首页|流延成型结合反应熔渗制备ZrB2-SiC陶瓷及其微观结构与氧化行为研究

流延成型结合反应熔渗制备ZrB2-SiC陶瓷及其微观结构与氧化行为研究

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ZrB2基陶瓷通常需要在高温高压条件下才能烧结致密,而利用反应熔渗Si的方式可在1500℃制得ZrB2-SiC致密陶瓷.相较于常规制备方法,反应制备法更容易获得晶粒细小、成分均匀的超高温陶瓷相.本研究以ZrSi2、B4C和C为原料,通过流延成型结合反应熔渗制备ZrB2-SiC陶瓷(简称ZBC陶瓷).此外,还以ZrB2和SiC为原料,通过相同的工艺制备了一组ZrB2-SiC陶瓷(简称ZS陶瓷)作为对比样品.对两组陶瓷的微观形貌进行表征,发现ZBC陶瓷中ZrB2相的颗粒尺寸较小且弥散分布在陶瓷中,而ZS陶瓷中ZrB2相的颗粒尺寸较大.在1600℃空气环境中对两组陶瓷进行循环氧化测试,总共循环氧化5次,每次2 h.分析两者的氧化行为,发现ZBC陶瓷与ZS陶瓷在氧化过程中表面都会形成玻璃态SiO2-ZrO2氧化层,起到阻隔氧气的作用.不同点在于ZBC陶瓷中ZrO2弥散分布在SiO2中,而ZS陶瓷是大尺寸的ZrO2与玻璃态SiO2共存.在降温过程中,弥散分布的ZrO2能够提高玻璃态SiO2的黏度,抑制其结晶,所以ZBC陶瓷的表面氧化层能够保持致密的结构;而ZS陶瓷氧化层中SiO2大量结晶并与ZrO2共晶反应产生ZrSiO4,由于热应力导致氧化层开裂,使其阻隔氧气的作用大大减弱.分析两者的抗氧化性能,发现ZBC陶瓷的氧化层厚度变化与质量增加均小于ZS陶瓷,表明ZBC陶瓷的抗氧化性能优于ZS陶瓷.
Microstructure and Oxidation Behavior of ZrB2-SiC Ceramics Fabricated by Tape Casting and Reactive Melt Infiltration
ZrB2-based ceramics typically necessitate high temperature and pressure for sintering,whereas ZrB2-SiC ceramics can be fabricated at 1500℃using the process of reactive melt infiltration with Si.In comparison to the conventional preparation method,reactive synthesis allows for the more facile production of ultra-high temperature ceramics with fine particle size and homogeneous composition.In this work,ZrSi2,B4C,and C were used as raw materials to prepare ZrB2-SiC via combination of tape casting and reactive melt infiltration herein referred to as ZBC ceramics.Control sample of ZrB2-SiC was also prepared using ZrB2 and SiC as raw materials through an identical process designated as ZS ceramics.Microscopic analysis of both ceramic groups revealed smaller and more uniformly distributed particles of the ZrB2 phase in ZBC ceramics compared to the larger particles in ZS ceramics.Both sets of ceramics underwent cyclic oxidation testing in the air at 1600℃for a cumulative duration of 5 cycles,each cycle lasting 2 h.Analysis of the oxidation behavior showed that both ZBC ceramics and ZS ceramics developed a glassy SiO2-ZrO2 oxide layer on their surfaces during the oxidation.This layer severed as a barrier against oxygen.In ZBC ceramics,ZrO2 is finely distributed in SiO2,whereas in ZS ceramics,larger ZrO2 particles coexist with glassy SiO2.The surface oxide layer of ZBC ceramics maintains a dense structure because the well-dispersed ZrO2 increases the viscosity of glassy SiO2,preventing its crystallization during the cooling.Conversely,some SiO2 in the oxide layer of ZS ceramics may crystallize and form a eutectic with ZrO2,leading to the formation of ZrSiO4.This leads to cracking of the oxide layer due to differences in thermal expansion coefficients,weakening its barrier effect.An analysis of the oxidation resistance shows that ZBC ceramics exhibit less increase in oxide layer thickness and mass compared to ZS ceramics,suggesting superior oxidation resistance of ZBC ceramics.

ultra-high temperature ceramicZrB2-SiCoxidation behaviorreactive melt infiltration

谭敏、陈小武、杨金山、张翔宇、阚艳梅、周海军、薛玉冬、董绍明

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中国科学院 上海硅酸盐研究所,高性能陶瓷和超精密微结构国家重点实验室,上海 200050

中国科学院大学 材料与光电研究中心,北京 100049

超高温陶瓷 ZrB2-SiC 氧化行为 反应熔渗

国家重点研发计划Shanghai Science and Technology Innovation Action Plan国家自然科学基金国家科技重大专项中国科学院重点研究项目Science Center for Gas Turbine Project of China

2022YFB370770021511104800521721112017-IV-0005-0042ZDRW-CN-2021-2-2P2022-B-IV-001-001

2024

无机材料学报
中国科学院上海硅酸盐研究所

无机材料学报

CSTPCD北大核心
影响因子:0.768
ISSN:1000-324X
年,卷(期):2024.39(8)
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