Pore evolution and compaction behaviour of spray-dried bodies for porcelain stoneware slabs

The compaction behavior of spray-dried powders has turned into concern in porcelain stoneware manufacturing due to the increasing diffusion of large slabs. It is necessary to fill a knowledge gap between the compaction behavior with conventional presses and novel technologies. For this purpose, eighteen industrially-manufactured spray dried bodies were characterized for specific properties connected to the compaction behavior (curves of bulk density, intergranular and intragranular porosity in function of applied load, apparent yield strength). In addition, the firing behavior was investigated in order to reveal any effect of dry bulk density on firing shrinkage and bulk density of fired samples. Powder compressibility is within 50% and 55% (Carr index) and is primarily controlled by moisture. Two regimes are found: low pressure (fast density increasing by granule cave in and closure of intergranular porosity) and high pressure (slow density gain by downsizing microporosity). A peculiar mechanism is unveiled: granules squeeze in the low-P regime and further densification is achieved through microfracture around individual agglomerate. A phenomenological model is illustrated for the compaction of spray-dried powders. In conclusion, the performance of spray dried bodies during compaction is crucial to control the uniformity, in terms of porosity and bulk density, which has important repercussions on the properties of final slabs, especially differential shrinkages and deformation during firing due to density gradients.     

Effect of Relative Humidity on the Viscoelastic and Mechanical Properties of Spray-Dried Powder Compacts

Spray-dried powder compacts exhibit viscoelastic properties such as stress relaxation, creep, and delayed elastic strain. This behavior is attributed to the organic binder, which forms bridges between the particles in spray-dried granules, thereby affecting their deformation characteristics. The viscosity and distribution of the binder within the powder compact can affect its mechanical and viscoelastic properties. In this study, the powder was conditioned at different ambient relative humidity (RH) levels, to vary the binder viscosity. Load deformation, stress relaxation, fracture strength, and fracture toughness behavior of ferrite powder compacts were studied as a function of ambient RH both before and after compaction. The loading rate was found to significantly affect the time-dependent response, and the relaxation times decreased at high humidity levels during compaction. It is proposed that increasing the humidity level during compaction increases the number of particle–particle contacts. This simple mechanism of binder redistribution led to slower relaxation times, increases in fracture strength, and elastic modulus of the green bodies, without significantly altering the fracture toughness when powders were compacted at high humidity to a given density.     

Consolidation behavior and hardness of P/M molybdenum

In this study, the consolidation behavior and hardness of commercially available molybdenum powder were investigated. In order to analyze the compaction response of the powder theoretically, an elastoplastic constitutive equation based on the yield function presented by Shima and Oyane was applied to predict the compact density under uniaxial pressure from 100 MPa to 700 MPa. The compacts were sintered at 1400-1600 °C for 20-60 min. The sintered density and grain size of molybdenum were increased with increasing the compacting pressure and processing temperature and time. The effect of the porosity and grain size on the hardness of the specimens was explained based on the modified plasticity theory of porous material and the Hall-Petch type equation.     

Effect of Moisture on the Structure and Fracture Strength of Ceramic Green Bodies

To study independently the effects of moisture on the structure and the mechanical strength of the binder in green bodies, specimens of the system alumina/PVA were formed with spray-dried granules of various moisture contents. The structure and fracture strength of these specimens then were examined after their moisture contents had been adjusted to specified values. As moisture content increased in the granules during compaction, the density and strength of the green body also increased. The accompanying change in the fracture mode, from intergranular to transgranular, showed that the strength of the green bodies was affected more significantly by bonding between granules than by bonding between powder particles.     

Effect of Pressing Method on Organic Burnout

Sintered Y-TZPs formed using cold isostatic compaction exhibit a lower sintered density and more porosity than ceramics formed using conventional uniaxial die compaction, although the isostatically pressed powder compact has a higher and more uniform green density. For the 3 wt% PEG1500-doped zirconia powder, the sintered density decreases in a near-linear manner with increasing isostatic pressing pressure. It was identified that the low sintered density and the poor microstructure were due to the incomplete burnout of PEG1500 at the low and intermediate temperatures when the powder compacts were heated at a rate of 3°C/min. The delayed organic burnout at temperatures close to and/or at the sintering temperature results in the formation of largely swollen intergranular pores.     

喷雾造粒ZrO2粉料坯体性能的研究

以喷雾造粒ＺｒＯ２粉料为研究对象,通过对粉料的压力－密度曲线及坯体的ＳＥＭ显微结构分析,发现喷雾造粒粉料的粒度分布对坯体密度的影响较小;颗粒强度的大小是获得均匀的坯体结构的关键,颗粒的强度与其大小及环境湿度有关,因此颗粒适当的增塑及去除大颗粒均有利于坯体显微结构的改善。     

Fabrication and characteristics of porous Ni and NiO(Li) cathodes for MCFC

In-situ Ni andex-situ NiO(Li) cathodes were fabricated by cold pressing using Ni powder and Li₂CO₃ (in case ofexsitu cathode) with paraffin wax as a binder. The effects of compaction pressure, amount of binder, and sintering temperature on porosity, the average size of pore, Li^* cation fraction, and the fracture strength were investigated in this study. The optimum compaction pressure was 100 kg/cm² to prevent the brittleness and stress concentration caused by high compaction pressure. Also, 10 wt% of binder yielded best results and the strength decreased dramatically and revealed nonuniform pore and pore distribution beyond 10 wt%. To obtain reasonably high electric conductivity inexsitu cathode, the sintering temperature was chosen to be below 950°C to maintain the ration fraction of Li* is in the range of 0.02–0.06. In terms of the Ni-dissolution rate,exsitu cathode was more efficient thaninsitu cathode in the long-term operation except the initial 24hr period.     

Industrial Quantitative Control of the Pressing Behavior of Spray-Dried MnZn-Ferrite Granules

In the first stage of a broad factory stabilization program, the compaction properties of spray-dried granulated powders are investigated. Certain compaction process parameters are identified and include (i) the slide coefficient between powder material and die wall during compaction, which mainly affects the pressing tool life time, (ii) the ratio of the pressure drop over the compact to the axial mechanical strength of the compact, basically related to the chance of chipping and crack occurrence upon ejection, and (iii) the homogeneity of the density profile along the compact, basically related to the chance of crack development and product deformation during sintering. The effect of important factors, such as binder and lubricant content, granulate storage humidity, and compaction temperature, on those parameters is investigated. Based on factory data, specification values for the previously mentioned parameters are derived and used to control the compaction quality of the industrially spray-dried powders with satisfactory results.     

The compaction and mechanical properties of agglomerated materials

Following a discussion of the stages of powder compaction as presented in the literature, the authors propose extension of the generally accepted two stage compaction process to a four stage process for agglomerated materials. The mechanisms of compaction for two different spray-dried ceramic powders, a wall-tile granulate, and a ferrite granulate are described. After an adaptation of the compaction formulae of Kawakita for the highly porous spray-dried granulates a set of equations with a better fit is given, describing the relationships between pressure and volume compaction or density, and between porosity and strength and modulus of elasticity. All proposed equations are closely related to Kawakita's empirical equation and the theoretical relationship of Hasselman, and give an accurate fit over the whole range of pressures.     

Application of partial sintering of waste glasses for preparation of porous glass bodies

Porous glasses were prepared by partial sintering of waste glasses. Polyvinyl alcohol was added as a binder to the glass powder and the mixture was un-axially cold pressed under two different forces, followed by sintering at 700 °C. The effects of thermal history, particle size of glass powder, binder content and applied pressing forces on pore size and total porosity of fabricated porous glasses were investigated and final products with the porosity of 15–32 % were prepared. The average pore size of the specimens was determined using mercury porosimetry. The morphology of the porous glasses was observed by scanning electron microscopy. These produced porous glasses can be used for selective and accurate filtration.     

Material characteristics affecting formcoke

The influence of aggregate and binder phase characteristics on formcoke products has been studied by investigating the compaction kinetics of the system and determining the mechanical strength of the briquettes produced. The char phase was characterized in terms of density, hardness and porosity and the binder phase with respect to rheological properties. Results indicate that binder phase fluidity affects compaction viscosity during the particle flow stage of compaction and that char porosity influences final briquette bulk density by affecting the amount of total compaction required to obtain a given bulk density. In general, increased total compaction was shown to result in higher product bulk density with the attendent higher gross composite strength. The latter relationship was seen to be approximately linear over the range of bulk porosity found in this study. A higher briquette strength was found for systems with aggregates carbonized at lower temperatures. Similarly the binder phase fluidity was also seen to affect briquette strength, higher fluidity resulting in higher strength. It was concluded that this was due to increased binder penetration in the highly porous char carbonized at lower temperatures. With no significant pore structure in the aggregate, as found with high temperature char, briquette strength was seen to become approximately constant for the three binder coals used.     

Experimental modelling of copper foams processed through powder metallurgy route using a compressible space holder material

The present work is focused on the processing of open cellular copper foams through space holder technique without the use of binders. In this work, moderate pressures were used during the cold compaction of the powders. The main objective was to obtain dense cell walls by limiting the use of binders and use a compressible and lubricant type of space holder material. It has been shown in this study that the use of high compaction pressure helps to decrease/limit the quantity of binder required and this, in turn, yields relatively dense cell walls necessary for better mechanical strength of foams. Using 2N factorial method, mathematical models have been developed to express the final porosity and pore size as functions of the various processing parameters viz compaction pressure, sintering temperature/ time and space holder content. The most significant sintering parameters influencing the porosity and pore size of the processed foams have also been found out.     

Fabrication and characterization of silica ceramic compact prepared using Aloe-Vera mucilage as a binder

In this study, silica compacts were fabricated through a powder processing route at different compaction pressure, using Aloe-Vera (AV) mucilage as a binder. The silica compacts were prepared at 90, 100, and 110 MPa compaction pressure using 0%–16 wt% of AV binder. The optimum amount of AV binder was 14 wt% for both 90 and 100 MPa and 12 wt% for 110 MPa. The maximum achieved green density and green strength of silica compacts at the optimum binder amount were 62.3% and 4 MPa, respectively at 110 MPa compaction pressure. The green silica compacts prepared at 110 MPa compaction pressure exhibited a minimum porosity of 21% and maximum flexural strength of 15 MPa after sintering at 1400°C. The green silica compacts with the optimum amount of binder were strong enough for machining. The Fourier transform infrared spectroscopy analysis revealed the functional groups present in AV mucilage. The binder burnout characteristic of AV mucilage in the silica compact was determined by thermogravimetric analysis and differential thermal analysis. Additionally, AV gel acted as a binder and solvent simultaneously for ceramic compaction.     

Compaction behavior of Al6061 powder in the semi-solid state

Semi-solid powder processing involves compaction of metallic alloy powders in temperature ranges when both solid and liquid phases coexist. However, modeling of such process has been very scarce. In this study, compaction behavior of Al6061 powder in the presence of liquid phase was investigated. The relationship between compaction pressure and relative density of powder in the semi-solid state was modeled and verified against experimental measurements. The results showed that the powder compaction behavior can be accurately predicted by Shima-Oyane model when the liquid fraction was below 20%. In this range, all the normalized pressure-relative density curves merged into one, which could be expressed in a simple exponential form. When the liquid fraction was higher than 20%, the model failed to predict the compaction behavior because of the non-uniform distribution of the liquid phase. Squeezing-out of the liquid phase and interlocking of the irregular solid phase were speculated to occur during the compaction process.     

Effect of Externally Applied Plasticizer on Compaction Behavior of Spray-Dried Powders

The effects of an externally applied plasticizer on compaction behavior and green microstructure quality of spray-dried powders was investigated. The plasticizer was applied to the external surfaces of already spray-dried powders by spraying it on tumbling spray-dried granules. The apparent yield point of the spray-dried powder was reduced when the plasticizer was added. Microstructures of compacts made from these granules (with and without the externally applied plasticizer) were compared at different compaction pressures. Better knitting across granule interfaces and fewer defects were obtained for the granules with the externally applied plasticizer.     

Cleaner production of porcelain tile powders. Fired compact properties

A new ceramic powder preparation process, the droplet-powder granulation process (DPGP), was recently proposed for the cleaner production of ceramic tiles. The DPGP granules and resulting pressed compacts were characterized and compared with the granules and compacts obtained by spray-drying (SD) and dry granulation (G) processes in a previous paper. The results showed the feasibility of using the DPGP in the pre-firing stage of porcelain tile manufacture.This study compares the firing behaviour and fired properties of compacts pressed from three different types of granulated powders: DPGP, SD, and G and from a non-granulated powder (NG) obtained by dry milling. The evolution of compact microstructure (porosity and pore size distribution) with firing temperature was monitored and the fired compact properties (bulk density, water absorption, and stain resistance) were determined.The study shows that the DPGP improved the sintering behaviour and final properties of the resulting porcelain tiles with respect to those obtained by the G process. However, the fired compacts prepared from the DPGP powder exhibited a higher porosity and pore size compared with those of the compacts obtained from the SD granules at the same pressing pressure. The results obtained open up the possibility of manufacturing glazed porcelain tiles with a more eco-friendly process. However, the results also indicate that polished porcelain tile manufacture by the DPGP requires further research in order to improve granule characteristics, in particular green granule deformability, which is the critical factor in porcelain tile densification and vitrification during firing.     

Compaction behaviour of agglomerated alumina powders

The effects of agglomerate properties, such as the binder type, binder content, moisture level, and agglomerate size, on a model compaction process was investigated by using green density-pressure interrelationships for a range of agglomerated alumina powders. The model compaction process involved single ended nominal uniaxial stress transmission in a cylindrical die. The influences of the sample aspect ratio, die wall lubrication, and compaction rate were also investigated. Two types of water soluble polymeric agents, a poly(vinyl alcohol) (PVA) and a poly(ethylene glycol) (PEG), were used. It was shown that certain agglomerate properties have a strong influence upon the compaction behaviour of these ceramic powders. The extent of the compaction is enhanced by using agglomerates with a low agglomerate yield point. In the PVA system, the agglomerate yield points decreased with increasing moisture content. The compaction behaviour of the agglomerates showed a rate dependency, that is, the compaction is retarded with increased pressing rate. The green densities of the compacts prepared in the unlubricated die were lower than those of the compacts prepared in the lubricated die due to the higher wall frictional forces operating in the unlubricated die.     

Selection of operational parameters for the production of instant soy protein isolate by pulsed fluid bed agglomeration

The objective of this study was to select the optimal operational conditions for the production of instant soy protein isolate (SPI) by pulsed fluid bed agglomeration. The spray-dried SPI was characterized as being a cohesive powder, presenting cracks and channeling formation during its fluidization (Geldart type A). The process was carried out in a pulsed fluid bed, and aqueous maltodextrin solution was used as liquid binder. Air pulsation, at a frequency of 600 rpm, was used to fluidize the cohesive SPI particles and to allow agglomeration to occur. Seventeen tests were performed according to a central composite design. Independent variables were (i) feed flow rate (0.5-3.5 g/min), (ii) atomizing air pressure (0.5-1.5 bar) and (iii) binder concentration (10-50%). Mean particle diameter, process yield and product moisture were analyzed as responses. Surface response analysis led to the selection of optimal operational parameters, following which larger granules with low moisture content and high process yield were produced. Product transformations were also evaluated by the analysis of size distribution, flowability, cohesiveness and wettability. When compared to raw material, agglomerated particles were more porous and had a more irregular shape, presenting a wetting time decrease, free-flow improvement and cohesiveness reduction.     

Amino acid-modified spray-dried powders with enhanced aerosolisation properties for pulmonary drug delivery

In this study, the amino acids arginine, aspartic acid, leucine, phenylalanine and threonine were investigated as ‘dispersibility enhancers’ in spray-dried powders for inhalation. Parameters such as spray-dried yield, tapped density, and Carr's Index were not predictive of aerosolisation performance. In addition, whilst the majority of amino acid-modified powders displayed suitable particle size distribution for pulmonary administration and potentially favourable low moisture content, in vitro particle deposition was only enhanced for the leucine-modified powder. In summary, leucine can be used to enhance the dispersibility and aerosolisation properties of spray-dried powders for pulmonary drug delivery.