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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 NTRS1998

Surface Area, and Oxidation Effects on Nitridation Kinetics of Silicon Powder Compacts

Commercially available silicon powders were wet-attrition-milled from 2 to 48 hr to achieve surface areas (SA's) ranging from 1.3 to 70 sq m/g. The surface area effects on the nitridation kinetics of silicon powder compacts were determined at 1250 or 1350 C for 4 hr. In addition, the influence of nitridation environment, and preoxidation on nitridation kinetics of a silicon powder of high surface area (approximately equals 63 sq m/g) was investigated. As the surface area increased, so did the percentage nitridation after 4 hr in N2 at 1250 or 1350 C. Silicon powders of high surface area (greater than 40 sq m/g) can be nitrided to greater than 70% at 1250 C in 4 hr. The nitridation kinetics of the high-surface-area powder compacts were significantly delayed by preoxidation treatment. Conversely, the nitridation environment had no significant influence on the nitridation kinetics of the same powder. Impurities present in the starting powder, and those accumulated during attrition milling, appeared to react with the silica layer on the surface of silicon particles to form a molten silicate layer, which provided a path for rapid diffusion of nitrogen and enhanced the nitridation kinetics of high surface area silicon powder.

Bhatt, R. T.↗

NASA NTRS1994

Resistance of Silicon Nitride Turbine Components to Erosion and Hot Corrosion/oxidation Attack

Silicon nitride turbine components are under intensive development by AlliedSignal to enable a new generation of higher power density auxiliary power systems. In order to be viable in the intended applications, silicon nitride turbine airfoils must be designed for survival in aggressive oxidizing combustion gas environments. Erosive and corrosive damage to ceramic airfoils from ingested sand and sea salt must be avoided. Recent engine test experience demonstrated that NT154 silicon nitride turbine vanes have exceptional resistance to sand erosion, relative to superalloys used in production engines. Similarly, NT154 silicon nitride has excellent resistance to oxidation in the temperature range of interest - up to 1400 C. Hot corrosion attack of superalloy gas turbine components is well documented. While hot corrosion from ingested sea salt will attack silicon nitride substantially less than the superalloys being replaced in initial engine applications, this degradation has the potential to limit component lives in advanced engine applications. Hot corrosion adversely affects the strength of silicon nitride in the 850 to 1300 C range. Since unacceptable reductions in strength must be rapidly identified and avoided, AlliedSignal and the NASA Lewis Research Center have pioneered the development of an environmental life prediction model for silicon nitride turbine components. Strength retention in flexure specimens following 1 to 3300 hour exposures to high temperature oxidation and hot corrosion has been measured and used to calibrate the life prediction model. Predicted component life is dependent upon engine design (stress, temperature, pressure, fuel/air ratio, gas velocity, and inlet air filtration), mission usage (fuel sulfur content, location (salt in air), and times at duty cycle power points), and material parameters. Preliminary analyses indicate that the hot corrosion resistance of NT154 silicon nitride is adequate for AlliedSignal's initial engine applications. Protective coatings and/or inlet air filtration may be required to achieve required ceramic component lives in more aggressive environments.

Strangmen, Thomas E.↗

NASA NTRS1982

Method of densifying an article formed of reaction bonded silicon nitride

A method of densifying an article formed of reaction bonded silicon nitride is disclosed. The reaction bonded silicon nitride article is packed in a packing mixture consisting of silicon nitride powder and a densification aid. The reaction bonded silicon nitride article and packing powder are sujected to a positive, low pressure nitrogen gas treatment while being heated to a treatment temperature and for a treatment time to cause any open porosity originally found in the reaction bonded silicon nitride article to be substantially closed. Thereafter, the reaction bonded silicon nitride article and packing powder are subjected to a positive high pressure nitrogen gas treatment while being heated to a treatment temperature and for a treatment time to cause a sintering of the reaction bonded silicon nitride article whereby the strength of the reaction bonded silicon nitride article is increased.

Mangels, John A.↗

NASA NTRS2008

Group-III Nitride Field Emitters

Field-emission devices (cold cathodes) having low electron affinities can be fabricated through lattice-mismatched epitaxial growth of nitrides of elements from group III of the periodic table. Field emission of electrons from solid surfaces is typically utilized in vacuum microelectronic devices, including some display devices. The present field-emission devices and the method of fabricating them were developed to satisfy needs to reduce the cost of fabricating field emitters, make them compatible with established techniques for deposition of and on silicon, and enable monolithic integration of field emitters with silicon-based driving circuitry. In fabricating a device of this type, one deposits a nitride of one or more group-III elements on a substrate of (111) silicon or other suitable material. One example of a suitable deposition process is chemical vapor deposition in a reactor that contains plasma generated by use of electron cyclotron resonance. Under properly chosen growth conditions, the large mismatch between the crystal lattices of the substrate and the nitride causes strains to accumulate in the growing nitride film, such that the associated stresses cause the film to crack. The cracks lie in planes parallel to the direction of growth, so that the growing nitride film becomes divided into microscopic growing single-crystal columns. The outer ends of the fully-grown columns can serve as field-emission tips. By virtue of their chemical compositions and crystalline structures, the columns have low work functions and high electrical conductivities, both of which are desirable for field emission of electrons. From examination of transmission electron micrographs of a prototype device, the average column width was determined to be about 100 nm and the sharpness of the tips was determined to be characterized by a dimension somewhat less than 100 nm. The areal density of the columns was found to about 5 x 10(exp 9)/sq cm . about 4 to 5 orders of magnitude greater than the areal density of tips in prior field-emission devices. The electric field necessary to turn on the emission current and the current per tip in this device are both lower than in prior field-emission devices, such that it becomes possible to achieve longer operational lifetime. Moreover, notwithstanding the lower current per tip, because of the greater areal density of tips, it becomes possible to achieve greater current density averaged over the cathode area. The thickness of the grown nitride film (equivalently, the length of the columns) could lie between about 0.5 microns and a few microns; in any event, a thickness of about 1 micron is sufficient and costs less than do greater thicknesses. It may be possible to grow nitride emitter columns on glass or other substrate materials that cost less than silicon does. What is important in the choice of substrate material is the difference between the substrate and nitride crystalline structures. Inasmuch as the deposition process is nondestructive, an ability to grow emitter columns on a variety of materials would be advantageous in that it would facilitate the integration of field-emitter structures onto previously processed integrated circuits.

Bensaoula, Abdelhak↗

NASA NTRS1979

Feasibility study of silicon nitride protection of plastic encapsulated semiconductors

The application of low temperature silicon nitride protective layers on wire bonded integrated circuits mounted on lead frame assemblies is reported. An evaluation of the mechanical and electrical compatibility of both plasma nitride and photochemical silicon nitride (photonitride) passivations (parallel evaluations) of integrated circuits which were then encapsulated in plastic is described. Photonitride passivation is compatible with all wire bonded lead frame assemblies, with or without initial chip passivation. Plasma nitride passivation of lead frame assemblies is possible only if the chip is passivated before lead frame assembly. The survival rate after the environmental test sequence of devices with a coating of plasma nitride on the chip and a coating of either plasma nitride or photonitride over the assembled device is significantly greater than that of devices assembled with no nitride protective coating over either chip or lead frame.

Peters, J. W.↗

NASA NTRS1984

RF sputtered silicon and hafnium nitrides as applied to 440C steel

Silicon nitride and hafnium nitride coatings were deposited 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. The coatings and the interface between the coating and substrate were investigated by X-ray diffractometry, scanning electron microscopy, energy dispersive X-ray analysis and Auger electron spectroscopy. Oxide was found at all interfaces with an interface width of at least 600 A for the oxidized substrates and at least 300 A for the unoxidized substrates. 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. Coatings of both nitrides deposited at 8 mtorr were found to have increased adhesion to both oxidized and unoxidized 440C over those deposited at 20 mtorr.

Grill, A.↗

NASA NTRS2001

Feasibility of Actively Cooled Silicon Nitride Airfoil for Turbine Applications Demonstrated

Nickel-base superalloys currently limit gas turbine engine performance. Active cooling has extended the temperature range of service of nickel-base superalloys in current gas turbine engines, but the margin for further improvement appears modest. Therefore, significant advancements in materials technology are needed to raise turbine inlet temperatures above 2400 F to increase engine specific thrust and operating efficiency. Because of their low density and high-temperature strength and thermal conductivity, in situ toughened silicon nitride ceramics have received a great deal of attention for cooled structures. However, the high processing costs and low impact resistance of silicon nitride ceramics have proven to be major obstacles for widespread applications. Advanced rapid prototyping technology in combination with conventional gel casting and sintering can reduce high processing costs and may offer an affordable manufacturing approach. Researchers at the NASA Glenn Research Center, in cooperation with a local university and an aerospace company, are developing actively cooled and functionally graded ceramic structures. The objective of this program is to develop cost-effective manufacturing technology and experimental and analytical capabilities for environmentally stable, aerodynamically efficient, foreign-object-damage-resistant, in situ toughened silicon nitride turbine nozzle vanes, and to test these vanes under simulated engine conditions. Starting with computer aided design (CAD) files of an airfoil and a flat plate with internal cooling passages, the permanent and removable mold components for gel casting ceramic slips were made by stereolithography and Sanders machines, respectively. The gel-cast part was dried and sintered to final shape. Several in situ toughened silicon nitride generic airfoils with internal cooling passages have been fabricated. The uncoated and thermal barrier coated airfoils and flat plates were burner rig tested for 30 min without and with air cooling. Without cooling, the surface temperature of the flat plate reached approximately 2350 F. Starting with computer aided design (CAD) files of an airfoil and a flat plate with internal cooling passages, the permanent and removable mold components for gel casting ceramic slips were made by stereolithography and Sanders machines, respectively. The gel-cast part was dried and sintered to final shape. Several in situ toughened silicon nitride generic airfoils with internal cooling passages have been fabricated. The uncoated and thermal barrier coated airfoils and flat plates were burner rig tested for 30 min without and with air cooling. Without cooling, the surface temperature of the flat plate reached approximately 2350 F. With cooling, the surface temperature decreased to approximately 1910 F--a drop of approximately 440 F. This preliminary study demonstrates that a near-net-shape silicon nitride airfoil can be fabricated and that silicon nitride can sustain severe thermal shock and the thermal gradients induced by cooling and, thus, is a viable candidate for cooled components.

Bhatt, Ramakrishna T.↗

NASA NTRS1987

Stability and rheology of dispersions of silicon nitride and silicon carbide

The relationship between the surface and colloid chemistry of commercial ultra-fine silicon carbide and silicon nitride powders was examined by a variety of standard characterization techniques and by methodologies especially developed for ceramic dispersions. These include electrokinetic measurement, surface titration, and surface spectroscopies. The effects of powder pretreatment and modification strategies, which can be utilized to augment control of processing characteristics, were monitored with these technologies. Both silicon carbide and nitride were found to exhibit silica-like surface chemistries, but silicon nitride powders possess an additional amine surface functionality. Colloidal characteristics of the various nitride powders in aqueous suspension is believed to be highly dependent on the relative amounts of the two types of surface groups, which in turn is determined by the powder synthesis route. The differences in the apparent colloidal characteristics for silicon nitride powders cannot be attributed to the specific absorption of ammonium ions. Development of a model for the prediction of double-layer characteristics of materials with a hybrid site interface facilitated understanding and prediction of the behavior of both surface charge and surface potential for these materials. The utility of the model in application to silicon nitride powders was demonstrated.

Feke, Donald L.↗

NASA NTRS2018

Friction and Wear of Unlubricated NiTiHf with Nitriding Surface Treatments

The unlubricated friction and wear properties of the superelastic materials NiTi and NiTiHf, treated by either gas nitriding or plasma nitriding, have been investigated. Pin on disk testing of the studied materials was performed at sliding speeds from 0.01 to 1m/s at normal loads of 1, 5 or 10N. For all of the studied friction pairs (NiTiHf pins vs. NiTi and NiTiHf disks) over the given parameters, the steady-state coefficients of friction varied from 0.22 to 1.6. Pin wear factors ranged from approximately 1E-6 against the NiTiHf and plasma nitrided disks to approximately 1E-4 for the gas nitrided disks. The plasma nitrided disks provided wear protection in several cases and tended to wear by adhesion. The gas nitrided treatment generated the most pin wear but had essentially no disk wear except at the most severe of the studied conditions (1N load and 1m/s sliding speed). The results of this study are expected to provide guidance for design of components such as gears and fasteners.

friction↗

NASA NTRS1972

Rolling-element fatigue life of silicon nitride balls: Preliminary test results

Hot pressed silicon nitride was evaluated as a rolling element bearing material. The five-ball fatigue tester was used to test 12.7 mm (0.500 in.) diameter balls at a maximum Hertz stress of 800,000 psi at a race temperature of 130 F. The fatigue spalls in the silicon nitride resembled those in typical bearing steels. The ten-percent fatigue life of the silicon nitride balls was approximately one-eighth to one-fifth that of typical bearing steels (52100 and M-50). The load capacity of the silicon nitride was approximately one-third that of typical bearing steels. The load capacity of the silicon nitride was significantly higher than previously tested ceramic materials for rolling element bearings.

Parker, R. J.↗

NASA NTRS1974

Fatigue life of high-speed ball bearings with silicon nitride balls

Hot-pressed silicon nitride was evaluated as a rolling-element bearing material. The five-ball fatigue tester was used to test 12.7-mm- diameter silicon nitride balls at maximum Hertz stresses ranging from 4.27 x 10 to the 9th power n/sq m to 6.21 x 10 to the 9th power n/sq m at a race temperature of 328K. The fatigue life of NC-132 hot-pressed silicon nitride was found to be equal to typical bearing steels and much greater than other ceramic or cermet materials at the same stress levels. A digital computer program was used to predict the fatigue life of 120-mm- bore angular-contact ball bearings containing either steel or silicon nitride balls. The analysis indicates that there is no improvement in the lives of bearings of the same geometry operating at DN values from 2 to 4 million where silicon nitride balls are used in place of steel balls.

Parker, R. J.↗

NASA NTRS1975

The preparation and properties of aluminum nitride films

Aluminum nitride films have been deposited on silicon substrates at 800-1200 C by the pyrolysis of an aluminum trichloride-ammonia complex, AlCl3.3NH3, in a gas flow system. The deposit was transparent, tightly adherent to the substrate, and was confirmed to be aluminum nitride by X-ray and electron diffraction techniques. The deposited aluminum nitride films were found to be polycrystalline with the crystallite size increasing with increasing temperature of deposition. Other properties of aluminum nitride films relevant to device applications, including density, refractive index, dissolution rate, dielectric constant, and masking ability, have been determined. These properties indicate that aluminum nitride films have potential as a dielectric in electronic devices.

Chu, T. L.↗

NASA NTRS1976

Friction and transfer behavior of pyrolytic boron nitride in contact with various metals

Sliding friction experiments were conducted with pyrolytic boron nitride in sliding contact with itself and various metals. Auger emission spectroscopy was used to monitor transfer of pyrolytic boron nitride to metals and metals to pyrolytic boron nitride. Results indicate that the friction coefficient for pyrolytic boron nitride in contact with metals can be related to the chemical activity of the metals and more particularly to the d valence bond character of the metal. Transfer was found to occur to all metals except silver and gold and the amount of transfer was less in the presence than in the absence of metal oxide. Friction was less for pyrolytic boron nitride in contact with a metal in air than in vacuum.

Buckley, D. H.↗

NASA NTRS1979

Formation of porous surface layers in reaction bonded silicon nitride during processing

An effort was undertaken to determine if the formation of the generally observed layer of large porosity adjacent to the as-nitride surfaces of reaction bonded silicon nitrides could be prevented during processing. Isostatically pressed test bars were prepared from wet vibratory milled Si powder. Sintering and nitriding were each done under three different conditions:(1) bars directly exposed to the furnance atmosphere; (2) bars packed in Si powder; (3) bars packed in Si3N4 powder. Packing the bars in either Si of Si3N4 powder during sintering retarded formation of the layer of large porosity. Only packing the bars in Si prevented formation of the layer during nitridation. The strongest bars (316 MPa) were those sintered in Si and nitrided in Si3N4 despite their having a layer of large surface porosity; failure initiated at very large pores and inclusions. The alpha/beta ratio was found to be directly proportional to the oxygen content; a possible explanation for this relationship is discussed.

Shaw, N. J.↗

NASA NTRS1981

Nitridation of silicon

Silicon powders with three levels of impurities, principally Fe, were sintered in He or H2. Non-densifying mechanisms of material transport were dominant in all cases. High purity Si showed coarsening in He while particle growth was suppressed in H2. Lower purity powder coarsened in both He and H2. The same three Si powders and Si /111/ single crystal wafers were nitrided in both N2 and N2/H2 atmospheres. Hydrogen increased the degree of nitridation of all three powders and the alpha/beta ratio of the lower purity powder. Some Si3N4 whiskers and open channels through the surface nitride layer were observed in the presence of Fe, correlating with the nitridation-enhancing effects of Fe. Thermodynamic calculations showed that when SiO2 is present on the Si, addition of H2 to the nitriding atmosphere decreases the amount of SiO2 and increases the partial pressure of Si-containing vapor species, that is, Si and SiO. Large amounts of NH3 and SiH4 were also predicted to form.

Shaw, N. J.↗

NASA NTRS1983

Nitriding of titanium and titanium: 8 percent aluminum, 1 percent molybdenum, 1 percent vanadium alloy with an ion-beam source

Titanium and Ti-8Al-1Mo-1V alloy were nitrided with an ion-beam source of nitrogen or argon and nitrogen at a total pressure of 2 x 10 to the minus 4th power to 10 x 10 to the minus 4th power torr. The treated surface was characterized by surface profilometry, X-ray diffractometry, Auger electron spectroscopy and microhardness measurements. The tetragonal Ti2N phase formed in pure titanium and Ti-8Al-1Mo-1V alloy with traces of AlN in the alloy. Two opposite processes competed during the ion-beam-nitriding process: (1) formation of nitrides in the surface layer and (2) sputtering of the nitrided layers by the ion beam. The highest surface hardnesses, about 500 kg/sq mm in titanium and 800 kg/sq mm in Ti-8Al-1Mo-1V, were obtained by ion nitriding with an ion beam of pure nitrogen at 4.2 x 10 to the minus 4th power torr at a beam voltage of 1000 V.

Gill, A.↗

NASA NTRS1985

Study of the kinetics and mechanism of the thermal nitridation of SiO2

X-ray photoelectron spectroscopy (XPS) has been used to study the nitridation time and temperature dependence of the nitrogen distribution in thermally nitrided SiO2 films. The XPS data show that the maximum nitrogen concentration near the (SiO(x)N(y)/Si interface is initially at the interface, but moves 20-25 A away from the interface with increasing nitridation time. Computer modeling of the kinetic processes involved is carried out and reveals a mechanism in which diffusing species, initially consisting primarily of nitrogen, react with the substrate, followed by formation of the oxygen-rich oxynitride due to reaction of the diffusing oxygen displaced by the slower nitridation of the SiO2. The data are consistent with this mechanism provided the influence of the interfacial strain on the nitridation and oxidation kinetics is explicitly accounted for.

Vasquez, R. P.↗