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34 records · Page 2

All sources NASA NTRS DOE OSTI

NASA NTRS2003

Characterization of a Ultra-high Temperature Ceramic Composite

Ultra-high temperature ceramics (UHTC) are of interest for hypersonic vehicle leading edge applications. Monolithic UHTCs are of concern because of their low fracture toughness and brittle behavior. UHTC composites (UHTCC) are being investigated as a possible approach to overcome these deficiencies. In this study a small sample of a UHTCC was evaluated by limited mechanical property tests, furnace oxidation exposures, and oxidation exposures in a flowing environment. The composite was prepared from a carbon fiber perform using ceramic particulates and a preceramic polymer. The as-received composite plate was non-uniform from front to back surface. Plate dimensions were 150 x 150 x 6 mm. The back surface had a fibrous, uniform appearance; XRD analysis revealed the presence of Sic and C. The front surface was smooth and non-uniform in appearance with evidence of a coarse grain structure produced by a liquid phase; XRD analysis revealed the presence of HfB2. Microcracks were present throughout the thickness as one might expect from a carbon fiber reinforced composite with attendant large thermal expansion mismatch between the matrix phases and the fibers. The HfB2 phase on the front surface was comparable in thickness to a fiber ply or about 0.6 mm, and surface microcracks were evident. Limited four point flexural tests were carried out at span to depth ratios of approximately 14 and 16 with markedly different results. Tests were run with the front or the back surface in tension. At the shorter span to depth failures occurred under a loading pin for both orientations. At a span to depth of 16 failures occurred in the center of the span with fracture clearly initiating from a tensile failure. Ultimate flexural strength, strain at ultimate stress, stress and strain at deviation from linear elastic behavior are reported. Strains at ultimate stress ranged from about 0.6 to 0.7 % for the back surface in tension, and 0.4 to 0.6 for the front surface in tension. At constant span to depth the strain at ultimate stress was about 0.2% greater for the back surface in tension and the ultimate strength was also higher. Strengths were in line with predictions from theory. Furnace oxidation studies were carried out at 1627 and 1927OC in a static furnace environment using ten minute cycles and one, five, and ten cycles. Limited oxidation studies were also carried out in a flowing oxyacetylene torch environment. Specimens were photographed, and weight and dimensional changes were determined. XRD and SEM characterizations were performed. Weight losses were attributed primarily to carbon fiber oxidation. The composite survived the torch test with little visible distress. Further details will be determined once metallographic studies are completed.

Levine, Stanley R.↗

NASA NTRS2003

Ultra-High-Temperature Ceramics Evaluated for Aeropropulsion Use

Ultra-high-temperature ceramics (UHTC) are a group of materials consisting of zirconium diboride (ZrB2) or hafnium diboride (HfB2) plus silicon carbide (SiC), and in some instances, carbon (C). They offer a combination of properties that make them candidates for airframe leading edges on sharp-bodied reentry vehicles. These UHTCs perform well in the environment for such applications (i.e., air at low pressures). The purpose of this study at the NASA Glenn Research Center was to examine three of these materials under conditions more representative of a propulsion environment: that is, higher oxygen partial pressure and total pressure. Relatively long, multiple-exposure cycles were emphasized. We completed an in-house study of ZrB2 plus 20 vol% SiC (abbreviated as ZS), ZrB2 plus 14 vol% SiC and 30 vol% C (ZSC), and SCS-9a SiC fiber-reinforced ZrB2 plus 20 vol% SiC (ZSS). HfB2-based compositions were not included in the study because of their high cost. The capability of UHTC for propulsion applications must be compared with that of mature, available, and commercially used ceramics such as silicon nitride (e.g., AS-800) to put things in proper perspective. In terms of mechanical properties, UHTCs fall short in terms of strength and fracture toughness. At about 1300 C, the creep resistance of ZS appears to be superior to the creep resistance reported for AS-800. However, the stress rupture life for Si3N4 under stress and temperature conditions similar to those used in this study is measured in hundreds of hours. Because of oxidation, ZS could not achieve such lives. In terms of oxidation resistance, acceptable amounts of material recession in 1 hour to thousands of hours, depending on the specific propulsion application, are on the order of 100 to 300 mm. This converts to an acceptable range of parabolic recession rate constants kp" of approximately less than or equal to 10(exp -1) to 10(exp -2) square millimeters per hour for a 1-hr application. For a 100-hr application, an acceptable range of kp" would be less than or equal to those values divided by 100. For the more oxidation resistant ZS material, measured parabolic recession rate constants were 4.7 x 10(exp -3) millimeters per hour at 1327 C, 7.8 x 10(exp -2) square millimeters per hour at 1627 C, and 1.3 millimeters per hour at 1927 C. Thus, recession rate constants for ZS are acceptable at 1327 C for a 1-hr application, but here silicon nitride is a superior material. At 1627 C, ZS oxidation is marginal for a 1-hr application, but dimensional growth would be an issue. In a 100-hr application, ZS cannot be considered at any temperature. Our cursory examination of thermal shock, both from a theoretical and experimental viewpoint, indicated that the ZS and ZSC UHTCs are inferior to AS-800 silicon nitride. On the basis of this limited study, UHTCs are not ready to be considered as aeropropulsion materials for any applications longer than a few minutes. Current materials suffer from aggressive oxidation and moisture attack (Quynhgiao Nguyen, NASA Glenn, and Raymond C. Robinson, QSS Group, Inc., Cleveland, OH, 2002, private communication), and they are susceptible to thermal shock. For long-term propulsion applications, major improvements in environmental durability are needed. Work is in progress to improve the oxidation resistance of UHTC materials.

Levine, Stanley R.↗

DOE OSTI2020

Materials Data on HfZrB4 by Materials Project

ZrB2(HfB2) is hexagonal omega structure-derived structured and crystallizes in the orthorhombic Pmmm space group. The structure is three-dimensional. Hf4+ is bonded to twelve B+1.50- atoms to form HfB12 cuboctahedra that share edges with four equivalent HfB12 cuboctahedra, edges with eight equivalent ZrB12 cuboctahedra, faces with four equivalent HfB12 cuboctahedra, and faces with four equivalent ZrB12 cuboctahedra. All Hf–B bond lengths are 2.53 Å. Zr2+ is bonded to twelve B+1.50- atoms to form ZrB12 cuboctahedra that share edges with four equivalent ZrB12 cuboctahedra, edges with eight equivalent HfB12 cuboctahedra, faces with four equivalent HfB12 cuboctahedra, and faces with four equivalent ZrB12 cuboctahedra. All Zr–B bond lengths are 2.54 Å. There are two inequivalent B+1.50- sites. In the first B+1.50- site, B+1.50- is bonded in a 9-coordinate geometry to two equivalent Hf4+, four equivalent Zr2+, and three B+1.50- atoms. There is two shorter (1.83 Å) and one longer (1.84 Å) B–B bond length. In the second B+1.50- site, B+1.50- is bonded in a 9-coordinate geometry to four equivalent Hf4+, two equivalent Zr2+, and three B+1.50- atoms. The B–B bond length is 1.81 Å.

36 MATERIALS SCIENCE↗

NASA NTRS1959

Stability of Ceramics in Hydrogen between 4000 and 4500 F

The various reactions that are possible between hydrogen and certain ceramic materials are discussed as well as the means of measuring the extent of such reactions. Powdered carbides, nitrides, borides, and oxides were tested. These materials were heated inductively in a tungsten cup between 4000 and 4500 F for two 1-hour periods under a static hydrogen atmosphere. Weight, pressure, and diffraction pattern changes were observed, and these served to indicate the extent of reaction. Most of the ceramics, HfC, ZrC, TiC, TaC, NbC, WC, MO2C, HfN, ZrN, NbN, ZrB2, NbB2, and WB, showed less reaction than the minimum detectable value. However, the ceramics, TiN, TaN, HfB2, TiB2, ZrO2, and Cr2O3, apparently reacted to a measurable extent with hydrogen. Reactions of SiC, VC, and TaB2 with hydrogen were not determinable because of their incompatibility with the tungsten container.

May, Charles E.↗

NASA NTRS2001

Thermal Protection Materials for Reentry Applications

Thermal protection materials and systems (IRS) are used to protect spacecraft during reentry into Earth's atmosphere or entry into planetary atmospheres. As such, these materials are subject to severe environments with high heat fluxes and rapid heating. Catalytic effects can increase the temperatures substantially. These materials are also subject to impact damage from micrometeorites or other debris during ascent, orbit, and descent, and thus must be able to withstand damage and to function following damage. Thermal protection materials and coatings used in reusable launch vehicles will be reviewed, including the needs and directions for new materials to enable new missions that require faster turnaround and much greater reusability. The role of ablative materials for use in high heat flux environments, especially for non-reusable applications and upcoming planetary missions, will be discussed. New thermal protection system materials may enable the use of sharp nose caps and leading edges on future reusable space transportation vehicles. Vehicles employing this new technology would have significant increases in maneuverability and out-of-orbit cross range compared to current vehicles, leading to increased mission safety in the event of the need to abort during ascent or from orbit. Ultrahigh temperature ceramics, a family of materials based on HfB2 and ZrB2 with SiC, will be discussed. The development, mechanical and thermal properties, and uses of these materials will be reviewed.

Johnson, Sylvia M.↗

NASA NTRS2001

Property and Microstructural Characterization of Diboride Composites for High Temperature Aerospace Applications

Previous work on refractory diboride composites has shown these systems to have potential for use in high temperature leading edge applications for reusable reentry vehicles. These composites, based on compositions of HfB2 or ZrB2 with SiC particulate reinforcements, have shown good oxidation resistance in reentry environments. In this work we are investigating the effects of composition and microstructure on properties. Preliminary studies of composite mechanical properties and oxidation behavior will be discussed.

Gusman, Michael I.↗

NASA NTRS2003

Oxidation of Ultra-High Temperature Ceramics in Water Vapor

Ultra high temperature ceramics (UHTCs) including HfB2 + SiC (20% by volume), ZrB2 + SiC (20% by volume) and ZrB2 + SiC (14% by volume) + C (30% by volume) have historically been evaluated as reusable thermal protection systems for hypersonic vehicles. This study investigates UHTCs for use as potential combustion and aeropropulsion engine materials. These materials were oxidized in water vapor (90%) using a cyclic vertical furnace at 1 atm. The total exposure time was 10 hours at temperatures of 1200, 1300, and 1400 C. CVD SiC was also evaluated as a baseline comparison. Weight change measurements, X-ray diffraction analyses, surface and cross-sectional SEM and EDS were performed. These results will be compared with tests ran in static air at temperatures of 1327, 1627, and 1927 C. Oxidation comparisons will also be made to the study by Tripp. A small number of high pressure burner rig (HPBR) results at 1100 and 1300 C will also be discussed. Specific weight changes at all three temperatures along with the SIC results are shown. SiC weight change is negligible at such short duration times. HB2 + SiC (HS) performed the best out of all the tested UHTCS for all exposure temperatures. ZrB2 + Sic (ZS) results indicate a slightly lower oxidation rate than that of ZrBl + SiC + C (ZCS) at 1200 and 1400 C, but a clear distinction can not be made based on the limited number of tested samples. Scanning electron micrographs of the cross-sections of all the UHTCs were evaluated. A representative area for HS is presented at 1400 C for 26 hours which was the composition with the least amount of oxidation. A continuous SiO2 scale is present in the outer most edge of the surface. An image of ZCS is presented at 1400 C for 10 hours, which shows the most degradation of all the compositions studied. Here, the oxide surface is a mixture of ZrSiO4, ZrO2 and SO2.

Nguyen, QuynhGiao N.↗

NASA NTRS2003

Sintering Behavior of Diboride Based Materials

A brief history of diboride research, an overview of processing, and sintering studies are covered in this viewgraph presentation. UHTCs are a family of ceramic materials, including diborides of Hf and Zr, with extremely high melting temperatures. Spark Plasma Sintering (SPS) is a novel processing technique useful in consolidating difficult materials. The presentation also contains microphotographs of the microstructure of HfB2 and ZrB2 processed in different ways.

Gasch, Matt↗

NASA NTRS2004

Oxidation of Ultra-High Temperature Ceramics in Water Vapor

Ultra High Temperature Ceramics (UHTCs) including HfB2 + 20% SiC (HS), and ZrB2 + 20% SiC (ZC), and ZrB2 + 30% C + 14% SiC (ZCS) have been investigated for use as potential aeropropolsion engine materials. These materials were oxidized in water vapor (90%) using a cyclic vertical furnace at 1 atm. The total exposure time was 10 hours at temperature of 1200, 1300, and 1400 C. CVD SiC was also evaluate as a baseline for comparison. Weight change, X-ray diffraction analysis, surface and cross-sectional SEM and EDS were performed. These results are compared with tests conducted in a stagnant air furnace at temperatures of 1327 C for 100 minutes, and with high pressure burner rig (HPBR) results at 1100 and 1300 C at 6 atm for 50 h. Total recession measurements are also reported for the two tests environments.

Nguyen, QuynGiao N.↗

NASA NTRS2004

Oxidation of Ultra High Temperature Ceramics in Water Vapor

Ultra High Temperature Ceramics (UHTCs) including HfB2 + 20v/0 SiC (HS), ZrB2 + 20v/0 SiC (ZS), and ZrB2 + 30v/0 C + 14v/0 SiC (ZCS) have been investigated for use as potential aeropropulsion engine materials. These materials were oxidized in water vapor (90 percent) using a cyclic vertical furnace at 1 atm. The total exposure time was 10 h at temperatures of 1200, 1300, and 1400 C. CVD SiC was also evaluated as a baseline for comparison. Weight change, X-ray diffraction analyses, surface and cross-sectional SEM and EDS were performed. These results are compared with tests ran in a stagnant air furnace at temperatures of 1327 C for 100 min, and with high pressure burner rig (HPBR) results at 1100 and 1300 C at 6 atm for 50 h. Low velocity water vapor does not make a significant contribution to the oxidation rates of UHTCs when compared to stagnant air. The parabolic rate constants at 1300 C, range from 0.29 to 16.0 mg(sup 2)cm(sup 4)/h for HS and ZCS, respectively, with ZS results between these two values. Comparison of results for UHTCs tested in the furnace in 90 percent water vapor with HPBR results was difficult due to significant sample loss caused by spallation in the increased velocity of the HPBR. Total recession measurements are also reported for the two test environments.

Nguyen, QuynhGiao N.↗

NASA NTRS2004

Characterization of an Ultra-High Temperature Ceramic Composite

Levine, Stanley R.↗

NASA NTRS2001

Ultra-High Temperature Ceramic (UHTC) Development

During the last decade, NASA Ames has been developing new, Ultra-High Temperature Ceramic (UHTC) materials for Thermal Protection Systems applications. The UHTC s are a family of materials including compositions of HfE32 and ZrB2 with a Sic second phase. A collaboration with Glenn was recently initiated to evaluate the viability of some UHTC materials that had been produced by an outside vendor for use in gas turbine en,@ne environments. Results from this collaboration have indicated that compositions based on HfB2 show the most promise, among the UHTC compositions evaluated, for use in these environments. Work at ARC has been initiated to fabricate these materials in-house and evaluate methods of improving their properties for use in engine environments.

Johnson, Sylvia↗

NASA NTRS2009

Ultra High Temperature Ceramics' Processing Routes and Microstructures Compared

Ultra High Temperature Ceramics (UHTCs), such as HfB2 and ZrB2 composites containing SiC, are known to have good thermal shock resistance and high thermal conductivity at elevated temperatures. These UHTCs have been proposed for a number of structural applications in hypersonic vehicles, nozzles, and sharp leading edges. NASA Ames is working on controlling UHTC properties (especially, mechanical properties, thermal conductivity, and oxidation resistance) through processing, composition, and microstructure. In addition to using traditional methods of combining additives to boride powders, we are preparing UHTCs using coat ing powders to produce both borides and additives. These coatings and additions to the powders are used to manipulate and control grain-boundary composition and second- and third-phase variations within the UHTCs. Controlling the composition of high temperature oxidation by-products is also an important consideration. The powders are consolidated by hot-pressing or field-assisted sintering (FAS). Comparisons of microstructures and hardness data will be presented.

Gusman, Michael↗

NASA NTRS2012

Multiscale Modeling of UHTC: Thermal Conductivity

We are developing a multiscale framework in computational modeling for the ultra high temperature ceramics (UHTC) ZrB2 and HfB2. These materials are characterized by high melting point, good strength, and reasonable oxidation resistance. They are candidate materials for a number of applications in extreme environments including sharp leading edges of hypersonic aircraft. In particular, we used a combination of ab initio methods, atomistic simulations and continuum computations to obtain insights into fundamental properties of these materials. Ab initio methods were used to compute basic structural, mechanical and thermal properties. From these results, a database was constructed to fit a Tersoff style interatomic potential suitable for atomistic simulations. These potentials were used to evaluate the lattice thermal conductivity of single crystals and the thermal resistance of simple grain boundaries. Finite element method (FEM) computations using atomistic results as inputs were performed with meshes constructed on SEM images thereby modeling the realistic microstructure. These continuum computations showed the reduction in thermal conductivity due to the grain boundary network.

Lawson, John W.↗

NASA NTRSDate not supplied

Unified Material-Environment Interaction Model for Binary UHTC Composites

A new model for the surface chemistry of zirconium and hafnium diborides containing silicon-carbide when exposed to high temperature conditions in air is formulated. Oxidation dynamics are simplified by considering the diffusion-limited equilibrium regime within the material at elevated temperatures. This model is first assessed against experimental mass-gain data taken from UHTC samples heated to high temperature in an oxygen environment. Then, further evaluations of the new model are conducted using hypersonic CFD simulations to analyze conditions experienced by HfB2-SiC in arc jet experiments conducted at NASA Ames Research Center. Measurements of stagnation point heat transfer and pressure are then used to calibrate the simulations. Results of coupled CFD-material response simulations are then compared to the surface temperatures measured during the Ames arc jet test. Results support the use of the proposed model while highlighting the need for improved gas-phase data on the additional constituents considered.

ultra high temperature ceramic↗

DOE OSTI2021

Stability Evaluation of Candidate Precursors for Chemical Vapor Deposition of Hafnium Diboride (HfB 2 )

Not Available

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗