Low-firing of BiSbO4 microwave dielectric ceramic with V2O5–CuO addition

Effects of 1.0 wt.% V₂O₅–CuO mixture addition on the sintering behavior, phase composition and microwave dielectric properties of BiSbO₄ ceramics have been investigated. BiSbO₄ ceramics can be well densified below temperature about 930 °C with 1.0 wt.% V₂O₅–CuO mixtures addition with different ratios of CuO to V₂O₅. The formation of BiVO₄ phase and substitution of Cu²⁺ can explain the decrease of sintering temperature. Dense BiSbO₄ ceramics sintered at 930 °C for 2 h exhibited good microwave dielectric properties with permittivity between 19 and 20.5, Qf values between 19,000 and 40,000 GHz and temperature coefficient of resonant frequency shifting between ?71.5 ppm °C^?1 and ?77.8 ppm °C^?1. BiSbO₄ ceramics could be a candidate for microwave application and low temperature co-fired ceramics technology.     

The rock salt oxide Li2MgTiO4: Type I dielectric and ionic conductor

The exploration of the Li–Ti–Mg–O system, using both sol–gel technique and solid state reaction method, allowed a new phase, Li₂MgTiO₄, with disordered rock salt structure (a = 4.159 Å) to be synthesized. The latter is shown to be a good type I dielectric material, with a relative constant of 15 at high frequency and low dielectric loss (tanδ < 10⁻³) over the temperature range −60 to 160 °C. It is also observed that the sintering temperature of this phase is strongly lowered by adopting the sol–gel technique compared to solid state reaction (1150 °C instead of 1300 °C). Finally we show that this phase exhibits cationic conductivity above 400 °C (σ_600 °C = 9 × 10⁻⁵ S cm⁻¹).     

Hot top design and its influence on feeder channel segregates in 100-ton steel ingots

The influence of hot top design on feeder channel segregates (F-CS) and centerline shrinkage porosities (C-SP) were investigated both experimentally and numerically. Two 100-ton 30Cr2Ni4MoV steel ingots with different insulating hot tops were longitudinally sectioned. The experimental results showed few channel segregates but severe shrinkage porosities appeared in the ingot with poorly insulated hot top, while it was the opposite case after the improved hot topping practice. By employing the finite element numerical simulation, the critical condition for the formation of F-CS in 30Cr2Ni4MoV steel was verified to be R^2.1G ≤ 1.0 × 10^− 5 °C mm^1.1 s^− 2.1. Through coupling with the published C-SP criterion (GR^− 0.5 ≤ 2.5 °C mm^− 1.5 s^0.5), it was found out that the increase of hot-top height and preheating temperature would aggravate F-CS while alleviate C-SP contrarily. Hence, to comprehensively control those two defects, the optimum hot-top height and preheating temperature for 100-ton ingot were suggested to be 700 mm and 600 °C, respectively. Ultimately, the ratio of the solidification time for the whole ingot to the ingot body (t_f/t_b) was proposed as a novel criterion for hot top design. This practical criterion has been successfully utilized to optimize the hot top of a 5-ton steel ingot.     

Rapid carbothermal synthesis of nanostructured silicon carbide particles and whiskers from rice husk by microwave heating method

This paper reported a simple and rapid route to large-scale synthesis of nanostructured SiC powders using rice husk as the precursor. Rapid carbothermal reduction reactions were achieved in a 2.45 GHz microwave field in an argon atmosphere. The XRD patterns revealed that complete carbothermal reduction of silica was achieved at 1300 °C for 60 min or at 1500 °C for only 15 min by microwave heating, resulting in β-SiC formation. The FE-SEM images showed that the β-SiC powders were mixtures of particles and whiskers. The β-SiC particles had diameters of 60–130 nm and the β-SiC whiskers, which were several to tens of micrometers in length, had diameters of 110–170 nm. The β-SiC powder synthesized at 1500 °C for 15 min showed the highest BET surface area of 12.2 m²/g. Compared to the conventional heating method, the microwave heating method proved to be an efficient approach for synthesis of SiC in terms of energy and time saving, as well as for fabrication of nanostructured SiC.     

Effect of V2O5 additive to 0.4SrTiO3–0.6La(Mg0.5Ti0.5)O3 ceramics on sintering behavior and microwave dielectric properties

The effect of V₂O₅ addition on the microwave dielectric properties and the microstructures of 0.4SrTiO₃–0.6La(Mg_0.5Ti_0.5)O₃ ceramics sintered for 5 h at different sintering temperature were investigated systematically. It was found that the sintering temperature was effectively lowered about 200 °C by increasing V₂O₅ addition content. The grain sizes, bulk density as well as microwave dielectric properties were greatly dependent on sintering temperature and V₂O₅ content. The 4ST–6LMT ceramics with 0.25% V₂O₅ sintered at 1400 °C for 5 h in air exhibited optimum microwave dielectric properties of ɛ_r = 50.7, Q × f = 15049.6 GHz, T_f = −1.7 ppm/°C.     

Effect of sintering temperature on properties of Al2O3 whisker reinforced 3 mol% Y2O3 stabilized tetragonal ZrO2 (TZ-3Y) nanocomposites

In present study, effect of sintering temperature on density and hardness of 3 mol% yttria-stabilized tetragonal zirconia (referred to as TZ-3Y) composite reinforced with alumina whiskers (5, 10, 15 and 20 wt.%) has been studied. Initially, Ammonium Aluminum Carbonate Hydroxide (AACH) whiskers were added in TZ-3Y composite and transformed into alumina during sintering performed at different temperatures i.e. 1400, 1500 and 1650 °C. Results revealed that for all sintering temperatures, with increase in whisker concentration, sintered density decreased and hardness increased conversely. Maximum hardness of 14.47 GPa was achieved with 10 wt.% whiskers addition when sintered at 1500 °C. However, with addition of CTAB (1 wt.%) as deflocculating agent the hardness was further improved to 15.11 GPa. While sintering at 1650 °C a decrease in hardness was observed. It was mainly due to high temperature morphological change of whiskers i.e. transformation of whiskers into alumina rich grains.     

Friction and wear behaviors of B4C/6061Al composite

The friction and wear behaviors of B₄C/6061Al composite were studied by considering the effect of sliding time, applied load, sliding velocity and heat treatment. The results show that, when the sliding time, applied load and sliding velocity reach critical values (namely 120 min, 30 N and 240 r min⁻¹, respectively), the mass loss and friction coefficient (COF) increase significantly. Severe delamination wear is the main wear mechanism after sliding for 120 min and under an applied load of 30 N. While fretting wear happens at a sliding velocity of 240 r min⁻¹. After solution-treated at 550 °C for 1 h and then aged at 180 °C for 15 h, the composite shows the highest wear resistance owing to the precipitation of β″ (Mg₂Si) phases in the matrix and the strong interface bonding between B₄C particles and the matrix alloy.     

Constitutive modeling of alumina sintering: grain-size effect on dominant densification mechanism

In the present work, alumina powders with the initial grain sizes of 0.9 and 7.0 μm, respectively, were sintered at different temperatures. Constitutive laws for densification were employed to model the sintering process of alumina ceramics. Based on the constitutive laws employed and the experimental results obtained, the dominant densification mechanism was identified and the effect of grain size on dominant densification mechanism was discussed. The activation energy for densification was also evaluated. In the investigated sintering temperature range, interface reaction was identified as the controlling process in sintering of alumina powders with the initial grain size of 0.9 μm, while grain-boundary diffusion was identified as the dominant process in sintering of alumina powders with the initial grain size of 7.0 μm. The activation energies for densification of the finer and coarser grain size alumina ceramics were determined as 342 and 384 kJ mol⁻¹, respectively, which provided a strong support on the densification mechanism investigation.     

Surface phenomena during the early stages of sintering in steels modified with Fe–Mn–Si–C master alloys

The characteristics of the metallic powder surface play a critical role in the development of strong bonds between particles during sintering, especially when introducing elements with a high affinity for oxygen. In this study, Mn and Si have been combined in a Fe–Mn–Si–C master alloy powder in order to reduce their chemical activity and prevent oxidation during the heating stage of the sintering process. However, when this master alloy powder is mixed with an iron base powder, differences in chemical activity between both components can lead to an oxygen transfer from the iron base powder to the surface of the master alloy particles. The present research is focused on studying the evolution of the master alloy particle surface during the early stages of sintering. Surface characterization by X-ray Photoelectron Spectroscopy (XPS) shows that the master alloy powder surface is mostly covered by a thin easily reducible iron oxide layer (~ 1 nm). Mn–Si particulate oxides are found as inclusions in specific areas of the surface. Evolution of oxides during sintering was studied on green compacts containing iron powder, graphite and Fe–Mn–Si–C master alloy powder that were heat treated in vacuum (10^− 6 mbar) at different temperatures (from 400, 600, 800 to 1000 °C) and analyzed by means of XPS. Vacuum sintering provides the necessary conditions to remove manganese and silicon oxides from the powder surface in the range of temperatures between 600 °C and 1000 °C. When sintering in vacuum, since the gaseous products from reduction processes are continuously eliminated, oxidation of master alloy particles due to oxygen transfer through the atmosphere is minimized.     

Structural and optical properties of chlorinated plasma polymers

Amorphous hydrogenated chlorinated carbon (a-C:H:Cl) films were produced by the plasma polymerization of chloroform–acetylene–argon mixtures in a radiofrequency plasma enhanced chemical vapor deposition system. The main parameter of interest was the proportion of chloroform in the feed, R_C, which was varied from 0 to 80%. Deposition rates of 80 nm min^? 1 were typical for the chlorinated films. Infrared reflection–absorption spectroscopy revealed the presence of C–Cl groups in all the films produced with chloroform in the feed. X-ray photoelectron spectroscopy confirmed this finding, and revealed a saturation of the chlorine content at ~ 47 at.% for R_C ≥ 40%. The refractive index and optical gap, E₀₄, of the films were roughly in the 1.6 to 1.7, and the 2.8 to 3.7 eV range. These values were calculated from transmission ultraviolet–visible-near infrared spectra. Chlorination leads to an increase in the water surface contact angle from ~ 40° to ~ 77°.     

Enhanced properties of alumina–aluminium titanate composites obtained by spark plasma reaction-sintering of slip cast green bodies

Full dense alumina + 40 vol.% aluminium titanate composites were obtained by colloidal filtration and fast reaction-sintering of alumina/titania green bodies by spark plasma sintering at low temperatures (1250–1400 °C). The composites obtained had near-to-theoretical density (>99%) with a bimodal grain size distribution. Phase development analysis demonstrated that aluminium titanate has already formed at 1300 °C. The mechanical properties such as Vickers hardness, flexural strength and fracture toughness of bulk composites are significantly higher than those reported elsewhere, e.g. the composite sintered at 1350 °C show values of about 24 GPa, 424 MPa and 5.4 MPa m^1/2, respectively. The improved mechanical properties of these composites are attributed to the enhanced densification and the finer and more uniform nanostructure achieved by non-conventional fast sintering of slip-cast dense green compacts.     

Structural,optical, thermal,photoconductivity, laser damage threshold and fluorescence analysis of an organic material: β-P-amino benzoic acid single crystal

β-P-amino benzoic acid, an organic single crystal was grown by slow evaporation technique. Single crystal X-ray diffraction studies show that the grown crystal has β-polymorph of P-amino benzoic acid [β-PABA] form and the lattice parameters are a = 6.30 Å, b = 8.61 Å, c = 12.43 Å α = γ = 90° and β = 100.20°. FTIR analysis confirms that bands at 1588 cm⁻¹, 1415 cm⁻¹ are assigned to ring skeletal vibrations of title compound. The molecular structure of the grown crystal has been identified by Nuclear Magnetic Resonance spectral study. The optical absorbance spectrum from 200 to 1100 nm shows that there is an edge absorbance in UV region. Optical band gap of the crystal has been assessed from the absorbance spectrum. The thermal properties of crystals were evaluated from TG-DTA analysis, it exhibits that there is no weight loss up to 187 °C. Laser damage threshold indicates that the grown crystal has no surface damage up to 35 mJ. Photoconductivity and fluorescence spectral experiments are also carried out and the results are discussed.     

Sol–gel derived solid chiral materials and their optical activity

The chiral organic molecules glucose (C₆H₁₂O₆) and griseofulvin (C₁₇H₁₇ClO₆) were first uniformly incorporated in sol–gel derived materials. The polarity response, absorption spectra and thermal stability were measured and discussed. The DTA results indicated that the C₆H₁₂O₆ and C₁₇H₁₇ClO₆ in gels were stable in air at the temperature lower than 210 and 350 °C, respectively. An absorption band at about 1.4 μm due to OH⁻ existed in the infrared absorption spectra of the gels. The similar behaviors of optical activity for the organic chiral molecules in solutions were hold in solid gels. The specific rotations for C₆H₁₂O₆ and C₁₇H₁₇ClO₆ in gels were −0.95 and −1.45°/cm, corresponding to the chiral parameter 1.55 × 10⁻⁷ and 2.37 × 10⁻⁷, respectively.     

Preparation,phase structure and microwave dielectric properties of CoLi2/3Ti4/3O4 ceramic

A new low loss microwave dielectric ceramic with composition of CoLi_2/3Ti_4/3O₄ was prepared by a conventional solid-state reaction method. The compound has a cubic spinel structure [Fd-3m (227)] similar to MgFe₂O₄ with lattice parameters of a = 8.3939 Å, V = 591.42 Å³, Z = 8 and ρ = 4.30 g/cm³. This ceramic has a low sintering temperature (～1050 °C) and good microwave dielectric properties with relative permittivity of 21.4, Q × f value of 35,000 GHz and τ_f value of ?22 ppm/°C. Furthermore, the addition of BaCu(B₂O₅) (BCB) can effectively lower the sintering temperature from 1050 °C to 900 °C and does not induce much degradation of the microwave dielectric properties. Compatibility with Ag electrode indicates that the BCB added CoLi_2/3Ti_4/3O₄ ceramics are good candidates for LTCC applications.     

A new and clean method on synthesis of gold nanoparticles from bulk gold substrates

In this work, we report a new pathway to prepare clean gold nanoparticles in neutral solutions with aid of natural chitosan. First, an Au substrate was cycled in a deoxygenated aqueous solution containing 0.1N NaCl and 1 g L^?1 chitosan from ?0.28 to +1.22 V vs. Ag/AgCl at 500 mV s^?1 for 200 scans. The durations at the cathodic and anodic vertices are 10 and 5 s, respectively. After this process, positively charged Au- and chitosan-containing complexes were produced in the solution. Then the solution was heated from room temperature to boiling at a heating rate of 6 °C min^?1 to prepare Au nanoparticles. The particle sizes of prepared Au (1 1 1) nanoparticles are ca. 10 nm. Moreover, the prepared Au nanoparticles in solutions are capable for anti-oxidation and stable in an ambient atmosphere for at least three months.     

Enhanced photoactivity and anatase thermal stability of silica–alumina mixed oxide additives on sol–gel nanocrystalline titania

Nanocrystalline titania with silica and silica–alumina mixed oxide as additives has been prepared through a sequential approach sol–gel method starting from titanyl sulphate in aqueous medium. The mixed oxide added titania shows increased anatase phase stability and high surface area. The complete transformation of anatase to rutile in the mixed oxide added titania occurs only above 1100 °C. The silica and silica–alumina added titania precursor even after calcination at 800 °C show specific surface area of 53 m² g^− 1 and 63 m² g^− 1 respectively. Further, the mixed oxide added titania sample shows excellent photoactivity compared to the commercially available Hombikat UV 100 titania, with respect to degradation of methylene blue. The addition of mixed oxide has resulted in better properties with respect to specific surface area, increased anatase to rutile phase transformation and photocatalytic activity of titania.     

Dilatometry of attrition milled nanocrystalline titanium powders

The sintering behavior of nanosized titanium powders was investigated by dilatometry. The nanosized Ti powders (40 nm) were produced by the attrition milling of micron sized Ti powders (12 μm) in Ar atmosphere. Sintering was carried out in Ar atmosphere in the temperature range of 450–1250 °C for nanosized Ti and 650–1250 °C for micron sized Ti by heating at 10 °C/min, up to the sintering temperature followed by isothermal holding for 1 h. The nanosized Ti powders exhibited a lower sintering onset temperature, larger shrinkage, larger shrinkage rate, and lower activation energy for sintering as compared to the micron sized Ti powders. The sintered micron sized Ti specimens exhibited both intraagglomerate and interagglomerate porosity while the nanosized Ti specimens exhibited well densified agglomerates (almost no interagglomerate porosity) and large intraagglomerate porosity. In nanosized Ti grain growth was found to take place beyond 700 °C and reached a maximum of 66 nm in samples sintered at 1100 °C.     

Characterization of hot compression behavior of a new HIPed nickel-based P/M superalloy using processing maps

Isothermal forging was a critical step process to fabricate the high-performance nickel-based superalloy. The temperature and strain rate served the most critical role in determining its microstructure and mechanical properties. In this article, we employed the hot compression to simulate the isothermal forging process upon the temperature ranging from 1000 °C to 1100 °C in combination with a strain rate of 0.001–1.0 s^− 1 for a new P/M nickel-based alloy. The activation energy was determined as 903.58 kJ/mol and the processing maps at a strain range of 0.4–0.7 were developed. The instability domains were more inclined to occur at strain rates higher than 0.1 s^− 1 and manifested in the form of adiabatic shear bands. The map further demonstrated that the regions with peak efficiency of 55% were located at 1080 °C/0.0015 s^− 1 and 1095 °C/0.014 s^− 1, respectively. Obvious dynamic recrystallization could be detected at the strain rate 0.01 s^− 1 leading to a significant flow stress drop and the grain growth was remarkably triggered under 1100 °C. The findings can shed light on the forging processing optimization of the new nickel-based superalloy.     

Temperature effects on the time dependent viscoelastic behaviour of carbon/epoxy composite materials: Application to T700GC/M21

In this study, strain rate and low temperature dependencies of the viscoelastic behaviour of the T700GC/M21 composite material are characterised and analysed. Dynamic tests for various environmental temperatures are performed on hydraulic jack equipped with an environmental chamber. Three speeds, between 8.33 · 10⁻⁴ m s⁻¹ and 0.5 m s⁻¹, at three temperatures (20 °C, −40 °C and −100 °C) are tested. The increase of the shear modulus with the decrease of the temperature is more pronounced between −40 °C and −100 °C than between 20 °C and −40 °C. Complementary DMA (Dynamic Mechanical Analysis) tests are performed on the M21 epoxy resin to characterise the viscoelastic behaviour of the matrix which contributes to the viscoelastic behaviour of the laminate. DMA tests highlight a low temperature transition called β transition (−67 °C for the 1 Hz test) which is responsible of the larger increase of the storage modulus, for the epoxy matrix, between −40 °C and −100 °C. Consequently the β transition could also be at the origin, for the composite, of the observed larger increase of the shear modulus with respect to the strain rate, for strain rates higher than 10 s⁻¹.     

Synthesis and characterization of nanocrystalline ferroelectric Sr0.8Bi2.2Ta2O9 by conventional and microwave sintering: A comparative study

In recent years mechanical activation technique has been utilized to synthesize the nanocrystalline form of compounds resulting in enhancement in the properties. Also, microwave sintering is being preferred over conventional sintering due to rapid processing and uniform temperature distribution throughout the specimen. In the present work, nanocrystalline non-stoichiometric strontium bismuth tantalate (SBT) of the composition Sr_0.8Bi_2.2Ta₂O₉ ferroelectric ceramics were synthesized by microwave sintering process (with sintering temperatures of 1000 °C and 1100 °C) and conventional solid state reaction process (with sintering temperature of 1100 °C) with an objective of comparing the properties of the synthesized specimens by the two processes. X-ray diffraction analysis shows the formation of single phase layered perovskite structure formation by both the processes. Scanning electron microscopy reveals the formation of a finer granular microstructure in the specimen synthesized by microwave sintering compared to that in the specimen prepared by conventional sintering. The specimen prepared by microwave sintering process exhibits improved electrical properties with higher dielectric constant, higher piezoelectric and pyroelectric coefficients and lower dielectric loss.