Annealing effect on phase transformation in nano structured Ni–Mn–Ga ferromagnetic shape memory alloy

Nano structured Ni_52.6Mn_23.7Ga_24.3 alloy was prepared using the ball milling technique. High martensitic transition temperatures are observed in the range between 336 and 367 K. The X-ray diffraction profile revealed that annealed Ni–Mn–Ga powder at 1073 K displays mixture phases of austenite and martensite. Annealing at 1173 K induces phase transformation from mixture phase to Heusler L2₁ structure, which confirms the high-temperature shape memory effect. On the contrary, the milled sample shows no evidence of shape memory effect. Furthermore, annealing at higher temperature (1273 K) shows the accumulation of oxidation, which leads to the loss of shape memory effect. The grain size increases with increasing annealing temperature and causes deterioration in the soft magnetic properties.     

Effect of Addition of Process Control Agent (PCA) on the Nanocrystalline Behavior of Elemental Silver during High Energy Milling

Mechanical Alloying (MA) or High Energy Milling has been a subject of great interest for last few decades. However, in the majority of the cases the investigations are confined to areas like alloying in binary or multi-component systems from premixed powders. Very little work has been reported on high-energy milling of pure metals. There are some reports on mechanical alloying of pure metals that undergo polymorphic transformation on milling, but relatively few papers have been reported in the literature pertaining to attrition milling of pure metals, which do not fall under this category. One such attempt has been made in this investigation by subjecting a noble metal like silver with fcc crystal structure to attrition milling. The present work deals with the investigation of the effect of addition of a process control agent (PCA) on the nanocrystalline behavior of elemental silver powder subjected to high energy milling in an attritor. Elemental silver powder was subjected to attrition milling with and without addition of stearic acid as PCA. The powder samples drawn at periodic intervals during the course of milling were subjected to characterization using techniques like XRD, SEM and DSC. The variation in particle shape morphology, crystallite size and lattice strain as a function of PCA was studied.     

Phase formation and change of magnetic properties in mechanical alloyed Ni0.5Co0.5Fe2O4 by annealing

The effects of milling time and annealing temperature on phase formation, microstructure and magnetic properties of nickel-cobalt ferrite synthesized from oxide precursors by mechanical alloying were studied. The study of milling time effects on phase formation of milled materials showed that if milling continues up to 55 h, single phase nano-sized nickel-cobalt ferrite is obtained. Also, magnetic properties of powders versus milling time and annealing at different temperatures extensively changed, so that annealing at 1200 °C increased the magnetization saturation of the as-milled powder from 15.1 to 53.6 emu/g. X-ray powder diffraction technique (XRD) with Cu-Ka radiation was employed for phase identification. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were also used to determine the morphology and size of the particles. The magnetic properties were measured by a vibration sample magnetometer (VSM).     

60keV质子辐照对TiNi记忆合金薄膜马氏体相变的影响

 利用磁控溅射的方法在氧化后的单晶Si基片上制备了TiNi形状记忆合金薄膜，利用示差扫描量热法和原位X射线衍射研究了薄膜的马氏体相变特征。通过60keV质子注入（辐照）薄膜样品研究了H+离子对合金薄膜马氏体相变特征的影响，结果表明氢离子注入后引起了马氏体相变开始Ms和结束点Mf以及逆马氏体相变开始As和结束温度Af的下降，而对R相变开始Rs和结束温度Rf影响不大。掠入射X射线衍射表明H+离子注入后有氢化物形成。H⁺离子注入形成的氢化物是引起相变点的变化的主要因素。     

Characterization of phase transformation in shape memory alloys by atomic force microscope

An atomic force microscope operated at various temperatures is introduced to evaluate phase transformation temperature and to observe microstructure for a shape memory alloy at same time in this paper. A commercial hot-rolled TiNi shape memory alloy bar is ground, polished and etched. The specimen is then observed by atomic force microscopy at the temperature range of 20–100 C in nitrogen gas. The topographies of a TiNi specimen show twinning martensite with rough surface and smooth austenite at various temperatures. The shape memory effect of the TiNi alloy is analyzed based on the shifts of the topographies obtained at various temperatures, which are used to evaluate the phase transformation temperature between martensite and austenite. The phase transformation temperature is also confirmed in a differential scanning calorimeter (DSC) experiment.     

Effect of thermo-mechanical process on structure and high temperature shape memory properties of Ti–15Ta–15Zr alloy

The effect of thermo-mechanical treatment on microstructure evolution, martensite transformation, and shape memory behavior of Ti–15Ta–15Zr high temperature shape memory alloy were investigated. Different martensite morphologies were found with different annealing temperatures. The Ti–15Ta–15Zr alloy exhibits almost perfect shape memory recovery strain of 6% after annealing at 973 K for 0.5 h.     

Transformation plasticity and shape memory effects in TiNi alloy after low-temperature treatment

The effect of low-temperature annealing on the structure, kinetics of martensitic transformations, and functional properties of an equiatomic TiNi shape memory alloy is studied. Low-temperature annealing of the TiNi alloy is shown to decrease the temperature of the end of the forward martensite transformation M _f and the temperature of the onset of the reverse transformation A _s , which increases the transformation temperature range. As a result, the shape memory effect is improved due to a decrease in the irreversible strain. These phenomena are assumed to be caused by the hardening of the TiNi alloy induced by low-temperature annealing.     

Surfactants in Mechanical Alloying/Milling: A Catch-22 Situation

Mechanical alloying/milling technique is characterized by the repeated welding and fracturing of powder particles in a high-energy ball mill, which often results in excessive cold welding and agglomeration of ductile particles. To achieve the critical balance between cold welding and fracturing, the surface of the deforming particles is modified by introducing a suitable organic material, called surfactant or process control agent (PCA). However, the use of surfactants is self-contradictory by nature and requires further consideration of the milling variables and type/amount of surfactant. The current article provides a practical approach to the promises and challenges associated with surfactants in mechanical alloying/milling. An attempt has been made to address the most crucial aspects correlated with surfactants, including contamination, the morphology and size of powder particles, formation of alloy and microstructural evolution, and powder yield, as well as the physico-mechanical properties, such as magnetism, density, hardness, and compressive strength. An overview is also given on the adsorption mechanism of surfactants onto the surface of powder particles, with a special emphasis on type, amount, and the addition time of surfactants in the mechanical alloying process.     

Powder metallurgy technology of NiTi shape memory alloy

Powder metallurgy technology was elaborated for consolidation of shape memory NiTi powders. The shape memory alloy was compacted from the prealloyed powder delivered by Memry SA. The powder shows M_s = 10°C and A_s = -34°C as results from DSC measurements. The samples were hot pressed in the as delivered spherical particle's state. The hot compaction was performed in a specially constructed vacuum press, at temperature of 680°C and pressure of 400 MPa. The alloy powder was encapsulated in copper capsules prior to hot pressing to avoid oxidation or carbides formation. The alloy after hot vacuum compaction at 680°C (i.e. within the B2 NiTi stability range) has shown similar transformation range as the powder. The porosity of samples compacted in the as delivered state was only 1%. The samples tested in compression up to ε = 0.06 have shown partial superelastic effect due to martensitic reversible transform- ation which started at the stress above 300 MPa and returned back to ε = 0.015 after unloading. They have shown also a high ultimate compression strength of 1600 MPa. Measurements of the samples temperature changes during the process allowed to detect the temperature increase above 12°C for the strain rate 10^-2 s^-1 accompanied the exothermic martensite transformation during loading and the temperature decrease related to the reverse endothermic transformation during unloading.     

AlCrFeCuNi高熵合金力学性能的分子动力学模拟

高熵合金具有传统合金无法比拟的高强度、高硬度和高耐磨耐腐蚀性,具有广阔的应用前景。为研究AlCrFeCuNi高熵合金(High entropy alloy,HEA)在轴向载荷作用下的力学性能,采用分子动力学方法,模拟高熵合金的实验制备过程并建立原子模型,研究温度和Al的含量对AlCrFeCuNi高熵合金力学性能的影响,从材料学角度分析了变形过程及其具有高塑性的原因。模拟结果表明,AlCrFeCuNi高熵合金在拉伸载荷作用下依次经历弹性、屈服、塑性3个变形阶段。在屈服阶段,开始出现孪晶和层错,孪晶和层错的产生和生长是合金产生不均匀塑性变形的主要原因之一。高熵合金的杨氏模量和屈服应力随着Al含量的增加近似线性降低,同时具有很强的温度效应,温度越低,Al含量越小,其杨氏模量和屈服应力的下降幅度越大。     

Mixing of iron with various metals by high-energy ball milling of elemental powder mixtures

The alloying of Fe with T=V, Cr and Mn by high-energy ball milling of elemental powder mixtures has been studied from the scale of a powder particle down to the atomic scale using X-ray and neutron diffraction, Mössbauer spectrometry and magnetic measurements for Fe_1?x T _x alloys with x=0.50, 0.65 for T=V, x=0.50, 0.70 for T=Cr and x=0.72 for T=Mn. Different alloying behaviours are observed according to T once powder particles have the final composition. The rather fast mechanical alloying of Fe with Mn reflects the statistical nature of the milling process in contrast to the slow mixing of Fe with V and of Fe with Cr. Hyperfine magnetic field distributions remain stationary in shape in the last milling stage at room temperature both for T=V and T=Cr. Magnetic measurements evidence the persistence with milling time of a large population of nanometer-sized Fe-Cr zones that are superparamagnetic at room temperature and at 400 K. By contrast, room-temperature Mössbauer spectra show only a single line for long milling times. The unmixed stationary state of milled p-Fe_0.7Cr_0.3 is discussed in the light of a recent model of systems driven by competing dynamics.     

Macroscale and microscale evolutions of mechanically alloyed FeZn systems

The present work aims to correlate, in time, macroscale and microscale phenomenological evolutions of the microstructure of Fe and FeZn alloys processed by mechanical milling (MM) and alloying (MA), respectively. Powders were characterized for particle size distribution (PSD), particle morphology (optical microscopy, OM, scanning electron microscopy, SEM), microhardness, crystallite size, differential scanning calometry (DSC) and transmission electron microscopy (TEM). Two macroscopic regimes of PSD behavior were distinguished: the first one dominated by the cold welding process; and, the other where both fracture and agglomeration play a significant role. Solid solubilization of Zn on bcc Fe was found to reduce the final microhardness as well as increase the lattice parameter and is very well predicted by Miedema's thermodynamical approach. Microhardness and solid solution formation kinetics were correlated in time and both could be precisely described by a logistic function. After 5 h of planetary milling, microhardness and the lattice parameter become stable as well as the PSD and particle morphology, indicating that the system has already reached steady state. Indeed, this condition can be monitored by both macroscopic and microscopic parameters. Prior to an homogeneous powder, DSC results suggest an endothermic solid-state amorphization reaction for samples processed for up to 1 h as a result of the formation of clean Fe/Zn interfaces during MA.     

Crystallization of mechanically alloyed amorphous W-Mg alloy under high pressure

Pure metal powder mixtures of W and Mg at the desired composition were milled in conventional high-energy ball mill, and amorphous alloy W₅₀Mg₅₀ was obtained after milling for 20 h. The structure evolution of elemental powder mixtures was studied following milling and subsequent high pressure and high temperature treatment. The amorphous alloy transform into a nanocrystalline material below 1050 °C at 4.0 GPa. On increasing the temperature, it transforms into a mixture of several new crystal phases under high-pressure condition. It also found that both mechanical alloying and high pressure treatment are the two necessary processes to form the nanocrystalline and the new phases.     

Synthesis, characterization, and microwave absorption properties of Fe-40 wt%Ni alloy prepared by mechanical alloying and annealing

Fe-40 wt%Ni alloys with granular shape and flake shape were prepared by a mechanical alloying (MA) and annealing method. The phase composition and morphology of the FeNi alloys, electromagnetic parameters, and microwave absorbing properties of the silicone rubber composite absorbers filled with the as-prepared FeNi alloy particles were characterized using X-ray diffraction (XRD), scanning electron microscope (SEM) and vector network analyzer. The XRD results indicate that the crystalline structures of the Fe-40 wt%Ni alloys prepared by both one-step and two-step MA processes are face-centered cubic (fcc) Ni (Fe) solid solutions, and the structures can be retained after annealing at 600 °C for 2 h. SEM images show that the FeNi alloy powders for one-step process have a granular shape; however the particles turned into flake form when they were sequentially milled with absolute ethyl alcohol. With the increase in thickness of composite absorber, the reflection loss (RL) decreases, and the peak for minimum reflection loss shifts towards the lower frequency range. Compared to the absorbers filled with the granular FeNi alloy, the absorbers filled with flaky FeNi alloys possess higher complex permittivities and permeabilities and have a lower RL and peak frequency under the same thickness. Microwave absorbing materials with a low reflection loss peak in the range of 1-4 GHz are obtained, and their microwave absorbing properties can be adjustable by changing their thicknesses.     

Magnetocaloric properties in a FeNiGaMnSi high entropy alloy

We investigated a new Fe_26.7Ni_26.7Ga_15.6Mn₂₀Si₁₁ high entropy alloy (HEA) without the rare earth element. The structural, magnetic and magnetocaloric properties of the resulting materials are presented. The HEAs successfully is produced by the arc melting with suction casting method. The crystal structures are characterised through multiphase Rietveld refinement of X-ray diffraction data. The structure of the HEAs was found to be the body centred cubic (bcc). In the magnetic measurements, the ferromagnetic to paramagnetic transition was obtained in the range of 300–400 K. With the employed suction casting method; the Fe_26.7Ni_26.7Ga_15.6Mn₂₀Si₁₁ HEA shows the best magnetocaloric properties as 1.59 Jkg⁻¹K⁻¹ maximum magnetic entropy change (0–2 T) and 75.68 Jkg^-1 refrigeration capacity after the annealing process.     

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。}     

退火诱导机械合金化Fe42.5Al42.5Ti5B10合金的结构演变与晶粒生长动力学

利用XRD和TEM方法研究Fe_42.5Al_42.5Ti₅B₁₀合金在机械合金化及等温热处理过程中的结构演变及晶粒生长动力学,讨论了机械合金化合成机理和热处理过程中的晶粒生长机理.结果表明,球磨过程中Al,Ti,B原子向Fe晶格中扩散,形成Fe(Al,Ti,B)固溶体.机械合金化合成Fe(Al,Ti,B)遵循连续扩散混合机理.球磨50h后,金属Fe,Al,Ti,B已完全合金化,球磨终产物为纳米晶Fe(Al,Ti,B).球 关键词： XRD TEM 42.5Al_42.5Ti₅B₁₀合金')" href="#">Fe_42.5Al_42.5Ti₅B₁₀合金 机械合金化     

In-situ TiC particle reinforced Ti–Al matrix composites: Powder preparation by mechanical alloying and Selective Laser Melting behavior

Mechanical alloying of Ti–Al–graphite elemental powder mixture was performed to synthesize nanocomposite powder with Ti(Al) solid solution matrix reinforced by in-situ formed TiC particles. The evolutions in phases, microstructures, and compositions of milled powders with the applied milling times were investigated. It showed that with increasing the milling time, the starting irregularly shaped powder underwent a successive change in its morphology from a flattened shape (10 h) to a highly coarsened spherical one (15 h) and, eventually, to a fine, equiaxed and uniform one (above 25 h). The prepared TiC/Ti(Al) composite powder was nanocrystalline, with the estimated average crystallite size of 12 nm and of 7 nm for Ti(Al) and TiC, respectively. Formation mechanisms behind the microstructural development of powders were elucidated. The Ti(Al) solid solution is formed through a gradual and progressive solution of Al into Ti lattice. The formation of TiC is through an abrupt, exothermic, and self-sustaining reaction between Ti and C elements. Selective Laser Melting (SLM) of as-prepared TiC/Ti(Al) composite powder was performed. The TiC particle reinforced TiAl₃ (a major phase) and Ti₃AlC₂ (a minor phase) matrix composite part was obtained after SLM. Although a slight grain growth occurred as relative to as-milled powder, the SLM processed composites still exhibited a refined microstructure.     

Mössbauer and X-ray diffraction studies of mechanically alloyed Fe-Al

Powder samples of Fe₂₅Al₇₅ were prepared by the mechanical alloying method. Mössbauer effect, X-ray diffraction and DSC measurements indicate that Fe and Al crystalline powder transform into Fe-Al amorphous powder with increasing milling time. The X-ray diffraction patterns of the milled Fe₂₅Al₇₅ do not clearly show a sign of the existence of the intermetallic phases or Fe-Al solid solution. However, Mössbauer measurements reveal two sites with hyperfine magnetic fields 30.2 and 26.0 T. These sites form locally during the milling process and then they disappear.     

Critical point of martensitic transformation under stress in an Fe-31.2Pd (at.%) shape memory alloy

We have examined the transformation strain, Δε, in the [0 0 1] direction of an Fe-31.2Pd (at.%) shape memory alloy under compressive stress applied in the same direction. When the stress is absent, the alloy exhibits a cubic to tetragonal martensitic transformation at 230 K with |Δε| of 1.4%. As the stress increases, the transformation temperature increases linearly and |Δε| decreases linearly and vanishes at 40 MPa (280 K). This point is the critical point of this transformation at which the first-order nature disappears, and the critical exponent β is evaluated to be 0.47?±?0.04.