Micronization of salicylic acid and taxol (paclitaxel) by rapid expansion of supercritical fluids (RESS)

The particle sizes of the pharmaceutical substances are important for their bioavailability. The bioavailability can be improved by reducing the particle size of the drug. In this study, salicylic acid and taxol were micronized by the rapid expansion of supercritical fluids (RESS). Supercritical CO₂ and CO₂ + ethanol mixture were used as solvent. Experiments were carried out to investigate the effect of extraction temperature (318–333 K) and pressure (15–25 MPa), pre-expansion temperature (353–413 K), expansion chamber temperature (273–293 K), spray distance (6–13 cm), co-solvent concentration (ethanol, 1, 2, 3, v/v, %) and nozzle configuration (capillary and orifice nozzle) on the size and morphology of the precipitated salicylic acid particles. For taxol, the effects of extraction pressure (25, 30, 35 MPa) and co-solvent concentration (ethanol, 2, 5, 7, v/v, %) were investigated. The characterization of the particles was determined by scanning electron microscopy (SEM), optical microscopy, and LC–MS analysis.The particle size of the original salicylic acid particles was L/D: 171/29–34/14 μm/μm. Depending upon the different experimental conditions, smaller particles (L/D: 15.73/4.06 μm/μm) were obtained. The particle size of taxol like white crystal powders was reduced from 0.6–17 μm to 0.3–1.7 μm The results showed that the size of the precipitated salicylic acid and taxol particles were smaller than that of original particles and RESS parameters affect the particle size.     

Influence of silicon carbide particle size on the microstructure and mechanical properties of zirconium diboride–silicon carbide ceramics

The influence of silicon carbide (SiC) particle size on the microstructure and mechanical properties of zirconium diboride–silicon carbide (ZrB₂–SiC) ceramics was investigated. ZrB₂-based ceramics containing 30 vol.% SiC particles were prepared from four different α-SiC precursor powders with average particle sizes ranging from 0.45 to 10 μm. Examination of the dense ceramics showed that smaller starting SiC particle sizes led to improved densification, finer grain sizes, and higher strength. For example, ceramics prepared from SiC with the particle size of 10 μm had a strength of 389 MPa, but the strength increased to 909 MPa for ceramics prepared from SiC with a starting particle size of 0.45 μm. Analysis indicates that SiC particle size controls the strength of ZrB₂–SiC.     

Effects of inert filler addition on the structure and properties of porous SiOC ceramics derived from silicone resin

Porous SiOC ceramics were obtained from a new self-blowing precursor silicone resin DC217, by pyrolysis at 1200 °C in argon. Silicon carbide powders were incorporated into the silicone resin as inert fillers. The effects of the mean particle size of SiC fillers on the porosity, compressive strength and microstructure of the porous ceramics were investigated. With the mean particle size of SiC powders increasing from 5 μm to 10 μm, the porosity (total and open) of the porous ceramic increased and the compressive strength decreased. However, the porosity, compressive strength and cell morphology of the porous ceramics showed no evident changes when the mean particle size of fillers increased from 10 μm to 15 μm. Micrographs indicated that, when the mean particle size of fillers exceeded 5 μm, the porous ceramics could have a well-defined and regular pore structure. Furthermore, comparing with the porous ceramics which fabricated under the same condition with the SiOC powders as fillers, the cell morphology was similar. But the compressive strength and the oxidation resistance of the porous ceramics with SiC powders as fillers were much better.     

Investigation of flow properties of metal powders from narrow particle size distribution to polydisperse mixtures through an improved Hall-flowmeter

Initially, we critically examined the results provided by the improved Hall-flowmeter, based on bulk volume flow rate, with narrow particle size distribution metal powders (iron, aluminium and copper) of different sizes (fine to coarse) and shapes (nearly spherical to non-spherical). Binary and ternary mixtures of various combinations of fine (< 100 μm) and coarse (> 100 μm) metal powders at different size ratios and weight fractions were allowed to discharge from a mass flow hopper. The results show that the mass flow rate of polydisperse mixtures of metal powders is affected by four factors: the size ratio, the volume fraction of the smallest sieved fraction, the initial mass flow rate and the shape of metal powders.     

Characteristics of BaNd2Ti5O14 powders directly prepared by high-temperature spray pyrolysis

BaNd₂Ti₅O₁₄ powders were directly prepared by high-temperature spray pyrolysis. The powders prepared at temperatures of 1300 and 1500 °C exhibited a pure BaNd₂Ti₅O₁₄ phase. The powders prepared at 1300 °C were spherical in shape. However, the powders prepared at 1500 °C showed non-spherical shapes. The BaNd₂Ti₅O₁₄ powders had a composition similar to that of the spray solution. The mean sizes of the BaNd₂Ti₅O₁₄ powders increased from 0.23 to 0.60 μm when the concentration of the spray solution was increased from 0.01 to 0.2 M. At a sintering temperature of 1100 °C, bridge-like structures were formed between the powders. Pellets sintered at 1300 °C exhibited a dense structure comprising rod-like crystals.     

Influence of powder size on characteristics of air plasma sprayed silicon coatings

Silicon powders with different medium sizes (114 μm, 79 μm and 31 μm, respectively) were used to fabricate coatings by air plasma spraying. The velocity and temperature of in-flight silicon particles during plasma spraying were determined. The composition and microstructure of the coatings were characterized and some physical properties of the coatings were measured. The obtained results showed that the size of silicon particles had great influence on their velocity and temperature in plasma flame. The oxidation of silicon particles in the spraying process was observed and is higher for particles of smaller sizes. Areas of silicon oxide in micrometer size are embedded and randomly distributed in the coating. The surface roughness and void content of silicon coatings increase with an increase in the particle size of the powders. The microhardness and oxygen content of coatings decrease with an increase in the particle size. However, the size of silicon particles has little impact on the deposition efficiency of silicon under the same deposition conditions.     

Sintering behavior of La2O3–B2O3–TiO2 glass powders prepared by spray pyrolysis for low temperature co-fired ceramics

Fine-sized La₂O₃–B₂O₃–TiO₂ glass powders with spherical shape were directly prepared by spray pyrolysis at a temperature of 1500 °C. The optimum flow rate of the carrier gas to prepare the glass powders with dense inner structure and fine size by complete melting was 10 L/min. The ratio of La/Ti was identified to be 2.06:1, which was close to the original starting ratio of La/Ti in mixture of the spray solution. The T_g and T_c of the powders were 614 and 718 °C. The crystal structures within the powders were observed from the sintered disc at 630 °C. The mean sizes of the powders changed from 0.24 to 0.71 μm when the concentrations of the spray solution were changed from 0.025 to 0.5 M. The BET surface areas of the powders changed from 4.4 to 1.6 m²/g. The grain sizes of the sintered discs increased with increasing the sintering temperatures. The main crystal structure of the sintered discs was LaBO₃.     

Sinter forging of rapidly quenched eutectic Al2O3–ZrO2(Y2O3)-glass powders

Spray dried agglomerates of Al₂O₃–ZrO₂ (1% Y₂O₃) with 4 wt.% borosilicate glass were arc plasma sprayed and rapidly quenched into water. Because of the rapid quenching the particles <25 μm were mostly amorphous. After annealing 1 h at 1200 °C the scale of the microstructure of the particles was on the order 30 nm. Hot forging of this powder yielded dense specimens with the width of the ZrO₂ phase still less than 100 nm. Since the particle size ranged from 5 to 25 μm and the scale of the particle microstructure was <100 nm, densification was controlled by creep of the particles rather than by the typical hot pressing mechanism of diffusion along the neck between particles to fill the pores. Thus, the scale of the microstructure controls densification rather than the particle size. These powders offer an alternate source for manufacturing nanostructured parts and should be more suitable for hot pressing or forging than nanoparticulate powders.     

Copper(I) oxide and metallic copper particles formed in 1,2-propane diol

Chemical composition, particle size, and structure formation of colloidal Cu₂O and metallic Cu synthesized from Cu(II) acetate in an environmentally friendly 1,2-propane diol were studied dependent on the temperature and concentration of the precursor. Cu₂O as a reaction intermediate is formed between 150 and 170 °C, while its reduction to metallic Cu occurs between 170 and 180 °C. Average particle sizes of non-agglomerated Cu powders varied from 100 nm to 1 μm.     

Effect of the solvent composition and annealing process on the preparation of spray freeze-dried acetaminophen powder

The analgesic and physical properties of acetaminophen powder suitable as an inhaled drug produced by spray freeze-drying (SFD) were compared with those of raw acetaminophen. A laser particle size analyzer and scanning electron microscopy (SEM) were applied to estimate physical structure and properties of the particles. A cyclooxygenase (COX) inhibitor screening assay was used to compare the antipyretic and analgesic activity of raw and SFD acetaminophen. According to SEM, SFD acetaminophen particles had various shapes and sizes with porous structures. The optimized conditions for solvent, annealing temperature, and annealing time were water/ethanol mixture (60% water and 40% ethanol), ?40°C, and 7?h, respectively. The diameter of optimized acetaminophen powder was 7.33?µm, and the aerodynamic particle size was 3.38?µm. The antipyretic and analgesic activities of acetaminophen after SFD were from 84.3 to 97.1% for COX-1 and from 91.6 to 102.9% for COX-2 compared to those of raw acetaminophen, respectively.     

Particle size effects in flash sintering

The study of 3 mol% yttria stabilized zirconia (3YSZ) with different particle sizes provides new insights into flash sintering. Four powders, all with the same crystallite size but various particle size were investigated: described as nominally 1 μm (D80 = 0.51 μm, meaning 80 vol% has a size less than 0.51 μm), 2 μm (D80 = 0.90 μm), 5 μm (D80 = 2.11 μm) and 10 μm (D80 = 3.09 μm). While the furnace temperature for flash sintering, at a field of 100 V cm^?1, increased from 920 °C to 1040 °C with particle size, the specimen temperature in all instances remained at ～1200 °C. The quantum increase in density decreased with larger particles. The grain size distribution of conventionally and flash sintered specimens remained similar, with some evidence of a preponderance of nanograins in the flash sintered specimens. Joule heating was well below the temperatures that would have been required for sintering in a few seconds. An explanation based upon the nucleation of Frenkel pairs is proposed.     

Micronization of fenofibrate by rapid expansion of supercritical solution

Micronization of fenofibrate was investigated using rapid expansion of supercritical solution (RESS) process. Effects of pressure, temperature and nozzle on particle size were optimized using Taguchi's orthogonal array and analyzed using XRD, DSC, FT-IR, SEM, laser diffractometer and dissolution testing. Processed fenofibrate retained crystalline structure and has a similar chemical structure with unprocessed fenofibrate. The average particle size of fenofibrate was reduced from its original 68.779 ± 0.146 μm to 3.044 ± 0.056 μm under the optimum condition (T at 35 °C, P at 200 bar and nozzle diameter at 200 μm). The processed fenofibrate showed an enhanced dissolution rate by 8.13 times.     

Characteristics of Y3Al5O12:Ce phosphor powders prepared by spray pyrolysis from ethylenediaminetetraacetic acid solution

Nanometer and submicron-sized YAG:Ce phosphor powders were prepared by spray pyrolysis from the spray solutions with ethylenediaminetetraacetic acid (EDTA). The precursor powders with hollow and thin wall structure turned to the fine-sized YAG:Ce phosphor powders after post-treatment at high temperatures of 1400 and 1500 °C. The mean size of the phosphor powders post-treated at a temperature of 1500 °C was 0.72 μm. The white LEDs formed from the YAG:Ce phosphor powders post-treated at 1400 and 1500 °C showed (0.2781, 0.2871) and (0.2731, 0.2795) on the CIE chromaticity diagram, and about 78.20 and 79.04 of Ra. The luminous efficiency of the white LED formed from the commercial YAG:Ce phosphor powders was 84.36 lm/W. However, the luminous efficiencies of the white LEDs formed from the YAG:Ce phosphor powders post-treated at 1400 and 1500 °C were 47.74 and 76.64 lm/W.     

Diamond-like carbon sintered compacts formed by spark plasma sintering

A spark plasma sintering (SPS) method was utilized for the novel production of diamond-like carbon (DLC) compacts. Two amorphous carbon powders with different particle sizes (45 μm and 24 nm diameter) were employed as starting materials for the sintering experiments. The carbon powders were sintered using a SPS system at various sintering temperatures and holding times. The structural properties of the sintered compacts were evaluated using X-ray diffraction (XRD) analysis and high-resolution transmission electron microscopy (HRTEM). Disk-shaped compacts were obtained by sintering the powder with a particle diameter of 45 μm, although the compacts were very brittle and easily broken. However, sintering of the 24 nm diameter powder particles at temperatures of 1473 to 1573 K with a holding time of 300 s led to the successful production of sintered compacts without breakage. Reflection peaks related to graphite structure were observed in XRD patterns of the compacts sintered from the 24 nm diameter particles. HRTEM analysis revealed that the compacts sintered at 1473 K with a holding time of 300 s had an amorphous structure and consisted of 34% sp³ carbon bonding. Evaluation of the structural properties indicated that sintered compacts with DLC structure could be created by the SPS method with 24 nm diameter amorphous carbon particles.     

Mechanochemical synthesis and structural characterization of nano-sized amorphous tricalcium phosphate

Nano-sized amorphous tricalcium phosphate powders were synthesized through different mechanochemical reactions. The influence of milling parameters and chemical composition of reagents on the formation of amorphous tricalcium phosphate was investigated. In all the experiments, the mole ratio of calcium to phosphorous oxide was 3:1, i.e. the stoichiometric Ca/P content in the composition of amorphous tricalcium phosphate (Ca/P=1.5). Results revealed that the phase purity, structural features, and morphological characteristics of products were significantly influenced by the chemical composition of raw materials and milling parameters. For all the reactions, amorphous tricalcium phosphate was formed as the main product of mechanical activation after 10 h. After annealing at 1100 °C, crystallization of amorphous phase occurred, and consequently high crystalline β-tricalcium phosphate was generated. According to FT-IR findings, the synthesized powders had high chemical purity. After 10 h of milling, the obtained nanopowders through four distinct reactions exhibited crystallite sizes about 20, 69, 58 and 55 nm. The results from scanning electron micrographs showed that the mean size of agglomerate was in the range of 1–5 μm. Detailed study of morphological features by using transmission electron microscopy confirmed the formation of nano-sized amorphous tricalcium phosphate with spheroidal and ellipse-like morphologies.     

Preparation and properties of bimodal porous apatite ceramics through slip casting using different hydroxyapatite powders

A bimodal porous hydroxyapatite (HAp) body with high flexural strength was prepared through slip casting. The effect of different particle sizes on the flexural strength and microstructure of three different types of hydroxyapatite (HAp) powders was studied. The powder characteristic of laboratory-synthesized HAp powder (L-HAp) was obtained through a wet-milling method, drying and heating of a mixture of calcium hydrogen phosphate di-hydrate and calcium carbonate. The median particle size of L-HAp was 0.34 μm, and the specific surface area was 38.01 m²/g. The commercial HAp had median particle sizes for the K-HAp (Kishida chemical Co. Ltd., K-HAp) and T-HAp (Taihei chemical Co. Ltd., T-HAp) of 1.13 and 3.65 μm, and specific surface areas of 11.62 and 6.23 m²/g, respectively. The different powder characteristics affected the slip characteristics, and the flexural strength and microstructure of the sintered porous HAp bodies were also different. The flexural strengths of the porous HAp ceramics prepared by heating at 1200 °C for 3 h in air were 17.59 MPa for L-HAp with a porosity of 60.48%, 3.92 MPa for commercial K-HAp with a porosity of 79.37%, and 4.55 MPa for commercial T-HAp with a porosity of 76.46%.     

Synthesis of sub-micro sized high purity zirconium diboride powder through carbothermal and borothermal reduction method

Sub-micro sized zirconium diboride (ZrB₂) powders were successfully prepared via the boro/carbothermal reduction method using zirconium oxide and boron carbide as the primary raw materials. The prepared mixtures were thermally reacted at 1250 °C for 1 h. The optimized composition range containing the lowest oxide and carbide impurity, which was 0.14% of oxygen and 0.3% of carbon contents, was determined using crystallographic and elemental analysis. The particle size was reduced from 5 µm to 245 nm by the addition of B₄C as a reductant within a composition range that maintained the highest purity. The morphology changed from faceted to angular hexagonal bar-like with a simultaneous growth in particle size. Changes in the particle structure were a result of the existing liquid B₂O₃ phase during the reaction. The 245-nm particles contained 12.1% oxygen content and 16.2% oxygen content for the 5-μm particle in the circumstance in which limited oxides could be produced.     

Nanosized barium ferrite powders prepared by spray pyrolysis from citric acid solution

Highly crystalline nanosized barium ferrite (BaFe₁₂O₁₉) powders were prepared by spray pyrolysis from a spray solution containing a high concentration of the metal components. The precursor powders obtained from the spray solution containing citric acid were amorphous with a porous and hollow structure. Purely crystalline and fine BaFe₁₂O₁₉ powders were obtained after post-treatment between 700 and 1000 °C and subsequent mechanical grinding in an agate mortar. The mean sizes of the powders post-treated at 700 and 1000 °C were 125 and 550 nm, respectively. The specific magnetization of the powders prepared from the spray solution containing citric acid was 57 emu/g.     

Synthesis of triclinic and hexagonal SmBO3 powders by mechanically activated annealing of Sm2O3 and B2O3 blends

Samarium borate (SmBO₃) powders were fabricated from oxide raw materials by a two-step solid-state synthesis method including mechanical activation and annealing. Blends containing stoichiometric amounts of samarium oxide (Sm₂O₃) and boron oxide (B₂O₃) were mechanically activated in a high-energy ball mill and subsequently annealed in air. Afterwards, mechanically activated and annealed powders were washed with distilled water in order to remove probable unreacted B₂O₃ phase. The effects of mechanical activation duration (15 min, 1 h, 3 h and 9 h) and annealing temperature (700–1250 °C) on the resultant powders were investigated. Compositional, microstructural, physical, thermal and optical properties of the powders obtained throughout the different process steps were characterized by using an X-ray diffractometry (XRD), particle size analysis (PSA), stereomicroscopy (SM), scanning electron microscopy (SEM), transmission electron microscopy (TEM), gas pycnometry, differential scanning calorimetry (DSC), heating stage microscopy (HSM), atomic absorption spectrometry (AAS), Fourier transform infrared (FTIR) spectrometry and ultraviolet-visible spectrophotometry (UV–vis) techniques. Fine-grained and pure SmBO₃ powders were successfully synthesized via a simple, feasible and scalable route, yielding both triclinic and hexagonal crystal structures. Triclinic SmBO₃ powders were synthesized after mechanical activation for 1 h and annealing at 700 °C for 2 h. The polymorphic transformation temperature of SmBO₃ powders from triclinic to hexagonal is about 1080 °C. Due to the effect of mechanical activation, the synthesis of triclinic SmBO₃ phase and its transformation to hexagonal form were found to take place at ∼50–100 °C lower temperatures than those reported in other methods. Mainly hexagonal SmBO₃ powders were obtained after annealing at 1150 °C in the presence of a very small amount of triclinic SmBO₃. The resultant powders showed intense UV absorptions in the range between 1025 and 1150 nm with minimum reflectivity of 0.57% (triclinic SmBO₃ phase) and 0.68% (hexagonal SmBO₃ phase) depending on their crystal structures.     

Low temperature synthesis of polycrystalline explosion phase boron nitride submicron-powders

High purity quasi-octahedral polycrystalline explosion phase boron nitride (e-BN) submicron-powders were synthesized in an autoclave at 600 °C for 6 h using Mg, FeB_1.3 and NH₄Cl as the raw materials. Samples were characterized by SEM, FSEM, EDX, TEM, HRTEM, SAED, X-ray powder diffraction (XRD) and Fourier transform infrared (FTIR) spectroscopy. The as-synthesized e-BN powders demonstrated a face-centered cubic structure with lattice parameter of 8.300 Å. Besides the e-BN samples presented a quasi-octahedral morphology with an average diameter of 0.8 μm. The effects of time, temperature, raw materials and possible catalytic reaction mechanism of the growth of quasi-octahedral polycrystalline e-BN were also discussed.