuum Cleanliness in the Semiconductor Industry Alan Webb, Consultant

12:30 Vacuum Support, whatever that might be? Tom Weston, STFC Daresbury Laboratory

12:50 - Meeting close -

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5th Vacuum Symposium UK Training Sessions

Our specialist trainers, Dr Austin Chambers & Dr Ron Reid will deliver two training seminars on each day as follows:

VTC1 Vacuum – the basic Principles 10:30 – 12:30 This course will deal with the principals involved in creating and maintaining a vacuum.

VTC2 Vacuum in Practice 14:30 – 16:30 The subject of this course is how vacuum is proceeded and measured in a few typical devices whose operation reflects the application of the principles described in the VTC1 course.

VTC3 Clean vacuum and UHV 14:30 – 16:30 The course is primarily aimed at those who need to use equipment operating at vacuum levels of 10-9 mbar or lower and is approached mainly from the physics aspects of vacuum science.

Note: VTC3 is only being run Thursday afternoon and clashes with VTC2 which is being held at the same time. If you want to attend both VTC2 & VTC3 you must book VTC2 on Wednesday PM, and VTC3 on Thursday PM.

If you have not already reserved a place please check at the front desk for availability.

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Surface Modification and Analysis

Wednesday 15th October 2014 - Lounge One South

Meeting Agenda

0915 – 0930 Welcome

0930 – 1030 Session 1

1030 – 1050 Refreshment Break

1050 – 1150 Session 2

1150 – 1400 Session 3 including Lunch

1400 – 1530 Session 4

1530 – 1600 Refreshment Break inc. Poster Prize Presentation

1600 – 1700 Session 5

1700 – 1800 Session 6

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Page 8: Surface Modification and Analysis - VACUUM SYMPOSIUMAtomic Layer Deposition: a Process Technology for Functional Ultra-Thin Films Paul Chalker School of Engineering, University of

Structure-Property Relationships in Submicron Thin Films

Steve Bull School of Chemical Engineering and Advanced Materials, Newcastle University, Newcastle Upon Tyne, NE1 7RU, UK In most coating applications damage resistance is controlled by the mechanical properties of the coating, interface and substrate. However, for electronic and optical applications the design of coating-substrate systems has been predominantly controlled by their functional properties except in a few cases where the mechanical response of the system has been used to enhance functional properties. As coatings become thinner and more complex, with multilayer and graded architectures now in widespread use, it is very important to obtain the mechanical properties (such as hardness, elastic modulus, fracture toughness, etc.) of individual coating layers for use in design calculations as a function of process parameters and have failure-related design criteria which are valid for such multilayer or multicomponent systems. This presentation will discuss the assessment of the mechanical properties of very thin coatings used in electronic and optical coatings as a function of processing and how these may be used for mechanical design of functional devices. Single, multilayer, superlattice and nanocomposite coating architectures will be considered and the role of grain size, shape and orientation in the mechanical response of coatings and nanostructures will be highlighted.

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Page 9: Surface Modification and Analysis - VACUUM SYMPOSIUMAtomic Layer Deposition: a Process Technology for Functional Ultra-Thin Films Paul Chalker School of Engineering, University of

A Study of Nanoparticle Biomolecular Coatings by XPS and Particle Sizing Techniques Caterina Minelli National Physical Laboratory, Teddington, UK

The intentional and unintentional attachment of molecules, e.g. proteins, to nanoparticles’ surface is of increasing interest in medicine for applications such as drug delivery and diagnostics. Understanding and refinement of the performance of nanoparticle products require accurate and quantitative characterisation of their interface. Our efforts are focussed upon developing measurement methods to enable useful characterisation of this biomolecular interface. We show that parallel characterisation of nanoparticles in their colloidal form and in vacuum provides consistent results and reveals farther insight into nanoparticles’ molecular interfaces. The complementarity of the approaches also allows for validation of the methods, which is important for their application to a wide range of nanoparticle types. For example, dynamic light scattering and localised surface plasmon resonance analysis are not suitable for dealing with aggregated samples, but X-ray photoelectron spectroscopy (XPS) is, while XPS measurements of organic nanoparticles are challenging and liquid based techniques may be preferred.

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Page 10: Surface Modification and Analysis - VACUUM SYMPOSIUMAtomic Layer Deposition: a Process Technology for Functional Ultra-Thin Films Paul Chalker School of Engineering, University of

Every Atom Counts: Manipulation of Single Functional Molecules on Surfaces Leonhard Grill Department of Physical Chemistry,University of Graz, Austria

Functional molecules on surfaces and their assembly into pre-defined architectures are key challenges in nanotechnology and of interest in various fields from molecular electronics over novel materials to molecular machines. Furthermore, they provide detailed insight into fundamental physical and chemical processes. Various examples of functional molecules, studied by scanning tunneling microscopy under ultrahigh vacuum conditions will be discussed. Specifically designed molecular building blocks are connected to two-dimensional networks or one-dimensional chains [1], which can for instance act as molecular wires [2].

The focus of this presentation will be on the challenge how chemical processes within individual molecules can be controlled via their local environment. Such a phenomenon was observed for molecular switches, where the atomic-scale surroundings cause drastic changes in their switching probability, resulting in periodic switching patterns [3]. Recently, we could show that the rate of an intramolecular hydrogen transfer reaction can be tuned up and down by single atoms in the vicinity of the molecule [4]. This effect can even be extended to molecular assemblies where cooperativity effects are then imaged in real space via the modification of the switching rates in each individual molecule.

[1] L. Lafferentz et al., Nature Chem. 4, 215 (2012); [2] M. Koch et al., Nature Nanotech. 7, 712 (2012); [3] C. Dri et al., Nature Nanotech. 3, 649 (2008); [4] T. Kumagai et al., Nature Chem. 6, 41 (2014).

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Page 11: Surface Modification and Analysis - VACUUM SYMPOSIUMAtomic Layer Deposition: a Process Technology for Functional Ultra-Thin Films Paul Chalker School of Engineering, University of

Atomic Layer Deposition: a Process Technology for Functional Ultra-Thin Films

Paul Chalker School of Engineering, University of Liverpool, Liverpool

Atomic layer deposition (ALD) is a thermo-chemical process, which exploits sequential cycles pulsed precursor reagents are onto a heated substrate to deposit thin films layer-by-layer. As the process occurs on the surface and is self-limiting, highly uniform and conformal layers can be deposited with ultra-precise thickness control, even onto high-aspect ratio or porous materials.

A brief introduction of the process parameters required for ALD growth will be presented. Then the application of ALD to the manufacture of ultra-thin functional films in power electronics and thin film solar cells will be discussed. Finally the prospects for the wider applications of ALD will be considered.

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Page 12: Surface Modification and Analysis - VACUUM SYMPOSIUMAtomic Layer Deposition: a Process Technology for Functional Ultra-Thin Films Paul Chalker School of Engineering, University of

Interpretation of Scanning Tunnelling Spectroscopy of Semiconductor Nanostructures Philipp Ebert1 and Holger Eisele2 1 Peter Grünberg Institut, Forschungszentrum Jülich, 52425 Jülich Germany, 2 Institut für Festkörperphysik, Technische Universität Berlin, Hardenbergstr. 36, 10623 Berlin, Germany

Optoelectronic properties of semiconductor materials often improve with reduced spatial size. For example, state of the art bright light emitters are nowadays almost exclusively based on two-dimensional thin layers, but three-dimensional nanostructures increasingly attract interest. Particular promising are semiconductor nanowires, which exhibit diameters down to a few tens on nanometers with lengths of micrometers. Scanning tunneling microscopy (STM) is an excellent choice to characterize the structural and electronic properties and the sidewall surface of nanowires. However, the interpretation of spectroscopic data measured by STM on semiconductor surfaces is a rather difficult task, which in the past led to many wrong conclusions about the underlying properties. For example, unlike in metals, tunneling spectra of semiconductors may probe in certain cases empty conduction band states only, but no filled valence band states [1]. Hence it is critical to identify and describe the main physical effects occurring during tunneling spectroscopy of semiconductors and their nanostructures. Among other examples, we will illustrate the interpretation of tunneling spectra using the example of zincblende (ZB)-wurtzite (WZ) GaAs nanowires, where the band structure and the Fermi level pinning at clean and well-ordered sidewall surfaces is investigated and extracted by scanning tunneling spectroscopy [2]. We show how a potential change can be determined and demonstrate the presence of a p-i junction at the WZ-ZB phase transition in GaAs nanowires at the sidewall surfaces.

[1] Ph. Ebert, L. Ivanova, and H. Eisele, Phys. Rev. B 80, 085316 (2009). [2] P. Capiod, T. Xu, J. P. Nys, M. Berthe, G. Patriarche, L. Lymperakis, J. Neugebauer, P. Caroff, R. E. Dunin-Borkowski, Ph. Ebert, and B. Grandidier, Appl. Phys. Lett. 103, 122104 (2013).

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Page 13: Surface Modification and Analysis - VACUUM SYMPOSIUMAtomic Layer Deposition: a Process Technology for Functional Ultra-Thin Films Paul Chalker School of Engineering, University of

Atomic Force Microscopy at the Picometer Length Scale

Alfred J. Weymouth and Franz J. Giessibl

Institute of Experimental and Applied Physics, University of Regensburg, Universitätsstrasse 31, D-93053 Regensburg,Germany ,

Why did it take so long for the AFM to catch up to the STM? The spatial resolution that can now be achieved is the result of years of steady advancements. One step was the switch to a frequency-modulation mode, allowing non-contact AFM greater sensitivity to short-range interactions [1]. A second step was the adoption of stiff cantilevers, making controllable small oscillations possible. Most recently, characterization and control of the tip apex at the atomic level make it possible to select inert tips that can be used to approach surfaces and adsorbates at distances where their internal structure can be visualized [2]. We have used these techniques to look at a range of surfaces from reactive silicon surfaces [3] to inert graphene. Furthermore, we have started to take everything that we have learned from a vacuum environment and to apply it to ambient conditions, where we have demonstrated atomic resolution on KBr [4] and on graphene [5] in a table-top setting.

[1] T.R. Albrecht, P. Grütter, D. Horne, D. Rugar. 69, 668 J. Appl. Phys. (1991) [2] L. Gross, F. Mohn, N. Moll, P. Liljeroth, G. Meyer. 325, 1110 Science (2009) [3] J. Welker, A.J. Weymouth, F.J. Giessibl 7, 7377 ACS Nano (2013) [4] D. Wastl, A.J. Weymouth, F.J. Giessibl 87, 245415 Phys. Rev. B (2013) [5] D. Wastl, A.J. Weymouth, F.J. Giessibl, 8, 5233 ACS Nano (2014)

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Page 14: Surface Modification and Analysis - VACUUM SYMPOSIUMAtomic Layer Deposition: a Process Technology for Functional Ultra-Thin Films Paul Chalker School of Engineering, University of

Production of Superconducting Coatings

Reza Valizadeh STFC Daresbury Laboratory, Daresbury, UK

The production of superconducting coatings for superconducting radio frequency (SRF) cavities is an intensively developing field that should ultimately lead to acceleration gradients better than those obtained by bulk Nb RF cavities. Nb and NbN thin-films were deposited by magnetron sputtering in DC, pulsed DC mode (100 to 350 kHz with 50% duty cycle) and HIPIMS with powers ranging from 100 to 600 W at various temperatures ranging from room temperature to 800 °C on Si (100), Cu and MgO substrates. The films are also deposited by CVD/ALD using NbCl5 at various temperatures ranging from 400 to 1000 °C. The first results gave residual resistivity ratios in the range from 2 to 22 with a critical temperature Tc ≈ 9.5 K. Scanning electron microscopy, x-ray diffraction, electron back-scattering diffraction and DC SQUID magnetometry revealed significant correlations between the film structure, morphology and superconducting properties.

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Page 15: Surface Modification and Analysis - VACUUM SYMPOSIUMAtomic Layer Deposition: a Process Technology for Functional Ultra-Thin Films Paul Chalker School of Engineering, University of

A Layman’s View of Ion-Surface Modelling

Roger Smith School of Science, Loughborough University, Loughborough LE11 3TU, UK This talk will give an overview of the work that has been done over the years modelling the interaction of energetic particle beams with solids from the Boltzmann transport approach of the 1960’s which led to the Thompson and Sigmund models of sputtering, to the present day. In the 1970’s, molecular dynamics computer simulation of sputtering were developed by Don Harrison and his co-workers which allowed a visual representation of the process and the analysis of more complicated systems than those that were accessible by analytical methods. It is this approach that has found much success over the years for modelling the energetic particles from solids.

When the energy of the incoming ions is low, the arriving particles stick to the surface instead of ejecting particles. So thin film growth can also be studied using the same molecular dynamics approach but it is only recently that interactions involving successive particle impacts have been able to be accurately modelled. In this approach molecular dynamics is combined with an on-the-fly kinetic Monte Carlo technique to bridge the disparate time scales so that diffusion between particle impacts can be considered.

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Page 16: Surface Modification and Analysis - VACUUM SYMPOSIUMAtomic Layer Deposition: a Process Technology for Functional Ultra-Thin Films Paul Chalker School of Engineering, University of

Lost Image Recovery for Stained Glass Panels from the Rosslyn Chapel

C. Jeynes, A. Hamilton1, G.W. Grime, V.V. Palitsin, L. Antwis, R.P.Webb, M. Bambrough2 University of Surrey ION Beam Centre, Guilford, UK 1 Department of Civil and Environmental Engineering, University of Strathclyde, Scotland 2 Scottish Glass Studios, Glasgow, Scotland Using Surrey’s in-air scanning focussed 4He++ beam, with a large-range motorised sample manipulator and a high count-rate spectrometry system for both particle and X-ray detectors, we have analysed deteriorated stained glass from Rosslyn chapel (built in 1446). The glass panels were manufactured around 1875 with a “grisaille” technique: the image is defined by Fe-rich monochrome paints fired into the glass. Many panels have suffered extreme image loss due to an aggressive internal environment and this work aims to uncover the lost imagery by revealing the original artists’ paint strokes.

Using Total-IBA (self-consistent ion beam analysis) methods we have demonstrated that the lost grisaille leaves an (invisible) surface enrichment of Fe. The Fe concentration is low, but can be detected and mapped using He-PIXE. We show that the lost image can efficiently be recovered by PIXE (particle-induced X-ray emission) with high acuity, providing invaluable guidance for the restorers and conservators.

This project is partially funded by The Rosslyn Chapel Trust (Registered Charity number SC024324); Lord and Lady Rosslyn, Owners and Trustees and WREN Heritage Fund (www.wren.org.uk)

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Functional Thin Films

Thursday 16th October 2014 – Lounge One South

Meeting Agenda

0945 – 1020 Welcome

1020 – 1130 Session 1

1130 – 1150 Refreshment Break

1150 – 1300 Session 2

1300 – 1430 Poster Session inc. Lunch

1430 – 1600 Session 3

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Page 18: Surface Modification and Analysis - VACUUM SYMPOSIUMAtomic Layer Deposition: a Process Technology for Functional Ultra-Thin Films Paul Chalker School of Engineering, University of

Rapid Optimisation Techniques for Thin-Film Materials and Devices. Dr Dr. Rob Treharne, Ken Durose

Stephenson Institute for Renewable Energy, University of Liverpool, Liverpool. UK

One of the biggest obstacles to the development of new functional thin-film materials is the wide range of parameter space assosiated with any given deposition technique (e.g. temperature, pressure, composition) that must be fully explored to find the optimum conditions for deposition. Here we provide an overview of the combinatorial techniques being used at Liverpool University to dramatically increase the rate at which these parameters are sampled. A case study is presented for the development of high performance transparent conductors for application in thin-film photovoltaics. A full description of the automated, rapid characterisation and analysis tools – that include scanning four point probe, spectrophotometric and ellipsometric techniques - is provided. The key outcome of these combinatorial methodologies is the determination of an almost continuous relationship between material composition and the opto-electric properties (e.g. resistivity, band gap, transport properties). Such data enables materials to be tailored for specific device applications and provides an excellent opportunity for semiconductor device optimisation.

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Page 19: Surface Modification and Analysis - VACUUM SYMPOSIUMAtomic Layer Deposition: a Process Technology for Functional Ultra-Thin Films Paul Chalker School of Engineering, University of

Chamberless coater for flexible thin film solutions

Dr.Vincent Barrioz Centre for Solar Energy Research, Glyndŵr University, St Asaph, LL17 0JD

CSER has developed a unique world-first process to enable chamberless inline deposition of semiconductor layers and thin film PV structures on rigid or flexible substrates, at atmospheric pressure. Safe process gas containment and highly uniform deposition of the resulting films are achieved with a novel balanced flow system. This presentation will give an overview of the semi-automated chamberless inline process developed at Glyndŵr University containing 6 chamberless coating heads and its capability to deposit thin film PV structures, at surface temperatures up to 500˚C (tested so far).

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Page 20: Surface Modification and Analysis - VACUUM SYMPOSIUMAtomic Layer Deposition: a Process Technology for Functional Ultra-Thin Films Paul Chalker School of Engineering, University of

Advanced Functional Coatings using HIPIMS

H. Gerdes, R. Bandorf, G. Braeuer

Fraunhofer Institute for Surface Engineering and Thin Films IST

High power impulse magnetron sputtering (HIPIMS) is the newest

development in the field of physical vapour deposition. This technology is based on a pulsed discharge, where the pulse time of the plasma is short, followed by a long pause time. Within these pulses a very high power density (up to MW/cm2) can be achieved, while the average power delivered to the cathode is comparable to a conventional process. The increased power density lead to a significant influence on the growing film since the plasma is containing more ionized target atoms than in the conventional case.

This contribution will show the effect of HIPIMS for different coatings. In detail the advantages will be discussed on NiCr, TiO2, and ITO. Improved NiCr coatings as strain gauge sensor material show a different thin film growth and a better long term stability. Using HIPIMS for sputtering TiO2 and ITO lead to unique properties like bendable thin film coating and deposition at room temperature. Another application of the HIPIMS technique is the metal ion etching, which lead a better thin film adhesion to the substrate.

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Page 21: Surface Modification and Analysis - VACUUM SYMPOSIUMAtomic Layer Deposition: a Process Technology for Functional Ultra-Thin Films Paul Chalker School of Engineering, University of

Solution Processed Perovskite Solar Cells via Scalable Methods

Dr James McGettrick Sustainable Product Engineering Centre for Innovative Functional Industrial Coatings, Swansea University, UK

Solution processible solar cells remain the focus of considerable research as they offer substantial power conversion efficiencies (PCE) in combination with the opportunity for high-throughput reel-to-reel (R2R) processing and the associated potential for low cost manufacture. Hybrid organic-inorganic perovskite systems that combine an organo lead trihalide light absorber, such as CH3NH4PbI3 or CH3NH4PbI2-xClx, and an organic hole transport material have recently emerged as a viable material route for solution-processible photovoltaic devices. At Swansea University SPECIFIC considerable effort is being made to adopt more scalable methodologies as a precursor to R2R processing. Doctor-blading is one technique analogous to high throughput roll-to-roll techniques, capable of large area coating with reduced raw material usage. Small perovskite devices with power conversion efficiencies as high as 8.55% are produced under ambient conditions, with typical deposition areas of 49 cm2.

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Page 22: Surface Modification and Analysis - VACUUM SYMPOSIUMAtomic Layer Deposition: a Process Technology for Functional Ultra-Thin Films Paul Chalker School of Engineering, University of

Smart Thin Films and Nanostructures for Microactuation, Microfluidics and Biosensing

Richard Yongqing Fu Thin Film Centre, University of West of Scotland, Paisley, UK, PA1 2BE This talk will discuss about recent work on thin film shape memory alloy and shape memory polymer for microactuator applications, as well as piezoelectric ZnO films for acoustic wave-based microfluidics and bio-sensors. TiNi thin film based micro-actuators become the actuator of choice in many aspects in the rapidly growing field of MEMS, microsurgery, and biomedical applications, Different types of TiNi thin film based microdevices, such as microgrippers, microswitches, microvalves and pumps, microsensors are described and discussed. Recently, shape memory polymer and nanocomposites have also been applied in microactuation, microsurgery and tissue and cell applications. Its low cost and non-vacuum preparation method could find wide industry applications. Piezoelectric ZnO film based acoustic wave devices can be successfully used as bio-sensors, based on the biomolecule recognition using highly sensitive surface acoustic waves and film bulk acoustic resonator devices. The acoustic wave generated on the ZnO acoustic devices can also induce significant acoustic streaming, small scale fluid mixing, pumping, ejection and atomization or nebulisation, particle concentration, call manipulation, etc. The potential to fabricate an integrated lab-on-a-chip diagnostic system based on these ZnO acoustic wave technologies is introduced.

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Page 23: Surface Modification and Analysis - VACUUM SYMPOSIUMAtomic Layer Deposition: a Process Technology for Functional Ultra-Thin Films Paul Chalker School of Engineering, University of

Ionized Jet Deposition – a new class of thin film deposition equipment

Dr. Petr Nozar1 and Francesco Vittori2 1CNR IMEM Via alla Cascata, 56/C Povo 38123 Trento, Italy 2Noivion Srl Piazza Manifattura, 1 Rovereto 38068 Trento Italy

A new thin film deposition method – Ionised Jet Deposition (IJD) – based on pulsed energy delivered by sub-microsecond gas jet discharge to the material source (target) is investigated.

This technique belongs to the PVD family and could represent a substantial improvement over conventional techniques, particularly in those fields in which high directionality and the capability to deposit stoichiometric materials, high melting point or hard material are required. First results from laboratory experiments involving refractory and high melting point metals deposition for lift-off processes are reported.

IJD electrodynamics allows the ionised coating material to impinge the substrate with far more energy per unit area than in evaporation or sputtering, representing a better option when a good adhesion is mandatory without using buffer layers.

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Page 24: Surface Modification and Analysis - VACUUM SYMPOSIUMAtomic Layer Deposition: a Process Technology for Functional Ultra-Thin Films Paul Chalker School of Engineering, University of

Advances in Thermochromic Vanadium Dioxide Thin Films

Dr Russell Binions

School of Engineering and Materials Science, Queen Mary University of London, UK

Nanostructured thin films of vanadium dioxide have been deposited using a novel electric field assisted chemical vapour deposition methodology onto glass substrates. Electric fields were generated during the deposition reaction by applying a potential difference between two transparent conducting oxide coated glass substrates. The deposited films were analysed and characterized using scanning electron microscopy, Raman spectroscopy, X-ray photoelectron spectroscopy and X-ray diffraction. It was found that applying an electric field led to large changes in film microstructure, preferential orientation and in the film growth rate. This led to improved materials properties such as increased enhanced wetting behaviour, reduction in thermochromic transition temperature and improved supercapacitor electrode behaviour. Electric field assisted chemical vapour deposition shows great promise as a method for nano-structuring and tailoring the properties of metal oxide thin films.

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New Agilent Cary 7000 Universal Measurement Spectrophotometer for Analysis of Thin Film

Rob Wills

Agilent Technologies UK Ltd., Stockport, SK8 3GR, UK

Designers and manufacturers of high quality multilayer optical coatings require reliable methods to measure optical constants of thin film materials with a high degree of accuracy. This is normally achieved using UV-Visible-IR spectrophotometry to acquire normal and quasi-normal transmittance (T) and reflectance (R) spectra of a sample. Understanding the accuracy of the data produced and the source of any errors (random or systematic) will lead to more reliable sample characterization.

This presentation will introduce the new Agilent Cary 7000 “Universal Measurement Spectrophotometer” and discuss how this new development has already enabled thin film researchers to gain a better understanding of thin film response.

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Page 26: Surface Modification and Analysis - VACUUM SYMPOSIUMAtomic Layer Deposition: a Process Technology for Functional Ultra-Thin Films Paul Chalker School of Engineering, University of

Abnormal photovoltaic effects in oxide perovskites

Professor Marin Alexe University of Warwick, Department of Physics, CV4 7AL, UK

In the recent past, the field of anomalous photovoltaic effect in non-centrosymmetric perovskite ferroelectric oxides has been revitalized by the reports of photovoltaic effect (PVE) in BiFeO3 (BFO). Unlike traditional semiconductors the open circuit voltages in these materials are not limited by band gap Eg, they can exceed Eg by orders of magnitude. The microscopic origins of this effect are still under debate. Initial investigations on BFO films assumed that the PVE in BFO is primarily due to the presence of a potential step at the ferroelectric domain walls. However, our recent work has shown that the generation and recombination of photo-generated non-equilibrium carriers are primarily affected by the presence of the shallow energy levels and the anomalous bulk photovoltaic effect plays the major role in PVE.

This talk will address fundamentals of photoferroelectrics and anomalous bulk photovoltaic effect in perovskite oxides, particularly in BiFeO3. Besides of that, newly characterization methods based on local photoelectric measurement such as photo-induced transient spectroscopy (PITS) which bring valuable data regarding generation and recombination of the photo-excited carriers will be tackled. We will also discuss complementary characterization methods such as thermally stimulated current and variable temperature PV effect and show that these can provide information on electronic structure of material, respectively shallow or deep levels in the band gap.

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Page 27: Surface Modification and Analysis - VACUUM SYMPOSIUMAtomic Layer Deposition: a Process Technology for Functional Ultra-Thin Films Paul Chalker School of Engineering, University of

Laser printing of organic light-emitting diode pixels by LIFT

Dr. James Shaw-Stewart Coventry University, Empa and PSI, Switzerland

Laser-induced forward transfer (LIFT) is a laser-based, dry, non-contact, patterned deposition technique, shown to be applicable to a variety of thin films. At present the technique is still in the research stage, but an EU FP7 research grant called “e-LIFT” has sped up and intensified the development of LIFT.

LIFT deposition of organic semiconductor thin films to fabricate functional organic light-emitting diode (OLED) pixels is demonstrated here, and an overview of the advances obtained to this goal by the groups at Empa and PSI in Switzerland are outlined. These include the successful and reliable transfer of functional OLED pixel material stacked with the metal electrode across a 10 um gap, the fabrication by LIFT of a range of different OLEDs, and the fabrication of an OLED by sequential transfer of the organic and metal layers.

Alongside this research there has been work by other members of the e-LIFT consortium on the deposition of organic thin-film transistors (TFTs) and organic photovoltaics (OPVs), as well as for a whole host of other applications for inorganic thin films, such as sensors and RFIDs.

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Page 28: Surface Modification and Analysis - VACUUM SYMPOSIUMAtomic Layer Deposition: a Process Technology for Functional Ultra-Thin Films Paul Chalker School of Engineering, University of

Contamination Control, Cleaning and Surface Preparation for Vacuum Applications

Thursday 16th October 2014 – Jaguar Suite

Meeting Agenda

1030 – 1115 Session 1

1115 – 1130 Refreshment Break

1130 – 1250 Session 2

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Page 29: Surface Modification and Analysis - VACUUM SYMPOSIUMAtomic Layer Deposition: a Process Technology for Functional Ultra-Thin Films Paul Chalker School of Engineering, University of

An Introduction to ‘Contamination Control, Cleaning and Surface Preparation for Vacuum Applications’

Joe Herbert ASTeC Vacuum Group, STFC Daresbury Laboratory To be confirmed

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Page 30: Surface Modification and Analysis - VACUUM SYMPOSIUMAtomic Layer Deposition: a Process Technology for Functional Ultra-Thin Films Paul Chalker School of Engineering, University of

Concerned about the upcoming sunset date for Trichloroethylene.

Mark Duggan Acota Limited, Shrewsbury, UK

Acota Ltd specialise in precision cleaning solutions. An informative presentation on potential solutions available and equipment otion to run the chemistries. An overview to products both past and present; in light of the Monteral Protocal and Reach registration. With reference to a case study within the industry on how they substituted Trichloroethylene.

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Page 31: Surface Modification and Analysis - VACUUM SYMPOSIUMAtomic Layer Deposition: a Process Technology for Functional Ultra-Thin Films Paul Chalker School of Engineering, University of

Surface cleaning with gas cluster ion sources

Tim S. Nunney Thermo Fisher Scientific, East Grinstead, UK

Devices based on thin organic or polymer layers are becoming increasingly important. These devices are typically composed of stacks of thin layers of organic and inorganic materials. Traditional argon monomer ion cleaning can result in chemical modification during analysis, invalidating the data. New cluster ion sources limit the chemical damage to the surface, making analysis possible.

We will present data from a monatomic and gas cluster ion source, showing how it can be used for surface cleaning, and depth profile analysis of multilayers.

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Page 32: Surface Modification and Analysis - VACUUM SYMPOSIUMAtomic Layer Deposition: a Process Technology for Functional Ultra-Thin Films Paul Chalker School of Engineering, University of

Developing cleaning for XHV at Daresbury

Keith Middleman STFC Daresbury Laboratory, Warrington, Cheshire, UK

Modern particle accelerators such as the ALICE at Daresbury Laboratory have increasingly more difficult vacuum challenges to overcome and require pressures lower than 10-11 mbar for satisfactory cathode lifetimes. Pushing the boundary from UHV to XHV has posed many problems and this talk will detail our improved cleaning procedures, in-situ RGA monitoring and its importance, particle control and other aspects of XHV vacuum.

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Page 33: Surface Modification and Analysis - VACUUM SYMPOSIUMAtomic Layer Deposition: a Process Technology for Functional Ultra-Thin Films Paul Chalker School of Engineering, University of

RGA’s for Vacuum Diagnostics and Outgassing Measurements

Dr. Günter J. Peter Inficon Ltd. LI-9496 Balzers, Principality of Liechtenstein

The Quadrupole Mass Spectrometer was invented 1958 at the University of Bonn. Starting in the early 60s these instrument were used for vacuum diagnostics. Today a wide variety of instruments is on the market. Instruments are used for gas-analysis in general, trace analysis in environmental- and biological applications.

After calibration a quadrupole can be used for partial pressure analysis. With the effective pumping speed the partial pressure can be converted easily to an outgassing rate. Thus, since decades, quadrupole mass spectrometers are used as sensor for material characterisation.

In the present talk the application of RGA’s in UHV / XHV and as sensor for outgassing measurements will be described.

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Page 34: Surface Modification and Analysis - VACUUM SYMPOSIUMAtomic Layer Deposition: a Process Technology for Functional Ultra-Thin Films Paul Chalker School of Engineering, University of

Case Study

Stephen Fletcher X-Tek Systems Ltd, Nikon To be Confirmed

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Page 35: Surface Modification and Analysis - VACUUM SYMPOSIUMAtomic Layer Deposition: a Process Technology for Functional Ultra-Thin Films Paul Chalker School of Engineering, University of

Vacuum Cleanliness in the Semiconductor Industry

Alan Webb Consultant (The Open University)

Dry process techniques are fundamental in being able to produce the desired architectures required for today and future semiconductor devices. Economic considerations dictate large device densities on wafers, implying smaller and smaller chips. As device sizes shrink, the need to work in cleaner conditions becomes more apparent.

What is meant by cleaner conditions and to what level of cleanliness?

A process route from an as grown wafer to completed device chips involves many process steps, which means the wafers are transported in and out of process equipment a considerable number of times.

How are wafers handled and transported in these type of environments?

How are they tracked and monitored to ensure the process steps have been successful?

Why are clean-rooms necessary and clean environments required for device fabrication?

How does the air quality, temperature and humidity affect wafer processing?

If wafers have to be protected to these type of levels, at what cost?

This presentation addresses these issues and the implication of cleanliness in semiconductor processing.

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Page 36: Surface Modification and Analysis - VACUUM SYMPOSIUMAtomic Layer Deposition: a Process Technology for Functional Ultra-Thin Films Paul Chalker School of Engineering, University of

Vacuum support, whatever that might be?

Tom Weston STFC Daresbury Laboratory Vacuum support is a service provided at Daresbury labs for accelerators by small dedicated group of staff. Their skills are many and varied, from pump repair to system fault diagnosis and many others in between. Each day can be totally different to the preceding one, many days never go to plan. Processing of vacuum components plays a key role and requires a job tracking system to keep the work flow on course. Hopefully this short presentation will provide an insight into what the black art of vacuum entails.

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Page 37: Surface Modification and Analysis - VACUUM SYMPOSIUMAtomic Layer Deposition: a Process Technology for Functional Ultra-Thin Films Paul Chalker School of Engineering, University of

5th Vacuum Symposium UK Poster Sessions

Authors will be available by their poster during the lunch- break on the day(s) their poster is on display to discuss their research

Day One: The IOP Vacuum Group will be awarding a £100 prize and certificate on Wednesday 15th October. (The prize may be shared if one or more Posters are judged to be of equal standard). The prize is open to ALL Poster presentations (except any submitted by Vacuum Group Committee members) and will be judged independently at 3.30pm on 15th October with the presentation taking place shortly afterwards in the main exhibition area.

Day Two: The Vacuum Symposium Poster Prize (£100), sponsored by PlasmaQuest Limited, will be awarded Thursday afternoon between 12.40 and 14.10 in the main exhibition area. A certificate will also be presented.

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Page 38: Surface Modification and Analysis - VACUUM SYMPOSIUMAtomic Layer Deposition: a Process Technology for Functional Ultra-Thin Films Paul Chalker School of Engineering, University of

Poster Ref Poster Title Authors

VS5.01 Al-doped ZnO by In-line MOCVD

W.S.M. Brooks, V. Barrioz, D. Lamb, P. Siderfin, S.J.C. Irvine

VS5.02 Pumping and Electron Stimulated Desorption properties of a dual layer Non Evaporable Getter

A.N. Hannah

VS5.03 Preparation of atomically clean metal surfaces for use as photocathodes in normally conducting RF guns

Sonal Mistry

VS5.04 Developing of modern superconducting coatings for particle accelerators RF cavities

Paolo Pizzol

VS5.05 Active screen plasma co-alloying of Inconel 625 with V/Ag and N

Z. Zhang, X. Li and H. Dong

VS5.06 Development of an Electrospray Deposition Source Coupled with VT-STM for Imaging Large Molecules

Jonathan Blohm

VS5.07 STM Study of 2D Self-Assembled Ketone-based Metal-Organic Frameworks

James Lawrence

VS5.08 Ag doped S-phase layer formed on 316L stainless steel by a new hybrid plasma technology

Tian Linahi

VS5.09 Monitoring Interface Formation with Real-time Electron Emission Spectroscopy

S. P. Cooil, D. Hu, D. P. Langstaff, Z. Zhou, D.A. Evans

VS5.10 Quantum States and Molecular Structures on Silicon

H. Hedgeland, A. M. Suleman, M. Siegl, K. A. Rahnejat, S. R. Schofield

VS5.11 Investigating the sublimation limit of peptides Daniel Warr, Jonathan Blohm and Giovanni Costantini

VS5.12 Poster Ref

Secondary electron yield from transition metals Poster Title

Sihui Wang Authors

VS5.01 Al-doped ZnO by In-line MOCVD

W.S.M. Brooks, V. Barrioz, D. Lamb, P. Siderfin, S.J.C. Irvine

VS5.02 Pumping and Electron Stimulated Desorption properties of a dual layer Non Evaporable Getter

A.N. Hannah

VS5.03 Preparation of atomically clean metal surfaces for use as photocathodes in normally conducting RF guns

Sonal Mistry

VS5.04 Developing of modern superconducting coatings for particle accelerators RF cavities

Paolo Pizzol

VS5.13 Low temperature removal of surface oxides and hydrocarbons from Ge(100) using atomic hydrogen cleaning

M. Walker, M. Tedder, J. Palmer, J.J. Mudd and C.F. McConville

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Page 39: Surface Modification and Analysis - VACUUM SYMPOSIUMAtomic Layer Deposition: a Process Technology for Functional Ultra-Thin Films Paul Chalker School of Engineering, University of

VS5.14 Magnetron sputtering deposition of TiO2 based

photodiodes for direct water splitting

X. Zhang, K. Cooke, D. Hazafy, D. Jose, A. Mills

VS5.15 In situ measurements of the relative density changes at phase transition in thin solid films according to electron microscopic data

A. Bagmut, I. Bagmut

VS5.16 PVD and PACVD for the Deposition of Coatings for Flexible Electronic Devices

Parnia Navabpour, Joanne Stallard, Kevin Cooke, Sue Field, Alexander Goruppa, Katrin Zorn, Manuel Auer, Katrin Koren, Andreas Klug and Emil List-Kratochvil

VS5.17 Thin Film CdTe Photovoltaics on Ultra-thin Space Qualified Cover Glass

D. A. Lamb et al.

VS5.18 Portable mass spectrometry for threat detection

Stamatios Giannoukos, Boris

Brkić, Stephen Taylor

VS5.19 Poster Ref

DEVELOPMENT OF THIN FILMS FOR SUPERCONDUCTING RF CAVITIES Poster Title

Stuart Wilde Authors

VS5.20 CHARACTERIZATION OF A CdTe THIN FILM SOLAR CELL FOR SPACE APPLICATION

Rossana Grilli

VS5.21 Synthesis and Optical Absorption of Organic-Inorganic Hybrid Perovskite Solar Cell Materials

Laurie Phillips

VS5.22 Roll-to-roll deposition of highly flexible polymer-inorganic transparent gas barrier layers

Vincent Tobin

VS5.23 MOCVD of SnSx thin films for solar cell application

A.J. Clayton, S.J.C. Irvine, V. Barrioz, A. Masciullo

VS5.24 A thermal energy, neutral atom beam microscope for imaging delicate surfaces

David Ward

VS5.25 Ionized Jet Deposition – a new option for challenging thin film coating applications

Petr Nozar and Francesco Vittori

VS5.26 Fabrication of ordered composite nanosystems by ion implantations

W Guan, J Wang, N Peng, C Jeynes, R Gwilliam, R Webb, G Moebus and B Inkson

VS5.27 Correlation between the surface and the bulk octahedral distortion in short period superlattices: in-situ RHEED versus ex-situ HR-TEM

Nessa Fereshteh Saniee, Sean McMitchell, Ana Sanchez, Chris McConville

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NOTES

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