低温放电等离子烧结制备铱薄膜与碳化锆之间的相形成

B.A.B. Alawad, E. Njoroge, T. Ntsoane, M. Legodi, T. Thabethe, T. Hlatshwayo, J. Malherbe
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引用次数: 0

摘要

采用火花等离子烧结(SPS)技术,在温度为1700℃、1900℃和2100℃、50 MPa下烧结10 min,制备了碳化锆(ZrC)样品。研究了烧结后的相和显微组织。测定了在1700℃、1900℃和2100℃下形成的ZrC陶瓷球团的相对密度分别为96.5%、98.9%和99.5%。计算ZrC陶瓷球团的晶粒尺寸,发现随着烧结温度从1700℃、1900℃升高到2100℃,ZrC陶瓷球团的晶粒尺寸分别从71.88 nm、79.15 nm和83.59 nm增大。在1700℃、1900℃~ 2100℃温度下,ZrC陶瓷球团的硬度分别为7.40 GPa、17.00 GPa ~ 18.40 GPa。在1700°C、1900°C和2100°C时,首选的取向是(200)平面。采用电子束沉积法在ZrC陶瓷上沉积铱(Ir)薄膜,并在600℃和800℃真空退火2h。利用掠入射x射线衍射(GIXRD)和扫描电镜(SEM)研究了材料的相组成、固相反应和表面形貌。采用x射线衍射(XRD)分析了沉积态和退火态样品中存在的相。XRD分析表明,在600℃时形成的初始相为Ir2Zr。在800℃时,Ir与ZrC反应生成IrZr。1700℃、1900℃和2100℃时烧结试样的SEM图像表明,ZrC表面呈非均质、不均匀状,由颗粒凝聚而成,气孔较少。气孔数量随烧结温度的升高而减少。在ZrC衬底上沉积Ir膜后,Ir膜的结构与衬底的结构一致。在600°C和800°C退火后,观察到表面颗粒进一步团聚。
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Phase Formation Between Iridium Thin Films and Zirconium Carbide Prepared by Spark Plasma Sintering at Relatively Low Temperatures
Zirconium carbide (ZrC) samples were prepared by spark plasma sintering (SPS), at temperatures of 1700 °C, 1900 °C and 2100 °C at 50 MPa for 10 minutes. The phase and microstructure after the sintering process was investigated. The relative density of ZrC ceramic pellets formed at 1700 °C, 1900 °C and 2100 °C was measured and found to be 96.5 %, 98.9 % and 99.5 % respectively. The grain size of ZrC ceramic pellets was calculated and it was found to increase from 71.88 nm, 79.15 nm and 83.59 nm as the sintering temperature increased from 1700 °C, 1900 °C to 2100 °C respectively. The hardness of ZrC ceramic pellets was found to be 7.40 GPa, 17.00 GPa to 18.40 GPa at 1700 °C, 1900 °C to 2100 °C respectively. The preferred orientation at 1700 °C, 1900 °C and 2100 °C was the (200) plane. Iridium (Ir) thin films were deposited on ZrC ceramics by electron beam deposition method and annealed in vacuum at temperatures of 600 °C and 800 °C for 2h. The phase composition, solid-state reactions and surface morphology were investigated by grazing incidence x-ray diffraction (GIXRD), and scanning electron microscopy (SEM). XRD was used to identify the phases present in the as-deposited and annealed samples. XRD analysis showed that Ir2Zr was the initial phase formed at 600 °C. At temperature 800 °C, Ir reacted with the ZrC to form IrZr. The SEM images of as-sintered samples at 1700 °C, 1900 °C and 2100 °C showed that the ZrC surface was heterogeneous and uneven consisting of agglomerated granules with a few pores. The number of pores was observed to reduce with sintering temperature. After depositing Ir films on ZrC substrate, the structure of the Ir film followed that of the substrates. After annealing the Ir-ZrC samples at 600 °C and 800 °C, the further agglomeration of surface granules was observed.
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