针对光固化Al2O3陶瓷在脱脂烧结后易形成孔洞、力学性能差的问题,系统研究了石墨烯添加对陶瓷浆料流变性、沉降性、固化行为及烧结体力学性能的影响。采用γ-缩水甘油醚氧丙基三甲氧基硅烷(KH560)对Al2O3粉体进行表面改性,并加入不同含...针对光固化Al2O3陶瓷在脱脂烧结后易形成孔洞、力学性能差的问题,系统研究了石墨烯添加对陶瓷浆料流变性、沉降性、固化行为及烧结体力学性能的影响。采用γ-缩水甘油醚氧丙基三甲氧基硅烷(KH560)对Al2O3粉体进行表面改性,并加入不同含量的石墨烯,制备高固相、低粘度的光固化浆料。通过傅里叶红外光谱、旋转流变仪、沉降试验及Beer-Lambert模型分析,优化了浆料配方与光固化工艺参数。结果表明:当KH560含量为2.5wt%、石墨烯含量为0.01wt%时,浆料粘度最低、沉降分层最少;在曝光时间4 s条件下,添加0.01wt%石墨烯的浆料透射深度为382μm,临界曝光能量为44.3 m J/cm2。经1750℃烧结后,陶瓷零件致密度达99.7%,弯曲强度为27.61 MPa,维氏硬度为13.45GPa。石墨烯通过位阻效应及裂纹偏转机制有效促进了烧结致密化并改善了力学性能。本研究为光固化增材制造高致密、高性能氧化铝陶瓷提供了试验依据。展开更多
The ineluctable introduction of lithium salt to polymer solid-state electrolytes incurs a compromise between strength,ionic conductivity,and thickness.Here,we propose Al2O3-coated polyimide(AO/PI)porous film as ...The ineluctable introduction of lithium salt to polymer solid-state electrolytes incurs a compromise between strength,ionic conductivity,and thickness.Here,we propose Al2O3-coated polyimide(AO/PI)porous film as a high-strength substrate to support fast-ion-conducting polymer-in-salt(PIS)solid-state electrolytes,aiming to suppress lithium dendrite growth and improve full-cell performance.The Al2O3coating layer not only refines the wettability of polyimide porous film to PIS,but also performs as a high modulus protective layer to suppress the growth of lithium dendrites.The resulting PI/AO@PIS exhibits a small thickness of only 35μm with an outstanding tensile strength of 11.3 MPa and Young's modulus of 537.6 MPa.In addition,the PI/AO@PIS delivers a high ionic conductivity of 0.1 m S/cm at 25°C.As a result,the PI/AO@PIS enables symmetric Li cells to achieve exceptional cyclability for over 1000 h at 0.1 m A/cm2without noticeable lithium dendrite formation.Moreover,the PI/AO@PIS-based LiFePO4||Li full cells demonstrate outstanding rate performance(125.7 m Ah/g at 5 C)and impressive cycling stability(96.1%capacity retention at 1 C after 200 cycles).This work highlights the efficacy of enhancing the mechanical properties of polymer matrices and extending cell performance through the incorporation of a dense inorganic interface layer.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
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 tem...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
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
摘要针对光固化Al2O3陶瓷在脱脂烧结后易形成孔洞、力学性能差的问题,系统研究了石墨烯添加对陶瓷浆料流变性、沉降性、固化行为及烧结体力学性能的影响。采用γ-缩水甘油醚氧丙基三甲氧基硅烷(KH560)对Al2O3粉体进行表面改性,并加入不同含量的石墨烯,制备高固相、低粘度的光固化浆料。通过傅里叶红外光谱、旋转流变仪、沉降试验及Beer-Lambert模型分析,优化了浆料配方与光固化工艺参数。结果表明:当KH560含量为2.5wt%、石墨烯含量为0.01wt%时,浆料粘度最低、沉降分层最少;在曝光时间4 s条件下,添加0.01wt%石墨烯的浆料透射深度为382μm,临界曝光能量为44.3 m J/cm2。经1750℃烧结后,陶瓷零件致密度达99.7%,弯曲强度为27.61 MPa,维氏硬度为13.45GPa。石墨烯通过位阻效应及裂纹偏转机制有效促进了烧结致密化并改善了力学性能。本研究为光固化增材制造高致密、高性能氧化铝陶瓷提供了试验依据。
基金the financial support from the 261Project of MIIT and Natural Science Foundation of Jiangsu Province(No.BK20240179)。
摘要The ineluctable introduction of lithium salt to polymer solid-state electrolytes incurs a compromise between strength,ionic conductivity,and thickness.Here,we propose Al2O3-coated polyimide(AO/PI)porous film as a high-strength substrate to support fast-ion-conducting polymer-in-salt(PIS)solid-state electrolytes,aiming to suppress lithium dendrite growth and improve full-cell performance.The Al2O3coating layer not only refines the wettability of polyimide porous film to PIS,but also performs as a high modulus protective layer to suppress the growth of lithium dendrites.The resulting PI/AO@PIS exhibits a small thickness of only 35μm with an outstanding tensile strength of 11.3 MPa and Young's modulus of 537.6 MPa.In addition,the PI/AO@PIS delivers a high ionic conductivity of 0.1 m S/cm at 25°C.As a result,the PI/AO@PIS enables symmetric Li cells to achieve exceptional cyclability for over 1000 h at 0.1 m A/cm2without noticeable lithium dendrite formation.Moreover,the PI/AO@PIS-based LiFePO4||Li full cells demonstrate outstanding rate performance(125.7 m Ah/g at 5 C)and impressive cycling stability(96.1%capacity retention at 1 C after 200 cycles).This work highlights the efficacy of enhancing the mechanical properties of polymer matrices and extending cell performance through the incorporation of a dense inorganic interface layer.
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
摘要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Funded by the Shanghai Leading Academic Discipline Project(B502)Shanghai Key Laboratory Project(08DZ2230500)
摘要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
摘要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
摘要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.