Lightweight geopolymer made of highly porous siliceous materials with various Na2O/Al2O3 and SiO2/Al2O3 ratios

The syntheses of lightweight geopolymeric materials from highly porous siliceous materials viz. diatomaceous earth (DE) and rice husk ash (RHA) with high starting SiO₂/Al₂O₃ ratios of 13.0-33.5 and Na₂O/Al₂O₃ ratios of 0.66-3.0 were studied. The effects of fineness and calcination temperature of DE, concentrations of NaOH and KOH, DE to RHA ratio; curing temperature and time on the mechanical properties and microstructures of the geopolymer pastes were investigated. The results indicated that the optimum calcination temperature of DE was 800 °C. Increasing fineness of DE and starting Na₂O/Al₂O₃ ratio resulted in an increase in compressive strength of geopolymer paste. Geopolymer pastes activated with NaOH gave higher compressive strengths than those with KOH. The optimum curing temperature and time were 75 °C and 5 days. The lightweight geopolymer material with mean bulk density of 0.88 g/cm³ and compressive strength of 15 kg/cm² was obtained. Incorporation of 40% RHA to increase starting SiO₂/Al₂O₃ and Na₂O/Al₂O₃ ratios to 22.5 and 1.7 and enhanced the compressive strength of geopolymer paste to 24 kg/cm² with only a marginal increase of bulk density to 1.01 g/cm³. However, the geopolymer materials with high Na₂O/Al₂O₃ (>1.5) were not stable in water submersion.     

Influence of flue gas SO2 on the toxicity of heavy metals in municipal solid waste incinerator fly ash after accelerated carbonation stabilization

The influence of CO₂ content and SO₂ presence on the leaching toxicity of heavy metals in municipal solid waste incinerator (MSWI) fly ash was studied by examining the carbonation reaction of MSWI fly ash with different combinations of simulated incineration flue gases. Compared with raw ash, the leaching solution pH of carbonated ash decreased by almost 1 unit and the leaching concentrations of heavy metals were generally lower, with that of Pb decreasing from 19.45 mg/L (raw ash) to 4.08 mg/L (1# carbonated ash). The presence of SO₂ in the incineration flue gas increased the leaching concentrations of heavy metals from the fly ash to different extents after the carbonation stabilization reaction. The pH of the leaching solution was the main factor influencing the leaching concentrations of heavy metals. The increase in buffer capacity with the pH of carbonated ash caused an increase in heavy metal stability after the carbonation reaction. Accelerated carbonation stabilization of MSWI fly ash could reduce its long-term leaching concentrations (toxicity) of Cu, Pb, Se, and Zn. The leaching concentrations of heavy metals from carbonated ash also likely had better long-term stability than those from raw ash. The presence of SO₂ in the incineration flue gas increased the proportion of exchangeable state species of heavy metals; slightly increased the long-term leaching toxicity of Cu, Pb, Se, and Zn; and reduced the long-term stability of these metals in the fly ash after the carbonation reaction.     

Mechanical properties and microstructure of Al2O3/TiAl in situ composites doped with Cr2O3

Al₂O₃/TiAl composites were successfully fabricated from powder mixtures of Ti, Al, TiO₂ and Cr₂O₃ by a hot-press-assisted exothermic dispersion method. The effect of the Cr₂O₃ addition on the microstructures and mechanical properties of Al₂O₃/TiAl composites was characterized, and the results showed that the Rockwell hardness, flexural strength and fracture toughness of the composites increased as the Cr₂O₃ content increased. When the Cr₂O₃ content was 2.5 wt%, the flexural strength and the fracture toughness attained peak values of 925 MPa and 8.55 MPa m^1/2, respectively. This improvement of mechanical properties was due to the more homogeneous and finer microstructure developed from the addition of Cr₂O₃ and an increase in the ratio of α₂-Ti₃Al to γ-TiAl matrix phases.     

Tensile strength and microstructure of Al2O3-ZrO2 hypo-eutectic fibers

Al₂O₃-ZrO₂(Y₂O₃) eutectic materials possess good fracture strengths and creep resistance. Increased Al₂O₃ content is one means to further improve creep resistance. The objective of this study is to examine fracture strength of Al₂O₃-rich (hypoeutectic) compositions at varying Y₂O₃ contents. Fibers 160-220 μm in diameter with 68 m/o Al₂O₃ and 1.1-7.6 m/o Y₂O₃ (30.5 to 16 m/o ZrO₂) were directionally solidified at 0.11 mm/s using the laser-heated float-zone process. Defect populations increased in size and severity with higher Y₂O₃ contents. However, fibers maintained 1 GPa fracture strength in the presence of numerous pores and shrinkage cavities, which extend with crack-like morphology along the fiber axis.     

Observation of broadband infrared luminescence in a novel Bi-doped P2O5-B2O3-Al2O3 glass

A novel Bi-doped P₂O₅-B₂O₃-Al₂O₃ glass was investigated, and strong broadband NIR (near infrared) luminescence was observed when the sample was excited by 445 nm, 532 nm, 808 nm and 980 nm lasers, respectively. The max FWHM with 312 nm, the lifetime with 580 μs and the σ_emτ product with 5.3 × 10^− 24 cm² s were obtained which indicates that this glass is a promising material for broadband optical amplifier and tunable laser. The effect of the introduction of B₂O₃ on the glass structure and Bi-ions illuminant mechanism were discussed and analyzed. It is suggested that the introduction of B₂O₃ makes the glass structure closer, and the broadband NIR emission derives from Bi⁰:²D_3/2 → ⁴S_3/2 and Bi⁺:³P₁ → ³P₀ transitions.     

Optical properties of transparent Dy doped Ba2TiSi2O8 glass ceramic

The Ba₂TiSi₂O₈ is a well known piezoelectric, ferroelectric and non-linear crystal. Nanocrystals of Ba₂TiSi₂O₈ doped with 1.5 Dy³⁺ have been obtained by thermal treatment of a precursor glass and their optical properties have been studied. X-ray diffraction patterns and optical measurements have been carried out on the precursor glass and glass ceramic samples. The emission spectra corresponding to the Dy³⁺: ⁴F_9/2 → ⁶H_13/2 (575 nm), ⁴F_9/2 → ⁶H_11/2 (670 nm) and ⁴F_9/2 → ⁶H_9/2 (757 nm) transitions have been obtained under laser excitation at 473 nm. These measurements confirm the incorporation of the Dy³⁺ ions into the Ba₂TiSi₂O₈ nanocrystals which produces an enhancement of luminescence at 575 nm. At this wavelength has been demonstrated a maximum optical amplification around 1.9 cm⁻¹ (∼8.2 dB/cm).     

Preparation and properties of nano-SiC strengthening Al2O3 composite ceramics

The processing and mechanical behaviors of Al₂O₃-xwt.%SiC (x = 1, 2, 5, ASx) nano-composites prepared by the in situ synthesis of SiC from polycarbosilane (PCS) were investigated. The composites were densified by hot pressing. The microstructure and mechanical properties of the sintered composites were analyzed. The results showed that a fully dense structure was obtained when a few nano-SiC were doped and that the fracture toughness and strength were highly improved compared with those of monolithic Al₂O₃. The fracture toughness reached 5.1 MPa m^1/2 in AS2 composite. The maximum flexural strength was 516 MPa obtained in AS1 composite.     

Fabrication of nanostructure Al2O3/ZrO2 (Y2O3) eutectic by combustion synthesis melt-casting under ultra-high gravity

A novel method for preparing Al₂O₃/ZrO₂ (Y₂O₃) eutectic was developed by combining combustion synthesis with melt-casting under ultra-high gravity (CSMC-UHG). The application of UHG = 800 g resulted in a high relative density of 99.8%, and an orientation-growth along the UHG direction. The microstructure was composed of aligned growth regimes containing a triangular dispersion of orderly ZrO₂ rods in Al₂O₃ matrix with a spacing of 300 nm. The eutectic had a high fracture toughness up to 17.9 MPa·m^1/2, which was mainly attributed to the nanostructure and the elastic bridge effects of the aligned ZrO₂ rods.     

Combined spectroscopic ellipsometry and attenuated total reflection analyses of Al2O3/HfO2 nanolaminates

The microstructure of thin HfO₂-Al₂O₃ nanolaminate high κ dielectric stacks grown by atomic vapor deposition has been studied by attenuated total reflection spectroscopy (ATR) and 8 eV spectroscopic ellipsometry (SE). The presence of Al₂O₃ below HfO₂ prevents the crystallisation of HfO₂ if an appropriate thickness is used, which depends on the HfO₂ thickness. A thicker Al₂O₃ is required for thicker HfO₂ layers. If crystallisation does occur, we show that the HfO₂ signature in both ATR and 8 eV SE spectra allows the detection of monoclinic crystallites embedded in an amorphous phase.     

Effects of ZnNb2O6 addition on BaTiO3 ceramics for energy storage

BaTiO₃ ceramics were prepared using solid state reaction with addition of ZnNb₂O₆, to investigate the effects of ZnNb₂O₆ addition on structure and properties. The results show that the ZnNb₂O₆ addition lowers sintering temperature, decreases grain size, while introduces second phase (Ba₂Ti₅O₁₂) for x ≥ 7.26 wt%. The dielectric breakdown strength is enhanced with the increasing doping level of ZnNb₂O₆ and reaches a maximum value at x = 7.26 wt%, exhibiting a maximum energy storage capability.     

White light generation in Al2O3:Ce:Tb:Mn films deposited by ultrasonic spray pyrolysis

Aluminium oxide (Al₂O₃) films doped with CeCl₃, TbCl₃ and MnCl₂ were deposited at 300 °C with the ultrasonic spray pyrolysis technique. The films were analysed using the X-ray diffraction technique and they exhibited a very broad band without any indication of crystallinity, typical of amorphous materials. Sensitization of Tb³⁺ and Mn²⁺ ions by Ce³⁺ ions gives rise to blue, green and red simultaneous emission when the film activated by such ions is excited with UV radiation. The overall efficiency of such energy transfer results to be about 85% upon excitation at 312 nm. Energy transfer from Ce³⁺ to Tb³⁺ ions through an electric dipole-quadrupole interaction mechanism appears to be more probable than the electric dipole-dipole one. A strong white light emission for the Al₂O₃:Ce³⁺(1.3 at.%):Tb³⁺(0.2 at.%):Mn²⁺(0.3 at.%) film under UV excitation is observed. The high efficiency of energy transfer from Ce³⁺ to Tb³⁺ and Mn²⁺ ions, resulting in cold white light emission (x = 0.30 and y = 0.32 chromaticity coordinates) makes the Ce³⁺, Tb³⁺ and Mn²⁺ triply doped Al₂O₃ film an interesting material for the design of efficient UV pumped phosphors for white light generation.     

Gravitational waves detector mirrors: Spectroscopic ellipsometry study of Ta2O5 films on SiO2 substrates

A stack of Ta₂O₅/SiO₂ layers is presently used as coating layer of mirrors in interferometric detectors for gravitational waves. The sensitivity of these detectors is limited in the 50-300 Hz frequency range by the mirror thermal noise, and it was suggested that mechanical losses in the Ta₂O₅ are the dominant source of noise. We focus here on Spectroscopic Ellipsometry (SE) results (in the 0.75 ÷ 5 eV spectral range) obtained on high quality Ta₂O₅ films deposited on SiO₂ substrates by Double Ion Beam Sputtering at the Laboratoire des Matériaux Avancés (Lyon, France). The films are extremely flat as indicated by the 0.2 nm RMS roughness determined by Atomic Force Microscopy (AFM) on (20 × 20) μm² areas. The comparison of the optical properties determined by SE with literature data, corroborated by X-ray Photoelectron Spectroscopy (XPS) data, suggests that the films present a non-ideal bulk stoichiometry and/or some degree of nanoporosity. The possible influence of an interface layer is also discussed.     

The etching characteristics of Al2O3 thin films in an inductively coupled plasma

In this study, the etching characteristics of ALD deposited Al₂O₃ thin film in a BCl₃/N₂ plasma were investigated. The experiments were performed by comparing the etch rates and the selectivity of Al₂O₃ over SiO₂ as functions of the input plasma parameters, such as the gas mixing ratio, the DC-bias voltage, the RF power, and the process pressure. The maximum etch rate was obtained at 155.8 nm/min under a 15 mTorr process pressure, 700 W of RF power, and a BCl₃ (6 sccm)/N₂ (14 sccm) plasma. The highest etch selectivity was 1.9. We used X-ray photoelectron spectroscopy (XPS) to investigate the chemical reactions on the etched surface. Auger electron spectroscopy (AES) was used for the elemental analysis of the etched surfaces.     

Synthesis, structure and exchange bias in Cr2O3/CrO2/Cr2O5 particles

We report on the synthesis, structure and magnetic properties of a novel exchange bias system with Cr₂O₃/CrO₂/Cr₂O₅ interfaces. Chromium oxide particles with mixed chromium valences were prepared by sintering CrO₃ in air. X-ray diffraction patterns show that CrO₃ lost its oxygen gradually with increasing temperature and time through Cr₃O₈, Cr₂O₅, CrO₂, and finally Cr₂O₃ at temperatures above 760 K. X-ray photoelectron spectra indicate a low CrO₂ content and a binding energy of 579.3 eV for Cr 2p_3/2 photoelectrons in Cr₂O₅. Chromium dioxide was found to stably coexist with Cr₂O₃ and Cr₂O₅ in the particles. Magnetic measurements show hysteresis loop shifts in the sample, indicating an exchange bias induced by antiferromagnetic Cr₂O₃/Cr₂O₅ in ferromagnetic CrO₂. An exchange bias of 9 mT at 5 K and a coercivity of 26.3 mT were observed in the chromium oxide particles containing CrO₂.     

Effect of Nb2O5 on the microstructure and mechanical properties of TiAl based composites produced by hot pressing

In situ composites of TiAl reinforced with Al₂O₃ particles are successfully synthesized from an elemental powder mixture of Ti, Al and Nb₂O₅ by the hot-press-assisted reaction synthesis (HPRS) method. The as-prepared composites are mainly composed of TiAl, Al₂O₃, NbAl₃, as well as small amounts of the Ti₃Al phase. The in situ formed fine Al₂O₃ particles tend to disperse on the matrix grain boundaries of TiAl resulting in an excellent combination of matrix grain refinement and uniform Al₂O₃ distribution in the composites. The Rockwell hardness and densities of TiAl based composites increase gradually with increasing Nb₂O₅ content, and the flexural strength and fracture toughness of the composites have the maximum values of 634 MPa and 9.78 MPa m^1/2, respectively, when the Nb₂O₅ content reaches 6.62 wt.%. The strengthening mechanism was also discussed.     

Influence of excitation wavelengths on luminescent properties of Sr3Al2O6:Eu, Dy phosphors prepared by sol-gel-combustion processing

Eu²⁺ and Dy³⁺ ion co-doped Sr₃Al₂O₆ red-emitting long afterglow phosphor was synthesized by sol-gel-combustion methods using Sr(NO₃)₂, Al(NO₃)₃·9H₂O, Eu₂O₃, Dy₂O₃, H₃BO₃ and C₆H₈O₇·H₂O as raw materials. The crystalline structure of the phosphors were characterized by X-ray diffraction, luminescent properties of phosphors were analyzed by fluorescence spectrophotometer. The effect of excitation wavelengths on the luminescent properties of Sr₃Al₂O₆:Eu²⁺, Dy³⁺ phosphors was discussed. The emission peak of Sr₃Al₂O₆:Eu²⁺, Dy³⁺ phosphor lays at 516 nm under the excitation of 360 nm, and at 612 nm under the excitation of 468 nm. The results reveal that the Sr₃Al₂O₆:Eu²⁺, Dy³⁺ phosphor will emit a yellow-green light upon UV illumination, and a bright red light upon visible light illumination. The emission mechanism was discussed according to the effect of nephelauxetic and crystal field on the 4f⁶5d¹ → 4f⁷ transition of the Eu²⁺ ions in Sr₃Al₂O₆. The afterglow time of (Sr_0.94Eu_0.03Dy_0.03)₃ Al₂O₆ phosphors lasts for over 600s after the excited source was cut off.     

Single-step sputtered Cu2SnSe3 films using the targets composed of Cu2Se and SnSe2

Cu₂SnSe₃ thin films were prepared by single-step D.C. sputtering at 100-400 °C for 3 h using targets composed of Cu₂Se and SnSe₂ in three different ratios of 2/1 (target A), 1.8/1 (target B), and 1.6/1 (target C). The advantages of self-synthesized SnSe₂ instead of commercially available SnSe for depositing Cu₂SnSe₃ thin films were demonstrated. Effects of target composition and substrate temperature on the properties of Cu₂SnSe₃ thin films were investigated. Structure, surface morphology, composition, electrical and optical properties at different process conditions were measured. The 400 °C-sputtered films obtained from target B display with direct band gap of 0.76 eV, electrical resistivity of 0.12 Ω cm, absorption coefficient of 10⁴-10⁵ cm^− 1, carrier concentration of ∼ 1.8 × 10¹⁹ cm^− 3, and electrical mobility of 2.9 cm²/V s.     

Conversion of green emission into white light in Gd2O3 nanophosphors

Gd₂O₃ nanophosphors were prepared by combustion synthesis with and without doping of Dy³⁺ ions. The X-ray powder diffraction patterns indicate that as-prepared Gd₂O₃ and 0.1 mol% Dy₂O₃ doped Gd₂O₃ nanophosphors have monoclinic structures. The transmission electron microscope (TEM) studies revealed that the as-prepared phosphors had an average crystallite sizes around 37 nm. The excitation and emission properties have been investigated for Dy³⁺ doped and undoped Gd₂O₃ nanophosphors. New emission bands were observed in the visible region for Gd₂O₃ nanophosphors without any rare earth ion doping under different excitations. A tentative mechanism for the origin of luminescence from Gd₂O₃ host was discussed. Emission properties also measured for 0.1 mol% Dy³⁺ doped Gd₂O₃ nanophosphors and found the characteristic Dy³⁺ visible emissions at 489 and 580 nm due to ⁴F_9/2 → ⁶H_15/2 and ⁴F_9/2 → ⁶H_13/2 transitions, respectively. The chromaticity coordinates were calculated based on the emission spectra of Dy³⁺ doped and undoped Gd₂O₃ nanophosphors and analyzed with Commission Internationale de l'Eclairage (CIE) chromaticity diagram. These nanophosphors exhibit green color in undoped Gd₂O₃ and white color after adding 0.1 mol% Dy₂O₃ to Gd₂O₃ nanophosphors under UV excitation. These phosphors could be a promising phosphor for applications in flat panel displays.     

High pressure luminescence and time resolved spectra of La2Be2O5:Pr

We present luminescence, luminescence excitation and luminescence time resolved spectra of La₂Be₂O₅:Pr³⁺ system. We used high pressure spectroscopy approaches, with high pressure applied in diamond anvil cell (DAC) and sapphire anvil cell (SAC), for detailed analysis of luminescence related to the 4f5d → 4f² and 4f² → 4f² transitions. We present effect of up-converted luminescence related to 4f5d → 4f² transition excited with 488 nm. We also discussed possibility of existence of praseodymium trapped exciton (PTE) states in La₂Be₂O₅:Pr³⁺ system. Lack of the PTE is attributed to high quantity of bulk modulus of this material.     

Basic study of single crystal fibers of Pr:Lu3Al5O12 scintillator for gamma-ray imaging applications

Single-crystalline fibers were grown from 0.25, 0.70, and 1.50 mol% Pr-doped Lu₃Al₅O₁₂ (LuAG) melts by the micro-pulling down (μ-PD) method with a diameter of 0.3-0.5 mm and a length of about 200 mm. They were cut to 10 mm long specimens, and their scintillation properties, including light yield and decay time profile, were examined. These results were compared with corresponding properties of the specimens (0.8×0.8×10 mm³) cut from the bulk crystals produced by conventional Czochralski (CZ) growth. The μ-PD-grown fibers demonstrated relatively low light yield and had the same decay time constant when compared with those of the samples cut from the CZ-grown crystals. The fiber crystals were used to assemble scintillating arrays with dimensions of Ø 0.5×10 mm²×20 pixels and Ø 0.3×10 mm²×30 pixels coated by a BaSO₄ reflector. After optical coupling with a position sensitive photomultiplier tube, the fiber-based arrays demonstrated acceptable imaging capability with a spatial resolution of about 0.5 mm.