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At least 307 records · Page 17

Surface characterization and adhesion of oxygen plasma-modified LARC-TPI

LARC-TPI, an aromatic thermoplastic polyimide, was exposed to an oxygen plasma as a surface pretreatment for adhesive bonding. Chemical and physical changes which occurred in the polyimide surface as a result of the plasma treatment were investigated using X-ray photoelectron spectroscopy (XPS), infrared reflection-absorption spectroscopy (IR-RAS), contact-angle analysis, ellipsometry, and high resolution SEM. A 180-deg peel test with an acrylate-based pressure sensitive adhesive as a flexible adherent was utilized to study the interactions of the plasma-treated polyimide surface with other polymeric materials. The surface characterization and adhesion testing results showed that the oxygen plasma treatment, while creating a more hydrophilic, polar surface, also caused chain scission, resulting in the formation of a weak boundary layer which inhibited adhesion.

Chin, J. W.↗

Optical properties and spectral emissivities at 632.8 nm in the titanium-aluminum system

Optical properties (including spectral emissivity, refractive index, and extinction coefficient) of liquid Ti-Al alloys were measured as functions of temperature (including temperatures up to 350 K below the equilibrium liquidus temperatures), using laser ellipsometry at 632.8 nm. The experiments were conducted under containerless conditions, using electromagnetic levitation and heating supplemented by CO2 laser beam heating. It is shown that the emissivities of liquid Ti-Al alloy vary with temperature in a manner that can be understood by the same theories which are applicable to solid metals, for regions near to and above the liquidus temperature. At temperatures below the liquidus temperature, the optical properties of highly undercooled liquid Ti-Al alloys are not dependent on temperature.

Krishnan, S.↗

Low earth simulation and materials characterization

Oxygen plasma ashers and an electron cyclotron resonance (ECR) sources are currently being used for low Earth orbit (LEO) simulation. The suitability of each of these simulation techniques is considered. Thin film coatings are characterized by optical techniques, including variable-angle spectroscopic ellipsometry, optical spectrophotometry, and laser light scatterometry. Atomic force microscopy (AFM) has been used to characterize the surface morphology of thin aluminum films as a function of substrate temperature during deposition. Results on diamondlike carbon (DLC) films show that DLC degrades with simulated atomic oxygen (AO) exposure at a rate comparable to Kapton polyimide. Since DLC is not as susceptible as Kapton to environmental factors such as moisture absorption, it could potentially provide more accurate measurements of AO fluence on short space flights.

Synowicki, R. A.↗

Production and optical constraints of ice tholin from charged particle irradiation of (1:6) C2H6/H2O at 77 K

Fifty separate irradiations of a 6:1 mixture of H2O/C2H6 ice conducted over a 5-month period have yielded sufficient tholin for the determination of its physical constants in the 0.06 to 40 micron range. While the imaginary part of the refractive index k was obtained by transmission measurements on thin-film samples and Kramers-Kronig analysis (KKA), the real part of the refractive index was obtained by KKA and ellipsometry; these data may prove useful in cometary and outer solar system spectrometric interpretation.

Khare, B. N.↗

General technique for discrete retardation-modulation polarimetry

The general theory and rigorous solutions of the Stokes parameters of light of a new technique in time-resolved ellipsometry are outlined. In this technique the phase of the linear retarder is stepped over three discrete values over a time interval for which the Stokes vector is determined. The technique has an advantage over synchronous detection techniques, as it can be implemented as a digitizable system.

Saxena, Indu↗

Ellipsometric characterization of In(0.52)Al(0.48)As and of modulation doped field effect transistor structures on InP substrates

The dielectric function of a thick layer of In(0.52)Al(0.48)As lattice matched to InP was measured by variable angle spectroscopic ellipsometry in the range 1.9-4.1 eV. The In(0.52)Al(0.48)As was protected from oxidation using a thin In(0.53)Ga(0.47)As cap that was mathematically removed for the dielectric function estimate. The In(0.52)Al(0.48)As dielectric function was then verified by ellipsometric measurements of other In(0.53)Ga(0.47)As/In(0.52)Al(0.48)As structures, including (MODFET), and is shown to provide accurate structure layer thicknesses.

Alterovitz, S. A.↗

Tribological evaluation and analysis of coating materials

A physical characterization of coating materials by analytical techniques such as XPS, AES, ellipsometry, and nuclear reaction analysis can contribute to the understanding of adhesion and friction of the coatings and can partially predict the tribological properties of the coatings. This two-part paper describes the tribological properties and physical characteristics of (1) diamondlike carbon (DLC) films and (2) silicon nitride (SiN(x)) films. Emphasis is to relate plasma deposition conditions to the film chemistry and composition and to the adhesion and friction of the films. With the DLC films, the higher the plasma deposition power, the less the hydrogen concentration and the greater the film density and the hardness. The friction behavior of DLC films deposited at higher deposition powers (200 to 300 W) is similar to that of bulk diamond. Even in a vacuum, the DLC films effectively lubricate ceramic surfaces (Si3N4) at temperatures to 500 C. With SiN(x) films, the silicon to nitrogen ratios and the amount of amorphous silicon depend on deposition frequency. The presence of rich amorphous silicon in the high-frequency plasma-deposited SiN(x) films increases their adhesion and friction above 500 C in vacuum.

Miyoshi, Kazuhisa↗

Thermal oxidation of single-crystal silicon carbide - Kinetic, electrical, and chemical studies

This paper presents kinetic data from oxidation studies of the polar faces for 3C and 6H SiC in wet and dry oxidizing ambients. Values for the linear and parabolic rate constants were obtained, as well as preliminary results for the activation energies of the rate constants. Examples are presented describing how thermal oxidation can be used to map polytypes and characterize defects in epitaxial layers grown on low tilt angle 6H SiC substrates. Interface widths were measured using Auger electron spectroscopy (AES) with Ar ion beam depth profiling and variable angle spectroscopic ellipsometry (VASE) with effective medium approximation (EMA) models. Preliminary electrical measurements of MOS capacitors are also presented.

Petit, J. B.↗

Measurement of birefringence for optical recording disk substrates

The birefringence of bare and coated substrates for magneto-optical recording is experimentally investigated using ellipsometry at the wavelengths of 632.8 nm and 780 nm. The rotation and ellipticity of the polarization state of the reflected or transmitted light is measured for different incident angles and different orientations of the incident linear polarization. The measured data is then fitted by a computer program which solves the Maxwell equations for the plane-wave propagation in a multilayer structure and minimizes the error between the measured and calculated data by adjusting the unknown parameters of the multilayer. This approach enables us to determine orientations of the three principal axes in the substrate and the corresponding refractive indices. A special feature of our ellipsometers is that a glass hemisphere is placed in contact with the substrate, which eliminates the refraction of the incident light and enables a maximum propagation angle of 70 degrees (with respect to the normal) in the substrate. This increases the sensitivity of the measurement. Certain anomalies were observed, which we believe are associated with the presence of grooves on these substrates.

Fu, Hong↗

Spectroscopic ellipsometric characterization of Si/Si(1-x)Ge(x) strained-layer superlattices

Spectroscopic ellipsometry (SE) was employed to characterize Si/Si(1-x)Ge(x) strained-layer superlattices. An algorithm was developed, using the available optical constants measured at a number of fixed x values of Ge composition, to compute the dielectric function spectrum of Si(1-x)Ge(x) at an arbitrary x value in the spectral range 17 to 5.6 eV. The ellipsometrically determined superlattice thicknesses and alloy compositional fractions were in excellent agreement with results from high-resolution x ray diffraction studies. The silicon surfaces of the superlattices were subjected to a 9:1 HF cleaning prior to the SE measurements. The HF solution removed silicon oxides on the semiconductor surface, and terminated the Si surface with hydrogen-silicon bonds, which were monitored over a period of several weeks, after the HF cleaning, by SE measurements. An equivalent dielectric layer model was established to describe the hydrogen-terminated Si surface layer. The passivated Si surface remained unchanged for greater than 2 h, and very little surface oxidation took place even over 3 to 4 days.

Yao, H.↗

New technique for oil backstreaming contamination measurements

Due to the large size and the number of diffusion pumps, space simulation chambers cannot be easily calibrated by the usual test dome method for measuring backstreaming from oil diffusion pumps. In addition, location dependent contamination may be an important parameter of the test. The backstreaming contamination in the Space Power Facility (SPF) near Sandusky, Ohio, the largest space simulation vacuum test chamber in the U.S.A. was measured. Small size clean silicon wafers as contamination sensors placed at all desired measurement sites were used. The facility used diffusion pumps with DC 705 oil. The thickness of the contamination oil film was measured using ellipsometry. Since the oil did not wet uniformly the silicon substrate, two analysis models were developed to measure the oil film: continuous, homogeneous film and islands of oil with the islands varying in coverage fraction and height. In both cases, the contamination film refractive index was assumed to be that of DC 705. The second model improved the ellipsometric analysis quality parameter by up to two orders of magnitude, especially for the low coverage cases. Comparison of the two models for our case shows that the continuous film model overestimates the oil volume by less than 50 percent. Absolute numbers for backstreaming are in good agreement with published results for diffusion pumps. Good agreement was also found between the ellipsometric results and measurements done by x ray photoelectron spectroscopy (XPS) and by scanning electron microscopy (SEM) on samples exposed to the same vacuum runs.

Alterovitz, S. A.↗

Optical properties and emissivities of liquid metals and alloys

This paper presents the results from our on-going program to investigate the optical properties of liquid metals and alloys at elevated temperatures. Ellipsometric and polarimetric techniques have been used to investigate the optical properties of materials in the 1000 - 3000 K temperature range and in the 0.3 - 0.1 mu m wavelength range. The ellipsometric and polarimetric techniques are described and the characteristics of the instruments are presented. The measurements are conducted by reflecting a polarized laser beam from an electromagnetically levitated liquid metal or alloy specimen. A Rotating Analyzer Ellipsometer (RAE) or a four-detector Division-of-Amplitude Photopolarimeter (DOAP) is used to determine the polarimetric properties of the light reflected at an angle of incidence of approximately 68 deg. Optical properties of the specimen which are calculated from these measurements include the index of refraction, extinction coefficient, normal spectral emissivity, and spectral hemispherical emissivity. These properties have been determined at various wavelengths and temperatures for liquid Ag, Al, Au, Cu, Nb, Ni, Pd, Pt, Si, Ti, Ti-Al alloys, U, and Zr. We also describe new experiments using pulsed-dye laser spectroscopic ellipsometry for studies of the wavelength dependence of the emissivities and optical properties of materials at high temperature. Preliminary results are given for liquid Al. The application of four-detector polarimetry for rapid determination of surface emissivity and true temperature is also described. Characteristics of these devices are presented. An example of the accuracy of this instrument in measurements of the melting point of zirconium is illustrated.

Krishnan, Shankar↗

Surface characterization and contamination analysis

The research activity for this first year has focussed on three distinct activities: (1) the use of an integrating sphere to improve upon the gathering of spectral data from a variety of surfaces; (2) the use of optical fiber spectrometry to determine levels of contamination from tape residues on critical bonding surfaces; and (3) an exploratory activity in the use of spectroscopic ellipsometry for the analysis of thin films of contaminants on critical surfaces has also begun.

Workman, Gary L.↗

Evaluation of space environmental effects on metals and optical thin films on EOIM-3

Metals and optical thin films exposed to the space environment on the Third Flight of the Evaluation of Oxygen Interactions with Materials (EOIM-3) payload, onboard Space Shuttle mission STS-46 were evaluated. The materials effects described in this paper include the effects of space exposure on various pure metals, optical thin films, and optical thin film metals. The changes induced by exposure to the space environment in the material properties were evaluated using bidirectional reflectance distribution function (BRDF), specular reflectance (250 nm to 2500 nm), ESCA, VUV reflectance (120 nm to 200 nm), ellipsometry, FTIR and optical properties. Using these analysis techniques gold optically thin film metal mirrors with nickel undercoats were observed to darken due to nickel diffusion through the gold to the surface. Also, thin film nickel mirrors formed nickel oxide due to exposure to both the atmosphere and space.

Vaughn, Jason A.↗

Surface contamination analysis technology team overview

A team was established which consisted of representatives from NASA (Marshall Space Flight Center and Langley Research Center), Thiokol Corporation, the University of Alabama in Huntsville, AC Engineering, SAIC, Martin Marietta, and Aerojet. The team's purpose was to bring together the appropriate personnel to determine what surface inspection techniques were applicable to multiprogram bonding surface cleanliness inspection. In order to identify appropriate techniques and their sensitivity to various contaminant families, calibration standards were developed. Producing standards included development of consistent low level contamination application techniques. Oxidation was also considered for effect on inspection equipment response. Ellipsometry was used for oxidation characterization. Verification testing was then accomplished to show that selected inspection techniques could detect subject contaminants at levels found to be detrimental to critical bond systems of interest. Once feasibility of identified techniques was shown, selected techniques and instrumentation could then be incorporated into a multipurpose inspection head and integrated with a robot for critical surface inspection. Inspection techniques currently being evaluated include optically stimulated electron emission (OSEE); near infrared (NIR) spectroscopy utilizing fiber optics; Fourier transform infrared (FTIR) spectroscopy; and ultraviolet (UV) fluorescence. Current plans are to demonstrate an integrated system in MSFC's Productivity Enhancement Complex within five years from initiation of this effort in 1992 assuming appropriate funding levels are maintained. This paper gives an overview of work accomplished by the team and future plans.

Burns, H. Dewitt↗

Standardization of surface contamination analysis systems

Corrosion products, oils and greases can potentially degrade material bonding properties. The Marshall Space Flight Center (MSFC) Surface Contamination Analysis Team (SCAT) utilizes a variety of analytical equipment to detect identify and quantify contamination on metallic and non-metallic substrates. Analysis techniques include FT-IR Microscopy (FT-IR), Near Infrared Optical Fiber Spectrometry (NIR), Optically Stimulated Electron Emission (OSEE), Ultraviolet Fluorescence (UVF) and Ellipsometry. To insure that consistent qualitative and quantitative information are obtained, standards are required to develop analysis techniques, to establish instrument sensitivity to potential contaminants, and to develop calibration curves. This paper describes techniques for preparing and preserving contamination standards. Calibration of surface contamination analysis systems is discussed, and methods are presented for evaluating the effects of potential contaminants on bonding properties.

Boothe, Richard E.↗

Study of surfaces using near infrared optical fiber spectrometry

The measurement and control of cleanliness for critical surfaces during manufacturing and in service provides a unique challenge for fulfillment of environmentally benign operations. Of particular interest has been work performed in maintaining quality in the production of bondline surfaces in propulsion systems and the identification of possible contaminants. This work requires an in-depth study of the possible sources of contamination, methodologies to identify contaminants, discrimination between contaminants and chemical species caused by environment, and the effect of particular contaminants on the bondline integrity of the critical surfaces. This presentation will provide an introduction to the use of optical fiber spectrometry in a nondestructive measurement system for process monitoring and how it can be used to help clarify issues concerning surface chemistry. Correlation of the Near Infrared (NIR) spectroscopic results with Optical Stimulated Electron Emission (OSEE) and ellipsometry will also be presented.

Workman, G. L.↗

Oxygen plasma ashing effects on aluminum and titanium space protective coatings

Using variable angle spectroscopic ellipsometry and atomic force microscopy (AFM), the surface roughness and oxidation of aluminum and titanium thin films have been studied as a function of substrate deposition temperature and oxygen plasma exposure. Increasing substrate deposition temperatures affect film microstructure by greatly increasing grain size. Short exposures to an oxygen plasma environment produce sharp spikes rising rapidly above the surface as seen by AFM. Ellipsometric measurements were made over a wide range of plasma exposure times, and results at longer exposure times suggest that the surface is greater than 30% void. This is qualitatively verified by the AFM images.

Synowicki, R.↗