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NASA NTRS1994

Friction and Wear Properties of As-deposited and Carbon Ion-implanted Diamond Films

Recent work on the friction and wear properties of as-deposited and carbon ion-implanted diamond films was reviewed. Diamond films were produced by the microwave plasma chemical vapor deposition (CVD) technique. Diamond films with various grain sizes and surface roughnesses were implanted with carbon ions at 60 ke V ion energy, resulting in a dose of 1.2310(exp 17) carbon ions/cm(exp 2). Various analytical techniques, including Raman spectroscopy, proton recoil analysis, Rutherford backscattering, transmission and scanning electron microscopy, x-ray photoelectron spectroscopy, and x-ray diffraction, were utilized to characterize the diamond films. Sliding friction experiments were conducted with a polished natural diamond pin in contact with diamond films in the three environments: humid air (40 percent relative humidity), dry nitrogen (less than 1 percent relative humidity), and ultrahigh vacuum (10(exp -7) Pa). The CVD diamond films indeed have friction and were properties similar to those of natural diamond in the three environments. The as-deposited, fine-grain diamond films can be effectively used as self-lubricating, wear-resistant coatings that have low coefficients of friction (0.02 to 0.04) and low wear rates (10(exp -7) to 10(exp -8)mm(exp 3)/N-m) in both humid air and dry nitrogen. However, they have high coefficients of friction (1.5 to 1.7) and a high wear rate (10(exp -4)mm(exp 3/N-m) in ultrahigh vacuum. The carbon ion implanation produced a thin surficial layer (less than 0.1 micron thick) of amorphous, nondiamond carbon on the diamond films. In humid air and dry nitrogen, the ion-implanted, fine- and coarse-grain diamond films have a low coefficient of friction (around 0.1) and a low wear rate (10(exp -7)mm(exp 3/N-m). Even in ultrahigh vacuum, the presence of the nondiamond carbon layer reduced the coefficient of friction of fine-grain diamond films to 0.1 or lower and the wear rate to 10(exp -6)mm(exp 3)/N-m. Thus, the carbon ion-implanted, fine-grain diamond films can be effectively used as wear-resistant, self-lubricating coatings not only in air and dry nitrogen, but also in ultrahigh vacuum. The wear mechanism of diamond films is that of small fragments chipping off the surface. The size of wear particles is related to the extent of wear rates.

Miyoshi, Kazuhisa↗

NASA NTRS1998

The Development of an Edible Peanut Protein Film

The peanut is one of the crops chosen for use in NASA's Advanced Life Support Program (ALS). The peanut is a source of both oil and protein. After oil is extracted from the peanut, a protein rich flour remains. An edible peanut protein film is one use for this flour. Two types of film are developed for this study, one set of film contains 10% fat while the other set contains no fat. For film without fat the defatting of the peanut by the Soxhlet method is the first step in the manufacturing process of the film. Secondly, the protein is precipitated at its isoelectric point (pH 4.5) and centrifuged to separate the protein from the non-protein. After freeze-drying the protein it is milled in a ceramic ball mill to decrease particle size and sifted through a series of sieves to determine particle size distribution. Those particles retained on the 100 mesh sieves are utilized for film formation. Larger particles are re-ground and sifted. Five grams of protein is mixed with 50 mL of distilled water, 70 mL of 80% ethanol, 15 mL of 6N ammonium hydroxide and a plasticizer. This mixture is heated for 30 minutes until the temperature reaches 70 C. The mixture is then poured onto a level Teflon coated glass surface. After allowing the film to form overnight under a ventilation hood, it is manually removed from the plate. The processes and methods adopted have created flexible films of uniform thickness that are free of air bubbles. Thickness of films made from defatted peanut protein and partially defatted peanut protein were 0.10 Lm and 0.13 Lm respectively. Films with natural peanut fat are approximately three times as flexible and almost four times as strong as the films made without fat. Further research will be performed to evaluate its mechanical properties. This paper will greatly contribute to food preservation and waste management. Potential applications of this film are edible/biodegradable containers, wrapping for food preservation (against water, oxygen and oil), storage packets for seasonings or other ingredients and encapsulation for pharmaceutical use.

Patrick, N.↗

NASA NTRS2001

Low Temperature Growth of Nanostructured Diamond Films on Metals

The field of nanocrystalline diamond and tetrahedral amorphous carbon films has been the focus of intense experimental activity in the last few years for applications in field emission display devices, optical windows, and tribological coatings, The choice of substrate used in most studies has typically been silicon. For metals, however, the thermal expansion mismatch between the diamond film and substrate gives rise to thermal stress that often results in delamination of the film. To avoid this problem in conventional CVD deposition low substrate temperatures (less than 700 C) have been used, often with the incorporation of oxygen or carbon monoxide to the feedgas mixture. Conventionally grown CVD diamond films are also rough and would require post-deposition polishing for most applications. Therefore, there is an obvious need to develop techniques for deposition of well-adhered, smooth nano-structured diamond films on metals for various tribological applications. In our work, nanostructured diamond films are grown on a titanium alloy substrate using a two-step deposition process. The first step is performed at elevated temperature (820 C) for 30 minutes using a H2/CH4/N2 gas mixture in order to grow a thin (approx. 600 nm) nanostructured diamond layer and improve film adhesion. The remainder of the deposition involves growth at low temperature (less than 600 C) in a H2/CH4/O2 gas mixture. Laser reflectance Interferometry (LRI) pattern during growth of a nanostructured diamond film on Ti-6Al-4V alloy. The first 30 minutes are at a high temperature of 820 C and the rest of the film is grown at a low temperature of 580 T. The fringe pattern is observed till the very end due to extremely low surface roughness of 40 nm. The continuation of the smooth nanostructured diamond film growth during low temperature deposition is confirmed by in-situ laser reflectance interferometry and by post-deposition micro-Raman spectroscopy and surface profilometry. Similar experiments performed without the starting nanostructured diamond layer resulted in poorly adhered films with a more crystalline appearance and a higher surface roughness. This low temperature deposition of nanostructured diamond films on metals offers advantages in cases where high residual thermal stress leads to delamination at high temperatures.

Baker, Paul A.↗

NASA NTRS2020

Novel High Barrier Films for Packaging Food and Medicine

Long manned missions require food packaging to maintain food safety, nutrition, and acceptability for the length of 3-5 years1,2 while the shelf life assigned by NASA for current provisions is 18-24 months1. The focus of this design project was to make a polymer film specifically to function as a high oxygen barrier to later be included in an improved multi-layer packaging system of other specialized polymers with capabilities to allow for a 5-year shelf-life. To qualify as a high oxygen barrier film and to be a successful design for the future packaging, the resulting film is required to have an oxygen transmission rate (OTR) less than 0.06 cc/ m2/24 hr/atm, the standard for the current packaging3. This new film was designed to have a decreased permeability by increasing the “tortuous path” a gas molecule travels to permeate through a film. The increase in the “tortuous path” of a gas molecule is accomplished by introducing a 2D material additive. The additive chosen for this project was hexagonal boron nitride (h-BN) which exfoliates into boron nitride nanosheets (BNNs). Nylon 6 was chosen as the candidate for the matrix. This project is required to determine the best methods to synthesize the sample film and then to test the OTR of the film to determine if this design was successful. This project examined methods for pulverizing polymer resin pellets, h-BN exfoliation, and film fabrication using a hot press. This report includes the exfoliation and analysis of h-BN, procedural preparations for films, and a modeling study of estimated OTR of the h-BN/Nylon. The work in this report did not yield a high barrier composite film because of the laboratory closure in response to COVID -19 guidance but provides a concise method of the additive preparation and film synthesis. This gives a good starting point for future research in high barrier films by 2D additive composites.

Polymer, Nylon, PET, boron nitride, nanocomposite↗

NASA NTRS1965

Dry film lubricants

The Space Age has necessitated accelerated development of many technologies which have direct application to commercial, earthbound hardware. One striking example is dry film lubrication. The stimulus for the development of dry film lubricants was provided by the unsatisfactory condition created when commercial liquid lubricants were exposed to the multiple environs of space. In the search for a satisfactory solution to lubrication in space, dry films were investigated. The dry film lubrication concept has proven most desirable for space, and a natural fallout is the potential shown by such films for consumer item application. On the acceptance that the coefficient of friction of dry films is not equivalent to that of a liquid lubricant under ideal conditions, this paper discusses how the ideal condition for liquid lubrication is rarely achieved in practical applications. Comparisons are made between the performance of dry film and liquid lubricants as a function of temperature, environmental pressure, and life. Furthermore, consideration is given to the comparative costs of liquid versus dry film lubricants to show the practicality and desirability of dry film lubrication to consumer items. Although no data on the performance of consumer items lubricated with dry films are presented, the comparisons clearly establish the potential of dry film lubricants in a competitive consumer market.

SOLID LUBRICANT↗

NASA NTRS1987

Mechanical strength and tribological behavior of ion-beam deposited boron nitride films on non-metallic substrates

An investigation was conducted to examine the mechanical strength and tribological properties of boron nitride (BN) films ion-beam deposited on silicon (Si), fused silica (SiO2), gallium arsenide (GaAs), and indium phosphide (InP) substrates in sliding contact with a diamond pin under a load. The results of the investigation indicate that BN films on nonmetallic substrates, like metal films on metallic substrates, deform elastically and plastically in the interfacial region when in contact with a diamond pin. However, unlike metal films and substrates, BN films on nonmetallic substrates can fracture when they are critically loaded. Not only does the yield pressure (hardness) of Si and SiO2 substrates increase by a factor of 2 in the presence of a BN film, but the critical load needed to fracture increases as well. The presence of films on the brittle substrates can arrest crack formation. The BN film reduces adhesion and friction in the sliding contact. BN adheres to Si and SiO2 and forms a good quality film, while it adheres poorly to GaAs and InP. The interfacial adhesive strengths were 1 GPa for a BN film on Si and appreciably higher than 1 GPa for a BN film on SiO2.

Miyoshi, Kazuhisa↗

NASA NTRS1987

Mechanical strength and tribological behavior of ion-beam-deposited boron nitride films on non-metallic substrates

Miyoshi, Kazuhisa↗

NASA NTRS1990

Study of diamond film growth and properties

The objective was to study diamond film growth and its properties in order to enhance the laser damage threshold of substrate materials. Calculations were performed to evaluate laser induced thermal stress parameter, R(sub T) of diamond. It is found that diamond has several orders of magnitude higher in value for R(sub T) compared to other materials. Thus, the laser induced damage threshold (LIDT) of diamond is much higher. Diamond films were grown using a microwave plasma enhanced chemical vapor deposition (MPECVD) system at various conditions of gas composition, pressure, temperature, and substrate materials. A 0.5 percent CH4 in H2 at 20 torr were ideal conditions for growing of high quality diamond films on substrates maintained at 900 C. The diamond films were polycrystalline which were characterized by scanning electron microscopy (SEM) and Raman scattering spectroscopy. The top surface of the growing film is always rough due to the facets of polycrystalline film while the back surface of the film replicates the substrate surface. An analytical model based on two dimensional periodic heat flow was developed to calculate the effective in-plane (face parallel) diffusivity of a two layer system. The effective diffusivity of diamond/silicon samples was measured using a laser pulse technique. The thermal conductivity of the films was measured to be 13.5 W/cm K, which is better than that of a type Ia natural diamond. Laser induced damage experiments were performed on bare Si substrates, diamond film coated Si, and diamond film windows. Significant improvements in the LIDT were obtained for diamond film coated Si compared to the bare Si.

Albin, Sacharial↗

NASA NTRS1991

Synthesis and superconducting properties of Tl-Ba-Ca-Cu-O films

Tl-Ba-Ca-Cu-O superconducting films were synthesized by sputtering either from a single target or from two oxide targets in a symmetric configuration. Films with zero resistance Tc of up to 122 K were obtained after various postannealing treatments at 870-950 C under an oxygen atmosphere. The composition of the films is not very homogeneous on the submicrometer scale. The critical current of these films at 77 K is in the 1000 A/sq cm to 10,000 A/sq cm range, which is much smaller than that of films prepared on SrTiO3 and LaAlO3 substrates. The low critical current density in these films is probably due to the granularity in the films. The morphology, structure, and magnetic and superconducting properties of the films were studied. Films prepared by two different sputtering techniques have similar results which depend mostly on the film compositions and their annealing conditions. It is found that the induced magnetic flux in the film decreases rapidly with increasing temperature, indicating weak flux pinning.

Liou, S. H.↗

NASA NTRS1996

The Effect of Wake Passing on Turbine Blade Film Cooling

The effect of upstream blade row wake passing on the showerhead film cooling performance of a downstream turbine blade has been investigated through a combination of experimental and computational studies. The experiments were performed in a steady-flow annular turbine cascade facility equipped with an upstream rotating row of cylindrical rods to produce a periodic wake field similar to that found in an actual turbine. Spanwise, chordwise, and temporal resolution of the blade surface temperature were achieved through the use of an array of nickel thin-film surface gauges covering one unit cell of showerhead film hole pattern. Film effectiveness and Nusselt number values were determined for a test matrix of various injectants, injectant blowing ratios, and wake Strouhal numbers. Results indicated a demonstratable reduction in film effectiveness with increasing Strouhal number, as well as the expected increase in film effectiveness with blowing ratio. An equation was developed to correlate the span-average film effectiveness data. The primary effect of wake unsteadiness was found to be correlated well by a chordwise-constant decrement of 0.094-St. Measurable spanwise film effectiveness variations were found near the showerhead region, but meaningful unsteady variations and downstream spanwise variations were not found. Nusselt numbers were less sensitive to wake and injection changes. Computations were performed using a three-dimensional turbulent Navier-Stokes code which was modified to model wake passing and film cooling. Unsteady computations were found to agree well with steady computations provided the proper time-average blowing ratio and pressure/suction surface flow split are matched. The remaining differences were isolated to be due to the enhanced mixing in the unsteady solution caused by the wake sweeping normally on the pressure surface. Steady computations were found to be in excellent agreement with experimental Nusselt numbers, but to overpredict experimental film effectiveness values. This is likely due to the inability to match actual hole exit velocity profiles and the absence of a credible turbulence model for film cooling.

Heidmann, James David↗

NASA NTRS1996

Friction and Wear Properties of As-Deposited and Carbon Ion-Implanted Diamond Films

Recent work on the friction and wear properties of as-deposited and carbon ion-implanted diamond films was reviewed. Diamond films were produced by the microwave plasma chemical vapor deposition (CVD) technique. Diamond films with various grain sizes and surface roughnesses were implanted with carbon ions at 60 keV ion energy, resulting in a dose of 1.2 x 10(exp 17) carbon ions per cm(exp 2). Various analytical techniques, including Raman spectroscopy, proton recoil analysis, Rutherford backscattering, transmission and scanning electron microscopy, X-ray photoelectron spectroscopy, and X-ray diffraction, were utilized to characterize the diamond films. Sliding friction experiments were conducted with a polished natural diamond pin in contact with diamond films in the three environments: humid air (40% relative humidity), dry nitrogen (less than 1 percent relative humidity), and ultrahigh vacuum (10(exp -7) Pa). The CVD diamond films indeed have friction and wear properties similar to those of natural diamond in the three environments. The as-deposited, fine-grain diamond films can be effectively used as self-lubricating, wear-resistant coatings that have low coefficients of friction (0.02 to 0.04) and low wear rates (10(exp -7) to lO(exp -8) mm(exp 3) N(exp -1) m(exp -1)) in both humid air and dry nitrogen. However, they have high coefficients of friction (1.5 to 1.7) and a high wear rate (10(exp -4) mm(exp 7) N(exp -1) m(exp -1)) in ultrahigh vacuum. The carbon ion implantation produced a thin surficial layer (less than 0.1 micron thick) of amorphous, non-diamond carbon on the diamond films. In humid air and dry nitrogen, the ion-implanted, fine and coarse-grain diamond films have a low coefficient of friction (around 0.1) and a low wear rate (10(exp -7) mm(exp 3) N(exp -1) m(exp-1)). Even in ultrahigh vacuum, the presence of the non-diamond carbon layer reduced the coefficient of friction of fine-grain diamond films to 0.1 or lower and the wear rate to 10(exp -6) mm(exp 3) N(exp -1) m(exp -1). Thus, the carbon ion-implanted, fine-grain diamond films can be effectively used as wear-resistant, self-lubricating coatings not only in air and dry nitrogen, but also in ultrahigh vacuum.

Miyoshi, Kazuhisa↗

NASA NTRS2004

CuInS2 Films Deposited by Aerosol-Assisted Chemical Vapor Deposition Using Ternary Single-Source Precursors

Polycrystalline CuInS2 films were deposited by aerosol-assisted chemical vapor deposition using both solid and liquid ternary single-source precursors (SSPs) prepared in-house. Films with either (112) or (204/220) preferred orientation were obtained, and compositional analysis showed that (112)-oriented films contained more copper than (204/220)-oriented films. Using X-ray diffraction, the signature of chalcopyrite structure was often confirmed for (112)-oriented films. The preferred orientation of the film is likely related to the decomposition and reaction kinetics associated with the molecular structure of the precursors at the substrate. Interestingly, the (204/220)-oriented films were always accompanied by a secondary phase, which was identified as an unknown In-rich compound from the results of post-growth annealing, etching experiments, and Raman spectroscopic data. By increasing Cu to In ratio in the film, (112)-oriented films were obtained with a maximum grain size of about 0.5 micrometers, and their X-ray diffractions did not show any observable signature of the In secondary phase. Electrical and optical properties of all the films grown were characterized. They all showed p-type conduction with an electrical resistivity between 0.1 omega cm and 30 omega cm, and an optical band gap of 1.46eV +/- 0.02, as deposited. The material properties of deposited films revealed this methodology of using SSPs for fabricating chalcopyrite-based solar cells to be highly promising.

Jin, Michael H.-C.↗

NASA NTRS2005

Film Delivery Module For Fiber Placement Fabrication of Hybridized Composite Structures

A new fabrication technology has been developed at the NASA Marshall Space Flight Center that will allow for the fabrication of hybridized composite structures using fiber placement processing. This technology was originally developed in response to a need to address the issue of hydrogen permeation and microcracking in cryogenic propellant tanks. Numerous thin polymeric and metallized films were investigated under low temperatures conditions for use as barrier films in a composite tank. Manufacturing studies conducted at that time did not address the processing issues related to fabrication of a hybridized tank wall. A film processing head was developed that will allow for the processing of thin polymeric and metallized films, metallic foils, and adhesives using fiber placement processing machinery. The film head is designed to enable the simultaneous processing of film materials and composite tape/tow during the composite part layup process and is also capable of processing the film during an independent operation. Several initial demonstrations were conducted to assess the performance of the film module device. Such assessments included film strip lay-up accuracy, capability to fabricate panels having internal film liners, and fabrication of laminates with embedded film layers.

Hulcher, Anthony Bruce↗

NASA NTRS1979

Lubricating and wear mechanisms for a hemisphere sliding on polyimide-bonded graphite fluoride film

Friction, wear life, rider wear, and film wear for a 440 C high-temperature-stainless-steel, hemispherically tipped rider sliding against polyimide-bonded graphite fluoride films were evaluated in a moist-air atmosphere at 25 C. Optical microscope and surface profilometry observations were made at various sliding intervals to determine how film thickness affected the lubricating and failure mechanisms of the films. Two lubrication regimes operated for the same load. In the first, the film supported the load and the lubricating mechanism consisted of the shear (plastic flow) of a thin layer of the lubricant between the metallic rider and the film surface. In the second, the film did not support the load (it was worn away) and the lubricating mechanism consisted of the shear of very thin lubricant films between flat areas generated on the rider and on sandblasted metallic asperities in the film wear track. Lubricant was supplied from the valleys between the asperities or from the sides of the wear track. With thicker films, wear life increased since a greater lubricant supply was available from the sides of the wear track.

Fusaro, R. L.↗

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

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 percent Au + 95 wt percent MoS2, to investigate the frictional and morphological film growth characteristics. The gold dispersion effects in MoS2 films are of interest to increase the densification 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

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 pct. Au + 95 wt pct. 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 NTRS1990

Preparation and characteristics of superconducting cuprate thin films: Nd(2-x)Ce(x)CuO4 and substituted Bi-system

Characteristics of the electron-doped-type Nd(2-x)Ce(x)CuO4 systems and substituted Bi2(Sr,Ln)3Cu2Oy system were systematically studied using the high quality thin-film samples. The Nd(2-x)Ce(x)CuO4 thin films with various Ce concentrations, x, were prepared by RF magnetron sputtering on SrTiO3 heated at around 500 C. After subsequent annealing at 1100 C in air, the films showed the c-axis orientation normal to the substrates. By means of the reducing treatment (annealing in a vacuum), superconductivity was induced for the films with 0.14 is less than or equal to x is less than or equal to 0.18. The superconductivity and transport properties of the films were strongly affected by the reducing treatment. The x = 0.15 film exhibited a sharp superconducting transition with zero resistivity at 22 K, in consistent with the diamagnetic properties. The resistivity of the films was fairly low with metallic characteristics, and the sight of the Hall coefficient was negative in the normal state. On the other hand, the normal-state optical measurements showed that the undoped Nd2CuO4 is a semiconductor with a charge transfer gap of 1.3 eV, and that, when Ce ions were doped, a plasma reflection due to the free-carriers came to be seen with the plasma frequency of 1.07 eV for 0.14 is less than or equal to x is less than or equal to 0.18. Moreover, x ray photoemission study revealed that the Cu valence of the film decreased for 2(+) for x = 0 to 1(+) for x = 0.15. These physical properties are in contrast with those of hole-doped-type cuprate superconductors. Bi2(Sr,Ln)3Cu2Oy thin films were also prepared on MgO substrates heated at 600 to 700 C by similar methods. It was found that the growth conditions for Bi-systems with two CuO2 planes were different for each composition and species of lanthanoid in the films. Moreover, preparation of Bi-system with three CuO2 planes was very difficult when lanthanoid atoms were doped in the system. Their electric transport properties and x ray photoemission spectroscopy were investigated. Carrier concentration and Cu valence were discussed with regard to the superconductivity.

Adachi, H.↗