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NASA NTRS2012

Enhanced-Adhesion Multi-Walled Carbon Nanotubes on Titanium Substrates for Stray Light Control

Carbon nanotubes previously grown on silicon have extremely low reflectance, making them a good candidate for stray light suppression. Silicon, however, is not a good structural material for stray light components such as tubes, stops, and baffles. Titanium is a good structural material and can tolerate the 700 C nanotube growth process. The ability to grow carbon nanotubes on a titanium substrate that are ten times blacker than the current NASA state-of-the-art paints in the visible to near infrared spectra has been achieved. This innovation will allow significant improvement of stray light performance in scientific instruments or any other optical system. This innovation is a refinement of the utilization of multiwalled carbon nano tubes for stray light suppression in spaceflight instruments. The innovation is a process to make the surface darker and improve the adhesion to the substrate, improving robustness for spaceflight use. Bright objects such as clouds or ice scatter light off of instrument structures and components and make it difficult to see dim objects in Earth observations. A darker material to suppress this stray light has multiple benefits to these observations, including enabling scientific observations not currently possible, increasing observational efficiencies in high-contrast scenes, and simplifying instruments and lowering their cost by utilizing fewer stray light components and achieving equivalent performance. The prior art was to use commercially available black paint, which resulted in approximately 4% of the light being reflected (hemispherical reflectance or total integrated scatter, or TIS). Use of multiwalled carbon nanotubes on titanium components such as baffles, entrance aperture, tubes, and stops, can decrease this scattered light by a factor of ten per bounce over the 200-nm to 2,500-nm wavelength range. This can improve system stray light performance by orders of magnitude. The purpose of the innovation is to provide an enhanced stray light control capability by making a blacker surface treatment for typical stray light control components. Since baffles, stops, and tubes used in scientific observations often undergo loads such as vibration, it was critical to develop this surface treatment on structural materials. The innovation is to optimize the carbon nanotube growth for titanium, which is a strong, lightweight structural material suitable for spaceflight use. The titanium substrate carbon nanotubes are more robust than those grown on silicon and allow for easier utilization. They are darker than current surface treatments over larger angles and larger wavelength range. The primary advantage of titanium substrate is that it is a good structural material, and not as brittle as silicon.

Hagopian, John↗

NASA NTRS1980

Effect of mechanical surface and heat treatments on erosion resistance

The effects of mechanical surface treatments as well as heat treatments on the erosion resistance of 6061 aluminum alloy and 1045 steel were studied. Mechanical surface treatments were found to have little or no effect on the erosion resistance. This is due to the formation by particle impact of a work hardened surface layer regardless of the initial surface condition. The erosion resistance of Al single crystals is found to be independent of orientation. This is due to destruction of the surface microstructure and formation of a polycrystalline surface layer by the impact of erodant particles as observed by X-ray diffraction. While upon solution treatment of annealed 6061 aluminum the increase in hardness is accompanied by an increase in erosion resistance, precipitation treatment which causes a further increase in hardness results in slightly lower erosion resistance. Using two types of erodant particles, glass beads and crushed glass, the erosion rate is found to be strongly dependent on erodant particle shape, being an order of magnitude higher for erosion with crushed glass as compared to glass beads. While for erosion with glass beads heat treatment of 1045 steel had a profound effect on its erosion resistance, little or no such effect was observed for erosion with crushed glass.

Salik, J.↗

NASA NTRS1991

Advances in silicon carbide Chemical Vapor Deposition (CVD) for semiconductor device fabrication

Improved SiC chemical vapor deposition films of both 3C and 6H polytypes were grown on vicinal (0001) 6H-SiC wafers cut from single-crystal boules. These films were produced from silane and propane in hydrogen at one atmosphere at a temperature of 1725 K. Among the more important factors which affected the structure and morphology of the grown films were the tilt angle of the substrate, the polarity of the growth surface, and the pregrowth surface treatment of the substrate. With proper pregrowth surface treatment, 6H films were grown on 6H substrates with tilt angles as small as 0.1 degrees. In addition, 3C could be induced to grow within selected regions on a 6H substrate. The polarity of the substrate was a large factor in the incorporation of dopants during epitaxial growth. A new growth model is discussed which explains the control of SiC polytype in epitaxial growth on vicinal (0001) SiC substrates.

Powell, J. Anthony↗

NASA NTRS1992

Durable, Low-Surface-Energy Treatments

Chemical treatment for creation of durable, low-surface-energy coatings for glass, ceramics and other protonated surfaces easily applied, and creates very thin semipermanent film with extremely low surface tension. Exhibits excellent stability; surfaces retreated if coating becomes damaged or eroded. Uses include water-repellent surfaces, oil-repellent surfaces, antimigration barriers, corrosion barriers, mold-release agents, and self-cleaning surfaces. Film resists wetting by water, alcohols, hydrocarbon solvents, and silicone oil. Has moderate resistance to abrasion, such as rubbing with cloths, and compression molding to polymers and composite materials.

Willis, Paul B.↗

NASA NTRS2018

Joint Strength Optimization and Damping Assessment of NiTi-Polymer Matrix Hybrid Composites

Approaches to optimize the adhesive joint strength between shape memory alloy ribbons and carbon fiber-reinforced epoxy composites were investigated for potential use as either an actuating structure or a dampening composite for structural applications. The interfacial bond strength between nickel-titanium (NiTi) and a polymer matrix composite (PMC) was measured by double lap shear testing as a function of NiTi surface treatment and adhesive material. The effect of NiTi surface treatment on damping was investigated using dynamic mechanical analysis. Lap shear data show that treating the surfaces of NiTi ribbons by light sandblasting and primer application increased the interfacial bond strength by 20 percent over the baseline composite structure. Lap shear data also reveal that out of three different film adhesives investigated, samples bonded with AF 191U and Hysol® 9696U display the highest adhesive joint strengths. Optical microscopy reveals that most samples failed by either cohesive failure within the adhesive or by adhesive failure at either the adhesive/PMC or NiTi/adhesive interface. Adhering NiTi to the PMC did not appear to negatively impact damping performance; however, a more thorough examination into NiTi's role on vibration damping should be investigated.

lap shear↗

NASA NTRS2024

Advanced Lightweight TUFROC Thermal Protection System for Space Plane Applications

Toughened Uni-piece Fibrous Reinforced Oxidation-resistant Composite (TUFROC) represents the state of the art in low-cost, reusable spacecraft Thermal Protection Systems (TPS) with high temperature capability and is flight proven on the USAF X-37B. The two-piece design takes advantage of a low-conductivity porous silica substrate combined with high-temperature-capable carbon cap and surface treatments. NASA has updated the chemical composition of the surface treatments resulting in improved high-heating capability and reusability. The new system, called Advanced TUFROC, experiences a lower surface temperature (by ~80 K) at identical aerothermal heating conditions compared to the original formulation, now called Standard TUFROC. The reduced heating is attributed to the lower catalytic efficiency of the new formulation, which results in reduced exothermic atom recombination rates at the surface. Multiple arc-jet test campaigns demonstrate that Advanced TUFROC has the ability to withstand long and repeated exposures at 1866 K or a shorter duration exposure at 1980 K without recession or damage to TPS. Furthermore, an improved arc-jet article design for assessing 3-dimensional flow over a wing leading edge has been developed and tested. This article allows for assessment of heating at a tile gap under flight-relevant conditions at significantly reduced article fabrication and arc-jet facility configuration costs compared to prior work.

TUFROC↗

NASA NTRS1986

Fracture surface analysis in composite and titanium bonding

Carbon fibers were obtained from several manufacturers. Surface treatments were performed on these fibers by anodization. The surfaces of these fibers were analyzed by X-ray photoelectron spectroscopy and wetting force measurement. The breaking strength of these fibers was measured at 2.5 cm length. It was seen that the surface treatments reduces the strength of the fibers. It was also seen that the Hercules fibers had a higher breaking strength than the Union Carbide fibers. Fiber critical length measurements showed no difference in critical lengths between AS-4 and AU-4 fibers embedded in polysulfone. However, the fiber lengths were much shorter for the surface treated fibers. This effect could be related to increased adhesion between fiber and matrix, or it could be due to the lower breaking strength of the surface treated fiber.

Devilbiss, T. A.↗

NASA NTRS2010

Fabrication and Modification of Nanoporous Silicon Particles

Silicon-based nanoporous particles as biodegradable drug carriers are advantageous in permeation, controlled release, and targeting. The use of biodegradable nanoporous silicon and silicon dioxide, with proper surface treatments, allows sustained drug release within the target site over a period of days, or even weeks, due to selective surface coating. A variety of surface treatment protocols are available for silicon-based particles to be stabilized, functionalized, or modified as required. Coated polyethylene glycol (PEG) chains showed the effective depression of both plasma protein adsorption and cell attachment to the modified surfaces, as well as the advantage of long circulating. Porous silicon particles are micromachined by lithography. Compared to the synthesis route of the nanomaterials, the advantages include: (1) the capability to make different shapes, not only spherical particles but also square, rectangular, or ellipse cross sections, etc.; (2) the capability for very precise dimension control; (3) the capacity for porosity and pore profile control; and (4) allowance of complex surface modification. The particle patterns as small as 60 nm can be fabricated using the state-of-the-art photolithography. The pores in silicon can be fabricated by exposing the silicon in an HF/ethanol solution and then subjecting the pores to an electrical current. The size and shape of the pores inside silicon can be adjusted by the doping of the silicon, electrical current application, the composition of the electrolyte solution, and etching time. The surface of the silicon particles can be modified by many means to provide targeted delivery and on-site permanence for extended release. Multiple active agents can be co-loaded into the particles. Because the surface modification of particles can be done on wafers before the mechanical release, asymmetrical surface modification is feasible. Starting from silicon wafers, a treatment, such as KOH dipping or reactive ion etching (RIE), may be applied to make the surface rough. This helps remove the nucleation layer. A protective layer is then deposited on the wafer. The protective layer, such as silicon nitride film or photoresist film, protects the wafer from electrochemical etching in an HF-based solution. A lithography technique is applied to pattern the particles onto the protective film. The undesired area of the protective film is removed, and the protective film on the back side of the wafer is also removed. Then the pattern is exposed to HF/surfactant solution, and a larger DC electrical current is applied to the wafers for a selected time. This step removes the nucleation layer. Then a DC current is applied to generate the nanopores. Next, a large electrical current is applied to generate a release layer. The particles are mechanically suspended in the solvent and collected by filtration or centrifuge.

Ferrari, Mauro↗

NASA NTRS1984

Influence of aluminum oxide film on thermocompression bonding of gold wire to evaporated aluminum film

The influence of Al surface condition on the thermocompression bonding of Au wires to Al electrodes for integrated electric circuits was studied. Au wires were connected to Al electrodes by nail-head bonding after various Al surface treatments. Bonding was evaluated by measuring the wire pull strength and fraction of the number of failures at Au-Al bonds to the total number of failures. Dependence of the fraction on applied load was derived theoretically with a parameter named critical load to take into consideration the differences in Al surface condition. The relation also held explicately for various surface treatments. Characterization of the Al surface was carried out by electron microscopy for chemical analysis.

Iwata, S.↗

NASA NTRS1985

Selected fretting-wear-resistant coatings for Ti-6 pct Al-4 pct V alloy

The ability of several wear-resistant coatings to reduce fretting in the Ti-6Al-4V alloy is investigated. The experimental apparatus and procedures for evaluating fretting in uncoated Ti-6Al-4V alloy and in the alloy with plasma-sprayed coatings, polymer-bonded coating, and surface treatments are described. The wear volume and wear rate for the alloys are measured and compared. It is concluded that Al2O3 with 13 percent TiO2, preoxidation and nitride surface treatments, and MoS2 sputtering result in wear-resistant surfaces; however, the polyimide coating is the most wear resistant coating in both dry and moist air, and it causes the least wear to the uncoated alloy surface.

Bill, R. C.↗

NASA NTRS1981

The effect of mechanical surface and heat treatments on the erosion resistance of 6061 aluminum alloy

The effects of both mechanical surface treatments and heat treatments on the erosion resistance of 6061 aluminum alloy were studied in order to gain a better understanding of material properties which affect erosion behavior. It was found that mechanical surface treatments have little or no effect on the erosion resistance. This is due to the formation by particle impact of a work-hardened surface layer, independent of the initial surface condition. The erosion resistance of aluminum single crystals was found to be independent of orientation, which is due to destruction of the surface microstructure and formation of a polycrystalline surface layer by the particle impact as observed by X-ray diffraction. Although on solution treatment of annealed aluminum 6061 the increase in hardness is accompanied by an increase in erosion resistance, precipitation treatment (which causes a further increase in hardness) results in a slightly lower erosion resistance.

Salik, J.↗

NASA NTRS1987

Surface characterization of InP using photoluminescence

Photoluminescence (PL) measurements have been performed on InP samples in situ during various surface treatments including chemical etching, wet anodization, and low-pressure chemical vapor deposition. It was found, in agreement with previously published results, that the magnitude of the PL signal varies markedly with surface treatment due presumably to changes in either surface-state density, and/or surface potential. In an attempt to assess the effectiveness of this noninvasive method as a tool for characterizing and monitoring the progressive development of a semiconductor surface during processing, a number of experiments on InP have been performed. The results indicate that although some uncertainty may exist in assigning a mechanism for the PL change in any given experiment, the general trend appears to be that surface degradation results in a reduced signal. As a result, process steps which enhance the PL intensity are likely to be beneficial in the preparation of a high-quality interface.

Chang, R. R.↗

NASA NTRS1994

Thermo-Oxidative Stability of Graphite/PMR-15 Composites: Effect of Fiber Surface Modification on Composite Shear Properties

Experiments were conducted to establish a correlation between the weight loss of a polyimide (PMR- 15) matrix and graphite fibers and the in-plane shear properties of their unidirectional composites subjected to different isothermal aging times up to 1000 hr at 316 C. The role of fiber surface treatment on the composite degradation during the thermo-oxidative aging was investigated by using A4 graphite fibers with three surface modifications: untreated (AU-4), surface treated (AS-4), and surface treated and sized with an epoxy-compatible sizing (AS-4G). The weight loss of the matrix fibers, and composites was determined during the aging. The effect of thermal aging was seen in all the fiber samples in terms of weight loss and reduction in fiber diameter. Calculated values of weight loss fluxes for different surfaces of rectangular unidirectional composite plates showed that the largest weight loss occurred at those cut surfaces where fibers were perpendicular to the surface. Consequently, the largest amount of damage was also noted on these cut surfaces. Optical observation of the neat matrix and composite plates subjected to different aging times revealed that the degradation (such as matrix microcracking and void growth) occurred in a thin surface layer near the specimen edges. The in-plane shear modulus of the composites was unaffected by the fiber surface treatment and the thermal aging. The shear strength of the composites with the untreated fibers was the lowest and it decreased with aging. A fracture surface examination of the composites with untreated fibers suggested that the weak interface allowed the oxidation reaction to proceed along the interface and thus expose the inner material to further oxidation. The results indicated that the fiber-matrix interface affected the composite degradation process during its thermal aging and that the the weak interface accelerated the composite degradation.

Madhukar, Madhu S.↗

NASA NTRS2003

Analysis of the Effect of Surface Modification on Polyimide Composites Coated with Erosion Resistant Materials

The aim of this research is to enhance performance of composite coatings through modification of graphite-reinforced polyimide composite surfaces prior to metal bond coat/ hard topcoat application for use in the erosive and/or oxidative environments of advanced engines. Graphite reinforced polyimide composites, PMR-15 and PMR-II-50, formed by sheet molding and pre-pregging will be surface treated, overlaid with a bond coat and then coated with WC-Co. The surface treatment will include cleaning, RF plasma or ultraviolet light- ozone etching, and deposition of SiO(x) groups. These surface treatments will be studied in order to investigate and improve adhesion and oxidation resistance. The following panels were provided by NASA-Glenn Research Center(NASA-GRC): Eight compression molded PMR-II-50; 6 x 6 x 0.125 in. Two vacuum-bagged PMR-II-50; 12 x 12 x 0.125 in. Eight compression molded PMR-15; 6 x 6 x 0.125 in. One vacuum-bagged PMR-15; 12 x 12 x 0.125 in. All panels were made using a 12 x 12 in. T650-35 8HS (3K-tow) graphite fabric. A diamond-wafering blade, with deionized water as a cutting fluid, was used to cut PMR-II-50 and PMR-15 panels into 1 x 1 in. pieces for surface tests. The panel edges exhibiting delamination were used for the preliminary surface preparation tests as these would be unsuitable for strength and erosion testing. PMR-15 neat resin samples were also provided by NASA GRC. Surface profiles of the as-received samples were determined using a Dektak III Surface profile measuring system. Two samples of compression molded PMR-II-50 and PMR-15, vacuum-bagged PMR-II-50 and PMR-15 were randomly chosen for surface profile measurement according to ANSI/ASME B46.1. Prior to each measurement, the samples were blasted with compressed air to remove any artifacts. Five 10 mm-long scans were made on each sample. The short and long wavelength cutoff filter values were set at 100 and 1000 m, diamond stylus radius was 12.5 microns. Table 1 is a summary of the arithmetic average roughness (Ra) and waviness (Wa) for the composite surfaces.

Ndalama, Tchinga↗

NASA NTRS1989

Surface modification of Monel K-500 as a means of reducing friction and wear in high-pressure oxygen

A study is conducted of the tribological characteristics of Monel K-500 during rubbing in a high pressure oxygen atmosphere, upon surface treatment by ion-implanted oxygen, chromium, lead, and silver, as well as electrolyzed chromium and an electroless nickel/SiC composite. The electrolyzed chromium dramatically increased total sample wear, while other surface treatments affected sample wear only moderately. Although the ion-implant treatments reduced the average coefficient of friction at low contact pressure, higher contact pressures eliminated this improvement.

Gunaji, Mohan↗

NASA NTRS1973

Synthetic sea water - An improved stress corrosion test medium for aluminum alloys

A major problem in evaluating the stress corrosion cracking resistance of aluminum alloys by alternate immersion in 3.5 percent salt (NaCl) water is excessive pitting corrosion. Several methods were examined to eliminate this problem and to find an improved accelerated test medium. These included the addition of chromate inhibitors, surface treatment of specimens, and immersion in synthetic sea water. The results indicate that alternate immersion in synthetic sea water is a very promising stress corrosion test medium. Neither chromate inhibitors nor surface treatment (anodize and alodine) of the aluminum specimens improved the performance of alternate immersion in 3.5 percent salt water sufficiently to be classified as an effective stress corrosion test method.

Humphries, T. S.↗

NASA NTRS1984

Analysis and testing for rotordynamic coefficients of turbulent annular seals with different, directionally-homogeneous surface-roughness treatment for rotor and stator elements

A combined analytical-computational method has been developed to calculate the transient pressure field and rotordynamic coefficients for high-pressure annular seals. The solution procedure applies to constant-clearance or the convergent tapered geometries of multistage centrifugal pumps which may have different surface roughness conditions on the stator and rotor seal elements. In experimental calculations with the method, the turbulent equations of Hirs (1973) are modified slightly to account for different surface roughness conditions, and a perturbation analysis is employed to develop zeroth and first order perturbation equations. Zeroth equations are also used to define both the leakage and circumferential flow due to shear stresses around the stator and rotor surfaces. The solution to analytical equations for four different surface roughnesses confirm the predicted net damping for the seals. A round-holed stator pattern yielded the highest net damping and lowest leakage of all the seals tested.

Childs, D. W.↗

NASA NTRS1993

Fuel injector design for high temperature aircraft engine

The objective of the Innovative High Temperature Aircraft Engine Fuel Nozzle Program was to design and evaluate a nozzle capable of operating at a combustor inlet air temperature of 1600 F (1144 K) and a fuel temperature of 350 F (450 K). The nozzle was designed to meet the same performance requirements and fit within the size envelope of a current production dual orifice fuel nozzle. The design approach was to use improved thermal protection and fuel passage geometry in combination with fuel passage surface treatment to minimize coking at these extreme fuel and air temperatures. Heat transfer models of several fuel injector concepts were used to optimize the thermal protection, while sample tube coking tests were run to evaluate the effect of surface finish, coatings and tube material on the coking rate. Based on heat transfer analysis, additional air gaps, reduced fuel passage flow area and use of ceramic tip components reduced local fuel wetted wall temperatures by more than 200 F (100 K) when compared to a current production fuel nozzle. Sample tube coking test results showed the importance of surface finish on the fuel coking rate. Therefore, a one micro-inch (0.025 micron) roughness was specified for all fuel passage surfaces. A novel flow divider valve in the tip was also employed to reduce weight, allow room for additional thermal protection, and provide back pressure to reduce the risk of fuel vaporization. The fuel nozzle was fabricated and evaluated in a series of high temperature coking tests. Initial results of these tests indicate that thermal protection and surface treatments were partially successful in preventing nozzle fouling, but additional refinement of the internal flowpath is needed to prevent buildup of coke particles that partially blocked the spin slots which meter the nozzle fuel flow.

R. W. Stickles↗