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NASA NTRS1989

Rolling contact fatigue of surface modified 440C using a 'Ge-Polymet' type disc rod test rig

Through hardened 440 C martensitic stainless steel test specimens were surface modified and tested for changes in rolling contact fatigue using a disc on rod test rig. The surface modifications consisted of nitrogen, boron, titanium, chromium, tantalum, carbon, or molybdenum ion implantation at various ion fluences and energies. Tests were also performed on specimens reactively sputtered with titanium nitride.

Thom, Robert L.↗

NASA NTRS1993

Application of hard coatings to substrates at low temperatures

BIRL, the industrial research laboratory of Northwestern University, has conducted unique and innovative research, under sponsorship from the NASA Marshall Space Flight Center (MSFC), in the application of hard, wear resistant coatings to bearing steels using the high-rate reactive sputtering (HRRS) process that was pioneered by Dr. William Sproul, the principal investigator on this program. Prior to this program, Dr. Sproul had demonstrated that it is possible to apply hard coatings such as titanium nitride (TiN) to alloy steels at low temperatures via the HRRS process without changing the metallurgical properties of the steel. The NASA MSFC program at BIRL had the specific objectives to: apply TiN to 440C stainless steel without changing the metallurgical properties of the steel; prepare rolling contact fatigue (RCF) test samples coated with binary hard coatings of TiN, zirconium nitride (ZrN), hafnium nitride (HfN), chromium nitride (CrN), and molybdenum nitride (MoN), and metal coatings of copper (Cu) and gold (Au); and develop new alloyed hard coatings of titanium aluminum nitride (Ti(0.5)Al(0.5)N), titanium zirconium nitride (Ti(0.5)Zr(0.5)N), and titanium aluminum vanadium nitride.

Sproul, William D.↗

NASA NTRS1998

High Temperature - Thin Film Strain Gages Based on Alloys of Indium Tin Oxide

A stable, high temperature strain gage based on reactively sputtered indium tin oxide (ITO) was demonstrated at temperatures up to 1050 C. These strain sensors exhibited relatively large, negative gage factors at room temperature and their piezoresistive response was both linear and reproducible when strained up to 700 micro-in/in. When cycled between compression and tension, these sensors also showed very little hysteresis, indicating excellent mechanical stability. Thin film strain gages based on selected ITO alloys withstood more than 50,000 strain cycles of +/- 500 micro-in/in during 180 hours of testing in air at 1000 C, with minimal drift at temperature. Drift rates as low as 0.0009%/hr at 1000 C were observed for ITO films that were annealed in nitrogen at 700 C prior to strain testing. These results compare favorably with state of the art 10 micro-m thick PdCr films deposited by NASA, where drift rates of 0.047%/hr at 1050 C were observed. Nitrogen annealing not only produced the lowest drift rates to date, but also produce the largest dynamic gage factors (G = 23.5). These wide bandgap, semiconductor strain sensors also exhibited moderately low temperature coefficients of resistance (TCR) at temperatures up to 1100 C, when tested in a nitrogen ambient. A TCR of +230 ppm/C over the temperature range 200 C < T < 500 C and a TCR of -469 ppm/C over the temperature range 600 C < T < 1100 C was observed for the films tested in nitrogen. However, the resistivity behavior changed considerably when the same films were tested in oxygen ambients. A TCR of -1560 ppm/C was obtained over the temperature range of 200 C < T < 1100 C. When similar films were protected with an overcoat or when ITO films were prepared with higher oxygen contents in the plasma, two distinct TCR's were observed. At T < 800 C, a linear TCR of -210 ppm/C was observed and at T > 800 C, a linear TCR of -2170 DDm/C was observed. The combination of a moderately low TCR and a relatively large gage factor make these semiconducting oxide films promising candidates for the active strain elements in high temperature thin film strain gages, particularly in applications where static strain measurement is desired.

Gregory, Otto J.↗

NASA NTRS1999

Growth of Homoepitaxial ZnO Semiconducting Films

As a high temperature semiconductor, ZnO has been used for many applications such as wave-guide, solar cells, and surface acoustic wave devices. Since the ZnO material has an energy gap of 3.3 eV at room temperature and an excitonic binding energy (60 meV) that is possible to make excitonic lasering at room temperature a recent surge of interest is to synthesize ZnO films for electro-optical devices. These applications require films with a smooth surface, good crystal quality, and low defect density. Homoepitaxial films have been studied in terms of morphology, crystal structure, and electrical and optical properties. ZnO single crystals are grown by the hydrothermal method. Substrates are mechanically polished and annealed in air for four hours before deposited films. The annealing temperature-dependence of ZnO substrates is studied. Films are synthesized by the off-axis reactive sputtering deposition. The films have very smooth surface with a roughness </= 5 nm on a 5 micrometers x 5 micrometers area. The full width at half maximum of film theta rocking curves measured by the x-ray diffraction is slightly larger than the crystal substrate. The film quality is determined by measuring the film resistivity, the Hall mobility, carrier densities and the energy band gap. The properties of ZnO films grown of (0001) ZnO and (0001) sapphire substrates will be also compared and discussed in the presentation.

Zhu, Shen↗

NASA NTRS1999

Growth of Homoepitaxial ZnO Semiconducting Films

As a high temperature wide-band-gap (3.3 eV at room temperature) semiconductor, ZnO has been used for many applications such as wave-guides, solar cells, and surface acoustic wave devices, Since ZnO has a 60 meV excitonic binding energy that makes it possible to produce excitonic lasing at room temperature, a recent surge of interest is to synthesize ZnO films for UV/blue/green laser diodes. These applications require films with a smooth surface, good crystal quality, and low defect density. Thus, homoepitaxial film growth is the best choice. Homoepitaxial films have been studied in terms of morphology, crystal structure, and electrical and optical properties. ZnO single crystal substrates grown by the hydrothermal method are mechanically polished and annealed in air for four hours before the films are deposited. The annealing temperature-dependence on ZnO substrate morphology and electrical properties is investigated. Films are synthesized by off-axis reactive sputtering deposition. This produces films that have very smooth surfaces with roughness less than or equal to 5 nm on a 5 microns x 5 microns area. The full width at half maximum of film theta rocking curves measured by the x-ray diffraction is slightly larger than that of the crystal substrate. Films are also characterized by measuring resistivity, optical transmittance, and photoluminescence. The properties of ZnO films grown on (0001) ZnO and (0001) sapphire substrates will also be compared and discussed.

Zhu, Shen↗

NASA NTRS2000

\A Gravity-Related Transport in Reactive Off-Axis Sputtering Deposition

An experiment was designed to investigate the transport characterization of reactive off- axis sputtering deposition. Three transport regions were observed when the growth pressures vary from 5 mtorr to 150 mtorr. A new gravity-related phenomenon was revealed in film growth at relatively high growth pressures. This effect is related to the collision process or thermalization of transport species. This study also suggests a design for the substrate holder orientation in the off-axis sputtering system.

Zhu, Shen↗

NASA NTRS1978

Industrial ion source technology

An analytical model was developed to describe the development of a coned surface texture with ion bombardment and simultaneous deposition of an impurity. A mathematical model of sputter deposition rate from a beveled target was developed in conjuction with the texturing models to provide an important input to that model. The establishment of a general procedure that will allow the treatment of manay different sputtering configurations is outlined. Calculation of cross sections for energetic binary collisions was extened to Ar, Kr.. and Xe with total cross sections for viscosity and diffusion calculated for the interaction energy range from leV to 1000eV. Physical sputtering and reactive ion etching experiments provided experimental data on the operating limits of a broad beam ion source using CF4 as a working gas to produce reactive species in a sputtering beam. Magnetic clustering effects are observed when Al is seeded with Fe and sputtered with Ar(?) ions. Silicon was textured at a micron scale by using a substrate temperature of 600 C.

Kaufman, H. R.↗

NASA NTRS1982

Plasma deposition and surface modification techniques for wear resistance

The ion-assisted or plasma coating technology is discussed as it applies to the deposition of hard, wear resistant refractory compound films. Of the many sputtering and ion plating modes and configurations the reactive magnetron sputtering and the reactive triode ion plating techniques are the preferred ones to deposit wear resistant coatings for tribological applications. Both of these techniques incorporate additional means to enhance the ionization efficiency and chemical reaction to precision tailor desirable tribological characteristics. Interrelationships between film formation, structure, and ribological properties are strictly controlled by the deposition parameters and the substrate condition. The enhanced ionization contributes to the excellent adherence and coherence, reduced internal stresses and improved structural growth to form dense, cohesive, equiaxed grain structure for improved wear resistance and control.

Spalvins, T.↗

NASA NTRS1982

Some properties of RF sputtered hafnium nitride coatings

Hafnium nitride coatings were deposited by reactive RF sputtering from a hafnium target in nitrogen and argon gas mixtures. The rate of deposition, composition, electrical resistivity and complex index of refraction were investigated as a function of target substrate distance and the fraction nitrogen, (fN2) in the sputtering atmosphere. The relative composition of the coatings is independent on fN2 for values above 0.1. The electric resistivity of the hafnium nitride films changes over 8 orders of magnitude when fN2 changes from 0.10 to 0.85. The index of refraction is almost constant at 2.8(1-0.3i) up to fN2 = 0.40 then decreases to 2.1(1 - 0.01i) for higher values of fN2.

Aron, P. R.↗

NASA NTRS1995

Reactively Deposited Aluminum Oxide and Fluoropolymer Filled Aluminum Oxide Protective Coatings for Polymers

Reactive ion beam sputter deposition of aluminum simultaneous with low energy arrival of oxygen ions at the deposition surface enables the formation of highly transparent aluminum oxide films. Thick (12 200 A), adherent, low stress, reactively deposited aluminum oxide films were found to provide some abrasion resistance to polycarbonate substrates. The reactively deposited aluminum oxide films are also slightly more hydrophobic and more transmitting in the UV than aluminum oxide deposited from an aluminum oxide target. Simultaneous reactive sputter deposition of aluminum along with polytetrafluoroethylene (PTFE Teflon) produces fluoropolymer-filled aluminum oxide films which are lower in stress, about the same in transmittance, but more wetting than reactively deposited aluminum oxide films. Deposition properties, processes and potential applications for these coatings will be discussed.

Rutledge, Sharon K.↗

NASA NTRS1999

Pressure Effect in ZnO Films Using Off-Axis Sputtering Deposition

ZnO films are deposited on (0001) sapphire, (001) Si and quartz substrates using the off-axis reactive magnetron sputtering deposition. Based on film thickness measurements, three transport regions of sputtered particles are observed when films are deposited in the pressure regions of 5 mtorr - 150 mtorr. X-ray diffraction, scanning probes microscopy, and electrical measurements are also used to characterize these films. The full width at half maximum of theta rocking curves for epitaxial films is less than 0.5 deg. In textured films, it rises to several degrees. The epitaxial films deposited at high pressure reveal a flat surface with some hexagonal facets. The density of hexagonal facets decreases when the growth pressure is reduced. The resistivity of these epitaxial films also depends on the growth pressures. A relationship between the pressure effects and film properties are discussed.

Zhu, Shen↗

NASA NTRS1982

RF sputtered silicon and hafnium nitrides: Properties and adhesion to 440C stainless steel

Silicon nitride and hafnium nitride coatings were deposited by reactive RF sputtering on oxidized and unoxidized 440C stainless steel substrates. Sputtering was done in mixtures of argon and nitrogen gases from pressed powder silicon nitride and from hafnium metal targets. Depositions were at two background pressures, 8 and 20 mtorr, and at two different fractions (f) of nitrogen in argon, 0.25 and 0.60, for hafnium nitride and at f = 0.25 for silicon nitride. The coatings and the interface between the coating and substrates were investigated by X-ray diffractometry, scanning electron microscopy, energy dispersive X-ray analysis and Auger electron spectroscopy. A Knoop microhardness of 1650 + or - 100 kg/sq mm was measured for hafnium nitride and 3900 + or - 500 kg/sq mm for silicon nitride. The friction coefficients between a 440C rider and the coatings were measured under lubricated conditions. Scratch test results demonstrate that the adhesion of hafnium nitride to both oxidized and unoxidized 440C is superior to that of silicon nitride. Oxidized 440C is found to have increased adhesion, to both nitrides, over that of unoxidized 440C.

Grill, A.↗

NASA NTRS1983

RF-sputtered silicon and hafnium nitrides - Properties and adhesion to 440C stainless steel

Silicon nitride and hafnium nitride coatings were deposited by reactive RF sputtering on oxidized and unoxidized 440C stainless steel substrates. Sputtering was done in mixtures of argon and nitrogen gases from pressed powder silicon nitride and from hafnium metal targets. Depositions were at two background pressures, 8 and 20 mtorr, and at two different fractions (f) of nitrogen in argon, 0.25 and 0.60, for hafnium nitride and at f = 0.25 for silicon nitride. The coatings and the interface between the coating and substrates were investigated by X-ray diffractometry, scanning electron microscopy, energy dispersive X-ray analysis and Auger electron spectroscopy. A Knoop microhardness of 1650 + or 100 kg/sq mm was measured for hafnium nitride and 3900 + or 500 kg/sq mm for silicon nitride. The friction coefficients between a 440C rider and the coatings were measured under lubricated conditions. Scratch test results demonstrate that the adhesion of hafnium nitride to both oxidized and unoxidized 440C is superior to that of silicon nitride. Oxidized 440C is found to have increased adhesion, to both nitrides, over that of unoxidized 440C.

Grill, A.↗

NASA NTRS1991

Sputtered Ta-Si-N diffusion barriers in Cu metallizations for Si

Electrical measurements on shallow Si n+-p junction diodes with a 30-nm TiSi2 contacting layer demonstrate that an 80-nm-thick amorphous Ta36Si14N50 film prepared by reactive RF sputtering of a Ta5Si3 target in an Ar/N2 plasma very effectively prevents the interaction between the Si substrate with the TiSi2 contacting layer and a 500-nm Cu overlayer. The Ta36Si14N50 diffusion barrier maintains the integrity of the I-V characteristics up to 900 C for 30-min annealing in vacuum. It is concluded that the amorphous Ta36Si14N50 alloy is not only a material with a very low reactivity for copper, titanium, and silicon, but must have a small diffusivity for copper as well.

Kolawa, E.↗

NASA NTRS1989

Effects of microstructure and nonstoichiometry on electrical properties of vanadium dioxide films

Voided growth structures of sputter-deposited films affect strongly their optical and electrical properties. Vanadium dioxide is an interesting material to study effects of film microstructure and nonstoichiometry on electrical properties because its phase transition makes it possible to investigate electrical behavior both in a semiconducting phase and in a metallic phase. Vanadium oxide films were deposited with different vanadium oxygen ratios for substrate temperatures between 250 and 550 C by dc reactive magnetron sputtering. The resistivity ratios between a semiconducting phase and a metallic phase are limited to 1000 order by voided boundaries and oxygen vacancies. The voided boundaries are defined by columnar structure and agglomerated grain growth. The results emphasize the necessity of a combination of deposition to obtain the film with a favorable structure and postdeposition annealing to control the film stoichiometry.

Kusano, Eiji↗

NASA NTRS1985

High T(c) superconducting NbN films deposited at room temperature

The dc reactive magnetron sputtering process yields stoichiometric NbN films with superconducting transition temperature T(c) as high as 15.7 K on substrates as varied as glass, glazed ceramic, fused quartz, and sapphire. These films posses fcc (B1) structure and (111) texture. The most dominant factors governing the formation of the transition metal nitrides are the relative metal and nitrogen fluxes incident on the substrate and the background argon pressure (which dictates the overall reactive sites and residence times for nitrogen).

Thakoor, S.↗

NASA NTRS1986

Room-Temperature Deposition of NbN Superconducting Films

Films with high superconducting transition temperatures deposited by reactive magnetron sputtering. Since deposition process does not involve significantly high substrate temperatures, employed to deposit counter electrode in superconductor/insulator/superconductor junction without causing any thermal or mechanical degradation of underlying delicate tunneling barrier. Substrates for room-temperature deposition of NbN polymeric or coated with photoresist, making films accessible to conventional lithographic patterning techniques. Further refinements in deposition technique yield films with smaller transition widths, Tc of which might approach predicted value of 18 K.

Thakoor, S.↗

NASA NTRS1998

The Improvement of Ion Plated Ag and Au Film Adherence to Si3N4 and SiC Surfaces for Increased Tribological Performance

A modified dc-diode plating system, utilizing a metallic screen cage as a cathode and referred as SCREEN CAGE ION PLATING (SCIP), is used to deposit Ag and Au lubricating films on Si3N4 and SiC surfaces. When deposition is performed in Ar or N2, glow discharge, the surface displays poor adhesive strength (less than 5 MPa). A dramatic increase in adhesive strength (less than 80 MPa) is achieved when plating is performed in a reactive 50% 02 + 50% Ar glow discharge. The excited/ionized oxygen species (O2(+)/O(+) in the glow discharge contribute to the oxidation of the Si3N4 or SiC surfaces as determined by X-ray Photoelectron Spectroscopy (XTS) depth profiling. The reactively sputter-oxidized S3N4 or SiC surfaces and the activated-oxidized-metastable Ag or Au species formed in the plasma cooperatively contribute to the increased adherence. As a result, the linear thermal expansion coefficient mismatch at the interface is reduced. These lubricating Ag and Au films under sliding conditions reduce the friction coefficient by a factor of 2-1/2 to 4.

Spalvins, Talivaldis↗