Plastic Sintering Behavior of Large-sized La2O3-TiO2-ZrO2 Amorphous Bulk

doi:10.15541/jim20180289

Abstract

Abstract:

La₂O₃-TiO₂-ZrO₂glass has great potential applications in lens and upconversion host materials for its ultrahigh refractive index. However, due to its low glass forming ability, it can only be prepared by some extremely rapid melt cooling method, which is hard to produce large-sized materials. On the basis of amorphous plastic behavior above the glass transition temperature T_g, large-sized La₂O₃-TiO₂-ZrO₂ bulk glasses were obtained by hot pressed sintering within the thermodynamic window ΔT. 30.8% LaO_3/2-59.2% TiO₂-10% ZrO₂ amorphous spheres were firstly prepared by aerodynamic levitation furnace. Whereafter, these spheres were smashed and ground into powders. Then these glass powders were hot pressed into a bulk glass with dimension of ?20 mm×1 mm. The effects of sintering temperature and pressure on the process of hot pressed sintering were investigated. Microstructures and phase compositions of samples were studied by SEM and XRD. The results show that the samples sintered above 910 ℃ contain a few La₄Ti₉O₂₄ crystal phases, while the samples sintered below 900 ℃ are totally amorphous. When the sintering temperature is below 900 ℃, the increase of sintering temperature in a certain range can reduce the number of pores apparently to improve the density of samples. And with the increase of pressure from 20 MPa to 60 MPa, the density of bulk glass prepared by hot pressing at 900 ℃ increases from 4.8797 g/cm ³ to 5.1178 g/cm ³. The large-sized La₂O₃-TiO₂-ZrO₂ glass displays excellent optical performance with refractive index of 2.33 at the wavelength of 587.6 nm and the abbe number of 13.2. By analyzing the shrinkage curve of the samples, it is confirmed that the plastic flow is the main mass transfer way during densification process.

Key words: containerless method, amorphous, hot-pressed sintering, densification, plastic flow

CLC Number:

TQ174

Zhui WANG, Jian-Jun HAN, Jian-Qiang LI, Xiao-Yu LI, Jiang-Tao LI, Gang HE, Jun XIE. Plastic Sintering Behavior of Large-sized La₂O₃-TiO₂-ZrO₂ Amorphous Bulk[J]. Journal of Inorganic Materials, 2019, 34(4): 433-438.

Figures/Tables 8

Fig. 1 XRD pattern of the La2O3-TiO2-ZrO2 powders prepared by containerless method

Fig. 2 DTA results of La2O3-TiO2 and La2O3-TiO2-ZrO2 glass powders

Fig. 3 XRD patterns of the LTZO samples sintered at different temperatures

Fig. 4 Fracture SEM images of LTZO bulk glasses prepared by hot press sintering at different temperatures (a) 890 ℃; (b) 900 ℃; (c) 910 ℃

Fig. 5 Shrinkage behaviors of LTZO glass powders sintered at different pressures The inset shows the densities of LTZO samples sintered at different pressures

Fig. 6 Fracture SEM images of LTZO bulk glasses prepared by hot press and sintering at different pressures (a) 20 MPa; (b) 40 MPa; (c) 60 MPa

Fig. 7 Refractive index curves of LTO and LTZO samples obtained by hot-pressed sintering

Fig. 8 ln[1/(1-θ)]~t curve of LTZO samples in densification process

References 20

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Plastic Sintering Behavior of Large-sized La₂O₃-TiO₂-ZrO₂ Amorphous Bulk

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