Synthesis And Characterization Of Ball-Milled Nanocrystalline Fcc Metals

1991 ◽  
Vol 238 ◽  
Author(s):  
J. Eckert ◽  
J. C. Holzer ◽  
C. E. Krill ◽  
W. L. Johnson

ABSTRACTNanocrystalline fee metals (Al, Cu, Ni, Pd, Rh, Ir) have been prepared by ball milling. The development of the microstructure is investigated by x-ray diffraction, differential scanning calorimetry (DSC), and transmission electron microscopy (TEM). The final grain sizes range from 6 to 22 nm and scale with the melting point and the bulk modulus of the elements: metals with higher melting point and bulk modulus have a smaller final grain size. From this a general relation between the deformation mechanism during ball milling and the ultimate grain size achievable by this technique is inferred. With decreasing grain size the lattice strain is enhanced and deformation enthalpies of up to 40 % of the heat of fusion are stored in the material. The contributions of the lattice strain and of die excess enthalpy of the grain boundaries to the stored enthalpies are critically assessed. The kinetics of grain growth are investigated by mermal analysis. The activation energy for grain boundary migration is derived from a modified Kissinger analysis and estimates of the grain boundary enthalpy are given.

1992 ◽  
Vol 7 (7) ◽  
pp. 1751-1761 ◽  
Author(s):  
J. Eckert ◽  
J.C. Holzer ◽  
C.E. Krill ◽  
W.L. Johnson

Nanocrystalline fcc metals have been synthesized by mechanical attrition. The crystal refinement and the development of the microstructure have been investigated in detail by x-ray diffraction, differential scanning calorimetry, and transmission electron microscopy. The deformation process causes a decrease of the grain size of the fcc metals to 6–22 nm for the different elements. The final grain size scales with the melting point and the bulk modulus of the respective metal: the higher the melting point and the bulk modulus, the smaller the final grain size of the powder. Thus, the ultimate grain size achievable by this technique is determined by the competition between the heavy mechanical deformation introduced during milling and the recovery behavior of the metal. X-ray diffraction and thermal analysis of the nanocrystalline powders reveal that the crystal size refinement is accompanied by an increase in atomic-level strain and in the mechanically stored enthalpy in comparison to the undeformed state. The excess stored enthalpies of 10–40% of the heat of fusion exceed by far the values known for conventional deformation processes. The contributions of the atomic-level strain and the excess enthalpy of the grain boundaries to the stored enthalpies are critically assessed. The kinetics of grain growth in the nanocrystalline fcc metals are investigated by thermal analysis. The activation energy for grain boundary migration is derived from a modified Kissinger analysis, and estimates of the grain boundary enthalpy are given.


2021 ◽  
Author(s):  
Mark Coleman ◽  
Bernhard Grasemann ◽  
David Schneider ◽  
Konstantinos Soukis ◽  
Riccardo Graziani

<p>Microstructures may be used to determine the processes, conditions and kinematics under which deformation occurred. For a given set of these variables, different microstructures are observed in various materials due to the material’s physical properties. Dolomite is a major rock forming mineral, yet the mechanics of dolomite are understudied compared to other ubiquitous minerals such as quartz, feldspar, and calcite. Our new study uses petrographic, structural and electron back scatter diffraction analyses on a series of dolomitic and calcitic mylonites to document differences in deformation styles under similar metamorphic conditions. The Attic-Cycladic Crystalline Complex, Greece, comprises a series of core complexes wherein Miocene low-angle detachment systems offset and juxtapose a footwall of high-pressure metamorphosed rocks against a low-grade hanging wall. This recent tectonic history renders the region an excellent natural laboratory for studying the interplay of the processes that accommodate deformation. The bedrock of Mt. Hymittos, Attica, preserves a pair of ductile-then-brittle normal faults dividing a tripartite tectonostratigraphy. Field observations, mineral assemblages and observable microstructures suggests the tectonic packages decrease in metamorphic grade from upper greenschist facies (~470 °C at 0.8 GPa) in the stratigraphically lowest package to sub-greenschist facies in the stratigraphically highest package. Both low-angle normal faults exhibit cataclastic fault cores that grade into the schists and marbles of their respective hanging walls. The middle and lower tectonostratigraphic packages exhibit dolomitic and calcitic marbles that experienced similar geologic histories of subduction and exhumation. The mineralogically distinct units (calcite vs. dolomite) of the middle package deformed via different mechanisms under the same conditions within the same package and may be contrasted with mineralogically similar units that deformed under higher pressure and temperature conditions in the lower package. In the middle unit, dolomitic rocks are brittlely deformed. Middle unit calcitic marble are mylonitic to ultramylonitic with average grain sizes ranging from 30 to 8 μm. These mylonites evince grain-boundary migration and grain size reduction facilitated by subgrain rotation. Within the lower package, dolomitic and calcitic rocks are both mylonitic to ultramylonitic with grain sizes ranging from 28 to 5 μm and preserve clear crystallographic preferred orientation fabrics. Calcitic mylonites exhibit deformation microstructures similar to those of the middle unit. Distinctively, the dolomitic mylonites of the lower unit reveal ultramylonite bands cross-cutting and overprinting an older coarser mylonitic fabric. Correlated missorientation angles suggest these ultramylonites show evidence for grain size reduction accommodated by microfracturing and subgrain rotation. In other samples the dolomitic ultramylonite is the dominant fabric and is overprinting and causing boudinage of veins and relict coarse mylonite zones. Isolated interstitial calcite grains within dolomite ultramylonites are signatures of localized creep-cavitation processes. Following grain size reduction, grain boundary sliding dominantly accommodated further deformation in the ultramylonitic portions of the samples as indicated by randomly distributed correlated misorientation angles. This study finds that natural deformation of dolomitic rocks may occur by different mechanisms than those identified by published experiments; notably that grain-boundary migration and subgrain rotation may be active in dolomite at much lower temperatures than previously suggested.</p>


Author(s):  
Qingyu Liu ◽  
Qinhe Zhang ◽  
Min Zhang ◽  
Jianhua Zhang

The material removal process of micro electrical discharge machining is based on the instantaneous ultra-high temperature generated by a series of repetitive discharge pulses. Due to the size effects, the polycrystal cannot be considered as continuous and homogeneous material when machining is in micron scale, and the effects of material microstructure should not be neglected. In this article, the thermoelectric characteristics of grain and grain boundary are discussed, and the influence of grain size on the machining performances in micro electrical discharge machining is researched. Two kinds of austenitic stainless steels (AISI 304) which are different in grain size are chosen as the workpieces in experiments. It is verified by both theory models and experimental results that the smaller the grain size, the higher the material removal rate, under the same discharge conditions. Both thermal conductivity and melting point of the grain boundary are lower than those of the grain because of the grain boundary segregation. The effective thermal conductivity and local effective melting point of polycrystalline materials vary with their grain sizes since the grain boundary volume fractions change. As a consequence, the material removal rate of micro electrical discharge machining has direct relationship with grain size of the workpiece.


e-Polymers ◽  
2007 ◽  
Vol 7 (1) ◽  
Author(s):  
Ai Yafei ◽  
Jin Yong ◽  
Sun Jing ◽  
Wei Deqing

AbstractIn this study, suspension polymerization is described to fabricate microcapsules containing n-hexadecane as phase change material. In the suspension polymerization, casein is employed as emulsifier and stabilizer instead of synthetic surfactant. Microcapsules with polystyrene as shell and n-hexadecane as core have an average diameter of 3~15μm and the size distribution are narrow. Thermal properties are investigated by differential scanning calorimetry (DSC) showing that the microcapsules can store and release an amount of latent heat over a temperature range nearing the melting point of pure n-hexadecane. The latent heat of fusion of microencapsulated n-hexadecane decreases after microencapsulation. The melting point of microencapsulated n-hexadecane is near but higher than that of pure n-hexadecane, and the polymerization time has little effect on the melting point.


Author(s):  
Carlos Leonardo Di Prinzio ◽  
Pastor Ignacio Achaval

In this work, the migration of a three-dimensional (3D) spherical crystal in the presence of mobile particles using a Monte Carlo algorithm was studied. Different concentrations of particles (<i>f</i>) and different particle mobility (<i>M<sub>p</sub></i>) were used. It was found that the grain size reaches a critical radius (<i>R<sub>c</sub></i>) which depends exclusively on <i>f</i>. This dependence can be written as: <i>R<sub>c</sub></i>∝<i>f</i><sup>1/3</sup>. The dynamic equation of grain size evolution and its analytical solution were also found. The analytical solution proposed fits successfully the simulation results. The particle fraction in the grain boundary was also found analytically and it fits the computational data.


1994 ◽  
Vol 40 (134) ◽  
pp. 46-55
Author(s):  
C.J. L. Wilson ◽  
Y. Zhang

AbstractAn examination of both experiments and computer models of polycrystalline ice undergoing a simple shear suggests that there is good agreement. The model has correctly reproduced the deformational and microstructural features caused by glide on (0001) in the ice aggregates. This success is particularly prominent for those ice grains with a lattice orientation suitable for hard or easy glide or kinking, and where there is a sub-horizontal с axis and a larger grain-size. A limitation may be that the model cannot explicitly simulate recrystallization and grain-boundary migration, which are two other important processes operating jointly with glide in experimentally deformed ice. However, through the use of the models, it is possible to show how kinematic factors can control the processes of recrystallization. The localization of recrystallization in the polycrystalline ice aggregate is determined by the stress and strain variations between neighbouring grains.


2019 ◽  
Vol 58 (1) ◽  
pp. 98-106
Author(s):  
Haitao Ni ◽  
Jiang Zhu ◽  
Zhaodong Wang ◽  
Haiyang Lv ◽  
Yongyao Su ◽  
...  

Abstract This review focuses on grain growth behaviors and the underlying mechanisms of bulk electrodeposited nanocrystalline nickel and nickel-iron alloys. Effects of some important factors on grain growth are described. During thermal-induced grain growth process, grain boundary migration plays a key role. For similar thermal conditions, due to grain boundary mobility with solute drag, limited grain growth occurs in nanocrystalline alloys, as compared to pure metals. Nonetheless, in the case of stress-induced grain growth process, there are a variety of mechanisms in samples having various deformation histories. As an example the grain growth of nanocrystalline nickel and Ni-20%Fe alloy with nearly the same grain-size distribution and average grain size is compared in this paper. Thermal analysis indicates nanocrystalline nickel is much more prone to rapid grain growth than nanocrystalline Ni-20%Fe alloy. Nevertheless, grain growth of nanocrystalline Ni-20%Fe is found to be more pronounced than nanocrystalline nickel during rolling deformation.


1994 ◽  
Vol 40 (134) ◽  
pp. 46-55 ◽  
Author(s):  
C.J. L. Wilson ◽  
Y. Zhang

AbstractAn examination of both experiments and computer models of polycrystalline ice undergoing a simple shear suggests that there is good agreement. The model has correctly reproduced the deformational and microstructural features caused by glide on (0001) in the ice aggregates. This success is particularly prominent for those ice grains with a lattice orientation suitable for hard or easy glide or kinking, and where there is a sub-horizontalсaxis and a larger grain-size. A limitation may be that the model cannot explicitly simulate recrystallization and grain-boundary migration, which are two other important processes operating jointly with glide in experimentally deformed ice. However, through the use of the models, it is possible to show how kinematic factors can control the processes of recrystallization. The localization of recrystallization in the polycrystalline ice aggregate is determined by the stress and strain variations between neighbouring grains.


2020 ◽  
Author(s):  
Alexander Lusk ◽  
John Platt

&lt;p&gt;Present exposure of the ductile Caledonian retrowedge in northwestern Scotland records the evolution of a shear zone that was exhuming while actively deforming, providing a natural laboratory to study strain localization in a progressively cooling system. Examination of rocks from two detailed transects across this region consistently show a transition from microstructures that are dominated by interconnected phyllosilicate networks in a quartz-rich matrix with feldspar porphyroclasts, to interconnected fine-grained regions of mixed quartz + phyllosilicate + feldspar. These polyphase regions are demonstrably weaker than surrounding quartz layers and likely deform by grain-size sensitive mechanisms including diffusion-accommodated grain boundary sliding.&lt;/p&gt;&lt;p&gt;Microstructures characterized by a quartz-rich matrix and interconnected phyllosilicates undergo quartz recrystallization by high temperature grain boundary migration and are dominated by prism &lt;em&gt;a&lt;/em&gt; slip. In contrast, fine-grained polyphase microstructures record quartz recrystallization dominated by subgrain rotation and activation of rhomb &lt;em&gt;a&lt;/em&gt; and basal &lt;em&gt;a&lt;/em&gt; slip systems. We propose transient hardening occurs in quartz-dominated regions as quartz with a strong Y-axis maximum undergoes the switch from prism &lt;em&gt;a&lt;/em&gt; easy slip to basal &lt;em&gt;a&lt;/em&gt; easy slip during cooling, and thus partitions strain into interconnected phyllosilicate layers. In response, interconnected phyllosilicate layers undergo mechanical comminution, becoming increasingly mixed by grain-size sensitive creep processes to form polyphase layers as they accommodate an increased proportion of strain. This transition from quartz-rich matrix with phyllosilicate interconnected weak layers to fine-grained, polyphase weak layers could be of first-order importance in strain localization within polyphase mylonitic and ultramylonitic rocks.&lt;/p&gt;


1992 ◽  
Vol 286 ◽  
Author(s):  
Chrysanthe D. Terwilliger ◽  
Yet-Ming Chiang

ABSTRACTThe excess enthalpy and excess heat capacity of nanophase TiO2 prepared by a chemically-derived process and by inert gas condensation have been measured using differential scanning calorimetry. In comparison to the chemically-derived samples, the excess enthalpy of the inert gas condensed samples is significantly larger, perhaps due to the presence of intragranular planar defects that accomm oate oxygen deficiency. Significant extraneous contributions from planar defects, lattice strain, phase transformation, oxidation, or sintering have been ruled out for the chemically-derived samples. A grain boundary enthalpy of 13-1.6 J/m2 in the temperature range 600-1000°C is obtained from scanning measurements. However, the data also indicate a grain size and/or temperature dependence of the grain boundary enthalpy.


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