The effect of β phase on microstructure and texture evolution during thermomechanical processing of α + β Ti alloy

Microstructure and texture evolution have been investigated in both α and β phases during the hot rolling of β-quenched Ti–6Al–4V at 800 and 950 °C, followed by annealing at 950 °C and air cooling using detailed electron backscattered diffraction mapping. The textures of primary and secondary α in the bi-modal microstructure were analysed separately, and the high-temperature β orientations were calculated by a variant based reconstruction from the inherited α_s orientations. Crystal plasticity finite element modelling has been employed to predict the rolling texture based on common α phase slip systems and compare with the measured α texture. It was found that despite the severe deformation during rolling, a large proportion of the primary α grains retain a Burgers relationship with the β phase. Consequently, the β phase in combination with a variant selection mechanism seems to control the α texture, which explains the discrepancy between predicted and measured rolling textures. The consequence of this mechanism for macrozone formation is also discussed.     

固溶时效处理对BT25y钛合金显微组织及硬度的影响

研究了固溶处理和固溶时效处理对BT25y钛合金组织形态、物相组成和显微硬度的影响。结果表明,锻态组织呈现典型的双态组织特征。试样在相变点T_β之下固溶处理,随着固溶温度的升高,初生α相含量逐渐减少,β转变组织逐渐增多,β转变组织中片层状次生α相的厚度逐渐增大,β相含量逐渐增大。试样在相变点之上固溶处理,初生α相完全消失,显微组织转变为全片层组织。对固溶试样时效处理后,初生α相形态和尺寸变化不明显,β转变组织发生了明显分解。相变点之下固溶试样时效处理后β相含量有所减少,而在相变点之上固溶试样时效处理后β相含量有所增加。试样中片层状β转变组织含量增加与组织细化效应会有效强化两相钛合金,而β相含量提高会软化两相钛合金,与固溶处理试样相比,相变点之下固溶处理的试样时效后的硬度由于β相含量减少和组织细化综合作用而增幅显著,而相变点之上固溶处理的试样时效后硬度由于β相含量增加和组织细化的综合作用呈现少量增加。     

Kinetic behaviour of TiB2 particles in Al melt and their effect on grain refinement of aluminium alloys

Solidification experiments were carried out to investigate the kinetic behaviour of TiB₂ particles in Al melt and their effect on the grain refinement of commercially-pure Al. A model was proposed to describe the kinetic behaviour of TiB₂ particles during the whole process from the addition of TiB₂ to the melt to the freezing of the melt. The results indicate that TiB₂ particles are not stable in Al melt. They may dissolve and coarsen during the holding period and grow during the cooling period of the melt. The kinetic behaviour of TiB₂ particles in the melt has a great influence on their number density and the grain refinement. Solute Ti addition can suppress the dissolution, Ostwald ripening and growth behaviours of TiB₂ particles.     

Real-time observation of grain nucleation and growth during solidification of aluminium alloys

The crystallisation kinetics of liquid aluminium–titanium alloys with microscopic TiB₂ particles added to refine the grain size in the solidified material was studied by X-ray diffraction measurements at a synchrotron source. Real-time observation of the formation and growth of individual grains reveals the central role played by the added TiB₂ particles during solidification. Prior to the main transformation, weak reflections of a metastable TiAl₃ phase were detected. This observation finally pinpoints the highly debated mechanism responsible for enhanced grain nucleation in Al–Ti–B alloys.     

Influence of heat treatments on microstructure and mechanical properties of laser additive manufacturing Ti-5Al-2Sn-2Zr-4Mo-4Cr titanium alloy

The effect of heat treatments on laser additive manufacturing (LAM) Ti-5Al-2Sn-2Zr-4Mo-4Cr titanium alloy (TC17) was studied aiming to optimize its microstructure and mechanical properties. The as-deposited sample exhibits features of a mixed prior β grain structure consisting of equiaxed and columnar grains, intragranular ultra-fine α laths and numerous continuous grain boundary α (α_GB). After being pre-annealed in α+β region (840 °C) and standard solution and aging treated, the continuous α_GB becomes coarser and the precipitate free zone (PFZ) nearby the α_GB transforms into a zone filled with ultra-fine secondary α (α_S) but no primary α (α_P). When pre-annealed in single β region (910 °C), all α phases transform into β phase and the alloying elements distribute uniformly near the grain boundary. Discontinuous α_GB and uniform mixture of α_P and α_S near grain boundary form after subsequent solution and aging treatment. The two heat treatments can improve the tensile mechanical properties of LAM TC17 to satisfy the aviation standard for TC17.     

Study of structure formation in TiC–TiB2–MexOy ceramics fabricated by SHS and densification

Bulk ceramic materials based on TiC–TiB₂–Me_xO_y systems have been produced by means of pressure-assisted self-propagating high-temperature synthesis (SHS). The selection of the SHS systems was based on thermodynamic analyses in order to obtain regimes of synthesis with formation of liquid phase allowing a proper densification. The liquid phase formed in the products consisted of either melted oxides or TiC–TiB₂ eutectic depending on the combustion temperature. The mechanisms of structure formation and the effect of grain growth inhibition due to the metal oxide particles have been evaluated. The microstructural investigations have confirmed the role of the metal oxides as promoter of the final products densification and of the grain refinement in the SHS ceramic materials. A core–shell model is proposed to explain the structure formation of the SHS composites through a chemical interaction involving two stages. The good agreement between calculated and experimental results confirmed the validity of the core–shell mechanism.     

Microstructures and mechanical properties of in-situ TiB2/Al−xSi−0.3Mg composites

In-situ 2 vol.% TiB₂ particle reinforced Al?xSi?0.3Mg (x=7, 9, 12, 15 wt.%) composites were prepared by the salt–metal reaction, and the microstructures and mechanical properties were investigated. The results show that the TiB₂ particles with a diameter of 20–80 nm and the eutectic Si with a length of 1–10 μm are the main strengthening phases in the TiB₂/Al?xSi?0.3Mg composites. The TiB₂ particles promote grain refinement and modify the eutectic Si from needle-like to short-rod shape. However, the strengthening effect of TiB₂ particles is weakened as the Si content exceeds the eutectic composition, which can be attributed to the formation of large and irregular primary Si. The axial tensile test results and fractography observations indicate that these composites show more brittle fracture characteristics than the corresponding alloy matrixes.     

Effect of Mg on the Microstructure and Mechanical Properties of Al0.3Sc0.15Zr-TiB2 Composite

Al-0.3Sc-0.15Zr-TiB₂ composites with varying additions of Mg were cast through a novel processing technique using oil Quenched Investment Casting (QIC). Addition of Mg resulted in grain refinement of the composite. Al₃(Sc, Zr) primary particles and TiB₂ are responsible for grain refinement in these composites. Presence of fine nanosized uniformly distributed precipitates of Al₃(Sc, Zr) at the peak age condition together with TiB₂ particles increase the strength and ductility of the composites. The presence of Sc and Zr reduces the size of TiB₂ particles down to 10 nm. The optimum magnesium content in the composites studied lies between 3.5 and 6%.     

A mechanism for the poisoning effect of silicon on the grain refinement of Al–Si alloys

The poisoning effect of excess Si solute on the grain-refining potency of Al–Ti–B grain refiners in Al–Si casting alloys has been studied in a crystallographic investigation. The edge-to-edge matching model was used for investigating and comparing the possible poisoning effects of several binary and ternary intermetallic compounds containing Si and Ti. The results show that the poisoning effect is probably due to the formation of a Ti₅Si₃ coating on the surface of TiAl₃, because the Ti₅Si₃ phase has a much better crystallographic matching with TiAl₃ than it does with the Al matrix. However, TiB₂ particles appear to survive because an excessively large misfit prevents the Ti₅Si₃ phase from forming on the surface of TiB₂. The implications of this proposed mechanism are discussed in the light of current practical casting solutions and the continuing debate on the grain refinement mechanism.     

The grain refinement mechanism of cast aluminium by zirconium

The mechanism underlying the grain refinement of cast aluminium by zirconium has been studied through examination of a range of Al alloys with increasing Zr contents. Pro-peritectic Al₃Zr particles are reproducibly identified at or near the grain centres in grain-refined alloy samples based on the observations of optical microscopy, scanning electron microscopy and X-ray diffraction. From the crystallographic study using the edge-to-edge matching model, electron backscatter diffraction and transmission electron microscopy, it is substantiated that the Al₃Zr particles are highly potent nucleants for Al. In addition, the effects of Al₃Zr particle size and distribution on grain refinement has also been investigated. It has been found that the active Al₃Zr particles are bigger than previously reported other types of active particles, such as TiB₂ for heterogeneous nucleation in Al alloys. Considering the low growth restriction effect of Zr in Al (the maximum Q-value of Zr in Al is 1.0 K), it is suggested that the significant grain refinement of Al resulting from the addition of Zr can be mainly attributed to the heterogeneous nucleation facilitated by the in situ formed Al₃Zr particles.     

Formation and growth mechanism of a manganese phosphate coating on an as-cast Zr–Al binary alloy

The preparation of a manganese phosphate coating on an as-cast Zr–Al alloy is described. The alloy consisted of an α phase (α-Zr) and a β phase (Zr₂Al), where α-Zr is the matrix and Zr₂Al spreads along the grain boundaries discontinuously. The coating was divided by cracks to exhibit a network structure. The manganese phosphate coating showed a combination of crystalline and amorphous structure. The film consists of small particles densely packed. It is uniform and compact. The formation of the phosphate coating on substrates treated for short periods was investigated. Mn₅(PO₄)(OH)₂·H₂O and MnZr(PO₄)₂·4H₂O phases were found in the manganese phosphate coatings. The grain particles are preferentially deposited on the β phase rather than on the α phase.     

Effect of Various SPD Techniques on Structure and Superplastic Deformation of Two Phase MgLiAl Alloy

MgLiAl alloy containing 9 wt% Li and 1.5% Al composed of hexagonal α and bcc β phases was cast under protecting atmosphere and hot extruded. Various methods of severe plastic deformation were applied to study their effect on structure and grain refinement. Rods were subjected to 1–3 passes of Twist Channel Angular Pressing TCAP (with helical component), cyclic compression to total strain ε?=?5 using MAXStrain Gleeble equipment, both performed at temperature interval 160–200 °C and, as third SPD method, KOBO type extrusion at RT. The TCAP pass resulted in grain refinement of α phase from 30 μm down to about 2 μm and that of β phase from 12 to 5 μm. Maxstrain cycling 10?× up to ε?=?5 led to much finer grain size of 300 nm. KOBO method performed at RT caused average grain size refinement of α and β phases down to about 1 μm. Hardness of alloy decreased slightly with increasing number of TCAP passes due to increase of small void density. It was higher after MAXStrain cycling and after KOBO extrusion. TEM studies after TCAP passes showed higher dislocation density in the β region than in the α phase. Crystallographic relationship (001) α|| (110) β indicated parallel positioning of slip planes of both phases. Electron diffraction technique confirmed increase of grain misorientation with number of TCAP passes. Stress/strain curves recorded at temperature 200 °C showed superplastic forming after 1st and 3rd TCAP passes with better superplastic properties due to higher elongation with increasing number of passes. Values of strain rate sensitivity coefficient m were calculated at 0.29 after 3rd TCAP pass for strain rate range 10^?5 to 5?×?10^?3 s^?1. Deformation by MAXStrain cycling caused much more effective grain refinement with fine microtwins in α phase. Superplastic deformation was also observed in alloy deformed by KOBO method, however the value of m?=?0.21 was obtained at lower temperature of deformation equal to 160 °C and deformation rate in the range 10^?5 to 5?×?10^?3. Tensile samples deformed superplastically showed grain growth and void formation caused by grain boundary slip. Summarizing, all methods applied resulted in sufficient grain refinement to obtain the effect of superplastic deformation for alloys of two phase α?+?β structure.     

In situ formation of TiAl–TiB2 composite by SHS

The preparation of TiAl intermetallic compounds with or without the reinforcement phase TiB₂ was conducted by self-propagating high-temperature synthesis (SHS) from elemental powder compacts in this study. Effects of initial sample density, preheating temperature, particle size of the reactants, and TiB₂ content on the combustion characteristics, as well as on the composition and morphology of final products were studied. In this investigation, preheating was found to be required for the samples without boron addition to achieve self-sustained combustion, while boron-added compacts showed no need of prior heating, primarily due to the additional reaction heat liberated from the in situ formation of TiB₂. With the addition of boron, the reaction temperature and flame-front propagation velocity were correspondingly increased. Due to the melting of synthesized products caused by high-combustion temperatures, the TiAl–TiB₂ composite was contracted in dimension during the reaction. On the contrary, substantial volume expansion was observed in the sample without boron addition. This means that the in situ formed TiB₂ plays an important role not only in improving the mechanical property, but also in enhancing the densification of final products. XRD analysis of burned products identifies the in situ formed TiB₂ a reinforcing phase, and TiAl the dominant intermetallic phase. In addition to TiAl, another intermetallic compound Ti₃Al known as a major secondary phase in the Ti–Al reaction was detected in all end products of this study.     

Thermal stability of superhard Ti-B-N coatings

Ternary transition-metal boron nitride Ti-B-N offers outstanding hardness and thermal stability, which are increasingly required for wear resistant applications, as the protective coatings are subjected to high temperature, causing thermal fatigue. Ti-B-N coatings with chemical compositions close to the quasibinary TiN-TiB₂ tie line and boron contents below ∼ 18 at.% contain a crystalline supersaturated NaCl structure phase, where B substitutes for N. Annealing above the deposition temperature causes precipitation of TiB₂, which influence dislocation mobility and hence the hardness of TiB_0.40N_0.83 remains at a very high level of ∼ 43 GPa with annealing temperature T_a up to 900 °C. Growth of Ti-B-N coatings with B contents above ∼ 18 at.% results in the formation of nm sized TiN and TiB₂ crystallites embedded in a high volume fraction of disordered boundary layer. The compaction of this disordered phase during annealing results in a hardness increase of TiB_0.80N_0.83 coatings from the as-deposited value of ∼ 37 GPa to ∼ 42 GPa at T_a = 800 °C. Excess B during growth of TiB_2.4 coatings causes the formation of bundles of ∼ 5 nm wide TiB₂ subcolumns encapsulated in a B-rich tissue phase. This nanocolumnar structure is thermally stable up to temperatures of ∼ 900 °C, and consequently the hardness remains at the very high level of ~ 48 GPa, as nucleation and growth of dislocations is inhibited by the nm sized columns. Furthermore, the high cohesive strength of the B-rich tissue phase prevents grain boundary sliding.     

Effects of sintering additives on microstructure and mechanical properties of TiB2-WC ceramic-metal composite tool materials

TiB₂-WC ceramic-metal composite tool materials were fabricated using Co, Ni and (Ni, Mo) as sintering additives by vacuum hot-pressing technique. The microstructure and mechanical properties of the composite were investigated. The composite was analyzed by the observations of scanning electron microscope (SEM), X-ray diffraction (XRD) and energy dispersive spectrometry (EDS). The microstructure of TiB₂-WC ceramic-metal composites consisted of the fine WC grains and uniform TiB₂ grains. The brittle phase of Ni₃B₄ and a few pores were found in TiB₂-WC-Ni ceramic-metal composite. A lot of pores and brittle phases such as W₂CoB₂ and Co₂B were formed in TiB₂-WC-Co ceramic-metal composite. The liquid phase of Co was consumed by the reaction which led to the formation of the pores and the coarse grains of TiB₂. The pores, brittle phases and coarse grains of TiB₂ were harmful to the improvement of the mechanical properties of the composite. The sintering additive of (Ni, Mo) had a significant effect on the density and the mechanical properties of TiB₂-WC ceramic-metal composite. The formation of intermetallic compound of MoNi₄ inhibited the consumption of liquid phase of (Ni, Mo). The liquid phase of (Ni, Mo) not only inhibited the formation of the pores and the coarse grains of TiB₂ but also strengthened the interface energy between WC and TiB₂ grains. The grain size was fine and the average relative density of TiB₂-WC-(Ni, Mo) ceramic-metal composite reached 99.1%. The flexural strength, fracture toughness and Vickers hardness of TiB₂-WC-(Ni, Mo) ceramic-metal composite were 1307.0 ± 121.4 MPa, 8.19 ± 0.29 MPa m^1/2 and 22.71 ± 0.82 GPa, respectively.     

Columnar to equiaxed transition during growth of a univariant eutectic

Abstract

In this work the transition from columnar to equiaxed growth is studied during the solidification of the univariant eutectic L→ α(Al) + θ-Al₂Cu in the ternary Al–Cu–Ag system. The experimental technique used is upwards solidification with a controlled cooling rate. In the lower part of the sample where the temperature gradient is high, a cellular eutectic is observed. When the temperature gradient decreases, the morphology first changes into two-phase dendrites and finally into an equiaxed eutectic. When the amount of Ag is increased, the formation of eutectic colonies becomes easier. Also, a higher cooling rate facilitates the formation of eutectic colonies. The addition of TiB₂ does not influence the nucleation of eutectic colonies. Although the composition is on the eutectic groove, primary α(Al)-dendrites are found in the samples with TiB₂. This leads to segregation effects due to the density difference between α(Al) and the liquid.     

Characterization of hot pressed SiC whisker reinforced TiB2 based composites

TiB₂–SiC ceramic composites, with different contents of SiC whiskers (SiC_w), as a ceramic sinter-additive, were prepared by the hot pressing process at 1850 °C for 2 h under a pressure of 20 MPa. For comparison, a monolithic TiB₂ ceramic was also fabricated under the identical temperature, pressure, atmosphere, and holding time by the hot pressing process. The effects of fabrication process and SiC whiskers on microstructural features, phase evolution and mechanical properties were investigated. Hardness measurements revealed an initial increase in hardness for TiB₂–SiC compared to TiB₂. Also the improvement of the fracture toughness was attributed to the toughening and strengthening effects of SiC whiskers such as crack deflection. The results showed that promoted densification of TiB₂–SiC ceramic composites is due to addition of SiC whiskers and reduction of oxide impurities by reacting with SiC whiskers and removing them from the surface layer of TiB₂ particles. The reaction between TiB₂ particles and SiC whiskers led to in-situ formation of TiC phase in the matrix as well. In general, it is concluded that the sinterability of TiB₂-based composites was remarkably improved by introducing SiC whiskers compared to the single phase TiB₂ ceramic.     

Microstructure and mechanical properties of (TiB+La2O3)/Ti composites heat treated at different temperatures

Near-α titanium matrix composites reinforced with TiB and La₂O₃ were synthesized by common casting and hot-working technology. The effects of β heat treatment temperature on the microstructure and the tensile properties of the in situ synthesized (TiB+La₂O₃)/Ti were studied. Microstructure was studied by OM and TEM, and tensile tests were carried out at room temperature and 923 K, respectively. Results show that with the increase of β heat treatment temperature, prior β phase grain size increases and α colony size decreases. Room temperature tensile strength increases with the increase of β heat treatment temperature, which can be attributed to the decrease of α colony size with the increase of β heat treatment temperature. However, high-temperature tensile strength decreases with the increase of β heat treatment temperature and the decrease of the high-temperature tensile strength is due to the increase of the prior β phase grain size.     

Nucleation and variant selection of secondary α plates in a β Ti alloy

The microtexture of secondary α plates in Ti–4.5Fe–6.8Mo–1.5Al has been investigated by electron backscatter diffraction (EBSD) to obtain more insight in the nucleation and variant selection of these α plates. A statistical analysis of the EBSD data shows that for most β grain boundaries the variant selection of the α plates is in agreement with a commonly used variant selection criterion yielding that the α-{0 0 0 1} pole is nearly parallel to the closest β-{1 1 0} poles of the two adjacent β grains. For a small angle between the β-{1 1 0} poles nucleation is predominantly observed at both sides of the grain boundary, while with increasing angle some β grain boundaries exhibit nucleation of α plates at only one side. In the β grain interior many so-called Type 2 α–α grain boundaries are observed which are thought to originate from autocatalytic nucleation when a new α plate is formed at an existing α–β interface.     

E2EM's prediction of LaB6 as nucleation substrate for primary Mn-rich phase in Al-Si-Cu-Mn heat-resistant alloy and its refining effect

Edge-to-edge matching (E2EM) model was used to predict the potency of LaB₆ as the heterogeneous nucleation substrate for primary Al₁₃Mn₄Si₈ phase formed during the solidification of Al-Si-Cu-Mn heat-resistant alloy. There are five pairs of orientation relationships (ORs) between LaB₆ and Al₁₃Mn₄Si₈ phases which meet the criteria of E2EM model. One pair of plane ORs ((110)_LaB6//(110)_Al13Mn4Si8) are demonstrated by TEM observation. This strongly indicates that the LaB₆ phase can act as the heterogeneous nucleation substrate for the primary Al₁₃Mn₄Si₈ phase. 1.0 wt.% of Al-2La-1B master alloy was also added into Al-12Si-4Cu-2Mn alloy to evaluate the refining effect by microstructure observation and tensile test. Experimental results show that addition of Al-2La-1B master alloy can significantly refine the primary Al₁₃Mn₄Si₈ phase, supporting the prediction accuracy of E2EM model. However, such refinement of primary Al₁₃Mn₄Si₈ phase does not lead to an improvement in strength. This is due to the larger difference in elastic modulus between the finally formed Al₁₃Mn₄Si₈ phase and aluminum matrix than that of Al₁₅Mn₃Si₂ phase.