NDLI: Impurities in hydride gases part 2: Investigation of trace CO$_{2}$ in the liquid and vapor phases of ultra-pure ammonia

Content Provider	Springer Nature Link
Author	Funke, Hans H. Welchhans, Jon Watanabe, Tadaharu Torres, Robert Houlding, Virginia H. Rayr, Mark W.
Copyright Year	2004
Abstract	Ammonia (NH$_{3}$) as a precursor for epitaxial nitride films is required to be free of trace oxygenated impurities, such as CO$_{2}$, that have been shown to negatively affect growth processes and device performance. Carbon dioxide can react reversibly with the NH$_{3}$ gas to form ammonium carbamate, NH$_{4}$COONH$_{2}$ (a solid with low solubility in liquid NH$_{3}$) and, therefore, can be present in cylinder sources both in the free and chemically bound form. A gas chromatograph (GC)-based method has been developed to accurately quantify the total CO$_{2}$ content in both vapor- and liquid-phase NH$_{3}$ streams. A heated GC-sampling manifold is used to thermally decompose any NH$_{4}$COONH$_{2}$ present in the sample or calibration standard so that all CO$_{2}$ is analyzed in its free form. Several commercial cylinder sources maintained at room temperature were analyzed by this method, and in all cases, equilibrium concentrations of <75 parts-per-billion by volume (ppbv) CO$_{2}$ were present in the gas phase as long as residual liquid was present. Slightly higher concentrations were found in the liquid phase, and upon exhaustion of the liquid phase and heating, CO$_{2}$ levels strongly increased to parts-per-million by volume (ppmv) levels. The excess CO$_{2}$ is likely adsorbed on the cylinder walls or dispersed in the liquid as solid NH$_{4}$COONH$_{2}$. These results are consistent with thermodynamic calculations based on equilibrium data for the carbamate system available in the literature. To meet the purity requirements of organo-metallic vapor-phase epitaxy processes, the performance of an adsorbent-based purifier that is capable of removing residual CO$_{2}$ in both free and chemically bound forms from NH$_{3}$ streams is discussed.
Starting Page	873
Ending Page	880
Page Count	8
File Format	PDF
ISSN	03615235
Journal	Journal of Electronic Materials
Volume Number	33
Issue Number	8
e-ISSN	1543186X
Language	English
Publisher	Springer-Verlag
Publisher Date	2004-01-01
Publisher Place	New York
Access Restriction	One Nation One Subscription (ONOS)
Subject Keyword	Carbon dioxide impurities ammonia ammonium carbamate gas chromatography Optical and Electronic Materials Characterization and Evaluation of Materials Electronics and Microelectronics, Instrumentation Solid State Physics and Spectroscopy
Content Type	Text
Resource Type	Article
Subject	Materials Chemistry Electronic, Optical and Magnetic Materials Condensed Matter Physics Electrical and Electronic Engineering

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