The combinatorial approach applied to functional oxides has enabled the production of material libraries that formally contain infinite compositions. A complete ternary diagram can be obtained by pulsed laser deposition (PLD) on 100 mm silicon wafers. However, interest in such materials libraries is only meaningful if high-throughput characterization enables the information extraction from the as-deposited library in a reasonable time. While much commercial equipment allows for XY-resolved characterization at room temperature, very few sample holders have been made available to investigate structural, chemical, and functional properties at high temperatures in controlled atmospheres. In the present work, we present a furnace that enables the study of 100 mm wafers as a function of temperature. This furnace has a dome to control the atmosphere, typically varying from nitrogen gas to pure oxygen atmosphere with external control. We present the design of such a furnace and an example of X-ray diffraction (XRD) and fluorescence (XRF) measurements performed at the DiffAbs beamline of the SOLEIL synchrotron. We apply this high-throughput approach to a combinatorial library up to 735 {\textdegree}C in nitrogen and calculate the thermal expansion coefficients (TEC) of the ternary system using custom-made MATLAB codes. The TEC analysis revealed the potential limitations of Vegard's law in predicting lattice variations for high-entropy materials.
翻译:将组合方法应用于功能氧化物已能制备形式上包含无限组分的材料库。通过脉冲激光沉积(PLD)技术在100毫米硅片上可获得完整的三元相图。然而,此类材料库的价值仅在高通量表征技术能够在合理时间内从沉积态库中提取信息时才得以体现。虽然许多商用设备支持室温下的XY分辨表征,但能在受控气氛中研究高温下结构、化学及功能特性的样品台却极为稀少。本研究展示了一种可实现100毫米晶片随温度变化研究的加热炉。该炉配备穹顶以实现气氛控制,通常可在外部调控下实现从氮气到纯氧气氛的转换。本文介绍了该加热炉的设计方案,并提供了在SOLEIL同步辐射光源DiffAbs光束线进行X射线衍射(XRD)与荧光(XRF)测量的实例。我们运用此高通量方法对组合材料库在氮气环境中进行高达735°C的原位表征,并利用自主开发的MATLAB代码计算该三元体系的热膨胀系数(TEC)。TEC分析揭示了维加德定律在预测高熵材料晶格变化时存在的潜在局限性。