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Under the invented method, a compressed body of mix powder for ceramic is produced by mixing and stirring several raw powder materials with mixing liquid such as water, and, in the process of sending the resulted viscous material pressurized at 5 kg/cm to 7 kg/cm, using 1.5 to 2 times the pressure to filter and dehydrate, adjusting the water content to 10 to 20%.
Additively manufactured tungsten is a candidate refractory material for high-temperature aerospace and nuclear fusion/fission applications. The printability of pure tungsten is challenged by cracking defects arising from the metal’s high brittle-to-ductile transition temperature and low solubility of interstitial impurities. Furthermore, the cast microstructure inherent to the laser powder bed fusion (L-PBF) process has limited strength compared to worked microstructures common in wrought tungsten. Aside from process-related techniques to mitigate defects and increase strength (e.g., heated build chambers, multi-laser systems, low oxygen environmental control, etc.), micro-alloying additions can positively influence tungsten printability and strength. In this work, pure tungsten L-PBF feedstock was modified with 1 wt% additions of ceramic compound nano-powders. Wrought and printed bars were evaluated in four-point bending. Flexural strength and fractography were primary means of comparison to assess the effect of the feedstock modification on printed tungsten mechanical performance.
The Ultracapacitor Research and Development project is a collaborative effort between the NASA Marshall Space Flight Center's (MSFC's) ES43 Parts, Packaging, and Fabrication Branch and the EM41 Nonmetallic Materials Branch. NASA's Ultracapacitor Research is an effort to develop solid-state energy storage devices through processing of ceramic materials into printable dielectric inks, which can be formed and treated to produce solid state ultracapacitor cells capable of exceeding lithium-ion battery energy density at a fraction of the weight. Research and development efforts into solid state ultracapacitors have highlighted a series of technical challenges such as understanding as-received nature of ceramic powders, treatment and optimization of ceramic powders, dielectric and conductor ink formulation, and firing of printed (green) ultracapacitor cells. Two facilities have been continually developed since project inception: the Additive Electronics Lab in Bldg. 4487 and the Nanoelectric Materials Lab in Bldg. 4602. The Nanoelectric Materials Lab has become a unique facility at MSFC, capable of custom processing a wide range of media for additive electronics. As research has progressed, it was discovered that additional in-house processing was necessary to achieve smaller, more uniform particle diameters. A vibratory mill was obtained that can agitate powder and media in three directions, which has shown to be much more effective than ball milling. However, in order to understand the effects of milling, a particle size analysis system has been installed to characterize as-received and milled materials Continued research into the ultracapacitor technology included advanced milling and optimization of ceramic nanoparticles, fluidized bed treatment of atomic-layer deposition- (ALD-) coated ceramic particles, custom development of dielectric and conductor inks, as well as custom ink precursors such as polyvinylidene diflouride- (PVDF-) loaded vehicles. Experiments with graphene-based inks were also conducted.
As a result of this funded project high purity Zirconia-Toughened Alumina (ZTA) ceramic powders with and without yttria were produced using metal alkoxide precursors. ZTA ceramic powders with varying volume percents of zirconia were prepared (7, 15, and 22%). Aluminum tri-sec butoxide, zirconium propoxide, and yttrium isopropoxide were the reagents used. Synthesis conditions were varied to control the hydrolysis and the aging conditions for the sol to gel transition. FTIR analysis and rheological characterization were used to follow the structural evolution during the sol to gel transition. The greater extent of hydrolysis and the build-up of structure measured from viscoelastic properties were consistent. Heat treatment was conducted to produce submicron grain fully crystalline ZTA ceramic powders. This improved materials should have enhanced properties such strength, toughness, and wear resistance for advanced structural applications, for example engine components in high technology aerospace applications.
High purity ZTA ceramic powders with and without yttria were produced using metal alkoxide precursors. ZTA ceramic powders with varying volume percents of zirconia were prepared (7, 15, and 22%). Aluminum tri-sec butoxide, zirconium propoxide, and yttrium isopropoxide were the reagents used. Synthesis conditions were varied to control the hydrolysis and the aging conditions for the sol to gel transition. FTIR analysis and theological characterization were used to follow the structural evolution during the sol to gel transition. The greater extent of hydrolysis and the build-up of structure measured from viscoelastic properties were consistent. Heat treatment was conducted to produce submicron grain fully crystalline ZTA ceramic powders. In all experimental cases a-alumina and tetragonal zirconia phases were confirmed even in the absence of yttria.
A process is disclosed for manufacturing a low density ceramic powder which can be formed to make a lightweight material for insulation or other construction. The ceramic product made from the process has a final density of less than 25 to about 1 percent of the theoretical weight of the ceramic powder. The ceramic product is lightweight and can be made to withstand high temperatures greater than 1400 C.
A process for slip casting ceramic articles that does not employ parting agents and affords the casting of complete, detailed, precision articles that do not possess parting lines is presented. This process is especially useful for high temperature superconductors and water-sensitive ceramics. A wax pattern for a shell mold is provided, and an aqueous mixture of a calcium sulfate-bonded investment material is applied as a coating to the wax pattern. The coated wax pattern is then dried, followed by curing to vaporize the wax pattern and leave a shell mold of the calcium sulfate-bonded investment material. The shell mold is cooled to room temperature, and a ceramic slip, created by dispersing a ceramic powder in an organic liquid, is poured therein. After a ceramic shell of desired thickness or a solid article has set up in the shell mold, excess ceramic slip is poured out. The shell mold is misted with water and peeled away from the ceramic article, after which the ceramic is fired to provide a complete, detailed, precision, high temperature superconductive ceramic article without parting lines. The casting technique may take place in the presence of a magnetic field to orient the ceramic powders during the casting process.
Process for sintering compressed ceramic powders produces large ceramic disks for use as electrolytes in high-temperature electrolytic cells. Thin, strain-free uniformly dense disks as large as 30 cm squared have been fabricated by slicing ceramic slugs produced by this technique.
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.
A method for enhancing the cooling capability of a turbine component made from a ceramic matrix composite. The method improves the thermal performance of the component by producing a surface having increased cooling capacity, thereby allowing the component to operate at a higher temperature. The method tailors the available surface area on the cooling surface of the composite component by depositing a particulate layer of coarse grained ceramic powders of preselected size onto the surface of the ceramic matrix composite component. The size of the particulate is selectively tailored to match the desired surface finish or surface roughness of the article. The article may be designed to have different surface finishes for different locations, so that the application of different sized powders can provide different cooling capabilities at different locations, if desired. The compositions of the particulates are chemically compatible with the ceramic material comprising the outer surface or portion of the ceramic matrix composite. The particulates are applied using a slurry and incorporated into the article by heating to an elevated temperature without melting the matrix, the particulates or the fiber reinforcement.
The effects of BaF2-CaF2 particle size and size distribution on PS304 feedstock powder flowability have been investigated. Angular BaF2-CaF2 eutectic powders were produced by comminution and classified by screening to obtain 38 to 45 microns 45 to 106 microns, 63 to 106 microns, 45 to 53 microns, 63 to 75 microns, and 90 to 106 microns particle size distributions. The fluorides were added incrementally from 0 to 10 wt% to the other powder constituents of the PS304 feedstock: nichrome, chromia, and silver powders. The flow rate of the powder blends decreased linearly with increasing concentration of the fluorides. Flow was degraded with decreasing BaF2-CaF2 particle size and with increasing BaF2-CaF2 particle size distribution. A semiempirical relationship is offered to describe the PS304 powder blend flow behavior. The Hausner Ratio confirmed the funnel flow test results, but was slightly less sensitive to differences in BaF2-CaF2 particle size and size distribution. These findings may have applicability to other powders that do not flow easily, such as ceramic powders.
Polycrystalline ceramic laser materials are gaining importance in the development of novel diode-pumped solid-state lasers. Compared to single-crystals, ceramic laser materials offer advantages in terms of ease of fabrication, shape, size, and control of dopant concentrations. Recently, we have developed Neodymium doped Yttria (Nd:Y2O3) as a solid-state ceramic laser material. A scalable production method was utilized to make spherical non agglomerated and monodisperse metastable ceramic powders of compositions that were used to fabricate polycrystalline ceramic material components. This processing technique allowed for higher doping concentrations without the segregation problems that are normally encountered in single crystalline growth. We have successfully fabricated undoped and Neodymium doped Yttria material up to 2" in diameter, Ytterbium doped Yttria, and erbium doped Yttria. We are also in the process of developing other sesquioxides such as scandium Oxide (Sc2O3) and Lutesium Oxide (Lu2O3) doped with Ytterbium, erbium and thulium dopants. In this paper, we present our initial results on the material, optical, and spectroscopic properties of the doped and undoped sesquioxide materials. Polycrystalline ceramic lasers have enormous potential applications including remote sensing, chem.-bio detection, and space exploration research. It is also potentially much less expensive to produce ceramic laser materials compared to their single crystalline counterparts because of the shorter fabrication time and the potential for mass production in large sizes.
Fluidized-bed reactor produces highly pure polycrystalline silicon particles with diameters approximately greater than 400 micrometers. Operates by pyrolysis of silane in reaction zone, which is bed of silicon seed particles fluidized by flow of silane and carrier gas. Above reaction zone, gas mixture flows rapidly enough to entrain silicon powders, but not larger seed and product particles. Entrained particles swept out of reactor. Applicable to other processes such as production of fine metal and ceramic powders where control of sizes of product needed.
Two critical challenges facing the application of flames for synthesis of nanopowder materials are: (1) overcoming formation of agglomerates and (2) ensuring that the highly reactive nanopowders that are synthesized in flames can be produced in such a manner that their purity is maintained during subsequent processing. Agglomerates are produced in flames because particle formation occurs in a high temperature and high number density environment. They are undesirable in most advanced applications of powders. For example, agglomerates have a deleterious effect on compaction density, leading to voids when nanopowders are consolidated. Efforts to avoid agglomeration in flames without substantially reducing particle number density and, consequently, production rate, have had limited success. Powder purity must also be maintained during subsequent handling of nanopowders and this poses a significant challenge for any synthesis route because nanopowders, particularly metals and non-oxide ceramic powders, are inherently reactive. Impurities acquired during handling of nanopowders have slowed the advancement of the nanostructured materials industry. One promising approach that has been proposed to address these problems is nano-encapsulation. In this approach, the core particles are encapsulated in a removable material while they are within the flame but before excessive agglomeration has occurred. Condensation can be very rapid so that core particles are trapped within the condensed material and agglomeration is limited. Nano-encapsulation also addresses the handling concerns for post-synthesis processing. Results have shown that when nano-encapsulated powders are exposed to atmosphere the core particles are protected from oxidation and/or hydrolysis. Thus, handling of the powders does not require extreme care. If, for example, at the time of consolidation the encapsulation material is removed by vacuum annealing, the resulting powder remains unagglomerated and free of impurities. In this work, we described a novel aerosol model that has been developed to simulate particle encapsulation in flames. The model will ultimately be coupled to a one-dimensional spherical flame code and compared to results from microgravity flame experiments.
The NASA Glenn Research Center has developed a patented high-temperature solid lubricant coating, designated PS304, for reducing friction and wear in bearing systems. The material used to produce the coating is initially a blend of metallic and ceramic powders that are deposited on the bearing surface by the plasma spray process. PS304 was developed to lubricate foil air bearings in Oil-Free turbomachinery, where the moving surfaces are coated with a hydrodynamic air film except at the beginning and end of an operation cycle when the air film is not present. The coating has been successful in several applications including turbochargers, land-based turbines, and industrial drying furnace conveyor components, with current development activities directed at implementation in Oil-Free aeropropulsion engines.
Ceramic structures having high strength at temperatures above 1000 C after sintering are made by mixing ceramic powders with binder deflocculants such as guanidine salts of polymeric acids, guanidine salts of aliphatic organic carboxylic acids or guanidine alkylsulfates with the foregoing guanidine salts. The novelty of the invention appears to lie in the substitution of guanidine salts for the alkalai metal salt components or organic fatty acids of the prior art binder-deflocculant, ceramic processing aids whereby no undesirable metal contaminants are present in the final ceramic structure. Guanidine alkylsulfates also replace the Na or K alkylsulfates commonly used with binder-deflocculants in making high temperature ceramic structures.
An ultracapacitor made from a polymer loaded with ceramic powder would have several advantages over current ultracapacitors and batteries. First is the possibility of it being printable, which would allow for printing the energy storage device along with the circuit instead of having to find a way to add one later without damaging the rest of the components. When not printed in a specific design for use on a printed wiring board, this type of ultracapacitor could still be cured via a mold to a shape suitable to specific applications. Many polymers maintain some flexibility even after curing, such as the silicone used in this study. The manufacturing process would also be far simpler than that of conventional ultracapacitors.In this work, solid-state ultracapacitors were made by adding the dielectric powder to a two-part polymer (resin and hardener) at the same time. The mixture was then cured in the desired shape at a low temperature until completely set. The addition of the powder to the polymer increased its dielectric properties while leaving most of its physical properties unaltered. At higher powder loading percentages, there were some physical changes as the maximum loading point was approached. To determine the efficiency of these solid-state ultracapacitors, their capacitances were tested, and their dielectric constants (DCs) were measured and compared.
A precursor of a ceramic adhesive suitable for use in a vacuum, thermal, and microgravity environment. The precursor of the ceramic adhesive includes a silicon-based, preceramic polymer and at least one ceramic powder selected from the group consisting of aluminum oxide, aluminum nitride, boron carbide, boron oxide, boron nitride, hafnium boride, hafnium carbide, hafnium oxide, lithium aluminate, molybdenum silicide, niobium carbide, niobium nitride, silicon boride, silicon carbide, silicon oxide, silicon nitride, tin oxide, tantalum boride, tantalum carbide, tantalum oxide, tantalum nitride, titanium boride, titanium carbide, titanium oxide, titanium nitride, yttrium oxide, zirconium diboride, zirconium carbide, zirconium oxide, and zirconium silicate. Methods of forming the ceramic adhesive and of repairing a substrate in a vacuum and microgravity environment are also disclosed, as is a substrate repaired with the ceramic adhesive.