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放电等离子烧结制备La2O3/LaB6改性ZrC-SiC陶瓷及其抗烧蚀性能
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长安大学 材料科学与工程学院,陕西 西安 710061

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TQ174.75+8.22

基金项目:

国家自然科学基金(51902028,52272034);陕西省重点研发计划(2023JBGS-15);长安大学中央高校基本科研业务费专项资金(300102312406,300102313202)


Preparation of La2O3/LaB6-Modified ZrC-SiC Ceramics by Spark Plasma Sintering and Their Ablation Resistance
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School of Materials Science and Engineering, Chang'an University, Xi'an 710061, China

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    摘要:

    为了提高ZrC-SiC陶瓷的抗烧蚀性能,采用放电等离子烧结法在1600℃/50 MPa条件下制备了一系列不同含量La2O3和LaB6改性的ZrC-SiC复相陶瓷,在热流密度为2380 kW/m2的氧乙炔焰下考核了材料的抗烧蚀性能。结果表明:La2O3和LaB6的加入不仅提高了ZrC-SiC的烧结性能,致密度增加,还提升了其抗热震性能。随着添加量的加大,烧蚀后试样表面氧化层从破裂逐渐趋于完整。相比而言,La2O3改性后烧蚀表面形成的ZrO2-La2Zr2O7固溶层仍存在较多的孔洞和裂纹,而且与内部陶瓷结合差,防护效果有限。LaB6加入后,烧蚀过程中低熔点硼化物的挥发可将材料的烧蚀温度降低约300 ℃,试样烧蚀中心表面形成热稳定性好的La2Zr2O7-LaBO3-ZrO2外氧化层和粘结性佳的富镧Zr-O-La-B内氧化层,该双层结构的保护膜成为阻挡氧化气流进入材料内部的密实屏障,有效提高了材料的抗烧蚀性能,添加20vol% LaB6的ZrC-SiC综合抗烧蚀性能最佳。氧乙炔烧蚀60 s后,其质量烧蚀率和线性烧蚀率分别为7.5×10-4 g/s和2.1×10-3 mm/s。

    Abstract:

    To improve the ablative properties of ZrC-SiC ceramics, a series of ZrC-SiC multiphase ceramics modified with different contents of La2O3 and LaB6 were prepared by discharge plasma sintering method at 1600 ℃ and 50 MPa. The ablative properties of the materials were tested under oxygen-acetylene flame with a heat flux of 2380 kW/m2. The results show that the addition of La2O3 and LaB6 not only improves the sintering performance and density of ZrC-SiC, but also improves the thermal shock resistance. With the increase in addition amount, the surface oxide layer of the samples gradually becomes intact from fracture after ablation. In contrast, the ZrO2-La2Zr2O7 solid solution layer formed on the ablative surface after La2O3 modification still has more holes and cracks, and the combination with internal ceramics is poor, resulting in the poor protection effect. With the addition of LaB6, the volatilization of low melting-point borides during ablative process can reduce the ablative temperature of the material by nearly 300 ℃. La2Zr2O7-LaBO3-ZrO2 outer oxide layer with good thermal stability and lanthanum-rich Zr-O-La-B inner oxide layer with good adhesion are formed on the surface of the ablation center of the sample. The double-layer protective film becomes a dense barrier to prevent the oxidation air from entering the inside of the material, which effectively improves the ablation resistance of the material. The ZrC-SiC ceramic with 20vol% LaB6 has the best comprehensive ablative performance. After oxygen-acetylene ablation for 60 s, its mass and linear ablative rate are 7.5×10-4 g/s and 2.1×10-3 mm/s, respectively.

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解静,滕程程,孙国栋,李辉,贾研,赵鹏.放电等离子烧结制备La2O3/LaB6改性ZrC-SiC陶瓷及其抗烧蚀性能[J].稀有金属材料与工程,2025,54(4):975~982.[Xie Jing, Teng Chengcheng, Sun Guodong, Li Hui, Jia Yan, Zhao Peng. Preparation of La2O3/LaB6-Modified ZrC-SiC Ceramics by Spark Plasma Sintering and Their Ablation Resistance[J]. Rare Metal Materials and Engineering,2025,54(4):975~982.]
DOI:10.12442/j. issn.1002-185X.20230768

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  • 收稿日期:2023-11-28
  • 最后修改日期:2024-01-09
  • 录用日期:2024-01-31
  • 在线发布日期: 2025-04-23
  • 出版日期: 2025-04-21