Experimental and statistical assessments of the mechanical strength reliability of gamma alumina catalyst supports

The mechanical strength of solid catalysts is considered an important factor in terms of ensuring the reliable performance of industrial reactors. In this work, a pelletizing method was used to form gamma alumina support for catalysts. Response surface methodology (RSM) was employed to analyze and model the effects of various manufacturing parameters on the crushing strength of the supports. These parameters were binder concentration, compaction pressure, calcination temperature, and drying mode. The suggested model was verified by applying an analysis of variance to assess its validity with regard to crushing strength. The mechanical reliability of various supports was also determined by calculating their Weibull modulus values through linear regression of the Weibull equation. The material with the highest mechanical strength reliability will have both a high mean crushing strength and a high Weibull modulus, and the best values obtained for a support in this work were 70.7 MPa and 6.63, respectively. The conditions used to form this sample were: 20 mass% binder concentration, 861 MPa compaction pressure, 466 °C calcination temperature, and gentle drying.     

Novel self assembly behavior for γ-alumina nanoparticles

In this study, self assembly behavior was induced for γ-alumina nanoparticles by adsorption of dimethyl disulfide. Following this trend, we have developed a chemical process to obtain γ-alumina in the nano scale. Scanning electron microscopy images of the prepared γ-alumina showed big and strong agglomeration of the nanoparticles indicating that these nanoparticles have strong surface forces. Transmission electron microscopy images confirmed that the γ-alumina nanoparticles 3–7 nm in size were converted to uniform spherical shape in the size range of 1–2 mm after shaking with dimethyl disulfide in the presence of n-hexane at room temperature. This phenomenon did not appear in the case of alumina in the micro scale. The surface properties of the prepared γ-alumina in the nano scale were characterized and compared with the γ-alumina in the micro scale by using low temperature nitrogen adsorption–desorption system, indicating that the specific surface area of the prepared γ-alumina nanoparticles is larger than that of the γ-alumina in the micro scale. Furthermore, micro- and meso-pores were observed for the γ-alumina nanoparticles while only mesoporous structure was detected for the γ-alumina in the micro scale. These experimental results suggested that the self assembly behavior of the γ-alumina nanoparticles may be due to the selective adsorption of dimethyl disulfide in the micropores of these nanoparticles to act as bridge linking the nanoparticles.     

Microstructure and mechanical properties of ZrO2 (Y2O3)–Al2O3 nanocomposites prepared by spark plasma sintering

Zirconia (yttria)–alumina ceramic nanocomposites were fabricated from different powders by spark plasma sintering (SPS). One powder was a commercially available nanocomposite powder TZP-3Y20A, consisting of 3 mol% yttria-stabilized zirconia (3-YSZ) reinforced with 20 wt% alumina, and the other, used as a comparison, was a conventional mechanically mixed powder 3YSZ-20A, a blend made of 3 mol% yttria-stabilized zirconia powder ZrO₂ (3Y) and 20 wt% α-alumina powder. The effect of the sintering temperature on the densification, the sintering behavior, the mechanical properties and the microstructure of the composites was investigated. The results showed that the density increased with increasing sintering temperature, and thus, the mechanical properties were strengthened because of the increased densification. The nanocomposite powder TZP-3Y20A was easily sintered, and good mechanical properties were achieved as compared with the powder from the conventional mechanically mixed method, the maximum flexural strength and fracture toughness of which were 967 MPa and 5.27 MPa m^1/2, respectively.     

Fabrication of magnetic nanosized γ-FeNi-coated ceramic core–shell microspheres by heterogeneous precipitation and thermal reduction

Precursors with NiCO₃·2Ni(OH)₂·2H₂O- and Fe₂O₃·nH₂O-coated alumina, graphite and cenosphere were synthesized by precipitation using ferrous sulfate, nickel sulfate, ammonium bicarbonate, alumina, graphite and cenosphere as the main starting materials. Magnetic γ-FeNi-coated alumina, graphite and cenosphere core–shell structural microspheres were subsequently prepared by thermal reduction of the as-prepared precursors at 600 °C for 2 h. Precipitation parameters, e.g. concentration of ceramic micropowders (10 g/L), sulfate solution (0.2 mol/L), rate of adding reactants (3 mL/min) and pH value were optimized by a trial-and-error method. Powders of the precursors and the resulting coating of γ-FeNi with grain size below 40 nm on alumina, graphite and cenosphere microspheres were characterized by scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS) and X-ray diffraction (XRD). The magnetic properties of the nanosize γ-FeNi-coated alumina, graphite and cenosphere microspheres were measured by vibrating sample magnetometer (VSM). The results show that the core–shell structural γ-FeNi-coated ceramic microspheres exhibited higher coercivity than pure γ-FeNi powders, indicating that these materials can be used for high-performance functional materials and devices.     

Green synthesis and enhanced photocatalytic activity of Ce-doped TiO2 nanoparticles supported on porous glass

A facile and green method to prepare Ce-doped TiO₂ nanoparticles supported on porous glass beads is reported. An ion exchange process and subsequent calcination yielded Ce-doped TiO₂ nanoparticles with a mean size of 4.8 ± 0.3 nm. The nanoparticles were dispersed on the surface of porous glass beads. The addition of Ce enhanced the visible light absorption of the TiO₂ nanoparticles in the 400–500 nm spectral window. The band gap of the as-prepared catalyst was 2.80 eV. The Ce-doped TiO₂ nanoparticles immobilized on porous glass beads exhibited excellent photocatalytic activity for the visible-light-degradation of methyl orange (MO) and rhodamine B (RhB); with rate constants of 0.095 and 0.230 min⁻¹; respectively. The effects of Ce dosage; reaction duration; and initial solution pH on the conversion of MO and RhB dyes were investigated. The green synthesis and favorable photocatalytic activity makes the Ce-doped TiO₂ nanoparticles immobilized on porous glass an attractive alternative for the efficient degradation of organic pollutants.     

Effect of gravity on the mechanical properties of lunar regolith tested using a low gravity simulation device

Simulations of the bearing capacity and shear strength of regolith under Earth’s gravity produce different results from those under low gravity. A low-gravity simulation device was developed in this study, and an internal stress model of regolith simulant was established to correct the errors. The model revealed additional force on both shear plane in the shear test and the press plate area in the pressure–sinkage test. The sinkage and shear test results showed that low gravity decreased the deformable index n, frictional modulus k_φ and cohesion c, whereas there were no obvious changes to the cohesive modulus k_c and internal friction angle φ. The sinkage generally increased as the gravity decreased under a consistent normal load larger than 50 N, but when the wheel load was lower than 50 N, the sinkage of the TYII-1 simulant was larger under 1 G than 1/6 G. Gravity had little effect on the shear strength of the regolith. However, the tractive thrust of the TYII-1 simulant was lower under 1/6 G than 1 G. The smaller difference was due to differences in the way the soils responded to changes in the gravity level for the TYII-2 simulant.     

Synthesis of mesoporous γ-AlOOH@Fe3O4 magnetic nanomicrospheres

Mesoporous γ-AlOOH@Fe₃O₄ magnetic nanomicrospheres were synthesized using superparamagnetic Fe₃O₄ nanoparticles as the core and aluminum isopropoxide (AIP) as the aluminum source. The obtained magnetic nanomicrospheres were characterized by X-ray powder diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), N₂ adsorption–desorption and vibrating sample magnetometry (VSM). The effects of preparation parameters such as hydrolysis time of AIP, concentration of AIP and coating layer number on microspheres were investigated. The results indicated that the mesoporous γ-AlOOH@Fe₃O₄ magnetic nanomicrospheres consisted of a mesoporous γ-AlOOH shell and a Fe₃O₄ magnetic core. The diameter of γ-AlOOH@Fe₃O₄ nanomicrospheres was about 200 nm, the thickness of mesoporous γ-AlOOH shell was about 5 nm and the average pore size was 3.8 nm. The thickness of the mesoporous γ-AlOOH shell could be controlled via layer-by-layer coating times. The formation mechanism of the mesoporous γ-AlOOH shell involved a “chemisorption–hydrolysis” process.     

Synthesis and phase evolution of LiNb0.6Ti0.5O3 powder via a sol–gel method

A simple sol–gel route was demonstrated for the synthesis of LiNb_0.6Ti_0.5O₃ (M-phase) powder, using cheap and manageable starting materials at a relatively low temperature. The phase transitions in both chemical and solid-state processes were studied by X-ray diffraction (XRD) in detail. The results showed that in the sol–gel process the anatase TiO₂ phase first appeared at 400 °C and then LiNbO₃ solid solution (LiNbO₃ ss) emerged at 500 °C. When calcined to 600 °C, the M-phase started to appear along with the decrease of TiO₂ and LiNbO₃ ss. Single M-phase could be formed at 700 °C, which is 300 °C lower than that by the traditional solid-state method. A plausible evolution mechanism of the as-synthesized powder in calcination was proposed. The produced powder has potential applications in microelectronics systems.     

Preparation of SiO2/TiO2 Janus particles by electrostatic assembly,hydrolysis and calcination

This paper describes a novel chemical method for preparing SiO₂/TiO₂ Janus particles. First, polystyrene (PSt)/SiO₂ particles with a raspberry-like structure are prepared by electrostatic assembly. The influences of the reaction time of sulfonation and the treatment times of polyelectrolyte solutions (PDADMAC, PSS) on PSt and SiO₂ are investigated with respect to the surface charge density of the particles. SiO₂/TiO₂ Janus particles are then obtained by hydrolysis of butyl titanate on the surface of PSt/SiO₂ particles followed by a calcination process. Particle size analyzer, Zeta potential instrument, FTIR, TEM and SEM are used to characterize the particle size, the amount of charge on the surface of PSt and SiO₂ particles and the compositions and morphologies of PSt/SiO₂, SiO₂/TiO₂ and PSt/SiO₂/TiO₂. The diameters of the PSt, SiO₂, PSt/SiO₂ and SiO₂/TiO₂ particles are 2.0 μm, 303 nm, 2.7 μm and 330 nm, respectively.     

Static and dynamic compaction of ceramic powders

The static and dynamic compaction of ceramic powders was investigated experimentally using a high-pressure friction-compensated press to achieve static stresses of 1.6 GPa and with a novel gas gun setup to stresses of 5.9 GPa for a tungsten carbide powder. Experiments were performed in the partial compaction region to nearly full compaction. The effects of variables including initial density, particle size distribution, particle morphology, and loading path were investigated in the static experiments. Only particle morphology was found to significantly affect the compaction response. Post-test examination of the powder reveals fracture of the grains as well as breaking at particle edges. In dynamic experiments, steady structured compaction waves traveling at very low velocities were observed. The strain rate within the compaction waves was found to scale nearly linearly with the shock stress, in contrast with many fully dense materials where strain rate scales with stress to the fourth power. Similar scaling is found for data from the literature on TiO₂ powder. The dynamic response of WC powder is found to be significantly stiffer than the static response, probably because deformation in the dynamic case is confined to the relatively narrow compaction wave front. Comparison of new static powder compaction results with shock data from the literature for SiO₂ also reveals a stiffer dynamic response.     

Solid-state synthesis of Li[Li0.2Mn0.56Ni0.16Co0.08]O2 cathode materials for lithium-ion batteries

Layered Li[Li_0.2Mn_0.56Ni_0.16Co_0.08]O₂ cathode materials were synthesized via a solid-state reaction for Li-ion batteries, in which lithium hydroxide monohydrate, manganese dioxide, nickel monoxide, and cobalt monoxide were employed as metal precursors. To uncover the relationship between the structure and electrochemical properties of the materials, synthesis conditions such as calcination temperature and time as well as quenching methods were investigated. For the synthesized Li[Li_0.2Mn_0.56Ni_0.16Co_0.08]O₂ materials, the metal components were found to be in the form of Mn⁴⁺, Ni²⁺, and Co³⁺, and their molar ratio was in good agreement with stoichiometric ratio of 0.56:0.16:0.08. Among them, the one synthesized at 800 °C for 12 h and subsequently quenched in air showed the best electrochemical performances, which had an initial discharge specific capacity and coulombic efficiency of 265.6 mAh/g and 84.0%, respectively, and when cycled at 0.5, 1, and 2 C, the corresponding discharge specific capacities were 237.3, 212.6, and 178.6 mAh/g, respectively. After recovered to 0.1 C rate, the discharge specific capacity became 259.5 mAh/g and the capacity loss was only 2.3% of the initial value at 0.1 C. This work suggests that the solid-state synthesis route is easy for preparing high performance Li[Li_0.2Mn_0.56Ni_0.16Co_0.08]O₂ cathode materials for Li-ion batteries.     

Experimental study on the compressive behaviors of CFRP tube-encased concrete columns

Nine square concrete columns including 6 CFRP/ECCs and 3 concrete columns are prepared, which have cross-section of 200 mm × 200 mm and height of 600 mm. The CFRP tubes with fibers oriented at hoop direction were manufactured to have 3 or 5 layers of CFRP with 10 mm, 20 mm, or 40 mm rounding corner radii at vertical edges. A 100 mm overlap in the direction of fibers was provided to ensure proper bond. Uniaxial compression tests were conducted to investigate the compressive behavior. It is evident that the CFRP tube confinement can improve the behavior of concrete core, in terms of axial compressive strength or axial deformability. Test results show that the stress-strain behavior of CFRP/ECCs vary with different confinement parameters, such as the number of confinement layers and the rounding corner radius.     

Hydrothermal synthesis of ultrathin hexagonal nickel hydroxide nanosheets

Nickel hydroxide, Ni(OH)₂ is widely used in electrodes of nickel-based alkaline secondary batteries. Ultrathin hexagonal Ni(OH)₂ nanosheets of space group P-3m1 were hydrothermally prepared at 200 °C for 10 h. Their diameter and thickness were 200–300 and 3–5 nm, respectively. Their formation was attributed to the oriented assembly of growing particles, which was assisted by surfactant molecules. The specific surface area of the Ni(OH)₂ nanosheets was 8.66 m²/g. Their magnetization curve exhibited linear paramagnetic behavior across the entire measurement region.     

Thermo-mechanical behaviour of TRIP 1000 steel sheets subjected to low velocity perforation by conical projectiles at different temperatures

This paper presents and analyzes the behaviour of TRIP 1000 steel sheets subjected to low velocity perforation by conical projectiles. The relevance of this material resides in the potential transformation of retained austenite to martensite during impact loading. This process leads to an increase in strength and ductility of the material. However, this transformation takes place only under certain loading conditions strongly dependent on the initial temperature and deformation rate. In order to study the material behaviour under impact loading, perforation tests have been performed using a drop weight tower. Experiments were carried out at two different initial temperatures T₀ = 213 K and T₀ = 288 K, and within the range of impact velocities 2.5 m/s ? V₀ ? 4.5 m/s. The experimental setup enabled the measuring of impact velocity, residual velocity, load-time history and failure mode. In addition, dry and lubricated contacts between the striker and the plate have been investigated. Finally, by using X-ray diffraction it has been shown that no martensitic transformation takes place during the perforation process. The causes involving the none-appearance of martensite are examined.     

Spatiotemporal variations of PM2.5 and PM10 concentrations between 31 Chinese cities and their relationships with SO2, NO2, CO and O3

The variations of mass concentrations of PM_2.5, PM₁₀, SO₂, NO₂, CO, and O₃ in 31 Chinese provincial capital cities were analyzed based on data from 286 monitoring sites obtained between March 22, 2013 and March 31, 2014. By comparing the pollutant concentrations over this length of time, the characteristics of the monthly variations of mass concentrations of air pollutants were determined. We used the Pearson correlation coefficient to establish the relationship between PM_2.5, PM₁₀, and the gas pollutants. The results revealed significant differences in the concentration levels of air pollutants and in the variations between the different cities. The Pearson correlation coefficients between PMs and NO₂ and SO₂ were either high or moderate (PM_2.5 with NO₂: r = 0.256–0.688, mean r = 0.498; PM₁₀ with NO₂: r = 0.169–0.713, mean r = 0.493; PM_2.5 with SO₂: r = 0.232–0.693, mean r = 0.449; PM₁₀ with SO₂: r = 0.131–0.669, mean r = 0.403). The correlation between PMs and CO was diverse (PM_2.5: r = 0.156–0.721, mean r = 0.437; PM₁₀: r = 0.06–0.67, mean r = 0.380). The correlation between PMs and O₃ was either weak or uncorrelated (PM_2.5: r = −0.35 to 0.089, mean r = −0.164; PM₁₀: r = −0.279 to 0.078, mean r = −0.127), except in Haikou (PM_2.5: r = 0.500; PM₁₀: r = 0.509).     

X-ray spectral measurements and collisional-radiative modeling of hot,gold plasmas at the omega laser

M-Band and L-Band Gold spectra between 3 and 5 keV and 8 and 13 keV, respectively, have been recorded by a photometrically calibrated crystal spectrometer. The spectra were emitted from the plasma in the laser deposition region of a ‘hot hohlraum’. This is a reduced-scale hohlraum heated with ≈9 kJ of 351 nm light in a 1 ns square pulse at the OMEGA laser. The space- and time-integrated spectra included L-Band line emission from Co-like to Ne-like gold. The three L-Band line features were identified to be the 3s → 2p, 3d_5/2 → 2p_3/2 and 3d_3/2 → 2p_1/2 transitions at ≈9 keV, ≈10 keV and ≈13 keV, respectively. M-Band 5f → 3d, 4d → 3p, and 4p → 3s transition features from Fe-like to P-like gold were also recorded between 3 and 5 keV. Modeling from the radiation–hydrodynamics code LASNEX, the collisional-radiative codes FLYCHK and SCRAM, and the atomic structure code FAC were used to model the plasma and generate simulated spectra for comparison with the recorded spectra. Through these comparisons, we have determined the average electron temperature of the emitting plasma to be between 6.0 and 6.5 keV. The electron temperatures predicted by LASNEX appear to be too large by a factor of about 1.5.     

The influence of temperature on limestone sulfation and attrition under fluidized bed combustion conditions

The influence of temperature on attrition of two limestones during desulfurization in a fluidized bed reactor was investigated. Differences in the microstructure of the two limestones were reflected by a different thickness of the sulfate shell formed upon sulfation and by a different value of the ultimate calcium conversion degree. Particle attrition and fragmentation were fairly small under moderately bubbling fluidization conditions for both limestones. An increase of temperature from 850 °C to 900 °C led to an increase of the attrition rate, most likely because of a particle weakening effect caused by a faster CO₂ evolution during calcination. This weakening effect, however, was not sufficiently strong to enhance particle fragmentation in the bed. The progress of sulfation, associated to the build-up of a hard sulfate shell around the particles, led in any case to a decrease of the extent of attrition. Sulfation at 900 °C was less effective than at 850 °C, and this was shown to be related to the porosimetric features of the different samples.     

Microwave-assisted polyol synthesis of LiMnPO4/C and its use as a cathode material in lithium-ion batteries

We synthesized LiMnPO₄/C with an ordered olivine structure by using a microwave-assisted polyol process in 2:15 (v/v) water–diethylene glycol mixed solvents at 130 °C for 30 min. We also studied how three surfactants—hexadecyltrimethylammonium bromide, polyvinylpyrrolidone k30 (PVPk30), and polyvinylpyrrolidone k90 (PVPk90)—affected the structure, morphology, and performance of the prepared samples, characterizing them by using X-ray diffraction, scanning electron microscopy, transmission electron microscopy, charge/discharge tests, and electrochemical impedance spectroscopy. All the samples prepared with or without surfactant had orthorhombic structures with the Pnmb space group. Surfactant molecules may have acted as crystal-face inhibitors to adjust the oriented growth, morphology, and particle size of LiMnPO₄. The microwave effects could accelerate the reaction and nucleation rates of LiMnPO₄ at a lower reaction temperature. The LiMnPO₄/C sample prepared with PVPk30 exhibited a flaky structure coated with a carbon layer (∼2 nm thick), and it delivered a discharge capacity of 126 mAh/g with a capacity retention ratio of ∼99.9% after 50 cycles at 1C. Even at 5C, this sample still had a high discharge capacity of 110 mAh/g, demonstrating good rate performance and cycle performance. The improved performance of LiMnPO₄ likely came from its nanoflake structure and the thin carbon layer coating its LiMnPO₄ particles. Compared with the conventional polyol method, the microwave-assisted polyol method had a much lower reaction time.     

Emission of organic carbon,elemental carbon and water-soluble ions from crop straw burning under flaming and smoldering conditions

Emissions from major agricultural residues were measured using a self-designed combustion system. Emission factors (EFs) of organic carbon (OC), elemental carbon (EC), and water-soluble ions (WSIs) (K⁺, NH₄⁺, Na⁺, Mg²⁺, Ca²⁺, Cl⁻, NO₃⁻, SO₄^2–) in smoke from wheat and rice straw were measured under flaming and smoldering conditions. The OC₁/TC (total carbon) was highest (45.8% flaming, 57.7% smoldering) among carbon fractions. The mean EFs for OC (EF_OC) and EC (EF_EC) were 9.2 ± 3.9 and 2.2 ± 0.7 g/kg for wheat straw and 6.4 ± 1.9 and 1.1 ± 0.3 g/kg for rice straw under flaming conditions, while they were 40.8 ± 5.6 and 5.8 ± 1.0 g/kg and 37.6 ± 6.3 and 5.0 ± 1.4 g/kg under smoldering conditions, respectively. Higher EC ratios were observed in particulate matter (PM) mass under flaming conditions. The OC and EC for the two combustion patterns were significantly correlated (p < 0.01, R = 0.95 for wheat straw; p < 0.01, R = 0.97 for rice straw), and a higher positive correlation between OC₃ and EC was observed under both combustion conditions. WSIs emitted from flaming smoke were dominated by Cl⁻ and K⁺, which contributed 3.4% and 2.4% of the PM mass for rice straw and 2.2% and 1.0% for wheat straw, respectively. The EFs of Cl⁻ and K⁺ were 0.73 ± 0.16 and 0.51 ± 0.14 g/kg for wheat straw and 0.25 ± 0.15 and 0.12 ± 0.05 g/kg for rice straw under flaming conditions, while they were 0.42 ± 0.28 and 0.12 ± 0.06 g/kg and 0.30 ± 0.27 and 0.05 ± 0.03 g/kg under smoldering conditions, respectively. Na⁺, Mg²⁺, and NH₄⁺ were vital components in PM, comprising from 0.8% (smoldering) to 3.1% (flaming) of the mass. Strong correlations of Cl⁻ with K⁺, NH₄⁺, and Na⁺ ions were observed in rice straw and the calculated diagnostic ratios of OC/EC, K⁺/Na⁺ and Cl⁻/Na⁺ could be useful to distinguishing crop straw burning from other sources of atmospheric pollution.     

Preparation of calcium sulfate whiskers from FGD gypsum via hydrothermal crystallization in the H2SO4–NaCl–H2O system

Little attention has thus far been paid to the potential effect of solution composition on the hydrothermal crystallization of calcium sulfate whiskers prepared from flue-gas desulfurization (FGD) gypsum. When purified FGD gypsum was used as raw material, the morphology and phase structure of the hydrothermal products grown in pure water, H₂SO₄–H₂O, NaCl–H₂O, and H₂SO₄–NaCl–H₂O solutions as well as the solubility of purified FGD gypsum in these solutions were investigated. The results indicate that calcium sulfate whiskers grow favorably in the H₂SO₄–NaCl–H₂O system. When prepared using 10–70 g NaCl/kg gypsum −0.01 M H₂SO₄–H₂O at 130 °C for 60 min, the obtained calcium sulfate whiskers had diameters ranging from 3 to 5 μm and lengths from 200 to 600 μm, and their phase structure was calcium sulfate hemihydrate (HH). Opposing effects of sulfuric acid and sodium chloride on the solubility of the purified FGD gypsum were observed. With the co-presence of sulfuric acid and sodium chloride in the reaction solution, the concentrations of Ca²⁺ and SO₄²⁻ can be kept relatively stable, which implies that the crystallization of the hydrothermal products can be controlled by changing the concentrations of sulfuric acid and sodium chloride.