Strempel V E, Naumann d'Alnoncourt R, Driess M, Rosowski F
BasCat-UniCat BASF JointLab, Technische Universität Berlin, Hardenbergstraße 36, 10623 Berlin, Germany.
Rev Sci Instrum. 2017 Jul;88(7):074102. doi: 10.1063/1.4992023.
A modular setup for Atomic Layer Deposition (ALD) on high-surface powder substrates in fixed bed reactors with a gravimetric in situ monitoring was developed. The design and operation are described in detail. An integrated magnetically suspended balance records mass changes during ALD. The highly versatile setup consists of three modular main units: a dosing unit, a reactor unit, and a downstream unit. The reactor unit includes the balance, a large fixed bed reactor, and a quartz crystal microbalance. The dosing unit is equipped with a complex manifold to deliver gases and gaseous reagents including three different ALD precursors, five oxidizing or reducing agents, and two purge gas lines. The system employs reactor temperatures and pressures in the range of 25-600 °C and 10 to 1 bar, respectively. Typically, powder batches between 100 mg and 50 g can be coated. The capabilities of the setup are demonstrated by coating mesoporous SiO powder with a thin AlO (submono) layer using three cycles with trimethylaluminium and HO. The self-limiting nature of the deposition has been verified with the in situ gravimetric monitoring and full saturation curves are presented. The process parameters were used for a scale-up in a large fixed bed reactor. The samples were analyzed with established analytics such as X-ray diffraction, N adsorption, transmission electron microscopy, and inductively coupled plasma optical emission spectrometry.
开发了一种用于固定床反应器中高比表面积粉末基材上原子层沉积（ALD）的模块化装置，并带有重量法原位监测。详细描述了其设计和操作。一个集成的磁悬浮天平记录ALD过程中的质量变化。这种高度通用的装置由三个模块化主要单元组成：一个计量单元、一个反应器单元和一个下游单元。反应器单元包括天平、一个大型固定床反应器和一个石英晶体微天平。计量单元配备有一个复杂的歧管，用于输送气体和气态试剂，包括三种不同的ALD前驱体、五种氧化剂或还原剂以及两条吹扫气体管线。该系统分别采用25 - 600°C的反应器温度和10至1巴的压力。通常，可以涂覆100毫克至50克之间的粉末批次。通过使用三甲基铝和H₂O进行三个循环，在介孔SiO粉末上涂覆一层薄的Al₂O₃（亚单层）来展示该装置的能力。通过原位重量监测验证了沉积的自限性，并给出了完全饱和曲线。将工艺参数用于大型固定床反应器的放大。使用诸如X射线衍射、N₂吸附、透射电子显微镜和电感耦合等离子体发射光谱等既定分析方法对样品进行分析。
