Influence of Grain Boundary Character on Creep Void Formation in Alloy 617

Alloy 617, a high-temperature creep-resistant, nickel-based alloy, is being considered for the primary heat exchanger for the Next Generation Nuclear Plant (NGNP), which will operate at temperatures exceeding 760 °C and a helium pressure of approximately 7 MPa. Observations of the crept microstructure using optical microscopy indicate creep stress does not significantly influence the creep void fraction at a given creep strain over the relatively narrow set of creep conditions studied. Void formation was found to occur only after significant creep in the tertiary regime (>5 pct total creep strain) had occurred. Also, orientation imaging microscopy (OIM) was used to characterize the grain boundaries in the vicinity of creep voids that develop during high-temperature creep tests (900 °C to 1000 °C at creep stresses ranging from 20 to 40 MPa) terminated at creep strains ranging from 5 to 40 pct. Preliminary analysis of the OIM data indicates voids tend to form on grain boundaries parallel, perpendicular, or 45 deg to the tensile axis, while few voids are found at intermediate inclinations to the tensile axis. Random grain boundaries intersect most voids, while coincident site lattice (CSL)–related grain boundaries did not appear to be consistently associated with void development. Similar results were found in oxygen-free, high-conductivity (OFHC) copper, severely deformed using equal channel angular extrusion, and creep tested at 450 °C and 14 MPa.     

Ni-30Cr-1Cu合金晶粒度及晶界沉淀与脆性的关系

用晶界萃取复型技术研究了晶界一次相极少、二次相析出倾向很大的Ni-30Cr-1Cu合金的晶界沉淀规律.采用不同温度固溶后盐水快速冷却以抑制晶界二次相的析出,获得了晶界沉淀状态相近的不同尺寸晶粒.结果表明,随单纯晶粒长大,合金的室温冲击韧性、拉伸塑性均有不同程度的升高.于1180℃固溶后以不同速度冷却,结果显示随冷却速度的减慢,晶界M23C6显著增多、分布密度增大;其沉淀形态分别由空冷的精细薄片状向缓冷的颗粒状、棒状、薄膜状乃至枝晶状转变,使晶界在室温脆化,冲击韧性和拉伸塑性显著下降;断裂方式由以穿晶为主的混合型断裂向沿晶脆性断裂转变.     

Effect of Heat Treatment on Solute Concentration at Grain Boundaries in 7075 Aluminum Alloy

The effect of heat treatment on the relative amounts of magnesium, zinc, copper, iron and silicon in grain boundaries of aluminum 7075 alloy was investigated with Auger electron spectroscopy in a scanning Auger microprobe. It was observed that both aging and solution treatments affect the distribution of these elements at grain boundaries. If identical solution heat treatments were employed, the aging treatment determined the solute distribution at the grain boundaries, and for fixed final aging treatment, the temperature of solution anneal determined the solute distribution. Among specimens given a T6 final aging treatment (24 h at 394 K (250 °F)) with prior solution treatment temperatures in the 666 K (740 °F) to 800 K (980 °F) range, 711 K (820 °F) solution treated specimen was found to have the least solute concentration at grain boundaries. The observed behavior is explained on the basis of equilibrium and nonequilibrium segregation of solute elements to grain boundaries occurring on quenching and during aging.     

Ni-30Cr-1Cu合金晶粒尺寸及晶界沉淀与脆性的关系

用晶界萃取复型技术研究了晶界一次相极少、二次相析出倾向很大的Ni-30Cr-1Cu合金的晶界沉淀规律。采用不同温度固溶后盐水快速冷却以抑制晶界二次相的析出获得了晶界沉淀状态相近的不同尺寸晶粒,结果表明,随单纯晶粒长大,合金的室温冲击韧性、拉伸塑性均有不同程度的升高。于1180℃固溶后以不同速度冷却,结果显示了随冷却速度减慢,晶界M23C6显著增多、分布密度增大;其沉淀特征分别由空冷的精细薄片状向缓冷的颗粒状、棒状、薄膜状乃至枝晶状转变,使晶界在室温脆化,冲击韧性和拉伸塑性显著下降;断裂特征由以穿晶为主的混合型断裂向沿晶脆性断裂转化。     

Pinning of Austenite Grain Boundaries by

The growth behavior of austenite grains in the presence of A1N precipitates varies with the temperature and time of anneal. To study this behavior, two iron alloys, (in weight percent) a 0.1 carbon base chemistry with 0.03A1/0.01N and 0.09A1/0.04N, respectively, were annealed between 1000 °C and 1200 °C for times of up to 180 minutes. Using optical microscopy, as many as 1000 austenite grains per heat-treatment condition were measured. Conditions of sup- pressed, abnormal, and uniform grain growth were observed. Using an extraction replica tech- nique, the size, shape, and distribution of the A1N particles were determined using transmission electron microscopy (TEM). The largest grain boundary curvatures calculated, using the Hellman- Hillert pinning model, were in close agreement with independent calculations of curvatures using the grain size data. The largest grains in the lognormal size distribution of austenite grains were found to be the ones with the potential to grow to abnormally large sizes.     

Precipitate Redistribution during Creep of Alloy 617

Nickel-based superalloys are being considered for applications within advanced nuclear power generation systems due to their high-temperature strength and corrosion resistance. Alloy 617, a candidate for use in heat exchangers, derives its strength from both solid solution strengthening and the precipitation of carbide particles. However, during creep, carbides that are supposed to retard grain boundary motion are found to dissolve and reprecipitate on boundaries in tension. To quantify the redistribution, we have used electron backscatter diffraction (EBSD) and energy-dispersive spectroscopy (EDS) to analyze the microstructure of 617 after creep testing at 900 °C and 1000 °C. The data were analyzed with respect to the location of the carbides (e.g., intergranular vs intragranular), grain boundary character, and precipitate type (i.e., Cr rich or Mo rich). We find that grain boundary character is the most important factor in carbide distribution; some evidence of preferential distribution to boundaries in tension is also observed at higher applied stresses. Finally, the results suggest that the observed redistribution is due to the migration of carbides to the boundaries and not the migration of boundaries to the precipitates.     

晶界在超塑性变形中的作用

超塑性材料所具有的微细晶粒组织,意味着材料的单位体积内存在着大量的晶界。本文结合作者及其合作者近几年来所进行的研究工作,详细地论述了晶界在超塑性变形中所起的重要作用。     

Effect of Grain Boundaries and Grain Orientation on Structure and Properties

The evolution of deformation microstructures in metals follows a universal pattern of grain subdivision. However, the structure in the grain boundary region may be different from that in the grain interior, although a characteristic region cannot be identified for polycrystals with medium to high stacking fault energy. In the grain interior, the dislocation structure is predominantly composed of almost planar boundaries (geometrically necessary boundaries) and cell boundaries (incidental dislocation boundaries) forming a cell block structure. For grains with grain sizes reaching down to about 4 μm deformed in tension and by rolling, a clear correlation has been established between the characteristics of the deformation structure and the orientation of the grain in which it evolves. A similar correlation is observed for single crystals of different orientations. Such correlations form the basis for a general analysis of active slip systems and for modeling of the flow stress and flow stress anisotropy of polycrystalline samples.     

Segregation at Melted Grain Boundaries in Steel

Abstract

Test samples from continuously cast steels have been fractured by grain boundary melting. The faceted fracture surfaces have been examined by Auger spectroscopy. Sulphur has been found to be segregated on the surface of all of the facets examined. The amount of segregation varies appreciably for different facets in a given sample; on average the segregation increases significantly with an increase in sulphur level from 0.014 to 0.024% S. No segregation of P was detected on the fractured surfaces.

Résumé

Des échantillons d'aciers de coulée continue ont été rupturés par fusion aux joints de grains. Les surfaces de rupture à facettes ont été examinées par spectroscopie Auger. On.a trouvé, sur toutes les surfaces des facettes examinées, une ségrégation de soufre. Le montant de la ségrégation varie appréciablement pour différentes facettes d'un même échantillon. En moyenne, l'étendue de la ségrégation augmente quand la concentration en soufre passe de 0.014 à 0.024%. On n'a pas détecté de ségrégation de P sur les surfaces de rupture.     

Grain Boundaries and Mechanical Properties of Ultrafine-Grained Metals

The concept of grain boundary (GB) engineering of ultrafine-grained (UFG) metals and alloys is developed for enhancement of their properties by tailoring different GBs (low-angle and high-angle ones, special and random, or equilibrium and nonequilibrium) and formation of GB segregations and precipitations by severe plastic deformation (SPD) processing. In this article, using this approach and varying regimes and routes of SPD processing, we show for several light alloys (Al and Ti) the ability to produce UFG materials with different GBs, and this can have a dramatic effect on the mechanical behavior of the processed materials. This article demonstrates also several new examples of attaining superior strength and ductility as well as enhanced superplasticity at low temperatures and high strain rates in various UFG metals and alloys.     

Calculating Dislocation Spacings in Pile-Ups at Grain Boundaries

Dislocation pile-ups near planar grain boundaries have been analyzed employing full anisotropic elastic solutions, single-crystal anisotropic approximations, and isotropic approximations. The calculations were performed for a series of iron-silicon bicrystal configurations and results from the various methods compared. Three of the bicrystal/slip system combinations exhibited repulsive image forces, allowing elastically self-consistent position calculations. Based on these results, either linear elastic or nonlinear effects can dominate the behavior of these pile-ups, depending on specific boundary conditions.     

Threshold Stress Creep Behavior of Alloy 617 at Intermediate Temperatures

Creep of Alloy 617, a solid solution Ni-Cr-Mo alloy, was studied in the temperature range of 1023 K to 1273 K (750 °C to 1000 °C). Typical power-law creep behavior with a stress exponent of approximately 5 is observed at temperatures from 1073 K to 1273 K (800 °C to 1000 °C). Creep at 1023 K (750 °C), however, exhibits threshold stress behavior coinciding with the temperature at which a low volume fraction of ordered coherent γ′ precipitates forms. The threshold stress is determined experimentally to be around 70 MPa at 1023 K (750 °C) and is verified to be near zero at 1173 K (900 °C)—temperatures directly correlating to the formation and dissolution of γ′ precipitates, respectively. The γ′ precipitates provide an obstacle to continued dislocation motion and result in the presence of a threshold stress. TEM analysis of specimens crept at 1023 K (750 °C) to various strains, and modeling of stresses necessary for γ′ precipitate dislocation bypass, suggests that the climb of dislocations around the γ′ precipitates is the controlling factor for continued deformation at the end of primary creep and into the tertiary creep regime. As creep deformation proceeds at an applied stress of 121 MPa and the precipitates coarsen, the stress required for Orowan bowing is reached and this mechanism becomes active. At the minimum creep rate at an applied stress of 145 MPa, the finer precipitate size results in higher Orowan bowing stresses and the creep deformation is dominated by the climb of dislocations around the γ′ precipitates.     

Low-Angle Grain Boundaries in Sublimation Grown 6H-SiC Crystals

High-resolution X-ray diffractometry (HRXRD) was used to assess the quality of 6H-SiC crystals grown by sublimation method. The results show the occurrence of low-angle grain boundaries (LB) is close relative to the inclination of the crystal interface. At the central faceted region with 0° inclination the crystal is of high structural perfection. However, at the region close to the facet with less than 5° inclination LB occurs slightly and at the region close to the peripheral polytype ring with more than 5° inclination LB defect occurs heavily. The density of LB can be drastically reduced by decreasing radial temperature gradient that determines the shape of the crystal growth interface.     

分步冷却过程中磷的非平衡晶界偏聚

研究了分步冷却过程中12Cr1MoV钢磷的非平衡晶界偏聚。从理论上计算了磷的晶界偏聚等效时间和晶界偏聚量，并用实验验证了根据动力学计算得出的磷的晶界偏聚浓度。试验结果与理论计算值相符．可为预测钢在实际服役状况下的晶界脆性提供依据。     

The Use and Control of Grain Boundaries in Thin Films

Abstract

Polycrystalline thin films are widely used in the electronics industry and in surface protection applications. For most cases, a single crystal film would be preferable but is too costly or simply impossible to achieve. Thus, the grain boundaries are regarded as a necessary evil. We discuss the behavior of grain boundaries during film formation, processing and utilization, illustrating beneficial as well as deleterious effects. Some potential strategies for the control of grain boundary behavior are derived by the application of basic interfacial science.

Résumé

L'utilisation de films finspolycristallins est largement répandue dans l'industrie électronique et dans les applications de protection de surfaces. Dans la plupart des cas, un film monocristallin serait préférable, mais ceci est en fait trop coûteux et bien trop difficile à réaliser, alors les grains sont perçus comme une nécessité malencontreuse. Nous considérons le comportement des joints des grains durant la formation, le traitement et l'utilisation des films, en illustrant tout aussi bien les effets bénéfiques que nuisibles. Nous avons tiré une stratégie potentielle pour le contrôle du comportement des joints de grains par l'application de la science fondamentale des interfaces.     

AES Analysis of Ce and P Cosegregation at Grain Boundaries

The chemical state of grain boundary cosegregation of Ce and P in Fe-P-Ce alloy system was studied bymeans of Auger Electron Spectroscopy(AES).The Auger peaks of Ce segregated at grain boundaries are foundwithin the range of 60～180 eV.By comparing with the Auger spectra of the Fe-Ce-P intermetallic compound,it is supposed that there is a two-dimensional interfacial phase at grain boundaries with Ce and P cosegregationwhich is similar to the structure of the Fe-Ce-P compound.