Mechanical Properties of Polycrystalline Lithium Orthosilicate

Room-temperature mechanical properties and high-temperature creep deformation of lithium orthosilicate (Li₄SiO₄) were studied. Elastic constants, flexural strength, and fracture toughness were determined for specimens with densities between 68% and 98% of theoretical. Critical quenching temperature and thermal-shock resistance parameters for 90% dense specimens were also measured. High-temperature creep deformation was investigated by a constant-strain-rate test in an argon atmosphere at temperatures between 750° and 1025°C and strain rates ranging from about 10⁻⁶ to 10⁻³ s⁻¹. At 950°C and above, the stress exponent, n , was determined to be 3.6, with a creep activation energy of 715 kJ/mol. Selected results obtained for Li₄SiO₄ are compared with results obtained for other Li-containing ceramics that are under consideration as candidates for fusion reactor breeder blankets.     

Low-Temperature Creep of Nanocrystalline Titanium(IV) Oxide

Nanocrystalline TiO₂ with densities higher than 99% of rutile has been deformed in compression without fracture at temperatures between 600° and 800°C. The total strains exceed 0.6 at strain rates as high as 10⁻³ s⁻¹. The original average grain size of 40 nm increases during the creep deformation to final values in the range of 120 to 1000 nm depending on the temperature and total deformation. The stress exponent of the strain rate, n , is approximately 3 and the grain size dependence is d ^{− q} with q in the range of 1 to 1.5. It is concluded that the creep deformation occurs by an interface reaction controlled mechanism.     

Effects of Temperature and Strain Rate on the Plastic Deformation of Fully Dense Polycrystalline Y1Ba2Cu3O7−x Superconductor

The knowledge of the steady-state stress for plastic deformation as a function of temperature and strain rate is essential for hot-forming superconducting material into commercially useful shapes. In this paper, results are presented on the experimental determination of the rheology of fully dense polycrystalline Y₁Ba₂Cu₃O_7−x superconducting material at temperatures ranging from 750° to 950°C and strain rates of 10⁻⁴, 10⁻⁵, and 10⁻⁶ s⁻¹. The data are best fitted by a power law: ε(s⁻¹)=8.9 × 10⁻¹⁷. (s⁻¹) σ^2.5 (Pa) exp [−2.01 × 10⁵(J·mol⁻¹)|RT]. X-ray analysis shows that the superconducting material retains its phase composition after nearly 70% total strain of the sample. A strong anisotropy in the resistivity of the deformed samples is observed because of the development of a preferred orientation of the a or b axis of Y₁Ba₂Cu₃O_7−x orthorhombic perovskite single crystals perpendicular to the principal maximum compressive stress.     

Superplastic Alumina Ceramics with Grain Growth Inhibitors

Superplastic deformation of alumina ceramics was studied at 1400° to 1450°C and at a strain rate of 4 × 10⁻⁵ to 5 × 10⁻⁴ s⁻¹. MgO and ZrO₂ were introduced to suppress dynamic grain growth. The latter was especially effective; grain growth was minimal in 10-vol%-ZrO₂-containing material. Both materials were superplastically stretched under biaxial tension to 100% engineering strain with good surface finishing, demonstrating the feasibility of superplastic forming for alumina ceramics.     

Superplasticity of Hot Isostatically Pressed Hydroxyapatite

Dense and translucent hydroxyapatite polycrystals (Ca₁₀(PO₄)₆(OH)₂ with a grain size of 0.64 μMm) were obtained by hot isostatic pressing at 203 MPa and 1000°C for 2 h in argon. The material exhibited superplastic elongation (>150%) in a tension test at temperatures from 1000° to 1100°C and at strain rates from 7.2×10⁻⁵ to 3.6 × 10⁻⁴ s⁻¹. Extensive strain hardening was observed. The stress exponent of the yield stress was larger than 3.     

Superplastic Behavior of Fine-Grained β-Silicon Nitride Material under Compression

The deformation behavior of a hot-pressed, fine-grained β-Si₃N₄ ceramic was investigated in the temperature range 1450°—1650°C, under compression, and the results for strain rate and temperature dependence of the flow stress are presented here. The present results show that the material is capable of high rates of deformation (∼10⁻⁴—10⁻³ s⁻¹) within a wide range of deformation temperatures and under a pressure of 5—100 MPa; no strain hardening occurs in the material, even at slow deformation rates, because of its stable microstructure; Newtonian flow occurs, with a stress exponent of approximately unity; and the material has activation energy values for flow in the range 344—410 kJ·mol⁻¹. Grain-boundary sliding and grain rotation, accommodated by viscous flow, might be the mechanisms of superplasticity for the present material.     

Plastic Deformation of Hydroxyapatites and Its Application to Joining

A plastic deformation process was demonstrated to self-join hydroxyapatite (HA), fabricating pore-free joints at 1275°C at a strain rate of 10⁻⁵ s⁻¹. To determine optimum joining conditions, high-temperature compressive deformation of HA was investigated for strain rates between 5 × 10⁻⁶ and 10⁻⁴ s⁻¹ at temperatures 1175–1275°C. X-ray diffraction revealed primarily the HA phase with the presence of tri- and tetra-calcium phosphate phases. Steady-state flow stresses were 0.6–45 MPa and increased with increasing strain rates. Stress exponents of ≈1 indicated a viscous diffusion-controlled deformation mechanism with an activation energy of ≈354±36 kJ/mol. Absence of cavitation and grain shape changes was consistent with grain boundary sliding.     

Superplastic Deformation of Zinc Sulfide Near Its Transformation Temperature [1020°]

Polycrystalline ZnS was deformed in compression to large strains (up to 100%), near its α⇄β transformation temperature (1020°), at strain rates that ranged from 10⁻⁵ to 3 × 10⁻³ s⁻¹. The flow stress showed a minimum near 1020°. The strain rate sensitivity and the grain size dependence of the flow stress suggest a superplastic mechanism of deformation. There was some evidence of dynamic recrystallization and stress-induced β (fcc) to α (hcp) phase transformation. The polycrystals had a tendency to form in tergranular cavities at the higher temperatures and at faster strain rates.     

Superplastic Bulging of Fine-Grained Zirconia

A tetragonal zirconia containing 2 mol% Y₂O₃, with 0.3 mol% CuO addition as a grain-boundary phase, was superplastically stretched at 1150°C using a hemispherical punch. Mechanical analyses were performed to establish that a biaxial tensile stress/strain state was achieved in the process with a maximal strain of 0.5 in the thinned hemispherical shell. The material was damage tolerant up to a critical strain rate, approximately 10⁻³ s⁻¹.     

Rapid Densification and Deformation of Li-Doped Sialon Ceramics

Two lithium-doped sialon ceramics were densified and superplastically deformed by spark plasma sintering (SPS). Rapid densification with linear shrinkage rates of approximately 5 × 10⁻³ s⁻¹ were observed for samples heated at a rate of 100°C/min up to ∼1400°C under a uniaxial pressure of 40 MPa. Isothermal deformation by SPS-preprepared, fully densified ceramics performed at T ≥ 1450°C yielded strain rates in the order of 10⁻² s⁻². It is suggested that a high heating rate promotes material transport via formation of a nonequilibrated oxygen-rich liquid of low viscosity. This finding most likely holds true for other liquid-phase sintered ceramics as well and has implications for cost-effective manufacturing of ceramic components.     

Diffusional Creep and Kinetic Demixing in Yttria-Stabilized Zirconia

The creep behavior of fine-grained yttria-stabilized zirconia with 25 mol% Y₂O₃ has been characterized as part of an investigation of kinetic demixing in solid-solution oxides which are subjected to a nonhydrostatic state of stress. At temperatures between 1400° and 1600°C, the steady-state strain rate of (Zr_0.6Y_0.4)O_1.8 samples with average grain sizes between 2.5 and 14.5 μm can be summarized by the flow law ɛ= 6.5 × 10⁻⁷σ^1.2 exp[−550 (kJ/mol)/ RT ] d ^−2.2 (s⁻¹) for stresses in the range 8 to 60 MPa, where σ is in pascals and d is in meters. This flow law indicates that deformation occurs by a Nabarro-Herring creep mechanism in which the creep rate is limited by cation lattice diffusion. Kinetic demixing was not observed in deformed polycrystalline samples even though diffusional creep was rate limited by cation lattice diffusion. This result can be explained if the cation diffusivities are approximately equal or if extensive grain rotation occurs during diffusional creep.     

Effect of Dynamic Microstructural Change on Deformation Behavior in Liquid-Phase-Sintered Silicon Carbide with Al2O3–Y2O3–CaO Additions

Nanocrystalline β-SiC with additions of 7 wt% Al₂O₃, 2 wt% Y₂O₃, and 1 wt% CaO was subjected to tensile deformation to study its microstructural behavior under the dynamic process. The liquid-phase-sintered body had a relative density of >97% and an average grain size of 170 nm. Tension tests were conducted at initial strain rates ranging from 2 × 10⁻⁵ to 5 × 10⁻⁴ s⁻¹, in the temperature range 1973–2023 K, in both argon and N₂ atmospheres. Although grain-boundary liquids formed by the additions vaporized concurrently with the decomposition of SiC and extensive grain growth, the maximum tensile elongation of 48% was achieved in argon. Annealing experiments under the same conditions revealed that vaporization and grain growth were both dependent on experimental time. Therefore, high strain rates suffered less from the hardening effect when cavitation damage was more severe. Testing in an N₂ atmosphere brought about crystallization of the grain-boundary phase and prevented severe vaporization; however, fracture occurred at only 8% elongation. Grain-boundary sliding was still the dominant mechanism for deformation.     

Intergranular Fracture of Lithium Fluoride–22% Calcium Fluoride Hypereutectic Salt at 800 K

Constant-velocity compression tests were conducted at 800 K on as-cast LiF-22 mol% CaF₂ hypereutectic salt with engineering strain rates varying between 1.8 × 10⁻⁶ and 2.3 × 10⁻¹ s⁻¹. Considerable stain hardening was observed during the initial stages of deformation, and the true stress-strain curves exhibited maxima. Plots of the true strain rate against the flow stress at the proportional limit and the peak stress exhibited a power-law relation with stress exponents of 7.7. Microstructural examination of the deformed specimens showed extensive grain-boundary cracking and cavitation. These results suggest that grain-boundary cracking and interfacial sliding is important for cavity nucleation at the grain boundaries and at the LiF-CaF₂ interfaces, and cavity growth and interlinkage, which appear to depend on the morphological differences between different grain boundaries, occur through the preferential failure of the weaker LiF phase.     

Vapor Pressures of Simple Silicate Glass Melts

Partial and total vapor pressures over Na₂O.3SiO₂ anhd Rb₂O.3SiO_z melts were determined at 1150° to 1300°C with the Knudsen-effusion method. A Pt Knudsen cell was placed on a microbalance so that the weight loss due to effusion from the Knudsen hole could be recorded continuously. The specific vaporization rates are between ∼3.10⁻⁶ and 3.10⁻⁴ gcm⁻² s⁻¹; the corresponding vapor pressures are between ∼3.10⁻² and 3 Pa.     

Superplastic Deformation in Fine-Grained YBa2Cu3O7−x

The superplastic behavior of YBa₂Cu₃O_{7− x} ceramic superconductors was studied. Large compressive deformation over 100% strain was measured in the temperature range of 775°–875°C, with a strain rate of 1 × 10⁻⁵ to 1 × 10⁻³/s, and a grain size of 0.5–1.4 μm. The nature of the deformation was investigated in terms of three deformation parameters: the stress exponent ( n ), the grain size exponent ( p ), and the activation energy ( Q ). The measured values of these parameters were n = 2 ± 0.3, p = 2.7 ± 0.7, and Q = 745 ± 100 kJ/mol. With the aid of the deformation map, the deformation mechanism was identified as grain boundary sliding accommodated by grain boundary diffusion. The conclusion is consistent with the microstructural observations made by SEM and TEM: the invariance of equiaxed grain shape, the absence of significant dislocation activity, no grain boundary second phases, and no significant texture development.     

Tensile Creep and Creep-Strain Recovery Behavior of Silicon Carbide Fiber/Calcium Aluminosilicate Matrix Ceramic Composites

The tensile creep and creep strain recovery behavior of 0° and 0°/90° Nicalon-fiber/calcium aluminosilicate matrix composites was investigated at 1200°C in high-purity argon. For the 0° composite, the 100-h creep rate ranged from approximately 4.6 × 10⁻⁹ s⁻¹ at 60 MPa to 2.2 × 10⁻⁸ s⁻¹ at 200 MPa. At 60 MPa, the creep rate of the 0°/90° composite was approximately the same as that found for the 0° composite, even though the 0°/90° composite had only one-half the number of fibers in the loading direction. Upon unloading, the composites exhibited viscous strain recovery. For a loading history involving 100 h of creep at 60 MPa, followed by 100 h of recovery at 2 MPa, approximately 27% of the prior creep strain was recovered for the 0° composite and 49% for the 0°/90° composite. At low stresses (60 and 120 MPa), cavities formed in the matrix, but there was no significant fiber or matrix damage. For moderate stresses (200 MPa), periodic fiber rupture occurred. At high stresses (250 MPa), matrix fracture and rupture of the highly stressed bridging fibers limited the creep life to under 70 min.     

Electromechanical Properties of Pb(Yb1/2Nb1/2)O3-PbZrO3-PbTiO3 Ceramics

The electromechanical and electric-field-induced strain properties of x Pb(Yb_1/2Nb_1/2)O₃· y PbZrO₃·(1− x − y )PbTiO₃ ( x = 0.12, 0.25, 0.37; y = 0.10–0.40) ceramics have been studied systematically as a function of Pb(Yb_1/2Nb_1/2)O₃ (PYN) content and PbZrO₃/PbTiO₃ (PZ/PT) ratio. In addition, the effect of MnO₂ on the electromechanical properties of 0.12Pb(Yb_1/2Nb_1/2)O₃·0.40PbZrO₃·0.48PbTiO₃ was also investigated. The maximum transverse strain values of 1.6 × 10⁻³ for x = 0.12, 1.45 × 10⁻³ for x = 0.25, and 1.36 × 10⁻³ for x = 0.37 were obtained at the compositions which were regarded as the morphotropic phase boundary (MPB). The transverse strain was maximized at the MPB composition. The value of the maximum electromechanical coupling coefficient was 0.69 for y = 0.40 and x = 0.12 composition. In the 0.12Pb(Yb_1/2Nb_1/2)O₃·0.40PbZrO₃·0.48PbTiO₃ composition, the temperature of the maximum dielectric constant decreased and the grain size increased with an addition of MnO₂. The electromechanical coupling coefficient decreased while the mechanical quality factor rapidly increased with an addition of MnO₂. These resulted mainly from the acceptor effect of manganese ions that were produced by doping MnO₂ into the perovskite structure.     

In Situ Reaction Synthesis, Electrical and Thermal, and Mechanical Properties of Nb4AlC3

In this work, a bulk Nb₄AlC₃ ceramic was prepared by an in situ reaction/hot pressing method using Nb, Al, and C as the starting materials. The reaction path, microstructure, physical, and mechanical properties of Nb₄AlC₃ were systematically investigated. The thermal expansion coefficient was determined as 7.2 × 10⁻⁶ K⁻¹ in the temperature range of 200°–1100°C. The thermal conductivity of Nb₄AlC₃ increased from 13.5 W·(m·K)⁻¹ at room temperature to 21.2 W·(m·K)⁻¹ at 1227°C, and the electrical conductivity decreased from 3.35 × 10⁶ to 1.13 × 10⁶Ω⁻¹·m⁻¹ in a temperature range of 5–300 K. Nb₄AlC₃ possessed a low hardness of 2.6 GPa, high flexural strength of 346 MPa, and high fracture toughness of 7.1 MPa·m^1/2. Most significantly, Nb₄AlC₃ could retain high modulus and strength up to very high temperatures. The Young's modulus at 1580°C was 241 GPa (79% of that at room temperature), and the flexural strength could retain the ambient strength value without any degradation up to the maximum measured temperature of 1400°C.     

Fabrication of Mullite Body Using Superplastic Transient Phase

Mullite, an extremely creep-resistant ceramic, has been fabricated using a novel processing/forming approach taking advantage of superplastic transitional phases. Starting with a mixture of alumina, silica, and a small amount of lithia additive (0.8 wt%), a processing window of about 50°C around 1350°C has been found within which the material can be densified and superplastically deformed with negligible mullitization. The lithia additive promotes a transient lithium aluminosilicate glassy phase that greatly enhances sintering and deformation. The superplastic premullite maintains a nearly constant grain size during deformation between 1250° and 1400°C, over a strain rate from 6 × 10⁻⁷ to 10⁻¹ s⁻¹, and has unusually high activation energy values in the range of 1150 to 2086 kJ/mol. An increase in the transient glassy phase content due to the increased matrix dissolution at higher temperatures contributes in part to this anomaly. The mullite work pieces thus shaped become creep resistant again after a postforming annealing/mullitization treatment which decreases the creep rate by 6 orders of magnitude. The mechanical properties (hardness, toughness, and strength) of the finished mullite are compared to those of conventionally processed mullite.     

Flexural Creep of Coated SiC-Fiber-Reinforced Glass-Ceramic Composites

This study reports the flexural creep behavior of a fiber-reinforced glass-ceramic and associated changes in micro-structure. SiC fibers were coated with a dual layer of SiC/BN to provide a weak interface that was stable at high temperatures. Flexural creep, creep-rupture, and creep-strain recovery experiments were conducted on composite material and barium-magnesium aluminosilicate matrix from 1000° to 1200°C. Below 1130°C, creep rates were extremely low (∼10⁻⁹ S⁻¹), preventing accurate measurement of the stress dependence. Above 1130°C, creep rates were in the 10⁻⁸ s⁻¹ range. The creep-rupture strength of the composite at 1100°C was about 75–80% of the fast fracture strength. Creep-strain recovery experiments showed recovery of up to 90% under prolonged unloading. Experimental creep results from the composite and the matrix were compared, and microstructural observations by TEM were employed to assess the effectiveness of the fiber coatings and to determine the mechanism(s) of creep deformation and damage.