Nondispersive Infrared Gas Analyzer for Partial Pressure Measurements of a Tantalum Alkylamide During Vapor Deposition Processes

• Published in: Applied spectroscopy Vol. 74; no. 10; pp. 1219 - 1229
• Main Authors: Maslar, James E., Kimes, William A., Sperling, Brent A., Kanjolia, Ravindra K.
• Format: Journal Article
• Language: English
• Published: London, England SAGE Publications 01-10-2020
• Subjects: CVD; pentakis(dimethylamido) tantalum; Atomic layer deposition; nondispersive infrared gas analyzer; chemical vapor deposition; ALD; dimethylamine; DMA; NDIR; PDMAT; infrared absorption
• ISSN: 0003-7028; 1943-3530
• DOI: 10.1177/0003702819885182

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.