X-ray diffraction and TEM analysis of Fe–Al alloy layer in coating of new hot dip aluminised steel

Abstract

The phase structure in the Fe-Al alloy layer of a new hot dip aluminised steel has been researched by means of electron probe microanalysis, X-ray diffraction and TEM, etc. The test results indicated that the Fe-Al alloy layer of the new aluminised steel was composed of Fe₃Al, FeAl, a few Fe₂Al₅ and α-Fe (Al) solid solution. There was no brittle phase containing higher aluminium content, such as FeAl₃ (59.18 wt-%Al) and Fe₂Al₇ (62.93 wt-%Al). The tiny cracks and brittlement, formerly caused by these brittle phases in the conventional aluminium coated steel, were effectively eliminated. There was no microscopic defect (such as tiny cracks, pores or loose) in the coating. This is favourable for resisting high temperature oxidation and corrosion of the aluminised steel.     

Characteristics of phase constitution in the Fe-Al alloy layer of calorized steel pipe

Microhardness, aluminium content and phase constitution characteristics in the Fe-Al alloy layer of calorized steel pipe were investigated by optical microscopy, microhardness measurements, SEM, electron probe microanalysis, TEM and X-ray diffractometry, etc. Experimental results indicate that the Fe-Al alloy layer of calorized steel pipe was mainly composed of FeAl phase (2.0%–36% Al), Fe₃Al phase (13.9%–20% Al) and α-Fe (Al) solid solution, and the microhardness in the Fe-Al alloy layer was 600-310 HM from the surface layer to the inside. There were no higher aluminium content phases, such as brittle FeAl₂, Fe₂Al₅ and FeAl₃. The ability to resist deformation and the weldability of the calorized steel pipe were remarkably improved.     

The crack propagating behavior of composite coatings prepared by PEO on aluminized steel during in situ tensile processing

This paper investigates the in situ tensile cracks propagating behavior of composite coatings on the aluminized steel generated using the plasma electrolytic oxidation (PEO) technique. Cross-sectional micrographs and elemental compositions were investigated by scanning electron microscopy (SEM) equipped with energy dispersive spectroscopy (EDS). The composite coatings were shown to consist of Fe-Al, Al and Al₂O₃ layers. The cracks propagating behavior was observed in real-time in situ SEM tensile test. In tensile process, the cracks were temporarily stopped when cracks propagated from Fe-Al layer to Al layer. The critical crack opening displacement δ_c was introduced to quantitatively describe the resistance of the Al layer. There was a functional relation among the thickness ratio tAl/tAl₂O₃, the δ_c of composite coatings and tensile cracks’ spacing. The δ_c increased with the increasing of the thickness ratio (tAl/tAl₂O₃). The high δ_c value means high fracture resistance. Therefore, a control of the thickness ratio tAl/tAl₂O₃ was concerned as a key to improve the toughness and strength of the aluminized steel.     

Interfacial microstructures and properties of aluminum alloys/galvanized low-carbon steel under high-pressure torsion

A new composite processing technology characterized by hot-dip Zn–Al alloy process was developed to achieve a sound metallurgical bonding between Al–7 wt% Si alloy (or pure Al) castings and low-carbon steel inserts, and the variations of microstructure and property of the bonding zone were investigated under high-pressure torsion (HPT). During hot-dipping in a Zn–2.2 wt% Al alloy bath, a thick Al₅Fe₂Zn_x phase layer was formed on the steel surface and retarded the formation of Fe–Zn compound layers, resulting in the formation of a dispersed Al₃FeZn_x phase in zinc coating. During the composite casting process, complex interface reactions were observed for the Al–Fe–Si–Zn (or Al–Fe–Zn) phases formation in the interfacial bonding zone of Al–Si alloy (or Al)/galvanized steel reaction couple. In addition, the results show that the HPT process generates a number of cracks in the Al–Fe phase layers (consisting of Al₅Fe₂ and Al₃Fe phases) of the Al/aluminized steel interface. Unexpectedly, the Al/galvanized steel interface zone shows a good plastic property. Beside the Al/galvanized steel interface zone, the microhardnesses of both the interface zone and substrates increased after the HPT process.     

Analysis of the microstructure and phase constitution of the Fe3Al/18-8 diffusion interface after re-heating

The existence of coarse precipitation blocked the diffusion of the atoms and caused the uneven distribution of elements at the Fe₃Al/18-8 interface zone. Especially, the brittle precipitation could induce welding cracks directly. Consequently, it was one of the main factors that caused the failure of the joint. The Fe₃Al/18-8 diffusion-bonded joint was re-heated and the precipitation and phase constitution of the interface were analysed by means of scanning electron microscope (SEM), energy dispersive spectrum (EDS) and X-ray diffraction (XRD). The results indicated that the precipitation became tiny and regular and distributed evenly due to re-heating. The brittle precipitation zone was liquified to become a smooth and homogeneous diffusion zone. There were no high-microhardness brittle phases such as FeAl₂ and Fe₂Al₅ near the Fe₃Al/18-8 diffusion interface after re-heating.     

Oxidation Resistance of the Aluminide Coating Formed on Carbon Steels

Low and medium carbon steels were aluminized by the pack aluminizing technique using halideactivated pure-Al and Fe-Al packs. The effect of mixture composition, aluminizing temperatureand time and C content of the steel substrate on the structure and thickness of the aluminidelayer, and on the oxidation resistance was investigated. The optimum oxidation resistance canbe achieved with a low carbon steel substrate when the intermetallic phases Fe3Al and FeAlform the surface of the aluminide layer. In this case, the Al concentration at the surface of thealuminide coating is at least ≥15 wt pct. Formation of high Al concentration phases (FeAl3 andFe2Al5) during aluminizing should be avoided as they tend to embrittle the aluminide layer andreduce its oxidation resistance.     

Investigation of the formation of Al,Fe, N intermetallic phases during Al pack cementation followed by plasma nitriding on plain carbon steel

Plain carbon steels are not suitable for nitriding as they form an extremely brittle case that spalls off readily, and the hardness increment of the diffusion zone is small. In this research, the effect of plasma nitriding time and temperature variation on the microstructure of the pack cemented aluminized plain carbon steel is investigated. All samples were aluminized at 900 °C for 2 h; the aluminized samples were subsequently plasma nitrided at 500 °C, 550 °C and 600 °C for 2.5, 5, 7.5 and 10 h. The phases formed on the sample surface were detected by X-ray diffraction (XRD). The cross section and samples surface were investigated by optical and scanning electron microscopy (SEM). Microhardness test was conducted to determine hardness change from the surface to the sample core. Results showed that by aluminizing the steel, Fe₃Al phases as well as Fe–Al solid solution were formed on the surface and some aluminum rich precipitates were formed in solid solution grain boundaries. Plasma nitriding of the aluminized layer caused the formation of aluminum and iron nitride (AlN, Fe₄N) on the sample surface. Consequently, surface hardness was improved up to about eight times. By increasing the nitriding temperature and time, aluminum-rich precipitates dissociated. Moreover, due to the diffusion of nitrogen through aluminized region during ion nitriding, iron and aluminum nitrides were formed in aluminized grain boundaries. Increasing nitriding time and temperature lead to the growth of these nitrides in the grain boundaries of the substrate. This phenomenon results in the increment of sample hardness depth. Plasma nitriding of aluminized sample in low pressure chamber with nitrogen and hydrogen gas mixture reduced surface aluminum oxides which were formed in aluminizing stage.     

汽车用热镀锌板Fe—Al合金层的研究

用Ｘ射线衍射，萃取碳复型样品的电子衍射等方法对汽车用热镀反Ｆｅ－Ａｌ合金的组织结构进行了分析，结果表明，当锌液中的Ａｌ浓度小于０．１５％时，Ｆｅ－Ａｌ层主要由Ｆｅ２Ａｌ５金属间化合物组成。     

热浸镀铝球墨铸铁失效机理研究

采用VK-9710型激光共聚焦显微镜对热浸镀铝球墨铸铁试样的三点弯曲失效过程进行原位观察,分析镀层和基体的裂纹萌生和扩展机理。结果表明:对于纯Al浸镀球墨铸铁,在拉应力作用下,铁铝合金镀层率先萌生裂纹,诱导临近基体中铁素体撕裂与石墨球剥离,裂纹近似垂直于拉应力方向并沿着临近石墨球最短途径扩展;压应力导致表面纯Al层剥离和铁铝合金层破碎,镀层失效对球墨铸铁基体基本无影响。对于Al-3.7Si-1.0RE浸镀球墨铸铁,拉应力作用下的失效机理与纯Al浸镀相似;压应力作用下纯Al层和铁铝合金层与基体脱开,表现为铁素体基体失效。     

不同基体热浸镀铝镀层组织和高温磨损行为

选取45钢和H13钢进行热浸镀铝和高温扩散处理,采用X射线衍射(XRD)、扫描电镜(SEM)、能谱仪(EDS)等微观分析手段表征镀层物相、形貌和成分。采用销盘式高温磨损试验机对比研究不同基体下镀层的干滑动高温磨损行为,并探讨其磨损机制。结果表明:扩散层均以FeAl和Fe_3Al韧性相为主,两相之间界面周围存在平行于表面的Kikendall孔洞;镀层与45钢基体过渡平缓,结合良好,而与H13钢界面之间存在颗粒聚集,导致镀层与H13钢基体结合较差;45钢镀层在400℃/50~200N具有较好耐磨性,随环境温度升高,出现轻微-严重的磨损转变;H13钢镀层在400℃磨损率较低,在600℃也仅略高于400℃;Fe-Al镀层的磨损机制以氧化轻微磨损为主,45钢镀层在600℃出现塑性挤出磨损。     

镁含量和硅对铁-锌铝镁合金固-液扩散偶中Fe-Al反应层的影响

在热浸镀锌中,铁基表面Fe-Al化合物层的形成会影响镀层的生长和质量。将Fe/(Zn-11%Al-3%Mg)和Fe/(Zn-11%Al-x%Mg-0.2%Si)扩散偶在600℃下进行25min的固-液扩散实验,利用扫描电子显微镜(SEM)和能谱仪(EDS)研究了镁含量和硅对铁-锌铝镁合金固-液界面Fe-Al合金层形成的影响。结果表明,Fe/(Zn-11%Al-3%Mg)固-液扩散偶反应层由FeAl3和Fe2Al5相层组成;随着Mg含量的增加,Fe/(Zn-11%Al-x%Mg-0.2%Si)扩散偶中反应层的厚度呈现先增加后减少再增加的变化趋势,当镁含量为3%时反应层厚度最薄;Fe/(Zn-11%Al-3%Mg)扩散偶中Fe-Al反应层的平均厚度比Fe/(Zn-11%Al-3%Mg-0.2%Si)扩散偶中反应层的厚度大60μm,证明Si元素起到抑制Fe-Al反应层形成的作用。研究结果为解释Super Dyma合金镀层中不形成明显的Fe-Al抑制层提供了实验依据。     

Improving the wear resistance of AA 6061 by laser surface alloying with NiTi

To improve the wear resistance of a popular aluminum alloy AA 6061, a 1.5 mm thick hard surface layer consisting of Ni–Al and Ti–Al intermetallic compounds was synthesized on the alloy by laser surface alloying technique. NiTi powder was preplaced on the aluminum alloy substrate and irradiated with a high-power CW Nd:YAG laser in an argon atmosphere. With optimized processing parameters, a modified surface layer free of cracks and pores was formed by reaction synthesis of Al with Ni and Ti. X-ray diffractometry (XRD) confirmed the main phases in the layer to be TiAl₃ and Ni₃Al. The surface hardness increased from below 100 HV for untreated AA 6061 to more than 350 HV for the laser-treated sample. Accompanying the increase in hardness, the wear resistance of the modified layer reached about 5.5 times that of the substrate.     

A study of microstructure and phase constitutions of the Cr–Ni surfacing layers deposited on Fe<Subscript>3</Subscript>Al intermetallic by SMAW

Three different Cr–Ni alloys were deposited on the surface of Fe₃Al intermetallic by shielded metal arc welding (SMAW) to investigate the weldability of this material. The microstructure, phase constitutions, and fine structures of Cr–Ni surfacing layers were analyzed via metalloscope, SEM, XRD, and TEM. The results indicated that the Fe₃Al/Cr–Ni joint shows no cracks when Cr25–Ni13 alloy was deposited. The surfacing layer consisted of austenite (A), pro-eutectoid ferrite (PF), carbide-free bainite (CFB), lath martensite (LM), and little acicular ferrite (AF). Phase constitutions of the joint included Fe₃Al, FeAl, γ-(Fe,C), γ-(Fe,Ni), NiAl, and Ni₃Al. The lattice orientation for CFB between α and γ phases was (110)_α//(111) _γ . Typical LM was composed of interlayer-carbide and α ferrite of 400 nm in length and 40 nm in width.     

钢/铝添加粉末激光焊接头界面组织与性能

基于密度泛函理论的第一性原理,利用层技术构建钢/铝激光焊接的Fe/Al界面模型,研究金属原子X(X=Sn,Sr,Zr,Ce,La)置换Fe/Al界面模型中Fe(Al)原子的合金形成热及其体系电子结构。结果表明:Sn,Sr,Ce优先置换Fe/Al界面处的Al原子,而La,Zr优先置换Fe/Al界面处的Fe原子,合金化促进Fe/Al界面电子在不同轨道之间的转移,增强Fe-Al的离子键性能,提高Fe/Al界面结合能力,改善Fe/Al界面的脆性断裂,其中Sn的合金化效果最显著。在此基础上,进行1.4mm厚DC51D+ZF镀锌钢和1.2mm厚6016铝合金试件添加Sn,Zr粉的激光搭接焊实验,结果显示:添加粉末可促进焊接熔池的流动性,改变接头界面成分和显微组织,添加Sn粉激光焊钢/铝接头的抗拉强度327.41MPa,伸长率22.93%,较添加Zr粉和未添加粉末有了明显提高。     

Effect of Applied Pressure on the Joining of Combustion Synthesized Ni3Al Intermetallics with Al Alloy

We focused on the surface reinforcement of ligth weight casting alloys with Ni-AI intermetallic compounds by in-situ combustion reaction to improve the surface properties of non-ferrous casting components.In our previous works,green compact of elemental Ni and Al powders were reacted to form Ni-3Al intermetallic compound by SHS （Self-propagating high temperature synthesis） reaction with the heat of molten Al alloy and simultaneously bonded with Al casting alloy.But some defects such as tiny cracks and porosities were remained in the reacted compact.So we applied pressure to prevent thermal cracks and fill up the pores with liquid Al alloy by squeeze casting process.The compressed Al alloy bonded with the Ni-3Al intermetallic compound was sectioned and observed by optical microscopy and scanning electron microscopy （SEM）.The stoichiometric compositions of the intermetallics formed around the bonded interface and in the reacted compact were identified by energy dispersive spectroscopy （EDS） and electron probe micro analysis （EPMA）. Si rich layer was formed on the Al alloy side near the bonded interface by the sequential solidification of Al alloy.The porosities observed in the reacted Ni-3Al compact were filled up with the liquid AI alloy.The Si particles from the molten Al alloy were detected in the pores of reacted Ni-3Al intermetallic compact.The Al casting alloy and Ni-3Al intermetallic compound were joined very soundly by applying pressure to the liquid Al alloy.     

Improving the wear resistance of AZ91D magnesium alloys by laser cladding with Al-Si powders

To improve the wear resistance of AZ91D magnesium alloy, laser surface cladding with Al and Si powders was investigated using a Nd:YAG pulsed laser. With appropriate processing parameters and the suitable weight ratio of Al to Si in powders, a modified surface layer free of cracks and pores was formed by reaction synthesis of Mg with Al and Si. X-ray diffractometry (XRD) confirmed the main phases in the layer to be Mg₂Si and Mg₁₇Al₁₂. The surface hardness increased from 35 HV for as-received magnesium alloy to more than 170 HV for laser treated sample. Accompanying the increase in hardness, the wear resistance of the clad layer increased more than 4 times that of the substrate.     

Cyclic oxidation of aluminized Ti-14Al-24Nb alloy

Titanium aluminides are considered as replacements for superalloys in applications in gas turbine engines because of their outstanding properties. Ti₃Al has a superior creep strength up to 815° C, but has poor oxidation resistance above 650° C. Two approaches can be followed to improve the oxidation resistance of Ti₃Al above 650° C. One is alloying and the other obtaining a protective surface coating. Niobium was found to improve the oxidation resistance, when added as an alloying element. Recent investigations showed that a TiAl₃ surface layer considerably improves the oxidation resistance of titanium. In the present work, a TiAl₃ layer was obtained on a Ti-14Al-24Nb (wt%) alloy using a pack aluminizing process. The cyclic oxidation behaviour of aluminized and uncoated samples was evaluated.     

Fine structure at the diffusion welded interface of Fe3Al/Q235 dissimilar materials

The interface of Fe ₃ Al/Q235 dissimilar materials joint, which was made by vacuum diffusion welding, combines excellently. There are Fe ₃ Al, FeAl phases and α-Fe (Al) solid solution at the interface of Fe ₃ Al/Q235. Aluminum content decreases from 28% to 1.5% and corresponding phase changes from Fe ₃ Al with DO ₃ type body centred cubic bcc structure to α-Fe (Al) solid solution with B2 type bcc structure. All phases are present in sub-grain structure level and there is no obvious brittle phases or micro-defects such as pores and cracks at the interface of Fe ₃ Al/Q235 diffusion joint.     

Dissimilar metals TIG welding-brazing of aluminum alloy to galvanized steel

Dissimilar metals TIG welding-brazing of aluminum alloy to galvanized steel was investigated, and the wettability and spreadability of aluminum filler metal on the steel surface were analyzed. The resultant joint was characterized in order to determine the brittle intermetallic compound (IMC) in the interfacial layer, and the mechanical property of the joint was tested. The results show that the zinc coated layer can improve the wettability and spreadability of liquid aluminum filler metal on the surface of the steel, and the wetting angle can reach less than 20°. The lap joint has a dual characteristic and can be divided into a welding part on the aluminum side and a brazing part on the steel side. The interfacial IMC layer in the steel side is about 9.0 μm in thickness, which transfers from (α-Al + FeAl₃) in the welded seam side to (Fe₂Al₅+ FeAl₂) and (FeAl₂+ FeAl) in the steel side. The crystal grain of the welded seam is obviously larger in size in the aluminum side. The local incomplete brazing is found at the root of the lap joint, which weakens the property of the joint. The fracture of the joint occurs at the root and the average tensile strength reaches 90 MPa.     

Research on explosive welding of aluminum alloy to steel with dovetail grooves

In order to explore a new method for the explosive welding of aluminum alloy to steel, a 5083 aluminum alloy plate and a Q345 steel plate with dovetail grooves were respectively employed as the flyer and base plates. The parameters adopted in the explosive welding experiment were close to the lower limit of weldable window of 5083 aluminum alloy to Q345 steel. The bonding properties of 5083/Q345 clad plate were studied through mechanical performance tests and microstructure observations. The results showed that the aluminum alloy and steel plates were welded under the actions of metallurgical bonding and meshing of dovetail grooves. The tensile shear strength of 5083/Q345 clad plate met the requirements of the bonding strength of Al/Fe clad plate. The interfaces between aluminum alloy and the upper and lower surfaces of dovetail grooves were mainly welded through direct bonding, and discontinuous molten zone emerged in the local region; while the interface between aluminum alloy and the inclined surface of dovetail grooves was bonded by continuous molten layer. The brittle intermetallic compounds FeAl₂ and Al₅Fe₂ were generated at the bonding interfaces of 5083/Q345 clad plate. The fracture surface of the tensile specimen exhibited ductile and quasi-cleavage fractures.