Grain boundary character information via individual imaging or statistical analyses: complexion transitions and grain boundary segregation

Author(s):  
Katharina Marquardt ◽  
David Dobson ◽  
Simon Hunt ◽  
Ulrich Faul

<p>Grain boundaries affect bulk properties of polycrystalline materials, such as electrical conductivity, melting or bulk viscosity. In the past two decades, observations of marked bulk material property changes have been associated with changes in the structure and composition of grain boundaries. This led to the term “grain boundary complexions” to mark the phase-like behaviour of grain boundaries while differing from phases in the sense of Gibbs (Cantwell 2014).</p><p>Here we introduce the principles of grain boundary structure to property relations and potent methods to study these. The focus is on the combination of structural, chemical and statistical analysis as obtainable using transmission electron microscopy and electron backscatter diffraction. Data from these complementary methods will be discussed on two systems; garnet and olivine polycrystals.</p><p>Past elasticity measurements showed that the Youngs modulus of garnet polycrystals changes as a function of sintering pressure (Hunt et al. 2016). Here we used high resolution transmission electron microscopy to study the structure of grain boundaries from polycrystals synthesized at low (4-8 GPa) and high (8-15) GPa sintering pressure. The HRTEM data were acquired using an image-corrected JEOL ARM 300 to achieve the highest resolution at low electron doses using a OneView camera. Our data indicate a grain boundary structural change occurs from “low-pressure” to “high pressure” grain boundaries, where the grain boundary facets change from >100 nm – 20 nm to 3-7 nm length scale, respectively. We conclude that sintering pressure affects grain-boundary strength and we will evaluate how this may influence anelastic energy loss of seismic waves through elastic or diffusional accommodation of grain-boundary sliding.</p><p>Polycrystalline olivine samples show different viscosity related to grain boundary segregation of impurities. To investigate if the distribution of grain boundaries is affected by grain boundary chemistry, we analysed grain orientation data from over 4x10<sup>4</sup> grains, corresponding to more than 6000 mm grain boundary length per sample. Using stereology, we extract the geometry of the interfacial network. The thus obtained grain boundary character distribution (GBCD) is discussed in relation to bulk viscosity.</p>

2011 ◽  
Vol 484 ◽  
pp. 82-88
Author(s):  
Koji Matsui ◽  
Hidehiro Yoshida ◽  
Yuichi Ikuhara

Microstructure development during sintering in 3 mol% Y2O3-stabilized tetragonal ZrO2 polycrystal (Y-TZP) was systematically investigated in two sintering conditions: (a) 1100-1650°C for 2 h and (b) 1300°C for 0-50 h. In the sintering condition (a), the density and grain size in Y-TZP increased with the increasing sintering temperature. Scanning transmission electron microscopy (STEM) and nanoprobe X-ray energy dispersive spectroscopy (EDS) measurements revealed that the Y3+ ion distribution was nearly homogeneous up to 1300°C, i.e., most of grains were the tetragonal phase, but cubic-phase regions with high Y3+ ion concentration were clearly formed in grain interiors adjacent to the grain boundaries at 1500°C. High-resolution transmission electron microscopy (HRTEM) and nanoprobe EDS measurements revealed that no amorphous or second phase is present along the grain-boundary faces, and Y3+ ions segregated not only along the tetragonal-tetragonal phase boundaries but also along tetragonal-cubic phase boundaries over a width below about 10 nm, respectively. These results indicate that the cubic-phase regions are formed from the grain boundaries and/or the multiple junctions in which Y3+ ions segregated. We termed this process a “grain boundary segregation-induced phase transformation (GBSIPT)” mechanism. In the sintering condition (b), the density was low and the grain-growth rate was much slow. In the specimen sintered at 1300°C for 50 h, the cubic-phase regions were clearly formed in the grain interiors adjacent to the grain boundaries. This behavior shows that the cubic-phase regions were formed without grain growth, which can be explained by the GBSIPT model.


2014 ◽  
Vol 616 ◽  
pp. 8-13
Author(s):  
Koji Matsui ◽  
Hidehiro Yoshida ◽  
Yuichi Ikuhara

We systematically investigated the phase transformation and grain-growth behaviors during sintering in 2 and 3 mol% Y2O3-stabilized tetragonal ZrO2 (2Y and 3Y) and 8 mol% Y2O3-stabilized cubic ZrO2 polycrystals (8Y). In particular, grain-boundary segregation and grain-interior distribution of Y3+ ions were examined by high-resolution transmission electron microscopy (HRTEM)- and scanning transmission electron microscopy (STEM)-nanoprobe X-ray energy dispersive spectroscopy (EDS) techniques. Above 1200°C, grain growth during sintering in 8Y was much faster than that in 2Y and 3Y. In the grain boundaries in these specimens, amorphous layers did not present; however, Y3+ ions segregated at the grain boundaries over a width of about 10 nm. The amount of segregated Y3+ ions in 8Y was significantly less than in 2Y and 3Y. This indicates that the amount of segregated Y3+ ions is related to grain growth behavior; i.e., an increase in segregated Y3+ ions retards grain growth. Therefore, grain-growth behavior during sintering can be reasonably explained by the solute-drag mechanism of Y3+ ions segregating along the grain boundary. In 2Y and 3Y, the cubic-phase regions were formed in grain interiors adjacent to the grain boundaries and/or the multiple junctions in which Y3+ ions segregated, which can be explained by a grain boundary segregation-induced phase transformation (GBSIPT) mechanism.


Author(s):  
J. R. Michael ◽  
D. B. Williams

Bismuth is known to segregate to grain boundaries in copper resulting in embrittlement and intergranular failure at low stress levels. This segregation has been studied primarily by Auger Electron Spectroscopy (AES). The applicability of scanning transmission electron microscopy (STEM)and Energy Dispersive Spectroscopy (EDS) to the study of equilibrium grain boundary segregation has already been demonstrated and the aim of this study is to determine the degree of segregation as a function of time and temperature. The major advantage of STEM over AES is that STEM does not require fracturing of the specimen, so the boundaries to be studied are left undisturbed. Thus, this technique is also applicable to systems which do not exhibit intergranular fracture.Cu-Bi specimens were prepared by evaporating Bi onto both sides of 3mm Cu discs, which were then heated for 1 week at 400°C to allow the Bi to diffuse into the Cu. The samples were then aged at 450, 550, 600, 650, and 700°C for 3 days and 12 days, ion-thinned and then examined in a Philips EM 400T TEM/STEM with an EDAX detector and EDAX 9100 analyzer. If necessary, the specimens were tilted such that the boundaries were parallel to the electron beam.


1991 ◽  
Vol 238 ◽  
Author(s):  
Elsie C. Urdaneta ◽  
David E. Luzzi ◽  
Charles J. McMahon

ABSTRACTBismuth-induced grain boundary faceting in Cu-12 at ppm Bi polycrystals was studied using transmission electron microscopy (TEM). The population of faceted grain boundaries in samples aged at 600°C was observed to increase with heat treatment time from 15min to 24h; aging for 72h resulted in de-faceting, presumably due to loss of Bi from the specimen. The majority of completely faceted boundaries were found between grains with misorientation Σ=3. About 65% of the facets of these boundaries were found to lie parallel to crystal plane pairs of the type {111}1/{111]2- The significance of these findings in light of recent high resolution electron microscopy experiments is discussed.


Author(s):  
L. E. Murr

Grain boundaries represent the single, most dominant imperfection in structural materials of engineering and industrial importance, and are a controlling factor in the strength of materials. Transmission electron microscopy, combined with the ability to gain direct crystallographic information from associated selected-area electron diffraction patterns, represents perhaps the most effective means for the investigation of the nature and behavior of grain boundaries in solids.Any segment of a grain boundary has associated with it five degrees of freedom. The electron microscope has the capability to characterize these degrees of freedom and to uniquely define the geometrical and crystallographic nature of a grain boundary. In addition, once the true geometry of intersecting grain boundaries or grain boundaries intersecting with other interfaces is determined, interfacial free energy ratios can be calculated from which the average energy associated with particular types of interfaces can be determined.


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