Assessment of the thermodynamic dimension of the stacking fault energy

Especially with respect to high Mn and other austenitic TRansformation and/or TWinning Induced Plasticity (TRIP/TWIP) steels, it is a current trend to model the stacking fault energy of a stacking fault that is formed by plastic deformation with an equilibrium thermodynamic formalism as proposed by Olson and Cohen in 1976. In the present paper, this formalism is critically discussed and its ambiguity is stressed. Suggestions are made, how the stacking fault energy and its relation to the formation of hexagonal ?-martensite might be treated appropriately. It is further emphasized that a thermodynamic treatment of deformation-induced stacking fault phenomena always faces some ambiguity. However, an alternative thermodynamic approach to stacking faults, twinning and the formation of ?-martensite in austenitic steels might rationalize the specific stacking fault arrangements encountered during deformation of TRIP/TWIP alloys.     

Neutron diffraction study of the plastic phases of polycrystalline SF6 and CBr4

An investigation of the plastic phases of polycrystalline specimens of sulphur hexafluoride (SF₆) and carbon tetrabromide (CBr₄) by neutron elastic scattering and neutron diffraction experiments is reported. A theory of neutron diffraction in plastic crystals, which treats the Bragg scattering and the diffuse scattering from a unified point of view, is developed and applied in the interpretation of the neutron results. The Debye-Scherrer peaks are analysed, both by a cumulant expansion technique and a cubic harmonic analysis, to determine the crystal structures of the plastic phase which are found to be body-centred cubic (space group Im3_m) for SF₆ and face-centred cubic (space group Fm3m) for CBr₄. The bond-orientation distribution function, f(Ω), has maxima in the <100> directions for SF₆ and in the <110> directions for CBr₄. Since, in both cases, f(Ω) is appreciably different from zero for all orientations, it is apparent that significant thermal reorientation takes place in both these crystals. The translational and librational displacements in CBr₄ are exceptionally large and give rise to extensive diffuse scattering which is analysed on the basis of a simple Einstein model. The model predicts that the centre-of-mass thermal vibration and the orientational disorder give approximately equal contributions to the total diffuse scattering. The calculated scattering is in good agreement with experiment for all wave vector transfers outside the range 2 to 3 Å^-1. Inside this range discrepancies occur which are interpreted as evidence for the existence of orientational short-range order in CBr₄.     

Residual stresses in biaxially fatigued austenitic stainless steel sample of cruciform geometry

A specifically designed cruciform-shaped austenitic stainless steel AISI 321 sample was subjected to ex-situ biaxial tension-compression cycling to establish ferromagnetic martensitic phase conversion under the action of plastic deformation. The time-of-flight neutron diffraction technique was employed for in-plane residual stress determination in this sample for both the austenitic and martensitic phases. The 2D data enabled determination of the macro-, micro-, hydro- and deviatoric contributions to the total phase stresses.     

Phase transformation of ZrO2 nanoparticles produced from zircon

This article focuses on the phase transformation of zirconia (ZrO₂) nanoparticles produced from zircon using a bottom-up approach. The influence of mechanical milling and thermal annealing on crystalline phase transformation of ZrO₂ nanoparticles was explored. It was found that the iron oxide, as an inherent impurity present in ZrO₂ nanoparticles, produced from zircon stabilises the cubic phase after calcination at 600°C. The stabilised cubic phase of ZrO₂ nanoparticles was disappeared and transformed into partial tetragonal and monoclinic phases after mechanical milling. The phase transformation occurred on account of the crystal defect induced by high-energy mechanical milling. The destabilisation of cubic phase into monoclinic phase was observed after the thermal annealing of ZrO₂ nanoparticles at 1000°C. The phase transitions observed are correlated to the exclusion of iron oxide from the zirconia crystal structure.     

中子衍射分析时效处理对镍基单晶高温合金相结构的影响

采用φ振荡和φ固定两种数据采集模式的中子衍射实验结果表明较高的时效温度对消除枝晶最有效,微应变(晶粒区域间的变形不协调性)主要存在于γ'相.利用中子衍射结合扫描电子显微镜对合金的微观组织形貌进行了细致观察,给出了时效温度和时间对γ'相的影响状况,超晶格测量发现了γ'相晶粒之间出现的独特取向差.由不同晶面的中子衍射结果判断时效后合金出现了轻微的四方对称性(a < c)畸变,对这种畸变起主要作用的是基体相.实验结果同时证实了不同方向的应变差异,因而为筏化驱动模型的定量 关键词： 单晶高温合金 中子衍射 超晶格 时效处理     

Baroelastic shape memory effects in titanium nickelide alloys subjected to plastic deformation under high pressure

The effects of a high pressure and torsional plastic deformation in Bridgman anvils on the structure and phase transformations in titanium nickelide-based shape memory alloys are studied by electron microscopy, neutron diffraction, and X-ray diffraction. The physical properties of the alloys are measured. It is found that the baroelastic effects related to the highly reversible B2 ? B19?? martensitic transformation can occur in metastable austenitic titanium nickelide alloys in both the standard polycrystalline and nanocrystalline states under high pressure.     

Effect of calcination temperature on phase transformation,structural and optical properties of sol–gel derived ZrO2 nanostructures

Zirconia (ZrO₂) nanostructures of various sizes have been synthesized using sol–gel method followed by calcination of the samples from 500 to 700 °C. The calcined ZrO₂ powder samples were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), Fourier-transform infra-red spectroscopy (FT-IR), UV–visible spectroscopy (UV–vis.), Raman spectroscopy (RS) and thermogravimetric analysis (TGA). The phase transformation from tetragonal (t) to monoclinic (m) was observed. The average diameter of the ZrO₂ nanostructures calcined at 500, 600 and 700 °C was calculated to be 8, 17 and 10 nm, respectively. The ZrO₂ sample calcined at 500 °C with tetragonal phase shows a direct optical band gap of 5.1 eV. The value of optical band gap is decreased to 4.3 eV for the ZrO₂ calcined at 600 °C, which contains both tetragonal (73%) and monoclinic (27%) phases. On further calcination at 700 °C, where the ZrO₂ nanostructures have 36% tetragonal and 64% monoclinic phases, the optical band gap is calculated to be 4.8 eV. The enhancement in optical band gap for ZrO₂ calcined at 700 °C may be due to the rod like shape of ZrO₂ nanostructures. The tetragonal to monoclinic phase transformation was also confirmed by analyzing Raman spectroscopic data. The TG analysis revealed that the ZrO₂ nanostructure with dominance of monoclinic phase is found to be more stable over the tetragonal phase. In order to confirm the phase stability of the two phases of ZrO₂, single point energy is calculated corresponding to its monoclinic and tetragonal structures using density functional theory (DFT) calculations. The results obtained by theoretical calculations are in good agreement with the experimental findings.     

Plasticity enhancement in 25Cr15Co hard magnetic alloy deformed in bridgman anvils

In the work, we studied the evolution of structural and mechanical properties of 25Cr15Co hard magnetic alloy under shear deformation in Bridgman anvils at different rotation angles. It is shown that at the initial stage, severe plastic strains in a highly coercive (α₁ + α₂) state are localized in shear bands, in which the α₁ and α₂ phases are dissolved and an oversaturated a solid solution is formed. As this takes place, there arises a mixed structure consisting of misoriented fragments of the (α₁ + α₂) phase surrounded by interlayers of the a solid solution. A further increase in strain degree results in a single-phase nanocrystalline structure with a grain size of about 50 nm. It is found that the dissolution of the α₁ phases in the α₂ matrix under severe plastic deformation causes an increase in the strength characteristics and plasticity of 25Cr15Co alloy at all strain degrees under study. Maximum plasticity is found in the alloy with a mixed structure consisting of submicrocrystalline and cellular sites, and formation of nanocrystalline grains causes the plasticity to decrease somewhat.     

Neutron spectroscopy study of magnons in the austenite and martensite phases of a Ni-Mn-Ga Heusler alloy

The low energy region of magnon excitations of an off-stoichiometric Ni_49.1Mn_29.4Ga_21.5 single crystal has been investigated by neutron spectroscopy. The lowest magnetic exchange stiffness constant D of 97±2 meV Å² has been found in the cubic austenite phase. In the two martensitic phases the exchange stiffness constants are significantly larger with values of 149±4 meV Å² in the tetragonal phase and 198±7 meV Å² in the low temperature martensite. The large value of D in the low temperature phase compared to the other phases cannot be explained solely by renormalization effects due to magnon-magnon interaction and is attributed to a stronger magnetic coupling. In both the martensitic phases a gap of magnon excitation at the Γ-point of about 0.2 meV was observed.     

Structural, thermal, and electrical properties of (100?x) ZrO2 (x) Bi2O3 compound

Composition (100?x) ZrO₂ (x) Bi₂O₃ (x?=?15, 20, 25) is synthesized by solid-state reaction method to study the effect of Bi₂O₃ doping on ZrO₂. The as-prepared samples are characterized by various methods. The X-ray diffraction pattern of all these samples exhibits three phases, namely, m-ZrO₂, ??_III-Bi₂O₃, and ??-Bi₂O₃. The differential thermal analysis curves do not show any phase transition/decomposition, which clearly indicated the stabilization of ??-Bi₂O₃ phase. The conductivity changes in all the samples are discussed in terms of different phase formations and their volume fractions. The microstructural and energy dispersive analyses indicate the presence of different phases. A maximum conductivity at high temperature (800?°C) was observed for the x?=?25 composition, i.e., ???=?4.21?×?10^?2 S/cm.     

Neutron quasi-elastic scattering of n-triacosane

A neutron quasi-elastic investigation on a well-orientated chain axis crystal of n-triacosane has been undertaken using the twin rotor spectrometer on the Pluto reactor at Harwell with an incident neutron wavelength of 2·64 Å. Data taken in the plastic phase show considerable quasi-elastic broadening, both perpendicular and parallel to the chain axis. Good agreement with experiment is obtained using a continuous rotation diffusion model with translational diffusion. On cooling below the plastic phase transition, slight quasi-elastic broadening isalso seen in both configurations.     

Neutron Diffraction Study of the p - T Phase Diagram for Erbium

Electrical resistivity measurements performed on a single crystal of erbium as a function of temperature and hydrostatic pressure have provided a preliminary p - T phase diagram. The results have been interpreted in terms of a model for the magnetic structures of Er deduced from neutron diffraction studies at ambient pressure. This model predicted the existence of a magnetic structure with a wave vector of Q =2/7 c * at 4.2 K, when the applied pressure is larger than 3 kbar. This paper reports a neutron diffraction study of erbium made in the temperature range of 4 to 100 K, at pressures between 0.5 and 6 kbar. We have observed the predicted suppression of the low temperature conical ferromagnetic phase and the emergence of a new phase with Q =8/33 c *. The neutron diffraction measurements has enabled us to identify the various phases that develop from the cycloidal phases previously observed at atmospheric pressure.     

Neutron scattering studies of the reentrant spin-glass system PdFeMn

Small angle neutron scattering (SANS) and inelastic neutron scattering studies were performed on a polycrystalline sample of (Pd_{9 9.65}Fe_0.35)₉₅Mn₅. This system exhibits a sequence of phase transitions from a paramagnetic to ferromagnetic state and then a transition to spin-glass-like behavior near T_SG = 3.0 K. The temperature dependence of the SANS exhibits a peak at T_c = 9.0 K and then a Q-dependent increase at low temperatures. This low temperature behavior contrasts sharply with that observed at low temperatures for a normal ferromagnet. No spin waves were observed within the ferromagnetic phase for the momenta values probed. Instead, a broad (FWHM ～ 5.0 meV) quasielastic distribution which was almost temperature independent was observed. This scattering was interpreted as a measure of the distribution of the magnetic energies of the Mn²⁺ ions.     

Mathematical modeling of the plastic deformation of a material with an FCC matrix and strengthening particles with L12 superstructure

A mathematical model of the plastic deformation of metallic materials containing a strengthening phase with L1₂-type ordering that exhibits both coherent and incoherent coupling with a matrix in various ratios is used to study the effect the scale characteristics of the strengthening phase has on the features of deformation strengthening at different temperatures and strain rates.     

Evolution of crystallization structure during deep deformation and annealing of single crystals of austenitic carbon steel

The distribution of alloying elements, impurities, and secondary phases in axial and interaxial regions was studied for single crystals of the austenitic carbon steel, 04Kh17N14M3BG2, with the classical cross-shaped dendritic structure. It was shown that the interaxial regions are enriched with chromium, molybdenum, and carbon and contain precipitates of Cr₂₃C₆ and Mo₂C. The chemical and phase inhomogeneities, connected with dendritic crystallization, are stable with respect to the effect of deep deformation and annealing, and in the finished product evolve into bands with a different content of impurities and second phase particles.Translated from Izvestiya Vysshikh Uchebnykh Zavedenii, Fizika, No. 11, pp. 62–66, November, 1991.     

Allotropic forms of carbon in the Invar Fe–Ni–C alloy before and after plastic deformation by upsetting

The effect of cold plastic deformation by upsetting (e = 1.13) on structure and hybridised bonds of carbon in the fcc Invar Fe-30.9%Ni-1.23% C alloy was studied by means of X-ray phase analysis and X-ray photoelectron spectroscopy. Carbon precipitates along grain boundaries and inside of grains in the alloy after annealing and plastic deformation were revealed. The presence of mainly sp²- and sp³-hybridised C–C bonds attributing to graphite and amorphous carbon as well as the carbon bonds with impurity atoms and metallic Fe and Ni atoms in austenitic phase were revealed in the annealed and deformed alloy. It was shown for the first time that plastic deformation of the alloy results in partial destruction of the graphite crystal structure, increasing the relative part of amorphous carbon, and redistribution of carbon between structural elements as well as in a solid solution of austenitic phase.     

Neutron laue diffraction in a weakly deformed crystal at the Bragg angles close to π/2

An essential magnification of an external force acting on a diffracting neutron for the Bragg angles θ_B close to the right one is observed. Any external action (caused by either crystal deformation or external force affected the neutron) results in a bend of the so called “Kato trajectories” inside the crystal and, for the case of a finite crystal, gives considerable variation of the intensities of both diffracted neutron beams (direct and reflected). It is shown that the magnification factor is proportional to tan² (θ_b) and can reach (10²−10³) for Bragg angles surfficiently close to 90°. The text was submitted by the authors in English.     

Dry sliding wear behaviour of magnesium oxide and zirconium oxide plasma electrolytic oxidation coated magnesium alloy

Two types of PEO coatings, one consisting of magnesium oxide (MgO) and the other comprising zirconium oxide (ZrO₂) as the main phase composition were produced on AM50 magnesium alloy from alkaline and acidic electrolytes, respectively. The ZrO₂ coating was found to be spongy and thicker with a higher roughness, whilst the relatively more compact MgO coating was having contrasting features. In the dry sliding oscillating wear tests under two different loads viz., 2 N and 5 N, the ZrO₂ coating exhibited a very poor wear resistance. The MgO coating showed an excellent resistance to sliding wear under 2 N load; however, the load bearing capacity of the coating was found to be insufficient to resist the wear damage under 5 N load. The higher specific wear rates of the MgO coating under 5 N load and that of the ZrO₂ coating under 2 N and 5 N loads were attributed to the poor load bearing capacity and a three-body-abrasive wear mechanism.     

Neutron diffraction investigation of phase separation in La2CuO4+y single crystals

La₂CuO_4+y single crystals with y=0.03 and 0.04 are investigated with a high-resolution neutron diffractometer in the temperature range 10<T<293 K. Althouogh the excess oxygen concentration y falls in the range of the dissolution gap, the crystal with y=0.03 does not undergo phase separation (PS)—the oxygen distribution in this crystal remains uniform over the entire experimental temperature interval. Macroscopic PS is observed in the crystal with y=0.04. An analysis of the dependence of the widths of the reflection orders on the interplanar separation gives the sizes of the coherent regions of the two coexisting phases: (970±30) Å in the direction of the tetragonal axis c and (1460 645) Å in the basal plane.