SiO2 Soot Body at Vacuum Sintering Process: Densification and Transparency Mechanism

doi:10.15541/jim20180603

Abstract

Abstract:

Low density and amorphous SiO₂ soot body was prepared by chemical vapor deposition. Its macro deformation and micro-structure evolution rule in the sintering process were characterized by TG-DSC, SEM, TEM, XRD, mercury intrusion method, nitrogen adsorption method, and high temperature melting observation system, etc. The results indicated that SiO₂ soot body began to shrink at the sintering temperature of 1000 ℃. The macro scale soot body stopped shrinking when the sintering temperature rose to 1200 ℃, with 30% ratios shrinkage. When the sintering temperature was higher than 1200 ℃, the small particles of SiO₂ started to melt. There is a clear transition boundary between solid-phase soot body and liquid-phase glass body when the sintering temperature is higher than 1250 ℃. Meanwhile, it is interesting that the pores shape of soot body evolved gradually from connective to isolated, spherical and hole-closed. When the sintering temperature reached 1500 ℃, but the transparent silica glass is obtained without pores. More importantly, the state of SiO₂ soot body remains amorphous throughout the sintering process.

Key words: SiO₂ soot body, vacuum sintering, pore structure, densification, transparency

CLC Number:

TQ174

NIE Lan-Jian, GU Zhen-An, WANG Yu-Fen, XIANG Zai-Kui, ZHANG Chen-Yang, RAO Chuan-Dong. SiO₂ Soot Body at Vacuum Sintering Process: Densification and Transparency Mechanism[J]. Journal of Inorganic Materials, 2019, 34(10): 1060-1066.

Figures/Tables 13

Fig. 1 TG-DSC curves of SiO2 soot body

Fig. 2 Photographs of intact SiO2 soot body and sintered body under 1500 ℃ and vacuum condition

Fig. 3 In-situ dynamic sintering photographs of SiO2 soot body

Fig. 4 SEM images of SiO2 soot bodies sintered at different temperatures

Fig. 5 TEM images of unsintered SiO2 soot bodies

Fig. 6 Schematic of neck formation and growth of SiO2 soot body during the sintering process[16]

Fig. 7 Corrdinates for a closed pore initiated in viscous glass[17]

Fig. 8 Temperature dependence of viscosity of clear silica glass[18]

Fig. 9 XRD patterns of SiO2 soot bodies sintered at different temperatures

Fig. 10 Cumulative intrusion volume curves of SiO2 soot bodies sintered at different temperatures

Fig. 11 Pore size distribution curves of SiO2 soot bodies sintered at different temperatures

Table 1 Data analysis of pore structure of SiO2 soot bodies by mercury porosimetry

Sample	Pore volume/ (mL?g^-1)	Surface area/ (m²?g^-1)	Porosity/%	Average pore size/nm	Median pore diameter (Volume)/nm	Median pore diameter (Area)/nm
A (1250 ℃)	0.03	3.36	3.50	30.76	288.10	10.39
B (1000 ℃)	3.80	78.79	56.70	192.90	468.80	118.50
C (Unsintered)	5.33	60.55	67.52	351.90	10059.40	114.20

Fig. 12 Spectral transmittance curves of transparent sample of SiO2 soot body

References 18

[1]	NIE L J, JIA Y N, WANG L ,et al. Microstructural study on the low density SiO₂ soot body. Key Engineering Materials, 2017,726:383-387.
[2]	MARTIN T, STEFAN O, STEFFEN Z ,et al.Method for Producing an Optical Component Made of Quartz Glass. Germany, C03B19/14, DE112008003728T5. 2011. 03. 03.
[3]	STEFAN O, KLAUS B . Method for Producing a Blank from Titanium- and Fluorine-doped Glass Having a High Silicic-acid Content. USA, C03B19/14, US2017/0217814A2. 2017. 08. 03.
[4]	ACHIM H, THOMAS K, MATTHIAS O ,et al. Method for Producing Synthetic Quartz Glass of SiO₂ Granulate and SiO₂ Granulate Suited Therefor. USA, C03B19/066, US10029938B2. 2018. 07. 24.
[5]	KLAUS B, STEFAN O, STEPHAN T . Blank Made of Titanium- doped Silica Glass and Method for the Production Thereof. USA, C03C3/06, US9540271B2. 2017. 01. 10.
[6]	STEVEN B D, LISA A H, KENNETH E H ,et al. Basic Additives for Silica Soot Compacts and Methods For Forming Optical Quality Glass.USA, C03C3/06, US2018/0148366A1. 2018. 05. 31.
[7]	SEZHIAN A, CARLOS A D, KENNETH E H . Doped Ultra-low Expansion Glass and Methods for Making the Same.USA, C03C3/ 06, US9611169B2. 2017. 04. 04.
[8]	DANIEL R B, CHRISTOPHER S T, WANG J . Methods and Apparatuses for Forming Optical Preforms from Glass Soot. USA, C03B37/014, US9376338B2. 2016. 06. 28.
[9]	DANIEL W H, ERIC J M . Locally-sintered Porous Soot Parts and Methods of Forming. USA, C03B19/06, US9452946B2. 2016. 09. 27.
[10]	KASHIWAGI Y, OTSUSAKA T . Soot Deposition Body Manufacturing Apparatus and Manufacturing Method. USA, C03B37/ 0142, US2018/0050950A1. 2018. 02. 02.
[11]	MAKOTO Y. MAKOTOY . Porous Glass Preform Production Apparatus. USA, C03B37/014, US8656743. 2014. 02. 25.
[12]	SANTOS J S, ONO E ,SUZUKI C K . Effect of the nanostructure control on the novel optical properties of silica photonic glass synthesized by VAD method. Materials Science Forum, 2010,636- 637:361-368.
[13]	SANTOS J S, EDMILTON GUSKEN, ONO E , , et al. EXAFS. EXAFS and XANES study of annealed VAD silica glass. Photon Factory Activity Report, 2007: 11B/2006P020-1.
[14]	SANTOS J S, ONO E, FUJIWARA E ,et al. Ultra-low Birefringence Silica Glass Synthesized by VAD Method for Photonic Components for UV Photolithography. 11^th International Conference on Advanced Materials,Rio de Janeiro Brazil, 2009. 1.
[15]	SANTOS J S, ONO E, FUJIWARA E ,et al. Control of optical properties of silica glass synthesized by VAD method for photonic components. Optical Materials, 2011,33(12):1879-1883.
[16]	ROBERT W B, SAMUEL M A, CARTER W C . Kinetics of Materials. New Jersey: John Wiley & Sons,Inc., 2005,417.
[17]	SAKAGUCHI S . Behavior of closed pores formed in consolidation process for silica soot precursor. Journal of Non-Crystalline Solids, 1995,189(1/2):43-49.
[18]	FANDERLIK I . Silica Glass and Its Application. Amsterdam: Elsevier, 1991: 218.

SiO₂ Soot Body at Vacuum Sintering Process: Densification and Transparency Mechanism

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