Department of Textile Engineering, Chemistry and Science, North Carolina State University, Raleigh, North Carolina 27695, USA.
ACS Appl Mater Interfaces. 2011 Feb;3(2):299-308. doi: 10.1021/am100940g. Epub 2011 Jan 25.
Improving nanoscale thin film deposition techniques such as atomic layer deposition (ALD) to permit operation at ambient pressure is important for high-throughput roll-to-roll processing of emerging flexible substrates, including polymer sheets and textiles. We present and investigate a novel reactor design for inorganic materials growth by ALD at atmospheric pressure. The reactor uses a custom "pressure boost" approach for delivery of low vapor pressure ALD precursors that controls precursor dose independent of reactor pressure. Analysis of continuum gas flow in the reactor shows key relations among reactor pressure, inert gas flow rate, and species diffusion that define conditions needed to efficiently remove product and adsorbed reactive species from the substrate surface during the inert gas purge cycle. Experimental results, including in situ quartz crystal microbalance (QCM) characterization and film thickness measurements for deposition of ZnO and Al(2)O(3) are presented and analyzed as a function of pressure and gas flow rates at 100 °C. At atmospheric pressure and high gas flow, ZnO deposition can proceed at the same mass uptake and growth rate as observed during more typical low pressure ALD. However, under the same high pressure and flow conditions the mass uptake and growth rate for Al(2)O(3) is a factor of ∼1.5-2 larger than at low pressure. Under these conditions, Al(2)O(3) growth at atmospheric pressure in a "flow-through" geometry on complex high surface area textile materials is sufficiently uniform to yield functional uniform coatings.
改进纳米薄膜沉积技术,如原子层沉积(ALD),以实现常压操作,对于新兴的柔性基底(包括聚合物薄片和纺织品)的高通量卷对卷处理至关重要。我们提出并研究了一种用于常压下无机材料生长的新型 ALD 反应器设计。该反应器采用定制的“压力提升”方法来输送低蒸气压 ALD 前体,可独立于反应器压力控制前体剂量。对反应器中连续气体流动的分析表明,反应器压力、惰性气体流速和物种扩散之间存在关键关系,这些关系定义了在惰性气体吹扫循环中从基底表面有效去除产物和吸附反应性物种所需的条件。实验结果包括原位石英晶体微天平(QCM)表征和 ZnO 和 Al2O3 的薄膜厚度测量,结果表明,在 100°C 时,压力和气体流速的函数。在常压和高气流条件下,ZnO 的沉积可以在与更典型的低压 ALD 中观察到的相同的质量吸收和生长速率下进行。然而,在相同的高压和流量条件下,Al2O3 的质量吸收和生长速率比低压时大 1.5-2 倍。在这些条件下,在复杂的高表面积纺织品材料上以“直通”几何形状在常压下进行的 Al2O3 生长足以产生功能均匀的涂层。