Development of a Continuous Segmented Flow Tubular Reactor and the “Scale‐out” Concept – In Search of Perfect Powders

The synthesis of powders with controlled shape and narrow particle size distributions is still a major challenge for many industries. A continuous Segmented Flow Tubular Reactor (SFTR) has been developed to overcome homogeneity and scale‐up problems encountered when using batch reactors. Supersaturation is created by mixing the co‐reactants in a micromixer inducing precipitation; the suspension is then segmented into identical micro‐volumes by a non‐miscible fluid and sent through a tube. These micro‐volumes are more homogeneous when compared to large batch reactors leading to narrower size distributions, better particle morphology, polymorph selectivity and stoichiometry. All these features have been demonstrated on single tube SFTR for different chemical systems. To increase productivity for commercial application the SFTR is being “scaled‐out” by multiplying the number of tubes running in parallel instead of scaling‐up by increasing their size. The versatility of the multi‐tube unit will allow changes in type of precipitate with a minimum of new investment as new chemistry can be researched, developed and optimised in a single tube SFTR and then transferred to the multi‐tube unit for powder production.     

Effect of calcination conditions on phase formation and particle size of nickel niobate powders synthesized by solid-state reaction

The solid-state mixed oxide method via a rapid vibro-milling technique is explored in the preparation of single-phase nickel niobate (NiNb₂O₆) powders. The formation of the NiNb₂O₆ phase in the calcined powders has been investigated as a function of calcination conditions by TG-DTA and XRD techniques. Morphology, particle size and chemical composition have been determined via a combination of SEM and EDX techniques. It has been found that the minor phases of unreacted NiO and Nb₂O₅ precursors and the Ni₄Nb₂O₉ phase tend to form together with the columbite NiNb₂O₆ phase, depending on calcination conditions. More importantly, it is seen that optimization of calcination conditions can lead to a single-phase NiNb₂O₆ in an orthorhombic phase.     

Potential of vibro-milling technique for preparation of electroceramic nanopowders

The potential of the vibro-milling technique as a simple method to obtain usable quantities of single-phase electroceramic powders with nanosized particles was examined. A detailed study considering the role of both milling time and firing condition on phase formation and particle size of the final product was performed. The calcination temperature for the formation of the desired phase was lower when longer milling times have been applied. More importantly, by employing an appropriate choice of the milling time and calcination condition, high purity electroceramic nanopowders have been successfully prepared with a simple solid-state reaction method.     

Effect of powder painting procedures on the filiform corrosion of aluminium profiles

In this work, the filiform corrosion behaviour of powder painted aluminium profiles was studied, and the coating barrier properties together with adhesion to the substrate were analysed. Samples coated with a traditional painting procedure (one powder layer application followed by curing), and other samples coated using a special cycle to obtain wood grain effect were compared using accelerated filiform corrosion tests. Moreover, in order to better understand the degradation mechanisms of painted metal substrates, thermal stresses were applied to accelerate the natural weathering. The effects of the thermal aging were analysed by electrochemical impedance spectroscopy.     

Kinetic investigation of the carbothermal reduction of an Iranian clay

The kinetics of the carbothermal reduction of clay under argon atmosphere has been investigated by the X-ray diffraction method. The clay-carbon (excess) mixture was formed into 2 cm diameter disks of different thicknesses. Experimental data evidences the significant effect of sample thickness on the reaction rate at 1400 °C. Decreasing thickness promotes mullite dissociation and formation of SiC and alumina powders. Mathematical modeling of the reaction system showed the gas diffusion in the Knudsen regime through the pellet to be the rate controlling step. Diffusivity of CO and reacted core tortuosity factor have been calculated.     

Entropy of fluidized bed—a measure of particles mixing

The paper presents an attempt to define the physical entropy of the dense phase of a fluidized bed, based on liquid-like properties of fluidized systems. The quantity U was used as the analogy of temperature in classical thermodynamics. The obtained expression for physical entropy was compared to the correlation suggested for the Kolmogorov entropy in bubbling bed.     

Fluidization behavior in a circulating slugging fluidized bed reactor. Part I: Residence time and residence time distribution of polyethylene solids

Square nosed slugging fluidization behavior in a circulating fluidized bed riser using a polyethylene powder with a very wide particle size distribution was studied. In square nosed slugging fluidization the extent of mixing of particles of different size depends on the riser diameter, gas velocity, hold up and solids flux in the riser. Depending on the operating conditions the particle residence time distribution of a riser in the slugging fluidization regime can vary from that of a plug flow reactor to that of a well-mixed system.Higher gas velocities cause shorter particle residence times because of a significant decrease in the hold-up of particles in the riser at higher gas velocities. A higher solids flux also shortens the average residence time. Both influences have been quantified for a given polyethylene-air system.Residence time and residence time distribution were determined for different particle size and the influence of gas velocity, solids flux, hold up and riser diameter was studied. When comparing data from segregation and residence time experiments it is clear that segregation data can predict the spread in residence time as a function of overall residence time, particle size and gas velocity. The differential velocity between small and large particles found in the segregation experiments can predict the spread in residence time as found in the residence time distribution experiments with a powder with a broad particle size distribution. Raining of particles through the slugs was studied as a function of plug length, gas velocity and pulse length. It was found that raining is not the determining mechanism for segregation of particles.     

ZnO纳米晶粉末和电沉积Ni薄层透射电镜样品的制备和观察

制备了ZnO纳米晶粉末和电沉积Ni镀层的透射电子显微镜样品,并利用透射电子显微镜对其进行了观察。     

纳米钨粉粒度分布的表征研究

采用X射线小角散射法（SAXS）和光子相关谱法（PCS）测试了纳米钨（W）粉的粒度分布。结果表明,采用SAXS测试出的纳米W粉的粒度分布与透射电镜观察和比表面积法测试结果十分接近,能较为准确地表征纳米W粉的一次颗粒的粒度分布;但为了得到可信的结果,所选择的X射线衍射仪的最小可测试角必须足够小。PCS法测试的纳米W粉的粒度随分散条件的变化而变化,所提供的最佳分散条件可用于测定二次颗粒的粒度分布。     

Hydrothermal synthesis of carbonate-free submicron-sized barium titanate from an amorphous precursor: Synthesis and characterization

In this paper, the amorphous barium titanate precursor was prepared by the peroxo-hydroxide method and post-treated by various drying procedures, such as: room temperature drying, room temperature vacuum drying and vacuum drying at 50 °C. The objective in the latter two treatments was to increase the Ti-O-Ba bonds of the precursor. The post-treated precursors were compared with the untreated (i.e., ‘wet’) precursor. Also, a barium titanate precursor was prepared by an alkoxide route. Afterwards, the precursors were hydrothermally treated at 200 °C in a 10 M NaOH solution. Vacuum drying of the precursor seemingly promoted the formation of Ti-O-Ti bonds in the hydrothermal end-product. The low Ba:Ti ratio (0.66) of the alkoxide-route prepared precursor lead to a multi-phase hydrothermal product with BaTiO₃ as the main phase. In contrast, phase pure BaTiO₃, i.e. without BaCO₃ contamination, was obtained for the precursor which was dried at room temperature. Cube-shaped and highly crystalline BaTiO₃ particles were observed by electron microscopy for the hydrothermally treated peroxo-hydroxide-route prepared precursor.