Pct Ni Alloy Research Articles

Aluminum Deoxidation Equilibrium of Fe-Ni Alloy at 1773 K and 1873 K

The aluminum deoxidation equilibrium in molten Fe-36 mass pct Ni and Fe-46 mass pct Ni alloys was experimentally determined at 1773 K and 1873 K to obtain the thermodynamic parameters around the liquidus temperature, which is required to predict the deoxidation reaction for the ingot-casting process. Automatic SEM-EDS inclusion analysis was performed to estimate the undissolved oxygen content. Thermodynamic analysis on Al deoxidation was carried out using Miki and Hino’s formula, which is based on Darken’s quadratic formalism and the Redlich–Kister polynomial. From the composition dependence of the apparent equilibrium constant in Fe-Ni alloy, the necessity of the third-order interaction parameter of Ni-Al was found. Then, the interaction parameters of Fe-Al, Al-O and Ni-Al were evaluated.

Hydrogen Storage Characteristics of Nanocrystalline and Amorphous Nd-Mg-Ni-Based NdMg12-Type Alloys Synthesized via Mechanical Milling

In this study, Mg was partially substituted by Ni with the intent of improving the hydrogen storage kinetics performance of NdMg12-type alloy. Mechanical milling technology was adopted to fabricate the nanocrystalline and amorphous NdMg11Ni + x wt pct Ni (x = 100, 200) alloys. The effects of Ni content and milling duration on the microstructures and hydrogen storage kinetics of as-milled alloys have been systematically investigated. The structures were characterized by XRD and HRTEM. The electrochemical hydrogen storage properties were tested by an automatic galvanostatic system. Moreover, the gaseous hydrogen storage properties were investigated by Sievert apparatus and a differential scanning calorimeter connected with a H2 detector. Hydrogen desorption activation energy of alloy hydrides was estimated by using Arrhenius and Kissinger methods. The results reveal that the increase of Ni content dramatically ameliorates the gaseous and electrochemical hydrogen storage kinetics performance of the as-milled alloys. Furthermore, high rate discharge ability (HRD) reach the maximum value with the variation of milling time. The maximum HRDs of the NdMg11Ni + x wt pct Ni (x = 100, 200) alloys are 80.24 and 85.17 pct. The improved gaseous hydrogen storage kinetics of alloys via increasing Ni content and milling time can be attributed to a decrease in the hydrogen desorption activation energy.

Enhancement of Physical and Mechanical Properties of Oxide Dispersion-Strengthened Tungsten Heavy Alloys

Oxide dispersion-strengthened (ODS) tungsten heavy alloys are well known for their excellent mechanical properties which make them useful for a wide range of high-temperature applications. In this investigation, microstructural, magnetic, and mechanical properties of W-5 wt pct Ni alloys reinforced with 2 wt pct Y2O3, ZrO2 or TiO2 particles were investigated. Cold-pressed samples were sintered under vacuum at 1773 K (1500 °C) for 1 hour. The results show that, among three kinds of oxides, Y2O3 is the most efficient oxide to consolidate W powder by sintering. W-Ni-Y2O3 alloys form relatively uniform interconnected structure and also show higher density and compressive strength than those of W-Ni-ZrO2 and W-Ni-TiO2. On the other hand, W-Ni-TiO2 and W-Ni-ZrO2 alloys have non-homogeneous microstructure due to the formation of Ni globules in some areas in the matrix and almost nickel-free zones in other areas causing the appearance of pores. The Vickers hardness values for W-Ni-TiO2 alloys are slightly higher than those of W-Ni-ZrO2 and Ni-W-Y2O3 due to the smaller particle size of TiO2 than the other oxides. At room temperature, the investigated alloys have very weak magnetic properties. This is due to the combination of the ferromagnetic nickel metal binder with the non-magnetic tungsten forming the weak magnetic W-Ni solid solution. Moreover, the measured (mass) magnetizations had small values of the power of 10−3 emu/g. Additionally, the values of coercivity (H C) and remanence (M r) for the W-Ni-TiO2 alloy were higher than that of the W-Ni-Y2O3 and W-Ni-ZrO2 alloys due to the particle size effect of TiO2 nanoparticles.

Effects of Electromagnetic Stirring on the Microstructure and High-Temperature Mechanical Properties of a Hyper-eutectic Al-Si-Cu-Ni Alloy

A liquid treatment method by electromagnetic stirring was applied to a hyper-eutectic Al-15wt pctSi-4wt pctCu-3wt pctNi alloy for the piston manufacturing with diecasting process in order to improve high-temperature mechanical properties of the piston heads. The mechanical properties, such as hardness, high-temperature tensile stress, thermal expansion, and high-temperature relative wear resistance, were estimated using the specimens taken from the liquid-treated diecast products, and the results were compared with those of a conventional metal-mold-cast piston.

Effect of Water Vapor During Secondary Cooling on Hot Shortness in Fe-Cu-Ni-Sn-Si Alloys

Residual Cu in recycled steel scrap can cause hot shortness when the iron matrix is oxidized. Hot shortness can occur directly after the solid steel is formed from continuous casting as the steel undergoes a cooling process known as secondary cooling where water is first sprayed on the surface to promote cooling. This is followed by a radiant cooling stage where the steel is cooled in air to room temperature. This investigation examines the roles of water vapor, Si content, temperature, and the presence of Sn in a Fe-0.2 wt pct Cu-0.05 wt pct Ni alloy on oxidation, separated Cu and Cu induced-hot shortness during simulations of the secondary cooling process. The secondary cooling from 1473 K (1200 °C) resulted in a slight increase in liquid quantity and grain boundary penetration as compared to the isothermal heating cycles at 1423 K (1150 °C) due to the higher temperatures experienced in the non-isothermal cycle. The addition of water vapor increased the sample oxidation as compared to samples processed in dry atmospheres due to increased scale adherence, scale plasticity, and inward transport of oxygen. The increase in weight gain of the wet atmosphere increased the liquid formation at the interface in the non-Si containing alloys. The secondary cooling cycle with water vapor and the effect of Sn lead to the formation of many small pools of Cu-rich liquid embedded within the surface of the metal due to the Sn allowing for increased grain boundary decohesion and the water vapor allowing for oxidation within liquid-penetrated grain boundaries. The presence of Si increased the amount of occlusion of Cu and Fe, significantly decreasing the quantity of liquid at the interface and the amount of grain boundary penetration.

Determination of Solid Fraction from Cooling Curve

A new method to determine directly the solid fraction using the cooling curve was proposed for solidification of undercooled melts. Then, to construct three different baselines, a sudden function ξα(x) is introduced. In terms of the ξα(x) function, accordingly, the solid fractions during solidification of Ni-3.3 wt pct B, Al-7 wt pct Si, Al-14 wt pct Cu, and Fe-4.56 wt pct Ni alloys were predicted. The predictions of the primary, the regular lamellar eutectic, the anomalous eutectic, and the peritectic phases from cooling curves of the solidified samples coincide with the results of measurement or the available methods.

In-Situ Scanning Electron Microscopy/Electron Backscattered Diffraction Observation of Microstructural Evolution during α → γ Phase Transformation in Deformed Fe-Ni Alloy

This article presents in-situ observation of ferrite (α)/austenite (γ) phase transformation in an Fe-8.5 at. pct Ni alloy deformed by rolling using an automated scanning electron microscopy/energy backscattered diffraction (SEM/EBSD) system. During heating, recrystallization in α phase and α → γ phase transformation independently occurred. The γ grains nucleated in unrecrystallized α grains were most probably incorporated into the grain interior of recrystallized α grains. They did not have any specific orientation relation (OR) with recrystallized α grains and grew in an isotropic manner. On the other hand, the intragranular γ grains nucleated in recrystallized α grains had a Kurdjumov–Sachs (K-S) OR with the α grains and grew in a considerably anisotropic manner. They preferentially grew along the common direction of surface traces of {110}α/{111}γ. Approximately half of grain boundary (GB) allotriomorphs had either the K-S OR or the Nishiyama–Wasserman (N-W) OR with the parent α grains. The γ allotriomorphs predominantly grew into the α grain having the special OR with themselves. The GB character distribution of γ phase at high temperatures was measured. The fraction of CSL boundaries was as high as 63 pct, particularly that of Σ3 grain boundaries (GBs) was 54 pct.

Thermal Stability in Nanocrystalline Fe-30 Wt Pct Ni Alloy Induced by Surface Mechanical Attrition Treatment

By means of surface mechanical attrition treatment (SMAT), a nanocrystalline surface layer is produced in Fe-30 wt pct Ni alloy, accompanying the formation of the strain-induced martensite. The thermal stability of nanocrystalline martensite and parent phase austenite in Fe-30 wt pct Ni alloy is studied by X-ray diffraction (XRD) and transmission electron microscope (TEM). The grain growth kinetics parameters, time exponent, n, and activation energy, Q, for both martensite and austenite, are determined, respectively. The TEM observations indicate that abnormal grain growth occurs during annealing at high temperatures.

Microstructural Development in Al-Ni Alloys Directionally Solidified under Unsteady-State Conditions

Three Al-Ni hypoeutectic alloys were directionally solidified under upward unsteady-state heat-flow conditions. Primary (λ1) and secondary (λ2) dendrite arm spacings were measured along the castings for all alloys and correlated with transient solidification thermal variables. A combined theoretical and experimental approach was used to quantitatively determine such thermal variables, i.e., transient metal/mold heat-transfer coefficients, tip growth rates, thermal gradients, tip cooling rates, and local solidification time. The article also focuses on the dependence of dendrite arm spacings on the alloy solute content. Furthermore, the experimental data concerning the solidification of Al-1.0, 2.5, and 4.7 wt pct Ni alloys are compared with the main predictive dendritic models from the literature.

In-Situ and Real-Time Analysis of the Formation of Strains and Microstructure Defects during Solidification of Al-3.5 Wt Pct Ni Alloys

Alloy solidification was investigated in situ and real time by using a unique experimental setup developed at the European Synchrotron Radiation Facility (ESRF) combining both synchrotron X-ray radiography and topography. Although synchrotron X-ray radiography enables the investigation of the solid-liquid interface of metallic alloys, white-beam synchrotron X-ray topography enables the investigation of the formation of strains and defects formation in the growing solid microstructure. In this article, we present results obtained during directional solidification experiments performed with Al-3.5 wt pct Ni samples. First, the initial state after thermal stabilization is characterized. Next, the interface morphological instability and the transition to the columnar growth regime are thoroughly investigated. Topography observation shows that several parts of each dendrite become disoriented while the microstructure is developing. Disorientations are quantified and the aluminum yield stress at the melting point is estimated from the bending of secondary arms. Last, coupled growth of eutectic and dendrites settles with the formation of the eutectic phase. The eutectic grains grow strained and the dendrites concomitantly undergo additional stress.

Carbon Diffusion Measurement in Austenite in the Temperature Range 500 °C to 900 °C

Carbon diffusion in austenite plays a critical role in phase transformation in steel. However, it can only be estimated in the fully austenitic range and has then to be extrapolated to the temperature range of the phase transformation. Therefore, published data are limited to temperatures above 750 °C. In this study, new experiments are carried out to determine the carbon diffusion coefficient in austenite at temperatures as low as 500 °C. Carburization experiments are performed in the austenitic range for a Fe-1.5 pct Mn 0.13 pct C and a Fe-31 pct Ni alloy (wt pct). Composition profile measurements, which are done using glow discharge optical emission spectrometry (GDOES), show that the surface composition is not constant with time. A methodology has been developed to assess the diffusion coefficient of carbon in austenite combining the measured carbon profiles and a numerical method to compute the diffusion profile taking into account the time evolution of the boundary condition. This method is first validated on the Fe-C-Mn steel. Carburization experiments are carried out on a Fe-31 pct Ni alloy at 900 °C, 800 °C, 700 °C, 600 °C, and 500 °C. The carbon diffusion coefficient is assessed using the method described above and fitted with the following expression (T in Kelvin): \( D = 1.23\cdot10^{{ - 6}} \cdot e^{{ - \frac{{15,050}} {{T{\left( {\text{K}} \right)}}}}} ({\text{m}}^{{\text{2}}} {\text{/s}}) \). The new expression is compared with previous experimental results measured for comparable nickel content at higher temperatures, and it shows a reasonable agreement. The model proposed by Agren for carbon diffusion has been modified to take into account the thermodynamic contribution of nickel. This model also shows good agreement with the present experimental results, even if it was fitted to experiments performed at higher temperatures.

In-Situ and Real-Time Investigation of Columnar-to-Equiaxed Transition in Metallic Alloy

In this article, we present a review of observations during Al-3.5 wt pct Ni alloy solidification experiments performed at the European Synchrotron Radiation Facility (ESRF) in Grenoble. These experiments provide direct access to dynamical phenomena during columnar growth (initial transient and breakdown of a planar solid-liquid interface), and for the first time to the transition from columnar-to-equiaxed microstructure (nucleation ahead of a columnar front and blocking of a columnar front by an equiaxed microstructure) and fully equiaxed growth (propagation of an effective front). Based on these experimental observations, critical parameters such as columnar growth velocity variation during the transition or equiaxed-grain diameter are measured and discussed.

Nanocrystallization and magnetic properties of Fe-30 weight percent Ni alloy by surface mechanical attrition treatment

A nanostructured surface layer was formed in Fe-30 wt pct Ni alloy by surface mechanical attrition treatment (SMAT). The microstructure of the surface layer after SMAT was investigated using optical microscopy, X-ray diffraction, and transmission electron microscopy. The analysis shows that the nanocrystallization process at the surface layer starts from dislocation tangles, dislocation cells, and subgrains to highly misoriented grains in both original austenite and martensite phases induced by strain from SMAT. The magnetic properties were measured for SMAT Fe-30 wt pct Ni alloy. The saturation magnetization (M s ) and coercivity (H c ) of the nanostructured surface layers increase significantly compared to the coarse grains sample prior to SMAT. The increase of M s for SMAT Fe-30 wt pct Ni alloy was attributed to the change of lattice structure resulting from strain-induced martensitic transformation. Meanwhile, H c was further increased from residual microstress and superfined grains. These were verified by experiments on SMAT pure Ni and Co metal as well as liquid nitrogen-quenched Fe-30 wt pct Ni alloy.

Crystallography and interphase boundary of (MnS+VC) complex precipitate in austenite

Crystallography and interphase boundary of (MnS + VC) complex precipitates formed in austenite (γ) matrix are studied by transmission electron microscopy (TEM) in an austenitic Fe-36 mass pct Ni alloy containing small amounts of manganese, sulfur, vanadium, and carbon. When VC is formed directly within the γ matrix grain, it displays a cube-cube orientation relationship (OR) with respect to γ. When VC is formed on MnS, which precipitated in γ with a cube-on-edge OR, three distinctive VC/γ ORs are found: (1) \(\left( {111} \right)_\gamma \parallel \left( {001} \right)_{VC} , \left[ {1\bar 10} \right]_\gamma \parallel \left[ {1\bar 10} \right]_{VC} \), (2) the cube-cube OR, and (3) the cube-on-edge OR. The MnS/γ OR becomes irrational after γ recrystallization. When VC forms on such incoherent MnS particles, which hold irrational ORs with respect to γ matrix, a wide variety of VC/γ ORs are observed. Geometrical analysis by near coincidence site lattice (NCS) model achieves reasonable success in explanation of the observed planar facets for VC precipitates having rational ORs with respect to γ. However, as for the VC formed on the incoherent MnS with irrational ORs, there is rather poor agreement between observation and prediction.

Comparison of shape memory characteristics of a Ti-50.9 At. Pct Ni alloy aged at 473 and 673 K

The effect of aging on transformation and deformation behavior, i.e., the transformation temperatures, shape memory behavior, and multistage martensitic and R-phase transformations, was investigated for a Ti-50.9 at. pct Ni alloy aged at a low temperature ( 600 K) conventionally used for practical applications. It was found that there are many differences between aging at 473 and 673 K. The martensitic and R-phase transformation temperatures significantly varied depending on aging time and temperature. It is found that two-stage R-phase and multistage martensitic transformations appear in both the specimens aged at 473 and 673 K, respectively. The two-stage R-phase transformation appeared by aging at 473 K over 36 ks, while the multistage martensitic transformation (MSMT) appeared by aging at 673 K in the range of aging times between 1.2 and 36 ks. It is found that the critical stress for slip increases with increasing aging time in specimens aged at 473 K, while that of specimens aged at 673 K increases with increasing aging time until reaching a maximum, then it decreases with a further increase in aging time. It is also found that the critical stress for slip is superior for specimens aged at 473 K than that for specimens aged at 673 K. It was confirmed that dense and fine lenticular precipitates of about 10 nm in length were formed through aging, resulting in superior shape memory characteristics.

In-situ observed dynamics of peritectic solidification and δ/γ transformation of Fe-3 to 5 At. pct Ni alloys

The characteristics of liquid→delta ferrite and delta ferrite→gamma austenite transformation in Fe-3.50 at. pct Ni alloy, and of the peritectic solidification of Fe-4.83 and 5.01 at. pct Ni alloys, have been dynamically observed in situ with a confocal scanning laser microscope (CSLM) combined with an infrared image furnace (IIF). The unique sequence, morphologies, and rates of these transformations have been determined at a temperature gradient of 4 K/mm and growth rates of 2 to 3 µm/s, in unidirectional solidification experiments. These observations have been discussed in terms of the constitutional undercooling description of solidification theory.

Roughening of the interface between grains and liquid matrix in sintered TaC-20Ni

The grains in TaC-20 wt pct Ni alloy prepared by liquidphase sintering at 1480°C have orthorhombic shapes with flat {100} faces and sharp edges. These grains show abnormal growth. When sintered at 2020°C, the grains develop round edges and corners, and the grain growth is nearly normal. Such a grain shape change indicates that the interface between the grains and the liquid matrix undergoes roughening transition with temperature increase. The interface roughening transition is reversed when a specimen initially sintered at 2020°C is heat treated again at 1400°C.

Three-dimensional analysis and classification of grain-boundary-nucleated proeutectoid ferrite precipitates

The three-dimensional (3-D) shapes and distributions of grain-boundary-nucleated proeutectoid ferrite precipitates have been obtained by computer-aided 3-D reconstruction of serial sections of an Fe-0.12 wt pct C-3.28 wt pct Ni alloy. Isothermal transformation for short times at 650 °C was used to produce a low volume fraction of ferrite, which appeared as both Widmanstatten shapes and more-equiaxed grain-boundary precipitates. While the two-dimensional (2-D) cross sections of these precipitates appeared to fit into the previously accepted categories of precipitate morphologies, 3-D reconstructions revealed important aspects of connectivity and shape that were not observed earlier. A partially revised morphological classification based on these 3-D observations is provided here. Significant differences between the 3-D morphology of proeutectoid ferrite and that of proeutectoid cementite are also discussed, indicating (among other things) that the 3-D morphological classifications of ferrite are generally more complex than those of proeutectoid cementite.

Analysis of multistep transformations in single-crystal NiTi

The effects of composition and heat treatment on the thermally induced phase-transformation behavior of single-crystal NiTi with compositions of 50.1, 50.4, 50.8, and 51.5 at. pct Ni are presented in this article. Differential scanning calorimetry (DSC) experiments reveal that a heat-treated 50.1 at. pct Ni alloy exhibits an unprecedented multiple-step transformation (MST) on both heating and cooling, with up to four peaks. This behavior is absent in the higher-Ni-content alloys. In polycrystalline NiTi alloys, MSTs have been attributed to microstructure heterogeneities such as grain boundaries and dislocations, which influence precipitation. In-situ scanning electron microscopy (SEM) results show that the MST in the 50.1 at. pct Ni alloy is associated with single-crystal defects such as dendrites and low-angle boundaries. A heterogeneous precipitate distribution is observed in transmission electron microscopy (TEM) images of the same low-Ni alloy, also associated with the defects, creating conditions that have been shown in other studies to promote the MST in polycrystals. These MSTs are not observed for high-Ni single-crystal alloys containing the same defects. In this article, we describe the origin of the extraordinary forward and reverse MSTs in the low-Ni alloy and the absence of the MST in high-Ni alloys. Transformation sequences are proposed based on the contrasting precipitate microstructures.

The effect of severe marforming on shape memory characteristics of a Ti-rich NiTi alloy processed using equal channel angular extrusion

A Ti-49.8 at. pct Ni alloy was severely deformed at three different temperatures using equal-channel angular extrusion (ECAE). Three deformation temperatures—room temperature (below the martensite finish temperature), 50 °C (below the austenite start temperature), and 150 °C (above the austenite finish temperature)—were selected such that the initial deforming phase (B2 austenite or B19’ martensite) and the initial governing deformation mechanism (martensite reorientation, stress-induced martensitic transformation, or dislocation slip in martensite) would be different. The X-ray analysis results revealed that all processed samples mostly contained a deformed martensitic phase, regardless of the initial deforming phase and the deformation mechanism. Although the martensite start temperature did not change, the austenite start temperature decreased significantly in all deformation conditions, probably because of the effect of the internal stress field caused by the deformed microstructure. All deformation conditions led to an increase in the strength levels and some deterioration of shape-memory characteristics. However, a subsequent low-temperature annealing treatment significantly improved pseudoelastic strain levels while preserving the ultrahigh strength levels. The sample deformed at room temperature followed by the low-temperature annealing resulted in the most promising strength and shape-memory characteristics under compression, such that a 5.3 pct shape-memory strain at a 2200 MPa strength level and a 3.3 pct pseudoelastic strain at a 1900 MPa strength level were achieved. The differences between the strength levels and the shape-memory characteristics after severe deformation at different temperatures were attributed to the different amounts of plastic deformation and the resulting deformation textures, since at each deformation temperature the deformation mechanism was different. It is concluded that the severe marforming using ECAE could easily improve strength levels of NiTi alloys while preserving the shape-memory and pseudoelasticity (PE) characteristics and, thus, improve the thermomechanical fatigue behavior. However, lower deformation temperatures are necessary to hinder formation of macroshear bands, and ECAE angles larger than 90 deg should be used to reduce the amount of strain applied in one pass.