Compaction Behavior of Spray-Dried Alumina

Compaction behavior and resultant porosity of spray-dried alumina were examined over a range of pressures from 18 to 345 MPa. The variability in pressed density and pore size was measured as a function of spray-dried granule size, binder concentration, and powder moisture content. An exponential behavior was found between pressed density and compaction pressure, density increasing with the logarithm of the compaction pressure. Pore size also displays an exponential behavior, pore diameter decreasing with the log of increasing pressure. The distribution width about the median pore size was noted to decrease approximately in a log-log response to increasing compaction pressure. The behavior of the compaction and porosity curves is related to the degree to which the polymer binder is plasticized which, in turn, affects the pressure at which the spray-dried granules begin to crush. This apparent yield pressure, although dependent on amount of binder and powder moisture, is intrinsically dependent on the water/binder ratio. Finally, by analogy to soil mechanics, an empirical equation relating compact density, yield pressure, and slope is presented.     

Effect of freeze-drying treatment on the optical properties of SPS-sintered alumina

This study looks at the influence of alumina powder processing on the preparation of transparent alumina by Spark Plasma Sintering (SPS). Zeta potential measurements were carried out on alumina suspensions in order to determine the best dispersion conditions. Stable slurries were submitted to a spray freeze drying process and their sintering behavior was compared with the corresponding non spray freeze dried powders. Transparent alumina samples were successfully prepared from alumina powders by Spark Plasma Sintering. An optical model considering pore and grain size distributions has been developed to obtain information about porosity in dense materials. It was found that the final density and, accordingly, the optical properties were improved when spray freeze dried starting powder was used.     

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.     

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.     

Powder Processing for the Fabrication of Si3N4 Ceramics: I, Influence of Spray-Dried Granule Strength on Pore Size Distribution in Green Compacts

The effect of spray-dried granule strength on the micro-structure of green compacts obtained by isostatic pressing was quantitatively analyzed. The fracture strength of single granules of Si₃N₄ powder made with ultrafine A1₂O₃ and Y₂O₃ powders was measured directly by diametral compression. It was found that fracture strength increased notably with the increasing relative density of the granule and the decreasing size of agglomerates in suspension before spray-drying. Even when green bodies were prepared at an isostatic pressure of 200 MPa, intergranular pores, which negatively affected densification of the sintered bodies, occurred between unfractured granules. The volume and size of these pores in the green compacts increased with the increasing fracture strength of the granules. In the case of closely packed granules, an isostatic pressure of 800 MPa was required to completely collapse the intergranular pores. A simple equation was derived to calculate the isostatic pressure necessary for complete collapse of intergranular pores in the green compacts, and it was determined that granule strength must be kept as low as possible to obtain uniform green compacts.     

Influence of Dryer Type on Surface Characteristics of Milk Powders

Reconstituted milk powders (skim milk, whole milk, and milk protein concentrate powders) were spray dried using research-scale (laboratory- and pilot-scale) spray dryers to investigate the influence of type on the dryer on the surface composition (protein, fat, lactose) and morphological characteristics (size and surface structure) of the powder particles. Milk powders produced by these research-scale dryers were compared to commercially produced and freeze-dried powders. The powders produced by the laboratory- and pilot-scale dryers were significantly different from the commercially dried powders in both surface composition and morphology. The milk powders produced by laboratory- and pilot-scale dryers provided reproducible results with similar surface morphologies between dryer types, despite varying surface compositions. The surface composition of the freeze-dried powder was also significantly different from than that of the spray-dried powders. The freeze-dried skim milk powder (SMP) was similar in surface protein to its bulk protein composition, indicating relative homogeneity of particle composition of the freeze-dried powder.     

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.     

氧化锆料浆性能对其喷雾造粒粉料性质的影响

本文研究了料浆含固量和粘度对其喷雾造粒粉料性质影响。结果表明：氧化锆料浆含固量是喷雾造粒（ＳＤ．）粉料填充密度的主要控制因素，高含固量料浆能得到高填充密度喷雾造粒粉料，且其颗粒显微结构相对致密；随着ＺｒＯ２料浆含固量、粘度增加，喷雾造粒粉料平均粒径增大，粗颗粒含量增多，细颗粒含量减少。     

Characteristics of Alumina Powders Prepared by Spray-Drying of Boehmite Sol

Boehmite sol prepared from aluminum nitrate has been spray-dried to obtain micrometer-size spherical particles consisting of submicrometer crystallites. The spray-dried powder was further washed with solvents of varying polarities such as acetone, 2-propano1, and 2-methyl-2-propanol. Particle-size distribution, morphology, density, compaction, and sintering characteristics of powders washed with different solvents are reported. The effect of posttreatments on the boehmite-sol-derived powders toward reducing agglomeration and obtaining high-density bodies is discussed.     

Three-Stage Spray Drying: New Process Involving Instant Controlled Pressure Drop

The goal of this article is to define a new industrial operation called three-stage spray drying that can increase the specific surface area of powder while reducing the amount of fine dust. Because of their compact structure, spray-dried granules have an exchange surface limited to their surface area. We performed experiments inserting the instant controlled pressure drop (DIC®) treatment between the atomization (first stage of spray drying) and the final drying stage. As a high-temperature, short time (HTST) process, DIC treatment expanded granule texture at a rate depending on pore distribution, mesopore volume, and the mean porosity thus generated; the cumulative specific surface area thus induced evolved as a function of the DIC treatment conditions: the higher the DIC steam pressure, the higher the expansion rate. Both specific surface area and mean particle diameter may then simultaneously increase. Technological properties were investigated in order to compare DIC textured powders and conventional spray-dried powders and optimize the treatment; such an optimization can include the rate of decontamination thus generated.     

Three-Stage Spray Drying: New Process Involving Instant Controlled Pressure Drop

The goal of this article is to define a new industrial operation called three-stage spray drying that can increase the specific surface area of powder while reducing the amount of fine dust. Because of their compact structure, spray-dried granules have an exchange surface limited to their surface area. We performed experiments inserting the instant controlled pressure drop (DIC®) treatment between the atomization (first stage of spray drying) and the final drying stage. As a high-temperature, short time (HTST) process, DIC treatment expanded granule texture at a rate depending on pore distribution, mesopore volume, and the mean porosity thus generated; the cumulative specific surface area thus induced evolved as a function of the DIC treatment conditions: the higher the DIC steam pressure, the higher the expansion rate. Both specific surface area and mean particle diameter may then simultaneously increase. Technological properties were investigated in order to compare DIC textured powders and conventional spray-dried powders and optimize the treatment; such an optimization can include the rate of decontamination thus generated.     

Sintering of magnesium hydroxide obtained from magnesium chloride solutions

Conclusions We studied two batches of magnesium hydroxide obtained by precipitating out (using dolomite milk) from magnesium chloride solution formed when processing potassium ores.The effect of the compaction pressure, the firing temperature, and prior heat treatment on the sintering process of magnesium hydroxide was investigated.The experimental samples of magnesium hydroxide exhibit high sinterability and facilitate the production of periclase powders (powder bodies) having a porosity of 6.8–9.9% at a firing temperature of 1600°C. The degree of sintering of magnesium hydroxide increases with increasing compaction pressure and firing temperature. Prior heat treatment of the material at 800–1000°C intensifies the sintering process with simultaneous reduction of shrinkage.The studies conducted on the specimens prepared from a fired briquette established that the periclase (magnesite) powder obtained from magnesium hydroxide is suitable for the production of magnesia refractories.A. V. Kushchenko and G. G. Eliseeva (UkrNIIO) participated in this investigation.Translated from Ogneupory, No. 2, pp. 7–10, February, 1988.     

A Taguchi approach production of spray-dried whey powder enriched with nanoencapsulated vitamin D3

Abstract

The objective of the present study was to investigate the effect of inlet air temperature of spray drying and different combinations of carrier agents (maltodextrin (MD), gum Arabic (GA), modified starch (MS), and whey protein concentrate (WPC)) on the physicochemical characteristics of spray-dried whey powder, enriched with vitamin D₃ to improve its usage as a functional ingredient. Firstly, vitamin D₃ was nanoencapsulated by nanoliposome prepared with egg yolk lecithin, sesame oil, and glycerol through thin-film dispersion method. The mean particle size of prepared nanoliposomes was 140?nm. Then, the prepared nanocarriers loaded with vitamin D₃ were added into the feed solution and dried through spray dryer. The effect of carrier agent types and inlet air temperature on the physicochemical (moisture content, solubility, porosity, color, and powder yield) and microstructure properties of obtained spray-dried powders were investigated. The optimal carrier agents and condition of spray drying were selected by Taguchi design. Our results showed that the inlet air temperature and carrier agent had significant effects on the characterization of powders. Powders produced by 2% WPC, 3% MS, and 25% MD at 170?°C inlet air temperature showed the highest powder yield (96.4%). Also, the morphology of powders was affected by carrier agent types; increase in MD concentration in feed solution causes to create smoother and spherical spray-dried powder particles.     

Advancing spray granulation by ultrasound atomization

The influence of the atomization technique on the suitability of granules for dry pressing is the focus of the presented investigations. Therefore, destabilized alumina, zirconia, and zirconia toughened alumina (ZTA) slurries were spray dried and the obtained granules were used to fabricate green and finally sintered bodies for evaluation. Granules made in a laboratory spray dryer with a two-fluid nozzle served as a reference. An ultrasonic atomizer was integrated into the same spray dryer and the influence on the granule properties was evaluated. Untapped bulk density, granule size distribution, and flowability are among the evaluated granule-related properties as well as the granule yield which is used as an indicator of the process efficiency. Yield and flowability as most important granule properties are clearly improved when atomization is realized with ultrasound. The investigated sinter body properties include porosity, sinter body density, and biaxial strength and are as well positively affected by switching the atomization technique to ultrasound. Therefore, the approach to improve the compressibility of granules by ultrasonic atomization, which leads to an improved microstructure, density, and strength of sintered bodies, has proven to be successful for single-component ceramics (alumina and zirconia) as well as for the multicomponent ceramic ZTA.     

Physicochemical Characterization of Whole Egg Powder Microencapsulated by Spray Drying

Physical characterization and oxidative stability of egg powder microencapsulated by spray drying were studied in this work. The wall material (gelatin, lactose, pullulan, and their mixtures) and liquid egg mixtures were prepared by homogenization at 22,000 rpm for 60 s. The spray drying was carried out at pilot-scale spray dryer (Niro Mobile Minor, Søborg, Denmark). The spray-dried egg powders were analyzed for moisture content, water activity, peroxide value, total cholesterol oxidation products (TCOPs), particle properties, and bulk properties. Using gelatin as wall material resulted in a significant increase in the moisture content and water activity of egg powder during storage and it improved flowability. Egg powders containing pullulan as wall material showed a fibrous structure and had the lowest bulk density. Adding lactose as wall material increased the oxidative stability, which was indicated with lowest peroxide value and TCOPs level of egg powder.     

An Investigation of Milk Powders Produced by a Laboratory-Scale Spray Dryer

ABSTRACT

A mini spray dryer has been used to investigate morphological changes that occur to milk particles during the spray drying process. We have found that the mini spray dryer is ideal for such investigations, because phenomena such as skin and vacuole formation in particles can be analyzed without the added complication of particle agglomeration, which only occurs in much larger spray dryers where particle number concentrations are higher. We have confirmed observations made by various researchers that the bulk density of spray-dried milk powder is greatly affected by the drying temperature, due to the strong influence of the latter on the porosity of the particles. In addition, we have attempted to explain observations made by various workers that fat accumulates preferentially at the surface of a particle during drying by postulating that fluid fat is transported towards the surface, via a network of cracks and pores, by the development of a vacuole overpressure which is also responsible for the inflation of the particle. Finally, we have shown that milk powders can be spray dried a second time, by reconstitution with water, with no change to the thermodynamic characteristics of the resultant powder. Thus, milk concentrates for spray drying research can be prepared from already-spray-dried milk powders rather than using the more arduous evaporation method to concentrate unprocessed milk.     

TiB2/Al2O3复合粉体的喷雾干燥造粒与特性研究

利用喷雾干燥技术对TiB_2/Al_2O_3复合粉体进行造粒,研究了浆料固相含量及粘结剂含量对喷雾干燥粉体颗粒形貌、结构、松装密度、流动性等的影响。结果表明：当浆料固相含量为47．6%,分散剂和粘结剂分别为固相质量的0．4%和1．0%时,浆料具有合适的粘度和最佳的分散稳定性,喷雾造粒得到的粉体为球形或近球形,具有较高的松装密度和流动性,能满足各种压制成型的需要。     

Additional high-energy milling to enhance the performance of porcelain stoneware manufacturing

Porcelain stoneware tile is the best class of ceramic tiles regarding technical performance. Low porosity and high glass content are some of its highlighted characteristics. The manufacturing cost is highly dependent on the feldspar content and the processing flow rate. Certain technical bottlenecks in the manufacturing steps, such as milling, forming, and firing, are intrinsically associated with limitations in the processing properties, such as the dry strength, bulk density, and pyroplastic deformation. In this work, improvements in these properties were achieved using high-energy milling (HEM) after conventional milling (CM). This study was carried out on a pilot industrial scale in the milling stage. Six experimental runs were evaluated. Slurries were spray-dried. The powders were humidified with 6.5% moisture. Specimens were conformed under a specific pressure of 45 MPa. The firing was performed using temperature ranging from 1150 to 1230°C. The use of HEM, in comparison to traditional milling for the similar particle-size distributions, has increased the dry density, +0.2 g.cm⁻³, dry bending strength, +1.0 MPa, and decreased the pyroplastic deformation index, −1.10⁻⁵ cm⁻¹. These results allow an estimated thickness reduction of 10%.     

Comparative study of methods for producing gum arabic powder and the impact of DIC treatment (instant controlled pressure drop) on the properties of the product

In this study, gum arabic powder was produced according to four methods by inserting a restructuring stage by DIC treatment (instant controlled pressure drop) in the classic process of grinding and spray drying. Properties of the final product were compared, and the results show that DIC treatment enables to control and improve the properties of the powder. The DIC treatment can cause a controlled increase in the tapped bulk density, filling rate, compressibility, porosity; and a reduction in interstitial air volume and the loose bulk density. It also facilitated the subsequent grinding and intensified the drying kinetics. The impacts of pressure and DIC treatment time were examined. Pressure was the strongest factor influencing the properties of the gum arabic powder. Selecting an optimal pressure and treatment time plays a decisive role in controlling the properties of powders.