Nondispersive ultraviolet monitoring of pulsed H2S gas delivery

Abstract

This article describes time-resolved optical measurements of H2S partial pressure and mass flow in a pulsed gas delivery system approximating injection conditions encountered during atomic layer deposition. A high-speed nondispersive ultraviolet (NDUV) gas analyzer design is employed for in-line H2S detection in a gas delivery line with flowing carrier gas. An in-place analyzer calibration performed in a reference cell yields an H2S detection limit of ≈1.4 Pa (at 22 °C) at a sampling rate of 1 kHz. Flow measurements performed on the delivery line are used to evaluate the effects of adjustable delivery parameters on the time-dependent injection system output. Short pulse widths exhibit partial pressure transients attributed to flow development within the different volumes of the delivery system. After ≈1.0 s of injection, steady-state flow is established across flow elements. A partial pressure of H2S in the delivery line is found to vary linearly with upstream H2S pressure, consistent with choked flow. A stronger scaling of partial pressure is evident when the flow coefficient of the downstream metering valve is adjusted. Estimated steady-state H2S flow rates in the range of 0.05–0.21 mg/s are observed within a limited range of valve flow coefficients. However, further increases in the flow coefficient do not result in increased flow, likely due to conductance limitations in downstream flow system components. The utility of NDUV absorption measurements for high-pressure pulsed gas delivery systems is discussed.