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
ZrO2-mullite nano-ceramics were fabricated by in-situ controlled crystallizing from SiO2-Al2O3-ZrO2 amorphous bulk. The thermal transformation sequences of the SiO2-Al2O3-ZrO2 amorphous bulk were investigated by X-ray...ZrO2-mullite nano-ceramics were fabricated by in-situ controlled crystallizing from SiO2-Al2O3-ZrO2 amorphous bulk. The thermal transformation sequences of the SiO2-Al2O3-ZrO2 amorphous bulk were investigated by X-ray diffraction, infrared spectrum, scanning electron microscope and differential scanning calorimetric. And the mechanical properties of the nano-ceramics were studied. The results show that the bulks are still in amorphous state at 900 ℃ and the t-ZrO2 forms at about 950 ℃ with a faint spinel-like phase which changes into mullite on further heating. ZrO2 and mullite become major phases at 1 100 ℃ and an amount of m-ZrO2 occur at the same time. The sample heated at 950 ℃ for 2 h and then at 1 100 ℃ for 1 h shows very dense and homogenous microstructure with ball-like grains in size of 20-50 nm. With the increase of crystallization temperature up to 1 350 ℃, the grains grow quickly and some grow into lath-shaped grains with major diameter of 5 μm. After two-step treatment the highest micro-hardness, flexural strength and fracture toughness of the samples are 13.72 GPa, 520 MPa and 5.13 MPa·m1/2, respectively.展开更多
SiO2-Al2O3-ZrO2 glasses with different nucleating agents were crystallized under special processing schedule. The microstructure and mechanical properties of the glass-ceramics in SiO2-Al2O3-ZrO2 system were investiga...SiO2-Al2O3-ZrO2 glasses with different nucleating agents were crystallized under special processing schedule. The microstructure and mechanical properties of the glass-ceramics in SiO2-Al2O3-ZrO2 system were investigated by differential scanning calorimetry, scanning electron microscopy, X-ray diffraction and three-point bending method. The results show that ZrO2 is not an effective nucleating agent in SiO2-Al2O3-ZrO2 system, while TiO2 is effective for the separation of spinel, and P2O5 facilitates solubility of ZrO2 in glass and crystallization. The main crystalline phases of the glass-ceramics are spinel, anorthite and tetragonal zirconia. With the increase of ZrO2 content in the glass, glass-ceramics show higher bending strength (120MPa) than others.展开更多
Composite powders of nanocrystalline WC-10Co (15wt%),Y2O3 (8mol%) stabilized nanocrystalline ZrO2 (30wt%),industrial cobalt powder (4.5wt%) and submicron Al2O3 (55wt%) composite powders were fabricated by hi...Composite powders of nanocrystalline WC-10Co (15wt%),Y2O3 (8mol%) stabilized nanocrystalline ZrO2 (30wt%),industrial cobalt powder (4.5wt%) and submicron Al2O3 (55wt%) composite powders were fabricated by high-energy ball-milling process.The nanocomposite powders were consolidated by microwave sintering process at temperature ranged 1300℃-1550℃ for 15min,respectively.The optimum consolidation conditions,such as temperature,were researched during microwave sintering process.Vickers Hardness of the consolidated cermets was measured by using a Vickers indentation test,and density of specimens was also determined by Archimedes' principle.Microwave sintering process could not only increase the density of Al2O3-ZrO2-WC-Co cermets and reduce the porosity,but also inhibit abnormal grain growth.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Project(2003AA332040) supported by the National High Technology Research and Development Program of China
摘要ZrO2-mullite nano-ceramics were fabricated by in-situ controlled crystallizing from SiO2-Al2O3-ZrO2 amorphous bulk. The thermal transformation sequences of the SiO2-Al2O3-ZrO2 amorphous bulk were investigated by X-ray diffraction, infrared spectrum, scanning electron microscope and differential scanning calorimetric. And the mechanical properties of the nano-ceramics were studied. The results show that the bulks are still in amorphous state at 900 ℃ and the t-ZrO2 forms at about 950 ℃ with a faint spinel-like phase which changes into mullite on further heating. ZrO2 and mullite become major phases at 1 100 ℃ and an amount of m-ZrO2 occur at the same time. The sample heated at 950 ℃ for 2 h and then at 1 100 ℃ for 1 h shows very dense and homogenous microstructure with ball-like grains in size of 20-50 nm. With the increase of crystallization temperature up to 1 350 ℃, the grains grow quickly and some grow into lath-shaped grains with major diameter of 5 μm. After two-step treatment the highest micro-hardness, flexural strength and fracture toughness of the samples are 13.72 GPa, 520 MPa and 5.13 MPa·m1/2, respectively.
摘要SiO2-Al2O3-ZrO2 glasses with different nucleating agents were crystallized under special processing schedule. The microstructure and mechanical properties of the glass-ceramics in SiO2-Al2O3-ZrO2 system were investigated by differential scanning calorimetry, scanning electron microscopy, X-ray diffraction and three-point bending method. The results show that ZrO2 is not an effective nucleating agent in SiO2-Al2O3-ZrO2 system, while TiO2 is effective for the separation of spinel, and P2O5 facilitates solubility of ZrO2 in glass and crystallization. The main crystalline phases of the glass-ceramics are spinel, anorthite and tetragonal zirconia. With the increase of ZrO2 content in the glass, glass-ceramics show higher bending strength (120MPa) than others.
基金Funded by the Youth Science Plan for Light of the Morning Sun of Wuhan City (200750731270)
摘要Composite powders of nanocrystalline WC-10Co (15wt%),Y2O3 (8mol%) stabilized nanocrystalline ZrO2 (30wt%),industrial cobalt powder (4.5wt%) and submicron Al2O3 (55wt%) composite powders were fabricated by high-energy ball-milling process.The nanocomposite powders were consolidated by microwave sintering process at temperature ranged 1300℃-1550℃ for 15min,respectively.The optimum consolidation conditions,such as temperature,were researched during microwave sintering process.Vickers Hardness of the consolidated cermets was measured by using a Vickers indentation test,and density of specimens was also determined by Archimedes' principle.Microwave sintering process could not only increase the density of Al2O3-ZrO2-WC-Co cermets and reduce the porosity,but also inhibit abnormal grain growth.