Low OH content germanate glass prepared by batch soaking process in CCl 4

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18 8 2008 8 Vol.18 No.8 The Chinese Journal of Nonferrous Metals Aug. 2008 1004-0609(2008)08-1504-08 ( 410083) CCl 4 40GeO 2-30SiO 2-12Al 2 O 3-6BaO-6CaO-6MgO OH 3 338 /cm (3.0 µm) Gauss 5 OH 1.71 /cm OH 0.25 /cm DTA XRD OH TB 321 A Low OH content germanate glass prepared by batch soaking process in CCl 4 XIAO Zhuo-hao, CHEN Yuan-yuan, ZUO Cheng-gang, LU An-xian (School of Materials Science and Engineering, Central South University, Changsha 410083, China) Abstract: 40GeO 2-30SiO 2-12Al 2 O 3-6BaO-6CaO-6MgO glass was prepared by using batch soaking process with CCl 4 as dehydration agent. The influence of this process on the infrared transmittance and crystallization behavior of the germanium glass was investigated. The results show that the infrared spectra contains a single band at approximately 3 338 /cm for the germanate glass. This broad absorption band is deconvoluted into five bands and some possible reasons for each band have been given. The absorption coefficient of hydroxyl in the germanate glass prepared by conventional melt quenching technique is 1.71 /cm while that of the one prepared by batch soaking process in CCl 4 is 0.25 /cm. The analyses of DTA and XRD indicate that the glass prepared by batch soaking process crystallizes at lower temperature and has bigger crystallization rate for the residual chlorine acting as a nucleation agent in the interspaces of the glass network structure. The SEM images show that the residual chlorine promotes the formation of crystallite and changes the shape of the crystallite cluster. Key words: germanate glass; infrared transmittance; crystallization; OH absorption; batch soaking process DENNIS LAUBENGAYER [1] 1926 (JPPT-115-332) 2007-12-27 2008-04-23 0731-8830351 E-mail: axlu@mail.csu.edu.cn

18 8 1505 [2] [3] [4] (Reaction atmosphere process, RAP [5 8] ) [9 10] [9, 11] [9 10, 12 14] [15] CCl 4 POCl 4 SOCl 2 [16] CCl 4 YANG [8] Er 3+ OH 15.39 /cm 0.28 /cm ZHAI [17] Nd 2 O 3 Al 2 O 3 -SiO 2 CCl 4 OH 150 10 6 10 10 6 WANG [18] CCl 4 OH MARTUCCI [19] SOKOLNICKI [20] LI [11] CCl 4 [21 22] (BSP Batch soaking process) CCl 4 1 1.1 1 CCl 4 CCl 4 10 min 1 (BSP) Fig.1 Schematic diagram of experimental apparatus for BSP CCl 4 600 1 h 2H 2 O+CCl 4 4HCl+CO 2 (1) 2HO + CCl 4 2HCl + CO 2 + 2Cl (2) CCl 4 H 2 O OH H 2 O OH H 2 O 1.2 40GeO 2-30SiO 2-12Al 2 O 3-6BaO-6CaO- 6MgO ( %) GeO 2 5 N 149 µm 200 g 10 h A B A B 600 1 h 1 580 3 h 600 2 h 1.3 1.3.1 (IR)

1506 2008 8 15 mm 15 HOSONO [23] Na 2 O( ) mm 3 mm 240 SiC 0 5% 28% OH 0.06 µm 3 550 /cm Na 2 O Perkin 5% 3 300 /cm 28% 2 800 2 350 /cm HALL Elmer Lanbda 900UV/VIS/NIR [24] Na Thermo Nicolet Nexus FT IR 2 O 0~10% OH 3 560 /cm 3 450 /cm Na 2 O 400 /cm 10 000 /cm 10% 2 800 2 350 /cm 1.3.2 (DTA) 2 800 /cm 2 TAS100 DTA 350 /cm 2 10 /min 25~1 000 Gauss 3 1.3.3 X (XRD) 3014 X X 149 µm 1.3.4 (SEM) 4%HF 80 s X 650 2 2.1 BSP BSP 2 A B 80% 5 µm 3 338 /cm OH 2 Fig.2 IR absorption profile of samples A and B 3 OH Fig.3 Spectral deconvolution of IR absorbance of samples A and B: (a) 3 338 /cm; (1) 3 560 /cm; (2) 3 473 /cm; (3) 3 340 /cm; (4) 3 138 /cm; (5) 2 859 /cm A 3 338 /cm 3 560 3 473 3 340 3 138 2 859 /cm 5 Gauss 4 3 560 /cm OH (Fig.4(a)) OH 3 672 /cm [24] PLOTNICHENKO [25] 3 473 /cm 3 138 /cm OH 3 473 /cm 3 340 /cm OH (Fig.4(b)) (Fig.4(c)) 3 138 /cm OH (Fig.4(d)) 2 859 /cm

18 8 1507 4 OH Fig.4 Hydroxyl in different configurations in germanate glass MCMILLAN [26] ENGHOLM [27] IR Raman 2 859 /cm [21 22] Ge [22, 28 29] Ge O OH Ge O (Fig.4(e)) B OH Gauss 3 560 3 473 3 340 3 138 /cm 2 859 /cm BSP OH Lambert-Beer 3 OH OH OH 3 338 /cm α(oh) OH 1 T0 α(oh) = ln( ) (3) L T L cm T 0 T 3 338 /cm (3) α(oh) A =1.71 /cm α(oh) B =0.25 /cm BSP OH BSP OH α(oh) 1.71 /cm OH α(oh) 0.25 /cm OH 26.28% 72.41% 2.2 BSP 5 DTA DTA BSP A 641 756 783 BSP B 620 732 779 BSP 20 OH [2] BSP B OH BSP

1508 2008 8 6 730 1 h Fig.6 Photograph of glass samples at 730 for 1 h 5 DTA Fig.5 DTA curves of glass samples A OH B A DTA BSP OH 5 DTA BSP B 897 B [12] B CCl 4 (2) CCl 4 [30] DTA BSP XRD 6 730 730 A B B A 7(a) 730 XRD A A B PDF (19-0015) (Ge 2 Al 6 O 13 ) XRD BSP 6 750 XRD 7(b) A B B 750 730 A B 800 A B MgGeO 3 ( 7(c)) B BaMgSi 900 ( 7(d)) A B BaMgSi 7 B A DTA ( 5) B A 900 B 7(d) A B X XRD 2.3 SEM 8 9 730 1 h 50~80 nm BSP A BSP

18 8 1509 7 XRD Fig.7 XRD patterns of glass samples under different thermal condition: (a) 730, 1 h; (b) 750, 1 h; (c) 800, 1 h; (d) 900, 1 h 8 A 730 1 h SEM Fig.8 SEM photograph of sample A at 730 for 1 h 9 B 730 1 h SEM Fig.9 SEM photograph of sample B at 730 for 1 h BSP HAN [30] 3 1) CCl 4

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