D. EHRT, W. SEEBER Friedrich-Schiller-Universität Jena, Otto-Schott-Intitut, Fraunhoferstr. 6, D Jena, Germany

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1 SPECTROSCOPIC DETERMINATION OF THE REDOX STATE OF POLYVALENT IONS IN OPTICAL GLASSES D. EHRT, W. SEEBER Friedrich-Schiller-Universität Jena, Otto-Schott-Intitut, Fraunhoferstr. 6, D Jena, Germany INTRODUCTION The demand^ for UV-transmitting materials in the range, below 300 nm has increased for lens systems in microlithography equipment and substrate materials. Fiuoroaluminate and fluoride phosphate glasses with a low content of phosphate, so called fluor crown (FK) glasses, are attractive candidates as UV-transmitting materials (2-6, 8,9). The intrinsic absorption in the UV region is due to electron transitions. The values for the UV resonance wavelengths of FK glasses calculated using a two term Sellmeier dispersion formula are comparable with those of CaF 2 (1). However, the UV transmission of glass is frequently limited by extrinsic absorption of trace impurities introduced by raw materials and the possible contamination from the melting technique and method of processing used. Trace impurities are mainly transition metals. Their charge transfer bands having high absorption coefficients are preferred over electron transition bands. The UV- VIS transmission characteristics of a FK laser glass doped with the metallic impurities: Ce, Pt, Cr, Cu, Fe, Ni in the ppm-range were investigated by Cook and Mader (5). They found that the UV absorption of the glass depends on the melting conditions used, with wide variations in UV absorbance intensity observed when different atmospheres and container materials are used. Changes in UV absorption observed in the glass appear to be container-dependent and are due to oxidation and reduction of iron present in the raw materials. It is known that FK glasses melted under reducing conditions in carbon crucibles have much higher UV transmission than glasses melted under oxidizing conditions in platinum crucibles. The increase of the UV transmission is mainly attributed to a reduction of Fe J * to Fe'* due to carbon crucible melt interaction. In previous papers we have studied the effect of the redox state of Fe in some detail (2, 4, 9). In this work we investigated the temperature dependence of the redox states of Fe, Cu and Pb ions by means of absorption and luminescence spectroscopy. We tried to determine the contribution of the redox state of individual impurities to the total transmission loss in FK glasses. EXPERIMENTAL Two hundred gram melts of fluoride phosphate optical glasses composition FK 90 (90 mol% fluorides AlF,, MgF 2, CaF 2, SrF 2 and 10 mol% M(PO,),) were doped with Supplement to "Rivista della Stazione Sperimentale del Vetro" Vol. XXIII,

2 known impurities in the ppm range. Added concentrations ranged from 5 to 500 ppm of the metal, depending on the magnitude of absorption and luminescence effect. At first, glasses were melted under normal conditions in platinum crucibles in air atmosphere at ¾. To achieve oxidizing conditions througth the melts oxygen was bubbled at the same temperature. For reducing conditions depending on melting temperature 30 g glass was remelted in amorphous carbon crucibles in a special graphite furnace under flowing argon atmosphere at 900 to 1200¾ and cooled to room temperature in this furnace. One undoped glass was melted under the same conditions for comparison about background loss. The castings were cut, ground and polished into plates of 11 mm and 2 mm thickness. Some 1500 g melts of FK90 were produced in a special C,5 1 coated carbon crucible under argon atmosphere in a glove box at different refining temperatures from 850 to 1100¾. The large melts were stirred during refining and cooling to the casting temperature. The resulting glass quality was very high with an excellent homogeneity. Sample plates of 1, 2, 11, 26 and 51 mm thickness were produced for absorption and luminescence measurements. In some cases raw materials of special high purity (ultrapure) were used. These glasses are signed with index s. The optical absorption spectra were obtained using UV 3101 PC spectrometer from SHIMADZU and a special equipment for the VUV region. The luminescence excitation and emission spectra were measured using RF 5001 PC spectrometer from SHIMADZU. RESULTS and DISCUSSION Figure 1 shows VUV transmission spectra of undoped glasses FK90 melted under normal conditions (air, 1050¾, Pt crucible) and under reducing conditions (Ar, 0,5 1 carbon crucible) at 850¾ and 1050¾. Figure 1: VUV transmission spectra of undoped glasses FK Supplement to "Rivista della Stazione Sperimentale del Vetro" Vol. XXIII, 1993

3 fundamentals of Glass Science and Technology - ESG 1993, Venice ~he analyzed iron content of all glasses was nearly the same, 15 ppm Fe. But there re large differences in VUV and UV transmission. Two broad bands near 250 nm and 00 nm are attributed to Pt ions too but mainly depending on the Fe 3 VFe 2 * ratio. It s known, that glasses melted under reducing conditions posses higher UV transmit- ;ance near 250 nm due to the reduction of Fe 3 * to Fe 2 *. The results demonstrate a strongly dependence of the reducing effect on the melting temperature. With increasing temperature the Fe 3 VFe 2 * ratio is shifted to Fe 2 * (9). The broad bands are attributed to more than one site of Fe 3 * and Fe 2 * (2, 3) and to the presence of other -\etai ions. Luminescence spectra reveal that minority species are efficient emitters indei special excitation (7-). ~igure 2 shows the luminescence emission spectra of the same FK90 glasses of Fi-J^re excitated at 230 nm. The normal melted glass has only weak luminescence bands. But he intensity of all luminescence bands increase with increasing melting temperature t glasses melted under reducing conditions. 'igure 2: Luminescence emission spectra of undoped glasses FK90 (to Fig. 1). 'K90 glasses doped with Cu demonstrate analogous effects (10): strongly decreasing bsorbance near 240 nm (Fig. 3) and increasing luminescence (Fig. 4) melted under educing conditions at increasing temperature. he Cu 2 VCu* ratio is shifted to Cu* with increasing reducing temperature; the uminescence emission of Cu* near 400 and 430 nm is strongly increased under educing conditions. η glass melted under normal conditions (air) at the same excitation condition no u' luminescence could be recognized. lass melted under reducing conditions at 1200¾ became an orange colour due to Cu 0 olloids. Supplement to "Rivista della Stazione Sperimentale del Vetro" Vol. XXIII,

4 Figure 3: Absorbance spectra of glass FK90 doped with 25 ppm Cu. Figure 4: Luminescence emission spectra of glasses FK90 doped with 25 ppm Cu. By means of luminescence spectroscopy it is possible to distinguish between the individual impurity content below 1 ppm of FK90 glasses melted under the same reducing conditions (Figure 5). At the excitation wavelength of 230 nm the band at 295 nm, is typical for the S > P luminescence of Pb 2 *, the band near 550 nm too. The double band near 400 nm is mainly due to Cu*. It increases used higher excitation wavelength at nm. Glass FK90. posses only the half of the Pb 2 * and Cu* content of the glass FK Supplement to "Rivista della Stazione Sperimentale del Vetro" Vol. XXIII, 1993

5 r unaamentals of Glass Science and Technology - ESG 1993, Venice Figure 5: Luminescence emission spectra of FK90 glasses melted under the same reducing conditions at 1100¾ used raw materials of different purity. By means of spectra simulation and separation of absorption band of doped and undoped FK90 $ glasses it is possible estimating the impurity content of individual ions at different redox states (Figure 6). The results are in good agreement with the values of chemical and luminescence analysis. "igure 6: Spectra simulation and separation. Supplement to "Rivista della Stazione Sperimentale del Vetro" Vol. XXIII,

6 First review of the contribution of the redox states of individual impurities to the total absorption loss in FK glasses is given in table 1. The values below 200 nm and from other metal ions will be determined in the next time. Table 1. Absorption wavelength and absorption coefficient for the redox states of metal impurities (cm" 1 per ppm) (E/d) Ion 1 / nm E/d / crrf! per ppm Fe 3 ' ,2-0,3 0,15-0,20 Fe 2 - < , 01 Cu 2 - < ,12 0, 001 Cu* < < 0,04 Pb 2 * 205 0, 11 CONCLUSIONS - Fe 3 ', Pb 2 * and Cu 2 * have a large influence on the UV absorption. Absorption coefficients between 0,1 and 0,2 cm" 1 per ppm were determined. - FK glasses melted under reducing conditions have much higher UV transmission at about 250 nm than glasses melted under oxidizing conditions. - The UV absorption of the glass is strongly dependent on the reducing temperature of the melt. - The UV absorption decreases and the luminescence increases drastically with increasing reducing temperature from 850 to 1100¾. The redox states are shifted to Fe 2 * and Cu', over 1100¾ to Cu colloids. - The absorption coefficients in the UV range of Fe 2 ' and Cu" are with 0,01 and < 0,04 one order lower than this of their high redox states. - Luminescence spectroscopy is an effective tool to distinguish between different redox states of transition metal ions and to estimate impurity contents, e. g. of Cu*, Pb 2 ', below 1 ppm. ACKNOWLEDGMENTS The authors wish to thank R. Atzrodt, M. Carl, T. Kittel and M. Müller for their assistance in experiments and helpful discussions. Work performed under the auspices of BMFT under contract number 03 M 2713 D Supplement to "Rivista delta Stazione Sperimentale del Vetro" Vol. XXIII, 1993

7 HEFERENCZS 1. IKRT D., ATZRODT R., VOGEL W. Struktur-Sigenschaftsbeziehungen optischer Gläser mit anomaler Teilc.ispenon. Proc.2nd Inc. Otto Schott: Colloquium July 1982 Jena, wiss. Z.?rieärich-5chiiier-Univ. Jena, Mach.-Naturwiss. Reihe 32 (1983) EHRT D., Mikkeleit W., 3urckhardt W., Mehner H. Proc. 2nd Int. Ernst-Abbe- Conference (EAC), Univ. Jena, KITAMURA N., HAYAKAWA J., YAMASHITA H. Optical properties of fluoroalumiaats glasses in the UV region. J. Non-Cryst. Sol. 126!190) EHRT D., Seeber W., Glass for high performance optics and laser technology. J. Non-Cryst. Sol. 129 (1991) COOK L., Mader K.-H. Ultraviolet Transmission Characteristics of a Fluorophosphate Laser Glass. J. Am. Ceram. Soc. 55 :1982) TOOK L., Liepmann M.J., Marker A.J. Large-scaie melting of fluorophosphate CDTICAI glasses. Sei. Forum :1987) WHITE W.3., KNIGHT D.S. Transition metal ion species in glass: A comparison of optical ADSORPTION and luminescence eviaence. Mater. Res. Soc. Proc. 51 (1986) Kloss T. Solarization and fluorescence phenomena in DUV-transmitting boron crown glass. SPIE Vol (1992) EHRT D. Structure and properties of fluoride phospnate glasses. SPIE Vol (1992) Seeber W., Ehrt D. Spectroscopic properties of Cu" and Tm-* in glasses, phys. stat. sol. (a) 130 ;1992) K Seeber W., Arnold P., Ehrt D. Luminescence properties ana energy transfer in Ce** and/or Tm 3 * doped fluoride phosphat\e glasses, phys. stat. sol. (a) 130 (1992) K

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