Showing papers on "Grain size published in 1988"

Magnetic properties of some synthetic sub-micron magnetites

Abstract: The grain size dependence of various mineral (rock) magnetic parameters has been determined, using a series of essentially pure, fine-grained (single domain, SD) and ultrafine-grained (superparamagnetic, SP) magnetites. The parameters measured include low-field susceptibility, frequency-dependent susceptibility, saturation remanence (SIRM), anhysteretic susceptibility (XARM), and coercivity of remanence ((B0)CR). The magnetites were produced in experiments designed to simulate possible pedogenic and biogenic pathways of magnetite formation. Their mean grain sizes range from 0.012 um to 0.06 um, and hence span the SP/SD boundary. Isothermal magnetic measurements were performed on two separate subsets of differing packing densities. The response of the magnetic parameters is modified by interaction effects, but they display continuous variation across the entire grain size range, confirming their value for rapid magnetic granulometry. Within the fine and ultrafine end of the magnetite grain size spectrum, susceptibility, frequency dependent susceptibility and XARM are notably responsive to grain size change. In terms of magnetic response (and also possibly of grain size, shape and absence of cation substitution), these synhtetic magnetites represent close analogues of those found in some soils and sediments.

Microcracking in Ceramics Induced by Thermal Expansion or Elastic Anisotropy

Abstract: The effect of crystal anisotropy on the formation of grain-boundary microcracks is analyzed, by considering a planar array of hexagonal grains as a model of a polycrystalline ceramic. The stress singularities at triple-grain junctions are analyzed by an asymptotic method as well as by a numerical solution, and the critical size of a grain-boundary defect is investigated by a crack analysis. It is found that elastic anisot-ropies can significantly increase the stress levels near triple points, which results in a smaller critical grain size for microcracking.

Synthesis, characterization, and properties of nanophase TiO 2

Abstract: Ultrafine-grained, nanophase samples of TiO2 (rutile) were synthesized by the gas-condensation method and subsequent in situ compaction. The samples were studied by a number of techniques, including transmission electron microscopy, Vickers microharness measurements, and positron annihilation spectroscopy, as a function of sintering temperature. The nanophase compacts with average initial grain sizes of 12 nm were found to densify rapidly above 500 °C, with only a small increase in grain size. The hardness values obtained by this method are comparable to or greater than those for coarser-grained compacts, but are achieved at temperatures 400 to 600 °C lower than conventional sintering temperatures and without the need for sintering aids.

Large grain polycrystalline silicon by low‐temperature annealing of low‐pressure chemical vapor deposited amorphous silicon films

Abstract: The crystallization of undoped amorphous silicon films deposited by low‐pressure chemical vapor deposition in the temperature range 580–530 °C and annealed from 550 to 950 °C has been studied by transmission electron microscopy. The average grain size of the crystallized films depends on the annealing temperature and the deposition conditions. The nucleation rate of new grains during annealing decreases as the deposition temperature decreases from 580 to 545 °C and/or when the deposition rate increases. The final grain size is also influenced by the annealing temperature with the largest grain size obtained at low annealing temperatures. A simple model is described which explains the dependence of grain size on the annealing temperature. An average grain size of 500 nm has been obtained in a 200‐nm film deposited at 545 °C and annealed at 550 °C.

Experimental deformation of partially melted granitic aggregates

Abstract: The effects of varying amounts of partial melt on the deformation of granitic aggregates have been tested experimentally at conditions (900°C, 1500 MPa, 10-4 to 10-6/s) where melt-free samples deform by dislocation creep, with microstructures approximately equivalent to those of upper greenschist facies. Experiments were performed on samples of various grain sizes, including an aplite (150 μm) and sintered aggregates of quartz-albitemicrocline (10–50 and 2–10 μm). Water was added to the samples to obtain various amounts of melt (1–15% in the aplite, 1–5% in the sintered aggregates). Optical and TEM observations of the melt distribution in hydrostatically annealed samples show that the melt in the sintered aggregates is homogeneously distributed along an interconnected network of triple junction channels, while the melt in the aplites is inhomogeneously distributed. The effect of partial melt on deformation depends an melt amount and distribution, grain size and strain rate. For samples deformed with ˜ 1% melt, all grain sizes exhibit microstructures indicative of dislocation creep. For samples deformed with 3–5% melt, the 150 μm and 10–50 μm grain size samples also exhibit dislocation creep microstructures, but the 2–10 μm grain size samples exhibit abundant TEM-scale evidence of dissolution-precipitation and little evidence of dislocation activity, suggesting a switch in deformation mechanism to predominantly melt-enhanced diffusion creep. At natural strain rates melt-enhanced diffusion creep would predominate at larger grain sizes, although probably not for most coarse-grained granites. The effects of melt percentage and strain rate have been studied for the 150 μm aplites. For samples with ˜ 5 and 10% melt, deformation at 10–6/s squeezes excess melt out of the central compressed region allowing predominantly dislocation creep. Conversely, deformation at 10-5/s produces considerable cataclasis presumably because the excess melt cannot flow laterally fast enough and a high pore fluid pressure results. For samples with 15% melt, deformation at both strain rates produces cataclasis, presumably because the inhomogeneous melt distribution resulted in regions of decoupled grains, which would produce high stress concentrations at point contacts. At natural strain rates there should be little or no cataclasis if an equilibrium melt texture exists and if the melt can flow as fast as the imposed strain rate. However, if the melt is confined and cannot migrate, a high pore fluid pressure should promote brittle deformation.

Weakly coupled grain model of high‐frequency losses in high Tc superconducting thin films

Abstract: We propose a model of Josephson coupling between grains to explain the millimeter‐wave surface impedance of oriented, polycrystalline thin films of high Tc superconductors. An effective junction IcR product and effective grain size are calculated based on recent measurements of the surface impedance. We suggest a criterion on film quality for the observation of losses intrinsic in the superconductor. The effects of crystalline orientation on surface impedance are considered.

Magnetization reversal in nucleation controlled magnets. II. Effect of grain size and size distribution on intrinsic coercivity of Fe‐Nd‐B magnets

Abstract: Results of experiments to study the effect of grain size and grain‐size distribution on the intrinsic coercivity and the hysteresis loop of sintered Fe‐Nd‐B magnets are presented. It is shown that the intrinsic coercivity decreases as the average grain size of the magnet is increased. It is also shown that the intrinsic coercivity decreases linearly with the logarithm of the square of the grain size. This is consistent with the predictions made based upon the statistical model developed in Part I. An increase in the sintering temperature leads to an increase in the average grain size, which consequently leads to a narrower hysteresis loop and lower intrinsic coercivity compared to magnets sintered at a lower temperature. It is also shown that a heterogeneous grain‐size distribution, such as a bimodal distribution, causes kinks to appear in the second quadrant of the hysteresis loop. By examining magnets with different fractions of large grains, the prediction that the magnitude of the kinks increases with...

Experimental study of incipient motion in mixed‐size sediment

Abstract: Transport rates of five sediments were measured in a laboratory flume. Three of these sediments had the same mean size, the same size distribution shape, and different values of grain size distribution standard deviation. The critical shear stress for incipient motion of the individual size fractions within these sediments was estimated as that shear stress that produced a small dimensionless transport rate. The sorting of the sediment mixture had little effect on the critical shear stress of individual fractions, once the median size (D50) of the mixture and a fraction's relative size (Di/D50) are accounted for. Our data, combined with previously published data, show a remarkably consistent relation between the critical shear stress of individual fractions and the fraction's relative grain size, despite a broad variation in the available data of mixture sorting, grain size distribution shape, mean grain size, and grain shape. All fractions in a size mixture begin moving at close to the same value of bed shear stress during steady state transport conditions. This result is apparently true for transport systems where the transport rates of individual fractions are determined solely by the flow and bed sediment (recirculating systems), as well as for systems where the fractional transport rates are imposed on the system (feed systems). This equivalence in initial-motion results is important because natural transporting systems often show attributes of both types of behavior in an unknown combination.

Columnar growth in thin films.

Abstract: A theory for the growth of columnar microstructures in thin films is presented. The zone-I to zone-II transition temperature is predicted. The surface morphology and the columnar grain structure are obtained both analytically and numerically, and the scaling behavior of the columnar grain size with film thickness is derived. Monte Carlo simulations are used to follow the evolution of the three-dimensional zone-II microsctuctures and to account for the formation of film texture. These results agree with experimental observations.

Grain‐Growth Transition During Sintering of Colloidally Prepared Alumina Powder Compacts

Abstract: When the grain size in partially sintered compacts of alumina was measured as a function of density, we found that the grain-growth behavior fell into two distinct regions. In the region where the porosity remained interconnected, grain growth was negligible; when the continuous pore network collapsed into isolated pores, grains grew rapidly. The transition in grain-growth behavior was observed at approximately 90% of theoretical density. A simple phenomenological method for obtaining the transition in grain growth is suggested. It is based on the idea that an abrupt increase in grain size should be accompanied by a significant decrease in the rate of sintering since the sintering rate changes as the third or fourth power of the grain size. The method consists of fitting the sintering data to an exponential function. The transition then appears as a change in the time constant for the exponential. The low rate of grain growth in the region where the pores are interconnected contradicts earlier work in the literature where significant grain growth during intermediate-stage sintering has been reported. This difference is explained in terms of the homogeneity of packing of our powder compacts, which were prepared by colloidal processing.

Ion‐bombardment‐enhanced grain growth in germanium, silicon, and gold thin films

Abstract: Grain growth has been studied in polycrystalline thin films of Ge, Si, and Au during ion bombardment. The phenomenon has been characterized by varying the ion dose, ion energy, ion flux, ion species, substrate temperature, and thin‐film deposition conditions. Films bombarded with Si+, Ar+, Ge+, Kr+, and Xe+ exhibited enhanced grain growth which was weakly temperature dependent and proportional to the energy deposited in elastic collisions at or very near grain boundaries. The effect of these parameters on grain size and microstructure was analyzed both qualitatively and quantitatively using transmission electron microscopy. A transition state model describing the motion of grain boundaries during ion bombardment has been applied to the present experimental data. The results suggest that bombardment‐enhanced grain growth may be due to thermal migration of bombardment‐generated defects across the boundary. The calculated defect yield per incident ion was found to be directly related to enhanced grain growth...

Low‐Temperature Sintering of Aluminum Oxide

Abstract: A fine-sized (∼0.1 μm), agglomerate-free Al2O3 dispersion was used to prepare homogeneous green bodies with ∼69% relative density and ∼10-nm median pore radius. Samples could be sintered at 1150°C to a relative density >99.5% and an average grain size of 0.25 μm.

Grain growth in synthetic marbles with added mica and water

Abstract: Evolution of grain size in synthetic marbles was traced from compaction of unconsolidated powder, through primary recrystallization and normal grain growth, to a size stabilized by second phases. To form the marbles, reagent grade CaCO3 was mixed with 0, 1 and 5 volume% mica and heat-treated under pressure with added water. Densification with negligible recrystallization occurred within one hour at 500° C and 500 MPa confining pressure. Primary recrystallization occurred at 500–550° C, causing increases of grain size of factors of 2–5. Resulting samples had uniform grain size, gently curved grain boundaries, and near-equilibrium triple junctions; they were used subsequently for normal grain growth studies. Normal grain growth occurred above 550° C; at 800° C, grain size (D) increased from 7 μm (D 0) to 65 μm in 24 hours. Growth rates fit the equation, D n -D 0 =Kt, where K is a constant and n≃2.6. Minor amounts of pores or mica particles inhibit normal grain growth and lead to a stabilized grain size, D max, which depends on the size of the second phases and the inverse of their volume fraction raised to a power between 0.3 and 1. Once D max is reached, normal growth continues only if second phases are mobile or coarsen, or if new driving forces are introduced that cause unpinning of boundaries. Normal grain growth in Solnhofen limestone was significantly slower than in pure synthetic marble, suggesting that migration is also inhibited by second phases in the limestone.

The microstructural and compositional influence upon HIREM behavior in Nd2Fe14B

Abstract: Enhanced magnetically isotropic properties are observed in melt‐spun flakes of the Nd2Fe14B(Si) type. The magnetic enhancement, referred to as HIREM, includes a remanent magnetization equal to 8–9.3 kG (with saturation magnetization measured between 15.2 and 15.7 kG), and an energy product up to 19 MGOe. Both of these properties are significantly above the conventional limits permissible for noninteracting magnetic grains. Microanalysis in an analytical electron microscope (AEM) indicates that there are two requirements for the HIREM phenomenon to arise: (1) a substantial absence of an intergranular phase between the 2‐14‐1 crystallites, and (2) a specific grain size range. These results support a model for the enhancement resulting from intergrain magnetic exchange coupling.

Analytical and numerical modeling of columnar evolution in thin films

Abstract: A theory for the growth of columnar microstructure in thin films is presented. The zone II columnar microstructure is shown to result from a balance between shadowing (which results in zone I microstructures) and surface diffusion (which tends to smooth the surface). The zone I to zone II transition temperature is predicted together with the type of unstable modes. The surface morphology and the columnar grain structure are obtained both analytically and numerically. The scaling behavior of the grain size with film thickness is derived. Monte Carlo computer simulations follow the temporal evolution of three‐dimensional zone II microstructures, and account for growth competition between adjacent grains, and the formation of film texture. These results agree with experimental data.

Solid solution and grain size hardening of nitrogen-alloyed austenitic steels

Abstract: The influence of interstitially dissolved nitrogen on the yield strength of various austenitic steels is investigated. A Hall-Petch analysis of the yield strength is made and it is shown that nitrogen increases the yield strength by solid solution and grain size hardening.

Computer simulation of microstructural evolution in thin films

Abstract: The nature of the microstructure of a thin film strongly affects its functionality in electronic applications. For example, the rate of electromigration-induced failure is a function not only of the grain size in an interconnect line, but also of the width and shape of the grain size distribution. We are developing techniques which allow prediction of the relationships between the conditions for thin film processing and the topology and geometry of resulting grain structures. We have simulated two-dimensional microstructural evolution by determining the location of grain boundaries after nucleation and growth of crystalline domains. We have allowed for nucleation under a variety of conditions including constant nucleation rates, decreasing nucleation rates and instantaneous saturation of nucleation sites. We have also allowed for increasing and decreasing growth rates which depend in various ways on the domain size. We have simulated grain growth in two-dimensional structures by allowing boundary and triple point motion in order to reduce the total grain boundary area. The rate and nature of the initial stages of grain growth are strongly affected by the conditions for nucleation and growth. Eventually, however, grain growth appears to proceed as expected from analytical treatments.

Granular metal films as recording media

Abstract: High‐density recording media require materials with a high magnetization and high coercivity as well as chemical stability, wear, and corrosion resistance. We explore the potential of granular metal films for recording media. Films of Fe granules about 150 A in size embedded in an amorphous SiO2 matrix exhibit coercivities as high as 3 kOe at low temperatures and 1.1 kOe at room temperature, and magnetizations of about 150 emu/g. The methods with which these materials are fabricated, the essential microstructure characterization, and magnetic measurements are described.

Study on the substructure evolution and flow behaviour in type 316L stainless steel over the temperature range 21-900°C

Abstract: Tensile specimens of type 316L stainless steel with a grain size of 5.0 μm have been deformed at a constant strain rate of 10−3 s−1 over the temperature range 21–900°C and by differential strain-rate test technique over strain rates from about 10−5 to 10−3 s−1 at temperatures in the range 750–900°C. The normalized yield and flow stresses against temperature plots exhibit three regions. While in regions I and III the stresses decrease with increasing temperature, they increase with increasing temperature in region II. Transmission electron microscopy studies on deformed specimens show that at small strains the dislocations generated at grain boundaries have characteristic distributions: in region I the dislocations are confined to the vicinity of the grain boundary, in region II the dislocations are spread into the grain interior, and in region III the dislocations rearrange to form walls. The evolution of substructure and the work-hardening behaviour are explained by considering both intragranula...

Grain growth and alignment in hot deformed Nd‐Fe‐B magnets

Abstract: Formation of grain oriented Nd‐Fe‐B magnets from melt‐spun ribbons by hot deformation has been studied using electron microscopy. It is shown that deformation and alignment of Nd2Fe14B magnets result from a combination of plastic deformation, grain boundary migration, and grain boundary sliding. Due to a limited number of available slip systems in this material, samples with large grains deform less easily. Small grain size materials, as encountered in the melt‐spun ribbons, are well suited for die‐upsetting to produce oriented magnets.

Effect of Particle Size Distribution on the Sintering of Alumina

Abstract: The effect of particle size distribution on the sintering of Al2O3 was investigated. Samples could be sintered to high relative density (∼99%), small average grain size (1 μm), and no growth of exaggerated grains using powders with either broad or narrow particle size distribution. However, the broad particle size distribution provided the advantage that powder compacts could be prepared with higher green density and, therefore, samples could be densified with less total shrinkage.

Aerosol flow reactor production of fine Y1Ba2Cu3O7 powder: Fabrication of superconducting ceramics

Abstract: An aerosol flow reactor operating at 900–1000 °C is used to prepare high‐purity Y1Ba2Cu3O7 powders with a uniform chemical composition and a submicron to micron average particle size by thermally decomposing aerosol droplets of a solution consisting of the nitrate salts of Y, Ba, and Cu in a 1:2:3 ratio. The powders were at least 99% reacted based on thermogravimetric analysis, and the x‐ray diffraction pattern is essentially that of Y1Ba2Cu3O7. Magnetic susceptibility measurements showed the powders to be superconducting with a transition at 90 K even for average reactor residence times as short as 20 s. Sintering cold‐pressed pellets between 900 and 1000 °C provides dense, fine grained (average size on the order of 1 μm) superconducting ceramics with sharp 90 K transitions. The grain size and shape of a final sintered part could be varied depending on powder production, processing, and sintering conditions.

Rare earth-iron-boron magnet powder and process of producing same

Abstract: In a rare earth-iron-boron alloy magnet powder, each individual particle includes a recrystallized grain structure containing a R2 Fe14 B intermetallic compound phase as a principal phase thereof, wherein R represents a rare earth element. The intermetallic compound phase are formed of recrystallized grains of a tetragonal crystal structure having an average crystal grain size of 0.05 μm to 50 μm. For producing the above magnet powder, a rear earth-iron-boron alloy material is first prepared. Then, hydrogen is occluded inot the alloy material by holding the material at a temperature of 500° C. to 1,000° C. either in an atmosphere of hydrogen gas or in an atmosphere of hydrogen and inert gases. Subsequently, the alloy material is subjected to dehydrogenation at a temperature of 500° C. to 1,000° C. until the pressure of hydrogen in the atmosphere is decreased to no greater than 1×10-1 torr, and is subjected to cooling.

Synthesis and sintering behaviour in CeO2−ZrO2 ceramics

Abstract: The co-precipitation method has been employed to prepare CeO2-ZrO2 ceramics. The application of a wet chemical method is expected to yield highly sinterable material at lower sintering temperatures. The characteristics of the synthesized powders are evaluated with respect to the particle size distribution, calcination step, and the degree of agglomeration. The sintering behaviour of the prepared powder is studied at various temperatures to obtain different phase distributions and grain sizes. The amount of the monoclinic phase in the as-sintered specimen is decreased with increasing CeO2 contents in CeO2-ZrO2. 13.7 mol% CeO2 is sufficient to achieve a tetragonal phase in the CeO2-ZrO2 system. In addition, Y2O3 and MgO dopants in CeO2-ZrO3 reduce the grain size and result in a fully tetragonal phase for the 10 mol% CeO2 matrix.