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At least 19 records

Pressureless sintered beta-prime-Si3N4 solid solution - Fabrication, microstructure, and strength

Pressureless sintering of beta-prime-Si3N4 solid solution was studied as a function of temperature using Si3N4, A1N, and Al2O3 as basic constituents. Y2O3-SiO2 additions were used to promote liquid-phase sintering. The sintered specimens were characterized with respect to density, microstructure, strength, oxidation, and thermal shock resistance. Density greater than 98 percent of theoretical was achieved by pressureless sintering at 1750 C. The microstructure consisted essentially of fine-grained beta-prime-Si3N4 solid solution as the major phase. Modulus of rupture strengths up to 483 M Pa were achieved at moderate temperature (1000 C), but decreased to 228 M Pa at 1380 C. This substantial strength loss was attributed to a 'glassy' grain boundary phase formed during cooling from the sintering temperature. The best oxidation resistance was exhibited by a composition containing 3 mol % Y2O3-SiO2 additives. Water quench thermal shock resistance was equivalent to that of reaction sintered silicon nitride but lower than hot-pressed silicon nitride.

Dutta, S.↗

Pressureless sintering of dual-phase, high-entropy boride–carbide ceramics

Here, dual-phase, high-entropy boride–carbide ceramics were densified by pressureless sintering. Relative densities up to approximately 96% were obtained for ceramics containing about 30 vol% high-entropy boride and 70 vol% high-entropy carbide. Isostatic pressing at 200 MPa resulted in higher relative densities of both the green bodies and final ceramics compared to uniaxial pressing. The highest relative density of 96.3% was achieved for a ceramic that was isostatically pressed at 200 MPa and sintered at 2300°C for 2 h. Grain sizes of the resulting ceramics were approximately 2 µm. This is the first report of pressureless sintering of dual-phase, high-entropy boride–carbide ceramics.

36 MATERIALS SCIENCE↗

Pressureless sintered beta prime-Si3N4 solid solution: Fabrication, microstructure, and strength

Si3N4, AlN, and Al2O3 were used as basic constituents in a study of the pressureless sintering of beta prime-Si3N4 solid solution as a function of temperature. Y2O3-SiO2 additions were used to promote liquid-phase sintering. The sintered specimens were characterized with respect to density, microstructure, strength, oxidation, and thermal shock resistance. Density greater than 98 percent of theoretical was achieved by pressureless sintering at 1750 C. The microstructure consisted essentially of fine-grained beta prime-Si3N4 solid solution as the major phase. Modulus of rupture strengths up to 483 MPa were achieved at moderate temperature (1000 C), but decreased to 228 MPa at 1380 C. This substantial strength loss was attributed to a glassy grain boundary phase formed during cooling from the sintering temperature. The best oxidation resistance was exhibited by a composition containing 3 mol % Y2O3-SiO2 additives. Water quench thermal shock resistance was equivalent to that of reaction sintered silicon nitride but lower than hot-pressed silicon nitride.

Dutta, S.↗

Pressureless sintering of lithium hydride

Lithium Hydride is a material of growing importance for addressing technological challenges related to nuclear fusion, long-term human space travel, and thermal energy storage. Pressureless sintering provides a straightforward, scalable approach to produce dense LiH parts of all sizes and shapes. Pressed LiH green compacts were sintered at heating rates from 2.5 to 20 °C/min to 650 °C, yielding densities up to 96 ± 1.4 %, with densification initiating at 500 °C. Here, a validated master sintering curve was constructed with a sintering apparent activation energy of 135 kJ/mol. X-ray diffraction and simultaneous thermal analysis revealed Li 2 O formation from 300 – 550 °C and decomposition of LiH into Li metal at 550 °C, each reflected as deviations in the master sintering curve. Computed tomography after thermal treatment to 550 °C showed the formation of corrosion products, and after thermal treatment to 650 °C LiH reduction to Li most significantly at exposed surfaces.

36 MATERIALS SCIENCE↗

Pressureless Sintering of Pre-Alloyed Nanostructured Bainitic Steel Powders

A recent study shows that powder metallurgy and pressureless sintering are a viable pathway to realize full-density bulk components of nanostructure bainitic steels. A scalable, pressureless supersolidus liquid phase sintering (SLPS) approach to process nanostructured bainitic steel is evaluated. Furthermore, to address the oxidation issues associated with the mechanical alloying of elemental powders, powder atomization is used to produce pre-alloyed nanostructured bainitic steel powders.

mechanical alloying↗

Tensile test of pressureless-sintered silicon nitride at elevated temperature

Uniaxial tensile strength tests of pressureless sintered silicon nitride were carried out in air at temperatures ranging from room temperature up to 1600 C. Silicon nitrides containing Y2O3, Al2O3, Al2O3-MgO, or MgO-CeO2 additives were tested. The results show that the composition of the additive used influences the strength characteristics of the silicon nitride. The tensile strength rapidly decreased at temperatures above 1000 C for the materials containing MgO as the additive and above 1000 C for the material with Y2O3. When the temperature increased to as high as 1300 C, the strength decreased to about 10 percent of the room temperature strength in each case. Observations of the fracture origin and of the crack propagation on the fracture surfaces are discussed.

Matsusue, K.↗

Pressureless sintered Sialons with low amounts of sintering aid

Two Beta prime - Sialons of composition Si2.6Al0.393y0.007O0.4N3.6 and Si2.6Al0.384Y0.014O0.4N3.6 were pressureless sintered from mixtures of Y2O3 and separately milled Beta -Si3N4, AlN, and SiO2. These Sialons had densities of over 98% of theoretical, four-point bend strengths of 460 and 155 MPa at room temperature and 1400 C, respectively, and 1400 C oxidation rates lower than those reported for hot pressed Si3N4 and for a stronger Sialon with 2.5 weight percentage Y2O3.

Arias, A.↗

Improved silicon carbide for advanced heat engines. II - Pressureless sintering and mechanical properties of injection molded silicon carbide

The influence on density and strength of pressureless sintering in vacuum and argon environments has been evaluated with injection molded SiC materials. Main effects and two factor interactions of sintering (cycle variables temperature, time, heating rate, and atmosphere) were assessed. An improved understanding of the influence of the processing flaws and sintering conditions has been obtained. Strength and density have improved from a baseline level of 299 MPa (43.3 Ksi) and 94 pct of theoretical density to values greater than 483 MPa (70 Ksi) and 97 pct.

Whalen, Thomas J.↗

Effect of Yttria additives on properties of pressureless-sintered silicon nitride

Si3N4-base ceramics were made from milled Si3N4 containing 11.1 wt% SiO2 and oxide additives by pressureless sintering at 1760 C. The four-point-average moduli of rupture were 460, 515, and 515 MPa at room temperature and 270, 256, and 227 MPa at 1400 C for compositions with 3.67, 7.22, and 14.0 wt% Y2O3, respectively. The oxidation resistance of these compositions decreased with increasing Y2O3 in the 600 to 1400 C range, and no surface oxide cracking or spalling was noted. Partial substitution of Al2O3 for Y2O3 reduced both strength and oxidation resistance.

Arias, A.↗

Strength evaluation test of pressureless-sintered silicon nitride at room temperature

In order to study strength characteristics at room temperature and the strength evaluating method of ceramic materials, the following tests were conducted on pressureless sintered silicon nitride specimens: bending tests, the three tensile tests of rectangular plates, holed plates, and notched plates, and spin tests of centrally holed disks. The relationship between the mean strength of specimens and the effective volume of specimens are examined using Weibull's theory. The effect of surface grinding on the strength of specimens is discussed.

Matsusue, K.↗

Melt-Infiltration Process For SiC Ceramics And Composites

Reactive melt infiltration produces silicon carbide-based ceramics and composites faster and more economically than do such processes as chemical vapor infiltration (CVI), reaction sintering, pressureless sintering, hot pressing, and hot isostatic pressing. Process yields dense, strong materials at relatively low cost. Silicon carbide ceramics and composites made by reactive melt infiltration used in combustor liners of jet engines and in nose cones and leading edges of high-speed aircraft and returning spacecraft. In energy industry, materials used in radiant-heater tubes, heat exchangers, heat recuperators, and turbine parts. Materials also well suited to demands of advanced automobile engines.

Behrendt, Donald R.↗

Synthesis, sintering, and grain growth kinetics of Hf 6 Ta 2 O 17

Here Aasystematic study of the solid-state synthesis, pressureless sintering, and grain growth kinetics of Hf 6 Ta 2 O 17 is presented. The ideal conditions for solids-state synthesis of Hf 6 Ta 2 O 17 powder with minimal particle necking was 1250 °C for 2 h in air. The resultant powder has an average particle size of 210 ± 70 nm. The combined synthesis and ball-milling procedure produces highly sinterable Hf 6 Ta 2 O 17 powder, achieving > 97 % of theoretical density after pressureless sintering at 1600 °C for 2 h in air. The grain growth mechanism was sensitive to processing conditions, appearing to be primarily driven by surface diffusion below 1600 °C and grain boundary diffusion above 1650 °C. The respective activation energies for grain growth were found to be Q S = 659 ± 79 kJ mol -1 and Q GB = 478 ± 63 kJ mol -1 .

36 MATERIALS SCIENCE↗

Sintering and properties of Si3N4 with and without additives by HIP treatment

Hot Isostatic Pressing (HIP) of Si3N4 powders with and without additives was performed using a glass container, and various kinds of pressureless-sintered Si3N4 were HIP'ed without a container. The effects of HIP treatment on density, microstructure, flexural strength, microhardness, and fracture toughness on Si3N4 ceramics were studied. Using a glass container it was difficult to reach theoretical density. The microhardness of HIP'ed Si3N4 without additives was low, and the fracture toughness of HIP'ed Si3N4 with and without additives was 22 to 25 W/m-K, and it decreased with increasing the amount of additives. The density and flexural strength, and hardness of pressureless-sintered Si3N4 which contained Al2O and Y2O3 as oxide additives were remarkably improved by HIP treatment using nitrogen as a pressure transmitting gas. It is very important to select the sintering conditions for fabricating the presintered body of Si3N4 in order to improve the mechanical properties of Si3N4 by HIP treatment.

Kuratani, S.↗

Tape casting and characterizations of MgO ceramics

Herein we report a high density MgO ceramic substrate produced by the tape casting technology. The tape casting formulation and process produced a uniform tape free of cracking. Y 2 O 3 and SiO 2 were used as the sintering aid for the pressureless sintering of the green tape. X-ray diffraction phase identification indicates that MgO is the main phase, while both Y 2 O 3 and SiO 2 sintering aids react with MgO to form MgY 4 Si 3 O 13 as the second phase. Liquid phase sintering occurs in the temperature range from 1030°C to ~1500°C, which is confirmed by the simultaneous Thermal Gravitation Analysis/ Differential Scanning Calorimeter (TGA/DSC) and the percent linear shrinkage and densification. A 96.5% theoretical density was achieved by presureless sintering at 1650°C for 2 hours, which was further increased to a fully dense structure using hotisostatic- pressing(HIP) at 1650°C and 207 MPa in argon. Scanning electron microscopy (SEM) and energy dispersive(EDS) spectroscopic analysis on the HIP’ed sample show that MgY 4 Si 3 O 13 is located at the MgO grain boundary and the sample has a fully dense structure. The refractive indices and extinction coefficient were measured on the HIP’ed sample along with thermal properties and dielectric properties. Thermal diffusivity and heat capacity were measured to calculate the thermal conductivity.

36 MATERIALS SCIENCE↗

Compositional Exploration of Additively Manufactured Ultra-High-Temperature Ceramic Composites for Use in Concentrated Solar Power Plant Heat Exchangers

The DOE has research interest in new technologies for high temperature concentrated solar power plants. Our project this summer was to explore the use of additively manufactured ultra-high-temperature ceramics in a heat exchanger. The heat exchanger would transfer heat between a molten chloride salt and supercritical CO 2 . We selected 22 compositions to test and were able to mix 14 of these compositions. We sintered these compositions using pressureless sintering and direct current sintering. We also conducted high temperature TGA on some ceramic samples. We also performed preliminary binder jet additive manufacturing trials with tungsten carbide powder. Our work so far points towards one of our titanium diboride samples being promising, but much more research needs to be done.

14 SOLAR ENERGY↗

Silicon carbide sintered products and a method for their manufacturing

SiC based sinters are produced by pressureless sintering from a SiC-AlN solid solution containing Al2 to 20, N 0.2 to 10, O 0.2 to 5, a Group IIIB element 0 to 15 percent, the remainder being Si and C. Thus, a 90:10 mixture of SiC and AlN powders were cold pressed at 2000 kg/sq cm and sintered for 5 hours at 2100 C in a nitrogen atmosphere. The resulting product had density of 3.11 g/cu cm and bending strength at ambient and 1400 C at 68.5 and 66.3 kg/sq mm.

Suzuki, K.↗

On the sintering of silicon carbide

This document deals with the sintering of silicon carbide using pressureless sintering. This technique makes it possible to sinter a primarily covalent material to usable densities up to over 98% thD without having to use a high amount of sinter additives as is the case with other non-oxide ceramic materials. The process takes place rapidly, and it is also possible to produce relatively thick-walled structural parts without major problems. This sheds more light on the true characteristics of silicon carbide in one structural part, since there is no second or nearly no second phase. Heat pressing has improved stability.

Gugel, E.↗

Microstructure and property characterization of sintered Si3N4, SiC, and SiAlON

Commercially-produced, pressureless sintered Si3N4, SiC, and SiAlON were characterized with respect to density, phases present, bend strength, and oxidation resistance. The room-temperature bend strengths of sintered Si3N4, SiC, and SiAlON are comparable. However, the room-temperature strengths are much lower (approximately 40 to 50%) than the room-temperature strength of hot-pressed Si3N4 (NC-132). The strength loss in Si3N4 and SiAlON materials at high temperature was attributed to a viscous grain-boundary phase, retained during cooling from the sintering temperature. The oxidation resistance of sintered alpha-SiC was the best of any materials tested.

Dutta, S.↗