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Photosensitive Glass and Glass-Ceramics Photosensitive Glass-Ceramics This article was downloaded by: 10.3.98.104 On: 02 Oct 2021 Access details: subscription number Publisher: CRC Press Informa Ltd Registered in England and Wales Registered Number: 1072954 Registered office: 5 Howick Place, London SW1P 1WG, UK Photosensitive Glass and Glass-Ceramics Nicholas F. Borrelli Photosensitive Glass-Ceramics Publication details https://www.routledgehandbooks.com/doi/10.1201/9781315368801-4 Nicholas F. Borrelli Published online on: 29 Jun 2016 How to cite :- Nicholas F. Borrelli. 29 Jun 2016, Photosensitive Glass-Ceramics from: Photosensitive Glass and Glass-Ceramics CRC Press Accessed on: 02 Oct 2021 https://www.routledgehandbooks.com/doi/10.1201/9781315368801-4 PLEASE SCROLL DOWN FOR DOCUMENT Full terms and conditions of use: https://www.routledgehandbooks.com/legal-notices/terms This Document PDF may be used for research, teaching and private study purposes. Any substantial or systematic reproductions, re-distribution, re-selling, loan or sub-licensing, systematic supply or distribution in any form to anyone is expressly forbidden. The publisher does not give any warranty express or implied or make any representation that the contents will be complete or accurate or up to date. The publisher shall not be liable for an loss, actions, claims, proceedings, demand or costs or damages whatsoever or howsoever caused arising directly or indirectly in connection with or arising out of the use of this material. Photosensitive 3 Glass-Ceramics Biscotti: An Italian cookie that is twice baked. 3.1 INTRODUCTION AND BACKGROUND The subject and content of this chapter continue and significantly add to the mate- rial in previous chapter. It is a continuation because we start with the formation of the noble metal nanophase in the first step, and it is an addition because crystal- line nanophases are subsequently produced from the initially formed noble metal particles formed by the method described in Chapter 2. In other words, the photo- sensitively formed Ag and Au nanoparticles can act as the nuclei for the growth of a variety of crystalline nanophases from the glass matrix. This class of photosensi- tively produced nanophase materials was initially discovered by S. Donald Stookey while working at the Corning Incorporated (formerly Corning Glass Works) research laboratory in the early 1950s.1 From then on and even up to the present, new crystal- line phases have been produced in this novel and useful way. The advantages stem from the altered chemical, mechanical, and optical properties of the composite glass/ crystalline phases with the distinct advantage of being produced essentially by a photolithographic technique; that is, to be able to spatially pattern the regions that are crystalline. It should be appreciated that all glass-ceramics derive from a glass composition that is in a thermodynamically metastable state produced by the rapid cooling of the glass from a molten state, literally a thousand degrees in a few minutes. Reheating the glass can cause it to crystallize if it is heated above the liquidus temperature and the glass is fluid enough (i.e., the viscosity is sufficiently low at the liquidus temperature). However, it is desirable to control the size of the crystallites, and therefore it is often necessary to provide nucleating agents. This means that it is not necessary to reach as high a temperature, thereby exercising more control of the rate of crystallization. Nucleating agents are constituents added to the glass composition to provide some type of compositional fluctuation that influences the crystalline formation. Nucleating agents can be Ti or Zr or phosphate.2,3 The relevant point here is that noble metal nanoparticle can provide this function as well. It is beyond the scope of this book to describe what the physical and chemical mechanism(s) are or the various nucleation processes for various phases but it is certainly interesting to speculate exactly how the nucleating process works. In the case of TiO2 additions, it is speculated that it may form some sort of localized titanate immiscible phase that in turn provides a place where a major crystalline phase can begin to segregate from the glass. From a thermodynamic point of view, one could view the phenomenon as 31 Downloaded By: 10.3.98.104 At: 02:48 02 Oct 2021; For: 9781315368801, chapter3, 10.1201/9781315368801-4 32 Photosensitive Glass and Glass-Ceramics a lowering of the free energy barrier to crystallization by the composition changes in a local area. In other words, any local composition fluctuation alters the free energy and hence produces diffusion, further altering the composition. In all cases we will deal with the phase that is to be produced in a controlled manner which is invariably the phase that would be produced by heating the glass to a higher temperature but with no control of the amount or grain size. In other words, glass- ceramics is really just another word for controlled crystallization. A much more complete discussion of the physics of nucleation is provided in Holand and Beall’s book on glass-ceramics technology.4 3.2 NOBLE METAL NUCLEATION In some glasses, certain noble metal particles can nucleate certain phases and even more surprising is that these phases can act as nuclei for additional phases to form the kind of twice-baked situation alluded to at the beginning of the chapter. The extension of this process to have the Ag nanoparticle act as a nucleation center for a nanocrystalline phase derived from the glass has been known and reported in both the open and patent literature.5,6 Examples from both will be covered here. Schematically, one adds another reaction equation, shown below as Equation 3.4, to the simplified version of the schema given in Chapter 2, which is repeated here for convenience: Ce+3 + hv → e + Ce+3+ (250–350 nm) (3.1) + Ag + e + heat → Ag0 (3.2) n(Ag0) + heat → (Ag0)n (3.3) (Ag0)n + X + Y + heat → XY (3.4) Here, XY represents the nanophase material produced by the glass constituents X and Y nucleated by the Ag nanoparticle. In reality Equations 3.3 and 3.4 occur together as a consequence of the thermal treatment. The chemistry of the actual nucleation process is not known; that is, by what reaction(s) actually occur aided and abetted by the Ag nanoparticle. Clearly, this involves a heterogeneous nucleation mechanism, which has been discussed in some detail in Holand and Beall4 in the case of a metal agent. It is described in terms of the interplay of the various inter- facial energies, metal/liquid, crystal/liquid, and metal/solid, as well as the contact angle. However, there is one study that sheds some light (forgive the pun) on the initial stage of the process. Borrelli et al.5 used the shift in the spectral position of the silver plasmon resonance that is a function of the complex dielectric constant of the Ag and the dielectric constant of the medium m in which the Ag is embedded (see Section 2.5) to track the change in composition surrounding the Ag nuclei as a function of the thermal treatment. We copy the expression for the absorption here for Downloaded By: 10.3.98.104 At: 02:48 02 Oct 2021; For: 9781315368801, chapter3, 10.1201/9781315368801-4 Photosensitive Glass-Ceramics 33 convenience of the reader. Note how the spectral position of the resonance absorp- tion depends on the condition when 1 =−2 m. 2πV C m 2 abs = 2 2 (3.5) λ ()2 1 ++m 2 A glass was chosen to study the halide crystal growth for a typical photosensitive glass composition where the halide in this case was Br. Figure 3.1 shows a typical transmission spectra after a 560°C heat treatment for the glass without bromine and with bromine, respectively. For the bromine-free glass, the absorption peak was seen to shift only slightly in wavelength as a function of the temperature of the thermal treatment. This indicated that only a small effect due to the change in the silver speck size occurred. The variation of the absorption peak was used to estimate the silver speck size as a function of the thermal treat- ment by the use of the above expression.5 The size effect on the absorption is due to the size dependence of 2 expressed by 22=+B C/r as discussed in Section 2.5. The absorption peak shift was used rather than the change in the absorption band half-width because the latter was significantly altered by the absorption edge owing to the cerium contained in the glass. The inset in Figure 3.2 shows the computed radius versus the heat-treatment temperature. Using this computed variation of the silver particle size with heat-treating temperature, the absorption data for the bromine- containing glass was analyzed to determine the value of the refractive index of the surrounding medium required to match the observed wavelength of maximum absorption at each temperature. The result of the calculation is shown in Figure 3.2. 100 A 80 B ansmission Tr % 60 40 0.35 0.45 0.55 Wavelength (µm) FIGURE 3.1 Surface plasmon absorption of an Ag nanoparticle in a glass with and without Br to show that in the glass containing Br, the refractive index surrounding the Ag particle is being increased by Br enrichment, thus shifting the peak position according to Equation 3.5. (From N.F. Borrelli, J.B. Chodak, D.A. Nolan, and T.P. Seward, J. Opt. Soc. Am. 69(11), 1514, 1979.5) Downloaded By: 10.3.98.104 At: 02:48 02 Oct 2021; For: 9781315368801, chapter3, 10.1201/9781315368801-4 34 Photosensitive Glass and Glass-Ceramics 1.65 No Br 1.60 ) 1 1.55 2.0 o Refractive index (n ln 1.8 1.50 Index of glass 1.6 1.20 1.25 1.30 1.35 1000/T 1.45 500 600 Temperature (°C) FIGURE 3.2 Computed refractive index of the region surrounding the Ag speck from the shift in the peak of the Ag surface plasmon absorption to indicate the Br enrichment.
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