Stacking faults of metastable γ″ phase precipitated in an Ni-15Cr-8Fe-6Nb alloy

Abstract

The stacking faults of a metastable γ″ phase precipitated in a nickel base superalloy, a modified JIS NCF 3 type alloy (X–750M), are investigated by TEM and an X-ray diffraction method. The γ″ precipitates are circular shaped plates at the early stage of aging and they become elliptic or irregular shaped plates at the latter stage of aging at temperatures up to 1033 K. Contrast which suggests the existence of stacking faults on {112}_γ″ planes can be seen in many of the large γ″ precipitates extracted from the specimens aged at 1033 K for 36 ks or more. It is clear that the values of γ″ ?γ lattice mismatch increase with increasing aging time from the measurement of lattice constants of the γ and the γ″ phases. The formation of stacking faults on {112}_γ″ planes in the large γ″ precipitates is due to the movement of an a/6 <disp-formula><graphic href="splitsection1-m1.tif"/></disp-formula> partial dislocation introduced by γ″ ?γ coherency strain. Since a part of the stacking sequence has a similar crystal structure to that of stable δ phase precipitates in a γ″ phase, the formation of stacking faults in the γ″ precipitates is considered to be favourable for their stabilisation.     

A new type face-centered cubic zirconium phase in pure zirconium

So far,only two orientation relationships (OR) between hexagonal close-packed (HCP) (α phase) and face-centered cubic (FCC) structures in zirconium and titanium alloys have been reported.Here a new type FCC phase (named γphase) with OR:< 11(2)0 >αll< 100 >γ and {0001}αll{002}γ was observed for the first time in annealed pure zirconium by means of transmission electron microscopy (TEM) technique.The α→γphase transformation can be accomplished via expansion along[1(1)00]direction and slip of Shockley partial dislocation with 1/3[1(1)00]on (0001) basal planes.     

Isothermal decomposition of the ß′ phase in a Cu-Zn-Al alloy

The isothermal decomposition of theβ′ phase in a Cu-25 wt % Zn-6 wt % Al alloy was investigated using transmission electron microscopy and electron probe microanalysis. The ordering of theβ phase was too rapid to be suppressed during quenching from the solution annealing temperature. On ageing the alloy in the temperature range 603 to 703 K, theβ′ phase was found to decompose into a mixture of α+γ phases by the precipitation of fine and equiaxed γ-phase particles distributed uniformly throughout the matrix of α. The orientation relationship between α and γ was identified as $$\begin{gathered} (001)_\alpha ||(001)_\gamma \hfill \\ [010]_\alpha ||[010]_\gamma \hfill \\ \end{gathered} $$ The growth rate of the γ phase precipitates exhibited a maximum at 653 K. Electron probe microanalysis showed that the γ phase precipitates were enriched in aluminimum and depleted in zinc, compared to the α matrix. In addition to the uniform distribution of intragranular γ phase precipitates, heterogeneous precipitation of the α phase was observed along the grain boundaries indicative of a direct transformation ofβ′ to α in these regions: this reaction was found to be pronounced as the ageing temperature was increased up to 773 K.     

Effects of temperature and ferromagnetism on the γ-Ni/γ′-Ni3Al interfacial free energy from first principles calculations

The temperature dependencies of the γ(f.c.c.)-Ni/γ′-Ni₃Al(L1₂) interfacial free energy for the {100}, {110}, and {111} interfaces are calculated using first-principles calculations, including both coherency strain energy and phonon vibrational entropy. Calculations performed including ferromagnetic effects predict that the {100}-type interface has the smallest free energy at different elevated temperatures, while alternatively the {111}-type interface has the smallest free energy when ferromagnetism is absent; the latter result is inconsistent with experimental observations of γ′-Ni₃Al-precipitates in Ni–Al alloys faceted strongly on {100}-type planes. The γ(f.c.c.)-Ni/γ′-Ni₃Al interfacial free energies for the {100}, {110}, and {111} interfaces decrease with increasing temperature due to vibrational entropy. The predicted morphology of γ′-Ni₃Al(L1₂) precipitates, based on a Wulff construction, is a Great Rhombicuboctahedron (or Truncated Cuboctahedron), which is one of the 13 Archimedean solids, with 6-{100}, 12-{110}, and 8-{111} facets. The first-principles calculated morphology of a γ′-Ni₃Al(L1₂) precipitate is in agreement with experimental three-dimensional atom-probe tomographic observations of cuboidal L1₂ precipitates with large {100}-type facets in a Ni-13.0 at.% Al alloy aged at 823 K for 4096 h. At 823 K this alloy has a lattice parameter mismatch of 0.004 ± 0.001 between the γ(f.c.c.)-Ni-matrix and the γ′-Ni₃Al-precipitates.     

Deformation-induced α2 → γ phase transformation in TiAl alloys

Deformation-induced α₂ → γ phase transformation in high Nb containing TiAl alloys was investigated using high-resolution transmission electron microscopy (HREM) and energy dispersive X-ray spectroscopy (EDS). The dislocations appearing at the tip of deformation-induced γ plate (DI-γ) and the stacking sequence change of the α₂ matrix were two key evidences for determining the occurrence of the deformation-induced α₂ → γ phase transformation. Compositional analysis revealed that the product phase of the room-temperature transformation was not standard γ phase; on the contrary, the product phase of the high-temperature transformation was standard γ phase.     

Effect of Coiling Temperature on the Evolution of Texture in Ferritic Rolled Ti-IF Steel

The effect of coiling temperatures on the evolution of texture in Ti-IF steel during ferritic hot rolling, cold rolling and annealing was studied. It was found that texture evolution at high temperature coiling is absolutely different from that at low temperature one. The hot band texture includes a strong α-fiber as well as a weak γ-fiber after ferritic hot rolling and low temperature coiling. Both of them intensify after cold rolling and a γ-fiber with peak at {111}〈112〉 is the main texture of annealed samples. However, the main component of the hot band texture after high temperature coiling is v-fiber. After cold rolling, the intensity of γ texture reduces; α fiber （except {111}〈110〉 component） intensifies and a strong and well-proportioned γ-fiber forms in the annealed samples.     

A high-resolution-electron-microscopy study of γ/γ′-α directionally solidified eutectic alloy

A master alloy with eutectic compositions of Ni-30.26Mo-6.08Al-1.43 V (wt%) has been directionally solidified (DS) into γ/γ′-α alloy. The microstructural as-ageing treatment was studied by means of high resolution electron microscopy (HREM). A majority of α fibres still display the Bain orientation relationship with the γ′/γ matrix. In a few cases, however, the so-called Nishiyama-Wasserman (NW) orientation relationship is found in specimens aged at 850 °C for 2000 h. Different microdomain structures of the γ phase, corresponding to different ageing temperatures, were revealed. Orthorhombic Ni₃Mo phase, with a size of tens of nanometres, was found to precipitate inside α fibres after ageing at both 850 and 650 °C. Occasionally, an γ′-Ni₃Al phase with lamellar twin structure was also found to coexist with Ni₃Mo precipitate inside the α fibres. The orientation relationships between the precipitates and the α fibres were determined. Energy dispersive X-ray analysis (EDX) showed that the precipitation of Ni₃Mo and Ni₃Al is due to solid solution of Ni and Al in the α fibres.     

Cyclic deformation and lattice strain distribution of high Nb containing TiAl alloy

Low cycle fatigue of lamellar TiAl with 8.5 at.-%Nb was studied with a total strain amplitude of 0.28% at three temperatures: room temperature, 750°C and 900°C. At room temperature, the material exhibited cyclic hardening and the fracture mode was mainly interlamellar. At 750°C and 900°C, the material showed cyclic softening and the fracture mode was translamellar. The lattice strain in γ phase was almost tensile and larger tensile lattice strain in γ phase seems detrimental. Besides, the opposite direction of {201}_γ and {100}_α2 lead to crack propagation along α₂/γ interfaces. B2/β_o phase always suffered compressive lattice strain in the tests. The destruction of lamellar microstructure was the reason for colony refinement at 750°C and 900°C.     

A method for the calculation of interfacial energies in Al2O3 and ZrO2/liquid-metal and liquid-alloy systems

A method is proposed by which the interfacial energy, γ_SL, of polycrystalline solid oxides (Al₂O₃, ZrO₂) in contact with liquid metals and certain binary liquid alloys can be calculated from the values of the surface energy of the oxides, γ_SV, and the liquid metals or liquid alloys, γ_LV, respectively. According to this method, the interfacial energy depends on the geometric mean of surface interactions, (γ_SV γ_LV)^1/2, the molar volumes, V, of the solid and liquid phases, and a parameter, K, which depends on the geometric details of the oxide surface defined by the ion sites in the oxide as well as the stoichiometry of the elements in the oxide and is given by the equation, $$\gamma _{SL} = \left( {K\frac{{V_{metal} }}{{V_{oxide} }} + 1} \right)^{2/3} (\gamma _{SV} \gamma _{LV} )^{1/2}$$ The method was verified using interfacial energy data obtained by measurements of the contact angle, θ, formed between the oxides and the liquid metals and liquid alloys with the sessile drop technique. A good agreement was observed between the calculated and the experimentally estimated values of γ_SL at the melting point of the metals and alloys.     

一种4.5%Re镍基单晶合金在980℃蠕变期间的变形与损伤机制

通过蠕变性能测试和组织形貌观察,研究了一种Re含量为4.5%Re(质量分数,下同)的镍基单晶合金的高温蠕变行为、变形和损伤机制。结果表明,4.5%Re合金在980℃/300MPa的蠕变寿命为169h。蠕变初期,合金中立方γ′相转变为垂直于应力轴的N型筏状结构。稳态蠕变期间,合金的变形机制为位错在基体中滑移和攀移越过筏状γ′相。蠕变后期,合金的变形机制为位错在基体中滑移和剪切进入筏状γ′相。由于γ基体通道较窄,位错在基体通道中滑移所需的阻力较大。剪切进入γ′相的110超位错可由{111}面交滑移至{100}面,形成K-W锁,从而抑制位错的滑移和交滑移,这是合金具有较好蠕变抗力的主要原因。主/次滑移位错的交替开动,可致使筏状γ′相扭曲,并促使裂纹在筏状γ/γ′两相界面萌生;裂纹沿垂直于应力轴方向扩展,直至断裂,这是合金的蠕变断裂机制。     

Ta掺杂对γ-TiAl基合金块状组织和力学性能的影响

研究了Ti-48Al-2Nb-2Cr-xTa(x=0,1.0,2.0)(原子分数,%)合金α单相区淬火,块状组织(γ_m相)的演变规律,采用EBSD(电子背散射衍射)技术对晶粒取向进行表征。结果表明,在快速冷却条件下,微量Ta元素的添加能够促进γ_m相的析出,促进(体积分数大于50%)或者抑制(体积分数小于50%)γ_m相析出的Ta元素临界含量为2%(原子分数)。Ta元素能够细化γ_m相亚颗粒,同时,不同种类γ_m变体可直接在α₂晶粒内以BOR形核,在生长过程中发生了沿着{111}γ密排面的变体选择,使得第二代γ_m变体偏离BOR。     

GH742中γ′相和γ基体成分随时效时间和温度的变化规律研究

利用透射电镜能谱法(TEM-EDX)研究了GH742合金中γ′和γ基体两相成分随温度和时效时间的变化规律.结果表明:合金在1050℃时效时,γ′相和γ基体的成分在时效初期变化较大,当时效时间超过1440min后,γ′相和γ基体的成份基本稳定.合金在750～1100℃时效时,γ′相和γ基体的成分均随着温度的升高而发生变化,其中γ基体的成分随温度变化较明显.合金中各元素在γ′和γ两相中的偏析率Cγ′/ Cγ变化规律研究表明:Ti,Al,Nb,Ni等γ′形成元素的偏析率均随着时效温度的升高而降低,而Cr,Co,Mo等γ形成元素的偏析率均随着时效温度的升高而增大.     

Plasma nitriding response at 400 °C of the single crystalline Ni-based superalloy MC2

Plasma nitriding of MC2, a single crystalline (γ/γ′) Ni-based superalloy, was performed at 400 °C for 1 and 4 h. Owing to its monomodal γ′ particle size distribution, MC2 was used as a model material in an attempt to investigate the behavior of precipitates during the nitriding of a γ matrix. The nitrogen profiles, the morphology, and the nature of the phases in the nitrided layer were characterized by glow discharge optical emission spectroscopy, scanning electron microscopy, and X-ray diffraction. The γ matrix appeared to be nitrided similarly to the γ solid solution in austenitic stainless steels with the development of an expanded γ_N phase. The amount of nitrogen in the γ matrix varies from ~30 at.% at the surface till ~20 at.% at the interface with the non nitrided matrix. On the contrary, the γ′ precipitates accommodate no more than few at.% of nitrogen. This disparity modifies the morphology and the average γ channel width increased by ~25 %.     

Study by electrical conductivity and infrared spectrometry of the thermal stability of defective iron spinels with aluminium and chromium

Precipitation in defective chromium- or aluminium-substituted magnetites, \(\gamma - \left( {Fe_{\left( {8/3} \right) - \left( {8/9} \right)x}^{3 + } M_{\left( {8/9} \right)x}^{3 + } \square _{1/3} } \right)O_4^{2 - } \left( {M^{3 + } = Al^{3 + } ,Cr^{3 + } ;0< x< 2} \right)\) , and defective iron aluminium chromium spinels, \(\gamma - \left( {Fe_{8/9}^{3 + } Al_{\left( {8/9} \right)\left( {2 - x} \right)}^{3 + } Cr_{\left( {8/9} \right)x}^{3 + } \square _{1/3} } \right)O_4^{2 - } \) has been investigated by electrical conductivity and infrared spectrometry in the temperature range 600 to 1200° C. For highly γ-AI-substituted magnetites and γ-iron aluminium chromium spinels the transformation of the spinel lattice into an α-rhombohedral lattice has been found to be preceded by the formation of an intermediate phase at about 900° C with a high alumina content, approximately identical to disordered γ-Al₂O₃. It is only at higher temperatures (> 1100° C) that the formation of an α-rhombohedral phase is observed. In the case of γ-Cr-substituted magnetites, temperatures of only about 700° C are required for the transformation γ → α.     

The development of <100> texture in Fe-Cr-Co-Mo permanentmagnet alloys

The cold-rolled and recrystallization textures of Fe-Cr-Co-Mo permanent magnet alloys are described. The studied composition is Fe-30%Cr-15%Co-3%Mo (in wt.%). The cold-rolled texture can be considered to be {111}<110>, {111}<112>, {100}<110>, and {211}<110>, while the recrystallization texture can be considered to be {111}<100>, {110}<112>, {211}<110>, and {110}<110>. The secondary recrystallization is caused by heat-treating the alloys in the sequence of α, α+γ, α+γ+σ, α phase region. This results in a favorable texture of {110}<110> and <100> direction, aligning along the transverse direction (TD) of the strips. The best magnetic properties obtained in this study were 1.2 T (12.0 kG), iH _c=82.0 kAm^-1 (1025 Oe), and (BH)max= 60.8 kJm^-3 (7.6 MGOe) with TD alloys     

Significant effect of as-cast microstructure on texture evolution and magnetic properties of strip cast non-oriented silicon steel

In this study, two types of as-cast microstructure produced by strip casting were cold rolled and annealed to investigate the effect of initial microstructure on the textural evolution and magnetic properties of non-oriented silicon steel. The results indicated that the cold-rolled sheets of coarse-grained strip with pronounced {100} components exhibited stronger λ fiber (〈100〉//ND) and weaker γ fiber (〈111〉//ND) texture as composed to the fine-grained strip with strong Goss ({110}〈001〉) texture. After annealing, the former was dominated by η fiber (〈001〉//RD) texture with a peak at {110}〈001〉 orientation, while the latter consisted of strong {111}〈112〉 and relatively weak {110}〈001〉 texture. In addition, a number of precipitates of size ～30–150?nm restricted the grain growth during annealing, resulting in recrystallization of grain size of ～46?μm in the coarse-grained specimen and ～41?μm in the fine-grained specimen. Ultimately, higher magnetic induction (～1.72?T) and lower core loss (～4.04?W/kg) were obtained in the final annealed sheets of coarse-grained strip with strong {100} texture.     

Stability of Several Oxide Dispersion Strengthened Alloys and a directionally solidified y/y′ -α eutectic alloy in a thermal gradient

Thermal gradient testing of three oxide dispersion strengthened alloys (two Ni-base alloys, MA 754 and MA 6000E, and the Fe-base MA 956) and the directionally solidified eutectic alloy, γ/γ′-α, have been conducted. Experiments were carried out with maximum temperatures up to 1200°C and thermal gradients on the order of 100°C/mm. The oxide dispersion strengthened alloys were difficult to test because the thermal stresses promoted crack nucleation and growth; thus the ability of these alloys to maintain a thermal gradient may be limited. The stability of individual fibers in γ/γ′-α was found to be excellent; however, microstructural changes were observed in the vicinity of grain boundaries. Similar structures were also observed in isothermally annealed material; therefore thermal gradients do not affect the microstructure of γ/γ′-α in any significant manner.     

Concurrent design for NiAl-based (β/γ′) two-phase alloys by controlling microstructure and texture

Control of the crystallography of Ni₃Al(γ′) precipitates along grain boundaries of NiAl(β) was systematically studied using β bicrystals with controlled orientations. γ′ phase preferentially precipitated along β grain boundaries showing a film-like shape. The variants of γ′ precipitates were uniquely selected, which satisfies the Kurdjumov–Sachs (K–S) relation with a neighboring β grain and deviates from the relation with another adjacent β grain. In the course of tensile deformation, fracture occurred preferentially at the (β/γ′-film) interface deviating from the K–S relation and the fracture stress decreased with increasing deviation angle from the K–S relation. For improvement of the coherency at the irrational (β/γ′-film) boundaries, the control of microstructure and crystal orientation distribution in (β/γ′) two-phase polycrystals was next attempted by thermomechanical processing. After hot-compression in β phase region and subsequently annealing in (β/γ′) two-phase region, γ′ phase transformed from β phase with 〈111〉_β fiber texture satisfying the K–S relation, resulting in the formation of 〈110〉_γ′ fiber texture. In particular, a large number of (β/γ′-film) boundaries became partially coherent. This thermomechanical processing was effective in controlling the crystallography of γ′-film along β grain boundaries and leads to the harmonic design of strength and ductility for (β/γ′) two-phase alloys.     

TEM study of Mg-Zn precipitates in Mg-Zn-Y alloys

The precipitates in Mg-Zn-Y alloys in the as-cast state with nominal atomic composition of Mg₉₆Zn₁Y₃, Mg₉₆Zn₂Y₂ and Mg₉₇Zn₁Y₂ were studied by means of TEM as well as XRD techniques. The results show that there is a phase separation of Zn on the nanometer scale in these alloys. Two kinds of nano-sized precipitates were found, namely MgZn and MgZn₂. TEM observation shows that MgZn precipitates are distributed in both the Mg matrix and in Mg₂₄Y₅ grains, which is the typical precipitate in Mg-Zn-Y alloys. There is an inherent crystallographic relationship between MgZn and Mg₂₄Y₅ precipitates: // , // . The size of MgZn₂ precipitates is much smaller than that of MgZn precipitates. They are distributed only in Mg₂₄Y₅ grains, not in the Mg matrix. It is suggested that the nano-sized precipitates, MgZn and MgZn₂, can improve the mechanical properties of the Mg-Zn-Y alloys studied.     

Concurrent design for NiAl-based (β/γ′) two-phase alloys by controlling microstructure and texture

Control of the crystallography of Ni₃Al (γ′) precipitates along grain boundaries of NiAl(β) was systematically studied using β bicrystals with controlled orientations. γ′ phase preferentially precipitated along β grain boundaries showing a film-like shape. The variants of γ′ precipitates were uniquely selected, which satisfies the Kurdjumov–Sachs K–S) relation with a neighboring β grain and deviates from the relation with another adjacent β grain. In the course of tensile deformation, fracture occurred preferentially at the (β/γ′-film) interface deviating from the K–S relation and the fracture stress decreased with increasing deviation angle from the K–S relation. For improvement of the coherency at the irrational (β/γ′-film) boundaries, the control of microstructure and crystal orientation distribution in (β/γ′) two-phase polycrystals was next attempted by thermomechanical processing. After hot-compression in β phase region and subsequently annealing in (β/γ′) two-phase region, γ′ phase transformed from β phase with 〈111〉_β fiber texture satisfying the K–S relation,resulting in the formation of 〈110〉γ′ fiber texture. In particular, a large number of ′/γ′-film) boundaries became partially coherent. This thermomechanical processing was effective in controlling the crystallography of γ′-film along β grain boundaries and leads to the harmonic design of strength and ductility for (β/γ′) two-phase alloys.