Microstructural evolution of intermetallic layer in hot-dipped aluminide mild steel with silicon addition

Mild steel was coated by hot-dipping into molten pure aluminum, Al-0.5 Si, Al-2.5 Si, Al-5 Si and Al-10 Si (wt.%) baths at 700 °C for 180 seconds. The microstructure and phase constitution of the aluminide layers were characterized by means of optical microscope, scanning electron microscope with energy dispersive X-ray spectroscopy, X-ray diffraction and electron backscatter diffraction. Also, the thicknesses of the intermetallic layers and the metal losses of the steel substrate were measured to investigate the interaction between mild steel and aluminum baths. The results revealed that the additions of silicon to the aluminum baths caused Al₇Fe₂Si and Al₂Fe₃Si₃ phases to form above the FeAl₃ layer and in the Fe₂Al₅ layer, respectively. As the silicon content in the aluminum bath increased, the thickness of the intermetallic layer decreased, and the intermetallic layer/steel substrate interface transformed from an irregular morphology into a flat morphology. The decrease of the thickness of the intermetallic layer was principally attributed to the detachment of the Al₇Fe₂Si layer from the intermetallic layer into the aluminum bath. The flattened intermetallic layer/mild steel substrate interface was due to the formation of Al₂Fe₃Si₃ precipitates in the Fe₂Al₅ layer by the serration-like steel substrate reacting with the Fe₂Al₅ layer containing solid-solute silicon.     

Si对铁铝固液扩散反应中间化合物生长动力学的影响(英文)

利用扫描电子显微镜能谱仪和热浸镀铝实验研究Si对铁铝固液扩散反应中间化合物生长动力学的影响。结果表明,中间层主要由Fe2Al5和薄层FeAl3组成。当向浸镀熔体中加入硅后,在镀层的Fe2Al5相中出现颗粒状的AlFeSi三元相(τ1/τ9)。舌状形貌的Fe2Al5层随着合金浴中Si含量的增加而逐步平整。合金浴中的Si显著抑制Fe2Al5和FeAl3的生长。当Si含量为0、0.5%、1.0%、1.5%、2.0%和3.0%时,Fe2Al5相的激活能分别为207、186、169、168、167和172kJ/mol。当Si原子进入Fe2Al5相时会引起晶格畸变,从而导致Fe2Al5的扩散激活能下降。Si原子占据空位时能够阻止扩散通道,抑制Fe2Al5相的生长,从而导致舌状形貌的消失。     

Effect of silicon on the formation of intermetallic phases in aluminide coating on mild steel

Mild steel was coated by hot-dipping into molten baths containing pure aluminum, Al–0.5Si, Al–2.5Si, Al–5Si and Al–10Si (wt.%) at 700 °C for 180 s. Silicon’s effect on the formation of the intermetallic phase in the aluminide layer was investigated by using a combination of scanning electron microscope (SEM), energy dispersive X-ray spectroscopy (EDS) and electron backscatter diffraction (EBSD). The micrograph observation showed that the aluminide layer resulting from hot-dipping in pure aluminum possesses the thickest intermetallic layer and a rough interface between intermetallic layer and steel substrate. As the silicon content in the molten bath increased, the thickness of the intermetallic layer decreased substantially and the interface between the intermetallic layer and the steel substrate became flat. On the other hand, EDS and EBSD observation revealed the aluminide layer resulting from hot-dipping in Al–2.5Si not only possessed FeAl₃ and Fe₂Al₅, but also formed cubic τ_5(C)-Al₇(Fe,M)₂Si (M = Mn, Cr or Cu) above the FeAl₃ and scattered τ₁-(Al,Si)₅Fe₃ in the Fe₂Al₅. However, as the content of silicon in the molten aluminum bath increased, τ_5(C)-Al₇(Fe,M)₂Si began to be replaced by hexagonal τ_5(H)-Al₇Fe₂Si and τ₆-Al₄FeSi.     

Microstructure and high temperature oxidation behavior of hot-dip aluminized coating on high silicon ductile iron

High silicon ductile iron was coated by hot-dipping into an Al molten bath. The oxidation behavior of the aluminized alloy and the bare substrate was studied in air at 750 °C. The results showed that the coating layers consisted of three layers, in the sequence of Al, Fe-Al intermetallic and Si pile-up layers from the external topcoat to the substrate. The intermetallic layer was composed of outer FeAl₃ and inner Fe₂Al₅. The outer rod-shaped FeAl₃ dispersed in the aluminum topcoat, while the inner tongue-like Fe₂Al₅ formed in the metallic layer becoming the major phase in the aluminide coating layer. Those three layers of aluminum, Fe₂Al₅ and silicon pile-up layer exhibited hardness of HV 50, HV 1100 and HV 450, respectively. In this study, when the as-coated specimens were examined, Fe-Al-Si compounds could not be found. But the silicon pile-up at the interface between the substrate and the Fe-Al intermetallic layer could be seen in all the as-coated specimens. The graphite nodules were noticed in the substrate. The presence of graphite nodules in the substrate might be markers of hot-dipping. After hot-dipping in Al all the specimens contained graphite nodules in the aluminide layer.The oxidized graphite nodules resulted in cracks propagating in aluminide coating. Even though graphite nodules meant the existence of crack in the aluminide coating, the high temperature oxidation experiments indicated that the aluminide coating could prevent the oxidation of substrate effectively even at 750 °C.     

Effect of alloying element segregation on the work of adhesion of metallic coating on metallic substrate: Application to zinc coatings on steel substrates

A thermodynamic model based on the ‘Macroscopic Atom’ approach is proposed to assess the effect of alloying element segregation on the adhesion of metallic coating on metallic substrate. The interfaces that occur in hot-dip galvanized steels are considered, which include: Zn/Fe, Zn/Fe₂Al₅, Zn/FeZn₁₃, FeZn₁₃/Fe₂Al₅, and Fe₂Al₅/Fe. The effect of the alloying element on the work of adhesion of these interfaces is investigated, which includes Mg, Al, Si, P, Ti, V, Cr, Mn, Fe, Ni, Zn, Nb, Mo, Sn and Bi. Among these elements, Bi, Sn and Mg are predicted to decrease the work of adhesion of the Zn/Fe interface, whereas P, Nb, Mo, V, Ti and Ni tend to enhance this adhesion. The effect of element M (M = Al, Si, Cr, Mn) is positive when it exists in the zinc coating or negative when it occurs in the iron substrate. Among these interfaces, the Fe₂Al₅/Fe interface with a value of 3.8 J m⁻² is the strongest, whereas the Zn/FeZn₁₃ interface with of a value of 1.7 J m⁻² is the weakest. Delamination of the coating upon deformation is predicted to occur along the FeZn₁₃/Fe₂Al₅ and Zn/Fe₂Al₅ interfaces. This agrees with microscopic observations of hot dip galvanized steel after tensile testing.     

The corrosion behavior of plasma sprayed Fe2Al5 coating in molten Zn

Aluminum coating was plasma sprayed on Fe-0.14-0.22 wt.% C steel substrate, and heat diffusion treatment at 923 °C for 4 h was preformed to the aluminum coating to form Fe₂Al₅ inter-metallic compound coating. The corrosion mechanism of the Fe₂Al₅ coating in molten zinc was investigated. SEM and EDS analysis results show that the corrosion process of the Fe₂Al₅ layer in molten zinc is as follows: Fe₂Al₅ → Fe₂Al₅Zn_x (η) → η + L(liquid phase) → L + η + δ(FeZn₇) → L + δ → L. The η phase and the eutectic structure (η + δ) prevent the diffusion of zinc atoms efficiently. Therefore the Fe₂Al₅ coating delays the reaction between the substrate and molten zinc, promoting the corrosion resistance of the substrate.     

The effect of hot-dipped aluminum coatings on Fe-8Al-30Mn-0.8C alloy

The morphology and microstructure of an intermetallic layer formed on the surface of Fe-8Al-30Mn-0.8C alloy by hot-dip aluminization treatment have been examined in detail. The phases present in the coating are unambiguously identified by means of transmission electron microscopy. After aluminization, a two layer coating was formed consisting of an external Al layer and a (Fe, Mn)₂Al₅ intermetallic on top of the substrate. The (Fe,Mn)₂Al₅ compound has an orthorhombic structure with lattice parameters a = 0.752 nm, b = 0.667 nm and c = 0.417 nm. The activation energy (E_FeMnAl) for the growth of such an intermetallic layer is calculated to be 52.7 kJ/mol. These results are different from those observed in aluminized low-carbon steel (E_Fe). The difference between E_FeMnAl and E_Fe is attributed to the alloying elements (Mn) in the present alloy. Environmental salt fog corrosion and high temperature oxidation tests were carried out to examine the corrosion and oxidation resistance. The results indicated that both the corrosion and oxidation resistance of the Fe-8Al-30Mn-0.8C alloy treated by hot-dip aluminization can be significantly increased.     

Effect of Si content on interfacial reaction and properties between solid steel and liquid aluminum

The effect of Si content on the microstructures and growth kinetics of intermetallic compounds (IMCs) formed during the initial interfacial reaction (<10 s) between solid steel and liquid aluminum was investigated by a thermophysical simulation method. The influence of Si addition on interfacial mechanical properties was revealed by a high-frequency induction brazing. The results showed that IMCs layers mainly consisted of η-Fe₂Al₅ and θ-Fe₄Al₁₃. The addition of Si reduced the thickness of the IMCs layer. The growth of the η phase was governed by the diffusion process when adding 2 wt.% Si to the aluminum melt. When 5 wt.% or 8 wt.% Si was added to aluminum, the growth was governed by both the diffusion process and interfacial reaction, and ternary phase τ₁/τ₉-(Al,Si)₅Fe₃ was formed in the η phase. The apparent activation energies of the η phase decreased gradually with increasing Si content. The joint with pure aluminum metal had the highest tensile strength and impact energy.     

Effect of Al‐Fe‐Si intermetallic compound phases on initiation and propagation of pitting attacks for aluminum 1100

It is well known that iron and silicon are major elements in industrial pure aluminum alloy 1100. These elements form Al‐Fe‐Si ternary intermetallic compounds such as FeAl₃, Fe₃SiAl₁₂, Fe₃Si₂Al₉, Fe₂Si₂Al₉ etc. The corrosion characteristics of the 1100 specimen and the Al‐Fe‐Si intermetallic compound specimens are experimentally investigated in NaCl and AlCl₃ solutions. The electrochemical measurements, SEM surface observation and EPMA analysis reveal that (1) the iron content of the compounds influences the initiation of pitting attacks: the higher content of iron in the compound is, the more easily occurs the initiation of pitting attack, and (2) an existence of the compound in the bottom of the active pitting cavity, whether the iron content of the compound is higher or not, contributes to the further propagation of pitting attack as a cathodic site.     

Analysis of intermetallic layer in dissimilar TIG welding–brazing butt joint of aluminium alloy to stainless steel

Abstract

Intermetallic layer of dissimilar tungsten inert gas welding–brazing butt joint of aluminium alloy/ stainless steel has been studied. A visible unequal thickness intermetallic layer has formed in welded seam/steel interface, and the thickness of the whole layer is <10 μm. The interface with Al–12Si filler metal consists of τ ₅-Al₈Fe₂Si layer in welded seam side and θ-(Al,Si)₁₃Fe₄ layer in steel side with the hardness values of 1025 and 835 HV respectively, while the interface with Al–6Cu filler metal consists of θ-Al₁₃(Fe,Cu)₄ layer with the hardness of 645 HV. The average tensile strength of the joint with Al–12Si filler metal is 100–120 MPa, and the fracture occurs at θ-(Al,Si)₁₃Fe₄ layer, while the joint with Al–6%Cu filler metal presents high crack resistance with tensile strength of 155–175 MPa, which reaches more than 50% of aluminium base metal strength.     

Microstructure evolution and mechanical properties of nanocrystalline FeAl obtained by mechanical alloying and cold consolidation

In the present study high energy mechanical milling followed by cold temperature pressing consolidation has been used to obtain bulk nanocrystalline FeAl alloy. Fully dense disks with homogenous microstructure were obtained and bulk material show grain size of 40 nm. Thermal stability of the bulk material is studied by XRD and DSC techniques. Subsequent annealing at a temperature up to 480 °C for 2 h of the consolidated samples enabled supersaturated Fe(Al) solid solution to precipitate out fine metastable Al₅Fe₂, Al₁₃Fe₄ and Fe₃Al intermetallic phases. Low temperature annealing is responsible for the relaxation of the disordered structure by removing defects initially introduced by severe plastic deformation. Microhardness shows an increase with grain size reduction, as expected from Hall-Petch relationship at least down to a grain size of 74 nm, then a decrease at smallest grain sizes. This could be an indication of some softening for finest nanocrystallites. The peak hardening for the bulk nanocrystalline FeAl is detected after isochronal ageing at 480 °C.     

Sequential interfacial intermetallic compound formation of Cu6Sn5 and Ni3Sn4 between Sn-Ag-Cu solder and ENEPIG substrate during a reflow process

The interfacial reactions between Sn-3.0 wt.% Ag-0.5 wt.% Cu solder and an electroless nickel-electroless palladium-immersion gold (ENEPIG) substrate were investigated. After initial reflowing, discontinuous polygonal-shape (Cu,Ni)₆Sn₅ intermetallic compounds (IMCs) formed at the interface. During reflowing for up to 60 min, the interfacial IMCs were sequentially changed in the following order: discontinuous (Cu,Ni)₆Sn₅, (Cu,Ni)₆Sn₅ and (Ni,Cu)₃Sn₄, and embedded (Cu,Ni)₆Sn₅ in (Ni,Cu)₃Sn₄. The interfacial product variation resulted from the preferential consumption of Cu atoms within the solder and continuous Ni diffusion from the Ni(P) layer.     

Suppressing effect of 0.5 wt.% nano-TiO2 addition into Sn-3.5Ag-0.5Cu solder alloy on the intermetallic growth with Cu substrate during isothermal aging

This study investigated the effects of adding 0.5 wt.% nano-TiO₂ particles into Sn3.5Ag0.5Cu (SAC) lead-free solder alloys on the growth of intermetallic compounds (IMC) with Cu substrates during solid-state isothermal aging at temperatures of 100, 125, 150, and 175 °C for up to 7 days. The results indicate that the morphology of the Cu₆Sn₅ phase transformed from scallop-type to layer-type in both SAC solder/Cu joints and Sn3.5Ag0.5Cu-0.5 wt.% TiO₂ (SAC) composite solder/Cu joints. In the SAC solder/Cu joints, a few coarse Ag₃Sn particles were embedded in the Cu₆Sn₅ surface and grew with prolonged aging time. However, in the SAC composite solder/Cu aging, a great number of nano-Ag₃Sn particles were absorbed in the Cu₆Sn₅ surface. The morphology of adsorption of nano-Ag₃Sn particles changed dramatically from adsorption-type to moss-type, and the size of the particles increased.The apparent activation energies for the growth of overall IMC layers were calculated as 42.48 kJ/mol for SAC solder and 60.31 kJ/mol for SAC composite solder. The reduced diffusion coefficient was confirmed for the SAC composite solder/Cu joints.     

Microstructure characterization of as-fabricated and 475 °C annealed U-7 wt.% Mo dispersion fuel in Al-Si alloy matrix

High-density uranium (U) alloys with an increased concentration of U are being examined for the development of research and test reactors with low enriched metallic fuels. The U-Mo fuel alloy dispersed in Al-Si alloy has attracted particular interest for this application. This paper reports our detailed characterization results of as-fabricated and annealed (475 °C for 4 h) U-Mo dispersion fuels in Al-Si matrix with a Si concentration of 2 and 5 wt.%, named as “As2Si”, “As5Si”, “An2Si”, “An5Si” accordingly. Techniques employed for the characterization include scanning electron microscopy and transmission electron microscopy with specimen prepared by focused ion beam in situ lift-out. Fuel plates with Al-5 wt.% Si matrix consistently yielded thicker interaction layers developed between U-Mo particles and Al-Si matrix, than those with Al-2 wt.% Si matrix, given the same processing parameters. A single layer of interaction zone was observed in as-fabricated samples (i.e., “As2Si”, “As5Si”), and this layer mainly consisted of U₃Si₃Al₂ phase. The annealed samples contained a two-layered interaction zone, with a Si-rich layer near the U-Mo side, and an Al-rich layer near the Al-Si matrix side. The U₃Si₅ appeared as the main phase in the Si-rich layer in “An2Si” sample, while both U₃Si₅ and U₃Si₃Al₂ were identified in sample “An5Si”. The Al-rich layer in sample “An2Si” was amorphous, whereas that in sample “An5Si” mostly consisted of crystalline U(Al,Si)₃, along with a small fraction of U(Al,Si)₄ and U₆Mo₄Al₄₃ phases. The influence of Si on the diffusion and reaction in the development of interaction layers in U(Mo)/Al(Si) is discussed in the light of growth-controlling mechanisms and irradiation performance.     

Effect of Ce and La additions in low temperature aluminization process by CVD-FBR on 12%Cr ferritic/martensitic steel and behaviour in steam oxidation

Two different coatings based of iron aluminide on 12% Cr ferritic-martensitic steel have been developed by CVD-FBR technique, which is modified by the introduction of Ce and La as powder in the fluidized bed. These elements change the gaseous environment, which composition is predicted by a thermodynamic approximation. Partial pressures of all gaseous precursors are drastically modified; in consequence AlCl has the highest partial pressure in the system leading to an increment of the coating thickness. Coatings are composed by (Fe, Cr)₂Al₅ or (Fe, Cr)₂Al₅ and (Fe, Cr)Al₃ intermetallic phases. On the other hand, steam oxidation test at 650 °C was performed in order to observe improvements in the HCM12A oxidation resistant.     

Effect of brazing parameters on microstructure and mechanical properties of titanium joints

This study investigates the influences of brazing temperature and time on microstructures and mechanical properties of commercially pure (CP) titanium. Bonding was performed in a high-vacuum furnace using Incusil-ABA (Ag–27.2Cu–12.5In–1.25Ti, wt.%), as filler metal. Brazing temperatures employed in this study were 710, 750, and 800 °C. At the same time, the investigated holding times at the brazing temperatures were 5, 30, and 90 min. Microstructure and phase constitution of the bonded joints were analyzed by means of metallography, scanning electron microscope (SEM) and X-ray diffraction pattern (XRD). An intense diffusion of Ti to the interface and a strong reaction between the braze alloy and the base metal were observed especially at a temperature of 800 °C. A number of intermetallic phases such as TiCu, Ti₂Cu, Ti₃In, Cu–In, and TiAg have been identified. Both brazing temperature and holding time are critical factors to control the microstructure and hence the mechanical properties of the brazed joints. The optimum brazing parameter was achieved at a temperature of 750 °C and a holding time of 90 min.     

Brazing of 6061 aluminum alloy/Ti-6Al-4V using Al-Si-Cu-Ge filler metals

Al-8.4Si-20Cu-10Ge and mixed rare-earth elements (Re) containing Al-8.4Si-20Cu-10Ge-0.1Re filler metals were used for brazing of 6061 aluminum alloy/Ti-6Al-4V. The addition of 20 wt.% copper and 10 wt.% germanium into the Al-12Si filler metal lowered the solidus temperature from 586 °C to 489 °C and the liquidus temperature from 592 °C to 513 °C. The addition of 0.1 wt.% rare-earth elements into Al-8.4Si-20Cu-10Ge alloy caused remarkable Al-rich phase refinement and transformed the needle-like Al₂Cu intermetallic compounds into block-like shapes. Shear strengths of the 6061 aluminum alloy/Ti-6Al-4V joints with the two brazing filler metals, Al-8.4Si-20Cu-10Ge and Al-8.4Si-20Cu-10Ge-0.1Re, varied insignificantly with brazing periods of 10-60 min. The average shear strength of the 6061 aluminum alloy/Ti-6Al-4V joints brazed with Al-8.4Si-20Cu-10Ge at 530 °C was about 20 MPa. Rare-earth elements appeared to improve the reaction of the Al-8.4Si-20Cu-10Ge filler metal with Ti-6Al-4V. The joint shear strength of the 6061 aluminum alloy/Ti-6Al-4V with Al-8.4Si-20Cu-10Ge-0.1Re reached about 51 MPa.     

Effect of iron-containing intermetallic particles on the corrosion behaviour of aluminium

The effect of heat treatment on the corrosion behaviour of binary Al-Fe alloys containing iron at levels between 0.04 and 0.42 wt.% was investigated by electrochemical measurements in both acidic and alkaline chloride solutions. Comparing solution heat-treated and quenched materials with samples that had been subsequently annealed to promote precipitation of Al₃Fe intermetallic particles, it was found that annealing increases both the cathodic and anodic reactivity. The increased cathodic reactivity is believed to be directly related to the increased available surface area of the iron-containing intermetallic particles acting as preferential sites for oxygen reduction and hydrogen evolution. These particles also act as pit initiation sites. Heat treatment also causes depletion in the solute content of the matrix, increasing its anodic reactivity. When breakdown occurs, crystallographic pits are formed with {1 0 0} facets, and are observed to contain numerous intermetallic particles. Fine facetted filaments also radiate out from the periphery of pits. The results demonstrate that the corrosion of aluminium is thus influenced by the presence of low levels of iron, which is one of the main impurities, and its electrochemical behaviour can be controlled by heat treatment.