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
The crystallization behavior and kinetics of CaO-MgO-Al2O3 SiO2（CMAS） glass with the Fe2O3 content ranging from zero to 5%were investigated by differential scanning calorimetry（DSC）.The structure and phase analyse...The crystallization behavior and kinetics of CaO-MgO-Al2O3 SiO2（CMAS） glass with the Fe2O3 content ranging from zero to 5%were investigated by differential scanning calorimetry（DSC）.The structure and phase analyses were made by Fourier transform infrared spectroscopy（FT-IR） and X-ray diffraction（XRD）.The experiment results show that the endothermic peak temperature about 760℃ is associated with transition and the exothermic peak temperature about 1000℃ is associated with crystallization.The crystallization peak temperature decreases with increasing the Fe203 content.The crystallization mechanism is changed from two-dimensional crystallization to one-dimensional growth,and the intensity of diopside peaks becomes stronger gradually.There is a saltation for the crystallization temperature with the addition of 0.5%Fe2O3 due to the decomposition of Fe2O3.Si-O-Si,O-Si-O and T-O-T（T=Si,Fe,Al） linkages are observed in Fe2O3-CaO-MgO-Al2O3-SiO2 glass.展开更多
The effects of B2O3 addition on both the sintering behavior and microwave dielectric properties of CaO-B2O3-SiO2 （CBS） glass ceramics were investigated by Fourier transform infrared spectroscopy （FTIR）, X-ray diff...The effects of B2O3 addition on both the sintering behavior and microwave dielectric properties of CaO-B2O3-SiO2 （CBS） glass ceramics were investigated by Fourier transform infrared spectroscopy （FTIR）, X-ray diffractometry （XRD） and scanning electron microscopy （SEM）. The results show that the increasing amount of B203 causes the increase of the contents of [BO3], [BO4] and [SiO4], which deduces the increase of CaB204 and a-SiO2 and the decrease of CaSiO3 correspondingly. No new phase is observed throughout the entire experiments. A bulk density of 2.54 g/cm3, a thermal expansion coefficient value of 11.95× 10-6 ℃-1 （20-500℃）, a dielectric constant er value of 6.42 and a dielectric loss tanδ value of 0.000 9 （measured at 9.7 GHz） are obtained for CBS glass ceramics containing 35%-B203 （mass fraction） sintered at 850 ℃ for 15 min.展开更多
Through measuring the coefficient of linear expansion, the structure and properties of the Li2O-Al2O3-SiO2 low expansion glass ceramics containing B2O3 are studied by JR and XRD. It is shoutn that the IR method is eff...Through measuring the coefficient of linear expansion, the structure and properties of the Li2O-Al2O3-SiO2 low expansion glass ceramics containing B2O3 are studied by JR and XRD. It is shoutn that the IR method is efficient in the study of the glass-ceramics structure. There is a " Boron abnormality" in the system which has an important influence on the properties of the glass-ceramics.展开更多
CaO-B203-SiO2 （CBS） glass powders are prepared by conventional glass melting method at different melting temperatures whose properties and microstructures are characterized by X-ray diffraction （XRD） and scanning ...CaO-B203-SiO2 （CBS） glass powders are prepared by conventional glass melting method at different melting temperatures whose properties and microstructures are characterized by X-ray diffraction （XRD） and scanning electron microscopy （SEM）. It is found that there are SiO2 and some unknown phases in CBS glass melting liquid from 1 300 ℃ to 1 500 ℃ and the amount of these phases decreases with the increase of the melting temperature. The CBS glass melted at 1 450 ℃ could be sintered from 830 ℃ to 930 ℃ and the bulk densities of the samples are all higher than 2.4 g/cm^3. From the points of the properties and energy conservation, the melting temperature of 1 450 ℃ is the optimal melting temperature. The glass ceramic sintered at 850 ℃ exhibits better dielectric properties： er=6.33, tan6=2.2×10^-3 at 10 GHz, and the major phases of the samples are CaSiO3, CaB2O4 and SiO2.展开更多
A near infrared to visible blue, green, and red upconversion luminescence in a Tb^3＋-doped CaO-Al2O3-SiO2 glass was studied, which was excited using 800 nm femtosecond laser irradiation. The upconversion luminescence...A near infrared to visible blue, green, and red upconversion luminescence in a Tb^3＋-doped CaO-Al2O3-SiO2 glass was studied, which was excited using 800 nm femtosecond laser irradiation. The upconversion luminescence was attributed to ^5D3→^7F5, ^5D3→^7F4, ^5D3→^7F3, ^5D4→^7F6, ^5D4→^7F5, ^5D4→^7F4, and ^5D4→^7F3 transitions of Tb^3＋. The relationship between upconversion luminescence intensity and the pump power indicated that a three-photon simultaneous absorption process was dominant in this upconversion luminescence. The intense red, green, and blue upconversion luminescence of Tb^3＋-doped CaO-Al2O3-SiO2 glass may be potentially useful in developing three-dimensional display applications.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
B_2O_3-SiO_2-ZnO-BaO-Al_2O_3 glass with different Al_2O_3 contents（1mol%, 3mol%, 5mol%, and 7mol%） was prepared, and it was intended to be used as lead-free and low-melting glass sealants for solid oxide fuel cells....B_2O_3-SiO_2-ZnO-BaO-Al_2O_3 glass with different Al_2O_3 contents（1mol%, 3mol%, 5mol%, and 7mol%） was prepared, and it was intended to be used as lead-free and low-melting glass sealants for solid oxide fuel cells. The effects of Al_2O_3 content on the structures, thermal properties, and sintering behaviors of the B_2O_3-SiO_2-ZnO-BaO-Al_2O_3 glass were investigated in detail. The Al_2O_3 content largely influenced the structures and thermal properties of the glass. When the Al_2O_3 content 5mol%, the transition temperature of the glass decreased with the Al_2O_3 content, while the crystallization temperature increased with the Al_2O_3 content. However, higher Al_2O_3 content degraded the stability of the glass. The B_2O_3-SiO_2-ZnO-BaO-Al_2O_3 glass with 5 mol% Al_2O_3 content exhibits the optimal sintering densification characteristics and can be used as glass sealants for solid oxide fuel cells.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
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
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
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.
基金Projects(51264023,51364020,U1202271)supported by the National Natural Science Foundation of ChinaProject(IRT1250)supported by the Program for Innovative Research Team in University of Ministry of Education of ChinaProject(2014HA003)supported by the Science and Technology Leading Talent of Yunnan Province,China
文摘The crystallization behavior and kinetics of CaO-MgO-Al2O3 SiO2（CMAS） glass with the Fe2O3 content ranging from zero to 5%were investigated by differential scanning calorimetry（DSC）.The structure and phase analyses were made by Fourier transform infrared spectroscopy（FT-IR） and X-ray diffraction（XRD）.The experiment results show that the endothermic peak temperature about 760℃ is associated with transition and the exothermic peak temperature about 1000℃ is associated with crystallization.The crystallization peak temperature decreases with increasing the Fe203 content.The crystallization mechanism is changed from two-dimensional crystallization to one-dimensional growth,and the intensity of diopside peaks becomes stronger gradually.There is a saltation for the crystallization temperature with the addition of 0.5%Fe2O3 due to the decomposition of Fe2O3.Si-O-Si,O-Si-O and T-O-T（T=Si,Fe,Al） linkages are observed in Fe2O3-CaO-MgO-Al2O3-SiO2 glass.
基金Project(2007AA03Z0455) supported by the National High-Technology Research and Development Program of ChinaProject(BE2009168) supported by the Natural Science Foundation of Jiangsu Province in ChinaProject supported by the Priority Academic Program Development of Jiangsu Higher Education Institution,China
文摘The effects of B2O3 addition on both the sintering behavior and microwave dielectric properties of CaO-B2O3-SiO2 （CBS） glass ceramics were investigated by Fourier transform infrared spectroscopy （FTIR）, X-ray diffractometry （XRD） and scanning electron microscopy （SEM）. The results show that the increasing amount of B203 causes the increase of the contents of [BO3], [BO4] and [SiO4], which deduces the increase of CaB204 and a-SiO2 and the decrease of CaSiO3 correspondingly. No new phase is observed throughout the entire experiments. A bulk density of 2.54 g/cm3, a thermal expansion coefficient value of 11.95× 10-6 ℃-1 （20-500℃）, a dielectric constant er value of 6.42 and a dielectric loss tanδ value of 0.000 9 （measured at 9.7 GHz） are obtained for CBS glass ceramics containing 35%-B203 （mass fraction） sintered at 850 ℃ for 15 min.
文摘Through measuring the coefficient of linear expansion, the structure and properties of the Li2O-Al2O3-SiO2 low expansion glass ceramics containing B2O3 are studied by JR and XRD. It is shoutn that the IR method is efficient in the study of the glass-ceramics structure. There is a " Boron abnormality" in the system which has an important influence on the properties of the glass-ceramics.
基金Project(2007AA03Z0455) supported by the National High Technology Research and Development Program of ChinaProject(BE2010194) supported by Science&Technology Pillar Program of Jiangsu Province, China+1 种基金Project(KF201103) supported by the State Key Laboratory of New Ceramic and Fine Processing, Tsinghua University, ChinaProject supported by the Priority Academic Development of Jiangsu Higher Education Institutions, China
文摘CaO-B203-SiO2 （CBS） glass powders are prepared by conventional glass melting method at different melting temperatures whose properties and microstructures are characterized by X-ray diffraction （XRD） and scanning electron microscopy （SEM）. It is found that there are SiO2 and some unknown phases in CBS glass melting liquid from 1 300 ℃ to 1 500 ℃ and the amount of these phases decreases with the increase of the melting temperature. The CBS glass melted at 1 450 ℃ could be sintered from 830 ℃ to 930 ℃ and the bulk densities of the samples are all higher than 2.4 g/cm^3. From the points of the properties and energy conservation, the melting temperature of 1 450 ℃ is the optimal melting temperature. The glass ceramic sintered at 850 ℃ exhibits better dielectric properties： er=6.33, tan6=2.2×10^-3 at 10 GHz, and the major phases of the samples are CaSiO3, CaB2O4 and SiO2.
基金supported by the Education Department of Zhejiang Province (20050359)
文摘A near infrared to visible blue, green, and red upconversion luminescence in a Tb^3＋-doped CaO-Al2O3-SiO2 glass was studied, which was excited using 800 nm femtosecond laser irradiation. The upconversion luminescence was attributed to ^5D3→^7F5, ^5D3→^7F4, ^5D3→^7F3, ^5D4→^7F6, ^5D4→^7F5, ^5D4→^7F4, and ^5D4→^7F3 transitions of Tb^3＋. The relationship between upconversion luminescence intensity and the pump power indicated that a three-photon simultaneous absorption process was dominant in this upconversion luminescence. The intense red, green, and blue upconversion luminescence of Tb^3＋-doped CaO-Al2O3-SiO2 glass may be potentially useful in developing three-dimensional display applications.
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 Jiangxi Provincial Department of Education(KJLD13008)the National Natural Science Foundation of China(number 51362020)the Research Fund for the Doctoral Program of Higher Education(20123601110006)
文摘B_2O_3-SiO_2-ZnO-BaO-Al_2O_3 glass with different Al_2O_3 contents（1mol%, 3mol%, 5mol%, and 7mol%） was prepared, and it was intended to be used as lead-free and low-melting glass sealants for solid oxide fuel cells. The effects of Al_2O_3 content on the structures, thermal properties, and sintering behaviors of the B_2O_3-SiO_2-ZnO-BaO-Al_2O_3 glass were investigated in detail. The Al_2O_3 content largely influenced the structures and thermal properties of the glass. When the Al_2O_3 content 5mol%, the transition temperature of the glass decreased with the Al_2O_3 content, while the crystallization temperature increased with the Al_2O_3 content. However, higher Al_2O_3 content degraded the stability of the glass. The B_2O_3-SiO_2-ZnO-BaO-Al_2O_3 glass with 5 mol% Al_2O_3 content exhibits the optimal sintering densification characteristics and can be used as glass sealants for solid oxide fuel cells.
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.
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.
