The Dependence of Pore Size Distribution on Porosity in Hot Isostatically Pressed Porous Alumina

Pore size distributions in porous alumina bodies produced by the capsule-free hot isostatic pressing technique have been determined experimentally. The distribution of pore diameter has been found to be dependent on the size of the pre-sintered powders and the amount of open porosity in the sintered body. An empirical model has been developed to predict the modal pore size as a function of median particle size and open porosity. The pore size distributions were found to widen with reduced porosity. They were also shown to be positively skewed. The skew reduced with decreasing porosity. The pore size variation with porosity for specimens produced with a sintering aid could not be described by the same mathematical functions developed for specimens produced by solid-state sintering.     

Effect of Pore Size Distribution of Carbon-Covered Alumina on the Preparation of Submicrometer α-Alumina Powders

Calcining carbon-covered alumina (CCA) samples at 800°C in an oxygen flow is an efficient method to prepare α-alumina powders. It is found that the pore size distribution of CCA samples, which depends on the carbon content and the pore size distribution of the precursor alumina used, is one of the key factors for the total conversion of γ-alumina to α-alumina and the complete combustion of carbon in the pores of alumina. No matter how high the carbon content, total conversion does not occur for CCA samples prepared from alumina possessing the most probable pore size of about 5.2 nm. Using γ-alumina with the most probable pore size of 6.1 nm as the precursor of CCA samples, total transformation occurs when the carbon content of CCA ranges from 11.9 to 17.3 wt%, but the color of as-prepared α-alumina is not pure white but light gray. Polyethylene glycol (PEG 20 000), added to the sucrose/γ-alumina system, can expand the pores of CCA samples after carbonization, and calcining of thus-prepared CCA results in a complete transformation of γ-alumina to pure white α-alumina with a particle size of about 1 μm when the carbon content of CCA is between 6 and 19 wt%.     

Dependence of Compaction Efficiency in Dry Pressing on the Particle Size Distribution

The compact densification with pressing pressure (compaction efficiency) was determined to be sensitive to the particle size distribution. For the three types of alumina powders used in this research, the compaction efficiency increased with increasing particle size. It has been demonstrated that if the compact density versus log (pressure) has a linear relationship for any two types of powders, so do the blends of the two powders. A model is proposed which can predict the compaction efficiency of a binary particle system based on the Furnas particle packing model and consider the packing efficiency as a function of forming pressure. The composition of the binary mixture at which the highest density is obtained under high pressures is also the composition having the largest compaction efficiency. When coarse particles were added to this composition, the compaction efficiency slowly decreased, and when fine particles were added, the compaction efficiency rapidly decreased. For a continuous particle size distribution, the highest compaction efficiency is related to the average value of -log (porefraction).     

Evolution of the Pore Size Distribution in Final-Stage Sintering of Alumina Measured by Small-Angle X-ray Scattering

Small-angle X-ray scattering was used to follow the evolution of the pore size distribution during final-stage sintering of alumina and of alumina doped with 0.25 wt% magnesia. The volume-weighted (Guinier) results indicate that the effective size of the largest pores increases as the body goes from 97% to more than 99% dense. The surface-area-weighted (Porod) results show that the median size of the smallest pores decreases slightly over the same density range. Taken together, these data indicate that the pore size distribution becomes broader as final-stage densification proceeds. This was confirmed by a maximum entropy analysis, which was used to derive pore size distributions directly from the data. Finally, the evolution of the pore size distributions in alumina, with and without sintering aid, were compared.     

致密超细球形氧化铝制备性能良好的陶瓷超滤膜

热等离子体制备的超细球形氧化铝具有表面致密光滑、分散性好等特点,本工作以超细球形氧化铝为原料,通过浸渍提拉烧结法,制备了孔径分布窄、渗透通量高的陶瓷超滤膜,研究了烧结温度对陶瓷膜微孔结构的演化、孔径分布和渗透通量的影响。随后对1250℃下烧结的陶瓷膜进行了纳米硅水分散液过滤处理,采用不同堵塞模型分析了陶瓷膜过滤纳米硅水分散液的膜污染过程。结果表明,通过调节烧结温度调控陶瓷膜的微孔结构,当烧结温度为1250℃时,陶瓷膜的孔径分布较窄,孔径大小为25?65 nm,渗透通量为986.4 L/(m2?h)。超细球形氧化铝粒径分布较窄及表面致密光滑有助于1250℃下烧结形成均匀的烧结颈,提供了陶瓷膜较窄的孔径分布。对1250℃下烧结的陶瓷膜进行了纳米硅水分散液过滤处理后其浊度下降为0.231 NTU,浊度去除率达99.96%。采用不同堵塞模型分析了陶瓷膜过滤纳米硅水分散液的膜污染过程,结果表明,纳米硅水分散液的堵塞模型是滤饼过滤,属于可逆污染。     

Influence of Particle Size Distribution of Bimodal Reactive Alumina on Properties of LCC Refractory Castables

The effect of particle size distribution of alumina has been investigated for silica-free tabular alumina low cement castables( LCC). Three different combinations of alumina have been included in the matrix formulation of the castables. All the three combinations are composed of a bimodal reactive alumina and a fine ground monomodal reactive alumina. The first A1 and second A2 combinations are respectively composed of bimodal and monomodal aluminas from Alteo,with a different fine /coarse particles ratio for the bimodal alumina. The two Alteo combinations have been compared with a third combination C composed of a bimodal commercially available grade and a monomodal commercially available grade. Optimization of particle size packing has been performed for the three different formulations using the Dinger and Funk model. With this optimization,the two formulations based on Alteo material( PFR,PBR and PFR40) achieve the same level of performance in applicative tests( flowability,cold physical properties,mechanical resistance,crystalline phases,thermal shocks and corrosion) as reference solutions on the market.     

Improved Equation of the Continuous Particle Size Distribution for Dense Packing

The Furnas model describes the discrete particle size distribution for densest packing. Using a model that considers a continuous particle size distribution for the densest packing to be a mixture of infinite Furnas discrete particle size groups, an equation for the cumulative particle size distribution providing the densest packing was derived. Monosize particles with different shapes have a different packing pore fraction. One parameter in the equation is the pore fraction of packed monosize particles; the particle size distribution for achieving densest packing is a function of this pore fraction. A reduced form of this equation is also presented as a working equation. The equation derived here is compared to the modified Andreasen equation for dense packing. An equation and the correlated graph for calculating theoretically the geometric mean particle size and an equation for calculating the specific surface area of the particle size distribution of the improved equation are also derived.     

颗粒粒径和膜孔径对陶瓷膜微滤微米级颗粒悬浮液的影响

通过测定颗粒悬浮液通过陶瓷微滤膜时的参透通量及污染阻力,确定了陶瓷膜处理微米级颗粒悬浮液时,颗粒粒径和膜孔径对微滤过程的影响和膜污染机理,获得了微米级颗粒悬浮液微滤过程中膜孔径的选择方法。     

Effect of Pore Size and Particle Size Distribution on Granular Bed Filtration and Microfiltration

Abstract

The paper reviews the effect of particle size distribution and pore size distribution on granular bed filter and crossflow microfiltration performance. The experimental results of the granular bed filter with pollen particles in suspension showed that the presence of large particles improved the filter efficiency of smaller particles in suspension. Microfiltration results with bi and tri‐modal latex suspensions showed that the permeate flux and the quality were significantly affected by the particle size and its distribution, especially when the particle size was smaller than the pore size of the membrane. The mathematical model simulation results of granular bed filtration show that media pore size distribution is an important parameter of filtration for the particle removal and pressure drop across the filter.     

Three-dimensional printing of high-flux ceramic membranes with an asymmetric structure via digital light processing

In this study, a novel method was proposed for preparing high-flux ceramic membranes via digital light processing (DLP) three-dimensional (3D) printing technology. Two different alumina powders were well dispersed in a photosensitive resin to form a UV-curable slurry for DLP 3D printing. The effects of the grading ratio on the viscosity of the slurry and the porosity, pore size distribution, mechanical strength, roughness, and permeability of the ceramic membranes were systematically investigated. The thermal treatment conditions were also studied and optimized. The obtained ceramic membranes exhibited a uniform pore size distribution, a high porosity, a low tortuosity factor, and an asymmetric structure. The combination of these factors led to a high flux for the 3D-printed ceramic membranes. DLP 3D printing exhibited a good potential to be a strong candidate for the next generation of ceramic membrane fabrication technology.     

Particle Size Distribution of Coprecipitated Mn-Zn Ferrite Powders

The particle size distribution of 0.07- to 0.35-μm powders was measured by quantitative electron microscopy using an areal analysis. Measurements of at least 15 particles were required to characterize each size distribution. The specific surface area calculated from the size distributions satisfactorily agreed with that measured by the BET method. For the powders with surface area of 4.4 to 9.7 m²/g, the particle size distributions were generally narrow. In many cases the distributions were near log normal.     

Spheroidization of low-cost alumina powders for the preparation of high-flux flat-sheet ceramic membranes

Two kinds of low-cost alumina powders with irregular morphology were pretreated by spheroidization and the two spherical powders were used to prepare high-flux flat-sheet support and microfiltration (MF) membrane with high separation accuracy, respectively. It was found that the spheroidization pretreatment not only unified the morphology of alumina powder particles into spherical shape, but also narrowed the particle size distribution of the powders, which both were conducive to optimizing the performance of the as-prepared ceramic membranes. After sintering at 1350 °C, the open porosity, bending strength, average pore diameter and pure water permeability of alumina flat-sheet support from spheroidized alumina coarse powder were 44.3%, 36.3 MPa, 3.3 μm and 3240 L/h m² bar, respectively. The slurry derived from spheroidized alumina fine powder was dip-coated on the flat-sheet support to prepare MF membrane. The crack-free MF membrane with a thickness of 23.5 μm had a pore diameter of 0.12 μm and pure water permeability of 850 L/h m² bar. Additionally, the elaborated MF membrane was used to clarify aqueous suspension of carbon black with the maximum rejection rate of up to 99.7%, exhibiting excellent cleaning performance at the same time by completely restore the virgin permeate flux after backwash.     

Gel Casting of Free‐Shapeable Ceramic Membranes with Adjustable Pore Size for Ultra‐ and Microfiltration

The growing demand of reliable high‐performance membrane materials for separation processes requires new simple, straightforward, environmental friendly, sustainable approaches for membrane fabrication. In this study, we present an environmentally friendly gel‐casting, one‐pot process based on ionotropic‐gelation for obtaining alumina membranes. A slurry of alumina particles and the biopolymer alginate, which acts in combination with calcium iodate like a resin, was gelled in a controllable temperature dependent manner. Alumina membranes are obtained by three different shaping routes (extrusion, free‐forming, casting). The suitability of extruded capillaries in a polymer‐ceramic hybrid state (green body) and after sintering (1150°C for 2 h) for potential application in micro‐ and ultrafiltration is evaluated by monitoring the chemical and mechanical stability, permeability and separation behavior. Varying the initial alumina particle size from 200 to 900 nm, membranes with a narrow pore size distribution, predictable and tunable average pore diameters from 70 up to 480 nm and a constant open porosity of ~40%, are obtained. The permeability behavior is tested with fluorescence labeled submicron‐ and nano‐particles. Our novel colloidal processing route represents a very versatile tool for designing and manufacturing ceramic membranes with complex shapes for micro‐ (>0.1 μm) and ultrafiltration (0.1–0.01 μm).     

Effect of sintering temperature on functional properties of alumina membranes

Supported membranes were prepared from different submicron alumina powders. The evolution of pore size, hardness and permeability were monitored after sintering the films at temperatures ranging from 1000 to 1400 °C. These functional properties and the microstructure of the films were compared with the free-standing membranes. Sintering at temperature range from 1000 to 1200 °C maintained the narrow, monomodal pore size distribution of the supported membranes. The effect of sintering temperature on the hardness of the membranes was weak. The permeability was also independent on the sintering temperature. When sintering temperature was raised up to 1300 and 1400 °C, the pore size increased significantly and distribution was changed to bimodal containing fraction of large pores. The hardness of the membranes increased while significant densification was not observed. Permeability increased due to the large pore size and the high porosity. In sintering of the free-standing membranes pore size remained almost unchanged, density increased when sintering temperature was raised, hardness was dependent on the density and permeability decreased continuously. The substrate did not have effect on the grain growth, which was dependent on the sintering temperature. Evolution of the properties of the free-standing membranes suggests local densification. The rigid substrate restricts the sintering shrinkage leading to densification of small areas. This local densification opens large flow channels between agglomerates. This increases the pore size, broadens the pore size distribution and increases the permeability. The macroscopic densification of the film is small.     

Cyclic cold isostatic pressing and improved particle packing of coarse grained oxide ceramics for refractory applications

This study investigated the cold isostatic pressing of coarse grained alumina refractories applying either a cyclic pressure increase or a cycling at maximum pressure. Additionally the effects of the maximum pressure and the particle size distribution on physical, mechanical and thermomechanical properties were analyzed. The cyclic pressure increase resulted in a slightly higher apparent density and lower apparent porosity. A cycling at maximum pressure decreased the median pore size to some extent. Remarkably, an optimized particle size distribution resulted in a lower apparent porosity, lower median pore size and in a higher Young's modulus before and after thermal shock together with a slightly lower relative decrease of the Young's modulus. A higher pressing pressure which decreased the apparent porosity did not affect the Young's modulus. Thus, apparently the optimized particle size distribution improved the particle packing which was associated with a smaller median pore size. This smaller pore size increased the number of pores relative to the total porosity, which then acted as points of crack initiation and crack deflection limiting the length of propagating cracks in case of thermal shock. Thus, tailoring the pore size distribution is a promising starting point to improve the thermomechanical properties of refractories.     

Effect of Particle Size Distribution on the Sintering of Alumina

The effect of particle size distribution on the sintering of Al₂O₃ was investigated. Samples could be sintered to high relative density (∼99%), small average grain size (1 μm), and no growth of exaggerated grains using powders with either broad or narrow particle size distribution. However, the broad particle size distribution provided the advantage that powder compacts could be prepared with higher green density and, therefore, samples could be densified with less total shrinkage.     

支撑体孔径大小对Al2O3微滤膜完整性的影响

无机微滤膜不仅具有优良的热稳定性、机械稳定性和结构稳定性,而且化学稳定性高,耐腐蚀,不会被微生物分解,使用寿命较长,易于清洗和再生,更重要是无机微滤膜无毒．因此,它在食品、生化制药、催化反应等领域中作为物料的预处理和催化载体有着广阔的应用前景．然而,无机微滤膜真正起作用的是一层薄膜,     

Monoclinic Zirconia Microfiltration Membranes: Preparation and Characterization

Microfiltration zirconia membranes were prepared by slip casting from two pure zirconia powders derived from different processing techniques. Powders had almost the same mean particle size but were different in surface area, particle size distribution and morphology. Rheology of zirconia slips was studied in order to prepare a well-dispersed slip suitable for slip casting. The powders showed different dispersibility in the preparation of slips by colloidal processing. The effect of sintering temperature and holding time on porosity, pore size distribution, phase composition, microhardness and microstructure of unsupported membranes are studied and discussed in relation to the membrane processing and properties of powders resulting from different processing routes. Pore size distribution of membranes reflected the differences in morphology of particles and the state of agglomeration in the green samples.Isothermal sintering at 1100°C resulted in some tetragonal phase retained at room temperature in the monoclinic structure. Cracking occurred in membranes sintered above 1150°C due to the volume change in phase transformation. Densification behavior, removal of porosity and the hardness property showed differences that are attributed to the differences in powder processing and characteristics of powders. Crackfree membranes can be prepared by sintering at 1100°C from both powders.     

Modeling of the Relationship Between Pore Size Distribution and Thickness of Ceramic MF Membrane

The pore size distribution(PSD)measured by the gas bubble point(GBP)method ofceramic microfiltration(MF)membranes prepared by suspension technique was found to be signifi-cantly influenced by the membrane thickness.A culm-like model for pore structure was introduced tocharacterize the membrane pores instead of the conventional model which does not reflect the radiusvariation along the pore passages and is unable to explain the thickness effect on the membrane PSD.A laminate structure,taking the culm-like model for pore structure into consideration,was hypoth-esized for ceramic MF membranes.A mathematical model was then established to quantitativelydescribe the relationship between the membrane number PSD and the membrane thickness.Goodresults were obtained for the correlation of mean pore size and simulation of the PSD for ceramicMF membranes.     

Influence of solid loading and particle size distribution on the porosity development of green alumina ceramic mouldings

Alumina ceramic mouldings with different solid contents ranging from 55 to 70 vol% and different ratios of coarse/fine powders, i.e. 0.4 μm (fine) and 3 μm (coarse), respectively, were prepared by compression moulding at 75 °C under a compressive stress of 10 MPa. The porous parameters, such as porosity, pore size and pore size distribution, of the green compacts were evaluated after removal of organic vehicles. Experimental evidence showed that the green density, as well as the sintered density, of the moulded alumina increased linearly with increased solid loading to an optimum of 65 vol% and decreased roughly linearly with increased coarse/fine ratio. Further increase in solid loading reduced particle packing efficiency, resulting in lower green and fired densities. No considerable improvement in green and sintered density of the moulded alumina was achieved by adjusting the coarse/fine ratio, which is due to the fact that coarse particles suppress the driving force of densification. The green compacts generally showed a bimodal pore size distribution character which may be the most important factor in dominating the densification of the powder compacts. The peak frequency at larger pore region is approximately 20–35 μm in diameter and at the smaller pore region is ˜50–95 nm in diameter. The larger pores are believed to be due to the presence of internal voids originating from entrapped gas and are probably caused by the removal of organic vehicles.