Contributions of phase and structural transformations in multicomponent Al-Mg alloys to the linear and nonlinear mechanisms of anelasticity

NASA Astrophysics Data System (ADS)

Golovin, I. S.; Bychkov, A. S.; Mikhailovskaya, A. V.; Dobatkin, S. V.

2014-02-01

The effects of the processes of severe plastic deformation (SPD), recrystallization, and precipitation of the β phase in multicomponent alloys of the Al-5Mg-Mn-Cr and Al-(4-5%)Mg-Mn-Zn-Sc systems on the mechanisms of grain-boundary relaxation and dislocation-induced microplasticity have been studied in some detail. To stabilize the ultrafine-grained structure and prevent grain growth, dispersed Al-transition-metal particles, such as Al3Zr, Al6Mn, Al7Cr, Al6(Mn,Cr), Al18Cr2Mg3 have been used. We have special interest in alloys with additions of scandium, which forms compounds of the Al3Sc type and favors the precipitation of finer particles compared to the aluminides of other transition metals. After SPD, Al-(4-5%)Mg-Mn-Zr-Sc alloys exhibit an enhanced recrystallization temperature. The general features of the dislocation and grain-boundary anelasticity that have been established for the binary Al-Mg alloys are retained; i.e., (1) the decrease in the dislocation density in the process of recrystallization of cold-worked alloys leads to the formation of a pseudo-peak in the curves of the temperature dependences of internal friction (TDIF) and to a decrease in the critical amplitude of deformation corresponding to the onset of dislocation motion in a stress field; (2) the precipitation of the β phase suppresses the grain-boundary relaxation; (3) the dissolution of the β phase, the passage of the magnesium atoms into the solid solution, and the precipitation of the β' phase upon heating hinder the motion of dislocations; (4) the coarsening of the highly dispersed particles containing Zr and Sc increases the dislocation mobility. The grain-boundary relaxation and dislocation-impurity interaction and their temperature dependences, as well as processes of the additional alloying of the binary alloys by Mn, Cr, Zr, and Sc, have been estimated quantitatively.

Reduction of the allotropic transition temperature in nanocrystalline zirconium: Predicted by modified equation of state (MEOS) method and molecular dynamics simulation

NASA Astrophysics Data System (ADS)

Salati, Amin; Mokhtari, Esmail; Panjepour, Masoud; Aryanpour, Gholamreza

2013-04-01

The temperature at which polymorphic phase transformation occurs in nanocrystalline (NC) materials is different from that of coarse-grained specimens. This anomaly has been related to the role of grain boundary component in these materials and can be predicted by a dilated crystal model. In this study, based on this model, a modified equation of state (MEOS) method (instead of equation of state, EOS, method) is used to calculate the total Gibbs free energy of each phase (β-Zr or α-Zr) in NC Zr. Thereupon, the change in the total Gibbs free energy for β-Zr to α-Zr phase transformation (ΔGβ→α) via the grain size is calculated by this method. Similar to polymorphic transformation in other NC materials (Fe, Nb, Co, TiO2, Al2O3 and ZnS), it is found that the estimated transformation temperature in NC Zr (β→α) is reduced with decreasing grain size. Finally, a molecular dynamics (MD) simulation is employed to confirm the theoretical results.

Defects versus grain size effects on the ferromagnetism of ZrO2 nanocrystals clarified by positron annihilation

NASA Astrophysics Data System (ADS)

Wang, D. D.; Qi, N.; Jiang, M.; Chen, Z. Q.

2013-01-01

Undoped ZrO2 nanocrystals were annealed in open air from 100 °C to 1300 °C. X-ray diffraction and transmission electron microscope were used to study the structure change and grain growth. Both the methods reveal that the ZrO2 grain size has very slight increase after annealing up to 900 °C. Positron annihilation measurements reveal a high concentration of vacancy defects which most probably exist in the grain boundary region. Thermal annealing above 500 °C causes recovery of these defects, and after annealing at 1200 °C, most of them are removed. Room temperature ferromagnetism is observed for the sample annealed at 100 °C and 500 °C. The magnetization becomes very weak after the nanocrystals are annealed at 700 °C, and it almost disappears at 1000 °C. It is clear that the intrinsic ferromagnetism in our ZrO2 nanocrystals is mostly related with the interfacial defects instead of grain size effects.

Synthesis and electrical characterization of BaZr0.9Ho0.1O3-δ electrolyte ceramic for IT - SOFCs

NASA Astrophysics Data System (ADS)

Saini, Deepash S.; Singh, Lalit K.; Bhattacharya, D.

2018-04-01

A cost-effective modified combustion method using citric acid and glycine has recently been developed to synthesize high quality, and nanosized BaZr0.9Ho0.1O3 ceramic powder. BaZr0.9Ho0.1O3-δ ceramic powder was characterized by X-ray diffraction (XRD), high-resolution transmission electron microscopy (HRTEM) and field emission scanning electron microscopy (FESEM). XRD pattern of BaZr0.9Ho0.1O3-δ ceramic sintered at 1600 °C has shown that pure phase of BaZr0.9Ho0.1O3-δ with cubic Pm3¯m space group symmetry. The transmission electron microscopic investigation has shown that the particle size of the powder calcined at 1100 °C was in the range 30-80 nm. The FESEM image of sintered pellet at 1600 °C for 4 h reveals porous nature of BaZr0.9Ho0.1O3-δ with 83.7 relative density. Impedance analysis reveal three type relaxations in the temperature range 250 °C to 500 °C as studied at different frequencies over 100 Hz to 1 MHz in air. The grain boundary conductivity of BaZr0.9Ho0.1O3-δ ceramic is found lower then grain (bulk) conductivity due to core-space charge layer behavior in grain boundary.

Grain boundary engineering for structure materials of nuclear reactors

NASA Astrophysics Data System (ADS)

Tan, L.; Allen, T. R.; Busby, J. T.

2013-10-01

Grain boundary engineering (GBE), primarily implemented by thermomechanical processing, is an effective and economical method of enhancing the properties of polycrystalline materials. Among the factors affecting grain boundary character distribution, literature data showed definitive effect of grain size and texture. GBE is more effective for austenitic stainless steels and Ni-base alloys compared to other structural materials of nuclear reactors, such as refractory metals, ferritic and ferritic-martensitic steels, and Zr alloys. GBE has shown beneficial effects on improving the strength, creep strength, and resistance to stress corrosion cracking and oxidation of austenitic stainless steels and Ni-base alloys.

High Temperature Deformation of Twin-Roll Cast Al-Mn-Based Alloys after Equal Channel Angular Pressing.

PubMed

Málek, Přemysl; Šlapáková Poková, Michaela; Cieslar, Miroslav

2015-11-12

Twin roll cast Al-Mn- and Al-Mn-Zr-based alloys were subjected to four passes of equal channel angular pressing. The resulting grain size of 400 nm contributes to a significant strengthening at room temperature. This microstructure is not fully stable at elevated temperatures and recrystallization and vast grain growth occur at temperatures between 350 and 450 °C. The onset of these microstructure changes depends on chemical and phase composition. Better stability is observed in the Al-Mn-Zr-based alloy. High temperature tensile tests reveal that equal channel angular pressing results in a softening of all studied materials at high temperatures. This can be explained by an active role of grain boundaries in the deformation process. The maximum values of ductility and strain rate sensitivity parameter m found in the Al-Mn-Zr-based alloy are below the bottom limit of superplasticity (155%, m = 0.25). However, some features typical for superplastic behavior were observed-the strain rate dependence of the parameter m , the strengthening with increasing grain size, and the fracture by diffuse necking. Grain boundary sliding is believed to contribute partially to the overall strain in specimens where the grain size remained in the microcrystalline range.

High Temperature Deformation of Twin-Roll Cast Al-Mn-Based Alloys after Equal Channel Angular Pressing

PubMed Central

Málek, Přemysl; Šlapáková Poková, Michaela; Cieslar, Miroslav

2015-01-01

Twin roll cast Al-Mn- and Al-Mn-Zr-based alloys were subjected to four passes of equal channel angular pressing. The resulting grain size of 400 nm contributes to a significant strengthening at room temperature. This microstructure is not fully stable at elevated temperatures and recrystallization and vast grain growth occur at temperatures between 350 and 450 °C. The onset of these microstructure changes depends on chemical and phase composition. Better stability is observed in the Al-Mn-Zr-based alloy. High temperature tensile tests reveal that equal channel angular pressing results in a softening of all studied materials at high temperatures. This can be explained by an active role of grain boundaries in the deformation process. The maximum values of ductility and strain rate sensitivity parameter m found in the Al-Mn-Zr-based alloy are below the bottom limit of superplasticity (155%, m = 0.25). However, some features typical for superplastic behavior were observed—the strain rate dependence of the parameter m, the strengthening with increasing grain size, and the fracture by diffuse necking. Grain boundary sliding is believed to contribute partially to the overall strain in specimens where the grain size remained in the microcrystalline range. PMID:28793667

Grain neighbour effects on twin transmission in hexagonal close-packed materials

NASA Astrophysics Data System (ADS)

Arul Kumar, M.; Beyerlein, I. J.; McCabe, R. J.; Tomé, C. N.

2016-12-01

Materials with a hexagonal close-packed (hcp) crystal structure such as Mg, Ti and Zr are being used in the transportation, aerospace and nuclear industry, respectively. Material strength and formability are critical qualities for shaping these materials into parts and a pervasive deformation mechanism that significantly affects their formability is deformation twinning. The interaction between grain boundaries and twins has an important influence on the deformation behaviour and fracture of hcp metals. Here, statistical analysis of large data sets reveals that whether twins transmit across grain boundaries depends not only on crystallography but also strongly on the anisotropy in crystallographic slip. We show that increases in crystal plastic anisotropy enhance the probability of twin transmission by comparing the relative ease of twin transmission in hcp materials such as Mg, Zr and Ti.

Grain neighbour effects on twin transmission in hexagonal close-packed materials.

PubMed

Arul Kumar, M; Beyerlein, I J; McCabe, R J; Tomé, C N

2016-12-19

Materials with a hexagonal close-packed (hcp) crystal structure such as Mg, Ti and Zr are being used in the transportation, aerospace and nuclear industry, respectively. Material strength and formability are critical qualities for shaping these materials into parts and a pervasive deformation mechanism that significantly affects their formability is deformation twinning. The interaction between grain boundaries and twins has an important influence on the deformation behaviour and fracture of hcp metals. Here, statistical analysis of large data sets reveals that whether twins transmit across grain boundaries depends not only on crystallography but also strongly on the anisotropy in crystallographic slip. We show that increases in crystal plastic anisotropy enhance the probability of twin transmission by comparing the relative ease of twin transmission in hcp materials such as Mg, Zr and Ti.

High strength Sn-Mo-Nb-Zr alloy tubes and method of making same

DOEpatents

Cheadle, Brian A.

1977-01-01

Tubes for use in nuclear reactors fabricated from a quaternary alloy comprising 2.5-4.0 wt% Sn, 0.5-1.5 wt% Mo, 0.5-1.5 wt% Nb, balance essentially Zr. The tubes are fabricated by a process of hot extrusion, heat treatment, cold working to size and age hardening, so as to produce a microstructure comprising elongated .alpha. grains with an acicular transformed .beta. grain boundary phase.

Effects of Zr Addition on Strengthening Mechanisms of Al-Alloyed High-Cr ODS Steels.

PubMed

Ren, Jian; Yu, Liming; Liu, Yongchang; Liu, Chenxi; Li, Huijun; Wu, Jiefeng

2018-01-12

Oxide dispersion strengthened (ODS) steels with different contents of zirconium (denoted as 16Cr ODS, 16Cr-0.3Zr ODS and 16Cr-0.6Zr ODS) were fabricated to investigate the effects of Zr on strengthening mechanism of Al-alloyed 16Cr ODS steel. Electron backscatter diffraction (EBSD) results show that the mean grain size of ODS steels could be decreased by Zr addition. Transmission electron microscope (TEM) results indicate that Zr addition could increase the number density but decrease the mean diameter and inter-particle spacing of oxide particles. Furthermore, it is also found that in addition to Y-Al-O nanoparticles, Y-Zr-O oxides with finer size were observed in 16Cr-0.3Zr ODS and 16Cr-0.6Zr ODS steels. These changes in microstructure significantly increase the yield strength (YS) and ultimate tensile strength (UTS) of ODS steels through mechanisms of grain boundary strengthening and dispersion strengthening.

Effects of Zr Addition on Strengthening Mechanisms of Al-Alloyed High-Cr ODS Steels

PubMed Central

Ren, Jian; Yu, Liming; Liu, Yongchang; Liu, Chenxi; Li, Huijun; Wu, Jiefeng

2018-01-01

Oxide dispersion strengthened (ODS) steels with different contents of zirconium (denoted as 16Cr ODS, 16Cr-0.3Zr ODS and 16Cr-0.6Zr ODS) were fabricated to investigate the effects of Zr on strengthening mechanism of Al-alloyed 16Cr ODS steel. Electron backscatter diffraction (EBSD) results show that the mean grain size of ODS steels could be decreased by Zr addition. Transmission electron microscope (TEM) results indicate that Zr addition could increase the number density but decrease the mean diameter and inter-particle spacing of oxide particles. Furthermore, it is also found that in addition to Y-Al-O nanoparticles, Y-Zr-O oxides with finer size were observed in 16Cr-0.3Zr ODS and 16Cr-0.6Zr ODS steels. These changes in microstructure significantly increase the yield strength (YS) and ultimate tensile strength (UTS) of ODS steels through mechanisms of grain boundary strengthening and dispersion strengthening. PMID:29329260

Irradiation effects on multilayered W/ZrO2 film under 4 MeV Au ions

NASA Astrophysics Data System (ADS)

Wang, Hongwei; Gao, Yuan; Fu, Engang; Yang, Tengfei; Xue, Jianming; Yan, Sha; Chu, Paul K.; Wang, Yugang

2014-12-01

Irradiation induced structural changes in multilayered W/ZrO2 nanocomposites with periodic bilayer thicknesses of (7/14 nm) and (70/140 nm) were investigated following Au+ ion irradiation. The samples were irradiated by 4 MeV Au ions with fluences ranging from 6 × 1014 to 1 × 1016 ions/cm2. The immiscible W/ZrO2 interfaces remained unchanged without intermixing of the layers upon the irradiation. No voids were observed in the samples with different periodic layer thicknesses. The XRD and XTEM studies reveal thickness dependent microstructural changes in the samples. W and ZrO2 grains in the thinner (7/14 nm) bilayer sample exhibit significant resistance to grain growth compared to the thicker (70/140 nm) bilayer sample as well as a W monolayer film. The high fraction of flat interfaces as well as grain boundaries in multilayer films plays a role in suppressing ion irradiation-induced grain growth and void formation.

Nanocrystalline Al7075 + 1 wt % Zr Alloy Prepared Using Mechanical Milling and Spark Plasma Sintering

PubMed Central

Málek, Přemysl; Minárik, Peter; Chráska, Tomáš; Novák, Pavel; Průša, Filip

2017-01-01

The microstructure, phase composition, and microhardness of both gas-atomized and mechanically milled powders of the Al7075 + 1 wt % Zr alloy were investigated. The gas-atomized powder exhibited a cellular microstructure (grain size of a few µm) with layers of intermetallic phases along the cell boundaries. Mechanical milling (400 revolutions per minute (RPM)/8 h) resulted in a grain size reduction to the nanocrystalline range (20 to 100 nm) along with the dissolution of the intermetallic phases. Milling led to an increase in the powder’s microhardness from 97 to 343 HV. Compacts prepared by spark plasma sintering (SPS) exhibited negligible porosity. The grain size of the originally gas-atomized material was retained, but the continuous layers of intermetallic phases were replaced by individual particles. Recrystallization led to a grain size increase to 365 nm in the SPS compact prepared from the originally milled powder. Small precipitates of the Al3Zr phase were observed in the SPS compacts, and they are believed to be responsible for the retainment of the sub-microcrystalline microstructure during SPS. A more intensive precipitation in this SPS compact can be attributed to a faster diffusion due to a high density of dislocations and grain boundaries in the milled powder. PMID:28930192

Effect of sintering conditions on the electrical-transport properties of the SrZrO3-based protonic ceramic electrolyser membrane

NASA Astrophysics Data System (ADS)

Heras-Juaristi, Gemma; Pérez-Coll, Domingo; Mather, Glenn C.

2016-11-01

The effects of sintering temperature and addition of 4 mol.% ZnO as sintering additive on the crystal structure, microstructure and electrical properties of SrZr0.9Y0.1O3-δ are reported. The presence of ZnO as sintering aid brings about high densification at 1300 °C (relative density ∼97%); gas-tightness is not achieved for ZnO-free samples sintered below 1600 °C. Bulk conductivity (σB) is considerably higher in wet and dry O2 on doping with ZnO, but only slight variations of σB with sintering temperature are observed for the Zn-containing phases. Similarly, the apparent grain-boundary conductivities are much greater for the Zn-doped samples. The grain-boundary volume and accompanying resistances are much reduced on sintering at 1500 °C with ZnO addition in comparison to Zn-modified samples sintered below 1500 °C, with only minor changes in grain-boundary relaxation frequency observed. Conversely, in comparison to the undoped sample with sintering temperature of 1600 °C, there is an enormous improvement in the specific grain-boundary conductivity of two orders of magnitude for the ZnO-containing samples. Analysis on the basis of the core space-charge-layer model relates the enhancement of the grain-boundary transport to a higher concentration of charge carriers in the space-charge layer and associated lower potential barrier heights.

The influence of Sr on the microstructure, degradation and stress corrosion cracking of the Mg alloys - ZK40xSr.

PubMed

Chen, Lianxi; Bin, Yuanhong; Zou, Wenqi; Wang, Xiaojian; Li, Wei

2017-02-01

In the present work, new magnesium (Mg) alloys (Mg-4Zn-0.6Zr-xSr, x=0, 0.4, 0.8, 1.2, 1.6wt%; ZK40xSr) were prepared and studied as potential biodegradable materials. The influence of strontium (Sr) addition on the properties of the new Mg alloys was investigated, which included microstructure, corrosion degradation, and the stress corrosion cracking (SCC) susceptibility. The average grain size of the ZK40Sr was approximately 100µm, which was significantly smaller than that of ZK40 alloy without Sr (402.3±40.2µm). The size of grain boundaries precipitates in the ZK40xSr alloys gradually increased with the increase of Sr content. The grain boundaries finally showed a continuously distribution and net-like shape. The degradation test showed that the average degradation rate of the ZK40xSr alloys increased with the increase of Sr addition. In the case of Mg-4Zn-0.6Zr, the degradation rate was 2.2mgcm -2 day -1 , which was lower than that of Mg-4Zn-0.6Zr-1.6Sr (4.93mgcm -2 day -1 ). When the ZK40xSr alloys were immersed in m-SBF, the rod-like Sr-contained hydroxyapatite (HA) substance was detected, which was known to enhance cell growth around bone implants. The fracture surfaces of the as-cast Mg-4Zn-0.6Zr-1.6Sr were shown intergranular stress corrosion cracking (IGSCC) patterns. The increase of SCC susceptibility of the higher Sr ZK40xSr alloys was attributed to the increase of micro-galvanic corrosion between the α-Mg and the grain boundaries precipitates. The SCC susceptibility values were ≈0.13 and ≈0.41 for the Mg-4Zn-0.6Zr-0.4Sr and the Mg-4Zn-0.6Zr-1.6Sr, respectively. Copyright © 2016 Elsevier Ltd. All rights reserved.

Effect of doping ions on the structural defect and the electrical behavior of CaCu{sub 3}Ti{sub 4}O{sub 12} ceramics

DOE Office of Scientific and Technical Information (OSTI.GOV)

Xue, Renzhong; Department of Technology and Physics, Zhengzhou University of Light Industry, Zhengzhou 450002; Zhao, Gaoyang, E-mail: zhaogy@xaut.edu.cn

Graphical abstract: The dielectric constant decreases with Ta doping, increases with Y doping and keeps almost constant with Zr doping compared with that of pure CCTO. - Highlights: • Y and Ta doping cause different defect types and concentration. • Defect influences the grain boundary mobility and results in different grain size. • Y doping increases the dielectric constant and decreases the nonlinear property. • Ta doping decreases the dielectric constant and enhances the nonlinear property. • Zr doped sample has nearly the defect type and dielectric properties as CaCu{sub 3}Ti{sub 4}O{sub 12}. - Abstract: The microstructure, dielectric and electricalmore » properties of CaCu{sub 3}Ti{sub 4−x}R{sub x}O{sub 12} (R = Y, Zr, Ta; x = 0 and 0.005) ceramics were investigated by XRD, Raman spectra, SEM and dielectric spectrum measurements. Positron annihilation measurements have been performed to investigate the influence of doping on the defects. The results show that all samples form a single crystalline phase. Y and Ta doping cause different defect types and increase the defect size and concentration, which influence the mobility of grain boundary and result in the different grain size. Y doping increases the dielectric constant and decreases the nonlinear property while Ta doping lead to an inverse result. Zr-doped sample has nearly the defect type, grain morphology and dielectric properties as pure CaCu{sub 3}Ti{sub 4}O{sub 12}. The effects of microstructure including the grain morphology and the vacancy defects on the mechanism of the dielectric and electric properties by doping are discussed.« less

Surface Modification of Solution-Processed ZrO2 Films through Double Coating for Pentacene Thin-Film Transistors

NASA Astrophysics Data System (ADS)

Kwon, Jin-Hyuk; Bae, Jin-Hyuk; Lee, Hyeonju; Park, Jaehoon

2018-03-01

We report the modification of surface properties of solution-processed zirconium oxide (ZrO2) dielectric films achieved by using double-coating process. It is proven that the surface properties of the ZrO2 film are modified through the double-coating process; the surface roughness decreases and the surface energy increases. The present surface modification of the ZrO2 film contributes to an increase in grain size of the pentacene film, thereby increasing the field-effect mobility and decreasing the threshold voltage of the pentacene thin-film transistors (TFTs) having the ZrO2 gate dielectric. Herein, the molecular orientation of pentacene film is also studied based on the results of contact angle and X-ray diffraction measurements. Pentacene molecules on the double-coated ZrO2 film are found to be more tilted than those on the single-coated ZrO2 film, which is attributed to the surface modification of the ZrO2 film. However, no significant differences are observed in insulating properties between the single-and the double-coated ZrO2 dielectric films. Consequently, the characteristic improvements of the pentacene TFTs with the double-coated ZrO2 gate dielectric film can be understood through the increase in pentacene grain size and the reduction in grain boundary density.

Grain neighbour effects on twin transmission in hexagonal close-packed materials

DOE PAGES

Arul Kumar, Mariyappan; Beyerlein, Irene Jane; McCabe, Rodney James; ...

2016-12-19

Materials with a hexagonal close-packed (hcp) crystal structure such as Mg, Ti and Zr are being used in the transportation, aerospace and nuclear industry, respectively. Material strength and formability are critical qualities for shaping these materials into parts and a pervasive deformation mechanism that significantly affects their formability is deformation twinning. The interaction between grain boundaries and twins has an important influence on the deformation behaviour and fracture of hcp metals. Here, statistical analysis of large data sets reveals that whether twins transmit across grain boundaries depends not only on crystallography but also strongly on the anisotropy in crystallographic slip.more » As a result, we show that increases in crystal plastic anisotropy enhance the probability of twin transmission by comparing the relative ease of twin transmission in hcp materials such as Mg, Zr and Ti.« less

Study of twin-roll cast Aluminium alloys subjected to severe plastic deformation by equal channel angular pressing

NASA Astrophysics Data System (ADS)

Poková, M.; Cieslar, M.

2014-08-01

Aluminium alloys prepared by twin-roll casting method become widely used in industry applications. Their high solid solution supersaturation and finer grains ensure better mechanical properties when compared with the direct-chill cast ones. One of the possibilities how to enhance their thermal stability is the addition of zirconium. After heat treatment Al3Zr precipitates form and these pin moving grain boundaries when the material is exposed to higher temperatures. In the present work twin-roll cast aluminium alloys based on AA3003 with and without Zr addition were annealed for 8 hours at 450 °C to enable precipitation of Al3Zr phase. Afterwards they were subjected to severe plastic deformation by equal channel angular pressing, which led to the reduction of average grain size under 1 μm. During subsequent isochronal annealing recovery and recrystallization took place. These processes were monitored by microhardness measurements, light optical microscopy and in-situ transmission electron microscopy. The addition of Zr stabilizes the grain size and increases the recrystallization temperature by 100 °C.

Sub-kT/q subthreshold slope p-metal-oxide-semiconductor field-effect transistors with single-grained Pb(Zr,Ti)O3 featuring a highly reliable negative capacitance

NASA Astrophysics Data System (ADS)

Park, Jae Hyo; Joo, Seung Ki

2016-03-01

A reliable on/off switching with an sub-kT/q subthreshold slope (38 mV/dec at room temperature) is experimentally demonstrated with using selectively nucleated laterally crystallized single-grain Pb(Zr,Ti)O3 (PZT) ferroelectric and ZrTiO4 paraelectric thin-film. The combination of ferroelectric and paraelectric thin-film is enabled to form a negative capacitance (NC) at the weak inversion region. However, the PZT grain-boundary easily degrades the NC properties after switching the on/off more than 108 times. It is found that the polarization of PZT is diminished from the path of grain-boundary. Here, we effectively suppress the degradation of NC MOS-FET which did not showed any fatigue even after 108 on/off switching. At the request of the authors this article is retracted due to duplication of figures and significant overlap with other publications by the authors and because of concerns about the accuracy of the description of the devices and materials from which the reported results were obtained. The authors recognize that these represent serious errors and sincerely apologize for any inconvenience they may have caused. The article is retracted from the scientific record with effect from 17 February 2017.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Arul Kumar, Mariyappan; Beyerlein, Irene Jane; McCabe, Rodney James

Materials with a hexagonal close-packed (hcp) crystal structure such as Mg, Ti and Zr are being used in the transportation, aerospace and nuclear industry, respectively. Material strength and formability are critical qualities for shaping these materials into parts and a pervasive deformation mechanism that significantly affects their formability is deformation twinning. The interaction between grain boundaries and twins has an important influence on the deformation behaviour and fracture of hcp metals. Here, statistical analysis of large data sets reveals that whether twins transmit across grain boundaries depends not only on crystallography but also strongly on the anisotropy in crystallographic slip.more » As a result, we show that increases in crystal plastic anisotropy enhance the probability of twin transmission by comparing the relative ease of twin transmission in hcp materials such as Mg, Zr and Ti.« less

Mechanisms of grain refinement in aluminum alloys in the process of severe plastic deformation

NASA Astrophysics Data System (ADS)

Kaibyshev, R. O.; Mazurina, I. A.; Gromov, D. A.

2006-01-01

A study of the mechanisms of grain refinement in the process of severe plastic deformation of two aluminum alloys, i.e., 2219 bearing nanometric particles of Al3Zr and low-alloy Al-3% Cu, is described. The alloys are deformed by the method of equal channel angular pressing at 250°C to a maximum strain degree of about 12. The angles of (sub)grain boundaries in alloy 2219 are determined with the help of transmission electron microscopy by the method of Kikuchi lines. The evolution of the microstructure in alloy Al-3% Cu is studied with the help of grain-boundary maps obtained by the method of electron back-scattered diffraction.

Microstructure and Mechanical Properties of W-ZrC Composites Synthesized by Reactive Melt Infiltration of Zr2Cu into Porous Preforms from Partially Carburized W Powders

NASA Astrophysics Data System (ADS)

Wang, Dong; Wang, Yu-Jin; Huo, Si-Jia; Zhao, Yan-Wei; Ouyang, Jia-Hu; Song, Gui-Ming; Zhou, Yu

2018-03-01

W-ZrC composites with different W contents from 48 to 73 vol.% have been synthesized by reactive melt infiltration of Zr2Cu melt into porous preforms from partially carburized W powders at 1300 °C for 1 h in vacuum. The influences of carbon content and porosity in the preforms on microstructure and mechanical properties of W-ZrC composites are investigated. Cold isostatic pressing followed by pre-sintering process is used to produce porous preforms with suitable porosities of 53.6-47% under a pressure of 100 MPa to allow sufficient penetration of Zr2Cu melt into the preforms. Small amounts of Cu-rich phases form in the synthesized W-ZrC composites after a complete reaction of y/2xZr2Cu(l) + WC y (s) = y/xZrC x (s) + W(s) + y/2xCu(l). These Cu-rich phases are distributed not only at the phase boundaries of W matrix and ZrC grains, but also in the interior of ZrC x grains. With decreasing W content from 73 to 48 vol.% in the W-ZrC composites, the flexural strength and fracture toughness increase from 519 to 657 MPa and from 9.1 to 10.6 MPa m1/2, respectively.

In-situ observation of recrystallization in an AlMgScZr alloy using confocal laser scanning microscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Taendl, J., E-mail: johannes.taendl@tugraz.atl; Nambu, S.; Orthacker, A.

2015-10-15

In this work we present a novel in-situ approach to study the recrystallization behavior of age hardening alloys. We use confocal laser scanning microscopy (CLSM) at 400 °C to investigate the static recrystallization of an AlMg4Sc0.4Zr0.12 alloy in-situ. The results are combined with electron backscatter diffraction (EBSD) and transmission electron microscopy (TEM) analyses. It was found that CLSM is a powerful tool to visualize both the local initiation and temporal sequence of recrystallization. After fast nucleation and initial growth, the grain growth rate decreases and the grain boundary migration stops after some minutes due to Zener pinning from Al{sub 3}(Sc,Zr)more » precipitates produced during the heat treatment. EBSD and TEM analyses confirm both the boundary movements and the particle-boundary interactions. - Highlights: • First time that CLSM is used to study recrystallization in-situ. • The start and end of recrystallization can be directly observed. • The procedure is easy to apply and requires only simple data interpretation. • In-situ observations on the surface correlate to modifications inside the bulk. • In-situ observations correlate to EBSD and EFTEM analyses.« less

Half-Heusler Alloys as Promising Thermoelectric Materials

NASA Astrophysics Data System (ADS)

Page, Alexander A.

This thesis describes Ph.D. research on the half-Heusler class of thermoelectric materials. Half-Heusler alloys are a versatile class of materials that have been studied for use in photovoltaics, phase change memory, and thermoelectric power generation. With respect to thermoelectric power generation, new approaches were recently developed in order to improve the thermoelectric figure of merit, ZT, of half-Heusler alloys. Two of the strategies discussed in this work are adding excess Ni within MNiSn (M = Ti, Zr, or Hf) compounds to form full-Heusler nanostructures and using isoelectronic substitution of Ti, Zr, and Hf in MNiSn compounds to create microscale grain boundaries. This work uses computational simulations based on density functional theory, combined with the cluster expansion method, to predict the stable phases of pseudo-binary and pseudo-ternary composition systems. Statistical mechanics methods were used to calculate temperature-composition phase diagrams that relate the equilibrium phases. It is shown that full-Heusler nanostructures are predicted to remain stable even at high temperatures, and the microscale grain boundaries observed in (Ti,Zr,Hf)NiSn materials are found to be thermodynamically unstable at equilibrium. A new strategy of combining MNiSn materials with ZrNiPb has also recently emerged, and theoretical and experimental work show that a solid solution of the two materials is stable.

The evolution of helium from aged Zr tritides: A thermal helium desorption spectrometry study

NASA Astrophysics Data System (ADS)

Cheng, G. J.; Huang, G.; Chen, M.; Zhou, X. S.; Liu, J. H.; Peng, S. M.; Ding, W.; Wang, H. F.; Shi, L. Q.

2018-02-01

The evolution of He from Zr-tritides was investigated for aging times up to about 6.5 years using analytical thermal helium desorption spectrometry (THDS). Zr films were deposited onto Mo substrates and then converted into Zr-tritides (ZrT1.70∼1.95) inside a tritiding apparatus loaded with pure tritium gas. During aging, there are at least five forms of He in Zr-tritides, and more than 99% of He atoms are in the form of He bubbles. The isolated He bubbles in lattices begin to link with each other when the He/Zr atom ratio reaches about 0.21, and are connected to grain boundaries or dislocation networks at He concentration of He/Zr ≈ 0.26. An interconnected system of channels decorated by bubbles evolves from the network dislocations, dislocation loops and internal boundaries. These He filled networks are formed completely when the He/Zr atom ratio is about 0.38. Once the He/Zr reached about 0.45, the networks of He bubble penetrate to the film surface and He begins an "accelerated release". This critical ratio of He to Zr for He accelerated release is much greater than that found previously for Ti-tritides (0.23-0.30). The difference of He retention in Zr-tritides and Ti-tritides was also discussed in this paper.

Microstructural analysis of biodegradable Mg-0.9Ca-1.2Zr alloy

NASA Astrophysics Data System (ADS)

Istrate, B.; Munteanu, C.; Geanta, V.; Baltatu, S.; Focsaneanu, S.; Earar, K.

2016-08-01

Magnesium alloys have applications in aerospace and medical applications as biodegradable orthopedic implants. Alloying with biocompatible elements, such as calcium or zirconium contribute to refining the the microstructure and improves corrosion resistance with the formation of an eutectic compound - Mg2Ca at boundary alpha-Mg grains. The purpose of this paper is to present the microstructure throw optical and scanning electron methods and phase and constituents identification with X-ray analysis. The results showed the presence of alpha-Mg grains with formation of a mechanical compound - Mg2Ca and appearance of alpha- Zr phase relatively uniformly distributed in nests.

Compatibility of grain-stabilized platinum with candidate propellants for resistojets

NASA Technical Reports Server (NTRS)

Whalen, M. V.; Grisnik, S. P.

1985-01-01

Resistojets are candidates for space station auxiliary propulsion, and should be characterized by both long life and multipropellant operations, requirements limited by available materials. Grain stabilized platinum is examined for use as a resistojet thruster material. Use of platinum in other applications indicates it can be used at moderately high temperatures for extended periods of time. Past results indicate that grain-stabilized platinum should be sufficiently inert in candidate propellant environments. Therefore, compatibility of platinum-yttria (P/Y2O3) and platinum-zirconia (Pt/ZrO2) with carbon dioxide, methane, hydrogen and ammonia is examined. A series of 1000 hr tests in CO2, H2, and NH3 is conducted at 1400 C and a series of 1000 hr tests in CH4 is conducted at about 500 C. Scanning electron microscopy, Auger electron spectroscopy and depth profiling analysis are then used to determine the effects of propellants on the material surface, to evaluate possible material contamination and to evaluate grain growth. The results indicate that there is carbon deposition on the surface of the Pt/Y2O3 and Pt/ZrO2 in both the CO2 and CH4 environments. In the H2 environment, the Pt/Y2O3 and Pt/ZrO2 specimen surfaces are roughened. After exposure to the NH3 environment, the Pt/Y2O3 and Pt/ZrO2 are roughened and pitted over the entire heated area with some pitted areas along the grain boundaries. SEM photos show grain growth in cross-sectional views of all the Pt/Y2O3 samples and the Pt/ZrO2 samples, except that tested in methane. Mass loss measurements indicate that Pt/Y2O3 and Pt/ZrO2 would last in excess of 200,000 hr in each propellant environment. However, in NH3 both Pt/Y2O3 and Pt/ZrO2 are severely pitted, with voids up to 50 percent into the material. Pt/Y2O3 and Pt/ZrO2 are not recommended for high temperature service in NH3.

Sodium Ion Diffusion in Nasicon (Na3Zr2Si2PO12) Solid Electrolytes: Effects of Excess Sodium.

PubMed

Park, Heetaek; Jung, Keeyoung; Nezafati, Marjan; Kim, Chang-Soo; Kang, Byoungwoo

2016-10-04

The Na superionic conductor (aka Nasicon, Na 1+x Zr 2 Si x P 3-x O 12 , where 0 ≤ x ≤ 3) is one of the promising solid electrolyte materials used in advanced molten Na-based secondary batteries that typically operate at high temperature (over ∼270 °C). Nasicon provides a 3D diffusion network allowing the transport of the active Na-ion species (i.e., ionic conductor) while blocking the conduction of electrons (i.e., electronic insulator) between the anode and cathode compartments of cells. In this work, the standard Nasicon (Na 3 Zr 2 Si 2 PO 12 , bare sample) and 10 at% Na-excess Nasicon (Na 3.3 Zr 2 Si 2 PO 12 , Na-excess sample) solid electrolytes were synthesized using a solid-state sintering technique to elucidate the Na diffusion mechanism (i.e., grain diffusion or grain boundary diffusion) and the impacts of adding excess Na at relatively low and high temperatures. The structural, thermal, and ionic transport characterizations were conducted using various experimental tools including X-ray diffraction (XRD), differential scanning calorimetry (DSC), scanning electron microscopy (SEM), and electrochemical impedance spectroscopy (EIS). In addition, an ab initio atomistic modeling study was carried out to computationally examine the detailed microstructures of Nasicon materials, as well as to support the experimental observations. Through this combination work comprising experimental and computational investigations, we show that the predominant mechanisms of Na-ion transport in the Nasicon structure are the grain boundary and the grain diffusion at low and high temperatures, respectively. Also, it was found that adding 10 at% excess Na could give rise to a substantial increase in the total conductivity (e.g., ∼1.2 × 10 -1 S/cm at 300 °C) of Nasicon electrolytes resulting from the enlargement of the bottleneck areas in the Na diffusion channels of polycrystalline grains.

Microstructure and mechanical properties investigation of in situ TiB2 and ZrB2 reinforced Al-4Cu composites

NASA Astrophysics Data System (ADS)

Lutfi Anis, Ahmad; Ramli, Rosmamuhammadani; Darham, Widyani; Zakaria, Azlan; Talari, Mahesh Kumar

2016-02-01

Conventional Al-Cu alloys exhibit coarse grain structure leading to inferior mechanical properties in as-cast condition. Expensive thermo-mechanical treatments are needed to improve microstructure and corresponding mechanical properties. In situ Al-based composites were developed to improve mechanical properties by dispersion strengthening and grain refinement obtained by the presence of particulates in the melt during solidification. In this work Al-4Cu - 3TiB2 and Al-4Cu-3ZrB2 in situ composites were prepared by liquid casting method. XRD, electron microscopy and mechanical tests were performed on suitably sectioned and metallographically prepared surfaces to investigate the phase distribution, hardness and tensile properties. It was found that the reinforcement particles were segregated along the grain boundaries of Al dendrites. Tensile fracture morphology for both Al-4Cu - 3TiB2 and Al-4Cu-3ZrB2 were analyzed and compared to determine the fracture propagation mechanism in the composites. Al-4Cu-3ZrB2 in situ composites displayed higher strength and hardness compared to Al-4Cu-3TiB2 which could be ascribed to the stronger interfacial bonding between the Al dendrites and ZrB2 particulates as evidenced from fractographs.

Effect of Nd doping on structural, dielectric and thermodynamic properties of PZT (65/35) ceramic

NASA Astrophysics Data System (ADS)

Mohiddon, Md Ahamad; Kumar, Abhishek; Yadav, K. L.

2007-05-01

The influence of neodymium (Nd) addition on the phase formation and dielectric properties of Pb(Zr 0.65Ti 0.35)O 3 composition prepared from mixed oxide method was analyzed. Pellets were sintered in air and PbZrO 3 (PZ) atmosphere separately. Non-perovskite ZrO 2 phase was observed in samples which were sintered in air, also grain size was found to decrease with Nd doping in non-PZ environment samples. Decrease in transition temperature by 80 °C with increasing Nd concentration was observed in both set of samples. Maximum dielectric constant and dielectric losses are found to decrease with Nd doping. Complex impedance analysis revealed that grain boundary resistance increases with Nd doping. Thermodynamic parameters such as change in enthalpy, free energy and change in entropy were studied.

Relations between temperature coefficients of permittivity and elastic compliances in PZT ceramics near the morphotropic phase boundary.

PubMed

Boudys, M

1991-01-01

Variations of temperature coefficients of permittivity epsilon(33)(T), elastic compliances at constant electric fields s(11)(E), and constant polarization s(11)(P) with a Zr/Ti ratio of Pb(Zr(x)Ti(1-x))O(3) and Pb[(Sb(1/3)Mn(2/3))(0.05)Zr(x)Ti (0.95-x)]O(3) solid solutions, were investigated. Relations between temperature coefficients of epsilon(33)(T ), S(11)(E), and S(11) (P) were theoretically derived; a discrepancy was found between theoretical relations and experimental results. On the basis of the observed discrepancy, it is proposed that some extrinsic effects arising from the motion of interphase boundaries between the tetragonal and the rhombohedral phases which exist in grains contribute to values of both elastic compliances.

Effect of carbide additions on grain growth in TiC-Ni cermets

NASA Astrophysics Data System (ADS)

Shin, Soon-Gi; Lee, Jun-Hee

2006-02-01

The growth of carbide particles in TiC-XC-2 vol.% Ni and TiC-XC-30 vol.% Ni alloys, where X=Zr, Cr, W, Ta and Mo, was fitted to an equation of the form d3-do 3=Kt. The grain growth behavior during liquid phase sintering at 1673K decreased markedly with the addition of Mo2C or WC, changed little for TaC, and increased with the addition of ZrC or Cr3C2. The grain contiguity decreased with increasing Ni content in the TiC-Mo2C-Ni alloy and was greater in the alloys with smaller growth rate constant. Consequently, the effect of carbide addition on the grain growth of 2 vol.% Ni alloys was found to be similar to that of 30 vol.% Ni alloys. The grain growth mechanism could be explained by the effect of contiguous carbide grain boundaries in restricting the overall grain growth, as well as the area of the solid/liquid interfaces in the alloy by the usual solution/reprecipitation model.

Thermal stability of Cu-Cr-Zr alloy processed by equal-channel angular pressing

DOE Office of Scientific and Technical Information (OSTI.GOV)

Abib, Khadidja

Thermal stability of a Cu-Cr-Zr alloy processed by equal-channel angular pressing up to16 passes was investigated using isochronal annealing ranging from 250 to 850 °C for 1 h. The microstructure, crystallographic texture and micro hardness of samples were characterized through electron back scatter diffraction and Vickers micro hardness measurements. The recrystallized grain size was stable between 250 °C and 500 °C then increased quickly. The achieved mean grain size, after 1, 4 and 16 ECAP passes, was around 5.5 μm. A discontinuous mode of recrystallization was found to occur and a Particle Simulated Nucleation mechanism was evidenced. The evolution ofmore » the high angle grain boundary fraction increased notably after annealing above 550 °C. The crystallographic texture after isochronal annealing was similar to that of ECAP simple shear, no change of the texture during annealing was observed but only slight intensity variations. Micro hardness of all Cu–Cr–Zr samples showed a hardening with two peaks at 400 and 500 °C associated with precipitation of Cu cluster and Cu{sub 5}Zr phase respectively, followed by a subsequent softening upon increasing the annealing temperature due to recrystallization. - Highlight: •The Cu-1Cr-0.1Zr alloy shows a very good thermal stability up to 550 °C after ECAP. •A discontinuous recrystallization was found to occur and PSN mechanism was evidenced. •The annealing texture was found weak and some new components appear. •Hardening is attributed to the Cr clustering followed by the Cu{sub 51}Zr{sub 14} precipitation. •Softening is a result of recrystallization and grain growth progressing.« less

Properties of Cu-Based Shape-Memory Alloys Prepared by Selective Laser Melting

NASA Astrophysics Data System (ADS)

Gustmann, T.; dos Santos, J. M.; Gargarella, P.; Kühn, U.; Van Humbeeck, J.; Pauly, S.

2017-03-01

Two shape-memory alloys with the nominal compositions (in wt.%) Cu-11.85Al-3.2Ni-3Mn and Cu-11.35Al-3.2Ni-3Mn-0.5Zr were prepared by selective laser melting (SLM). The parameters were optimised to identify the process window, in which almost fully dense samples can be obtained. Their microstructures were analysed and correlated with the shape-memory behaviour as well as the mechanical properties. Suction-cast specimens were also produced for comparison. Mainly, β 1' martensite forms in all samples, but 0.5 wt.% of Zr stabilises the Y phase (Cu2AlZr), and its morphology depends on the thermal history and cooling rate. After annealing, the Y phase is primarily found at the grain boundaries hampering grain coarsening. Due to the relative high cooling rates applied here, Zr is mostly dissolved in the martensite in the as-prepared samples and it has a grain-refining effect only up to a critical cooling rate. The Zr-containing samples have increased transformation temperatures, and the Y phase seems to be responsible for the jerky martensite-to-austenite transformation. All the samples are relatively ductile because they mostly fracture in a transgranular manner, exhibiting the typical double yielding. Selective laser melting allows the adjustment of the transformation temperatures and the mechanical properties already during processing without the need of a subsequent heat treatment.

Intrinsic stress in ZrN thin films: Evaluation of grain boundary contribution from in situ wafer curvature and ex situ x-ray diffraction techniques

DOE Office of Scientific and Technical Information (OSTI.GOV)

Koutsokeras, L. E.; Department of Materials Science and Engineering, University of Ioannina, Ioannina 45110; Abadias, G.

2012-05-01

Low-mobility materials, like transition metal nitrides, usually undergo large residual stress when sputter-deposited as thin films. While the origin of stress development has been an active area of research for high-mobility materials, atomistic processes are less understood for low-mobility systems. In the present work, the contribution of grain boundary to intrinsic stress in reactively magnetron-sputtered ZrN films is evaluated by combining in situ wafer curvature measurements, providing information on the overall biaxial stress, and ex situ x-ray diffraction, giving information on elastic strain (and related stress) inside crystallites. The thermal stress contribution was also determined from the in situ stressmore » evolution during cooling down, after deposition was stopped. The stress data are correlated with variations in film microstructure and growth energetics, in the 0.13-0.42 Pa working pressure range investigated, and discussed based on existing stress models. At low pressure (high energetic bombardment conditions), a large compressive stress is observed due to atomic peening, which induces defects inside crystallites but also promotes incorporation of excess atoms in the grain boundary. Above 0.3-0.4 Pa, the adatom surface mobility is reduced, leading to the build-up of tensile stress resulting from attractive forces between under-dense neighbouring column boundary and possible void formation, while crystallites can still remain under compressive stress.« less

Electrical resistance oscillations during plastic deformation in A Ti-Al-Nb-Zr alloy at 4·2 K

NASA Astrophysics Data System (ADS)

Nikiforenko, V. N.; Lavrentev, F. F.

1986-10-01

The serrated plastic flow in titanium alloy containing 5% Al, 2·5% Zr and 2% Nb has been investigated by measuring its electrical resistance and applying selective chemical etching. The electrical resistance was found to oscillate under active deformation at 4·2 K. Analysis of the possible causes seems to indicate a dominant role of break by dislocation pile-ups through obstacles, viz second phase precipitates and grain boundaries.

Cross-Correlation for Automated Stitching of Two-Dimensional Multi-Tile Electron Backscatter Diffraction Data (Preprint)

DTIC Science & Technology

2012-08-01

270 350x 650 (25, 26) 2 20 Ni-15Al- 5Cr+C,B,Zr 187 x 187 500x 44 ( 4 , 11) 0.5 40 A. Coarse grain, single phase α- titanium The coarse grained... titanium alloy serves as an instructive example because, as evident in Figure 4 (a), only one triple point and one grain boundary appear in the search...wpafb.af.mil Figure 4 . Crystal orientation maps for the first (left) and second (current) tiles of (a) coarse grained α- Titanium , (b) a 2x2 array of a

Investigation of magnetic and structural properties of Ni-Zr co-doped M-type Sr-La hexaferrites

NASA Astrophysics Data System (ADS)

Yang, Yujie; Wang, Fanhou; Shao, Juxiang; Huang, Duohui; Tang, Jin; Rehman, Khalid Mehmood Ur

2018-02-01

In this research, Ni2+ and Zr4+ co-doped Sr-La hexaferrites Sr0.7La0.3Fe12.0-2 x (NiZr) x O19 (0.0 ≤ x ≤ 0.5) were synthesized by the standard ceramic method. The phase identification of the hexaferrites was confirmed by X-ray diffraction analysis. X-ray diffraction analysis showed that all the samples were in single phase M-type hexagonal structure and no impurity phase was observed. Lattice parameters ( c and a) increased with increasing NiZr content ( x) from 0.0 to 0.5. The morphology of the hexaferrites was analyzed by a field emission scanning electron microscopy (FE-SEM). FE-SEM micrographs showed that the grains exhibited hexagonal shape in a plate-like structure with clear grain boundaries. Magnetization properties of the hexaferrites were carried out at room temperature using a physical property measurement system-vibrating sample magnetometer. The values of saturation magnetization ( M s), remanent magnetization ( M r) and coercivity ( H c) were calculated from magnetic hysteresis ( M- H) loops. M s and H c decreased with increasing NiZr content ( x) from 0.0 to 0.5. M r and M r/ M s ratio first increased with increasing NiZr content ( x) from 0.0 to 0.1, and then decreased when NiZr content ( x) ≥ 0.1.

Effects of two-step homogenization on precipitation behavior of Al{sub 3}Zr dispersoids and recrystallization resistance in 7150 aluminum alloy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Guo, Zhanying; Key Laboratory for Anisotropy and Texture of Materials, Northeastern University, Shenyang 110819, China,; Zhao, Gang

2015-04-15

The effect of two-step homogenization treatments on the precipitation behavior of Al{sub 3}Zr dispersoids was investigated by transmission electron microscopy (TEM) in 7150 alloys. Two-step treatments with the first step in the temperature range of 300–400 °C followed by the second step at 470 °C were applied during homogenization. Compared with the conventional one-step homogenization, both a finer particle size and a higher number density of Al{sub 3}Zr dispersoids were obtained with two-step homogenization treatments. The most effective dispersoid distribution was attained using the first step held at 300 °C. In addition, the two-step homogenization minimized the precipitate free zonesmore » and greatly increased the number density of dispersoids near dendrite grain boundaries. The effect of two-step homogenization on recrystallization resistance of 7150 alloys with different Zr contents was quantitatively analyzed using the electron backscattered diffraction (EBSD) technique. It was found that the improved dispersoid distribution through the two-step treatment can effectively inhibit the recrystallization process during the post-deformation annealing for 7150 alloys containing 0.04–0.09 wt.% Zr, resulting in a remarkable reduction of the volume fraction and grain size of recrystallization grains. - Highlights: • Effect of two-step homogenization on Al{sub 3}Zr dispersoids was investigated by TEM. • Finer and higher number of dispersoids obtained with two-step homogenization • Minimized the precipitate free zones and improved the dispersoid distribution • Recrystallization resistance with varying Zr content was quantified by EBSD. • Effectively inhibit the recrystallization through two-step treatments in 7150 alloy.« less

In-situ analysis of the slip activity during tensile deformation of cast and extruded Mg-10Gd-3Y-0.5Zr (wt.%) at 250 °C

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, H.; The State Key Laboratory of Metal Matrix Composites, Shanghai Jiao Tong University, 800 Dongchuan Road, Shanghai 200240; Department of Chemical Engineering and Materials Science, Michigan State University, East Lansing, MI 48824

The slip activity and slip interaction in tensile deformation of peak-aged cast and extruded Mg-10Gd-3Y-0.5Zr (wt.%) at 250 °C was investigated using in-situ scanning electron microscopy. Basal slip was the most likely system to be activated during the tensile deformation, while prismatic < a > and pyramidal < c + a > slip also contributed to the deformation. No twinning was observed. The number of non-basal slip systems accounted for ~ 36% of the total active slip systems for the cast alloy, while non-basal slip accounted for 12–17% of the total deformation observations in the extruded alloy. Multiple-slip was observedmore » within grains, and the basal/prismatic pairing type dominated the multiple-slip observations. Slip transfer occurred across grain boundaries and most of the slip transfer observations showed basal-basal type. The involved slip systems of slip transfer pairs were always associated with the same < a > direction. The slip transfer occurred more easily at low angle boundaries (LABs) and boundaries with misorientations greater than 75°. - Highlights: • Slip deformation of a Mg-RE alloy at 250 °C was investigated using in-situ SEM. • The extruded-T5 GW103 alloy did not exhibit a high anisotropic behavior. • Multiple-slip was observed within grains, and basal/prismatic type dominated. • Slip transfer occurred and most of the observations showed basal-basal type. • Slip transfer occurred more easily at LABs and boundaries with misorientations > 75°.« less

Computational and Experimental Studies of Microstructure-Scale Porosity in Metallic Fuels for Improved Gas Swelling Behavior

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mllett, Paul; McDeavitt, Sean; Deo, Chaitanya

This proposal will investigate the stability of bimodal pore size distributions in metallic uranium and uranium-zirconium alloys during sintering and re-sintering annealing treatments. The project will utilize both computational and experimental approaches. The computational approach includes both Molecular Dynamics simulations to determine the self-diffusion coefficients in pure U and U-Zr alloys in single crystals, grain boundaries, and free surfaces, as well as calculations of grain boundary and free surface interfacial energies. Phase-field simulations using MOOSE will be conducted to study pore and grain structure evolution in microstructures with bimodal pore size distributions. Experiments will also be performed to validate themore » simulations, and measure the time-dependent densification of bimodal porous compacts.« less

Microstructure and Mechanical Properties of Nano-Size Zirconium Carbide Dispersion Strengthened Tungsten Alloys Fabricated by Spark Plasma Sintering Method

NASA Astrophysics Data System (ADS)

Xie, Zhuoming; Liu, Rui; Fang, Qianfeng; Zhang, Tao; Jiang, Yan; Wang, Xianping; Liu, Changsong

2015-12-01

W-(0.2, 0.5, 1.0)wt% ZrC alloys with a relative density above 97.5% were fabricated through the spark plasma sintering (SPS) method. The grain size of W-1.0wt% ZrC is about 2.7 μm, smaller than that of pure W and W-(0.2, 0.5)wt% ZrC. The results indicated that the W-ZrC alloys exhibit higher hardness at room temperature, higher tensile strength at high temperature, and a lower ductile to brittle transition temperature (DBTT) than pure W. The tensile strength and total elongation of W-0.5wt% ZrC alloy at 700 °C is 535 MPa and 24.8%, which are respectively 59% and 114% higher than those of pure W (337 MPa, 11.6%). The DBTT of W-(0.2, 0.5, 1.0)wt% ZrC materials is in the range of 500°C-600°C, which is about 100 °C lower than that of pure W. Based on microstructure analysis, the improved mechanical properties of the W-ZrC alloys were suggested to originate from the enhanced grain boundary cohesion by ZrC capturing the impurity oxygen in tungsten and nano-size ZrC dispersion strengthening. supported by the Innovation Program of Chinese Academy of Sciences (No. KJCX2-YW-N35), the National Magnetic Confinement Fusion Science Program of China (No. 2011GB108004), National Natural Science Foundation of China (Nos. 51301164, 11075177, 11274305), and Anhui Provincial Natural Science Foundation of China (No. 1408085QE77)

Effects of hot compression deformation temperature on the microstructure and properties of Al-Zr-La alloys

NASA Astrophysics Data System (ADS)

Yue, Xian-hua; Liu, Chun-fang; Liu, Hui-hua; Xiao, Su-fen; Tang, Zheng-hua; Tang, Tian

2018-02-01

The main goal of this study is to investigate the microstructure and electrical properties of Al-Zr-La alloys under different hot compression deformation temperatures. In particular, a Gleeble 3500 thermal simulator was used to carry out multi-pass hot compression tests. For five-pass hot compression deformation, the last-pass deformation temperatures were 240, 260, 300, 340, 380, and 420°C, respectively, where the first-pass deformation temperature was 460°C. The experimental results indicated that increasing the hot compression deformation temperature with each pass resulted in improved electrical conductivity of the alloy. Consequently, the flow stress was reduced after deformation of the samples subjected to the same number of passes. In addition, the dislocation density gradually decreased and the grain size increased after hot compression deformation. Furthermore, the dynamic recrystallization behavior was effectively suppressed during the hot compression process because spherical Al3Zr precipitates pinned the dislocation movement effectively and prevented grain boundary sliding.

Spark Plasma Sintering of Commercial Zirconium Carbide Powders: Densification Behavior and Mechanical Properties

PubMed Central

Wei, Xialu; Back, Christina; Izhvanov, Oleg; Khasanov, Oleg L.; Haines, Christopher D.; Olevsky, Eugene A.

2015-01-01

Commercial zirconium carbide (ZrC) powder is consolidated by Spark Plasma Sintering (SPS). Processing temperatures range from 1650 to 2100 °C. Specimens with various density levels are obtained when performing single-die SPS at different temperatures. Besides the single-die tooling setup, a double-die tooling setup is employed to largely increase the actual applied pressure to achieve higher densification in a shorter processing time. In order to describe the densification mechanism of ZrC powder under SPS conditions, a power-law creep constitutive equation is utilized, whose coefficients are determined by the inverse regression of the obtained experimental data. The densification of the selected ZrC powder is shown to be likely associated with grain boundary sliding and dislocation glide controlled creep. Transverse rupture strength and microhardness of sintered specimens are measured to be up to 380 MPa and 24 GPa, respectively. Mechanical properties are correlated with specimens’ average grain size and relative density to elucidate the co-factor dependencies. PMID:28793550

Effects of long-term aging on ductility of the columbium alloys C-103, Cb-1Zr, and Cb-752 and the molybdenum alloy Mo-TZM

NASA Technical Reports Server (NTRS)

Stephens, J. R.

1975-01-01

A program was conducted to determine if aging embrittlement occurs in the columbium alloys C-103, CB-1Zr, and Cb-752 or in the molybdenum alloy Mo-TZM. Results showed that aging embrittlement does not occur in C-103, Cb-1Zr, or Mo-TZM during long-term (1000 hr) aging at temperatures in the range 700 to 1025 C. In contrast, aging embrittlement did occur in the Cb-752 alloy after similar aging at 900 C. A critical combination of the solute additions W and Zr in Cb-752 led to Zr segregation at grain boundaries during long-term aging. This segregation subsequently resulted in embrittlement as indicated by an increase in the ductile-brittle transition temperature from below -1960 C to about -150 C.

Effect of LPSO and SFs on microstructure evolution and mechanical properties of Mg-Gd-Y-Zn-Zr alloy

NASA Astrophysics Data System (ADS)

Xu, Chao; Nakata, Taiki; Qiao, Xiaoguang; Zheng, Mingyi; Wu, Kun; Kamado, Shigeharu

2017-01-01

High performance Mg-8.2Gd-3.8Y-1.0Zn-0.4Zr alloy with high strength and excellent ductility has been successfully developed by hot extrusion. The effect of plate-shaped long period stacking ordered (LPSO) phases and solute-segregated stacking faults (SFs) on the dynamically recrystallization (DRX) behavior was analyzed. The plate-shaped LPSO phases stimulate the DRX by particle stimulated nucleation mechanism, leading to higher DRX ratio and weaker basal texture. While for the alloy with dense fine SFs inside the original grains, discontinuous DRX initially occurs at the original grain boundaries, and the DRX is obviously restricted. Consequently, alloy containing dense SFs exhibits higher strength but lower ductility compared with alloy with plated-shaped LPSO phases.

Effect of LPSO and SFs on microstructure evolution and mechanical properties of Mg-Gd-Y-Zn-Zr alloy

PubMed Central

Xu, Chao; Nakata, Taiki; Qiao, Xiaoguang; Zheng, Mingyi; Wu, Kun; Kamado, Shigeharu

2017-01-01

High performance Mg-8.2Gd-3.8Y-1.0Zn-0.4Zr alloy with high strength and excellent ductility has been successfully developed by hot extrusion. The effect of plate-shaped long period stacking ordered (LPSO) phases and solute-segregated stacking faults (SFs) on the dynamically recrystallization (DRX) behavior was analyzed. The plate-shaped LPSO phases stimulate the DRX by particle stimulated nucleation mechanism, leading to higher DRX ratio and weaker basal texture. While for the alloy with dense fine SFs inside the original grains, discontinuous DRX initially occurs at the original grain boundaries, and the DRX is obviously restricted. Consequently, alloy containing dense SFs exhibits higher strength but lower ductility compared with alloy with plated-shaped LPSO phases. PMID:28134297

Self-ion irradiation effects on mechanical properties of nanocrystalline zirconium films

DOE PAGES

Wang, Baoming; Haque, M. A.; Tomar, Vikas; ...

2017-07-13

Zirconium thin films were irradiated at room temperature with an 800 keV Zr + beam using a 6 MV HVE Tandem accelerator to 1.36 displacement per atom damage. Freestanding tensile specimens, 100 nm thick and 10 nm grain size, were tested in-situ inside a transmission electron microscope. Significant grain growth (>300%), texture evolution, and displacement damage defects were observed. Here, stress-strain profiles were mostly linear elastic below 20 nm grain size, but above this limit the samples demonstrated yielding and strain hardening. Experimental results support the hypothesis that grain boundaries in nanocrystalline metals act as very effective defect sinks.

Structural, Optical and Impedance Spectroscopic Characterizations of Nanocrystalline A2Ti2Zr5O16 (A = Mg, Ca, Ba and Sr)

NASA Astrophysics Data System (ADS)

Sandeep, K.; Thomas, Jijimon K.; Solomon, Sam

2018-04-01

A nanocrystalline A2Ti2Zr5O16 (A = Mg, Ca, Ba and Sr) system has been synthesized by a modified combustion technique. The cation-deficient calzirtite (Ca2Ti2Zr5O16) is found to be a tetragonal structure with the space group I4(1)/acd. The average size of the particle from the transmission electron microscopy image is estimated to be 23.30 nm and 20.16 nm for Ca2Ti2Zr5O16 and Ba2Ti2Zr5O16, respectively. The optical bandgap calculated using a Tauc plot is between 3.01 eV and 3.46 eV. Raman and Fourier transform infrared spectroscopy (FTIR) studies were carried out to confirm the phase purity of the sample. The scanning electron microscopy (SEM) image of a Ca2Ti2Zr5O16 sample sintered at 1360°C for 3 h shows minimum porosity with 96% of the theoretical density. The frequency-dependent dielectric study shows that the dielectric constant is maximized at low frequencies and decreases as the frequency increases. The Cole-Cole plot reveals that the material exhibits conduction due to the contributions of grain, grain boundary and electrode effects. The photoluminescence spectra of the samples were recorded and the transitions causing emission have been identified.

An intermetallic powder-in-tube approach to increased flux-pinning in Nb 3Sn by internal oxidation of Zr

DOE PAGES

Motowidlo, Leszek R.; Lee, P. J.; Tarantini, C.; ...

2017-11-28

We report on the development of multifilamentary Nb 3Sn superconductors by a versatile powder-in-tube technique (PIT) that demonstrates a simple pathway to a strand with a higher density of flux-pinning sites that has the potential to increase critical current density beyond present levels. The approach uses internal oxidation of Zr-alloyed Nb tubes to produce Zr oxide particles within the Nb 3Sn layer that act as a dispersion of artificial pinning centres (APCs). In this design, SnO 2 powder is mixed with Cu 5Sn 4 powder within the PIT core that supplies the Sn for the A15 reaction with Nb1Zr filamentmore » tubes. Initial results show an average grain size of ~38 nm in the A15 layer, compared to the 90–130 nm of typical APC-free high-J c strands made by conventional PIT or Internal Sn processing. Furthermore, there is a shift in the peak of the pinning force curve from H/H irr of ~0.2 to ~0.3 and the pinning force curves can be deconvoluted into grain boundary and point-pinning components, the point-pinning contribution dominating for the APC Nb-1wt%Zr strands.« less

An intermetallic powder-in-tube approach to increased flux-pinning in Nb3Sn by internal oxidation of Zr

NASA Astrophysics Data System (ADS)

Motowidlo, L. R.; Lee, P. J.; Tarantini, C.; Balachandran, S.; Ghosh, A. K.; Larbalestier, D. C.

2018-01-01

We report on the development of multifilamentary Nb3Sn superconductors by a versatile powder-in-tube technique (PIT) that demonstrates a simple pathway to a strand with a higher density of flux-pinning sites that has the potential to increase critical current density beyond present levels. The approach uses internal oxidation of Zr-alloyed Nb tubes to produce Zr oxide particles within the Nb3Sn layer that act as a dispersion of artificial pinning centres (APCs). In this design, SnO2 powder is mixed with Cu5Sn4 powder within the PIT core that supplies the Sn for the A15 reaction with Nb1Zr filament tubes. Initial results show an average grain size of ˜38 nm in the A15 layer, compared to the 90-130 nm of typical APC-free high-J c strands made by conventional PIT or Internal Sn processing. There is a shift in the peak of the pinning force curve from H/H irr of ˜0.2 to ˜0.3 and the pinning force curves can be deconvoluted into grain boundary and point-pinning components, the point-pinning contribution dominating for the APC Nb-1wt%Zr strands.

An intermetallic powder-in-tube approach to increased flux-pinning in Nb 3Sn by internal oxidation of Zr

DOE Office of Scientific and Technical Information (OSTI.GOV)

Motowidlo, Leszek R.; Lee, P. J.; Tarantini, C.

We report on the development of multifilamentary Nb 3Sn superconductors by a versatile powder-in-tube technique (PIT) that demonstrates a simple pathway to a strand with a higher density of flux-pinning sites that has the potential to increase critical current density beyond present levels. The approach uses internal oxidation of Zr-alloyed Nb tubes to produce Zr oxide particles within the Nb 3Sn layer that act as a dispersion of artificial pinning centres (APCs). In this design, SnO 2 powder is mixed with Cu 5Sn 4 powder within the PIT core that supplies the Sn for the A15 reaction with Nb1Zr filamentmore » tubes. Initial results show an average grain size of ~38 nm in the A15 layer, compared to the 90–130 nm of typical APC-free high-J c strands made by conventional PIT or Internal Sn processing. Furthermore, there is a shift in the peak of the pinning force curve from H/H irr of ~0.2 to ~0.3 and the pinning force curves can be deconvoluted into grain boundary and point-pinning components, the point-pinning contribution dominating for the APC Nb-1wt%Zr strands.« less

Calcium-Magnesium-Aluminosilicate (CMAS) Reactions and Degradation Mechanisms of Advanced Environmental Barrier Coatings

NASA Technical Reports Server (NTRS)

Ahlborg, Nadia L.; Zhu, Dongming

2013-01-01

The thermochemical reactions between calcium-magnesium-aluminosilicate- (CMAS-) based road sand and several advanced turbine engine environmental barrier coating (EBC) materials were studied. The phase stability, reaction kinetics and degradation mechanisms of rare earth (RE)-silicates Yb2SiO5, Y2Si2O7, and RE-oxide doped HfO2 and ZrO2 under the CMAS infiltration condition at 1500 C were investigated, and the microstructure and phase characteristics of CMAS-EBC specimens were examined using Scanning Electron Microscopy (SEM) and X-ray Diffraction (XRD). Experimental results showed that the CMAS dissolved RE-silicates to form crystalline, highly non-stoichiometric apatite phases, and in particular attacking the silicate grain boundaries. Cross-section images show that the CMAS reacted with specimens and deeply penetrated into the EBC grain boundaries and formed extensive low-melting eutectic phases, causing grain boundary recession with increasing testing time in the silicate materials. The preliminary results also showed that CMAS reactions also formed low melting grain boundary phases in the higher concentration RE-oxide doped HfO2 systems. The effect of the test temperature on CMAS reactions of the EBC materials will also be discussed. The faster diffusion exhibited by apatite and RE-doped oxide phases and the formation of extensive grain boundary low-melting phases may limit the CMAS resistance of some of the environmental barrier coatings at high temperatures.

Multiscale Modeling of Ultra High Temperature Ceramics (UHTC) ZrB2 and HfB2: Application to Lattice Thermal Conductivity

NASA Technical Reports Server (NTRS)

Lawson, John W.; Daw, Murray S.; Squire, Thomas H.; Bauschlicher, Charles W.

2012-01-01

We are developing a multiscale framework in computational modeling for the ultra high temperature ceramics (UHTC) ZrB2 and HfB2. These materials are characterized by high melting point, good strength, and reasonable oxidation resistance. They are candidate materials for a number of applications in extreme environments including sharp leading edges of hypersonic aircraft. In particular, we used a combination of ab initio methods, atomistic simulations and continuum computations to obtain insights into fundamental properties of these materials. Ab initio methods were used to compute basic structural, mechanical and thermal properties. From these results, a database was constructed to fit a Tersoff style interatomic potential suitable for atomistic simulations. These potentials were used to evaluate the lattice thermal conductivity of single crystals and the thermal resistance of simple grain boundaries. Finite element method (FEM) computations using atomistic results as inputs were performed with meshes constructed on SEM images thereby modeling the realistic microstructure. These continuum computations showed the reduction in thermal conductivity due to the grain boundary network.

Highly-translucent, strong and aging-resistant 3Y-TZP ceramics for dental restoration by grain boundary segregation.

PubMed

Zhang, Fei; Vanmeensel, Kim; Batuk, Maria; Hadermann, Joke; Inokoshi, Masanao; Van Meerbeek, Bart; Naert, Ignace; Vleugels, Jef

2015-04-01

Latest trends in dental restorative ceramics involve the development of full-contour 3Y-TZP ceramics which can avoid chipping of veneering porcelains. Among the challenges are the low translucency and the hydrothermal stability of 3Y-TZP ceramics. In this work, different trivalent oxides (Al2O3, Sc2O3, Nd2O3 and La2O3) were selected to dope 3Y-TZP ceramics. Results show that dopant segregation was a key factor to design hydrothermally stable and high-translucent 3Y-TZP ceramics and the cation dopant radius could be used as a controlling parameter. A large trivalent dopant, oversized as compared to Zr(4+), exhibiting strong segregation at the ZrO2 grain boundary was preferred. The introduction of 0.2 mol% La2O3 in conventional 0.1-0.25 wt.% Al2O3-doped 3Y-TZP resulted in an excellent combination of high translucency and superior hydrothermal stability, while retaining excellent mechanical properties. Copyright © 2015 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Effects of grain size and humidity on fretting wear in fine-grained alumina, Al{sub 2}O{sub 3}/TiC, and zirconia

DOE Office of Scientific and Technical Information (OSTI.GOV)

Krell, A.; Klaffke, D.

Friction and wear of sintered alumina with grain sizes between 0.4 and 3 {micro}m were measured in comparison with Al{sub 2}O{sub 3}/TiC composites and with tetragonal ZrO{sub 2} (3 mol% Y{sub 2}O{sub 3}). The dependence on the grain boundary toughness and residual microstresses is investigated, and a hierarchical order of influencing parameters is observed. In air, reduced alumina grain sizes improve the micromechanical stability of the grain boundaries and the hardness, and reduced wear is governed by microplastic deformation, with few pullout events. Humidity and water slightly reduce the friction of all of the investigated ceramics. In water, this effectmore » reduces the wear of coarser alumina microstructures. The wear of aluminas and of the Al{sub 2}O{sub 3}/TiC composite is similar; it is lower than observed in zirconia, where extended surface cracking occurs at grain sizes as small as 0.3 {micro}m.« less

Electrical characterization of Mn doped-(Ba{sub 0.3}Sr{sub 0.7})Mn{sub x}(Ti{sub 0.9}Zr{sub 0.1}){sub 1-x}O{sub 3} ceramics

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mahmood, A.; Materials Research Laboratory, Institute of Physics & Electronics, University of Peshawar, 25120; Department of Engineering Materials, University of Sheffield, Sheffield S1 3JD

2015-12-15

Highlights: • Solid state processing of the (Ba{sub 0.3}Sr{sub 0.7})Mn{sub x}(Ti{sub 0.9}Zr{sub 0.1}){sub 1−x}O{sub 3} ceramics. • Mn incorporated on the Ti-site into the host lattice of (Ba{sub 0.3}Sr{sub 0.7})Mn{sub x}(Ti{sub 0.9}Zr{sub 0.1}){sub 1−x}O{sub 3}. • NTCR behavior was observed in the sintered samples. - Abstract: (Ba{sub 0.3}Sr{sub 0.7})Mn{sub x}(Ti{sub 0.9}Zr{sub 0.1}){sub 1-x}O{sub 3} (x = 0.00, 0.013, 0.015 and 0.05) ceramics were prepared by solid state sintering route at the 1500 °C for 6 h in air. Effect of Mn substitution on the structure of Ba{sub 0.3}Sr{sub 0.7}(Ti0{sub .9}Zr{sub 0.1}){sub 1−x}O{sub 3} perovskite was investigated systematically. Dielectric and impedancemore » spectroscopic studies were conducted to understand the electronic microstructure of the Ba{sub 0.3}Sr{sub 0.7}(Ti0{sub .9}Zr{sub 0.1}){sub 1−x}O{sub 3} ceramics. Sample with x = 0.05 showed the highest dielectric constant (ϵ{sub r} = 1826) and low dielectric loss (tanδ = 0.001) at 10 kHz, around the room temperature, while the sample with x = 0.00 showed good microwave (MW) dielectric properties (Qf{sub o} = 838 and ϵ{sub r} = 550). The impedance spectroscopic analysis confirmed the electrical homogeneity of the samples with x = 0.013, 0.015 and 0.05, where grain boundaries dominated the conduction mechanism. Similarly, the sample with x = 0.00 was found to possess both grain boundary and bulk resistive contributions.« less

Microstructural evolution and thermal stability of Fe-Zr metastable alloys developed by mechanical alloying followed by annealing

NASA Astrophysics Data System (ADS)

Sooraj, S.; Muthaiah, V. M. Suntharavel; Kang, P. C.; Koch, Carl C.; Mula, Suhrit

2016-09-01

The effect of Zr (up to 1 at.%) addition on the formation of Fe-Zr metastable alloys and their thermal stability were investigated for their possible nuclear applications. Fe-xZr (x = 0.25, 0.5, 1%) alloys were synthesised by mechanical alloying under a high-purity argon atmosphere using stainless steel grinding media in a SPEX 8000M high energy mill. The milling was conducted for 20 h with a ball-to-powder weight ratio of 10:1. The formation of metastable solid solutions after milling was confirmed from the change in the Gibbs free energy analysis as per Miedema's model. The microstructural characterisation was carried out by analysis of X-ray diffraction, atomic force microscopy and transmission electron microscopy. The effect of Zr on the thermal stability of Fe-Zr alloys was investigated by extensive annealing experiments followed by microstructural analysis and microhardness measurements. The stabilisation was found to occur at 800 °C and thereafter, no significant change in the crystallite size was observed for the samples annealed between 800 and 1200 °C. The supersaturated solid solution, especially 1% Zr alloy, found to be highly stable up to 800 °C and the microhardness value of the same measured to be as high as 8.8 GPa corresponding to a crystallite size of 57 nm. The stabilisation effect has been discussed in the light of both the thermodynamic and kinetic mechanisms and the grain size stabilisation is attributed to the grain boundary segregation of Zr atoms and/or Zener pinning by nanoscale precipitation of the Fe2Zr phase.

Tensile and compressive creep behavior of extruded Mg–10Gd–3Y–0.5Zr (wt.%) alloy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, H.; The State Key Laboratory of Metal Matrix Composites, Shanghai Jiao Tong University, 800 Dongchuan Road, Shanghai 200240; Wang, Q.D., E-mail: wangqudong@sjtu.edu.cn

2015-01-15

The tensile and compressive creep behavior of an extruded Mg–10Gd–3Y–0.5Zr (wt.%) alloy was investigated at temperatures ranging from 200 °C to 300 °C and under stresses ranging from 30 MPa to 120 MPa. There existed an asymmetry in the tensile and compressive creep properties. The minimum creep rate of the alloy was slightly greater in tension than in compression. The measured values of the transient strain and initial creep rate in compression were greater than those in tension. The creep stress exponent was approximately 2.5 at low temperatures (T < 250 °C) and 3.4 at higher temperatures both in tensionmore » and in compression. The compression creep activation energy at low temperatures and high temperatures was 83.4 and 184.3 kJ/mol respectively, while one activation energy (184 kJ/mol) represented the tensile–creep behavior over the temperature range examined. Dislocation creep was suggested to be the main mechanism in tensile creep and in the high-temperature regime in compressive creep, while grain boundary sliding was suggested to dominate in the low-temperature regime in compressive creep. Precipitate free zones were observed near grain boundaries perpendicular to the loading direction in tension and parallel to the loading direction in compression. Electron backscattered diffraction analysis revealed that the texture changed slightly during creep. Non-basal slip was suggested to contribute to the deformation after basal slip was introduced. In the tensile–creep ruptured specimens, intergranular cracks were mainly observed at general high-angle boundaries. - Highlights: • Creep behavior of an extruded Mg–RE alloy was characterized by EBSD. • T5 aging treatment enhanced the tension–compression creep asymmetry. • The grains grew slightly during tensile creep, but not for compressive creep. • Precipitate free zones (PFZs) were observed at specific grain boundaries. • Intergranular fracture was dominant and cracks mainly originated at GHABs.« less

Microstructure and magnetic behavior studies of processing-controlled and composition-modified Fe-Ni and Mn-Al alloys

NASA Astrophysics Data System (ADS)

Geng, Yunlong

L10-type (Space group P4/mmm) magnetic compounds, including FeNi and MnAl, possess promising technical magnetic properties of both high magnetization and large magnetocrystalline anisotropy energy, and thus offer potential in replacing rare earth permanent magnets in some applications. In equiatomic Fe-Ni, the disorder-order transformation from fcc structure to the L10 structure is a diffusional transformation, but is inhibited by the low ordering temperature. The transformation could be enhanced through the creation of vacancies. Thus, mechanical alloying was employed to generate more open-volume defects. A decrease in grain size and concomitant increase in grain boundary area resulted from the mechanical alloying, while an initial increase in internal strain (manifested through an increase in dislocation density) was followed by a subsequent decrease with further alloying. However, a decrease in the net defect concentration was determined by Doppler broadening positron annihilation spectroscopy, as open volume defects utilized dislocations and grain boundaries as sinks. An alloy, Fe32Ni52Zr3B13, formed an amorphous structure after rapid solidification, with a higher defect concentration than crystalline materials. Mechanical milling was utilized in an attempt to generate even more defects. However, it was observed that Fe32Ni52Zr3B13 underwent crystallization during the milling process, which appears to be related to enhanced vacancy-type defect concentrations allowing growth of pre-existing Fe(Ni) nuclei. The milling and enhanced vacancy concentration also de-stabilizes the glass, leading to decreased crystallization temperatures, and ultimately leading to complete crystallization. In Mn-Al, the L10 structure forms from the parent hcp phase. However, this phase is slightly hyperstoichiometric relative to Mn, and the excess Mn occupies Al sites and couples antiparallel to the other Mn atoms. In this study, the Zr substituted preferentially for the Mn atoms in the Al layer, resulting in an increase in saturation magnetization, from 115 emu/g in the alloys without Zr to 128 emu/g in Mn53Al43C 3Zr1. To further improve the coercivity in Mn53Al 43C3Zr1, microstructure modification was achieved through the addition of excessive C and through surfactant-assisted mechanical milling. Enhancement in coercivity was accomplished through the microstructure modification, however, the loss of saturation magnetization was observed due to the formation of other equilibrium phases, including epsilon, beta-Mn and ZrO.

The fatigue response of the aluminium-lithium alloy, 8090

NASA Technical Reports Server (NTRS)

Birt, M. J.; Beevers, C. J.

1989-01-01

The fatigue response of an Al-Li-Cu-Mg-Zr (8090) alloy has been studied at room temperature. The initiation and growth of small and long cracks has been examined at R = 0.1 and at a frequency of 100 Hz. Initiation was observed to occur dominantly at sub-grain boundaries. The growth of the small cracks was crystallographic in character and exhibited little evidence of retardation or arrest at the grain boundaries. The long crack data showed the alloy to have a high resistance to fatigue crack growth with underaging providing the optimum heat treatment for fatigue crack growth resistance. In general, this can be attributed to high levels of crack closure which resulted from the presence of extensive microstructurally related asperities.

Paving the way to nanoionics: atomic origin of barriers for ionic transport through interfaces.

PubMed

Frechero, M A; Rocci, M; Sánchez-Santolino, G; Kumar, Amit; Salafranca, J; Schmidt, Rainer; Díaz-Guillén, M R; Durá, O J; Rivera-Calzada, A; Mishra, R; Jesse, Stephen; Pantelides, S T; Kalinin, Sergei V; Varela, M; Pennycook, S J; Santamaria, J; Leon, C

2015-12-17

The blocking of ion transport at interfaces strongly limits the performance of electrochemical nanodevices for energy applications. The barrier is believed to arise from space-charge regions generated by mobile ions by analogy to semiconductor junctions. Here we show that something different is at play by studying ion transport in a bicrystal of yttria (9% mol) stabilized zirconia (YSZ), an emblematic oxide ion conductor. Aberration-corrected scanning transmission electron microscopy (STEM) provides structure and composition at atomic resolution, with the sensitivity to directly reveal the oxygen ion profile. We find that Y segregates to the grain boundary at Zr sites, together with a depletion of oxygen that is confined to a small length scale of around 0.5 nm. Contrary to the main thesis of the space-charge model, there exists no evidence of a long-range O vacancy depletion layer. Combining ion transport measurements across a single grain boundary by nanoscale electrochemical strain microscopy (ESM), broadband dielectric spectroscopy measurements, and density functional calculations, we show that grain-boundary-induced electronic states act as acceptors, resulting in a negatively charged core. Besides the possible effect of the modified chemical bonding, this negative charge gives rise to an additional barrier for ion transport at the grain boundary.

Paving the way to nanoionics: Atomic origin of barriers for ionic transport through interfaces

DOE PAGES

Frechero, M. A.; Rocci, M.; Sanchez-Santolino, G.; ...

2015-12-17

The blocking of ion transport at interfaces strongly limits the performance of electrochemical nanodevices for energy applications. The barrier is believed to arise from space-charge regions generated by mobile ions by analogy to semiconductor junctions. Here we show that something different is at play by studying ion transport in a bicrystal of yttria (9% mol) stabilized zirconia (YSZ), an emblematic oxide ion conductor. Aberration-corrected scanning transmission electron microscopy (STEM) provides structure and composition at atomic resolution, with the sensitivity to directly reveal the oxygen ion profile. We find that Y segregates to the grain boundary at Zr sites, together withmore » a depletion of oxygen that is confined to a small length scale of around 0.5 nm. Contrary to the main thesis of the space-charge model, there exists no evidence of a long-range O vacancy depletion layer. Combining ion transport measurements across a single grain boundary by nanoscale electrochemical strain microscopy (ESM), broadband dielectric spectroscopy measurements, and density functional calculations, we show that grain-boundary-induced electronic states act as acceptors, resulting in a negatively charged core. In conclusion, besides the possible effect of the modified chemical bonding, this negative charge gives rise to an additional barrier for ion transport at the grain boundary.« less

Selective Detection of Target Volatile Organic Compounds in Contaminated Humid Air Using a Sensor Array with Principal Component Analysis

PubMed Central

Itoh, Toshio; Akamatsu, Takafumi; Tsuruta, Akihiro; Shin, Woosuck

2017-01-01

We investigated selective detection of the target volatile organic compounds (VOCs) nonanal, n-decane, and acetoin for lung cancer-related VOCs, and acetone and methyl i-butyl ketone for diabetes-related VOCs, in humid air with simulated VOC contamination (total concentration: 300 μg/m3). We used six “grain boundary-response type” sensors, including four commercially available sensors (TGS 2600, 2610, 2610, and 2620) and two Pt, Pd, and Au-loaded SnO2 sensors (Pt, Pd, Au/SnO2), and two “bulk-response type” sensors, including Zr-doped CeO2 (CeZr10), i.e., eight sensors in total. We then analyzed their sensor signals using principal component analysis (PCA). Although the six “grain boundary-response type” sensors were found to be insufficient for selective detection of the target gases in humid air, the addition of two “bulk-response type” sensors improved the selectivity, even with simulated VOC contamination. To further improve the discrimination, we selected appropriate sensors from the eight sensors based on the PCA results. The selectivity to each target gas was maintained and was not affected by contamination. PMID:28753948

Relationships between microstructure and mechanical properties of Ti-5Al-5Mo-5V-3Cr-1Zr alloy

NASA Astrophysics Data System (ADS)

Li, Z. Y.; Wu, G. Q.; Huang, Z.

2018-03-01

Through a statistical, quantitative analysis on microstructure of Ti-5Al-5Mo-5V-3Cr-1Zr (Ti55531) alloy, the relationships between microstructure and mechanical properties and heat treatment temperatures were investigated. The results show that in Widmanstätten structure, the size of β grain is greatly increased with increasing annealing temperature. Static toughness is related to grain boundary alpha phase discontinuity, the tensile strength is related to acicular alpha phase interface length and acicular alpha phase proportion. In duplex microstructure, the tensile strength is related to the equiaxed alpha proportion. Elongation, static toughness and crack forming work are related to the equiaxed alpha proportion and negatively related to secondary phase proportion. The microstructure can be described quantitatively and the mechanical properties can be predicted by analysis of microstructure.

Nb-Base FS-85 Alloy as a Candidate Structural Material for Space Reactor Applications: Effects of Thermal Aging

NASA Astrophysics Data System (ADS)

Leonard, Keith J.; Busby, Jeremy T.; Hoelzer, David T.; Zinkle, Steven J.

2009-04-01

The proposed uses of fission reactors for manned or deep space missions have typically relied on the potential use of refractory metal alloys as structural materials. Throughout the history of these programs, a leading candidate has been Nb-1Zr, due to its good fabrication and welding characteristics. However, the less-than-optimal creep resistance of this alloy has encouraged interest in the more complex FS-85 (Nb-28Ta-10W-1Zr) alloy. Despite this interest, only a relatively small database exists for the properties of FS-85. Database gaps include the potential microstructural instabilities that can lead to mechanical property degradation. In this work, changes in the microstructure and mechanical properties of FS-85 were investigated following 1100 hours of thermal aging at 1098, 1248, and 1398 K. The changes in electrical resistivity, hardness, and tensile properties between the as-annealed and aged materials are compared. Evaluation of the microstructural changes was performed through optical microscopy (OM), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The development of intragranular and grain-boundary precipitation of Zr-rich compounds as a function of aging temperature was followed. Brittle tensile behavior was measured in the material aged at 1248 K, while ductile behavior occurred in samples aged above and below this temperature. The effect of temperature on the under- and overaging of the grain-boundary particles is believed to have contributed to the mechanical property behavior of the aged materials.

Grain Refinement and Mechanical Properties of Cu–Cr–Zr Alloys with Different Nano-Sized TiCp Addition

PubMed Central

Zhang, Dongdong; Bai, Fang; Wang, Yong; Wang, Jinguo; Wang, Wenquan

2017-01-01

The TiCp/Cu master alloy was prepared via thermal explosion reaction. Afterwards, the nano-sized TiCp/Cu master alloy was dispersed by electromagnetic stirring casting into the melting Cu–Cr–Zr alloys to fabricate the nano-sized TiCp-reinforced Cu–Cr–Zr composites. Results show that nano-sized TiCp can effectively refine the grain size of Cu–Cr–Zr alloys. The morphologies of grain in Cu–Cr–Zr composites changed from dendritic grain to equiaxed crystal because of the addition and dispersion of nano-sized TiCp. The grain size decreased from 82 to 28 μm with the nano-sized TiCp content. Compared with Cu–Cr–Zr alloys, the ultimate compressive strength (σUCS) and yield strength (σ0.2) of 4 wt% TiCp-reinforced Cu–Cr–Zr composites increased by 6.7% and 9.4%, respectively. The wear resistance of the nano-sized TiCp-reinforced Cu–Cr–Zr composites increased with the increasing nano-sized TiCp content. The wear loss of the nano-sized TiCp-reinforced Cu–Cr–Zr composites decreased with the increasing TiCp content under abrasive particles. The eletrical conductivity of Cu–Cr–Zr alloys, 2% and 4% nano-sized TiCp-reinforced Cu–Cr–Zr composites are 64.71% IACS, 56.77% IACS and 52.93% IACS, respectively. PMID:28786937

Grain boundary modification to suppress lithium penetration through garnet-type solid electrolyte

NASA Astrophysics Data System (ADS)

Hongahally Basappa, Rajendra; Ito, Tomoko; Morimura, Takao; Bekarevich, Raman; Mitsuishi, Kazutaka; Yamada, Hirotoshi

2017-09-01

Garnet-type solid electrolytes are one of key materials to enable practical usage of lithium metal anode for high-energy-density batteries. However, it suffers from lithium growth in pellets on charging, which causes short circuit. In this study, grain boundaries of Li6.5La3Zr1.5Ta0.5O12 (LLZT) pellets are modified with Li2CO3 and LiOH to investigate the influence of the microstructure of grain boundaries on lithium growth and to study the mechanism of the lithium growth. In spite of similar properties (relative density of ca. 96% and total ionic conductivity of 7 × 10-4 S cm-1 at 25 °C), the obtained pellets exhibit different tolerance on the short circuit. The LLZT pellets prepared from LiOH-modified LLZT powders exhibit rather high critical current density of 0.6 mA cm-2, at which short circuit occurs. On the other hand, the LLZT pellets without grain boundary modification short-circuited at 0.15 mA cm-2. Microstructural analyses by means of SEM, STEM and EIS suggest that lithium grows through interconnected open voids, and reveal that surface layers such as Li2CO3 and LiOH are not only plug voids but also facilitate the sintering of LLZT to suppress the lithium growth. The results indicate a strategy towards short-circuit-free lithium metal batteries.

Thermal Stabilization and Mechanical Properties of Nanocrystalline Iron-Nickel-Zirconium Alloys

NASA Astrophysics Data System (ADS)

Kotan, Hasan

Ultrafine grained and nanostructured materials are promising for structural applications because of the high strength compared to coarse grained counterparts. However, their widespread application is limited by an inherently high driving force for thermally induced grain growth, even at low temperatures. Accordingly, the understanding of and control over grain growth in nanoscale materials is of great technological and scientific importance as many physical properties (i.e. mechanical properties) are functions of the average grain size and the grain size distribution within the microstructure. Here, we investigate the microstructural evolution and grain growth in Fe-Ni alloys with Zr addition and differentiate the stabilization mechanisms acting on grain boundaries. Fe-Ni alloys are chosen for stability investigations since they are important for understanding the behavior of many steels and other ferrous alloys. Zirconium is proven to be an effective grain size stabilizer in pure Fe and Fe-base systems. In this study, nanocrystalline alloys were prepared by high energy ball milling. In situ and ex situ experiments were utilized to directly follow grain growth and microstructural evolution as a function of temperature and composition. The information obtained from these experiments enables the real time observation of microstructural evolution and phase transformation and provides a unique view of dynamic reactions as they occur. The knowledge of the thermal stability will exploit the potential high temperature applications and the consolidation conditions (i.e. temperature and pressure) to obtain high dense materials for advanced mechanical tests. Our investigations reveal that the grain growth of Fe-Ni alloys is not affected by Ni content but strongly inhibited by the addition of 1 at% Zr up to about 700 °C. The microstructural stability is lost due to the bcc-to-fcc transformation (occurring at 700°C) by the sudden appearance of abnormally grown fcc grains. However it was determined grain growth can be suppressed kinetically at higher temperatures for high Zr containing alloys by precipitation of intermetallic compounds. Eventually at high enough temperatures the retention of nanocrystallinity was lost, leaving behind fine micron grains filled with nanoscale intermetallic precipitates. Despite the loss of stability the in-situ formed precipitates were found to induce an Orowan hardening affect. The results from the mechanical tests show that Orowan particle strengthening can be as significant as Hall Petch hardening is at the smallest grain sizes.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Arul Kumar, M.; Beyerlein, Irene Jane; Tomé, Carlos N.

Here we study the effect of nearest neighboring grains on the propensity for {1012} twin growth in Mg and Zr. Twin lamellae lying within one grain flanked by two neighboring grains with several orientations are considered. The fields of resolved shear stress on the twin system are calculated in the multicrystal using a three-dimensional full-field crystal plasticity Fast Fourier Transform approach. The calculations were carried out for Mg and Zr using slip threshold stresses corresponding to 300K and 76K, respectively, where twin activity is important. We show that the neighboring grain constraint tends to oppose further growth and that themore » critical applied stress needed to overcome this resistance depends on neighboring grain orientation, more strongly in Zr than in Mg. We also present results for a pair of adjacent and parallel twins at various spacings. It is found that their paired interaction increases the resistive forces for twin growth above that for an isolated twin. The critical spacing above which this enhanced resistance is removed is smaller for Zr than Mg. Our analysis reveals that these two disparate responses of Zr and Mg are both a consequence of the fact that Zr is elastically and plastically more anisotropic than Mg. Additional calculations carried out on Ti support this conclusion. Finally, these findings can help explain why, for the same grain size, more twins per grain form in Zr than in Mg, twins in Zr tend to be thinner than those in Mg, and the relationship between the thickness of the twin and its Schmid factor in Zr is not as strong as in Mg.« less

Enhanced thermoelectric figure-of-merit in Bi-Sb-Te nanocomposites with homogenously dispersed oxide ceramic ZrO2 nanoparticles

NASA Astrophysics Data System (ADS)

Madavali, B.; Kim, H. S.; Lee, K. H.; Hong, S. J.

2017-06-01

In this research, p-type BiSbTe/ZrO2 nanocomposite powders were fabricated by high-energy ball milling. Different weight percentages of ZrO2 (2, 4, and 6 wt. %) nanoparticles were incorporated into the bulk (BiSbTe) matrix by consolidation of as-synthesized nanocomposites (NCs) powder by spark plasma sintering at 673 K. The phase and existence of ZrO2 nano-inclusions was confirmed by X-ray diffraction and transmission electron microscopy-selected area electron diffraction analysis. The Seebeck coefficient of the BiSbTe/ZrO2 NCs was significantly improved (˜36% for 4 wt. % added NCs) by a decrease in the carrier concentration and energy filtering effect, whereas the thermal conductivity was much reduced via strong scattering of carriers/phonons. The peak thermoelectric figure-of-merit (1.34 ± 0.06) was obtained for BiSbTe into which 2 wt. % ZrO2 was dispersed, which was approximately 20% greater than that of the undispersed sample. The hardness of the nanocomposites was significantly improved (˜27%) due to grain-boundary hardening and a dispersion strengthening mechanism.

Effect of surface microstructure on electrochemical performance of garnet solid electrolytes.

PubMed

Cheng, Lei; Chen, Wei; Kunz, Martin; Persson, Kristin; Tamura, Nobumichi; Chen, Guoying; Doeff, Marca

2015-01-28

Cubic garnet phases based on Al-substituted Li7La3Zr2O12 (LLZO) have high ionic conductivities and exhibit good stability versus metallic lithium, making them of particular interest for use in next-generation rechargeable battery systems. However, high interfacial impedances have precluded their successful utilization in such devices until the present. Careful engineering of the surface microstructure, especially the grain boundaries, is critical to achieving low interfacial resistances and enabling long-term stable cycling with lithium metal. This study presents the fabrication of LLZO heterostructured solid electrolytes, which allowed direct correlation of surface microstructure with the electrochemical characteristics of the interface. Grain orientations and grain boundary distributions of samples with differing microstructures were mapped using high-resolution synchrotron polychromatic X-ray Laue microdiffraction. The electrochemical characteristics are strongly dependent upon surface microstructure, with small grained samples exhibiting much lower interfacial resistances and better cycling behavior than those with larger grain sizes. Low area specific resistances of 37 Ω cm(2) were achieved; low enough to ensure stable cycling with minimal polarization losses, thus removing a significant obstacle toward practical implementation of solid electrolytes in high energy density batteries.

Grain Refinement and Mechanical Properties of Cu-Cr-Zr Alloys with Different Nano-Sized TiCp Addition.

PubMed

Zhang, Dongdong; Bai, Fang; Wang, Yong; Wang, Jinguo; Wang, Wenquan

2017-08-08

The TiC p /Cu master alloy was prepared via thermal explosion reaction. Afterwards, the nano-sized TiC p /Cu master alloy was dispersed by electromagnetic stirring casting into the melting Cu-Cr-Zr alloys to fabricate the nano-sized TiC p -reinforced Cu-Cr-Zr composites. Results show that nano-sized TiC p can effectively refine the grain size of Cu-Cr-Zr alloys. The morphologies of grain in Cu-Cr-Zr composites changed from dendritic grain to equiaxed crystal because of the addition and dispersion of nano-sized TiC p . The grain size decreased from 82 to 28 μm with the nano-sized TiC p content. Compared with Cu-Cr-Zr alloys, the ultimate compressive strength (σ UCS ) and yield strength (σ 0.2 ) of 4 wt% TiC p -reinforced Cu-Cr-Zr composites increased by 6.7% and 9.4%, respectively. The wear resistance of the nano-sized TiCp-reinforced Cu-Cr-Zr composites increased with the increasing nano-sized TiCp content. The wear loss of the nano-sized TiC p -reinforced Cu-Cr-Zr composites decreased with the increasing TiC p content under abrasive particles. The eletrical conductivity of Cu-Cr-Zr alloys, 2% and 4% nano-sized TiCp-reinforced Cu-Cr-Zr composites are 64.71% IACS, 56.77% IACS and 52.93% IACS, respectively.

Effect of the Microstructure and Distribution of the Second Phase on the Stress Corrosion Cracking of Biomedical Mg-Zn-Zr-xSr Alloys

PubMed Central

Chen, Lianxi; Sheng, Yinying; Zhao, Xueyang; Liu, Hui; Li, Wei

2018-01-01

The stress corrosion cracking (SCC) properties of the bi-directional forged (BDF) Mg-4Zn-0.6Zr-xSr (ZK40-xSr, x = 0, 0.4, 0.8, 1.2, 1.6 wt %) alloys were studied by the slow strain rate tensile (SSRT) testing in modified simulated body fluid (m-SBF). The average grain size of the BDF alloys were approximately two orders of magnitude smaller than those of the as-cast alloys. However, grain refinement increased the hydrogen embrittlement effect, leading to a higher SCC susceptibility in the BDF ZK40-0/0.4Sr alloys. Apart from the grain refinements effect, the forging process also changed the distribution of second phase from the net-like shape along the grain boundary to a uniformly isolated island shape in the BDF alloys. The SCC susceptibility of the BDF ZK40-1.2/1.6Sr alloys were lower than those of the as-cast alloys. The change of distribution of the second phase suppressed the adverse effect of Sr on the SCC susceptibility in high Sr–containing magnesium alloys. The results indicated the stress corrosion behavior of magnesium alloys was related to the average grain size of matrix and the distribution and shape of the second phase. PMID:29614043

[delta] precipitation in an Al-Li-Cu-Mg-Zr alloy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Prasad, K.S.; Mukhopadhyay, A.K.; Gokhale, A.A.

1994-05-15

AlLi based [delta] phase has an NaTl structure (i.e., a diamond cubic) with a = 0.637nm and is an equilibrium phase in the binary Al-Li system. In heat treated binary Al-Li alloys of appropriate compositions, [delta] phase can format grain boundaries as well as within the grains. In commercially heat treated Al-Li-Cu alloys of 2090 specification, the grain boundary precipitate [delta] of the binary Al-Li system is replaced by a combination of T[sub 2](Al[sub 6]CuLi[sub 3]), R(Al[sub 5]CuLi[sub 3]) and T[sub 1](Al[sub 2]CuLi) phases. In similarly treated Al-Li-Cu-Mg alloys of 8090 specification, the copper rich T[sub 2] phase, present inmore » the form of Al[sub 6]CuLi[sub 3[minus]x]Mg[sub x], is known to be the major coarse g.b. precipitate. The presence of an Al-Li-Cu-Mg based C phase at the grain boundaries of the commercially heat treated 8090 alloys has also been documented. No detailed study has yet been carried out to verify whether the [delta] phase can be present at the grain boundaries of the commercially heat treated 8090 alloys. Given the correlations between the g.b. phase morphology, g.b. phase chemistry, and the stress corrosion cracking resistance of these alloys, it is important that the g.b. precipitates be examined and identified. In this paper results using TEM are presented to show that the [delta] phase can be present in varying amounts at the grain boundaries in an 8090 alloy when heat treated in the temperature range of 170--350 C. An examination is also made of the [delta] precipitation within the grain to establish that the T[sub 2]/[alpha]-Al interface is the dominant nucleation site for the noncoherent [delta] phase.« less

Mechanical Properties and Microstructure of TIG and FSW Joints of a New Al-Mg-Mn-Sc-Zr Alloy

NASA Astrophysics Data System (ADS)

Xu, Guofu; Qian, Jian; Xiao, Dan; Deng, Ying; Lu, Liying; Yin, Zhimin

2016-04-01

A new Al-5.8%Mg-0.4%Mn-0.25%Sc-0.10%Zr (wt.%) alloy was successfully welded by tungsten inert gas (TIG) and friction stir welding (FSW) techniques, respectively. The mechanical properties and microstructure of the welded joints were investigated by microhardness measurements, tensile tests, and microscopy methods. The results show that the ultimate tensile strength, yield strength, and elongation to failure are 358, 234 MPa, and 27.6% for TIG welded joint, and 376, 245 MPa and 31.9% for FSW joint, respectively, showing high strength and superior ductility. The TIG welded joint fails in the heat-affected zone and the fracture of FSW joint is located in stirred zone. Al-Mg-Mn-Sc-Zr alloy is characterized by lots of dislocation tangles and secondary coherent Al3(Sc,Zr) particles. The superior mechanical properties of the TIG and FSW joints are mainly derived from the Orowan strengthening and grain boundary strengthening caused by secondary coherent Al3(Sc,Zr) nano-particles (20-40 nm). For new Al-Mg-Mn-Sc-Zr alloy, the positive effect from secondary Al3(Sc, Zr) particles in the base metal can be better preserved in FSW joint than in TIG welded joint.

Effect of local stress fields on twin characteristics in HCP metals

DOE PAGES

Arul Kumar, M.; Beyerlein, Irene Jane; Tomé, Carlos N.

2016-09-01

Here we study the effect of nearest neighboring grains on the propensity for {1012} twin growth in Mg and Zr. Twin lamellae lying within one grain flanked by two neighboring grains with several orientations are considered. The fields of resolved shear stress on the twin system are calculated in the multicrystal using a three-dimensional full-field crystal plasticity Fast Fourier Transform approach. The calculations were carried out for Mg and Zr using slip threshold stresses corresponding to 300K and 76K, respectively, where twin activity is important. We show that the neighboring grain constraint tends to oppose further growth and that themore » critical applied stress needed to overcome this resistance depends on neighboring grain orientation, more strongly in Zr than in Mg. We also present results for a pair of adjacent and parallel twins at various spacings. It is found that their paired interaction increases the resistive forces for twin growth above that for an isolated twin. The critical spacing above which this enhanced resistance is removed is smaller for Zr than Mg. Our analysis reveals that these two disparate responses of Zr and Mg are both a consequence of the fact that Zr is elastically and plastically more anisotropic than Mg. Additional calculations carried out on Ti support this conclusion. Finally, these findings can help explain why, for the same grain size, more twins per grain form in Zr than in Mg, twins in Zr tend to be thinner than those in Mg, and the relationship between the thickness of the twin and its Schmid factor in Zr is not as strong as in Mg.« less

The Impact of Updated Zr Neutron-capture Cross Sections and New Asymptotic Giant Branch Models on our Understanding of the s process and the origin of stardust

DOE PAGES

Lugaro, M.; Tagliente, Giuseppe; Karakas, Amanda I.; ...

2013-12-13

We present model predictions for the Zr isotopic ratios produced by slow neutron captures in C-rich asymptotic giant branch (AGB) stars of masses 1.25-4 M-circle dot and metallicities Z = 0.01-0.03, and compare them to data from single meteoritic stardust silicon carbide (SiC) and high-density graphite grains that condensed in the outflows of these stars. We compare predictions produced using the Zr neutron-capture cross sections from Bao et al. and from n_TOF experiments at CERN, and present a new evaluation for the neutron-capture cross section of the unstable isotope Zr-95, the branching point leading to the production of Zr-96. Themore » new cross sections generally present an improved match with the observational data, except for the Zr-92/Zr-94 ratios, which are on average still substantially higher than predicted. The Zr-96/Zr-94 ratios can be explained using our range of initial stellar masses, with the most Zr-96-depleted grains originating from AGB stars of masses 1.8-3 M-circle dot and the others from either lower or higher masses. The Zr-90,Zr-91/Zr-94 variations measured in the grains are well reproduced by the range of stellar metallicities considered here, which is the same needed to cover the Si composition of the grains produced by the chemical evolution of the Galaxy. The Zr-92/Zr-94 versus Si-29/Si-28 positive correlation observed in the available data suggests that stellar metallicity rather than rotation plays the major role in covering the Zr-90,Zr-91,Zr-92/Zr-94 spread« less

Fatigue crack propagation of nickel-base superalloys at 650 deg C

NASA Technical Reports Server (NTRS)

Gayda, J.; Gabb, T. P.; Miner, R. V.

1988-01-01

The 650 C fatigue crack propagation behavior of two nickel-base superalloys, Rene 95 and Waspaloy, is studied with particular emphasis placed on understanding the roles of creep, environment, and two key grain boundary alloying additions, boron and zirconium. Comparison of air and vacuum data shows the air environment to be detrimental over a wide range of frequencies for both alloys. More in-depth analysis on Rene 95 shows at lower frequencies, such as 0.02 Hz, failure in air occurs by intergranular, environmentally-assisted creep crack growth, while at higher frequencies, up to 5.0 Hz, environmental interaction are still evident but creep effects are minimized. The effect of B and Zr in Waspaloy is found to be important where environmental and/or creep interactions are presented. In those instances, removal of B and Zr dramatically increases crack growth and it is therefore plausible that effective dilution of these elements may explain a previously observed trend in which crack growth rates increase with decreasing grain size.

Fatigue crack propagation of nickel-base superalloys at 650 deg C

NASA Technical Reports Server (NTRS)

Gayda, J.; Gabb, T. P.; Miner, R. V.

1985-01-01

The 650 C fatigue crack propagation behavior of two nickel-base superalloys, Rene 95 and Waspaloy, is studied with particular emphasis placed on understanding the roles of creep, environment, and two key grain boundary alloying additions, boron and zirconium. Comparison of air and vacuum data shows the air environment to be detrimental over a wide range of frequencies for both alloys. More in-depth analysis on Rene 95 shows at lower frequencies, such as 0.02 Hz, failure in air occurs by intergranular, environmentally-assisted creep crack growth, while at higher frequencies, up to 5.0 Hz, environmental interactions are still evident but creep effects are minimized. The effect of B and Zr in Waspaloy is found to be important where environmental and/or creep interactions are presented. In those instances, removal of B and Zr dramatically increases crack growth and it is therefore plausible that effective dilution of these elements may explain a previously observed trend in which crack growth rates increase with decreasing grain size.

Deformation mechanism study of a hot rolled Zr-2.5Nb alloy by transmission electron microscopy. I. Dislocation microstructures in as-received state and at different plastic strains

DOE Office of Scientific and Technical Information (OSTI.GOV)

Long, Fei; Daymond, Mark R., E-mail: mark.daymond@queensu.ca; Yao, Zhongwen

Thin foil dog bone samples prepared from a hot rolled Zr-2.5Nb alloy have been deformed by tensile deformation to different plastic strains. The development of slip traces during loading was observed in situ through SEM, revealing that deformation starts preferentially in certain sets of grains during the elastic-plastic transition region. TEM characterization showed that sub-grain boundaries formed during hot rolling consisted of screw 〈a〉 dislocations or screw 〈c〉 and 〈a〉 dislocations. Prismatic 〈a〉 dislocations with large screw or edge components have been identified from the sample with 0.5% plastic strain. Basal 〈a〉 and pyramidal 〈c + a〉 dislocations were found in themore » sample that had been deformed with 1.5% plastic strain, implying that these dislocations require larger stresses to be activated.« less

Investigation of ZrO/sub 2//mullite solid solution by energy dispersive X-ray spectroscopy and electron diffraction

DOE Office of Scientific and Technical Information (OSTI.GOV)

Dinger, T.R.; Krishnam, K.M.; Moya, J.S.

1984-10-01

A mullite/15 vol.%ZrO/sub 2/ composite was analyzed using the techniques of microdiffraction and energy dispersive X-ray spectroscopy (EDXS). The EDXS results indicate that there is a significantly high solid solubility of mullite in zirconia and zirconia in mullite; microdiffraction results suggest that ordering occurs in the ZrO/sub 2/(ss) phase based on the presence of forbidden reflections for the P 2/sub 1//c space group of monoclinic zirconia. The presence of a secondary phase at the grain boundaries, either amorphous or crystalline, has not been generally detected throughout the bulk. The results provide experimental evidence for the hypothesis of Moya and Osendimore » that the increased toughness and flexural strength of these composites are related to solid solution effects rather than to transformation or microcrack toughening mechanisms.« less

Oxygen Permeability and Grain-Boundary Diffusion Applied to Alumina Scales

NASA Technical Reports Server (NTRS)

Smialek, James L.; Jacobson, Nathan S.; Gleeson, Brian; Hovis, David B.; Heuer, Arthur H.

2013-01-01

High-temperature oxygen permeability measurements had determined grain-boundary diffusivities (deltaD(sub gb)) in bulk polycrystalline alumina (Wada, Matsudaira, and Kitaoka). They predict that oxygen deltaD(sub gb,O) varies with oxygen pressure as P(O2)(sup -1/6) at low pressure whereas aluminum deltaD(sub gb),Al varies with P(O2)(sup +3/16) at high pressure. These relations were used to evaluate alumina scale growth in terms of diffusivity and grain size. A modified Wagner treatment for dominant inward oxygen growth produces the concise solution: ?(sub i) = k(sub p,i)×G(sub i) = 12 deltaD(sub gb,O,int), where ?(sub i) is a constant and k(sub p,i) and G(sub i) refer to instantaneous values of the scale parabolic growth constant and grain size, respectively. A commercial FeCrAl(Zr) alloy was oxidized at 1100 to 1400 degC to determine k(sub p,i), interfacial grain size, ?, and thus deltaD(sub gb,O,int). The deltaD(sub gb,O,int) values predicted from oxidation at (375 kJ/mole) were about 20 times less than those obtained above (at 298 kJ/mole), but closer than extrapolations from high-temperature bulk measurements. The experimental oxidation results agree with similar FeCrAl(X) studies, especially where both k(sub p,i) and G(sub i) were characterized. This complete approach accounts for temperature-sensitive oxidation effects of grain enlargement, equilibrium interface pressure variation, and grain-boundary diffusivity.

Structural, Dielectric, and Electrical Properties of Bi1- x Pb x Fe1- x (Zr0.5Ti0.5) x O3

NASA Astrophysics Data System (ADS)

Panda, Niranjan; Pattanayak, Samita; Choudhary, R. N. P.

2015-12-01

Polycrystalline samples of Bi1- x Pb x Fe1- x (Zr0.5Ti0.5) x O3 (BPFZTO) with x = 0.0, 0.2, 0.3, and 0.4 were prepared by high-temperature solid-state reaction. Preliminary structural analysis of calcined powders of the materials by use of x-ray powder diffraction confirmed formation of single-phase systems with the tetragonal structure. Room-temperature scanning electron micrographs of the samples revealed uniform distribution of grains of low porosity and different dimensions on the surface of the samples. The frequency-temperature dependence of dielectric and electric properties was studied by use of dielectric and complex impedance spectroscopy over a wide range of frequency (1 kHz to 1 MHz) at different temperatures (25-500°C). The dielectric constant of BiFeO3 (BFO) was enhanced by substitution with Pb(Zr0.5Ti0.5)O3 (PZT) whereas the dielectric loss of the BPFZTO compounds decreased with increasing PZT content. A significant contribution of both grains and grain boundaries to the electrical response of the materials was observed. The frequency-dependence of the ac conductivity of BPFZTO followed Jonscher's power law. Negative temperature coefficient of resistance behavior was observed for all the BPFZTO samples. Conductivity by thermally excited charge carriers and oxygen vacancies in the materials was believed to be of the Arrhenius-type.

Formation and corrosion of a 410 SS/ceramic composite

NASA Astrophysics Data System (ADS)

Chen, X.; Ebert, W. L.; Indacochea, J. E.

2016-11-01

This study addressed the possible use of alloy/ceramic composite waste forms to immobilize metallic and oxide waste streams generated during the electrochemical reprocessing of spent reactor fuel using a single waste form. A representative composite material was made to evaluate the microstructure and corrosion behavior at alloy/ceramic interfaces by reacting 410 stainless steel with Zr, Mo, and a mixture of lanthanide oxides. Essentially all of the available Zr reacted with lanthanide oxides to generate lanthanide zirconates, which combined with the unreacted lanthanide oxides to form a porous ceramic network that filled with alloy to produce a composite puck. Alloy present in excess of the pore volume of the ceramic generated a metal bead on top of the puck. The alloys in the composite and forming the bead were both mixtures of martensite grains and ferrite grains bearing carbide precipitates; FeCrMo intermetallic phases also precipitated at ferrite grain boundaries within the composite puck. Micrometer-thick regions of ferrite surrounding the carbides were sensitized and corroded preferentially in electrochemical tests. The lanthanide oxides dissolved chemically, but the lanthanide zirconates did not dissolve and are suitable host phases. The presence of oxide phases did not affect corrosion of the neighboring alloy phases.

Thermal stability of the microstructure of an aged Nb-Zr-C alloy

NASA Technical Reports Server (NTRS)

Uz, Mehmet; Titran, Robert H.

1990-01-01

The effects of thermal aging with and without an applied stress on the microstructure of a Nb-Zr-C alloy containing 0.9 wt percent Zr and 0.06 wt percent C were studied. Chemical analysis, metallographic examination, energy dispersive x-ray spectra of the bulk material, and chemical and x-ray analyses of the phase-extracted residue were used to characterize the microstructure. The samples examined were from a creep strength study involving hot and cold working, and various combinations of exposure to temperatures ranging from 1350 to 1755 K with and without applied load for times as long as 34,000 plus hours. The results showed that the initial microstructure consisted primarily of orthorombic precipitates of Nb sub 2 C which were partially or completely transformed to face-centered cubic carbides of nb and Zr, (Zr, Nb)C, upon prolonged exposure to elevated temperatures. Furthermore, it was found that the microstructure of the alloy is extremely stable owing to the very finely distributed precipitates throughout its matrix and along the grain boundaries. The lattice parameters of the cubic carbides were determed to vary from 0.458 to 0.465 nm as the Zr/Nb ratio varied from 38/62 to 75/25.

Ferroelectric relaxor behaviour and impedance spectroscopy of Bi2O3-doped barium zirconium titanate ceramics

NASA Astrophysics Data System (ADS)

Mahajan, Sandeep; Thakur, O P; Bhattacharya, D K; Sreenivas, K

2009-03-01

Bi2O3-doped barium zirconate titanate ceramics, Ba1-xBix(Zr0.05Ti0.95)O3, have been prepared by the conventional solid-state reaction method. The ferroelectric relaxor behaviour and dielectric properties have been investigated in detail. By XRD analysis, it is suggested that up to x = 0.04, Bi3+ substitutes A-site ion, and thereafter with higher Bi3+ content, it enters the B-site sub lattice. Substitution of Bi3+ ions induces ferroelectric relaxor behaviour and the degree of relaxation behaviour increases with bismuth concentration. The remanent polarization and strain behaviour show a slight increase with the substitution level. The degree of hysteresis (strain versus electric field) also reduces from 21.4% to 4.6% with bismuth substitution. Impedance measurements were made on the prepared sample over a wide range of temperatures (300-723 K) and frequencies (40 Hz-1 MHz), which show the presence of both bulk and grain boundary effects in the material. The bulk and grain boundary conductivities determined from impedance study indicate the Arrhenius-type thermally activated process. Impedance spectroscopy is shown to be an efficient method capable of detecting the contributions of the resistances of grains and grain boundaries to the complex impedance of a ceramic system, accurately estimating its electrical conductivity as well as its corresponding activation energies and drawing conclusions on its structural properties.

Effect of Nd Doping on Dielectric and Impedance Properties of PZT Nanoceramics

NASA Astrophysics Data System (ADS)

Kour, P.; Pradhan, S. K.; Kumar, Pawan; Sinha, S. K.; Kar, Manoranjan

2018-02-01

Neodymium-doped lead zirconate tianate, i.e. Pb1-x Nd x Zr0.52Ti0.48O3 (PNZT) ceramics, with x = 0-10 mol.% has been prepared by the sol-gel process. X-ray diffraction pattern at room temperature shows the pyrochlore free phase for all samples. The structural analysis suggests the coexistence of both rhombohedral (R3m space group) and tetragonal (P4 mm space group) crystal symmetries. Scanning electron micrographs of the samples show uniform distribution of grain and grain boundaries. Dielectric constant increases with the increase in neodymium concentration in the crystal lattice. Degree of diffuse phase transition increases with the increase in Nd3+ concentration in the sample. Nd3+ incorporation into the lead zirconatetitanate (PZT) lattice enhances the spreading factor. Interaction between neighbouring dipoles decreases with the increase of Nd3+ in PZT lattice. The conduction mechanism of the sample can be attributed to the overlapping large polar tunnelling. Second-order dielectric phase transition has been observed at the Curie temperature. The electrical properties of the sample can be explained by considering grain and grain boundaries contributions. All the samples show the poly-dispersive non-Debye type relaxation.

Effect of surfactant and mineralizer on the dielectric properties of zirconia nanocrsytals

NASA Astrophysics Data System (ADS)

Maheswari, A. Uma; Mohan, Sreedevi R.; Sivakumar, M.

2018-01-01

The combined effect of surfactants (PVP/CTAB) and alkaline mineralizers (NaOH/NH4OH) on dielectric properties of zirconia nanocrystals is analyzed. It is found that, the stabilization of zirconia tetramers by surfactants and the rate of hydroxyl ions released by alkaline mineralizers have significant impact on the dielectric properties of nanocrystals. The PVP capped tetramers form highly conducting grains with insulating boundaries, whereas the grains of CTAB capped tetramers are highly insulating with conducting grain boundaries, as revealed by Nyquist plots. Consequently, the space charge polarization would be quite large in highly conducting grains resulting in higher dielectric constant values at lower frequencies. The higher dielectric constant of PVP capped nanocrystals is due to greater tetragonal coordination of 3d5/2 and 3d3/2 electrons of Zr4+ ions than that of CTAB capped nanocrystals. Further, the surface oxygen vacancies of PVP samples are higher, resulting in a high space charge polarization. The ESR signal corresponding to F+ centers appears stronger for PVP/NH4OH nanocrystals. Moreover, the larger ESR line width of PVP/NH4OH nanocrystals corresponding to more oxygen vacancies is in accordance with the inference attained from the XPS analysis.

ZrB2-CNTs Nanocomposites Fabricated by Spark Plasma Sintering

PubMed Central

Jin, Hua; Meng, Songhe; Xie, Weihua; Xu, Chenghai; Niu, Jiahong

2016-01-01

ZrB2-based nanocomposites with and without carbon nanotubes (CNTs) as reinforcement were prepared at 1600 °C by spark plasma sintering. The effects of CNTs on the microstructure and mechanical properties of nano-ZrB2 matrix composites were studied. The results indicated that adding CNTs can inhibit the abnormal grain growth of ZrB2 grains and improve the fracture toughness of the composites. The toughness mechanisms were crack deflection, crack bridging, debonding, and pull-out of CNTs. The experimental results of the nanograined ZrB2-CNTs composites were compared with those of the micro-grained ZrB2-CNTs composites. Due to the small size and surface effects, the nanograined ZrB2-CNTs composites exhibited stronger mechanical properties: the hardness, flexural strength and fracture toughness were 18.7 ± 0.2 GPa, 1016 ± 75 MPa, and 8.5 ± 0.4 MPa·m1/2, respectively. PMID:28774087

ZrB₂-CNTs Nanocomposites Fabricated by Spark Plasma Sintering.

PubMed

Jin, Hua; Meng, Songhe; Xie, Weihua; Xu, Chenghai; Niu, Jiahong

2016-11-29

ZrB₂-based nanocomposites with and without carbon nanotubes (CNTs) as reinforcement were prepared at 1600 °C by spark plasma sintering. The effects of CNTs on the microstructure and mechanical properties of nano-ZrB₂ matrix composites were studied. The results indicated that adding CNTs can inhibit the abnormal grain growth of ZrB₂ grains and improve the fracture toughness of the composites. The toughness mechanisms were crack deflection, crack bridging, debonding, and pull-out of CNTs. The experimental results of the nanograined ZrB₂-CNTs composites were compared with those of the micro-grained ZrB₂-CNTs composites. Due to the small size and surface effects, the nanograined ZrB₂-CNTs composites exhibited stronger mechanical properties: the hardness, flexural strength and fracture toughness were 18.7 ± 0.2 GPa, 1016 ± 75 MPa, and 8.5 ± 0.4 MPa·m 1/2 , respectively.

Effects of cobalt, boron, and zirconium on the microstructure of Udimet 738. M.S. Thesis. Final Report

NASA Technical Reports Server (NTRS)

Nakanishi, T. G.

1984-01-01

A structural study was carried out on Co modified Udimet 738 alloys containing 0.04, 0.10, and 0.20 wt % Zr at 0.01 and 0.03 wt % B levels. Samples in the as-cast and solution-treated conditions were exposed at 843 C to study structural stability. The structures produced by the interactions of Co, Zr, and B were studied by SEM, X-ray diffraction, and dispersive analysis techniques. The additions of large amounts of Zr and B were found to increase the solidification range of the U-738. Structural changes involved eutectic gamma prime islands, formation of low melting point compounds, and precipitation of borides and Zr rich phases. Boron and zirconium additions did not show substantial changes in mechanical properties. Removal of Co from the alloys resulted in reduction of the matrix solubility for carbon and increase in the gamma prime solvus. Structural instabilities found were continuous grain boundary M23C6 films, MC breakdown, and plate-like phases. Removal of cobalt resulted in a slight decrease in tensile and stress rupture properties. Detailed structural results presented.

Carbide/nitride grain refined rare earth-iron-boron permanent magnet and method of making

DOEpatents

McCallum, R.W.; Branagan, D.J.

1996-01-23

A method of making a permanent magnet is disclosed wherein (1) a melt is formed having a base alloy composition comprising RE, Fe and/or Co, and B (where RE is one or more rare earth elements) and (2) TR (where TR is a transition metal selected from at least one of Ti, Zr, Hf, V, Nb, Ta, Cr, Mo, W, and Al) and at least one of C and N are provided in the base alloy composition melt in substantially stoichiometric amounts to form a thermodynamically stable compound (e.g. TR carbide, nitride or carbonitride). The melt is rapidly solidified in a manner to form particulates having a substantially amorphous (metallic glass) structure and a dispersion of primary TRC, TRN and/or TRC/N precipitates. The amorphous particulates are heated above the crystallization temperature of the base alloy composition to nucleate and grow a hard magnetic phase to an optimum grain size and to form secondary TRC, TRN and/or TRC/N precipitates dispersed at grain boundaries. The crystallized particulates are consolidated at an elevated temperature to form a shape. During elevated temperature consolidation, the primary and secondary precipitates act to pin the grain boundaries and minimize deleterious grain growth that is harmful to magnetic properties. 33 figs.

Integrating Epitaxial-Like Pb(Zr,Ti)O3 Thin-Film into Silicon for Next-Generation Ferroelectric Field-Effect Transistor

PubMed Central

Park, Jae Hyo; Kim, Hyung Yoon; Jang, Gil Su; Seok, Ki Hwan; Chae, Hee Jae; Lee, Sol Kyu; Kiaee, Zohreh; Joo, Seung Ki

2016-01-01

The development of ferroelectric random-access memory (FeRAM) technology with control of grain boundaries would result in a breakthrough for new nonvolatile memory devices. The excellent piezoelectric and electrical properties of bulk ferroelectrics are degraded when the ferroelectric is processed into thin films because the grain boundaries then form randomly. Controlling the nature of nucleation and growth are the keys to achieving a good crystalline thin-film. However, the sought after high-quality ferroelectric thin-film has so far been thought to be impossible to make, and research has been restricted to atomic-layer deposition which is extremely expensive and has poor reproducibility. Here we demonstrate a novel epitaxial-like growth technique to achieve extremely uniform and large rectangular-shaped grains in thin-film ferroelectrics by dividing the nucleation and growth phases. With this technique, it is possible to achieve 100-μm large uniform grains, even made available on Si, which is large enough to fabricate a field-effect transistor in each grain. The electrical and reliability test results, including endurance and retention test results, were superior to other FeRAMs reported so far and thus the results presented here constitute the first step toward the development of FeRAM using epitaxial-like ferroelectric thin-films. PMID:27005886

Carbide/nitride grain refined rare earth-iron-boron permanent magnet and method of making

DOEpatents

McCallum, R. William; Branagan, Daniel J.

1996-01-23

A method of making a permanent magnet wherein 1) a melt is formed having a base alloy composition comprising RE, Fe and/or Co, and B (where RE is one or more rare earth elements) and 2) TR (where TR is a transition metal selected from at least one of Ti, Zr, Hf, V, Nb, Ta, Cr, Mo, W, and Al) and at least one of C and N are provided in the base alloy composition melt in substantially stoichiometric amounts to form a thermodynamically stable compound (e.g. TR carbide, nitride or carbonitride). The melt is rapidly solidified in a manner to form particulates having a substantially amorphous (metallic glass) structure and a dispersion of primary TRC, TRN and/or TRC/N precipitates. The amorphous particulates are heated above the crystallization temperature of the base alloy composition to nucleate and grow a hard magnetic phase to an optimum grain size and to form secondary TRC, TRN and/or TRC/N precipitates dispersed at grain boundaries. The crystallized particulates are consolidated at an elevated temperature to form a shape. During elevated temperature consolidation, the primary and secondary precipitates act to pin the grain boundaries and minimize deleterious grain growth that is harmful to magnetic properties.

Refining As-cast β-Ti Grains Through ZrN Inoculation

NASA Astrophysics Data System (ADS)

Qiu, Dong; Zhang, Duyao; Easton, Mark A.; St John, David H.; Gibson, Mark A.

2018-03-01

The columnar-to-equiaxed transition and remarkable refinement of β-Ti grains occur in an as-cast Ti-13Mo alloy when a new grain refiner, ZrN, was inoculated at a nitrogen level as low as 0.4 wt pct. The grain refining effect is attributed to in situ-formed TiN particles that provide active nucleation sites and solute Zr that promotes constitutional supercooling. Reproducible orientation relationships were identified between TiN nucleants and β-Ti matrix, and well explained by the edge-to-edge matching model.

Interfacial Engineering of Inorganic Materials for Energy Storage and Conversion Applications

NASA Astrophysics Data System (ADS)

Samiee, Mojtaba

Since the micrometer-sized bulk materials have reached their inherent limits, development of new materials with high performance is essential for low cost and environmentally friendly electrochemical energy storage and conversion devices. One approach is to take advantage of interfacial engineering in order to modify currently developed materials, thus improving their properties for specific applications. The advantage of interfacial engineering is that it can also be applied to newly developed materials to further improve their properties for the specific applications. In first part of this dissertation, a systematic study is performed to investigate the effect of annealing in reducing atmospheres with different oxygen partial pressures and presence of other species (Ar, H2, N2, vacuum or hydrocarbon) on visible-light photocatalytic activity of TiO2. In second part, a facile nitridation method is used to improve the rate capability of TiO 2 as anode material for Li ion batteries. The enhanced high-rate capacities are attributed to moderate surface nitridation with less-disordered nitridated regions, which may enhance the surface electronic conductivity without forming discrete, nanoscale, and surface amorphous films to block the lithium transport. In third part, pseudocapacitive properties of V2O5-based adsorbates supported on TiO2 nanoparticles is systematically measured. Surface amorphous films (SAFs), which form naturally at thermodynamic equilibria at 550-600 °C with self-regulating or "equilibrium" thicknesses on the order of 1 nm, exhibit superior electrochemical performance at moderate and high scan rates (20-500 mV/s) that are of prime importance for supercapacitor applications, as compared with submonolayer and monolayer adsorbates formed at lower equilibration temperatures. In fourth part, we perform a combined experimental and computational investigation into the effects of aliovalent doping in NASICON on both bulk and grain boundary ionic conductivity. Our results show that the dopants with low solid solubility limits in NASICON solid solution lead to the formation of a conducting secondary phase at grain boundaries, thereby improving effective grain boundary conductivity that is otherwise hindered by the poorly-conducting Na3PO4 and ZrO2 secondary phases in undoped NASICON. In fifth part, inline electron holography technique is used to directly observe and investigate the space charge layers at grain boundaries of Y-doped BaZrO3.

Effect of transition metal impurities on the strength of grain boundaries in vanadium

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wu, Xuebang; Kong, Xiang-Shan; You, Yu-Wei

2016-09-07

Effects of 3d (Ti-Ni), 4d (Zr-Pd), and 5d (Hf-Pt) transition metal impurities on strength of two representative vanadium grain boundaries (GBs), symmetric Σ3(111) and asymmetric Σ5(210), were studied by first-principles calculations within the framework of the Rice-Wang thermodynamic model and within the computational tensile test. The desirable elements to increase the GB cohesion were predicted based on their segregation and strengthening behaviors across the different GB sites. It reveals that the elements Ti, Zr, Hf, Nb, and Ta are good choices for the GB cohesion enhancers. In addition, the GB strengthening by solutes is sensitive to the GB structures. Themore » elements Cr, Mn, Fe, Co, and Ni decrease the GB strength of the Σ3(111) GB but they can increase the cohesion of the Σ5(210) GB. Furthermore, the origin of Ti-induced change of the GB strength was uncovered by analyzing the atomic bonds and electronic structures as well as the tensile strength. This work provides a theoretical guidance to screen promising alloying elements in V-based materials with improved resistance to GB decohesion and also helps us to understand the formation mechanism of Ti-rich precipitates in the V-Cr-Ti alloys under neutron or ion irradiation environments.« less

Zirconia-alumina-nanodiamond composites with gemological properties

NASA Astrophysics Data System (ADS)

Díaz, Luis A.; Montes-Morán, Miguel A.; Peretyagin, Pavel Y.; Vladimirov, Yuriy G.; Okunkova, Anna; Moya, José S.; Torrecillas, Ramón

2014-02-01

Nanodiamonds have excellent mechanical and optical properties with a wide range of potential applications as a filler material for nanocomposites. Here, we present a new family of zirconia-alumina-nanodiamond composites using two main processing routes: (1) a colloidal method, and (2) power mixing homogenization. Composites with detonation nanodiamonds quantities ranging within 0.3-5 vol.% followed by a pulsed electrical current sintering at a temperature range from 1,200 to 1,500 °C have been analyzed, and a significant enhancement in mechanical properties, i.e., indentation hardness (16.17 GPa), fracture toughness (15.5 MPa m1/2), and bending strength (1,600 MPa), could be observed. To support these excellent properties, TEM, color, reflectivity, and Raman spectroscopy measurements were also carried out. The microstructure of the composites is very homogeneous with average grain sizes between 200 and 500 nm depending on the processing temperature. Two morphologies are present: (a) intergranular dispersion of alumina grains and nanodiamonds distributed along the grain boundaries of the ZrO2 matrix, and (b) intragranular nano-dispersion of ZrO2 particles with sizes 20-80 nm located inside the alumina grains. In the present article, we show, for the first time in the scientific literature, a continuous palette of gray color gradation of new ceramic materials of metalized colors (white index L* 98-40) for gemological applications.

The role of dispersed particles in strengthening and fracture mechanisms in a Mo-ZrC alloy processed by mechanical alloying

DOE Office of Scientific and Technical Information (OSTI.GOV)

Takida, T.; Mabuchi, M.; Nakamura, M.

2000-03-01

The tensile properties of a ZrC particle-dispersed Mo, which was processed by spark plasma sintering with mechanically alloyed powder, were investigated at room temperature and at elevated temperatures of 1,170 to 1,970 K. The Mo-ZrC alloy showed much higher strength at room temperature than a fully recrystallized pure Mo. The high strength of Mo-ZrC is mainly attributed to a very small grain size (about 3 {micro}m). The main role of the ZrC particle is not to increase strength due to the particle-dislocation interaction, but to limit grain growth during sintering and to attain the very small grain size. The elongationmore » at room temperature of No-ZrC was much lower than that of pure Mo. This is probably related to the higher interstitial contents. However, Mo-ZrC showed a large elongation of 180 pct at 1,970 K and 6.7 x 10{sup {minus}4} s{sup {minus}1}. It was suggested that the ZrC particles stabilized the fine-grained microstructure yet provided no cavitation sites at 1,970 K; as a result, the large elongation was attained.« less

Microstructural stability of wrought, laser and electron beam glazed NARloy-Z alloy at elevated temperatures

NASA Technical Reports Server (NTRS)

Singh, J.; Jerman, G.; Bhat, B.; Poorman, R.

1993-01-01

Microstructure of wrought, laser, and electron-beam glazed NARloy-Z(Cu-3 wt.% Ag-0.5 wt.% Zr) was investigated for thermal stability at elevated temperatures (539 to 760 C (1,100 to 1,400 F)) up to 94 h. Optical and scanning electron microscopy and electron probe microanalysis were employed for studying microstructural evolution and kinetics of precipitation. Grain boundary precipitation and precipitate free zones (PFZ's) were observed in the wrought alloy after exposing to temperatures above 605 C (1,120 F). The fine-grained microstructure observed in the laser and electron-beam glazed NARloy-Z was much more stable at elevated temperatures. Microstructural changes correlated well with hardness measurements.

Microstructural and Textural Differences Induced by Water and Furnace Cooling in Commercially Pure Zr Annealed in the α + β Region

NASA Astrophysics Data System (ADS)

Chai, Linjiang; Wang, Tingting; Ren, Yi; Song, Bo; Guo, Ning; Chen, Liangyu

2018-07-01

In this work, a commercially pure Zr sheet with a typical bimodal basal texture was annealed in an α + β region and then subjected to different coolings (in water and furnace). Microstructures and textures of both the as-received and the heat-treated specimens were investigated by electron channeling contrast imaging and electron backscatter diffraction techniques. Results show that a duplex microstructure consisting of untransformed bulk α grains and twinned martensitic plates is produced in the water-cooled specimen, which possesses a weakened texture compared to the initial one. For the specimen cooled in furnace, however, a uniform microstructure fully comprised of coarser equiaxed grains with a strengthened texture is obtained. Analyses reveal that the rapid cooling in water could suppress variant selection behaviors during β → α transformation and allow α plates with scattered orientations to be nucleated inside β phases, contributing to the weakened texture. In contrast, during slow cooling in furnace, β boundaries would act as preferred nucleation sites of α embryos, resulting in a strong variant selection that accounts for the intensified texture.

Microstructural and Textural Differences Induced by Water and Furnace Cooling in Commercially Pure Zr Annealed in the α + β Region

NASA Astrophysics Data System (ADS)

Chai, Linjiang; Wang, Tingting; Ren, Yi; Song, Bo; Guo, Ning; Chen, Liangyu

2018-03-01

In this work, a commercially pure Zr sheet with a typical bimodal basal texture was annealed in an α + β region and then subjected to different coolings (in water and furnace). Microstructures and textures of both the as-received and the heat-treated specimens were investigated by electron channeling contrast imaging and electron backscatter diffraction techniques. Results show that a duplex microstructure consisting of untransformed bulk α grains and twinned martensitic plates is produced in the water-cooled specimen, which possesses a weakened texture compared to the initial one. For the specimen cooled in furnace, however, a uniform microstructure fully comprised of coarser equiaxed grains with a strengthened texture is obtained. Analyses reveal that the rapid cooling in water could suppress variant selection behaviors during β → α transformation and allow α plates with scattered orientations to be nucleated inside β phases, contributing to the weakened texture. In contrast, during slow cooling in furnace, β boundaries would act as preferred nucleation sites of α embryos, resulting in a strong variant selection that accounts for the intensified texture.

Domain structures and local switching in lead-free piezoceramics Ba0.85Ca0.15Ti0.90Zr0.10O3

NASA Astrophysics Data System (ADS)

Turygin, A. P.; Neradovskiy, M. M.; Naumova, N. A.; Zayats, D. V.; Coondoo, I.; Kholkin, A. L.; Shur, V. Ya.

2015-08-01

Lead-free piezoelectrics are becoming increasingly important in view of environmental problems of currently used lead-based perovskites such as lead zirconate titanate (PZT). One of the recent candidates for PZT replacement, solid solutions of BaZr0.2Ti0.8O3 and Ba0.7Ca0.3TiO3, are investigated in this work by piezoresponse force microscopy. Coexistence of the tetragonal and rhombohedral phases in this material is observed, which probably gives rise to easy polarization switching due to multiple domain states. The period of observed domain lamella scales with the grain size obeying well-known square root dependence characteristic of BaTiO3 ceramics. Domain switching and relaxation are investigated at the nanoscale as a function of the applied voltage and duration of the applied voltage pulses. The observed distortion of piezoresponse hysteresis loops near grain boundaries is attested to the increased concentration of defects. Nanoscale piezoelectric properties of these materials are discussed.

Unipolar resistive switching behaviors and mechanisms in an annealed Ni/ZrO2/TaN memory device

NASA Astrophysics Data System (ADS)

Tsai, Tsung-Ling; Ho, Tsung-Han; Tseng, Tseung-Yuen

2015-01-01

The effects of Ni/ZrO2/TaN resistive switching memory devices without and with a 400 °C annealing process on switching properties are investigated. The devices exhibit unipolar resistive switching behaviors with low set and reset voltages because of a large amount of Ni diffusion with no reaction with ZrO2 after the annealing process, which is confirmed by ToF-SIMS and XPS analyses. A physical model based on a Ni filament is constructed to explain such phenomena. The device that undergoes the 400 °C annealing process exhibits an excellent endurance of more than 1.5  ×  104 cycles. The improvement can be attributed to the enhancement of oxygen ion migration along grain boundaries, which result in less oxygen ion consumption during the reset process. The device also performs good retention up to 105 s at 150 °C. Therefore, it has great potential for high-density nonvolatile memory applications.

Effects of MAR-M247 substrate (modified) composition on coating oxidation coating/substrate interdiffusion. M.S. Thesis. Final Report; [protective coatings for hot section components of gas turbine engines

NASA Technical Reports Server (NTRS)

Pilsner, B. H.

1985-01-01

The effects of gamma+gamma' Mar-M247 substrate composition on gamma+beta Ni-Cr-Al-Zr coating oxidation and coating/substrate interdiffusion were evaluated. These results were also compared to a prior study for a Ni-Cr-Al-Zr coated gamma Ni-Cr-Al substrate with equivalent Al and Cr atomic percentages. Cyclic oxidation behavior at 1130 C was investigated using change in weight curves. Concentration/distance profiles were measured for Al, Cr, Co, W, and Ta. The surface oxides were examined by X-ray diffraction and scanning electron microscopy. The results indicate that variations of Ta and C concentrations in the substrate do not affect oxidation resistance, while additions of grain boundary strengthening elements (Zr, Hf, B) increase oxidation resistance. In addition, the results indicate that oxidation phenomena in gamma+beta/gamma+gamma' Mar-M247 systems have similar characteristics to the l gamma+beta/gamma Ni-Cr-Al system.

Competitive Heterogeneous Nucleation Between Zr and MgO Particles in Commercial Purity Magnesium

NASA Astrophysics Data System (ADS)

Peng, G. S.; Wang, Y.; Fan, Z.

2018-04-01

Grain refining of commercial purity (CP) Mg by Zr addition with intensive melt shearing prior to solidification has been investigated. Experimental results showed that, when intensive melt shearing is imposed prior to solidification, the grain structure of CP Mg exhibits a complex changing pattern with increasing Zr addition. This complex behavior can be attributed to the change of nucleating particles in terms of their crystal structure, size, and number density with varied Zr additions. Naturally occurring MgO particles are found to be {100} faceted with a cubic morphology and 50 to 300 nm in size. Such MgO particles are usually populated densely in a liquid film (usually referred as oxide film) and can be effectively dispersed by intensive melt shearing. It has been confirmed that the dispersed MgO particles can act as nucleating substrates resulting in a significant grain refinement of CP Mg when no other more potent particles are present in the melt. However, Zr particles in the Mg-Zr alloys are more potent than MgO particles for nucleation of Mg due to their same crystal structure and similar lattice parameters with Mg. With the addition of Zr, Zr and the MgO particles co-exist in the melt. Grain refining efficiency is closely related to the competition for heterogeneous nucleation between Zr and the MgO particles. The final solidified microstructure is mainly determined by the interplay of three factors: nucleation potency (measured by lattice misfit), particle size, and particle number density.

Development in corrosion resistance by microstructural refinement in Zr-16 SS 304 alloy using suction casting technique

DOE Office of Scientific and Technical Information (OSTI.GOV)

Das, N., E-mail: nirupamd@barc.gov.in; Sengupta, P.; Abraham, G.

Highlights: • Grain refinement was made in Zr–16 wt.% SS alloy while prepared by suction casting process. • Distribution of Laves phase, e.g., Zr{sub 2}(Fe, Cr) was raised in suction cast (SC) Zr–16 wt.% SS. • Corrosion resistance was improved in SC alloy compared to that of arc-melt-cast alloy. • Grain refinement in SC alloy assisted for an increase in its corrosion resistance. - Abstract: Zirconium (Zr)-stainless steel (SS) hybrid alloys are being considered as baseline alloys for developing metallic-waste-form (MWF) with the motivation of disposing of Zr and SS base nuclear metallic wastes. Zr–16 wt.% SS, a MWF alloymore » optimized from previous studies, exhibit significant grain refinement and changes in phase assemblages (soft phase: Zr{sub 2}(Fe, Cr)/α-Zr vs. hard phase: Zr{sub 3}(Fe, Ni)) when prepared by suction casting (SC) technique in comparison to arc-cast-melt (AMC) route. Variation in Cr-distribution among different phases are found to be low in suction cast alloy, which along with grain refinement restricted Cr-depletion at the Zr{sub 2}(Fe, Cr)/Zr interfaces, prone to localized attack. Hence, SC alloy, compared to AMC alloy, showed lower current density, higher potential at the breakdown of passivity and higher corrosion potential during polarization experiments (carried out under possible geological repository environments, viz., pH 8, 5 and 1) indicating its superior corrosion resistance.« less

Competitive Heterogeneous Nucleation Between Zr and MgO Particles in Commercial Purity Magnesium

NASA Astrophysics Data System (ADS)

Peng, G. S.; Wang, Y.; Fan, Z.

2018-06-01

Grain refining of commercial purity (CP) Mg by Zr addition with intensive melt shearing prior to solidification has been investigated. Experimental results showed that, when intensive melt shearing is imposed prior to solidification, the grain structure of CP Mg exhibits a complex changing pattern with increasing Zr addition. This complex behavior can be attributed to the change of nucleating particles in terms of their crystal structure, size, and number density with varied Zr additions. Naturally occurring MgO particles are found to be {100} faceted with a cubic morphology and 50 to 300 nm in size. Such MgO particles are usually populated densely in a liquid film (usually referred as oxide film) and can be effectively dispersed by intensive melt shearing. It has been confirmed that the dispersed MgO particles can act as nucleating substrates resulting in a significant grain refinement of CP Mg when no other more potent particles are present in the melt. However, Zr particles in the Mg-Zr alloys are more potent than MgO particles for nucleation of Mg due to their same crystal structure and similar lattice parameters with Mg. With the addition of Zr, Zr and the MgO particles co-exist in the melt. Grain refining efficiency is closely related to the competition for heterogeneous nucleation between Zr and the MgO particles. The final solidified microstructure is mainly determined by the interplay of three factors: nucleation potency (measured by lattice misfit), particle size, and particle number density.

The formation mechanisms of surface nanocrystallites in β-type biomedical TiNbZrFe alloy by surface mechanical attrition treatment

NASA Astrophysics Data System (ADS)

Jin, Lei; Cui, Wenfang; Song, Xiu; Zhou, Lian

2015-08-01

A nanostructured surface layer was successfully performed on a biomedical β-type TiNbZrFe alloy by surface mechanical attrition treatment (SMAT). The results reveal that the surface layer along the depth from treated surface to strain-free matrix could be divided into an outer nanocrystalline layer (0-30 μm), a high-density dislocation region (30-200 μm) and an inner region with low-density dislocations and twins (200-700 μm) when the surface was treated for 60 min. The microhardness of the surface layer is enhanced and increases with increasing treatment time. Although the {1 1 2} <1 1 1> twin coordinates the deformations with dislocations, this coordination only occurs in the low strain area and cannot affect the nanocrystalline formation. The self-nanocrystallization of TiNbZrFe alloy is mainly attributed to dislocation movements. First, the dislocations start to move and easily form dislocation bands along certain crystal directions; then, multiple slips of dislocations gradually form dislocation tangles; after that, high-density dislocation tangles increases, which divides primary grains into many small domain areas. As high strain energies accumulate on the interfaces among these areas, the lattice rotation can be driven between the adjacent small domain areas, finally resulting in a large number of nanocrystalline regions with low or large angle grain boundaries.

Polaron-electron assisted giant dielectric dispersion in SrZrO{sub 3} high-k dielectric

DOE Office of Scientific and Technical Information (OSTI.GOV)

Borkar, Hitesh; Barvat, Arun; Pal, Prabir

2016-06-07

The SrZrO{sub 3} is a well known high-k dielectric constant (∼22) and high optical bandgap (∼5.8 eV) material and one of the potential candidates for future generation nanoelectronic logic elements (8 nm node technology) beyond silicon. Its dielectric behavior is fairly robust and frequency independent till 470 K; however, it suffers a strong small-polaron based electronic phase transition (T{sub e}) linking 650 to 750 K. The impedance spectroscopy measurements revealed the presence of conducting grains and grain boundaries at elevated temperature which provide energetic mobile charge carriers with activation energy in the range of 0.7 to 1.2 eV supporting the oxygen ions and proton conduction.more » X-ray photoemission spectroscopy measurements suggest the presence of weak non-stoichiometric O{sup 2−} anions and hydroxyl species bound to different sites at the surface and bulk. These thermally activated charge carriers at elevated temperature significantly contribute to the polaronic based dielectric anomaly and conductivity. Our dielectric anomaly supports pseudo phase transition due to high degree of change in ZrO{sub 6} octahedral angle in the temperature range of 650–750 K, where electron density and phonon vibration affect the dielectric and conductivity properties.« less

Investigations on the effect of grain size on hot tearing susceptibility of MgZn1Y2 alloy

NASA Astrophysics Data System (ADS)

Zhou, Z. J.; Liu, Z.; Wang, Y.; Mao, P. L.; Tang, W. R.; Zhou, Y.

2018-05-01

Effect of grain size on hot tearing susceptibility of MgZn1Y2 alloy was explored in the present paper. Based on the microstructure observation and phase constitution analysis results by the method of OM, SEM, EBSD and XRD, it was found that the addition of 0.2 wt% C2Cl6 or 0.5 wt% Zr could reduced the grain size significantly. The addition of Zr had the better effect than that of 0.2 wt% C2Cl6. The average grain size reduced from 55.48 μm to 20.64 μm, and the average grain shape aspect ratio reduced from 1.859 to 1.49 with the addition of Zr. Although the addition of 0.2 wt% C2Cl6 refined grain, it also reduced the amount of LPSO phase. It was also found that the dendrite coherent temperature (Tcoh) decreased with decreasing of the grain size of the alloy, while the dendrite coherent solid fraction ({{{{f}}}{{s}}}{{coh}}) increased with decreasing of the alloy. The modified Clyne-Davies model was used to predict the hot cracking susceptibility of the alloy. The predicted results indicated that the hot tearing susceptibility decreased with grain refinement. With addition of 0.2 wt% Zr, the predicted hot tearing sensitivity value was reduced by about 2.5 times than that of the alloy without the addition of Zr.

Microstructure and hot compression deformation of the as-cast Mg-5.0Sn-1.5Y-0.1Zr alloy

NASA Astrophysics Data System (ADS)

Luo, Xiaoping; Kang, Li; Li, Qiushu; Chai, Yuesheng

2015-08-01

The hot compression deformation behavior and microstructure of as-cast Mg-5.0Sn-1.5Y-0.1Zr alloy were investigated by performing isothermal hot compression tests. The tests were conducted using a thermal mechanical simulator at 250-450 °C and strain rates ranging from 0.002 to 2 s-1, with a maximum deformation strain of 50 %. The effects of the deformation parameters on the microstructure evolution of the Mg-5.0Sn-1.5Y-0.1Zr alloy were discussed. The study revealed the flow behavior and the deformation mechanism of the Mg-5.0Sn-1.5Y-0.1Zr alloy. The dependence of flow stress on temperature and strain rate was described by a hyperbolic sine constitutive equation. Through regression analysis, the activation energy of 223.26 kJ mol-1 for plastic deformation was determined by considering flow stress at a strain rate of 0.2. Microstructure observation showed that dynamic recrystallization occurred extensively along grain boundaries at temperatures higher than 300 °C and strain rates lower than 0.02 s-1. This observation provides a theoretical basis for the manufacture and application of the Mg-5.0Sn-1.5Y-0.1Zr alloy.

SrZrO 3 Formation at the Interlayer/Electrolyte Interface during (La 1-xSr x) 1-δCo 1-yFe yO 3 Cathode Sintering

DOE PAGES

Lu, Zigui; Darvish, Shadi; Hardy, John; ...

2017-07-19

This work probes the formation of SrZrO 3 at the SDC/YSZ interface (Sm doped ceria, SDC; Y stabilized zirconia, YSZ) during (La 1-xSr x) 1-δCo1 -yFe yO 3 (LSCF) cathode sintering. SEM/EDS and grazing incidence X-ray diffraction results of annealed LSCF and YSZ samples reveal that even without physical contact between LSCF and YSZ, SrZrO 3 was formed on the surface of YSZ, preferentially at the grain boundaries. It was suspected that the SrZrO 3 formation is due to the Sr-containing gas species diffused through the pores of the SDC layer and reacted with the YSZ electrolyte. Computational thermodynamics wasmore » adopted to predict the gas species formed in air during sintering by using the La-Sr-Co-Fe-O-H thermodynamic database. Sr(OH) 2 is identified as the dominant Sr-containing gas species under the experimental conditions. In addition, it was found that A-site deficiency in LSCF could effectively suppress the SrZrO 3 formation while a dense and pore-free SDC interlayer is required to totally block the SrZrO 3 formation. As a result, cell performance was significantly improved for a cell with a dense SDC interlayer fabricated by pulsed laser deposition, due to elimination of SrZrO 3 formation and therefore reduced interfacial resistance.« less

SrZrO 3 Formation at the Interlayer/Electrolyte Interface during (La 1-xSr x) 1-δCo 1-yFe yO 3 Cathode Sintering

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lu, Zigui; Darvish, Shadi; Hardy, John

This work probes the formation of SrZrO 3 at the SDC/YSZ interface (Sm doped ceria, SDC; Y stabilized zirconia, YSZ) during (La 1-xSr x) 1-δCo1 -yFe yO 3 (LSCF) cathode sintering. SEM/EDS and grazing incidence X-ray diffraction results of annealed LSCF and YSZ samples reveal that even without physical contact between LSCF and YSZ, SrZrO 3 was formed on the surface of YSZ, preferentially at the grain boundaries. It was suspected that the SrZrO 3 formation is due to the Sr-containing gas species diffused through the pores of the SDC layer and reacted with the YSZ electrolyte. Computational thermodynamics wasmore » adopted to predict the gas species formed in air during sintering by using the La-Sr-Co-Fe-O-H thermodynamic database. Sr(OH) 2 is identified as the dominant Sr-containing gas species under the experimental conditions. In addition, it was found that A-site deficiency in LSCF could effectively suppress the SrZrO 3 formation while a dense and pore-free SDC interlayer is required to totally block the SrZrO 3 formation. As a result, cell performance was significantly improved for a cell with a dense SDC interlayer fabricated by pulsed laser deposition, due to elimination of SrZrO 3 formation and therefore reduced interfacial resistance.« less

Electron beam physical vapor deposition of YSZ electrolyte coatings for SOFCs

NASA Astrophysics Data System (ADS)

He, Xiaodong; Meng, Bin; Sun, Yue; Liu, Bochao; Li, Mingwei

2008-09-01

YSZ electrolyte coatings were prepared by electron beam physical vapor deposition (EB-PVD) at a high deposition rate of up to 1 μm/min. The YSZ coating consisted of a single cubic phase and no phase transformation occurred after annealing treatment at 1000 °C. A typical columnar structure was observed in this coating by SEM and feather-like characteristics appeared in every columnar grain. In columnar grain boundaries there were many micron-sized gaps and pores. In TEM image, many white lines were found, originating from the alignment of nanopores existing within feather-like columnar grains. The element distribution along the cross-section of the coating was homogeneous except Zr with a slight gradient. The coating exhibited a characteristic anisotropic behavior in electrical conductivity. In the direction perpendicular to coating surface the electrical conductivity was remarkably higher than that in the direction parallel to coating surface. This mainly attributed to the typical columnar structure for EB-PVD coating and the existence of many grain boundaries along the direction parallel to coating surface. For as-deposited coating, the gas permeability coefficient of 9.78 × 10 -5 cm 4 N -1 s -1 was obtained and this value was close to the critical value of YSZ electrolyte layer required for solid oxide fuel cell (SOFC) operation.

Multiscale Modeling of UHTC: Thermal Conductivity

NASA Technical Reports Server (NTRS)

Lawson, John W.; Murry, Daw; Squire, Thomas; Bauschlicher, Charles W.

2012-01-01

We are developing a multiscale framework in computational modeling for the ultra high temperature ceramics (UHTC) ZrB2 and HfB2. These materials are characterized by high melting point, good strength, and reasonable oxidation resistance. They are candidate materials for a number of applications in extreme environments including sharp leading edges of hypersonic aircraft. In particular, we used a combination of ab initio methods, atomistic simulations and continuum computations to obtain insights into fundamental properties of these materials. Ab initio methods were used to compute basic structural, mechanical and thermal properties. From these results, a database was constructed to fit a Tersoff style interatomic potential suitable for atomistic simulations. These potentials were used to evaluate the lattice thermal conductivity of single crystals and the thermal resistance of simple grain boundaries. Finite element method (FEM) computations using atomistic results as inputs were performed with meshes constructed on SEM images thereby modeling the realistic microstructure. These continuum computations showed the reduction in thermal conductivity due to the grain boundary network.

Properties-Adjustable Alumina-Zirconia Nanolaminate Dielectric Fabricated by Spin-Coating.

PubMed

Peng, Junbiao; Wei, Jinglin; Zhu, Zhennan; Ning, Honglong; Cai, Wei; Lu, Kuankuan; Yao, Rihui; Tao, Hong; Zheng, Yanqiong; Lu, Xubing

2017-11-29

In this paper, an alumina-zirconia (Al₂O₃-ZrO₂) nanolaminate dielectric was fabricated by spin-coating and the performance was investigated. It was found that the properties of the dielectric can be adjusted by changing the content of Al₂O₃/ZrO₂ in nanolaminates: when the content of Al₂O₃ was higher than 50%, the properties of nanolaminates, such as the optical energy gap, dielectric strength (V ds ), capacitance density, and relative permittivity were relatively stable, while the change of these properties became larger when the content of Al₂O₃ was less than 50%. With the content of ZrO₂ varying from 50% to 100%, the variation of these properties was up to 0.482 eV, 2.12 MV/cm, 135.35 nF/cm², and 11.64, respectively. Furthermore, it was demonstrated that the dielectric strength of nanolaminates were influenced significantly by the number (n) of bilayers. Every increment of one Al₂O₃-ZrO 2 bilayer will enhance the dielectric strength by around 0.39 MV/cm (V ds ≈ 0.86 + 0.39n). This could be contributed to the amorphous alumina which interrupted the grain boundaries of zirconia.

Production, microstructure and mechanical properties of two different austenitic ODS steels

NASA Astrophysics Data System (ADS)

Gräning, T.; Rieth, M.; Hoffmann, J.; Möslang, A.

2017-04-01

This article is to summarize and examine processing parameters of novel developed austenitic oxide dispersed strengthened (ODS) steels. Comparing hot-rolled and extruded conditions after the same degree of deformation after and before annealing, are just some examples to give insights into the complex processing of austenitic ODS steels. One of the major drawbacks of the material is the more sophisticated production process. Due to a ductile matrix material with an increased stickiness during milling, a two-step milling procedure with the use of ZrO2 milling balls was applied to raise the production yield and to use the abrasion of the ZrO2 as an additional element to facilitate the formation of nano-sized precipitates. To get a better understanding how the different powder particle sizes after milling affect final properties, sieving was applied and revealed a serious effect in terms of precipitate size, distribution and mechanical properties. Grain sizes in relation to the precipitate size, annealing time and processing parameters were determined and compared to the mechanical properties. Hardness and tensile test have pointed out, that the precipitate size and number are more important in respect to the ultimate tensile strength than the grain size and that in this study hot-rolled material exhibited the better properties. The investigation of the microstructure illustrated the stability of precipitates during annealing at 1100 °C for 40 h. These heat treatments also led to a consistent grain size, due to the pinning effect of the grain boundaries, caused by precipitates.

Isotopic Composition of Molybdenum and Barium in Single Presolar Silicon Carbide Grains of Type A+B

NASA Technical Reports Server (NTRS)

Savina, M. R.; Tripa, C. E.; Pellin, M. J.; Davis, A. M.; Clayton, R. N.; Lewis, R. S.; Amari, S.

2003-01-01

Presolar SiC grains fall into several groups based on C, N, and Si isotopic compositions. Approximately 93% are defined as mainstream, having 10 less than C-12/C-13 less than 100 and N-14/N-15 ranging from 50 to 20,000. A number of studies have shown that the most likely sources of mainstream grains are low mass asymptotic giant branch stars. Models of nucleosynthesis in AGB stars reproduce the s-process enhancements seen in the heavy elements in mainstream SiC grains. Among the less common grains, A+B grains, which comprise approximately 3-4% of presolar SiC, are perhaps the least well understood. Recent studies by Amari et al. show that A+B grains can be divided into at least 4 groups based on their trace element concentration patterns. Of 20 grains studied, 7 showed trace element patterns consistent with condensation from a gas of solar system composition, while the rest had varying degrees of process enhancements. Our previous measurements on 3 A+B grains showed Mo of solar isotopic composition, but Zr with a strong enhancement in 96Zr, which is an r-process isotope but can be made in an sprocess if the neutron density is high enough to bridge the unstable Zr-95 (T(sub 1/2)= 64 d). The observation of Mo with solar system isotopic composition in the same grains is puzzling however. Meyer et al. have recently shown that a neutron burst mechanism can produce a high Zr-96/Zr-94 without enhancing Mo-100, however this model leads to enhancements in Mo-95 and Mo-97 not observed in A+B grains. We report here results of Mo measurements on 7 additional A+B grains, and Ba measurements on 2 A+B grains, and compare these to the previous studies.

Excess lithium salt functions more than compensating for lithium loss when synthesizing Li6.5La3Ta0.5Zr1.5O12 in alumina crucible

NASA Astrophysics Data System (ADS)

Liu, Kai; Ma, Jiang-Tao; Wang, Chang-An

2014-08-01

Garnet type electrolyte "Li6.5La3Ta0.5Zr1.5O12" (LLZTO) was prepared by conventional solid-state reaction in alumina crucibles and excess lithium salt (from 0% to 50 mol%) was added into the starting materials to investigate the effects of excess lithium salt on the property of LLZTO. SEM, XRD and AC impedance were used to determine the microstructure, phase formation and Li-ion conductivity. Cubic garnet with a minor second phase LiAlO2 in the grain boundary was obtained for the pellets with excess lithium salt. As the amount of excess lithium salt increased, more Al element diffused from alumina crucibles to LLZTO pellets and reacted with excess lithium salt to form liquid Li2O-Al2O3 phase in the grain boundary, which accelerated the pellets' densification and reduced lithium loss at a high temperature. Ionic conductivity of LLZTO pellets increased with the amount of excess lithium salt added and leveled off at ∼4 × 10-4 S cm-1 when lithium salt exceeded 30 mol%. The performance of Li-air batteries with hybrid electrolytes, using homemade LLZTO thin pellets as solid electrolytes, was investigated. The LLZTO thin pellet with more excess lithium salt in starting material had a higher density and resulted in better cell performance.

Intermetallic Growth and Interfacial Properties of the Grain Refiners in Al Alloys.

PubMed

Li, Chunmei; Cheng, Nanpu; Chen, Zhiqian; Xie, Zhongjing; Hui, Liangliang

2018-04-20

Al₃TM(TM = Ti, Zr, Hf, Sc) particles acting as effective grain refiners for Al alloys have been receiving extensive attention these days. In order to judge their nucleation behaviors, first-principles calculations are used to investigate their intermetallic and interfacial properties. Based on energy analysis, Al₃Zr and Al₃Sc are more suitable for use as grain refiners than the other two intermetallic compounds. Interfacial properties show that Al/Al₃TM(TM = Ti, Zr, Hf, Sc) interfaces in I-ter interfacial mode exhibit better interface wetting effects due to larger Griffith rupture work and a smaller interface energy. Among these, Al/Al₃Sc achieves the lowest interfacial energy, which shows that Sc atoms should get priority for occupying interfacial sites. Additionally, Sc-doped Al/Al₃(Zr, Sc) interfacial properties show that Sc can effectively improve the Al/Al₃(Zr, Sc) binding strength with the Al matrix. By combining the characteristics of interfaces with the properties of intermetallics, the core-shell structure with Al₃Zr-core or Al₃Zr(Sc1-1)-core encircled with an Sc-rich shell forms.

Oxidant effect of La(NO3)3·6H2O solution on the crystalline characteristics of nanocrystalline ZrO2 films grown by atomic layer deposition

NASA Astrophysics Data System (ADS)

Oh, Nam Khen; Kim, Jin-Tae; Kang, Goru; An, Jong-Ki; Nam, Minwoo; Kim, So Yeon; Park, In-Sung; Yun, Ju-Young

2017-02-01

Nanocrystalline ZrO2 films were synthesized by atomic layer deposition method using CpZr[N(CH3)2]3 (Cp = C5H5) as the metal precursor and La(NO3)3·6H2O solution as the oxygen source. La element in the deposited ZrO2 films could not be detected as its content was below the resolution limit of the X-ray photoelectron spectroscopy. The alternative introduction of La(NO3)3·6H2O solution to conventionally used H2O as the oxidant effectively altered the crystalline structure, grain size, and surface roughness of the grown ZrO2 films. Specifically, the crystalline structure of the ZrO2 film changed from a mixture of tetragonal and monoclinic phases to monoclinic phase. The average grain size also increased, and the resulting film surface became rougher. The average grain sizes of the ZrO2 films prepared from La(NO3)3·6H2O solution at concentrations of 10, 20, 30, and 40% were 280, 256, 208, and 200 nm, respectively, whereas that prepared using H2O oxidant was 142 nm. However, the concentration of La(NO3)3·6H2O solution minimally influenced the crystalline characteristics of the nanocrystalline ZrO2 films i.e., the crystalline structure, grain size, and surface roughness except for crystallite size.

Modeling of hydride precipitation and re-orientation

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tikare, Veena; Weck, Philippe F.; Mitchell, John Anthony

In this report, we present a thermodynamic-­based model of hydride precipitation in Zr-based claddings. The model considers the state of the cladding immediately following drying, after removal from cooling-pools, and presents the evolution of precipitate formation upon cooling as follows: The pilgering process used to form Zr-based cladding imparts strong crystallographic and grain shape texture, with the basal plane of the hexagonal α-Zr grains being strongly aligned in the rolling-­direction and the grains are elongated with grain size being approximately twice as long parallel to the rolling direction, which is also the long axis of the tubular cladding, as itmore » is in the orthogonal directions.« less

Investigation of conduction and relaxation phenomena in BaZrxTi1-xO3 (x=0.05) by impedance spectroscopy

NASA Astrophysics Data System (ADS)

Mahajan, Sandeep; Haridas, Divya; Ali, S. T.; Munirathnam, N. R.; Sreenivas, K.; Thakur, O. P.; Prakash, Chandra

2014-10-01

In present study we have prepared ferroelectric BaZrxTi1-xO3 (x=0.05) ceramic by conventional solid state reaction route and studied its electrical properties as a function of temperature and frequency. X-ray diffraction (XRD) analysis shows single-phase formation of the compound with orthorhombic crystal structure at room temperature. Impedance and electric modulus spectroscopy analysis in the frequency range of 40 Hz-1 MHz at high temperature (200-600 °C) suggests two relaxation processes with different time constant are involved which are attributed to bulk and grain boundary effects. Frequency dependent dielectric plot at different temperature shows normal variation with frequency while dielectric loss (tanδ) peak was found to obey an Arrhenius law with activation energy of 1.02 eV. The frequency-dependent AC conductivity data were also analyzed in a wide temperature range. In present work we have studied the role of grain and grain boundaries on the electrical behaviour of Zr-doped BaTiO3 and their dependence on temperature and frequency by complex impedance and modulus spectroscopy (CIS) technique in a wide frequency (40 Hz-1 MHz) and high temperature range.

Effects of Zr on microstructure and mechanical properties of Al-Cu base ribbons spun by planar flow casting

NASA Astrophysics Data System (ADS)

Lee, S. M.; Hong, C. P.

1998-04-01

The effects of the Zr addition on the solidification behavior and mechanical properties of the AI-Cu alloy ribbon have been investigated. Zr addition reduced the average grain size of the ribbon at the wheel-side surface, and promoted the microstructural transition into cellular/dendritic structure. Another noteworthy effect of Zr was the homogenization of the microstructure. The addition of Zr up to 0.5 wt.% in the /U-4.3 wt.% Cu ribbon resulted in a considerable increase in hardness at both the wheel-side and the air-side surfaces. The yield strength increased with the addition of Zr due to the grain refincment and more homogeneous distribution of ZrAI, particles. despite no noticeable improvement of the ductility.

Effects of homogenization treatment on recrystallization behavior of 7150 aluminum sheet during post-rolling annealing

DOE Office of Scientific and Technical Information (OSTI.GOV)

Guo, Zhanying; Department of Applied Science, University of Québec at Chicoutimi, Saguenay, QC G7H 2B1; Zhao, Gang

2016-04-15

The effects of two homogenization treatments applied to the direct chill (DC) cast billet on the recrystallization behavior in 7150 aluminum alloy during post-rolling annealing have been investigated using the electron backscatter diffraction (EBSD) technique. Following hot and cold rolling to the sheet, measured orientation maps, the recrystallization fraction and grain size, the misorientation angle and the subgrain size were used to characterize the recovery and recrystallization processes at different annealing temperatures. The results were compared between the conventional one-step homogenization and the new two-step homogenization, with the first step being pretreated at 250 °C. Al{sub 3}Zr dispersoids with highermore » densities and smaller sizes were obtained after the two-step homogenization, which strongly retarded subgrain/grain boundary mobility and inhibited recrystallization. Compared with the conventional one-step homogenized samples, a significantly lower recrystallized fraction and a smaller recrystallized grain size were obtained under all annealing conditions after cold rolling in the two-step homogenized samples. - Highlights: • Effects of two homogenization treatments on recrystallization in 7150 Al sheets • Quantitative study on the recrystallization evolution during post-rolling annealing • Al{sub 3}Zr dispersoids with higher densities and smaller sizes after two-step treatment • Higher recrystallization resistance of 7150 sheets with two-step homogenization.« less

Transport and magnetic properties of HITPERM alloys

NASA Astrophysics Data System (ADS)

Pekala, K.; Latuch, J.; Pekala, M.; Skorvanek, I.; Jaskiewicz, P.

2003-02-01

Nanocrystalline HITPERM alloys Fe44.6Co43.3X7.4B3.7Cu1 (X = Nb, Zr, Hf) prepared by crystallization of amorphous precursors are studied by magnetization and electrical resistivity measurements for the first time. Structural and magnetic components of the electrical resistivity are separated. The electrical resistivity of the nanocrystalline α' (FeCo) phase calculated using the Maxwell Garnett relation proves strong electron scattering on the grain boundaries. The temperature variation of the crystalline fraction during the first crystallization stage is calculated for the Hf based alloy.

Zr-in-rutile resetting in aluminosilicate bearing ultra-high temperature granulites: Refining the record of cooling and hydration in the Napier Complex, Antarctica

NASA Astrophysics Data System (ADS)

Mitchell, Ruairidh J.; Harley, Simon L.

2017-02-01

The relative validity and closure temperature of the Zr-in-rutile thermometer for recording UHT metamorphism are process dependent and hotly debated. We present an integrated petrological approach to Zr-in-rutile thermometry including phase equilibrium (pseudosection) modelling in complex chemical systems with updated mineral a-X models and systematic in-situ microanalysis of rutile. This study is centred on high-pressure rutile bearing UHT granulites from Mt. Charles, Napier Complex, Antarctica. P-T phase equilibrium modelling of two garnet bearing granulites (samples 49677, 49701) constrains an overall post-peak near isobaric cooling (IBC) evolution for the Napier Complex at Mt. Charles; from 14 kbar, 1100 °C with moderate decompression to 11 kbar, 800-900 °C. Local hydration on cooling over this temperature range is recorded in a kyanite bearing granulite (sample 49688) with an inferred injection of aqueous fluid equivalent to up to 9 mol% H2O from T-MH2O modelling. Further late stage cooling to < 740 °C is recorded by voluminous retrograde mica growth and partial preservation of a ky-pl-kfs-bt-liq bearing equilibrium assemblage. Overall, Zr-in-rutile temperatures at 11 kbar (Tomkins et al., 2007) are reset to between 606 °C and 780 °C across all samples, with flat core-rim Zr concentration profiles in all rutiles. However, zircon precipitates as inclusions, needle exsolutions, or rods along rutile grain boundaries are recrystallised from rutiles in qz/fsp domains. Reintegrating the Zr-in-rutile concentration 'lost' via the recrystallisation of these zircon precipitates (e.g. Pape et al., 2016) can recover maximum concentrations of up to 2.2 wt% and thus maximum peak temperatures of 1149 °C at 11 kbar. Rutile Nb-Ta signatures and rounded rutile grains without zircon precipitates in hydrated mica domains in sample 49688 provide evidence for fluid-mediated mobility of Zr and Nb during retrograde cooling in hydrated lithologies. Aqueous fluid supplemented excess H2O liberated by melt crystallisation, interacting with rutile on cooling of sample 49688 to reset Zr-in-rutile temperatures (606-780 °C) at the Mt. Charles locality. The wide range of geochemical and petrological characteristics of Napier Complex rutile highlights that Zr-in-rutile reintegration and a broad petrological approach are required for successful interpretation of Zr-in-rutile geothermometry for long-lived regional UHT metamorphism.

Modeling the effect of neighboring grains on twin growth in HCP polycrystals

DOE PAGES

Kumar, M. Arul; Beyerlein, I. J.; Lebensohn, R. A.; ...

2017-08-04

In this paper, we study the dependence of neighboring grain orientation on the local stress state around a deformation twin in a hexagonal close packed (HCP) crystal and its effects on the resistance against twin thickening. We use a recently developed, full-field elasto-visco-plastic formulation based on fast Fourier transforms that accounts for the twinning shear transformation imposed by the twin lamella. The study is applied to Mg, Zr and Ti, since these HCP metals tend to deform by activation of different types of slip modes. The analysis shows that the local stress along the twin boundary are strongly controlled bymore » the relative orientation of the easiest deformation modes in the neighboring grain with respect to the twin lamella in the parent grain. A geometric expression that captures this parent-neighbor relationship is proposed and incorporated into a larger scale, mean-field visco-plastic self-consistent model to simulate the role of neighboring grain orientation on twin thickening. We demonstrate that the approach improves the prediction of twin area fraction distribution when compared with experimental observations.« less

Modeling the effect of neighboring grains on twin growth in HCP polycrystals

NASA Astrophysics Data System (ADS)

Kumar, M. Arul; Beyerlein, I. J.; Lebensohn, R. A.; Tomé, C. N.

2017-09-01

In this paper, we study the dependence of neighboring grain orientation on the local stress state around a deformation twin in a hexagonal close packed (HCP) crystal and its effects on the resistance against twin thickening. We use a recently developed, full-field elasto-visco-plastic formulation based on fast Fourier transforms that account for the twinning shear transformation imposed by the twin lamella. The study is applied to Mg, Zr and Ti, since these HCP metals tend to deform by activation of different types of slip modes. The analysis shows that the local stress along the twin boundary are strongly controlled by the relative orientation of the easiest deformation modes in the neighboring grain with respect to the twin lamella in the parent grain. A geometric expression that captures this parent-neighbor relationship is proposed and incorporated into a larger scale, mean-field visco-plastic self-consistent model to simulate the role of neighboring grain orientation on twin thickening. We demonstrate that the approach improves the prediction of twin area fraction distribution when compared with experimental observations.

Synthesis of nano-scale fast ion conducting cubic Li7La3Zr2O12.

PubMed

Sakamoto, Jeff; Rangasamy, Ezhiylmurugan; Kim, Hyunjoung; Kim, Yunsung; Wolfenstine, Jeff

2013-10-25

A solution-based process was investigated for synthesizing cubic Li7La3Zr2O12 (LLZO), which is known to exhibit the unprecedented combination of fast ionic conductivity, and stability in air and against Li. Sol-gel chemistry was developed to prepare solid metal-oxide networks consisting of 10 nm cross-links that formed the cubic LLZO phase at 600 ° C. Sol-gel LLZO powders were sintered into 96% dense pellets using an induction hot press that applied pressure while heating. After sintering, the average LLZO grain size was 260 nm, which is 13 times smaller compared to LLZO prepared using a solid-state technique. The total ionic conductivity was 0.4 mS cm(-1) at 298 K, which is the same as solid-state synthesized LLZO. Interestingly, despite the same room temperature conductivity, the sol-gel LLZO total activation energy is 0.41 eV, which 1.6 times higher than that observed in solid-state LLZO (0.26 eV). We believe the nano-scale grain boundaries give rise to unique transport phenomena that are more sensitive to temperature when compared to the conventional solid-state LLZO.

Evolution of the structure and mechanical properties of sheets of the Al-4.7Mg-0.32Mn-0.21Sc-0.09Zr alloy due to deformation accumulated upon rolling

NASA Astrophysics Data System (ADS)

Zolotorevskiy, V. S.; Dobrojinskaja, R. I.; Cheverikin, V. V.; Khamnagdaeva, E. A.; Pozdniakov, A. V.; Levchenko, V. S.; Besogonova, E. S.

2016-11-01

The mechanical properties and microstructure of sheets of an Al-4.7Mg-0.32Mn-0.21Sc-0.09Zr alloy deformed and annealed after rolling have been investigated. The total accumulated true strain was ɛf = 3.33-5.63, and the true strain at room temperature and at 200 °C was ɛc = 0.25-2.3. The strength properties of the sheets (yield stress σ0.2 = 495 MPa and ultimate tensile strength σu = 525 MPa) in the deformed state were greater than those after equal-channel angular pressing (ECAP) deformation. The mechanical properties of the deformed sheets after annealing depended on the size of subgrains inside the deformed grains bands with high-angle grain boundaries (HABs). With the increase in the annealing temperature from 150 to 300°C, the subgrain size increased from 80 to 300 nm. The relative elongation δ in the as-cast state and after annealing at 200-250°C (δ = 40-50%) was higher than that after annealing at 300-370°C (δ = 24-29%).

Intermetallic Growth and Interfacial Properties of the Grain Refiners in Al Alloys

PubMed Central

Li, Chunmei; Cheng, Nanpu; Chen, Zhiqian; Xie, Zhongjing; Hui, Liangliang

2018-01-01

Al3TM(TM = Ti, Zr, Hf, Sc) particles acting as effective grain refiners for Al alloys have been receiving extensive attention these days. In order to judge their nucleation behaviors, first-principles calculations are used to investigate their intermetallic and interfacial properties. Based on energy analysis, Al3Zr and Al3Sc are more suitable for use as grain refiners than the other two intermetallic compounds. Interfacial properties show that Al/Al3TM(TM = Ti, Zr, Hf, Sc) interfaces in I-ter interfacial mode exhibit better interface wetting effects due to larger Griffith rupture work and a smaller interface energy. Among these, Al/Al3Sc achieves the lowest interfacial energy, which shows that Sc atoms should get priority for occupying interfacial sites. Additionally, Sc-doped Al/Al3(Zr, Sc) interfacial properties show that Sc can effectively improve the Al/Al3(Zr, Sc) binding strength with the Al matrix. By combining the characteristics of interfaces with the properties of intermetallics, the core-shell structure with Al3Zr-core or Al3Zr(Sc1-1)-core encircled with an Sc-rich shell forms. PMID:29677155

Mechanical properties and corrosion behavior of Mg-Gd-Ca-Zr alloys for medical applications.

PubMed

Shi, Ling-Ling; Huang, Yuanding; Yang, Lei; Feyerabend, Frank; Mendis, Chamini; Willumeit, Regine; Ulrich Kainer, Karl; Hort, Norbert

2015-07-01

Magnesium alloys are promising candidates for biomedical applications. In this work, influences of composition and heat treatment on the microstructure, the mechanical properties and the corrosion behavior of Mg-Gd-Ca-Zr alloys as potential biomedical implant candidates were investigated. Mg5Gd phase was observed at the grain boundaries of Mg-10Gd-xCa-0.5Zr (x=0, 0.3, 1.2wt%) alloys. Increase in the Ca content led to the formation of additional Mg2Ca phase. The Ca additions increased both the compressive and the tensile yield strengths, but reduced the ductility and the corrosion resistance in cell culture medium. After solution heat treatment, the Mg5Gd particles dissolved in the Mg matrix. The compressive strength decreased, while the corrosion resistance improved in the solution treated alloys. After ageing at 200°C, metastable β' phase formed on prismatic planes and a new type of basal precipitates have been observed, which improved the compressive and tensile ultimate strength, but decreased the ductility. Copyright © 2015 Elsevier Ltd. All rights reserved.

Effect of sol temperature on structural, morphological and magnetic properties of PZT thin films on alumina substrate

NASA Astrophysics Data System (ADS)

Sreelalitha, K.; Thyagarajan, K.

2016-01-01

In the present study, we investigate the structural, morphological and magnetic properties of sol-gel spin-coated PZT thin films on alumina substrate. The morphotropic phase boundary (MPB) of PZT [Pb (Zr1-xTix)03] between the tetragonal and rhombohedral phases occurs at the Zr/Ti ratio of 52/48. At the MPB the physical properties of PZT are of far-reaching importance due to their possible crystalline phases. In this study Pb(Zr0.52Ti0.48)03 sols are prepared at room temperature and at 125 °C. The gels are coated onto alumina substrate using a spin-coating unit as two and three layers. The structural studies using XRD confirm the perovskite phase formation at an annealing temperature of 660 °C for both films. The structural parameter grain size, dislocation density, lattice parameters and strain were dependent on the sol temperature. The SEM morphology of the samples represents well-developed dense grain structure and thickness in micrometer ranges. The VSM analysis shows diamagnetic and ferromagnetic hysteresis loop. The ferromagnetism at low fields in PZT films is confirmed by studying the magnetic properties of powder made of the same gel. The effect of heat treatment on the gel preparation is observed on structural, morphological and magnetic properties of PZT thin films. The ferromagnetism in PZT can be attributed to oxygen vacancies. The squareness ratio of the films shows the application of the films as a high-density recording medium.

Zirconium Carbide Produced by Spark Plasma Sintering and Hot Pressing: Densification Kinetics, Grain Growth, and Thermal Properties

PubMed Central

Wei, Xialu; Back, Christina; Izhvanov, Oleg; Haines, Christopher D.; Olevsky, Eugene A.

2016-01-01

Spark plasma sintering (SPS) has been employed to consolidate a micron-sized zirconium carbide (ZrC) powder. ZrC pellets with a variety of relative densities are obtained under different processing parameters. The densification kinetics of ZrC powders subjected to conventional hot pressing and SPS are comparatively studied by applying similar heating and loading profiles. Due to the lack of electric current assistance, the conventional hot pressing appears to impose lower strain rate sensitivity and higher activation energy values than those which correspond to the SPS processing. A finite element simulation is used to analyze the temperature evolution within the volume of ZrC specimens subjected to SPS. The control mechanism for grain growth during the final SPS stage is studied via a recently modified model, in which the grain growth rate dependence on porosity is incorporated. The constant pressure specific heat and thermal conductivity of the SPS-processed ZrC are determined to be higher than those reported for the hot-pressed ZrC and the benefits of applying SPS are indicated accordingly. PMID:28773697

Zirconium Carbide Produced by Spark Plasma Sintering and Hot Pressing: Densification Kinetics, Grain Growth, and Thermal Properties

DOE PAGES

Wei, Xialu; Back, Christina; Izhvanov, Oleg; ...

2016-07-14

Spark plasma sintering (SPS) has been employed to consolidate a micron-sized zirconium carbide (ZrC) powder. ZrC pellets with a variety of relative densities are obtained under different processing parameters. The densification kinetics of ZrC powders subjected to conventional hot pressing and SPS are comparatively studied by applying similar heating and loading profiles. Due to the lack of electric current assistance, the conventional hot pressing appears to impose lower strain rate sensitivity and higher activation energy values than those which correspond to the SPS processing. A finite element simulation is used to analyze the temperature evolution within the volume of ZrCmore » specimens subjected to SPS. The control mechanism for grain growth during the final SPS stage is studied via a recently modified model, in which the grain growth rate dependence on porosity is incorporated. Finally, the constant pressure specific heat and thermal conductivity of the SPS-processed ZrC are determined to be higher than those reported for the hot-pressed ZrC and the benefits of applying SPS are indicated accordingly.« less

Pulsed-Laser Crystallization of Ferroelectric/Piezoelectric Oxide Thin Films

NASA Astrophysics Data System (ADS)

Rajashekhar, Adarsh

Integration of ferroelectric/piezoelectric thin films, such as those of lead zirconate titanate (PZT), with temperature sensitive substrates (complementary metal oxide semiconductors (CMOS), or polymers) would benefit from growth at substrate temperatures below 400°C. However, high temperatures are usually required for obtaining good quality PZT films via conventional routes like rapid thermal processing (>550°C). Those conditions are not compatible either with polymer substrates or completed CMOS circuits and dictate exploration of alternative methods to realize integration with such substrates. In part of this work, factors influencing KrF excimer laser induced crystallization of amorphous sputtered Pb(Zr0.30Ti0.70)O3 thin films at substrate temperatures < 215°C were investigated. (111) Pt/Si substrates were utilized to understand the process window. Laser energy densities studied were in the range 35 - 85 mJ/cm2. The Pb content in the films was varied via the Ar gas pressure (in the range 5 mTorr - 9 mTorr) during sputtering of amorphous films. It was seen that a higher Pb content in the asdeposited films aided nucleation of the perovskite phase. Ozone-containing ambients (10% O3/90% O2) during the annealing promoted the formation of the metastable Pb-rich pyrochlore/fluorite phase, while annealing in pure oxygen produced the perovskite phase at relatively lower annealing laser energy densities. Heterogeneous nucleation from the substrate is favored on utilizing a layer-by-layer growth and crystallization process. Films were also grown on polymers using this method. Ferroelectric switching was demonstrated, but extensive process optimization would be needed to reduce leakage and porosity. Real time laser annealing during growth allows for scaling of the layer-by-layer growth process. A pulsed laser deposition system with in situ laser annealing was thus designed, built, and utilized to grow Pb(Zr 0.52Ti0.48)O3 thin films on a laser crystallized Pb(Zr0.20Ti0.80)O3 seed layer, at a temperature of 370°C. Polycrystalline 1.1 microm thick films exhibited columnar grains with small grain sizes ( 30 nm). The films showed well-saturated hysteresis loops (with a remanent polarization of 25 microC/cm2, and a coercive field of 50 kV/cm) and exhibited loss tangents <2.5% with a permittivity of 730. Film orientation could be controlled via the substrate choice; {111} Pb(Zr0.52Ti0.48)O3 films were grown on oriented (111) Pb(Zr0.30Ti0.70)O3 sol-gel seed layers, while epitaxial {001} films were prepared on (100) SrTiO 3 single crystals. In order to study the microstructure evolution in these films, in situ pulsed-laser annealing was used to grow crystalline lead zirconate titanate (PbZr0.52Ti0.48O3) thin films at a substrate temperature of 370°C on PbZr0.30Ti 0.70O3-buffered platinized silicon substrates. Transmission electron microscopy (TEM) analysis indicated that the films were well crystallized into columnar grains, but with pores segregated at the grain boundaries. Lateral densification of the grain columns was significantly improved by reducing the partial pressure of oxygen from 120 mTorr to 50 mTorr, presumably due to enhanced adatom mobility at the surface accompanying increased bombardment. It was found that varying the fractional annealing duration with respect to the deposition duration produced little effect on lateral grain growth. However, increasing the fractional annealing duration led to shift of 111 PZT X-ray diffraction peaks to higher 2theta values, suggesting residual in-plane tensile stresses in the films. Thermal simulations were used to understand the annealing process. Evolution of the film microstructure is described in terms of transient heating from the pulsed laser determining the nucleation events, while the energy of the arriving species dictates grain growth/coarsening.

Microanalytical characterization of multi-rare earth nanocrystalline magnets by TEM and APT

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wu, Y. Q.; Tang, W.; Miller, Michael K

2006-01-01

The partitioning behavior of various rare-earth (RE) elements during solidification and their segregation behavior at the grain boundaries were investigated in nanocrystalline (Y{sub 0.5}Dy{sub 0.5}{sub 2.2}Fe{sub 14}B and (Nd{sub 0.5}Y{sub 0.25}Dy{sub 0.25}){sub 1.8}Zr{sub 0.4}Co{sub 1.5}Fe{sub 12.5}B alloys by transmission electron microscopy and atom probe tomography. The best hard magnetic properties obtained are H{sub cj} = 22 kOe, B{sub r}=5.10 kG, and (BH){sub max} = 5.97 MG Oe for the Y-Dy-based alloy and H{sub cj}=10.6 kOe, B{sub r}=6.64 kG, and (BH){sub max}=9.56 MG Oe for the Y-Nd-Dy based alloy. The grain size of the Y-Dy based alloy was {approx} 50 nm.more » The Y-Nd-Dy based alloy had an overall finer, bimodal grain size. An intergranular (Y{sub 0.36}Dy{sub 0.64}){sub 6}Fe{sub 23} phase was detected in the Y-Dy based alloy. A uniform distribution of RE elements was found within the 2-14-1 grains in both alloys. The Y:(Dy+Nd) ratio in the Y-Nd-Dy alloy was lower than its nominal composition, indicating that the Y is segregating to grain boundaries or forming a second phase.« less

Improvement of perpendicular anisotropy of columnar FePt-ZrO2-C films with FePt insert layer

NASA Astrophysics Data System (ADS)

Dong, Kaifeng; Mo, Wenqin; Jin, Fang; Song, Junlei; Cheng, Weimin; Wang, Haiwei

2018-05-01

The effects of various thicknesses of FePt insert layer on the microstructure and magnetic properties of FePt-ZrO2-C thin films have been investigated. It is found that with inserting 0.4 nm FePt films between the TiON intermediate layer and FePt-ZrO2-C layer, the perpendicular anisotropy indicated by Hc⊥/Hc//ratio would increase from 4 to 13.1, suggesting the perpendicular anisotropy could be improved a lot with using FePt insert layer. Simultaneously, the FePt grains of FePt-ZrO2-C thin films maintained columnar structure and the grain isolation could also be improved in a certain degree. With further increase of the FePt insert layer thickness, although the perpendicular anisotropy was still larger than that without FePt insert layer, the grain size of the FePt-ZrO2-C films would increase and the isolation would be deteriorated.

Non-stick syringe needles: Beneficial effects of thin film metallic glass coating

PubMed Central

Chu, Jinn P.; Yu, Chia-Chi; Tanatsugu, Yusuke; Yasuzawa, Mikito; Shen, Yu-Lin

2016-01-01

This paper reports on the use of Zr-based (Zr53Cu33Al9Ta5) thin film metallic glass (TFMG) for the coating of syringe needles and compares the results with those obtained using titanium nitride and pure titanium coatings. TFMG coatings were shown to reduce insertion forces by ∼66% and retraction forces by ∼72%, when tested using polyurethane rubber block. The benefits of TFMG-coated needles were also observed when tested using muscle tissue from pigs. In nano-scratch tests, the TFMG coatings achieved a coefficient of friction (COF) of just ∼0.05, which is about one order of magnitude lower than those of other coatings. Finite-element modeling also indicates a significant reduction in injection and retraction forces. The COF can be attributed to the absence of grain boundaries in the TFMG coating as well as a smooth surface morphology and low surface free energy. PMID:27573062

Scaling effects in sodium zirconium silicate phosphate (Na 1+ xZr 2Si xP 3- xO 12) ion-conducting thin films

DOE PAGES

Ihlefeld, Jon F.; Gurniak, Emily; Jones, Brad H.; ...

2016-05-04

Preparation of sodium zirconium silicate phosphate (NaSICon), Na 1+xZr 2Si xP 3–xO 12 (0.25 ≤ x ≤ 1.0), thin films has been investigated via a chemical solution approach on platinized silicon substrates. Increasing the silicon content resulted in a reduction in the crystallite size and a reduction in the measured ionic conductivity. Processing temperature was also found to affect microstructure and ionic conductivity with higher processing temperatures resulting in larger crystallite sizes and higher ionic conductivities. The highest room temperature sodium ion conductivity was measured for an x = 0.25 composition at 2.3 × 10 –5 S/cm. In conclusion, themore » decreasing ionic conductivity trends with increasing silicon content and decreasing processing temperature are consistent with grain boundary and defect scattering of conducting ions.« less

Thermal Aging Behavior of Axial Suspension Plasma-Sprayed Yttria-Stabilized Zirconia (YSZ) Thermal Barrier Coatings

NASA Astrophysics Data System (ADS)

Zhao, Yuexing; Wang, Liang; Yang, Jiasheng; Li, Dachuan; Zhong, Xinghua; Zhao, Huayu; Shao, Fang; Tao, Shunyan

2015-02-01

7.5YSZ thermal barrier coatings (TBCs) were deposited onto the stainless steel substrates using axial suspension plasma spraying (ASPS). Free-standing coatings were isothermally aged in air from 1200 to 1600 °C for 24 h and at 1550 °C for 20 to 100 h, respectively. Thermal aging behavior such as phase composition, microstructure evolutions, grain growth, and mechanical properties for thermal-aged coatings were investigated. Results show that the as-sprayed metastable tetragonal (t'-ZrO2) phase decomposes into equilibrium tetragonal (t-ZrO2) and cubic (c-ZrO2) phases during high-temperature exposures. Upon further cooling, the c-ZrO2 may be retained or transform into another metastable tetragonal (t″-ZrO2) phase, and tetragonal → monoclinic phase transformation occurred after 1550 °C/40 h aging treatment. The coating exhibits a unique structure with segmentation cracks and micro/nano-size grains, and the grains grow gradually with increasing aging temperature and time. In addition, the hardness ( H) and Young's modulus ( E) significantly increased as a function of temperature due to healing of pores or cracks and grain growth of the coating. And a nonmonotonic variation is found in the coatings thermal aged at a constant temperature (1550 °C) with prolonged time, this is a synergetic effect of coating sintering and m-ZrO2 phase formation.

Tensile and Compressive Responses of Ceramic and Metallic Nanoparticle Reinforced Mg Composites

PubMed Central

Tun, Khin Sandar; Wong, Wai Leong Eugene; Nguyen, Quy Bau; Gupta, Manoj

2013-01-01

In the present study, room temperature mechanical properties of pure magnesium, Mg/ZrO2 and Mg/(ZrO2 + Cu) composites with various compositions are investigated. Results revealed that the use of hybrid (ZrO2 + Cu) reinforcements in Mg led to enhanced mechanical properties when compared to that of single reinforcement (ZrO2). Marginal reduction in mechanical properties of Mg/ZrO2 composites were observed mainly due to clustering of ZrO2 particles in Mg matrix and lack of matrix grain refinement. Addition of hybrid reinforcements led to grain size reduction and uniform distribution of hybrid reinforcements, globally and locally, in the hybrid composites. Macro- and micro- hardness, tensile strengths and compressive strengths were all significantly increased in the hybrid composites. With respect to unreinforced magnesium, failure strain was almost unchanged under tensile loading while it was reduced under compressive loading for both Mg/ZrO2 and Mg/(ZrO2 + Cu) composites. PMID:28809245

Parametric Study on the Tensile Properties of Ni-Based Alloy for a VHTR

NASA Astrophysics Data System (ADS)

Kim, Dong-Jin; Jung, Su Jin; Mun, Byung Hak; Kim, Sung Woo; Lim, Yun Soo

2015-01-01

A very high-temperature reactor (VHTR) has been studied among generation IV nuclear power plants owing to its many advantages such as high-electric efficiency and massive hydrogen production. The material used for the heat exchanger should sustain structural integrity for its life even though the material is exposed to a harsh environment at 1223 K (950 °C) in an impure helium coolant. Therefore, an enhancement of the material performance at high temperature gives a margin in determining the operating temperature and life time. This work is an effort to find an optimum combination of alloying elements and processing parameters to improve the material performance. The tensile property and microstructure for nickel-based alloys fabricated in a laboratory were evaluated as a function of the heat treatment, cold working, and grain boundary strengthener using a tension test at 1223 K (950 °C), scanning electron microscopy, and transmission electron microscopy. Elongation to rupture was increased by additional heat treatment and cold working, followed by additional heat treatment in the temperature range from 1293 K to 1383 K (1020 °C to 1110 °C) implying that the intergranular carbide contributes to grain boundary strengthening. The temperature at which the grain boundary is improved by carbide decoration was higher for a cold-worked specimen, which was described by the difference in carbide stability and carbide formation kinetics between no cold-worked and cold-worked specimens. Zr and Hf played a scavenging effect of harmful elements causing an increase in ductility.

Ab initio calculations for industrial materials engineering: successes and challenges.

PubMed

Wimmer, Erich; Najafabadi, Reza; Young, George A; Ballard, Jake D; Angeliu, Thomas M; Vollmer, James; Chambers, James J; Niimi, Hiroaki; Shaw, Judy B; Freeman, Clive; Christensen, Mikael; Wolf, Walter; Saxe, Paul

2010-09-29

Computational materials science based on ab initio calculations has become an important partner to experiment. This is demonstrated here for the effect of impurities and alloying elements on the strength of a Zr twist grain boundary, the dissociative adsorption and diffusion of iodine on a zirconium surface, the diffusion of oxygen atoms in a Ni twist grain boundary and in bulk Ni, and the dependence of the work function of a TiN-HfO(2) junction on the replacement of N by O atoms. In all of these cases, computations provide atomic-scale understanding as well as quantitative materials property data of value to industrial research and development. There are two key challenges in applying ab initio calculations, namely a higher accuracy in the electronic energy and the efficient exploration of large parts of the configurational space. While progress in these areas is fueled by advances in computer hardware, innovative theoretical concepts combined with systematic large-scale computations will be needed to realize the full potential of ab initio calculations for industrial applications.

Analysis of Slip Activity and Deformation Modes in Tension and Tension-Creep Tests of Cast Mg-10Gd-3Y-0.5Zr (Wt Pct) at Elevated Temperatures Using In Situ SEM Experiments

NASA Astrophysics Data System (ADS)

Wang, Huan; Boehlert, Carl J.; Wang, Qudong; Yin, Dongdi; Ding, Wenjiang

2016-05-01

The tension and tension-creep deformation behavior at elevated temperatures of a cast Mg-10Gd-3Y-0.5Zr (wt pct, GW103) alloy was investigated using in situ scanning electron microscopy. The tests were performed at temperatures ranging from 473 K to 598 K (200 °C to 325 °C). The active slip systems were identified using an EBSD-based slip trace analysis methodology. The results showed that for all of the tests, basal slip was the most likely system to be activated, and non-basal slip was activated to some extent depending on the temperature. No twinning was observed. For the tension tests, non-basal slip consisted of ~35 pct of the deformation modes at low temperatures (473 K and 523 K (200 °C and 250 °C)), while non-basal slip accounted for 12 and 7 pct of the deformation modes at high temperatures (573 K and 598 K (300 °C and 325 °C)), respectively. For the tension-creep tests, non-basal slip accounted for 31 pct of the total slip systems at low temperatures, while this value decreased to 10 to 16 pct at high temperatures. For a given temperature, the relative activity for prismatic slip in the tension-creep tests was slightly greater than that for the tension tests, while the activity for pyramidal slip was lower. Slip-transfer in neighboring grains was observed for the low-temperature tests. Intergranular cracking was the main cracking mode, while some intragranular cracks were observed for the tension-creep tests at high temperature and low stress. Grain boundary ledges were prevalently observed for both the tension and tension-creep tests at high temperatures, which suggests that besides dislocation slip, grain boundary sliding also contributed to the deformation.

Trace element composition of rutile and Zr-in-rutile thermometry in meta-ophiolitic rocks from the Kazdağ Massif, NW Turkey

NASA Astrophysics Data System (ADS)

Şengün, Fırat; Zack, Thomas

2016-08-01

In northwest Turkey, ophiolitic meta-gabbros are exposed on the Kazdağ Massif located in the southern part of the Biga Peninsula. Trace element composition of rutile and Zr-in-rutile temperatures were determined for meta-gabbros from the Kazdağ Massif. The Zr content of all rutiles range from 176 to 428 ppm and rutile grains usually have a homogeneous Zr distribution. The rutile grains from studied samples in the Kazdağ Massif are dominated by subchondritic Nb/Ta (11-19) and Zr/Hf ratios (20-33). Nb/Ta and Zr/Hf show positive correlation, which is probably produced by silicate fractionation. The Nb/Ta and Zr/Hf ratios increase with a decrease in Ta and Hf contents. The core of rutile grains are generally characterized by low Nb/Ta ratios of 17-18 whereas the rims exhibit relatively high Nb/Ta ratios of 19-23. Trace element analyses in rutile suggest that these rutile grains were grown from metamorphic fluids. The P-T conditions of meta-gabbros were estimated by both Fe-Mg exchange and Zr-in-rutile thermometers, as well as by the Grt-Hb-Plg-Q geothermobarometer. The temperature range of 639 to 662 °C calculated at 9 kbar using the Zr-in-rutile thermometer is comparable with temperature estimates of the Fe-Mg exchange thermometer, which records amphibolite-facies metamorphism of intermediate P-T conditions. The P-T conditions of meta-ophiolitic rocks suggest that they occur as a different separate higher-pressure tectonic slice in the Kazdağ metamorphic sequence. Amphibolite-facies metamorphism resulted from northward subduction of the İzmir-Ankara branch of the Neo-Tethyan Ocean under the Sakarya Zone. Metamorphism was followed by internal imbrication of the Kazdağ metamorphic sequence resulting from southerly directed compression during the collision.

Grain Boundary Engineering of Lithium-Ion-Conducting Lithium Lanthanum Titanate for Lithium-Air Batteries

DTIC Science & Technology

2015-01-01

Tojo T, Sakurai Y. Synthesis and lithium - ion conductivity for perovskite-type Li3/8Sr7/16Ta3/4Zr1/4O3 solid electrolyte by powder-bed sintering...battery performance is limited by the electrolytic membrane, which needs high Li-ionic conductivity. Lithium lanthanum titanate (Li3xLa(2/3)-xTiO3, or...of the A-site ions and lithium ion conductivity in the perovskite solid solution La0.67-xLi3xTiO3 (x=0.11). Journal of Solid State Ionics. 1999;121

On the use of copper-based substrates for YBCO coated conductors

NASA Astrophysics Data System (ADS)

Vannozzi, A.; Fabbri, F.; Augieri, A.; Angrisani Armenio, A.; Galluzzi, V.; Mancini, A.; Rizzo, F.; Rufoloni, A.; Padilla, J. A.; Xuriguera, E.; De Felicis, D.; Bemporad, E.; Celentano, G.

2014-05-01

It is well known that the recrystallization texture of heavily cold-rolled pure copper is almost completely cubic. However, one of the main drawbacks concerning the use of pure copper cube-textured substrates for YBCO coated conductor is the reduced secondary recrystallization temperature. The onset of secondary recrystallization (i.e., the occurrence of abnormal grains with unpredictable orientation) in pure copper substrate was observed within the typical temperature range required for buffer layer and YBCO processing (600-850 °C). To avoid the formation of abnormal grains the effect of both grain size adjustment (GSA) and recrystallization annealing was analyzed. The combined use of a small initial grain size and a recrystallization two-step annealing (TSA) drastically reduced the presence of abnormal grains in pure copper tapes. Another way to overcome the limitation imposed by the formation of abnormal grains is to deposit a buffer layer at temperatures where secondary recrystallization does not occur. For example, La2Zr2O7 (LZO) film with a high degree of epitaxy was grown by metal-organic decomposition (MOD) at 1000 °C on pure copper substrate. In several samples the substrate underwent secondary recrystallization. Our experiments indicate that the motion of grain boundaries occurring during secondary recrystallization process does not affect the quality of LZO film.

Analysis techniques for tracer studies of oxidation. M. S. Thesis Final Report

NASA Technical Reports Server (NTRS)

Basu, S. N.

1984-01-01

Analysis techniques to obtain quantitative diffusion data from tracer concentration profiles were developed. Mass balance ideas were applied to determine the mechanism of oxide growth and to separate the fraction of inward and outward growth of oxide scales. The process of inward oxygen diffusion with exchange was theoretically modelled and the effect of lattice diffusivity, grain boundary diffusivity and grain size on the tracer concentration profile was studied. The development of the tracer concentration profile in a growing oxide scale was simulated. The double oxidation technique was applied to a FeCrAl-Zr alloy using 0-18 as a tracer. SIMS was used to obtain the tracer concentration profile. The formation of lacey oxide on the alloy was discussed. Careful consideration was given to the quality of data required to obtain quantitative information.

The Relationship between Polyamines and Hormones in the Regulation of Wheat Grain Filling

PubMed Central

Liu, Yang; Gu, Dandan; Wu, Wei; Wen, Xiaoxia; Liao, Yuncheng

2013-01-01

The grain weight of wheat is strongly influenced by filling. Polyamines (PA) are involved in regulating plant growth. However, the effects of PA on wheat grain filling and its mechanism of action are unclear. The objective of the present study was to investigate the relationship between PAs and hormones in the regulation of wheat grain filling. Three PAs, spermidine (Spd), spermine (Spm), and putrescine (Put), were exogenously applied, and the grain filling characteristics and changes in endogenous PA and hormones, i.e., indole-3-acetic acid (IAA), zeatin (Z) + zeatin riboside (ZR), abscisic acid (ABA), ethylene (ETH) and gibberellin 1+4 (GAs), were quantified during wheat grain filling. Exogenous applications of Spd and Spm significantly increased the grain filling rate and weight, but exogenous Put had no significant effects on these measures. Exogenous Spd and Spm significantly increased the endogenous Spd, Spm, Z+ZR, ABA, and IAA contents and significantly decreased ETH evolution in grains. The endogenous Spd, Spm and Z+ZR contents were positively and significantly correlated with the grain filling rate and weight of wheat, and the endogenous ETH evolution was negatively and significantly correlated with the wheat grain filling rate and weight. Based upon these results, we concluded that PAs were involved in the balance of hormones that regulated the grain filling of wheat. PMID:24205154

Polarity of translation boundaries in antiferroelectric PbZrO{sub 3}

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wei, Xian-Kui, E-mail: xiankui.wei@epfl.ch; Peter Grünberg Institute and Ernst Ruska Center for Microscopy and Spectroscopy with Electrons, Research Center Jülich, 52425 Jülich; Jia, Chun-Lin

2015-02-15

Graphical abstract: Strain-free rigid model and aberration-corrected transmission electron microscopes are used to investigate the polarity of translation boundaries in antiferroelectric PbZrO{sub 3}. - Highlights: • Domain boundaries in antiferroelectric PbZrO{sub 3} show polar and antipolar property. • The antiphase boundary can split into “sub-domains”. • Polarization reversal possibly exists inside the translation boundaries. • Thermal treatment can alter morphology and density of the translation boundaries. - Abstract: The polarity of translation boundaries (TBs) in antiferroelectric PbZrO{sub 3} is investigated. We show that previous experimentally reported polar property of R{sub III-1} type TB can be well approximated by a strain-freemore » rigid model. Based on this, the modeling investigation suggests that there are two additional polar TBs, three antipolar-like TBs and one antipolar antiphase boundary. High-resolution scanning-transmission-electron-microscopy study reveals that the straight R{sub III-1} type TB can split into “sub-domains” with possible polarization reversal, suggesting the occurrence of ferroic orders at the TBs. In addition, dependence of morphology and density of the TBs on thermal treatments is discussed according to our results.« less

Effects of Cr-N-ZrO 2 seed layer formed on glass substrates for longitudinal recording media

NASA Astrophysics Data System (ADS)

Suzuki, Hiroyuki; Djayaprawira, David D.; Takahashi, Yoshio; Ishikawa, Akira; Ono, Toshinori; Yahisa, Yotsuo

1999-03-01

Effects of Cr-N-ZrO 2 seed layer deposited on glass substrates before the deposition of C/Co-Cr-Pt/Cr-Ti layers for longitudinal recording media have been investigated. The product of v and Is, the activation volume and the saturation magnetization per unit volume, media noise Nd and S0/ Nd, which is the half value of peak-to-peak output voltage of an isolated pulse over Nd at 11.8 kFC/mm, are evaluated. We find that vIs is decreased by adding N and ZrO 2 to Cr seed layer. Nd is reduced as vIs decreases by adding nitrogen to the Cr seed layer. This is mainly due to the decreased grain sizes of both Cr-Ti underlayer and Co-Cr-Pt magnetic layer. The Nd is further reduced by the addition of ZrO 2 to the Cr-N seed layer. Highest S0/ Nd is achieved for the media with Cr-N-ZrO 2 seed layer. On the other hand, the media with Cr-ZrO 2 seed layer deposited without nitrogen show the higher Nd. Therefore the decrease of the grain size by addition of nitrogen into Ar is essential to reduce Nd, and the ZrO 2 addition to the Cr-N seed layer seems to enhance the effect of grain size reduction by nitrogen addition.

Thermomechanical processing of aluminum micro-alloyed with Sc, Zr, Ti, B, and C

NASA Astrophysics Data System (ADS)

McNamara, Cameron T.

Critical exploration of the minimalistic high strength low alloy aluminum (HSLA-Al) paradigm is necessary for the continued development of advanced aluminum alloys. In this study, scandium (Sc) and zirconium (Zr) are examined as the main precipitation strengthening additions, while magnesium (Mg) is added to probe the synergistic effects of solution and precipitation hardening, as well as the grain refinement during solidification afforded by a moderate growth restriction factor. Further, pathways of recrystallization are explored in several potential HSLA-Al syste =ms sans Sc. Aluminum-titanium-boron (Al-Ti-B) and aluminum-titanium-carbon (Al-Ti-C) grain refining master alloys are added to a series of Al-Zr alloys to examine both the reported Zr poisoning effect on grain size reduction and the impact on recrystallization resistance through the use of electron backscattered diffraction (EBSD) imaging. Results include an analysis of active strengthening mechanisms and advisement for both constitution and thermomechanical processing of HSLA-Al alloys for wrought or near-net shape cast components. The mechanisms of recrystallization are discussed for alloys which contain a bimodal distribution of particles, some of which act as nucleation sites for grain formation during annealing and others which restrict the growth of the newly formed grains.

Microstructural Evolution of Al2O3-ZrO2 (Y2O3) Composites and its Correlation with Toughness

NASA Astrophysics Data System (ADS)

Kim, Hee Seung; Seo, Mi Young; Kim, Ik Jin

2008-02-01

The microstructure of zirconia (ZrO2) toughened alumina (Al2O3) ceramics was carefully controlled so as to obtain dense and fine-grained ceramics, thereby improving the properties and reliability of the ceramics for capillary applications in semiconductor bonding technology. Al2O3-ZrO2(Y2O3) composite was produced via Ceramic Injection Molding (CIM) technology, followed by Sinter-HIP process. Room temperature strength, hardness, Young's modulus, thermal expansion coefficient and toughness were determined, as well as surface strengthening induced by the fine grained homogenous microstructure and the thermal treatment. The changes in alumina/zirconia grain size, sintering condition and HIP treatment were found to be correlated.

Extraordinary high ductility/strength of the interface designed bulk W-ZrC alloy plate at relatively low temperature

PubMed Central

Xie, Z. M.; Liu, R.; Miao, S.; Yang, X. D.; Zhang, T.; Wang, X. P.; Fang, Q. F.; Liu, C. S.; Luo, G. N.; Lian, Y. Y.; Liu, X.

2015-01-01

The refractory tungsten alloys with high ductility/strength/plasticity are highly desirable for a wide range of critical applications. Here we report an interface design strategy that achieves 8.5 mm thick W-0.5 wt. %ZrC alloy plates with a flexural strength of 2.5 GPa and a strain of 3% at room temperature (RT) and ductile-to-brittle transition temperature of about 100 °C. The tensile strength is about 991 MPa at RT and 582 MPa at 500 °C, as well as total elongation is about 1.1% at RT and as large as 41% at 500 °C, respectively. In addition, the W-ZrC alloy plate can sustain 3.3 MJ/m2 thermal load without any cracks. This processing route offers the special coherent interfaces of grain/phase boundaries (GB/PBs) and the diminishing O impurity at GBs, which significantly strengthens GB/PBs and thereby enhances the ductility/strength/plasticity of W alloy. The design thought can be used in the future to prepare new alloys with higher ductility/strength. PMID:26531172

The oxidation of Ni-rich Ni-Al intermetallics

NASA Technical Reports Server (NTRS)

Doychak, Joseph; Smialek, James L.; Barrett, Charles A.

1988-01-01

The oxidation of Ni-Al intermetallic alloys in the beta-NiAl phase field and in the two phase beta-NiAl/gamma'-Ni3Al phase field has been studied between 1000 and 1400 C. The stoichiometric beta-NiAl alloy doped with Zr was superior to other alloy compositions under cyclic and isothermal oxidation. The isothermal growth rates did not increase monotonically as the alloy Al content was decreased. The characteristically ridged alpha-Al2O3 scale morphology, consisting of cells of thin, textured oxide with thick growth ridges at cell boundaries, forms on oxidized beta-NiAl alloys. The correlation of scale features with isothermal growth rates indicates a predominant grain boundary diffusion growth mechanism. The 1200 C cyclic oxidation resistance decreases near the lower end of the beta-NiAl phase field.

Transformations to granular zircon revealed: Twinning, reidite, and ZrO2 in shocked zircon from Meteor Crater (Arizona, USA)

USGS Publications Warehouse

Cavosie, Aaron; Timms, Nicholas E.; Erickson, Timmons M.; Hagerty, Justin J.; Hörz, Friedrich

2016-01-01

Granular zircon in impact environments has long been recognized but remains poorly understood due to lack of experimental data to identify mechanisms involved in its genesis. Meteor Crater in Arizona (United States) contains abundant evidence of shock metamorphism, including shocked quartz, the high pressure polymorphs coesite and stishovite, diaplectic SiO2 glass, and lechatelierite (fused SiO2). Here we report the presence of granular zircon, a new shocked mineral discovery at Meteor Crater, that preserve critical orientation evidence of specific transformations that occurred during its formation at extreme impact conditions. The zircon grains occur as aggregates of sub-µm neoblasts in highly shocked Coconino Formation Sandstone (CFS) comprised of lechatelierite. Electron backscatter diffraction shows that each grain consists of multiple domains, some with boundaries disoriented by 65°, a known {112} shock-twin orientation. Other domains have crystallographic c-axes in alignment with {110} of neighboring domains, consistent with the former presence of the high pressure ZrSiO4 polymorph reidite. Additionally, nearly all zircon preserve ZrO2 + SiO2, providing evidence of partial dissociation. The genesis of CFS granular zircon started with detrital zircon that experienced shock-twinning and reidite formation from 20 to 30 GPa, ultimately yielding a phase that retained crystallographic memory; this phase subsequently recrystallized to systematically oriented zircon neoblasts, and in some areas partially dissociated to ZrO2. The lechatelierite matrix, experimentally constrained to form at >2000 °C, provided an ultra high-temperature environment for zircon dissociation (~1670 °C) and neoblast formation. The capacity of granular zircon to preserve a cumulative P-T record has not been recognized previously, and provides a new method for retrieving histories of impact-related mineral transformations in the crust at conditions far beyond which most rocks melt.

Surface diffusivity measurements on 8mol.% yttrium oxide-zirconia bicrystals via grain boundary grooving experiments

NASA Astrophysics Data System (ADS)

Nassirou, Maissarath

Thermal grooving at grain boundaries (GBs) is a capillary-driven evolution of surface topography in the region where the grain boundary emerges at a free surface. The study of these topographic changes can provide insight into surface energetics, and in our particular case, the measurement of surface diffusivity. We have measured the surface diffusion coefficient of 8mol% Y 2O3-ZrO2 by studying the formation of thermal grooves. We studied a total of five bicrystals, with well defined orientation relationships; random [110] -60°, random [001] -30°, Sigma13 [001]/{510}, Sigma13 [001]/{320}, Sigma5 [001]/{210}. Our calculations employed the Herring relation (1951), in which the variation in the chemical potential is related to changes in topography. The samples were annealed at 1300°C and 1400°C for various period of time. Atomic Force Microscopy was used to determine the exact geometry of the thermal grooves. A first approach consisted of estimating the diffusion coefficient by using Mullins' equation. yx=0= dsDs1/ 4gb2g s12G 5/4( WkTgs) 1/4t 1/4 Where y(x =0) is the groove depth at the GB triple junction, O is the atomic volume, gs is the surface tension, gb is the grain boundary surface energy, ds is the thickness of the diffusion layer, t is the annealing time, and Ds is the surface diffusion coefficient. In Mullins' derivation, the atomic structure of the surface was ignored and it was assumed that the surface energy is independent of crystallographic orientation. In the case of zirconia, the surface energy is anisotropic. We will describe in this work a new approach to measuring surface diffusivity which accounts for the surface energy anisotropy. The study of these bicrystals will emphasize the effect of grain boundary structure on the surface diffusion coefficient, and it is for that purpose that we selected bicrystals with different tilt axes and angles. The results obtained using the equation set we have developed will be compared to those obtained by Mullins, and we show that the anisotropic groove evolution, even when perfectly symmetrical, is much slower than the corresponding isotropic case.

Properties of nanostructured undoped ZrO{sub 2} thin film electrolytes by plasma enhanced atomic layer deposition for thin film solid oxide fuel cells

DOE Office of Scientific and Technical Information (OSTI.GOV)

Cho, Gu Young; Noh, Seungtak; Lee, Yoon Ho

2016-01-15

Nanostructured ZrO{sub 2} thin films were prepared by thermal atomic layer deposition (ALD) and by plasma-enhanced atomic layer deposition (PEALD). The effects of the deposition conditions of temperature, reactant, plasma power, and duration upon the physical and chemical properties of ZrO{sub 2} films were investigated. The ZrO{sub 2} films by PEALD were polycrystalline and had low contamination, rough surfaces, and relatively large grains. Increasing the plasma power and duration led to a clear polycrystalline structure with relatively large grains due to the additional energy imparted by the plasma. After characterization, the films were incorporated as electrolytes in thin film solidmore » oxide fuel cells, and the performance was measured at 500 °C. Despite similar structure and cathode morphology of the cells studied, the thin film solid oxide fuel cell with the ZrO{sub 2} thin film electrolyte by the thermal ALD at 250 °C exhibited the highest power density (38 mW/cm{sup 2}) because of the lowest average grain size at cathode/electrolyte interface.« less

Microstructural Evolution of Nanocrystalline ZrO2 in a Fe Matrix During High-Temperature Exposure

NASA Astrophysics Data System (ADS)

Raghavendra, K. G.; Dasgupta, Arup; Athreya, C. N.; Jayasankar, K.; Saroja, S.; Subramanya Sarma, V.

2018-06-01

The current study examines the evolution of nanocrystallites of ZrO2 with time and temperature in a Fe-ZrO2 composite. The crystallite sizes were determined through X-ray peak broadening analysis by the Williamson-Hall method together with dark field transmission electron microscopy. The ZrO2 crystallites were found to be stable and retained their sizes at 973 K and 1073 K for hold durations up to 600 minutes. On the other hand, the crystallites were seen to grow at 1173 K and reached up to 200 nm for a hold time of 600 minutes. The Ostwald ripening model was adopted to understand crystallite growth while a dislocation-driven pipe diffusion was adopted for understanding the kinetics of grain growth. The activation energy of grain growth was calculated as 379 kJ mol-1. The modeled and experimentally calculated size evolutions with time and temperature were shown to be in good agreement with each other. A detailed discussion on the kinetics and activation energy of grain growth of ZrO2 crystallites in a Fe matrix is presented in this manuscript.

Effects of Co contents on the microstructures and properties of the electrodeposited NiCo–Zr composite coatings

DOE Office of Scientific and Technical Information (OSTI.GOV)

Cai, Fei; Jiang, Chuanhai, E-mail: chuanhaijiang1963@163.com; Zhao, Yuantao

2015-05-15

Highlights: • The novel NiCo–Zr coatings were prepared by electro-deposition. • Surface morphology, crystal structure, grain size and microstrain were examined. • Texture, residual stress and corrosion resistance were investigated. • Addition of Co increased the hardness and corrosion resistance of the coatings. - Abstract: In this study, the NiCo–Zr composite coatings were prepared from the electrolytes with different Co{sup 2+} concentrations by electrodeposition method. The effects of Co contents on the crystal structure, surface morphology, grain size, microstrain and residual stress were examined by X-ray diffractometer (XRD), field emission scanning electron microscopy (FESEM), Energy dispersive X-ray spectroscopy (EDX) andmore » atomic force microscope (AFM). The corrosion resistance of the composite coatings was also examined by the potentiodynamic polarization and electrochemical impedance (EIS) measurements. The results revealed that the crystal structures of the coatings were dependent on the Co contents and addition of Co content of 58 wt% resulted in the formation of hexagonal (hcp) Co. The increasing Co contents in the NiCo–Zr composite coatings resulted in the smoother and more compact surface, decreased the grain size and increased the microstrain. The micro-hardness and residual stress also increased with increasing Co contents. The addition of Co increased the corrosion resistance of the NiCo–Zr composite coatings compared with the Ni–Zr coating while the corrosion resistance of the NiCo–Zr composite coatings decreased as the Co contents increased.« less

Examination of Multiphase (Zr,Ti)(V,Cr,Mn,Ni)2 Ni-MH Electrode Alloys: Part II. Solid-State Transformation of the Interdendritic B2 Phase

NASA Astrophysics Data System (ADS)

Bendersky, L. A.; Wang, K.; Boettinger, W. J.; Newbury, D. E.; Young, K.; Chao, B.

2010-08-01

Solidification microstructure of multicomponent (Zr,Ti)-Ni-(V,Cr,Mn,Co) alloys intended for use as negative electrodes in Ni-metal hydride (Ni-MH) batteries was studied in Part I of this series of articles. Part II of the series examines the complex internal structure of the interdendritic grains formed by solid-state transformation and believed to play an important role in the electrochemical charge/discharge characteristics of the overall alloy composition. By studying one alloy, Zr21Ti12.5V10Cr5.5Mn5.1Co5.0Ni40.2Al0.5Sn0.3, it is shown that the interdendritic grains solidify as a B2 (Ti,Zr)44(Ni,TM)56 phase, and then undergo transformation to Zr7Ni10-type, Zr9Ni11-type, and martensitic phases. The transformations obey orientation relationships between the high-temperature B2 phase and the low-temperature Zr-Ni-type intermetallics, and consequently lead to a multivariant structure. The major orientation relationship for the orthorhombic Zr7Ni10 type is [011]Zr7Ni10//[001]B2; (100)Zr7Ni10//(100)B2. The orientation relationship for the tetragonal Zr9Ni11 type is [001]Zr9Ni11//[001]B2; (130)Zr9Ni11//(100)B2. Binary Ni-Zr and ternary Ti-Ni-Zr phase diagrams were used to rationalize the formation of the observed domain structure.

Processing - microstructure relationships of chemically vapor deposited zirconia fiber coating for environmentally durable silicon carbide/silicon carbide composites

NASA Astrophysics Data System (ADS)

Lee, Jinil

In SiC/SiC ceramic matrix composites, toughness is obtained by adding a fiber coating which provides a weak interface for crack deflection and debonding between the fiber and the matrix. However, the most commonly used fiber coatings, carbon and boron nitride, are unstable in oxidative environments. In the present study, the feasibility of using a chemically vapor deposited zirconia (CVD-ZrO 2) fiber coating as an oxidation-resistant interphase for SiC/SiC composites was investigated. The feasibility of the CVD-ZrO2 coating as a useful interphase for SiC/SiC composites was investigated with emphasis on developing critical processing-microstructure relationships. A study of morphological evolution in the CVD-ZrO2 coating suggested that a size-controlled displacive phase transformation from tetragonal ZrO2 (t-ZrO2) to monoclinic ZrO2 (m-ZrO2) was the key mechanism responsible for the weak interface behavior exhibited by the ZrO2 coating. The pre-delamination occurred as a result of (i) continuous formation of t-ZrO2 nuclei on the deposition surface; (ii) martensitic transformation of the tetragonal phase to a monoclinic phase upon reaching a critical grain size; and (iii) development of significant compressive hoop stresses due to the volume dilation associated with the transformation. We also discovered that low oxygen partial pressure in the CVD reactor was required for the nucleation of t-ZrO2 and was ultimately responsible for the delamination behavior. The effects of oxygen partial pressure on the nucleation behavior of the CVD-ZrO2 coating was systematically studied by intentionally adding the controlled amount of O2 into the CVD chamber. Characterization results suggested that the number density of t-ZrO2 nuclei apparently decreased with increasing the oxygen partial pressure from 0.004 to 1.6 Pa. Also, the coating layer became more columnar and contained larger m-ZrO2 grains. The observed relationships between the oxygen partial pressure and the morphological characteristics of the ZrO 2 coating were explained in the context of the grain size and oxygen deficiency effects which have been previously reported to cause the stabilization of the t-ZrO2 phase in bulk ZrO2 specimens.

About properties of ZrO2 thermal protective coatings obtained from spherical powder mixtures

NASA Astrophysics Data System (ADS)

Berdnik, O. B.; Tsareva, I. N.; Tarasenko, Yu P.

2017-05-01

It is developed the technology of high-energy plasma spraying of the zirconium dioxide (ZrO2) thermal protective coating on the basis of ZrO2 tetragonal and cubic phases with the spheroidal grain shape and the columnar substructure, with the total porosity P = 4 %, the hardness HV = 12 GPa, the roughness parameter R a ˜ 6 μm, the thickness 0.3-3 mm. As a sublayer it is used the heat-resistant coating of “Ni-Co-Cr-Al-Y” system with an intermetallic phase composition and the layered microstructure of the grains.

Ultra high temperature ceramics for hypersonic vehicle applications.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tandon, Rajan; Dumm, Hans Peter; Corral, Erica L.

2006-01-01

HfB{sub 2} and ZrB{sub 2} are of interest for thermal protection materials because of favorable thermal stability, mechanical properties, and oxidation resistance. We have made dense diboride ceramics with 2 to 20 % SiC by hot pressing at 2000 C and 5000 psi. High-resolution transmission electron microscopy (TEM) shows very thin grain boundary phases that suggest liquid phase sintering. Fracture toughness measurements give RT values of 4 to 6 MPam{sup 1/2}. Four-pt flexure strengths measured in air up to 1450 C were as high as 450-500 MPa. Thermal diffusivities were measured to 2000 C for ZrB{sub 2} and HfB{sub 2}more » ceramics with SiC contents from 2 to 20%. Thermal conductivities were calculated from thermal diffusivities and measured heat capacities. Thermal diffusivities were modeled using different two-phase composite models. These materials exhibit excellent high temperature properties and are attractive for further development for thermal protection systems.« less

Effect of solution treatment on the fatigue behavior of an as-forged Mg-Zn-Y-Zr alloy

NASA Astrophysics Data System (ADS)

Wang, S. D.; Xu, D. K.; Wang, B. J.; Han, E. H.; Dong, C.

2016-04-01

Through investigating and comparing the fatigue behavior of an as-forged Mg-6.7Zn-1.3Y-0.6Zr (wt.%) alloy before and after solid solution treatment (T4) in laboratory air, the effect of T4 treatment on fatigue crack initiation was disclosed. S-N curves illustrated that the fatigue strength of as-forged samples was 110 MPa, whereas the fatigue strength of T4 samples was only 80 MPa. Observations to fracture surfaces demonstrated that for as-forged samples, fatigue crack initiation sites were covered with a layer of oxide film. However, due to the coarse grain structure and the dissolution of MgZn2 precipitates, the activation and accumulation of {10-12} twins in T4 samples were much easier, resulting in the preferential fatigue crack initiation at cracked twin boundaries (TBs). Surface characterization demonstrated that TB cracking was mainly ascribed to the incompatible plastic deformation in the twinned area and nearby α-Mg matrix.

Development of exothermically cast single-crystal Mar-M 247 and derivative alloys

NASA Technical Reports Server (NTRS)

Strangman, T. E.; Hoppin, G. S., III; Phipps, C. M.; Harris, K.; Schwer, R. E.

1980-01-01

A low-cost, exothermic directional-solidification (DS) process was developed to produce single-crystal (SC) Mar-M 247 high-pressure turbine blades. Stress-rupture data indicated that SC Mar-M 247 provides only marginal improvements in longitudinal strength relative to the columnar grained DS material. Removal of grain boundary strengthening elements (B, C, Zr, Hf) from the Mar-M 247 composition (which are also melting point depressants) permitted the alloy to be solutioned at significantly higher temperatures. An order of magnitude improvement in rupture life relative to SC Mar-M 247 was observed for several derivative alloys at 103.5 MPa (15 KSI) and 1093 C. Rupture lives of the modified SC alloys were significantly affected by both alloy purity and heat treatment. Critical aspects of vacuum induction refining, exothermic casting technology, alloy development and heat treatment, which contributed to this new class of turbine blades, are reviewed

Microstructural characterization of a Zr-Ti-Ni-Mn-V-Cr based AB 2-type battery alloy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Shi, Zhan

1999-01-01

Transmission Electron Microscopy (TEM), combined with X-ray Diffraction (XRD) and Scanning Electron Microscopy (SEM) was employed to investigate a proprietary and multicomponent AB 2 type Nickel-Metal Hydride (Ni-MH) battery alloy. This material was prepared by High Pressure Gas Atomization (HPGA) and examined in both the as-atomized and heat treated condition. TEM examination showed a heavily faulted dendritic growth structure in as-atomized powder. Selected Area Diffraction (SAD) showed that this region consisted of both a cubic C15 structure with lattice constant a=7.03 and a hexagonal C14 structure with lattice parameter a=4.97 Å, c=8.11 Å. The Orientation Relationship (OR) between the C14 and C15 structures was determined to be (111)[1more » $$\\bar{1}$$0] C15//(0001)[11$$\\bar{2}$$0] C14. An interdendritic phase possessing the C14 structure was also seen. There was also a very fine grain region consisting of the C14 structure. Upon heat treatment, the faulted structure became more defined and appeared as intercalation layers within the grains. Spherical particles rich in Zr and Ni appeared scattered at the grain boundaries instead of the C14 interdendritic phase. The polycrystalline region also changed to a mixture of C14 and C15 structures. These results as well as phase stability of the C15 and C14 structures based on a consideration of atomic size factor and the average electron concentration are discussed.« less

CuCrZr alloy microstructure and mechanical properties after hot isostatic pressing bonding cycles

NASA Astrophysics Data System (ADS)

Frayssines, P.-E.; Gentzbittel, J.-M.; Guilloud, A.; Bucci, P.; Soreau, T.; Francois, N.; Primaux, F.; Heikkinen, S.; Zacchia, F.; Eaton, R.; Barabash, V.; Mitteau, R.

2014-04-01

ITER first wall (FW) panels are a layered structure made of the three following materials: 316L(N) austenitic stainless steel, CuCrZr alloy and beryllium. Two hot isostatic pressing (HIP) cycles are included in the reference fabrication route to bond these materials together for the normal heat flux design supplied by the European Union (EU). This reference fabrication route ensures sufficiently good mechanical properties for the materials and joints, which fulfil the ITER mechanical specifications, but often results in a coarse grain size for the CuCrZr alloy, which is not favourable, especially, for the thermal creep properties of the FW panels. To limit the abnormal grain growth of CuCrZr and make the ITER FW fabrication route more reliable, a study began in 2010 in the EU in the frame of an ITER task agreement. Two material fabrication approaches have been investigated. The first one was dedicated to the fabrication of solid CuCrZr alloy in close collaboration with an industrial copper alloys manufacturer. The second approach investigated was the manufacturing of CuCrZr alloy using the powder metallurgy (PM) route and HIP consolidation. This paper presents the main mechanical and microstructural results associated with the two CuCrZr approaches mentioned above. The mechanical properties of solid CuCrZr, PM CuCrZr and joints (solid CuCrZr/solid CuCrZr and solid CuCrZr/316L(N) and PM CuCrZr/316L(N)) are also presented.

On the interaction of solutes with grain boundaries

DOE PAGES

Dingreville, Remi Philippe Michel; Berbenni, Stephane

2015-11-01

Solute segregation to grain boundaries is considered by modeling solute atoms as misfitting inclusions within a disclination structural unit model describing the grain boundary structure and its intrinsic stress field. The solute distribution around grain boundaries is described through Fermi–Dirac statistics of site occupancy. The susceptibility of hydrogen segregation to symmetric tilt grain boundaries is discussed in terms of the misorientation angle, the defect type characteristics at the grain boundary, temperature, and the prescribed bulk hydrogen fraction of occupied sites. Through this formalism, it is found that hydrogen trapping on grain boundaries clearly correlates with the grain boundary structure (i.e.more » type of structural unit composing the grain boundary), and the associated grain boundary misorientation. Specifically, for symmetric tilt grain boundaries about the [001] axis, grain boundaries composed of both B and C structural units show a lower segregation susceptibility than other grain boundaries. A direct correlation between the segregation susceptibility and the intrinsic net defect density is provided through the Frank–Bilby formalism. Moreover, the present formulation could prove to be a simple and useful model to identify classes of grain boundaries relevant to grain boundary engineering.« less

On the interaction of solutes with grain boundaries

DOE Office of Scientific and Technical Information (OSTI.GOV)

Dingreville, Remi Philippe Michel; Berbenni, Stephane

Solute segregation to grain boundaries is considered by modeling solute atoms as misfitting inclusions within a disclination structural unit model describing the grain boundary structure and its intrinsic stress field. The solute distribution around grain boundaries is described through Fermi–Dirac statistics of site occupancy. The susceptibility of hydrogen segregation to symmetric tilt grain boundaries is discussed in terms of the misorientation angle, the defect type characteristics at the grain boundary, temperature, and the prescribed bulk hydrogen fraction of occupied sites. Through this formalism, it is found that hydrogen trapping on grain boundaries clearly correlates with the grain boundary structure (i.e.more » type of structural unit composing the grain boundary), and the associated grain boundary misorientation. Specifically, for symmetric tilt grain boundaries about the [001] axis, grain boundaries composed of both B and C structural units show a lower segregation susceptibility than other grain boundaries. A direct correlation between the segregation susceptibility and the intrinsic net defect density is provided through the Frank–Bilby formalism. Moreover, the present formulation could prove to be a simple and useful model to identify classes of grain boundaries relevant to grain boundary engineering.« less

Influence of Sc on microstructure and mechanical properties of Al-Si-Mg-Cu-Zr alloy

NASA Astrophysics Data System (ADS)

Li, Yukun; Du, Xiaodong; Zhang, Ya; Zhang, Zhen; Fu, Junwei; Zhou, Shi'ang; Wu, Yucheng

2018-02-01

In the present study, the effects of Mg, Cu, Sc and Zr combined additions on the microstructure and mechanical properties of hypoeutectic Al-Si cast alloy were systematically investigated. Characterization techniques such as optical microscopy (OM), scanning electron microscope (SEM), energy dispersive spectrometer (EDS), electron back-scatter diffraction (EBSD), atomic force microscopy (AFM), transmission electron microscope (TEM), Brinell hardness tester and universal testing machine were employed to analyze the microstructure and mechanical properties. The results showed that Sc served as modifier on the microstructure of Al-3Si-0.45Mg-0.45Cu-0.2Zr alloys, including modification of eutectic Si and grains. Extraordinarily, grain refinement was found to be related to the primary particles, which exhibited a close orientation to matrix. After T6 heat treatment, the grain structures were composed of nano-scaled secondary Al3(Sc, Zr) precipitates and spherical eutectic Si. Combined with T6 heat treatment, the highest hardness, yield strength, ultimate tensile strength and elongation were achieved in 0.56 wt.% Sc-modified alloy. Interestingly, the strength and ductility had a similar tendency. This paper demonstrated that combined additions of Mg, Cu, Sc and Zr could significantly improve the microstructure and performance of the hypoeutectic Al-Si cast alloy.

Effects of Al3(Sc,Zr) and Shear Band Formation on the Tensile Properties and Fracture Behavior of Al-Mg-Sc-Zr Alloy

NASA Astrophysics Data System (ADS)

Huang, Hongfeng; Jiang, Feng; Zhou, Jiang; Wei, Lili; Qu, Jiping; Liu, Lele

2015-11-01

The mechanical properties and microstructures of Al-6Mg-0.25Sc-0.1Zr alloy (wt.%) during annealing were investigated by means of uniaxial tensile testing, optical microscope, scanning electron microscope, transmission electron microscope, and high-resolution transmission electron microscope. The results show that a large number of micro and grain-scale shear bands form in this alloy after cold rolling. As the tensile-loading force rises, strain softening would generate in shear bands, resulting in the occurrence of shear banding fracture in cold-rolled Al-Mg-Sc-Zr alloys. Recrystallization takes place preferentially in shear bands during annealing. Due to the formation of coarse-grain bands constructed by new subgrains, recrystallization softening tends to occur in these regions. During low-temperature annealing, recrystallization is inhibited by nano-scale Al3(Sc,Zr) precipitates which exert significant coherency strengthening and modulus hardening. However, the strengthening effect of Al3(Sc,Zr) decreases with the increasing of particle diameter at elevated annealing temperature. The mechanical properties of the recrystallized Al-Mg-Sc-Zr alloy decrease to a minimum level, and the fracture plane exhibits pure ductile fracture characteristics.

Hyperthermal atomic oxygen generator

NASA Technical Reports Server (NTRS)

Khandelwal, Govind S.; Wu, Dongchuan

1990-01-01

Characterization of the transport properties of oxygen through silver was continued. Specifically, experiments measuring the transport through Ag(111), Ag(110), Ag(100) single crystals and through Ag0.05 Zr alloy were completed. In addition, experiments using glow discharge excitation of oxygen to assist in the transport were completed. It was found that the permeability through the different orientations of single crystal Ag was the same, but significant differences existed in the diffusivity. The experimental ratio of diffusivities, however, was in reasonable agreement with theoretical estimates. Since the solubilities of orientations must be the same, this suggests some problems with the assumption K = DS. The glow discharge experiments show that there is a substantial increase in transport (factor of six) when the upstream pressure is dissociated to some fraction of atoms (which have a much higher sticking coefficient). These results indicate that there is a significant surface limitation because of dissociative adsorption of the molecules. Experiments with the Ag0.05 Zr alloy and its high-grain boundary and defect density show a permeability of greater than a factor of two over ordinary polycrystalline Ag, but it is unclear as to whether this is because of enhanced transport through these defects or whether the Zr and defects on the surface increased the sticking coefficient and therefore the transport.

Electronic structure and bonding interactions in Ba1- x Sr x Zr0.1Ti0.9O3 ceramics

NASA Astrophysics Data System (ADS)

Mangaiyarkkarasi, Jegannathan; Sasikumar, Subramanian; Saravanan, Olai Vasu; Saravanan, Ramachandran

2017-06-01

An investigation on the precise electronic structure and bonding interactions has been carried out on Ba1- x Sr x Zr0.1Ti0.9O3 (short for BSZT, x = 0, 0.05, 0.07 and 0.14) ceramic systems prepared via high-temperature solid state reaction technique. The influence of Sr doping on the BSZT structure has been examined by characterizing the prepared samples using PXRD, UV-visible spectrophotometry, SEM and EDS. Powder profile refinement of X-ray data confirms that all the synthesized samples have been crystallized in cubic perovskite structure with single phase. Charge density distribution of the BSZT systems has been completely analyzed by the maximum entropy method (MEM). Co-substitution of Sr at the Ba site and Zr at the Ti site into the BaTiO3 structure presents the ionic nature between Ba and O ions and the covalent nature between Ti and O ions, revealed from MEM calculations. Optical band gap values have been evaluated from UV-visible absorption spectra. Particles with irregular shapes and well defined grain boundaries are clearly visualized from SEM images. The phase purity of the prepared samples is further confirmed by EDS qualitative spectral analysis.

Chemically sensitive free-volume study of amorphization of Cu60Zr40 induced by cold rolling and folding

NASA Astrophysics Data System (ADS)

Puff, Werner; Rabitsch, Herbert; Wilde, Gerhard; Dinda, Guru P.; Würschum, Roland

2007-06-01

With the aim to contribute to a microscopical understanding of the processes of solid-state amorphization, the chemically sensitive technique of background—reduced Doppler broadening of positron-electron annihilation radiation in combination with positron lifetime spectroscopy and microstructural characterization is applied to a free volume study of the amorphization of Cu60Zr40 induced by consecutive folding and rolling. Starting from the constituent pure metal foils, a nanosale multilayer structure of elemental layers and amorphous interlayers develops in an intermediate state of folding and rolling, where free volumes with a Zr-rich environment occur presumably located in the hetero-interfaces between the various layers or in grain boundaries of the Cu layers. After complete intermixing and amorphization, the local chemical environment of the free volumes reflects the average chemical alloy composition. In contrast to other processes of amorphization, free volumes of the size of few missing atoms occur in the rolling-induced amorphous state. Self-consistent results from three different methods for analyzing the Doppler broadening spectra, i.e., S-W-parameter correlation, multicomponent fit, and the shape of ratio curves, demonstrate the potential of the background-reduced Doppler technique for chemically sensitive characterization of structurally complex materials on an atomic scale.

C-Cr segregation at grain boundary before the carbide nucleation in Alloy 690

DOE Office of Scientific and Technical Information (OSTI.GOV)

Li Hui, E-mail: huili@shu.edu.cn; Laboratory for Microstructures, Shanghai University, Shanghai, 200444; Xia Shuang

2012-04-15

The grain boundary segregation in Alloy 690 was investigated by atom probe tomography. B, C and Si segregated at the grain boundary. The high concentration regions for each segregation element form a set of straight arrays that are parallel to each other in the grain boundary plane. The concentration fluctuation has a periodicity of about 7 nm in the grain boundary plane. Before the Cr{sub 23}C{sub 6} nucleation at grain boundaries, the C-Cr co-segregate on one side of the grain boundaries while not the exact grain boundary core regions have been detected. The reasons why grain boundary carbides have coherentmore » orientation relationship only with one side of nearby grain which grain boundary is located at high index crystal plane were discussed. - Highlights: Black-Right-Pointing-Pointer Grain boundary segregation in Alloy 690 was investigated by atom probe tomography. Black-Right-Pointing-Pointer B, C and Si segregate at the grain boundary. Black-Right-Pointing-Pointer Concentration of segregated atoms periodicity fluctuated in the grain boundary plane. Black-Right-Pointing-Pointer C and Cr co-segregate on one side of the grain boundary before carbide nucleation.« less

Micro/nano composited tungsten material and its high thermal loading behavior

NASA Astrophysics Data System (ADS)

Fan, Jinglian; Han, Yong; Li, Pengfei; Sun, Zhiyu; Zhou, Qiang

2014-12-01

Tungsten (W) is considered as promising candidate material for plasma facing components (PFCs) in future fusion reactors attributing to its many excellent properties. Current commercial pure tungsten material in accordance with the ITER specification can well fulfil the performance requirements, however, it has defects such as coarse grains, high ductile-brittle transition temperature (DBTT) and relatively low recrystallization temperature compared with its using temperature, which cannot meet the harsh wall loading requirement of future fusion reactor. Grain refinement has been reported to be effective in improving the thermophysical and mechanical properties of W. In this work, rare earth oxide (Y2O3/La2O3) and carbides (TiC/ZrC) were used as dispersion phases to refine W grains, and micro/nano composite technology with a process of "sol gel - heterogeneous precipitation - spray drying - hydrogen reduction - ordinary consolidation sintering" was invented to introduce these second-phase particles uniformly dispersed into W grains and grain-boundaries. Via this technology, fine-grain W materials with near-full density and relatively high mechanical properties compared with traditional pure W material were manufactured. Preliminary transient high-heat flux tests were performed to evaluate the thermal response under plasma disruption conditions, and the results show that the W materials prepared by micro/nano composite technology can endure high-heat flux of 200 MW/m2 (5 ms).

Ionic conductivity and thermal stability of magnetron-sputtered nanocrystalline yttria-stabilized zirconia

NASA Astrophysics Data System (ADS)

Sillassen, M.; Eklund, P.; Sridharan, M.; Pryds, N.; Bonanos, N.; Bøttiger, J.

2009-05-01

Thermally stable, stoichiometric, cubic yttria-stabilized zirconia (YSZ) thin-film electrolytes have been synthesized by reactive pulsed dc magnetron sputtering from a Zr-Y (80/20 at. %) alloy target. Films deposited at floating potential had a ⟨111⟩ texture. Single-line profile analysis of the 111 x-ray diffraction peak yielded a grain size of ˜20 nm and a microstrain of ˜2% regardless of deposition temperature. Films deposited at 400 °C and selected bias voltages in the range from -70 to -200 V showed a reduced grain size for higher bias voltages, yielding a grain size of ˜6 nm and a microstrain of ˜2.5% at bias voltages of -175 and -200 V with additional incorporation of argon. The films were thermally stable; very limited grain coarsening was observed up to an annealing temperature of 800 °C. Temperature-dependent impedance spectroscopy analysis of the YSZ films with Ag electrodes showed that the in-plane ionic conductivity was within one order of magnitude higher in films deposited with substrate bias corresponding to a decrease in grain size compared to films deposited at floating potential. This suggests that there is a significant contribution to the ionic conductivity from grain boundaries. The activation energy for oxygen ion migration was determined to be between 1.14 and 1.30 eV.

Electronic structure study of Ce1-xAxO2 (A = Zr & Hf) nanoparticles: NEXAFS and EXAFS investigations.

PubMed

Sharma, Aditya; Varshney, Mayora; Shin, Hyun-Joon; Park, Yong Jun; Kim, Min-Gyu; Ha, Tae-Kyun; Chae, Keun Hwa; Gautam, Sanjeev

2014-10-07

Single phase nanoparticles (NPs) of CeO2, Ce0.5Zr0.5O2, Ce0.5Hf0.5O2 and Ce0.5Hf0.25Zr0.25O2 were successfully synthesized by co-precipitation method at constant pH and temperature. The X-ray diffraction results revealed that the additive atoms did not segregate to form secondary phases but led to grain size variation in the NPs. The 10 Dq values in the near edge X-ray absorption fine structure (NEXAFS) spectra at the O K-edge did not vary in the same way as the average grain size was changed for the doped CeO2 NPs. The deconvolution of Ce M5-edge and detailed analysis of O K pre-edge peak have shown the higher Ce(+3)/(Ce(+3) + Ce(+4)) ratio in the Zr- and Hf-doped samples. The local atomic structure around the Ce, Zr and Hf atoms was investigated using extended X-ray absorption fine structure (EXAFS) spectroscopy at Ce K-edge, Zr K-edge and Hf L3-edge, respectively, and the EXAFS data were fitted with the theoretical calculations. The 4f occupancy, Ce(+3)/(Ce(+3) + Ce(+4)) ratio of Ce ions, coordination number of Ce and Ce-Ce/Ce-O bond distances were sensitive to the additive atoms but not explicitly changed according to the grain size variation in the NPs.

Morphological Evolution and Weak Interface Development within CVD-Zirconia Coating Deposited on Hi-Nicalon Fiber

NASA Technical Reports Server (NTRS)

Li, Hao; Lee, Jinil; Libera, Matthew R.; Lee, Woo Y.; Kebbede, Anteneh; Lance, Michael J.; Wang, Hongyu; Morscher, Gregory N.; Gray, Hugh R. (Technical Monitor)

2002-01-01

The phase contents and morphology of a ZrO2 fiber coating deposited at 1050 C on Hi-Nicalon(Tm) by chemical vapor deposition were examined as a function of deposition time from 5 to 120 min. The morphological evolution in the ZrO2 coating was correlated to the development of delamination within the ZrO2 coating. The delamination appears to occur as a result of: (1) continuous formation of tetragonal ZrO2 nuclei on the deposition surface; (2) martensitic transformation of the tetragonal phase to a monoclinic phase upon reaching a critical grain size; and (3) development of significant compressive hoop stresses due to the volume dilation associated with the transformation. Our observations suggest that it will be of critical importance to further understand and eventually control the nucleation and grain growth behavior of CVD ZrO2 and its phase transformation behavior for its potential applications for composites.

The dependence of carbide morphology on grain boundary character in the highly twinned Alloy 690

NASA Astrophysics Data System (ADS)

Li, Hui; Xia, Shuang; Zhou, Bangxin; Chen, Wenjue; Hu, Changliang

2010-04-01

The dependence of morphology of grain boundary carbides on grain boundary character in Alloy 690 (Ni-30Cr-10Fe, mass fraction, %) with high fraction of low Σ coincidence site lattice (CSL) grain boundaries was investigated by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Some of the surface grains were removed by means of deep etching. It was observed that carbides grow dendritically at grain boundaries. The carbide bars observed near incoherent twin boundaries and twin related Σ9 grain boundaries are actually secondary dendrites of the carbides on these boundaries. Higher order dendrites could be observed on random grain boundaries, however, no bar-like dendrites were observed near Σ27 grain boundaries and random grain boundaries. The morphology difference of carbides precipitated at grain boundaries with different characters is discussed based on the experimental results in this paper.

Atomistic modeling of grain boundary behavior under shear conditions in magnesium and magnesium-based binary alloys

NASA Astrophysics Data System (ADS)

Nahhas, M. K.; Groh, S.

2018-02-01

In this study, the structure, the energetic, and the strength of a { 10 1 bar 1 } < 11 2 bar 0 > symmetric tilt grain boundary in magnesium and magnesium binary alloys were analyzed in the framework of (semi-)empirical potentials. Following a systematic investigation of the transferability and accuracy of the interatomic potentials, atomistic calculations of the grain boundary energy, the grain boundary sliding energy, and the grain boundary strength were performed in pure magnesium and in binary MgX alloys (X = Al, Ca, Gd, Li, Sn, Y, Ag, Nd, and Pb). The data gained in this study were analyzed to identify the most critical material parameters controlling the strength of the grain boundary, and their consequence on atomic shuffling motions occurring at the grain boundary. From the methodology perspective, the role of in-plane and out-of plane relaxation on the grain boundary sliding energy curves was investigated. In pure magnesium, the results showed that in-plane relaxation is critical in activating b2{ 10 1 bar 1 } twinning dislocation resulting in grain boundary migration. In the alloy systems, however, grain boundary migration was disabled as a consequence of the pinning of the grain boundary by segregated elements. Finally, while the grain boundary energy, the shape of the grain boundary sliding energy curves, and the grain boundary sliding energy are critical parameters controlling the grain boundary strength in pure magnesium, only the grain boundary energy and the segregation energy of the alloying elements at the grain boundary were identified as critical material parameters in the alloys system.

Properties and rapid low-temperature consolidation of nanocrystalline Fe-ZrO2 composite by pulsed current activated sintering

NASA Astrophysics Data System (ADS)

Kang, Hyun-Su; Ko, In-Yong; Yoon, Jin-Kook; Doh, Jung-Mann; Hong, Kyung-Tae; Shon, In-Jin

2011-02-01

Nanopowders of Fe and ZrO2 were synthesized from Fe2O3 and Zr by high-energy ball milling. The powder sizes of Fe and ZrO2 were 70 nm and 12 nm, respectively. Highly dense nanostructured 4/3Fe-ZrO2 composite was consolidated by a pulsed current activated sintering method within 1 minute from the mechanically synthesized powders (Fe-ZrO2) and horizontal milled Fe2O3+Zr powders under the 1 GPa pressure. The grain sizes of Fe and ZrO2 in the composite were calculated. The average hardness and fracture toughness values of nanostuctured 4/3Fe-ZrO2 composite were investigated.

Influence of SiC grain boundary character on fission product transport in irradiated TRISO fuel

NASA Astrophysics Data System (ADS)

Lillo, T. M.; van Rooyen, I. J.

2016-05-01

In this study, the fission product precipitates at silicon carbide grain boundaries from an irradiated TRISO particle were identified and correlated with the associated grain boundary characteristics. Precession electron diffraction in the transmission electron microscope provided the crystallographic information needed to identify grain boundary misorientation and boundary type (i.e., low angle, random high angle or coincident site lattice (CSL)-related). The silicon carbide layer was found to be composed mainly of twin boundaries and small fractions of random high angle and low angle grain boundaries. Most fission products were found at random, high-angle grain boundaries, with small fractions at low-angle and CSL-related grain boundaries. Palladium (Pd) was found at all types of grain boundaries while Pd-uranium and Pd-silver precipitates were only associated with CSL-related and random, high-angle grain boundaries. Precipitates containing only Ag were found only at random, high-angle grain boundaries, but not at low angle or CSL-related grain boundaries.

Atomic scale study of grain boundary segregation before carbide nucleation in Ni-Cr-Fe Alloys

NASA Astrophysics Data System (ADS)

Li, Hui; Xia, Shuang; Liu, Wenqing; Liu, Tingguang; Zhou, Bangxin

2013-08-01

Three dimensional chemical information concerning grain boundary segregation before carbide nucleation was characterized by atom probe tomography in two Ni-Cr-Fe alloys which were aged at 500 °C for 0.5 h after homogenizing treatment. B, C and Si atoms segregation at grain boundary in Alloy 690 was observed. B, C, N and P atoms segregation at grain boundary in 304 austenitic stainless steel was observed. C atoms co-segregation with Cr atoms at the grain boundaries both in Alloy 690 and 304 austenitic stainless steel was found, and its effect on the carbide nucleation was discussed. The amount of each segregated element at grain boundaries in the two Ni-Cr-Fe alloys were analyzed quantitatively. Comparison of the grain boundary segregation features of the two Ni-Cr-Fe alloys were carried out based on the experimental results. The impurity and solute atoms segregate inhomogeneously in the same grain boundary both in 304 SS and Alloy 690. The grain boundary segregation tendencies (Sav) are B (11.8 ± 1.4) > P (5.4 ± 1.4) > N (4.7 ± 0.3) > C (3.7 ± 0.4) in 304 SS, and B (6.9 ± 0.9) > C (6.7 ± 0.4) > Si (1.5 ± 0.2) in Alloy 690. Cr atoms may co-segregate with C atoms at grain boundaries before carbide nucleation at the grain boundaries both in 304 SS and Alloy 690. Ni atoms generally deplete at grain boundary both in 304 SS and Alloy 690. The literature shows that the Ni atoms may co-segregate with P atoms at grain boundaries [28], but the P atoms segregation do not leads to Ni segregation in the current study. In the current study, Fe atoms may segregate or deplete at grain boundary in Alloy 690. But Fe atoms generally deplete at grain boundary in 304 SS. B atoms have the strongest grain boundary segregation tendency both in 304 SS and Alloy 690. The grain boundary segregation tendency and Gibbs free energy of B in 304 SS is higher than in Alloy 690. C atoms are easy to segregate at grain boundaries both in 304 SS and Alloy 690. The grain boundary segregation tendency and Gibbs free energy of C in Alloy 690 is higher than in 304 SS, due to the higher bulk C concentration and the site competition of P atoms which segregate at grain boundary [29,30]. It is imply that the segregation tendency is influenced by the bulk concentration of the segregates. Si atoms slightly segregate at grain boundaries in Alloy 690, but do not segregate at grain boundaries in 304 SS. N and P atoms segregate at grain boundary in 304 SS, and their segregation Gibbs free energy are similar. N atoms may be exhausted by the TiN precipitated in the matrix and can not be observed in the grain boundary of Alloy 690 [19]. Mn atoms deplete at grain boundary in 304 SS. This phenomenon is similar to that of proton irradiation induced segregation in 304 SS [32]. B, C, N, P segregation Gibbs energies are similar both in 304 SS and Alloy 690. B and C atoms segregate at grain boundary both in Alloy 690 and 304 SS, P and N segregate at grain boundary in 304 SS. Si atoms segregate at grain boundary in Alloy 690, but do not segregate at grain boundary in 304 SS. Cr enriches at grain boundary both in Alloy 690 and 304 SS, although carbide does not nucleate. Ni and Fe may segregate, deplete or homogeneously distribute at grain boundary in Alloy 690, but they deplete at grain boundary in 304 SS. C and Cr atoms co-segregate at grain boundaries before carbide nucleation in Alloy 690 and 304 SS. Combination with other results in literatures, the evolution of Cr concentration at grain boundary should be enrichment at grain boundary before carbide nucleation, depletion at grain boundary after carbide precipitation, and healing after obvious growth of carbide. After aging treatment at 500 °C for 0.5 h, the total reduction of grain boundary free energy due to segregation is 27.489 kJ/mol for Alloy 690 and 45.207 kJ/mol for 304.

The 13C-Pocket Structure In AGB Models: Constraints From Zirconium Isotope Abundances In Single Mainstream SiC Grains

DOE PAGES

Liu, Nan; Gallino, Roberto; Bisterzo, Sara; ...

2014-06-04

In this paper, we present postprocess asymptotic giant branch (AGB) nucleosynthesis models with different 13C-pocket internal structures to better explain zirconium isotope measurements in mainstream presolar SiC grains by Nicolussi et al. and Barzyk et al. We show that higher-than-solar 92Zr/ 94Zr ratios can be predicted by adopting a 13C-pocket with a flat 13C profile, instead of the previous decreasing-with-depth 13C profile. Finally, the improved agreement between grain data for zirconium isotopes and AGB models provides additional support for a recent proposal of a flat 13C profile based on barium isotopes in mainstream SiC grains by Liu et al.

Characterization of Ultra-high Temperature Ceramics via Transmission Electron Microscopy Relevant ZrB2-based Composites, TaC-based Composites and Oxides Containing SiC Chopped Fibers

DTIC Science & Technology

2015-03-06

was formed by ZrO2 rounded grains containing W traces and covered by H3BO3 acicular crystals deriving from hydration of B2O3 after exposure to...TaSi2 grains tended to form large pockets as wide as 3-8 m. Other spurious phases formed upon decomposition of the additive, were identified as SiC

Orthopyroxene as a recorder of primitive achondrite petrogenesis: Major-, minor-, and trace-element systematics of orthopyroxene in Lodran. [Abstract only

NASA Technical Reports Server (NTRS)

Papike, J. J.; Spilde, M. N.; Fowler, G. W.; Shearer, C. K.

1994-01-01

Considerable attention has been paid recently to the primitive achondrites because they may form a link between chondrites and more differentiated achondrite meteorites. A recent paper by Miyamoto and Takeda addresses the thermal history of lodranites Yamato 74357 and MAC 88177 as inferred from chemical zoning of pyroxene and olivine determined by electron microprobe analyses. Their results suggested that interstitial melt was present and then extracted. We have taken the analysis of Lodran-type meteorites one step further by incorporating the techniques of Electromagnetic Pulse/Wavelength Dispersive Spectroscopy (EMP/WDS) compositional imaging and scanning ion mass spectroscopy (SIMS) analysis. Orthopyroxene in Lodran is strongly zoned in CaO, Al2O3, TiO2, and Cr2O3 within the last 10-30 microns from the grain boundaries. The rims are reversely zoned in Mg-Fe, exhibiting Mg enrichment, and compositions change from a fairly uniform Wo3En94 within the grains to Wo1En96 at the rims. CaO drops from 1.6 to 0.6 wt% and Al2O3, TiO2, and Cr2O3 exhibit similar depletions. MnO is fairly uniform throughout the grains at around 0.5 wt%. Olivine is also reversely zoned with respect to not only grain boundaries but also to fractures within the grains, giving many olivine grains a complex, patchy zoning pattern. Some of the core-rim trace-element systematics for orthopyroxene are illustrated. Because of the rather narrow zoned rims in Lodran orthopyroxene and the low trace-element abundances, it is difficult to clearly resolve the trace-element systematics. Nevertheless it is evident that the cores are enriched in the incompatible trace elements Ce, Nd, Dy, Er, Yb, Y, and Zr relative to the rims.

Diffusivity in Alumina Scales Grown on Al-MAX Phases

NASA Technical Reports Server (NTRS)

Smialek, James L.

2014-01-01

Ti3AlC2, Ti2AlC, and Cr2AlC are oxidation resistant MAX phase compounds distinguished by the formation of protective Al2O3 scales with well controlled kinetics. A modified Wagner treatment was used to obtain interfacial grain boundary diffusivity, deltaD(sub gb,O,int.), from scale growth rates and corresponding grain size. It is based on the p(O2)(exp -1/6) dependency of the double charged oxygen vacancy and oxygen diffusivity, coupled with the effective diffusion constant for short circuit grain boundary paths. Data from the literature for MAX phases was analyzed accordingly, and deltaD(sub gb,O,int.) was found to nearly coincide with the Arrhenius line developed for Zr-doped FeCrAl, where: deltaD(sub gb,O,int.) = 1.8x10(exp -10) exp(-375 kJ/RT) cubic meters/s. Furthermore, this oxidation relation suggests the more general format applicable to bulk samples under ambient conditions: deltaD(sub gb,O) = 7.567x10(exp -8) exp(-544 kJ/RT) p(O2)(exp -1/6) cubic meters/[s x Pa(exp -1/6)]. Data from many other FeCrAl(X) studies were similarly assessed to show general agreement with the relation for deltaD(sub gb,O,int.). This analysis reinforces the view that protective alumina scales grow by similar mechanisms for these Al-MAX phases and oxidation resistant FeCrAl alloys.

Influence of SiC grain boundary character on fission product transport in irradiated TRISO fuel

DOE PAGES

Lillo, T. M.; Rooyen, I. J.

2016-02-26

The relationship between grain boundary character and fission product migration is identified as an important knowledge gap in order to advance the understanding of fission product release from TRISO fuel particles. Precession electron diffraction (PED), a TEM-based technique, was used in this study to quickly and efficiently provide the crystallographic information needed to identify grain boundary misorientation, grain boundary type (low or high angle) and whether the boundary is coincident site lattice (CSL) – related, in irradiated SiC. Analysis of PED data showed the grain structure of the SiC layer in an irradiated TRISO fuel particle from the AGR-1 experimentmore » to be composed mainly of twin boundaries with a small fraction of low angle grain boundaries (<10%). In general, fission products favor precipitation on random, high angle grain boundaries but can precipitate out on low angle and CSL-related grain boundaries to a limited degree. Pd is capable of precipitating out on all types of grain boundaries but most prominently on random, high angle grain boundaries. Pd-U and Pd-Ag precipitates were found on CSL-related as well as random high angle grain boundaries but not on low angle grain boundaries. In contrast, precipitates containing only Ag were found only on random, high angle grain boundaries but not on either low angle or CSL-related grain boundaries.« less

Influence of SiC grain boundary character on fission product transport in irradiated TRISO fuel

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lillo, T. M.; Rooyen, I. J.

The relationship between grain boundary character and fission product migration is identified as an important knowledge gap in order to advance the understanding of fission product release from TRISO fuel particles. Precession electron diffraction (PED), a TEM-based technique, was used in this study to quickly and efficiently provide the crystallographic information needed to identify grain boundary misorientation, grain boundary type (low or high angle) and whether the boundary is coincident site lattice (CSL) – related, in irradiated SiC. Analysis of PED data showed the grain structure of the SiC layer in an irradiated TRISO fuel particle from the AGR-1 experimentmore » to be composed mainly of twin boundaries with a small fraction of low angle grain boundaries (<10%). In general, fission products favor precipitation on random, high angle grain boundaries but can precipitate out on low angle and CSL-related grain boundaries to a limited degree. Pd is capable of precipitating out on all types of grain boundaries but most prominently on random, high angle grain boundaries. Pd-U and Pd-Ag precipitates were found on CSL-related as well as random high angle grain boundaries but not on low angle grain boundaries. In contrast, precipitates containing only Ag were found only on random, high angle grain boundaries but not on either low angle or CSL-related grain boundaries.« less

Local piezoelectric behavior in PZT-based thin films for ultrasound transducers

NASA Astrophysics Data System (ADS)

Griggio, Flavio

Piezoelectric microelectromechanical systems (MEMS) are currently used in inkjet printers and precision resonators; numerous additional applications are being investigated for sensors, low-voltage actuators, and transducers. This work was aimed at improving piezoelectric MEMS by taking two approaches: 1) identifying factors affecting the piezoelectric response of ferroelectric thin films and 2) demonstrating integration of these films into a high frequency array transducer. It was found that there are several key factors influencing the piezoelectric response of thin films for a given material composition. First, large grain size improves the piezoelectric response. This was demonstrated using chemical solution deposited lead nickel niobate -- lead zirconate titanate (0.3)Pb(Ni 0.33Nb0.67)O3 - (0.7)Pb(Zr0.45Ti 0.55O3), (PNN-PZT) ferroelectric thin films. It was shown that this composition allows greater microstructural control than does PZT. Dielectric permittivities ranging from 1350 to 1520 and a transverse piezoelectric coefficient e31,f as high as -- 9.7 C/m 2 were observed for films of about 0.25 mum in thickness. The permittivity and piezoelectric response as well as extrinsic contributions to the dielectric constant increased by 14 and 12 % respectively for samples with grain sizes ranging from 110 to 270 nm. A second factor influencing the piezoelectric response is film composition with respect to the morphotropic phase boundary (MPB). The composition dependence of the dielectric and piezoelectric nonlinearities was characterized in epitaxially grown (0.3)Pb(Ni0.33Nb0.67)O3-(0.7)Pb(Zr xTi1-xO3) thin films deposited on SrTiO 3 to minimize the influence of large-angle grain boundaries. Tetragonal, MPB and rhombohedral films were prepared by changing the Zr/Ti ratio. The largest dielectric and piezoelectric nonlinearities were observed for the rhombohedral sample; this resulted from a higher domain wall mobility due to a smaller ferroelectric distortion and superior crystal quality. Thirdly, changes in the mechanical boundary conditions experienced by a ferroelectric thin film were found to influence both the properties and the length scale for correlated motion of domain walls. Microfabrication was employed to release the PZT films from the Si substrate. Nonlinear piezoelectric maps, by band excitation piezoforce microscopy, showed formation of clusters of higher nonlinear activities of similar size for clamped PZT films with different microstructures. However PZT films that had been released from the Si substrate showed a distinct increase in the correlation length associated with coupled domain wall motion, suggesting that the local mechanical boundary conditions, more than microstructure or composition govern the domain wall dynamics. Release of both the local and the global stress states in films produced dielectric nonlinearities comparable to those of bulk ceramics. The second research direction was targeted at demonstrating the functionality of a one dimensional transducer array. A diaphragm geometry was used for the transducer arrays in order to benefit from the unimorph-type displacement of the PZT-SiO2 layers. For this purpose, the PZT and remaining films in the stack were patterned using reactive ion etching and partially released from the underlying silicon substrate by XeF2 etching from the top. Admittance measurements on the fabricated structures showed resonance frequencies at ˜40 MHz for a 80 mum diameter-wide diaphragms with a PZT thickness of 1.74 mum. In-water transmit and receive functionalities were demonstrated. A bandwidth on receive of 80 % centered at 40 MHz was determined during pitch-mode tests.

Investigation into the stress corrosion cracking properties of AA2099, an aluminum-lithium-copper alloy

NASA Astrophysics Data System (ADS)

Padgett, Barbara Nicole

Recently developed Al-Li-Cu alloys show great potential for implementation in the aerospace industry because of the attractive mix of good mechanical properties and low density. AA2099 is an Al-Li-Cu alloy with the following composition Al-2.69wt%Cu-1.8wt%Li-0.6wt%Zn-0.3wt%Mg-0.3wt%Mn-0.08wt%Zr. The environmental assisted cracking and localized corrosion behavior of the AA2099 was investigated in this thesis. The consequences of uncontrolled grain boundary precipitation via friction stir welding on the stress corrosion cracking (SCC) behavior of AA2099 was investigated first. Using constant extension rate testing, intergranular corrosion immersion experiments, and potentiodynamic scans, the heat-affected zone on the trailing edge of the weld (HTS) was determined to be most susceptible of the weld zones. The observed SCC behavior for the HTS was linked to the dissolution of an active phase (Al2CuLi, T1) populating the grain boundary. It should be stated that the SCC properties of AA2099 in the as-received condition were determined to be good. Focus was then given to the electrochemical behavior of precipitate phases that may occupy grain and sub-grain boundaries in AA2099. The grain boundary micro-chemistry and micro-electrochemistry have been alluded to within the literature as having significant influence on the SCC behavior of Al-Li-Cu alloys. Major precipitates found in this alloy system are T1 (Al 2CuLi), T2 (Al7.5Cu4Li), T B (Al6CuLi3), and theta (Al2 Cu). These phases were produced in bulk form so that the electrochemical nature of each phase could be characterized. It was determined T1 was most active electrochemically and theta was least. When present on grain boundaries in the alloy, electrochemical behavior of the individual precipitates aligned with the observed corrosion behavior of the alloy (e.g. TB was accompanied by general pitting corrosion and T 1 was accompanied by intergranular corrosion attack). In addition to the electrochemical behavior of the above-mentioned intermetallics, the phenomenon of Zn substituting for Cu in T1 was also studied. It was determined that for Zn substitutions up to 8.4wt%, improved corrosion behavior of T 1 would occur by dealloying of Zn and Li. Lastly, isothermal aging treatments at 160°C and 190°C were conducted to vary the grain boundary structures in a systematic way. The SCC behaviors for the under-aged, peak-aged, and over-aged condition were studied using CERT and alternate immersion testing at each temperature. The severely under-aged condition (≤ 9 hours) at 160°C proved to have poorest SCC resistance. The over-aged condition at 160°C (≥ 24 hours) also had degraded SCC resistance. In contrast the 190°C isothermal aging condition produced better SCC resistance than 160°C isothermal aging temperature for all conditions. The differences in behavior were linked to the species populating the grain boundaries in each isothermal aging condition (T2 at 190°C and T1 at 160°C).

On the Effects of Hot Forging and Hot Rolling on the Microstructural Development and Mechanical Response of a Biocompatible Ti Alloy

PubMed Central

Okazaki, Yoshimitsu

2012-01-01

Zr, Nb, and Ta as alloying elements for Ti alloys are important for attaining superior corrosion resistance and biocompatibility in the long term. However, note that the addition of excess Nb and Ta to Ti alloys leads to higher manufacturing cost. To develop low-cost manufacturing processes, the effects of hot-forging and continuous-hot-rolling conditions on the microstructure, mechanical properties, hot forgeability, and fatigue strength of Ti-15Zr-4Nb-4Ta alloy were investigated. The temperature dependences with a temperature difference (ΔT) from β-transus temperature (Tβ) for the volume fraction of the α- and β-phases were almost the same for both Ti-15Zr-4Nb-4Ta and Ti-6Al-4V alloys. In the α-β-forged Ti-15Zr-4Nb-4Ta alloy, a fine granular α-phase structure containing a fine granular β-phase at grain boundaries of an equiaxed α-phase was observed. The Ti-15Zr-4Nb-4Ta alloy billet forged at Tβ-(30 to 50) °C exhibited high strength and excellent ductility. The effects of forging ratio on mechanical strength and ductility were small at a forging ratio of more than 3. The maximum strength (σmax) markedly increased with decreasing testing temperature below Tβ. The reduction in area (R.A.) value slowly decreased with decreasing testing temperature below Tβ. The temperature dependences of σmax for the Ti-15Zr-4Nb-4Ta and Ti-6Al-4V alloys show the same tendency and might be caused by the temperature difference (ΔT) from Tβ. It was clarified that Ti-15Zr-4Nb-4Ta alloy could be manufactured using the same manufacturing process as for previously approved Ti-6Al-4V alloy, taking into account the difference (ΔT) between Tβ and heat treatment temperature. Also, the manufacturing equivalency of Ti-15Zr-4Nb-4Ta alloy to obtain marketing approval of implants was established. Thus, it was concluded that continuous hot rolling is useful for manufacturing α-β-type Ti alloy.

Irradiation-induced grain growth and defect evolution in nanocrystalline zirconia with doped grain boundaries

DOE PAGES

Dey, Sanchita; Mardinly, John; Wang, Yongqiang; ...

2016-05-27

Grain boundaries are effective sinks for radiation-induced defects, ultimately impacting the radiation tolerance of nanocrystalline materials (dense materials with nanosized grains) against net defect accumulation. However, irradiation-induced grain growth leads to grain boundary area decrease, shortening potential benefits of nanostructures. A possible approach to mitigate this is the introduction of dopants to target a decrease in grain boundary mobility or a reduction in grain boundary energy to eliminate driving forces for grain growth (using similar strategies as to control thermal growth). Here, in this study, we tested this concept in nanocrystalline zirconia doped with lanthanum. Although the dopant is observedmore » to segregate to the grain boundaries, causing grain boundary energy decrease and promoting dragging forces for thermally activated boundary movement, irradiation induced grain growth could not be avoided under heavy ion irradiation, suggesting a different growth mechanism as compared to thermal growth. Furthermore, it is apparent that reducing the grain boundary energy reduced the effectiveness of the grain boundary as sinks, and the number of defects in the doped material is higher than in undoped (La-free) YSZ.« less

Improve sensitization and corrosion resistance of an Al-Mg alloy by optimization of grain boundaries

NASA Astrophysics Data System (ADS)

Yan, Jianfeng; Heckman, Nathan M.; Velasco, Leonardo; Hodge, Andrea M.

2016-05-01

The sensitization and subsequent intergranular corrosion of Al-5.3 wt.% Mg alloy has been shown to be an important factor in stress corrosion cracking of Al-Mg alloys. Understanding sensitization requires the review of grain boundary character on the precipitation process which can assist in developing and designing alloys with improved corrosion resistance. This study shows that the degree of precipitation in Al-Mg alloy is dependent on grain boundary misorientation angle, adjacent grain boundary planes and grain boundary types. The results show that the misorientation angle is the most important factor influencing precipitation in grain boundaries of the Al-Mg alloy. Low angle grain boundaries (≤15°) have better immunity to precipitation and grain boundary acid attack. High angle grain boundaries (>15°) are vulnerable to grain boundary acid attack. Grain boundaries with adjacent plane orientations near to {100} have potential for immunity to precipitation and grain boundary acid attack. This work shows that low Σ (Σ ≤ 29) coincident site lattice (CSL) grain boundaries have thinner β precipitates. Modified nitric acid mass loss test and polarization test demonstrated that the global corrosion resistance of sputtered Al-Mg alloy is enhanced. This may be attributed to the increased fractions of low Σ (Σ ≤ 29) CSL grain boundaries after sputtering.

[Microwave sintering of nanometer powder of alumina and zirconia-based dental ceramics].

PubMed

Chen, Yi-Fan; Lu, Dong-Mei; Wan, Qian-Bing; Jin, Yong; Zhu, Ju-Mu

2006-02-01

The objective of the present study was to investigate the feasibility and reliability of sintering alumina and zirconia-based all-ceramic materials through a recently introduced microwave heating technique. The variation of crystal phases, the growth of grain sizes and microstructural features of these materials were evaluated after sintering. Four different groups of powder (l00%Al2O3, 60%Al2O3+40%ZrO2, 40% Al2O3+60%ZrO2, 100% ZrO2) were respectively press-compacted to fabricate green disk samples, 5 specimen of each group were prepared. All the samples were surrounded by refractory materials for heat containment and processed at 1 600 degrees C in a domestic microwave oven (850 W, 2 450 MHz), 1 600 degrees C/5 min for heating rate, 10 min for holding time. After sintering, the phase composition and average grain size of these ceramics were examined using X-ray diffraction (XRD). Their microstructure characteristics were studied by scanning electron microscopy (SEM). All the specimens were successfully sintered with the application of microwave heating system in combination with a suitable thermal insulator. No phase change was found in alumina while monoclinic-zirconia was found to be transformed to tetragonal-zirconia. A little grain size growth of Al2O3 and ZrO2 has been observed with Al2O3 24.1 nm/before and 51.8 nm/after; ZrO2 25.3 nm/before and 29.7 nm/after. The SEM photos indicated that the microwave-sintered Al2O3-ZrO2 ceramics had a uniform crystal distribution and their crystal sizes could be maintained within the range of nanometers. It is expected that in the near future microwave heating system could be a promising substitute for conventional processing methods due to its unparalled advantages, including more rapid heating rate, shortened sintering time, superfine grain size, improved microstructure and much less expensive equipment.

Meso-scale anisotropic hydrogen segregation near grain-boundaries in polycrystalline nickel characterized by EBSD/SIMS

DOE Office of Scientific and Technical Information (OSTI.GOV)

Oudriss, A.; Le Guernic, Solenne; Wang, Zhaoying

2016-02-15

To study anisotropic hydrogen segregation and diffusion in nickel polycrystalline, Secondary Ion Mass Spectrometry (SIMS) and Electron Back Scattered Diffraction (EBSD) are integrated to investigate hydrogen distribution around grain boundaries. Hydrogen distribution in pre-charged samples were correlated with grain boundary character by integrating high-resolution grain microstructure from EBSD inverse pole figure map and low-resolution hydrogen concentration profile map from SIMS. This multimodal imaging instrumentation shows that grain boundaries in nickel can be categorized into two families based on behavior of hydrogen distribution crossing grain boundary: the first one includes random grain boundaries with fast hydrogen diffusivity, showing a sharp gapmore » for hydrogen concentration profile cross the grain boundaries. The second family are special Σ3n grain boundaries with low hydrogen diffusivity, showing a smooth gradient of hydrogen concentration cross the grain boundary. Heterogeneous hydrogen distributions due to grain boundary family revealed by SIMS/EBSD on mesoscale further validate the recent hydrogen permeation data and anisotropic ab-initio calculations in nanoscale. The results highlight the fact that grain boundaries character impacts hydrogen distribution significantly.« less

Fusion zone microstructure and porosity in electron beam welds of an α+β titanium alloy

NASA Astrophysics Data System (ADS)

Mohandas, T.; Banerjee, D.; Kutumba Rao, V. V.

1999-03-01

The effect of electron beam welding parameters on fusion zone (FZ) microstructure and porosity in a Ti -6.8 Al -3.42 Mo -1.9 Zr -0.21 Si alloy (Russian designation VT 9) has been investigated. It has been observed that the FZ grain width increased continuously with increase in heat input when the base metal was in the β heat-treated condition, while in the α+β heat-treated base metal welds, the FZ grain width increased only after a threshold energy input. The difference is attributed to both the weld thermal cycle and the pinning effect of equiaxed primary alpha on grain growth in the heat-affected zone (HAZ) of α+β heat-treated base metal. Postweld heat treatment (PWHT) in the subtransus and supertransus regions did not alter the columnar grain morphology in the FZ, possibly due to the lack of enough driving force for the formation of new grains by the breaking up of the columnar grains and grain boundary movement for grain growth. As the PWHTs were conducted in a furnace, the role of thermal gradients can be ruled out. Intragranular microstructure in the aswelded condition consisted of hexagonal martensite. The scale of the martensite laths depended on welding speed. The highest porosity was observed at intermediate welding speeds. At low speeds, a majority of pores formed at the fusion boundary, while at high speeds, occurrence of porosity was maximum at the weld center. The trends on porosity can be explained on the basis of solubility of hydrogen in titanium as a function of temperature and the influence of weld thermal cycle on nucleation, growth, and escape of hydrogen gas bubbles. The porosity at slow welding speeds is low because sufficient time exists for the nucleation, growth, and escape of hydrogen gas bubbles, while insufficient time exists for the nucleation of gas bubbles at high welding speeds. The effect of pickling of joint surface, vacuum annealing of the base metal, and successive remelting of the weld metal has also been investigated.

Effects of SnO2, WO3, and ZrO2 addition on the magnetic and mechanical properties of NiCuZn ferrites

NASA Astrophysics Data System (ADS)

Wang, Sea-Fue; Yang, Hsiao-Ching; Hsu, Yung-Fu; Hsieh, Chung-Kai

2015-01-01

In this study, the effects of SnO2, WO3 and ZrO2 addition at levels up to 5 wt% on the magnetic and mechanical properties of Ni0.5Cu0.3Zn0.2Fe2O4 ceramics were investigated. Only Ni0.5Cu0.3Zn0.2Fe2O4 ceramic with a SnO2 addition of ≥3.5 wt% required a densification temperature of 1150 °C, while the others reached maximum densification at 1075 °C. All samples revealed a pure spinel phase and a uniform microstructure, except for the Ni0.5Cu0.3Zn0.2Fe2O4 ceramic with the WO3 addition, which showed an exaggerated grain growth accompanied with a small amount of needle-shaped Cu0.85Zn0.15WO4 second phase. The fracture mode in the pure Ni0.5Cu0.3Zn0.2Fe2O4 ceramic revealed a transgranular phase, as the CuO second phase increased the grain boundary strength; the Ni0.5Cu0.3Zn0.2Fe2O4 ceramics sintered with 5 wt% additives showed an intergranular phase. The Vickers hardness and the bending strength of the Ni0.5Cu0.3Zn0.2Fe2O4 ceramic were 733.6 and 62.0 MPa, respectively. The Vickers hardness of the ferrite with added SnO2 or ZrO2 showed only a slight improvement, while an apparent change (832.7) was observed with the addition of 5.0 wt% WO3. The bending strength of the ferrite was optimized at 75.7 MPa with 2.0 wt% SnO2 and at 90.5 MPa with 3.5 wt% ZrO2, while that of the ferrite sintered with WO3 added dropped gradually from 62.0 to 47.7 MPa as the amount of WO3 was increased from 0 to 5.0 wt% due to the non-uniform microstructure. The pure Ni0.5Cu0.3Zn0.2Fe2O4 ceramic sintered at 1075 °C had an initial permeability of 356.9 and a quality factor of 71.2. The addition of ZrO2 led to a significant increase in the initial permeability (588.4 at 5.0 wt% ZrO2), but a slight decline in the quality factor (56.6 at 5.0 wt% ZrO2).

Surface defects on the Gd{sub 2}Zr{sub 2}O{sub 7} oxide films grown on textured NiW technical substrates by chemical solution method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhao, Y., E-mail: yuezhao@sjtu.edu.cn

2017-02-15

Epitaxial growth of oxide thin films has attracted much interest because of their broad applications in various fields. In this study, we investigated the microstructure of textured Gd{sub 2}Zr{sub 2}O{sub 7} films grown on (001)〈100〉 orientated NiW alloy substrates by a chemical solution deposition (CSD) method. The aging effect of precursor solution on defect formation was thoroughly investigated. A slight difference was observed between the as-obtained and aged precursor solutions with respect to the phase purity and global texture of films prepared using these solutions. However, the surface morphologies are different, i.e., some regular-shaped regions (mainly hexagonal or dodecagonal) weremore » observed on the film prepared using the as-obtained precursor, whereas the film prepared using the aged precursor exhibits a homogeneous structure. Electron backscatter diffraction and scanning electron microscopy analyses showed that the Gd{sub 2}Zr{sub 2}O{sub 7} grains present within the regular-shaped regions are polycrystalline, whereas those present in the surrounding are epitaxial. Some polycrystalline regions ranging from several micrometers to several tens of micrometers grew across the NiW grain boundaries underneath. To understand this phenomenon, the properties of the precursors and corresponding xerogel were studied by Fourier transform infrared spectroscopy and coupled thermogravimetry/differential thermal analysis. The results showed that both the solutions mainly contain small Gd−Zr−O clusters obtained by the reaction of zirconium acetylacetonate with propionic acid during the precursor synthesis. The regular-shaped regions were probably formed by large Gd−Zr−O frameworks with a metastable structure in the solution with limited aging time. This study demonstrates the importance of the precise control of chemical reaction path to enhance the stability and homogeneity of the precursors of the CSD route. - Highlights: •We investigate microstructure of Gd{sub 2}Zr{sub 2}O{sub 7} films grown by a chemical solution route. •The aging effect of precursor solution on formation of surface defect was thoroughly studied. •Gd−Zr−O clusters are present in the precursor solutions.« less

Hot isostatic pressing of silicon nitride with boron nitride, boron carbide, and carbon additions

NASA Technical Reports Server (NTRS)

Mieskowski, Diane M.; Sanders, William A.

1989-01-01

Si3N4 test bars containing additions of BN, B4C, and C, were hot isostatically pressed in Ta cladding at 1900 and 2050 C to 98.9 percent to 99.5 percent theoretical density. Room-temperature strength data on specimens containing 2 wt pct BN and 0.5 wt pct C were comparable to data obtained for Si3N4 sintered with Y2O3, Y2O3 and Al2O3, or ZrO2. The 1370 C strengths were less than those obtained for additions of Y2O3 or ZrO2 but greater than those obtained from a combination of Y2O3 and Al2O3. SEM fractography indicated that, as with other types of Si3N4, room-temperature strength was controlled by processing flaws. The decrease in strength at 1370 C was typical of Si3N4 having an amorphous grain-boundary phase. The primary advantage of nonoxide additions appears to be in facilitating specimen removal from the Ta cladding.

Two-Step Reactive Aid Sintering of BaZr0.8Y0.2O3- δ Proton-Conducting Ceramics

NASA Astrophysics Data System (ADS)

Wang, Siwei; Chen, Yan; Zhang, Lingling; Ren, Cong; Chen, Fanglin; Brinkman, Kyle S.

2015-12-01

Ceramic-based proton conductors enable high-temperature hydrogen economy applications such as hydrogen separation membranes, fuel cells, and steam electrolyzers. BaZr0.8Y0.2O3- δ (BZY) proton-conducting oxide possesses the highest level of proton conductivity reported to date, but poor sinterability hinders its widespread utilization. In this paper, we report a two-step reactive aid sintering (TRAS) method involving the introduction of BaCO3 and B2O3-Li2O for the preparation of dense BZY ceramics sintered at 1500°C. The resulting BZY samples showed a pure perovskite structure with a dramatic increase in the relative density to 91.5%. In addition, the shrinkage during sintering was improved to 19.3% by a TRAS method as compared to 2.6% by the conventional solid date reaction method. The bulk conductivity was improved due to enhanced densification, while the grain boundary conductivity decreased due to the blocking behavior of the sintering aid resulting in a decrease in the total conductivity of the samples.

Two-Step Reactive Aid Sintering of BaZr 0.8Y 0.2O 3-δ Proton-Conducting Ceramics

DOE PAGES

Wang, Siwei; Chen, Yan; Zhang, Lingling; ...

2015-10-14

Ceramic-based proton conductors enable high-temperature hydrogen economy applications such as hydrogen separation membranes, fuel cells, and steam electrolyzers. BaZr 0.8Y 0.2O 3-δ (BZY) proton-conducting oxide possesses the highest level of proton conductivity reported to date, but poor sinterability hinders its widespread utilization. Here, we report a two-step reactive aid sintering (TRAS) method involving the introduction of BaCO 3 and B 2O 3-Li 2O for the preparation of dense BZY ceramics sintered at 1500°C. The resulting BZY samples showed a pure perovskite structure with a dramatic increase in the relative density to 91.5%. In addition, the shrinkage during sintering was improvedmore » to 19.3% by a TRAS method as compared to 2.6% by the conventional solid date reaction method. Moreover, the bulk conductivity was improved due to enhanced densification, while the grain boundary conductivity decreased due to the blocking behavior of the sintering aid resulting in a decrease in the total conductivity of the samples.« less

Defect studies of nanocrystalline zirconia powders and sintered ceramics

NASA Astrophysics Data System (ADS)

Čížek, Jakub; Melikhova, Oksana; Procházka, Ivan; Kuriplach, Jan; Kužel, Radomír; Brauer, Gerhard; Anwand, Wolfgang; Konstantinova, Tatyana E.; Danilenko, Igor A.

2010-01-01

The main objective of the present paper is to communicate a study of defects behavior in zirconia-based nanomaterials—pressure-compacted yttria-stabilized zirconia (YSZ) nanopowders with different contents of Y2O3 and ceramics obtained by sintering the YZS nanopowders. In addition, YZS single crystals were also investigated. Positron annihilation techniques including positron lifetime and coincidence Doppler broadening with a conventional positron source and Doppler broadening experiments on a monoenergetic positron beam were involved in this study as the principal tools. These techniques were supplemented with transmission electron microscopy and x-ray diffraction observations. In order to get better support of the experimental data interpretation, the state-of-art theoretical calculations of positron parameters were performed for the perfect ZrO2 lattice and selected defect configurations in the YSZ. Theoretical calculations have indicated that neither the oxygen vacancies nor their neutral complexes with substitutional yttrium atoms are capable of positron trapping. On the other hand, the zirconium vacancies are deep positron traps and obviously are responsible for the saturated positron trapping observed in the YSZ single crystals. In the compacted YSZ nanopowders, a majority of positrons is trapped either in the vacancylike defects situated in the negative space-charge layers along grain boundaries (τ1≈185ps) or in vacancy clusters at intersections of grain boundaries (τ2≈370ps) . The intensity ratio I2/I1 was found to be correlated with the mean grain size d as I2/I1˜d-2 . A small fraction of positrons (≈10%) form positronium in large pores (τ3≈2ns,τ4≈30ns) . A significant grain growth during sintering of the YSZ nanopowders above 1000°C was observed.

Microstructure and mechanical properties of rapidly solidified B2-type Zr–Co alloys containing a second phase of Zr2Co

NASA Astrophysics Data System (ADS)

Li, Peiyou

2018-04-01

Microstructure and mechanical properties of B2-type Zr–Co alloys containing a second phase (Zr2Co) were investigated. Results show that the as-cast Zr52Co48, Zr54Co46, and Zr56Co44 alloys are composed of a eutectic structure of B2 and Zr2Co phases. Relative amounts of Zr2Co phases increase with an increase in Zr content. Zr54Co46 exhibits high yield strength, high Vickers hardness, good ductility, and high toughness values, and thus, Zr54Co46 can be considered to be a novel engineering material. The increase in strength and decrease in plastic strain of the alloys are mainly attributed to the increase in high strength of the brittle Zr2Co phase and to grain refining of the B2 matrix phase.

Phase-field model with plastic flow for grain growth in nanocrystalline material

NASA Astrophysics Data System (ADS)

Steinbach, Ingo; Song, Xiaoyan; Hartmaier, Alexander

2010-01-01

A phase-field model is presented which considers the accumulation of structural defects in grain boundaries by an isotropic eigenstrain associated with the grain boundaries. It is demonstrated that the elastic energy caused by dilatation of the grain boundary with respect to the bulk crystal contributes largely to the grain boundary energy. The sign of this contribution can be both positive and negative dependent on the local stress state in the grain boundary. Self-diffusion of atoms is taken into account to relax the stress caused by the dilatation of the grain boundary. Application of the model to discontinuous grain growth in pure nanocrystalline cobalt material is presented. Linear grain growth is found in the nanocrystalline state, which is explained by the interpretation of grain boundary motion as a diffusive process defining an upper limit of the grain boundary velocity independent of the grain boundary curvature but dependent on temperature. The transition to regular grain growth at a critical temperature, as observed experimentally, is explained by the drop of theoretical grain boundary velocity due to its mean curvature during coarsening of the nanograin structure below the maximum velocity.

Zr-doped SnO2 thin films synthesized by spray pyrolysis technique for barrier layers in solar cells

NASA Astrophysics Data System (ADS)

Reddy, N. Nanda Kumar; Akkera, Harish Sharma; Sekhar, M. Chandra; Park, Si-Hyun

2017-12-01

In the present work, we investigated the effect of Zr doping (0-6 at%) on the structural, electrical, and optical properties of tin oxide (SnO2) thin films deposited onto glass substrates using a spray pyrolysis technique. The room-temperature X-ray diffraction pattern shows that all deposited films exhibit polycrystalline tetragonal structure. The pure SnO2 film is grown along a preferred (200) direction, whereas Zr-doped SnO2 (Zr:SnO2) films started growing along the (220) orientation along with a high intensity peak of (200). Scanning electron microscope (SEM) and atomic force microscope (AFM) images showed that the grains of the films are spherical in structure, and the grain size decreased with increasing of Zr concentration. The optical transmission spectra of deposited films as a function of wavelength confirm that the average optical transmittance is > 85% for Zr:SnO2 films. The value of the optical bandgap is significantly decreased from 3.94 to 3.68 eV with increasing Zr concentration. Furthermore, the electrical measurements found that the sheet resistance ( R sh) and resistivity ( ρ) values are decreased with increasing of Zr doping. The lowest values of R sh = 6.82 Ω and ρ = 0.4 × 10- 3 Ω cm are found in 6-at% Zr-doped SnO2 film. In addition, a good efficiency value of the figure of merit ( ɸ = 3.35 × 10- 3 Ω-1) is observed in 6-at% Zr-doped SnO2 film. These outstanding properties of Zr-doped SnO2 films make them useful for several optoelectronic device applications.

Trace element abundances in single presolar silicon carbide grains by synchrotron X-ray fluorescence

NASA Astrophysics Data System (ADS)

Kashiv, Yoav

2004-12-01

Synchrotron x-ray fluorescence (SXRF) was applied to the study of presolar grains for the first time in this study. 41 single SiC grains of the KJF size fraction (mass-weighted median size of 1.86 μm) from the Murchison (CM2) Meteorite were analyzed. The absolute abundances of the following elements were determined (not every element in every grain): S, Ca, Ti, V, Cr, Mn, Fe, Co, Ni, Sr, Y, Zr, Nb, Mo, Ru, Os, Ir and Pt (underlined elements were detected here for the first time in single grains). There is good agreement between the heavier trace element abundances in the grains and s-process nucleosynthesis calculations. It suggests that smaller 13C pocket sizes are needed in the parent stars, a free parameter in the stellar models, than is deduced from isotopic analyses of s-, and s-mainly, elements, such as Zr and Mo. In addition, the data confirms the radiogenic nature of the Nb in the grains, due to the in situ decay of 93Zr (t 1/2 = 1.5 × 106 year). The data suggest that the trace elements condensed into the host SiC grains by a combination of condensation in solid solution and incorporation of subgrains. It seems that many of the trace elements reside mainly in subgrains of two solid solution: (1)a TiC based solid solution, and (2)a Mo-Ru carbide based solid solution. The presence of subgrains of an Fe-Ni alloy solid solution is suggested as well. Subgrains of all 3 solid solutions were observed previously in presolar graphite grains.* *This dissertation is a compound document (contains both a paper copy and a CD as part of the dissertation). The CD requires the following system requirements: Adobe Acrobat.

The Role of Grain Boundary Energy on Grain Boundary Complexion Transitions

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bojarski, Stephanie A.; Rohrer, Gregory S.

Grain boundary complexions are distinct equilibrium structures and compositions of a grain boundary and complexion transformations are transition from a metastable to an equilibrium complexion at a specific thermodynamic and geometric conditions. Previous work indicates that, in the case of doped alumina, a complexion transition that increased the mobility of transformed boundaries and resulted in abnormal grain growth also caused a decrease in the mean relative grain boundary energy as well as an increase in the anisotropy of the grain boundary character distribution (GBCD). The current work will investigate the hypothesis that the rates of complexion transitions that result inmore » abnormal grain growth (AGG) depend on grain boundary character and energy. Furthermore, the current work expands upon this understanding and tests the hypothesis that it is possible to control when and where a complexion transition occurs by controlling the local grain boundary energy distribution.« less

SILICON CARBIDE GRAIN BOUNDARY DISTRIBUTIONS, IRRADIATION CONDITIONS, AND SILVER RETENTION IN IRRADIATED AGR-1 TRISO FUEL PARTICLES

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lillo, T. M.; Rooyen, I. J.; Aguiar, J. A.

Precession electron diffraction in the transmission electron microscope was used to map grain orientation and ultimately determine grain boundary misorientation angle distributions, relative fractions of grain boundary types (random high angle, low angle or coincident site lattice (CSL)-related boundaries) and the distributions of CSL-related grain boundaries in the SiC layer of irradiated TRISO-coated fuel particles. Two particles from the AGR-1 experiment exhibiting high Ag-110m retention (>80%) were compared to a particle exhibiting low Ag-110m retention (<19%). Irradiated particles with high Ag-110m retention exhibited a lower fraction of random, high angle grain boundaries compared to the low Ag-110m retention particle. Anmore » inverse relationship between the random, high angle grain boundary fraction and Ag-110m retention is found and is consistent with grain boundary percolation theory. Also, comparison of the grain boundary distributions with previously reported unirradiated grain boundary distributions, based on SEM-based EBSD for similarly fabricated particles, showed only small differences, i.e. a greater low angle grain boundary fraction in unirradiated SiC. It was, thus, concluded that SiC layers with grain boundary distributions susceptible to Ag-110m release were present prior to irradiation. Finally, irradiation parameters were found to have little effect on the association of fission product precipitates with specific grain boundary types.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lee, Hak-Sung, E-mail: hslee@kims.re.kr; Park, Chanbum; Oh, Chang-Seok

Highlights: • We model the sample grain boundary of LiCoO2, one of important Li cathode materials. • Rigid body translation was found the asymmetric GB is more stable than symmetric GB. • The vacancy formation energy of Li and O was estimated with first principles calculations. • This model boundary can help to find a new dopant to improve Li diffusions. - Abstract: An atomic structure of LiCoO{sub 2} model grain boundary, Σ2 [1120](1102), is introduced and grain boundary energies with rigid body translations are investigated systematically to find the most stable interface structures. It is found that the coordinatedmore » structures of Co and O in the vicinity of grain boundary are strongly related to grain boundary energy. Examining nonstoichiometry at grain boundary, the defect energetics of Li and O site at grain boundary are estimated. In addition, the effect of grain boundary on Li diffusion is investigated to calculate Li diffusion across grain boundary.« less

Research on self-propagating high temperature synthesis prepared ZrC-ZrB2 composite ceramic

NASA Astrophysics Data System (ADS)

Yong, Cheng; Xunjia, Su; Genliang, Hou; YaKun, Xing

2013-03-01

ZrC-ZrB2 composite ceramic material is prepared by self-propagating high temperature synthesis, using Zr powders, CrO2 powders and Al powders as raw materials. Samples are studied by XRD and SEM, the results show that: ZrC-ZrB2 composite ceramic is attained after self-propagating high-temperature reaction, with Zr+ B4C as the main reactive system, and which is added respectively different content (CrO3 + Al) system. The study finds that the ceramic composite products are mainly composed of ZrC and ZrB2 phase, and other subphase. Compared to the main reactive system composite ceramic, composite ceramic grains grow up obviously, after introduction of the highly exothermic system (CrO3 + Al) in the main reactive system, and with the gradual increase of the content (CrO3 + Al).

Development of low-Cr ODS FeCrAl alloys for accident-tolerant fuel cladding

NASA Astrophysics Data System (ADS)

Dryepondt, Sebastien; Unocic, Kinga A.; Hoelzer, David T.; Massey, Caleb P.; Pint, Bruce A.

2018-04-01

Low-Cr oxide dispersion strengthened (ODS) FeCrAl alloys were developed as accident tolerant fuel cladding because of their excellent oxidation resistance at very high temperature, high strength and improved radiation tolerance. Fe-12Cr-5Al wt.% gas atomized powder was ball milled with Y2O3+FeO, Y2O3+ZrO2 or Y2O3+TiO2, and the resulting powders were extruded at 950 °C. The resulting fine grain structure, particularly for the Ti and Zr containing alloys, led to very high strength but limited ductility. Comparison with variants of commercial PM2000 (Fe-20Cr-5Al) highlighted the significant impact of the powder consolidation step on the alloy grain size and, therefore, on the alloy mechanical properties at T < 500 °C. These low-Cr compositions exhibited good oxidation resistance at 1400 °C in air and steam for 4 h but could not form a protective alumina scale at 1450 °C, similar to observations for fine grained PM2000 alloys. The effect of alloy grain size, Zr and Ti additions, and impurities on the alloy mechanical and oxidation behaviors are discussed.

Evolution of grain boundary character distributions in alloy 825 tubes during high temperature annealing: Is grain boundary engineering achieved through recrystallization or grain growth?

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bai, Qin; Zhao, Qing

Grain boundary engineering (GBE) of nickel-based alloy 825 tubes was carried out with different cold drawing deformations by using a draw-bench on a factory production line and subsequent annealing at various temperatures. The microstructure evolution of alloy 825 during thermal-mechanical processing (TMP) was characterized by means of the electron backscatter diffraction (EBSD) technique to study the TMP effects on the grain boundary network and the evolution of grain boundary character distributions during high temperature annealing. The results showed that the proportion of ∑ 3{sup n} coincidence site lattice (CSL) boundaries of alloy 825 tubes could be increased to > 75%more » by the TMP of 5% cold drawing and subsequent annealing at 1050 °C for 10 min. The microstructures of the partially recrystallized samples and the fully recrystallized samples suggested that the proportion of low ∑ CSL grain boundaries depended on the annealing time. The frequency of low ∑ CSL grain boundaries increases rapidly with increasing annealing time associating with the formation of large-size highly-twinned grains-cluster microstructure during recrystallization. However, upon further increasing annealing time, the frequency of low ∑ CSL grain boundaries decreased markedly during grain growth. So it is concluded that grain boundary engineering is achieved through recrystallization rather than grain growth. - Highlights: •The grain boundary engineering (GBE) is applicable to 825 tubes. •GBE is achieved through recrystallization rather than grain growth. •The low ∑ CSL grain boundaries in 825 tubes can be increased to > 75%.« less

Electrostatic Assembly Preparation of High-Toughness Zirconium Diboride-Based Ceramic Composites with Enhanced Thermal Shock Resistance Performance.

PubMed

Zhang, Baoxi; Zhang, Xinghong; Hong, Changqing; Qiu, Yunfeng; Zhang, Jia; Han, Jiecai; Hu, PingAn

2016-05-11

The central problem of using ceramic as a structural material is its brittleness, which associated with rigid covalent or ionic bonds. Whiskers or fibers of strong ceramics such as silicon carbide (SiC) or silicon nitride (Si3N4) are widely embedded in a ceramic matrix to improve the strength and toughness. The incorporation of these insulating fillers can impede the thermal flow in ceramic matrix, thus decrease its thermal shock resistance that is required in some practical applications. Here we demonstrate that the toughness and thermal shock resistance of zirconium diboride (ZrB2)/SiC composites can be improved simultaneously by introducing graphene into composites via electrostatic assembly and subsequent sintering treatment. The incorporated graphene creates weak interfaces of grain boundaries (GBs) and optimal thermal conductance paths inside composites. In comparison to pristine ZrB2-SiC composites, the toughness of (2.0%) ZrB2-SiC/graphene composites exhibited a 61% increasing (from 4.3 to 6.93 MPa·m(1/2)) after spark plasma sintering (SPS); the retained strength after thermal shock increased as high as 74.8% at 400 °C and 304.4% at 500 °C. Present work presents an important guideline for producing high-toughness ceramic-based composites with enhanced thermal shock properties.

The Role of Grain Orientation and Grain Boundary Characteristics in the Mechanical Twinning Formation in a High Manganese Twinning-Induced Plasticity Steel

NASA Astrophysics Data System (ADS)

Shterner, Vadim; Timokhina, Ilana B.; Rollett, Anthony D.; Beladi, Hossein

2018-04-01

In the current study, the dependence of mechanical twinning on grain orientation and grain boundary characteristics was investigated using quasi in-situ tensile testing. The grains of three main orientations (i.e., <111>, <110>, and <100> parallel to the tensile axis (TA)) and certain characteristics of grain boundaries (i.e., the misorientation angle and the inclination angle between the grain boundary plane normal and the TA) were examined. Among the different orientations, <111> and <100> were the most and the least favored orientations for the formation of mechanical twins, respectively. The <110> orientation was intermediate for twinning. The annealing twin boundaries appeared to be the most favorable grain boundaries for the nucleation of mechanical twinning. No dependence was found for the inclination angle of annealing twin boundaries, but the orientation of grains on either side of the annealing twin boundary exhibited a pronounced effect on the propensity for mechanical twinning. Annealing twin boundaries adjacent to high Taylor factor grains exhibited a pronounced tendency for twinning regardless of their inclination angle. In general, grain orientation has a significant influence on twinning on a specific grain boundary.

Damage Tolerance and Mechanics of Interfaces in Nanostructured Metals

NASA Astrophysics Data System (ADS)

Foley, Daniel J.

The concept of interface driven properties in crystalline metals has been one of the most intensely discussed topics in materials science for decades. Since the 1980s researchers have been exploring the concept of grain boundary engineering as route for tuning properties such as fracture toughness and irradiation resistance. This is especially true in ultra-fine grained and nanocrystalline materials where grain boundary mediated properties become dominant. More recently, materials composed of hierarchical nanostructures, such as amorphous-crystalline nanolaminates, have attracted considerable attention due to their favorable properties, ease of manufacture and highly tunable microstructure. While both grain boundary engineering and hierarchical nanostructures have shown promise there are still questions remaining regarding the role of specific attributes of the microstructure (such as grain boundaries, grain/layer size and inter/intralayer morphology) in determining material properties. This thesis attempts to address these questions by using atomistic simulations to perform deformation and damage loading studies on a series of nanolaminate and bicrystalline structures. During the course of this thesis the roles of layer thickness, interlayer structure and interlayer chemistry on the mechanical properties of Ni-NiX amorphous-crystalline nanolaminates were explored using atomistic simulations. This thesis found that layer thickness/thickness ratio and amorphous layer chemistry play a crucial role in yield strength and Young's modulus. Analysis of the deformation mechanisms at the atomic scale revealed that structures containing single crystalline, crystalline layers undergo plastic deformation when shear transformation zones form in the amorphous layer and impinge on the amorphous-crystalline interface, leading to dislocation emission. However, structures containing nanocrystalline, crystalline layers (both equiaxed and columnar nanocrystalline) undergo plastic deformation through a combination of grain boundary sliding and grain boundary mediated dislocation nucleation. Since grain boundaries were found to play a critical role as sources and sinks for dislocations in amorphous-crystalline nanolaminates a follow-up study on the effect of grain boundary character on damage accumulation/accommodation in copper symmetric tilt grain boundaries was performed. This study found that grain boundaries will become saturated with damage, a state where grain boundary energy and grain boundary free volume oscillate about a plateau during continuous defect loading (vacancy, interstitial and frenkel pair loading were all considered). Further, grain boundary character (specifically equilibrium grain boundary energy) was strongly correlated to the damage accommodation behavior of grain boundaries in copper. Finally, a study that attempted to link grain boundary damage saturation behavior to variations in grain boundary mechanical properties was performed. This study found no direct relationships between grain boundary damage saturation behavior and variations in grain boundary properties. The results of this thesis provide researchers with several strategies for tuning the properties of amorphous-crystalline nanolaminates. These strategies include manipulated bulk attributes such as layer thickness and morphology as well as manipulation of microscale attributes such as grain boundary engineering. Finally, this thesis provides valuable insight into the damage loading/accommodation behavior of FCC symmetric tilt grain boundaries.

Influence of attrition milling on nano-grain boundaries

DOE Office of Scientific and Technical Information (OSTI.GOV)

Rawers, J.; Cook, D.

1999-03-01

Nanostructured materials have a relatively large proportion of their atoms associated with the grain boundary, and the method used to develop the nano-grains has a strong influence on the resulting grain boundary structure. In this study, attrition milling iron powders and blends of iron powders produced micron-size particles composed of nano-size grains. Mechanical cold-working powder resulted in dislocation generation, multiplication, and congealing that produced grain refinement. As the grain size approached nano-dimensions, dislocations were no longer sustained within the grain and once generated, rapidly diffused to the grain boundary. Dislocations on the grain boundary strained the local lattice structure which,more » as the grain size decreased, became the entire grain. Mechanical alloying of substitutional aluminium atoms into iron powder resulted in the aluminium atoms substituting for iron atoms in the grain boundary cells and providing a grain boundary structure similar to that of the iron powder processed in argon. Attrition milling iron powder in nitrogen gas resulted in nitrogen atoms being adsorbed onto the particle surface. Continued mechanical milling infused the nitrogen atoms into interstitial lattice sites on the grain boundary which also contributed to expanding and straining the local lattice.« less

Al2O3/ZrO2/Y3Al5O12 Composites: A High-Temperature Mechanical Characterization

PubMed Central

Palmero, Paola; Pulci, Giovanni; Marra, Francesco; Valente, Teodoro; Montanaro, Laura

2015-01-01

An Al2O3/5 vol%·ZrO2/5 vol%·Y3Al5O12 (YAG) tri-phase composite was manufactured by surface modification of an alumina powder with inorganic precursors of the second phases. The bulk materials were produced by die-pressing and pressureless sintering at 1500 °C, obtaining fully dense, homogenous samples, with ultra-fine ZrO2 and YAG grains dispersed in a sub-micronic alumina matrix. The high temperature mechanical properties were investigated by four-point bending tests up to 1500 °C, and the grain size stability was assessed by observing the microstructural evolution of the samples heat treated up to 1700 °C. Dynamic indentation measures were performed on as-sintered and heat-treated Al2O3/ZrO2/YAG samples in order to evaluate the micro-hardness and elastic modulus as a function of re-heating temperature. The high temperature bending tests highlighted a transition from brittle to plastic behavior comprised between 1350 and 1400 °C and a considerable flexural strength reduction at temperatures higher than 1400 °C; moreover, the microstructural investigations carried out on the re-heated samples showed a very limited grain growth up to 1650 °C. PMID:28787961

Titanite chronology, thermometry, and speedometry of ultrahigh-temperature (UHT) calc-silicates from south Madagascar: U-Pb dates, Zr temperatures, and lengthscales of trace-element diffusion

NASA Astrophysics Data System (ADS)

Holder, R. M.; Hacker, B. R.

2017-12-01

Calc-silicate rocks are often overlooked as sources of pressure-temperature-time data in granulite-UHT metamorphic terranes due to the strong dependence of calc-silicate mineral assemblages on complex fluid compositions and a lack of thermodynamic data on common high-temperature calc-silicate minerals such as scapolite. In the Ediacaran-Cambrian UHT rocks of southern Madagascar, clinopyroxene-scapolite-feldspar-quartz-zircon-titanite calc-silicate rocks are wide-spread. U-Pb dates of 540-520 Ma from unaltered portions of titanite correspond to cooling of the rocks through upper-amphibolite facies and indicate UHT metamorphism occurred before 540 Ma. Zr concentrations in these domains preserve growth temperatures of 900-950 °C, consistent with peak temperatures calculated by pseudosection modeling of nearby osumilite-bearing gneisses. Younger U-Pb dates (510-490 Ma) correspond to fluid-mediated Pb loss from titanite grains, which occurred below their diffusive Pb-closure temperature, along fractures. The extent of fluid alteration is seen clearly in back-scattered electron images and Zr-, Al-, Fe-, Ce-, and Nb-concentration maps. Laser-ablation depth profiling of idioblastic titanite grains shows preserved Pb diffusion profiles at grain rims, but there is no evidence for Zr diffusion, indicating that it was effectively immobile even at UHT.

Grain boundary diffusion in olivine (Invited)

NASA Astrophysics Data System (ADS)

Marquardt, K.; Dohmen, R.

2013-12-01

Olivine is the main constituent of Earth's upper mantle. The individual mineral grains are separated by grain boundaries that have very distinct properties compared to those of single crystals and strongly affect large-scale physical and chemical properties of rocks, e.g. viscosity, electrical conductivity and diffusivity. Knowledge on the grain boundary physical and chemical properties, their population and distribution in polycrystalline materials [1] is a prerequisite to understand and model bulk (rock) properties, including their role as pathways for element transport [2] and the potential of grain boundaries as storage sites for incompatible elements [3]. Studies on selected and well characterized single grain boundaries are needed for a detailed understanding of the influence of varying grain boundaries. For instance, the dependence of diffusion on the grain boundary structure (defined by the lattice misfit) and width in silicates is unknown [2, 4], but limited experimental studies in material sciences indicate major effects of grain boundary orientation on diffusion rates. We characterized the effect of grain boundary orientation and temperature on element diffusion in forsterite grain boundaries by transmission electron microscopy (TEM).The site specific TEM-foils were cut using the focused ion beam technique (FIB). To study diffusion we prepared amorphous thin-films of Ni2SiO4 composition perpendicular to the grain boundary using pulsed laser deposition. Annealing (800-1450°C) leads to crystallization of the thin-film and Ni-Mg inter-diffuse into the crystal volume and along the grain boundary. The inter-diffusion profiles were measured using energy dispersive x-ray spectrometry in the TEM, standardized using the Cliff-Lorimer equation and EMPA measurements. We obtain volume diffusion coefficients that are comparable to Ni-Mg inter-diffusion rates in forsterite determined in previous studies at comparable temperatures, with similar activation energies. Grain boundary diffusion perpendicular to the dislocation lines of the small angle grain boundaries proved to be about an order of magnitude faster than volume diffusion, whereas diffusion in high angle grain boundaries is several orders of magnitude faster. We will discuss the variation of element diffusion rates with grain boundary orientation and the temperature- and/or time-induced transition from one diffusion regime to the next regime. This is done using time series experiments and two-dimensional grain boundary diffusion simulations. Finally, we will debate the differences between our data and other data sets that result from different experimental setups, conditions and analyses.

Mechanical properties and biocorrosion resistance of the Mg-Gd-Nd-Zn-Zr alloy processed by equal channel angular pressing.

PubMed

Zhang, Junyi; Kang, Zhixin; Wang, Fen

2016-11-01

A Mg-Gd-Nd-Zn-Zr alloy was processed by equal channel angular pressing (ECAP) at 375°C. The grain size of Mg-Gd-Nd-Zn-Zr alloy was refined to ~2.5μm with the spherical precipitates (β1 phase) distributing in the matrix. The mechanical properties of ECAPed alloy were significantly improved as a result of the grain refinement and precipitation strengthening. The corrosion rate of the ECAPed magnesium alloy in simulated body fluid dramatically decreased from 0.236mm/a to 0.126mm/a due to the strong basal texture and refined microstructure. This wrought magnesium alloy shows potentials in biomedical application. Copyright © 2016 Elsevier B.V. All rights reserved.

Role of string-like collective atomic motion on diffusion and structural relaxation in glass forming Cu-Zr alloys

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhang, Hao; Department of Chemical and Materials Engineering, University of Alberta, Edmonton, Alberta T6G 2V4; Zhong, Cheng

2015-04-28

We investigate Cu-Zr liquid alloys using molecular dynamics simulation and well-accepted embedded atom method potentials over a wide range of chemical composition and temperature as model metallic glass-forming (GF) liquids. As with other types of GF materials, the dynamics of these complex liquids are characterized by “dynamic heterogeneity” in the form of transient polymeric clusters of highly mobile atoms that are composed in turn of atomic clusters exhibiting string-like cooperative motion. In accordance with the string model of relaxation, an extension of the Adam-Gibbs (AG) model, changes in the activation free energy ΔG{sub a} with temperature of both the Cumore » and Zr diffusion coefficients D, and the alpha structural relaxation time τ{sub α} can be described to a good approximation by changes in the average string length, L. In particular, we confirm that the strings are a concrete realization of the abstract “cooperatively rearranging regions” of AG. We also find coexisting clusters of relatively “immobile” atoms that exhibit predominantly icosahedral local packing rather than the low symmetry packing of “mobile” atoms. These two distinct types of dynamic heterogeneity are then associated with different fluid structural states. Glass-forming liquids are thus analogous to polycrystalline materials where the icosahedrally packed regions correspond to crystal grains, and the strings reside in the relatively disordered grain boundary-like regions exterior to these locally well-ordered regions. A dynamic equilibrium between localized (“immobile”) and wandering (“mobile”) particles exists in the liquid so that the dynamic heterogeneity can be considered to be type of self-assembly process. We also characterize changes in the local atomic free volume in the course of string-like atomic motion to better understand the initiation and propagation of these fluid excitations.« less

Do s-Process Enhanced Planetary Nebulae Have Unusual Dust Emission Spectra?

NASA Astrophysics Data System (ADS)

Dinerstein, Harriet; Sellgren, Kris; Sterling, Nicholas

2006-05-01

We propose to obtain IRS observations of the mid-infrared dust emission of a sample of Galactic planetary nebulae (PNs) which are known to have enrichments of elements produced in the precursor star by slow neutron-capture nucleosynthesis (the "s-process"). These enhanced abundances result from captures of free neutrons by Fe-peak nuclei following by convective mixing during the AGB; this "third dredge-up" is also responsible for increasing the surface abundance of carbon. Since PNs are the descendants of AGB stars and are often C-rich, it is not surprising that we find substantial enrichments of s-process products such as Ge, Se, and Kr in some PNs. Despite their low initial abundances, 1e-9 to 1e-10 times H, modest enrichments of neutron-capture elements can have observable effects. The spectral type S, a transitional class between O-rich and C-rich AGB stars, is characterized by prominent ZrO bands; Zr is produced in the s-process. We have attempted, without success, to detect gas-phase Zr in PNs. However, Zr is highly refractory. It can condense into ZrO2 or be incorporated into high-temperature rocky condensates in O-rich environments, while in C-rich environments it may form metallic carbides (i.e. ZrC, an analog of TiC). Indeed, Zr-Mo carbide inclusions found in some meteoritic presolar grains are thought to originate in the atmospheres of C-rich AGB stars. Other refractory s-process products (e.g. Sr, Ba) may also be incorporated into grains. High-quality Spitzer spectra of the dust emission in a set of PNs with known s-process enhancements - determined by us from gas-phase measurements of undepleted elements - will be valuable for comparison with laboratory spectroscopy of grain analogs. These comparisons will help determine whether the dredge-up of n-capture products affects the dust chemistry of PNs and may offer some new insights into the dust composition.

Molecular microelectrostatic view on electronic states near pentacene grain boundaries

NASA Astrophysics Data System (ADS)

Verlaak, Stijn; Heremans, Paul

2007-03-01

Grain boundaries are the most inevitable and pronounced structural defects in pentacene films. To study the effect of those structural defects on the electronic state distribution, the energy levels of a hole on molecules at and near the defect have been calculated using a submolecular self-consistent-polarization-field approach in combination with atomic charge-quadrupole interaction energy calculations. This method has been benchmarked prior to application on four idealized grain boundaries: a grain boundary void, a void with molecules squeezed in between two grains, a boundary between two grains with different crystallographic orientations, and a grain boundary void in which a permanent dipole (e.g., a water molecule) has nested. While idealized, those views highlight different aspects of real grain boundaries. Implications on macroscopic charge transport models are discussed, as well as some relation between growth conditions and the formation of the grain boundary.

Atomistic simulations of dislocation pileup: Grain boundaries interaction

DOE PAGES

Wang, Jian

2015-05-27

Here, using molecular dynamics (MD) simulations, we studied the dislocation pileup–grain boundary (GB) interactions. Two Σ11 asymmetrical tilt grain boundaries in Al are studied to explore the influence of orientation relationship and interface structure on dislocation activities at grain boundaries. To mimic the reality of a dislocation pileup in a coarse-grained polycrystalline, we optimized the dislocation population in MD simulations and developed a predict-correct method to create a dislocation pileup in MD simulations. MD simulations explored several kinetic processes of dislocations–GB reactions: grain boundary sliding, grain boundary migration, slip transmission, dislocation reflection, reconstruction of grain boundary, and the correlation ofmore » these kinetic processes with the available slip systems across the GB and atomic structures of the GB.« less

Migration of grain boundaries and triple junctions in high-purity aluminum during annealing after slight cold rolling

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yin, Wenhong; School of Mechanical Engineering, Shandong University of Technology, Zibo 255049; Wang, Weiguo, E-mail: wang_weiguo@vip.163.com

Grain orientations and grain boundary migrations near triple junctions in a high purity aluminum were analyzed by electron back scattered diffraction. The results indicate that there are good correlations between the Schmid factors or Taylor factors and the misorientation values of point to original point in grains near the triple junctions in a slightly deformed sample. Grains with higher Schmid factors or lower Taylor factors typically correspond to higher misorientation values near the triple junctions. In a subsequent annealing at 400 °C, both grain boundaries and triple junctions migrate, but the former leave ghost lines. During such migration, a grainmore » boundary grows from the grain with lower Schmid factor (higher Taylor factor) into the grain with higher Schmid factor (lower Taylor factor). Usually, the amount of migration of a grain boundary is considerably greater than that of a triple junction, and the grain boundary becomes more curved after migration. These observations indicate that the triple junctions have drag effects on grain boundary migration. - Highlights: • Polycrystalline aluminum with fine grains about 30 μm were used. • Off-line in situ EBSD was used to identify TJs before and after annealing. • Grains with higher SFs have higher misorientation values near TJs after deformation. • Grain boundaries grow from hard grains into soft grains during annealing. • Triple junctions have drag effects on grain boundaries migration.« less

Effects of Intergranular Gas Bubbles on Thermal Conductivity

DOE Office of Scientific and Technical Information (OSTI.GOV)

K. Chockalingam; Paul C. Millett; M. R. Tonks

2012-11-01

Model microstructures obtained from phase-field simulations are used to study the effective heat transfer across bicrys- tals with stationary grain boundary bubble populations. We find that the grain boundary coverage, irrespective of the intergranular bubble radii, is the most relevant parameter to the thermal resistance, which we use to derive effec- tive Kapitza resistances that are dependent on the grain boundary coverage and Kaptiza resistance of the intact grain boundary. We propose a model to predict thermal conductivity as a function of porosity, grain-size, Kaptiza resistance of the intact grain boundary, and grain boundary bubble coverage.

Chemical signature of a migrating grain boundaries in polycrystalline olivine

NASA Astrophysics Data System (ADS)

Boneh, Y.; Marquardt, K.; Skemer, P. A.

2017-12-01

Olivine is the most abundant phase and influences strongly the physical and chemical properties of the upper mantle. The structure and chemistry of olivine grain-boundaries is important to understand, as these interfaces provide a reservoir for incompatible elements and partial melt, and serve as a fast pathway for chemical diffusion. This project investigates the chemical characteristics of grain boundaries in an olivine-rich aggregate. The sample is composed of Fo50 olivine crystals with minor amounts of enstatite. It was previously deformed (Hansen et al., 2016) and then annealed (Boneh et al., 2017) to investigate the microstructural changes during recrystallization. This transient microstructure has a bimodal grain size distribution and includes grains that experienced abnormal grain-growth, (porphyroblasts) and highly strained grains with no significant recrystallization or growth (matrix). Using high-resolution transmission electron microscopy (HR-TEM) with energy dispersive X-ray (EDX) at the Bayerisches Geoinstitut (BGI), we characterized boundaries between pairs of porphyroblasts, pairs of matrix grains, and mixed boundaries between porphyroblast and matrix grains. It was found that the boundary between porphyroblasts is enriched in Al and Ca and depleted in Mg, in comparison to grain interiors. However, matrix-matrix boundaries show less chemical segregation of these elements. The relatively high level of chemical segregation to porphyroblast grain boundaries offers different possible interpretations: 1) During grain boundary migration incompatible elements are swept up by the migrating grain boundary. 2) Large angle grain boundaries provide a large density of energetically favorable storage sites for incompatible elements. 3) Diffusion along low angle grain boundaries is too slow to allow for fast chemical equilibration between the different grain boundaries. 4) Dislocations cores serve as an important transport media for impurities (i.e., Cottrell atmosphere). We will further discuss these different interpretations, their feasibility, and implications for the geochemistry of the mantle.

Electrical properties of polycrystalline olivine: evidence for grain boundary transport

NASA Astrophysics Data System (ADS)

Ten Grotenhuis, S. M.; Drury, M. R.; Peach, C. J.; Spiers, C. J.

2003-12-01

The physical and chemical properties of grain boundaries are known to play an important role in determining the electrical properties of polycrystalline oxides. Grain boundaries can either enhance conductivity if the transport of charge carriers along the grain boundaries is faster than through the lattice, or grain boundaries can reduce conductivity if the grain boundaries block the transport of charge carriers. The purpose of the experiments presented here is to deduce the mechanisms responsible for electrical conductivity in fine-grained forsterite, the Mg-end member of olivine, in order to get a better understanding of the contribution of grain boundary transport, of the properties of the grain boundaries, and to determine any relation between grain size and conductivity. A relationship between grain size and conductivity at high temperature could potentially be used to interpret zones of anomalous conductivity in the upper mantle. The materials studied consist of fine-grained forsterite (Mg2SiO4) with a minor amount (5%) of enstatite (MgSiO3) added. The electrical conductivity of three melt-free synthetic polycrystalline samples, with grain sizes between 1.1 and 4.7 mm, was measured at temperatures up to 1470° C. The complex impedance plots display one clear arc, indicating a single dominant conduction mechanism. Bulk conductivity is inversely proportional to the grain size of the different samples. This relation suggests that grain boundary diffusion of the charge carriers is controlling the electrical conductivity of the samples. The activation energy for diffusion of the charge carriers lies between 315 and 323 kJ/mol. This resembles previous data on grain boundary diffusion of Mg in forsterite and grain boundary diffusion creep. A geometrical model of less conducting cubic grains and more conducting grain boundaries agrees well with the experimental data. This model is applied to a natural mantle shear zone to predict the conductivity contrast between fine-grained shear zones and less deformed regions in the lithosphere. Upper mantle shear zones are predicted to have 1.5 to 2 orders of magnitude higher conductivity than less deformed regions in the lithosphere. This may mean that fine-grained shear zones can be detected using magnetotelluric methods.

Three dimensional grain boundary modeling in polycrystalline plasticity

NASA Astrophysics Data System (ADS)

Yalçinkaya, Tuncay; Özdemir, Izzet; Fırat, Ali Osman

2018-05-01

At grain scale, polycrystalline materials develop heterogeneous plastic deformation fields, localizations and stress concentrations due to variation of grain orientations, geometries and defects. Development of inter-granular stresses due to misorientation are crucial for a range of grain boundary (GB) related failure mechanisms, such as stress corrosion cracking (SCC) and fatigue cracking. Local crystal plasticity finite element modelling of polycrystalline metals at micron scale results in stress jumps at the grain boundaries. Moreover, the concepts such as the transmission of dislocations between grains and strength of the grain boundaries are not included in the modelling. The higher order strain gradient crystal plasticity modelling approaches offer the possibility of defining grain boundary conditions. However, these conditions are mostly not dependent on misorientation of grains and can define only extreme cases. For a proper definition of grain boundary behavior in plasticity, a model for grain boundary behavior should be incorporated into the plasticity framework. In this context, a particular grain boundary model ([l]) is incorporated into a strain gradient crystal plasticity framework ([2]). In a 3-D setting, both bulk and grain boundary models are implemented as user-defined elements in Abaqus. The strain gradient crystal plasticity model works in the bulk elements and considers displacements and plastic slips as degree of freedoms. Interface elements model the plastic slip behavior, yet they do not possess any kind of mechanical cohesive behavior. The physical aspects of grain boundaries and the performance of the model are addressed through numerical examples.

Grain size engineering for ferroelectric Hf{sub 0.5}Zr{sub 0.5}O{sub 2} films by an insertion of Al{sub 2}O{sub 3} interlayer

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kim, Han Joon; Park, Min Hyuk; Kim, Yu Jin

2014-11-10

The degradation of ferroelectric (FE) properties of atomic layer deposited Hf{sub 0.5}Zr{sub 0.5}O{sub 2} films with increasing thickness was mitigated by inserting 1 nm-thick Al{sub 2}O{sub 3} interlayer at middle position of the thickness of the FE film. The large P{sub r} of 10 μC/cm{sup 2}, which is 11 times larger than that of single layer Hf{sub 0.5}Zr{sub 0.5}O{sub 2} film with equivalent thickness, was achieved from the films as thick as 40 nm. The Al{sub 2}O{sub 3} interlayer could interrupt the continual growth of Hf{sub 0.5}Zr{sub 0.5}O{sub 2} films, and the resulting decrease of grain size prevented the formation of non-ferroelectricmore » monoclinic phase. The Al{sub 2}O{sub 3} interlayer also largely decreased the leakage current of the Hf{sub 0.5}Zr{sub 0.5}O{sub 2} films.« less

Grain boundary engineering: fatigue fracture

NASA Astrophysics Data System (ADS)

Das, Arpan

2017-04-01

Grain boundary engineering has revealed significant enhancement of material properties by modifying the populations and connectivity of different types of grain boundaries within the polycrystals. The character and connectivity of grain boundaries in polycrystalline microstructures control the corrosion and mechanical behaviour of materials. A comprehensive review of the previous researches has been carried out to understand this philosophy. Present research thoroughly explores the effect of total strain amplitude on phase transformation, fatigue fracture features, grain size, annealing twinning, different grain connectivity and grain boundary network after strain controlled low cycle fatigue deformation of austenitic stainless steel under ambient temperature. Electron backscatter diffraction technique has been used extensively to investigate the grain boundary characteristics and morphologies. The nominal variation of strain amplitude through cyclic plastic deformation is quantitatively demonstrated completely in connection with the grain boundary microstructure and fractographic features to reveal the mechanism of fatigue fracture of polycrystalline austenite. The extent of boundary modifications has been found to be a function of the number of applied loading cycles and strain amplitudes. It is also investigated that cyclic plasticity induced martensitic transformation strongly influences grain boundary characteristics and modifications of the material's microstructure/microtexture as a function of strain amplitudes. The experimental results presented here suggest a path to grain boundary engineering during fatigue fracture of austenite polycrystals.

Grain boundary crystallography in polycrystalline yttria-stabilised cubic zirconia

NASA Astrophysics Data System (ADS)

Kini, Maya K.

2018-07-01

Properties of grain boundaries such as grain boundary energy, mobility and diffusion are reported to depend strongly on their crystallography. While studies on ceramic bicrystals with low Σ misorientations have shown highly ordered structures and low energies, studies on dense polycrystalline ceramics often show the significance of grain boundary planes. In the present study, grain boundary plane distributions were studied for yttria-stabilised cubic zirconia with varying grain sizes using Electron Back Scattered Diffraction technique combined with a stereological approach. Despite nearly isotropic grain boundary plane distributions, a highly anisotropic grain boundary character distribution is observed for specific misorientations. Certain low-energy symmetric tilts such as Σ3 and Σ11 are found to occur with high frequencies across the grain size range studied, leading to an inverse correlation between GB energy and frequency of occurrence, consistent with other ceramics studied in literature.

Re-exchange of Fe and Cu at the interface in sintered Nd-Fe-B magnets: A method to eliminate Fe precipitation at grain boundaries

NASA Astrophysics Data System (ADS)

Yang, YuQi; Si, HengGang; Yang, Hao; Zhang, Lan; Huang, DongFang; Chen, BaiYi; Xu, Fang; Hu, YongMei; Han, BaoJun

2018-01-01

According to the decoupling hypothesis for magnetic grains, the coercivity in sintered Nd-Fe-B magnets is increased after Cu doping, which is due to the formation of non-magnetic grain boundaries. However, this method partially fails, and ferromagnetic Fe-segregation occurs at the grain boundary. We discovered both experimentally and through calculation that the Fe content at the grain boundaries can be tuned across a wide range by introducing another element of Ag. Segregated Fe at high temperature at the grain boundary re-dissolves into Nd2Fe14B grains during annealing at low temperature. Both configurable and magnetic entropies contribute a large driving force for the formation of nonmagnetic grain boundaries. Almost zero Fe content could be achieved at the grain boundaries of sintered Nd-Fe-B magnet.

The Formation of Boundary Clinopyroxenes and Associated Glass Veins in Type B1 CAIs

DOE Office of Scientific and Technical Information (OSTI.GOV)

Paque, J M; Beckett, J R; Ishii, H A

2008-05-18

We used focused ion beam thin section preparation and scanning transmission electron microscopy (FIB/STEM) to examine the interfacial region between spinel and host melilite for three spinel grains, two from the mantle and one from the core of an Allende type B1 inclusion, and a second pair of spinel grains from a type B1 inclusion from the Leoville carbonaceous chondrite. The compositions of boundary clinopyroxenes decorating spinel surfaces are generally consistent with those of coarser clinopyroxenes from the same region of the inclusion, suggesting little movement of spinels between mantle and core regions after the formation of boundary clinopyroxenes. Themore » host melilite displays no anomalous compositions near the interface, and anorthite or other late-stage minerals are not observed, suggesting that crystallization of residual liquid was not responsible for the formation of boundary clinopyroxenes. Allende spinels display either direct spinel-melilite contact or an intervening boundary clinopyroxene between the two phases. In the core, boundary clinopyroxene is mantled by a thin (1-2 {micro}m thick) layer of normally zoned (X{sub Ak} increasing away from the melilite-clinopyroxene contact) melilite with X{sub Ak} matching that of the host melilite at the melilite-melilite contact. In the mantle, X{sub Ak} near boundary spinels is constant. Spinels in a Leoville type B1 inclusion are more complex with boundary clinopyroxene, as observed in Allende, but also variable amounts of glass ({approx}1 {micro}m width), secondary calcite, perovskite, and an unknown Mg-, Al-, OH-rich and Ca-, Si-poor crystalline phase that may be a layered double hydrate. Glass compositions are consistent to first order with a precursor consisting mostly of Mg-carpholite or sudoite with some aluminous diopside. One possible scenario of formation for the glass veins is that open system alteration of melilite produced a porous, hydrated aggregate of Mg-carpholite or sudoite + aluminous diopside that was shock melted and quenched to a glass. The unknown crystalline phase may be a shocked remnant of the precursor phase assemblage but is more likely to have formed later by alteration of the glass. Calcite appears to be an opportunistic fracture filling that postdated all major shock events. Boundary clinopyroxenes probably share a common origin with coarser-grained pyroxenes from the same region of the inclusion. In the mantle, these crystals may represent clinopyroxene crystallized in Ti-rich liquids caused by the direct dissolution of perovskite and an associated Sc-Zr-rich phase or as a reaction product between dissolving perovskite and liquid (i.e., indirect dissolution of perovskite). In the core, any perovskite and associated Ti-enriched liquids that may have originally been present disappeared before the growth of boundary clinopyroxene.« less

Algorithm based on regional separation for automatic grain boundary extraction using improved mean shift method

NASA Astrophysics Data System (ADS)

Zhenying, Xu; Jiandong, Zhu; Qi, Zhang; Yamba, Philip

2018-06-01

Metallographic microscopy shows that the vast majority of metal materials are composed of many small grains; the grain size of a metal is important for determining the tensile strength, toughness, plasticity, and other mechanical properties. In order to quantitatively evaluate grain size in metals, grain boundaries must be identified in metallographic images. Based on the phenomenon of grain boundary blurring or disconnection in metallographic images, this study develops an algorithm based on regional separation for automatically extracting grain boundaries by an improved mean shift method. Experimental observation shows that the grain boundaries obtained by the proposed algorithm are highly complete and accurate. This research has practical value because the proposed algorithm is suitable for grain boundary extraction from most metallographic images.

The hot deformation behavior and microstructure evolution of HA/Mg-3Zn-0.8Zr composites for biomedical application.

PubMed

Liu, Debao; Liu, Yichi; Zhao, Yue; Huang, Y; Chen, Minfang

2017-08-01

The hot deformation behavior of nano-sized hydroxylapatite (HA) reinforced Mg-3Zn-0.8Zr composites were performed by means of Gleeble-1500D thermal simulation machine in a temperature range of 523-673K and a strain rate range of 0.001-1s -1 , and the microstructure evolution during hot compression deformation were also investigated. The results show that the flow stress increases increasing strain rates at a constant temperature, and decreases with increasing deforming temperatures at a constant strain rate. Under the same processing conditions, the flow stresses of the 1HA/Mg-3Zn-0.8Zr specimens are higher than those of the Mg-3Zn-0.8Zr alloy specimens, and the difference is getting closer with increasing deformation temperature. The hot deformation behaviors of Mg-3Zn-0.8Zr and 1HA/Mg-3Zn-0.8Zr can be described by constitutive equation of hyperbolic sine function with the hot deformation activation energy being 124.6kJ/mol and 125.3kJ/mol, respectively. Comparing with Mg-3Zn-0.8Zr alloy, the instability region in the process map of 1HA/Mg-3Zn-0.8Zr expanded to a bigger extent at the same conditions. The optimum process conditions of 1HA/Mg-3Zn-0.8Zr composite is concluded as between the temperature window of 573-623K with a strain rate range of 0.001-0.1s -1 . A higher volume fraction and smaller grain size of dynamic recrystallization (DRX) grains was observed in 1HA/Mg-3Zn-0.8Zr specimens after the hot compression deformation compared with Mg-3Zn-0.8Zr alloy, which was ascribed to the presence of the HA particles that play an important role in particle-stimulated nucleation (PSN) mechanism and can effectively hinder the migration of interfaces. Copyright © 2017 Elsevier B.V. All rights reserved.

Grain boundary oxidation and its effects on high temperature fatigue life

NASA Technical Reports Server (NTRS)

Liu, H. W.; Oshida, Yoshiki

1986-01-01

Fatigue lives at elevated temperatures are often shortened by creep and/or oxidation. Creep causes grain boundary void nucleation and grain boundary cavitation. Grain boundary voids and cavities will accelerate fatigue crack nucleation and propagation, and thereby shorten fatigue life. The functional relationships between the damage rate of fatigue crack nucleation and propagation and the kinetic process of oxygen diffusion depend on the detailed physical processes. The kinetics of grain boundary oxidation penetration was investigated. The statistical distribution of grain boundary penetration depth was analyzed. Its effect on high temperature fatigue life are discussed. A model of intermittent micro-ruptures of grain boundary oxide was proposed for high temperature fatigue crack growth. The details of these studies are reported.

Magnetic properties and microstructure of gas atomized MRE2(Fe, Co)14B powder with ZrC addition (MRE=Nd + Y + Dy)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tang, W.; Wu, Y. Q.; Dennis, K.

2009-05-12

Gas atomization powder with Zr substitutions for the MRE and ZrC additions were systematically studied. The results show that the partial substitutions of Zr and the ZrC additions effectively improved glass formability in the alloys. Scanning electron microscopy (SEM) revealed that the as-atomized powder with a particle size of less than 32 {micro}m is predominately uniform equiaxed grains with an average grain size of 1.5 {micro}m. X-ray diffraction and differential thermal analysis measurements detected very tiny amounts of amorphous phase. After annealing at 700 C for 15 min, the SEM grain microstructure exhibits a minor change, but magnetic properties aremore » substantially improved. M versus T measurements reveal that the phase composition evolved from 2:14:1 plus a small amount of 2:17 phases to a single 2:14:1 phase during the annealing process. The sieve analysis of the powders showed a particle size distribution with 90 wt % of the powder less than 45 {micro}m. The magnetic properties of the annealed powder varied with particle size. (BH){sub max} first increases with increasing particle size from 5 {micro}m, reaches the peak value in the size range of 20-25 {micro}m, and then decreases with increasing particle size. For the 20-25 {micro}m powder sample annealed at 700 C for 15 min, the (BH){sub max} of 9.6 MG Oe at room temperature and 5.6 MG Oe at 200 C were obtained, respectively.« less

The neutron capture process in the He shell in core-collapse supernovae: Presolar silicon carbide grains as a diagnostic tool for nuclear astrophysics

NASA Astrophysics Data System (ADS)

Pignatari, Marco; Hoppe, Peter; Trappitsch, Reto; Fryer, Chris; Timmes, F. X.; Herwig, Falk; Hirschi, Raphael

2018-01-01

Carbon-rich presolar grains are found in primitive meteorites, with isotopic measurements to date suggesting a core-collapse supernovae origin site for some of them. This holds for about 1-2% of presolar silicon carbide (SiC) grains, so-called Type X and C grains, and about 30% of presolar graphite grains. Presolar SiC grains of Type X show anomalous isotopic signatures for several elements heavier than iron compared to the solar abundances: most notably for strontium, zirconium, molybdenum, ruthenium and barium. We study the nucleosynthesis of zirconium and molybdenum isotopes in the He-shell of three core-collapse supernovae models of 15, 20 and 25 M⊙ with solar metallicity, and compare the results to measurements of presolar grains. We find the stellar models show a large scatter of isotopic abundances for zirconium and molybdenum, but the mass averaged abundances are qualitatively similar to the measurements. We find all models show an excess of 96Zr relative to the measurements, but the model abundances are affected by the fractionation between Sr and Zr since a large contribution to 90Zr is due to the radiogenic decay of 90Sr. Some supernova models show excesses of 95,97Mo and depletion of 96Mo relative to solar. The mass averaged distribution from these models shows an excess of 100Mo, but this may be alleviated by very recent neutron-capture cross section measurements. We encourage future explorations to assess the impact of the uncertainties in key neutron-capture reaction rates that lie along the n-process path.

Correlation between grain boundary misorientation and M{sub 23}C{sub 6} precipitation behaviors in a wrought Ni-based superalloy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tang, Bin, E-mail: toby198489@163.com; Jiang, Li; Hu, Rui

2013-04-15

The correlation between the grain boundary misorientation and the precipitation behaviors of intergranular M{sub 23}C{sub 6} carbides in a wrought Ni–Cr–W superalloy was investigated by using the electron backscattered diffraction (EBSD) technique. It was observed that the grain boundaries with a misorientation angle less than 20°, as well as all coincidence site lattice (CSL) boundaries, are immune to precipitation of the M{sub 23}C{sub 6} carbides; in contrast, the random high-angle grain boundaries with a misorientation angle of 20°–40° provide preferential precipitation sites of the M{sub 23}C{sub 6} carbides at the random high-angle grain boundaries with a higher misorientation angle ofmore » 55°–60°/[2 2 3] turn to retard precipitation of M{sub 23}C{sub 6} carbides owing to their nature like the Σ3 grain boundaries and retard the precipitation of M{sub 23}C{sub 6} carbides. The low-angle and certain random grain boundary segments induced by twins were found to interrupt the precipitation of the M{sub 23}C{sub 6} carbides along the high-angle grain boundaries. - Highlights: ► The low angle grain boundaries and CSL boundaries are immune to precipitation. ► M23C6 precipitate preferentially at random grain boundaries within 20°–40°. ► Some certain random grain boundary segments interrupt M23C6 precipitation.« less

On the role of grain boundary character distribution in grain growth of Al-Mg alloys

DOE Office of Scientific and Technical Information (OSTI.GOV)

Matsumoto, K.; Shibayanagi, T.; Umakoshi, Y.

1997-02-01

Grain growth behavior of recrystallized Al-Mg alloys containing 0.3 and 2.7 mass% Mg was investigated, focusing on the interconnection between development of the texture and grain boundary character distribution. An Al-0.3 mass% Mg alloy showed two stages in the change of microstructure during grain growth: the frequency of cube oriented grains and the {Sigma}1 boundary significantly increased at an early stage and then decreased. In the second stage a small amount of isolated large grains with the non-cube component grew and consumed the surrounding cube grains. In contrast, the frequency of cube oriented grains and the grain boundary character distributionmore » showed no significant change during grain growth of Al-2.7 mass% Mg. Small clusters composed of several cube grains containing {Sigma}1 boundaries were formed and their spatial distribution played an important role in the change of microstructure during grain growth. The effect of the spatial distribution on the grain growth behavior was discussed considering the energy balance at triple junctions of grain boundaries.« less

Nature-Inspired Capillary-Driven Welding Process for Boosting Metal-Oxide Nanofiber Electronics.

PubMed

Meng, You; Lou, Kaihua; Qi, Rui; Guo, Zidong; Shin, Byoungchul; Liu, Guoxia; Shan, Fukai

2018-06-20

Recently, semiconducting nanofiber networks (NFNs) have been considered as one of the most promising platforms for large-area and low-cost electronics applications. However, the high contact resistance among stacking nanofibers remained to be a major challenge, leading to poor device performance and parasitic energy consumption. In this report, a controllable welding technique for NFNs was successfully demonstrated via a bioinspired capillary-driven process. The interfiber connections were well-achieved via a cooperative concept, combining localized capillary condensation and curvature-induced surface diffusion. With the improvements of the interfiber connections, the welded NFNs exhibited enhanced mechanical property and high electrical performance. The field-effect transistors (FETs) based on the welded Hf-doped In 2 O 3 (InHfO) NFNs were demonstrated for the first time. Meanwhile, the mechanisms involved in the grain-boundary modulation for polycrystalline metal-oxide nanofibers were discussed. When the high-k ZrO x dielectric thin films were integrated into the FETs, the field-effect mobility and operating voltage were further improved to be 25 cm 2 V -1 s -1 and 3 V, respectively. This is one of the best device performances among the reported nanofibers-based FETs. These results demonstrated the potencies of the capillary-driven welding process and grain-boundary modulation mechanism for metal-oxide NFNs, which could be applicable for high-performance, large-scale, and low-power functional electronics.

Energetics and structural properties of twist grain boundaries in Cu

NASA Technical Reports Server (NTRS)

Karimi, Majid

1992-01-01

Structural and energetics properties of atoms near a grain boundary are of great importance from theoretical and experimental standpoints. From various experimental work it is concluded that diffusion at low temperatures at polycrystalline materials take place near grain boundary. Experimental and theoretical results also indicate changes of up to 70 percent in physical properties near a grain boundary. The Embedded Atom Method (EAM) calculations on structural properties of Au twist grain boundaries are in quite good agreement with their experimental counterparts. The EAM is believed to predict reliable values for the single vacancy formation energy as well as migration energy. However, it is not clear whether the EAM functions which are fitted to the bulk properties of a perfect crystalline solid can produce reliable results on grain boundaries. One of the objectives of this work is to construct the EAM functions for Cu and use them in conjunction with the molecular static simulation to study structures and energetics of atoms near twist grain boundaries in Cu. This provides tests of the EAM functions near a grain boundary. In particular, we determine structure, single vacancy formation energy, migration energy, single vacancy activation energy, and interlayer spacing as a function of distance from grain boundary. Our results are compared with the available experimental and theoretical results from grain boundaries and bulk.

On the equilibrium charge density at tilt grain boundaries

NASA Astrophysics Data System (ADS)

Srikant, V.; Clarke, D. R.

1998-05-01

The equilibrium charge density and free energy of tilt grain boundaries as a function of their misorientation is computed using a Monte Carlo simulation that takes into account both the electrostatic and configurational energies associated with charges at the grain boundary. The computed equilibrium charge density increases with the grain-boundary angle and approaches a saturation value. The equilibrium charge density at large-angle grain boundaries compares well with experimental values for large-angle tilt boundaries in GaAs. The computed grain-boundary electrostatic energy is in agreement with the analytical solution to a one-dimensional Poisson equation at high donor densities but indicates that the analytical solution overestimates the electrostatic energy at lower donor densities.

Additive Manufacturing of Reactive In Situ Zr Based Ultra-High Temperature Ceramic Composites

NASA Astrophysics Data System (ADS)

Sahasrabudhe, Himanshu; Bandyopadhyay, Amit

2016-03-01

Reactive in situ multi-material additive manufacturing of ZrB2-based ultra-high-temperature ceramics in a Zr metal matrix was demonstrated using LENS™. Sound metallurgical bonding was achieved between the Zr metal and Zr-BN composites with Ti6Al4V substrate. Though the feedstock Zr power had α phase, LENS™ processing of the Zr powder and Zr-BN premix powder mixture led to the formation of some β phase of Zr. Microstructure of the Zr-BN composite showed primary grains of zirconium diboride phase in zirconium metal matrix. The presence of ZrB2 ceramic phase was confirmed by X-ray diffraction (XRD) analysis. Hardness of pure Zr was measured as 280 ± 12 HV and, by increasing the BN content in the feedstock, the hardness was found to increase. In Zr-5%BN composite, the hardness was 421 ± 10 HV and the same for Zr-10%BN composite was 562 ± 10 HV. It is envisioned that such multi-materials additive manufacturing will enable products in the future that cannot be manufactured using traditional approaches particularly in the areas of high-temperature metal-ceramic composites with compositional and functional gradation.

Processing and electrical properties of gallium-substituted lead zirconate titanate ceramics

NASA Astrophysics Data System (ADS)

Hajra, Sugato; Sharma, Pulkit; Sahoo, Sushrisangita; Rout, P. K.; Choudhary, R. N. P.

2017-12-01

In the present paper, the effect of gallium (Ga) substitution on structural, microstructural, electrical conductivity of Pb(ZrTi)O3 (PZT) in the morphotropic phase boundary (MPB) region (i.e., Pb0.96Ga0.04(Zr0.48Ti0.52)0.99O3 (PGaZT-4)) was investigated. Increased grain density increases the resistivity of the Ga-modified PZT system. Preliminary structural analysis using X-ray diffraction pattern and data showed the existence of two phases [major tetragonal (T) and minor monoclinic (M)]. Field emission scanning electron micrograph (FESEM) showed the distribution of spherical as well as platelet type grains with small pores. The behavior of dielectric constant with temperature of PGaZT-4 exhibited the suppression of the ferroelectric phase transition [i.e., disappearance of Curie temperature ( T c)]. The complex impedance spectroscopy (CIS) technique helped to investigate the impedance parameters of PGaZT-4 in MPB region in a wide range of temperature (250-500 °C) and frequency (1-1000 kHz) region. The impedance parameters of the material are found to be strongly dependent on frequency of AC electric field and temperature. The substitution of gallium at the Pb site of PZT generally enhances the dielectric constant and decreases loss tangent. The AC conductivity vs frequency ( f = ω2 π) in the region of dispersion follows the universal response of Jonscher's equation. Enhanced resistive characteristics were observed for Ga-substituted PZT in comparison to the pure PZT, which was well ensured from the studies of electrical parameters, such as impedance and AC conductivity.

Glass formation and crystallization in high-temperature glass-ceramics and Si3N4

NASA Technical Reports Server (NTRS)

Drummond, Charles H., III

1991-01-01

The softening of glassy grain boundaries in ceramic matrix composites and Si3N4 at high temperatures reduces mechanical strength and the upper-use temperature. By crystallizing this glass to a more refractory crystalline phase, a material which performs at higher temperatures may result. Three systems were examined: a cordierite composition with ZrO2 as a nucleating agent; celsian compositions; and yttrium silicate glasses both in bulk and intergranular in Si3N4. For the cordierite compositions, a series of metastable phases was obtained. The crystallization of these compositions was summarized in terms of metastable ternary isothermal sections. Zircon formed at the expense of ZrO2 and spinel. In SiC composites, the transformations were slower. In celsian, two polymorphs were crystallized. One phase, hexacelsian, which always crystallized, even when metastable, had an undesirable volume change. The other phase, celsian, was very difficult to crystallize. In yttrium silicate bulk glasses, similar in composition to the intergranular glass in Si3N4, a number of polymorphs of Y2Si2O7 were crystallized. The conditions under which these polymorphs formed are compared with crystallization in Si3N4.

Nanoionics and Nanocatalysts: Conformal Mesoporous Surface Scaffold for Cathode of Solid Oxide Fuel Cells

PubMed Central

Chen, Yun; Gerdes, Kirk; Song, Xueyan

2016-01-01

Nanoionics has become increasingly important in devices and systems related to energy conversion and storage. Nevertheless, nanoionics and nanostructured electrodes development has been challenging for solid oxide fuel cells (SOFCs) owing to many reasons including poor stability of the nanocrystals during fabrication of SOFCs at elevated temperatures. In this study, a conformal mesoporous ZrO2 nanoionic network was formed on the surface of La1−xSrxMnO3/yttria-stabilized zirconia (LSM/YSZ) cathode backbone using Atomic Layer Deposition (ALD) and thermal treatment. The surface layer nanoionic network possesses open mesopores for gas penetration, and features a high density of grain boundaries for enhanced ion-transport. The mesoporous nanoionic network is remarkably stable and retains the same morphology after electrochemical operation at high temperatures of 650–800 °C for 400 hours. The stable mesoporous ZrO2 nanoionic network is further utilized to anchor catalytic Pt nanocrystals and create a nanocomposite that is stable at elevated temperatures. The power density of the ALD modified and inherently functional commercial cells exhibited enhancement by a factor of 1.5–1.7 operated at 0.8 V at 750 °C. PMID:27605121

Photoconductivity induced by nanoparticle segregated grain-boundary in spark plasma sintered BiFeO3

NASA Astrophysics Data System (ADS)

Nandy, Subhajit; Mocherla, Pavana S. V.; Sudakar, C.

2017-05-01

Photoconductivity studies on spark plasma sintered BiFeO3 samples with two contrasting morphologies, viz., nanoparticle-segregated grain boundary (BFO-AP) and clean grain boundary (BFO-AA), show that their photo-response is largely influenced by the grain boundary defects. Impedance analyses at 300 K and 573 K clearly demarcate the contributions from grain, grain-boundary, and the nanoparticle-segregated grain-boundary conductivities. I-V characteristics under 1 sun illumination show one order of higher conductivity for BFO-AP, whereas conductivity decreases for BFO-AA sample. Larger photocurrent in BFO-AP is attributed to the extra conduction path provided by oxygen vacancies on the nanoparticle surfaces residing at the grain boundaries. Creation of photo-induced traps under illumination and the absence of surface conduction channels in BFO-AA are surmised to result in a decreased conductivity on illumination.

Grain-Boundary Roughening in Colloidal Crystals

NASA Astrophysics Data System (ADS)

Liao, Maijia; Xiao, Xiao; Chui, Siu Tat; Han, Yilong

2018-04-01

In polycrystals, faceted grains may become round and rough at high temperatures. Such a roughening phenomenon remains poorly understood, partly because of the lack of experimental observations. Here, we directly visualize the roughening dynamics of grain boundaries inside thin-film colloidal crystals at the single-particle level using video microscopy. The thermal fluctuations of grain boundaries appear to exhibit both static and dynamic critical-like behaviors, in contrast to the Kosterlitz-Thouless transition in typical free surface roughening. The roughening point shifts towards the melting point as the grain boundary's mismatch angle θ decreases and is preempted by melting when θ <18 ° . Counterintuitively, the amplitude of grain-boundary fluctuations decreases above the roughening point. This could be attributed to the observed widening of the grain boundary. The roughening strongly affects the mobility of the grain boundary but not the stiffness. These results provide new guidance for the control of microstructures in polycrystals and further development of roughening theory.

Continuum understanding of twin formation near grain boundaries of FCC metals with low stacking fault energy

NASA Astrophysics Data System (ADS)

Jung, Jaimyun; Yoon, Jae Ik; Kim, Jung Gi; Latypov, Marat I.; Kim, Jin You; Kim, Hyoung Seop

2017-12-01

Deformation twinning from grain boundaries is often observed in face-centered cubic metals with low stacking fault energy. One of the possible factors that contribute to twinning origination from grain boundaries is the intergranular interactions during deformation. Nonetheless, the influence of mechanical interaction among grains on twin evolution has not been fully understood. In spite of extensive experimental and modeling efforts on correlating microstructural features with their twinning behavior, a clear relation among the large aggregate of grains is still lacking. In this work, we characterize the micromechanics of grain-to-grain interactions that contribute to twin evolution by investigating the mechanical twins near grain boundaries using a full-field crystal plasticity simulation of a twinning-induced plasticity steel deformed in uniaxial tension at room temperature. Microstructures are first observed through electron backscatter diffraction technique to obtain data to reconstruct a statistically equivalent microstructure through synthetic microstructure building. Grain-to-grain micromechanical response is analyzed to assess the collective twinning behavior of the microstructural volume element under tensile deformation. Examination of the simulated results reveal that grain interactions are capable of changing the local mechanical behavior near grain boundaries by transferring strain across grain boundary or localizing strain near grain boundary.

The effect of heat treatment on the performance of the Ni/(Zr-Sm oxide) catalysts for carbon dioxide methanation

NASA Astrophysics Data System (ADS)

Takano, Hiroyuki; Izumiya, Koichi; Kumagai, Naokazu; Hashimoto, Koji

2011-07-01

The active catalysts for methane formation from the gas mixture of CO 2 + 4H 2 with almost 100% methane selectivity were prepared by reduction of the oxide mixture of NiO and ZrO 2 prepared by calcination of aqueous ZrO 2 sol with Sm(NO 3) 3 and Ni(NO 3) 2. The 50 at%Ni-50 at%(Zr-Sm oxide) catalyst consisting of 50 at%Ni-50 at%(Zr + Sm) with Zr/Sm = 5 calcined at 650 or 800 °C showed the highest activity for methanation. The active catalysts were Ni supported on tetragonal ZrO 2, and the activity for methanation increased by an increase in inclusion of Sm 3+ ions substituting Zr 4+ ions in the tetragonal ZrO 2 lattice as a result of an increase in calcination temperature. However, the increase in calcination temperature decreased BET surface area, metal dispersion and hydrogen uptake due to grain growth. Thus, the optimum calcination temperature existed.

Grain boundary character distribution in nanocrystalline metals produced by different processing routes

DOE PAGES

Bober, David B.; Kumar, Mukal; Rupert, Timothy J.; ...

2015-12-28

Nanocrystalline materials are defined by their fine grain size, but details of the grain boundary character distribution should also be important. Grain boundary character distributions are reported for ball-milled, sputter-deposited, and electrodeposited Ni and Ni-based alloys, all with average grain sizes of ~20 nm, to study the influence of processing route. The two deposited materials had nearly identical grain boundary character distributions, both marked by a Σ3 length percentage of 23 to 25 pct. In contrast, the ball-milled material had only 3 pct Σ3-type grain boundaries and a large fraction of low-angle boundaries (16 pct), with the remainder being predominantlymore » random high angle (73 pct). Furthermore, these grain boundary character measurements are connected to the physical events that control their respective processing routes. Consequences for material properties are also discussed with a focus on nanocrystalline corrosion. As a whole, the results presented here show that grain boundary character distribution, which has often been overlooked in nanocrystalline metals, can vary significantly and influence material properties in profound ways.« less

Determination of the five parameter grain boundary character distribution of nanocrystalline alpha-zirconium thin films using transmission electron microscopy

DOE PAGES

Ghamarian, I.; Samani, P.; Rohrer, G. S.; ...

2017-03-24

Grain boundary engineering and other fundamental materials science problems (e.g., phase transformations and physical properties) require an improvement in the understanding of the type and population of grain boundaries in a given system – yet, databases are limited in number and spare in detail, including for hcp crystals such as zirconium. One way to rapidly obtain databases to analyze is to use small-grained materials and high spatial resolution orientation microscopy techniques, such as ASTAR™/precession electron diffraction. To demonstrate this, a study of grain boundary character distributions was conducted for α-zirconium deposited at room temperature on fused silica substrates using physicalmore » vapor deposition. The orientation maps of the nanocrystalline thin films were acquired by the ASTARα/precession electron diffraction technique, a new transmission electron microscope based orientation microscopy method. The reconstructed grain boundaries were classified as pure tilt, pure twist, 180°-twist and 180°-tilt grain boundaries based on the distribution of grain boundary planes with respect to the angle/axis of misorientation associated with grain boundaries. The results of the current study were compared to the results of a similar study on α-titanium and the molecular dynamics results of grain boundary energy for α-titanium.« less

Electrical properties and scaling behaviour of rare earth based Ho{sub 2}CoZrO{sub 6} double perovskite ceramics

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mahato, Dev K., E-mail: drdevkumar@yahoo.com; Dutta, Alo; Sinha, T.P.

2012-12-15

Graphical abstract: The X-ray diffraction analysis suggests that the compound crystallizes in monoclinic phase at room temperature with β = 108.51 ± 0.021° (a = 8.1858 ± 0.0023 Å, b = 5.2599 ± 0.0027 Å, c = 7.9874 ± 0.0031 Å) and cell volume = 324.17 Å{sup 3}. The SEM image indicates the uniformity of the grains in the samples. The grain size of the microstructure of HCZ is found to be ∼0.48 μm on average. Display Omitted Highlights: ► The conduction mechanism in HCZ may be due to hopping of small polaron. ► The material shows semiconducting behaviour. ►more » Conductivity obeys Jonscher's power law with high frequency dispersion. ► Both long-range and localized relaxation are present. -- Abstract: The Ho{sub 2}CoZrO{sub 6} (HCZ) double perovskite has been prepared in polycrystalline form by solid state reaction technique. The analysis of the X-ray powder diffraction pattern indicates that the crystal structure is monoclinic at room temperature with cell parameters a = 8.1858 ± 0.0023 Å, b = 5.2599 ± 0.0027 Å, c = 7.9874 ± 0.0031 Å and β = 108.51 ± 0.021°. The compound shows significant frequency dispersion in its dielectric properties. The Cole–Cole model is used to determine the polydispersive nature of dielectric relaxation. The scaling behaviour of dielectric loss and imaginary electric modulus suggest that the relaxation describe same mechanism at various temperatures. Impedance data presented in the Nyquist plot (Z″ versus Z′) are used to identify an equivalent circuit and to know the bulk and interface contributions. The complex impedance analysis of HCZ exhibits the appearance of both the grain and the grain-boundary contribution. The frequency dependent conductivity spectra follow the universal power law. The magnitude of the activation energy indicates that the carrier transport is due to the hopping conduction.« less

Nanocrystallization of Zr-Cu-Ni-Al-Au glassy alloys during severe plastic deformation

NASA Astrophysics Data System (ADS)

Yamada, Masahiro; Kamisato, Ryo; Yamasaki, Tohru; Adachi, Hiroki; Tsuchiya, Koichi; Yokoyama, Yoshihiko

2014-08-01

A study has been carried out into the formation of nanocrystalline grains during high-pressure torsion (HPT) deformation of Zr65Cu17Ni5Al10Au3 bulk alloys prepared using tilt casting. As a preliminary to this, X-ray diffraction (XRD) and differential scanning calorimetry (DSC) analyses were carried out on as-cast Zr65+xCu17-xNi5Al10Au3 (x=0~5 at.%) and Zr65Cu20Ni5Al10Au3 alloys, in order to determine the effect on the microstructure of the excess Zr content x and the presence of Au. From the XRD patterns, it was determined that all of the alloys had a metallic glassy nature. For Zr65Cu17Ni5Al10Au3, the DSC results indicated the presence of a wide supercooled liquid region between the glass transition temperature (Tg) of 644 K and the crystallization temperature of 763 K, where the stable body-centered tetragonal Zr2Cu phase was formed. In contrast, for the Zr65+xCu17-xNi5Al10Au3 alloys, precipitation of an icosahedral quasicrystalline phase (I-phase) was observed in the supercooled liquid region at about 715 K. HPT deformation of the Zr65Cu17Ni5Al10Au3 alloys was carried out under a high pressure of 5 GPa. Both as-cast specimens and those annealed at Tg-50 K for 90 min were used. Following a single HPT rotation (N=1), transmission electron microscopy identified the presence of face- centered cubic Zr2Ni precipitates in the as-cast alloy, with a size of about 50 nm. For the annealed alloy, a high density of I-phase precipitates with sizes of less than 10 nm was observed following HPT with N=10, indicating that the combination of severe plastic deformation and annealing is effective at producing extremely small grains.

Microstructure and hydrogenation properties of a melt-spun non-stoichiometric Zr-based Laves phase alloy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhang, Tiebang, E-mail: tiebangzhang@nwpu.edu.cn; Zhang, Yunlong; Li, Jinshan

2016-01-15

Alloy with composition of Zr{sub 0.9}Ti{sub 0.1}V{sub 1.7} off normal stoichiometric proportion is selected to investigate the effect of defects introduced by non-stoichiometry on hydrogenation kinetics of Zr–Ti–V Laves phase alloys. Microstructure and phase constituent of melt-spun ribbons have been investigated in this work. The activation process, hydrogenation kinetics, thermodynamics characteristics and hydride phase constituent of as-cast alloy and melt-spun ribbons are also compared. Comparing with the as-cast alloy, the dominant Laves phase ZrV{sub 2} is preserved, V-BCC phase is reduced and α-Zr phase is replaced by a small amount of Zr{sub 3}V{sub 3}O phase in melt-spun ribbons. Melt-spun ribbonsmore » exhibit easy activation and fast initial hydrogen absorption on account of the increased specific surface area. However, the decrease in unit cell volume of the dominant phase leads to the decrease in hydrogen absorption capacity. Melt-spinning technique raises the equilibrium pressure and decreases the stability of hydride due to the decrease of unit cell volume and the elimination of α-Zr phase, respectively. Melt-spun ribbons with fine grains show improved hydrogen absorption kinetics comparing with that of the as-cast alloy. Meanwhile, the prevalent micro twins observed within melt-spun ribbons are believed to account for the improved hydrogen absorption kinetics. - Highlights: • Role of defects on hydrogenation kinetics of Zr-based alloys is proposed. • Microstructure and hydrogenation properties of as-cast/melt-spun alloy are compared. • Melt-spinning technique improves the hydrogenation kinetics of Zr{sub 0.9}Ti{sub 0.1}V{sub 1.7} alloy. • Refined grains and twin defects account for improved hydrogen absorption kinetics.« less

Analysis of defect structure in silicon. Effect of grain boundary density on carrier mobility in UCP material

NASA Technical Reports Server (NTRS)

Dunn, J.; Stringfellow, G. B.; Natesh, R.

1982-01-01

The relationships between hole mobility and grain boundary density were studied. Mobility was measured using the van der Pauw technique, and grain boundary density was measured using a quantitative microscopy technique. Mobility was found to decrease with increasing grain boundary density.

Defect character at grain boundary facet junctions: Analysis of an asymmetric Σ = 5 grain boundary in Fe

DOE Office of Scientific and Technical Information (OSTI.GOV)

Medlin, D. L.; Hattar, K.; Zimmerman, J. A.

Grain boundaries often develop faceted morphologies in systems for which the interfacial free energy depends on the boundary inclination. Although the mesoscale thermodynamic basis for such morphological evolution has been extensively studied, the influence of line defects, such as secondary grain boundary dislocations, on the facet configurations has not been thoroughly explored. In this paper, through a combination of atomistic simulations and electron microscopic observations, we examine in detail the structure of an asymmetric Σ = 5 [001] grain boundary in well-annealed, body-centered cubic (BCC) Fe. The observed boundary forms with a hill-and-valley morphology composed of nanoscale {310} and {210}more » facets. Our analysis clarifies the atomic structure of the {310}/{210} facet junctions and identifies the presence of an array of secondary grain boundary dislocations that are localized to these junctions. Analysis of the Burgers vectors of the grain boundary dislocations, which are of type (1/5)<310> and (1/5)<120>, shows that the defect density is consistent with that required to accommodate a small observed angular deviation from the exact Σ = 5 orientation relationship. As a result, these observations and analysis suggest a crucial role for secondary grain boundary dislocations in dictating the length-scale of grain boundary facets, a consideration which has not been included in prior analyses of facet evolution and equilibrium facet length.« less

Defect character at grain boundary facet junctions: Analysis of an asymmetric Σ = 5 grain boundary in Fe

DOE PAGES

Medlin, D. L.; Hattar, K.; Zimmerman, J. A.; ...

2016-11-16

Grain boundaries often develop faceted morphologies in systems for which the interfacial free energy depends on the boundary inclination. Although the mesoscale thermodynamic basis for such morphological evolution has been extensively studied, the influence of line defects, such as secondary grain boundary dislocations, on the facet configurations has not been thoroughly explored. In this paper, through a combination of atomistic simulations and electron microscopic observations, we examine in detail the structure of an asymmetric Σ = 5 [001] grain boundary in well-annealed, body-centered cubic (BCC) Fe. The observed boundary forms with a hill-and-valley morphology composed of nanoscale {310} and {210}more » facets. Our analysis clarifies the atomic structure of the {310}/{210} facet junctions and identifies the presence of an array of secondary grain boundary dislocations that are localized to these junctions. Analysis of the Burgers vectors of the grain boundary dislocations, which are of type (1/5)<310> and (1/5)<120>, shows that the defect density is consistent with that required to accommodate a small observed angular deviation from the exact Σ = 5 orientation relationship. As a result, these observations and analysis suggest a crucial role for secondary grain boundary dislocations in dictating the length-scale of grain boundary facets, a consideration which has not been included in prior analyses of facet evolution and equilibrium facet length.« less

Creep Strength of Nb-1Zr for SP-100 Applications

NASA Astrophysics Data System (ADS)

Horak, James A.; Egner, Larry K.

1994-07-01

Power systems that are used to provide electrical power in space are designed to optimize conversion of thermal energy to electrical energy and to minimize the mass and volume that must be launched. Only refractory metals and their alloys have sufficient long-term strength for several years of uninterrupted operation at the required temperatures of 1200 K and above. The high power densities and temperatures at which these reactors must operate require the use of liquid-metal coolants. The alloy Nb-1 wt % Zr (Nb-lZr), which exhibits excellent corrosion resistance to alkali liquid-metals at high temperatures, is being considered for the fuel cladding, reactor structural, and heat-transport systems for the SP-100 reactor system. Useful lifetime of this system is limited by creep deformation in the reactor core. Nb-lZr sheet procured to American Society for Testing and Materials (ASTM) specifications for reactor grade and commercial grade has been processed by several different cold work and annealing treatments to attempt to produce the grain structure (size, shape, and distribution of sizes) that provides the maximum creep strength of this alloy at temperatures from 1250 to 1450 K. The effects of grain size, differences in oxygen concentrations, tungsten concentrations, and electron beam and gas tungsten arc weldments on creep strength were studied. Grain size has a large effect on creep strength at 1450 K but only material with a very large grain size (150 μm) exhibits significantly higher creep strength at 1350 K. Differences in oxygen or tungsten concentrations did not affect creep strength, and the creep strengths of weldments were equal to, or greater than, those for base metal.

Grain Boundary Plane Orientation Fundamental Zones and Structure-Property Relationships

PubMed Central

Homer, Eric R.; Patala, Srikanth; Priedeman, Jonathan L.

2015-01-01

Grain boundary plane orientation is a profoundly important determinant of character in polycrystalline materials that is not well understood. This work demonstrates how boundary plane orientation fundamental zones, which capture the natural crystallographic symmetries of a grain boundary, can be used to establish structure-property relationships. Using the fundamental zone representation, trends in computed energy, excess volume at the grain boundary, and temperature-dependent mobility naturally emerge and show a strong dependence on the boundary plane orientation. Analysis of common misorientation axes even suggests broader trends of grain boundary energy as a function of misorientation angle and plane orientation. Due to the strong structure-property relationships that naturally emerge from this work, boundary plane fundamental zones are expected to simplify analysis of both computational and experimental data. This standardized representation has the potential to significantly accelerate research in the topologically complex and vast five-dimensional phase space of grain boundaries. PMID:26498715

Grain boundary plane orientation fundamental zones and structure-property relationships

DOE Office of Scientific and Technical Information (OSTI.GOV)

Homer, Eric R.; Patala, Srikanth; Priedeman, Jonathan L.

2015-10-26

Grain boundary plane orientation is a profoundly important determinant of character in polycrystalline materials that is not well understood. This work demonstrates how boundary plane orientation fundamental zones, which capture the natural crystallographic symmetries of a grain boundary, can be used to establish structure-property relationships. Using the fundamental zone representation, trends in computed energy, excess volume at the grain boundary, and temperature-dependent mobility naturally emerge and show a strong dependence on the boundary plane orientation. Analysis of common misorientation axes even suggests broader trends of grain boundary energy as a function of misorientation angle and plane orientation. Due to themore » strong structure-property relationships that naturally emerge from this work, boundary plane fundamental zones are expected to simplify analysis of both computational and experimental data. This standardized representation has the potential to significantly accelerate research in the topologically complex and vast five-dimensional phase space of grain boundaries.« less

Determination of grain boundary mobility during recrystallization by statistical evaluation of electron backscatter diffraction measurements

DOE Office of Scientific and Technical Information (OSTI.GOV)

Basu, I., E-mail: basu@imm.rwth-aachen.de; Chen, M.; Loeck, M.

One of the key aspects influencing microstructural design pathways in metallic systems is grain boundary motion. The present work introduces a method by means of which direct measurement of grain boundary mobility vs. misorientation dependence is made possible. The technique utilizes datasets acquired by means of serial electron backscatter diffraction (EBSD) measurements. The experimental EBSD measurements are collectively analyzed, whereby datasets were used to obtain grain boundary mobility and grain aspect ratio with respect to grain boundary misorientation. The proposed method is further validated using cellular automata (CA) simulations. Single crystal aluminium was cold rolled and scratched in order tomore » nucleate random orientations. Subsequent annealing at 300 °C resulted in grains growing, in the direction normal to the scratch, into a single deformed orientation. Growth selection was observed, wherein the boundaries with misorientations close to Σ7 CSL orientation relationship (38° 〈111〉) migrated considerably faster. The obtained boundary mobility distribution exhibited a non-monotonic behavior with a maximum corresponding to misorientation of 38° ± 2° about 〈111〉 axes ± 4°, which was 10–100 times higher than the mobility values of random high angle boundaries. Correlation with the grain aspect ratio values indicated a strong growth anisotropy displayed by the fast growing grains. The observations have been discussed in terms of the influence of grain boundary character on grain boundary motion during recrystallization. - Highlights: • Statistical microstructure method to measure grain boundary mobility during recrystallization • Method implementation independent of material or crystal structure • Mobility of the Σ7 boundaries in 5N Al was calculated as 4.7 × 10{sup –8} m{sup 4}/J ⋅ s. • Pronounced growth selection in the recrystallizing nuclei in Al • Boundary mobility values during recrystallization 2–3 orders of magnitude larger vis-à-vis curvature driven motion.« less

The Formation, Transport Properties and Microstructure of 45 Degrees (001) Tilt Grain Boundaries in Yttrium BARIUM(2) COPPER(3) OXYGEN(7-X) Thin Films

NASA Astrophysics Data System (ADS)

Vuchic, Boris Vukan

1995-01-01

Most high angle grain boundaries in high-T _{c} superconductors exhibit weak link behavior. The Josephson-like properties of these grain boundaries can be used for many device applications such as superconducting quantum interference devices (SQUIDs). The structure-property relationship of different types of 45 ^circ (001) YBa_2 Cu_3O_{7-x} thin film grain boundary junctions are examined to study their weak link nature. A technique, termed sputter-induced epitaxy, is developed to form 45^circ (001) tilt grain boundaries in YBa_2Cu _3O_{7-x} thin films on (100) MgO substrates. A low voltage ion bombardment pre-growth substrate treatment is used to modify the epitaxial orientation relationship between the thin film and the substrate in selected regions. By modifying the orientation of the thin film, grain boundary junctions can be placed in any configuration on the substrate. A variety of pre-growth sputtering conditions in conjunction with atomic force microscopy and Rutherford backscatter spectrometry are used to determine the role of the ions in modifying the substrate surface. Sputter-induced epitaxy is extended to a multilayer MgO/LaAlO_3 substrate, allowing integration of the sputter -induced epitaxy junctions into multilayer structures. The low temperature transport properties of the sputter-induced epitaxy junctions and a set of bi-epitaxial grain boundaries are studied. Individual grain boundaries are isolated and characterized for resistance vs. temperature, current vs. voltage as a function of temperature and magnetic field behavior. Resistive and superconducting grain boundaries are compared. Microstructural analysis is performed using scanning electron microscopy, transmission electron microscopy and high resolution electron microscopy (HREM). Marked differences are observed in the microstructure of resistive and superconducting grain boundaries. HREM studies suggest the importance of the local atomic scale structure of the grain boundary in transport properties. A phenomenological grain boundary model is proposed to describe the structure -property relationship of the boundaries.

Precipitation in cold-rolled Al–Sc–Zr and Al–Mn–Sc–Zr alloys prepared by powder metallurgy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Vlach, M., E-mail: martin.vlach@mff.cuni.cz; Stulikova, I.; Smola, B.

2013-12-15

The effects of cold-rolling on thermal, mechanical and electrical properties, microstructure and recrystallization behaviour of the AlScZr and AlMnScZr alloys prepared by powder metallurgy were studied. The powder was produced by atomising in argon with 1% oxygen and then consolidated by hot extrusion at 350 °C. The electrical resistometry and microhardness together with differential scanning calorimetry measurements were compared with microstructure development observed by transmission and scanning electron microscopy, X-ray diffraction and electron backscatter diffraction. Fine (sub)grain structure developed and fine coherent Al{sub 3}Sc and/or Al{sub 3}(Sc,Zr) particles precipitated during extrusion at 350 °C in the alloys studied. Additional precipitationmore » of the Al{sub 3}Sc and/or Al{sub 3}(Sc,Zr) particles and/or their coarsening was slightly facilitated by the previous cold rolling. The presence of Sc,Zr-containing particles has a significant antirecrystallization effect that prevents recrystallization at temperatures minimally up to 420 °C. The precipitation of the Al{sub 6}Mn- and/or Al{sub 6}(Mn,Fe) particles of a size ∼ 1.0 μm at subgrain boundaries has also an essential antirecrystallization effect and totally suppresses recrystallization during 32 h long annealing at 550 °C. The texture development of the alloys seems to be affected by high solid solution strengthening by Mn. The precipitation of the Mn-containing alloy is highly enhanced by a cold rolling. The apparent activation energy of the Al{sub 3}Sc particles formation and/or coarsening and that of the Al{sub 6}Mn and/or Al{sub 6}(Mn,Fe) particle precipitation in the powder and in the compacted alloys were determined. The cold deformation has no effect on the apparent activation energy values of the Al{sub 3}Sc-phase and the Al{sub 6}Mn-phase precipitation. - Highlights: • The Mn, Sc and Zr additions to Al totally suppresses recrystallization at 550 °C. • The Sc,Zr-containing particle precipitation is slightly facilitated by cold rolling. • The Mn-containing particle precipitation is highly enhanced by cold rolling. • Cold rolling has no effect on activation energy of the Al{sub 3}Sc and Al{sub 6}Mn precipitation. • The texture development is affected by high solid solution strengthening by Mn.« less

Grain boundary and triple junction diffusion in nanocrystalline copper

NASA Astrophysics Data System (ADS)

Wegner, M.; Leuthold, J.; Peterlechner, M.; Song, X.; Divinski, S. V.; Wilde, G.

2014-09-01

Grain boundary and triple junction diffusion in nanocrystalline Cu samples with grain sizes, , of ˜35 and ˜44 nm produced by spark plasma sintering were investigated by the radiotracer method using the 63Ni isotope. The measured diffusivities, Deff, are comparable with those determined previously for Ni grain boundary diffusion in well-annealed, high purity, coarse grained, polycrystalline copper, substantiating the absence of a grain size effect on the kinetic properties of grain boundaries in a nanocrystalline material at grain sizes d ≥ 35 nm. Simultaneously, the analysis predicts that if triple junction diffusion of Ni in Cu is enhanced with respect to the corresponding grain boundary diffusion rate, it is still less than 500ṡDgb within the temperature interval from 420 K to 470 K.

The identification of group II inclusions in carbonaceous chondrites by electron probe microanalysis of perovskite

NASA Technical Reports Server (NTRS)

Kornacki, A. S.; Wood, J. A.

1985-01-01

The technique developed by Kornacki (1984) for identifying group II Ca/Al-rich inclusions in carbonaceous chondrites by electron-microprobe analysis of the ZrO2 or Y2O3 content of their perovskite component is demonstrated using material from 20 Allende inclusions. The results are presented in tables and graphs and compared with findings obtained by other procedures. Group II inclusions are found to have perovskites generally containing less than 0.10 wt pct ZrO2 and/or Y2O3 (average of several grains), while those of groups I, III, V, and VI have more than 0.25 wt pct ZrO2. Analysis of data on eight Allende Ca/Al-rich inclusions shows that 75 percent of the fine-grained inclusions belong to group II. The implications of these findings for fractionation processes in the primitive solar nebula are indicated.

Microstructure modification and performance improvement of Mg-RE alloys by friction stir processing

NASA Astrophysics Data System (ADS)

Wu, Yujuan; Peng, Liming; Zheng, Feiyan; Li, Xuewen; Li, Dejiang; Ding, Wenjiang

Friction stir processing (FSP) is a severe plastic deformation (SPD) processing, which is very useful to refine grain size and secondary phase as well as change the texture of metal materials. Many FSP research were focused on aluminum alloys, while there are few reports on FSP of magnesium alloys, esp. on precipitation-hardening Mg-RE alloys. This paper overviewed the micro structures and mechanical properties of several FSPed Mg-RE alloys, such as Mg-Gd-Zn-Zr, Mg-Gd-Ag-Zr, and Mg-Nd-Zn-Zr with or without long period stacking ordering (LPSO) structure. The effects of processing parameters, such as rotation rate and traversing speed, on microstructure and mechanical properties were evaluated. It shows that FSP can effectively lend to performance improvement by micro structure modification, including obtaining remarkable finer and more homogenized grains, changing distribution and volume percentage of secondary phase etc.

Fabrication and characterization of controllable grain boundary arrays in solution-processed small molecule organic semiconductor films

NASA Astrophysics Data System (ADS)

Wo, Songtao; Headrick, Randall L.; Anthony, John E.

2012-04-01

We have produced solution-processed thin films of 6,13-bis(tri-isopropyl-silylethynyl) pentacene with grain sizes from a few micrometers up to millimeter scale by lateral crystallization from a rectangular stylus. Grains are oriented along the crystallization direction, and the grain size transverse to the crystallization direction depends inversely on the writing speed, hence forming a regular array of oriented grain boundaries with controllable spacing. We utilize these controllable arrays to systematically study the role of large-angle grain boundaries in carrier transport and charge trapping in thin film transistors. The effective mobility scales with the grain size, leading to an estimate of the potential drop at individual large-angle grain boundaries of more than 1 volt. This result indicates that the structure of grain boundaries is not molecularly abrupt, which may be a general feature of solution-processed small molecule organic semiconductor thin films, where relatively high energy grain boundaries are typically formed. Transient measurements after switching from positive to negative gate bias or between large and small negative gate bias reveal reversible charge trapping, with time constants on the order of 10 s and trap densities that are correlated with grain boundary density. We suggest that charge diffusion along grain boundaries and other defects is the rate-determining mechanism of the reversible trapping.

Pre- and post-irradiation characterization and properties measurements of ZrC coated surrogate TRISO particles

DOE Office of Scientific and Technical Information (OSTI.GOV)

Vasudevamurthy, Gokul; Katoh, Yutai; Hunn, John D

2010-09-01

Zirconium carbide is a candidate to either replace or supplement silicon carbide as a coating material in TRISO fuel particles for high temperature gas-cooled reactor fuels. Six sets of ZrC coated surrogate microsphere samples, fabricated by the Japan Atomic Energy Agency using the fluidized bed chemical vapor deposition method, were irradiated in the High Flux Isotope Reactor at the Oak Ridge National Laboratory. These developmental samples available for the irradiation experiment were in conditions of either as-fabricated coated particles or particles that had been heat-treated to simulate the fuel compacting process. Five sets of samples were composed of nominally stoichiometricmore » compositions, with the sixth being richer in carbon (C/Zr = 1.4). The samples were irradiated at 800 and 1250 C with fast neutron fluences of 2 and 6 dpa. Post-irradiation, the samples were retrieved from the irradiation capsules followed by microstructural examination performed at the Oak Ridge National Laboratory's Low Activation Materials Development and Analysis Laboratory. This work was supported by the US Department of Energy Office of Nuclear Energy's Advanced Gas Reactor program as part of International Nuclear Energy Research Initiative collaboration with Japan. This report includes progress from that INERI collaboration, as well as results of some follow-up examination of the irradiated specimens. Post-irradiation examination items included microstructural characterization, and nanoindentation hardness/modulus measurements. The examinations revealed grain size enhancement and softening as the primary effects of both heat-treatment and irradiation in stoichiometric ZrC with a non-layered, homogeneous grain structure, raising serious concerns on the mechanical suitability of these particular developmental coatings as a replacement for SiC in TRISO fuel. Samples with either free carbon or carbon-rich layers dispersed in the ZrC coatings experienced negligible grain size enhancement during both heat treatment and irradiation. However, these samples experienced irradiation induced softening similar to stoichiometric ZrC samples.« less

Grain boundary microstructure, chemistry, and IGSCC in Alloy 600 and Alloy 690

DOE Office of Scientific and Technical Information (OSTI.GOV)

Norring, K.; Stiller, K.; Nilsson, J.O.

1992-12-31

The resistance to intergranular stress corrosion cracking of six different Alloy 600 and Alloy 690 steam generator tubes has been investigated. The composition of the materials at grain boundaries has been investigated using analytical transmission electron microscopy and atom probe field ion microscopy techniques. The depletion of chromium at the grain boundaries has been related to the type of grain boundary precipitates. Segregation of carbon and boron to the grain boundaries has been observed and quantified.

Effects of local film properties on the nucleation and growth of tin whiskers and hillocks

NASA Astrophysics Data System (ADS)

Sarobol, Pylin

Whiskers and hillocks grow spontaneously on Pb-free Sn electrodeposited films as a response to thin film stresses. Stress relaxation occurs by atom deposition to specific grain boundaries in the plane of the film, with hillocks being formed when grain boundary migration accompanies growth out of the plane of the film. The implication for whisker formation in electronics is serious: whiskers can grow to be millimeters long, sometimes causing short circuiting between adjacent components and, thereby, posing serious electrical reliability risks. In order to develop more effective whisker mitigation strategies, a predictive physics-based model has been needed. A growth model is developed, based on grain boundary faceting, localized Coble creep, as well as grain boundary sliding for whiskers, and grain boundary sliding with shear induced grain boundary migration for hillocks. In this model of whisker formation, two mechanisms are important: accretion of atoms by Coble creep on grain boundary planes normal to the growth direction inducing a grain boundary shear and grain boundary sliding in the direction of whisker growth. The model accurately captures the importance of the geometry of "surface grains"---shallow grains on film surfaces whose depths are significantly less than their in-plane grain sizes. A critical factor in the analysis is the ratio of the grain boundary sliding coefficient to the in-plane film compressive stress. If the accretion-induced shear stresses are not coupled to grain boundary motion and sliding occurs, a whisker forms. If the shear stress is coupled to grain boundary migration, a hillock forms. Based on this model, long whiskers grow from shallow surface grains with easy grain boundary sliding in the direction of growth. Other observed growth morphologies will be discussed in light of our model. Additional insights into the preferred sites for whisker and hillock growth were developed based on elastic anisotropy, local film microstructure, grain misorientation, and elastic strain energy density (ESED) as the driving force for growth. Local grain orientations and strains measured by synchrotron micro-diffraction in regions containing whiskers or hillocks were compared with elastic finite element analysis simulations, including Sn elastic anisotropy. Whisker and hillock grains were observed to have higher crystallographic misorientations with neighboring grains than generally observed in the microstructure. While elastic simulations predicted higher local out-of-plane elastic strains and ESEDs for whisker and hillock grains, synchrotron measurements of out-of-plane strains of whisker and hillock grains after growth showed relaxation, with correspondingly low ESEDs calculated from measured strains. This suggests that, before whisker or hillock formation, highly misoriented grains with high out-of-plane elastic strains and ESEDs relative to their neighbors determined, at least in part, which grains became whiskers or hillocks. Based on the models and experiments in this thesis, a clearer picture emerges of the necessary and sufficient conditions for tin whisker and hillock formation in thin films.

Progressive Assessment on the Decomposition Reaction of Na Superionic Conducting Ceramics.

PubMed

Jung, Jae-Il; Kim, Daekyeom; Kim, Hyojin; Jo, Yong Nam; Park, Jung Sik; Kim, Youngsik

2017-01-11

The successful analysis on the microstructure of Hong-type Na superionic conducting (NASICON) ceramics revealed that it consists of several heterogeneous phases: NASICON grains with rectangular shapes, monoclinic round ZrO 2 particles, grain boundaries, a SiO 2 -rich vitrified phase, Na-rich amorphous particles, and pores. A dramatic microstructural evolution of NASICON ceramics was demonstrated via an in situ analysis, which showed that NASICON grains sequentially lost their original morphology and were transformed into comminuted particles (as indicated by the immersion of bulk NASICON samples into seawater at a temperature of 80 °C). The consecutive X-ray diffraction analysis represented that the significant shear stress inside NASICON ceramics caused their structural decomposition, during which H 3 O + ions occupied ceramic Na + sites (predominantly along the (1̅11) and (1̅33) planes), while the original Na + cations came out in the (020) plane of the NASICON ceramic crystalline structure. The results of time-of-flight secondary-ion mass spectrometry analysis confirmed that large concentrations of Cl - and Na + ions were distributed across the surface of NASICON ceramics, leading to local densification of a 20 μm thick surface layer after treatment within seawater solution at a temperature of 80 °C.

Multiscale Modeling of Grain-Boundary Fracture: Cohesive Zone Models Parameterized From Atomistic Simulations

NASA Technical Reports Server (NTRS)

Glaessgen, Edward H.; Saether, Erik; Phillips, Dawn R.; Yamakov, Vesselin

2006-01-01

A multiscale modeling strategy is developed to study grain boundary fracture in polycrystalline aluminum. Atomistic simulation is used to model fundamental nanoscale deformation and fracture mechanisms and to develop a constitutive relationship for separation along a grain boundary interface. The nanoscale constitutive relationship is then parameterized within a cohesive zone model to represent variations in grain boundary properties. These variations arise from the presence of vacancies, intersticies, and other defects in addition to deviations in grain boundary angle from the baseline configuration considered in the molecular dynamics simulation. The parameterized cohesive zone models are then used to model grain boundaries within finite element analyses of aluminum polycrystals.

Effects of heat treatment on U-Mo fuel foils with a zirconium diffusion barrier

NASA Astrophysics Data System (ADS)

Jue, Jan-Fong; Trowbridge, Tammy L.; Breckenridge, Cynthia R.; Moore, Glenn A.; Meyer, Mitchell K.; Keiser, Dennis D.

2015-05-01

A monolith fuel design based on U-Mo alloy has been selected as the fuel type for conversion of the United States' high performance research reactors (HPRRs) from highly enriched uranium (HEU) to low-enriched uranium (LEU). In this fuel design, a thin layer of zirconium is used to eliminate the direct interaction between the U-Mo fuel meat and the aluminum-alloy cladding during irradiation. The co-rolling process used to bond the Zr barrier layer to the U-Mo foil during fabrication alters the microstructure of both the U-10Mo fuel meat and the U-Mo/Zr interface. This work studied the effects of post-rolling annealing treatment on the microstructure of the co-rolled U-Mo fuel meat and the U-Mo/Zr interaction layer. Microscopic characterization shows that the grain size of U-Mo fuel meat increases with the annealing temperature, as expected. The grain sizes were ∼9, ∼13, and ∼20 μm for annealing temperature of 650, 750, and 850 °C, respectively. No abnormal grain growth was observed. The U-Mo/Zr interaction-layer thickness increased with the annealing temperature with an Arrhenius constant for growth of 184 kJ/mole, consistent with a previous diffusion-couple study. The interaction layer thickness was 3.2 ± 0.5 μm, 11.1 ± 2.1 μm, 27.1 ± 0.9 μm for annealing temperature of 650, 750, to 850 °C, respectively. The homogeneity of Mo improves with post rolling annealing temperature and with U-Mo coupon homogenization. The phases in the Zr/U-Mo interaction layer produced by co-rolling, however, differ from those reported in the previous diffusion couple studies.

Effects of heat treatment on U–Mo fuel foils with a zirconium diffusion barrier

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jue, Jan-Fong; Trowbridge, Tammy L.; Breckenridge, Cynthia R.

A monolith fuel design based on U–Mo alloy has been selected as the fuel type for conversion of the United States’ high performance research reactors (HPRRs) from highly enriched uranium (HEU) to low-enriched uranium (LEU). In this fuel design, a thin layer of zirconium is used to eliminate the direct interaction between the U–Mo fuel meat and the aluminum-alloy cladding during irradiation. The co-rolling process used to bond the Zr barrier layer to the U–Mo foil during fabrication alters the microstructure of both the U–10Mo fuel meat and the U–Mo/Zr interface. This work studied the effects of post-rolling annealing treatmentmore » on the microstructure of the co-rolled U–Mo fuel meat and the U–Mo/Zr interaction layer. Microscopic characterization shows that the grain size of U–Mo fuel meat increases with the annealing temperature, as expected. The grain sizes were ~9, ~13, and ~20 μm for annealing temperature of 650, 750, and 850 °C, respectively. No abnormal grain growth was observed. The U–Mo/Zr interaction-layer thickness increased with the annealing temperature with an Arrhenius constant for growth of 184 kJ/mole, consistent with a previous diffusion-couple study. The interaction layer thickness was 3.2 ± 0.5 μm, 11.1 ± 2.1 μm, 27.1 ± 0.9 μm for annealing temperature of 650, 750, to 850 °C, respectively. The homogeneity of Mo improves with post rolling annealing temperature and with U–Mo coupon homogenization. The phases in the Zr/U–Mo interaction layer produced by co-rolling, however, differ from those reported in the previous diffusion couple studies.« less

Interpretation of zircon coronae textures from metapelitic granulites of the Ivrea-Verbano Zone, northern Italy: two-stage decomposition of Fe-Ti oxides

NASA Astrophysics Data System (ADS)

Kovaleva, Elizaveta; Austrheim, Håkon O.; Klötzli, Urs S.

2017-07-01

In this study, we report the occurrence of zircon coronae textures in metapelitic granulites of the Ivrea-Verbano Zone. Unusual zircon textures are spatially associated with Fe-Ti oxides and occur as (1) vermicular-shaped aggregates 50-200 µm long and 5-20 µm thick and as (2) zircon coronae and fine-grained chains, hundreds of micrometers long and ≤ 1 µm thick, spatially associated with the larger zircon grains. Formation of such textures is a result of zircon precipitation during cooling after peak metamorphic conditions, which involved: (1) decomposition of Zr-rich ilmenite to Zr-bearing rutile, and formation of the vermicular-shaped zircon during retrograde metamorphism and hydration; and (2) recrystallization of Zr-bearing rutile to Zr-depleted rutile intergrown with quartz, and precipitation of the submicron-thick zircon coronae during further exhumation and cooling. We also observed hat-shaped grains that are composed of preexisting zircon overgrown by zircon coronae during stage (2). Formation of vermicular zircon (1) preceded ductile and brittle deformation of the host rock, as vermicular zircon is found both plastically and cataclastically deformed. Formation of thin zircon coronae (2) was coeval with, or immediately after, brittle deformation as coronae are found to fill fractures in the host rock. The latter is evidence of local, fluid-aided mobility of Zr. This study demonstrates that metamorphic zircon can nucleate and grow as a result of hydration reactions and mineral breakdown during cooling after granulite-facies metamorphism. Zircon coronae textures indicate metamorphic reactions in the host rock and establish the direction of the reaction front.

Grain-size-yield stress relationship: Analysis and computation

DOE Office of Scientific and Technical Information (OSTI.GOV)

Meyers, M.A.; Benson, D.J.; Fu, H.H.

1999-07-01

The seminal contributions of Julia Weertman to the understanding of the mechanical properties of nanocrystalline materials will be briefly outlined. A constitutive equation predicting the effect of grain size on the yield stress of metals, based on the model proposed by M.A. Meyers and E. Ashworth, is discussed and extended to the nanocrystalline regime. At large grain sizes, it has the Hall-Petch form, and in the nanocrystalline domain the slope gradually decreases until it asymptotically approaches the flow stress of the grain boundaries. The material is envisaged as a composite, comprised of the grain interior, with flow stress {sigma}{sub fB},more » and grain boundary work-hardened layer, with flow stress {sigma}{sub fGB}. Three principal factors contribute to the grain-boundary hardening: (1) the grain boundaries act as barriers to plastic flow; (2) the grain boundaries act as dislocation sources; and (3) elastic anisotropy causes additional stresses in grain-boundary surroundings. The predictions of this model are compared with experimental measurements over the mono, micro, and nanocrystalline domains. Computational predictions are made of plastic flow as a function of grain size incorporating elastic and plastic anisotropy as well as differences of dislocation accumulation rate in grain boundary regions and grain interiors. This is the first plasticity calculation that accounts for grain size effects in a physically-based manner. 58 refs., 7 figs., 1 tab.« less

Hydrogen segregation to inclined Σ3 < 110 >twin grain boundaries in nickel

DOE PAGES

O’Brien, Christopher J.; Foiles, Stephen M.

2016-08-04

Low-mobility twin grain boundaries dominate the microstructure of grain boundary-engineered materials and are critical to understanding their plastic deformation behaviour. The presence of solutes, such as hydrogen, has a profound effect on the thermodynamic stability of the grain boundaries. This work examines the case of a Σ3 grain boundary at inclinations from 0° ≤ Φ ≤ 90°. The angle Φ corresponds to the rotation of the Σ3 (1 1 1) < 1 1 0 > (coherent) into the Σ3 (1 1 2) < 1 1 0 > (lateral) twin boundary. To this end, atomistic models of inclined grain boundaries, utilisingmore » empirical potentials, are used to elucidate the finite-temperature boundary structure while grand canonical Monte Carlo models are applied to determine the degree of hydrogen segregation. In order to understand the boundary structure and segregation behaviour of hydrogen, the structural unit description of inclined twin grain boundaries is found to provide insight into explaining the observed variation of excess enthalpy and excess hydrogen concentration on inclination angle, but the explanatory power is limited by how the enthalpy of segregation is affected by hydrogen concentration. At higher concentrations, the grain boundaries undergo a defaceting transition. In order to develop a more complete mesoscale model of the interfacial behaviour, an analytical model of boundary energy and hydrogen segregation that relies on modelling the boundary as arrays of discrete 1/3 < 1 1 1 > disconnections is constructed. Lastly, the complex interaction of boundary reconstruction and concentration-dependent segregation behaviour exhibited by inclined twin grain boundaries limits the range of applicability of such an analytical model and illustrates the fundamental limitations for a structural unit model description of segregation in lower stacking fault energy materials.« less

Effect of HIP temperature on microstructure and low cycle fatigue strength of CuCrZr alloy

NASA Astrophysics Data System (ADS)

Nishi, Hiroshi; Enoeda, Mikio

2011-10-01

In order to investigate the effect of the HIP cycle temperatures on the metallurgic degradation and the mechanical properties of CuCrZr alloy, assessments of the microstructure, tensile test, Charpy impact test and low cycle fatigue test are performed for various heat treated CuCrZr alloys, which were solution-annealed followed by water-quenched and aged state of CuCrZr with simulated HIP cycle at temperatures of 980 and 1045 °C. Grain growth occurred on 1045 °C HIP CuCrZr, though slightly on 980 °C HIP CuCrZr. Metallurgic degradation such as voids was not found by optical and SEM observations. There were coarse precipitates in all the CuCrZr and the precipitates did not easily dissolve at 980 °C. The low cycle fatigue strength of 1045 °C HIP CuCrZr was lower than that of other CuCrZr because of the metallurgic degradation caused by the heat cycle, while that of other CuCrZr was corresponding to the best fit curve of ITER MPH.

First-principles study of the effect of phosphorus on nickel grain boundary

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liu, Wenguan; Ren, Cuilan; Han, Han, E-mail: hanhan@sinap.ac.cn, E-mail: xuhongjie@sinap.ac.cn

2014-01-28

Based on first-principles quantum-mechanical calculations, the impurity-dopant effects of phosphorus on Σ5(012) symmetrical tilt grain boundary in nickel have been studied. The calculated binding energy suggests that phosphorus has a strong tendency to segregate to the grain boundary. Phosphorus forms strong and covalent-like bonding with nickel, which is beneficial to the grain boundary cohesion. However, a too high phosphorus content can result in a thin and fragile zone in the grain boundary, due to the repulsion between phosphorus atoms. As the concentration of phosphorus increases, the strength of the grain boundary increases first and then decreases. Obviously, there exists anmore » optimum concentration for phosphorus segregation, which is consistent with observed segregation behaviors of phosphorus in the grain boundary of nickel. This work is very helpful to understand the comprehensive effects of phosphorus.« less

Introducing Overlapping Grain Boundaries in Chemical Vapor Deposited Hexagonal Boron Nitride Monolayer Films

PubMed Central

2017-01-01

We demonstrate the growth of overlapping grain boundaries in continuous, polycrystalline hexagonal boron nitride (h-BN) monolayer films via scalable catalytic chemical vapor deposition. Unlike the commonly reported atomically stitched grain boundaries, these overlapping grain boundaries do not consist of defect lines within the monolayer films but are composed of self-sealing bilayer regions of limited width. We characterize this overlapping h-BN grain boundary structure in detail by complementary (scanning) transmission electron microscopy techniques and propose a catalytic growth mechanism linked to the subsurface/bulk of the process catalyst and its boron and nitrogen solubilities. Our data suggest that the overlapping grain boundaries are comparatively resilient against deleterious pinhole formation associated with grain boundary defect lines and thus may reduce detrimental breakdown effects when polycrystalline h-BN monolayer films are used as ultrathin dielectrics, barrier layers, or separation membranes. PMID:28410557

Ionic Conductivity and Air Stability of Al-Doped Li₇La₃Zr₂O₁₂ Sintered in Alumina and Pt Crucibles.

PubMed

Xia, Wenhao; Xu, Biyi; Duan, Huanan; Guo, Yiping; Kang, Hongmei; Li, Hua; Liu, Hezhou

2016-03-02

Li7La3Zr2O12 (LLZO) is a promising electrolyte material for all-solid-state battery due to its high ionic conductivity and good stability with metallic lithium. In this article, we studied the effect of crucibles on the ionic conductivity and air stability by synthesizing 0.25Al doped LLZO pellets in Pt crucibles and alumina crucibles, respectively. The results show that the composition and microstructure of the pellets play important roles influencing the ionic conductivity, relative density, and air stability. Specifically, the 0.25Al-LLZO pellets sintered in Pt crucibles exhibit a high relative density (∼96%) and high ionic conductivity (4.48 × 10(-4) S cm(-1)). The ionic conductivity maintains 3.6 × 10(-4) S cm(-1) after 3-month air exposure. In contrast, the ionic conductivity of the pellets from alumina crucibles is about 1.81 × 10(-4) S cm(-1) and drops to 2.39 × 10(-5) S cm(-1) 3 months later. The large grains and the reduced grain boundaries in the pellets sintered in Pt crucibles are favorable to obtain high ionic conductivity and good air stability. X-ray photoelectron spectroscopy (XPS) and Raman spectroscopy results suggest that the formation of Li2CO3 on the pellet surface is probably another main reason, which is also closely related to the relative density and the amount of grain boundary within the pellets. This work stresses the importance of synthesis parameters, crucibles included, to obtain the LLZO electrolyte with high ionic conductivity and good air stability.

Mechanical Properties of TiTaHfNbZr High-Entropy Alloy Coatings Deposited on NiTi Shape Memory Alloy Substrates

NASA Astrophysics Data System (ADS)

Motallebzadeh, A.; Yagci, M. B.; Bedir, E.; Aksoy, C. B.; Canadinc, D.

2018-04-01

TiTaHfNbZr high-entropy alloy (HEA) thin films with thicknesses of about 750 and 1500 nm were deposited on NiTi substrates by RF magnetron sputtering using TiTaHfNbZr equimolar targets. The thorough experimental analysis on microstructure and mechanical properties of deposited films revealed that the TiTaHfNbZr films exhibited amorphous and cauliflower-like structure, where grain size and surface roughness increased concomitant with film thickness. More importantly, the current findings demonstrate that the TiTaHfNbZr HEA films with mechanical properties of the same order as those of the NiTi substrate constitute promising biomedical coatings effective in preventing Ni release.

Mechanical Properties of TiTaHfNbZr High-Entropy Alloy Coatings Deposited on NiTi Shape Memory Alloy Substrates

NASA Astrophysics Data System (ADS)

Motallebzadeh, A.; Yagci, M. B.; Bedir, E.; Aksoy, C. B.; Canadinc, D.

2018-06-01

TiTaHfNbZr high-entropy alloy (HEA) thin films with thicknesses of about 750 and 1500 nm were deposited on NiTi substrates by RF magnetron sputtering using TiTaHfNbZr equimolar targets. The thorough experimental analysis on microstructure and mechanical properties of deposited films revealed that the TiTaHfNbZr films exhibited amorphous and cauliflower-like structure, where grain size and surface roughness increased concomitant with film thickness. More importantly, the current findings demonstrate that the TiTaHfNbZr HEA films with mechanical properties of the same order as those of the NiTi substrate constitute promising biomedical coatings effective in preventing Ni release.

Central role of TiO2 anatase grain boundaries on resistivity of CaCu3Ti4O12-based materials probed by Raman spectroscopy

NASA Astrophysics Data System (ADS)

De Almeida-Didry, Sonia; Autret, Cécile; Honstettre, Christophe; Lucas, Anthony; Zaghrioui, Mustapha; Pacreau, François; Gervais, François

2016-11-01

This study focuses on characterization and control of grain boundaries to enhance the properties of CaCu3Ti4O12 (CCTO) ceramics capacitors for industrial applications. A novel factor deals with TiO2 anatase revealed by Raman scattering in grain boundaries, found as a dominant parameter of largest sample resistivity, consistent with higher grain boundary resistivity and higher breakdown voltage. Four selected samples of CCTO-based compositions showing very different properties in terms of permittivity ranging from 1000 to 684 000 measured at 1 kHz, capacitance of grain boundaries ranging from 8 10-10 to 4.5 10-7 F cm-1, grain boundary resistivity ranging from 193 to 30,000,000 Ω cm and sample resistivity extending from 450 to 1011 Ω cm. The relationship between permittivity weighted by grain size and capacitance of grain boundaries confirms the internal barrier layer capacitance model over 5 orders of magnitude.

Electrical characterization of grain boundaries of CZTS thin films using conductive atomic force microscopy techniques

DOE Office of Scientific and Technical Information (OSTI.GOV)

Muhunthan, N.; Singh, Om Pal; Toutam, Vijaykumar, E-mail: toutamvk@nplindia.org

2015-10-15

Graphical abstract: Experimental setup for conducting AFM (C-AFM). - Highlights: • Cu{sub 2}ZnSnS{sub 4} (CZTS) thin film was grown by reactive co-sputtering. • The electronic properties were probed using conducting atomic force microscope, scanning Kelvin probe microscopy and scanning capacitance microscopy. • C-AFM current flow mainly through grain boundaries rather than grain interiors. • SKPM indicated higher potential along the GBs compared to grain interiors. • The SCM explains that charge separation takes place at the interface of grain and grain boundary. - Abstract: Electrical characterization of grain boundaries (GB) of Cu-deficient CZTS (Copper Zinc Tin Sulfide) thin films wasmore » done using atomic force microscopic (AFM) techniques like Conductive atomic force microscopy (CAFM), Kelvin probe force microscopy (KPFM) and scanning capacitance microscopy (SCM). Absorbance spectroscopy was done for optical band gap calculations and Raman, XRD and EDS for structural and compositional characterization. Hall measurements were done for estimation of carrier mobility. CAFM and KPFM measurements showed that the currents flow mainly through grain boundaries (GB) rather than grain interiors. SCM results showed that charge separation mainly occurs at the interface of grain and grain boundaries and not all along the grain boundaries.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ghamarian, I.; Samani, P.; Rohrer, G. S.

Grain boundary engineering and other fundamental materials science problems (e.g., phase transformations and physical properties) require an improvement in the understanding of the type and population of grain boundaries in a given system – yet, databases are limited in number and spare in detail, including for hcp crystals such as zirconium. One way to rapidly obtain databases to analyze is to use small-grained materials and high spatial resolution orientation microscopy techniques, such as ASTAR™/precession electron diffraction. To demonstrate this, a study of grain boundary character distributions was conducted for α-zirconium deposited at room temperature on fused silica substrates using physicalmore » vapor deposition. The orientation maps of the nanocrystalline thin films were acquired by the ASTARα/precession electron diffraction technique, a new transmission electron microscope based orientation microscopy method. The reconstructed grain boundaries were classified as pure tilt, pure twist, 180°-twist and 180°-tilt grain boundaries based on the distribution of grain boundary planes with respect to the angle/axis of misorientation associated with grain boundaries. The results of the current study were compared to the results of a similar study on α-titanium and the molecular dynamics results of grain boundary energy for α-titanium.« less

A primer on selecting grain boundary sets for comparison of interfacial fracture properties in molecular dynamics simulations

DOE PAGES

Dingreville, Remi; Aksoy, Doruk; Spearot, Douglas E.

2017-08-21

In this study, all grain boundaries are not equal in their predisposition for fracture due to the complex coupling between lattice geometry, interfacial structure, and mechanical properties. The ability to understand these relationships is crucial to engineer materials resilient to grain boundary fracture. Here, a methodology is presented to isolate the role of grain boundary structure on interfacial fracture properties, such as the tensile strength and work of separation, using atomistic simulations. Instead of constructing sets of grain boundary models within the misorientation/structure space by simply varying the misorientation angle around a fixed misorientation axis, the proposed method creates setsmore » of grain boundary models by means of isocurves associated with important fracture-related properties of the adjoining lattices. Such properties may include anisotropic elastic moduli, the Schmid factor for primary slip, and the propensity for simultaneous slip on multiple slip systems. This approach eliminates the effect of lattice properties from the comparative analysis of interfacial fracture properties and thus enables the identification of structure-property relationships for grain boundaries. As an example, this methodology is implemented to study crack propagation along Ni grain boundaries. Segregated H is used as a means to emphasize differences in the selected grain boundary structures while keeping lattice properties fixed.« less

A primer on selecting grain boundary sets for comparison of interfacial fracture properties in molecular dynamics simulations

DOE Office of Scientific and Technical Information (OSTI.GOV)

Dingreville, Remi; Aksoy, Doruk; Spearot, Douglas E.

In this study, all grain boundaries are not equal in their predisposition for fracture due to the complex coupling between lattice geometry, interfacial structure, and mechanical properties. The ability to understand these relationships is crucial to engineer materials resilient to grain boundary fracture. Here, a methodology is presented to isolate the role of grain boundary structure on interfacial fracture properties, such as the tensile strength and work of separation, using atomistic simulations. Instead of constructing sets of grain boundary models within the misorientation/structure space by simply varying the misorientation angle around a fixed misorientation axis, the proposed method creates setsmore » of grain boundary models by means of isocurves associated with important fracture-related properties of the adjoining lattices. Such properties may include anisotropic elastic moduli, the Schmid factor for primary slip, and the propensity for simultaneous slip on multiple slip systems. This approach eliminates the effect of lattice properties from the comparative analysis of interfacial fracture properties and thus enables the identification of structure-property relationships for grain boundaries. As an example, this methodology is implemented to study crack propagation along Ni grain boundaries. Segregated H is used as a means to emphasize differences in the selected grain boundary structures while keeping lattice properties fixed.« less

Site energies and charge transfer rates near pentacene grain boundaries from first-principles calculations

NASA Astrophysics Data System (ADS)

Kobayashi, Hajime; Tokita, Yuichi

2015-03-01

Charge transfer rates near pentacene grain boundaries are derived by calculating the site energies and transfer integrals of 37 pentacene molecules using first-principles calculations. The site energies decrease considerably near the grain boundaries, and electron traps of up to 300 meV and hole barriers of up to 400 meV are generated. The charge transfer rates across the grain boundaries are found to be reduced by three to five orders of magnitude with a grain boundary gap of 4 Å because of the reduction in the transfer integrals. The electron traps and hole barriers also reduce the electron and hole transfer rates by factors of up to 10 and 50, respectively. It is essential to take the site energies into consideration to determine charge transport near the grain boundaries. We show that the complex site energy distributions near the grain boundaries can be represented by an equivalent site energy difference, which is a constant for any charge transfer pass. When equivalent site energy differences are obtained for various grain boundary structures by first-principles calculations, the effects of the grain boundaries on the charge transfer rates are introduced exactly into charge transport simulations, such as the kinetic Monte Carlo method.

Atomistic simulation of the trapping capability of He-vacancy defects at Ni {\\sum}^{}3\\left(1\\bar{1}2\\right)[110] grain boundary

NASA Astrophysics Data System (ADS)

Gong, Hengfeng; Wang, Chengbin; Zhang, Wei; Huai, Ping; Lu, Wei; Zhu, Zhiyuan

2016-12-01

He atoms tend to cluster and precipitate into bubbles that prefer to grow in the grain boundaries, resulting in high temperature He embrittlement with significantly degraded material properties. This is a major bottleneck in employing Ni-based alloys for applications such as molten salt reactors (MSRs). This paper focuses on understanding how the local grain boundary structure interacts with He atoms and how the local atomistic environment in the grain boundary influences the binding energy of He defects. Using molecular dynamics simulations, we have investigated the trapping capability of the Ni {\\sum}3≤ft(1 \\bar{1} 2\\right)≤ft[1 1 0\\right] grain boundary to He defects (He N ) and to He-vacancy defects (He N V M ). The two defects in the Ni grain boundary exhibit geometries with high symmetry. The binding energy of an interstitial He atom to He N V M defects is found to be generally larger in pure Ni than that in the grain boundary. We compared the binding energy of He N defects to the Ni vacancy and to the Ni grain boundary, finding that the Ni vacancy possesses a higher trapping strength to He N . We also found that the binding strength of He N to the grain boundary is stronger than that of He N V M to the grain boundary. The He-vacancy ratio in He N V M defects does not significantly affect the binding energy in the grain boundary plane. The current work will provide insight in understanding the experimentally observed He bubble formation in Ni-based alloys and bridge atomic scale events and damage with macroscopic failure.

Grain boundary engineering to control the discontinuous precipitation in multicomponent U10Mo alloy

DOE PAGES

Devaraj, Arun; Kovarik, Libor; Kautz, Elizabeth; ...

2018-03-30

Here, we demonstrate here that locally stabilized structure and compositional segregation at grain boundaries in a complex multicomponent alloy can be modified using high temperature homogenization treatment to influence the kinetics of phase transformations initiating from grain boundaries during subsequent low temperature annealing. Using aberration-corrected scanning transmission electron microscopy and atom probe tomography of a model multicomponent metallic alloy —uranium-10 wt% molybdenum (U-10Mo) a nuclear fuel, that is highly relevant to worldwide nuclear non-proliferation efforts, we demonstrate the ability to change the structure and compositional segregation at grain boundary, which then controls the subsequent discontinuous precipitation kinetics during sub-eutectoid annealing.more » A change in grain boundary from one characterized by segregation of Mo and impurities at grain boundary to a phase boundary with a distinct U 2MoSi 2C wetting phase precipitates introducing Ni and Al rich interphase complexions caused a pronounced reduction in area fraction of subsequent discontinuous precipitation. The broader implication of this work is in highlighting the role of grain boundary structure and composition in metallic alloys on dictating the fate of grain boundary initiated phase transformations like discontinuous precipitation or cellular transformation. This work highlights a new pathway to tune the grain boundary structure and composition to tailor the final microstructure of multicomponent metallic alloys.« less

Grain boundary engineering to control the discontinuous precipitation in multicomponent U10Mo alloy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Devaraj, Arun; Kovarik, Libor; Kautz, Elizabeth

Here, we demonstrate here that locally stabilized structure and compositional segregation at grain boundaries in a complex multicomponent alloy can be modified using high temperature homogenization treatment to influence the kinetics of phase transformations initiating from grain boundaries during subsequent low temperature annealing. Using aberration-corrected scanning transmission electron microscopy and atom probe tomography of a model multicomponent metallic alloy —uranium-10 wt% molybdenum (U-10Mo) a nuclear fuel, that is highly relevant to worldwide nuclear non-proliferation efforts, we demonstrate the ability to change the structure and compositional segregation at grain boundary, which then controls the subsequent discontinuous precipitation kinetics during sub-eutectoid annealing.more » A change in grain boundary from one characterized by segregation of Mo and impurities at grain boundary to a phase boundary with a distinct U 2MoSi 2C wetting phase precipitates introducing Ni and Al rich interphase complexions caused a pronounced reduction in area fraction of subsequent discontinuous precipitation. The broader implication of this work is in highlighting the role of grain boundary structure and composition in metallic alloys on dictating the fate of grain boundary initiated phase transformations like discontinuous precipitation or cellular transformation. This work highlights a new pathway to tune the grain boundary structure and composition to tailor the final microstructure of multicomponent metallic alloys.« less

Influence of free carbon on the characteristics of ZrC and deposition of near-stoichiometric ZrC in TRISO coated particle fuel

NASA Astrophysics Data System (ADS)

Kim, Daejong; Ko, Myeong Jin; Park, Ji Yeon; Cho, Moon Sung; Kim, Weon-Ju

2014-08-01

Advanced TRISO coated particles with a ZrC coating layer as a main pressure boundary were fabricated by a fluidized-bed chemical vapor deposition (FBCVD) method using a chloride process. Experiments were performed to determine the effect of codeposition of graphitic carbon on the hardness and obtain the stoichiometric ZrC phase. The ZrC coating layer was composed of a mixture of ZrC and graphitic carbon phases at a low ZrCl4/CH4 ratio. A near-stoichiometric ZrC without the free carbon can be obtained by employing an impeller-driven ZrCl4 vaporizer. The codeposition of the graphitic carbon significantly lowered the hardness of ZrC while increasing the fraction of the carbon. The hardness reached its maximum when ZrC was in a slight carbon deficit without free carbon. As the graphitic carbon increased up to 12 vol%, the hardness was reduced by approximately 50% compared to the near-stoichiometric ZrC.

Competing Grain Boundary and Interior Deformation Mechanisms with Varying Sizes

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhang, Wei; Gao, Yanfei; Nieh, T. G.

In typical coarse-grained alloys, the dominant plastic deformations are dislocation gliding or climbing, and material strengths can be tuned by dislocation interactions with grain boundaries, precipitates, solid solutions, and other defects. With the reduction of grain size, the increase of material strengths follows the classic Hall-Petch relationship up to nano-grained materials. Even at room temperatures, nano-grained materials exhibit strength softening, or called the inverse Hall-Petch effect, as grain boundary processes take over as the dominant deformation mechanisms. On the other hand, at elevated temperatures, grain boundary processes compete with grain interior deformation mechanisms over a wide range of the appliedmore » stress and grain sizes. This book chapter reviews and compares the rate equation model and the microstructure-based finite element simulations. The latter explicitly accounts for the grain boundary sliding, grain boundary diffusion and migration, as well as the grain interior dislocation creep. Therefore the explicit finite element method has clear advantages in problems where microstructural heterogeneities play a critical role, such as in the gradient microstructure in shot peening or weldment. Furthermore, combined with the Hall-Petch effect and its breakdown, the above competing processes help construct deformation mechanism maps by extending from the classic Frost-Ashby type to the ones with the dependence of grain size.« less

Influence of N2 partial pressure on structural and microhardness properties of TiN/ZrN multilayers deposited by Ar/N2 vacuum arc discharge

NASA Astrophysics Data System (ADS)

Naddaf, M.; Abdallah, B.; Ahmad, M.; A-Kharroub, M.

2016-08-01

The influence of N2 partial pressure on structural, mechanical and wetting properties of multilayered TiN/ZrN thin films deposited on silicon substrates by vacuum arc discharge of (N2 + Ar) gas mixtures is investigated. X-ray diffraction (XRD) results show that the average texturing coefficient of (1 1 1) orientation and the grain size of both TiN and ZrN individual layers increase with increasing the N2 partial pressure. The Rutherford back scattering (RBS) measurements and analysis reveal that incorporation of the nitrogen in the film increases with increasing the N2 partial pressure and both TiN and ZrN individual layers have a nitrogen over-stoichiometry for N2 partial pressure ⩾50%. The change in the film micro-hardness is correlated to the changes in crystallographic texture, grain size, stoichiometry and the residual stress in the film as a function of the N2 partial pressure. In particular, stoichiometry of ZrN and TiN individual is found to play the vital role in determining the multilayer hardness. The multilayer film deposited at N2 partial pressure of 25% has the best stoichiometric ratio of both TiN and ZrN layers and the highest micro-hardness of about 32 GPa. In addition, water contact angle (WCA) measurements and analysis show a decrease in the work of adhesion on increasing the N2 partial pressure.

Evolution of Grain Boundary Precipitates in an Al-Cu-Li Alloy During Aging

NASA Astrophysics Data System (ADS)

Ott, Noémie; Kairy, Shravan K.; Yan, Yuanming; Birbilis, Nick

2017-01-01

The grain boundary microstructure of Al-Cu-Li alloy AA2050 was investigated for different isothermal aging times to rationalize intergranular corrosion (IGC) characteristics. In the underaged condition, the dominant grain boundary precipitates are fine T1 (Al2CuLi). Extended aging revealed that grain boundaries were decorated by large T1 precipitates and S' phase (Al2CuMg), with S' growth not dimensionally constrained. Such a transition in the precipitate type at grain boundaries is a unique feature of the Al-Cu-Li system.

Effect of irradiation on mechanical properties of symmetrical grain boundaries investigated by atomic simulations

NASA Astrophysics Data System (ADS)

Wang, X. Y.; Gao, N.; Setyawan, W.; Xu, B.; Liu, W.; Wang, Z. G.

2017-08-01

Tensile response of irradiated symmetric grain boundaries to the externally applied strain has been studied using atomic simulation methods. The absorption of irradiation induced defects by grain boundaries has been confirmed to degrade the mechanical properties of grain boundaries through the change of its undertaken deformation mechanism. Atomic rearrangement, the formations of a stress accumulation region and vacancy-rich zone and the nucleation and movement of dislocations under stress effect have been observed after the displacement cascades in grain boundaries, which are considered as main reasons to induce above degradation. These results suggest the necessity of considering both trapping efficiency to defects and the mechanical property change of irradiated grain boundaries for further development of radiation resistant materials.

Spatially resolved mapping of electrical conductivity across individual domain (grain) boundaries in graphene.

PubMed

Clark, Kendal W; Zhang, X-G; Vlassiouk, Ivan V; He, Guowei; Feenstra, Randall M; Li, An-Ping

2013-09-24

All large-scale graphene films contain extended topological defects dividing graphene into domains or grains. Here, we spatially map electronic transport near specific domain and grain boundaries in both epitaxial graphene grown on SiC and CVD graphene on Cu subsequently transferred to a SiO2 substrate, with one-to-one correspondence to boundary structures. Boundaries coinciding with the substrate step on SiC exhibit a significant potential barrier for electron transport of epitaxial graphene due to the reduced charge transfer from the substrate near the step edge. Moreover, monolayer-bilayer boundaries exhibit a high resistance that can change depending on the height of substrate step coinciding at the boundary. In CVD graphene, the resistance of a grain boundary changes with the width of the disordered transition region between adjacent grains. A quantitative modeling of boundary resistance reveals the increased electron Fermi wave vector within the boundary region, possibly due to boundary induced charge density variation. Understanding how resistance change with domain (grain) boundary structure in graphene is a crucial first step for controlled engineering of defects in large-scale graphene films.

The cause of ‘weak-link’ grain boundary behaviour in polycrystalline Bi2Sr2CaCu2O8 and Bi2Sr2Ca2Cu3O10 superconductors

NASA Astrophysics Data System (ADS)

Wang, Guanmei; Raine, Mark J.; Hampshire, Damian P.

2018-02-01

The detrimental effects of grain boundaries have long been considered responsible for the low critical current densities ({J}{{c}}) in high temperature superconductors. In this paper, we apply the quantitative approach used to identify the cause of the ‘weak-link’ grain boundary behaviour in YBa2Cu3O7 (Wang et al 2017 Supercond. Sci Technol. 30 104001), to the Bi2Sr2CaCu2O8 and Bi2Sr2Ca2Cu3O10 materials that we have fabricated. Magnetic and transport measurements are used to characterise the grain and grain boundary properties of micro- and nanocrystalline materials. Magnetisation measurements on all nanocrystalline materials show non-Bean-like behaviour and are consistent with surface pinning. Bi2Sr2CaCu2O8: our microcrystalline material has very low grain boundary resistivity ({ρ }{{GB}}), which is similar to that of the grains ({ρ }{{G}}) such that {ρ }{{GB}}≈ {ρ }{{G}}=2× {10}-5 {{Ω }}{{m}} (assuming a grain boundary thickness (d) of 1 nm) equivalent to an areal resistivity of {ρ }{{G}}=2× {10}-14 {{{Ω }}{{m}}}2. The transport {J}{{c}} values are consistent with well-connected grains and very weak grain boundary pinning. However, unlike low temperature superconductors (LTS) in which decreasing grain size increases the pinning along the grain boundary channels, any increase in pinning produced by making the grains in our Bi2Sr2CaCu2O8 materials nanocrystalline was completely offset by a decrease in the depairing current density of the grain boundaries caused by their high resistivity. We suggest a different approach to increasing {J}{{c}} from that used in LTS materials, namely incorporating additional strong grain and grain boundary pinning sites in microcrystalline materials to produce high {J}{{c}} values. Bi2Sr2Ca2Cu3O10: both our micro- and nanocrystalline samples have {ρ }{{GB}}/{ρ }{{G}} of at least 103. This causes strong suppression of {J}{{c}} across the grain boundaries, which explains the low transport {J}{{c}} values we find experimentally. Our calculations show that low {J}{{c}} in untextured polycrystalline Bi2Sr2Ca2Cu3O10 material is to be expected and the significant effort in the community in texturing samples and removing grain boundaries altogether is well-founded.

Grain boundary engineering for control of tellurium diffusion in GH3535 alloy

NASA Astrophysics Data System (ADS)

Fu, Cai-Tao; Yinling, Wang; Chu, Xiang-Wei; Jiang, Li; Zhang, Wen-Zhu; Bai, Qin; Xia, Shuang; Leng, Bin; Li, Zhi-Jun; Ye, Xiang-Xi; Liu, Fang

2017-12-01

The effect of grain boundary engineering (GBE) on the Te diffusion along the surface grain boundaries was investigated in GH3535 alloy. It can be found that GBE treatment increases obviously the fraction of low-Σ coincidence site lattice (CSL) boundaries, especially the Σ3 ones, and introduces the large-size grain clusters. When the as-received (AR) and GBE-treated (GBET) specimens were exposed to Te vapor, only Σ3 boundaries were found to be resistant to Te diffusion. From the cross section and the surface, the fewer Te-attacked grain boundaries and the thinner corrosion layer can be observed in the GBET sample. The improvement of resistance to Te diffusion in the GBET sample can be attributed to the large size grain-clusters associated with high proportion of the Σ3n boundaries.

Grain boundary phases in bcc metals

DOE PAGES

Frolov, T.; Setyawan, W.; Kurtz, R. J.; ...

2018-01-01

Evolutionary grand-canonical search predicts novel grain boundary structures and multiple grain boundary phases in elemental body-centered cubic (bcc) metals represented by tungsten, tantalum and molybdenum.

Grain Cluster Microstructure and Grain Boundary Character Distribution in Alloy 690

NASA Astrophysics Data System (ADS)

Xia, Shuang; Zhou, Bangxin; Chen, Wenjue

2009-12-01

The effects of thermal-mechanical processing (TMP) on microstructure evolution during recrystallization and grain boundary character distribution (GBCD) in aged Alloy 690 were investigated by the electron backscatter diffraction (EBSD) technique and optical microscopy. The original grain boundaries of the deformed microstructure did not play an important role in the manipulation of the proportion of the Σ3 n ( n = 1, 2, 3…) type boundaries. Instead, the grain cluster formed by multiple twinning starting from a single nucleus during recrystallization was the key microstructural feature affecting the GBCD. All of the grains in this kind of cluster had Σ3 n mutual misorientations regardless of whether they were adjacent. A large grain cluster containing 91 grains was found in the sample after a small-strain (5 pct) and a high-temperature (1100 °C) recrystallization anneal, and twin relationships up to the ninth generation (Σ39) were found in this cluster. The ratio of cluster size over grain size (including all types of boundaries as defining individual grains) dictated the proportion of Σ3 n boundaries.

Structure and transport at grain boundaries in polycrystalline olivine: An atomic-scale perspective

NASA Astrophysics Data System (ADS)

Mantisi, Boris; Sator, Nicolas; Guillot, Bertrand

2017-12-01

Structure and transport properties at grain boundaries in polycrystalline olivine have been investigated at the atomic scale by molecular dynamics simulation (MD) using an empirical ionocovalent interaction potential. On the time scale of the simulation (a few tens of nanoseconds for a system size of ∼650,000 atoms) grain boundaries and grain interior were identified by mapping the atomic displacements along the simulation run. In the investigated temperature range (1300-1700 K) the mean thickness of the grain boundary phase is evaluated between 0.5 and 2 nm, a value which depends on temperature and grain size. The structure of the grain boundary phase is found to be disordered (amorphous-like) and is different from the one exhibited by the supercooled liquid. The self-diffusion coefficients of major elements in the intergranular region range from ∼10-13 to 10-10 m2/s between 1300 and 1700 K (with DSigb < DOgb < DFegb < DMggb) and are only one order of magnitude smaller than those evaluated in the supercooled melt. In using a newly derived expression for the bulk self-diffusion coefficient it is concluded that the latter one is driven by the grain boundary contribution as long as the grain size is smaller than a centimeter. In assuming that the electrical conduction at grain boundaries is purely ionic, the macroscopic grain boundary conductivity is found to be two orders of magnitude lower than in molten olivine, and one order of magnitude higher than the lattice conductivity. A consequence is that the conductivity of the olivine polycrystal is dominated by the grain interior contribution as soon as the grain size is larger than a micrometer or so. The grain boundary viscosity has been evaluated from the Green-Kubo relation expressing the viscosity as function of the stress tensor time correlation function. In spite of a slow convergence of the calculation by MD, the grain boundary viscosity was estimated about ∼105 Pa s at 1500 K, a value in agreement with high-temperature viscoelastic relaxation data. An interesting information gained from MD is that sliding at grain boundaries is essentially controlled by the internal friction between the intergranular phase and the grain edges.

Constraining cooling rates of UHP metamorphic rocks with closure temperature geospeedometry: a case study from the Dabie orogen

NASA Astrophysics Data System (ADS)

Lloyd, M. K.; Shimizu, N.; Wang, Z.; Zheng, Y.

2011-12-01

UHP metamorphic rocks can reach peak temperatures and pressures >800°C and >3GPa, and provide unique opportunities for studying geochemical processes in subduction zones. How and how fast they were exhumed are, however, still outstanding questions. Here we report SIMS-based Zr concentrations in rutiles from an eclogite sample from Huangzhen in the South Dabie low-T/UHP zone, east-central China, and present a closure temperature-based approach to constrain the cooling/exhumation rate of UHP rocks. Li et al. (2004) put peak metamorphism at a time prior to 236.1 ± 4.2 Ma., but estimates for peak temperatures and pressures in South Dabie vary wildly depending on the rock suite. The fine-grained eclogites in the Dabie orogen were estimated to have reached conditions of 641-839 °C and 2.00-3.54 GPa (Shi and Wang, 2006) based on Fe-Mg partition thermometry and metamorphic phase equilibria. These samples were reported to contain quartz, zircon, and rutile phases that reached thermodynamic equilibrium with each other. In this study, Zr concentrations of rutiles were obtained using the Cameca IMS 1280 ion microprobe at Northeast National Ion Microprobe Facility, by converting secondary ion intensity ratios, 90Zr/46Ti, to concentrations using rutile standards described by Luvizotto et al. (2009), with analytical uncertainties of 5.1%. Temperatures were then calculated using the method of Ferry and Watson (2007). It was found that Zr concentrations range from 38.6(2.4) to 134.6(4.5) ppm, resulting in a temperature range of 504(24) to 583(27)°C for 72 grains with size spanning from 62 to 440 microns cross in long axis. Minor rim-ward decrease of Zr content was observed with no appreciable temperature decrease. Assuming that the rutiles grew at one stage during the peak metamorphism and that their Zr concentrations were independent of pressure, a cooling rate can be estimated for the target sample. By applying the Dodson (1973) formula for closure temperature in conjunction with the Cherniak et al. (2007) diffusion rates for Zr in rutile to the core of each grain, we derived a maximum possible cooling rate to allow for complete peak temperature memory loss: i.e., since the largest grain requires most diffusion to reset, we are able to limit the maximum possible cooling rate for all grains in the sample to 5.4 ± 15.6 °C/my. This value is comparable to estimates for the Central Dabie mid-T/UHP eclogite (e.g., Li et al., 2000). Li XP et al. (2004) CMP, 148, 443-470. Shi & Wang (2006) J. Met. Geol., 24, 803-822. Luvizotto et al. (2009) Chem. Geol., 3-4, 346-369. Ferry & Watson (2007) CMP, 154, 429-437. Dodson (1973) CMP, 40, 259-274. Cherniak et al. (2007) EPSL, 261, 267-279. Li SG et al. (2000) GCA, 64, 1077-1093.

Grain-Boundary Resistance in Copper Interconnects: From an Atomistic Model to a Neural Network

NASA Astrophysics Data System (ADS)

Valencia, Daniel; Wilson, Evan; Jiang, Zhengping; Valencia-Zapata, Gustavo A.; Wang, Kuang-Chung; Klimeck, Gerhard; Povolotskyi, Michael

2018-04-01

Orientation effects on the specific resistance of copper grain boundaries are studied systematically with two different atomistic tight-binding methods. A methodology is developed to model the specific resistance of grain boundaries in the ballistic limit using the embedded atom model, tight- binding methods, and nonequilibrium Green's functions. The methodology is validated against first-principles calculations for thin films with a single coincident grain boundary, with 6.4% deviation in the specific resistance. A statistical ensemble of 600 large, random structures with grains is studied. For structures with three grains, it is found that the distribution of specific resistances is close to normal. Finally, a compact model for grain-boundary-specific resistance is constructed based on a neural network.

Combined measurement of surface, grain boundary and lattice diffusion coefficients on olivine bi-crystals

NASA Astrophysics Data System (ADS)

Marquardt, Katharina; Dohmen, Ralf; Wagner, Johannes

2014-05-01

Diffusion along interface and grain boundaries provides an efficient pathway and may control chemical transport in rocks as well as their mechanical strength. Besides the significant relevance of these diffusion processes for various geologic processes, experimental data are still very limited (e.g., Dohmen & Milke, 2010). Most of these data were measured using polycrystalline materials and the formalism of LeClaire (1951) to fit integrated concentration depth profiles. To correctly apply this formalism, certain boundary conditions of the diffusion problem need to be fulfilled, e.g., surface diffusion is ignored, and furthermore the lattice diffusion coefficient has to be known from other studies or is an additional fitting parameter, which produces some ambiguity in the derived grain boundary diffusion coefficients. We developed an experimental setup where we can measure the lattice and grain boundary diffusion coefficients simultaneously but independent and demonstrate the relevance of surface diffusion for typical grain boundary diffusion experiments. We performed Mg2SiO4 bicrystal diffusion experiments, where a single grain boundary is covered by a thin-film of pure Ni2SiO4 acting as diffusant source, produced by pulsed laser deposition. The investigated grain boundary is a 60° (011)/[100]. This specific grain boundary configuration was modeled using molecular dynamics for comparison with the experimental observations in the transmission electron microscope (TEM). Both, experiment and model are in good agreement regarding the misorientation, whereas there are still some disagreements regarding the strain fields along the grain boundary that are of outmost importance for the strengths of the material. The subsequent diffusion experiments were carried out in the temperature range between 800° and 1450° C. The inter diffusion profiles were measured using the TEMs energy dispersive x-ray spectrometer standardized using the Cliff-Lorimer equation and EMPA measurements. To evaluate the obtained diffusion profiles we adapted the isolated grain boundary model, first proposed by Fisher (1951) to match several observations: (i) Anisotropic diffusion in forsterite, (ii) fast diffusion along the grain boundary, (iii) fast diffusion on the surface of the sample. The latter process is needed to explain an additional flux of material from the surface into the grain boundary. Surface and grain boundary diffusion coefficients are on the order of 10000 times faster than diffusion in the lattice. Another observation was that in some regions the diffusion profiles in the lattice were greatly extended. TEM observations suggest here that surface defects (nano-cracks, ect.) have been present, which apparently enhanced the diffusion through the bulk lattice. Dohmen, R., & Milke, R. (2010). Diffusion in Polycrystalline Materials: Grain Boundaries, Mathematical Models, and Experimental Data. Reviews in Mineralogy and Geochemistry, 72(1), 921-970. Fisher, J. C. (1951). Calculations of Diffusion Penetration Curves for Surface and Grain Boundary Diffusion. Journal of Applied Physics, 22(1), 74-77. Le Claire, A. D. (1951). Grain boundary diffusion in metals. Philosophical Magazine A, 42(328), 468-474.

Investigation of olivine and orthopyroxene grain boundaries by atom probe tomography

NASA Astrophysics Data System (ADS)

Krawczynski, M.; Skemer, P. A.; Bachhav, M.; Dong, Y.; Marquis, E. A.

2016-12-01

Accurate chemical analysis at grain boundaries is challenging by traditional microscopic techniques, especially for poor conducting geological samples. Atom probe tomography (APT) is a unique technique that can elucidate chemistry and 3-D distribution of elements within a sample volume at the sub-nanometer length scale. With advances in laser and sample preparation techniques in the last decade, APT is now successfully applied to a wide range of poor conducting materials like metal oxides, ceramics, and biological minerals. In this study, we apply the APT technique to investigate the grain boundary chemistry of orthopyroxene (opx) and olivine. These minerals are the most abundant in the upper mantle and their grain boundaries may be important geochemical reservoirs in Earth. Moreover, physical properties such as grain boundary diffusivity, conductivity, and mobility, are likely influenced by the presence or absence of impurities. Single crystals of opx and olivine grains, separated from a San Carlos xenolith, were deformed at 1 GPa and 1500 K. Plastic deformation promoted dynamic recrystallization, creating new grain boundaries within a chemically homogeneous medium. Needle shaped specimens of opx-opx and olivine-olivine grain boundaries were prepared using standard lift out techniques and a dual beam focused ion beam (FIB). APT analyses were performed in laser mode with laser energy of 50 pJ/pulse, repetition rate of 200 kHz, and detection rate of 1%. A 3-D distribution of elements was reconstructed and 1-D profiles across the grain boundary have been calculated. Fe, Al, and Ca show enrichments at the grain boundaries for both phases, consistent with previous studies that used STEM/EDX or EPMA techniques. Although qualitatively similar, the spatial resolution of the APT method is significantly better than other methods, and our data show that the grain-boundary enrichment of minor elements in both olivine and pyroxene compositions is limited to a region no greater than 2-4 nm thick. These new data place constraints on the thickness of the grain boundary zone with unparalleled precision, allowing more accurate calculation of partition coefficients as well as diffusion coefficients from experimental studies of grain boundary diffusion.

Improvement of the Reliability of Dielectrics for MLCC

NASA Astrophysics Data System (ADS)

Nakamura, Tomoyuki; Yao, Takayuki; Ikeda, Jun; Kubodera, Noriyuki; Takagi, Hiroshi

2011-10-01

To achieve enough reliability of monolithic ceramic capacitor, it is important to know the contribution of grain boundary and grain interior to its reliability and insulation resistance. As the number of grain boundaries per layer increased, mean time to failure (MTTF) increased. In addition, as the number of grain boundaries per layer increased, samples showed lower current leakage in the measured electric field range. Using these data, the grain boundary E-J curves were determined by simulation. As a result, temperature and electric field dependence of insulation resistance of grain boundary were very low. The insulation characteristics of one BaTiO3 grain per layer were examined. The resistance and reliability of grain interior were very low. To improve the degradation resistance of grain interior, Ca-doped BaTiO3-based dielectrics were developed. The influence of Ca substitution on MTTF was investigated and it was found out that MTTF increased with the increase of Ca substitution.

How to interpret current-voltage relationships of blocking grain boundaries in oxygen ionic conductors.

PubMed

Kim, Seong K; Khodorov, Sergey; Chen, Chien-Ting; Kim, Sangtae; Lubomirsky, Igor

2013-06-14

A new model based on a linear diffusion equation is proposed to explain the current-voltage characteristics of blocking grain boundaries in Y-doped CeO2 in particular. One can also expect that the model can be applicable to the ionic conductors with blocking grain boundaries, in general. The model considers an infinitely long chain of identical grains separated by grain boundaries, which are treated as regions in which depletion layers of mobile ions are formed due to trapping of immobile charges that do not depend on the applied voltage as well as temperature. The model assumes that (1) the grain boundaries do not represent physical blocking layers, which implies that if there is a second phase at the grain boundaries, then it is too thin to impede ion diffusion and (2) the ions follow Boltzmann distribution throughout the materials. Despite its simplicity, the model successfully reproduces the "power law": current proportional to voltage power n and illustrated with the experimental example of Y-doped ceria. The model also correctly predicts that the product nT, where T is the temperature in K, is constant and is proportional to the grain boundary potential as long as the charge at the grain boundaries remains trapped. The latter allows its direct determination from the current-voltage characteristics and promises considerable simplification in the analysis of the electrical characteristics of the grain boundaries with respect to the models currently in use.

Analysis of the electron-beam-induced current of a polycrystalline p-n junction when the diffusion lengths of the material on either side of a grain boundary differ

NASA Technical Reports Server (NTRS)

Von Roos, O.; Luke, K. L.

1984-01-01

The short circuit current generated by the electron beam of a scanning electron microscope in p-n junctions is reduced by enhanced recombination at grain boundaries in polycrystalline material. Frequently, grain boundaries separate the semiconductor into regions possessing different minority carrier life times. This markedly affects the short circuit current I(sc) as a function of scanning distance from the grain boundary. It will be shown theoretically that (1) the minimum of the I(sc) in crossing the grain boundary with the scanning electron beam is shifted away from the grain boundary toward the region with smaller life time (shorter diffusion length), (2) the magnitude of the minimum differs markedly from those calculated under the assumption of equal diffusion lengths on either side of the grain boundary, and (3) the minimum disappears altogether for small surface recombination velocities (s less than 10,000 cm/s). These effects become negligible, however, for large recombination velocities s at grain boundaries. For p-type silicon this happens for s not less than 100,000 cm/s.

Local texture and grain boundary misorientations in high H(C) oxide superconductors

NASA Astrophysics Data System (ADS)

Kroeger, D. M.; Goyal, A.; Specht, E. D.; Tkaczyk, J. E.; Sutliff, J.; Deluca, J. A.; Wang, Z. L.; Riley, G. N., Jr.

The orientations of hundreds of contiguous grains in high J(C) TlBa2Ca2Cu3O(x) deposits and (Bi, Pb)2 Sr2Ca2Cu3O(y) powder-in-tube tapes have been determined from electron back scatter diffraction patterns (EBSP). The misorientation angles and axes of rotation (angle/axis pairs) for grain boundaries connecting these grains were calculated. For both materials the population of low angle boundaries was found to be much larger than expected from calculations based on the macroscopic texture. The TlBa2Ca2Cu3O(x) deposits exhibit pronounced local texture which has been defined by EBSP and x-ray diffraction. Locally grains show significant in-plane (a-axis) alignment even though macroscopically a-axes are random, indicating the presence of colonies of grains with similar a-axis orientations. In (Bi, Pb)2 Sr2Ca2Cu3O(x) tapes no local texture was observed. In both materials the existence of connected networks of small angle grain boundaries can be inferred. Coincident site lattice (CSL) grain boundaries are also present in higher than expected numbers. Grain boundary energy thus appears to play a significant role in enhancing the population of potentially strongly-linked boundaries. We propose that long range strongly-linked conduction occurs through a percolative network small angle (and perhaps CSL) grain boundaries.

Impact of Wide-Ranging Nanoscale Chemistry on Band Structure at Cu(In, Ga)Se 2 Grain Boundaries

DOE Office of Scientific and Technical Information (OSTI.GOV)

Stokes, Adam; Al-Jassim, Mowafak; Diercks, David

The relative chemistry from grain interiors to grain boundaries help explain why grain boundaries may be beneficial, detrimental or benign towards device performance. 3D Nanoscale chemical analysis extracted from atom probe tomography (APT) (10’s of parts-per-million chemical sensitivity and sub-nanometer spatial resolution) of twenty grain boundaries in a high-efficiency Cu(In, Ga)Se 2 solar cell shows the matrix and alkali concentrations are wide-ranging. The concentration profiles are then related to band structure which provide a unique insight into grain boundary electrical performance. Fluctuating Cu, In and Ga concentrations result in a wide distribution of potential barriers at the valence band maximummore » (VBM) (-10 to -160 meV) and the conduction band minimum (CBM) (-20 to -70 meV). Furthermore, Na and K segregation is not correlated to hampering donors, (In, Ga) Cu and V Se, contrary to what has been previously reported. In addition, Na and K are predicted to be n-type dopants at grain boundaries. An overall band structure at grain boundaries is presented.« less

Impact of Wide-Ranging Nanoscale Chemistry on Band Structure at Cu(In, Ga)Se 2 Grain Boundaries

DOE PAGES

Stokes, Adam; Al-Jassim, Mowafak; Diercks, David; ...

2017-10-26

The relative chemistry from grain interiors to grain boundaries help explain why grain boundaries may be beneficial, detrimental or benign towards device performance. 3D Nanoscale chemical analysis extracted from atom probe tomography (APT) (10’s of parts-per-million chemical sensitivity and sub-nanometer spatial resolution) of twenty grain boundaries in a high-efficiency Cu(In, Ga)Se 2 solar cell shows the matrix and alkali concentrations are wide-ranging. The concentration profiles are then related to band structure which provide a unique insight into grain boundary electrical performance. Fluctuating Cu, In and Ga concentrations result in a wide distribution of potential barriers at the valence band maximummore » (VBM) (-10 to -160 meV) and the conduction band minimum (CBM) (-20 to -70 meV). Furthermore, Na and K segregation is not correlated to hampering donors, (In, Ga) Cu and V Se, contrary to what has been previously reported. In addition, Na and K are predicted to be n-type dopants at grain boundaries. An overall band structure at grain boundaries is presented.« less

The role of boundary variability in polycrystalline grain-boundary diffusion

NASA Astrophysics Data System (ADS)

Moghadam, M. M.; Rickman, J. M.; Harmer, M. P.; Chan, H. M.

2015-01-01

We investigate the impact of grain-boundary variability on mass transport in a polycrystal. More specifically, we perform both numerical and analytical studies of steady-state diffusion in prototypical microstructures in which there is either a discrete spectrum of grain-boundary activation energies or else a complex distribution of grain-boundary character, and hence a continuous spectrum of boundary activation energies. An effective diffusivity is calculated for these structures using simplified multi-state models and, for the case of a continuous spectrum, employing experimentally obtained grain-boundary energy data. We identify different diffusive regimes for these cases and quantify deviations from Arrhenius behavior using effective medium theory. Finally, we examine the diffusion kinetics of a simplified model of an interfacial layering (i.e., complexion) transition.

Effect of one-step recrystallization on the grain boundary evolution of CoCrFeMnNi high entropy alloy and its subsystems.

PubMed

Chen, Bo-Ru; Yeh, An-Chou; Yeh, Jien-Wei

2016-02-29

In this study, the grain boundary evolution of equiatomic CoCrFeMnNi, CoCrFeNi, and FeCoNi alloys after one-step recrystallization were investigated. The special boundary fraction and twin density of these alloys were evaluated by electron backscatter diffraction analysis. Among the three alloys tested, FeCoNi exhibited the highest special boundary fraction and twin density after one-step recrystallization. The special boundary increment after one-step recrystallization was mainly affected by grain boundary velocity, while twin density was mainly affected by average grain boundary energy and twin boundary energy.

Insight into the grain boundary effect on the ionic transport of yttria-stabilized zirconia at elevated temperatures from a molecular modeling perspective

NASA Astrophysics Data System (ADS)

Chang, Kai-Shiun; Lin, Yi-Feng; Tung, Kuo-Lun

A molecular dynamics (MD) simulation is used to reveal the grain boundary effect on the ionic transport of yttria-stabilized zirconia (YSZ). The oxygen ion displacements and diffusivities of the ideal and grain boundary-inserted YSZ models are analyzed at elevated temperatures. An optimized Y 2O 3 concentration within YSZ for the best ionic conductivity is achieved by balancing the trade-off between the increased vacancies and the decreased accessible free space. The mass transfer resistance of the grain boundary in YSZ can be more easily found at higher temperatures by observing the oxygen ion diffusivities or traveling trajectories. At lower temperatures, the grain interior and the grain boundary control the ionic transport. In contrast, the grain boundary effect on the diffusion barrier is gradually eliminated at elevated temperatures. The modeled results in this work agree well with previous experimental data.

Microstructure and mechanical properties of Zr-Si-N films prepared by rf-reactive sputtering

NASA Astrophysics Data System (ADS)

Nose, M.; Chiou, W. A.; Zhou, M.; Mae, T.; Meshii, M.

2002-05-01

ZrN and ZrSiN films were prepared in an rf sputtering apparatus that has a pair of targets facing each other (referred to as the facing target-type rf sputtering). Films were deposited on silicon wafers without bias application or substrate heating in order to examine only the effect of silicon addition to the transition metal nitride films. The contents of zirconium, nitrogen, and silicon of the films were determined with an electron probe microanalyzer. The transmission electron microscopy studies were carried out in addition to x-ray diffraction. For the high resolution transmission electron microscopy observation, the field emission type transmission electron microscope was used, which provides a point-to-point resolution of 0.1 nm. The samples were observed both parallel and perpendicular to the film surface, which were plane and cross sectional views, respectively. In order to investigate the relationship between the mechanical properties and microstructure of films, the hardness was measured by a nanoindentation system at room temperature. The load was selected to keep the impression depth below 60 nm (not more than 5% of film thickness) so that the influence from the substrate can be neglected. The hardness of the films increases with small Si additions reaching the maximum value of 35 GPa at around 3 at. % Si. The tendency to grow columnar grains was strongest around this composition, while grains became equiaxial above 5 at. % of Si. The films containing 12.8% Si, which showed the lowest hardness of 18 GPa, consist of nanocrystal grains. The presence of ZrN nanocrystals embedded in Si3N4 was not observed in the present study. The hardening mechanism due to the addition of small amounts of Si in ZrN can not be determined at this time. The grain size and residual stress can make minor contributions to the hardening. A possibility of solid solution hardening due to atomistic strain, such as nitrogen atoms at interstitial sites or other point defects is postulated and should be examined further.

Understanding luminescence properties of grain boundaries in GaN thin films and their atomistic origin

NASA Astrophysics Data System (ADS)

Yoo, Hyobin; Yoon, Sangmoon; Chung, Kunook; Kang, Seoung-Hun; Kwon, Young-Kyun; Yi, Gyu-Chul; Kim, Miyoung

2018-03-01

We report our findings on the optical properties of grain boundaries in GaN films grown on graphene layers and discuss their atomistic origin. We combine electron backscatter diffraction with cathodoluminescence to directly correlate the structural defects with their optical properties, enabling the high-precision local luminescence measurement of the grain boundaries in GaN films. To further understand the atomistic origin of the luminescence properties, we carefully probed atomic core structures of the grain boundaries by exploiting aberration-corrected scanning transmission electron microscopy. The atomic core structures of grain boundaries show different ordering behaviors compared with those observed previously in threading dislocations. Energetics of the grain boundary core structures and their correlation with electronic structures were studied by first principles calculation.

Effective search for stable segregation configurations at grain boundaries with data-mining techniques

NASA Astrophysics Data System (ADS)

Kiyohara, Shin; Mizoguchi, Teruyasu

2018-03-01

Grain boundary segregation of dopants plays a crucial role in materials properties. To investigate the dopant segregation behavior at the grain boundary, an enormous number of combinations have to be considered in the segregation of multiple dopants at the complex grain boundary structures. Here, two data mining techniques, the random-forests regression and the genetic algorithm, were applied to determine stable segregation sites at grain boundaries efficiently. Using the random-forests method, a predictive model was constructed from 2% of the segregation configurations and it has been shown that this model could determine the stable segregation configurations. Furthermore, the genetic algorithm also successfully determined the most stable segregation configuration with great efficiency. We demonstrate that these approaches are quite effective to investigate the dopant segregation behaviors at grain boundaries.

Effect of irradiation on mechanical properties of symmetrical grain boundaries investigated by atomic simulations

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, X. Y.; Gao, N.; Setyawan, W.

Tensile response of irradiated symmetric grain boundaries to externally applied strain has been studied using atomic simulation methods. The absorption of irradiation induced defects by grain boundaries has been confirmed to degrade the mechanical properties of grain boundaries through the change of its under- taken deformation mechanism. Atomic rearrangement, the formations of a stress accumulation region and vacancy-rich zone and the nucleation and movement of dislocations under stress effect have been observed after the displacement cascades in grain boundaries, which are considered as main reasons to induce above degradation. These results suggest the necessity of considering both trap- ping efficiencymore » to defects and the mechanical property change of irradiated grain boundaries for further development of radiation resistant materials.« less

An Analysis of Hole Trapping at Grain Boundary or Poly-Si Floating-Body MOSFET.

PubMed

Jang, Taejin; Baek, Myung-Hyun; Kim, Hyungjin; Park, Byung-Gook

2018-09-01

In this paper, we demonstrate the characteristics of the floating body effect of poly-silicon with grain boundary by SENTAURUS™ TCAD simulation. As drain voltage increases, impact ionization occurs at the drain-channel junction. And these holes created by impact ionization are deposited on the bottom of the body to change the threshold voltage. This feature, the kink effect, is also observed in fully depleted silicon on insulator because grain boundary of the poly-silicon serve as a storage to trap the holes. We simulate the transfer curve depending on the density and position of the grain boundary. The trap density of the grain boundary affects the device characteristics significantly. However similar properties appear except where the grain boundary is located on the drain side.

Detection of expansion at large angle grain boundaries using electron diffraction

DOE Office of Scientific and Technical Information (OSTI.GOV)

Balluffi, R.W.; Bristowe, P.D.

1984-02-01

Lamarre and Sass (LS) (Scripta Metall. 17: 1141(1983)) observed a grain boundary electron diffraction effect from a large angle twist boundary which they claim can be used to obtain the volume expansion at the grain boundary in a direction normal to it. This paper considers the case where the intensity from the grain boundary region, is close to lattice reflections on the same element of the boundary diffraction lattice. Analysis of this complex problem show that the simplified model of LS is misleading in this case. (DLC)

Grain Boundary Character Distributions In Isostructural Materials

NASA Astrophysics Data System (ADS)

Ratanaphan, Sutatch

Anisotropic grain boundary character distributions (GBCDs), which influence macroscopic materials properties, are thought to be controlled by the grain boundary energy anisotropy. Structurally, grain boundary could be viewed as two free surfaces joined together. Grain boundary energy could be simply defined by the total excess energy for creating two free surfaces minus the energy gained when new bonds are formed between these surfaces. This implies that different crystal structure should have different GBEDs and GBCDs. It was recently discovered that grain boundary energy distributions (GBED) in isostructural materials, a class of materials that share the same crystal structure, are directly related to one another. This suggests that GBCDs in isostructural materials might also be related in a similar way. To test this hypothesis, electron backscatter diffraction (EBSD) was used to map grain orientations in Ag, Au, Cu, Fe, and Mo. The GBCDs were determined from the stereological interpretation of EBSD maps containing on the order of 100,000 grains. It was found that the GBCDs of face-centered cubic (FCC) metals are statistically correlated, while the GBCDs of body-centered cubic (BCC) Fe and Mo are not correlated to the GBCD of FCC metals. The degree of the correlations among the FCC metals is weaker if there are significant differences in grain shape or texture. For example, Ag has the weakest correlation to the other FCC materials and also has quantitatively different grain shapes and texture. The relationship between the populations and energies of grain boundaries was also studied. By comparing the GBCDs of Al, Au, Cu, and Ni to the energies of 388 grain boundaries previously calculated by the Embedded Atom Method (EAM), we observed a moderately inverse correlation between the relative areas of grain boundaries and their energies. Interestingly, there are strong inverse correlations between the energies and populations of the most common grain boundaries (Sigma3, Sigma9, and Sigma27). Because the enhancement of twin related boundaries due to the prevalence Sigma3 boundaries results in a decrease in the grain boundary populations for the other boundary types, this inverse correlation is influenced by the crystallographic constraints at triple junctions. In other words, having an anisotropic misorientation distribution with strong maxima for certain boundaries biases the inverse correlation between grain boundary population and energy for other boundaries and causes different slopes at each misorientation. Interestingly, the inverse correlation at each misorientation is consistent with the Boltzmann distribution. Based on our results, it is possible to predict the GBCDs and GBEDs in isostructural polycrystalline materials by using a single GBCD and GBED. This principle is demonstrated by predicting the GBCD and GBED of Actinium (Ac). To investigate the GBED in the isostructural BCC metals, the energies of 408 grain boundaries in Fe and Mo were computed using atomistic simulations based on the embedded-atom method (EAM) potential. We found that the calculated boundary energies in Fe and Mo were strongly correlated and scaled with the ratio of the cohesive energy divided by the square of the lattice constant (Ecoh/a02). We would expect that the GBCD of Fe and Mo might be correlated in a similar manner to that of FCC metals. To test this hypothesis, we compared the GBCDs of Fe and Mo. We found that the GBCDs of Fe and Mo are moderately and strongly correlated when all boundary types and only Sigma3 boundaries were considered, respectively. In this thesis, the results demonstrated that the GBCDs of isostructural materials are correlated with one another and the magnitudes of correlation coefficients varied. Reduced correlations were observed when there were differences in the microstructure and crystallographic texture. The inverse relationship between grain boundary population and energy is more strongly correlated at each misorientation than over the entire five macroscopic parameters of grain boundary, especially when there is significant misorientation texture. This relationship leads to GBCDs of isostructural materials that are also more strongly correlated at each misorientation than over the entire grain boundary space.

Discovering the Role of Grain Boundary Complexions in Materials

DOE Office of Scientific and Technical Information (OSTI.GOV)

Harmer, Martin P.

Grain boundaries are inherently an area of disorder in polycrystalline materials which define the transport and various other material properties. The relationship between the interfacial chemistry, structure and the material properties is not well understood. Among the various taxonomies for grain boundaries, Grain Boundary Complexion is a relatively new conceptual scheme that relates the structure and kinetic properties of grain boundaries. In this classification scheme, grain boundaries are considered to be distinct three dimensional (the thickness being considerably smaller as compared to the other two dimensions but nonetheless discernible) equilibrium thermodynamic phases abutted between two crystalline phases. The stability andmore » structure of these interfacial phases are dictated by various thermodynamic variables such as temperature, stress (pressure), interfacial chemistry (chemical potential) and most importantly by the energies of the adjoining crystal surfaces. These phases are only stable within the constraint of the adjoining grains. Although these interfacial phases are not stable in bulk form, they can transform from one complexion to another as a function of various thermodynamic variables analogous to the behavior of bulk phases. Examples of different complexions have been reported in various publications. However, a systematic investigation exploring the existence of grain boundary complexions in material systems other than alumina remains to be done. Although the role of interfacial chemistry on grain boundary complexions in alumina has been addressed, a clear understanding of the underlying thermodynamics governing complexion formation is lacking. Finally, the effects of grain boundary complexions in bulk material properties are widely unknown. Factors above urge a thorough exploration of grain boundary complexions in a range of different materials systems The purpose of the current program is to verify the existence of grain boundary complexion in a range of materials systems, and to characterize their structures, range of stability and selected physical properties. First, an Au-based bilayer interfacial phase was discovered at a bicrystal boundary in the Si-Au system. This bilayer transitioned abruptly to an intrinsic (“clean”) grain boundary phase, suggesting first-order phase behavior. This study represents the discovery of grain boundary complexions in a completely new system, i.e., a semiconductor-metal system, giving further support to the expectation that grain boundary complexions are a general phenomenon not limited to any particular class of materials. The TiO 2-CuO system exhibited four grain boundary interfacial phases: a monolayer, disordered bilayer, disordered trilayer, and non-wetting nanoscale amorphous drop (which likely resulted from dewetting of a nanoscale IGF). SiO 2 contamination was discovered in the TiO 2-CuO samples, and we hypothesize that this impurity may have caused an “order-disorder” transition to occur. In other words, we expect that pure TiO 2-CuO may have a higher tendency to exhibit ordered bilayer and trilayer complexions, which may also exhibit a well-defined order-disorder transition temperature. In this effort we have also identified unique complexion transitions in yttria and strontium titanate.« less

Revealing Grain Boundary Sliding from Textures of a Deformed Nanocrystalline Pd–Au Alloy

PubMed Central

Skrotzki, Werner; Zhao, Yajun; Pukenas, Aurimas; Birringer, Rainer

2018-01-01

Employing a recent modeling scheme for grain boundary sliding [Zhao et al. Adv. Eng. Mater. 2017, doi:10.1002/adem.201700212], crystallographic textures were simulated for nanocrystalline fcc metals deformed in shear compression. It is shown that, as grain boundary sliding increases, the texture strength decreases while the signature of the texture type remains the same. Grain boundary sliding affects the texture components differently with respect to intensity and angular position. A comparison of a simulation and an experiment on a Pd–10 atom % Au alloy with a 15 nm grain size reveals that, at room temperature, the predominant deformation mode is grain boundary sliding contributing to strain by about 60%. PMID:29370130

Grain boundary misorientations and percolative current paths in high-{ital J}{sub {ital c}} powder-in-tube (Bi,Pb){sub 2}Sr{sub 3}Ca{sub 3}Cu{sub 3}O{sub {ital x}}

DOE Office of Scientific and Technical Information (OSTI.GOV)

Goyal, A.; Specht, E.D.; Kroeger, D.M.

1995-05-22

Grain orientations and grain boundary misorientations in high-{ital J}{sub {ital c}}, powder-in-tube (PIT) (Bi,Pb){sub 2}Sr{sub 2}Ca{sub 2}Cu{sub 3}O{sub {ital x}} (Bi-2223) were determined using electron backscatter Kikuchi diffraction and x-ray microdiffraction. Data collected from over 113 spatially correlated grains, resulting in 227 grain boundaries, show that over 40% of the boundaries are {Sigma}1 or small angle (less than 15{degree}). In addition, 8% of the boundaries are within the Brandon criterion for CSLs (sigma larger than 1 and less than 50). Grain boundary ``texture maps`` derived from the electron microscope image and orientation data reveal the presence of percolative paths betweenmore » low energy boundaries.« less

Chevron Defect at the Intersection of Grain Boundaries with Free Surfaces in Au

NASA Astrophysics Data System (ADS)

Radetic, T.; Lançon, F.; Dahmen, U.

2002-08-01

We have identified a new defect at the intersection between grain boundaries and surfaces in Au using atomic resolution transmission electron microscopy. At the junction line of 90° <110> tilt grain boundaries of (110)-(001) orientation with the free surface, a small segment of the grain boundary, about 1nm in length, dissociates into a triangular region with a chevronlike stacking disorder and a distorted hcp structure. The structure and stability of these defects are confirmed by atomistic simulations, and we point out the relationship with the one-dimensional incommensurate structure of the grain boundary.

Grain boundary oxidation and fatigue crack growth at elevated temperatures

NASA Technical Reports Server (NTRS)

Liu, H. W.; Oshida, Y.

1986-01-01

Fatigue crack growth rate at elevated temperatures can be accelerated by grain boundary oxidation. Grain boundary oxidation kinetics and the statistical distribution of grain boundary oxide penetration depth were studied. At a constant delta K-level and at a constant test temperature, fatigue crack growth rate, da/dN, is a function of cyclic frequency, nu. A fatigue crack growth model of intermittent micro-ruptures of grain boundary oxide is constructed. The model is consistent with the experimental observations that, in the low frequency region, da/dN is inversely proportional to nu, and fatigue crack growth is intergranular.

Kinetics and thermodynamics associated with Bi adsorption transitions at Cu and Ni grain boundaries

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tai, Kaiping; Feng, Lin; Dillon, Shen J.

The grain boundary diffusivity of Au in Cu and Cu-Bi, and Cu in Ni and Ni-Bi are characterized by secondary ion mass spectroscopy depth profiling. Samples are equilibrated in a Bi containing atmosphere at temperatures above and below the onset of grain boundary adsorption transitions, sometimes called complexion transitions. A simple thermo-kinetic model is used to estimate the relative entropic contributions to the grain boundary energies. The results indicate that the entropy term plays a major role in promoting thermally and chemically induced grain boundary complexion transition.

Grain boundary character, and carbide size and spatial distribution in a ternary nickel alloy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liu, H.; Gao, M.; Harlow, D.G.

1995-06-01

A preliminary investigation of the grain boundary character and its relationship to carbide distribution in a Ni-18Cr-18Fe ternary alloy was conducted. The results showed that there was a strong preference for the formation of {Sigma}3 (44.6%) and twin-related {Sigma}9 and {Sigma}27 CSL boundaries. If the coherent {Sigma}3{sub c} twin and the twin-related boundaries are excluded, then the distribution would consist of nearly 80% random (high angle) boundaries and about 20% CSL (with {Sigma} {<=} 49) boundaries. The size and spacing of grain boundary carbides were influenced by grain boundary {Sigma}; the carbides being smaller and more closely spaced on themore » {Sigma}1, {Sigma}9 and {Sigma}27 boundaries, and none could be resolved on the coherent {Sigma}3 twin boundaries. The results could be understood, in part, in terms of the influence of grain boundary energy, but the understanding is incomplete. Further studies are in progress and will be reported.« less

O(minus 2) grain boundary diffusion and grain growth in pure dense MgO

NASA Technical Reports Server (NTRS)

Kapadia, C. M.; Leipold, M. H.

1973-01-01

Grain growth behavior in fully dense compacts of MgO of very high purity was studied, and the results compared with other similar behaving materials. The activation energy for the intrinsic self-diffusion of Mg(2minus) is discussed along with the grain boundary diffusion of O(2minus). Grain boundary diffusion of O(2minus) is proposed as the controlling mechanism for grain growth.

Atomistic Simulations of Grain Boundary Pinning in CuFe Alloys

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zepeda-Ruiz, L A; Gilmer, G H; Sadigh, B

2005-05-22

The authors apply a hybrid Monte Carlo-molecular dynamics code to the study of grain boundary motion upon annealing of pure Cu and Cu with low concentrations of Fe. The hybrid simulations account for segregation and precipitation of the low solubility Fe, together with curvature driven grain boundary motion. Grain boundaries in two different systems, a {Sigma}7+U-shaped half-loop grain and a nanocrystalline sample, were found to be pinned in the presence of Fe concentrations exceeding 3%.

DOE Office of Scientific and Technical Information (OSTI.GOV)

O’Brien, Christopher J.; Foiles, Stephen M.

Low-mobility twin grain boundaries dominate the microstructure of grain boundary-engineered materials and are critical to understanding their plastic deformation behaviour. The presence of solutes, such as hydrogen, has a profound effect on the thermodynamic stability of the grain boundaries. This work examines the case of a Σ3 grain boundary at inclinations from 0° ≤ Φ ≤ 90°. The angle Φ corresponds to the rotation of the Σ3 (1 1 1) < 1 1 0 > (coherent) into the Σ3 (1 1 2) < 1 1 0 > (lateral) twin boundary. To this end, atomistic models of inclined grain boundaries, utilisingmore » empirical potentials, are used to elucidate the finite-temperature boundary structure while grand canonical Monte Carlo models are applied to determine the degree of hydrogen segregation. In order to understand the boundary structure and segregation behaviour of hydrogen, the structural unit description of inclined twin grain boundaries is found to provide insight into explaining the observed variation of excess enthalpy and excess hydrogen concentration on inclination angle, but the explanatory power is limited by how the enthalpy of segregation is affected by hydrogen concentration. At higher concentrations, the grain boundaries undergo a defaceting transition. In order to develop a more complete mesoscale model of the interfacial behaviour, an analytical model of boundary energy and hydrogen segregation that relies on modelling the boundary as arrays of discrete 1/3 < 1 1 1 > disconnections is constructed. Lastly, the complex interaction of boundary reconstruction and concentration-dependent segregation behaviour exhibited by inclined twin grain boundaries limits the range of applicability of such an analytical model and illustrates the fundamental limitations for a structural unit model description of segregation in lower stacking fault energy materials.« less

Grain boundary phase transformations in PtAu and relevance to thermal stabilization of bulk nanocrystalline metals

DOE Office of Scientific and Technical Information (OSTI.GOV)

O’Brien, C. J.; Barr, C. M.; Price, P. M.

There has recently been a great deal of interest in employing immiscible solutes to stabilize nanocrystalline microstructures. Existing modeling efforts largely rely on mesoscale Monte Carlo approaches that employ a simplified model of the microstructure and result in highly homogeneous segregation to grain boundaries. However, there is ample evidence from experimental and modeling studies that demonstrates segregation to grain boundaries is highly non-uniform and sensitive to boundary character. This work employs a realistic nanocrystalline microstructure with experimentally relevant global solute concentrations to illustrate inhomogeneous boundary segregation. Furthermore, experiments quantifying segregation in thin films are reported that corroborate the prediction thatmore » grain boundary segregation is highly inhomogeneous. In addition to grain boundary structure modifying the degree of segregation, the existence of a phase transformation between low and high solute content grain boundaries is predicted. In order to conduct this study, new embedded atom method interatomic potentials are developed for Pt, Au, and the PtAu binary alloy.« less

Grain boundary phase transformations in PtAu and relevance to thermal stabilization of bulk nanocrystalline metals

DOE PAGES

O’Brien, C. J.; Barr, C. M.; Price, P. M.; ...

2017-10-31

There has recently been a great deal of interest in employing immiscible solutes to stabilize nanocrystalline microstructures. Existing modeling efforts largely rely on mesoscale Monte Carlo approaches that employ a simplified model of the microstructure and result in highly homogeneous segregation to grain boundaries. However, there is ample evidence from experimental and modeling studies that demonstrates segregation to grain boundaries is highly non-uniform and sensitive to boundary character. This work employs a realistic nanocrystalline microstructure with experimentally relevant global solute concentrations to illustrate inhomogeneous boundary segregation. Furthermore, experiments quantifying segregation in thin films are reported that corroborate the prediction thatmore » grain boundary segregation is highly inhomogeneous. In addition to grain boundary structure modifying the degree of segregation, the existence of a phase transformation between low and high solute content grain boundaries is predicted. In order to conduct this study, new embedded atom method interatomic potentials are developed for Pt, Au, and the PtAu binary alloy.« less

Structure and Geochemistry of the Continental-Oceanic Crust Boundary of the Red Sea and the Rifted Margin of Western Arabia

NASA Astrophysics Data System (ADS)

Dilek, Y.; Furnes, H.; Schoenberg, R.

2009-12-01

The continental-oceanic crust boundary and an incipient oceanic crust of the Red Sea opening are exposed within the Arabian plate along a narrow zone of the Tihama Asir coastal plain in SW Saudi Arabia. Dike swarms, layered gabbros, granophyres and basalts of the 22 Ma Tihama Asir (TA) continental margin ophiolite represent products of magmatic differentiation formed during the initial stages of rifting between the African and Arabian plates. Nearly 4-km-wide zone of NW-trending sheeted dikes are the first products of mafic magmatism associated with incipient oceanic crust formation following the initial continental breakup. Gabbro intrusions are composed of cpx-ol-gabbro, cpx-gabbro, and norite/troctolite, and are crosscut by fine-grained basaltic dikes. Granophyre bodies intrude the sheeted dike swarms and are locally intrusive into the gabbros. Regional Bouger gravity anomalies suggest that the Miocene mafic crust represented by the TA complex extends westward beneath the coastal plain sedimentary rocks and the main trough of the Red Sea. The TA complex marks an incipient Red Sea oceanic crust that was accreted to the NE side of the newly formed continental rift in the earliest stages of seafloor spreading. Its basaltic to trachyandesitic lavas and dikes straddle the subalkaline-mildly alkaline boundary. Incompatible trace element relationships (e.g. Zr-Ti, Zr-P) indicate two distinct populations. The REE concentrations show an overall enrichment compared to N-MORB; light REEs are enriched over the heavy ones ((La/Yb)n > 1), pointing to an E-MORB influence. Nd-isotope data show ɛNd values ranging from +4 to +8, supporting an E-MORB melt source. The relatively large variations in ɛNd values also suggest various degrees of involvement of continental crust during ascent and emplacement, or by mixing of another mantle source.

Growth of platinum fibers using the micro-pulling-down method

NASA Astrophysics Data System (ADS)

Nihei, Takayuki; Yokota, Yuui; Arakawa, Mototaka; Ohashi, Yuji; Kurosawa, Shunsuke; Kamada, Kei; Chani, Valery; Yoshikawa, Akira

2017-06-01

Platinum (Pt) crystalline fibers were grown from the melt by the micro-pulling-down (μ-PD) method using the ZrO2 ceramics crucible. The diameter of the grown Pt fiber was controlled by the ϕ1 mm outlet made at the bottom of the crucible and the Pt fiber of 0.95±0.03 mm in diameter and over 5 m in length was obtained at 10 mm/min pulling-down rate. In addition, the Pt fiber was grown at 1-110 mm/min pulling rates while the liquid-solid interface reached the bottom of the crucible and the crystal growth became unstable at 120 mm/min pulling rate. Few grain boundaries were observed in the scanning electron microscopy image of the Pt fibers and there were some spots with high intensity in the pole figures.

Quantitative image analysis of WE43-T6 cracking behavior

NASA Astrophysics Data System (ADS)

Ahmad, A.; Yahya, Z.

2013-06-01

Environment-assisted cracking of WE43 cast magnesium (4.2 wt.% Yt, 2.3 wt.% Nd, 0.7% Zr, 0.8% HRE) in the T6 peak-aged condition was induced in ambient air in notched specimens. The mechanism of fracture was studied using electron backscatter diffraction, serial sectioning and in situ observations of crack propagation. The intermetallic (rare earthed-enriched divorced intermetallic retained at grain boundaries and predominantly at triple points) material was found to play a significant role in initiating cracks which leads to failure of this material. Quantitative measurements were required for this project. The populations of the intermetallic and clusters of intermetallic particles were analyzed using image analysis of metallographic images. This is part of the work to generate a theoretical model of the effect of notch geometry on the static fatigue strength of this material.

Grain boundary, triple junction and quadruple point mobility controlled normal grain growth

NASA Astrophysics Data System (ADS)

Rios, P. R.; Glicksman, M. E.

2015-07-01

Reduction in stored free energy provides the thermodynamic driving force for grain and bubble growth in polycrystals and foams. Evolution of polycrystalline networks exhibit the additional complication that grain growth may be controlled by several kinetic mechanisms through which the decrease in network energy occurs. Polyhedral boundaries, triple junctions (TJs), and quadruple points (QPs) are the geometrically distinct elements of three dimensional networks that follow Plateau's rules, provided that grain growth is limited by diffusion through, and motion of, cell boundaries. Shvindlerman and co-workers have long recognized the kinetic influences on polycrystalline grain growth of network TJs and QPs. Moreover, the emergence of interesting polycrystalline nanomaterials underscored that TJs can indeed influence grain growth kinetics. Currently there exist few detailed studies concerned either with network distributions of grain size, number of faces per grain, or with 'grain trajectories', when grain growth is limited by the motion of its TJs or QPs. By contrast there exist abundant studies of classical grain growth limited by boundary mobility. This study is focused on a topological/geometrical representation of polycrystals to obtain statistical predictions of the grain size and face number distributions, as well as growth 'trajectories' during steady-state grain growth. Three limits to grain growth are considered, with grain growth kinetics controlled by boundary, TJ, and QP mobilities.

Processing and microstructure of Nb-1 percent Zr-0.1 percent C alloy sheet

NASA Technical Reports Server (NTRS)

Uz, Mehmet; Titran, Robert H.

1992-01-01

A systematic study was carried out to evaluate the effects of processing on the microstructure of Nb-1 wt. pct. Zr-0.1 wt. pct. C alloy sheet. The samples were fabricated by cold rolling different sheet bars that were single-, double- or triple-extruded at 1900 K. Heat treatment consisted on one- or two-step annealing of different samples at temperatures ranging from 1350 to 1850 K. The assessment of the effects of processing on microstructure involved characterization of the precipitates including the type, crystal structure, chemistry and distribution within the material as well as an examination of the grain structure. A combination of various analytical and metallographic techniques were used on both the sheet samples and the residue extracted from them. The results show that the relatively coarse orthorhombic Nb2C carbides in the as-rolled samples transformed to rather fine cubic monocarbides of Nb and Zr with varying Zr/Nb ratios upon subsequent heat treatment. The relative amount of the cubic carbides and the Zr/Nb ratio increased with increasing number of extrusions prior to cold rolling. Furthermore, the size and the aspect ratio of the grains appear to be strong functions of the processing history of the material. These and other results obtained will be presented with the emphasis on a possible relationship between processing and microstructure.

Fluid distribution in grain boundaries of natural fine-grained rock salt deformed at low differential stress (Qom Kuh salt fountain, central Iran): Implications for rheology and transport properties

NASA Astrophysics Data System (ADS)

Desbois, Guillaume; Urai, Janos L.; de Bresser, Johannes H. P.

2012-10-01

We used a combination of broad ion beam cross-sectioning and cryogenic SEM to image polished surfaces and corresponding pairs of fractured grain boundaries in an investigation of grain boundary microstructures and fluid distribution in naturally deformed halite from the Qom Kuh salt glacier (central Iran). At the scale of observations, four types of fluid-filled grain boundary can be distinguished by morphology (from straight to wavy), thickness (from 5000 to 50 nm) and the presence of fluid inclusions. The mobility of the brine is shown after cutting the inclusions by broad ion beam (BIB) in vacuum and fine-grained halite forms efflorescence and precipitates on internal walls of inclusions. At cryogenic temperature, grain boundary brine is shown either as continuous film or in isolated inclusions. The halite-halite grain boundary between isolated fluid inclusions is interpreted to have formed by fluid-assisted grain boundary healing. Preliminary experiments on the samples at shear stress conditions of natural salt glacier show very slow strain rates (7.4 × 10-10 s-1 and 1 × 10-9 s-1), which are less than expected for pressure solution creep. Both microstructures and deformation experiments suggest interfacial energy-driven grain boundary healing and therefore rendering inactive the pressure solution creep in our samples. This result disagrees with previous microstructural studies of the same sample, which showed microstructural evidence for pressure solution (and dislocation creep). Different explanations are discussed, which imply that both healing and reactivation of grain boundaries are important in salt glaciers, leading to heterogeneous distribution of deformation mechanisms and strain rates in both space and time.

Effect of one-step recrystallization on the grain boundary evolution of CoCrFeMnNi high entropy alloy and its subsystems

PubMed Central

Chen, Bo-Ru; Yeh, An-Chou; Yeh, Jien-Wei

2016-01-01

In this study, the grain boundary evolution of equiatomic CoCrFeMnNi, CoCrFeNi, and FeCoNi alloys after one-step recrystallization were investigated. The special boundary fraction and twin density of these alloys were evaluated by electron backscatter diffraction analysis. Among the three alloys tested, FeCoNi exhibited the highest special boundary fraction and twin density after one-step recrystallization. The special boundary increment after one-step recrystallization was mainly affected by grain boundary velocity, while twin density was mainly affected by average grain boundary energy and twin boundary energy. PMID:26923713

Effect of Grain Boundary Misorientation on Electromigration in Lead-Free Solder Joints

NASA Astrophysics Data System (ADS)

Tasooji, Amaneh; Lara, Leticia; Lee, Kyuoh

2014-12-01

Reduction in microelectronic interconnect size gives rise to solder bumps consisting of few grains, approaching a single- or bicrystal grain morphology in C4 bumps. Single grain anisotropy, individual grain orientation, presence of easy diffusion paths along grain boundaries, and the increased current density in these small solder bumps aggravate electromigration. This reduces the reliability of the entire microelectronic system. This paper focuses on electromigration behavior in Pb-free solder, specifically the Sn-0.7 wt.%Cu alloy. We discuss the effects of texture, grain orientation, and grain boundary misorientation angle on electromigration (EM) and intermetallic compound formation in EM-tested C4 bumps. The detailed electron backscatter diffraction (EBSD) analysis used in this study reveals the greater influence of grain boundary misorientation on solder bump electromigration compared with the effect associated with individual grain orientation.

A theoretical model of grain boundary self-diffusion in metals with phase transitions (case study into titanium and zirconium)

NASA Astrophysics Data System (ADS)

Semenycheva, Alexandra V.; Chuvil'deev, Vladimir N.; Nokhrin, Aleksey V.

2018-05-01

The paper offers a model describing the process of grain boundary self-diffusion in metals with phase transitions in the solid state. The model is based on ideas and approaches found in the theory of non-equilibrium grain boundaries. The range of application of basic relations contained in this theory is shown to expand, as they can be used to calculate the parameters of grain boundary self-diffusion in high-temperature and low-temperature phases of metals with a phase transition. The model constructed is used to calculate grain boundary self-diffusion activation energy in titanium and zirconium and an explanation is provided as to their abnormally low values in the low-temperature phase. The values of grain boundary self-diffusion activation energy are in good agreement with the experiment.

Influence of grain boundaries on the distribution of components in binary alloys

NASA Astrophysics Data System (ADS)

L'vov, P. E.; Svetukhin, V. V.

2017-12-01

Based on the free-energy density functional method (the Cahn-Hilliard equation), a phenomenological model that describes the influence of grain boundaries on the distribution of components in binary alloys has been developed. The model is built on the assumption of the difference between the interaction parameters of solid solution components in the bulk and at the grain boundary. The difference scheme based on the spectral method is proposed to solve the Cahn-Hilliard equation with interaction parameters depending on coordinates. Depending on the ratio between the interaction parameters in the bulk and at the grain boundary, temperature, and alloy composition, the model can give rise to different types of distribution of a dissolved component, namely, either depletion or enrichment of the grain-boundary area, preferential grainboundary precipitation, competitive precipitation in the bulk and at the grain boundary, etc.

TOPICAL REVIEW: Importance of low-angle grain boundaries in YBa2Cu3O7-δ coated conductors

NASA Astrophysics Data System (ADS)

Durrell, J. H.; Rutter, N. A.

2009-01-01

Over the past ten years the perception of grain boundaries in YBa2Cu3O7-δ conductors has changed greatly. They are now not a problem to be eliminated, but an inevitable and potentially favourable part of the material. This change has arisen as a consequence of new manufacturing techniques which result in excellent grain alignment, reducing the spread of grain boundary misorientation angles. At the same time there is considerable recent evidence which indicates that the variation of properties of grain boundaries with mismatch angle is more complex than a simple exponential decrease in critical current. This is due to the fact that low-angle grain boundaries represent a qualitatively different system to high-angle boundaries. The time is therefore right for a targeted review of research into low-angle YBa2Cu3O7-δ grain boundaries. This article does not purport to be a comprehensive review of the physics of grain boundaries as found in YBa2Cu3O7-δ in general; for a broader overview we would recommend that the reader consult the comprehensive review of Hilgenkamp and Mannhart (2002 Rev. Mod. Phys. 74 485). The purpose of this article is to review the origin and properties of the low-angle grain boundaries found in YBa2Cu3O7-δ coated conductors both individually and as a collective system.

Modeling of stresses at grain boundaries with respect to occurrence of stress corrosion cracking

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kozaczek, K.J.; Sinharoy, A.; Ruud, C.O.

The distributions of elastic stresses/strains in the grain boundary regions were studied by the analytical and the finite element models. The grain boundaries represent the sites where stress concentration occurs as a result of discontinuity of elastic properties across the grain boundary and the presence of second phase particles elastically different from the surrounding matrix grains. A quantitative analysis of those stresses for steels and nickel based alloys showed that the stress concentrations in the grain boundary regions are high enough to cause a local microplastic deformation even when the material is in the macroscopic elastic regime. The stress redistributionmore » as a result of such a plastic deformation was discussed.« less

Simulation of electron transport across charged grain boundaries

NASA Astrophysics Data System (ADS)

Srikant, V.; Clarke, D. R.; Evans, P. V.

1996-09-01

The I-V (current density-electric field) characteristics of low-angle grain boundaries consisting of periodic arrays of charged dislocations are computed using a quasiclassical molecular dynamics approach. Below a critical value of the grain boundary misorientation, the computed I-V characteristics are linear whereas above they are nonlinear. The degree of nonlinearity and the voltage onset of nonlinearity are found to be dependent on the grain boundary misorientation.

Direct Correlations of Grain Boundary Potentials to Chemical States and Dielectric Properties of Doped CaCu3Ti4O12 Thin Films.

PubMed

Cho, Ahra; Han, Chan Su; Kang, Meenjoo; Choi, Wooseok; Lee, Jihwan; Jeon, Jaecheol; Yu, Sujae; Jung, Ye Seul; Cho, Yong Soo

2018-05-09

Colossal dielectric constant CaCu 3 Ti 4 O 12 has been recognized as one of the rare materials having intrinsic interfacial polarization and thus unusual dielectric characteristics, in which the electrical state of the grain boundary is critical. Here, the direct correlation between the grain boundary potential and relative permittivity is proposed for the CaCu 3 Ti 4 O 12 thin films doped with Zn, Ga, Mn, and Ag as characterized by Kelvin probe force microscopy. The dopants are intended to provide the examples of variable grain boundary potentials that are driven by chemical states including Cu + , Ti 3+ , and oxygen vacancy. Grain boundary potential is nearly linearly proportional to the dielectric constant. This effect is attributed to the increased charge accumulation near the grain boundary, depending on the choice of the dopant. As an example, 1 mol % Ag-doped CaCu 3 Ti 4 O 12 thin films demonstrate the best relative permittivity as associated with a higher grain boundary potential of 120.3 mV compared with 82.6 mV for the reference film. The chemical states across grain boundaries were further verified by using spherical aberration-corrected scanning transmission electron microscopy with the simultaneous electron energy loss spectroscopy.

Dislocation Content Measured Via 3D HR-EBSD Near a Grain Boundary in an AlCu Oligocrystal

NASA Technical Reports Server (NTRS)

Ruggles, Timothy; Hochhalter, Jacob; Homer, Eric

2016-01-01

Interactions between dislocations and grain boundaries are poorly understood and crucial to mesoscale plasticity modeling. Much of our understanding of dislocation-grain boundary interaction comes from atomistic simulations and TEM studies, both of which are extremely limited in scale. High angular resolution EBSD-based continuum dislocation microscopy provides a way of measuring dislocation activity at length scales and accuracies relevant to crystal plasticity, but it is limited as a two-dimensional technique, meaning the character of the grain boundary and the complete dislocation activity is difficult to recover. However, the commercialization of plasma FIB dual-beam microscopes have made 3D EBSD studies all the more feasible. The objective of this work is to apply high angular resolution cross correlation EBSD to a 3D EBSD data set collected by serial sectioning in a FIB to characterize dislocation interaction with a grain boundary. Three dimensional high angular resolution cross correlation EBSD analysis was applied to an AlCu oligocrystal to measure dislocation densities around a grain boundary. Distortion derivatives associated with the plasma FIB serial sectioning were higher than expected, possibly due to geometric uncertainty between layers. Future work will focus on mitigating the geometric uncertainty and examining more regions of interest along the grain boundary to glean information on dislocation-grain boundary interaction.

Stress Distribution During Deformation of Polycrystalline Aluminum by Molecular-Dynamics and Finite-Element Modeling

NASA Technical Reports Server (NTRS)

Yamakov, V.; Saether, E.; Phillips, D.; Glaessgen, E. H.

2004-01-01

In this paper, a multiscale modelling strategy is used to study the effect of grain-boundary sliding on stress localization in a polycrystalline microstructure with an uneven distribution of grain size. The development of the molecular dynamics (MD) analysis used to interrogate idealized grain microstructures with various types of grain boundaries and the multiscale modelling strategies for modelling large systems of grains is discussed. Both molecular-dynamics and finite-element (FE) simulations for idealized polycrystalline models of identical geometry are presented with the purpose of demonstrating the effectiveness of the adapted finite-element method using cohesive zone models to reproduce grain-boundary sliding and its effect on the stress distribution in a polycrystalline metal. The yield properties of the grain-boundary interface, used in the FE simulations, are extracted from a MD simulation on a bicrystal. The models allow for the study of the load transfer between adjacent grains of very different size through grain-boundary sliding during deformation. A large-scale FE simulation of 100 grains of a typical microstructure is then presented to reveal that the stress distribution due to grain-boundary sliding during uniform tensile strain can lead to stress localization of two to three times the background stress, thus suggesting a significant effect on the failure properties of the metal.

Role of Grain Boundaries under Long-Time Radiation

NASA Astrophysics Data System (ADS)

Zhu, Yichao; Luo, Jing; Guo, Xu; Xiang, Yang; Chapman, Stephen Jonathan

2018-06-01

Materials containing a high proportion of grain boundaries offer significant potential for the development of radiation-resistant structural materials. However, a proper understanding of the connection between the radiation-induced microstructural behavior of a grain boundary and its impact at long natural time scales is still missing. In this Letter, point defect absorption at interfaces is summarized by a jump Robin-type condition at a coarse-grained level, wherein the role of interface microstructure is effectively taken into account. Then a concise formula linking the sink strength of a polycrystalline aggregate with its grain size is introduced and is well compared with experimental observation. Based on the derived model, a coarse-grained formulation incorporating the coupled evolution of grain boundaries and point defects is proposed, so as to underpin the study of long-time morphological evolution of grains induced by irradiation. Our simulation results suggest that the presence of point defect sources within a grain further accelerates its shrinking process, and radiation tends to trigger the extension of twin boundary sections.

Pore and grain boundary migration under a temperature gradient: A phase-field model study

DOE PAGES

Biner, S. B.

2016-03-16

In this study, the collective migration behavior of pores and grain boundaries under a temperature gradient is studied for simple single crystal, bi-crystal and polycrystal configurations with a phase-field model formulism. For simulation of the microstructure of solids, composed of pores and grain boundaries, the results indicate that not only the volume fraction of pores, but also its spatial partitioning between the grain boundary junctions and the grain boundary segments appears to be important. In addition to various physical properties, the evolution kinetics, under given temperature gradients, will be strongly influenced with the initial morphology of a poly-crystalline microstructure.

Correlating Atom Probe Tomography with Atomic-Resolved Scanning Transmission Electron Microscopy: Example of Segregation at Silicon Grain Boundaries.

PubMed

Stoffers, Andreas; Barthel, Juri; Liebscher, Christian H; Gault, Baptiste; Cojocaru-Mirédin, Oana; Scheu, Christina; Raabe, Dierk

2017-04-01

In the course of a thorough investigation of the performance-structure-chemistry interdependency at silicon grain boundaries, we successfully developed a method to systematically correlate aberration-corrected scanning transmission electron microscopy and atom probe tomography. The correlative approach is conducted on individual APT and TEM specimens, with the option to perform both investigations on the same specimen in the future. In the present case of a Σ9 grain boundary, joint mapping of the atomistic details of the grain boundary topology, in conjunction with chemical decoration, enables a deeper understanding of the segregation of impurities observed at such grain boundaries.

Stress-induced solid-state amorphization of nanocrystalline Ni and NiZr investigated by atomistic simulations

NASA Astrophysics Data System (ADS)

Meraj, Md.; Deng, Chuang; Pal, Snehanshu

2018-01-01

In this study, the feasibility of stress induced solid-state amorphization (SSA) of nanocrystalline (NC) Ni and NiZr alloys having ˜10 nm grain size has been investigated under constant tensile load (uniaxial and triaxial) via molecular dynamics simulations. In order to track the structural evaluation in both NC Ni and NiZr alloys during the SSA process, various types of analysis have been used, including simulated X-ray diffraction, centro-symmetry parameter, Voronoi cluster, common neighbor analysis, and radial distribution function. It is found that SSA in both NC Ni and NiZr alloys can only be achieved under triaxial loading conditions, and the hydrostatic tensile stress required for SSA is significantly lower when at. % Zr is increased in the NC NiZr alloy. Specifically, SSA in NC Ni and Ni-5 at. % Zr alloy was observed only when the temperature and hydrostatic tensile stress reached 800 K and 6 GPa, while SSA could occur in NC Ni-10 at. % Zr alloy under just 2 GPa of hydrostatic tensile stress at 300 K.

On the small angle twist sub-grain boundaries in Ti3AlC2.

PubMed

Zhang, Hui; Zhang, Chao; Hu, Tao; Zhan, Xun; Wang, Xiaohui; Zhou, Yanchun

2016-04-01

Tilt-dominated grain boundaries have been investigated in depth in the deformation of MAX phases. In stark contrast, another important type of grain boundaries, twist grain boundaries, have long been overlooked. Here, we report on the observation of small angle twist sub-grain boundaries in a typical MAX phase Ti3AlC2 compressed at 1200 °C, which comprise hexagonal screw dislocation networks formed by basal dislocation reactions. By first-principles investigations on atomic-scale deformation and general stacking fault energy landscapes, it is unequivocally demonstrated that the twist sub-grain boundaries are most likely located between Al and Ti4f (Ti located at the 4f Wyckoff sites of P63/mmc) layers, with breaking of the weakly bonded Al-Ti4f. The twist angle increases with the increase of deformation and is estimated to be around 0.5° for a deformation of 26%. This work may shed light on sub-grain boundaries of MAX phases, and provide fundamental information for future atomic-scale simulations.

Enhancing grain boundary ionic conductivity in mixed ionic–electronic conductors

DOE PAGES

Lin, Ye; Fang, Shumin; Su, Dong; ...

2015-04-10

Mixed ionic–electronic conductors are widely used in devices for energy conversion and storage. Grain boundaries in these materials have nanoscale spatial dimensions, which can generate substantial resistance to ionic transport due to dopant segregation. Here, we report the concept of targeted phase formation in a Ce 0.8Gd 0.2O 2₋δ–CoFe 2O 4 composite that serves to enhance the grain boundary ionic conductivity. Using transmission electron microscopy and spectroscopy approaches, we probe the grain boundary charge distribution and chemical environments altered by the phase reaction between the two constituents. The formation of an emergent phase successfully avoids segregation of the Gd dopantmore » and depletion of oxygen vacancies at the Ce 0.8Gd 0.2O 2₋δ–Ce 0.8Gd 0.2O 2₋δ grain boundary. This results in superior grain boundary ionic conductivity as demonstrated by the enhanced oxygen permeation flux. Lastly, this work illustrates the control of mesoscale level transport properties in mixed ionic–electronic conductor composites through processing induced modifications of the grain boundary defect distribution.« less

How grain boundaries affect the efficiency of poly-CdTe solar-cells: A fundamental atomic-scale study of grain boundary dislocation cores using CdTe bi-crystal thin films.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Klie, Robert

It is now widely accepted that grain boundaries in poly-crystalline CdTe thin film devices have a detrimental effect on the minority carrier lifetimes, the open circuit voltage and therefore the overall solar-cell performance. The goal of this project was to develop a fundamental understanding of the role of grain boundaries in CdTe on the carrier life-time, open-circuit voltage, Voc, and the diffusion of impurities. To achieve this goal, i) CdTe bi-crystals were fabricated with various misorientation angels, ii) the atomic- and electronic structures of the grain boundaries were characterized using scanning transmission electron microscopy (STEM), and iii) first-principles density functionalmore » theory modeling was performed on the structures determined by STEM to predict the grain boundary potential. The transport properties and minority carrier lifetimes of the bi-crystal grain boundaries were measured using a variety of approaches, including TRPL, and provided feedback to the characterization and modeling effort about the effectiveness of the proposed models.« less

Enhancing grain boundary ionic conductivity in mixed ionic–electronic conductors

PubMed Central

Lin, Ye; Fang, Shumin; Su, Dong; Brinkman, Kyle S; Chen, Fanglin

2015-01-01

Mixed ionic–electronic conductors are widely used in devices for energy conversion and storage. Grain boundaries in these materials have nanoscale spatial dimensions, which can generate substantial resistance to ionic transport due to dopant segregation. Here, we report the concept of targeted phase formation in a Ce0.8Gd0.2O2−δ–CoFe2O4 composite that serves to enhance the grain boundary ionic conductivity. Using transmission electron microscopy and spectroscopy approaches, we probe the grain boundary charge distribution and chemical environments altered by the phase reaction between the two constituents. The formation of an emergent phase successfully avoids segregation of the Gd dopant and depletion of oxygen vacancies at the Ce0.8Gd0.2O2−δ–Ce0.8Gd0.2O2−δ grain boundary. This results in superior grain boundary ionic conductivity as demonstrated by the enhanced oxygen permeation flux. This work illustrates the control of mesoscale level transport properties in mixed ionic–electronic conductor composites through processing induced modifications of the grain boundary defect distribution. PMID:25857355

Enhancing grain boundary ionic conductivity in mixed ionic-electronic conductors.

PubMed

Lin, Ye; Fang, Shumin; Su, Dong; Brinkman, Kyle S; Chen, Fanglin

2015-04-10

Mixed ionic-electronic conductors are widely used in devices for energy conversion and storage. Grain boundaries in these materials have nanoscale spatial dimensions, which can generate substantial resistance to ionic transport due to dopant segregation. Here, we report the concept of targeted phase formation in a Ce0.8Gd0.2O2-δ-CoFe2O4 composite that serves to enhance the grain boundary ionic conductivity. Using transmission electron microscopy and spectroscopy approaches, we probe the grain boundary charge distribution and chemical environments altered by the phase reaction between the two constituents. The formation of an emergent phase successfully avoids segregation of the Gd dopant and depletion of oxygen vacancies at the Ce0.8Gd0.2O2-δ-Ce0.8Gd0.2O2-δ grain boundary. This results in superior grain boundary ionic conductivity as demonstrated by the enhanced oxygen permeation flux. This work illustrates the control of mesoscale level transport properties in mixed ionic-electronic conductor composites through processing induced modifications of the grain boundary defect distribution.

Enhancing grain boundary ionic conductivity in mixed ionic–electronic conductors

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lin, Ye; Fang, Shumin; Su, Dong

Mixed ionic–electronic conductors are widely used in devices for energy conversion and storage. Grain boundaries in these materials have nanoscale spatial dimensions, which can generate substantial resistance to ionic transport due to dopant segregation. Here, we report the concept of targeted phase formation in a Ce 0.8Gd 0.2O 2₋δ–CoFe 2O 4 composite that serves to enhance the grain boundary ionic conductivity. Using transmission electron microscopy and spectroscopy approaches, we probe the grain boundary charge distribution and chemical environments altered by the phase reaction between the two constituents. The formation of an emergent phase successfully avoids segregation of the Gd dopantmore » and depletion of oxygen vacancies at the Ce 0.8Gd 0.2O 2₋δ–Ce 0.8Gd 0.2O 2₋δ grain boundary. This results in superior grain boundary ionic conductivity as demonstrated by the enhanced oxygen permeation flux. Lastly, this work illustrates the control of mesoscale level transport properties in mixed ionic–electronic conductor composites through processing induced modifications of the grain boundary defect distribution.« less

Three-dimensional study of grain boundary engineering effects on intergranular stress corrosion cracking of 316 stainless steel in high temperature water

NASA Astrophysics Data System (ADS)

Liu, Tingguang; Xia, Shuang; Bai, Qin; Zhou, Bangxin; Zhang, Lefu; Lu, Yonghao; Shoji, Tetsuo

2018-01-01

The intergranular cracks and grain boundary (GB) network of a GB-engineered 316 stainless steel after stress corrosion cracking (SCC) test in high temperature high pressure water of reactor environment were investigated by two-dimensional and three-dimensional (3D) characterization in order to expose the mechanism that GB-engineering mitigates intergranular SCC. The 3D microstructure shown that the essential characteristic of the GB-engineered microstructure is formation of many large twin-boundaries as a result of multiple-twinning, which results in the formation of large grain-clusters. The large grain-clusters played a key role to the improvement of intergranular SCC resistance by GB-engineering. The main intergranular cracks propagated in a zigzag along the outer boundaries of these large grain-clusters because all inner boundaries of the grain-clusters were twin-boundaries (∑3) or twin-related boundaries (∑3n) which had much lower susceptibility to SCC than random boundaries. These large grain-clusters had tree-ring-shaped topology structure and very complex morphology. They got tangled so that difficult to be separated during SCC, resulting in some large crack-bridges retained in the crack surface.

Softening due to disordered grain boundaries in nanocrystalline Co.

PubMed

Yuasa, Motohiro; Hakamada, Masataka; Nakano, Hiromi; Mabuchi, Mamoru; Chino, Yasumasa

2013-08-28

Nanocrystalline Co consisting of fcc and hcp phases was processed by electrodeposition, and its mechanical properties were investigated by hardness tests. In addition, high-resolution transmission electron microscopy observations and molecular dynamics (MD) simulations were performed to investigate the grain boundary structure and dislocation nucleation from the grain boundaries. A large amount of disorders existed at the grain boundaries and stacking faults were formed from the grain boundaries in the as-deposited Co specimen. The as-deposited specimen showed a lower hardness than did the annealed specimen, although the grain size of the former was smaller than that of the latter. The activation volume of the as-deposited specimen (=1.5b(3)) was lower than that of the annealed specimen (=50b(3)), thus indicating that nucleation of dislocations from grain boundaries is more active in the as-deposited specimen than in the annealed specimens. The MD simulations showed that dislocation nucleation was closely related to a change in the defect structures at the boundary. Therefore, it is suggested that a significant amount of defects enhance changes in the defect structures at the boundary, resulting in softening of the as-deposited specimen.

Softening due to disordered grain boundaries in nanocrystalline Co

NASA Astrophysics Data System (ADS)

Yuasa, Motohiro; Hakamada, Masataka; Nakano, Hiromi; Mabuchi, Mamoru; Chino, Yasumasa

2013-08-01

Nanocrystalline Co consisting of fcc and hcp phases was processed by electrodeposition, and its mechanical properties were investigated by hardness tests. In addition, high-resolution transmission electron microscopy observations and molecular dynamics (MD) simulations were performed to investigate the grain boundary structure and dislocation nucleation from the grain boundaries. A large amount of disorders existed at the grain boundaries and stacking faults were formed from the grain boundaries in the as-deposited Co specimen. The as-deposited specimen showed a lower hardness than did the annealed specimen, although the grain size of the former was smaller than that of the latter. The activation volume of the as-deposited specimen (=1.5b3) was lower than that of the annealed specimen (=50b3), thus indicating that nucleation of dislocations from grain boundaries is more active in the as-deposited specimen than in the annealed specimens. The MD simulations showed that dislocation nucleation was closely related to a change in the defect structures at the boundary. Therefore, it is suggested that a significant amount of defects enhance changes in the defect structures at the boundary, resulting in softening of the as-deposited specimen.

Influence of Deformation Mechanisms on the Mechanical Behavior of Metals and Alloys: Experiments, Constitutive Modeling, and Validation

NASA Astrophysics Data System (ADS)

Gray, G. T.; Cerreta, E.; Chen, Shuh Rong; Maudlin, P. J.

2004-06-01

Jim Williams has made seminal contributions to the field of structure / property relations and its controlling effects on the mechanical behavior of metals and alloys. This talk will discuss experimental results illustrating the role of interstitial content, grain size, texture, temperature, and strain rate on the operative deformation mechanisms, mechanical behavior, and substructure evolution in titanium, zirconium, hafnium, and rhenium. Increasing grain size is shown to significantly decrease the dynamic flow strength of Ti and Zr while increasing work-hardening rates due to an increased incidence of deformation twinning. Increasing oxygen interstitial content is shown to significantly alter both the constitutive response and α-ω shock-induced phase transition in Zr. The influence of crystallographic texture on the mechanical behavior in Ti, Zr, and Hf is discussed in terms of slip system and deformation twinning activity. An example of the utility of incorporation of operative deformation mechanisms into a polycrystalline plasticity constitutive model and validation using Taylor cylinder impact testing is presented.

Atom Probe Tomography of Phase and Grain Boundaries in Experimentally-Deformed and Hot-Pressed Wehrlite

NASA Astrophysics Data System (ADS)

Cukjati, J.; Parman, S. W.; Cooper, R. F.; Zhao, N.

2017-12-01

Atom probe tomography (APT) was used to characterize the chemistry of three grain boundaries: an olivine-olivine (ol-ol) and olivine-clinopyroxene (ol-cpx) boundary in fine-grained experimentally-deformed wehrlite and an ol-cpx boundary in a fine-grained, hot-pressed wehrlite. Grain boundaries were extracted and formed into APT tips using a focused ion beam (FIB). The tips were analyzed in a reflectron-equipped LEAP4000HR (Harvard University) at 1% or 0.5% detection rate, 5pJ laser energy and 100kHz pulse rate. Total ion counts are between 40 and 100 million per tip. Examination of grain and phase boundaries in wehrlite are of interest since slow-diffusing and olivine-incompatible cations present in cpx (e.g. Ca and Al) may control diffusion-accommodated grain boundary sliding and affect mantle rheology (Sundberg & Cooper, 2008). At steady state, ol-cpx aggregates are weaker than either ol or cpx end member, the results of which are not currently well-explained. We investigate grain boundary widths to understand the transport of olivine-incompatible elements. Widths of grain/phase boundary chemical segregation are between 3nm and 6nm for deformed ol-ol and ol-cpx samples; minimally-deformed (hot-pressed) samples having slightly wider chemical segregation widths. Chemical segregation widths were determined from profiles of Na, Al, P, Cl, K, Ca, or Ni, although not all listed elements can be used for all samples (e.g. Na, K segregation profiles can only be observed for ol-ol sample). These estimates are consistent with prior estimates of grain boundary segregation by atom probe tomography on ol-ol and opx-opx samples (Bachhav et al., 2015) and are less than ol-ol interface widths analyzed by STEM/EDX (Hiraga, Anderson, & Kohlstedt, 2007). STEM/EDX will be performed on deformed wehrlite to investigate chemical profile as a function of applied stress orientation and at length scales between those observable by APT and EPMA. Determination of phase boundary chemistry and structure allows for better modeling of the rheology of multiphase aggregates and better understanding of diffusive transport and storage of incompatible elements along grain boundaries.

Probing the bulk ionic conductivity by thin film hetero-epitaxial engineering

NASA Astrophysics Data System (ADS)

Pergolesi, Daniele; Roddatis, Vladimir; Fabbri, Emiliana; Schneider, Christof W.; Lippert, Thomas; Traversa, Enrico; Kilner, John A.

2015-02-01

Highly textured thin films with small grain boundary regions can be used as model systems to directly measure the bulk conductivity of oxygen ion conducting oxides. Ionic conducting thin films and epitaxial heterostructures are also widely used to probe the effect of strain on the oxygen ion migration in oxide materials. For the purpose of these investigations a good lattice matching between the film and the substrate is required to promote the ordered film growth. Moreover, the substrate should be a good electrical insulator at high temperature to allow a reliable electrical characterization of the deposited film. Here we report the fabrication of an epitaxial heterostructure made with a double buffer layer of BaZrO3 and SrTiO3 grown on MgO substrates that fulfills both requirements. Based on such template platform, highly ordered (001) epitaxially oriented thin films of 15% Sm-doped CeO2 and 8 mol% Y2O3 stabilized ZrO2 are grown. Bulk conductivities as well as activation energies are measured for both materials, confirming the success of the approach. The reported insulating template platform promises potential application also for the electrical characterization of other novel electrolyte materials that still need a thorough understanding of their ionic conductivity.

Linear Dichroism and Photoluminescence Microscopy Imaging of Grain Boundaries in Crystalline Metal-Free Phthalocyanine Thin Films

NASA Astrophysics Data System (ADS)

Pan, Zhenwen; Lamarche, Cody; Cour, Ishviene; Rawat, Naveen; Manning, Lane; Headrick, Randall; Furis, Madalina; Physics Dept.; Material Science Program, University of Vermont, Burlington, VT 05405 Team

2011-03-01

We employed a combination of linear dichroism and photoluminescence microscopy with spatial resolution of 5 μ m to study the excitonic properties of solution-processed metal-free phthalocyanine (H2Pc) crystalline thin films with millimeter-sized grains. We observe a highly-localized, sharp, monomer-like emission at the high angle grain boundaries, in contrast to samples with more uniform grain orientation where no such feature has been observed. The energy difference between the grain boundary luminescence and the HOMO-LUMO singlet exciton recombination of the crystalline H2Pc is measured to be 160meV. Our systematic survey of grain boundaries indicates this localized state is never present at low angle boundaries where the π -orbital overlap between adjacent grains is significant. It supports recent results which associated a decrease in carrier mobility with the presence of large angle boundaries in similar crystalline pentacene films. This project is supported by DMR- 0722451; DMR-0348354; DMR- 0821268.

Local probe microscopic studies on Al-doped ZnO: Pseudoferroelectricity and band bending at grain boundaries

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kumar, Mohit; Basu, Tanmoy; Som, Tapobrata, E-mail: tsom@iopb.res.in

2016-01-07

In this paper, based on piezoforce measurements, we show the presence of opposite polarization at grains and grain boundaries of Al-doped ZnO (AZO). The polarization can be flipped by 180° in phase by switching the polarity of the applied electric field, revealing the existence of nanoscale pseudoferroelectricity in AZO grown on Pt/TiO{sub 2}/SiO{sub 2}/Si substrate. We also demonstrate an experimental evidence on local band bending at grain boundaries of AZO films using conductive atomic force microscopy and Kelvin probe force microscopy. The presence of an opposite polarization at grains and grain boundaries gives rise to a polarization-driven barrier formation atmore » grain boundaries. With the help of conductive atomic force microscopy, we show that the polarization-driven barrier along with the defect-induced electrostatic potential barrier account for the measured local band bending at grain boundaries. The present study opens a new avenue to understand the charge transport in light of both polarization and electrostatic effects.« less

Atom probe study of grain boundary segregation in technically pure molybdenum

DOE Office of Scientific and Technical Information (OSTI.GOV)

Babinsky, K., E-mail: katharina.babinsky@stud.unileoben.ac.at; Weidow, J., E-mail: jonathan.weidow@chalmers.se; Knabl, W., E-mail: wolfram.knabl@plansee.com

2014-01-15

Molybdenum, a metal with excellent physical, chemical and high-temperature properties, is an interesting material for applications in lighting-technology, high performance electronics, high temperature furnace construction and coating technology. However, its applicability as a structural material is limited because of the poor oxidation resistance at high temperatures and a brittle-to-ductile transition around room temperature, which is influenced by the grain size and the content of interstitial impurities at the grain boundaries. Due to the progress of the powder metallurgical production during the last decades, the amount of impurities in the current quality of molybdenum has become so small that surface sensitivemore » techniques are not applicable anymore. Therefore, the atom probe, which allows the detection of small amounts of impurities as well as their location, seems to be a more suitable technique. However, a site-specific specimen preparation procedure for grain boundaries in refractory metals with a dual focused ion beam/scanning electron microscope is still required. The present investigation describes the development and successful application of such a site-specific preparation technique for grain boundaries in molybdenum, which is significantly improved by a combination with transmission electron microscopy. This complimentary technique helps to improve the visibility of grain boundaries during the last preparation steps and to evidence the presence of grain and subgrain boundaries without segregants in atom probe specimens. Furthermore, in industrially processed and recrystallized molybdenum sheets grain boundary segregation of oxygen, nitrogen and potassium is successfully detected close to segregated regions which are believed to be former sinter pores. - Highlights: • First study of grain boundary segregation in molybdenum by atom probe • Site-specific preparation technique by FIB and TEM successfully developed • Grain boundary segregation of oxygen, nitrogen and potassium found • Segregation in former sinter-pores detected • Presence of grain boundaries without segregation evidenced.« less

Investigation of the fracture mechanics of boride composites

NASA Technical Reports Server (NTRS)

Clougherty, E. V.; Pober, R. L.; Kaufman, L.

1972-01-01

Significant results were obtained in fabrication studies of the role of metallic additives of Zr, Ti, Ni, Fe and Cr on the densification of ZrB2. All elemental additions lower the processing temperatures required to effect full densification of ZrB2. Each addition effects enhanced densification by a clearly distinguishable and different mechanism and the resulting fabricated materials are different. A significant improvement in strength and fracture toughness was obtained for the ZrB2/Ti composition. Mechanical characterization studies for the ZrB2/SiC/C composites and the new ZrB2/Metal materials produced data relevant to the effect of impacting load on measured impact energies, a specimen configuration for which controlled fracture could occur in a suitably hard testing apparatus, and fracture strength data. Controlled fracture--indicative of measurable fracture toughness--was obtained for the ZrB2-SiC-C composite, and a ZrB2/Ti composite fabricated from ZrB2 with an addition of 30 weight per cent Ti. The increased strength and toughness of the ZrB2/Ti composite is consistent with the presence of a significantly large amount of a fine grained acicular phase formed by reaction of Ti with ZrB2 during processing.

Deformation Twins in Nanocrystalline Body-Centered Cubic Mo as Predicted by Molecular Dynamics Simulations

DOE Office of Scientific and Technical Information (OSTI.GOV)

Michael Tonks; Bulent biner; Yongfeng Zhang

2012-10-01

This work studies deformation twins in nanocrystalline body-centered cubic Mo, including the nucleation and growth mechanisms as well as their effects on ductility, through molecular dynamics simulations. The deformation processes of nanocrystalline Mo are simulated using a columnar grain model with three different orientations. The deformation mechanisms identified, including dislocation slip, grain-boundary-mediated plasticity, deformation twins and martensitic transformation, are in agreement with previous studies. In (1 1 0) columnar grains, the deformation is dominated by twinning, which nucleates primarily from the grain boundaries by successive emission of twinning partials and thickens by jog nucleation in the grain interiors. Upon arrestmore » by a grain boundary, the twin may either produce continuous plastic strain across the grain boundary by activating compatible twinning/slip systems or result in intergranular failure in the absence of compatible twinning/slip systems in the neighboring grain. Multiple twinning systems can be activated in the same grain, and the competition between them favors those capable of producing continuous deformation across the grain boundary.« less

Evidence for stable grain boundary melt films in experimentally deformed olivine-orthopyroxene rocks

NASA Astrophysics Data System (ADS)

de Kloe, R.; Drury, M. R.; van Roermund, H. L. M.

The microstructure of olivine-olivine grain boundaries has been studied in experimentally deformed (1200-1227°C, 300MPa) partially molten olivine and olivine-orthopyroxene rocks. In-situ melting produced 1vol% melt in all samples studied. Grain boundary analyses were carried out using a number of transmission electron microscopy techniques. The grain boundary chemistry in undeformed olivine-orthopyroxene starting material showed evidence for the presence of an intergranular phase along some, but not all, of the olivine-olivine boundaries. In the deformed samples, ultrathin Si-rich, Al- and Ca-bearing amorphous films have been observed along all investigated olivine-olivine grain boundaries. The chemistry of the grain boundaries, which is considered to be indicative for the presence of a thin film, was measured with energy-dispersive X-ray spectroscopy (EDX) and energy-filtering imaging. The amorphous nature of the films was confirmed with diffuse dark field imaging, Fresnel fringe imaging, and high-resolution electron microscopy. The films range in thickness from 0.6 to 3.0nm, and EDX analyses show that the presence of Al and Ca is restricted to this ultrathin film along the grain boundaries. Because thin melt films have been observed in all the samples, they are thought to be stable features of the melt microstructure in deformed partially molten rocks. The transition from the occasional presence of films in the undeformed starting material to the general occurrence of the films in deformed materials suggests that deformation promotes the formation and distribution of the films. Alternatively, hot-pressing may be too short for films to develop along all grain boundaries. A difference in creep strength between the studied samples could not be attributed to grain boundary melt films, as these have been found in all deformed samples. However, a weakening effect of grain boundary melt films on olivine rheology could not be ruled out due to the lack of confirmed melt-film free experiments.

Evidence of van Hove singularities in ordered grain boundaries of graphene.

PubMed

Ma, Chuanxu; Sun, Haifeng; Zhao, Yeliang; Li, Bin; Li, Qunxiang; Zhao, Aidi; Wang, Xiaoping; Luo, Yi; Yang, Jinlong; Wang, Bing; Hou, J G

2014-06-06

It has long been under debate whether the electron transport performance of graphene could be enhanced by the possible occurrence of van Hove singularities in grain boundaries. Here, we provide direct experimental evidence to confirm the existence of van Hove singularity states close to the Fermi energy in certain ordered grain boundaries using scanning tunneling microscopy. The intrinsic atomic and electronic structures of two ordered grain boundaries, one with alternative pentagon and heptagon rings and the other with alternative pentagon pair and octagon rings, are determined. It is firmly verified that the carrier concentration and, thus, the conductance around ordered grain boundaries can be significantly enhanced by the van Hove singularity states. This finding strongly suggests that a graphene nanoribbon with a properly embedded ordered grain boundary can be a promising structure to improve the performance of graphene-based electronic devices.

Bubble evolution in Kr-irradiated UO2 during annealing

NASA Astrophysics Data System (ADS)

He, L.; Bai, X. M.; Pakarinen, J.; Jaques, B. J.; Gan, J.; Nelson, A. T.; El-Azab, A.; Allen, T. R.

2017-12-01

Transmission electron microscopy observation of Kr bubble evolution in polycrystalline UO2 annealed at high temperature was conducted in order to understand the inert gas behavior in oxide nuclear fuel. The average diameter of intragranular bubbles increased gradually from 0.8 nm in as-irradiated sample at room temperature to 2.6 nm at 1600 °C and the bubble size distribution changed from a uniform distribution to a bimodal distribution above 1300 °C. The size of intergranular bubbles increased more rapidly than intragranular ones and bubble denuded zones near grain boundaries formed in all the annealed samples. It was found that high-angle grain boundaries held bigger bubbles than low-angle grain boundaries. Complementary atomistic modeling was conducted to interpret the effects of grain boundary character on the Kr segregation. The area density of strong segregation sites in the high-angle grain boundaries is much higher than that in the low angle grain boundaries.

Atomic structure and electronic properties of MgO grain boundaries in tunnelling magnetoresistive devices

PubMed Central

Bean, Jonathan J.; Saito, Mitsuhiro; Fukami, Shunsuke; Sato, Hideo; Ikeda, Shoji; Ohno, Hideo; Ikuhara, Yuichi; McKenna, Keith P.

2017-01-01

Polycrystalline metal oxides find diverse applications in areas such as nanoelectronics, photovoltaics and catalysis. Although grain boundary defects are ubiquitous their structure and electronic properties are very poorly understood since it is extremely challenging to probe the structure of buried interfaces directly. In this paper we combine novel plan-view high-resolution transmission electron microscopy and first principles calculations to provide atomic level understanding of the structure and properties of grain boundaries in the barrier layer of a magnetic tunnel junction. We show that the highly [001] textured MgO films contain numerous tilt grain boundaries. First principles calculations reveal how these grain boundaries are associated with locally reduced band gaps (by up to 3 eV). Using a simple model we show how shunting a proportion of the tunnelling current through grain boundaries imposes limits on the maximum magnetoresistance that can be achieved in devices. PMID:28374755

Effect of solute concentration on grain boundary migration with segregation in stainless steel and model alloys

NASA Astrophysics Data System (ADS)

Kanda, H.; Hashimoto, N.; Takahashi, H.

The phenomenon of grain boundary migration due to boundary diffusion via vacancies is a well-known process for recrystallization and grain growth during annealing. This phenomenon is known as diffusion-induced grain boundary migration (DIGM) and has been recognized in various binary systems. On the other hand, grain boundary migration often occurs under irradiation. Furthermore, such radiation-induced grain boundary migration (RIGM) gives rise to solute segregation. In order to investigate the RIGM mechanism and the interaction between solutes and point defects during the migration, stainless steel and Ni-Si model alloys were electron-irradiated using a HVEM. RIGM was often observed in stainless steels during irradiation. The migration rate of boundary varied, and three stages of the migration were recognized. At lower temperatures, incubation periods up to the occurrence of the boundary migration were observed prior to first stage. These behaviors were recognized particularly for lower solute containing alloys. From the relation between the migration rates at stage I and inverse temperatures, activation energies for the boundary migration were estimated. In comparison to the activation energy without irradiation, these values were very low. This suggests that the RIGM is caused by the flow of mixed-dumbbells toward the grain boundary. The interaction between solute and point defects and the effective defect concentration generating segregation will be discussed.

Role of microstructure in caustic stress corrosion cracking of Alloy 690

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mertz, D.A.; Duda, P.T.; Pica, P.N.

1995-12-31

Alloy 690 has been selected for nuclear heat transport system tubing application in recent commercial reactor plants due to its resistance to multiple types of corrosion attack. Typical corn final heat treatments for this material are a mill-anneal (MA, approximately 1,070 C) to completely dissolve the carbides and develop the final grain structure plus a thermal treatment (TT, approximately 700 C) to precipitate carbides at the grain boundaries. Tubing with grain boundary carbides and no or few intragranular carbides has been found resistant to intergranular stress corrosion cracking (IGSCC) in caustic environments. In this work, first, Alloy 690 plate wasmore » subjected to a variety of MA and MA-TT heat treatments to create microstructures of carbide-decorated grain boundaries and undecorated boundaries. Caustic IGSCC test results were consistent with tubing data. Second, experiments were conducted to understand the mechanism by which caustic-corrosion resistance is imparted to Alloy 690 by grain boundary carbides. Tubing with a fully-developed MA-TT carbide microstructure was strained and heat-treated to create a mixed microstructure of new grain boundaries with no carbide precipitate decoration, intermixed with intragranular carbide strings from prior grain boundaries. Caustic SCC performance of this material was identical to that of material with the MA-TT carbide-decorated grain boundaries. This work suggests that the fundamental cause of good IGSCC resistance of MA-TT Alloy 690 in caustic does not derive solely from grain boundary carbides. It is suggested that matrix strength, as measured by yield stress, could be a controlling factor.« less

Fusion boundary microstructure evolution in aluminum alloys

NASA Astrophysics Data System (ADS)

Kostrivas, Anastasios Dimitrios

2000-10-01

A melting technique was developed to simulate the fusion boundary of aluminum alloys using the GleebleRTM thermal simulator. Using a steel sleeve to contain the aluminum, samples were heated to incremental temperatures above the solidus temperature of a number of alloys. In alloy 2195, a 4wt%Cu-1wt%Li alloy, an equiaxed non-dendritic zone (EQZ) could be formed by heating in the temperature range from approximately 630 to 640°C. At temperatures above 640°C, solidification occurred by the normal epitaxial nucleation and growth mechanism. Fusion boundary behavior was also studied in alloys 5454-H34, 6061-T6, and 2219-T8. Additionally, experimental alloy compositions were produced by making bead on plate welds using an alloy 5454-H32 base metal and 5025 or 5087 filler metals. These filler metals contain zirconium and scandium additions, respectively, and were expected to influence nucleation and growth behavior. Both as-welded and welded/heat treated (540°C and 300°C) substrates were tested by melting simulation, resulting in dendritic and EQZ structures depending on composition and substrate condition. Orientation imaging microscopy (OIM(TM)) was employed to study the crystallographic character of the microstructures produced and to verify the mechanism responsible for EQZ formation. OIM(TM) proved that grains within the EQZ have random orientation. In all other cases, where the simulated microstructures were dendritic in nature, it was shown that epitaxy was the dominant mode of nucleation. The lack of any preferred crystallographic orientation relationship in the EQZ supports a theory proposed by Lippold et al that the EQZ is the result of heterogeneous nucleation within the weld unmixed zone. EDS analysis of the 2195 on STEM revealed particles with ternary composition consisted of Zr, Cu and Al and a tetragonal type crystallographic lattice. Microdiffraction line scans on EQZ grains in the alloy 2195 showed very good agreement between the measured Cu composition within the interior of the non-dendritic grains and the corresponding value the Scheil equation predicts for the first solid to form upon solidification for a binary Al-Cu alloy with identical Cu composition. In the context of the alloys, compositions and substrate conditions examined a mechanistic model for EQZ zone formation is proposed, helpful in adjusting base metal compositions and/or substrate conditions to control fusion boundary microstructure.

Coercivity degradation caused by inhomogeneous grain boundaries in sintered Nd-Fe-B permanent magnets

NASA Astrophysics Data System (ADS)

Chen, Hansheng; Yun, Fan; Qu, Jiangtao; Li, Yingfei; Cheng, Zhenxiang; Fang, Ruhao; Ye, Zhixiao; Ringer, Simon P.; Zheng, Rongkun

2018-05-01

Quantitative correlation between intrinsic coercivity and grain boundaries in three dimensions is critical to further improve the performance of sintered Nd-Fe-B permanent magnets. Here, we quantitatively reveal the local composition variation across and especially along grain boundaries using the powerful atomic-scale analysis technique known as atom probe tomography. We also estimate the saturation magnetization, magnetocrystalline anisotropy constant, and exchange stiffness of the grain boundaries on the basis of the experimentally determined structure and composition. Finally, using micromagnetic simulations, we quantify the intrinsic coercivity degradation caused by inhomogeneous grain boundaries. This approach can be applied to other magnetic materials for the analysis and optimization of magnetic properties.

Size-Dependent Grain-Boundary Structure with Improved Conductive and Mechanical Stabilities in Sub-10-nm Gold Crystals

NASA Astrophysics Data System (ADS)

Wang, Chunyang; Du, Kui; Song, Kepeng; Ye, Xinglong; Qi, Lu; He, Suyun; Tang, Daiming; Lu, Ning; Jin, Haijun; Li, Feng; Ye, Hengqiang

2018-05-01

Low-angle grain boundaries generally exist in the form of dislocation arrays, while high-angle grain boundaries (misorientation angle >15 ° ) exist in the form of structural units in bulk metals. Here, through in situ atomic resolution aberration corrected electron microscopy observations, we report size-dependent grain-boundary structures improving both stabilities of electrical conductivity and mechanical properties in sub-10-nm-sized gold crystals. With the diameter of a nanocrystal decreasing below 10 nm, the high-angle grain boundary in the crystal exists as an array of dislocations. This size effect may be of importance to a new generation of interconnects applications.

Grain boundary stability and influence on ionic conductivity in a disordered perovskite -- a first-principles investigation of lithium lanthanum titanate

DOE PAGES

Alexander, Kathleen C.; Ganesh, P.; Chi, Miaofang; ...

2016-12-01

The origin of ionic conductivity in bulk lithium lanthanum titanate, a promising solid electrolyte for Li-ion batteries, has long been under debate, with experiments showing lower conductivity than predictions. Recent microscopy images show Type I and Type II grain boundaries. Using first-principles based calculations we find that experimentally observed Type I boundaries are more stable compared to the Type II grain boundaries, consistent with their observed relative abundance. Grain boundary stability appears to strongly anti-correlate with the field strength as well as the spatial extent of the space charge region. Ion migration is faster along Type II grain boundaries thanmore » across, consistent with recent experiments of increased conductivity when Type II densities were increased.« less

An Explanation for Bends of 1-Dimensional Nanorods

NASA Astrophysics Data System (ADS)

Mukaida, Masashi; Ichinose, Ataru; Mele, Paolo; Mtsumoto, Kaname; Horii, Shigeru; Yoshida, Yutaka

Growth of artificial pinning centers (APCs) in YBa2Cu3O7-J (YBCO) films are discussed. The APCs used in this research are BaZrO3 and BaSnO3 nanorods which are reported by Mele et al. TEM images show these nanorods graduallybend accordinglywith approachingtoasurfaceof films. This featureshowedagrowth patternlikeafirework. Weexplainthe featureofthe nanorodsas follows;Atanearlygrowth stage, filmsgrowinalayerbylayergrowth mode. The surface of the films is flat and very smooth. After the early growth stage, the film surface gradually becomes rough, indicating the film grows in a Stranski-Krastanov growth mode. This roughness was caused by a spiral growth of films with manysteps. At the step of YBCO films, nanorod materials such as BaZrO3 are supplied from one direction. Then, the center of nanorods sifts to the same direction of the step flow. Then, the nanorods bend to the edge of the grains in the films. As a grain in spiral growth had a convex surface, nanorods bent to the direction perpendicular to the grain surface. Finally, nanorods in rough grains form firework structures.

Factors influencing the coupling between non-180° domain switching and lattice strain in perovskite piezoceramics

NASA Astrophysics Data System (ADS)

Kumar, Naveen; Khatua, Dipak Kumar; Mahale, Bhoopesh; Ranjan, Rajeev

2018-04-01

Domain switching and lattice strain are known to be important processes contributing to the large electromechanical response observed in perovskite-based piezoelectrics. However, there is a lack of clarity regarding the coupling between the two phenomena, and the factors which influence this coupling. Here, we report a systematic investigation to understand the factors influencing the coupling between domain switching and lattice strain in perovskite piezoelectrics by x-ray diffraction in situ with electric field. In a slight departure from the conventional approach, we employ a strategy which enables x-ray diffraction study in situ with electric field on randomly oriented piezoelectric grains in their unclamped (free) state. Experiments were carried out on two different systems (1 -x ) PbTi O3-(x ) BiSc O3 and (1 -x ) PbTi O3-(x ) PbZr O3 in their rhombohedral phase. We found that lattice strain along the nonpolar 〈100〉 R rhombohedral direction varies linearly with the non-180° domain switching fraction (η111). We introduce a parameter β to characterize the strength of coupling between the two phenomena and show that the coupling is enhanced when the system approaches the morphotropic phase boundary. We also demonstrate that the grain-to-grain interaction nearly doubles this coupling in a dense piezoelectric ceramic.

Microstructural investigation of current barriers in high temperature superconducting tapes and coated conductors

NASA Astrophysics Data System (ADS)

Reeves, Jodi Lynn

Microstructural barriers to supercurrent occur on many length scales in all high temperature oxide superconductors. Eliminating microstructural barriers is key to making these potentially valuable materials more favorable for commercial applications. In silver-sheathed Bi2Sr2CaCu 2Ox (Bi-2212) tapes and multifilaments, the principal barriers on the scale of 10--100's of micrometers are bubbling, porosity, second phase particles, and poorly aligned grains. In state-of-the-art YBa2 Cu3Ox (YBCO) coated conductors, supercurrent barriers on the 0.1--100mum scale are grain boundaries. This thesis work clarifies the role of grain boundaries in the nickel substrate of RABiTS (Rolling Assisted Biaxially Textured Substrate) coated conductors. Plan-view SEM imaging, focused ion beam cutting, magneto-optical imaging and grain orientation mapping were used to determine barriers to supercurrent. Experiments showed enhanced magnetic flux penetration, and hence reduced Jc, in the YBCO above nearly all nickel grain boundaries with misorientation angles (theta) greater than 5°, independent of the rotation axis. Monochromatic backscattered electron Kikuchi pattern percolation maps imply there is a fully connected current path through the YBCO microstructure within the chosen tolerance angle criterion of the map. However, it is the grain boundary map that displays the constrictions of the current path. Therefore, grain boundary maps are better tools for illustrating supercurrent barriers than percolation maps. Grain boundary maps and grain orientation maps were used to investigate how the texture of the substrate was transferred to the buffer layers and to the superconductor. Most grasp boundaries in the nickel were replicated in the buffer and superconductor layers with the same misorientation angle. Anisotropic growth and/or surface energy minimization may be responsible for the improvement in c-axis alignment in the YBCO over the buffer layer. However, the YBCO mosaic spread did not eliminate high angle grain boundaries, since >5° boundaries were still seen in YBCO grain boundary maps. The results of this study on microstructural current barriers show that Jc improvements in RABiTS-type coated conductors require eliminating theta > 5° boundaries in the nickel substrate.

Precession electron diffraction for SiC grain boundary characterization in unirradiated TRISO fuel

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lillo, T. M.; van Rooyen, I. J.; Wu, Y. Q.

Precession electron diffraction (PED), a transmission electron microscopy-based technique, has been evaluated for the suitability for evaluating grain boundary character in the SiC layer of tristructural isotropic (TRISO) fuel. Although the ultimate goal is to determine the grain boundary characteristics of fission product containing grain boundaries of neutron irradiated SiC, our work reports the effect of transmission electron microscope (TEM) lamella thickness on quality of data and establishes a baseline comparison on grain boundary characteristics determined previously using a conventional EBSD scanning electron microscope (SEM) based technique. In general, it was determined that the lamella thickness produced using the standardmore » FIB fabrication process, is sufficient to provide reliable PED measurements with thicker lamellae (~120 nm) produce higher quality orientation data. Analysis of grain boundary character from the TEM-based PED data showed a much lower fraction of low angle grain boundaries compared to SEM-based EBSD data from the SiC layer of the same TRISO-coated particle as well as a SiC layer deposited at a slightly lower temperature. The fractions of high angle and CSL-related grain boundaries determined by PED are similar to those found using SEM-based EBSD. Since the grain size of the SiC layer of TRSIO fuel can be as small as 250 nm [12], depending on the fabrication parameters, and grain boundary fission product precipitates can be nano-sized, the TEM-based PED orientation data collection method is preferred to determine an accurate representation of the relative fractions of low angle, high angle and CSL-related grain boundaries. It was concluded that although the resolution of the PED data is better by more than an order of magnitude, data acquisition times may be significantly longer or the number of areas analyzed significantly larger than the SEM-based method to obtain a statistically relevant distribution. Also, grain size could be accurately determined but significantly larger analysis areas than those used in this study would be required.« less

Precession electron diffraction for SiC grain boundary characterization in unirradiated TRISO fuel

DOE PAGES

Lillo, T. M.; van Rooyen, I. J.; Wu, Y. Q.

2016-06-16

Precession electron diffraction (PED), a transmission electron microscopy-based technique, has been evaluated for the suitability for evaluating grain boundary character in the SiC layer of tristructural isotropic (TRISO) fuel. Although the ultimate goal is to determine the grain boundary characteristics of fission product containing grain boundaries of neutron irradiated SiC, our work reports the effect of transmission electron microscope (TEM) lamella thickness on quality of data and establishes a baseline comparison on grain boundary characteristics determined previously using a conventional EBSD scanning electron microscope (SEM) based technique. In general, it was determined that the lamella thickness produced using the standardmore » FIB fabrication process, is sufficient to provide reliable PED measurements with thicker lamellae (~120 nm) produce higher quality orientation data. Analysis of grain boundary character from the TEM-based PED data showed a much lower fraction of low angle grain boundaries compared to SEM-based EBSD data from the SiC layer of the same TRISO-coated particle as well as a SiC layer deposited at a slightly lower temperature. The fractions of high angle and CSL-related grain boundaries determined by PED are similar to those found using SEM-based EBSD. Since the grain size of the SiC layer of TRSIO fuel can be as small as 250 nm [12], depending on the fabrication parameters, and grain boundary fission product precipitates can be nano-sized, the TEM-based PED orientation data collection method is preferred to determine an accurate representation of the relative fractions of low angle, high angle and CSL-related grain boundaries. It was concluded that although the resolution of the PED data is better by more than an order of magnitude, data acquisition times may be significantly longer or the number of areas analyzed significantly larger than the SEM-based method to obtain a statistically relevant distribution. Also, grain size could be accurately determined but significantly larger analysis areas than those used in this study would be required.« less

Sintering behavior of U 80 at.%Zr powder compacts in a vacuum environment

NASA Astrophysics Data System (ADS)

Kim, Tae-Kyu; Lee, Chong-Tak; Sohn, Dong-Seong

2008-01-01

Sintering behavior of U-80 at.%Zr powder compacts in a temperature range from 1100 to 1500 °C in a vacuum of 1 × 10 -4 Pa was evaluated. The sintered density depended more on the sintering temperature than on the sintering time. The sintered specimens consisted of the δ-UZr 2 matrix with acicular α-Zr precipitates, but it still had un-reacted zirconium when the sintering temperature was 1100 °C. The uranium depletion near the surface of the specimens sintered at temperatures above 1300 °C was detected. Massive Zr(O) grains in the sintered specimen were found, and their formation was restrained when the cooling rate from the sintering temperature was increased.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ahmed, K.; Tonks, M.; Zhang, Y.

A detailed phase field model for the effect of pore drag on grain growth kinetics was implemented in MARMOT. The model takes into consideration both the curvature-driven grain boundary motion and pore migration by surface diffusion. As such, the model accounts for the interaction between pore and grain boundary kinetics, which tends to retard the grain growth process. Our 2D and 3D simulations demonstrate that the model capture all possible pore-grain boundary interactions proposed in theoretical models. For high enough surface mobility, the pores move along with the migrating boundary as a quasi-rigid-body, albeit hindering its migration rate compared tomore » the pore-free case. For less mobile pores, the migrating boundary can separate from the pores. For the pore-controlled grain growth kinetics, the model predicts a strong dependence of the growth rate on the number of pores, pore size, and surface diffusivity in agreement with theroretical models. An evolution equation for the grain size that includes these parameters was derived and showed to agree well with numerical solution. It shows a smooth transition from boundary-controlled kinetics to pore-controlled kinetics as the surface diffusivity decreases or the number of pores or their size increases. This equation can be utilized in BISON to give accurate estimate for the grain size evolution. This will be accomplished in the near future. The effect of solute drag and anisotropy of grain boundary on grain growth will be investigated in future studies.« less

Method of making quasi-grain boundary-free polycrystalline solar cell structure and solar cell structure obtained thereby

DOEpatents

Gonzalez, Franklin N.; Neugroschel, Arnost

1984-02-14

A new solar cell structure is provided which will increase the efficiency of polycrystalline solar cells by suppressing or completely eliminating the recombination losses due to the presence of grain boundaries. This is achieved by avoiding the formation of the p-n junction (or other types of junctions) in the grain boundaries and by eliminating the grain boundaries from the active area of the cell. This basic concept can be applied to any polycrystalline material; however, it will be most beneficial for cost-effective materials having small grains, including thin film materials.

Effect of Aluminum on the Microstructure and Properties of Two Refractory High-Entropy Alloys (Postprint)

DTIC Science & Technology

2014-04-01

The chemical compositions of the recrystallized ic release; distribution unlimited. Fig. 5. (a) Equiaxed grain structure of the annealed...deformation bands crossing a grain boundary; (c) fine recrystallized grains formed at grain boundaries; (d) a higher magnification image shows the...presence of nano-precipitates at the boundaries of the recrystallized grains. 220 O.N. Senkov et al. / Acta Materialia 68 (2014) 214–228and non

Magnetization due to localized states on graphene grain boundary

PubMed Central

Dutta, Sudipta; Wakabayashi, Katsunori

2015-01-01

Magnetism in graphene has been found to originate from various defects, e.g., vacancy, edge formation, add-atoms etc. Here, we discuss about an alternate route of achieving magnetism in graphene via grain boundary. During chemical vapor deposition of graphene, several graphene nucleation centers grow independently and face themselves with unusual bonding environment, giving rise to the formation of grain boundaries. We investigate the origin of magnetism in such grain boundaries within first-principles calculations, by letting two nucleation centers interact with each other at their interface. We observe formation of unprecedented point defect, consisting of fused three-membered and larger carbon rings, which induces net magnetization to graphene quantum dots. In case of periodic lattices, the appearance of array of point defects leads to the formation of magnetic grain boundaries. The net magnetization on these defects arises due to the deviation from bipartite characteristics of pristine graphene. We observe magnetic grain boundary induced dispersion less flat bands near Fermi energy, showing higher localization of electrons. These flat bands can be accessed via small doping, leading to enhanced magnetism. Moreover, the grain boundaries can induce asymmetric spin conduction behavior along the cross boundary direction. These properties can be exploited for sensor and spin-filtering applications. PMID:26145161

Observation of thermally etched grain boundaries with the FIB/TEM technique

DOE Office of Scientific and Technical Information (OSTI.GOV)

Palizdar, Y., E-mail: y.palizdar@merc.ac.ir; San Martin, D.; Ward, M.

2013-10-15

Thermal etching is a method which is able to reveal and characterize grain boundaries, twins or dislocation structures and determine parameters such as grain boundary energies, surface diffusivities or study phase transformations in steels, intermetallics or ceramic materials. This method relies on the preferential transfer of matter away from grain boundaries on a polished sample during heating at high temperatures in an inert/vacuum atmosphere. The evaporation/diffusion of atoms at high temperatures results in the formation of grooves at the intersections of the planes of grain/twin boundaries with the polished surface. This work describes how the combined use of Focussed Ionmore » Beam and Transmission Electron Microscopy can be used to characterize not only the grooves and their profile with the surface, but also the grain boundary line below the groove, this method being complementary to the commonly used scanning probe techniques. - Highlights: • Thermally etched low-carbon steel samples have been characterized by FIB/TEM • Grain boundary (GB) lines below the groove have been characterized in this way • Absence of ghost traces and large θ angle suggests that GB are not stationary but mobile • Observations correlate well with previous works and Mullins' investigations [22].« less

Dislocation creep accommodated Grain Boundary Sliding: A high strain rate/low temperature deformation mechanism in calcite ultramylonites

NASA Astrophysics Data System (ADS)

Rogowitz, Anna; Grasemann, Bernhard

2014-05-01

Grain boundary sliding (GBS) is an important grain size sensitive deformation mechanism that is often associated with extreme strain localization and superplasticity. Another mechanism has to operate simultaneously to GBS in order to prevent overlaps and voids between sliding grains. One of the most common accommodating mechanisms is diffusional creep but, recently, dislocation creep has been reported to operate simultaneous to GBS. Due to the formation of a flanking structure in nearly pure calcite marble on Syros (Cyclades, Greece) at lower greenschist facies conditions, an extremely fine grained ultramylonite developed. The microstructure of the layer is characterized by (1) calcite grains with an average grain size of 3.6 µm (developed by low temperature/high strain rate grain boundary migration recrystallization, BLG), (2) grain boundary triple junctions with nearly 120° angles and (3) small cavities preferentially located at triple junctions and at grain boundaries in extension. These features suggest that the dominant deformation mechanism was GBS. In order to get more information on the accommodation mechanism detailed microstructural and textural analyses have been performed on a FEI Quanta 3D FEG instrument equipped with an EDAX Digiview IV EBSD camera. The misorientation distribution curves for correlated and uncorrelated grains follow almost perfect the calculated theoretical curve for a random distribution, which is typical for polycrystalline material deformed by GBS. However, the crystallographic preferred orientation indicates that dislocation creep might have operated simultaneously. We also report Zener-Stroh cracks resulting from dislocation pile up, indicating that dislocation movement was active. We, therefore, conclude that the dominant deformation mechanism was dislocation creep accommodated grain boundary sliding. This is consistent with the observed grain size range that plots at the field boundary between grain size insensitive and grain size sensitive creep, in a deformation mechanism map for calcite.

The effect of grain boundary misorientation on the intergranular M 23C 6 carbide precipitation in thermally treated Alloy 690

NASA Astrophysics Data System (ADS)

Lim, Yun Soo; Kim, Joung Soo; Kim, Hong Pyo; Cho, Hai Dong

2004-10-01

The precipitation characteristics of chromium carbides on various types of grain boundaries in Alloy 690 thermally treated at 720 °C for 10 h were studied through transmission electron microscopy. Precipitation of the intergranular chromium carbides, identified as Cr-rich M 23C 6, was retarded on the low angle grain boundaries, compared to that on the random high angle grain boundaries on which coarse and discrete ones were found. They were rarely found on the coherent twin boundaries, however, needle-like ones were evolved on the incoherent twin and twin related Σ9 boundaries. Precipitation of the chromium carbides was also suppressed on the nearly exact coincidence site lattice boundaries such as Σ11 and Σ15, for which the Brandon criterion was fulfilled. The results of the intergranular M 23C 6 carbide precipitation were explained in terms of the influence of the grain boundary energy.

Ferromagnetic behaviour of ZnO: the role of grain boundaries

PubMed Central

Protasova, Svetlana G; Mazilkin, Andrei A; Goering, Eberhard; Schütz, Gisela; Straumal, Petr B; Baretzky, Brigitte

2016-01-01

The possibility to attain ferromagnetic properties in transparent semiconductor oxides such as ZnO is very promising for future spintronic applications. We demonstrate in this review that ferromagnetism is not an intrinsic property of the ZnO crystalline lattice but is that of ZnO/ZnO grain boundaries. If a ZnO polycrystal contains enough grain boundaries, it can transform into the ferromagnetic state even without doping with “magnetic atoms” such as Mn, Co, Fe or Ni. However, such doping facilitates the appearance of ferromagnetism in ZnO. It increases the saturation magnetisation and decreases the critical amount of grain boundaries needed for FM. A drastic increase of the total solubility of dopants in ZnO with decreasing grain size has been also observed. It is explained by the multilayer grain boundary segregation. PMID:28144542

Temperature effects in accumulation of deuterium and helium at the grain boundaries of a nano-grained tungsten

NASA Astrophysics Data System (ADS)

Kaganovich, Igor; Krstic, Predrag; Startsev, Edward

2014-10-01

It has been known that defects in tungsten, in particular at the grain boundaries, are preferable sites for deuterium and helium retention. For the case of the nano-grained boundaries, we study by classical molecular dynamics the cumulative retention of deuterium and helium at impact energies below 100 eV as functions of tungsten temperature at models of the dislocation boundaries. We obtain a strong preference of the retention of the impact particles at the boundaries at high temperature of 1000 K. Support of PPPL LDRD grant acknowledged.

Heavy mineral sorting and distributions within massive sandstone divisions (Bouma A divisions) of Brushy Canyon Formation turbidites

NASA Astrophysics Data System (ADS)

Motanated, K.; Tice, M. M.

2009-12-01

KANNIPA MOTANATED and MICHAEL M. TICE Department of Geology and Geophysics, Texas A&M University, College Station, TX 77843-3115, USA Sediment sorting data are commonly used for interpreting depositional environments, analyzing mechanisms of deposition and transportation, and inferring relative transport distance of sediments. Typically, sorting in sandstones is estimated by point-counting thin sections which is a time consuming procedure and requires cutting sections of rock samples. We demonstrate a new technique for quantifying sediment sorting using element distribution maps obtained by x-ray fluorescence microscopy. We show that hydraulic sorting of Zr- and Ti- bearing grains (probably zircon and rutile, respectively) results in characteristic vertical profiles of Zr and Ti abundances within the Bouma A divisions of turbidites of the Brushy Canyon Formation, Delaware Basin, southern New Mexico. Zr- and Ti- bearing grains decrease in abundance and diameter from bases to tops of A divisions in every sample examined in this study. These results contrast with previous observations which suggest that grading in Brushy Canyon Formation structureless sandstones is absent or rare. The data support turbiditic interpretations of these rocks against traction current interpretations which rely on the lack of textural grading. Grading is reflected in vertical profiles of Ti/Al, Zr/Al and Zr/Ti ratios, which each decrease upward. These compositional variations could potentially be used as geochemical proxies for physical sorting, and might be useful for inferring depositional processes and relative transport distances.

Nanoscale Zirconium-(oxyhydr)oxide in Contaminated Sediments From Hanford, WA - A New Host for Uranium

NASA Astrophysics Data System (ADS)

Stubbs, J. E.; Elbert, D. C.; Veblen, L. A.; Zachara, J. M.; Davis, J. A.; Veblen, D. R.

2008-12-01

Zirconium-, uranium-, and copper-bearing wastes have leached from former disposal ponds into vadose zone sediments in the 300 Area at the Department of Energy's Hanford Site. Zirconium is enriched in the shallow portion of the vadose zone, and we have discovered an amorphous Zr-(oxyhydr)oxide that contains 16% of the total uranium budget (84.24 ppm) in one of the shallow samples. We have characterized the oxide using electron microprobe analysis (EMPA), a focused ion beam (FIB) instrument, and transmission electron microscopy (TEM). It occurs in fine-grained coatings found on lithic and mineral fragments in these sediments. The oxide is intimately intergrown with the phyllosilicates and other minerals of the coatings, and in places can be seen coating individual, nano-sized phyllosilicate mineral grains. Electron energy-loss spectroscopy (EELS) shows that the Zr-(oxyhydr)oxide has a P:Zr atomic ratio around 0.2, suggesting it is either intergrown with minor amounts of a Zr-phosphate or has adsorbed a significant amount of phosphate. This material has adsorbed or incorporated a substantial amount of uranium. Thus, understanding its nature is critical to predicting the long-term fate of U in the Hanford vadose zone. While the low-temperature uptake of U by Zr-(oxhydr)oxides and phosphates has been studied for several decades in laboratory settings, to our knowledge ours is the first report of such uptake in the field.

Study on Iron Distribution and Electrical Activities at Grain Boundaries in Polycrystalline Silicon Substrate for Solar Cells

NASA Astrophysics Data System (ADS)

Arafune, Koji; Ohishi, Eichiro; Sai, Hitoshi; Terada, Yasuko; Ohshita, Yoshio; Yamaguchi, Masafumi

2006-08-01

To clarify the role of grain boundaries in iron sinks and carrier recombination centers, iron distributions and their chemical states were studied before and after gettering. They were measured by the X-ray microprobe fluorescence and the X-ray absorption in the near-edge structure using the beamline 37XU at the SPring-8 third-generation synchrotron facility. To determine the crystallographic orientation of the grain boundaries, electron backscatter diffraction measurements were performed. The distribution of electric active defects was characterized by electron-beam-induced current measurements. Before gettering, the iron was distributed in the small grain and its chemical state was similar to that of iron oxide. After gettering, the iron was redistributed along the small angle grain boundary, and its chemical state was similar to the iron silicide complexed with the iron oxide. Regarding the electrical activity, high carrier recombination was observed along the small-angle grain boundary. On the contrary, Σ 3 grain boundaries were relatively weak impurity sinks and showed low recombination activity.

Magnetization reversal mechanism and coercivity enhancement in three-dimensional granular Nd-Fe-B magnets studied by micromagnetic simulations

NASA Astrophysics Data System (ADS)

Lee, Jae-Hyeok; Choe, Jinhyeok; Hwang, Shinwon; Kim, Sang-Koog

2017-08-01

We studied the mechanism of magnetization reversals and coercivity enhancements in three-dimensional (3D) granular Nd-Fe-B permanent magnets using finite-element micromagnetic simulations. The magnetization reversals in the hard magnets consisting of hard-phase grains separated by relatively soft-phase grain boundaries were analyzed with reference to the simulation results for the magnetic field-dependent distributions of the local magnetizations. The saturation magnetization of the grain-boundary phase plays a crucial role in the transition between nucleation- and domain-wall-propagation-controlled reversal processes. The smaller the saturation magnetization of the grain-boundary phase is, the more preferable is the nucleation-controlled process, which results in a larger coercivity. The exchange stiffness of the grain-boundary phase determines the preferred paths of domain-wall propagations, whether inward into grains or along the grain boundaries for relatively small and large exchange stiffness, respectively. However, the exchange stiffness of the grain-boundary phase alone does not significantly contribute to coercivity enhancement in cases where the size of hard-phase grains is much greater than the exchange length. This work paves the way for the design of high-performance hard magnets of large coercivity and maximum-energy-product values.

Grain Boundary Conformed Volumetric Mesh Generation from a Three-Dimensional Voxellated Polycrystalline Microstructure

NASA Astrophysics Data System (ADS)

Lee, Myeong-Jin; Jeon, Young-Ju; Son, Ga-Eun; Sung, Sihwa; Kim, Ju-Young; Han, Heung Nam; Cho, Soo Gyeong; Jung, Sang-Hyun; Lee, Sukbin

2018-07-01

We present a new comprehensive scheme for generating grain boundary conformed, volumetric mesh elements from a three-dimensional voxellated polycrystalline microstructure. From the voxellated image of a polycrystalline microstructure obtained from the Monte Carlo Potts model in the context of isotropic normal grain growth simulation, its grain boundary network is approximated as a curvature-maintained conformal triangular surface mesh using a set of in-house codes. In order to improve the surface mesh quality and to adjust mesh resolution, various re-meshing techniques in a commercial software are applied to the approximated grain boundary mesh. It is found that the aspect ratio, the minimum angle and the Jacobian value of the re-meshed surface triangular mesh are successfully improved. Using such an enhanced surface mesh, conformal volumetric tetrahedral elements of the polycrystalline microstructure are created using a commercial software, again. The resultant mesh seamlessly retains the short- and long-range curvature of grain boundaries and junctions as well as the realistic morphology of the grains inside the polycrystal. It is noted that the proposed scheme is the first to successfully generate three-dimensional mesh elements for polycrystals with high enough quality to be used for the microstructure-based finite element analysis, while the realistic characteristics of grain boundaries and grains are maintained from the corresponding voxellated microstructure image.

Grain Boundary Conformed Volumetric Mesh Generation from a Three-Dimensional Voxellated Polycrystalline Microstructure

NASA Astrophysics Data System (ADS)

Lee, Myeong-Jin; Jeon, Young-Ju; Son, Ga-Eun; Sung, Sihwa; Kim, Ju-Young; Han, Heung Nam; Cho, Soo Gyeong; Jung, Sang-Hyun; Lee, Sukbin

2018-03-01

We present a new comprehensive scheme for generating grain boundary conformed, volumetric mesh elements from a three-dimensional voxellated polycrystalline microstructure. From the voxellated image of a polycrystalline microstructure obtained from the Monte Carlo Potts model in the context of isotropic normal grain growth simulation, its grain boundary network is approximated as a curvature-maintained conformal triangular surface mesh using a set of in-house codes. In order to improve the surface mesh quality and to adjust mesh resolution, various re-meshing techniques in a commercial software are applied to the approximated grain boundary mesh. It is found that the aspect ratio, the minimum angle and the Jacobian value of the re-meshed surface triangular mesh are successfully improved. Using such an enhanced surface mesh, conformal volumetric tetrahedral elements of the polycrystalline microstructure are created using a commercial software, again. The resultant mesh seamlessly retains the short- and long-range curvature of grain boundaries and junctions as well as the realistic morphology of the grains inside the polycrystal. It is noted that the proposed scheme is the first to successfully generate three-dimensional mesh elements for polycrystals with high enough quality to be used for the microstructure-based finite element analysis, while the realistic characteristics of grain boundaries and grains are maintained from the corresponding voxellated microstructure image.

Thermodynamics, Diffusion, and Structure of Mg2SiO4 forsterite grain boundaries from atomistic modeling

NASA Astrophysics Data System (ADS)

Adjaoud, O.; Marquardt, K.; Jahn, S.

2011-12-01

Most materials are not single crystals but consist of crystalline grains of various sizes, misorientated with respect to each other and joint by grain boundaries. The latter influence many of the material properties. For instance, grain boundaries are short circuits for diffusion and thus they strongly influence transport properties of materials such as electrical conductivity, or mineral growth rates, creep, or phase transform. Olivine is a major component of the Earth's upper mantle and therefore it is of considerable importance to study its physical and thermodynamic polycrystalline properties. In the present study, we have used molecular dynamics simulations to model thermodynamics, self-diffusion and structure of a series of [100] symmetric tilt grain boundaries in forsterite. The interactions between the atoms are modeled by an advanced ionic interaction potential (Jahn and Madden, 2007). The parameters of the potential are fitted to ab initio results. The model was optimized for the Ca-Mg-Al-Si-O system and shows good transferability in a wide range of pressures, temperatures, and compositions. Thermodynamics and structure were simulated at ambient conditions, and self-diffusion coefficients were determined at ambient pressure and temperatures of 1250, 1500, 1750, and 2000 K. We find that the energy and excess free volume of the grain boundaries in forsterite depend significantly on the misorientation angle of the grain boundary. One of our modeled structures is compared with an high-resolution transmission electron micrograph (HRTEM) (Heinemann et al., 2005). We relate our findings to previous studies of grain boundaries in ionic materials and in metals. For small misorientation angles (up to 22.1°), grain boundary structures consist of an array of c-edge dislocations as suggested by Heinemann et al. (2005) and their energies can be readily fit with the Read-Shockley dislocation model for grain boundaries. For high misorientation angles (32.1° and 60.8°), the cores of dislocations overlap and form repeated structural units. Similar to energies and excess free volumes, the self-diffusion coefficients of Mg and O depend significantly on the misorientation angle of the grain boundaries and they are well fitted with Arrhenius law. We compare our results to MgO grain boundary diffusion in forsterite derived from reaction rim growth experiments (Gardés and Heinrich, 2010).

The habit of crystals in aggregates: five parameter grain boundary characterization of olivine

NASA Astrophysics Data System (ADS)

Marquardt, K.; Rohrer, G. S.; Morales, L. F. G.; De Graef, M.; Farla, R. J.

2016-12-01

There is growing evidence that the presence of interfaces in rocks, including phase and grain boundaries influence macroscopic properties. To model resulting bulk rock properties and ultimately interpret geophysical signals, such as electrical conductivity, knowledge about the relative abundance of specific grain boundaries is needed. To date, neither the anisotropic frequency of appearance of specific grain boundaries nor its dependence on chemical composition is known for rock forming minerals. Here, we report detailed interface characterizations in olivine, the most abundant phase in the upper mantle. To obtain the area distribution of the geometrically varying interfaces, which is among the most fundamental information, we used electron backscatter diffraction (EBSD) to detect the orientations of over 3x104grains corresponding to more than 6000 mm length of grain boundary separating them. Subsequently we used a stereological approach to determine the grain boundary character distribution (GBCD), defined as the relative areas of grain boundaries of different types, distinguished by their five degrees of freedom (Rohrer et al. 2004). We discuss data collected from different olivine aggregates with chemical compositions ranging from Mg2SiO4 forsterite to Mg1.8Fe0.2SiO4 derived from different synthesis methods. We show that standard EBSD indexing as commonly used is sufficient for many applications, but when characterizing grain boundaries higher accuracy and precision is fundamental and provided by the new dictionary indexing approach, where clean up procedures, that can cause artifacts, are superfluous. The grain boundary planes show a preference for low index planes, which is in agreement with observations on other materials (e.g. MgO, TiO2, SrTiO3, MgAl2O4). We find that the principal crystallographic planes have the lowest energies resulting in crystal habits dominated by (001) planes, followed by (010) and (001) planes and that 90°/[001] (100)(010) are the most frequent grain boundaries, for pure forsterite aggregates. However in the absence of any impurities such as Al or Ca on the grain boundaries the (001) planes dominate the crystal habits. Rohrer G. S. et al. (2004) The distribution of internal interfaces in polycrystals. Zeitschrift für Met. 95, 197-214.

Sintering, thermal stability and mechanical properties of ZrO2-WC composites obtained by pulsed electric current sintering

NASA Astrophysics Data System (ADS)

Huang, Shuigen; Vanmeensel, Kim; van der Biest, Omer; Vleugels, Jozef

2011-03-01

ZrO2-WC composites exhibit comparable mechanical properties as traditional WC-Co materials, which provides an opportunity to partially replace WC-Co for some applications. In this study, 2 mol.% Y2O3 stabilized ZrO2 composites with 40 vol.% WC were consolidated in the 1150°C-1850°C range under a pressure of 60 MPa by pulsed electric current sintering (PECS). The densification behavior, microstructure and phase constitution of the composites were investigated to clarify the role of the sintering temperature on the grain growth, mechanical properties and thermal stability of ZrO2 and WC components. Analysis results indicated that the composites sintered at 1350°C and 1450°C exhibited the highest tetragonal ZrO2 phase transformability, maximum toughness, and hardness and an optimal flexural strength. Chemical reaction of ZrO2 and C, originating from the graphite die, was detected in the composite PECS for 20 min at 1850°C in vacuum.

New ZrO2/Al2O3 Nanocomposite Fabricated from Hybrid Nanoparticles Prepared by CO2 Laser Co-Vaporization

PubMed Central

Bartolomé, José F.; Smirnov, Anton; Kurland, Heinz-Dieter; Grabow, Janet; Müller, Frank A.

2016-01-01

Alumina toughened zirconia (ATZ) and zirconia toughened alumina (ZTA) are currently the materials of choice to meet the need for tough, strong, and bioinert ceramics for medical devices. However, the mechanical properties of ZrO2/Al2O3 dispersion ceramics could be considerably increased by reducing the corresponding grain sizes and by improving the homogeneity of the phase dispersion. Here, we prepare nanoparticles with an intraparticular phase distribution of Zr(1−x)AlxO(2−x/2) and (γ-, δ-)Al2O3 by the simultaneous gas phase condensation of laser co-vaporized zirconia and alumina raw powders. During subsequent spark plasma sintering the zirconia defect structures and transition alumina phases transform to a homogeneously distributed dispersion of tetragonal ZrO2 (52.4 vol%) and α-Al2O3 (47.6 vol%). Ceramics sintered by spark plasma sintering are completely dense with average grain sizes in the range around 250 nm. Outstanding mechanical properties (flexural strength σf = 1500 MPa, fracture toughness KIc = 6.8 MPa m1/2) together with a high resistance against low temperature degradation make these materials promising candidates for next generation bioceramics in total hip replacements and for dental implants. PMID:26846310

New ZrO2/Al2O3 Nanocomposite Fabricated from Hybrid Nanoparticles Prepared by CO2 Laser Co-Vaporization

NASA Astrophysics Data System (ADS)

Bartolomé, José F.; Smirnov, Anton; Kurland, Heinz-Dieter; Grabow, Janet; Müller, Frank A.

2016-02-01

Alumina toughened zirconia (ATZ) and zirconia toughened alumina (ZTA) are currently the materials of choice to meet the need for tough, strong, and bioinert ceramics for medical devices. However, the mechanical properties of ZrO2/Al2O3 dispersion ceramics could be considerably increased by reducing the corresponding grain sizes and by improving the homogeneity of the phase dispersion. Here, we prepare nanoparticles with an intraparticular phase distribution of Zr(1-x)AlxO(2-x/2) and (γ-, δ-)Al2O3 by the simultaneous gas phase condensation of laser co-vaporized zirconia and alumina raw powders. During subsequent spark plasma sintering the zirconia defect structures and transition alumina phases transform to a homogeneously distributed dispersion of tetragonal ZrO2 (52.4 vol%) and α-Al2O3 (47.6 vol%). Ceramics sintered by spark plasma sintering are completely dense with average grain sizes in the range around 250 nm. Outstanding mechanical properties (flexural strength σf = 1500 MPa, fracture toughness KIc = 6.8 MPa m1/2) together with a high resistance against low temperature degradation make these materials promising candidates for next generation bioceramics in total hip replacements and for dental implants.

Improved toughness of refractory compounds. [with elimination of the grain boundary phase

NASA Technical Reports Server (NTRS)

Wright, T. R.; Niesz, D. E.

1974-01-01

The concept of grain-boundary-engineering through elimination of the grain-boundary silicate phase in silicon nitride was developed. The process involved removal of the silica from the nitride powder via a thermal treatment coupled with the use of nitride additives to compensate the remaining oxygen. Magnesium and aluminum nitrides are found to be the most effective additive for use as oxygen compensators. Strength decreases at elevated temperatures are not observed in the alumina containing material. The creep rate of a dual additive sialon composition was two orders of magnitude lower at 1400 C than commercial silicon nitride. A cursory analysis of the creep mechanism indicate that grain-boundary sliding is avoided through elimination of the grain-boundary silicate phase.

Uranium vacancy mobility at the Σ5 symmetric tilt and Σ5 twist grain boundaries in UO₂

DOE PAGES

Uberuaga, Blas Pedro; Andersson, David A.

2015-10-01

Ionic transport at grain boundaries in oxides dictates a number of important phenomena, from ionic conductivity to sintering to creep. For nuclear fuels, it also influences fission gas bubble nucleation and growth. Here, using a combination of atomistic calculations and object kinetic Monte Carlo (okMC) simulations, we examine the kinetic pathways associated with uranium vacancies at two model grain boundaries in UO 2. The barriers for vacancy motion were calculated using the nudged elastic band method at all uranium sites at each grain boundary and were used as the basis of the okMC simulations. For both boundaries considered – amore » simple tilt and a simple twist boundary – the mobility of uranium vacancies is significantly higher than in the bulk. For the tilt boundary, there is clearly preferred migration along the tilt axis as opposed to in the perpendicular direction while, for the twist boundary, migration is essentially isotropic within the boundary plane. These results show that cation defect mobility in fluorite-structured materials is enhanced at certain types of grain boundaries and is dependent on the boundary structure with the tilt boundary exhibiting higher rates of migration than the twist boundary.« less

Effect of annealing temperature on optical and electrical properties of ZrO2-SnO2 based nanocomposite thin films

NASA Astrophysics Data System (ADS)

Anitha, V. S.; Lekshmy, S. Sujatha; Berlin, I. John; Joy, K.

2014-01-01

Transparent nanocomposite ZrO2-SnO2 thin films were prepared by sol-gel dip-coating technique. Films were annealed at 500°C, 800°C and 1200°C respectively. X-ray diffraction(XRD) spectra showed a mixture of three phases: tetragonal ZrO2 and SnO2 and orthorhombic ZrSnO4. The grain size of all the three phases' increased with annealing temperature. An average transmittance greater than 85%(in UV-Visible region) is observed for all the films. The band gap for the films decreased from 4.79 eV to 4.62 eV with increase in annealing temperature from 500 to 1200 °C. The electrical resistivity increased with increase in annealing temperature. Such composite ZrO2-SnO2 films can be used in many applications and in optoelectronic devices.

Synthesis, microstructure and dielectric properties of zirconium doped barium titanate

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kumar, Rohtash; School of Physical Sciences, Jawaharlal Nehru University, New Delhi; Asokan, K.

2016-05-23

We report on synthesis, microstructural and relaxor ferroelectric properties of Zirconium(Zr) doped Barium Titanate (BT) samples with general formula Ba(Ti{sub 1-x}Zr{sub x})O{sub 3} (x=0.20, 0.35). These lead-free ceramics were prepared by solid state reaction route. The phase transition behavior and temperature dependent dielectric properties and composition dependent ferroelectric properties were investigated. XRD analysis at room temperature confirms phase purity of the samples. SEM observations revealed retarded grain growth with increasing Zr mole fraction. Dielectric properties of BZT ceramics is influenced significantly by small addition of Zr mole fraction. With increasing Zr mole fraction, dielectric constant decreases while FWHM and frequencymore » dispersion increases. Polarization vs electric field hysteresis measurements reveal ferroelectric relaxor phase at room temperature. The advantages of such substitution maneuvering towards optimizing ferroelectric properties of BaTiO{sub 3} are discussed.« less

Synthesis and Tribological Performance of Different Particle-Sized Nickel-Ion-Exchanged α-Zirconium Phosphates

NASA Astrophysics Data System (ADS)

Zhang, Xiaosheng; Xu, Hong; Dong, Jinxiang

2018-03-01

Nickel-ion-exchanged α-zirconium phosphate (Ni-α-ZrP) was synthesized by a mild hydrothermal synthesis method. Different raw material ratios (NaF/H3PO4/Ni(CH3COO)2·4H2O) influence the particle size of the Ni-α-ZrP samples. The grain size could be controlled and distributed from 20 to 600 nm. Ni-α-ZrP was evaluated as an additive in lithium grease in a four-ball test. A 3.0 wt.% addition of Ni-α-ZrP to lithium grease yielded maximum non-seizure load values of 1235 N, and the wear scar diameter on the lower balls is 0.42 mm at 294 N. Compared with smaller particles, the addition of Ni-α-ZrP with a larger particle size to grease yields a better load-carrying capacity.

Recombination activity of grain boundaries in high-performance multicrystalline Si during solar cell processing

NASA Astrophysics Data System (ADS)

Adamczyk, Krzysztof; Søndenâ, Rune; Stokkan, Gaute; Looney, Erin; Jensen, Mallory; Lai, Barry; Rinio, Markus; Di Sabatino, Marisa

2018-02-01

In this work, we applied internal quantum efficiency mapping to study the recombination activity of grain boundaries in High Performance Multicrystalline Silicon under different processing conditions. Wafers were divided into groups and underwent different thermal processing, consisting of phosphorus diffusion gettering and surface passivation with hydrogen rich layers. After these thermal treatments, wafers were processed into heterojunction with intrinsic thin layer solar cells. Light Beam Induced Current and Electron Backscatter Diffraction were applied to analyse the influence of thermal treatment during standard solar cell processing on different types of grain boundaries. The results show that after cell processing, most random-angle grain boundaries in the material are well passivated, but small-angle grain boundaries are not well passivated. Special cases of coincidence site lattice grain boundaries with high recombination activity are also found. Based on micro-X-ray fluorescence measurements, a change in the contamination level is suggested as the reason behind their increased activity.

Pipe and grain boundary diffusion of He in UO 2

DOE Office of Scientific and Technical Information (OSTI.GOV)

Galvin, C. O.T.; Cooper, M. W. D.; Fossati, P. C. M.

Molecular dynamics simulations have been conducted to study the effects of dislocations and grain boundaries on He diffusion inmore » $$\\text{U}{{\\text{O}}_{2}}$$ . Calculations were carried out for the {100}, {110} and {111} $$\\langle 1\\,1\\,0\\rangle $$ edge dislocations, the screw $$\\langle 1\\,1\\,0\\rangle $$ dislocation and Σ5, Σ13, Σ19 and Σ25 tilt grain boundaries. He diffusivity as a function of distance from the dislocation core and grain boundaries was investigated for the temperature range 2300–3000 K. An enhancement in diffusivity was predicted within 20 Å of the dislocations or grain boundaries. Further investigation showed that He diffusion in the edge dislocations follows anisotropic behaviour along the dislocation core, suggesting that pipe diffusion occurs. Here, an Arrhenius plot of He diffusivity against the inverse of temperature was also presented and the activation energy calculated for each structure, as a function of distance from the dislocation or grain boundary.« less

Pipe and grain boundary diffusion of He in UO 2

DOE PAGES

Galvin, C. O.T.; Cooper, M. W. D.; Fossati, P. C. M.; ...

2016-10-12

Molecular dynamics simulations have been conducted to study the effects of dislocations and grain boundaries on He diffusion inmore » $$\\text{U}{{\\text{O}}_{2}}$$ . Calculations were carried out for the {100}, {110} and {111} $$\\langle 1\\,1\\,0\\rangle $$ edge dislocations, the screw $$\\langle 1\\,1\\,0\\rangle $$ dislocation and Σ5, Σ13, Σ19 and Σ25 tilt grain boundaries. He diffusivity as a function of distance from the dislocation core and grain boundaries was investigated for the temperature range 2300–3000 K. An enhancement in diffusivity was predicted within 20 Å of the dislocations or grain boundaries. Further investigation showed that He diffusion in the edge dislocations follows anisotropic behaviour along the dislocation core, suggesting that pipe diffusion occurs. Here, an Arrhenius plot of He diffusivity against the inverse of temperature was also presented and the activation energy calculated for each structure, as a function of distance from the dislocation or grain boundary.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liu, Tingguang; Xia, Shuang, E-mail: xs@shu.edu.cn; Li, Hui

Grain boundary engineering was carried out on an aging-treated nickel based Alloy 690, which has precipitated carbides at grain boundaries. Electron backscatter diffraction technique was used to investigate the grain boundary networks. Results show that, compared with the solution-annealed samples, the aging-treated samples with pre-existing carbides at grain boundaries need longer duration or higher temperature during annealing after low-strain tensile deformation for forming high proportion of low-Σ coincidence site lattice grain boundaries (more than 75%). The reason is that the primary recrystallization is inhibited or retarded owing to that the pre-existing carbides are barriers to grain boundaries migration. - Highlights:more » • Study of GBE as function of pre-existing GB carbides, tensile strain and annealing • Recrystallization of GBE is inhibited or retarded by the pre-existing carbides. • Retained carbides after annealing show the original GB positions. • More than 80% of special GBs were formed after the modification of GBE processing. • Multiple twinning during recrystallization is the key process of GBE.« less

Reduced yield stress for zirconium exposed to iodine: Reactive force field simulation

DOE PAGES

Rossi, Matthew L.; Taylor, Christopher D.; van Duin, Adri C. T.

2014-11-04

Iodine-induced stress-corrosion cracking (ISCC), a known failure mode for nuclear fuel cladding, occurs when iodine generated during the irradiation of a nuclear fuel pellet escapes the pellet through diffusion or thermal cracking and chemically interacts with the inner surface of the clad material, inducing a subsequent effect on the cladding’s resistance to mechanical stress. To complement experimental investigations of ISCC, a reactive force field (ReaxFF) compatible with the Zr-I chemical and materials systems has been developed and applied to simulate the impact of iodine exposure on the mechanical strength of the material. The study shows that the material’s resistance tomore » stress (as captured by the yield stress of a high-energy grain boundary) is related to the surface coverage of iodine, with the implication that ISCC is the result of adsorption-enhanced decohesion.« less

Reconstruction of 3d grain boundaries from rock thin sections, using polarised light

NASA Astrophysics Data System (ADS)

Markus Hammes, Daniel; Peternell, Mark

2016-04-01

Grain boundaries affect the physical and chemical properties of polycrystalline materials significantly by initiating reactions and collecting impurities (Birchenall, 1959), and play an essential role in recrystallization (Doherty et al. 1997). In particular, the shape and crystallographic orientation of grain boundaries reveal the deformation and annealing history of rocks (Kruhl and Peternell 2002, Kuntcheva et al. 2006). However, there is a lack of non-destructive and easy-to-use computer supported methods to determine grain boundary geometries in 3D. The only available instrument using optical light to measure grain boundary angles is still the polarising microscope with attached universal stage; operated manually and time-consuming in use. Here we present a new approach to determine 3d grain boundary orientations from 2D rock thin sections. The data is recorded by using an automatic fabric analyser microscope (Peternell et al., 2010). Due to its unique arrangement of 9 light directions the highest birefringence colour due to each light direction and crystal orientation (retardation) can be determined at each pixel in the field of view. Retardation profiles across grain boundaries enable the calculation of grain boundary angle and direction. The data for all positions separating the grains are combined and further processed. In combination with the lateral position of the grain boundary, acquired using the FAME software (Hammes and Peternell, in review), the data is used to reconstruct a 3d grain boundary model. The processing of data is almost fully automatic by using MATLAB®. Only minor manual input is required. The applicability was demonstrated on quartzite samples, but the method is not solely restricted on quartz grains and other birefringent polycrystalline materials could be used instead. References: Birchenall, C.E., 1959: Physical Metallurgy. McGraw-Hill, New York. Doherty, R.D., Hughes, D.A., Humphreys, F.J., Jonas, J.J., Juul Jensen, D., Kassner, M.E., King, W.E., McNelley, T.R., McQueen, H.J., Rollett, A.D., 1997: Current issues in recrystallization: a review. Materials Science and Engineering A 238, 219-274. Hammes, D.M., Peternell, M., in review. FAME: Software for analysing rock microstructures. Computers & Geoscience. Kruhl, J.H., Peternell, M., 2002. The equilibration of high-angle grain boundaries in dynamically recrystallized quartz: the effect of crystallography and temperature. Journal of Structural Geology 24, 1125-1137. Kuntcheva, B., Kruhl, J.H. & Kunze, K., 2006. Crystallographic orientation of high-angle grain boundaries in dynamically recrystallized quartz: First results. Tectonophysics 421, 331-346. Peternell, M., Hasalová, P., Wilson, J.L., Piaziolo, S., Schulmann, K., 2010. Evaluating quartz crystallographic preferred orientations and the role of deformation partitioning using EBSD and fabric analyser techniques. Journal of Structural Geology 32, 803-817.

YSZ thin films with minimized grain boundary resistivity

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mills, Edmund M.; Kleine-Boymann, Matthias; Janek, Juergen

2016-03-31

In recent years, interface engineering of solid electrolytes has been explored to increase their ionic conductivity and improve the performance of solid oxide fuel cells and other electrochemical power sources. It has been observed that the ionic conductivity of epitaxially grown thin films of some electrolytes is dramatically enhanced, which is often attributed to effects (e. g. strain-induced mobility changes) at the heterophase boundary with the substrate. Still largely unexplored is the possibility of manipulation of grain boundary resistivity in polycrystalline solid electrolyte films, clearly a limiting factor in their ionic conductivity. Here we report that the ionic conductivity ofmore » yttria stabilized zirconia thin films with nano-­ columnar grains grown on a MgO substrate nearly reaches that of the corresponding single crystal when the thickness of the films becomes less than roughly 8 nm (smaller by a factor of three at 500°C). Using impedance spectroscopy, the grain boundary resistivity was probed as a function of film thickness. The resistivity of the grain boundaries near the film- substrate interface and film surface (within 4 nm of each) was almost entirely eliminated. This minimization of grain boundary resistivity is attributed to Mg2+ diffusion from the MgO substrate into the YSZ grain boundaries, which is supported by time of flight secondary ion mass spectroscopy measurements. We suggest grain boundary “design” as an attractive method to obtain highly conductive solid electrolyte thin films.« less

Density functional calculation of activation energies for lattice and grain boundary diffusion in alumina

NASA Astrophysics Data System (ADS)

Lei, Yinkai; Gong, Yu; Duan, Zhiyao; Wang, Guofeng

2013-06-01

To acquire knowledge on the lattice and grain boundary diffusion processes in alumina, we have determined the activation energies of elementary O and Al diffusive jumps in the bulk crystal, Σ3(0001) grain boundaries, and Σ3(101¯0) grain boundaries of α-Al2O3 using the first-principles density functional theory method. Specifically, we calculated the activation energies for four elementary jumps of both O and Al lattice diffusion in alumina. It was predicted that the activation energy of O lattice diffusion varied from 3.58 to 5.03 eV, while the activation energy of Al lattice diffusion ranged from 1.80 to 3.17 eV. As compared with experimental measurements, the theoretical predictions of the activation energy for lattice diffusion were lower and thus implied that there might be other high-energy diffusive jumps in the experimental alumina samples. Moreover, our results suggested that the Al lattice diffusion was faster than the O lattice diffusion in alumina, in agreement with experiment observations. Furthermore, it was found from our calculations for α-Al2O3 that the activation energies of O and Al grain boundary diffusion in the high-energy Σ3(0001) grain boundaries were significantly lower than those of the lattice diffusion. In contrast, the activation energies of O and Al grain boundary diffusion in the low-energy Σ3(101¯0) grain boundaries could be even higher than those of the lattice diffusion.

YSZ thin films with minimized grain boundary resistivity

DOE PAGES

Mills, Edmund M.; Kleine-Boymann, Matthias; Janek, Juergen; ...

2016-03-31

In recent years, interface engineering of solid electrolytes has been explored to increase their ionic conductivity and improve the performance of solid oxide fuel cells and other electrochemical power sources. It has been observed that the ionic conductivity of epitaxially grown thin films of some electrolytes is dramatically enhanced, which is often attributed to effects (e.g. strain-induced mobility changes) at the heterophase boundary with the substrate. Still largely unexplored is the possibility of manipulation of grain boundary resistivity in polycrystalline solid electrolyte films, clearly a limiting factor in their ionic conductivity. Here in this paper, we report that the ionicmore » conductivity of yttria stabilized zirconia thin films with nano-columnar grains grown on a MgO substrate nearly reaches that of the corresponding single crystal when the thickness of the films becomes less than roughly 8 nm (smaller by a factor of three at 500 °C). Using impedance spectroscopy, the grain boundary resistivity was probed as a function of film thickness. The resistivity of the grain boundaries near the film–substrate interface and film surface (within 4 nm of each) was almost entirely eliminated. This minimization of grain boundary resistivity is attributed to Mg 2+ diffusion from the MgO substrate into the YSZ grain boundaries, which is supported by time of flight secondary ion mass spectroscopy measurements. We suggest grain boundary “design” as an attractive method to obtain highly conductive solid electrolyte thin films.« less

TEM Study of Intergranular Fluid Distributions in Rocks at a Nanometer Scale

NASA Astrophysics Data System (ADS)

Hiraga, T.; Anderson, I. M.; Kohlstedt, D. L.

2002-12-01

The distribution of intergranular fluids in rocks plays an essential role in fluid migration and rock rheology. Structural and chemical analyses with sub-nanometer resolution is possible with transmission and scanning-transmission electron microscopy; therefore, it is possible to perform the fine-scale structural analyses required to determine the presence or absence of very thin fluid films along grain boundaries. For aqueous fluids in crustal rocks, Hiraga et al. (2001) observed a fluid morphology controlled by the relative values of the solid-solid and solid-fluid interfacial energies, which resulted in well-defined dihedral angles. Their high-resolution transmission electron microscopy (TEM) observations demonstrate that grain boundaries are tight even at a nanometer scale, consistent with the absence of aqueous fluid films. For partially molten ultra-mafic rocks, two conflicting conclusions have been reached: nanometer-thick melt films wet grain boundaries (Drury and Fitz Gerald 1996; De Kloe et al. 2000) versus essentially all grain boundaries are melt-free (Vaughan et al. 1982; Kohlstedt 1990). To resolve this conflict, Hiraga et al. (2002) examined grain boundaries in quenched partially molten peridotites. Their observations demonstrate the following: (i) Although a small fraction of the grains are separated by relatively thick (~1 μm) layers of melt, lattice fringe images obtained with a high-resolution TEM reveal that most of the remaining boundaries do not contain a thin amorphous phase. (ii) In addition, the composition of olivine-olivine grain boundaries was analyzed with a nano-beam analytical scanning TEM with a probe size of <2 nm. Although the grain boundaries contained no melt film, the concentration of Ca, Al and Ti were enhanced near the boundaries. The segregation of these elements to the grain boundaries formed enriched regions <7 nm wide. A similar pattern of chemical segregation was detected in subsolidus systems. Creep experiments on the partially molten rocks that were analyzed in this study reveal little weakening even at melt contents approaching 4 vol%, consistent with our observations of melt-free grain boundaries.

Austenite grain growth simulation considering the solute-drag effect and pinning effect.

PubMed

Fujiyama, Naoto; Nishibata, Toshinobu; Seki, Akira; Hirata, Hiroyuki; Kojima, Kazuhiro; Ogawa, Kazuhiro

2017-01-01

The pinning effect is useful for restraining austenite grain growth in low alloy steel and improving heat affected zone toughness in welded joints. We propose a new calculation model for predicting austenite grain growth behavior. The model is mainly comprised of two theories: the solute-drag effect and the pinning effect of TiN precipitates. The calculation of the solute-drag effect is based on the hypothesis that the width of each austenite grain boundary is constant and that the element content maintains equilibrium segregation at the austenite grain boundaries. We used Hillert's law under the assumption that the austenite grain boundary phase is a liquid so that we could estimate the equilibrium solute concentration at the austenite grain boundaries. The equilibrium solute concentration was calculated using the Thermo-Calc software. Pinning effect was estimated by Nishizawa's equation. The calculated austenite grain growth at 1473-1673 K showed excellent correspondence with the experimental results.

Role of grain and grain boundary on the electrical and thermal conductivity of Bi0.9Y0.1Fe0.9Mn0.1O3 ceramics

NASA Astrophysics Data System (ADS)

Pandey, Rabichandra; Panda, Chandrakanta; Kumar, Pawan; Pradhan, Lagen Kumar; Kar, Manoranjan

2017-05-01

Role of grain and grain boundary on electrical and thermal conductivity of Bi0.9Y0.1Fe0.9Mn0.1O3 ceramic was investigated systematically. Tartaric acid modified sol gel method was used to synthesize the compound. X-ray diffraction technique was used to confirm the formation of single phase orthorhombic (Pbnm) structure. Electrical properties of the sample were measured with a wide frequency range from 100Hz to 10MHz at different temperature from 40°C to 250°C. AC impedance studies indicate the presence of grain and grain boundary effect. The negative temperature coefficient of resistance (NTCR) behaviour of the compound has been confirmed by the cole-cole plot. DC electrical and thermal conductivities of the compound were explained on the basis of grain and grain boundaries.

Unraveling irradiation induced grain growth with in situ transmission electron microscopy and coordinated modeling

DOE PAGES

Bufford, D. C.; Abdeljawad, F. F.; Foiles, S. M.; ...

2015-11-09

Here, nanostructuring has been proposed as a method to enhance radiation tolerance, but many metallic systems are rejected due to significant concerns regarding long term grain boundary and interface stability. This work utilized recent advancements in transmission electron microscopy (TEM) to quantitatively characterize the grain size, texture, and individual grain boundary character in a nanocrystalline gold model system before and after in situ TEM ion irradiation with 10 MeV Si. The initial experimental measurements were fed into a mesoscale phase field model, which incorporates the role of irradiation-induced thermal events on boundary properties, to directly compare the observed and simulatedmore » grain growth with varied parameters. The observed microstructure evolution deviated subtly from previously reported normal grain growth in which some boundaries remained essentially static. In broader terms, the combined experimental and modeling techniques presented herein provide future avenues to enhance quantification and prediction of the thermal, mechanical, or radiation stability of grain boundaries in nanostructured crystalline systems.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, Weiguo, E-mail: wang_weiguo@vip.163.com

High purity (99.99%) iron samples were cold rolled with a thickness reduction of 87% followed by a annealing at 620 °C for 15 and 45 min, then the grain boundary plane distributions were characterized by electron backscatter diffraction and a stereology and statistics based five parameter analysis. The results showed that the grain boundary planes were mainly distributed on (1 0 0) and such distribution was enhanced obviously when the holding time of annealing increased from 15 to 45 min during which an extensive grain growth and a dramatic texture evolution took place. Further analysis indicated such distribution was largelymore » due to the rotation of grain boundary planes of the [1 0 0] misoriented grains. Additionally, it was also observed that some random boundaries of [1 0 0] misoriented grains were changing from asymmetrical tilt into (1 0 0)/(− 1 0 0) twist when annealing proceeded from 15 to 45 min. Based on the present work and the results reported by other investigators, it was suggested that the chemistry appeared to be critical in determining the grain boundary plane distribution in iron based materials. - Highlights: •Grain boundary (GB) plane distribution (GBPD) in a high purity (99.99%) was studied. •GB planes are mainly distributed on (1 0 0) in the cold rolled and annealed samples. •Such distribution is largely due to the rotation of GB planes of [100] misoriented grains. •Some [1 0 0] asymmetrical tilt boundaries are evolving into twist ones during annealing.« less

Electromigration in Cu(Al) and Cu(Mn) damascene lines

NASA Astrophysics Data System (ADS)

Hu, C.-K.; Ohm, J.; Gignac, L. M.; Breslin, C. M.; Mittal, S.; Bonilla, G.; Edelstein, D.; Rosenberg, R.; Choi, S.; An, J. J.; Simon, A. H.; Angyal, M. S.; Clevenger, L.; Maniscalco, J.; Nogami, T.; Penny, C.; Kim, B. Y.

2012-05-01

The effects of impurities, Mn or Al, on interface and grain boundary electromigration (EM) in Cu damascene lines were investigated. The addition of Mn or Al solute caused a reduction in diffusivity at the Cu/dielectric cap interface and the EM activation energies for both Cu-alloys were found to increase by about 0.2 eV as compared to pure Cu. Mn mitigated and Al enhanced Cu grain boundary diffusion; however, no significant mitigation in Cu grain boundary diffusion was observed in low Mn concentration samples. The activation energies for Cu grain boundary diffusion were found to be 0.74 ± 0.05 eV and 0.77 ± 0.05 eV for 1.5 μm wide polycrystalline lines with pure Cu and Cu (0.5 at. % Mn) seeds, respectively. The effective charge number in Cu grain boundaries Z*GB was estimated from drift velocity and was found to be about -0.4. A significant enhancement in EM lifetimes for Cu(Al) or low Mn concentration bamboo-polycrystalline and near-bamboo grain structures was observed but not for polycrystalline-only alloy lines. These results indicated that the existence of bamboo grains in bamboo-polycrystalline lines played a critical role in slowing down the EM-induced void growth rate. The bamboo grains act as Cu diffusion blocking boundaries for grain boundary mass flow, thus generating a mechanical stress-induced back flow counterbalancing the EM force, which is the equality known as the "Blech short length effect."

Reversal in the Size Dependence of Grain Rotation

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhou, Xiaoling; Tamura, Nobumichi; Mi, Zhongying

The conventional belief, based on the Read-Shockley model for the grain rotation mechanism, has been that smaller grains rotate more under stress due to the motion of grain boundary dislocations. However, in our high-pressure synchrotron Laue x-ray microdiffraction experiments, 70 nm nickel particles are found to rotate more than any other grain size. We infer that the reversal in the size dependence of the grain rotation arises from the crossover between the grain boundary dislocation-mediated and grain interior dislocation-mediated deformation mechanisms. The dislocation activities in the grain interiors are evidenced by the deformation texture of nickel nanocrystals. This new findingmore » reshapes our view on the mechanism of grain rotation and helps us to better understand the plastic deformation of nanomaterials, particularly of the competing effects of grain boundary and grain interior dislocations.« less

Reversal in the Size Dependence of Grain Rotation

DOE PAGES

Zhou, Xiaoling; Tamura, Nobumichi; Mi, Zhongying; ...

2017-03-01

The conventional belief, based on the Read-Shockley model for the grain rotation mechanism, has been that smaller grains rotate more under stress due to the motion of grain boundary dislocations. However, in our high-pressure synchrotron Laue x-ray microdiffraction experiments, 70 nm nickel particles are found to rotate more than any other grain size. We infer that the reversal in the size dependence of the grain rotation arises from the crossover between the grain boundary dislocation-mediated and grain interior dislocation-mediated deformation mechanisms. The dislocation activities in the grain interiors are evidenced by the deformation texture of nickel nanocrystals. This new findingmore » reshapes our view on the mechanism of grain rotation and helps us to better understand the plastic deformation of nanomaterials, particularly of the competing effects of grain boundary and grain interior dislocations.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Merkle, K. L.; Csencsits, R.; Rynes, K. L.

In the absence of high-order aberrations, the lattice fringe technique should allow measurement of grain boundary rigid-body displacements to accuracies about an order of magnitude better than the point-to-point resolution of the transmission electron microscope. The three-fold astigmatism, however, introduces shifts of the lattice fringe pattern that depend on the orientation of the lattice relative to the direction of the three-fold astigmatism and thus produces an apparent shift between the two grains bordering the grain boundary. By image simulation of grain boundary model structures, the present paper explores the effect of these extraneous shifts on grain boundary volume expansion measurements.more » It is found that the shifts depend, among others, on zone axis direction and the magnitude of the lattice parameter. For many grain boundaries of interest, three-fold astigmatism correction to better than 100 nm appears necessary to achieve the desired accuracies.« less

Measuring grain boundary character distributions in Ni-base alloy 725 using high-energy diffraction microscopy

DOE PAGES

Bagri, Akbar; Hanson, John P.; Lind, J. P.; ...

2016-10-25

We use high-energy X-ray diffraction microscopy (HEDM) to characterize the microstructure of Ni-base alloy 725. HEDM is a non-destructive technique capable of providing three-dimensional reconstructions of grain shapes and orientations in polycrystals. The present analysis yields the grain size distribution in alloy 725 as well as the grain boundary character distribution (GBCD) as a function of lattice misorientation and boundary plane normal orientation. We find that the GBCD of Ni-base alloy 725 is similar to that previously determined in pure Ni and other fcc-base metals. We find an elevated density of Σ9 and Σ3 grain boundaries. We also observe amore » preponderance of grain boundaries along low-index planes, with those along (1 1 1) planes being the most common, even after Σ3 twins have been excluded from the analysis.« less

Diffusion-coupled cohesive interface simulations of stress corrosion intergranular cracking in polycrystalline materials

DOE Office of Scientific and Technical Information (OSTI.GOV)

Pu, Chao; Gao, Yanfei; Wang, Yanli

To study the stress corrosion intergranular cracking mechanism, a diffusion-coupled cohesive zone model (CZM) is proposed for the simulation of the stress-assisted diffusional process along grain boundaries and the mechanical response of grain boundary sliding and separation. This simulation methodology considers the synergistic effects of impurity diffusion driven by pressure gradient and degradation of grain boundary strength by impurity concentration. The diffusion-coupled CZM is combined with crystal plasticity finite element model (CPFEM) to simulate intergranular fracture of polycrystalline material under corrosive environment. Significant heterogeneity of the stress field and extensive impurity accumulation is observed at grain boundaries and junction points.more » Deformation mechanism maps are constructed with respect to the grain boundary degradation factor and applied strain rate, which dictate the transition from internal to near-surface intergranular fracture modes under various strain amplitudes and grain sizes.« less

Defect and grain boundary scattering in tungsten: A combined theoretical and experimental study

NASA Astrophysics Data System (ADS)

Lanzillo, Nicholas A.; Dixit, Hemant; Milosevic, Erik; Niu, Chengyu; Carr, Adra V.; Oldiges, Phil; Raymond, Mark V.; Cho, Jin; Standaert, Theodorus E.; Kamineni, Vimal K.

2018-04-01

Several major electron scattering mechanisms in tungsten (W) are evaluated using a combination of first-principles density functional theory, a Non-Equilibrium Green's Function formalism, and thin film Kelvin 4-point sheet resistance measurements. The impact of grain boundary scattering is found to be roughly an order of magnitude larger than the impact of defect scattering. Ab initio simulations predict average grain boundary reflection coefficients for a number of twin grain boundaries to lie in the range r = 0.47 to r = 0.62, while experimental data can be fit to the empirical Mayadas-Schatzkes model with a comparable but slightly larger value of r = 0.69. The experimental and simulation data for grain boundary resistivity as a function of grain size show excellent agreement. These results provide crucial insights for understanding the impact of scaling of W-based contacts between active devices and back-end-of-line interconnects in next-generation semiconductor technology.

Microstructural characterization and electron backscatter diffraction analysis across the welded interface of duplex stainless steel

NASA Astrophysics Data System (ADS)

Zhang, Zhiqiang; Jing, Hongyang; Xu, Lianyong; Han, Yongdian; Gao, Zhanqi; Zhao, Lei; Zhang, Jianli

2017-08-01

The microstructural evolution, orientation relationships, boundary characteristics, grain type, local deformation, and microhardness across the welded interface of duplex stainless steel (DSS) were investigated. The DSS welded joint consisted of four typical zones: base metal (BM), low-temperature heat-affected zone (LTHAZ), high-temperature heat-affected zone (HTHAZ), and weld metal (WM). The apparent microstructural changes in the HTHAZ and LTHAZ were secondary austenite and Cr2N precipitation. A modified cooperative precipitation mechanism of secondary austenite and Cr2N at the interface was proposed. Furthermore, the ferrite in both the HTHAZ and LTHAZ maintained the same distribution as the ferrite texture in the BM, while this ferrite texture disappeared completely in the WM. Different austenite grains in the different zones exhibited different orientation relationships with the ferrite matrix. Special grain boundaries were mainly distributed between the austenite grains, while the ferrite grains primarily contained random grain boundaries. Austenite twins constituted the largest proportion of the special boundaries. The special austenite grain boundaries in the BM and LTHAZ were higher in relative frequency than those in the HTHAZ and WM. The ferrite grains in the HTHAZ and WM mainly consisted of substructured grains. In the BM, the recrystallization degree of ferrite was significantly lower than that of austenite grains. The local deformations were mainly generated in the grain boundaries and within the deformed grains. The HTHAZ exhibited the highest hardness, while the BM had the lowest hardness. The LTHAZ had a lower hardness than the HTHAZ and higher hardness than the BM.

STEM and APT characterization of scale formation on a La,Hf,Ti-doped NiCrAl model alloy.

PubMed

Unocic, Kinga A; Chen, Yimeng; Shin, Dongwon; Pint, Bruce A; Marquis, Emmanuelle A

2018-06-01

A thermally grown scale formed on a cast NiCrAl model alloy doped with lanthanum, hafnium, and titanium was examined after isothermal exposure at 1100 °C for 100 h in dry flowing O 2 to understand the dopant segregation along scale grain boundaries. The complex scale formed on the alloy surface was composed of two types of substrates: phase-dependent, thin (<250 nm) outer layers and a columnar-grained ∼3.5 μm inner alumina layer. Two types of oxides formed between the inner and outer scale layers: small (3-15 nm) La 2 O 3 and larger (≤50 nm) HfO 2 oxide precipitates. Nonuniform distributions of the hafnium, lanthanum, and titanium dopants were observed along the inner scale grain boundaries, with hafnium dominating in most of the grain boundaries of α-Al 2 O 3. The concentration of reactive elements (RE) seemed to strongly depend on the grain boundary structure. The level of titanium grain boundary segregation in the inner scale decreased toward the model alloy (substrate), confirming the fast outward diffusion of titanium. Hafnium was also observed at the metal-scale interface and in the γ' (Ni 3 Al) phase of the alloy. High-resolution scanning transmission electron microscopy (STEM) confirmed the substitution of REs for aluminum atoms at the scale grain boundaries, consistent with both the semiconducting band structure and the site-blocking models. Both STEM and atom probe tomography allowed quantification of REs along the scale grain boundaries across the scale thickness. Analysis of the scale morphology after isothermal exposure in flowing oxygen revealed a myriad of new precipitate phases, RE segregation dependence on grain boundary type, and atomic arrangement along scale grain boundaries, which is expected to influence the scale growth rate, stability, and mechanical properties. Copyright © 2018 Elsevier Ltd. All rights reserved.

Structural and Chemical Analysis of the Zirconia-Veneering Ceramic Interface.

PubMed

Inokoshi, M; Yoshihara, K; Nagaoka, N; Nakanishi, M; De Munck, J; Minakuchi, S; Vanmeensel, K; Zhang, F; Yoshida, Y; Vleugels, J; Naert, I; Van Meerbeek, B

2016-01-01

The interfacial interaction of veneering ceramic with zirconia is still not fully understood. This study aimed to characterize morphologically and chemically the zirconia-veneering ceramic interface. Three zirconia-veneering conditions were investigated: 1) zirconia-veneering ceramic fired on sandblasted zirconia, 2) zirconia-veneering ceramic on as-sintered zirconia, and 3) alumina-veneering ceramic (lower coefficient of thermal expansion [CTE]) on as-sintered zirconia. Polished cross-sectioned ceramic-veneered zirconia specimens were examined using field emission gun scanning electron microscopy (Feg-SEM). In addition, argon-ion thinned zirconia-veneering ceramic interface cross sections were examined using scanning transmission electron microscopy (STEM)-energy dispersive X-ray spectrometry (EDS) at high resolution. Finally, the zirconia-veneering ceramic interface was quantitatively analyzed for tetragonal-to-monoclinic phase transformation and residual stress using micro-Raman spectroscopy (µRaman). Feg-SEM revealed tight interfaces for all 3 veneering conditions. High-resolution transmission electron microscopy (HRTEM) disclosed an approximately 1.0-µm transformed zone at sandblasted zirconia, in which distinct zirconia grains were no longer observable. Straight grain boundaries and angular grain corners were detected up to the interface of zirconia- and alumina-veneering ceramic with as-sintered zirconia. EDS mapping disclosed within the zirconia-veneering ceramic a few nanometers thick calcium/aluminum-rich layer, touching the as-sintered zirconia base, with an equally thick silicon-rich/aluminum-poor layer on top. µRaman revealed t-ZrO2-to-m-ZrO2 phase transformation and residual compressive stress at the sandblasted zirconia surface. The difference in CTE between zirconia- and the alumina-veneering ceramic resulted in residual tensile stress within the zirconia immediately adjacent to its interface with the veneering ceramic. The rather minor chemical elemental shifts recorded in the veneering ceramic did not suffice to draw definitive conclusions regarding potential chemical interaction of the veneering ceramic with zirconia. Sandblasting damaged the zirconia surface and induced phase transformation that also resulted in residual compressive stress. Difference in CTE of zirconia versus that of the veneering ceramic resulted in an unfavorable residual tensile stress at the zirconia-veneering ceramic interface. © International & American Associations for Dental Research 2015.

Cellular interface morphologies in directional solidification. II - The effect of grain boundaries

NASA Technical Reports Server (NTRS)

Ungar, Lyle H.; Brown, Robert A.

1984-01-01

A singular perturbation analysis valid for small grain-boundary slopes is used with the one-sided model for solidification to show that grain boundaries introduce imperfections into the symmetry of the developing cellular interfaces which rupture the junction between the family of planar shapes and the bifurcating cellular families. Undulating interfaces are shown to develop first near grain boundaries, and to evolve with decreasing temperature gradient either by a smooth transition from the almost planar family or by a sudden jump to moderate-amplitude cellular forms, depending on the growth rate.

Ceramic transactions - Materials processing and design: Grain-boundary-controlled properties of fine ceramics II. Volume 44

DOE Office of Scientific and Technical Information (OSTI.GOV)

Niihara, Koichi; Ishizaki, Kozo; Isotani, Mitsuo

This volume contains selected papers presented at a workshop by the Japan Fine Ceramics Center, `Materials Processing and Design Through Better Control of Grain Boundaries: Emphasizing Fine Ceramics II,` which was held March 17-19, 1994, in Koda-cho, Aichi, Japan. The focus of the workshop was the application of grain boundary phenomena to materials processing and design. The topics covered included electronic materials, evaluation methods, structural materials, and interfaces. Also included is an illuminating overview of the current status of work on grain boundary assisted materials processing and design, particularly for fine ceramics. The volume`s chapter titles are: Electron Microscopy, Evaluation,more » Grain Boundary Control and Design, Functional Ceramics, Composite Materials, Synthesis and Sintering, and Mechanical Properties.« less

An improved procedure for determining grain boundary diffusion coefficients from averaged concentration profiles

NASA Astrophysics Data System (ADS)

Gryaznov, D.; Fleig, J.; Maier, J.

2008-03-01

Whipple's solution of the problem of grain boundary diffusion and Le Claire's relation, which is often used to determine grain boundary diffusion coefficients, are examined for a broad range of ratios of grain boundary to bulk diffusivities Δ and diffusion times t. Different reasons leading to errors in determining the grain boundary diffusivity (DGB) when using Le Claire's relation are discussed. It is shown that nonlinearities of the diffusion profiles in lnCav-y6/5 plots and deviations from "Le Claire's constant" (-0.78) are the major error sources (Cav=averaged concentration, y =coordinate in diffusion direction). An improved relation (replacing Le Claire's constant) is suggested for analyzing diffusion profiles particularly suited for small diffusion lengths (short times) as often required in diffusion experiments on nanocrystalline materials.

Grain Boundary Engineering the Mechanical Properties of Allvac 718Plus(Trademark) Superalloy

NASA Technical Reports Server (NTRS)

Gabb, Timothy P.; Telesman, Jack; Garg, Anita; Lin, Peter; Provenzano, virgil; Heard, Robert; Miller, Herbert M.

2010-01-01

Grain Boundary Engineering can enhance the population of structurally-ordered "low S" Coincidence Site Lattice (CSL) grain boundaries in the microstructure. In some alloys, these "special" grain boundaries have been reported to improve overall resistance to corrosion, oxidation, and creep resistance. Such improvements could be quite beneficial for superalloys, especially in conditions which encourage damage and cracking at grain boundaries. Therefore, the effects of GBE processing on high-temperature mechanical properties of the cast and wrought superalloy Allvac 718Plus (Allvac ATI) were screened. Bar sections were subjected to varied GBE processing, and then consistently heat treated, machined, and tested at 650 C. Creep, tensile stress relaxation, and dwell fatigue crack growth tests were performed. The influences of GBE processing on microstructure, mechanical properties, and associated failure modes are discussed.

Effects of the accumulated annealing parameter on the corrosion characteristics of a Zr-0.5Nb-1.0Sn-0.5Fe-0.25Cr alloy

NASA Astrophysics Data System (ADS)

Baek, Jong Hyuk; Jeong, Yong Hwan; Kim, In Sup

2000-07-01

Corrosion behavior, hydrogen pickup, oxide microstructure, and precipitate characterization have been studied in order to investigate the effect of the accumulated annealing parameter on the corrosion characteristics in a Zr-Nb-Sn-Fe-Cr alloy. An autoclave corrosion test was carried out in 400°C steam for 300 days on the Zr-0.5Nb-1.0Sn-0.5Fe-0.25Cr alloy, which had been given 18 different accumulated annealing parameters. The corrosion rate increased with increasing the accumulated annealing parameter. To investigate the crystal structure of oxide layer, the corroded specimens were prepared to have an equal oxide thickness (˜1.6 μm) by controlling exposure time. The relative fraction of tetragonal ZrO 2 also decreased gradually with increasing accumulated annealing parameter. From the hydrogen analysis of the corroded samples for 300 days, it was observed that, with increasing the size of precipitates, the hydrogen pickup was enhanced. It was revealed from transmission electron microscope (TEM) observation of the oxide that the larger precipitates still remained to be oxidized in the oxide layer and had undergone a reduction of Fe/Cr ratio from 2.1 to 1.5. The oxidation of the precipitates in the oxide gave rise to a volume expansion at the precipitate-oxide interface. This volume change could lead to the transformation in the oxide phase from tetragonal ZrO 2 to monoclinic ZrO 2 and in oxide structure from columnar grain to equiaxed grain. The precipitate in a Zr-0.5Nb-1.0Sn-0.5Fe-0.25Cr alloy is composed of Nb, Fe, and Cr and the Nb content in the precipitate increase with increasing accumulated annealing parameter. Thus, it can be thought that Nb within precipitates plays a key role in the microstructural change of oxide.

Calcium and zirconium as texture modifiers during rolling and annealing of magnesium–zinc alloys

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bohlen, Jan, E-mail: jan.bohlen@hzg.de; Wendt, Joachim; Nienaber, Maria

2015-03-15

Rolling experiments were carried out on a ternary Mg–Zn–Ca alloy and its modification with zirconium. Short time annealing of as-rolled sheets is used to reveal the microstructure and texture development. The texture of the as-rolled sheets can be characterised by basal pole figures with split peak towards the rolling direction (RD) and a broad transverse angular spread of basal planes towards the transverse direction (TD). During annealing the RD split peaks as well as orientations in the sheet plane vanish whereas the distribution of orientations tilted towards the TD remains. It is shown in EBSD measurements that during rolling bandsmore » of twin containing structures form. During subsequent annealing basal orientations close to the sheet plane vanish based on a grain nucleation and growth mechanism of recrystallisation. Orientations with tilt towards the TD remain in grains that do not undergo such a mechanism. The addition of Zr delays texture weakening. - Highlights: • Ca in Mg–Zn-alloys contributes to a significant texture weakening during rolling and annealing. • Grain nucleation and growth in structures consisting of twins explain a texture randomisation during annealing. • Grains with transverse tilt of basal planes preferentially do not undergo a grain nucleation and growth mechanism. • Zr delays the microstructure and texture development.« less

Precipitation process in a Mg–Gd–Y alloy grain-refined by Al addition

DOE Office of Scientific and Technical Information (OSTI.GOV)

Dai, Jichun; CAST Cooperative Research Centre, Department of Materials Engineering, Monash University, Victoria 3800; Zhu, Suming, E-mail: suming.zhu@monash.edu

2014-02-15

The precipitation process in Mg–10Gd–3Y (wt.%) alloy grain-refined by 0.8 wt.% Al addition has been investigated by transmission electron microscopy. The alloy was given a solution treatment at 520 °C for 6 h plus 550 °C for 7 h before ageing at 250 °C. Plate-shaped intermetallic particles with the 18R-type long-period stacking ordered structure were observed in the solution-treated state. Upon isothermal ageing at 250 °C, the following precipitation sequence was identified for the α-Mg supersaturated solution: β″ (D0{sub 19}) → β′ (bco) → β{sub 1} (fcc) → β (fcc). The observed precipitation process and age hardening response in themore » Al grain-refined Mg–10Gd–3Y alloy are compared with those reported in the Zr grain-refined counterpart. - Highlights: • The precipitation process in Mg–10Gd–3Y–0.8Al (wt.%) alloy has been investigated. • Particles with the 18R-type LPSO structure were observed in the solution state. • Upon ageing at 250 °C, the precipitation sequence is: β″ → β′ → β1 (fcc) → β. • The Al grain-refined alloy has a lower hardness than the Zr refined counterpart.« less

The 95Zr(n, γ)96Zr Cross Section from the Surrogate Ratio Method and Its Effect on s-process Nucleosynthesis

NASA Astrophysics Data System (ADS)

Yan, S. Q.; Li, Z. H.; Wang, Y. B.; Nishio, K.; Lugaro, M.; Karakas, A. I.; Makii, H.; Mohr, P.; Su, J.; Li, Y. J.; Nishinaka, I.; Hirose, K.; Han, Y. L.; Orlandi, R.; Shen, Y. P.; Guo, B.; Zeng, S.; Lian, G.; Chen, Y. S.; Liu, W. P.

2017-10-01

The 95Zr(n, γ)96Zr reaction cross section is crucial in the modeling of s-process nucleosynthesis in asymptotic giant branch stars because it controls the operation of the branching point at the unstable 95Zr and the subsequent production of 96Zr. We have carried out the measurement of the 94Zr(18O, 16O) and 90Zr(18O, 16O) reactions and obtained the γ-decay probability ratio of 96Zr* and 92Zr* to determine the 95Zr(n, γ)96Zr reaction cross sections with the surrogate ratio method. Our deduced Maxwellian-averaged cross section of 66 ± 16 mb at 30 keV is close to the value recommended by Bao et al., but 30% and more than a factor of two larger than the values proposed by Toukan & Käppeler and Lugaro et al., respectively, and routinely used in s-process models. We tested the new rate in stellar models with masses between 2 and 6 M ⊙ and metallicities of 0.014 and 0.03. The largest changes—up to 80% variations in 96Zr—are seen in models of mass 3–4 M ⊙, where the 22Ne neutron source is mildly activated. The new rate can still provide a match to data from meteoritic stardust silicon carbide grains, provided that the maximum mass of the parent stars is below 4 M ⊙, for a metallicity of 0.03.

Understanding the Effect of Grain Boundary Character on Dynamic Recrystallization in Stainless Steel 316L

NASA Astrophysics Data System (ADS)

Beck, Megan; Morse, Michael; Corolewski, Caleb; Fritchman, Koyuki; Stifter, Chris; Poole, Callum; Hurley, Michael; Frary, Megan

2017-08-01

Dynamic recrystallization (DRX) occurs during high-temperature deformation in metals and alloys with low to medium stacking fault energies. Previous simulations and experimental research have shown the effect of temperature and grain size on DRX behavior, but not the effect of the grain boundary character distribution. To investigate the effects of the distribution of grain boundary types, experimental testing was performed on stainless steel 316L specimens with different initial special boundary fractions (SBF). This work was completed in conjunction with computer simulations that used a modified Monte Carlo method which allowed for the addition of anisotropic grain boundary energies using orientation data from electron backscatter diffraction (EBSD). The correlation of the experimental and simulation work allows for a better understanding of how the input parameters in the simulations correspond to what occurs experimentally. Results from both simulations and experiments showed that a higher fraction of so-called "special" boundaries ( e.g., Σ3 twin boundaries) delayed the onset of recrystallization to larger strains and that it is energetically favorable for nuclei to form on triple junctions without these so-called "special" boundaries.

Investigation by Differential Scanning Calorimetry of Microstructure in a Superplastic Al-Mg-Zr Alloy.

DTIC Science & Technology

1987-06-01

cold-rolled zinc-copper-aluminum eutectic alloy exhibited this superplastic response. Superplasticity was initially viewed as a curious observation...limited to eutectic alloys when tested under the correct laboratory conditions. However, in 1962 Underwood [Ref. 23 reviewed Soviet work; this review...formation of a very fine dispersoid, ZrAI3. This dispersoid results in grain refinement, raises the recrystallization temperature (Ref. 7:p. 414] and gives

Deformation Mechanisms in Tube Billets from Zr-1%Nb Alloy under Radial Forging

NASA Astrophysics Data System (ADS)

Perlovich, Yuriy; Isaenkova, Margarita; Fesenko, Vladimir; Krymskaya, Olga; Zavodchikov, Alexander

2011-05-01

Features of the deformation process by cold radial forging of tube billets from Zr-1%Nb alloy were reconstructed on the basis of X-ray data concerning their structure and texture. The cold radial forging intensifies grain fragmentation in the bulk of billet and increases significantly the latent hardening of potentially active slip systems, so that operation only of the single slip system becomes possible. As a result, in radially-forged billets unusual deformation and recrystallization textures arise. These textures differ from usual textures of α-Zr by the mutual inversion of crystallographic axes, aligned along the axis of tube.

Enhanced ferroelectric polarization and possible morphotrophic phase boundary in PZT-based alloys

DOE PAGES

Parker, David S.; Singh, David; McGuire, Michael A.; ...

2016-05-16

We present a combined theoretical and experimental study of alloys of the high performance piezoelectric PZT (PbZr 0.5Ti 0.5O 3) with BZnT (BiZn 0.5Ti 0.5O 3) and BZnZr (BiZn 0.5Zr 0.5O 3), focusing on atomic displacements, ferroelectric polarization, and elastic stability. From theory we find that the 75-25 PZT-BZnT alloy has substantially larger cation displacements, and hence ferroelectric polarization than the PZT base material, on the tetragonal side of the phase diagram. We also find a possible morphotrophic phase boundary in this system by comparing displacement patterns and optimized c/a ratios. Elastic stability calculations find the structures to be essentiallymore » stable. Lastly, experiments indicate the feasibility of sample synthesis within this alloy system, although measurements do not find significant polarization, probably due to a large coercive field.« less

Creep of quartz by dislocation and grain boundary processes

NASA Astrophysics Data System (ADS)

Fukuda, J. I.; Holyoke, C. W., III; Kronenberg, A. K.

2015-12-01

Wet polycrystalline quartz aggregates deformed at temperatures T of 600°-900°C and strain rates of 10-4-10-6 s-1 at a confining pressure Pc of 1.5 GPa exhibit plasticity at low T, governed by dislocation glide and limited recovery, and grain size-sensitive creep at high T, governed by diffusion and sliding at grain boundaries. Quartz aggregates were HIP-synthesized, subjecting natural milky quartz powder to T=900°C and Pc=1.5 GPa, and grain sizes (2 to 25 mm) were varied by annealing at these conditions for up to 10 days. Infrared absorption spectra exhibit a broad OH band at 3400 cm-1 due to molecular water inclusions with a calculated OH content (~4000 ppm, H/106Si) that is unchanged by deformation. Rate-stepping experiments reveal different stress-strain rate functions at different temperatures and grain sizes, which correspond to differing stress-temperature sensitivities. At 600-700°C and grain sizes of 5-10 mm, flow law parameters compare favorably with those for basal plasticity and dislocation creep of wet quartzites (effective stress exponents n of 3 to 6 and activation enthalpy H* ~150 kJ/mol). Deformed samples show undulatory extinction, limited recrystallization, and c-axis maxima parallel to the shortening direction. Similarly fine-grained samples deformed at 800°-900°C exhibit flow parameters n=1.3-2.0 and H*=135-200 kJ/mol corresponding to grain size-sensitive Newtonian creep. Deformed samples show some undulatory extinction and grain sizes change by recrystallization; however, grain boundary deformation processes are indicated by the low value of n. Our experimental results for grain size-sensitive creep can be compared with models of grain boundary diffusion and grain boundary sliding using measured rates of silicon grain boundary diffusion. While many quartz mylonites show microstructural and textural evidence for dislocation creep, results for grain size-sensitive creep may apply to very fine-grained (<10 mm) quartz mylonites.

Fine Structure in Multi-Phase Zr8Ni21-Zr7Ni10-Zr2Ni7 Alloy Revealed by Transmission Electron Microscope

PubMed Central

Shen, Haoting; Bendersky, Leonid A.; Young, Kwo; Nei, Jean

2015-01-01

The microstructure of an annealed alloy with a Zr8Ni21 composition was studied by both scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The presence of three phases, Zr8Ni21, Zr2Ni7, and Zr7Ni10, was confirmed by SEM/X-ray energy dispersive spectroscopy compositional mapping and TEM electron diffraction. Distribution of the phases and their morphology can be linked to a multi-phase structure formed by a sequence of reactions: (1) L → Zr2Ni7 + L’; (2) peritectic Zr2Ni7 + L’ → Zr2Ni7 + Zr8Ni21 + L”; (3) eutectic L” → Zr8Ni21 + Zr7Ni10. The effect of annealing at 960 °C, which was intended to convert a cast structure into a single-phase Zr8Ni21 structure, was only moderate and the resulting alloy was still multi-phased. TEM and crystallographic analysis of the Zr2Ni7 phase show a high density of planar (001) defects that were explained as low-energy boundaries between rotational variants and stacking faults. The crystallographic features arise from the pseudo-hexagonal structure of Zr2Ni7. This highly defective Zr2Ni7 phase was identified as the source of the broad X-ray diffraction peaks at around 38.4° and 44.6° when a Cu-K was used as the radiation source. PMID:28793460

Influence of thermal and radiation effects on microstructural and mechanical properties of Nb-1Zr

NASA Astrophysics Data System (ADS)

Leonard, Keith J.; Busby, Jeremy T.; Zinkle, Steven J.

2011-07-01

The microstructural changes and corresponding effects on mechanical properties, electrical resistivity and density of Nb-1Zr were examined following neutron irradiation up to 1.8 dpa at temperatures of 1073, 1223 and 1373 K and compared with material thermally aged for similar exposure times of ˜1100 h. Thermally driven changes in the development of intragranular and grain boundary precipitate phases showed a greater influence on mechanical and physical properties compared to irradiation-induced defects for the examined conditions. Initial formation of the zirconium oxide precipitates was identified as cubic structured plates following a Baker-Nutting orientation relationship to the β-Nb matrix, with particles developing a monoclinic structure on further growth. Tensile properties of the Nb-1Zr samples showed increased strength and reduced elongation following aging and irradiation below 1373 K, with the largest tensile and hardness increases following aging at 1098 K. Tensile properties at 1373 K for the aged and irradiated samples were similar to that of the as-annealed material. Total elongation was lower in the aged material due to a strain hardening response, rather than a weak strain softening observed in the irradiated materials due in part to an irregular distribution of the precipitates in the irradiated materials. Though intergranular fracture surfaces were observed on the 1248 K aged tensile specimens, the aged and irradiated material showed uniform elongations >3% and total elongation >12% for all conditions tested. Cavity formation was observed in material irradiated to 0.9 dpa at 1073 and 1223 K. However, since void densities were estimated to be below 3 × 10 17 m -3 these voids contributed little to either mechanical strengthening of the material or measured density changes.

Zirconia based ceramic coating on a metal with plasma electrolytic oxidation

NASA Astrophysics Data System (ADS)

Akatsu, T.; Kato, T.; Shinoda, Y.; Wakai, F.

2011-10-01

We challenge to fabricate a thermal barrier coating (TBC) made of ZrO2 based ceramics on a Ni based single crystal superalloy with plasma electrolytic oxidation (PEO) by incorporating metal species from electrolyte into the coating. The PEO process is carried out on the superalloy galvanized with aluminium for 15min in Na4O7P4 solution for an oxygen barrier coating (OBC) and is followed by PEO in K2[Zr(CO3)2(OH)2] solution for TBC. We obtained the following results; (1) Monoclinic-, tetragonal-, cubic-ZrO2 crystals were detected in TBC. (2) High porosity with large pores was observed near the interface between OBC and TBC. The fine grain structure with a grain size of about 300nm was typically observed. (3) The adhesion strength between PEO coatings and substrate was evaluated to be 26.8±6.6MPa. At the adhesion strength test, PEO coatings fractured around the interface between OBC and TBC. The effect of coating structure on adhesion strength is explained through the change in spark discharge during PEO process.

Microstructural effects on damage evolution in shocked copper polycrystals

DOE PAGES

Lieberman, Evan J.; Lebensohn, Ricardo A.; Menasche, David B.; ...

2016-07-01

Three-dimensional crystal orientation fields of a copper sample, characterized before and after shock loading using High Energy Diffraction Microscopy, are used for input and validation of direct numerical simulations using a Fast Fourier Transform (FFT)-based micromechanical model. The locations of the voids determined by X-ray tomography in the incipiently-spalled sample, predominantly found near grain boundaries, were traced back and registered to the pre-shocked microstructural image. Using FFT-based simulations with direct input from the initial microstructure, micromechanical fields at the shock peak stress were obtained. Statistical distributions of micromechanical fields restricted to grain boundaries that developed voids after the shock aremore » compared with corresponding distributions for all grain boundaries. Distributions of conventional measures of stress and strain (deviatoric and mean components) do not show correlation with the locations of voids in the post-shocked image. Neither does stress triaxiality, surface traction or grain boundary inclination angle, in a significant way. On the other hand, differences in Taylor factor and accumulated plastic work across grain boundaries do correlate with the occurrence of damage. As a result, damage was observed to take place preferentially at grain boundaries adjacent to grains having very different plastic response.« less

Multiscale simulation of xenon diffusion and grain boundary segregation in UO₂

DOE PAGES

Andersson, David A.; Tonks, Michael R.; Casillas, Luis; ...

2015-07-01

In light water reactor fuel, gaseous fission products segregate to grain boundaries, resulting in the nucleation and growth of large intergranular fission gas bubbles. The segregation rate is controlled by diffusion of fission gas atoms through the grains and interaction with the boundaries. Based on the mechanisms established from earlier density functional theory (DFT) and empirical potential calculations, diffusion models for xenon (Xe), uranium (U) vacancies and U interstitials in UO₂ have been derived for both intrinsic (no irradiation) and irradiation conditions. Segregation of Xe to grain boundaries is described by combining the bulk diffusion model with a model formore » the interaction between Xe atoms and three different grain boundaries in UO₂ (Σ5 tilt, Σ5 twist and a high angle random boundary), as derived from atomistic calculations. The present model does not attempt to capture nucleation or growth of fission gas bubbles at the grain boundaries. The point defect and Xe diffusion and segregation models are implemented in the MARMOT phase field code, which is used to calculate effective Xe and U diffusivities as well as to simulate Xe redistribution for a few simple microstructures.« less

A three-dimensional polyhedral unit model for grain boundary structure in fcc metals

NASA Astrophysics Data System (ADS)

Banadaki, Arash Dehghan; Patala, Srikanth

2017-03-01

One of the biggest challenges in developing truly bottom-up models for the performance of polycrystalline materials is the lack of robust quantitative structure-property relationships for interfaces. As a first step in analyzing such relationships, we present a polyhedral unit model to classify the geometrical nature of atomic packing along grain boundaries. While the atomic structure in disordered systems has been a topic of interest for many decades, geometrical analyses of grain boundaries has proven to be particularly challenging because of the wide range of structures that are possible depending on the underlying macroscopic crystallographic character. In this article, we propose an algorithm that can partition the atomic structure into a connected array of three-dimensional polyhedra, and thus, present a three-dimensional polyhedral unit model for grain boundaries. A point-pattern matching algorithm is also provided for quantifying the distortions of the observed grain boundary polyhedral units. The polyhedral unit model is robust enough to capture the structure of high-Σ, mixed character interfaces and, hence, provides a geometric tool for comparing grain boundary structures across the five-parameter crystallographic phase-space. Since the obtained polyhedral units circumscribe the voids present in the structure, such a description provides valuable information concerning segregation sites within the grain boundary. We anticipate that this technique will serve as a powerful tool in the analysis of grain boundary structure. The polyhedral unit model is also applicable to a wide array of material systems as the proposed algorithm is not limited by the underlying lattice structure.

Magnetic properties enhancement of melt spun CoZrB ribbons by elemental substitutions

NASA Astrophysics Data System (ADS)

Chang, H. W.; Tsai, C. F.; Hsieh, C. C.; Shih, C. W.; Chang, W. C.; Shaw, C. C.

2013-11-01

Effect of elemental substitution of M (M=C, Cu, Ga, Al and Si) for Zr on the magnetic properties, phase evolution, and microstructure of melt spun Co80Zr18-xMxB2 (x=0-2) ribbons have been investigated. The x-ray diffraction (XRD) and thermal magnetic analysis (TMA) results showed that two magnetically soft phases, namely fcc-Co and Co23Zr6, coexisted with hard phase Co5Zr in Co80Zr17M1B2 ribbons with M=Cu, Ga, Al and Si, while an extra unknown magnetic phase was present in ribbons with M=C. The ribbons with M=C and Si were found to improve the remanence (σr) of the Co80Zr17M1B2 ribbons. However, only M=Si could improve the whole magnetic properties, including Br, intrinsic coercivity (iHc) and energy product ((BH)max) of the above ribbons. The optimal magnetic properties of Br=5.2 kG, iHc=4.5 kOe, and (BH)max=5.3 MGOe were obtained in Co80Zr17Si1B2 ribbons, which possessed Co5Zr and minor fcc-Co phases with much finer grain size (10-30 nm) in comparison with its counterpart Co80Zr18B2 (20-60 nm).

Role of Hf on Phase Formation in Ti45Zr(38-x)Hf(x)Ni17 Liquids and Solids

NASA Technical Reports Server (NTRS)

Wessels, V.; Sahu, K. K.; Gangopadhyay, A. K.; Huett, V. T.; Canepari, S.; Goldman, A. I.; Hyers, R. W.; Kramer, M. J.; Rogers, J. R.; Kelton, K. F.;

Symmetric Tilt Grain Boundaries of Synthetic Forsterite Bicrystals

NASA Astrophysics Data System (ADS)

Heinemann, S.; Wirth, R.; Dresen, G.

2002-12-01

{ indent1.5em skip0ex Structure and transport properties of grain boundaries in rocks are still poorly understood. For example, grain boundary diffusivity and mobility depend on orientation, and they are different for low and high angle grain boundaries. The transition from low to high angle grain boundaries in rock-forming minerals is not studied in detail, but a high angle grain boundary is commonly defined by a lattice misorientation of >10°-15°. To investigate the physical properties of olivine grain boundaries we produced a series of synthetic forsterite bicrystals with symmetric tilt grain boundaries by direct bonding [1,2]. For each bicrystal two oriented synthetic forsterite single crystals were joined at room temperature and annealed at 400°C for one week. All bicrystals were cut in two parts and one part was annealed further at 1650°C for 48h. The tilt axis of the boundary in the synthesized bicrystals is parallel to the a direction, and the tilt angles of the series range from 9° to 21°. Specimens were prepared for investigations in the transmission electron microscope (TEM) using focused ion beam (FIB) technique. High-resolution TEM investigations of symmetric tilt grain boundaries reveal dislocation arrays between undisturbed crystal regions in samples annealed at 400°C and 1650°C. This suggests that bonding of bicrystals occurred already below or at 400°C. The burgers vectors of the dislocations are parallel to c. Dislocation cores do not overlap up to a tilt angle of 21°. This indicates that for forsterite small angle grain boundaries exist up to tilt angles of 21°. The dislocation model of small angle grain boundaries can be applied and the observed dislocation spacings d are related to tilt angle θ and burgers vector length b by Franks formula [3]: d = b/(2sin(2/θ )) ~ b/θ . With tilt angles increasing from 9° to 21° the dislocation spacing decreased. Using Frank's equation and the observation that dislocations do not overlap at a misorientation of 21° allows to estimate the maximum radius of the dislocation cores, r0<1.4b.} {skip0ex \\small [1] Heinemann S et al. (2001) Phys Chem Minerals 28, 685 [2] Heinemann S et al. (2002) Beih Eur Mineral 14(1), 66 [3] Frank FC (1951) Pittsburgh Symposium on the Plastic Deformation of Solids. 150}

Colloidal crystal grain boundary formation and motion

PubMed Central

Edwards, Tara D.; Yang, Yuguang; Beltran-Villegas, Daniel J.; Bevan, Michael A.

2014-01-01

The ability to assemble nano- and micro- sized colloidal components into highly ordered configurations is often cited as the basis for developing advanced materials. However, the dynamics of stochastic grain boundary formation and motion have not been quantified, which limits the ability to control and anneal polycrystallinity in colloidal based materials. Here we use optical microscopy, Brownian Dynamic simulations, and a new dynamic analysis to study grain boundary motion in quasi-2D colloidal bicrystals formed within inhomogeneous AC electric fields. We introduce “low-dimensional” models using reaction coordinates for condensation and global order that capture first passage times between critical configurations at each applied voltage. The resulting models reveal that equal sized domains at a maximum misorientation angle show relaxation dominated by friction limited grain boundary diffusion; and in contrast, asymmetrically sized domains with less misorientation display much faster grain boundary migration due to significant thermodynamic driving forces. By quantifying such dynamics vs. compression (voltage), kinetic bottlenecks associated with slow grain boundary relaxation are understood, which can be used to guide the temporal assembly of defect-free single domain colloidal crystals. PMID:25139760

Grain boundary oxidation and an analysis of the effects of oxidation on fatigue crack nucleation life

NASA Technical Reports Server (NTRS)

Oshida, Y.; Liu, H. W.

1988-01-01

The effects of preoxidation on subsequent fatigue life were studied. Surface oxidation and grain boundary oxidation of a nickel-base superalloy (TAZ-8A) were studied at 600 to 1000 C for 10 to 1000 hours in air. Surface oxides were identified and the kinetics of surface oxidation was discussed. Grain boundary oxide penetration and morphology were studied. Pancake type grain boundary oxide penetrates deeper and its size is larger, therefore, it is more detrimental to fatigue life than cone-type grain boundary oxide. Oxide penetration depth, a (sub m), is related to oxidation temperature, T, and exposure time, t, by an empirical relation of the Arrhenius type. Effects of T and t on statistical variation of a (sub m) were analyzed according to the Weibull distribution function. Once the oxide is cracked, it serves as a fatigue crack nucleus. Statistical variation of the remaining fatigue life, after the formation of an oxide crack of a critical length, is related directly to the statistical variation of grain boundary oxide penetration depth.

Testing thermal gradient driving force for grain boundary migration using molecular dynamics simulations

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bai, Xian-Ming; Zhang, Yongfeng; Tonks, Michael R.

2015-02-01

Strong thermal gradients in low-thermal-conductivity ceramics may drive extended defects, such as grain boundaries and voids, to migrate in preferential directions. In this work, molecular dynamics simulations are conducted to study thermal gradient driven grain boundary migration and to verify a previously proposed thermal gradient driving force equation, using uranium dioxide as a model system. It is found that a thermal gradient drives grain boundaries to migrate up the gradient and the migration velocity increases under a constant gradient owing to the increase in mobility with temperature. Different grain boundaries migrate at very different rates due to their different intrinsicmore » mobilities. The extracted mobilities from the thermal gradient driven simulations are compared with those calculated from two other well-established methods and good agreement between the three different methods is found, demonstrating that the theoretical equation of the thermal gradient driving force is valid, although a correction of one input parameter should be made. The discrepancy in the grain boundary mobilities between modeling and experiments is also discussed.« less

Linking Grain Boundary Microstructure to Stress Corrosion Cracking of Cold Rolled Alloy 690 in PWR Primary Water

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bruemmer, Stephen M.; Olszta, Matthew J.; Toloczko, Mychailo B.

2012-10-01

Grain boundary microstructures and microchemistries are examined in cold-rolled alloy 690 tubing and plate materials and comparisons are made to intergranular stress corrosion cracking (IGSCC) behavior in PWR primary water. Chromium carbide precipitation is found to be a key aspect for materials in both the mill annealed and thermally treated conditions. Cold rolling to high levels of reduction was discovered to produce small IG voids and cracked carbides in alloys with a high density of grain boundary carbides. The degree of permanent grain boundary damage from cold rolling was found to depend directly on the initial IG carbide distribution. Formore » the same degree of cold rolling, alloys with few IG precipitates exhibited much less permanent damage. Although this difference in grain boundary damage appears to correlate with measured SCC growth rates, crack tip examinations reveal that cracked carbides appeared to blunt propagation of IGSCC cracks in many cases. Preliminary results suggest that the localized grain boundary strains and stresses produced during cold rolling promote IGSCC susceptibility and not the cracked carbides and voids.« less

Studies of electronic structure of ZnO grain boundary and its proximity by using spatially resolved electron energy loss spectroscopy

NASA Astrophysics Data System (ADS)

Ong, H. C.; Dai, J. Y.; Du, G. T.

2002-07-01

The low electron energy loss and complex dielectric functions of an arbitrary grain boundary and its proximity in ZnO thin films have been studied by using the spatially resolved electron energy loss spectroscopy. The critical point parameters have been determined by fitting the dielectric functions simultaneously with analytical line shape model. Gradual changes have been observed in the dielectric functions spectra. The critical points are found to redshift and then blueshift when the electron beam scanned across the grain boundary, which suggest the distinctive electronic structure not only of the grain boundary but also of the depletion region. In addition, comparison has been made between the experiment and the recent theoretical studies to account for the interband transitions that occur in the grain boundaries. Several features predicted by the theory are qualitatively found to be consistent with our results. The presence of dangling bonds instead of bond distortion is attributed to be the major cause of defects in the grain boundaries of ZnO.

Finite element modelling of creep cavity filling by solute diffusion

NASA Astrophysics Data System (ADS)

Versteylen, C. D.; Szymański, N. K.; Sluiter, M. H. F.; van Dijk, N. H.

2018-04-01

In recently discovered self healing creep steels, open-volume creep cavities are filled by the precipitation of supersaturated solute. These creep cavities form on the grain boundaries oriented perpendicular to the applied stress. The presence of a free surface triggers a flux of solute from the matrix, over the grain boundaries towards the creep cavities. We studied the creep cavity filling by finite element modelling and found that the filling time critically depends on (i) the ratio of diffusivities in the grain boundary and the bulk, and (ii) on the ratio of the intercavity distance and the cavity size. For a relatively large intercavity spacing 3D transport is observed when the grain boundary and volume diffusivities are of a similar order of magnitude, while a 2D behaviour is observed when the grain boundary diffusivity is dominant. Instead when the intercavity distance is small, the transport behaviour tends to a 1D behaviour in all cases, as the amount of solute available in the grain boundary is insufficient. A phase diagram with the transition lines is constructed.

Effect of Trace Levels of Si on Microstructure and Grain Boundary Segregation in DOP-26 Iridium Alloy

NASA Astrophysics Data System (ADS)

Pierce, Dean; Muralidharan, Govindarajan; Heatherly, Lee; Fox, Ethan

2018-03-01

The thermodynamics and kinetics of Silicon (Si) segregation to grain boundaries in Iridium alloy DOP-26 with added trace levels of Si of 6, 11, 29, and 36 wppm was studied by Auger Electron Spectroscopy. The four alloys were annealed at 1500 or 1535 °C for 19 or 76 hours followed by cooling at three different rates. Si enrichment at the grain boundaries (GB) increased with increasing bulk Si content, with the grain boundary Si enrichment factors ranging from 62 to 344, depending on the bulk Si content and the cooling rate. Grain boundary Si contents increased with decreasing cooling rate in all alloys, indicating that Si GB segregation is influenced by both thermodynamic and kinetic factors in the alloys and temperature ranges of the study. A Langmuir-McLean isotherm-based model was successfully used to predict the temperature dependence of GB Si segregation in DOP-26 alloys with Si additions and estimate the temperature independent free energy of Si segregation to grain boundaries in DOP-26.

Grain boundary oxidation and an analysis of the effects of pre-oxidation on subsequent fatigue life

NASA Technical Reports Server (NTRS)

Oshida, Y.; Liu, H. W.

1986-01-01

The effects of preoxidation on subsequent fatigue life were studied. Surface oxidation and grain boundary oxidation of a nickel-base superalloy (TAZ-8A) were studied at 600 to 1000 C for 10 to 1000 hours in air. Surface oxides were identified and the kinetics of surface oxidation was discussed. Grain boundary oxide penetration and morphology were studied. Pancake type grain boundary oxide penetrates deeper and its size is larger, therefore, it is more detrimental to fatigue life than cone-type grain boundary oxide. Oxide penetration depth, a (sub m), is related to oxidation temperature, T, and exposure time, t, by an empirical relation of the Arrhenius type. Effects of T and t on statistical variation of a (sub m) were analyzed according to the Weibull distribution function. Once the oxide is cracked, it serves as a fatigue crack nucleus. Statistical variation of the remaining fatigue life, after the formation of an oxide crack of a critical length, is related directly to the statistical variation of grain boundary oxide penetration depth.

Static Grain Growth in Contact Metamorphic Calcite: A Cathodoluminescence Study.

NASA Astrophysics Data System (ADS)

Vogt, B.; Heilbronner, R.; Herwegh, M.; Ramseyer, K.

2009-04-01

In the Adamello contact aureole, monomineralic mesozoic limestones were investigated in terms of grain size evolution and compared to results on numerical modeling performed by Elle. The sampled area shows no deformation and therefore represents an appropriate natural laboratory for the study of static grain growth (Herwegh & Berger, 2003). For this purpose, samples were collected at different distances to the contact to the pluton, covering a temperature range between 270 to 630°C. In these marbles, the grain sizes increase with temperature from 5 µm to about 1 cm as one approaches the contact (Herwegh & Berger, 2003). In some samples, photomicrographs show domains of variable cathodoluminescence (CL) intensities, which are interpreted to represent growth zonations. Microstructures show grains that contain cores and in some samples even several growth stages. The cores are usually not centered and the zones not concentric. They may be in touch with grain boundaries. These zonation patterns are consistent within a given aggregate but differ among the samples even if they come from the same location. Relative CL intensities depend on the Mn/Fe ratio. We assume that changes in trace amounts of Mn/Fe must have occurred during the grain size evolution, preserving local geochemical trends and their variations with time. Changes in Mn/Fe ratios can either be explained by (a) locally derived fluids (e.g. hydration reactions of sheet silicate rich marbles in the vicinity) or (b) by the infiltration of the calcite aggregates by externally derived (magmatic?) fluids. At the present stage, we prefer a regional change in fluid composition (b) because the growth zonations only occur at distances of 750-1250 m from the pluton contact (350-450°C). Closer to the contact, neither zonations nor cores were found. At larger distances, CL intensities differ from grain to grain, revealing diagenetic CL patterns that were incompletely recrystallized by grain growth. The role of infiltration of magmatic fluids is also manifest in the vicinity of dikes, where intense zonation patterns are prominent in the marbles. The software Elle was developed to simulate microstructural evolution in rocks. The numerical model with the title "Grain boundary sweeping" was performed by M. Jessell and was found on http://www.materialsknowledge.org/elle. It displays the grain size evolution and the development of growth zonations during grain boundary migration of a 2D foam structure. This simulation was chosen because the driving force is the minimization of isotropic surface energies. It will be compared to the natural microstructures. At the last stage of the simulation the average grain and core sizes have increased. All, even the smallest grains, show growth zonations. Grains can be divided into two groups: (a) initially larger grains, increasing their grain size and maintaining their core size and (b) initially smaller grains with decreasing grain and decreasing core size. Group (a) grains show large areas swept by grain boundaries into the direction of small grains. Grain boundaries between large grains move more slowly. Their cores do not touch any grain boundaries. Cores of group (b) grains are in contact with the grain boundary network and are on the way to be consumed. In the numerical model and in the natural example similar features can be observed: The cores are not necessarily centered, the zonations are not necessarily concentric and some of the cores touch the grain boundary network. In the simulation, grain boundary migration velocity between large grains is smaller than between a large and a small grain. From this we would predict that - given enough time - a well sorted grain size distribution of increased grain size could be generated. But since many small grains occur we infer that this equilibrium has not been obtained. Analytical results of some natural samples that could be analyzed up to now indicate a relatively well sorted grain size distribution suggesting a more mature state of static grain growth. In comparison to the simulation, grain and core boundaries in the marbles are not always straight. For lobate grain boundaries the surface area has not been minimized in respect to the grain size. An explanation for this might be grain boundary pinning or a local dynamic overprint. Some cores and growth zones in the investigated calcites show a continuous change in luminescence. This is interpreted to be an effect of late diffusion within the grain and/or a continuous change of fluid composition and supply. The absence of zonation in samples close to the contact might be explained by fast grain growth due to high temperatures and/or fast fluid transport. Possibly, this is combined with an enhanced component of volume diffusion. Thus concentration variations of Mn/Fe are diminished and not visible in form of a growth zonation. Herwegh M, Berger A (2003) Differences in grain growth of calcite: a field-based modeling approach. Contr. Min. Pet. 145: 600-611