机械合金化2Si-B-3C-N陶瓷的热压烧结行为与高温性能研究
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摘要
Si-B-C-N陶瓷因其优异的组织稳定性、抗高温蠕变和抗氧化等性能而逐渐成为陶瓷材料领域研究的热点之一，在航空、航天、冶金、能源、信息、微电子等领域具有广泛的应用前景。目前，Si-B-C-N陶瓷的制备方法主要包括有机聚合物前驱体裂解、物理气相沉积和机械合金化三种。其中机械合金化法因其采用的原料无毒，工艺简单，材料成本低廉，有利于制备致密块体陶瓷而受到研究人员的重视。目前，采用该方法可以较为容易地制备出室温弯曲强度约为300-500MPa，晶粒尺寸约为200-500nm的Si-B-C-N复相陶瓷。但该方法仍存在一些亟待深入研究的问题。例如，对非晶态Si-B-C-N粉末的微观结构、烧结行为、晶化过程，以及对陶瓷的组织演变规律尚不清楚；对陶瓷材料高温性能的研究尚需进一步加深等。本文针对上述问题，以c-Si、h-BN和石墨粉末为原料，采用行星式高能球磨机制备非晶态2Si-B-3C-N粉末，然后采用热压烧结工艺对该粉末进行烧结。采用X射线衍射、透射电镜、扫描电镜、激光粒度分析、热重-差热分析（TG-DTA）、力学性能测试等方法深入研究非晶态2Si-B-3C-N粉末的微观结构、烧结工艺、在热压烧结过程中的晶化行为，以及所制备陶瓷的微观结构和高温性能，进一步探讨采用机械合金化和热压烧结工艺制备Si-B-C-N陶瓷的可行性。
研究发现，采用本文所用原料及机械合金化工艺制备的非晶态2Si-B-3C-N粉末由近似球形的纳米颗粒硬团聚体构成，团聚体的平均粒径约为5μm；采用不同球磨工艺参数制备的非晶态2Si-B-3C-N粉末具有相似的粒度分布、表面结构及组织热稳定性；当球磨罐转速高于600rpm或球料质量比大于20:1时，会促使非晶组织发生晶化并生成尺寸约为1-5nm的SiC晶体。30h或40h的球磨时间有利于硅与碳原子之间反应成键，并且此时粉末中的非晶态组织没有发生明显的晶化；当非晶态2Si-B-3C-N粉末在氮气氛中被加热至约1000℃以上时，在粉末的表面出现SiC纳米线的生长现象；当被加热至约1350℃时，粉末因为表面氧化膜的碳热还原反应而快速生成并释放出CO或CO2气体。
在80MPa下热压烧结，当温度高于约1830℃时，非晶态2Si-B-3C-N粉末将发生快速的致密化。在1900℃/80MPa/30min/8bar N_2条件下热压烧结制备的2Si-B-3C-N复相陶瓷体积密度和相对密度，以及室温弯曲强度、弹性模量、断裂韧性和维氏硬度分别约为2.52g/cm~3，88.7%，331.1MPa，139.4GPa，2.81MPa·m~(1/2)和5.65GPa。当烧结温度降至1800℃或压力降至50MPa时，所制备材料的密度和力学性能会急剧下降。5mol%ZrO2或AlN添加剂使陶瓷坯体在相同工艺条件下发生快速烧结致密化的温度分别降低至约1720℃和1760℃，陶瓷材料的相对密度分别增至约97.7%和96.9%，室温弯曲强度分别增至约575.4MPa和415.7MPa。
在80MPa/30min/8bar N_2条件下热压烧结时，非晶态2Si-B-3C-N粉末的起始晶化温度约为1485℃。SiC和BN(C)通过各自密排面有序堆垛、相邻晶粒合并等方式实现晶粒生长。在1900℃/80MPa/30min/8bar N_2条件下热压烧结制备的2Si-B-3C-N陶瓷由平均晶粒尺寸小于100nm，且分布均匀的β-SiC、α-SiC和BN(C)构成。BN(C)相具有湍层结构，由分布不均匀的湍层氮化硼，湍层碳，以及B原子固溶的湍层碳和C原子固溶的湍层氮化硼等原子层构成。
热压烧结制备的纳米2Si-B-3C-N复相陶瓷具有优异的高温组织稳定性、高温抗蠕变性能和抗氧化性能。在1800℃/1bar N_2条件下保温处理3h后，材料的组织结构没有发生明显的变化。但由于局部亚稳相的热分解，致使材料出现约3.55%的质量损失，材料的密度、弯曲强度和弹性模量分别下降了约2%、13%和29%。同时，陶瓷样品在平行于及垂直于压力方向上分别产生了约0.535%和0.203%的体积收缩。当应力为125MPa时，材料在1400℃、1500℃或1600℃真空环境中的稳态蠕变速率分别约为5.5×10~(-10)/s、3.4×10~(-8)/s和8.5×10~(-8)/s。在静态干燥空气中，当温度低于1200℃或等于1600℃时，2Si-B-3C-N复相陶瓷具有良好的抗氧化性能；当温度约为1400℃时，材料会发生快速的氧化；少量ZrO2或AlN（5mol%）的加入使材料在1000℃即发生快速的氧化，当温度为1200℃时，样品表面至材料内部的氧化侵蚀层厚度约为0.25-1.00mm。
本文的研究优化了机械合金化非晶态2Si-B-3C-N粉末及热压烧结纳米2Si-B-3C-N陶瓷的制备工艺；阐明了ZrO2或AlN添加剂对材料烧结致密化的促进作用；揭示了材料的表面结构、热稳定性、晶化过程，BN(C)相的湍层结构，以及材料的室温与高温力学性能，为Si-B-C-N陶瓷及相关材料的进一步研究提供了理论依据和数据支持。
Because of its outstanding structural stability, creep resistance and oxidationresistance, Si-B-C-N ceramic attracts great attention in recent years, and maypossess extensive applications in aircraft, metallurgy, energy, information, etc.Methods used to prepare Si-B-C-N ceramic mainly include organic polymerpyrolyzing, physical vapor deposition and mechanical alloying. Much attention ispaid to the mechanical alloying method, due to its cheap and innocuous rawmaterials, simple process and advantage in the preparation of dense bulk ceramic.However, the sintering and crystallization process or mehanisms of the amorphousSi-B-C-N powder, and the high-temperature properties of the hot pressed nanoceramic, etc., are still needed to be further investigated. Aiming at these problems,amorphous2Si-B-3C-N powder was high-energy ball milled in this subject, and wasthen hot pressed to prepare bulk ceramic. Methods, including X-ray diffraction,SEM, TEM, TG-DTA, mechanical property testing, etc., were employed to carefullystudy the microstructure, sintering process, crystallization and property of2Si-B-3C-N powder or bulk ceramic. Main results are as follows.
The mechanically-alloyed amorphous2Si-B-3C-N powder consists of hardaggregates, with near spherical shapes and an average size of about5μm. Theamorphous2Si-B-3C-N powders, prepared employing different milling parameters,have similar size distribution, surface structure and thermal stability. When therotation speed of pot is higher than600rpm, or the ball to powder mass ratio islarger than20:1, nano SiC crystals with a size of about1-5nm appear in theamorphous matrix. When milling time is30h or40h, silicon atoms are ready toreact with carbon atoms, but crystals are hard to be found. At temperatures higherthan1000℃, SiC nano wires may grow on the surface of the heated2Si-B-3C-Npowder. At about1350℃in nitrogen, carbothermic reaction occurs on the surfaceof2Si-B-3C-N powder and hence CO or CO2is released.
Sintered at a temperature higher than1830℃(at80MPa), the2Si-B-3C-Nceramic body takes rapid volume shrinkage and its density is greatly enhanced. Thebulk density, relative density, room-temperature fracture strength, Young’s modulus, fracture toughness and Vickers hardness of the as-prepared2Si-B-3C-N ceramic,hot pressed at1900℃/80MPa/30min/8bar N_2, are about2.52g/cm~3,88.7%,331.1MPa,139.4GPa,2.81MPa·m~(1/2), and5.65GPa, respectively. Whentemperature is lowered to1800℃, or pressure is decreased to50MPa, the densityand mechanical property of the prepared ceramic sharply degrade. The addition ofZrO2or AlN (5mol%) reduces the temperature, at which notable sintering occurs,to about1720℃and1760℃, respectively, and the density and fracture strength ofthe prepared cramic are considerablely elevated.
Hot pressed under a pressure of80MPa, the amorphous2Si-B-3C-N powderstarts to crystallize at about1485℃. The growth of SiC and BN(C) grains relies onthe stacking of (111) or (0002) planes, or the incorporation of adjacent grains. The2Si-B-3C-N ceramic, hot pressed at1900℃/80MPa/30min/8bar N_2, is composedof uniformly distributed β-SiC、α-SiC and BN(C), with an average grain size lessthan100nm. BN(C) has a turbostratic structure and consists of unevenly distributedt-BN, t-carbon, boron adopted t-carbon and carbon adopted t-BN.
The nano2Si-B-3C-N ceramic prepared here has outstanding structuralstability, creep resistance and oxidation resistance. Annealed at1800℃in1bar N_2for3h, the ceramic shows little change in its microstructure. However, due to thedecomposition of ceramic, the sample has a mass loss of about3.55%. Under thepressure of125MPa, the2Si-B-3C-N ceramic exhibits a steady-creep rate of about5.5×10~(-10)/s at1400℃,3.4×10~(-8)/s at1500℃and8.5×10~(-8)/s at1600℃in vacuum.In static and dry air, the ceramic possesses excellent oxidation resistance attemperatures lower than1200℃or at1600℃. However, the ceramic rapidlyoxidizes at1400℃. The addition of ZrO2or AlN (5mol%) greatly degrade theoxidation resistance of the2Si-B-3C-N ceramic.
Current results give further comprehension on the preparation process,microstructure, thermal stability, crystallization, and high-temperature properties ofthe mechanically alloyed amorphous2Si-B-3C-N powder or the hot pressed2Si-B-3C-N ceramic, providing new theoretical insights or experimental data forthe further research of Si-B-C-N ceramic or related materials.
研究发现，采用本文所用原料及机械合金化工艺制备的非晶态2Si-B-3C-N粉末由近似球形的纳米颗粒硬团聚体构成，团聚体的平均粒径约为5μm；采用不同球磨工艺参数制备的非晶态2Si-B-3C-N粉末具有相似的粒度分布、表面结构及组织热稳定性；当球磨罐转速高于600rpm或球料质量比大于20:1时，会促使非晶组织发生晶化并生成尺寸约为1-5nm的SiC晶体。30h或40h的球磨时间有利于硅与碳原子之间反应成键，并且此时粉末中的非晶态组织没有发生明显的晶化；当非晶态2Si-B-3C-N粉末在氮气氛中被加热至约1000℃以上时，在粉末的表面出现SiC纳米线的生长现象；当被加热至约1350℃时，粉末因为表面氧化膜的碳热还原反应而快速生成并释放出CO或CO2气体。
在80MPa下热压烧结，当温度高于约1830℃时，非晶态2Si-B-3C-N粉末将发生快速的致密化。在1900℃/80MPa/30min/8bar N_2条件下热压烧结制备的2Si-B-3C-N复相陶瓷体积密度和相对密度，以及室温弯曲强度、弹性模量、断裂韧性和维氏硬度分别约为2.52g/cm~3，88.7%，331.1MPa，139.4GPa，2.81MPa·m~(1/2)和5.65GPa。当烧结温度降至1800℃或压力降至50MPa时，所制备材料的密度和力学性能会急剧下降。5mol%ZrO2或AlN添加剂使陶瓷坯体在相同工艺条件下发生快速烧结致密化的温度分别降低至约1720℃和1760℃，陶瓷材料的相对密度分别增至约97.7%和96.9%，室温弯曲强度分别增至约575.4MPa和415.7MPa。
在80MPa/30min/8bar N_2条件下热压烧结时，非晶态2Si-B-3C-N粉末的起始晶化温度约为1485℃。SiC和BN(C)通过各自密排面有序堆垛、相邻晶粒合并等方式实现晶粒生长。在1900℃/80MPa/30min/8bar N_2条件下热压烧结制备的2Si-B-3C-N陶瓷由平均晶粒尺寸小于100nm，且分布均匀的β-SiC、α-SiC和BN(C)构成。BN(C)相具有湍层结构，由分布不均匀的湍层氮化硼，湍层碳，以及B原子固溶的湍层碳和C原子固溶的湍层氮化硼等原子层构成。
热压烧结制备的纳米2Si-B-3C-N复相陶瓷具有优异的高温组织稳定性、高温抗蠕变性能和抗氧化性能。在1800℃/1bar N_2条件下保温处理3h后，材料的组织结构没有发生明显的变化。但由于局部亚稳相的热分解，致使材料出现约3.55%的质量损失，材料的密度、弯曲强度和弹性模量分别下降了约2%、13%和29%。同时，陶瓷样品在平行于及垂直于压力方向上分别产生了约0.535%和0.203%的体积收缩。当应力为125MPa时，材料在1400℃、1500℃或1600℃真空环境中的稳态蠕变速率分别约为5.5×10~(-10)/s、3.4×10~(-8)/s和8.5×10~(-8)/s。在静态干燥空气中，当温度低于1200℃或等于1600℃时，2Si-B-3C-N复相陶瓷具有良好的抗氧化性能；当温度约为1400℃时，材料会发生快速的氧化；少量ZrO2或AlN（5mol%）的加入使材料在1000℃即发生快速的氧化，当温度为1200℃时，样品表面至材料内部的氧化侵蚀层厚度约为0.25-1.00mm。
本文的研究优化了机械合金化非晶态2Si-B-3C-N粉末及热压烧结纳米2Si-B-3C-N陶瓷的制备工艺；阐明了ZrO2或AlN添加剂对材料烧结致密化的促进作用；揭示了材料的表面结构、热稳定性、晶化过程，BN(C)相的湍层结构，以及材料的室温与高温力学性能，为Si-B-C-N陶瓷及相关材料的进一步研究提供了理论依据和数据支持。
Because of its outstanding structural stability, creep resistance and oxidationresistance, Si-B-C-N ceramic attracts great attention in recent years, and maypossess extensive applications in aircraft, metallurgy, energy, information, etc.Methods used to prepare Si-B-C-N ceramic mainly include organic polymerpyrolyzing, physical vapor deposition and mechanical alloying. Much attention ispaid to the mechanical alloying method, due to its cheap and innocuous rawmaterials, simple process and advantage in the preparation of dense bulk ceramic.However, the sintering and crystallization process or mehanisms of the amorphousSi-B-C-N powder, and the high-temperature properties of the hot pressed nanoceramic, etc., are still needed to be further investigated. Aiming at these problems,amorphous2Si-B-3C-N powder was high-energy ball milled in this subject, and wasthen hot pressed to prepare bulk ceramic. Methods, including X-ray diffraction,SEM, TEM, TG-DTA, mechanical property testing, etc., were employed to carefullystudy the microstructure, sintering process, crystallization and property of2Si-B-3C-N powder or bulk ceramic. Main results are as follows.
The mechanically-alloyed amorphous2Si-B-3C-N powder consists of hardaggregates, with near spherical shapes and an average size of about5μm. Theamorphous2Si-B-3C-N powders, prepared employing different milling parameters,have similar size distribution, surface structure and thermal stability. When therotation speed of pot is higher than600rpm, or the ball to powder mass ratio islarger than20:1, nano SiC crystals with a size of about1-5nm appear in theamorphous matrix. When milling time is30h or40h, silicon atoms are ready toreact with carbon atoms, but crystals are hard to be found. At temperatures higherthan1000℃, SiC nano wires may grow on the surface of the heated2Si-B-3C-Npowder. At about1350℃in nitrogen, carbothermic reaction occurs on the surfaceof2Si-B-3C-N powder and hence CO or CO2is released.
Sintered at a temperature higher than1830℃(at80MPa), the2Si-B-3C-Nceramic body takes rapid volume shrinkage and its density is greatly enhanced. Thebulk density, relative density, room-temperature fracture strength, Young’s modulus, fracture toughness and Vickers hardness of the as-prepared2Si-B-3C-N ceramic,hot pressed at1900℃/80MPa/30min/8bar N_2, are about2.52g/cm~3,88.7%,331.1MPa,139.4GPa,2.81MPa·m~(1/2), and5.65GPa, respectively. Whentemperature is lowered to1800℃, or pressure is decreased to50MPa, the densityand mechanical property of the prepared ceramic sharply degrade. The addition ofZrO2or AlN (5mol%) reduces the temperature, at which notable sintering occurs,to about1720℃and1760℃, respectively, and the density and fracture strength ofthe prepared cramic are considerablely elevated.
Hot pressed under a pressure of80MPa, the amorphous2Si-B-3C-N powderstarts to crystallize at about1485℃. The growth of SiC and BN(C) grains relies onthe stacking of (111) or (0002) planes, or the incorporation of adjacent grains. The2Si-B-3C-N ceramic, hot pressed at1900℃/80MPa/30min/8bar N_2, is composedof uniformly distributed β-SiC、α-SiC and BN(C), with an average grain size lessthan100nm. BN(C) has a turbostratic structure and consists of unevenly distributedt-BN, t-carbon, boron adopted t-carbon and carbon adopted t-BN.
The nano2Si-B-3C-N ceramic prepared here has outstanding structuralstability, creep resistance and oxidation resistance. Annealed at1800℃in1bar N_2for3h, the ceramic shows little change in its microstructure. However, due to thedecomposition of ceramic, the sample has a mass loss of about3.55%. Under thepressure of125MPa, the2Si-B-3C-N ceramic exhibits a steady-creep rate of about5.5×10~(-10)/s at1400℃,3.4×10~(-8)/s at1500℃and8.5×10~(-8)/s at1600℃in vacuum.In static and dry air, the ceramic possesses excellent oxidation resistance attemperatures lower than1200℃or at1600℃. However, the ceramic rapidlyoxidizes at1400℃. The addition of ZrO2or AlN (5mol%) greatly degrade theoxidation resistance of the2Si-B-3C-N ceramic.
Current results give further comprehension on the preparation process,microstructure, thermal stability, crystallization, and high-temperature properties ofthe mechanically alloyed amorphous2Si-B-3C-N powder or the hot pressed2Si-B-3C-N ceramic, providing new theoretical insights or experimental data forthe further research of Si-B-C-N ceramic or related materials.
引文
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