Phase transformation studies in unirradiated and proton beam irradiated Ni–Ti alloy between 25 and 100°C

The stress-induced phase transformation characteristics of unirradiated and proton beam irradiated NiTi alloy were investigated at different tests temperatures. The wire-shaped NiTi specimens were irradiated by 2?MeV proton beam for 30?min at room temperature to a flux of 10¹⁹ protons/m² s. Engineering stress–strain (S-S) curves of both unirradiated and irradiated specimens were obtained using a materials testing machine at 25, 50, 75 and 100°C. The results indicate a single-stage phase transformation from austenite to martensite (B2–B19′) in unirraidated specimens at all the test temperatures. In contrast, in the case of the irradiated specimens, a two-stage austenite–rhombohedral–martensite (B2–R–B19′) phase transformation is observed at 25 and 50°C. The B2–R–B19′ phase transformation, however, is found to change into B2–B19′ transformation at 75 and 100°C. The stress required to initiate the B19′ phase transformation (σ_MS) and the plateau range are found to be lower in irradiated specimens compared with those of the unirradiated specimens. The results obtained are discussed on the basis of the formation of Ni₄Ti₃ precipitates in irradiated specimens and their consequences on the phase transformations.     

Characterization of aging-induced microstructural changes in M250 maraging steel using magnetic parameters

The best combinations of mechanical properties (yield stress and fracture toughness) of M250 maraging steel is obtained through short-term thermal aging (3–10 h) at 755 K. This is attributed to the microstructure containing precipitation of intermetallic phases in austenite-free low-carbon martensite matrix. Over-aged microstructure, containing reverted austenite degrades the mechanical properties drastically. Hence, it necessitates identification of a suitable non-destructive evaluation (NDE) technique for detecting any reverted austenite unambiguously during aging. The influence of aging on microstructure, room temperature hardness and non-destructive magnetic parameters such as coercivity (H_c), saturation magnetization (M_s) and magnetic Barkhausen emission (MBE) RMS peak voltage is studied in order to derive correlations between these parameters in aged M250 maraging steel. Hardness was found to increase with precipitation of intermetallics during initial aging and decrease at longer durations due to austenite reversion. Among the different magnetic parameters studied, MBE RMS peak voltage was found to be very sensitive to austenite reversion (non-magnetic phase) as they decreased drastically up on initiation of austenite reversion. Hence, this parameter can be effectively utilized to detect and quantify the reverted austenite in maraging steel specimen. The present study clearly indicates that the combination of MBE RMS peak voltage and hardness can be used for unambiguous characterization of microstructural features of technological and practical importance (3–10 h of aging duration at 755 K) in M250 grade maraging steel.     

Structure, magneto-structural transitions and magnetocaloric properties in Ni50−xMn37+xIn13 melt spun ribbons

Melt spun Ni_50−xMn_37+xIn₁₃ (2≤x≤5) ribbons were investigated for the structure, microstructure, magneto-structural transitions and inverse magnetocaloric effect (IMCE) associated with the first-order martensitic phase transition. The influence of excess Mn in Ni site (or Ni/Mn content) on the martensite transition and the associated magnetic and magnetocaloric properties are discussed. It was found that with the increase in Mn content, the martensitic transition shifted from 325 to 240 K as x is varied from 2 to 4, and the austenite phase was stabilized at room temperature. The x=5 ribbon did not show the martensitic transition. For the x=3 ribbon, the structural and magnetic transitions are close together unlike in the x=4 ribbon in which they are far (∼60 K) apart. The zero field cooled and field cooled curves support the presence of exchange bias blocking temperature due to antiferromagnetic interactions in the ribbons. A large change in the magnetization between the martensite and austenite phases was observed for a small variation in the Ni/Mn content, which resulted in large IMCE. A large positive magnetic entropy change (ΔS_M) of 32 J/kg K at room temperature (∼ 300 K) for a field change of 5 T with a net refrigeration capacity of 64 J/kg was obtained in the Ni₄₇Mn₄₀In₁₃ ribbon.     

18 MeV质子辐照对TiNi形状记忆合金R相变的影响

 研究了用HZ-B串列加速器的18MeV质子辐照对TiNi形状记忆合金R相变的影响，辐照在奥氏体母相状态下进行。示差扫描量热法（DSC）表明，辐照后R相变开始温度T^s_R和逆马氏体相变结束温度T^f_A随辐照注量的增加而降低。当注量为1.53×10¹⁴/cm²时，T^sR和T^f_A分别下降6K和13K，辐照未引起R相变结束温度T^s_R和逆马氏体相变开始温度T^f_A的变化。表明辐照后母相(奥氏体相)稳定。透射电镜（TEM）分析表明辐照后没有引起合金可观察的微观组织变化。辐照对R相变开始温度T^s_{R和逆马氏体相变结束温度Af的影响可能是由于质子辐照后产生了孤立的缺陷团，形成了局部应力场，引起晶格有序度的下降所造成的。}     

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.     

Sequence of structural and magnetic transitions in Ni48Co2Mn39Sn11 shape memory alloy

The structural and magnetic transitions in Ni₄₈Co₂Mn₃₉Sn₁₁ shape memory alloy were systematically investigated. During cooling, the paramagnetic austenite transforms into paramagnetic martensite at T_M∼375 K, followed by a gradual transition from paramagnetic to superparamagnetic martensite around T_S∼320 K. Upon further cooling through T_P∼100 K, the superparamagnetic clusters collectively freeze into a superspin glass state as corroborated by aging, rejuvenation, and memory effects. Consequently, the unique transition sequence of paramagnetic austenite→paramagnetic martensite→superparamagnetic martensite→superspin-glass martensite is disclosed.     

Characterization of martensite in Fe-25%Ni-15%Co-5%Mo alloy

Kinetic, morphological, crystallographical, magnetic and thermal characteristics of thermally induced martensite in Fe-25%Ni-15%Co-5%Mo alloy have been investigated by scanning electron microscope (SEM), transmission electron microscope (TEM), Mössbauer spectrometer, and differential scanning calorimeter (DSC). Kinetics of the transformation was found to be athermal. Also only lenticular martensite morphology was observed during microscope observations. In addition, martensite start temperature (M_s) was determined as −63 °C from differential scanning calorimeter. On the other hand, Mössbauer spectra revealed a paramagnetic character for the austenite phase and a ferromagnetic character for thermally induced martensite phase.     

Magnetocaloric effect in high Ni content Ni52Mn48−xInx alloys under low field change

Ni-rich Heusler alloys Ni₅₂Mn_48−xIn_x (x=15.5, 16 and 16.5) were prepared by the arc melting method. X-ray diffraction analysis revealed that the martensite has orthorhombic structure (S.G. Pmm2) at room temperature. The only alloy with x=15.5 has structural transmission from martensite to austenite without any magnetic transmission. The temperature dependence and the field dependence of the magnetization measurement indicated that the magnetization increased with the decreasing of the concerntration of Mn. The lesser the Mn atoms located in the In atom sites, the weaker the total AFM interaction in the system. Giant entropy changes ΔS_M(T, H) were found in Ni₅₂Mn_48−xIn_x alloys with the maximum ΔS_M value of 22.3 J kg K for the sample with x=16.5 at 270 K under the magnetic field change of 1.5 T.     

Electric and magnetic signatures of martensitic and intermartensitic transformations in Ni-Mn-Ga crystal

Results are reported on the temperature dependence of resistivity (200≤T≤360 K) and low-field magnetization (5≤T≤350 K) for the off-stoichiometric Ni₄₉Mn₂₉Ga₂₂ single crystal. Measurements are made for both heating and cooling cycles. The resistivity data show two first-order (hysteretic) transformations centered at about 340 and 250 K. The magnetization data show the same two transformations as the resistivity data as well as a third centered at 285 K. The results are consistent with a martensite/austenite transformation near 340 K and two intermartensitic transformations centered at 285 and 250 K (three martensite phases).     

Radiation forces of a focused partially coherent flattened vortex beam on a Rayleigh spherical particle

A focused partially coherent flattened vortex beam used to trap a Rayleigh dielectric spherical particle with relative refractive index p < 1 is studied. The dependence of radiation forces (RFs) on the beam order N, waist width w₀, correlation length σ₀, particle radius a and focal length f is analyzed and illustrated by numerical examples. By a suitable choice of N, w₀, σ₀ and f a stable trap of the Rayleigh particle is achievable. In particular, there exist critical values w0,c, σ_0,c for a partially coherent flattened vortex beam the particle can be trapped by the beam with w₀ less than w0,c and σ₀ larger than σ_0,c. A comparison with the previous work is made.     

Phase and electrical behaviour in the Bi14W1 − xLaxO24 − 3x/2 system

The compositional and thermal dependencies of phase and electrical behaviour of compositions in the system Bi₁₄W_1 − xLa_xO_{24 − 3x/2} (0.00 < x < 1.00) have been studied by X-ray powder diffraction, differential thermal analysis and a.c. impedance spectroscopy. The system exhibits polymorphism and phase separation, which shows both compositional and thermal dependence. Compositions with x = 0.25 and x = 0.50 exhibit a single phase tetragonal structure at room temperature. In contrast, the x = 0.75 composition at room temperature shows a mixture of a cubic phase and a secondary β-Bi₂O₃ related tetragonal phase. A full solid solution is observed at high temperatures, corresponding to the occurrence of a δ-Bi₂O₃ type phase. The appearance of the various phases correlates well with the observed electrical behaviour. The x = 0.75 composition exhibits exceptionally high conductivity at high temperatures (σ₈₀₀ = 1.34 S cm^− 1), but also shows significant phase separation at lower temperatures.     

The magnetic phase transition in titanium oxide induced by proton irradiation

We have studied the magnetic properties of ⁵⁷Fe-doped TiO₂ compounds irradiated by proton with 0, 5 and 10 pC/μm². We have observed the enhancement of the magnetic moment, measured by superconducting quantum interference device magnetometer, with increasing proton irradiation ranging from 0 to 10 pC/μm². Mössbauer spectra of proton irradiated Ti_0.99⁵⁷Fe_0.01O₂ samples were taken at room temperature. Two sites of the wing (sextet) and the central (doublet) are shown in the spectra, which suggest the magnetically ordered phase and the paramagnetic phase, respectively. With increasing proton irradiation, the part of Fe³⁺ ions was converted to Fe²⁺ ions by compensation charge. This clearly suggests that the enhancement of magnetic moment after proton irradiation is contributed to the moment by the spin-orbit coupling of Fe²⁺ ions.     

Grain oriented NiMnSn and NiMnIn Heusler alloys ribbons produced by melt spinning: Martensitic transformation and magnetic properties

We outline the microstructural, martensitic transformation and magnetic properties of Heusler alloys with starting compositions Ni₅₀Mn₃₇Sn₁₃, Ni₅₀Mn₃₆In₁₄, and Mn₅₀Ni₄₀In₁₀, produced by melt spinning. The ribbons were obtained in argon environment at a high wheel linear speed of 48 m s⁻¹ (typical dimensions: 1.2-2.0 mm in width, 4-12 mm in length, and 7-12 μm in thickness). EDS microanalysis showed that the resulting average elemental chemical composition is slightly shifted with respect to the starting one. Ribbons are fully crystalline and tend to show a highly ordered columnar-like microstructure with grains running through the entire ribbon thickness; the larger dimension of the grains is perpendicular to the ribbon plane. As-spun alloys were single-phase with ferromagnetic bcc L2₁ austenite as high-temperature parent phase. At low temperatures austenite transforms into a structurally modulated martensite with a lattice symmetry that depends on the system (7 M orthorhombic for Ni₅₀Mn₃₇Sn₁₃, 10 M monoclinic for Ni₅₀Mn₃₆In₁₄, and 14 M monoclinic for Mn₅₀Ni₄₀In₁₀). Magnetization isotherms measured in the temperature interval where martensite thermally transforms into austenite confirmed the occurrence of field-induced reverse martensitic transition in the alloys studied.     

Indentation studies on 〈1 0 0〉, 〈0 0 1〉 and 〈1 0 1〉 face of ammonium dihydrogen phosphate (ADP) single crystals: A novel nonlinear optical material

In the present work, Vickers microhardness measurements were carried out on different faces i.e. (1 0 0), (0 0 1) and (1 0 1) of ammonium dihydrogen phosphate (ADP) single crystals grown by slow evaporation solution technique at room temperature in the load ranging from 0.2 to 2 N. The obtained results show that the load independent hardness values are 0.8, 0.7 and 0.66 GPa, respectively at different faces of ADP crystal. From the crack length measurements, the fracture toughness values (K_c) was estimated using Evans and Anstis model and the present studies suggest that Evans model is more relevant when compared to Anstis model. The load variation of some mechanical properties viz. brittle index number (B_i) and yield strength (σ_y) for ADP have also been calculated for the first time.     

Martensitic transformation and magnetocaloric properties of Sn doping Mn-Ni-Ga alloys

The effects of Sn addition on phase transformation behavior and magnetocaloric properties of Mn₅₀Ni₂₅Ga_25−xSn_x (x=0, 0.1, 0.5, 1 and 2 at%) alloys were investigated in this work. The results show that the addition of Sn reduces the structural transformation temperatures. It is found that the second phase exists in the austenite matrix of the as-casted alloys at room temperature. After being annealed at 1073 K for 48 h, the precipitates totally soluted into the matrix. Magnetization measurements indicate that the saturation magnetizations of the alloys increase significantly with increase in Sn contents. In addition, the ΔM/ΔS obviously increases with increase in the Sn contents, implying the higher efficiency shift of the martensitic transformation temperature under the magnetic field.     

Charge kinetics in spinel and yttria-stabilized zirconia

Spinel and zirconia were studied by measuring the total secondary electron emission (SEE) yield σ in a dedicated scanning electron microscope (SEM) especially equipped to study the fundamental aspects of the charge trapping in insulating materials during a 1.1 keV electron irradiation at room temperature. The variation of the total SEE yield with the injected dose for both spinel and zirconia is different. In spinel the coefficient σ starts from its intrinsic value σ₀ = 4 and reaches a plateau at σ = 1 at the end of irradiation, which corresponds to the self-regulated regime. The continuity of the curves, shot after shot, proves that the trapped charges are stable and does not spread out in the material as injection proceeds. In this case spinel is called “trapper insulator”. In contrast with the spinel, σ in zirconia, never reaches unity while the injected charge increases: it evolves from its intrinsic yield σ₀ = 2.3 to a steady value a few percent above 1. The curve shows the relaxation of the positive generated charge. In this case zirconia is called “conductive insulator”. The difference in the charging kinetics of the two materials is attributed to the difference in conductivities.     

Observation of nonstationary effects in saturation spectroscopy

We have studied the nonstationary effects in saturated absorption spectroscopy of the ⁸⁷Rb D₂ line. Varying the size of the σ⁺ polarized pump laser beam, we observed saturated absorption spectra for the σ^± polarized probe beam. For equal polarizations of the pump and probe beams, we found that the resonance signal for the F_g = 1 → F_e = 2 line, and the crossover lines between F_g = 1 → F_e = 2 and F_g = 1 → F_e = 1 (and 0) lines increased to a greater extent than the others. This observation can be understood from the calculated time evolution of the populations of the ground-state sublevels by means of a rate equation model. We also compared experimental data for other conditions with the calculated results. We found good agreement between the calculated results and the data.     

Dielectric and AC ionic conductivity investigations in K3H(SeO4)2 single crystal

Optical observation under the polarizing microscope and DSC measurements on K₃H(SeO₄)₂ single crystal have been carried out in the temperature range 25-200 °C. It reveals a high-temperature structural phase transition at around 110 °C. The crystal system transformed from monoclinic to trigonal. Electrical impedance measurements of K₃H(SeO₄)₂ were performed as a function of both temperature and frequency. The electrical conduction and dielectric relaxation have been studied. The temperature dependence of electrical conductivity indicates that the sample crystal became a fast ionic conductor in the high-temperature phase. The frequency dependence of conductivity follows the Jonscher's universal dynamic law with the relation σ(ω)=σ(0)+Aωⁿ, where ω is the frequency of the AC field, and n is the exponent. The obtained n values decrease from 1.2 to 0.1 from the room temperature phase to fast ionic phase. The high ionic conductivity in the high-temperature phase is explained by the dynamical disordering of protons between the neighboring SeO₄ groups, which provide more vacant sites in the crystal.     

NiTi记忆合金中R相和马氏体相中孪晶界面的群论分析

利用母相群对低温相群陪集分解的理论,确定了NiTi形状记忆合金中R相存在四种变体,变体之间以{110}_p和{100}_p作为孪晶界面,四种变体可构成三种自适应群。马氏体相中存在三种变体,变体间的孪晶界面为{110}_p,三种变体可以构成四种呈三角形分布的自适应群。所得结果与实验工作基本一致。 关键词：     

The magnetic properties across the martensitic transition in the Co38Ni34Al28 alloy

The magnetic properties of the Co₃₈Ni₃₄Al₂₈ alloy have been studied. The alloy exhibits a first order austenite-martensite phase transition in the temperature region between 155 and 247 K. A strain of 0.07% is produced across this phase transition. The Arrott plots obtained from the isothermal magnetic field dependence of magnetization indicate the presence of spontaneous magnetization both in the austenite and martensite phases, confirming the ferromagnetic character of the alloy up to room temperature. The temperature dependence of the high field magnetization indicates the presence of spin wave excitations, spin wave excitation gap and spin wave-spin wave interactions in the martensite phase. The magnetic anisotropy energy constant for the Co₃₈Ni₃₄Al₂₈ alloy is estimated both with the help of the standard law of approach to saturation of magnetization, and also from the field dependence of magnetization using the field for technical saturation of magnetization. The temperature dependences of these energy terms are compared. The estimated values of the magnetic anisotropy constant seem to be in agreement with the magnitude of the spin wave excitation gap estimated from the temperature dependence of high field magnetization.