Surface Integrity Analysis when Milling Ultrafine-grained Steels

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

Surface integrity analysis when milling ultrafine-grained steels

This paper quantifies the effects of milling conditions on surface integrity of ultrafine-grained steels. Cutting speed, feed rate and depth of cut were related to microhardness and microstructure of the workpiece beneath machined surface. Low-carbon alloyed steel with 10.8 µm (as-received) and 1.7 µm (ultrafine) grain sizes were end milled using the down-milling and dry condition in a CNC machining center. The results show ultrafine-grained workpiece preserves its surface integrity against cutting parameters more than the as-received material. Cutting speed increases the microhardness while depth of cut deepens the hardened layer of the as-received material. Also, deformations of microstructure following feed rate direction were observed in workpiece subsurface.

Microstructure evolution during warm deformation of low carbon steel with dispersed cementite

The microstructure evolution and mechanical behavior during large strain of a 0.16%C-Mn steel has been investigated by warm torsion tests. These experiments were carried out at 685°C at equivalent strain rate of 0.1 s . The initial microstructure composed of a martensite matrix with uniformly dispersed fine cementite particles was attained by quenching and tempering. The microstructure evolution during tempering and straining was performed through interrupted tests. As the material was reheated to testing temperature, well-defined cell structure was created and subgrains within lath martensite were observed by TEM; strong recovery took place, decreasing the dislocation density. After 1 hour at the test temperature and without straining, EBSD technique showed the formation of new grains. The flow stress curves measured had a peculiar shape: rapid work hardening to a hump, followed by an extensive flow-softening region. 65% of the boundaries observed in the sample strained to ε = 1.0 were high angle grain boundaries. After straining to ε = 5.0, average ferrite grain size close to 1.5 μm was found, suggesting that dynamic recrystallization took place. Also, two sets of cementite particles were observed: large particles aligned with straining direction and smaller particles more uniformly dispersed. The fragmentation or grain subdivision that occurred during reheating and tempering time was essential for the formation of ultrafine grained microstructure.

Efeito do fresamento com alta velocidade de corte na usinabilidade de aços ferríticos com grãos ultrafinos

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

Magnetic extracts of three gravity cores located at the Ceará Rise, the Mid-Atlantic Ridge and the Sierra Leone Rise

The magnetic microparticle and nanoparticle inventories of marine sediments from equatorial Atlantic sites were investigated by scanning and transmission electron microscopy to classify all present detrital and authigenic magnetic mineral species and to investigate their regional distribution, origin, transport, and preservation. This information is used to establish source-to-sink relations and to constrain environmental magnetic proxy interpretations for this area. Magnetic extracts were prepared from sediments of three supralysoclinal open ocean gravity cores located at the Ceará Rise (GeoB 1523-1; 3°49.9'N/41°37.3'W), the Mid-Atlantic Ridge (GeoB 4313-2; 4°02.8'N/33°26.3'W), and the Sierra Leone Rise (GeoB 2910-1; 4°50.7'N/21°03.2'W). Sediments from two depths corresponding to marine isotope stages 4 and 5.5 were processed. This selection represents glacial and interglacial conditions of sedimentation for the western, central, and eastern equatorial Atlantic and avoids interferences from subsurface and anoxic processes. Crystallographic, elemental, morphological, and granulometric data of more than 2000 magnetic particles were collected by scanning and transmission electron microscopy. On basis of these properties, nine particle classes could be defined: detrital magnetite, titanomagnetite (fragmental and euhedral), titanomagnetite-hemoilmentite intergrowths, silicates with magnetic inclusions, microcrystalline hematite, magnetite spherules, bacterial magnetite, goethite needles, and nanoparticle clusters. Each class can be associated with fluvial, eolian, subaeric, and submarine volcanic, biogenic, or chemogenic sources. Large-scale sedimentation patterns are delineated as well: detrital magnetite is typical of Amazon discharge, fragmental titanomagnetite is a submarine weathering product of mid-ocean ridge basalts, and titanomagnetite-hemoilmenite intergrowths are common magnetic particles in West African dust. This clear regionalization underlines that magnetic petrology is an excellent indicator of source-to-sink relations. Hematite encrustations, magnetic spherules, and nanoparticle clusters were found at all investigated sites, while bacterial magnetite and authigenic hematite were only detected at the more oxic western site. At the eastern site, surface pits and crevices were seen on the crystal faces indicating subtle early diagenetic reductive dissolution. It was observed that paleoclimatic signatures of magnetogranulometric parameters such as the ratio of anhysteretic and isothermal remanent magnetizations can be formed either by mixing of multiple sources with separate, relatively narrow grain size ranges (western site) or by variable sorting of a single source with a broad grain size distribution (eastern site). Hematite, goethite, and possibly ferrihydrite nanoparticles occur in all sediment cores studied and have either high-coercive or superparamagnetic properties depending on their partly ultrafine grain sizes. These two magnetic fractions are generally discussed as separate fractions, but we suggest that they could actually be genetically linked.

Finite element analysis of mechanical properties in discontinuously reinforced metal matrix composites with ultrafine microstructure

This investigation focused on the finite element analyses of elastic and plastic properties of aluminium/alumina composite materials with ultrafine microstructure. The commonly used unit cell model was used to predict the elastic properties. By combining the unit cell model with an indentation model, coupled with experimental indentation measurements, the plastic properties of the composites and the associated strengthening mechanism within the metal matrix material were investigated. The grain size of the matrix material was found to be an important factor influencing the mechanical properties of the composites studied. (C) 1997 Elsevier Science S.A.

Sintering of ultrafine undoped SnO2 powder

The sintering process of nanometric undoped SnO2 powder was studied. No macroscopic shrinkage was observed during the sintening process. Grain growth kinetics investigation showed that surface diffusion is the dominant mechanism in the temperature range 500-1300 degreesC. For temperatures higher than 1300 degreesC, high weight loss was measured, suggesting evaporation-condensation as the dominant mass-transport mechanism. Thermogravimetric analysis (TG) and mass spectroscopy studies showed that the surface contamination of the SnO2 particles by chemical species like H2O, OH- and CO2, has a strong influence on the role of mass transport controlled by surface diffusion. (C) 2001 Elsevier B.V. Ltd. All rights reserved.

Second Phase Precipitation in Ultrafine-grained Ferrite Steel

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

Ballistic performance of nanocrystalline and nanotwinned ultrafine crystal steel

Because of their remarkable mechanical properties, nanocrystalline metals have been the focus of much research in recent years. Refining their grain size to the nanometer range (<100 nm) effectively reduces their dislocation mobility, thus achieving very high yield strength and surface hardness—as predicted by the Hall–Petch relation—as well as higher strain-rate sensitivity. Recent works have additionally suggested that nanocrystalline metals exhibit an even higher compressive strength under shock loading. However, the increase in strength of these materials is generally accompanied by an important reduction in ductility. As an alternative, efforts have been focused on ultrafine crystals, i.e. polycrystals with a grain size in the range of 500 nm to 1 μm, in which “growth twins” (twins introduced inside the grain before deformation) act as barriers against dislocation movement, thus increasing the strength in a similar way as nanocrystals but without significant loss of ductility. Due to their outstanding mechanical properties, both nanocrystalline and nanotwinned ultrafine crystalline steels appear to be relevant candidates for ballistic protection. The aim of the present work is to compare their ballistic performance against coarse-grained steel, as well as to identify the effect of the hybridization with a carbon fiber–epoxy composite layer. Hybridization is proposed as a way to improve the nanocrystalline brittle properties in a similar way as is done with ceramics in other protection systems. The experimental campaign is finally complemented by numerical simulations to help identify some of the intrinsic deformation mechanisms not observable experimentally. As a conclusion, nanocrystalline and nanotwinned ultrafine crystals show a lower energy absorption than coarse-grained steel under ballistic loading, but under equal impact conditions with no penetration, deformation in the impact direction is smaller by nearly 40%. This a priori surprising difference in the energy absorption is rationalized by the more important local contribution of the deviatoric stress vs. volumetric stress under impact than under uniaxial deformation. Ultimately, the deformation advantage could be exploited in the future for personal protection systems where a small deformation under impact is of key importance.

Microstructuration induced differences in the thermo-optical and luminescence properties of Nd:YAG fine grain ceramics and crystals

The temperature and compositional dependences of thermo- optical properties of neodymium doped yttrium aluminum garnet (YAG) crystals and fine grain ceramics have been systematically investigated by means of time- resolved thermal lens spectrometry. We have found that Nd:YAG ceramics show a reduced thermal diffusivity compared to Nd:YAG single crystals in the complete temperature range investigated (80-300 K). The analysis of the time- resolved luminescent properties of Nd(3+) has revealed that the reduction in the phonon mean free path taking place in Nd:YAG ceramics cannot be associated with an increment in the density of lattice defects, indicating that phonon scattering at grain boundaries is the origin of the observed reduction in the thermal diffusivity of Nd: YAG ceramics. Finally, our results showed the ability of the time- resolved thermal lens to determine and optimize the thermo- optical properties of Nd: YAG ceramic based lasers. (C) 2008 American Institute of Physics. [DOI: 10.1063/1.2975335]

The effect of agitation speed, enzyme loading and substrate concentration on enzymatic hydrolysis of cellulose from brewer`s spent grain

Brewer`s spent grain components (cellulose, hemicellulose and lignin) were fractionated in a two-step chemical pretreatment process using dilute sulfuric acid and sodium hydroxide solutions. The cellulose pulp produced was hydrolyzed with a cellulolytic complex, Celluclast 1.5 L, at 45 degrees C to convert the cellulose into glucose. Several conditions were examined: agitation speed (100, 150 and 200 rpm), enzyme loading (5, 25 and 45 FPU/g substrate), and substrate concentration (2, 5 and 8% w/v), according to a 2(3) full factorial design aiming to maximize the glucose yield. The obtained results were interpreted by analysis of variance and response surface methodology. The optimal conditions for enzymatic hydrolysis of brewer`s spent grain were identified as 100 rpm, 45 FPU/g and 2% w/v substrate. Under these conditions, a glucose yield of 93.1% and a cellulose conversion (into glucose and cellobiose) of 99.4% was achieved. The easiness of glucose release from BSG makes this substrate a raw material with great potential to be used in bioconversion processes.

Effect of hemicellulose and lignin on enzymatic hydrolysis of cellulose from brewer`s spent grain

Enzymatic hydrolysis of brewer`s spent grain in three different forms: original (untreated), pretreated by dilute acid (cellulignin), and pretreated by a sequence of dilute acid and dilute alkali (cellulose pulp), was studied to verify the effect of hemicellulose and lignin on cellulose conversion into glucose. The hydrolysis was carried out using a commercial cellulase concentrate (Celluclast 1.5 L) in an enzyme/substrate ratio of 45 FPU/g, 2% (w/v) substrate concentration, 45 degrees C for 96 h. According to the results, the cellulose hydrolysis was affected by the presence of hemicellulose and/or lignin in the sample. The cellulose conversion ratio (defined as glucose yield + cellobiose yield) from cellulignin was 3.5-times higher than that from untreated sample, whereas from cellulose pulp such value was 4-times higher, correspondent to 91.8% (glucose yield of 85.6%). This best result was probably due to the strong modification in the material structure caused by the hemicellulose and lignin removal from the sample. As a consequence, the cellulose fibers were separated being more susceptible to the enzymatic attack. It was concluded that the lower the hemicellulose and lignin contents in the sample, the higher the efficiency of cellulose hydrolysis. (C) 2007 Elsevier Inc. All rights reserved.

Hydrogen peroxide bleaching of cellulose pulps obtained from brewer`s spent grain

Brewer`s spent grain (BSG) was evaluated for bleached pulp production. Two cellulose pulps with different chemical compositions were produced by soda pulping: one from the original raw material and the other from material pretreated by dilute acid. Both of them were bleached by a totally chlorine-free sequence performed in three stages, using 5% hydrogen peroxide in the two initial, and a 0.25 N NaOH solution in the last one. Chemical composition, kappa number, viscosity, brightness and yield of bleached and unbleached pulps were evaluated. The high hemicellulose (28.4% w/w) and extractives (5.8% w/w) contents in original BSG affected the pulping and bleaching processes. However, soda pulping of acid pretreated BSG gave a cellulose-rich pulp (90.4% w/w) with low hemicellulose and extractives contents (7.9% w/w and < 3.4% w/w, respectively), which was easily bleached achieving a kappa number of 11.21, viscosity of 3.12 cp, brightness of 71.3%, cellulose content of 95.7% w/w, and residual lignin of 3.4% w/w. Alkaline and oxidative delignification of acid pretreated BSG was found as an attractive approach for producing high-purity, chlorine-free cellulose pulp.

Effects of medium supplementation and pH control on lactic acid production from brewer`s spent grain

A cellulose pulp obtained by chemical pre-treatment of brewer`s spent grain was saccharified by a commercial cellulase preparation and the produced hydrolysate (50 g/l glucose) was fermented to lactic acid by Lactobacillus delbrueckii. The effects of pH control and nutrient supplementation of the hydrolysate on fermentation performance were investigated. Addition of 5g/l yeast extract enhanced the lactic acid volumetric productivity that attained 0.53 g/l h, value 18% higher than that obtained from non-supplemented hydrolysate. Addition of the MRS broth medium components (except the carbon source) was still better, providing a productivity of 0.79 g/l h. In all the cases, the lactic acid yield factor was of 0.7 g/g glucose consumed, but the fermentations stopped after 24 h due to the pH drop from 6.0 to 4.2, resulting in large amounts of residual glucose (38-41 g/l). Fermentation runs pH-controlled at 6.0 gave better results than those where the initial pH was not further controlled. The best result, 35.54 g/l lactic acid (0.99 g/g glucose consumed) was obtained during the pH-controlled fermentation of hydrolysate medium supplemented with MRS components. The volumetric productivity at the end of this fermentation was 0.59 g/l h, with a maximum of 0.82 g/l h during the first 12 h. (c) 2008 Elsevier B.V. All rights reserved.

Establishment of the optimum initial xylose concentration and nutritional supplementation of brewer`s spent grain hydrolysate for xylitol production by Candida guilliermondii

The effects of initial xylose concentration and nutritional supplementation of brewer`s spent grain hydrolysate on xylitol production by Candida guilliermondii were evaluated using experimental design methodology. The hydrolysate containing 55, 75 or 95 g/l xylose, supplemented or not with nutrients (calcium chloride, ammonium sulfate and rice bran extract), was used as fermentation medium. The increase in xylitol yield and productivity was related to the increase of initial xylose concentration, but up to a certain limit. above of which the yeast performance was not improved. The hydrolysate supplementation with nutrients did not interfere with xylose-to-xylitol conversion. By using the statistic tool the best conditions for maximum xylitol production were found. which consisted in using the non-supplemented hydrolysate containing 70 g/l initial xylose concentration. Under these conditions, a xylitol yield of 0.78 g/g and productivity of 0.58 g/(l h) were achieved. (C) 2008 Elsevier Ltd. All rights reserved.