Evaluation of the turnover times of the bed particles and of the fine powders in a circulating powder-particle fluidized bed (CPPFB)

Circulating fluidizing system of binary Geldart C powders and Geldart A particles was formed, and was called a circulating powder-particle fluidized bed (CPPFB). Solid residence in the CPPFB was concerned in two aspects, namely, bed turnover time and average turnover time of fine powders. The former represented the average time needed for all the bed particles to be circulated, while the latter represented the time needed for all the fine powders in the bed to be discharged out of the bed. Both parameters were investigated under different operating conditions as to the superficial gas velocity, size and hold-up of fine powders. FCC particles of 66 μm were used as coarse particles and 1-5 wt.% Al(OH)₃ powders of different sizes ranging from 0.5 to 15 μm were used as fine powders.The bed turnover time decreased with increasing the size of fine powders to a certain level and then became almost constant with further increase of the size of fine powders. When the size of fine powders was larger than this critical size, neither the size nor the hold-up of fine powders affected the bed turnover time. The bed turnover time drastically increased with increasing the hold-up of fine powders for the cases of using very fine powders of 1.0 μm or smaller. On the other hand, the average turnover time of fine powders decreased with increasing the size of fine powders to a minimum at around 3.5 μm and then increased with increasing the size of fine powders. It also decreased with increasing the gas velocity and decreasing the hold-up of fine powders in the bed. The average turnover time of fine powders was several times larger than the bed turnover time at the same operating conditions.     

Synthesis of ultrafine WC‐Co composite powders under hydrogen atmosphere with in situ carbon via a one‐step reduction‐carbonization process

An inexpensive and facile direct method to synthesis ultrafine WC‐Co composite powders was proposed employing soluble starch as an in situ carbon source in a H₂ atmosphere via a one‐step reduction‐carbonization process. Influences of processing factors, such as temperature, H₂ flow rate, and reaction time have been investigated. The results revealed that the system of synthesis process was dynamic in nature where temperature, H₂ flow rate, and reaction time had a suitable value to achieve the desired product phase. Mainly due to the gas reaction and homogeneous in situ carbon, the synthesizing temperature and reaction time were greatly lower than the conventional method. Lowering the reaction temperature and increasing the reaction rate would lead to finer WC‐Co composite powders. Ultrafine WC‐Co composite powders with almost no unwanted phases were obtained under the H₂ flow rate of 0.75 m³/h at 950°C for 0.5 hour and the average particle size was 155 nm with good dispersion. Furthermore, the mechanism for the phase transformation was discussed in this study as well.     

Synthesis and growth mechanism of approximate spherical β‐Si3N4 particles via carbothermal reduction‐nitridation method

In this work, an efficient carbothermal reduction‐nitridation (CRN) strategy was rationally designed to directly synthesize β‐Si₃N₄ powders with eminent dispersity and granularity uniformity. With the aid of CaO additive, the obtained β‐Si₃N₄ particles were endowed with approximate spherical morphology and smooth surface. The size of β‐Si₃N₄ particles could be regulated in submicro and microscale by altering N₂ pressures. More significantly, the underlying growth mechanism of the β‐Si₃N₄ under elevated N₂ pressure was comprehensively analyzed and tentatively put forward. Benefiting from the remarkable merits, the as‐synthesized β‐Si₃N₄ powders showed great potential for alternative fillers in the application of high thermal conductivity plastic packages.     

Synthesis of well‐dispersed β‐Si3N4 with equiaxed structures using carbothermal reduction–nitridation method

Well‐dispersed β‐Si₃N₄ powders with a novel equiaxed structure and eminent crystal integrity were prepared by carbothermal reduction–nitridation (CRN) strategy with the assistance of CaF₂ additive. The growth mechanism of Si₃N₄ particles in the CRN process was elucidated. It is proposed that the liquid phase formed by SiO₂ and CaF₂ additive is crucial to the formation of equiaxed β‐Si₃N₄, and with an appropriate content of CaF₂, Si₃N₄ powders with pure β phase, superior dispersity and crystal integrity can be obtained.     

The microstructure,formation mechanism and sintering characteristics of Al2O3/ZrO2 supersaturated solid solution powders

In this study, the Al₂O₃/ZrO₂ supersaturated solid solution powders with different ZrO₂ contents were successfully synthesized by a novel combustion synthesis combined with water cooling (CS-WC) method. The solid solubility and formation mechanism of solid solution under the extremely non-equilibrium solidification condition were discussed in details. The ultra-high cooling rate greatly improves the solubility limit of Al₂O₃ in ZrO₂. When ZrO₂ content is 30 mol%, the Al₂O₃ has been almost dissolved into the ZrO₂ lattice. The formation mechanism of solid solution can be attributed to solute interception caused by the huge degree of supercooling. During the sintering process, the solid solution powders precipitate ZrO₂ particles and the Al₂O₃ matrix, which forms a fine and uniform nanostructure. Due to the synergistic effect of t-m phase transformation toughening and ZrO₂ nanoparticles toughening, the Al₂O₃/ZrO₂ nanoceramics exhibit excellent mechanical properties when ZrO₂ contents are at the range of 25–37 mol%.     

Water‐redispersible low‐Tg acrylic powders for the modification of hydraulic binder compositions

Water‐redispersible, low‐T_g acrylic polymer powders are obtained in a free‐flowing form by spray drying the structured aqueous dispersions. Powder sticking and caking phenomena are minimized thanks to the heterogeneous particle morphology achieved through a sequential polymerization technique. Redispersibility is reached by the presence of functional monomers containing acid groups, properly distributed in the polymer particles. The influence of the different synthesis parameters on the drying and redispersion processes is discussed. The acrylic powders developed here are well suited for the modification of Portland cement mortars, giving performances comparable to their corresponding “mother” latices. © 1999 John Wiley & Sons, Inc. J Appl Polym Sci 71: 1781–1787, 1999     

Impact of pressure in static and dynamic pressing of ultrafine plasmochemical ZrO2 (Y)-Al2O3 powders on compact density and compaction efficiency during sintering

The effect of different methods of pretreatment and compacting of ultrafine alumina-zirconia powders of composition (in mass%): 20 Al₂O₃-80 (ZrO₂-Y₂O₃) on densification processes during pressing and subsequent calcination has been studied. Ultrafine powders were prepared by plasma-chemical method. It was found that the initial nanocomposite is a mechanical mixture made up of zirconia nanoparticles and amorphous alumina in a thermodynamically nonequilibrium state. Grinding of powders did not affect their phase state. Powder compacts were produced by means of uniaxial static pressing and magnetic pulse compaction. The impact of mechanical processing of powders on ceramics density was studied. It was shown that dry grinding of powders in a planetary ball mill does not increase the ceramics density. The best and virtually identical results were obtained using preliminary static pressing of powders at increased pressure P?=?900?MPa and their subsequent grinding in a ball mill. Dilatometric studies showed that double-action magnetic pulse compaction provides the maximum shrinkage rate at lower temperatures in comparison to that observed under static pressing. The ceramic density achieved is higher than that obtained using other pressing methods.     

Vacuum Drying for Ultrafine Alumina Powders

It is well known that the drying of liquid-borne powders will create agglomerates and the problem of agglomeration is particularly acute in the nanoscale range. To eliminate/mitigate the agglomeration problem, in this study, a vacuum drying technique was used for drying the colloid solution with θ-Al₂O₃ ultrafine particles. For comparison purposes, other drying methods including oven drying, microwave drying, and freeze drying were also applied for drying of the same kind of colloid solution. The results indicate that the redispersibility, which is closely related to the degree of agglomeration, of the dried powders obtained from vacuum drying is better than that obtained from freeze drying. More surprisingly, results showed that the dried powders obtained from the vacuum drying assisted by microwave heating has the redispersibility close to 100%.     

Fluidization Characteristics in Micro‐Fluidized Beds of Various Inner Diameters

The fluidization characteristics of quartz sand and fluid catalytic crack (FCC) catalyst particles in six micro‐fluidized beds with inner diameters of 4.3, 5.5, 10.5, 15.5, 20.5, and 25.5 mm were investigated. The effects of bed diameter (D_t), static bed height (H_s), particles and gas properties on the pressure drop and minimum fluidization velocity (u_mf) were examined. The results show that the theoretical pressure drops of micro‐fluidized beds deviated from the experimental values under different particles and gas properties. The possible reason is due to an increase in bed voidage under smaller bed diameters. The equations for conventional fluidized beds did not fit for micro‐fluidized beds. u_mf increased with decreasing D_t. When the ratio of H_s to D_t ranged from 1:1 to 3:1, u_mf was characterized by a linear equation with H_s, while the slope of the equation u_mf versus H_s decreased with increasing D_t. In this paper, D_t/d_p and H_s/d_p were defined as dimensionless variables and a new equation was developed to predict u_mf in micro‐fluidized beds under the present experimental conditions.     

超细粉在导向管喷动床中的固体循环速率

Ultra-fine powders are difficult to be fluidized due to the strong particle to particle cohesiveness.However, the authors‘ experiments showed that the ultra-fine powder CaCO3 could be stably fluidized in a spouted bed with a draft tube. The effects of geometric and operating parameters on solid circulation rate of ultra-fine powder CaCO3 were investigated in a 120 mm diameter transparent semicircular spouted bed with a draft tube. Three draft tubes with different sizes were used in this study. It was found that the solids circulation rate was mainly dependent on the drawing rate of the gas jet from the nozzle, then on the gas transport capacity in the draft tube. With increasing gas feed rate, distance between the nozzle and the draft tube inlet and draft tube diameter, the solids circulation rate could be increased. Based on the jet theory, a quantitative correlation was proposed for predicting the solid circulation rate of ultra-fine powders in a spouted bed with a draft tube by taking into account the gas transport capacity in the draft tube.     

Numerical and experimental analyses of anti‐fouling and heat transfer in the heat exchanger with circulating fluidized bed

Fluidized bed type heat exchangers are known to increase the heat transfer and prevent the fouling. For proper design of circulating fluidized bed heat exchanger it is important to know the effect of design and operating parameters on the bed to the wall heat transfer coefficient. The numerical analysis by using CFX 11.0 commercial code was done for proper design of the heat exchanger. The present experimental studies were also conducted to investigate the effects of circulating solid particles on the characteristics of fluid flow, heat transfer, and cleaning effect in the fluidized bed vertical shell and tube type heat exchanger with counterflow, at which a variety of solid particles such as glass (3 mmØ), aluminum (2–3 mmØ), steel (2–2.5 mmØ), copper (2.5 mmØ), and sand (2–4 mmØ) were used in the fluidized bed with a smooth tube. Seven different solid particles have the same volume, and the effects of various parameters such as water flow rates, particle diameter, materials, and geometry were investigated. The present experimental and numerical results showed that the flow velocity range for collision of particles to the tube wall was higher with heavier density solid particles, and the increase in heat transfer was in the order of sand, copper, steel, aluminum, and glass. This behaviour might be attributed to the parameters such as surface roughness or particle heat capacity. Fouling examination using 25,500 ppm of ferric oxide (Fe₂O₃) revealed that the tube inside wall is cleaned by a mild and continuous scouring action of fluidized solid particles. The fluidized solid particles not only keep the surface clean, but they also breakup the boundary layer improving the heat transfer coefficient even at low‐fluid velocities.     

Fluidization of fine particles in a sound field and identification of group C/A particles using acoustic waves

Effects of sound field on the fluidization of fine particles have been comprehensively examined by using fine powders (4.8-65 μm average in size) including Al₂O₃, TiO₂, glass beads and FCC catalyst. It is found that the fluidization quality of fine particles can be enhanced with the assistance of a sound field, resulting in higher pressure drops and a lower u_mf. The effect of sound on the fluidization of fine particles is strongly dependent on the particle properties (Geldart type and particle size) as well as the parameters of the sound field such as sound pressure level (or intensity) and frequency. Given a fixed sound frequency, the effect becomes more significant at a higher sound pressure level. For the present sound-aided fluidized bed system, there is a resonant frequency at about 100-110 Hz, at which the effectiveness of the sound wave in improving fluidization of fine particles is most remarkable. In addition, based on the different attenuation features of sonic waves in the gas-solid suspension of group C and A particles, a novel acoustic method is explored to distinguish group C from group A particles.     

Low‐temperature molten salt synthesis of forsterite powders with controllable morphology

Forsterite powders with controllable morphology were synthesized using oxides as raw materials in NaCl–KCl molten salt media. The effects of MgO/SiO₂ ratio, calcining temperature, and salt/oxide ratio on the phase composition and morphology of the powders are investigated. The results indicate that single‐phase forsterite powders can be synthesized from a mixture of MgO and SiO₂ with a MgO/SiO₂ molar ratio of 2:1.3 at 700°C. With the increase in calcining temperature, the powders obtained changes from an irregular to a columnar morphology. In addition, the morphology of the forsterite powders produced can also be controlled by altering the salt/oxide ratio.     

Three-Dimension imaging of particle clusters in dilute gas—solid suspension flow

The three dimensional flow structure of dilute gas—solid suspensions in a small-scale circulating fluidized bed (0.200 m riser diameter) was visualized by applying the laser sheet technique. FCC particles were fluidized with sustained solid loading at gas velocities corresponding to the turbulent and the fast fluidization regimes in cases where the solid circulation was sufficient. Three typical shapes of clusters in the core section of the riser were observed. Clusters characterized by a paraboloidal shape heading downward were connected to neighboring clusters at their tail part, forming a three dimensional network structure.     

Preparation and characterization of ultrafine ZrB2–SiC composite powders by a combined sol–gel and microwave boro/carbothermal reduction method

A combined sol–gel and microwave boro/carbothermal reduction technique was investigated and used to synthesize ultrafine ZrB₂–SiC composite powders from raw starting materials of zirconium oxychloride, boric acid, tetraethoxysilane and glucose. The effects of reaction temperature, molar ratios of n(B)/n(Zr) and n(C)/n(Zr+Si) on the synthesis of ultrafine ZrB₂–SiC composite powders were studied. The results showed that the optimum molar ratios of n(B)/n(Zr) and n(C)/n(Zr+Si) for the preparation of phase pure ultrafine ZrB₂–SiC composite powders were 2.5 and 8.0, respectively, and the firing temperature required was 1300 °C. This temperature was 200 °C lower than that require by using the conventional boro/carbothermal reduction method. Microstructures and phase morphologies of as-prepared ultrafine ZrB₂–SiC composite powders were examined by field emission-scanning electron microscopy (FE-SEM) and transmission electron microscope (TEM), showing that SiC grains were formed evenly among the ZrB₂ grains, and the grain sizes of ZrB₂ in the samples prepared at 1300 °C for 3 h were about 1–2 μm. The average crystalline sizes of these two phases in the as-prepared samples were calculated by using the Scherrer equation as about 58 and 27 nm, respectively.     

Spray pyrolysis synthesis of nanostructured LiFexMn2−xO4 cathode materials for lithium-ion batteries

A series of partially Fe-substituted lithium manganese oxides LiFe_xMn_2−xO₄ (0 ≦ x ≦ 0.3) was successfully synthesized by an ultrasonic spray pyrolysis technique. The resulting powders were spherical nanostructured particles which comprised the primary particles with a few tens of nanometer in size, while the morphology changed from spherical and porous to spherical and dense with increasing Fe substitution. The densification of particles progressed with the amount of Fe substitution. All the samples exhibited a pure cubic spinel structure without any impurities in the XRD patterns.The as-prepared powders were then sintered at 750 °C for 4 h in air. However, the particles morphology and pure spinel phase of LiFe_xMn_2−xO₄ powders did not change after sintering. The as-sintered powders were used as cathode active materials for lithium-ion batteries, and cycle performance of the materials was investigated using half-cells Li/LiFe_xMn_2−xO₄. The first discharge capacity of Li/LiFe_xMn_2−xO₄ cell in a voltage 3.5-4.4 V decreased as the value x increased, however these cells exhibited stable cycling performance at wide ranges of charge-discharge rates.     

Bed-to-wall heat transfer characteristics in a circulating fluidized bed

The bed-to-wall heat transfer coefficients were measured in a circulating fluidized bed of FCC particles (d_p = 65 μm). The effects of gas velocity (1.0–4.0 m/s), solid circulation rate (10–50 kg/m²s) and particle suspension density (15–100 kg/m³) on the bed-to-wall heat transfer coefficient have been determined in a circulating fluidized bed (0.1 m-ID x 5.3 rn-high). The heat transfer coefficient strongly depends on particle suspension density, solid circulation rate, and gas velocity. The axial variation of heat transfer coefficients is a strong function of the axial solid holdup profile in the riser. The obtained heat transfer coefficient in terms of Nusselt number has been correlated with the pertinent dimensionless groups     

在具有锥形料腿的循环流化床中流化CaCO3超细颗粒

根据粘附性颗粒在流化过程中形成的聚团具有较宽粒径分布并因此导致大聚团在流化床中沉积和死床的问题,提出了循环流化床的锥形回料系统设计. 该回料系统包括两部分：锥形料腿和带辅助进气的V型阀. 实验证明,锥形料腿通过提供变化的表观流化气速,克服了流化聚团沉积死床等现象;而V型阀的辅助进气,对于保证V型阀顺利输送粘附性颗粒具有关键性作用. 借助这种回料系统,实现了高粘附性超细CaCO3颗粒在循环流化床的稳定快速流化. 从提升管内部拍摄的照片显示,尽管提升管采用较高的流化气体速度,但超细CaCO3颗粒仍然是以聚团的形式被流化. 对在提升管不同高度采集的聚团分析表明,处于快速流化状态的CaCO3聚团的直径远小于传统流化床中聚团的直径,并且在提升管高度方向聚团直径没有较大的变化. 同时实验还显示,提升管轴向空隙率呈S型分布,而径向则体现环-核结构,具有典型的快速床特征.     

Preparation and Characterization of UltraHigh‐Temperature Ternary Ceramics Ta4HfC5

Tantalum hafnium carbide (Ta₄HfC₅) powders were synthesized by solvothermal treatment and carbothermal reduction reactions from an inorganic hybrid. Tantalum pentachloride, hafnium chloride, and phenolic resin were used as the sources of tantalum, hafnium, and carbon, respectively. Pyrolysis of the complexes at 1000°C/1 h initiated the carbothermal reduction to result in multiplex phases including tantalum carbide and hafnium oxide which after heat treatment at 1400°C–1600°C transformed to single‐phase solid solution Ta₄HfC₅ by solid solution reaction. The mean crystallite size of Ta₄HfC₅ particles was less than 80 nm, and the composition of Ta, Hf, and C elements was near stoichiometric and homogeneously distributed in the powder samples. XRD pattern for Ta₄HfC₅ powders was analyzed.     

Atmospheric plasma spraying coatings from alumina–titania feedstock comprising bimodal particle size distributions

In this work, Al₂O₃–13 wt% TiO₂ submicron-nanostructured powders were deposited using atmospheric plasma spraying. The feedstocks were obtained by spray drying two starting suspensions of different solids content, prepared by adding nanosized TiO₂ and submicron-sized Al₂O₃ powders to water. The spray-dried granules were heat-treated to reduce their porosity and the powders were fully characterised in both untreated and thermally treated state. Comparison with two commercial feedstocks was carried out. Characterisation allowed a temperature for the thermal treatment to be chosen on the basis of the sprayability of the feedstock and the preservation as much as possible of the submicron-sized structure of the unfired agglomerates.Optimisation of the deposition conditions enabled the reconstituted powders to be successfully deposited, yielding coatings that were well bonded to the substrate. The coating microstructure, characterised by SEM, was mostly formed by a matrix of fully molten particles where the presence of semi-molten feedstock agglomerates was also observed.Moreover, microhardness, toughness, adhesion and tribological behaviours were determined, and the impact of the granule characteristics on these properties was studied. It was found that changing the feedstock characteristics allows controlling the coating quality and properties. In general, good mechanical properties were obtained using a feedstock comprising a binary mixture of submicrometric Al₂O₃ and nanometric TiO₂ particles in the spray-dried powder.