High-throughput, Chemical X-ray Microstructure Screening Center for Functional Glasses and Glass Ceramics

基于实验室的x射线显微镜（XRM）已经达到了50纳米空间分辨率的水平，可以在常规基础上使用。因此，它已被广泛用于金属和合金。这种新兴的微观结构诊断技术的大量非常具有挑战性的应用正在等待在复杂氧化物领域进行研究。对于这类材料，空间分辨率被认为是足够的。瓶颈在于，在XRM被广泛用于探索其微观结构之前，玻璃陶瓷等多组分系统中元素的3D分布以及样品制备的新方法必须可用。为了促进复合氧化物的化学对比XRM，提出了现有XRM技术的以下方法进步：首先，使用超短脉冲激光烧蚀来加工一端具有片状参考体积的完美圆柱形样品。离子束稀释后，在第二步中获得该参考体的SEM-EDXS元素图。第三，利用相关软件对XRM和SEM-EDXS数据进行叠加，得到化学XRM数据。使用这种显著改进的XRM核心设备，可以研究关于玻璃结晶和当前对复杂氧化物感兴趣的其他主题的基础研究。后一种研究显然受益于（与TEM相比）大大提高的体积与表面比，允许监测更具代表性（因此具有统计意义）的样品体积。此外，一个和相同体积的兴趣在热处理时的时间演变可以跟踪和样品退火在温度梯度将有助于提高吞吐量。以与基础研究高度相关的十个案例研究为例，上述概述的新工作流程将得到证明，并作为用户设施提供给对加速开发具有新性质的复合氧化物感兴趣的德国科学家社区。获得的实验数据集不仅将用于建立微观结构-性能关系，而且还将形成综合计算材料工程方法的基础，并有助于建立材料数据空间。因此，它将成为未来材料发展的关键。

Lab-based X-ray microscopy (XRM) has reached a level where a spatial resolution of 50 nm can be used on a routine basis. As such, it has been utilized intensely for metals and alloys. A plethora of very challenging applications of this emerging microstructure-diagnostics technique is waiting to become investigated in the realm of complex oxides. Spatial resolution is considered to be sufficient for this class of materials. The bottleneck is that 3D distributions of elements in multicomponent systems such as glass ceramics as well as new approaches to sample preparation have to become available before XRM can be widely used to explore their microstructure. In order to facilitate chemically contrasted XRM of complex oxides, the following methodological advancement of the existing XRM technique is proposed: First, ultrashort-pulsed laser ablation is used to machine perfectly cylindrical samples possessing a plate-like reference volume at its one end. After ion-beam thinning, SEM-EDXS elemental maps of this reference volume are acquired in a second step. Third, a correlation software is used to superimpose XRM and SEM-EDXS data to end up with chemical XRM data. Using this significantly improved XRM core facility, basic research regarding the crystallization in glasses and other topics of current interest for complex oxides can be studied. The latter investigations clearly do profit from a (compared to TEM) much improved volume-to-surface ratio, allowing to monitor much more representative (and thus statistically significant) sample volumes. Moreover, the temporal evolution of one and the same volume of interest upon heat treatment can be tracked and samples annealed in a temperature gradient will help enhancing throughput. Exemplified by ten case studies of high relevance for basic research, the new workflow sketched above will be proved and made available as a user facility to the German community of scientists interested in the accelerated development of complex oxides with new properties. The experimental datasets obtain will not just be used to establish microstructure-property relationships, but also form the basis for integrated computational materials engineering approaches and help building a materials data space. As such, it will become pivotal for future materials developments.