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
X-ray powder diffraction and Fourier transform infrared spectroscopy were applied for characterization of Li2O-Al2O3-SiO2 glass-ceramic powders doped with Eu2O3,Gd2O3 and Er2O3,respectively,in the conditions of differ...X-ray powder diffraction and Fourier transform infrared spectroscopy were applied for characterization of Li2O-Al2O3-SiO2 glass-ceramic powders doped with Eu2O3,Gd2O3 and Er2O3,respectively,in the conditions of different heat-treatment temperatures and with various amounts.The powders were derived from the polyacrylamide gel method.The results show that,the wet gels prepared by polyacrylamide perform a unique crystallization behavior in the process of drying,comparing with some customary preparation such as melt processing.The main crystal phase and crystallization sequence of Li2O-Al2O3-SiO2 micro-powders have no distinct with addition of Eu2O3,Gd2O3 or Er2O3,while the crystallization temperature of the β-spodumene decreased and the amount of the β-spodumene increased.展开更多
In order to study the relationship between thickness and residual stress in CaO-Al2O3-SiO2 glass-ceramics.The residual stress was measured in CaO-Al2O3-SiO2 system glass-ceramic with different thickness,and the format...In order to study the relationship between thickness and residual stress in CaO-Al2O3-SiO2 glass-ceramics.The residual stress was measured in CaO-Al2O3-SiO2 system glass-ceramic with different thickness,and the formation mechanism and characterization of residual stress in CAS system Glass-ceramic were analyzed by the X-ray diffraction analysis.The experimental results show the compressive residual stress increass with thickness of glass-ceramic increasing.展开更多
The Sm^(3+)-doped SrO-Al2O3-SiO2(SAS) glass-ceramics with excellent luminescence properties were prepared by batch melting and heat treatment. The crystallization behavior and luminescent properties of the glass-...The Sm^(3+)-doped SrO-Al2O3-SiO2(SAS) glass-ceramics with excellent luminescence properties were prepared by batch melting and heat treatment. The crystallization behavior and luminescent properties of the glass-ceramics were investigated by DTA, XRD, SEM and luminescence spectroscopy. The results indicate that the crystal phase precipitated in this system is monocelsian(SrAl2Si2O) and with the increase of nucleation/crystallization temperature, the crystallite increases from 66 % to 79 %. The Sm(3+)-doped SAS glass-ceramics emit green, orange and red lights centered at 565, 605, 650 and 715 nm under the excitation of 475 nm blue light which can be assigned to the 4 G5/2→6 Hj/2(j=5, 7, 9, 11) transitions ofSm^(3+), respectively. Besides, by increasing the crystallization temperature or the concentration ofSm^(3+), the emission lights of the samples located at 565, 605 and 650 nm are intensified significantly. The present results demonstrate that theSm^(3+)-doped SAS glassceramics are promising luminescence materials for white LED devices by fine controlling and combining of these three green, orange and red lights in appropriate proportion.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X-ray powder diffraction and Fourier transform infrared spectroscopy were applied for characterization of Li2O-Al2O3-SiO2 glass-ceramic powders doped with Eu2O3,Gd2O3 and Er2O3,respectively,in the conditions of different heat-treatment temperatures and with various amounts.The powders were derived from the polyacrylamide gel method.The results show that,the wet gels prepared by polyacrylamide perform a unique crystallization behavior in the process of drying,comparing with some customary preparation such as melt processing.The main crystal phase and crystallization sequence of Li2O-Al2O3-SiO2 micro-powders have no distinct with addition of Eu2O3,Gd2O3 or Er2O3,while the crystallization temperature of the β-spodumene decreased and the amount of the β-spodumene increased.
文摘In order to study the relationship between thickness and residual stress in CaO-Al2O3-SiO2 glass-ceramics.The residual stress was measured in CaO-Al2O3-SiO2 system glass-ceramic with different thickness,and the formation mechanism and characterization of residual stress in CAS system Glass-ceramic were analyzed by the X-ray diffraction analysis.The experimental results show the compressive residual stress increass with thickness of glass-ceramic increasing.
基金Funded by the National Natural Science Foundation of China(No.5137217)Hubei Province Foreign Science and Technology Project(No.2016AHB027)Science and Technology Planning Project of Hubei Province(No.2014BAA136)
文摘The Sm^(3+)-doped SrO-Al2O3-SiO2(SAS) glass-ceramics with excellent luminescence properties were prepared by batch melting and heat treatment. The crystallization behavior and luminescent properties of the glass-ceramics were investigated by DTA, XRD, SEM and luminescence spectroscopy. The results indicate that the crystal phase precipitated in this system is monocelsian(SrAl2Si2O) and with the increase of nucleation/crystallization temperature, the crystallite increases from 66 % to 79 %. The Sm(3+)-doped SAS glass-ceramics emit green, orange and red lights centered at 565, 605, 650 and 715 nm under the excitation of 475 nm blue light which can be assigned to the 4 G5/2→6 Hj/2(j=5, 7, 9, 11) transitions ofSm^(3+), respectively. Besides, by increasing the crystallization temperature or the concentration ofSm^(3+), the emission lights of the samples located at 565, 605 and 650 nm are intensified significantly. The present results demonstrate that theSm^(3+)-doped SAS glassceramics are promising luminescence materials for white LED devices by fine controlling and combining of these three green, orange and red lights in appropriate proportion.