Deformation behavior and joining of a MgF2 optical ceramic

Compressive deformation behavior of a polycrystalline magnesium fluoride (MgF₂) ceramic was investigated at temperatures ranging from 760 to 830 °C in an argon atmosphere at strain rates between 2 × 10⁻⁶ and 4 × 10⁻⁵ s⁻¹. Steady-state flow stresses increased with increasing strain rates and ranged between 2 and 38 MPa. Stress exponents of ≈1.4 ± 0.2 were determined at temperatures >760 °C, indicative of a viscous diffusion-controlled deformation mechanism. Activation energy, determined from flow stress as a function of temperature, at a constant strain rate, was ≈476 ± 60 kJ/mol. Self-joining by plastic deformation of MgF₂ was demonstrated at 830 °C at a strain rate of 5 × 10⁻⁶ s⁻¹. The joined samples were characterized by optical transmission measurements and their transmittivity was ≈80% of the unjoined sample in the 2.5–8 μm wavelength range.     

High-temperature deformation of amorphous AlPO4-based nano-composites

High-temperature compressive deformation of an amorphous aluminum phosphate nano-composite was investigated at 1200–1300 °C. Microstructural and X-ray diffraction investigations of sol–gel-derived material revealed an amorphous structure with relatively high fraction of closed porosity of ≈15 vol.%. Transmission electron microscopy revealed nanocrystallites, predominantly of carbon, dispersed in the amorphous matrix. Steady-state flow stresses were 10–50 MPa and 50–70 MPa for test temperatures of 1200 and 1300 °C, respectively, as the strain rates were varied from 5 × 10⁻⁶ to 2 × 10⁻⁵ s⁻¹. Flow stresses increased with strain rates at a fixed temperature: stress exponents were 2.2–2.8 for various test temperatures, indicative of non-Newtonian flow. The non-Newtonian flow was attributed to the presence of the nanocrystalline phases. The creep resistance was found to be on a par with those of conventional oxide ceramics.     

High temperature creep behaviour of 4 mol% yttria tetragonal zirconia polycrystals (4-YTZP) with grain sizes between 0.38 and 1.15 μm

The high temperature mechanical behaviour of 4% mol yttria tetragonal zirconia polycrystals (4-YTZP) with different grain sizes (0.38 < d < 1.15 μm) has been analyzed by means of compression creep tests. The working temperature was 1350 °C and the strain rates ranged between 5 × 10⁻⁷ and 2 × 10⁻⁴ s⁻¹. Experimental results have been fitted to the conventionally accepted creep law for superplastic ceramics. Thus, stress exponents and activation energies have been measured as a function of the grain size. The dependence of strain rate on grain size has also been determined. The experimental data are discussed with respect to the existing theoretical models for these materials.     

Dielectric and magnetic properties of Nickel ferrite ceramics using crystalline powders derived from DL alanine fuel in sol–gel auto-combustion

Dielectric and magnetic properties of NiFe₂O₄ ceramics prepared with powders using DL-alanine fuel in the sol–gel auto combustion technique are studied. DL-alanine fuel yields crystalline as-burnt powders, and when used for ceramic processing yields varying microstructure at different sintering temperatures. The dielectric properties are influenced by the resulting microstructure and the magnetic properties show slight change in saturation magnetization M_s (~44 – 46 emu/g). The coercive fields, dielectric losses and dispersion are reduced considerably at higher sintering temperatures (1200–1300 °C). The influence of changing microstructure is analyzed through dielectric response, complex impedance analysis and electrical modulus spectroscopy in the frequency range (10⁻²–10⁷ Hz) to understand the interactions from the grain and grain boundary phases. Sintering at 1200 °C, is found to be optimum, yields lower losses & reduced dielectric dispersion, and high resistivity (3.4×10⁸ Ω cm).     

Characteristics of samaria-doped ceria nanoparticles prepared by spray pyrolysis

Samaria-doped ceria (SDC) nanoparticles were prepared by spray pyrolysis. The means sizes of the samaria-doped ceria nanoparticles were controlled from 21 to 150 nm by changing the calcination temperatures between 700 and 1200 °C. The pellets formed from the SDC particles calcined at temperatures between 700 and 1000 °C had similar grain sizes between 0.75 and 0.82 μm. However, pellet formed from the SDC particles calcined at a temperature of 1200 °C had large grain size of 1.22 μm. The pellet formed from the SDC particles calcined at a temperature of 1000 °C had slightly smaller resistance of grain-boundary than those of the pellets formed from the SDC particles calcined at temperatures between 700 and 900 °C. However, the pellet formed from the SDC particles calcined at a temperature of 1200 °C had low resistance of grain-boundary. The pellet formed from the SDC particles calcined at a temperature of 1200 °C had conductivity of 44.65 × 10^?3 S cm^?1 at a measuring temperature of 700 °C that more twice than those of the pellets formed from the SDC calcined below 1000 °C.     

Investigation of the electrical conductivity of sintered monoclinic zirconia (ZrO2)

High-density monoclinic ZrO₂ was manufactured through sintering at ~1200 °C by using nanosized powders. Then, the electrical conductivity was measured at a range of high temperatures (700–900 °C) by electrical impedance spectroscopy (EIS). For the as-sintered monoclinic ZrO₂, the measured electrical conductivity was 3.2×10⁻⁵ s/cm (for 80% TD) and 4.4×10⁻⁵ s/cm (for 89% TD) at 900 °C. After aging at 900 °C for 100 h, the electrical conductivity of the monoclinic ZrO₂ of 80%-TD decreased by more than 50%. However, after reheating at 1200 °C for 1 h, approximately 80% of the conductivity was recovered compared to the value of the as-sintered monoclinic ZrO₂. The pure monoclinic crystal structure was retained despite the aging and reheating treatment. Based on microstructural observations of the aged and reheated monoclinic ZrO₂, the changes in electrical conductivity after aging and reheating were explained by the formation and recovery of micro-cracks, respectively.     

SPS processing of bismuth-layer structured ferroelectric ceramics yielding highly textured microstructures

The spark plasma sintering (SPS) behaviour of nano-sized Bi₄Ti₃O₁₂ (BIT) and micron-sized CaBi₂Nb₂O₉ (CBNO) powders is described. The densification process of both powders is very rapid, i.e. the densification occurs within a very narrow time interval (2–3 min using a heating rate of 100 °C min⁻¹ and a pressure of 50 MPa). The BIT powder exhibits a lower densification onset temperature (∼650 °C) and higher maximum shrinkage rate (8.9 × 10⁻³ s⁻¹ at 780 °C) than that of the CBNO powder (∼825 °C and 4.5 × 10⁻³ s⁻¹ at 950 °C). Isothermal compaction studies revealed that fully dense nano-sized BIT compacts could be obtained within the temperature region 750 °C < T_iso < 850 °C while for T_iso > 850 °C compacts containing elongated platelet grains are formed. A new preparation route to produce highly textured compacts is described in detail. Appropriate pre-forms are prepared by spark plasma sintering (SPS) and these fully dense compacts are subject to superplastic deformation in the SPS unit to achieve a total compressive strain of ∼60%. This strain was achieved within a period of 1.5 min and with a maximum strain rates of 1.1 × 10⁻² s⁻¹ achieved at ∼840 °C and 1.3 × 10⁻² s⁻¹ at 1020 °C for the BIT and CBNO compacts, respectively. The X-ray studies showed that the Lotgering orientation factors of grains in the deformed BIT and CBNO compacts are 99% and 70%. The formation of highly textured compacts is suggested to be governed by a superplastic deformation-induced directional dynamic ripening mechanism.     

Low-temperature reactive hot-pressing of cerium-doped titanate composite ceramics and their aqueous stability

Reactive hot-pressing was scarcely applied to fabricate titanate ceramic waste forms designed for immobilizing high-level radioactive waste (HLW). However, compared with non-reactive processes, there is an advantage of producing high-density ceramics at reduced temperatures by reactive hot-pressing. Ce^IV-doped titanate composite ceramics with relative densities in excess of 99% were prepared by reactive hot-pressing at temperature as low as 1150 °C and pressure of 30 MPa for 1–4 h. The results show that low-temperature densification of the composite ceramics might be attributed to the plastic deformation under hot-pressing condition. In addition, aqueous stability testing was carried out using the standard MCC-1 static leach test method. The results demonstrate that the normalized elemental leach rate of Ca, Ce and Zr were fairly constant in a low value below 5 × 10⁻² g m⁻² d⁻¹, 7 × 10⁻⁶ g m⁻² d⁻¹ and 6 × 10⁻⁶ g m⁻² d⁻¹ after 21 d.     

Structure and conductivity of NiO/YSZ composite prepared via modified glycine-nitrate process at varying sintering temperatures

Nickel oxide and Yttria-stabilized zirconia (NiO/YSZ) composite is one of the most promising mixed conducting electrode materials in both solid oxide electrolysis cell and solid oxide fuel cell applications. In this study, 50 wt% NiO and 50 wt% YSZ composite was synthesized via a modified glycine-nitrate combustion process (GNP) and the effect of sintering temperatures (1100 °C, 1300 °C and 1500 °C) on its microstructure and electrical properties were investigated. TG/DTA and in-situ high temperature XRD revealed the thermal property behavior and the structural changes of the as-combusted precursor material. For all the samples sintered at different temperatures, room temperature XRD patterns revealed a distinct cubic phases of both YSZ and NiO while SEM images showed a porous microstructure. The total conductivities at 700 °C are 9.87 × 10⁻³, 5.26 × 10⁻³, 4.02 × 10⁻³ S/cm for the 1100, 1300, and 1500 °C with activation energies of 0.1722, 0.3555, and 0.3768 eV, respectively. Conductivity measurements of the different sintered samples revealed that the total conductivities as well as the activation energies are greatly affected by different sintering temperatures.     

Signature of multiferroicity and pyroelectricity close to room temperature in BaFe12O19 hexaferrite

In this paper, we have reported the signature of multiferroicity and pyroelectricity in BaFe₁₂O₁₉ hexaferrite close to room temperature. The BaFe₁₂O₁₉ hexaferrite samples are synthesized by co-precipitation method at different sintering temperature ranging from 800 to 1200 °C and study their structural, ferroelectric, magnetic, magnetoelectric and pyroelectric properties. X-ray Diffraction patterns show the pure phase formation for all samples. Morphological changes are examined through the scanning electron microscope. The maximum ferroelectric polarization (0.66 μC/cm²) is observed for the sample sintered at 1200 °C, however maximum magnetic polarization 74 emu/g is observed for sample sintered at 1000 °C. Magneto-electric coupling measurements are also performed through dynamic method and average magneto-electric coupling coefficient (~ 7.05 × 10⁻⁷ mV/cm Oe²) is observed at room temperature for the sample sintered at 1200 °C. Furthermore, maximum pyroelectric constant (147 × 10⁻¹³C/cm² °C) is observed at 75 °C for BaFe₁₂O₁₉ samples sintered at 1200 °C. The observation of both multiferroicity and pyroelectricity close to room temperature in BaFe₁₂O₁₉ hexaferrite is interesting and useful for multifunctional devices.     

Tribological behavior of Ti3SiC2 and Ti3SiC2/Pb composites sliding against Ni-based alloys at elevated temperatures

The Ti₃SiC₂ and Ti₃SiC₂/Pb composites were tested under dry sliding conditions against Ni-based alloys (Inconel 718) at elevated temperatures up to 800 °C using a pin-on-disk tribometer. Detailed tribo-chemical changes of Pb on sliding surface were discussed. It was found that the tribological behavior were insensitive to the temperature from 25 °C (RT) to 600 °C (friction coefficient ≈0.61–0.72, wear rate ≈10⁻³ mm³ N m⁻¹). An amount of Pb in the composites played a key role in lubricating with the temperature below 800 °C. The friction coefficient (≈0.22) and wear rate (≈10⁻⁷ mm³ N m⁻¹) at elevated temperatures were both decreased by the added PbO. The wear mechanisms of Ti₃SiC₂/Pb-Inconel 718 tribo-pair at elevated temperatures were believed to be the combined effect of abrasive wear and tribo-oxidation wear. During the sliding, two oxidization reactions proceed, 2Pb+O₂=2PbO (below 600 °C) and 6PbO+O₂=2Pb₃O₄ (800 °C). The friction coefficient and wear rate of the composites were reduced due to the self-lubricating effect of the tribo-oxidation products.     

Effect of Nd-doping on structural,thermal and electrochemical properties of LaFe0.5Cr0.5O3 perovskites

The structural, thermal and electrochemical properties of the perovskite-type compound La_1−xNd_xFe_0.5Cr_0.5O₃ (x=0.10, 0.15, 0.20) are investigated by X-ray diffraction, thermal expansion, thermal diffusion, thermal conductivity and impedance spectroscopy measurements. Rietveld refinement shows that the compounds crystallize with orthorhombic symmetry in the space group Pbnm. The average thermal expansion coefficient decreases as the content of Nd increases. The average coefficient of thermal expansion in the temperature range of 30–850 °C is 10.12×10⁻⁶, 9.48×10⁻⁶ and 7.51×10⁻⁶ °C⁻¹ for samples with x=0.1, 0.15 and 0.2, respectively. Thermogravimetric analyses show small weight gain at high temperatures which correspond to filling up of oxygen vacancies as well as the valence change of the transition metals. The electrical conductivity measured by four-probe method shows that the conductivity increases with the content of Nd; the electrical conductivity at 520 °C is about 4.71×10⁻³, 6.59×10⁻³ and 9.62×10⁻³ S cm⁻¹ for samples with x=0.10, 0.15 and 0.20, respectively. The thermal diffusivity of the samples decreases monotonically as temperature increases. At 600 °C, the thermal diffusivity is 0.00425, 0.00455 and 0.00485 cm² s⁻¹ for samples with x=0.10, 0.15 and 0.20, respectively. Impedance measurements in symmetrical cell arrangement in air reveal that the polarization resistance decreases from 55 Ω cm⁻² to 22.5 Ω cm⁻² for increasing temperature from 800 °C to 900 °C, respectively.     

Coupled strain rate and temperature effects on the tensile behavior of strain-hardening cement-based composites (SHCC) with PVA fibers

This paper reports the experimental findings on the tensile behavior of Strain-hardening cement-based composites (SHCC) subjected to elevated temperatures and different strain rates and to combinations of these parameters. Uniaxial tension tests with in-situ temperature control were performed at 22 °C, 60 °C, 100 °C and 150 °C. In addition, the effect of loading rate was investigated using the strain rates of 10^? 5 s^? 1, 3 × 10^? 4 s^? 1 and 10^? 2 s^? 1 at all four temperatures considered. It was shown that tensile strength decreases both with an increase in temperature and with a decrease in the strain rate. The strain capacity increases with decreasing strain rate at temperatures of 22 °C and 60 °C, but for the temperature of 100 °C this material property increases when the strain rate increases. At 150 °C the investigated SHCC loses its ductility and no noticeable strain rate effect can be observed. Furthermore, the residual properties of SHCC were evaluated using uniaxial tensile tests at room temperature on the specimens which were previously heated to 60 °C, 100 °C or 150 °C. The residual tests showed that the strength, strain capacity, and work-to-fracture decrease with increasing pre-treatment temperature. However, in comparison with the results of the in-situ tests with elevated in-situ temperatures, the residual tests on SHCC yielded higher tensile strength and lower ductility. These results and possible mechanisms leading to changes in mechanical performance are discussed on the basis of the observed crack patterns on the specimens' surfaces as well as the microscopic investigations of the condition of fibers on fracture surfaces.     

Structural and electrical properties of Sr2NaNb4O13 thin film grown by electrophoretic method using nanosheets synthesized from K(Sr2Na)Nb4O13 compound

Sr₂NaNb₄O₁₃⁻ (SNNO⁻) nanosheets were exfoliated from the K(Sr₂Na)Nb₄O₁₃ compound that was synthesized at 1200 °C. The SNNO⁻ nanosheets were deposited on a Pt/Ti/SiO₂/Si substrate at room temperature by the electrophoretic method. Annealing was conducted at various temperatures to remove organic defects in the SNNO film. A crystalline SNNO phase without organic defects was formed in the film annealed at 500 °C. However, a SrNb₂O₆ secondary phase was formed in the films annealed above 600 °C, probably due to the evaporation of Na₂O. The SNNO thin film annealed at 500 °C showed a dielectric constant of 74 at 1.0 MHz with a dielectric loss of 2.2%. This film also exhibited a low leakage current density of 9.0 × 10⁻⁸ A/cm² at 0.6 MV/cm with a high breakdown electric field of 0.72 MV/cm.     

Nitrogen-containing apatite

Two commercial hydroxyapatites were treated in dry ammonia at temperatures between 800 and 1300°C for different times up to 30 h. Nitrogen was incorporated with a maximum content of 3·7 wt% in presence of graphite. X-ray diffraction studies show no important phase transformation by the incorporation of nitrogen up to 1200°C. Treatments at temperatures above 1200°C resulted in the formation of CaO or Ca(OH)₂. ³¹P NMR studies indicate no direct bonding of nitrogen and phosphorous. Infrared spectra show increasing intensities of four new bands at 3250, 2016, 1966 and 700 cm⁻¹ with increasing nitrogen contents, while the OH-bands at 3570 and 630 cm⁻¹ vanish. Taking into account results of the carbon content, XRD, NMR and IR spectra it is suggested that nitrogen enters into the structure as [CN₂]²⁻ ion, substituting [OH]⁻ groups, and forming cyanamidapatite Ca₁₀(PO₄)₆(CN₂). ©     

Investigations of BaFe0.5Nb0.5O3 nano powders prepared by a low temperature aqueous synthesis and resulting ceramics

A facile method to prepare nanoscaled BaFe_0.5Nb_0.5O₃ via synthesis in boiling NaOH solution is described herein. The nano-crystalline powder has a high specific surface area of 55 m² g⁻¹ and a crystallite size of 15 nm. The as-prepared powder does not show any significant crystallite growth up to 700 °C. The activation energy of the crystallite growth process was calculated as 590 kJ mol⁻¹. Dense ceramics can be obtained either after sintering at 1200 °C for 1 h or after two-step sintering at 1000 °C for 10 h. The average grain sizes of ceramic bodies can be tuned between 0.23 μm and 12 μm. The thermal expansion coefficient was determined as 11.4(3)·10⁻⁶ K⁻¹. The optical band gap varies between 2.90(5) and 2.63(3) eV. Magnetic measurements gave a Néel temperature of 20 K. Depending on the sintering regime, the ceramic samples reach permittivity values between 2800 and 137,000 at RT and 1 kHz.     

Fabrication and characterization of bone china using synthetic bone powder as raw materials

The synthetic bone powder was studied as a raw materials for bone china, completely replacing natural bone ash raw materials. The physical and thermal properties of samples obtained by the two bone powders were tested and comparatively studied. Performance tests included pyroplastic deformation, flexural strength, bulk density, sintering shrinkage, water absorption, transmittance, thermal expansion coefficient and the thermal shock resistance. The phase composition and morphology were investigated by X-ray diffraction (XRD) and scanning electron microscopy (SEM), respectively. The results indicated that using synthetic bone powder could shorten the preparation time, reduce the sintering temperature and result in high-quality bone china. The pyroplastic deformation decreased from 9.14% to 7.92%, the three-point flexural strength increased from 123 MPa to 191 MPa, the light transmittance (at a 2-mm thickness) increased from 6.7% to 11.2%, the thermal expansion coefficient decreased from 8.24×10⁻⁶ °C⁻¹ to 7.69×10⁻⁶ °C⁻¹, and the thermal shock resistance increased from 140 °C to 180 °C. A continuous interface layer without cracks was produced by using the synthetic bone powder.     

Correction of moisture and sucrose effective diffusivities for shrinkage during osmotic dehydration of apple in sucrose solution

Shrinkage, moisture and sucrose effective diffusivities were correlated for infinite slab shape samples of apple during osmotic dehydration in sucrose solution. Experiments were carried out in the sucrose solutions of different concentrations (30%, 40% and 50%) and temperatures (30 °C, 40 °C and 50 °C). The two parameter model, developed by Azuara et al. (1992), was used to predict water loss and solid gain at equilibrium condition. Moisture and sucrose diffusivities were estimated by fitting the experimental moisture loss and solid gain data to the modified form of Fick's second law of diffusion, considering the shrinkage of the apples during osmotic dehydration. Results showed that the volume of the samples decreased linearly with water loss (WL) and weight reduction (WR). For above conditions of osmotic dehydration, effective diffusivities without considering the shrinkage were found to be in the range of 1.36 × 10⁻¹⁰ m²/s–2.00 × 10⁻¹⁰ m²/s, and those with considering the shrinkage were in the range of 0.87 × 10⁻¹⁰ m²/s–1.27 × 10⁻¹⁰ m²/s. The values of the effective diffusivities estimated by considering the shrinkage were smaller than those without considering this phenomenon.     

The decrease of depolarization temperature and the improvement of pyroelectric properties by doping Ta in lead-free 0.94Na0.5Bi0.5TiO3-0.06BaTiO3 ceramics

Ta-doped lead-free 0.94NBT-0.06BT-xTa (x=0.0–1.0%) ceramics were synthesized by a conventional solid-state route. XRD shows that the compositions are at a morphotropic phase boundary where rhombohedral and tetragonal phases coexist. The depolarization temperature (T_d) shifted to lower temperature with the increase of Ta content. The pyroelectric coefficient (p) of doped ceramics greatly enhanced compared with undoped material and reached a maximum of 7.14×10⁻⁴ C m⁻² °C⁻¹ at room temperature (RT) and 146.1×10⁻⁴ C m⁻² °C⁻¹ at T_d at x=0.2%. The figure of merits, F_i and F_v, also showed a great improvement from 1.12×10⁻¹⁰ m v⁻¹ and 0.021 m² C⁻¹ at x=0.0 to 2.55×10⁻¹⁰ m v⁻¹ and 0.033 m² C⁻¹ at x=0.2% at RT. Furthermore, F_i and F_v show the huge improvement to 52.2×10⁻¹⁰ m v⁻¹ and 0.48×10⁻¹⁰ m v⁻¹ respectively at T_d at x=0.2%. F_C shows a value between 2.26 and 2.42 ×10⁻⁹ C cm⁻² °C⁻¹ at RT at x=0.2%. The improved pyroelectric properties make NBT-0.06BT-0.002Ta ceramics a promising infrared detector material.     

Densification and grain growth behaviour of high-purity MgO ceramics by hot-pressing

High-purity MgO ceramics with a relative density higher than 99.60% and a mean grain size of 8.1 µm were prepared by hot-pressing at 1450 °C and 35 MPa for 120 min. The MgO ceramic was 130 mm in diameter and 10 mm in height. The densification mechanism and grain growth of MgO powder during the sintering process were investigated based on the principles of general deformation and classical phenomenological kinetic theory. The threshold pressure of plastic deformation at the initial sintering stage was also analysed. The results suggest that plastic deformation is the dominant densification mechanism during the initial period and that an applied pressure of 20 MPa is sufficient for the deformation. During the final period, Mg²⁺ diffusion along the grain boundaries controls the densification process, and the grain growth activation energy at the final stage is estimated as 336.38±2.35 kJ mol⁻¹.