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Modification of Float Glass Surfaces by Ion Exchange
Linnaeus University, Faculty of Science and Engineering, School of Engineering. (Glass group)ORCID iD: 0000-0003-2160-6979
2012 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

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.

Place, publisher, year, edition, pages
Växjö, Kalmar: Linnaeus University Press, 2012. , p. 176
Series
Linnaeus University Dissertations ; 89/2012
Keywords [en]
Ion exchange, float glass, surface modification, surface colour, flexural strength
National Category
Other Materials Engineering
Research subject
Technology (byts ev till Engineering), Glass Technology
Identifiers
URN: urn:nbn:se:lnu:diva-18447ISBN: 978-91-86983-62-8 (print)OAI: oai:DiVA.org:lnu-18447DiVA, id: diva2:525482
Public defence
2012-06-14, Sal Myrdal, Hus K, Växjö, 14:00 (English)
Opponent
Supervisors
Available from: 2012-05-09 Created: 2012-04-23 Last updated: 2019-02-27Bibliographically approved
List of papers
1. The technology of chemical glass strengthening - a review.
Open this publication in new window or tab >>The technology of chemical glass strengthening - a review.
2010 (English)In: Glass Technology, ISSN 0017-1050, Vol. 51, no 2, p. 41-54Article, review/survey (Refereed) Published
Abstract [en]

The methods of chemical strengthening for improving the mechanical properties of oxide glasses are reviewed. Chemical strengthening in compared with thermal strengthening and different methods of measuring strength are discussed. Different ions, salts and other related methods for improving the ion exchange process and mechanical properties are described as well as applications of strengthening.

National Category
Chemical Sciences
Research subject
Technology (byts ev till Engineering), Glass Technology
Identifiers
urn:nbn:se:lnu:diva-5819 (URN)
Available from: 2010-06-04 Created: 2010-06-04 Last updated: 2019-02-27Bibliographically approved
2. Surface Analysis of float glass using Surface Ablation Cell (SAC) Part 2: Determination of the diffusion characteristics of K+-Na+ ion exchange
Open this publication in new window or tab >>Surface Analysis of float glass using Surface Ablation Cell (SAC) Part 2: Determination of the diffusion characteristics of K+-Na+ ion exchange
2010 (English)In: Glass Technology, ISSN 0017-1050, Vol. 51, no 2, p. 55-62Article in journal (Refereed) Published
Abstract [en]

The Surface Ablation Cell (SAC), a laboratory equipment for determining surface concentration profiles, has been utilised to characterise float glass surface ion exchange processes. In this paper, single-side ion exchange is reported. Data on the ion concentration profiles were used to calculate diffusion coefficients as well as the activation energy for K+-Na+ ion exchange. The air-sides of float glass samples were treated with two different salt mixtures, I) KNO3:KCl, 2:1 and II) KNO3:KCl, 1:2, and heated to different temperatures under Tg, 460-520 °C. The diffusion coefficients calculated with Green’s function were in the range I) 1.4x10-11 to 6.8x10-11 and II) 1.8x10-11 to 6.0x10-11 cm2/s while calculated according to Boltzmann-Matano I) 5.7x10-12 to 1.4x10-11 and II) 3.4x10-12 to 6.0x10-12 cm2/s. Average values of the activation energies obtained through Green’s function were I) 111.0 kJ/mol and II) 99.8 kJ/mol for the different salt mixtures.

National Category
Chemical Sciences
Research subject
Technology (byts ev till Engineering), Glass Technology
Identifiers
urn:nbn:se:lnu:diva-5820 (URN)
Available from: 2010-06-04 Created: 2010-06-04 Last updated: 2019-02-27Bibliographically approved
3. Copper, silver, rubidium and caesium ion exchange in soda-lime-silicate float glass by direct deposition and in line melting of salt pastes
Open this publication in new window or tab >>Copper, silver, rubidium and caesium ion exchange in soda-lime-silicate float glass by direct deposition and in line melting of salt pastes
2012 (English)In: European Journal of Glass Science and Technology. Part A: Glass Technology, ISSN 1753-3546, Vol. 53, no 1, p. 1-7Article in journal (Refereed) Published
Abstract [en]

We report the change of surface composition on commercial soda-lime-silica (SLS) float glass which results from single-side exchange of Na+ by Cu+, Ag+, Rb+ and Cs+, respectively. Ion exchange is achieved by in line melting of a directly deposited salt paste in a prolonged annealing procedure. Concentration profiles obtained and computed effective diffusion coefficients, as well as apparent activation energies for diffusion, are reported. Depending on exchange species, treatment time and treatment temperature, the penetration depths are in the range of 10-20 μm for K+, Cu+, Rb+ and Cs+. A penetration depth of >100 μm can readily be obtained for Ag+.

Keywords
Ion exchange, surface analysis, diffusion, concentration profile, float glass, monovalent cations
National Category
Other Materials Engineering
Research subject
Technology (byts ev till Engineering), Glass Technology
Identifiers
urn:nbn:se:lnu:diva-17922 (URN)
Available from: 2012-03-07 Created: 2012-03-07 Last updated: 2019-02-27Bibliographically approved
4. Surface ruby colouring of float glass by sodium-copper ion exchange
Open this publication in new window or tab >>Surface ruby colouring of float glass by sodium-copper ion exchange
2013 (English)In: European Journal of Glass Science and Technology. Part A: Glass Technology, ISSN 1753-3546, Vol. 54, no 3, p. 100-107Article in journal (Refereed) Published
Abstract [en]

In this paper, colouration of the tin side of commercial soda lime silicate float glass by copper ion exchange is described and characterised. Data on the resulting concentration vs. depth profiles, absorbance vs. depth profiles, UV-Vis spectra  and CIE-Lab colour coordinates are reported. Fundamental aspects of the process of colouration are described and discussed. Optimum saturation of colouration is achieved after ion exchange at 520 °C for 10 h, or at 500 °C for 20 h, respectively. The depth of the coloured layer increases with increasing treatment time. At the same time, a linear dependency is found between the value of a and b in the CIE-Lab colour space for variations of treatment time and temperature. The latter indicates broad tunability of colouration between different shades of ruby and varying colour saturation. It is shown that colour arises from a redox reaction between copper species and residual tin ions, and that the depth of the coloured layer is governed by the position of the tin hump. The critical concentration of tin and copper to achieve colour formation was found to be ~0.25 mol% and >1 mol%, respectively.

Place, publisher, year, edition, pages
Society of Glass Technology, 2013
Keywords
Float glass, copper ruby, ion exchange, staining, colouring
National Category
Other Materials Engineering
Research subject
Technology (byts ev till Engineering), Glass Technology
Identifiers
urn:nbn:se:lnu:diva-18448 (URN)000321155700002 ()2-s2.0-84881145236 (Scopus ID)
Note

Manuscript included in the PhD-thesis.

Available from: 2012-04-26 Created: 2012-04-23 Last updated: 2019-02-27Bibliographically approved
5. The effect of single-side ion exchange on the flexural strength of plain and holed float glass containing a drilled hole
Open this publication in new window or tab >>The effect of single-side ion exchange on the flexural strength of plain and holed float glass containing a drilled hole
2013 (English)In: European Journal of Glass Science and Technology. Part A: Glass Technology, ISSN 1753-3546, Vol. 54, no 2, p. 66-71Article in journal (Refereed) Published
Abstract [en]

The effect of single-side ion exchange (using a KNO3:KCl mixture) on the ring-on-ring flexural strength of float glass has been studied. Two ion exchanged series, treated at 450 and 515°C, were investigated. The ion exchanged samples showed approximately 160 respectively 100% increases in their arithmetic mean strength compared to as-received float glass. Furthermore, a series of samples containing drilled holes were studied in order to investigate the effect of single-side ion exchange on such common construction elements. The samples that contained drilled holes were ion exchanged at 450°C and showed around 140% increase of the fracture load compared to the untreated samples containing drilled holes. As a general observation, the ion exchange treatment induced ~110 MPa compressive stresses (515°C) and ~180 MPa compressive stresses (450°C). The ion exchanged samples showed no significant increase in stiffness. 

Keywords
Float glass, Ion exchange, Flexural strength, Coaxial double ring-test
National Category
Other Materials Engineering
Research subject
Technology (byts ev till Engineering), Glass Technology
Identifiers
urn:nbn:se:lnu:diva-18449 (URN)000318753100002 ()2-s2.0-84881146304 (Scopus ID)
Available from: 2012-04-26 Created: 2012-04-23 Last updated: 2019-02-27Bibliographically approved
6. Surface Analysis of float glass using Surface Ablation Cell (SAC) Part 1: Initial collaboration and comparison with SIMS.
Open this publication in new window or tab >>Surface Analysis of float glass using Surface Ablation Cell (SAC) Part 1: Initial collaboration and comparison with SIMS.
Show others...
2010 (English)In: Glass Technology, ISSN 0017-1050, Vol. 51, no 1, p. 13-21Article in journal (Refereed) Published
Place, publisher, year, edition, pages
Sheffield: The Society of Glass Technology, 2010
National Category
Engineering and Technology
Research subject
Technology (byts ev till Engineering), Glass Technology
Identifiers
urn:nbn:se:lnu:diva-235 (URN)
Available from: 2010-03-31 Created: 2010-03-31 Last updated: 2019-02-27Bibliographically approved

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