Combustion synthesis of SiC/Al2O3 composite powders with SiC nanowires and their growth mechanism

SiC/Al₂O₃ composite powders with SiC nanowires were synthesized using a one-step combustion synthesis method taking silica fume (SiO₂), aluminum powder (Al) and carbon black (CB) as raw materials, while ferrocene (C₁₀H₁₀Fe) was used as the catalyst. The calculated results for the relationship between the equilibrium phase and temperature of the Al–SiO₂–C system show that SiC and Al₂O₃ are the only equilibrium phases in the system. In addition, the effects of C₁₀H₁₀Fe on the combustion synthesis process and products were studied. It was found that with increasing catalyst content, the amount of residual Si in the products first decreases and then increases, the combustion temperature first increases and then decreases, and the nanowire content continues to increase. For an optimal amount of C₁₀H₁₀Fe of 0.75 wt%, almost no residual Si is observed in the product, while the combustion temperature (T_c) is high (2104 K), the SiC nanowire content is relatively high, and the nanowire aspect ratio is large. In addition, two growth mechanism models for SiC nanowires: VS and VLS were validated.     

Low pressure plasma-sprayed Al2O3 and Al2O3/SiC nanocomposite coatings from different feedstock powders

This paper describes a preliminary investigation of a nanocomposite ceramic coating system, based on Al₂O₃/SiC. Feedstock Al₂O₃/SiC nanocomposite powder has been manufactured using sol-gel and conventional freeze-drying processing techniques and then low pressure plasma sprayed onto stainless steel substrates using a CoNiCrAlY bond coat. Coatings of a commercial Al₂O₃ powder have also been manufactured as a reference for phase transformations and microstructure. The different powder morphology and size distribution resulting from the different processing techniques and their effect on coating microstructure has been investigated. Phase analysis of the feedstock powders and of the as-sprayed coatings by X-ray diffractometry (XRD) and nuclear magnetic resonance (NMR) showed that the nano-scale SiC particles were retained in the composite coatings and that equilibrium α-Al₂O₃ transformed to metastable γ- and δ-Al₂O₃ phases during plasma spraying. Other minority phases in the sol-gel Al₂O₃/SiC nanocomposite powder such as silica and aluminosilicate were removed by the plasma-spraying process. Microstructure characterisation by scanning electron microscopy (SEM) of the as-sprayed surface, polished cross-section, and fracture surface of the coatings showed evidence of partially molten and unmolten particles incorporated into the predominantly lamella microstructure of the coating. The extent of feedstock particle melting and consequently the character of the coating microstructure were different in each coating because of the effects of particle morphology and particle size distribution on particle melting in the plasma.     

Al-TiO2-C体系热力学分析及Al2O3-TiC复相陶瓷的燃烧合成

对Al-TiO2-C燃烧合成体系进行了热力学计算,并利用Al-O-N、Ti-O-N、C-O-N三个体系的叠加优势区相图分析了该燃烧合成体系的平衡产物相.结果表明,Al-TiO2-C燃烧合成体系的绝热燃烧温度为2398 K,燃烧合成平衡相为Al2O3和TiC.XRD检测结果与热力学分析结果相吻合,说明该燃烧合成反应进行得较为彻底,证实热力学分析结果可信.原位生成的Al2O3和TiC两相分布较均匀,燃烧合成产物疏松多孔,易于通过球磨方式达到破碎、磨细的目的.     

液相法制备棒状Al2O3及Al2O3-ZrO2陶瓷复合粉体

采用二乙三胺五乙酸（DTPA）为配合剂,以简易的液相法合成出微纳米纤维状Al和Al-Zr前体,煅烧处理制备了棒状α-Al₂O₃和Al₂O₃-ZrO₂复合陶瓷粉体。同时研究了DPTA∶Al³⁺质量比、反应温度与时间对陶瓷粉体形态的影响。利用X射线衍射（XRD）、热分析（TG/DSC）以及扫描电子显微镜（SEM）对粉体进行了表征。结果表明：较高的DTPA∶Al³⁺质量比以及较长的反应时间有利于制备高长径比的纤维棒状Al和Al-Zr配合物前体。合成纳米纤维状α-Al₂O₃和Al₂O₃-ZrO₂前体的最优条件是反应温度60℃,反应时间5.5h,DTPA∶Al³⁺比例为1.2∶1。相应地,该前体煅烧后可以制备出棒状α-Al₂O₃和Al₂O₃-ZrO₂复合陶瓷粉体。     

In situ preparation of SiC/Si3N4-NW composite powders by combustion synthesis

Large-scale composite powders containing silicon carbide (SiC) particles and silicon nitride nanowires (Si₃N₄-NWs) were synthesized in situ by combustion synthesis (CS). In this process, a mixture of silicon, carbon black, polytetrafluoroethylene (PTFE) and a small amount of iron powders was used as the precursor. The products were characterized by XRD, SEM, EDS and TEM. The particles are equiaxed with diameters in the micron range, and the in situ formed nanowires are straight with uniform diameters of 20-350 nm and lengths of tens of microns. The Si₃N₄-NWs are characterized to be α-phase single crystals grown along the [1 0 1] or [1 0 0] direction. VLS and SLGS processes are proposed as the growth mechanisms of the nanowires. The as-synthesized powders have great potential for use in the preparation of high-performance SiC/Si₃N₄-NW composites.     

Interaction of cationic and anionic polyelectrolyte with SiO2 and Al2O3 powders

The adsorption of anionic and cationic polyelectrolytes onto alumina and silica surfaces is studied. The results indicate that the polyelectrolyte-surface interaction is affected by various factors such as (i) polyelectrolyte nature, (ii) distribution and nature of the oxide surface sites, and (iii) medium properties. A strong interaction enhances the formation of a flat conformation of the adsorbed polyelectrolyte onto the surface, whereas a weak interaction leads to a loops conformation. The effect of the adsorbed polyelectrolyte on the electrokinetic behaviour of the two oxides was also investigated using an electrokinetic sonic amplitude analyser.     

Microstructural evolution of supra-nanostructure Al2O3/ZrO2 eutectic powders by combustion synthesis-spray cooling

Eutectic powders with fine microstructure are difficult to synthesize by crushing eutectic bulk because of the damage of crystal structure and the introduction of milling media during preparation process. In this work, a novel combustion synthesis-spray cooling (CSSC) method is developed to fabricate supra-nanostructure Al₂O₃/ZrO₂ eutectic powders. CSSC is a kind of self-heating technique, which simplifies operations, reduces costs and supplies ultra-high cooling rate. The phase composition and the microstructural evolution are investigated using experiment studies and ANSYS simulation. During the process, the t-ZrO₂ are stabilized at room temperature because of the solubility of Al₂O₃ in ZrO₂. The ultra-high cooling rate greatly refined eutectic structure. Although the eutectic structure coarsens with increases in particle size, the interphase spacing of all particles reaches supra nanoscale. The work provides a route for preparing supra-nanostructure Al₂O₃/ZrO₂ eutectic powders and for better understanding the microstructural evolution.     

Al2O3微粉和SiO2微粉对刚玉-莫来石材料性能的影响

在板状刚玉细粉中添加粘土或Al2O3微粉和不同种类的SiO2微粉制成刚玉-莫来石试样,分别于1200℃、1400℃和1600℃保温5 h烧成后,测定试样的体积密度、显气孔率和烧后线收缩率,利用XRD分析了试样在不同温度段的莫来石生成量,研究了添加Al2O3微粉和不同种类的SiO2微粉对材料的烧结性能和莫来石化的影响,并利用SEM观察了试样的显微结构.结果表明(1)加入Al2O3微粉和SiO2微粉均有利于材料的烧结;加入SiO2微粉的纯度和晶形不同,对试样莫来石化的影响也不同,无定形态SiO2微粉(即硅灰)的纯度越高,试样的莫来石生成量也越高.(2)加粘土的试样,其显微结构中柱状莫来石的晶体特征比较明显;而加入SiO2微粉的试样,其莫来石晶体和刚玉晶体相互交错,晶粒较小.     

炭黑包裹燃烧法制备Al_2O_3-ZrO_2复合粉

研究了采用炭黑包裹燃烧法制备Al2O3-ZrO2复合粉体溶液pH值和炭黑氧化温度对复合粉体制备团聚及粒度组成的影响。结果表明:pH值控制为3,经过500℃×10h+600℃×2h脱炭后制得的粉体粒径最小,通过激光粒度分布仪测定得Al2O3-ZrO2复合粉体粒径分布均匀,d10=0.6μm,d50=2.06μm,平均粒径为2.62μm,复合粉体的比表面积为440m2/cm3。     

Microwave-assisted solution combustion synthesis of Fe3O4 powders

Magnetite (Fe₃O₄) powders were synthesized by solution combustion method at different fuel to oxidant ratios (ϕ = 0.5, 0.75, 1 and 1.5) using conventional and microwave ignition. The ignition method and fuel content affected the phase evolution, microstructure and magnetic properties of Fe₃O₄ powders as characterized by X-ray diffractometry, infrared spectroscopy, N₂ adsorption–desorption, electron microscopy and vibrating sample magnetometry techniques. Single phase Fe₃O₄ powders were only obtained using conventional ignition at ϕ value of 1, while the impurity phases such as α-Fe₂O₃ and FeO together with Fe₃O₄ phase were formed by microwave ignition. The bulky microstructure of conventionally combusted powders with specific surface area of 71.5 m²/g was transformed to disintegrated structure (76.5 m²/g) by microwave heating. The microwave combusted powders showed the highest saturation magnetization of 86.5 emu/g at ϕ value of 0.5 and the lower coercivity than that of conventionally combusted powders at all ϕ values, due to their larger particles.     

ZrO2(3Y)包裹Al2O3纳米复合粉体的制备

以pH值缓冲溶液为沉淀剂,用非均匀成核和液相共沉淀相结合的方法合成出了ZrO₂（3Y）包裹Al₂O₃纳米复合粉体.用XRD、TEM对所制备粉体进行了表征.研究表明：加入分散剂使Al₂O₃悬浮液的等电点向酸性区移动,Zeta电位绝对值增大,其中pH值为9.56对应的Zeta电位绝对值最大,悬浮液最稳定.Al₂O₃悬浮液pH值为9.5,ZrOCl₂和YCl₃混合溶液浓度为0.2 mol•L^-1时前驱体的收得率最高.600℃煅烧后得到的粉体中只有α-Al₂O₃、t-ZrO₂两种物相,在Al₂O₃颗粒表面附着10 nm左右的ZrO₂（3Y）颗粒.     

Regeneration of S-poisoned Pd/Al2O3 and Pd/CeO2/Al2O3 catalysts for the combustion of methane

This work investigates the regeneration of S-poisoned Pd/Al₂O₃ and Pd/CeO₂/Al₂O₃ catalysts under different CH₄ containing atmospheres. Under lean combustion conditions in the presence of excess O₂, partial regeneration took place for both systems only above 750 °C after decomposition of stable sulphate species adsorbed on the support. Under alternate lean combustion/CH₄-reducing pulse regeneration is markedly anticipated down to 550–600 °C. Experiments evidenced an effective role of ceria in preventing PdO from sulphation and in promoting regeneration via sulphates decomposition under reducing conditions.     

Liquid phase formation in the system SiC,Al2O3, Y2O3

The liquid phase formation in the system SiC–Al₂O₃–Y₂O₃ was investigated via differential thermal analysis (DTA) combined with thermogravimetry (TG). For this purpose mixtures of various alumina and yttria mol ratios and 10 and 20 mol% silicon carbide were densified and heat treated at different temperatures. It was shown that silicon carbide in the examined amounts has low influence on the melting temperature of the oxide phase. The compositions and microstructures formed were studied by SEM, EDX and XRD. The results were compared to thermodynamic calculations.     

NiO-Al combustion synthesis as applied to joining Al2O3 ceramics

A method for joining Al₂O₃ ceramics has been investigated by utilizing NiO-Al volume combustion under various pre-heating gradients in air; the ignition temperature of the system has been made clear by changing starting composition, particle size of Al, and packing density of reaction powder compacts to optimize the conditions for ceramics joining. Combustion synthesized joining layers were mainly composed of NiAl₂O₄, Ni, and NiO. In order to prevent Al₂O₃ plates cracking during the combustion process, Al₂O₃ paste containing Al₂O₃ and water glass were deposited onto the Al₂O₃ surface, which formed intermediate layer joining the reactant layer and Al₂O₃ ceramics and decreased the temperature gradient between the two layers.     

Liquid phase sintering of Al2O3/SiC nanocomposites

Al₂O₃/SiC nanocomposites are usually prepared by hot pressing or using high sintering temperatures, viz. 1700°C. This is due to the strong inhibiting effect of the nano-sized SiC particles on the densification of the material. Liquid phase sintering (LPS) can be used to improve densification. This work explored two eutectic additive systems, namely MnO₂.SiO₂ (MS) and CaO.ZnO.SiO₂ (CZS). The additive content in Al₂O₃/5 wt% SiC nanocomposite material varied from 2 to 10 wt%. Densities of up to 99% of the theoretical value were achieved at temperatures as low as 1300°C. Characterisation of the materials by XRD, indicated the formation of secondary crystalline phases in addition to Al₂O₃ and SiC. SEM and TEM analysis showed the presence of a residual glassy phase in the grain boundaries, and an increase in the average grain size when compared to nanocomposites processed without LPS additives.     

Thermal conductivity of Al2O3/SiC platelet composites

The thermal conductivity of hot-pressed Al₂O₃/SiC platelet composites is determined as a function of the platelet content, from 0 to 30 vol.% of SiC. Existing heat conduction models are employed to discuss the experimental data. Data agree with the presence of an interfacial thermal resistance at the Al₂O₃/SiC grain boundaries, which precludes the effect of percolation on the thermal conductivity for the higher percentage of SiC platelets. The observed orientation effect on the thermal conductivity due to an alignment of the platelets is also modelled using the Hasselman's approach. The thermal conductivity of the SiC platelets is calculated from the effective thermal conductivity of the composites.     

Combustion synthesis of B4C/Al2O3/C composite powders and their effects on properties of low carbon MgO-C refractories

To improve the dispersity and oxidation resistance of nano carbon black (CB) in low carbon MgO-C refractories, B₄C/Al₂O₃/C composite powders were prepared by a combustion synthesis method using B₂O₃, CB and Al powders as the raw materials. The phase compositions and microstructures of the synthesized products were characterized by X-ray diffraction (XRD), Raman spectroscopy, and a scanning electron microscopy/energy dispersive spectrometry (SEM/EDS). The results show that an 80 wt% excess of CB is the maximum amount of CB that can be added under the condition of a self-propagating combustion wave, and the phase compositions of the products are B₄C, α-Al₂O₃ and CB. B₄C particles with uniform sizes and cubic polyhedral structures are embedded in the Al₂O₃ matrix. The combustion-synthesized B₄C/Al₂O₃/C powders and mechanically mixed B₄C/Al₂O₃/C powders were added to the low carbon MgO-C refractories, and their corresponding properties were compared. The apparent porosity (AP) of the refractories with the synthesized powders (labelled as M3) is lower than those of the refractories with mechanically mixed powders (labelled as M2) and without composite powders (labelled as M1). The oxidation ratio and slag erosion depth of M3 were lower than those of M2 and M1. The thickness of the decarburized layer of M3 was 10.2% and 22.4% less than that of M2 and M1, respectively. The penetration depth of M3 was 12.0% and 27.9% less than that of M2 and M1, respectively. The thermal shock resistance of M3 was better than that of M2 and M1. The residual strength ratio of M3 was 15.8% and 17.2% more than that of M2 and M1, respectively. These results suggest that the combustion-synthesized B₄C/Al₂O₃/C composite powders can be used as new and promising additives for low carbon MgO-C refractories.     

Al2O3/SiC纳米复合陶瓷的制备及性能

在Al2O3陶瓷基体中引入第2相纳米SiC颗粒,可以改善力学性能、耐磨损性能,是陶瓷领域研究的热点之一。纳米颗粒的均匀分散和适当的成型烧结决定了其性能。本文就目前存在的Al2O3/SiC纳米复合陶瓷粉体制备方法与烧结工艺进行了详细阐述。     

Corrosion of a unidirectionally solidified Al2O3/YAG eutectic composite in a combustion environment

Owing to their remarkable higher creep resistance, some oxides eutectic composites those fabricated by unidirectional solidification are prime candidates for structural components used in a severe corrosive environment at high temperatures. In this paper, the possibility of an Al₂O₃/YAG eutectic composite for high-temperature application, where the materials would be exposed to combustion gases, was investigated. The Al₂O₃/YAG eutectic composite was stable at 1700 °C in an atmosphere of oxygen/water vapor (O₂/H₂O), showing only slight changes in microstructure, volume and flexural strength after an exposure for 200 h. Thus, Al₂O₃/YAG eutectic composite is among the most promising ceramics for structural applications at high temperatures.     

Effect of Al2O3/SiO2 ratio on iron-based catalysts for Fischer–Tropsch synthesis

A systematic study was undertaken to investigate the effects of Al₂O₃/SiO₂ ratio on reduction, carburization and catalytic behavior of iron-based Fischer–Tropsch synthesis (FTS) catalysts promoted with potassium and copper. The catalysts were characterized by N₂ physical adsorption, CO₂ temperature-programmed desorption (TPD), H₂ temperature-programmed reduction (TPR) and Mössbauer effect spectroscopy (MES). CO₂-TPD indicated that Al₂O₃ binder has stronger acidity than SiO₂ binder and weakens the surface basicity of the catalysts. H₂-TPR profiles suggested that the lower Al₂O₃/SiO₂ ratio promotes the reduction of Fe₂O₃→Fe₃O₄. With further increasing Al₂O₃/SiO₂ ratio, the transformation of Fe₂O₃→Fe₃O₄ shifts to higher temperatures. The MES results showed that the increase of Al₂O₃/SiO₂ ratio leads to the relatively large crystallite size of α-Fe₂O₃ and inhibits carburization of the catalyst. During reaction tests in a fixed bed reactor it was found that a maximum in catalyst activity is noted at the Al₂O₃/SiO₂ ratio of 5/20 (weight basis). The selectivity to olefins shows a rapid decrease and the formations of methane and light hydrocarbons are promoted with increasing Al₂O₃/SiO₂ ratio. The oxygenate selectivity in total products increases with increasing Al₂O₃/SiO₂ ratio.