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In this study, we investigate the dependence of GaN surface morphology on the absolute strain values for thin (c-plane sapphire substrates of various miscut angles towards the m-plane. Results indicate an excellent correlation between the surface roughness observed employing an AFM tool and epilayer strain values. An overall increase of surface roughness (decrease of atomic terrace width) is found with decreasing compressive strain (epilayer vs. bulk value). In addition, sapphire substrates with increasing miscut angle (0.30 deg) appear to relax the inherent, built-in strain differently in the vertical (growth) direction when compared to just (0.00 deg) substrates. Strain relaxation by typical V-shaped, hexagonal pits is directly imaged through the comparison of surface features inside and outside of pits in the thin GaN epilayer films.

We investigate the formation of inAs-rich layers at the interface between InP and arsenicbased Ill-V alloys grown by chemical beam epitaxy (CBE). In-situ spectroscopic ellipsometry, low temperature photoluminescence, secondary ion mass spectrometry and transmission electron microscopy were used to characterize the formation of these layers. We present evidence for interfacial layer roughness that depends strongly on growth temperature and on the presence of surface steps, and show that modifications of the interface chemistry and of the gas-switching sequence can reduce interfacial layer thicknesses.

AlGaAs/InGaAs/GaAs heteroepitaxial layers grown by molecular beam epitaxy were studied by cross-sectional transmission electron microscopy (TEM) and energy dispersive spectroscopy (EDS). The presence of waviness/roughness, fine periodic striation contrast due to Al composition oscillations, and defects were observed by TEM in selected samples. EDS on the TEM was of limited utility in determining the composition of thin epitaxial layers and in comparing the composition near and away from a defect. Arguments are presented to rationalize these results.

A variety of optical methods are now available for studying surface processes and for monitoring layer thicknesses and compositions during semiconductor crystal growth by molecular beam epitaxy (MBE), organometallic chemical vapor deposition (OMCVD), and related techniques. New capabilities for surface analysis are being provided by developing techniques such as reflectance-difference spectroscopy (RDS), which use intrinsic symmetries to suppress ordinarily dominant bulk contributions. Bulk and microstructural properties such as compositions and layer thicknesses can be determined by techniques such as spectroellipsometry (SE), which return information integrated over the penetration depth of light. Recent advances include the application of reflectance to monitor dynamic surface processes, RDS to characterize (001) GaAs surfaces in OMCVD environments, and SE to control growth of AlxGa1-x, As materials and structures.

Silicon nitride films deposited from silane-nitrogen and silane-ammonia mixtures by PECVD contain large amounts of hydrogen. We have determined that adding argon to the gas mixture reduces the amount of hydrogen in the resulting films. Differences in film composition are obviously due to changes in the chemistry of the discharge which was characterized by line-of-sight mass spectrometry, optical emission spectroscopy and plasma double probe measurements. Substrate temperature was fixed at 325°C, pressure was 500 mtorr, the RF power was 0.25 watts cm−2, the silane to nitrogen ratio was varied from 0.003 to 0.02, the silane to ammonia ratio was varied from 0.01 to 0.5, and the argon additions were 10% of the total gas flow. Argon additions to the discharge increased the plasma density in both nitrogen and ammonia plasmas. Optical emission from N2 and Si-H species increased upon the addition of 10% argon to the silane-nitrogen discharge, whereas the N-H emission decreased upon addition of argon to the silane-ammonia discharge. Infrared transmission spectra of films deposited with and without argon show no change in peak position or intensity of Si-H and N-H absorption bands in the spectral range studied, despite a large (over 20%) reduction in hydrogen content, as determined by nuclear profiling, upon the addition of argon. These results suggest that a substantial fraction of the hydrogen in the films is not infrared active. We propose that the reduction in hydrogen content is due to bombardment of the growing film by argon ions, which sputter the adsorbed hydrogen molecules.

The pyrolytic conversion of an organosilsesquioxane (Owens-Illinois resin GR650) to SiO2 is characterized by ir spectroscopy, thermogravimetry and evolved gas analysis (line-of-sight mass spectroscopy). Scanning calorimetry, ramping at 10°C/min, on the as-received (room temperature annealed) resin indicates a glass transition temperature of 67°C which decreases to 58°C for an unrelaxed sample. The ir spectra have bands which can be assigned to Si-CH3 and Si-O-Si modes. For 30 minute isothermal anneals at temperatures above 420°C there is a continuous decrease in the bands associated with the Si-CH3 groups such that after 30 minutes at 650°C the ir spectrum has evolved to that for SiO2. Evolved gas analysis indicates that there are four major components evolving. Over the temperature range (ramping at 10°C/min) ∼180 to ∼500°C we observe C2H5OH and H2O, both of which are condensation reaction products from the curing reaction. Methane is a major evolving species over the temperature range ∼500 to ∼800°C and the thermal spectrum is double peaked which we attribute to CH3+ bound to the inside and outside of the polymer cage structures. The final major component detected was H2, over the temperature range ∼600 to ∼1100°C, which was attributed to pyrolysis of the organic components, both trapped and evolving. The features of the weight loss curve can be accounted for by the measured evolving species spectra.

The properties necessary for a material to be useful as a fiber cladding (appropriate Δn) and/or coating (provide mechanical protection) were evaluated for an organosilsesquioxane (Owens-Illinois Resin GR 650). The samples were 120 μm silica fibers coated with 12 μm of the cured organosilicon polymer. We observe, from an index profile of the clad fiber, that Δn = 0.04. The tensile strength measured in air (65% RH, 25 °C) was 765 ksi and the dynamic fatigue constant determined under the same ambient conditions was 29, both of which are typical of a mechanically protected fiber. From aging experiments in 90 °C distilled water we observe that the onset for a marked loss of strength with time is ∼1 day for an epoxy-acrylate coated fiber and slightly more than a week for the organosilicon polymer coated fiber, a notable improvement.