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NASA NTRS1991

Lubrication with sputtered MoS2 films: Principles, operation, limitations

The present practices, limitations, and understanding of thin sputtered MoS2 films are reviewed. Sputtered MoS2 films can exhibit remarkable tribological properties such as ultralow friction coefficients (0.01) and enhanced wear lives (millions of cycles) when used in vacuum or dry air. To achieve these favorable tribological characteristics, the sputtering conditions during deposition must be optimized for adequate film adherence and appropriate structure (morphology) and composition.

Spalvins, T.↗

NASA NTRS1987

A review of recent advances in solid film lubrication

Thin, adherent sputtered MoS2 and ion plated metallic (Au, Ag, Pb) lubricating films are primarily used in precision contacting triboelement surfaces where wear debris formation is critical and high reliability requirements have to be satisfied. Detailed structural and compositional characterization of solid film lubricants is of prime importance. It is this information from the nano-micro-macro level which is needed to interpret and improve the frictional behavior and assure long endurance lives. The purpose of this paper is to summarize in a concise review the solid lubricant film structure and morphology and their effects on the tribological properties of the lubricant systems. The tribological performance of thin lubricating films has significantly advanced through progressive understanding of the film parameters such as adhesion, cohesion, interface formation, nucleation and microstructural growth, critical film thickness and substrate finish, and temperature. Sputtered MoS2 and ion plated Au, Ag, and Pb films are separately discussed and evaluated in terms of the above film parameters to establish the most desirable film structures and thicknesses in order to achieve effective lubrication.

Spalvins, T.↗

NASA NTRS1987

Ion nitriding; Proceedings of the International Conference, Cleveland, OH, Sept. 15-17, 1986

The present conference discusses plasma-assisted surface coating/modification processes, the applications to date of ion nitriding, the effects of nitrogen on metal surfaces, ion nitriding mechanisms in Cr, Al and Cr + Al-containing 1040 steel, ion nitriding of Al and its alloys, life enhancement for forging dies, novel anode plasma nitriding developments, and a comparative study of the pulsed and dc ion-nitriding behavior in specimens with blind holes. Also discussed are the influence of heating method on ion nitriding, surface hardening of marage steels by ion nitriding without core hardness reduction, plasma nitriding of nodular cast iron sput gears, NbN composites for superconductors, the carburization of tungsten in a glow discharge methane plasma, economic considerations concerning plasma nitriding, and the corrosion properties obtained by ion nitriding.

Spalvins, T.↗

NASA NTRS1987

Plasma assisted surface coating/modification processes - An emerging technology

A broad understanding of the numerous ion or plasma assisted surface coating/modification processes is sought. An awareness of the principles of these processes is needed before discussing in detail the ion nitriding technology. On the basis of surface modifications arising from ion or plasma energizing and interactions, it can be broadly classified as deposition of distinct overlay coatings (sputtering-dc, radio frequency, magnetron, reactive; ion plating-diode, triode) and surface property modification without forming a discrete coating (ion implantation, ion beam mixing, laser beam irradiation, ion nitriding, ion carburizing, plasma oxidation. These techniques offer a great flexibility and are capable in tailoring desirable chemical and structural surface properties independent of the bulk properties.

Spalvins, T.↗

NASA NTRS1986

Ion-Plated Soft Metallic Films Reduce Friction and Wear

Ion plating is ion-assisted or glow-discharge surface-deposition technique. In this process, ions or energetic atoms transfer energy, momentum, and charge to substrate and deposited surface film. Process controlled to modify physical characteristics of surface, subsurface chemical conditions, and surface and subsurface microstructures as well. Ion plating with such soft, thin metallic films as gold, silver, or lead has great potential for producing self-contained lubricating surfaces. Such films reduce friction, wear, and corrosion on sliding or rotating mechanical surfaces used in wide range of environments.

Spalvins, T.↗

NASA NTRS1986

Tribological characteristics of gold films deposited on metals by ion plating and vapor deposition

The graded interface between an ion-plated film and a substrate is discussed as well as the friction and wear properties of ion-plated gold. X-ray photoelectron spectroscopy (XPS) depth profiling and microhardness depth profiling were used to investigate the interface. The friction and wear properties of ion-plated and vapor-deposited gold films were studied both in an ultra high vacuum system to maximize adhesion and in oil to minimize adhesion. The results indicate that the solubility of gold on the substrate material controls the depth of the graded interface. Thermal diffusion and chemical diffusion mechanisms are thought to be involved in the formation of the gold-nickel interface. In iron-gold graded interfaces the gold was primarily dispersed in the iron and thus formed a physically bonded interface. The hardness of the gold film was influenced by its depth and was also related to the composition gradient between the gold and the substrate. The graded nickel-gold interface exhibited the highest hardness because of an alloy hardening effect. The effects of film thickness on adhesion and friction were established.

Miyoshi, K.↗

NASA NTRS1986

Plasma assisted surface coating/modification processes: An emerging technology

A broad understanding of the numerous ion or plasma assisted surface coating/modification processes is sought. An awareness of the principles of these processes is needed before discussing in detail the ion nitriding technology. On the basis of surface modifications arising from ion or plasma energizing and interactions, it can be broadly classified as deposition of distinct overlay coatings (sputtering-dc, radio frequency, magnetron, reactive; ion plating-diode, triode) and surface property modification without forming a discrete coating (ion implantation, ion beam mixing, laser beam irradiation, ion nitriding, ion carburizing, plasma oxidation). These techniques offer a great flexibility and are capable in tailoring desirable chemical and structural surface properties independent of the bulk properties.

Spalvins, T.↗

NASA NTRS1985

Frictional and structural characterization of ion-nitrided low and high chromium steels

Low Cr steels AISI 41410, AISI 4340, and high Cr austenitic stainless steels AISI 304, AISI 316 were ion nitrided in a dc glow discharge plasma consisting of a 75 percent H2 - 25 percent N2 mixture. Surface compound layer phases were identified, and compound layer microhardness and diffusion zone microhardness profiles were established. Distinct differences in surface compound layer hardness and diffusion zone profiles were determined between the low and high Cr alloy steels. The high Cr stainless steels after ion nitriding displayed a hard compound layer and an abrupt diffusion zone. The compound layers of the high Cr stainless steels had a columnar structure which accounts for brittleness when layers are exposed to contact stresses. The ion nitrided surfaces of high and low Cr steels displayed a low coefficient of friction with respect to the untreated surfaces when examined in a pin and disk tribotester.

Spalvins, T.↗

NASA NTRS1985

Tribological properties of boron nitride synthesized by ion beam deposition

The adhesion and friction behavior of boron nitride films on 440 C bearing stainless steel substrates was examined. The thin films containing the boron nitride were synthesized using an ion beam extracted from a borazine plasma. Sliding friction experiments were conducted with BN in sliding contact with itself and various transition metals. It is indicated that the surfaces of atomically cleaned BN coating film contain a small amount of oxides and carbides, in addition to boron nitride. The coefficients of friction for the BN in contact with metals are related to the relative chemical activity of the metals. The more active the metal, the higher is the coefficient of friction. The adsorption of oxygen on clean metal and BN increases the shear strength of the metal - BN contact and increases the friction. The friction for BN-BN contact is a function of the shear strength of the elastic contacts. Clean BN surfaces exhibit relatively strong interfacial adhesion and high friction. The presence of adsorbates such as adventitious carbon contaminants on the BN surfaces reduces the shear strength of the contact area. In contrast, chemically adsorbed oxygen enhances the shear strength of the BN-BN contact and increases the friction.

Miyoshi, K.↗

NASA NTRS1985

Advances in sputtered and ion plated solid film lubrication

The glow discharge or ion assisted vacuum deposition techniques, primarily sputtering and ion plating, have rapidly emerged and offer great potential to deposit solid lubricants. The increased energizing of these deposition processes lead to improved adherence and coherence, favorable morphological growth, higher density, and reduced residual stresses in the film. These techniques are of invaluable importance where high precision machines tribo-components require very thin, uniform lubricating films (0.2 m), which do not interface with component tolerances. The performance of sputtered MoS2 films and ion plated Au and Pb films are described in terms of film thickness, coefficient of friction, and wear lives.

Spalvins, T.↗

NASA NTRS1985

Surface hardening of steel by boriding in a cold rf plasma

Scanning electron spectroscopy, X-ray diffractometry, Auger electron spectroscopy, and microhardness measurements, are used to study the surfaces of 4340-steel samples that have been borided in a cold RF plasma which had been initiated in a gas mixture of 2.7 percent diborane in Ar. As a result of the dislocation of the diborane in the plasma, boron is deposited on the surface of the steel substrate and two crystalline phases, tetragonal Fe2B and orthorhombic FeB, are formed. The formation of boride phases then increases the surface microhardness from 2650 MPa to a maximum value of 7740 MPa.

Finberg, I.↗

NASA NTRS1985

Tribological properties of boron nitride synthesized by ion beam deposition

The adhesion and friction behavior of boron nitride films on 440 C bearing stainless steel substrates was examined. The thin films containing the boron nitride were synthesized using an ion beam extracted from a borazine plasma. Sliding friction experiments were conducted with BN in sliding contact with itself and various transition metals. It is indicated that the surfaces of atomically cleaned BN coating film contain a small amount of oxides and carbides, in addition to boron nitride. The coefficients of friction for the BN in contact with metals are related to the relative chemical activity of the metals. The more active the metal, the higher is the coefficient of friction. The adsorption of oxygen on clean metal and BN increases the shear strength of the metal - BN contact and increases the friction. The friction for BN-BN contact is a function of the shear strength of the elastic contacts. Clean BN surfaces exhibit relatively strong interfacial adhesion and high friction. The presence of adsorbates such as adventitious carbon contaminants on the BN surfaces reduces the shear strength of the contact area. In contrast, chemically adsorbed oxygen enhances the shear strength of the BN-BN contact and increases the friction.

Miyoshi, K.↗

NASA NTRS1985

Frictional and structural characterization of ion-nitrided low and high chromium steels

Low Cr steels AISI 41410, AISI 4340, and high Cr austenitic stainless steels AISI 304, AISI 316 were ion nitrided in a dc glow discharge plasma consisting of a 75 percent H2 - 25 percent N2 mixture. Surface compound layer phases were identified, and compound layer microhardness and diffusion zone microhardness profiles were established. Distinct differences in surface compound layer hardness and diffusion zone profiles were determined between the low and high Cr alloy steels. The high Cr stainless steels after ion nitriding displayed a hard compound layer and an abrupt diffusion zone. The compound layers of the high Cr stainless steels had a columnar structure which accounts for brittleness when layers are exposed to contact stresses. The ion nitrided surfaces of high and low Cr steels displayed a low coefficient of friction with respect to the untreated surfaces when examined in a pin and disk tribotester.

Spalvins, T.↗

NASA NTRS1985

The structure of ion plated films in relation to coating properties

Ion plating is an ion assisted or glow discharge deposition technique, where ions or energetic atoms transfer energy, momentum and charge to the substrate and the growing film in a manner which can be controlled to favorably modify surface, subsurface chemistry, and microstructure. The glow discharge energizing effects from the initial nucleation stages to the final film growth are discussed. As a result, adherence, coherence, internal stresses, density and morphology of the coatings are significantly improved, over the conventional (nonion-assisted) techniques which in turn favorably affect the surface initiated failures caused by friction, wear, erosion, corrosion and fatigue. Ion plated films because of their graded coating/substrate interface, fine, uniform, densely packed film structure also induce a surface strengthening effect which improved the mechanical properties such as yield, tensile strength and fatigue life. Since a uniform, continuous film can be obtained at lower nominal film thickness, this effect is of great importance in solid film lubrication and in corrosion protection.

Spalvins, T.↗

NASA NTRS1985

Metallic glass as a temperature sensor during ion plating

The temperature of the interface and/or a superficial layer of a substrate during ion plating was investigated using a metallic glass of the composition Fe67Co18B14Si1 as the substrate and as the temperature sensor. Transmission electron microscopy and diffraction studies determined the microstructure of the ion-plated gold film and the substrate. Results indicate that crystallization occurs not only in the film, but also in the substrate. The grain size of crystals formed during ion plating was 6 to 60 nm in the gold film and 8 to 100 nm in the substrate at a depth of 10 to 15 micrometers from the ion-plated interface. The temperature rise of the substrate during ion plating was approximately 500 C. Discontinuous changes in metallurgical microstructure, and physical, chemical, and mechanical properties during the amorphous to crystalline transition in metallic glasses make metallic glasses extremely useful materials for temperature sensor applications in coating processes.

Miyoshi, K.↗

NASA NTRS1984

Frictional and morphological properties of Au-MoS2 films sputtered from a compact target

AuMoS2 films 0.02 to 1.2 microns thick were sputtered from target compacted from 5 wt % Au + 95 wt % MoS2, to investigate the frictional and morphological film growth characteristics. The gold dispersion effects in MoS2 films are of interest to increase the densitification and strengthening of the film structure. Three microstructural growth stages were identified on the nano-micro-macrostructural level. During sliding both sputtered Au-MoS2 and MoS2 films have a tendency to break within the columner region. The remaining or effective film, about 0.2 microns thick, performs the lubrication. The Au-MoS2 films displayed a lower friction coefficient with a high degree of frictional stability and less wear debris generation as compared to pure MoS2 films. The more favorable frictional characteristics of the Au-MoS2 films are attributed to the effective film thickness and the high density packed columner zone which has a reduced effect on the fragmentation of the tapered crystallites during fracture.

Spalvins, T.↗

NASA NTRS1984

Characteristic morphological and frictional changes in sputtered MoS/sub 2 films

Three microstructural growth stages of sputtered MoS2 films were identified with respect to film thickness: (1) ridge formation during nucleation, (2) an equiaxed transition zone, and (3) a columnar-fiber-like structure. Each of these growth stages are characterized in terms of microcrystallite size, shape, and orientation. The effective lubricating film thickness is established in terms of the microstructural growth stages during sliding experiments. The film has a tendency to break up within the columnar zone. Actual lubrication is performed by the remaining film which is 0.18 to 0.22 microns thick. Also a visual screening is proposed to evaluate the integrity of the as-sputtered MoS2 film. The lubricating properties are identified with respect to optical changes before and after wiping. The orientation of the microcrystallites are responsible for the optical reflective changes observed.

Spalvins, T.↗

NASA NTRS1984

Metallic glass as a temperature sensor during ion plating

The temperature of the interface and/or a superficial layer of a substrate during ion plating was investigated using a metallic glass of the composition Fe67Co18B14Si1 as the substrate and as the temperature sensor. Transmission electron microscopy and diffraction studies determined the microstructure of the ion-plated gold film and the substrate. Results indicate that crystallization occurs not only in the film, but also in the substrate. The grain size of crystals formed during ion plating was 6 to 60 nm in the gold film and 8 to 100 nm in the substrate at a depth of 10 to 15 micrometers from the ion-plated interface. The temperature rise of the substrate during ion plating was approximately 500 C. Discontinuous changes in metallurgical microstructure, and physical, chemical, and mechanical properties during the amorphous to crystalline transition in metallic glasses make metallic glasses extremely useful materials for temperature sensor applications in coating processes.

Miyoshi, K.↗