Knemeyer K, Baumgarten R, Ingale P, Naumann d'Alnoncourt R, Driess M, Rosowski F
BasCat-UniCat BASF JointLab, Technische Universität Berlin, Hardenbergstraße 36, 10623 Berlin, Germany.
Rev Sci Instrum. 2021 Feb 1;92(2):025115. doi: 10.1063/5.0037844.
Atomic layer deposition (ALD) is an industrially applied technique for thin film deposition. The vast majority of processes target flat substrates rather than powders. For ALD on powders, new processes are needed, as different reaction conditions are required. Here, two setups are described in detail, which enhance the ALD process development for powders. The first setup described is capable of directly measuring the vapor pressure of a given precursor by a capacitance diaphragm gauge. Promising precursors can be pre-selected, and suitable precursor saturation temperatures can be determined. The second setup consists of four parallel reactors with individual temperature zones to screen the optimal ALD temperature window in a time efficient way. Identifying the precursor saturation temperature beforehand and subsequently performing the first ALD half cycle in the parallel setup at four different reactor temperatures simultaneously will drastically reduce process development times. Validation of both setups is shown for the well-known ALD precursors, trimethylaluminum to deposit aluminum oxide and diethyl zinc to deposit zinc oxide, both on amorphous silica powder.
原子层沉积(ALD)是一种工业应用的薄膜沉积技术。绝大多数工艺针对的是平面基板而非粉末。对于粉末上的ALD,由于需要不同的反应条件,因此需要新的工艺。本文详细描述了两种装置,它们可促进粉末的ALD工艺开发。所描述的第一种装置能够通过电容式隔膜压力计直接测量给定前驱体的蒸气压。可以预先选择有前景的前驱体,并确定合适的前驱体饱和温度。第二种装置由四个带有独立温度区的平行反应器组成,以便以高效的方式筛选最佳的ALD温度窗口。事先确定前驱体饱和温度,随后在平行装置中于四个不同的反应器温度下同时进行第一个ALD半周期,将大幅缩短工艺开发时间。针对在无定形二氧化硅粉末上沉积氧化铝的著名ALD前驱体三甲基铝和沉积氧化锌的二乙基锌,展示了这两种装置的验证情况。