Preparation of Al2TiO5-Al2O3 and Al2TiO5-Al2O3-TiO2 Ceramics by High-Energy Ball Milling and Sintering

The present work reports on the preparation of Al2O3-TiO2 ceramics by high-energy ball milling and sintering, varying the molar fraction in 1:1 and 3:1. The powder mixtures were processed in a planetary Fritsch P-5 ball mill using silicon nitride balls (10 mm diameter) and vials (225 mL), rotary speed of 250 rpm and a ball-to-powder weight ratio of 5:1. Samples were collected into the vial after different milling times. The milled powders were uniaxially compacted and sintered at 1300 and 1500 degrees C for 4h. The milled and sintered materials were characterized by X-ray diffraction and electron scanning microscopy (SEM). Results indicated that the intensity of Al2O3 and TiO2 peaks were reduced for longer milling times, suggesting that nanosized particles can be achieved. The densification of Al2O3-TiO2 ceramics was higher than 98% over the relative density in samples sintered at 1500 degrees C for 4h, which presented the formation of Al2TiO5.

On Ti-18Si-6B and Ti-7.5Si-22.5B powder alloys prepared by high-energy ball milling and sintering

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Effect of ball milling on structural and physicochemical characteristics of cassava and Peruvian carrot starches

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Effect of ball milling on the physicochemical characteristics of Peruvian carrot and cassava starches

Peruvian carrot and cassava starches were ground in a ball mill for 4, 8, 16, and 32 h and their structural and physicochemical characteristics were determined. Results obtained from HPAEC-PAD, GPC, and amylose content indicated a breaking of hydrogen bounds and α-(1 [RIGHTWARDS ARROW] 6) linkages of the starch molecules after treatment. X-ray diffractograms showed that the milling provided a reduction in the crystalline area of the starch granules. Most of the starch granules displayed agglomeration after 4 h of milling, when observed under a scanning electron microscope, and after 16 h a shapeless mass was observed for Peruvian carrot starch. Solubility and water absorption capacity of the starches increased with an increase in the milling time, while RVA profiles showed a progressive reduction of peak, breakdown, and final viscosities, as well as the development of initial viscosity. Gelatinization temperatures and enthalpies were reduced. Prolonged ball milling accelerated the enthalpy relaxation in both starches. These results confirmed a partial gelatinization of the starches, which was 82.6% for Peruvian carrot and 65.4% for cassava starches after 32 h of milling. The Peruvian carrot starch was more affected by the ball milling because of both its lower amylose content and the defects in its crystalline structure

Structural Evaluation of Mechanically Alloyed and Heat-Treated Ti-25at-%Si Powders

This work discusses on the structural evaluation of mechanically alloyed and heat-treated Ti-25at%Si powders. The milling process was conducted in a planetary ball mill using stainless steel balls/vials, 200 rpm and ball-to-powder weight ratio of 5:1, whereas the heat treatment was conducted under Ar atmosphere at 1100 C for 4 h. Samples were characterized by X-ray diffraction, differential scanning calorimetry, scanning electron microscopy and energy dispersive spectrometry. The Si peaks disappeared after milling for 30h, indicating that the Si atoms were dissolved into the Ti lattice in order to form an extended solid solution. The Ti peaks were broadened and their intensities reduced for longer milling times whereas a halo was formed in Ti-25Si powders milled for 200h suggesting that an amorphous structure was achieved. The crystallite size was decreased with increasing milling times. A large Ti3Si amount was found in mechanically alloyed Ti-25at%Si powders after heating at 1100 degrees C for 4h.

Desenvolvimento de varistores à base de SnO2 para aplicação em redes de alta tensão

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

BaTiO3 obtained through metallic stearate precursors

Metallic stearates were used as precursors to obtain BaTiO3. Barium and titanium stearate mixtures were homogenized in ball mill containing some amount of ammonium stearate. The mixture of the precursors was evaluated by simultaneous TG/ DTA and TMA, and residues from thermal decomposition were characterized by XRD and SEM. It could be verified that the residues from the thermal decomposition in both oxidant and inert atmospheres were the BaTiO3 but with characteristic morphological and crystalline aspects depending on the experimental conditions in which the mixtures of precursors were obtained. (C) 2002 Elsevier B.V. B.V. All rights reserved.

Dielectric and piezoelectric properties of the mechanochemically prepared PZT ceramics

Mechanochemical synthesis was applied to obtain nanocrystalline powders of composition Pb(Zr0.52Ti0.48)O-3 (PZT). Milling was performed in a planetary ball mill using vials and balls made of zirconia or steel-in order to investigate influence of milling media on the electrical properties of resulting ceramics. PZT ceramics showed high values for dielectric constant (epsilon(r)), reaching 970 at room temperature, as well as low dielectric loss (tandelta) under the optimal processing conditions. High values of remanent polarization (P-r) indicate high internal polarizability. The best samples showed piezoelectric strain constant d(33) = 347 pC/N and planar coupling factor k(P) = 0.44. Milling in ZrO2 medium prevents powder contamination and provides reproducibility of milling process. Also, PZT obtained from the powders milled in ZrO2 exhibited lower values of dielectric loss, in comparison with the PTZ obtained from the powders milled in Fe. This suggests that contamination of the powder with Fe could result in an increase of conductivity in final product. (C) 2004 Kluwer Academic Publishers.

Mechanochemical synthesis of barium titanate

A powder mixture of BaO and TiO2, was mechanochemically treated in a planetary ball mill in an air atmosphere for up to 4 h, using zirconium oxide vial and zirconium oxide balls as the milling medium. Mechanochemical reaction leads to the gradual formation of BaTiO3 phase. Phase evolution during synthesis and changes in powder size and morphology were monitored by XRD, DSC, IR and TEM analysis and it was shown that the formation of BaTiO3 phase was initiated after 60 min. Extended time of milling directed to formation of higher amount of BaTiO3 perovskite phase. Barium titanate with good crystallinity was formed after 240 min sintering without pre-calcination step was performed at 1330 degrees C for 2 It within heating rate 10 degrees C/min. (c) 2005 Elsevier Ltd. All rights reserved.

Mechanochemical synthesis of PZT powders

PZT ceramic powders were successfully prepared from the mixture of PbO, ZrO2 and TiO2 by mechanochemical synthesis in a planetary ball mill, under different milling conditions. Phase evolution during synthesis was monitored by X-ray diffraction analysis. Intensive milling resulted in formation of the nanocrystalline, perovskite PZT powders after 1 h of milling. This is a significant improvement in comparison to milling conditions reported by other authors. Depending on milling parameters the presence of some other phases, such as unreacted ZrO2, was also detected in some samples. The changes in powder size and morphology due to intensive milling, were determined by SEM and TEM, while BET analysis was used to determine specific surface area of the powders. Conclusions about processes taking place during mechanochemical synthesis of PZT powders were made based on the results of characterization. (C) 2002 Elsevier B.V. B.V. All rights reserved.

Ferroelectric properties of mechanically synthesized nanosized barium titanate

Barium titanate ceramics were prepared through mechanochemical synthesis starting from fresh prepared barium oxide and titanium oxide in rutile form. Mixture of oxides was milled in zirconia oxide jar in the planetary ball-mill during 30, 60, 120 and 240 min. Extended time of milling directed to formation of higher amount of barium titanate perovskite phase. Barium titanate with good crystallinity was formed after 240 min. Sintering without pre-calcinations step was performed at 1330 degrees C for 2 hours with heating rate of 10 degrees C/min. The XRD, DSC, IR and TEM analyses were performed. Electric and ferroelectric properties were studied. Very well defined hysteresis loop was obtained.

Structure and Properties of Barium Bismuth Titanate Prepared by Mechanochemical Synthesis

Bi4Ti4O15 [BBT], a member of Aurivillius bismuth-based layer-structure perovskites, was prepared from stoichiometric amounts of BaTiO3 [BT] and Bi4Ti3O12 [BIT] obtained via mechanochemical synthesis. Mechanochemical synthesis was performed in air atmosphere in a planetary ball mill. BBT ceramics were sintered at 1100C for 4 h without pre-calcination step within heating rate 10C/min. The formation of phase and crystal structure of BT, BIT and BBT were approved using X-ray analysis. The morphology of obtained powders and microstructure were exhamined using scanning electron microscopy. The electrical properties of sintered samples were carried out.

Study of Structure and Properties of Bi4Ti3O12 Prepared by Mechanochemical Syntheses

Bi4Ti3O12 powder was synthesized from bismuth oxide and titanium oxide. Mixture of oxides was milled in zirconium oxide jar in the planetary ball-mill during 1, 3 and 6 h. Extended time of milling directed to formation of higher amount of titanates perovskite phase. Bi4Ti3O12 was formed between 1 and 3 h of milling time. The phase formation of Bi4Ti3O12, crystal structure and powder particle size were followed by XRD, Raman spectroscopy and SEM analysis. After milling for various times the powders were compacted by pressing and isothermal sintering. Sample milled for 3 h and subsequently sintered at 1000C for 24 h exhibit a hysteresis loop, confirming that the synthesized material possesses ferroelectric properties. All results affect that the structure Bi4Ti3O12 is strongly dependent on the milling time.

Mechanochemical synthesis of Bi4Ti3O12

Our efforts were directed to the preparation of bismuth titanate - Bi 4e;Ti3O12 (BIT) by mechanically assisted synthesis. The mechanical activation was applied to prepare bismuth titanate, Bi4e;Ti3O12, from bismuth oxide, Bi 2O3, and titanium oxide, TiO2 (in an anatase crystal form). Mechanochemical synthesis was performed in a planetary ball mill in air atmosphere. Bismuth titanate ceramics was obtained by sintering at 1000° C The formation of Bi4e;Ti3O12 in the sintered samples was confirmed by X-ray diffraction analysis. Scanning electron microscopy, SEM, was used to study the particle size and powder morphology. The obtained results indicate that Bi4e;Ti3O12 from the powder synthesized by high-energy ball milling exhibits good sinterability, showing advantage of the mechanochemical process over conventional solid-state reaction.

Determinação do teor de extrato etéreo de grãos de oleaginosas através de diferentes processamentos

The objective of this work was to determine the ether extract content of peanut and canola seeds, with extraction in Soxhlet apparatus and with three types of processing: grinding in ball mill type; maceration in mortar and grind into micro mill after maceration in mortar. Data were analyzed in an entirely randomized design with 3 treatments and 12 replicates, submitted to variance analysis and the means were compared using Tukey test (P<0.05) with routines of the SAS statistical package. The largest percentage of ether extract was obtained in the treatment which the peanuts were subjected to a greater number of extractions (56.43%), and all treatments presented different results(P <0.05). In canola grains, it was observed that the extraction with the method of grinding in ball mill and the method of sequential extraction (macerate + ground in micro mill) were statistically similar (43.52 and 42.35% respectively), and these methods were more efficient (P <0.05) to extract the ether extract than the treatment in which the grains were only macerated. For peanut grains it was concluded that the most efficient method was the sequential one and to the canola grain, it can be used only a grinding mill as samples processing witch will be submitted to ether extract extraction.