Evaluation of precipitation hardening in TiC-reinforced Ti<Subscript>2</Subscript>AlNb-based alloys

Ti₂AlNb-based alloys with 0.0wt%, 0.6wt%, and 2.0wt% carbon nanotube (CNT) addition were fabricated from spherical Ti-22Al-25Nb powder by sintering in the B2 single-phase region. Phase identification and microstructural examination were performed to evaluate the effect of carbon addition on the hardness of the alloys. Carbon was either in a soluble state or in carbide form depending on its concentration. The acicular carbides formed around 1050℃ were identified as TiC and facilitated the transformation of α₂+B2 → O. The TiC was located within the acicular O phase. The surrounding O phase was distributed in certain orientations with angles of 65° or 90° O phase particles. The obtained alloy was composed of acicular O, Widmanstatten B2+O, and acicular TiC. As a result of the precipitation of carbides as well as the O phase, the hardness of the alloy with 2.0wt% CNT addition increased to HV 429±9.     

Grain boundary characteristics and tensile properties of Ti14 alloy after semi-solid deformation

The microstructure and room-temperature tensile properties of Ti14, a new α+Ti₂Cu alloy, were investigated after conventional forging at 950℃ and semi-solid forging at 1000 and 1050℃, respectively. Results show that coarse grains and grain boundaries are obtained in the semi-solid alloys. The coarse grain boundaries are attributed to Ti₂Cu phase precipitations occurred on the grain boundaries during the solidification. It is found that more Ti₂Cu phase precipitates on the grain boundaries at a higher semi-solid forging temperature, which forms precipitated zones and coarsens the grain boundaries. Tensile tests exhibit high strength and low ductility for the semi-solid forged alloys, especially after forging at 1000℃. Fracture analysis reveals the evidence of ductile failure mechanisms for the conventional forged alloy and cleavage fracture mechanisms for the alloy after semi-solid forging at 1050℃.     

Influence of hot-rolling on the microstructure and mechanical properties of a near β-type Ti-5.2Mo-4.8Al-2.5Zr-1.7Cr alloy

In this work, the 90° clock rolling and the uni-directionally rolling processes at high temperature were carried out on the near β-type Ti-5.2Mo-4.8Al-2.5Zr-1.7Cr titanium alloy cutting from an ingot, respectively. The corresponding microstructures were quantitatively characterized, and its effect on the dynamic mechanical properties and fracture mechanism were emphatically investigated. It was found that after 90° clock rolling, the microstructure composed of equiaxed primary α phase(α_p) with an average size of about 2 ?μm and the β transformed regions containing the acicular secondary α phase(α_s) with an average thickness of about 50 ?nm and the separated β phase was obtained. However, in the uni-directionally rolled titanium alloy, no acicular α_s was observed, and the corresponding microstructure consisted elongated lamellar α phase (average thickness: about 1.3 ?μm), few equiaxed α phase (average grain size: about 300 ?nm) and the inlaid β phase. The microstructural difference of the hot-rolled titanium alloys was closely related to the deformation process. Moreover, a great number of α_p and α_s in the 90° clock rolled titanium alloy effectively enhanced the strength, and the dynamic compressive strength reached to 1730 ?MPa. Furthermore, equiaxed α_p was conducive to the homogeneous deformation, which counteracted the localized deformation caused by acicular α_s to a certain extent and made the 90° clock rolled titanium alloy exhibit an acceptable critical fracture strain of about 10.5%. Moreover, the fracture microstructures showed that the main failure mode of the 90° clock rolled and the uni-directionally rolled titanium alloy were ductile fracture and brittle fracture, respectively.     

Microstructure evolution and mechanical properties of Ti_2AlNb/TiAl brazed joint using newly-developed Ti–Ni–Nb–Zr filler alloy

Joining of Ti_2AlNb alloy to TiAl intermetallics was conducted by the newly-developed Ti–Ni–Nb–Zr brazing filler alloy.The microstructure evolution of the joints was investigated by scanning electron microscope (SEM),energy dispersive spectrometer (EDS) and electron backscatter diffraction (EBSD).The macro-micro mechanical properties were studied by shear test and nano-indentation test.Typical interfacial microstructures across the brazing seam were Ti_2AlNb substrate,α_2-Ti_3Al+β-Ti,γ-TiAl+Ti_2Ni+TiNi+α_2-Ti_3Al,α_2-Ti_3Al+β-Ti,TiAl substrate.The Ti_2Ni phase were firstly dissolved in the joints brazed at 1000°C for 10 min and then precipitated after a prolonged holding time of 15 min.The nano-indentation test revealed that Ti_2Ni phase exhibited the highest hardness of 12.60 GPa.The joints brazed at 1000°C/15 min presented the maximum shear strength of271 MPa.The dissolution and precipitation behavior of Ti_2Ni phase was also discussed.     

Formation mechanism of interfacial microstructures and mechanical properties of Ti2AlNb/Ni-based superalloy joints brazed with NiCrFeSiB filler metal

Dissimilar brazing of Ti₂AlNb-based alloy and Ni-based wrought superalloy (GH536) was studied using NiCrFeSiB filler metal. The Ti₂AlNb/GH536 joints were analyzed by scanning electron microscope (SEM) equipped with an electron probe micro-analyzer (EPMA), X-ray diffraction (XRD) and transmission electron microscopy (TEM). The formation mechanism of interfacial microstructure and mechanical properties of Ti₂AlNb/GH536 joints were studied. The results indicated that Ti₂Ni(Al,Nb), AlNi₂Ti and TiB₂ reaction layers were formed in the joint adjacent to Ti₂AlNb base metal. These layers resulted in high micro-hardness and the weak link of the joint. γ solid solution was formed through isothermal solidification and β₁-Ni₃Si phase precipitated in the γ solid solution during cooling process. Ni₃B, β₁-Ni₃Si and CrB phases appeared in the centre of the joint. Blocky and needle-like borides formed within the diffusion affected zone of GH536 base alloy. The maximum tensile strength of Ti₂AlNb/GH536 joints reached 425 ?MPa ?at room temperature and the strength value of 373 ?MPa was maintained at 923 ?K.     

The giant magnetocaloric effect in Gd<Subscript>5</Subscript>Si<Subscript>2</Subscript>Ge<Subscript>2</Subscript> with low purity gadolinium

The giant magnetocaloric effect Gd5Si2Ge2 alloy was prepared with 99wt% low purity commercial Gd. Powder XRD and magnetic measurements showed that the Gd5Si2Ge2 alloy annealed at 1200℃ for 1h had a significant magnetic- crystallographic first order phase transition at about 270 K. The maximal magnetic entropy change is 17.55 J· kg^-1· K^-1 under a magnetic field change of 0-5 T. The distinct increase of magnetic entropy change belongs to the first-order phase transition from the orthorhombic Gd5Si4-type to the monoclinic Gd5Si2Ge2-type after high temperature heat-treatment.     

静态再结晶处理对Co36Fe36Cr18Ni8Ti2合金力学性能与耐腐蚀性的影响

对冷变形后的Co₃₆Fe₃₆Cr₁₈Ni₈Ti₂合金在700 ℃和800 ℃下再结晶退火,制备成具有高强度及良好耐蚀性的多主元合金。采用电子背散射衍射（electron back-scattered diffraction, EBSD）表征了合金的相分布、再结晶组织以及晶界分布等微观结构特征,采用静态拉伸试验测试了合金的力学性能。结果表明,700 ℃退火的合金断后伸长率较低,但其抗拉强度与屈服强度分别达到了1 038和956 MPa。采用电化学工作站与扫描电子显微镜（scanning electron microscope, SEM）表征了合金在模拟体液中的耐蚀性。结果表明,700 ℃退火的样品具有较好的耐蚀性,腐蚀后的样品表面较为均匀。结合力学性能可知,700 ℃退火的样品具有作为新型医用金属材料的潜力。     

Microstructure and properties of Ag–Ti3SiC2 contact materials prepared by pressureless sintering

Ti₃SiC₂-reinforced Ag-matrix composites are expected to serve as electrical contacts. In this study, the wettability of Ag on a Ti₃SiC₂ substrate was measured by the sessile drop method. The Ag–Ti₃SiC₂ composites were prepared from Ag and Ti₃SiC₂ powder mixtures by pressureless sintering. The effects of compacting pressure (100–800 MPa), sintering temperature (850–950℃), and soaking time (0.5–2 h) on the microstructure and properties of the Ag–Ti₃SiC₂ composites were investigated. The experimental results indicated that Ti₃SiC₂ particulates were uniformly distributed in the Ag matrix, without reactions at the interfaces between the two phases. The prepared Ag–10wt%Ti₃SiC₂ had a relative density of 95% and an electrical resistivity of 2.76×10-3 mΩ·cm when compacted at 800 MPa and sintered at 950℃ for 1 h. The incorporation of Ti₃SiC₂ into Ag was found to improve its hardness without substantially compromising its electrical conductivity; this behavior was attributed to the combination of ceramic and metallic properties of the Ti₃SiC₂ reinforcement, suggesting its potential application in electrical contacts.     

Microstructure and mechanical properties of spark plasma sintered Ti-Mo alloys for dental applications

Ti-Mo alloys with various Mo contents from 6wt% to 14wt% were processed by spark plasma sintering based on elemental powders. The influence of sintering temperature and Mo content on the microstructure and mechanical properties of the resulting alloys were investigated. For each Mo concentration, the optimum sintering temperature was determined, resulting in a fully dense and uniform microstructure of the alloy. The optimized sintering temperature gradually increases in the range of 1100–1300℃ with the increase in Mo content. The microstructure of the Ti-(6–12)Mo alloy consists of acicular α phase surrounded by equiaxed grains of β phase, while the Ti-14Mo alloy only contains single β phase. A small amount of fine α lath precipitated from β phase contributes to the improvement in strength and hardness of the alloys. Under the sintering condition at 1250℃, the Ti-12Mo alloy is found to possess superior mechanical properties with the Vickers hardness of Hv 472, the compressive yield strength of 2182 MPa, the compression rate of 32.7%, and the elastic modulus of 72.1 GPa. These results demonstrate that Ti-Mo alloys fabricated via spark plasma sintering are indeed a perspective candidate alloy for dental applications.     

Preparation of Al<Subscript>72</Subscript>Ni<Subscript>8</Subscript>Ti<Subscript>8</Subscript>Zr<Subscript>6</Subscript>Nb<Subscript>3</Subscript>Y<Subscript>3</Subscript> amorphous powders and bulk materials

Amorphous Al₇₂Ni₈Ti₈Zr₆Nb₃Y₃ powders were successfully fabricated by mechanical alloying. The microstructure, glass-forming ability, and crystallization behavior of amorphous Al₇₂Ni₈Ti₈Zr₆Nb₃Y₃ powders were investigated by X-ray diffraction (XRD), transmission electron microscopy (TEM), and differential scanning calorimetry (DSC). The isothermal crystallization kinetics was analyzed by the Johnson–Mehl–Avrami equation. In the results, the supercooled liquid region of the amorphous alloy is as high as 81 K, as determined by non-isothermal DSC curves. The activation energy for crystallization is as high as 312.6 kJ·mol?1 obtained by Kissinger and Ozawa analyses. The values of Avrami exponent (n) imply that the crystallization is dominated by interface-controlled three-dimensional growth in the early stage and the end stage and by diffusion-controlled two- or three-dimensional growth in the middle stage. In addition, the amorphous Al₇₂Ni₈Ti₈Zr₆Nb₃Y₃ powders were sintered under 2 GPa at temperatures of 673 K and 723 K. The results show that the Vickers hardness of the compacted powders is as high as Hv 1215.     

Deformation and damage behaviors of as-cast TiAl-Nb alloy during creep

By means of creep properties measurement and microstructure observation,the deformation and damage behavior of an as-cast TiAl-Nb alloy during creep at temperature near 750°C were investigated.The results showed that the microstructure of the alloy consisted of lamellarγ/α_2 phase,and the boundaries consisted ofγphase located in between lamellarγ/α_2 phases with different orientations.In the latter stage of creep,the dislocation networks appeared in the interfaces of lamellarγ/α_2 phases due to the coarsening of them,which made the coherent interface transforming into the semi-coherent one for reducing its adhesive strength.The deformation mechanism of the alloy during creep was twinning and dislocations slipping within lamellarγ/α_2 phases.In the later period of creep,significant amount of dislocations plied up in the interfaces of lamellarγ/α_2 phases,which may cause the stress concentration to promote the initiation and propagation of the cracks along the lamellarγ/α_2interfaces perpendicular to the stress axis.Wherein,some cracks on the various cross-sections were connected by tearing edge along the direction of maximum shear stress,up to the creep fracture,which is considered to be the damage and fracture mechanism of alloy during creep at 750°C.     

Oxidation behavior of the Fe-36Al-0.09C-0.09B-0.04Zr alloy at 1250°C

To explore and study the Fe-Al system alloy presenting exceptional oxidation resistance at high temperature, the Fe-36Al-0.09C-0.09B-0.04Zr alloy was designed and developed. The microstructure and hardness of the backing at 1250°C were analyzed and measured. Thermodynamics and kinetics of the oxidation behavior were also analyzed by X-ray diffraction, scanning electron microscopy, and energy-dispersive X-ray spectroscopy techniques. The results show that the microstructure of the Fe-36Al-0.09C-0.09B-0.04Zr alloy is FeAl phase at ambient temperature and is stable at 1250°C. It displays the excellent property of oxidation resistance because the oxide film has only the Al₂O₃ layer, and its oxidation kinetics curve obeys the parabolic law at 1250°C. The oxidation mechanism at 1250°C is presumed that in the early oxidation period, the alloy oxidizes to form a large number of Al₂O₃ and a little Fe₂O₃, then, the enrichment of Al caused by Fe oxidization combines with O to form Al₂O₃.     

Effect of CO<Subscript>2</Subscript> and H<Subscript>2</Subscript>O on gasification dissolution and deep reaction of coke

To more comprehensively analyze the effect of CO₂ and H₂O on the gasification dissolution reaction and deep reaction of coke, the reactions of coke with CO₂ and H₂O using high temperature gas-solid reaction apparatus over the range of 950-1250℃ were studied, and the thermodynamic and kinetic analyses were also performed. The results show that the average reaction rate of coke with H₂O is about 1.3-6.5 times that with CO₂ in the experimental temperature range. At the same temperature, the endothermic effect of coke with H₂O is less than that with CO₂. As the pressure increases, the gasification dissolution reaction of coke shifts to the high-temperature zone. The use of hydrogen-rich fuels is conducive to decreasing the energy consumed inside the blast furnace, and a corresponding high-pressure operation will help to suppress the gasification dissolution reaction of coke and reduce its deterioration. The interfacial chemical reaction is the main rate-limiting step over the experimental temperature range. The activation energies of the reaction of coke with CO₂ and H₂O are 169.23 kJ·mol-1 and 87.13 kJ·mol-1, respectively. Additionally, water vapor is more likely to diffuse into the coke interior at a lower temperature and thus aggravates the deterioration of coke in the middle upper part of blast furnace.     

Effects of aging treatment on the microstructure and superelasticity of columnar-grained Cu<Subscript>71</Subscript>Al<Subscript>18</Subscript>Mn<Subscript>11</Subscript> shape memory alloy

The effect of aging treatment on the superelasticity and martensitic transformation critical stress in columnar-grained Cu₇₁Al₁₈Mn₁₁ shape memory alloy (SMA) at the temperature ranging from 250°C to 400°C was investigated. The microstructure evolution during the aging treatment was characterized by optical microscopy, scanning electron microscopy, transmission electron microscopy, and X-ray diffraction. The results show that the plate-like bainite precipitates distribute homogeneously within austenitic grains and at grain boundaries. The volume fraction of bainite increases with the increase in aging temperature and aging time, which substantially improves the martensitic transformation critical stress of the alloy, whereas the bainite only slightly affects the superelasticity. This behavior is attributed to a coherent relationship between the bainite and the austenite, as well as to the bainite and the martensite exhibiting the same crystal structure. The variations of the martensitic transformation critical stress and the superelasticity of columnar-grained Cu₇₁Al₁₈Mn₁₁ SMA with aging temperature and aging time are described by the Austin–Rickett equation, where the activation energy of bainite precipitation is 77.2 kJ·mol?1. Finally, a columnar-grained Cu₇₁Al₁₈Mn₁₁ SMA with both excellent superelasticity (5%–9%) and high martensitic transformation critical stress (443–677 MPa) is obtained through the application of the appropriate aging treatments.     

Micro-arc oxidization fabrication and ethanol sensing performance of Fe-doped TiO<Subscript>2</Subscript> thin films

In-situ pure TiO₂ and Fe-doped TiO₂ thin films were synthesized on Ti plates via the micro-arc oxidation (MAO) technique. The as-fabricated anatase TiO₂ thin film-based conductometric sensors were employed to measure the gas sensitivity to ethanol. The results showed that Fe ions could be easily introduced into the MAO-TiO₂ thin films by adding precursor K₄(FeCN)₆·3H₂O into the Na₃PO₄ electrolyte. The amount of doped Fe ions increased almost linearly with the concentration of K₄(FeCN)₆·3H₂O increasing, eventually affecting the ethanol sensing performances of TiO₂ thin films. It was found that the enhanced sensor signals obtained had an optimal concentration of Fe dopant (1.28at%), by which the maximal gas sensor signal to 1000 ppm ethanol was estimated to be 7.91 at 275°C. The response time was generally reduced by doped Fe ions, which could be ascribed to the increase of oxygen vacancies caused by Fe³⁺ substituting for Ti⁴⁺.     

Work toughening effect in Zr_（41）Ti_（14）Cu_（12.5）Ni_（10）Be_（22.5） bulk metallic glass

Work hardening is a well-known phenomenon occurring in crystalline metals during deformation,which has been widely used to increase the strength of metals although their ductility is usually reduced simultaneously. Here we report that the plastic strain of Zr41Ti14Cu12.5Ni10Be22.5 (at.%) bulk metallic glasses has been increased from 0.3% for the as-cast sample to 2.5%-8.0% for samples that have experienced pre-deformation under constrained conditions. The pre-deformed glassy alloys possess more free volume and abundant introduced shear bands,which are believed to promote the activation of shear bands in post-deformation and result in an increase in plasticity. The orientation of the pre-introduced shear bands relative to the loading direction will affect the deformation behavior of pre-deformed samples. The present results show that pre-deformation of this glassy alloy will result in work toughening. This work toughening effect can be removed by isothermal annealing at a sub-Tg (glass transition) temperature,which causes annihilation of free volume and healing of shear bands.     

Microwave sintering of Ca<Subscript>0.6</Subscript>La<Subscript>0.2667</Subscript>TiO<Subscript>3</Subscript> microwave dielectric ceramics

Ca_0.6La_0.2667TiO₃ ceramics were prepared by conventional and microwave sintering techniques and their sinterability, microstructure, and microwave dielectric properties were investigated in detail for comparison. Densified Ca_0.6La_0.2667TiO₃ ceramics were obtained by microwave sintering at 1350°C for 30 min and by conventional sintering at 1450°C for 4 h. An unusual phenomenon was found that some larger grains (grain size range: 8–10 μm) inclined to assemble in one area but some smaller ones (grain size range: 2–4 μm) inclined to gather in another area in the microwave sintered ceramics. The microwave dielectric properties of Ca_0.6La_0.2667TiO₃ ceramics prepared by microwave sintering at 1350°C were as follows: dielectric constant (ɛ _r) = 119.6, quality factor (Qf) = 17858.5 GHz, and temperature coefficient of resonant frequency (τ _f) = 155.5 ppm/°C. In contrast, the microwave dielectric properties of the ceramics prepared by conventional sintering at 1450°C were ɛ _r = 117.4, Qf = 13375 GHz, and τ _f = 217.2 ppm/°C.     

Fabrication and properties of aluminum silicate fibrous materials with <Emphasis Type="Italic">in situ</Emphasis> synthesized K<Subscript>2</Subscript>Ti<Subscript>6</Subscript>O<Subscript>13</Subscript> whiskers

To improve their mechanical and thermal insulation properties, aluminum silicate fibrous materials with in situ synthesized K₂Ti₆O₁₃ whiskers were prepared by firing a mixture of short aluminum silicate fibers and gel powders obtained from a sol-gel process. During the preparation process, the fiber surface was coated with K₂Ti₆O₁₃ whiskers after the fibers were subjected to a heat treatment carried out at various temperatures. The effects of process parameters on the microstructure, compressive strength, and thermal conductivity were analyzed systematically. The results show that higher treatment temperatures and longer treatment durations promoted the development of K₂Ti₆O₁₃ whiskers on the surface of aluminum silicate fibers; in addition, the intersection structure between whiskers modulated the morphology and volume of the multi-aperture structure among fibers, substantially increasing the fibers' compressive strength and reducing their heat conduction and convective heat transfer at high temperatures.     

Synthesis and Magnetic Properties of Spin-Liquid Tb2Ti2O7

Polycrystalline samples of a novel spin-liquid compound Tb2Ti2O7 were prepared by a standard solid-state reaction. X-ray diffraction at room temperature confirms that the synthesized compound of Tb2Ti2O7 is single phase with cubic unit cell constant a0 of 1.015 44 nm. Magnetic susceptibility measurements in the temperature range between 100 and 300 K give an effective moment of 9.44 μB and Curie-Weiss temperature of 12.68 K, respectively, indicating the dominance of antiferromagnetic interactions. However, below 50 K, the magnetic behavior of Tb2Ti2O7 deviates from Curie-Weiss law, whose origin remains suspicion.     

The electrical property of MnCo<Subscript>2</Subscript>O<Subscript>4</Subscript> and its application for SUS 430 metallic interconnect

The conductivity of MnCo₂O₄ spinel, the best route to form the MnCo₂O₄ protective coating applied by the sol-gel process, and its effect on the intermediate temperature oxidation behavior of SUS 430 alloy, a typical material for the interconnect of solid oxide fuel cell (SOFC), was investigated. The phase structure and surface morphology of the coating and surface oxides were characterized by XRD, SEM and EDS; the “4-probe” method was employed to determine the conductivity of MnCo₂O₄ spinel and the area specific resistance (ASR) of the surface oxides. The conductivity of MnCo₂O₄ spinel is excellent, which is 2 orders of magnitude better than that of MnCr₂O₄ spinel. Long-term thermally cyclic oxidation at 750°C in SOFC cathode atmosphere and ASR measurement have shown that calcined in reducing atmosphere followed by pre-oxidation in the air is the best technique for forming the MnCo₂O₄ protective coating, which enhances the oxidation resistance, and improves the electrical conductivity and adherence of coated SUS 430 alloy significantly. As a result, the MnCo₂O₄ spinel is the most potential candidate for SOFC metallic interconnect protective coating application.