Development of TiB<Subscript>2</Subscript> reinforced in-situ Ti aluminide matrix composite through reaction synthesis

TiB₂ reinforced in-situ titanium aluminide matrix composite was made through reaction synthesis process using high purity elemental powders of Ti, Al, Cr, Nb and B. XRD of the synthesized block showed presence of mainly Al₃Ti and TiB₂ phases. To obtain γ Ti aluminide based matrix, the material was homogenized in two phase region (α₂+γ). Presence of γ phase matrix alongwith α₂ was confirmed through XRD, SEM and TEM. Uniform distribution of TiB₂ phase was confirmed through elemental mapping and by analyzing specimens of different locations. Differential scanning calorimetry of powder mixture showed presence of endothermic peak for Al melting and exothermic peak of Ti aluminide and TiB₂ formation.     

Evaporation behavior of aluminum during the cold crucible induction skull melting of titanium aluminum alloys

Taking the Ti-Al binary alloy as an example, this article studied the evaporation behavior of Al during the cold crucible induction skull melting (ISM) process of titanium alloys. A formula was deduced to predict the activity of Al in a molten Ti-Al binary system. The calculated activity of Al negatively deviates from an ideal solution. A model was established to judge the evaporation controlling mode and, on this basis, several conclusions were obtained. (1) The evaporation controlling mode of Al in molten Ti-Al transfers from the evaporation reaction controlling mode to the double controlling mode (diffusion and evaporation reaction) with increasing melt temperature (T _ms) and/or Al content (x _Al) and/or decreasing pressure (P) in the melting chamber. (2) The expression P≤P _crit (P _crit≈0.44 P _e(Al)) is a criterion used to judge whether the evaporation is in the state of free evaporation. (3) The term P _impe (P _impe=(3.5 to 4) P _e(Al)) is a critical value which impedes the evaporation loss. Almost all of common used ternary additions could enhance the activity of Al in molten Ti-Al and, accordingly, aggravate the evaporation of Al, except for Zr. The enhancing sequence is Y, Ni, Nb, Mn, V, Fe, Cr, Mo, Cu, Si, W, Mg, B, and Sn. The Al evaporation mass-transfer losses, measured from the melting experiments of several titanium aluminum alloys, were in reasonable agreement with the calculated results.     

Electron Beam Melting of High Niobium Containing TiAl Alloy: Feasibility Investigation

Third generation γ‐TiAl alloys with a high niobium content, Ti–(47–48)Al–2Cr–8Nb, were processed by electron beam melting (EBM). This near‐net‐shape additive manufacturing process produces complex parts according to a CAD design. The starting powder is deposited layer by layer on the building table and selectively melted to progressively form the massive part. The EBM parameters such as layer thickness, melting temperature, scanning speed, or building strategy were set up to minimize porosity. The chemical composition of the built material is similar to the composition of the base powder despite a slight evaporation of aluminum and reveals a neglectable oxygen pick‐up. The very fine equiaxed microstructure resulting after EBM can be then set up by heat treatment (HT). According to the HT temperature in particular, an equiaxed microstructure, a duplex microstructure with different lamellar ratio and a fully lamellar microstructure is obtained. Not only test bars have been produced but also complex parts such as demo low pressure turbine blades.     

Effect of alloying additions on the structure and mechanical properties of Fe<Subscript>3</Subscript>Al -1C intermetallic alloy

Effect of titanium and nickel on the structure and properties of Fe₃Al intermetallic alloy containing about 1.0wt.% C have been investigated. The composition of the alloying element was substituted for Iron. The alloys were prepared by melting commercial grade raw materials iron, aluminum, titanium or nickel in air induction furnace with flux cover (AIMFC). Further these ingots were refined by electroslag refining (ESR) process. These ingots could be successfully hot-worked using conventional hot-forging and hot-rolling techniques. The hot-worked material was sound and free from cracks. ESR hot-rolled alloys were examined using optical microscopy, X-ray diffraction (XRD), scanning electron micrograph (SEM) to understand the microstructure of these alloys. The electron probe micro analysis (EPMA) studies were carried out to determine the matrix and precipitate compositions and to identify the phases present in the alloys. The base alloy and the alloy containing Ni exhibited a two-phase microstructure of Fe₃AlC_0.5 precipitates in Fe₃Al matrix. The alloy containing Ti exhibits three-phase microstructure, the additional phase being TiC precipitate. Ti addition resulted in no improvement in strength at room temperature and at 873 K whereas Ni addition has resulted in greater improvement in strength at room temperature and at 873 K and also improved the creep life significantly from 66 hrs to 111 hrs.     

Effect of Al antioxidant in MgO–C refractory on the formation of Al2O3-rich inclusions in high-carbon steel for saw wire under vacuum conditions

Al₂O₃-rich (>70?wt-%) inclusions generally hard and non-deformable are extremely detrimental for saw wire. In order to explore the source of this type of inclusion and provide solutions, experiments on the interaction between Al-containing MgO–C refractory and high-carbon steel for saw wire was conducted on a laboratorial scale using a cold crucible levitation melting furnace under vacuum conditions. [Al]_S (acid-soluble Al), [C] and [Mg] concentrations in steel, Al₂O₃ concentration in inclusions and microstructure of refractory/steel interface, etc. were analysed to clarify the influence of vacuum pressure, refractory addition amount and interaction time. Based on the experimental results and thermodynamic calculations, a presumable impact mechanism of Al antioxidant in MgO–C refractory on the formation of Al₂O₃-rich inclusions in high-carbon steel for saw wire under vacuum conditions was deduced, which in turn provided a reference for the control of Al₂O₃-rich inclusions in high-carbon steel for saw wire.     

超低氧精炼时钙处理对氧化物夹杂的影响

 研究了采用LF精炼顶渣控制技术对钢液进行超低氧冶炼时,钙处理对钢中非金属夹杂物的影响。试验在转炉出钢时采用铝终脱氧,LF精炼过程采用强脱氧、高碱度、强还原性精炼顶渣对钢液进行超低氧冶炼,比较了钙处理和不钙处理的钢液中非金属夹杂物转变的情况。结果表明,采用精炼顶渣控制技术冶炼超低氧钢时,钢液不需要进行钙处理就能实现铝脱氧产物Al2O3→MgO·Al2O3尖晶石→CaO-MgO-Al2O3类复合夹杂物的转变,得到炼钢温度下呈液态的复合氧化物夹杂,这些液态的夹杂物容易通过碰撞长大上浮去除,得到高洁净度的钢液,且残留在钢液的氧化物夹杂为较低熔点的复合氧化物,在浇注过程中不会产生水口结瘤。     

Effect of Acid-Soluble Aluminum on the Evolution of Non-metallic Inclusions in Spring Steel

The content of acidic soluble aluminum in molten steel ([Al]_s) is of significance to the control of total oxygen (TO), the formation of non-metallic inclusions, and the improvement of the surface quality of billets. Industrial trials and thermodynamic calculations were performed to study the effects of [Al]_s content on the TO and the evolution of non-metallic inclusions in 60Si2Mn-Cr spring steel that was deoxidized by Si-Mn ((low aluminum process (LAP)) and Si-Mn-Al (high aluminum process (HAP)). The results show that the [Al]_s contents in billets are within 0.0060 to 0.0069 mass pct in the LAP and 0.016 to 0.055 mass pct in the HAP. The TO content at each station of the LAP is higher than that in the HAP; the inclusions of billets were mainly of the CaO-Al₂O₃-SiO₂ type in the former, and of the CaO-Al₂O₃-MgO and CaS-Al₂O₃-MgO types in the latter. A tendency is found that the higher the [Al]_s, the easier it is to deviate from the low melting point region of the inclusion distribution and the larger the size of the inclusions. The relationships between [Al]_s and the melting point of the oxide inclusions and the Al₂O₃ content in the oxide inclusions are also discussed in terms of experiment and calculation.     

Development of Mo(Si,Al)<Subscript>2</Subscript>-base oxidation-resistant coating on Nb-base structural materials

Mo(Si,Al)₂-base oxidation-resistant coatings for Nb-base structural materials have been studied. The coating is composed of a Mo(Si,Al)₂-base Al reservoir and Al₂O₃ interlayer to suppress interface reactions between the Al reservoir and the substrate. To develop a suitable Al-reservoir material, some Mo(Si_0.6,Al_0.4)₂-HfB₂ composites were prepared. Their oxidation resistance and coefficients of thermal expansion were investigated, in addition to their chemical reactivity with the Nb substrate at high temperatures. As a result, Mo(Si_0.6,Al_0.4)₂-20 vol pct HfB₂ was selected as one of the satisfactory Al reservoirs. The introduction of a stable Al₂O₃ interlayer was attempted using a novel powder metallurgical process to overlay the Nb substrates with the Al reservoir, where the Nb substrates were subjected to a slight surface oxidation prior to the coating process. The Nb specimens, which are thoroughly coated with the Al reservoir and Al₂O₃ interlayer, can be successfully fabricated by this method. The coated Nb specimens are not damaged at all after prolonged exposure in flowing Ar-20 pct O₂ at 1673 K for 120 hours. Furthermore, the Al₂O₃ interlayer is very effective and no reactions occur at the interface. Thus, this Mo(Si,Al)₂-base oxidation-resistant coating is applicable to Nb. The utility of the coating system is also confirmed for a Nb_SS/Nb₅Si₃ composite. This article is based on a presentation made in the symposium entitled “Beyond Nickel-Base Superalloys,” which took place March 14–18, 2004, at the TMS Spring meeting in Charlotte, NC, under the auspices of the SMD-Corrosion and Environmental Effects Committee, the SMD-High Temperature Alloys Committee, the SMD-Mechanical Behavior of Materials Committee, and the SMD-Refractory Metals Committee.     

顶渣对帘线钢中夹杂物塑性化的控制

以某钢厂生产的帘线钢铸坯试样为原料,使用硅钼棒炉对其进行顶渣熔炼实验,研究顶渣成分对CaO-Al2O3-SiO2 类夹杂物塑性化的影响。结果表明, 在顶渣碱度为0.8～1.2时,随着顶渣中Al2O3 质量分数的增加夹杂物中的Al2O3 质量分数也随之增加。当顶渣中Al2O3质量分数低于10%时,CaO-Al2O3-SiO2 类夹杂物的成分在塑性区范围,对应的此时钢液中的w［Al］s低于8×10-6。通过控制顶渣的成分可以把CaO-Al2O3-SiO2 类夹杂物的成分控制在塑性区内。     

典型含钛超纯铁素体不锈钢冶炼-连铸过程夹杂物衍变研究

通过热力学分析、扫描电镜和EDS能谱分析等方法,系统研究了一种典型含钛超纯铁素体不锈钢（/%:≤0.01C,17.5～18.5Cr,0.40～0.55Nb,0.10～0.25Ti）80 t K-OBM-S-VOD-LF-200 mm×1 240 mm CCM过程夹杂物的衍变。结果表明,VOD还原期采用Si-Al复合脱氧,夹杂物类型以Al2O3-CaO-SiO2-MgO和Al2O3-CaO-MgO为主,钛合金化后夹杂物转变为Al2O3-CaO-TiOx-MgO,由于此类夹杂物熔点高、尺寸大,且很难通过钙处理变性,容易聚集造成水口堵塞。通过提高铝钛比至0.11以上,降低钛合金化前钢中全氧含量至25×10-6以下,使用纯净的钛铁合金可以避免形成大尺寸的含TiOx夹杂物。     

Inclusion modification in Al-killed valve spring steel by Na2CO3 addition

Hard inclusions with high melting temperatures such as Al₂O₃ (2054°C) and MgO·Al₂O₃ (2135°C) generate nozzle blockage problems during continuous casting of Al-killed valve spring steel and are very detrimental with respect to fatigue properties. In the present paper, inclusion modification in Al-killed valve spring steel by Na₂CO₃ addition was investigated in the laboratory using a graphite tube resistance furnace. The results show that inclusions with high melting temperature can be successfully modified into Na₂O-containing inclusions with lower melting temperatures by the addition of Na₂CO₃. The effectiveness of inclusion modification can be enhanced by increasing the Na₂CO₃ addition and/or decreasing the amount of Al. This suggests that Na₂CO₃ addition could possibly be a substitute for Ca treatment as a method for preventing nozzle blockage during continuous casting of Al-killed steel.     

真空电磁悬浮精炼钛铝基中间合金试验研究

利用真空电磁悬浮熔炼炉对铝热法还原攀枝花酸溶性钛渣所得的粗TiAl基合金进行精炼,研究了精炼前后合金物相组成、合金元素在微区中的分布、组织结构和杂质含量的变化。发现在精炼参数为熔炼电流60A,保温时间5min,冷却速率4A/min时,精炼后的合金层片状组织和裂纹减少,晶粒尺寸减小。Si、Fe元素置换Al元素形成置换固溶相,存在于TiAl、TiAl_2等相中,形成了Fe_2AlTi、Si_2Ti、Al_2FeSi、AlFe、FeTiSi等物相,接近于Ti-Al二元合金的双相组织。合金中夹杂物的含量减少了45%,去除了合金中的粒径5μm的大颗粒夹杂物。     

Amorphization of Al50(Fe2B)30Nb20 Mixture by Mechanical Alloying

An amorphous Al₅₀(Fe₂B)₃₀Nb₂₀ powder mixture was prepared by mechanical alloying in a high-energy planetary ball-mill under argon atmosphere. Morphologic, microstructural, and structural changes during the milling process were followed by scanning electron microscopy and X-ray diffraction. Rietveld analysis of X-ray diffraction patterns was used to follow the solid-state amorphization transformation during the milling process of the prepared powder. The reaction between elemental Al, Fe₂B, and Nb powders leads to the formation of the Al(Fe,B) and Al(Fe,Nb,B) solid solutions after 4 and 6 hours of milling, respectively. An amorphous structure is achieved after 20 of milling. These amorphous powders are crystallized on further milling time (36 hours). The observation by scanning electron microscope shows a phenomenon of fracturing followed by compaction of the powder particles.     

Layered composites made from bimetallic strips produced by plasma spraying of TiAl on niobium

The production and structure of a multilayer TiAl/Nb composite material made from bimetallic TiAl/Nb strips fabricated by plasma spraying of TiAl granules onto niobium plates are studied. Here, 3-mm-and 2-mm-thick plates of a layered composite material (LCM) are produced by hot isostatic pressing of a stack of 35 bimetallic plates followed by hot rolling (the total degree of reduction is 78.6 and 85.7%, respectively). The LCM consists of discontinuous TiAl layers separated by niobium layers, and the adhesion between the layers is good. Diffusional intermediate layers form at the TiAl/Nb interfaces in the 3-mm-thick LCM and consist of the following two solid solutions: an α₂-Ti₃Al-based solid solution contains up to 28 at % Nb, and a niobiumbased solid solution contains up to 27 at % Ti and 32 at % Al. The diffusional intermediate layers in the 2-mmthick LCM plates consist of an α₂-Ti₃Al-based solid solution with up to 16.0 at % Nb; a τ-Ti₃Al₂Nb-or Ti₄Al₃Nb-based solid solution with 51.5 at % Ti, 32 at % Al, and 16.5 at % Nb; and a niobium-based solid solution with up to 22 at % Ti and 30.5 at % Al. When a bimetallic TiAl/Nb strip is fabricated by plasma spraying of granules of the Ti-48 at % Al alloy, this alloy is depleted of aluminum to 42–45 at %, and the fraction of the α₂-Ti₃Al phase in the sprayed layer increases. When the LCM is produced by hot isostatic pressing followed by hot rolling, the layer of plain niobium (Nb1) dissolves up to 5 at % Ti and 7 at % Al.     

Intermetallic compound layer growth at the interface of solid refractory metals molybdenum and niobium with molten aluminum

The growth mechanisms and growth kinetics of intermetallic phases formed between the solid refractory metals Mo and Nb and molten aluminum have been studied for contact times ranging from 1 to 180 minutes at various temperatures in the range from 700 to 1100°C. The growth of the layers of the resulting intermetallic phases has been investigated under static conditions in a saturated melt and under dynamic conditions using forced convection in unsatured aluminum melts. The Nb/Al interfacial microstructure consisted of a single intermetallic phase layer, Al₃Nb, whereas two to four different phase layers were observed in the Mo/Al interface region, depending upon the operating temperature. It was found that, in a satured melt, the intermetallic phase growth process was diffusion-controlled. The parabolic growth constants of the first and second kind and integral values of the chemical diffusion coefficients over the widths of the phases were calculated for both Mo/Al and Nb/Al systems. It also was found that the AlNb₂ phase grew between the Nb and Al₃Nb phases after consumption of the saturated Al phase. Similarly, the AlMo₃ phase grew between the Mo and Al₈Mo₃ phases with diminishing of all the other existing compound phases. In an unsaturated melt, the intermetallic phase layer grows at the solid surface while, simultaneously, dissolution occurs at the solid/liquid interface. This behavior is compared to the growth mechanisms proposed in existing theories, taking into consideration that interaction occurs between neighboring phases. It was found that the intermetallic phase, Al₈Mo₃, adjoining the base metal, was not bonded strongly to the base metal Mo and was brittle; its hardness also was larger than that of the layer near the adhering aluminum and the adjacent phases.     

Research of microalloy elements to induce intragranular acicular ferrite in shipbuilding steel

Based on the minimum degree of disregistry mechanism in oxide metallurgy, laboratory and industrial research have been conducted on intragranular acicular ferrite (IAF) induced by microalloying elements in austenite. Based on the chemical compositions of DH36 steel and Mg, Al, Ti, V, Nb microalloyed steel, experimental results show that in ingots' organization, both V and Nb can induce IAF, but when the adding sequence was Al-Mg-Ti, smaller and dispersion inclusions were formed in austenite. When the Mg content was 0.005 wt%, the inclusion structure induced IAF in austenite is as follows: MgO and Al₂O₃ forms the core and TixOy adheres to the Al-Mg complex inclusions to produce smaller particle size and dispersions of Al, Mg, Ti complex inclusions. Finally, upon lowering the temperature, carbonitrides of Ti, V, and Nb were precipitated on the outermost layer of the inclusions. These carbonitrides with small disregistry contribute to induce intragranular acicular ferrite.     

钛对铌微合金化钢夹杂物析出行为的影响

采用高频真空感应炉在1 550℃的Ar气氛中冶炼不同钛含量的钛、铌微合金化钢并对其进行热处理。分析了钛加入量对钢的成分、组织结构、钢中典型夹杂物及宏观力学性能的影响。研究结果表明:采用Al脱氧后的钛、铌微合金化钢氧含量降低到0.002 0%左右,合金元素的利用率超过80%。钢中的夹杂物主要有球形或近似球形的Al2O3、SiO2、TiOx及其复合夹杂。(Ti,Nb)(C,N)、NbC、TiC夹杂以氧化物夹杂为核心析出。随着钛合金加入量的增加,钢样中的部分夹杂物形貌由球形发展成长方形。经共聚焦激光扫描高温显微镜热处理过的钢样中析出较多细小的(Ti,Nb)(C,N)夹杂物。随着钛含量的增加,热处理后的钢中小于1μm夹杂物数量急剧增加,尺寸大于1μm的夹杂物的数量呈现减少的趋势。高温在线金相组织分析表明:钢中钛加入量增加,高温奥氏体晶粒变小,钢的组织细化,从而钢的宏观硬度增高。     

钢包喂CaSi线对钢中夹杂物变性的影响

在生产铝镇静钢的工艺条件下,研究了钢包喂Ｃａｓｉ线处理后钢中夹杂物的组成、形态、尺寸和分布等的变化规律。结果表明,喂线后钢中钙铝比达到０．０９以上时,钢中的Ａｌ２Ｏ３类夹杂物能获得较好的变性;夹杂物中的钙铝比随喂线后钢中钙铝比的增大呈线笥增加趋势;较高的钢中钙铝比有利于连铸坯中大颗粒夹杂物的去除,有利于钢中夹杂物球化率的提高。     

Microstructure evolution of Ti48AlχNb γ intermetallics

The microstructures of Ti48Al alloys containing either 2 at.% or 8 at.% Nb have been studied in as-cast, as-HIPped and in heat-treated samples. The as-cast Ti48Al2Nb and Ti48Al8Nb are heterogeneous and lower Nb content has been detected in the interdentritic γ by EDX analysis. Depending on the heat-treatment temperature and cooling rate, the microstructure obtained vary from martensitic structure in the water quenched samples to duplex structure consisting of γ grains and lamellar α₂/γ and to fully lamellar structure in the furnace cooled samples. Nb was found to have a high solubility in both α and γ phases and to expand the γ phase region so that a fully γ structure is obtained in the Ti48Al8Nb sample by annealing at 1200°C. A dense array of planar defects (antiphase boundaries, stacking faults and microtwins) was obtained in the Ti48Al8Nb alloy water quenched from 1400°C.     

坩埚材质及顶渣成分对帘线钢夹杂物成分的影响

 使用碳管炉熔炼帘线钢72A,研究不同材质坩埚及不同成分顶渣对钢中夹杂物的影响。结果表明,MgO坩埚冶炼的帘线钢中夹杂物变形率高于ZrO2、SiO2、Al2O3坩埚。采用SiO2坩埚冶炼时,钢中夹杂物几乎不变形,其SiO2含量大于90%(质量分数,下同)。采用Al2O3坩埚,个别夹杂物Al2O3的含量达到40%左右,不适合冶炼帘线钢。钢中夹杂物成分进入较低熔点区(即不大于1500℃的区域)的条件为：采用MgO坩埚,顶渣碱度为10时,wAl2O3≤3%,或顶渣碱度为09时,wAl2O3为9%;采用ZrO2坩埚时,顶渣碱度为11~12时,wAl2O3为3%。