Study on microstructure of squeeze casting AZ91D alloy

Abstract

The present paper reports the investigation of the microstructure distribution of squeeze cast AZ91D alloy. The microstructure of squeeze cast AZ91D alloy is not uniform and is composed of four zones, which are chilled layer, segregation zone, pressured crystallisation area and hot spot area respectively. Moreover, in the pressured crystallisation area, the microstructure sequence in the transverse section from the outside to the inside could be divided into four sublayers, such as fine equiaxial dendrite area, dendrite area with a high directivity, confusion dendrite area and disorder dendrite area. The volume fraction of the intermetallic compound Mg₁₇Al₁₂ also varied with the location. The volume fraction of Mg₁₇Al₁₂ in the pressured crystallisation area is the largest except in the segregated zone.     

变形的AZ91D镁合金半固态等温压缩的力学行为

为了了解等径道角挤压(ECAE)的AZ91D镁合金在半固态压缩变形中的力学特征,利用半固态温压缩实验、Gleeble1500实验机和金相显微镜对其在半固态压缩变形中的力学行为进行了研究.结果表明:ECAE的AZ91D镁合金在半固态等温压缩中变形由固相晶粒本身的塑性变形、液相包围着固相晶粒的滑动和转动构成;该材料的真应力-真应变曲线由应力激增阶段、应力下降阶段、稳态阶段和应力增加阶段组成;随保温时间的增加或变形温度的升高,获得相同应变量的真应力明显下降,稳态应力和峰值应力也明显下降;随应变速率的增加,稳态应力增加.     

AZ91D镁合金化学镀Ni-P/Ni-W-P双层镀层研究

为了提高镁合金的耐磨耐蚀性,研究了一种镁合金直接化学镀Ni-P/Ni-W-P双层镀层的方法.采用扫描电镜(SEM)和X-射线衍分析射仪(XRD)分析了镀层的微观结构.对镀层进行了极化曲线分析,并进行了盐酸腐蚀试验和结合力试验.结果表明,该复合镀层组织致密无孔,具有较高的显微硬度和高耐蚀性.镀层硬度可达622HKV,试样在10%的HCl溶液中可保持近3h不腐蚀基体,对镁合金起到很好的保护作用.     

AZ91D镁合金托弹板半固态触变模锻研究

为了掌握半固态触变模锻中工艺参数对成形零件的微观组织和力学性能的影响规律,借助拉伸试验机和金相显微镜对AZ91D镁合金托弹板的半固态触变模锻过程进行了研究.AZ91D镁合金半固态坯料分别采用传统SIMA法和新SIMA法制备.结果表明:压力对托弹板零件的充型过程有很大影响,当压力为500 kN,托弹板零件充型不满;当压力为2000 kN,托弹板零件充型良好.坯料加热温度和保温时间对托弹板零件的力学性能有一定影响.当压力为2000 kN,模具预热温度为450 ℃,坯料在545 ℃保温20 min时,新SIMA法制备的半固态坯半固态触变模锻成形的托弹板零件获得最佳的力学性能.与传统SIMA法相比,新SIMA法制备的半固态坯成形的托弹板零件的室温力学性能和100℃的高温力学性有很大提高.     

AZ91D镁合金超疏水膜层的制备及其表征

采用简单易行的化学刻蚀方法,通过硝酸刻蚀、化学镀银和硬脂酸自组装改性处理,在AZ91D镁合金表面上成功制备出了超疏水膜层,进一步解释了该制备工艺的化学反应机理。利用扫描电子显微镜和视频光学接触角测量仪对AZ91D镁合金表面超疏水膜层的微观形貌和润湿性能进行了表征,利用能谱仪和光谱仪测定了膜层的表面化学组成。结果显示,釆用上述方法处理后的AZ91D镁合金表面呈现出良好的疏水性,水滴在试样表面的表观接触角为153°,滚动角为4°。     

Hot cracking in tungsten inert gas welding of magnesium alloy AZ91D

Abstract

Plates of 3–5 mm in thickness were extracted from an AZ91D ingot and then butt joints of the plates were produced using tungsten inert gas (TIG) welding method. The TIG arc was also used to deposit welding beads on some of the thin plates. No cracking was found in the butt joints. However, hot cracking was always observed to propagate from the heat affected zone (HAZ) under the welding bead into the weld metal right after a welding bead was deposited on the thin plate. Metallographic and fractographic evidence was obtained to show that the hot cracking is 'liquation cracking' in the partially melted HAZ under the high thermal stresses. In the butt joints, the weld metal has the finest grains, highest strength and best ductility, and the HAZ was found to be the 'weakest link'.     

电磁搅拌对半固态AZ91D镁合金组织的影响

研究了电磁搅拌参数对连续冷却条件下AZ91D镁合金组织的影响.结果表明:当电磁搅拌的频率达到或高于50 Hz时,半固态AZ91D镁合金浆料或坯料组织中的球状初生固相越来越多,越来越圆整;在电磁搅拌频率为200 Hz和冷却速率较低的条件下,搅拌的功率越大,半固态AZ91D镁合金组织中的球状初生固相越多,晶粒也越细小.在电磁搅拌条件下,AZ91D镁合金熔体的激烈流动导致较为均匀的温度场和溶质场、更加剧烈的温度起伏,促进了半固态AZ91D镁合金球状组织的形成.半固态重熔加热使半固态AZ91D镁合金坯料初生固相的形态发生进一步的球化.     

AZ91D镁合金阳极氧化与热扩散渗铝复合膜层的研究

将阳极氧化与热扩散相结合对AZ91D镁合金表面进行低温渗铝处理,利用扫描电镜、光学显微镜和X射线衍射仪对所得膜层的形貌、相结构及耐腐蚀性能进行了研究,并对复合膜层改善镁合金基体耐腐蚀性能的过程进行了分析.研究表明,该复合膜层是由MgO和金属间化合物Mg17Al12以及被γ相(Mg17Al12)包裹住的α-Mg晶粒共同组成;AZ91D镁合金表面的阳极氧化和热扩散渗铝复合膜层能显著提高镁合金基体材料的耐腐蚀性能.     

AZ91D镁合金锌系磷化膜成膜机理和生长过程的研究

以磷酸盐化学转化膜为研究体系,采用SEM、XRD、OCP等分析方法及检测手段,研究AZ91D镁合金系磷酸盐化学转化膜的成膜机理、膜层结构及生长过程。研究发现AZ91D镁合金在磷化液中成膜过程分5个阶段:初始成核(1～5s)、基体快速溶解(5～60s)、晶体快速生长(1～2min)、膜层稳态生长(2～10min)和膜层沉积溶解平衡阶段(10min以后)。AZ91D镁合金表面的磷酸盐晶核的形成并非在金属进入溶液的最初时刻一次形成,是分批形成。最先形成的晶核逐渐长大,新的晶核不断生成,磷酸盐晶粒对其表面的覆盖度逐渐增大,直至各个晶粒逐渐长大相互接界,将其表面完全覆盖,结晶过程结束。晶核的形成未优先发生在基体金属的晶界上,随着晶核的生长和外延而形成磷化膜。     

乙醇胺添加剂对AZ91D镁合金表面磷化膜耐蚀性能的影响研究

以磷酸盐化学转化膜为研究体系,采用动电位极化和交流阻抗分析方法及检测手段,研究乙醇胺添加剂及其浓度对AZ91D镁合金磷化膜耐蚀性能的影响.研究发现,(1)乙醇胺(MEA)作为添加剂可有效改善AZ91D镁合金表面磷化膜的耐蚀性能.在MEA添加量为1.2g/L时,磷化膜的耐蚀性最好.添加乙醇胺1.2g/L时制备的磷化膜,在3.5%(质量分数)NaCl溶液中的耐蚀性能比AZ91D镁合金基体提高了10倍;(2)MEA浓度在0.4～1.2g/L时,磷化膜的R_(ct)随MEA浓度增加成线性增长关系.MEA浓度1.2g/L时达到最大值.磷化膜的R_p在MEA浓度为1.2g/L时达到最高值.当MEA浓度继续增加时,R_p明显下降.MEA浓度控制在0.8＜C_(MEA)＜1.6g/L时获得的磷化膜的耐蚀性能最好.     

Effects of Ca combined with Sr additions on microstructure and mechanical properties of AZ91D magnesium alloy

Abstract

Weight reduction to improve automobile fuel economy has triggered renewed interest in magnesium. The effects of Ca/Sr separate and composite additions to AZ91D magnesium alloy on its microstructure and mechanical properties have been investigated. The results indicate Ca can refine both the grain and eutectic phase of AZ91D magnesium alloy. Sr hampers microstructure refinement when composite Ca/Sr additions are made. In addition, separate Ca additions to AZ91D magnesium alloy increase yield strength but decrease elongation of this alloy. By adjusting the Ca/Sr composite proportions, additions to AZ91D magnesium alloy are able to improve both microstructure and mechanical properties of the alloy.     

乙醇胺添加剂对AZ91D镁合金表面磷化膜微观结构的影响研究

以锌系磷酸盐化学转化膜为研究体系,采用SEM,XRD分析方法及检测手段,研究乙醇胺(MEA)添加剂及其浓度对AZ91D镁合金锌系磷酸盐化学转化膜微观结构的影响.研究发现由于锌系磷化液中乙醇胺的添加:(1)改变了AZ91D镁合金锌系磷化膜晶体层的微观结构,促进了晶核的形成和晶粒细化,晶簇间隙中晶核的形成对晶体膜层完整性和致密度起着关键作用;(2)对(Zn_3(PO_4)_2·_4H_2O)晶体的取向有影响,有控制晶簇尺寸使磷化结晶组织更均匀的作用;(3)MEA在1.2g/L时磷化膜层平整致密、晶簇的尺寸均匀缺陷最少;(4)锌系磷化膜有两层结构:(Zn_3(PO_4)_2·_4H_2O)晶体外层和非晶态内层;(5)MEA的不同添加量对晶体层孔隙的影响有3种类型:表面浅孔(a型),晶簇间缝隙或微裂纹(b型),开放缺陷(c型).     

Surface characterization and cytocompatibility evaluation of silanized magnesium alloy AZ91 for biomedical applications

Mg alloys with high Al contents have superior corrosion resistance in aqueous environments, but poor cytocompatibility compared to that of pure Mg. We have silanized the cast AZ91 alloy to improve its cytocompatibility using five different silanes: ethyltriethoxysilane (S1), 3-aminopropyltriethoxysilane (S2), 3-isocyanatopyltriethoxysilane (S3), phenyltriethoxysilane (S4) and octadecyltriethoxysilane (S5). The surface hydrophilicity/hydrophobicity was evaluated by water contact angle measurements. X-ray photoelectron analysis was performed to investigate the changes in surface states and chemical composition. All silane reagents increased adsorption of the albumin to the modified surface. In vitro cytocompatibility evaluation revealed that silanization improved cell growth on AZ91 modified by silane S1. Measurement of the concentration of Mg²⁺ ions released during the cell culture indicated that silanization does not affect substrate degradation.     

Surface characterization and cytocompatibility evaluation of silanized magnesium alloy AZ91 for biomedical applications

Abstract

Mg alloys with high Al contents have superior corrosion resistance in aqueous environments, but poor cytocompatibility compared to that of pure Mg. We have silanized the cast AZ91 alloy to improve its cytocompatibility using five different silanes: ethyltriethoxysilane (S1), 3-aminopropyltriethoxysilane (S2), 3-isocyanatopyltriethoxysilane (S3), phenyltriethoxysilane (S4) and octadecyltriethoxysilane (S5). The surface hydrophilicity/hydrophobicity was evaluated by water contact angle measurements. X-ray photoelectron analysis was performed to investigate the changes in surface states and chemical composition. All silane reagents increased adsorption of the albumin to the modified surface. In vitro cytocompatibility evaluation revealed that silanization improved cell growth on AZ91 modified by silane S1. Measurement of the concentration of Mg²⁺ ions released during the cell culture indicated that silanization does not affect substrate degradation.     

Effect of selective laser melting on microstructure and properties of AZ91D alloy

Selective laser melting technology is used to manufacture porous and solid AZ91D alloys. The effects of laser power and hatch spacing on the density, blowholes, microstructure and mechanical properties of AZ91D alloy are studied. The laser power and hatch spacing play a significant role in the density and blowholes of AZ91D specimens. The grains size of specimens increases from 1 μm–2 μm to 8 μm–10 μm from the bottom to the top in single molten pool. Compared with grain size of die‐casting alloy (30 μm), that of selective laser melted gets refinement. There is no significant change in microstructure in the bottom, middle and top of specimens. The micro‐hardness of AZ91D alloy, reaching up to 115.3 HV 0.1, is superior to that of die‐casting alloy (56 HV 0.1). The compression properties of porous and solid specimens reach the degree of die‐casting solid magnesium alloy. AZ91D alloy shows the potential in the application of medical biodegradable materials.     

Simulation and experimental investigation of FSP of AZ91 magnesium alloy

A thermo-mechanical simulation of the friction stir processing (FSP), using the DEFORM 3D software based on Lagrangian implicit, was developed and verified by the experimental results. Simulation can successfully predict the temperature and effective strain distributions. Material flow around the tool pin was examined using the point tracking. It was found that the major part of material flow occurs at the advancing side, and consequently, stirred zone (SZ) stretches toward the advancing side. However, material at the retreating side moves slightly in backward direction. The material deformation and the peak temperature influence on the microstructural characters and can determine the width of SZ. Based on the simulation, effective strain and temperature histories of material around the tool pin were also calculated. The amount of effective strain and peak temperature required for recrystallization at the advancing and retreating sides as well as at the bottom of SZ was determined. Therefore, the width of SZ can be predicted by the simulation.     

Study on tensile properties and microstructure of cast AZ91D/AlN nanocomposites

AZ91D is a widely used magnesium alloy, but its application is generally limited to below 150 °C because of its weak creep resistance and tensile properties at elevated temperatures. In this study, high temperature (200 °C) tensile properties including yield strength and tensile strength of AZ91D are much improved by adding only about 1.0 wt% AlN nanoparticles in the AZ91D matrix through an innovative ultrasonic cavitation based dispersion of nanoparticles. The good ductility of AZ91D is also retained in AZ91D/1%AlN nanocomposites. It is found that ultrasonic cavitation based solidification processing is very effective to disperse AlN nanoparticles in AZ91D melts, which is difficult to obtain by traditional mechanical stirring methods. With a good combination of high temperature yield strength, tensile strength and ductility, AZ91D/1%AlN nanocomposite is promising as a new class of structural materials to be used at temperatures up to 200 °C or higher.     

Comparison of superplastic forming abilities of as‐cast AZ91 magnesium alloy prepared by twin roll casting and WE43 magnesium alloy

This paper describes and compares the superplastic behaviour and microstructural evolution of twin roll cast AZ91 and WE43 rolled sheet alloys. Tests were carried out in uniaxial tension on both alloys across a range of temperatures (300 °C–525 °C) and strain rates (1?10^‐4 s^‐1–1?10^‐1 s^‐1). In the case of WE43 gas bulge testing was employed at 400 °C and 0.6 MPa to offer a better analogy to superplastic forming than uniaxial tensile testing. Elongations of over 400 % were observed within WE43 when tested at 450 °C and 1?10^‐3 s^‐1 strain rate, and over 200 % within AZ91 when tested at 350 °C and 1?10^‐3 s^‐1 strain rate. A peak cone height of 41 mm was achieved with WE43 at a temperature of 400 °C and pressure of 0.6 MPa. Electron back scattered detection technique was employed to analyse the microstructural evolution of the two alloys during the forming process. Both WE43 and AZ91 were observed to undergo dynamic recrystallization during elevated temperature tensile testing and failed at low strain rates mainly by means of coalescence of cavitation, in the case of AZ91 at high strain rates cracking of Al₁₂Mg₁₇ intermetallic particles was the dominating failure mechanism. Both alloys were seen to achieve good levels of superplastic ductility over 200 % elongation, which would be industrially useful in niche vehicle and aerospace manufacturing.     

Effects of SiCp size and volume fraction on the high cycle fatigue behavior of AZ91D magnesium alloy composites

High cycle fatigue tests (i.e., stress-controlled, axial) were conducted on monolithic AZ91D and AZ91D magnesinm alloy composites processed via squeeze casting and extrusion to contain either 15 gm or 52 gm size SiC particles, at both the 20% and 25% volume fraction reinforcement level. The effects of changes in SiC particle size and volume fraction on the high cycle fatigue behavior have been determined. In addition, the number of cracked particles on the fatigue fracture surfaces, as well as the level of damage beneath the fatigue fracture surfaces were quantified in order to determine the effects of particle size on the evolution of damage during fatigue and during overload failure. Commercial purity Mg specimens containing a large grain size were also tested in fatigue for comparison with the alloy and composite data.     

陈化对AZ91D镁合金上磷化膜的影响及磷化膜退化机制的研究

以磷酸盐化学转化膜为研究体系,采用交流阻抗(EIS)及红外(FT-IR)分析方法及检测手段,研究陈化时间对AZ91D镁合金磷化膜性能的影响及磷化膜的腐蚀退化机制.研究发现(1) EIS图谱和FT-IR图谱对比结果表明陈化时间对AZ91D磷化膜层性能有影响,磷化膜经陈化72h后更稳定.(2)磷化试样在硼酸缓冲液中浸泡实验的EIS测试表明,磷化膜的腐蚀退化机制分3个阶段:浸泡初期,中期和后期.浸泡初期(5～10h),电解质缓慢向磷化膜渗入,且有少量电解质浸入内层界面;浸泡中期(30～70h),随着内层界面腐蚀反应的发生,腐蚀产物开始对外层晶体层产生破坏作用,使缺陷扩大,导致电解质开始大量进入到内层界面;浸泡后期(80～120h),内层腐蚀反应达到平衡,膜层电阻等各项参数不再改变.