Strengths, fracture toughnesses, hardnesses, and dimensional changes have been measured for RBSN and RBSN/SiC composites. Samples were made from mixtures of Si and either Si- or C-rich SiC powders. For pure, 75 pct dense RBSN dispersed with octanol, strengths up to 858 MPa have been achieved. Improved strengths result from a combination of microstructural perfection and increased fracture toughness. The mechanical properties of the composites were approximately equal to those of methanol processed RBSN but not quite equal to those of the octanol-processed RBSN. Results are discussed in terms of observed microstructural features.

Lightfoot, A.↗

NASA NTRS1989

Nitriding kinetics of Si-SiC powder mixtures as simulations of reaction bonded Si3N4-SiC composites

The nitriding kinetics of Si and Si plus SiC powder mixtures were studied to simulate the fabrication of RBSN-SiC ceramic matrix composites. Very clean, assynthesized, and solvent-exposed powders were studied; C-rich and Si-rich SiC 0.04-0.05 micron diameter powders were mixed in varying concentrations with SiH4-derived 0.2-0.3 micron diameter Si powder. Complete nitridation is achieved with C-rich SiC powders in 140 min at 1250 C, and in the centers of Si-rich SiC powders in 15 min. The effects on the incubation periods, fast reaction periods, and slow reaction periods that characterize these nitriding processes were studied to explain unusual reverse reaction gradients and other effects of contamination.

Lightfoot, A.↗

NASA NTRS1987

Processing of laser formed SiC powder

Processing research was undertaken to demonstrate that superior SiC characteristics could be achieved through the use of ideal constituent powders and careful post-synthesis processing steps. Initial research developed the means to produce approximately 1000 A uniform diameter, nonagglomerated, spherical, high purity SiC powders. Accomplishing this goal required major revision of the particle formation and growth model from one based on classical nucleation and growth to one based on collision and coalescence of Si particles followed by their carburization. Dispersions based on pure organic solvents as well as steric stabilization were investigated. Test parts were made by the colloidal pressing technique; both liquid filtration and consolidation (rearrangement) stages were modeled. Green densities corresponding to a random close packed structure were achieved. After drying, parts were densified at temperatures ranging from 1800 to 2100 C. This research program accomplished all of its major objectives. Superior microstructures and properties were attained by using powders having ideal characteristics and special post-synthesis processing procedures.

Haggerty, J. S.↗

NASA NTRS1985

Processing of laser formed SiC powder

Superior SiC characteristics can be achieved through the use of ideal constituent powders and careful post-synthesis processing steps. High purity SiC powders of approx. 1000 A uniform diameter, nonagglomerated and spherical were produced. This required major revision of the particle formation and growth model from one based on classical nucleation and growth to one based on collision and coalescence of Si particles followed by their carburization. Dispersions based on pure organic solvents as well as steric stabilization were investigated. Although stable dispersions were formed by both, subsequent part fabrication emphasized the pure solvents since fewer problems with drying and residuals of the high purity particles were anticipated. Test parts were made by the colloidal pressing technique; both liquid filtration and consolidation (rearrangement) stages were modeled. Green densities corresponding to a random close packed structure (approx. 63%) were achieved; this highly perfect structure has a high, uniform coordination number (greater than 11) approaching the quality of an ordered structure without introducing domain boundary effects. After drying, parts were densified at temperatures ranging from 1800 to 2100 C. Optimum densification temperatures will probably be in the 1900 to 2000 C range based on these preliminary results which showed that 2050 C samples had experienced substantial grain growth. Although overfired, the 2050 C samples exhibited excellent mechanical properties. Biaxial tensile strengths up to 714 MPa and Vickers hardness values of 2430 kg/sq mm 2 were both more typical of hot pressed than sintered SiC. Both result from the absence of large defects and the confinement of residual porosity (less than 2.5%) to small diameter, uniformly distributed pores.

Haggerty, J. S.↗

NASA NTRS1985

Synthesis of ceramic powders and surface films from laser heated gases

Two new processes have been developed that are based on laser-heated gases. Both permit unusually precise levels of process control and, thereby, materials having superior properties. The power process yields Si, Si3N4 and SiC powders that are uniform in size, nonagglomerated, small diameter, spherically shaped and high purity. Manufacturing cost analyses show that submicron powders can be made with an energy cost of approximately 2 kWhr/kg and a dollar cost of 2-3.30 $/kg, exclusive of the costs of feed materials. The laser-induced chemical vapor deposition process (LICVD) causes reactant gases to be heated by absorbing IR light from a laser beam that passes parallel to the substrate surface. Laser heating permits independent control of gas and substrate temperatures while operating in a conventional, thermally activated chemical vapor deposition mode. Spin density, hydrogen content, electrical conductivity and mobility gap properties show the LICVD process capable of producing very high quality films.

Haggerty, J. S.↗

NASA NTRS1982

Laser materials processing facility

The laser materials processing facility and its capabilities are described. A CO2 laser with continuous wave, repetitive pulse, and shaped power-time cycles is employed. The laser heated crystal growth station was used to produce metal and metal oxide single crystals and for cutting and shaping experiments using Si3N4 to displace diamond shaping processes.

Haggerty, J. S.↗

NASA NTRS1976

Float-zone processing in a weightless environment

The results were reported of investigations to: (1) test the validity of analyses which set maximum practical diameters for Si crystals that can be processed by the float zone method in a near weightless environment, (2) determine the convective flow patterns induced in a typical float zone, Si melt under conditions perceived to be advantageous to the crystal growth process using flow visualization techniques applied to a dimensionally scaled model of the Si melt, (3) revise the estimates of the economic impact of space produced Si crystal by the float zone method on the U.S. electronics industry, and (4) devise a rational plan for future work related to crystal growth phenomena wherein low gravity conditions available in a space site can be used to maximum benefit to the U.S. electronics industry.

Fowle, A. A.↗

NASA NTRS1974

Float zone processing in a weightless environment

Results are given for investigations into: (1) the physical limits which set the maximum practical diameters of Si crystals that can be processed by the float-zone method in a near weightless environment, and (2) the economic impact of large, space-produced Si crystals on the electronics industry. The stability of the melt is evaluated. Heat transfer and fluid flow within the melt as dependent on the crystal size and the degree and type of rotation imparted to the melt are studied. Methods of utilizing the weightless environment for the production of large, stress-free Si crystals of uniform composition are proposed. The economic effect of large size Si crystals, their potential applications, likely utilization and cost advantages in LSI, integrated circuits, and power devices are also evaluated. Foreseeable advantages of larger diameter wafers of good characteristics and the possibilities seen for greater perfection resulting from stress-free growth are discussed.

Fowle, A. A.↗

NASA NTRS1972

Improved synthesis of intermetal compounds

Method in crystal growth using liquid encapsulation techniques permits GaAs synthesis of materials from constituent elements whose vapor pressures are high at temperature at which they react spontaneously. Techniques may be useful for synthesis of GaP.

Haggerty, J. S.↗

NASA NTRS1972

Production of fibers by a floating zone fiber drawing technique

A CO2 laser heated, floating zone fiber growth process was developed. The resulting Al2O3 fibers exhibited the high room temperature strengths for large diameter fibers as well as high specific creep rupture strengths observed at 1093 C and 1316 C (2000 F and 2400 F). Single crystal fibers of TiC and Y2O3 were also grown. An optical system was developed to focus four CO2 laser beams onto the surface of a feed rod permitting the formation of highly controllable molten zones. The optical system permitted energy densities and angle of incidence of the beams to be adjusted over wide ranges. This optical system was incorporated into a controlled atmosphere, fiber growth furnace. The two principal advantages of a CO2 laser heat source are that ambient atmospheres may be freely selected to optimize fiber properties and the laser has no inherent temperature limit, so extremely high melting point materials can be melted. Both advantages were demonstrated.

Haggerty, J. S.↗

NASA NTRS1971

Production of oxide fibers by a floating zone fiber drawing technique Final report

Production of aluminum oxide fibers by floating zone fiber drawing technique

Haggerty, J. S.↗