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Modification of Float Glass Surfaces by Ion Exchange

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Modification of Float Glass Surfaces by Ion Exchange Modification of Float Glass Surfaces by Ion Exchange Linnaeus University Dissertations No 89/2012 MODIFICATION OF FLOAT GLASS SURFACES BY ION EXCHANGE STEFAN KARLSSON LINNAEUS UNIVERSITY PRESS MODIFICATION OF FLOAT GLASS SURFACES BY ION EXCHANGE Doctoral dissertation, School of School of Engineering, Linnaeus University 2012 ISBN: 978-91-86983-62-8 Printed by: Ineko AB, Kållered ABSTRACT Karlsson, Stefan, (2012). Modification of Float Glass Surfaces by Ion Exchange. Linnaeus University Dissertations No 89/2012. ISBN: 978-91-86983-62-8. Written in English. Glass is a common material in each person’s life, e.g. drinking vessels, windows, displays, insulation and optical fibres. By modifying the glass surface it is possible to change the performance of the entire glass object, generally known as Surface Engineering. Ion exchange is a convenient technique to modify the glass surface composition and its properties, e.g. optical, mechanical, electrical and chemical properties, without ruining the surface finish of the glass. This thesis reports the findings of two different research tasks; characterisation of the single-side ion exchange process and the novel properties induced. The characterisation of the ion exchange process was mainly performed by utilising a novel analytical equipment: the Surface Ablation Cell (SAC), allowing continuous removal of the flat glass surface by controlled isotropic dissolution. SAC-AAS has provided concentration vs. depth profiles of float glass ion exchanged with K+, Cu+, Rb+ and Cs+. In addition, SEM-EDX has provided concentration vs. depth profiles of Ag+ ion exchanged samples and validation of a copper concentration vs. depth profile. From the concentration vs. depth profiles, the effective diffusion coefficients and activation energies of the ion exchange processes have been calculated. Depending on the treatment time and treatment temperature, penetration depths in the range of 5-10 μm (Rb+, Cs+), 20-30 μm (K+, Cu+) and 80-100 μm (Ag+) can be readily obtained. The effective diffusion coefficients followed the order Ag+>K+>Cu+>Rb+>Cs+. This is in accordance with the ionic radii for the alkali ions (K+<Rb+<Cs+) but reverse for the noble metal ions (Cu+<Ag+). The glass properties modified by single-side ion exchange have mainly been characterised by UV-VIS spectroscopy and flexural strength measurements. Cu+ and Ag+ ion exchange give rise to surface colouration, Cu+ copper-ruby and Ag+ yellow/amber. The surface-ruby colouration was found to depend on the residual tin ions in the tin-side of the float glass. The flexural strength was studied using the coaxial double ring-test method which also was suitable for holed specimens. The flexural strength of K+ ion exchanged float glass samples was found to substantially increase compared to untreated. Keywords: Ion exchange, float glass, surface modification, surface colour, flexural strength LIST OF PAPERS This thesis is based on the following papers, which will be referred to by Ro- man numerals in the text. I The Technology of Chemical Glass Strengthening – A Review Stefan Karlsson, Bo Jonson and Christina Stålhandske Glass Technology – European Journal of Glass Science & Technology Part A, 2010.51(1): p. 41-54. II Surface Analysis of float glass using Surface Ablation Cell (SAC) Part 2: Determination of the diffusion characteristics of K+-Na+ Ion Exchange Stefan Karlsson, Bo Jonson, Peter Sundberg and Christina Stålhandske Glass Technology – European Journal of Glass Science & Technology Part A, 2010.51(2): p. 55-62. III Copper, silver, rubidium and caesium ion exchange in soda-lime-silicate float glass by direct deposition and in line melting of salt pastes Stefan Karlsson, Bo Jonson and Lothar Wondraczek Glass Technology - European Journal of Glass Science and Technology Part A, 2012. 53(1): p. 1-7. IV Surface ruby colouring of float glass by sodium - copper ion exchange Stefan Karlsson, Bo Jonson, Sindy Reibstein and Lothar Wondraczek Manuscript V The effect of single-side ion exchange on the flexural strength of plain and holed float glass Stefan Karlsson, Bo Jonson, Marie Johansson and Bertil Enquist Submitted to Glass Technology - European Journal of Glass Science and Tech- nology Part A VI Surface Analysis of float glass using Surface Ablation Cell (SAC) Part 1: Initial collaboration and comparison with SIMS Peter Sundberg, Stefan Karlsson, Dominique Brochot, José Simons, and Christine Strubel Glass Technology – European Journal of Glass Science & Technology Part A, 2010.51(1): p. 13-21. vi Results related to this thesis have also been presented at scientific conferences: Determination of diffusion characteristics of ion exchanged float glass by use of a Surface Ablation Cell (SAC) Stefan Karlsson Glass Science session, Annual Meeting of Society of Glass Technology, Lan- caster, United Kingdom, 16-18th September 2009. Ion exchange of monovalent ions in float glass Stefan Karlsson New researchers session, Annual Meeting of Society of Glass Technology, Cambridge, United Kingdom, 8-10th September 2010. Glass strengthening and ion exchange phenomena Stefan Karlsson 60th Annual Meeting of the Scandinavian Society of Glass Technology, Kosta, Sweden, 26-28th September 2010. Colouration of float glass by copper ion exchange Stefan Karlsson, Bo Jonson and Lothar Wondraczek Poster session, 85th Glastechnische Tagung der Deutsche Glastechnischen Gesellschaft, Saarbrücken, Germany, 30th May – 1st June 2011 Copper colouration of the surface of float glass by ion exchange Stefan Karlsson, Bo Jonson and Lothar Wondraczek Glass fibre and Glass colour session, 11th European Society of Glass conferenc to- gether with 86th Glastechnische Tagung der Deutsche Glastechnischen Gesell- schaft and International Commission on Glass Annual Meeting, Maastricht, The Netherlands, 3rd –6th June 2012. vii AUTHOR’S CONTRIBUTION The following is the author’s contribution to the papers on which this thesis is based: I Made improvements after the first draft; adding patents, figures and re- structuration of the paper. II Performed all experiments, analyses and numerical procedures as well as writing the draft of the paper. Planned parts of the experimental work. III Performed all experiments and numerical procedures. Made all analyses and wrote the draft of the paper. Planned most of the experimental work. IV Performed all experiments and made all analyses apart from XRD and TEM. Planned most of the experimental work and wrote the draft of the paper. V Peformed all experiments and numerical procedures as well as writing the draft of the paper. Planned the major part of the experimental work. VI Made contributions through discussions on experimental issues and gave suggestions on the draft of the paper. viii CONTENTS List of papers.....................................................................................................vi Author’s contribution..................................................................................... viii 1. Introduction .................................................................................................. 1 2. Diffusion and ion exchange in silicate glasses .............................................. 7 2.1 Diffusion................................................................................................ 7 2.2 Ion exchange.......................................................................................... 8 2.2.1 Ion exchange and the glass structure............................................. 9 2.3 Kinetics of ionic diffusion and ion exchange....................................... 10 2.4 Modification of properties by ion exchange........................................ 12 2.4.1 Chemical strengthening.............................................................. 12 2.4.1.1 Differences in thermal expansion ............................................ 13 2.4.1.2 Ion stuffing............................................................................... 13 2.4.2 Hardness...................................................................................... 16 2.4.3 Ion exchanged glass waveguides.................................................. 16 2.4.4 Colouration of glass surfaces by ion exchange............................ 17 3. Experimental and numerical procedures..................................................... 18 3.1 Experimental........................................................................................ 18 3.1.1 Float glass used for the investigations......................................... 18 3.1.2 Ion exchange treatment............................................................... 18 3.1.3 Surface ablation procedure.......................................................... 20 3.1.3.1 SAC mounted in UV-VIS spectrophotometer ....................... 21 3.1.4 Chemical analyses and other instruments................................... 22 3.1.5 Mechanical properties measurements......................................... 22 3.1.5.1 Flexural strength ...................................................................... 22 3.1.3.2 Scratch hardness....................................................................... 24 3.2 Numerical procedures.......................................................................... 24 3.2.1 Surface chemical composition..................................................... 24 3.2.1 Effective diffusion coefficient ..................................................... 25 3.2.2 Flexural strength and fracture probability................................... 26 4. Results
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