Herbell, T. P. | Engineering Papers

NASA NTRS1993

Ceramic Composites Survive Severe Thermal Shocks

Ceramic-composite turbine blades and other components that must withstand severe thermal shocks developed for aerospace and, potentially, for terrestrial applications. Made of silicon carbide reinforced by continuous carbon fibers. Materials withstand high temperatures, exhibit high toughness, and fail gradually. Commercial applications include brake linings for fast trains and aircraft, industrial heat exchangers, and nozzles and other devices for handling molten metals.

Eckel, A. J.↗

NASA NTRS1986

Particle-size reduction of Si3N4 powder with Si3N4 milling hardware

The grinding of Si3N4 powder using reaction bonded Si3N4 attrition, vibratory, and ball mills with Si3N4 media was examined. The rate of particle size reduction and the change in the chemical composition of the powder were determined in order to compare the grinding efficiency and the increase in impurity content resulting from mill and media wear for each technique. Attrition and vibratory milling exhibited rates of specific surface area increase that were approximately eight times that observed in ball milling. Vibratory milling introduced the greatest impurity pickup.

Herbell, T. P.↗

NASA NTRS1986

Particle size reduction of Si3N4 with Si3N4 milling hardware

The grinding of Si3N4 powder using reaction bonded Si3N4 attrition, vibratory, and ball mills with Si3N4 media was examined. The rate of particle size reduction and the change in the chemical composition of the powder were determined in order to compare the grinding efficiency and the increase in impurity content resulting from mill and media wear for each technique. Attrition and vibratory milling exhibited rates of specific surface area increase that were approximately eight times that observed in ball milling. Vibratory milling introduced the greatest impurity pickup.

Herbell, T. P.↗

NASA NTRS1986

High-temperature effect of hydrogen on sintered alpha-silicon carbide

Sintered alpha-silicon carbide was exposed to pure, dry hydrogen at high temperatures for times up to 500 hr. Weight loss and corrosion were seen after 50 hr at temperatures as low as 1000 C. Corrosion of SiC by hydrogen produced grain boundary deterioration at 1100 C and a mixture of grain and grain boundary deterioration at 1300 C. Statistically significant strength reductions were seen in samples exposed to hydrogen for times greater than 50 hr and temperatures above 1100 C. Critical fracture origins were identified by fractography as either general grain boundary corrision at 1100 C or as corrosion pits at 1300 C. A maximum strength decrease of approximately 33 percent was seen at 1100 and 1300 C after 500 hr exposure to hydrogen. A computer assisted thermodynamic program was also used to predict possible reaction species of SiC and hydrogen.

Hallum, G. W.↗

NASA NTRS1985

Factors influencing the ball milling of Si3N4 in water

A statistical study of the ball milling of Si3N4 powder in Si3N4 hardware was undertaken to understand how the resulting increase in specific surface area is related to solids loading and mill speed. An attempt was made to optimize milling conditions. The degree of communication was more dependent upon solids loading than mill speed. A practical grinding limit between 0.5 and 0.75 microns was achieved in 144 hr independent of solids loading. Ball mill wear and media wear were independent of both solids loading and mill speed.

Freedman, M. R.↗

NASA NTRS1985

Parametric evaluation of ball milling of SiC in water

A statistically designed experiment was conducted to determine optimum conditions for ball milling alpha-SiC in water. The influence of pH adjustment, volume percent solids loading, and mill rotational speed on grinding effectiveness was examined. An equation defining the effect of those milling variables on specific surface area was obtained. The volume percent solids loading of the slurry had the greatest influence on the grinding effectiveness in terms of increase in specific surface area. As grinding effectiveness improved, mill and media wear also increased. Contamination was minimized by use of sintered alpha-SiC milling hardware.

Kiser, J. D.↗

NASA NTRS1985

Parametric evaluation of ball milling of SiC in water

A statistically designed experiment was conducted to determine optimum conditions for ball milling alpha-SiC in water. The influence of pH adjustment, volume percent solids loading, and mill rotational speed on grinding effectiveness was examined. An equation defining the effect of those milling variables on specific surface area was obtained. The volume percent solids loading of the slurry had the greatest influence on the grinding effectiveness in terms of increase in specific surface area. As grinding effectiveness improved, mill and media wear also increased. Contamination was minimized by use of sintered alpha-SiC milling hardware.

Kiser, J. D.↗

NASA NTRS1984

Demonstration of a silicon nitride attrition mill for production of fine pure Si and Si3N4 powders

To avoid metallic impurities normally introduced by milling ceramic powders in conventional steel hardware, an attrition mill (high-energy stirred ball mill) was constructed with the wearing parts (mill body, stirring arms, and media) made from silicon nitride. Commercial silicon and Si3N4 powders were milled to fine uniform particles with only minimal contamination - primarily from wear of the sintered Si3N4 media.

Herbell, T. P.↗

NASA NTRS1983

Characteristics of Si3N4-SiO2-Ce2O3 compositions sintered in high-pressure nitrogen

Full-density Si3N4-SiO2-Ce2O3 compositions were prepared by sintering with 2.5 MPa nitrogen pressure at temperatures of 1900 and 2090 C. Room-temperature flexural strengths near 700 MPa for sintered material compared favorably with the strength of hot-pressed material. At 1370 C, where flexural strengths as high as 363 MPa were obtained, it was observed that the coarsest structure was the strongest and the finest structure was the weakest. One of the compositions tested, Si3N4-8.7 wt pct SiO2-8.3 wt pct-Ce2O3, was found to have excellent 200-h oxidation resistance at 700, 1000, and 1370 C, without incidence of 700 to 1000 C phase instability and cracking.

Sanders, W. A.↗

NASA NTRS1982

Improved Ceramic for Heat Exchangers

Most promising composition developed in investigation consisted of mixed oxides described generically as ZrMAS. Has been commercially designated as GE-7808. Material was obtained from low-cost clay/talc mixture. Overall assessment of ZrMAS indicates it is a viable candidate for heat-exchanger application in automotive gas-turbine engines and possibly other areas that require dielectric materials of moderate refractoriness, good corrosion resistance, and excellent thermal-shock resistance.

Herbell, T. P.↗

NASA NTRS1981

Ultrasonic velocity for estimating density of structural ceramics

The feasibility of using ultrasonic velocity as a measure of bulk density of sintered alpha silicon carbide was investigated. The material studied was either in the as-sintered condition or hot isostatically pressed in the temperature range from 1850 to 2050 C. Densities varied from approximately 2.8 to 3.2 g cu cm. Results show that the bulk, nominal density of structural grade silicon carbide articles can be estimated from ultrasonic velocity measurements to within 1 percent using 20 MHz longitudinal waves and a commercially available ultrasonic time intervalometer. The ultrasonic velocity measurement technique shows promise for screening out material with unacceptably low density levels.

Klima, S. J.↗

NASA NTRS1980

Effect of milling and leaching on the structure of sintered silicon

The effects of attrition milling and acid leaching on the sintering behavior and the resultant structures of two commercial silicon powders were investigated. Sintering was performed in He for 16 hours at 1200, 1250, and 1300 C. Compacts of as-received Si did not densify during sintering. Milling reduced the average particle size to below 0.5 microns and enhanced densification (1.75 g/cc). Leaching milled Si further enhanced densification (1.90 g/cc max.) and decreased structural coarsening. After sintering, the structure of the milled and leached powder compacts appears favorable for the production of reaction bonded silicon nitride.

Yeh, H. C.↗

NASA NTRS1980

Reaction bonded silicon nitride prepared from wet attrition-milled silicon

Silicon powder wet milled in heptane was dried, compacted into test bar shape, helium-sintered, and then reaction bonded in nitrogen-4 vol% hydrogen. As-nitrided bend strengths averaged approximately 290 MPa at both room temperature and 1400 C. Fracture initiation appeared to be associated with subsurface flaws in high-strength specimens and both subsurface and surface flaws in low-strength specimens.

Herbell, T. P.↗

NASA NTRS1980

Effect of milling and leaching on the structure of sintered silicon

Sintering was performed in He for 16 hours at 1200, 1250, and 1300 C. Compacts of as-received Si did not densify during sintering. Milling reduced the average particle size to below 0.5 micrometer and enhanced densification (1.75 g/cc). Leaching milled Si further enhanced densification (1.90 g/cc max.) and decreased structural coarsening. After sintering, the structure of the milled and leached powder compacts appears favorable for the production of reaction bonded silicon nitride.

Yeh, H. C.↗

NASA NTRS1979

Bend strengths of reaction bonded silicon nitride prepared from dry attrition milled silicon powder

Dry attrition milled silicon powder was compacted, sintered in helium, and reaction bonded in nitrogen-4 volume percent hydrogen. Bend strengths of bars with as-nitrided surfaces averaged as high as 210 MPa at room temperature and 220 MPa at 1400 C. Bars prepared from the milled powder were stronger than those prepared from as-received powder at both room temperature and at 1400 C. Room temperature strength decreased with increased milling time and 1400 C strength increased with increased milling time.

Herbell, T. P.↗

NASA NTRS1978

Effect of attrition milling on the reaction sintering of silicon nitride

Silicon powder was ground in a steel attrition mill under nitrogen. Air-exposed powder was compacted, prefired in helium, and reaction-sintered in nitrogen-4 v/o hydrogen. For longer grinding times, oxygen content, surface area and compactability of the powder increased; and both alpha/beta ratio and degree of nitridation during sintering increased. Iron content remained constant.

Herbell, T. P.↗

NASA NTRS1978

Effect of attrition milling on the reaction sintering of silicon nitride

Silicon powder was ground in a steel attrition mill under nitrogen. Air exposed powder was compacted, prefired in helium, and reaction sintered in nitrogen-4 v/o hydrogen. For longer grinding times, oxygen content, surface area and compactability of the powder increased; and both alpha/beta ratio and degreee of nitridation during sintering increased. Iron content remained constant.

Herbell, T. P.↗

NASA NTRS1976

Thermogravimetric study of reduction of oxides present in oxidized nickel-base alloy powders

Carbon, hydrogen, and hydrogen plus carbon reduction of three oxidized nickel-base alloy powders (a solid solution strengthened alloy both with and without the gamma prime formers aluminum and titanium and the solid solution strengthened alloy NiCrAlY) were evaluated by thermogravimetry. Hydrogen and hydrogen plus carbon were completely effective in reducing an alloy containing chromium, columbium, tantalum, molybdenum, and tungsten. However, with aluminum and titanium present the reduction was limited to a weight loss of about 81 percent. Carbon alone was not effective in reducing any of the alloys, and none of the reducing conditions were effective for use with NiCrAlY.

Herbell, T. P.↗