Atomic layer deposition (ALD) is evolving beyond binary compounds to complex oxides and doped structures, taking advantage of the nanometer precision ALD provides. In practice, the development of complex ALD-processes usually means performing many ALD-runs, as success at first attempt is unlikely. One factor at a time methods, where only one factor is altered and the rest are kept constant, are most often chosen due to their intuitive communication of control. However, they do have several drawbacks, being slow, neglecting secondary effects, and are usually not randomized—meaning that errors that arise over time can easily be overlooked. We here dig into our statistical toolbox and show how design of experiments (DoE) can be used to efficiently develop an ALD-process to deposit crystalline, luminescent CaMoO₄—a proposed material for optoelectronic applications, like light emitting diodes or as a host for solar down-converters. Using DoE enables screening for a wider range of deposition temperatures, pulsed composition, and annealing parameters, by only performing nine ALD-runs in our case. We moreover look into how these parameters affect crystallinity, composition, and the photoluminescence properties and use DoE to show which factors have the greatest effects on these properties. The work also lays out the basic theory of the DoE-field and how to implement DoE in developing ALD-processes, in general, to ease the usage of DoE for the ALD-community.

中文翻译：

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原子层沉积发光CaMoO4的实验方法设计

利用ALD提供的纳米精度，原子层沉积（ALD）已从二元化合物发展到复杂的氧化物和掺杂结构。在实践中，开发复杂的ALD过程通常意味着执行许多ALD运行，因为首次尝试不太可能成功。一次只选择一个因素的方法，由于仅凭一种直观的控制方式，因此通常只选择一个因素，其余因素保持不变。但是，它们确实有几个缺点，它们速度慢，忽略了次要效果，并且通常不是随机的，这意味着随时间推移出现的错误很容易被忽略。我们在这里进入统计工具箱，并展示如何使用实验设计（DoE）有效地开发ALD工艺以沉积结晶的发光CaMoO ₄—一种用于光电应用的建议材料，例如发光二极管或作为太阳能下变频器的主体。通过使用DoE，仅在本例中执行9次ALD运行就可以筛选更宽范围的沉积温度，脉冲成分和退火参数。此外，我们研究了这些参数如何影响结晶度，组成和光致发光特性，并使用DoE来显示哪些因素对这些特性的影响最大。该工作还列出了DoE领域的基本理论，以及如何在开发ALD过程中实施DoE，以简化在ALD社区使用DoE的工作。