Thermal Reaction Characteristics of Nano/Micron-Sized Aluminum Mixtures in Carbon Dioxide

Thermal reaction characteristics of nano/micron-sized aluminum mixtures in a carbon dioxide atmosphere were investigated by thermogravimetry that aimed to examine the interactions between nanosized aluminum powder and micron-sized aluminum powder. Thermal reaction characteristics of nano/micron-sized aluminum mixtures at different ratios were studied. The synergistic effect mechanism was discussed by comparing experiment result and theoretical calculation. The morphologies and compositions of products were obtained by scanning electron microscopy and X-ray diffraction technologies. Results indicated that there were three weight gain stages for nano/micron-sized aluminum mixtures at different ratios. Although the temperature range of synergistic effect of nano/micron-sized aluminum mixtures with various ratios had somewhat differences, there was a significant synergistic effect from about 900 to 1040°C. The products analyses indicated that the products morphologies of nano/micron-sized aluminum particles showed molten and stuck together, and products contained aluminum and α-Al₂O₃.     

The formation of Al<Subscript>2</Subscript>O<Subscript>3</Subscript> nanoparticles in the oxidation of aluminum by water under sub- and supercritical conditions

Massive aluminum samples were oxidized by sub- and supercritical water with the formation of (AlOOH) _n and (Al₂O₃) _n nanoparticles. The release of H₂ began at 523 K when the reagents were heated uniformly to 700 K. The time lag of the beginning of oxidation was 140 s when supercritical water was injected into a reactor with aluminum samples at 665 K and 23.1 MPa. Oxidized aluminum powders were analyzed using a transmission electron microscope. Predominantly large (300–400 nm) α-Al₂O₃ particles were formed when supercritical water was injected into a reactor with aluminum. Smaller (20–50 nm) γ-Al₂O₃ particles were also observed in samples oxidized by water vapor under temperature increase conditions. Kinetic equations describing the rate of H₂ formation in the reaction of H₂O with aluminum were obtained. Possible nanostructuring mechanisms are discussed.     

Optical properties of anodic aluminum oxide produced in a complex electrolyte

Features of the absorption, transmission, photoluminescence, and infrared (IR) spectra of anodic aluminum oxide (AAO) formed in a complex electrolyte and annealed at 800, 900, 1000, and 1300°C are investigated. The variations in the phase composition changes of the anodic aluminum oxide are reflected in the respective features of its optical properties. A decrease in the transmission coefficient in the visible range of the spectrum is shown for the phase series: amorphous AOA → γ-Al₂O₃, γ-, θ-, δ-Al₂O₃ mixture → α-Al₂O₃. It is established that the highest absorption coefficient is characteristic of α-Al₂O₃, and the amorphous samples are the most transparent in the visible range. An intensive luminescence band in the red region of the spectrum with maxima at 678 and 694 nm is found for α-Al₂O₃. The emergence of this band is explained by the presence of octahedrally coordinated Mn₊₄ and Cr₊₃ impurity ions in the structure. A luminescence band at 700–800 nm is observed for the mixture of low-temperature phases. Intense luminescence in the region 350–500 nm is found for amorphous AAO and γ-Al₂O₃.     

Structural and phase transition of α-Al2O3 powders obtained by co-precipitation method

Aluminium oxide has been synthesized by co-precipitation technique at different annealing temperature. Powder XRD confirms the formation of α-Al₂O₃ with rhombohedral crystal structure having lattice constant a = 4.76 Å and b = 12.99 Å by the Scherer formula, the average crystallite size is estimated to be 66 nm. The scanning electron microscope results expose the fact that the α-Al₂O₃ nanomaterials are seemingly porous in nature and highly agglomerated. Chemical composition of aluminium oxide is confirmed by energy dispersive spectroscopy. The molecular functional group is confirmed by FTIR. Optical absorption of α-Al₂O₃ has been studied in the UV–vis region and its direct band gap is estimated to be 5.97 eV. This study involves the structural and phase transition of Al₂O₃ and also indicates that α-Al₂O₃ has considerable properties, deserving further investigation for the energetic materials with excellent properties for the possibility of using thin-layer α-Al₂O₃ as a thermo luminescence material.     

Deposition of duplex Al2O3/aluminum coatings on steel using a combined technique of arc spraying and plasma electrolytic oxidation

Plasma electrolytic oxidation (PEO) is a cost-effective technique that can be used to prepare ceramic coatings on metals such as Ti, Al, Mg, Nb, etc., and their alloys, but this promising technique cannot be used to modify the surface properties of steels, which are the most widely used materials in engineering. In order to prepare metallurgically bonded ceramic coatings on steels, a combined technique of arc spraying and plasma electrolytic oxidation (PEO) was adopted. In this work, metallurgically bonded ceramic coatings on steels were obtained using this method. We firstly prepared aluminum coatings on steels by arc spraying, and then obtained the metallurgically bonded ceramic coatings on aluminum coatings by PEO. The characteristics of duplex coatings were analyzed by X-ray diffractometer (XRD) and scanning electron microscopy (SEM). The corrosion and wear resistance of the ceramic coatings were also studied. The results show that, duplex Al₂O₃/aluminum coatings have been deposited on steel substrate after the combined treatment. The ceramic coatings are mainly composed of α-Al₂O₃, γ-Al₂O₃, θ-Al₂O₃ and some amorphous phase. The duplex coatings show favorable corrosion and wear resistance properties. The investigations indicate that the combination of arc spraying and plasma electrolytic oxidation proves a promising technique for surface modification of steels for protective purposes.     

XRD and Mössbauer spectroscopy investigation of Fe2O3–Al2O3 nano-composite

Fe₂O₃–Al₂O₃ nano-composites were synthesized by sol–gel means. The properties of samples sintered at various thermal treatment temperatures were investigated by X-ray diffraction (XRD) and Mössbauer spectroscopy (MS). The experimental results show that the γ- to α-Al₂O₃ transformation occurs at lower temperature after iron oxide doping. The samples obtained at 1173 K contained poorly crystallized γ-Al₂O₃ phase and an amorphous iron oxide. When the temperature of heating was increased to 1373 K, the sample was composed of α-Fe₂O₃/α-Al₂O₃ nano-composite and some solid solution. A superparamagnetic phenomenon was observed until the thermal treatment temperature reached 1373 K.     

Fabrication and luminous properties of phosphor ceramic for application in automotive laser headlight

We report on the optimization of fabrication of a ceramic phosphor plate (CPP) using α-Al₂O₃ as functional materials for an automotive laser headlamp. The prepared CPP shows the high luminous characteristics with increasing α-Al₂O₃ contents because of the light scattering of the hexagonal structure of α-Al₂O₃ materials. We investigated the correlation between α-Al₂O₃ and thickness of CPP. The luminous properties of the CPP are improved and optimized according to the variables of one. We found that the prepared sample is a potential material for future solid-state laser lighting in application as an automotive headlamp.     

Thermoluminescence of α-Al 2O 3 by neutron irradiation at low temperature

Thermoluminescence (TL) mechanisms of neutron-irradiated α-Al₂O₃ at 20 K is reported. The TL glow curves of neutron-irradiated and γ-ray-irradiated α-Al₂O₃ were observed. The TL emission bands near 340, 430, 530 and 694 nm were observed in the neutron-irradiated α-Al₂O₃. The γ-ray-irradiated α-Al₂O₃ only showed the TL emission line nearly at 694 nm, corresponding to the R lines of α-Al₂O₃:Cr³⁺. Therefore, the first three emission bands are related to the atomic displacement defects as F-type centers caused by neutron irradiation.     

Phase transformation and controllable size of γ-Al2O3 nanocrystals through Li doping using sol–gel method

The effects of Li, as the ‘additive’, on the structures of nano-sized Al₂O₃ were investigated. Li evidently increased the crystallite size of γ-Al₂O₃, whereas it showed evident effects on neither LiAl₂(OH)₇ precursors nor α-Al₂O₃ nanocrystals. α-Al₂O₃ and γ-Al₂O₃ co-existed in samples calcined at 1000 °C and 1100 °C, and the composition can be adjusted by altering Li concentration. When the calcination temperature reached 1200 °C, high purity of α-phase Al₂O₃ formed and Li showed no effects. In addition, mechanisms of doping Li on the structrure of Al₂O₃ were discussed.     

Influence of treating frequency on microstructure and properties of Al2O3 coating on 304 stainless steel by cathodic plasma electrolytic deposition

Alumina ceramic coatings were fabricated on 304 stainless steel by cathodic plasma electrolytic deposition (CPED). Influence of treating frequency of the power supply on the microstructure and properties of the coatings were studied. The results indicated that coatings obtained at various frequencies on 304 stainless steels were all composed of α-Al₂O₃ and γ-Al₂O₃, and α-Al₂O₃ was the dominant phase. The contents of α-Al₂O₃ decreased gradually in a very small rate with increasing the frequency and γ-Al₂O₃ gradually increased. The surface of alumina ceramic coating was porous. With increasing the frequency, the coating surface gradually became less rough and more compact, resulting in low surface roughness. The bonding strength of Al₂O₃ coating was higher than 22 MPa and was not strongly affected by treating frequency. With increasing the frequency, the alumina coated steels showed better and gradually increasing corrosion resistance than the uncoated one in 3.5% NaCl solution. The coating steel with desirable corrosion resistance was obtained at 800 Hz whose corrosion current potential and corrosion density were −0.237 V and 7.367 × 10⁻⁸ A/cm², respectively.     

电解等离子体法制备Al2O3陶瓷层及其特性研究

利用电弧喷铝并重熔后进行电解等离子体处理(EPP)的方法在Q235钢基体上制备出呈冶金结 合的Al₂O₃陶瓷层.利用XRD，SEM和EDS等手段对陶瓷层的成分和显 微组织进行了分析， 测定了陶瓷层的耐蚀性能和耐磨性能.实验结果表明，陶瓷层主要由α-Al₂O3，γ-Al₂O₃，θ-Al₂O₃以及一 些非晶相组成，组织致密，耐蚀性能和耐磨性能良好. 关键词： 电解等离子体处理 陶瓷层 复合技术 生长机理     

Synthesis and characterization of (h 0 h)-oriented silicalite-1 films on α-Al2O3 substrates

A simple and well-designed synthesis procedure is proposed to fabricate silicalite-1 films on porous α-Al₂O₃ substrates on purpose of preventing the aluminum leaching. The continuous and 2 μm thick seed layer of silicalite-1 crystals is fabricated by using a spin coater. The first-time seeded growth is performed to synthesize a thin layer of intergrown ZSM-5 crystals on the silicalite-1 seed layer, where the use of low alkalinity and short synthesis time is to reduce the aluminum leaching. The intergrown layer of ZSM-5 crystals serves as a barrier to block the aluminum leaching from porous α-Al₂O₃ substrates in the second-time seeded growth, leading to the formation of ca. 11 μm thick intergrown and oriented silicalite-1 films with an extremely high Si/Al ratio. According to SEM images and XRD measurements, the as-synthesized silicalite-1 film is dense, continuous, and (1 0 1)-oriented. The electron probe microanalysis (EPMA) of the resulting film demonstrates that there is no aluminum leaching in the second-time seeded growth. The leaking tests confirm that non-zeolitic pores in the silicalite-1 film are negligible.     

Thermoluminescence study of aluminum oxide doped with therbium and thulium

In this work, α-Al₂O₃ doped either with Tb³⁺ or Tm³⁺ was prepared by combustion synthesis techniques for thermoluminescent (TL) ionizing radiation dosimetry applications. In this method, the reactants (aluminum nitrate, urea and therbium or thulium nitrate) are ignited in a muffle furnace at temperatures as low as 500 °C. This synthesis route is an alternative technique to the conventional fabrication methods of materials based on α-Al₂O₃ (Czochralsky, Vernuil), where high melting temperatures and reducing atmospheres are required. After combustion, the samples were annealed at temperatures ranging from 1000 to 1400 °C for 4 h in order to obtain the pure α-phase structure and were then irradiated with a Co-60 gamma radiation source. The annealed samples present a well defined TL glow peak with a maximum at approximately 200 °C and linear TL response in the dose range 0.5–5 Gy. It was observed that a 0.1 mol% concentration of Tb³⁺ or Tm³⁺ and annealing at 1400 °C optimize the TL sensitivity. The highest sensitivity was found for Tm³⁺ doped samples which were approximately 25 times more sensitive than Tb³⁺ doped samples. These results strongly suggest that combustion synthesis is a suitable technique to prepare doped aluminum oxide material and that Tm³⁺ doped aluminum oxide is a potential material for TL radiation dosimetry.     

Effects of preheating on diaspore: Modifications in colour centres, structure and light emission

The thermal properties and thermal stability of diaspore-corundum (AlOOH-Al₂O₃), from Goian (Pontevedra, Spain) were studied by means of differential thermal analysis (DTA), thermogravimetry (TG), high temperature X-ray diffraction (HTXRD) and thermally stimulated luminescence (TL) techniques. The samples were annealed to link the combined effect of (i) dehydroxylation, (ii) oxidation-reduction of chromophores (Mn 0.5%, Fe₂O₃ 0.12%, TiO₂ 0.021% and Cr 80 ppm) determined by inductively coupled plasma-atomic emission spectrometry (ICP-AES) and (iii) phase transitions whilst sample heating (i.e. α-AlOOH→α′-Al₂P₃→α-Al₂O₃). The blue colour of diaspore, attributed to the Ti⁴⁺-Fe²⁺ intervalence-charge-transfer mechanism, turns to white (circa 500 °C) in good agreement with the DTA endothermic peak (dehydroxylation). The coexistence of α-AlOOH and α′-Al₂P₃ phases has been detected by in situ HTXRD and could be correlated to the thermoluminescence tests performed on preheated aliquots (up to 500 °C).     

Specific features of the magneto-optical properties of α-Al<Subscript>2</Subscript>O<Subscript>3</Subscript> in the IR region

The spectra of reflection and magnetoreflection of light from the crystalline insulator α-Al₂O₃ in the IR spectral region (λ = 2.5–25 μm) are investigated. Some features in the magnetoreflection spectra in the wavelength range corresponding to the excitation of optical phonon modes in α-Al₂O₃ are found. A significant increase in magnetoreflection is observed near these wavelengths. The amplitude and shape of the magnetore-flection spectra for the p and s polarizations of probe light are determined. It is shown that the optical and magneto-optical properties of α-Al₂O₃ in the IR region can be described on the basis of the theory of polaron excitation. A satisfactory correlation between the theoretical and experimental spectra is obtained, which indicates that polarons play an important role in determining the optical characteristics of nonmagnetic insulators and make the dominant contribution to the magnetoreflection spectra.     

Investigation of phase transition of γ-alumina to α-alumina via mechanical milling method

In this research, the results obtained from studying the phase transition of γ-alumina (γ-Al₂O₃) to α-alumina (α-Al₂O₃) during intense mechanical activation in high-energy ball milling are presented. The powder samples were characterized by scanning electron microscope (SEM), X-ray diffraction (XRD), thermogravimetric and Differential thermal analyses (TG-DTA). With respect to the results achieved from above analyses, the transition of γ → α-alumina through δ- and θ-phases, can be initiated. Also, it was found that the pure γ-alumina phase showed a great stability during high-energy ball milling and there was no transformation to any other phase after a long milling time (30 h). On the other hand, γ-alumina containing a small amount of the α-alumina seed, showed a gradual phase transition from γ-alumina to α-alumina in milling. The phase transition mechanism during milling is nucleation and growth, which is promoted by the α-alumina seed.     

聚丙烯酰胺凝胶法制备大孔α-氧化铝及其发光性能研究

采用聚丙烯酰胺凝胶法制备了大孔α-氧化铝材料.利用X射线衍射仪、扫描电镜、荧光分光光度计表征了所制备的氧化铝样品.结果表明,在1150℃烧结温度下可获得高纯的α-氧化铝陶瓷材料,其形貌呈类电路板型(monolithic)大孔结构.荧光光谱测试分析发现,在228 nm波长的光激发下,其荧光光谱在300-400 nm范围内由两个主发射带组成,其峰值分别位于330 nm和365nm.基于实验结果,探讨了多孔氧化铝的形成机理和发光机制.     

Preparation and high-temperature properties of Au nano-particles doped α-Al2O3 composite coating on TiAl-based alloy

Au nano-particles doped α-Al₂O₃ composite coatings were successfully prepared on TiAl-based alloy by electrodeposition, using the Al₂O₃ sols with minor addition of HAuCl₄ solution. The even distribution of Au nano-particles (<2.0 wt.%) in the α-Al₂O₃ matrix has been observed. Isothermal oxidation tests of the samples coated with the as-prepared novel coatings at 900 °C in static air for 200 h shown that the oxygen inward diffusion can be effectively suppressed to a low level. The results of high-temperature cyclic oxidation test at 900 °C in air revealed that the oxidation and spallation resistance of TiAl-based alloy were improved significantly under thermal cycling. In the as-prepared coatings, cracks were shielded by means of crack bridging and the fracture resistance of the formed scales can be improved by toughening effects of the composite structure. Surface scratching tests after the cyclic oxidation exhibited that the adhesion of the formed composite scale on TiAl-based alloy was remarkably improved by the Au nano-particles doped α-Al₂O₃ composite coating.     

Electronic and optical properties of Ti3+ doped α-Al2O3 crystals: First-principles calculations

Based on density functional theory, the geometric and electronic structures of the Ti doped α-Al₂O₃ system (Ti:α-Al₂O₃) are calculated by using a first-principles method. Due to the Ti-doping, both the lengths and angles of bonds in the local geometries are distorted, from which a trigonal–triclinic structural transition may be expected. With increasing Ti-doping, an insulator–semimetal transition is observed in the Ti:α-Al₂O₃ system, mainly due to a complete spin polarization of electrons at the Fermi level. The dielectric function and absorption edge are further calculated. It is found that the absorption edge is decreased, and is much lower than that of pure Al₂O₃ crystals, which is in good agreement with the experiment. The results indicate the potential applications of the Ti:α-Al₂O₃ optical system.     

Preparation and Properties of Nano‐SiO2/Epoxy Composites Cured by Mannich Amine

Nano‐SiO₂/epoxy composites cured by Mannich Amine (type T‐31) were prepared and studied and the results are reported in this paper. The nano‐SiO₂ was pretreated by a silane coupling agent (type KH‐550) and mixed with epoxy resin (type E‐51) using an ultrasonic processor. Amounts of filler loading ranged from 1% to 5% of the weight of the epoxy resin. Some properties of the resulting composites were characterized by X‐ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), and thermogravimetric analysis (TGA). The results of tensile tests and impact tests showed that the composite with 3% nano‐SiO₂ loading presented the best mechanical performances. The tribological performance and thermal stability of the materials were also improved with the addition of nano‐SiO₂.