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At least 307 records · Page 17

Simultaneous Spark Plasma Sintering of Multiple Complex Shapes

This work addresses the two great challenges of the spark plasma sintering (SPS) process: The sintering of complex shapes and the simultaneous production of multiple parts. A new controllable interface method is employed to concurrently consolidate two nickel gear shapes by SPS. A graphite deformable sub-mold is specifically designed for the mutual densification of both complex parts in a unique 40 mm powder deformation space. An energy efficient SPS configuration is developed to allow the sintering of a large-scale powder assembly under electric current lower than 900 A. The stability of the developed process is studied by electro-thermal-mechanical (ETM) simulation. The ETM simulation reveals that homogeneous densification conditions can be attained by inserting an alumina powder at the sample/punches interfaces, enabling the energy efficient heating and the thermal confinement of the nickel powder. Finally, the feasibility of the fabrication of the two near net shape gears with a very homogeneous microstructure is demonstrated.

36 MATERIALS SCIENCE↗

A Comprehensive Characterization of Pyrolysis Oil from Softwood Barks

Pyrolysis of raw pine bark, pine, and Douglas-Fir bark was examined. The pyrolysis oil yields of raw pine bark, pine, and Douglas-Fir bark at 500 °C were 29.18%, 26.67%, and 26.65%, respectively. Both energy densification ratios (1.32–1.56) and energy yields (48.40–54.31%) of char are higher than pyrolysis oils (energy densification ratios: 1.13–1.19, energy yields: 30.16–34.42%). The pyrolysis oils have higher heating values (~25 MJ/kg) than bio-oils (~20 MJ/kg) from wood and agricultural residues, and the higher heating values of char (~31 MJ/kg) are comparable to that of many commercial coals. The elemental analysis indicated that the lower O/C value and higher H/C value represent a more valuable source of energy for pyrolysis oils than biomass. The nuclear magnetic resonance results demonstrated that the most abundant hydroxyl groups of pyrolysis oil are aliphatic OH groups, catechol, guaiacol, and p-hydroxy-phenyl OH groups. The aliphatic OH groups are mainly derived from the cleavage of cellulose glycosidic bonds, while the catechol, guaiacol, and p-hydroxy-phenyl OH groups are mostly attributed to the cleavage of the lignin β–O-4 bond. Significant amount of aromatic carbon (~40%) in pyrolysis oils is obtained from tannin and lignin components and the aromatic C–O bonds may be formed by a radical reaction between the aromatic and aliphatic hydroxyl groups. In this study, a comprehensive analytical method was developed to fully understand and evaluate the pyrolysis products produced from softwood barks, which could offer valuable information on the pyrolysis mechanism of biomass and promote better utilization of pyrolysis products.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Infiltration of Nanoparticles into Porous Binder Jet Printed Parts

The densification of parts that are produced by binder jetting Additive Manufacturing (AM; a.k.a. “3D Printing”) is an essential step in making them mechanically useful. By increasing the packing factor of the powder bed by incorporating nanoparticles into the binder has potential to alleviate the amount of shrinkage needed for full densification of binder jet parts. We present preliminary data on the use of 316L Stainless Steel Nanoparticles (SSN) to densify 316L stainless steel binder jet parts. Aqueous solutions of Diethylene Glycol (DEG) or Ethylene Glycol (EG) were prepared at different DEG/water and EG/water molar ratios; pH of the solutions was adjusted by the use of 0.10 M sodium hydroxide. Nanoparticles were suspended in a resulted solution at a volume percentage of SSN/solution at 0.5%. The suspension was then sonicated for thirty minutes. One milliliter of the suspension was added stepwise to a sintered, printed disk with the dimensions: (d = 10 mm, h = 3 mm) in the presence of a small magnet. The 3D part was then sintered again. Moreover, the increase in the mass of the 3D part was used as indication of the amount of nanoparticles that diffused in the 3D part. This mass percent increase was studied as a function of pH of the suspension and as function DEG/water molar ratio. Unlike EG, data show that change in pH affects the mass percent when the suspension was made with DEG. Finally, optical analysis of the discs’ cross sections revealed trends metallic densities similar to trends in the data for mass increase with changing pH and water molar ratio.

36 MATERIALS SCIENCE↗

Miniature lowpass filters in low loss 9k7 LTCC

DuPont 9k7 low temperature cofired ceramic (LTCC) is a low loss, or high quality factor Q, tape system targeting at radio frequency (RF) applications. This paper reports the effect of a critical process parameter, heating rate, on the densification and dielectric properties of the 9k7 LTCC. The role of competing densification and crystallization during the sintering of 9k7 is discussed. The high Q of DuPont 9K7 can be used to improve RF system performance, for example a better receiver noise figure, by designing embedded passive RF components such as inductors, capacitors and filters. As a result, miniaturized multilayer low pass filters (LPF) with a wide stopband were fabricated to showcase the technology.

36 MATERIALS SCIENCE↗

Chemical Preconversion: Application of Low-Severity Pretreatment Chemistries for Commoditization of Lignocellulosic Feedstock

Securing biofuels project financing is challenging, in part because of risks in feedstock supply. Commoditization of the feedstock and decoupling its supply from the biorefinery will promote greater economies of scale, reduce feedstock supply risk and reduce the need for overdesign of biorefinery pretreatment technologies. We present benefits and detractions of applying low-severity chemical treatments or ‘chemical preconversion treatments’ to enable this approach through feedstock modification and densification early in the supply chain. General structural modifications to biomass that support cost-effective densification and transportation are presented, followed by available chemistries to achieve these modifications with minimal yield loss and the potential for harvesting value in local economies. A brief review of existing biomass pretreatment technologies for cellulolytic hydrolysis at biorefineries is presented, followed by a discussion toward economically applying the underlying chemistries at reduced severity in light of capital and operational limitations of small-scale feedstock depots.

09 BIOMASS FUELS↗

Sintered-reaction Bonded Silicon Nitride Densified by a Gas Pressure Sintering Process Effects of Rare Earth Oxide Sintering Additives

Reaction-bonded silicon nitrides containing rare-earth oxide sintering additives were densified by gas pressure sintering. The sintering behavior, microstructure and mechanical properties of the resultant specimens were analyzed. For that purpose, Lu2O3-SiO2 (US), La2O3-MgO (AM) and Y2O3-Al2O3 (YA) additive systems were selected. Among the tested compositions, densification of silicon nitride occurred at the lowest temperature when using the La2O3-MgO system. Since the Lu2O3-SiO2 system has the highest melting temperature, full densification could not be achieved after sintering at 1950oC. However, the system had a reasonably high bending strength of 527 MPa at 1200oC in air and a high fracture toughness of 9.2 MPa m1/2. The Y2O3-Al2O3 system had the highest room temperature bending strength of 1.2 GPa

36 MATERIALS SCIENCE↗

Miniature low-pass filter in low-loss 9k7 LTCC

DuPont 9k7 low-temperature cofired ceramic (LTCC) is a low-loss, or high-quality-factor Q, tape system targeting at radio frequency (RF) applications. This paper reports on the effect of a critical process parameter, the heating rate, on the densification and dielectric properties of the 9k7 LTCC. The role of competing densification and crystallization during the sintering of 9k7 is discussed. The high Q of DuPont 9K7 can be used to improve RF system performance, for example a better receiver noise figure, by designing embedded passive RF components such as inductors, capacitors and filters. Furthermore, miniaturized multilayer low-pass filters (LPF) with a wide stopband were fabricated to showcase the technology.

36 MATERIALS SCIENCE↗

Changes in the firn structure of the western Greenland Ice Sheet caused by recent warming

Atmospheric warming over the Greenland Ice Sheet during the last 2 decades has increased the amount of surface meltwater production, resulting in the migration of melt and percolation regimes to higher altitudes and an increase in the amount of ice content from refrozen meltwater found in the firn above the superimposed ice zone. Here we present field and airborne radar observations of buried ice layers within the near-surface (0–20 m) firn in western Greenland, obtained from campaigns between 1998 and 2014. We find a sharp increase in firn-ice content in the form of thick widespread layers in the percolation zone, which decreases the capacity of the firn to store meltwater. The estimated total annual ice content retained in the near-surface firn in areas with positive surface mass balance west of the ice divide in Greenland reached a maximum of 74 ± 25 Gt in 2012, compared to the 1958–1999 average of 13 ± 2 Gt, while the percolation zone area more than doubled between 2003 and 2012. Increased melt and column densification resulted in surface lowering averaging –0.80 ± 0.39 m yr⁻¹ between 1800 and 2800 m in the accumulation zone of western Greenland. Since 2007, modeled annual melt and refreezing rates in the percolation zone at elevations below 2100 m surpass the annual snowfall from the previous year, implying that mass gain in the region is retained after melt in the form of refrozen meltwater. If current melt trends over high elevation regions continue, subsequent changes in firn structure will have implications for the hydrology of the ice sheet and related abrupt seasonal densification could become increasingly significant for altimetry-derived ice sheet mass balance estimates.

58 GEOSCIENCES↗

High temperature compounds for turbine vanes

Fabrication and microstructure control studies were conducted on SiC, Si3N and composites based on Si3N. Charpy mode impact testing to 2400 F established that Si3N4/Mo composites have excellent potential. Attempts to fabricate composites of Si3N4 with superalloys, both by hot pressing and infiltration were largely unsuccessful in comparison to using Mo, Re, and Ta which are less reactive. Modest improvements in impact strength were realized for monolithic Si3N4; however, SiC strengths increased by a factor of six and now equal values achieved for Si3N4. Correlations of impact strength with material properties are discussed. Reduced MgO densification aid additions to Si3N4 were found to decrease densification kinetics, increase final porosity, decrease room temperature bend strength, increase high temperature bend strength, and decrease bend stress rupture properties. The decrease in bend strength at high temperature for fine grain size SiC suggested that a slightly larger grain size material with a nearly constant strength-temperature relation may prove desirable in the creep and stress rupture mode.

Rhodes, W. H.↗

Effects of pressure and temperature on hot pressing a sialon

The combined effects of temperature and pressure on the resulting density of a sialon (i.e., a ceramic composed of Si, Al, O, and N) are evaluated. Pressures in the 3.5-27.5 MPa range and temperatures in the 1550-1750 C range are considered. It is found that: (1) fully dense sialon bodies may be produced at lower temperatures than those usually used in the field, (2) the phase equilibrium reaction is increased by increased pressure, (3) the iso-density contour may be used to help design the desired microstructure, (4) phase changes occurring in the sample during hot pressing influenced sialon densification to a large extent, and (5) microstructures exceeding 98% theoretical density suggest that plastic deformation has contributed to densification.

Yeh, H. C.↗

Microstructural characterization of the HRSI thermal protection system for space shuttle

Components of the space shuttle high temperature reusable surface insulation (HRSI) system were microscopically characterized, both separately and as a system, to obtain information needed for stress analysis models of the thermal protection system. A tension specimen of the HRSI system was loaded in steps and was microscopically observed at each load condition to demonstrate the tension failure mode associated with strain isolation pad (SIP) behavior. A local failure occurred which should be associated with transfer of load through transverse fibers in the SIP. Stress concentrations attributed to the SIP behavior necessitated strengthening of the HRSI by densification of the RSI at the bondline. An HRSI tile was microscopically characterized after the densification process. The densified surface layer blended into the RSI which caused a gradual change in density. The gradation in density does not appear to represent a sharp discontinuity in elastic modulus between the densified layer and the parent material.

Ransone, P. O.↗

Effect of starting powder characteristics on density, microstructure and low temperature oxidation behavior of a Si3N48w/o Y2O3 ceramic

The densification and oxidation behavior of Si3N4 - 8w/oY2O3 prepared from three commercial starting powders were studied. Bars of SN 402, SN 502, and CP 85/15 were sintered for 3 to 4.5 hours at 1750 C. A second set was hot pressed for 2 hours at 1750 C. The microstructures were studied by transmission electron microscopy and scanning electron microscopy, densities were determined, and the phase compositions were determined by X-ray diffraction. Densification and microstructure were greatly influenced by the starting powder morphology and impurity content. Although SN 402 exhibited the maximum weight lose, the highest sintered and hot pressed densities were obtained with this powder. All powders had both equiaxed and elongated grains. Sintered bars were composed of beta silicon nitride and n-melelite. In contrast, hot pressed bars contained beta silicon nitride, H-phase, and J-phase, but no melelite. Yttria distribution in sintered bars was related to the presence of cation impurities such as Ca, Fe, and Mg. A limited oxidation study at 750 C in air showed no instability in these Si3N4 - 8 w/oY2O3 specimens, regardless of startin powder.

Schuon, S.↗

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.↗

Development of an improved toughness hyperpure silica reflective heat shield

High purity three dimensionally woven silica-silica materials were evaluated for use as a tough reflective heat shield for planetary entry probes. A special weave design was selected to minimize light piping effects through the heat shield thickness. Various weave spacings were evaluated for densification efficiency with an 0.7 micron particle size high purity silica. Spectral hemispherical reflectance was measured from 0.2 to 2.5 microns at room temperature. Reflectance increases due to densification and purity of material were measured. Reflectance of 3D hyperpure silica was higher than 3D astroquartz silica for all wavelengths. Mechanical properties were measured in beam flexure and beam shear tests. Results indicated strengths lower than reported for slip cast fused silica. Low strengths were attributed to low densities achieved through vacuum impregnation.

Rusert, E. L.↗

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.↗

Integral throat entrance development, qualification and production for the Antares 3 nozzle

Although design analyses of a G-90 graphite integral throat entrance for the Antares 3 solid rocket motor nozzle indicated acceptable margins of safety, the nozzle throat insert suffered a thermostructural failure during the first development firing. Subsequent re-analysis using properties measured on material from the same billet as the nozzle throat insert showed negative margins. Carbon-carbon was investigated and found to result in large positive margins of safety. The G-90 graphite was replaced by SAI fast processed 4-D material which uses Hercules HM 10000 fiber as the reinforcement. Its construction allows powder filling of the interstices after preform fabrication which accelerates the densification process. Allied 15V coal tar pitch is then used to complete densification. The properties were extensively characterized on this material and six nozzles were subjected to demonstration, development and qualification firings.

Clayton, F. I.↗

Effects of various additives on sintering of aluminum nitride

Effects of thirty additives on sintering A/N were investigated. The addition of alkali earth oxides and rare earth oxides gave fully densified aluminum nitride. This is due to the formation of nitrogen-containing aluminate liquid in the system aluminum nitride-alkali earth oxides or rare earth oxides. Microstructural studies of the sintered specimens with the above two types of additives suggested that the densification was due to the liquid phase sintering. Additions of silicon compounds resulted in poor densification by the formation of highly refractory compounds such as A/N polytypes.

Komeya, K.↗

Mechanisms of devitrification of grain boundary glassy phases in Si3N4 materials

Changes in the grain boundary (g.b.) phases of Si3N4 are analyzed, the effects of composition and thermal history on devitrification of the g.b. phases are determined, devitrification of the g.b. phases of Si3N are related to mechanical behavior and oxidation sensitivity of the material. The phase relationships that occur within the grain boundaries of Si3N4 containing various densification aids are reviewed. Comparisons of the effects of MgO, Y2O3, CeO2, and Y2O3 + AL2O3 are made in terms of the phase equilibria of the Si3N4 + SiO2 + additive compositional system. Two new equilibrium phase diagrams for the Si3N4-SiO2 and Y2O3 and Si3N4-SiO2-Ce2O3 systems are preented. The effects of Y2O3 vs CeO2 densification aids on the fracture surfaces of Si3N4 are compared. Auger electron spectroscopy shows that both oxides are concentrated within the fracture surface. Scanning electron microscopy shows evidence that Si3N4 with CeO2 formed an intergranular structure of fine grained oxynitride reaction products, as predicted by phase quilibria, whereas the Y2O3 containing sample shows evidence of an intergranular glassy phase.

Hench, L. L.↗