Correlation of microstructure with high-temperature hardness of (TiC,TiN)/Ti–6Al–4V surface composites fabricated by high-energy electron-beam irradiation

Correlation of microstructure with high-temperature hardness of (TiC,TiN)/Ti–6Al–4V surface composites fabricated by high-energy electron-beam irradiation was investigated in this study. TiC, TiN and TiC+TiN powder mixtures containing 50% CaF₂ flux were deposited on the surface of a Ti–6Al–4V alloy substrate, and irradiated by high-energy electron beam to form 1-mm-thick, defect-free surface composite layers. The surface composite layers contained a large amount (over 30 vol.%) of precipitates such as TiC, TiN, (Ti_xAl_1−x)N and Ti(C_xN_1−x) in the martensitic or N-rich acicular α-Ti matrix. This microstructural modification including the formation of hard precipitates and hardened matrices in the surface composite layers improved hardness and high-temperature hardness two to four times greater than that of the substrate. In particular, the surface composite fabricated with TiN powders had the highest hardness because of the highest volume fraction of TiN and (Ti_xAl_1−x)N distributed in the hardened N-rich acicular α-Ti matrix. These findings suggest that the (TiC,TiN)/Ti–6Al–4V surface composites can be used for structural materials requiring excellent thermal resistance.     

Cu + TiB2 composite filler for brazing Al2O3 and Ti-6Al-4V alloy

Al₂O₃ and Ti-6Al-4V alloy were brazed using Cu + TiB₂ composite filler, which manufactured by mechanical milling of Cu and TiB₂ powders. Typical interface microstructure of joint was Al₂O₃/Ti₄(Cu,Al)₂O/Ti₂Cu + Ti₃Al + Ti₂(Cu,Al)/Ti₂(Cu,Al) + AlCu₂Ti/Ti₂Cu + AlCu₂Ti + Ti₃Al + Ti₂(Cu,Al) + TiB/Ti(s.s) + Ti₂Cu/Ti-6Al-4V alloy. Based on temperature- and time-dependent compositional change, the formation of intermetallics in joint was basically divided into four stages: formation of interfacial Ti₄(Cu,Al)₂O in Al₂O₃ side, formation of Ti₂Cu, Ti₃Al, TiB, Ti₂Cu, and AlCu₂Ti in layers II and IV, formation of Ti₂(Cu,Al) and AlCu₂Ti in layer III, formation of Ti + Ti₂Cu hypereutectoid organization adjacent to Ti-6Al-4V alloy. TiB in situ synthesized in joint not only acted as low thermal expansion coefficient reinforcement to improve the mechanical properties at room temperature, but also as skeleton ceramic of joint to increase high temperature mechanical properties of Al₂O₃/Ti-6Al-4V alloy joint increasing. When the joint containing 30 vol.% TiB brazed at 930 °C and 10 min of holding time, the maximum room temperature shear strength of joint was 96.76 MPa, and the high temperature shear strength of joint was 115.16 MPa at 800 °C.     

C/Al2O3复合材料的固体粒子冲蚀行为与磨擦磨损性能研究

以溶胶浸渍热处理技术路线制备的碳纤维布叠层缝合预制件增强Al₂O₃(C/Al₂O₃)复合材料为对象,以刚玉粉为介质,研究了复合材料的固体粒子冲蚀行为,按照GB5763-2008规定的条件研究了复合材料的磨擦磨损性能。室温下,复合材料冲蚀率随着冲击角度与送粉量的增大而增加;温度升高,由于机械冲击和热冲击的双重作用,冲蚀率显著变大。在GB5763-2008规定的条件下,C/Al₂O₃复合材料具有稳定的摩擦系数和很低的磨损率。结合微观形貌分析,探讨了复合材料的冲蚀与磨损机理。得益于连续碳纤维的补强增韧作用,即使基体致密度低于单体Al2O3陶瓷,C/Al₂O₃复合材料在冲蚀和磨损时不会发生脆性断裂,使用安全性优于单体Al₂O₃陶瓷。     

Rapid consolidation of nanocrystalline Ti<Subscript>3</Subscript>Al-Al<Subscript>2</Subscript>O<Subscript>3</Subscript> composites from mechanically synthesized powders by high frequency induction heated sintering

Nano-powders of Ti₃Al and ²Al₂O₃ were synthesized from 3TiO₂ and 5Al powders by high energy ball milling. Nanocrystalline Al₂O₃ reinforced composite was consolidated by high frequency induction heated sintering within 2 minutes from mechanochemically synthesized powders of 2Al₂O₃ and Ti₃Al. The relative density of the composite was 99.5%. The average hardness and fracture toughness were 1340 kg/mm² and 8 MPa·m^1/2, respectively.     

Al_2O_3-TiC复合陶瓷与Q235钢扩散连接界面组织结构

采用Ti/Cu/Ti复合中间层通过液相扩散连接技术实现了Al2O3-TiC复合陶瓷与Q235低碳钢的扩散连接.采用扫描电镜、电子探针及X射线衍射等测试手段对Al2O3-TiC/Q235扩散连接接头的显微组织、断口形貌及相组成进行了分析.结果表明,Al2O3-TiC/Q235界面结合紧密,没有显微孔洞、裂纹及未连接区域;Al2O3-TiC/Q235界面附近有各种各样的新相生成,如TiO,Ti3Al,Cu2Ti4O及Cu3Ti3O,所生成的TiO相及复杂结构氧化物Cu3Ti3O和Cu2Ti4O都具有金属特性,对于促进Al2O3-TiC/Q235的可靠连接起到重要作用;接头抗剪强度达143MPa,断口表现为脆性断裂特征,Al2O3-TiC/Q235接头断在界面附近的Al2O3-TiC内.     

BN/Al2O3 复合粉末及其聚合物基复合材料的制备与导热性能

采用固-液相共混法制备了多种BN/Al₂O₃复合粉末,通过冻融法和表面修饰法对BN进行了改性处理,改变表面修饰剂类型和摩尔比得到了前驱体和烧结态BN/Al₂O₃复合粉末,并利用机械混合法制备了聚合物基BN/Al₂O₃复合材料,并测试分析了其导热性能。结果表明,经冻融处理的BN分散性和界面相容性明显优于未经冻融处理的BN。多巴胺对BN的改性效果优于聚乙二醇。采用多巴胺作为表面修饰剂且BN与Al(NO₃)₃的摩尔比为1:1时,能够得到纳米Al₂O₃均匀包覆的微米BN粉末,即BN/Al₂O₃微纳复合粉末,其聚合物基复合材料的导热系数可达0.62 W·m^-1·K^-1,是纯聚合物导热系数的3倍,是采用纯微米BN粉末制备的聚合物基复合材料导热系数的1.5倍。在BN表面附着的Al₂O₃可以形成层状热传导通道,能够有效提高聚合物基BN/Al₂O₃复合材料的热导率。     

铝镁合金等离子喷涂复相陶瓷涂层微观组织

为解决铝镁合金表面耐磨性差的问题,利用机械球磨法和PVA造粒技术制备复合陶瓷粉末,采用等离子喷涂技术在XGFH-3铝镁合金表面制备了反应复相陶瓷涂层,利用扫描电镜(SEM)、X射线衍射仪(XRD)分析了喷涂复合粉末和复相陶瓷涂层的形貌及组成.结果表明,复合粉末随着球磨时间的延长明显趋于扁平化和均匀化,并且生成了Al₃Ti,Ni₄Ti₃等新相.而在喷涂过程中Al₃Ti和Ni₄Ti₃中间相又会消失,涂层中出现了MgAl₂O₄和Ti₅Si₃等新相,基体和涂层之间有元素扩散,这使得涂层有良好的结合强度.     

Wear and oxidation resistance of Al2O3 particle dispersed Al3Ti composite with a nanostructure prepared by pulsed electric current sintering of mechanically alloyed powders

Al₃Ti-matrix composite layers containing Al₂O₃ particles were formed on Ti substrate by pulsed electric current sintering (PECS) of mechanically alloyed (MA) powders to improve the wear and oxidation properties of the Ti substrate. Reducing the grain size of each element by MA makes the combustion synthesis of Al₃Ti possible at a lower temperature. The grain size formed by the combustion synthesis of Al–Ti–Al₂O₃ powder mechanically alloyed for 720 ks was about 10 nm and its growth during sintering was suppressed by the existence of Al₂O₃. The densification behavior of the powder was investigated quantitatively. The obtained Al₃Ti/Al₂O₃ composite layer showed better wear and oxidation resistance than the monolithic Al₃Ti layer.     

Fabrication of Al matrix composite reinforced with submicrometer-sized Al<Subscript>2</Subscript>O<Subscript>3</Subscript> particles formed by combustion reaction between HEMM Al and V<Subscript>2</Subscript>O<Subscript>5</Subscript> composite particles during sintering

To fabricate an Al-V matrix composite reinforced with submicron-sized Al₂O₃ and Al_xV_y (Al₃V, Al₁₀V) phases, high energy mechanical milling (HEMM) and sintering were employed. By increasing the milling time, the size of mechanically milled powder was significantly reduced. In this study, the average powder size of 59 μm for Al, and 178 μm for V₂O₅ decreased with the formation of a new product, Al-Al₂O₃-Al_xV_y, with a size range from 1.3 μm to 2.6 μm formed by the in-situ combustion reaction during sintering of HEM milled Al and V₂O₅ composite powders. The in-situ reaction between Al and V₂O₅ during the HEMM and sintering transformed the Al₂O₃ and Al_xV_y (Al₃V, Al₁₀V) phases. Most of the reduced V reacted with excess the Al to form Al_xV_y (Al₃V, Al₁₀V) with very little V dissolved into Al matrix. By increasing the milling time and weight percentage of V₂O₅, the hardness of the Al-Al₂O₃-Al_xV_y composite sintered at 1173 K increased. The composite fabricated with the HEMM Al-20wt.%V₂O₅ composite powder and sintering at 1173 K for 2 h had the highest hardness.     

Oxidation Behavior of a TiAl–Al2Ti4C2–TiC–Al2O3 in situ Composite

A TiAl–Al₂Ti₄C₂–TiC–Al₂O₃ in situ composite was fabricated using TiO₂, Al, and C as starting materials through a mechanical-milling and subsequently a pressureless-sintering process. Discontinuous and cyclic-oxidation tests were then carried out at 800 and 900° C in air up to 500 hr or 1000 cycles to evaluate its oxidation and oxide-scale-spallation resistance. The present results demonstrated that this composite had extremely high oxidation resistance in comparison with a Ti–48Al–2Cr alloy. The oxidation mass gains measured on the composite were about two orders of magnitude lower than that of the alloy. Moreover, the oxide on this composite showed superior spallation resistance; scale cracking or spalling could never be detected, while the alloy samples suffered severe scale cracking and spallation. Based on the morphological and cross-sectional observations, it is believed that α-Al₂O₃ and Al₂Ti₄C₂ formed and incorporated in the composite could significantly influence the scaling behavior and then improve oxidation and spallation resistance of this composite.     

Ti活度对Al2O3/AgCuTi/Fe-Ni-Co钎焊接头机械性能和微观组织结构的影响

采用AgCuTi钎料实现了Al₂O₃陶瓷与Fe-Co-Ni合金的钎焊连接,并调查了不同钛含量的钎料对Al₂O₃/AgCuTi/Fe-Ni-Co钎焊接头机械性能和微观组织结构的影响。扫描电子显微镜(SEM), X射线能量色散光谱仪(EDS), X射线衍射仪(XRD)及电子万能试验机用于分析钎焊接头的机械性能和微观组织结构,结果表明:钛含量的增加明显提高AgCuTi钎料与Al₂O₃陶瓷的相互作用,在Al₂O₃/Ag-Cu-Ti界面生成一层由Ti-Al 和 Ti-O化合物组成的反应层。Al₂O₃/AgCuTi/Fe-Ni-Co钎焊接头的抗拉强度随钛含量的增加而增加,当钛含量提高到8wt.%时,抗拉强度达到最大值78Mpa。通过微观组织结构分析发现,采用AgCu4Ti在890℃保温5min的条件下可以获得较好的钎焊接头,典型接头的微观组织结构为Al₂O₃/TiAl+Ti₃O₅/NiTi+Cu₃Ti+Ag(s,s)/Ag(s,s)+Cu(s,s)+(Cu,Ni)/Fe-Ni-Co。采用AgCu8Ti获得的钎焊接头的界面反应层与AgCu4Ti差异不大,但反应层稍微增厚,并伴有TiO和Ti3Al在Al₂O₃/Ag-Cu-Ti界面生成。     

Reactive mechanism and mechanical properties of in situ composites fabricated from an Al–TiO2 system by friction stir processing

In situ (Al₃Ti + Al₂O₃)/Al composites were fabricated from powder mixtures of Al and TiO₂ using hot pressing, forging and subsequent multiple-pass friction stir processing (FSP). The reactive mechanism and mechanical properties of the FSPed composites were investigated. Four-pass FSP with 100% overlapping induced the Al–TiO₂ reaction, as a result of the enhanced solid diffusion and mechanical activation effect caused by the severe deformation of FSP. Decreasing the size of TiO₂ from 450 to 150 nm resulted in the formation of more Al₃Ti and Al₂O₃ particles. The formation mechanisms of Al₂O₃ and Al₃Ti during FSP are understood to be a deformation-assisted interfacial reaction and deformation-assisted solution-precipitation, respectively, based on detailed microstructural observations. The microhardness, Young’s modulus and tensile strength of the FSPed composites were substantially enhanced compared with those of FSPed pure Al with the same processing history, and increased as the TiO₂ size decreased from 450 to 150 nm. The strengthening mechanisms of the FSPed composites included load transferring, grain refinement and Orowan strengthening, among which Orowan strengthening contributed the most to the yield strength of the composites.     

The Microstructures and Mechanical Properties of V2O5-Doped Al2O3/TiAl In-Situ Composites by Reactive Hot Pressing Process

Al₂O₃/TiAl composites are successfully fabricated by the in-situ hot pressing method from the elemental powders of Ti, Al, TiO₂, and V₂O₅. The effect of V₂O₅ addition on the microstructure and mechanical properties of the Al₂O₃/TiAl in-situ composites is investigated in detail. It is found that the as-synthesized composites mainly consist of V-dissolved γ-TiAl, α₂-Ti₃Al, and Al₂O₃ particles along with a small amount of V₃Al phase, and the in-situ-formed fine Al₂O₃ particles tend to disperse on the grain boundaries of TiAl matrix. With increasing V₂O₅ content, the density and Vickers hardness of the resulting composites gradually increase, whereas the fracture toughness and flexural strength first increase and then decrease with the increase of V₂O₅ content. The composite with 3.5 wt.% V₂O₅ has the maximum value of 9.35 MPa m^1/2 and 713.36 MPa for the fracture toughness and flexural strength, respectively. The toughening mechanism is also discussed in detail.     

Effect of reacted compounds in Al2O3+Ti investment mold on alpha-case formation for Ti casting

This paper proposes a newly developed alpha-case controlled mold material for Ti castings. An Al₂O₃ mold containing alpha-case reaction compounds, titanium oxide (TiO₂, Ti₂O and Ti₆O) and titanium silicide (Ti₅Si₃) was manufactured via a reaction between Al₂O₃ and Ti powder under different firing conditions in air and a vacuum. In comparison with the Al₂O₃ and Al₂O₃+Ti mold fired in a vacuum, the micro-Vickers hardness and nano indentation profiles of Al₂O₃+Ti indicated that the alpha-case thickness was significantly reduced from 350 μm to ～45 μm. The alpha-case formation in the Al₂O₃+Ti mold was reduced due to the presence of TiO₂, which formed the TiO intermediate phase that acted as a diffusion barrier. In addition, Ti₅Si₃ was effective in minimizing Si contamination at the casting surface due to the reaction between Ti and the colloidal SiO₂ binder. Therefore, alpha-case reaction compounds, such as TiO₂ and Ti₅Si₃ in Al₂O₃, can effectively reduce alpha-case formation at the casting surface.     

In situ formation of various intermetallic particles in Al–Ti–X(Cu,Mg) systems during friction stir processing

In situ Al composites reinforced by various intermetallic particles were fabricated from Al–Ti–X(Cu, Mg) systems by hot pressing, forging and subsequent 4-pass friction stir processing (FSP). The formation of various intermetallic particles during FSP and the tensile properties of in situ composites were investigated. For Al–Ti–Cu system, Cu enhanced the Al–Ti reaction and resulted in the formation of more Al₃Ti particles due to the presence of a small amount of liquid phase during FSP. After FSP, part of Cu was kept in the Al matrix as solute, whereas the other formed Al₂Cu particles. For Al–Ti–Mg system, except for Al₃Ti, some Ti₂Mg₃Al₁₈ particles with fine twin lamellas were formed during FSP, resulting in an increase in the total volume fraction of reinforcing particles. Cu and Mg addition increased the strength of the in situ composites substantially due to introduction of more strengthening modes and more reinforcing particles, however the elongation decreased dramatically.     

Ti3AlC2-Al2O3-TiAl3 composite fabricated by reactive melt infiltration

Porous preforms were fabricated by cold-pressing process using powder mixture of TiC, TiO₂ and dextrin. After pyrolysis and sintering, Al melt was infiltrated into the porous preforms, leading to the formation of Ti₃AlC₂-Al₂O₃-TiAl₃ composite. Effects of cold-pressing pressure of preforms on microstructures and mechanical properties of the composites were studied. Synthesis mechanism and toughening mechanism of composite were also analyzed. The results shows that TiO₂ is reduced into Ti₂O₃ by carbon, the decomposition product of dextrin, which causes the spontaneous infiltration of Al melt into TiC/Ti₂O₃ preform. Then, Ti₃AlC₂-Al₂O₃-TiAl₃ composite is in-situ formed from the simultaneous reaction of Al melt with TiC and Ti₂O₃. With the increase of cold-pressing pressure from 10 MPa to 40 MPa, the pore size distribution of the preforms becomes increasingly uniform after pre-sintering, which results in the reduction of defects, and the decrease of property discrepancy of composites. Nano-laminated Ti₃AlC₂ grains and Al₂O₃ particles make the fracture toughness of TiAl₃ increase remarkably by various toughening mechanisms including stress-induced microcrack, crack deflection and crack bridging.     

SiO2–Al2O3–glass composite coating on Ti–6Al–4V alloy: Oxidation and interfacial reaction behavior

A SiO₂–Al₂O₃–glass composite coating was prepared on Ti–6Al–4V alloy by air spraying and subsequent firing. The oxidation behavior of the specimens at 800 °C and 900 °C for 100 h was studied. The thermal shock resistance of the coating was tested by heating up to 900 °C and then quenching in water. The composite coating acted as an oxygen migration barrier and exhibited good resistance against high temperature oxidation, thermal shock, and oxygen permeation on the Ti–6Al–4V alloy. Coating/alloy interfacial reaction occurred, forming a Ti₅Si₃/Ti₃Al bilayer structure. A thin Al₂O₃ rich layer formed beneath the composite coating during oxidation at 900 °C.     

Combustion synthesis of FeAl−Al2O3 composites with TiB2 and TiC additions via metallothermic reduction of Fe2O3 and TiO2

Combustion synthesis involving metallothermic reduction of Fe₂O₃ and TiO₂ was conducted in the mode of self-propagating high-temperature synthesis (SHS) to fabricate FeAl-based composites with dual ceramic phases, TiB₂/Al₂O₃ and TiC/Al₂O₃. The reactant mixture included thermite reagents of 0.6Fe₂O₃+0.6TiO₂+2Al, and elemental Fe, Al, boron, and carbon powders. The formation of xFeAl−0.6TiB₂−Al₂O₃ composites with x=2.0−3.6 and yFeAl−0.6TiC−Al₂O₃ composites with y=1.8−2.75 was studied. The increase of FeAl causes a decrease in the reaction exothermicity, thus resulting in the existence of flammability limits of x=3.6 and y=2.75 for the SHS reactions. Based on combustion wave kinetics, the activation energies of E_a=97.1 and 101.1 kJ/mol are deduced for the metallothermic SHS reactions. XRD analyses confirm in situ formation of FeAl/TiB₂/Al₂O₃ and FeAl/TiC/Al₂O₃ composites. SEM micrographs exhibit that FeAl is formed with a dense polycrystalline structure, and the ceramic phases, TiB₂, TiC, and Al₂O₃, are micro-sized discrete particles. The synthesized FeAl−TiB₂−Al₂O₃ and FeAl−TiC−Al₂O₃ composites exhibit the hardness ranging from 12.8 to 16.6 GPa and fracture toughness from 7.93 to 9.84 MPa·m^1/2.     

First-principles study of the bonding characteristics of TiAl(111)/Al2O3(0001) interface

First principles calculations were carried out for α-Al₂O₃(0001) surface and γ-TiAl(111)/α-Al₂O₃(0001) interface to study the adhesion properties of the interface and to clarify the mechanisms that govern the adhesion of TiAl and its oxidation product Al₂O₃. Two type interface models, the TiAl(111) with Al- and O-terminated α-Al₂O₃(0001) surfaces denoted as T(A₁)-type and T(O_T)-type interface, respectively, were considered. The Universal Binding Energy Relation (UBER) was used to determine the separation between TiAl and Al₂O₃ and the work of adhesion of the γ-TiAl(111)/α-Al₂O₃(0001) interface. Optimization was then performed for all interfaces considered here using the separation obtained with UBER. The lowest work of adhesion is −1.05 J/m² for the T(A₁)-type interface and is −4.04 J/m² for the T(O_T)-type interface. There exists competition between O–Ti and O–Al (on the TiAl side) interactions; however O–Al bond is stronger than O–Ti bond because the main body of the Al valences is involved in the hybriding with O p electrons, while only part of the Ti d valence is involved in the O–Ti bonding. Thus the O–Al interaction dominates the adhesion between TiAl(111) and Al₂O₃(0001) surfaces, and it can be inferred that an Al-rich TiAl surface will favor the adhesion between TiAl/Al₂O₃.     

Correlation between oxidation resistance and crystallinity of Ti–Al as a barrier layer for high-density memories

The Ti–Al intermetallic material system has been investigated for application as a conducting diffusion barrier in a three-dimensional stacked capacitor–transistor geometry. La–Sr–Co–O (LSCO)/Pb–Zr–Ti–Nb–O/La–Sr–Co–O ferroelectric capacitors were fabricated on Ti–Al/polycrystalline-Si/Si substrates. The electrical and ferroelectric properties are found to correlate strongly with the crystallinity of the Ti–Al layer. The crystalline Ti–Al layer shows a distinct chemical reaction with the bottom LSCO electrode thus preventing ohmic electrical contact between the ferroelectric capacitor and transistor. In contrast, the amorphous Ti–Al layer does not react and forms an ohmic contact to LSCO. For crystalline Ti–Al, X-ray photoelectron spectroscopy (XPS) shows the formation of Al₂O₃ induced by the segregation of Al to the LSCO/Ti–Al interface. For amorphous Ti–Al, XPS reveals that no Al₂O₃ layer is formed. In addition, Rutherford backscattering analysis shows almost no difference in the Ti-peak spectrum before and after deposition of LSCO.