A nondispersive infrared gas analyzer was demonstrated for investigating metal alkylamide precursor delivery for microelectronics vapor deposition processes. The nondispersive infrared analyzer was designed to simultaneously measure the partial pressure of pentakis(dimethylamido) tantalum, a metal precursor employed in high volume manufacturing vapor deposition processes to deposit tantalum nitride, and dimethylamine, the primary decomposition product of pentakis(dimethylamido) tantalum at typical delivery conditions for these applications. This sensor was based on direct absorption of pentakis(dimethylamido) tantalum and dimethylamine in the fingerprint spectral region. The nondispersive infrared analyzer optical response was calibrated by measuring absorbance as a function of dimethylamine and pentakis(dimethylamido) tantalum density. The difference between the mass of material removed from the ampoule during flow tests as measured gravimetrically and as determined optically, by calculating flow rates from the nondispersive infrared analyzer measurements, was only ≈2 %. The minimum detectable molecular densities for pentakis(dimethylamido) tantalum and dimethylamine were ≈2 × 1013 cm−3 and ≈5 × 1014 cm−3, respectively (with no signal averaging and for a sampling rate of 200 Hz), and the corresponding partial pressures were ≈0.1 Pa and ≈2 Pa for pentakis(dimethylamido) tantalum and dimethylamine, respectively (for an optical flow cell temperature of 93 ℃). Pentakis(dimethylamido) tantalum could be detected at all conditions of this investigation and likely the majority of conditions relevant to high volume manufacturing tantalum nitride deposition. Dimethylamine was not detected at all conditions in this study, because of a lower nondispersive infrared analyzer sensitivity to dimethylamine compared to pentakis(dimethylamido) tantalum and because conditions of this study were selected to minimize DMA production. While this nondispersive infrared gas analyzer was specifically developed for pentakis(dimethylamido) tantalum and dimethylamine, it is suitable for characterizing the vapor delivery of other metal alkylamide precursors and the corresponding amine decomposition products, although in the case of some metal alkylamides a different bandpass filter would be required.

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用于气相沉积过程中烷基酰胺钽分压测量的非分散红外气体分析仪

展示了一种非分散红外气体分析仪，用于研究微电子气相沉积过程中金属烷基酰胺前体的输送。非色散红外分析仪旨在同时测量五（二甲基酰胺）钽（一种用于大批量制造气相沉积工艺以沉积氮化钽的金属前体）和二甲胺（五（二甲基酰胺）钽在典型温度下的主要分解产物）的分压这些应用的交货条件。该传感器基于指纹光谱区域中五（二甲基酰胺）钽和二甲胺的直接吸收。通过测量吸光度作为二甲胺和五（二甲基酰胺）钽密度的函数来校准非色散红外分析仪光学响应。在流动测试期间从安瓿中取出的材料质量之间的差异（通过重量分析测量和光学确定，通过计算非色散红外分析仪测量的流速）仅为 ≈2%。五（二甲基酰胺基）钽和二甲胺的最小可检测分子密度分别为 ≈2 × 1013 cm−3 和 ≈5 × 1014 cm−3（无信号平均且采样率为 200 Hz），相应的部分五（二甲基酰胺基）钽和二甲胺的压力分别为 ≈0.1 Pa 和 ≈2 Pa（光学流通池温度为 93 ℃）。Pentakis（二甲基酰胺基）钽可以在本次调查的所有条件下检测到，并且可能在与大批量制造氮化钽沉积相关的大多数条件下检测到。在本研究中的所有条件下均未检测到二甲胺，因为与五（二甲氨基）钽相比，非分散红外分析仪对二甲胺的灵敏度较低，并且本研究的条件选择为最大限度地减少 DMA 产生。虽然这种非分散红外气体分析仪是专门为五（二甲基酰胺）钽和二甲胺而开发的，但它适用于表征其他金属烷基酰胺前体和相应胺分解产物的蒸气传输，尽管在某些金属烷基酰胺的情况下，使用不同的带通滤波器将需要。这是因为与五（二甲基酰胺）钽相比，非分散红外分析仪对二甲胺的灵敏度较低，并且本研究的条件选择为最大限度地减少 DMA 产生。虽然这种非分散红外气体分析仪是专门为五（二甲基酰胺）钽和二甲胺而开发的，但它适用于表征其他金属烷基酰胺前体和相应胺分解产物的蒸气传输，尽管在某些金属烷基酰胺的情况下，使用不同的带通滤波器将需要。这是因为与五（二甲基酰胺）钽相比，非分散红外分析仪对二甲胺的灵敏度较低，并且本研究的条件选择为最大限度地减少 DMA 产生。虽然这种非分散红外气体分析仪是专门为五（二甲基酰胺）钽和二甲胺而开发的，但它适用于表征其他金属烷基酰胺前体和相应胺分解产物的蒸气传输，尽管在某些金属烷基酰胺的情况下，使用不同的带通滤波器将需要。