A lithium ion conductive solid electrolyte, L20-AI203-TiO2-SiO2-P20s glass with NASICON- type structure have been synthesized and transformed into glass-ceramic through thermal-treatment at various temperatures from 7...A lithium ion conductive solid electrolyte, L20-AI203-TiO2-SiO2-P20s glass with NASICON- type structure have been synthesized and transformed into glass-ceramic through thermal-treatment at various temperatures from 700 to 1 000 ~C for 12 h. The differential scanning calorimetry （DSC）, X-ray diffraction （XRD）, scanning electron microscopy （SEM） and complex impedance techniques were employed to characterize the samples. The experimental results indicated that the capability of glass forming in this system is superior to that of L20-A1203-TiO2-PzO~. The glass has an amorphous structure and resultant glass-ceramic mainly consisting of LiTi2（PO4）3 phases. Impurity phases AIPO4, TiO2, TiP207 and unidentified phase were observed. With the enhanced heat-treatment temperature, grain grew gradually and lithium ion conductivity of glass-ceramics increased accordingly, the related impedance semicircles were depressed gradually and even disappeared, which could be analytically explained by the coordinate action of the ＇Constant phase element＇ （CPE） model and the ＇Concept of Mismatch and Relaxation＇ model （CMR）. When the sample is devitrified at 1 000 ~C, the maximum room temperature lithium ion conductivity comes up to 4.1 x 10-4 S/cm, which is suitable for the application as an electrolyte of all-solid-state lithium batteries.展开更多
ZrO2, TiO2 and P2O5 were doped in CaO-B2O3-SiO2 glass-ceramics as nucleating additives. Effects of different nucleating additives on the phase separation and crystalline behaviors were investigated by using gradient t...ZrO2, TiO2 and P2O5 were doped in CaO-B2O3-SiO2 glass-ceramics as nucleating additives. Effects of different nucleating additives on the phase separation and crystalline behaviors were investigated by using gradient temperature furnace, DTA and XRD. Then, sintering process of the glass-ceramics was investigated by testing sintering shrinkage, dielectric constant and loss. The experimental results shows that the glass-ceramics doped with nucleating additives represents higher crystallization, with ZrO2 as an exceptional effective dopant to promote the precipitation of wollastonite crystal. Finally, ZrO2 containing glass-ceramics was chosen to study the influence of sintering temperature and soaking time with the help of X-ray diffraction analysis and density measurement. The glass-ceramics can be well consolidated at 850 ℃ for 10 min, with low dielectric constant （5.87） and loss （3.21×10^-4）, which is desirable for LTCC application.展开更多
Na2O-Al2O3-SiO2 glass-ceramics doped with Er^3＋ ions were synthesized by the conventional melt quenching technique at a low melting temperature.The samples were characterized by differential scanning calorimetry（DSC...Na2O-Al2O3-SiO2 glass-ceramics doped with Er^3＋ ions were synthesized by the conventional melt quenching technique at a low melting temperature.The samples were characterized by differential scanning calorimetry（DSC）,X-ray diffraction（XRD）,scanning electron microscopy（SEM）,UV-vis-NIR scanning spectrophotometry,and fluorescence spectrometry.The results show that the main crystalline phase of glass-ceramics is nepheline.The best heat-treatment process is at 520 ℃ for 2 h.Because the up-conversion luminescence and near infrared luminescence properties of glass doped with Eu^3＋ are studied in detail.展开更多
The crystallization behavior and mechanical properties of CaO-Al2O3-SiO2 (CAS) system glass-ceramics with addition of Y2O3 were investigated. The optimal sintering temperatures of all heat-treated glasses were altered...The crystallization behavior and mechanical properties of CaO-Al2O3-SiO2 (CAS) system glass-ceramics with addition of Y2O3 were investigated. The optimal sintering temperatures of all heat-treated glasses were altered and the crystallization was accelerated with Y2O3 addition, and only wollastonite as a main crystalline phase was precipitated. The volume fraction of crystalline phase and density were increased with Y2O3 addition. The results suggest that the CAS glass-ceramics would get the lowest sintering temperature and optimal microstructure with the addition of Y2O3 by 3.25 %. The bending strength has a maximum due to the oriented and interlocked wollastonite crystal, which causes crack divert or blunts to limit the further development of the flaw size and increases the surface energy of fracture.展开更多
基金National Basic Research Program of China (No.2009CB939704)National Natural Science Foundation of China (Nos.51032005, 60808024)the Fundamental Research Funds for the Central Universities (Wuhan University of Technology)
文摘A lithium ion conductive solid electrolyte, L20-AI203-TiO2-SiO2-P20s glass with NASICON- type structure have been synthesized and transformed into glass-ceramic through thermal-treatment at various temperatures from 700 to 1 000 ~C for 12 h. The differential scanning calorimetry （DSC）, X-ray diffraction （XRD）, scanning electron microscopy （SEM） and complex impedance techniques were employed to characterize the samples. The experimental results indicated that the capability of glass forming in this system is superior to that of L20-A1203-TiO2-PzO~. The glass has an amorphous structure and resultant glass-ceramic mainly consisting of LiTi2（PO4）3 phases. Impurity phases AIPO4, TiO2, TiP207 and unidentified phase were observed. With the enhanced heat-treatment temperature, grain grew gradually and lithium ion conductivity of glass-ceramics increased accordingly, the related impedance semicircles were depressed gradually and even disappeared, which could be analytically explained by the coordinate action of the ＇Constant phase element＇ （CPE） model and the ＇Concept of Mismatch and Relaxation＇ model （CMR）. When the sample is devitrified at 1 000 ~C, the maximum room temperature lithium ion conductivity comes up to 4.1 x 10-4 S/cm, which is suitable for the application as an electrolyte of all-solid-state lithium batteries.
基金Funded by the Shanghai Leading Academic Discipline Project (B502)Shanghai Key Laboratory Project (08DZ2230500)
文摘ZrO2, TiO2 and P2O5 were doped in CaO-B2O3-SiO2 glass-ceramics as nucleating additives. Effects of different nucleating additives on the phase separation and crystalline behaviors were investigated by using gradient temperature furnace, DTA and XRD. Then, sintering process of the glass-ceramics was investigated by testing sintering shrinkage, dielectric constant and loss. The experimental results shows that the glass-ceramics doped with nucleating additives represents higher crystallization, with ZrO2 as an exceptional effective dopant to promote the precipitation of wollastonite crystal. Finally, ZrO2 containing glass-ceramics was chosen to study the influence of sintering temperature and soaking time with the help of X-ray diffraction analysis and density measurement. The glass-ceramics can be well consolidated at 850 ℃ for 10 min, with low dielectric constant （5.87） and loss （3.21×10^-4）, which is desirable for LTCC application.
基金Funded by the National High Technology Research and Development Program of China(No.2011AA030204)Key Research Project of Jilin Provincial Science and Technology Department(No.20150204051GX)
文摘Na2O-Al2O3-SiO2 glass-ceramics doped with Er^3＋ ions were synthesized by the conventional melt quenching technique at a low melting temperature.The samples were characterized by differential scanning calorimetry（DSC）,X-ray diffraction（XRD）,scanning electron microscopy（SEM）,UV-vis-NIR scanning spectrophotometry,and fluorescence spectrometry.The results show that the main crystalline phase of glass-ceramics is nepheline.The best heat-treatment process is at 520 ℃ for 2 h.Because the up-conversion luminescence and near infrared luminescence properties of glass doped with Eu^3＋ are studied in detail.
文摘The crystallization behavior and mechanical properties of CaO-Al2O3-SiO2 (CAS) system glass-ceramics with addition of Y2O3 were investigated. The optimal sintering temperatures of all heat-treated glasses were altered and the crystallization was accelerated with Y2O3 addition, and only wollastonite as a main crystalline phase was precipitated. The volume fraction of crystalline phase and density were increased with Y2O3 addition. The results suggest that the CAS glass-ceramics would get the lowest sintering temperature and optimal microstructure with the addition of Y2O3 by 3.25 %. The bending strength has a maximum due to the oriented and interlocked wollastonite crystal, which causes crack divert or blunts to limit the further development of the flaw size and increases the surface energy of fracture.
