Microstructure of martensitic phase in the Co39Ni33Al28 shape memory alloys revealed by transmission electron microscopy

In the Co₃₉Ni₃₃Al₂₈ alloy, the ferromagnetic shape memory effect was investigated. A martensitic transformation (MT) occurred in the Co₃₉Ni₃₃Al₂₈ alloy when the temperature was lower than the martensitic start transformation temperature, M_S = 233 K. The morphologies and microstructures of the martensitic phase characterized by transmission electron microscope (TEM) showed a new 28-layered (28M) modulated martensite consisting of pinstripes and co-existing with the non-modulated martensite. Anomalies in magnetic properties and strain emerging around the MT have been briefly discussed.     

Temperature memory effect of Ti50Ni30Cu20 (at.%) alloy

After the reverse thermal induced martensitic transformation process of shape memory alloy is arrested at a temperature between the reverse transformation start and finish temperatures (A_s and A_f), and then cooled to a temperature below M_f, a kinetic stop will occur in the next heat flow curve during the heating process. The kinetic stop is closely related to the arrested temperature. This phenomenon is called temperature memory effect (TME). TME of Ti₅₀Ni₃₀Cu₂₀ (at.%) shape memory alloy with phase transformation between B2 austenite and B19 martensite has been investigated by differential scanning calorimeter in this paper. The results indicate that TME of Ti₅₀Ni₃₀Cu₂₀ alloy only exists in the heating process.     

Structural changes of Co70Fe5Si10B15 amorphous alloy induced during heating

In this study we present the results on complex structural changes of the Co₇₀Fe₅Si₁₀B₁₅ amorphous alloy induced during heating in the temperature range between 20 and 1000 °C. The structural and phase transformation changes were correlated with DTA, XRD and SEM properties. It is shown that initial Co₇₀Fe₅Si₁₀B₁₅ alloy during heating undergoes complex crystallochemical changes. In the range between ambient temperature and near 400 °C, investigated alloy retains the solid-state amorphous properties. Prolonged heating induces complete transformation to crystalline solid state. The solid–solid amorphous to crystalline state transformation process is completed at 500 °C, when two nanocrystalline phase alloy systems are formed. Prolonged thermal treatment between 600 and 1000 °C, influenced further elemental segregation and phase transition. At 1000 °C, the composite material consisting of two FCC cobalt-rich alloys and a hexagonal unidentified alloy are formed.     

Effect of ageing on the microstructure and mechanical behaviour of a directionally solidified Ni3Al-based alloy

The effect of ageing in the temperature range from 1023 to 1373 K on the micro-structure and mechanical behaviour of a directionally solidified (DS) Ni₃Al-based alloy modified with additions of chromium and iron was investigated. The microstructure of the as-grown alloy consisted of well-aligned and equally spaced lamellas composed of β(B2) intermetallic compound NiAl (Cr, Fe), some β′(L1₀) martensite and spherical -Cr precipitates. The matrix consisted of γ′(L1₂) intermetallic compound Ni₃Al (Cr, Fe), γ-phase (Ni-based solid solution) and lath-shaped -Cr precipitates. Ageing at 1123 and at 1173 K was found to be the most effective in transforming the unstable lamellae to γ′-phase and -Cr precipitates. The change of microstructural characteristics such as volume fraction of lamellae, size, morphology and distribution of γ′-phase, γ-phase and -Cr precipitates significantly influenced the room-temperature yield strength and elongation of DS alloy after ageing. The strain-hardening exponent varied with the ageing temperature between 0.30 and 0.46 and the quasi-steady work-hardening rate between 2710 and 5340 MPa. In the specimens with the lowest amount of disordered regions, the strain-hardening exponent was found to be 0.46 and the quasisteady work hardening rate was determined to be 3340 MPa.     

Magnetic and electrical properties of the UCu2T3Al7 alloys

The UCu₂T₃Al₇-type compounds with T = Cr, Mn and Fe crystallize in the tetragonal ThMn₁₂-type structure (I4/mmm space group). Magnetic properties have been examined in magnetic fields up to 50 kOe in the temperature range 1.9–400 K using a SQUID magnetometer. The Cr based pseudoternary alloy is paramagnetic with the linear field dependence of the magnetization at 1.9 K. The temperature dependence of the magnetic susceptibility is described by a modified Curie–Weiss (MCW) law. The Mn containing compound is ferrimagnetic and the field dependence of the magnetization does not reach saturation while the magnetic susceptibility follows the MCW law at high temperature. The Fe alloy is ferromagnetic and at higher temperature the MCW law is fulfilled. The temperature dependence of the electrical resistivity of all materials was examined between 4.2 and 300 K showing metallic character. The Mn and Fe based compounds demonstrate some anomalies in the ρ(T) plot at low temperature. The results are discussed in relation to the anomalies observed in magnetic measurements.     

Oxidation behavior of the (Cu78Y22)98Al2 bulk metallic glass containing Cu5Y-particle composite at 400–600 °C

The oxidation behavior of the (Cu₇₈Y₂₂)₉₈Al₂ bulk metallic glass containing 55% Cu₅Y particles (CYA-composite) was studied over the temperature range of 400–600 °C in dry air. The results generally showed that the oxidation kinetics of the composite obeyed a two-stage parabolic-rate law, with its steady-state parabolic-rate constants (k_p values) increased with temperature. In addition, the oxidation rates of the composite were significantly lower than those of the polycrystalline Cu–20%Y alloy. The scales formed on the composite consisted mostly of hexagonal-Y₂O₃ (h-Y₂O₃) and minor CuO, while significant amounts of Cu₂O and CuO, with minor amounts of Y₂O₃ were detected for the Cu–20%Y alloy. It was found that the absence of Cu₂O is responsible for the slower oxidation rates of CYA-composite.     

Temperature memory effect of Ni47Ti44Nb9 wide hysteresis shape memory alloy

The temperature memory effect (TME) phenomenon of Ni₄₇Ti₄₄Nb₉ wide hysteresis shape memory alloy was studied. It was found that TME occurred during the reverse transformation for the thermally-induced martensite (TIM) but not for the stress-induced martensite after incomplete transformation cycling. The reverse transformation temperature interval of TIM can be doubly broadened after 10 incomplete transformation cycles.     

马氏体TiAl合金的热变形行为

为研究马氏体TiAl合金的热变形行为,对Ti-42.1Al-8.3V合金进行1320 ℃油淬,得到马氏体,然后利用Gleeble-1500D热模拟试验机研究了马氏体在变形温度为1000~1150 ℃、应变速率为0.001~1 s^-1下的热变形行为。利用背散射电子成像(BSE)和背散射衍射(EBSD)研究了热变形参数对TiAl合金显微组织的影响,通过分析真应力-真应变曲线,结合双曲正弦方程建立了本构方程。结果表明,马氏体TiAl合金的流变应力曲线符合动态再结晶特征,峰值应力随着变形温度的降低和应变速率的增大而增大;通过计算得到n为2.175,变形激活能Q为595.79 kJ/mol,并构建了马氏体TiAl合金的本构方程;在热变形后,TiAl合金中近等边三角形排布的马氏体转变成α₂/γ片层结构。随着变形温度的升高和应变速率的减小,α₂/γ片层逐步被再结晶晶粒替代,最后在变形温度为1100 ℃、应变速率为0.001 s^-1条件下全部转化为等轴晶。另外,随着应变速率的降低和变形温度的升高,晶粒充分长大,逐渐粗化。     

镍基合金718在H2S/CO2环境中的腐蚀行为研究

运用腐蚀失重和电化学测量技术,研究了镍基合金718在模拟苛刻油田环境中的H₂S/CO₂腐蚀行为。结果表明,在模拟高温高压H₂S/CO₂腐蚀环境中,718合金腐蚀轻微,表现出良好的抗均匀腐蚀和局部腐蚀能力。电化学测试结果表明,在模拟CO₂腐蚀环境中,718合金的阳极极化曲线存在明显的钝化区,而在模拟H₂S/CO₂腐蚀条件下的阳极极化曲线呈现多次活化-钝化转变现象,表明腐蚀产物膜的稳定性降低;EIS表明阻抗谱均有明显的容抗弧特征,不含H₂S时材料显示单一的容抗弧,加入H₂S时低频显示扩散阻抗控制,饱和CO₂溶液中718合金具有相对较大的极化电阻。     

Al25Nb20Ti30Zr25低密度高熵合金的组织和性能

通过Thermo-Calc软件计算、微观组织多尺度表征以及热模拟试验等研究了Al₂₅Nb₂₀Ti₃₀Zr₂₅合金的组织结构、高温组织稳定性和热加工性能。结果表明,Al₂₅Nb₂₀Ti₃₀Zr₂₅合金的铸锭组织主要由BCC基体相和Zr₅Al₃析出相组成,Zr₅Al₃相在BCC晶界连续析出,晶粒内部的Zr₅Al₃相呈块状分布,平均尺寸在750 nm左右;合金在750~1000 ℃保温24 h后,基体中的晶粒尺寸并未发生明显变化;随着温度的增加,Zr₅Al₃相含量小幅度降低,合金的高温组织稳定性较好。建立了合金的本构方程为$\dot{ε}$=4.5×10¹⁴×[sinh(0.0063σ_p)]^2.8exp(-419/RT),并绘制了合金的能量耗散系数图;在1050 ℃/1 s^-1变形条件下,能量耗散系数达到峰值0.69,在该变形条件下等温锻造出尺寸为$\phi$ 180 mm×20 mm完整无开裂的圆形块体材料。锻造消除了原始晶界处连续分布的Zr₅Al₃相,使其分解成短杆状均匀分布于合金基体中,BCC基体组织发生了动态回复和部分再结晶。     

Effect of thermal cycling through the martensitic transition on the internal friction and Young’s modulus of a Ni50.8Ti49.2 alloy

The internal friction (IF) and Young’s modulus (E) of a Ni_50.8Ti_49.2 is affected by thermal cycling. With increasing the number n of thermal cycles, the IF peak P_AM (P_MA) occurring at the austenite/martensite transition temperature decreases to disappear almost completely. Meanwhile the associated E(T) minimum at the beginning (n<250) deepens and then becomes progressively shallower and wider (3×10³≤n<18×10³). The strong sensitivity of P_AM (P_MA) to thermal cycling and to impurity (hydrogen) contents suggests that this peak is predominantly associated with stress-assisted collective motions of twin boundaries located inside the martensite platelets embedded within the austenite phase, rather than with the martensitic transition itself. However, as the high temperature tail of P_AM starts at temperatures appreciably higher than the martensite start-temperature M_s, a premartensitic contribution to damping is also present. The widening of the E(T) minimum indicates that, for n≥3×10³, the direct transformation is to some extent hindered by the dislocation network introduced by thermal cycling. A not thermally activated IF peak P_TWM, which is believed to be due to stress-assisted motions of (001) compound twin boundaries in the homogeneous martensite state, grows with increasing n.     

钎焊温度对Ti60合金与Si3N4陶瓷接头界面组织及性能的影响

为研究钎焊温度对Ti60/Si₃N₄接头组织与力学性能的影响,采用Ag-28Cu共晶钎料在870~910℃温度区间,保温10 min条件下进行钎焊连接.利用扫描电子显微镜、能谱仪对钎焊接头界面组织进行分析,得到的典型接头界面组织结构为Ti60/Ti-Cu化合物/Ag（s,s）+Cu（s,s）/Ti-Cu化合物/Ti₅Si₃+TiN/Si₃N₄,并对钎焊接头的组织演变过程进行了分析.结果表明,随着钎焊温度的升高,Ti60侧的Ti-Cu化合物反应层与Si₃N₄陶瓷侧的Ti₅Si₃+TiN反应层厚度逐渐增加,Ag（s,s）与Cu（s,s）含量减少,同时,扩散至Si₃N₄陶瓷侧的Ti元素与液相中Cu元素反应生成Ti-Cu化合物并在Ti₅Si₃+TiN反应层中形核.剪切测试表明,在钎焊温度880℃,保温10 min工艺参数条件下获得的接头最大抗剪强度为61.7 MPa.     

Martensitic transitions and mechanical spectroscopy of Ni50.8Ti49.2 alloy containing hydrogen

Hydrogen additions [n_H=H/(Ni+Ti)=0.003; 0.008; 0.013; 0.021; 0.029; 0.045 at.] to a Ni_50.8Ti_49.2 alloy produce several effects in the elastic and anelastic properties of the material. At temperatures between 100 and 150 K hydrogen atoms act as fixed pinning points for dislocations, as they cancel a newly observed dislocation relaxation. At low H contents (0<n_H≤0.008) the internal friction peak P_AM (P_RM) associated with austenite/martensite (A→M) or R-phase/martensite (R→M) transitions dramatically increases with increasing the H content, while the dip occurring in the Young's modulus (E) vs temperature curves becomes gradually wider and shallower. The enhancement of peak P_AM (P_RM) can be accounted for in terms of a mechanism involving the excitation of collective vibration modes (dyadons) of twin boundaries interacting with H or the stress-induced motion of parent/product interfaces. The widening of the dip in the Young's modulus is due to the introduction by H of a two-step transition (A→R→M). With increasing the H content n_H from 0.008 to 0.045 the height of peak P_AM (P_RM) decreases and a higher temperature peak (P_H) appears and progressively grows becoming the only internal friction feature for n_H=0.045. With increasing H content the thermal hysteresis in the E(T) curves occurring over the coexistence region of the A and M (R and M) phases decreases due to the inhibition caused by H of the martensitic transition. Peak P_H is most likely associated with stress-induced motion of H in solid solution within the R-phase or within a hydride.     

Microstructural evolution of Fe3B/Nd2Fe14B nanocomposite magnets microalloyed with Cu and Nb

The microalloying effect of Cu and Nb on the microstructure and magnetic properties of an Fe₃B/Nd₂Fe₁₄B nanocomposite permanent magnet has been studied by transmission electron microscopy (TEM) and atom probe field ion microscopy (APFIM). Additions of Cu are effective in refining the nanocomposite microstructure and the temperature range of the heat treatment to optimize the hard magnetic properties is significantly extended compared with that of the ternary alloy. Combined addition of Cu and Nb is further effective in reducing the grain size. Optimum magnetic properties obtained by annealing a melt-spun Nd_4.5Fe_75.8B_18.5Cu_0.2Nb₁ amorphous ribbon at 660°C for 6 min are B_r=1.25 T, H_cJ=273 kA/m and (BH)_max=125 kJ/m³. The soft magnetic Fe₂₃B₆ phase coexists with the Fe₃B and Nd₂Fe₁₄B phases in the optimum microstructure of the Cu and Nb containing quinternary alloy. Three-dimensional atom probe (3DAP) results show that the finer microstructure is due to the formation of a high number density of Cu clusters prior to the crystallization reaction, which promote the nucleation of the Fe₃B phase. The Nb atoms appear to induce the formation of the Fe₂₃B₆ phase when the remaining amorphous phase is crystallized.     

Elastic constant softening and martensite nucleation in a CuZnAl single crystal

The ultrasonic attenuation A and the elastic constants C₄₄, C_L and C′ have been measured during thermal cycles carried out above the martensite start-temperature M_s (M_s=267 K) in a single crystal of the Cu_67.93Zn_19.03Al_13.04 alloy. The ultrasonic attenuation displays a sharp maximum at a temperature which is about 6 degrees higher than M_s. This temperature difference can be accounted for either in terms of the Clausius–Clapeyron law for the martensite induced by the applied ultrasonic stress-field or in terms of premartensitic effects. Thermal hysteresis occurs for all the elastic constants C₄₄, C_L and C′ and the data are consistent with those previously obtained for the Young’s modulus in a polycrystalline alloy of the same system. The thermal hysteresis is attributed to the formation of stable nuclei of martensite at strong defects.     

Na2SiF6活性激光焊接TC4钛合金焊缝成形和组织

采用Na₂SiF₆作为表面活性剂激光焊接TC4钛合金,通过观察焊缝表面,确定了Na₂SiF₆对TC4钛合金激光焊焊缝表面成形的影响;采用高速摄像技术,观察分析了焊件上方高温光致等离子体形态特征变化;借助光学显微镜观察分析了焊缝熔深和熔宽的变化及微观组织. 结果表明,涂覆Na₂SiF₆活性剂后TC4钛合金激光焊焊缝表面成形良好,可使焊缝熔深增加约0.8% ~ 12%,焊缝表面熔宽降低约10% ~ 29%,能够有效提高焊缝的深宽比;Na₂SiF₆活性剂改善了焊缝微观组织的不均匀性,改变了焊缝上部β柱状晶的结晶方向,细化了焊缝的晶粒尺寸和微观组织.     

以Ti-Zr-Cu-Ni-Fe合金为中间层的Ti3Al/TiAl瞬间液相扩散连接

采用瞬间液相扩散焊方法,以自主设计的Ti-Zr-Cu-Ni-Fe系新型合金作为中间层,实现了Ti₃Al基合金与TiAl异种材料之间的连接.利用扫描电镜、电子探针以及X射线衍射分析等方法对接头界面微观组织和物相进行了分析.结果表明,Ti₃Al/TiAl接头主要由富Ti相、Ti₂Al反应层、α₂-Ti₃Al相以及溶入了Al元素的残余中间层组成;随着焊接温度的升高,中间层与母材的溶解与扩散变得更加强烈,使得Ti₂Al反应层厚度增加,残余中间层的数量减少.抗剪测试结果显示,焊接接温度在880~1010℃范围内时,提高焊接温度有利于接头强度的提高;接头在室温下的最大抗剪强度达到502 MPa,在500℃下为196 MPa.     

Microstructure and mechanical properties of mechanically alloyed and spark plasma sintered amorphous–nanocrystalline Al65Cu20Ti15 intermetallic matrix composite reinforced with TiO2 nanoparticles

Multiphase Al₆₅Cu₂₀Ti₁₅ intermetallic alloy matrix composite, dispersed with 10 wt.% of TiO₂ nanoparticles, has been processed by mechanical alloying, followed by spark plasma sintering under pressure in the temperature range of 623–873 K. Differential scanning calorimetry and X-ray diffraction suggest that equilibrium crystalline phases evolve from the amorphous or intermediate crystalline phases. Transmission electron microscopy shows that the composite sintered at 873 K has partially amorphous microstructure, with dispersion of equilibrium, crystalline, intermetallic precipitates of Al₅CuTi₂, Al₃Ti, and Al₂Cu of 25–50 nm size, besides the TiO₂. The composite sintered at 873 K exhibits little porosity, hardness of 5.6 GPa, indentation fracture toughness in the range of 3.1–4.2 MPa√m, and compressive strength of 1.1 GPa. Indentation crack deflection by TiO₂ particle aggregates causes increase in fracture resistance with crack length, and suggests R-curve type behaviour. The study provides guidelines for processing high strength amorphous–nanocrystalline intermetallic composites based on the Al–Cu–Ti ternary system.     

表面活化Al2O3陶瓷与5005铝合金真空钎焊

采用Al-Si钎料对经过Ag-Cu-Ti粉末活性金属化处理的Al₂O₃陶瓷与5005铝合金进行了真空钎焊,研究了钎焊接头的典型界面组织,分析了钎焊温度对接头界面结构特征及力学性能的影响. 结果表明,接头典型界面结构为5005铝合金/α-Al+θ-Al₂Cu+ξ-Ag₂Al/ξ-Ag₂Al+θ-Al₂Cu+Al₃Ti/Ti₃Cu₃O/Al₂O₃陶瓷. 钎焊过程中,Al-Si钎料与活性元素Ti及铝合金母材发生冶金反应,实现对两侧母材的连接. 随着钎焊温度的升高,陶瓷侧Ti₃Cu₃O活化反应层的厚度逐渐变薄,溶解进钎缝中的Ag和Cu与Al反应加剧,生成ξ-Ag₂Al+θ-Al₂Cu金属间化合物的数量增多,铝合金的晶间渗入明显;随钎焊温度的升高,接头抗剪强度先增加后降低,当钎焊温度为610 ℃时,接头强度最高达到15 MPa.     

Superelastic behavior of nanostructured Ti50Ni48Co2 shape memory alloy with cold rolling processing

Effects of cold rolling followed by annealing on microstructural evolution and superelastic properties of the Ti₅₀Ni₄₈Co₂ shape memory alloy were investigated. Results showed that during cold rolling, the alloy microstructure evolved through six basic stages including stress-induced martensite transformation and plastic deformation of martensite, deformation twinning, accumulation of dislocations along twin and variant boundaries in martensite, nanocrystallization, amorphization and reverse transformation of martensite to austenite. After annealing at 400 °C for 1 h, the amorphous phase formed in the cold-rolled specimens was completely crystallized and an entirely nanocrystalline structure was achieved. The value of stress level of the upper plateau in this nanocrystalline alloy was measured as high as 730 MPa which was significantly higher than that of the coarse-grained Ni₅₀Ti₅₀ and Ti₅₀Ni₄₈Co₂ alloys. Moreover, the nanocrystalline Ti₅₀Ni₄₈Co₂ alloy had a high damping capacity and considerable efficiency for energy storage.