Thermal stability of ultrafine grained aluminium alloy prepared by large strain extrusion machining

Abstract

In the present study, ultrafine grained (UFG) Al alloy chips with average grain sizes of ～200 nm were successfully prepared by large strain extrusion machining (LSEM) process using a combined cutting tool with rake angle of 10° and chip compression ratio of 1.0. The tests showed that the Vickers hardness of the UFG Al alloy is significantly improved due to grain size reduction. To understand effect of heat on the microstructure and mechanical properties, the UFG chips were subjected to heat treatment at different temperatures and different annealing time durations. When annealed <100°C, most of fine grains within the UFG chips were found to be replaced by elongated grains whose grain sizes increased with a significant increase in the aspect ratio as the annealing time increased. Despite such increase in grain size, the Vickers hardness was not reduced as expected because of the precipitation of secondary phases. When annealed at temperatures up to 200°C, recrystallisation occurred, along with grain growth, but the Vickers hardness did not deteriorate because of precipitation of secondary phases, as before. However, annealing at temperatures of 300°C and above resulted in significant reduction in hardness of the chips due to dominance of grain growth over secondary precipitation. These results indicated that UFG Al alloy chips have a good thermal stability at temperatures <200°C.     

人工时效对激光选区熔化AlMg4.5Sc0.55Mn0.5Zr0.2合金显微组织和力学性能的影响

采用激光选区熔化制备AlMg_4.5Sc_0.55Mn_0.5Zr_0.2合金,研究人工时效工艺参数对合金维氏硬度的影响规律,分析沉积态和优选时效态合金的室温拉伸性能和显微组织。结果表明：人工时效使该合金的维氏硬度由102HV提升至140HV以上。随着时效温度升高（305~335℃）或时效时间延长（1.5~48 h）,维氏硬度呈现先增加、再降低、最后逐渐趋于稳定的规律。在315℃时效3 h或12 h后,合金的室温拉伸性能基本相当,无明显的各向异性;抗拉强度和屈服强度分别达到470 MPa和410 MPa,断后伸长率保持在15.0%。力学性能的提升得益于人工时效过程中弥散析出且与基体共格的纳米增强颗粒Al₃（Sc,Zr）。     

A DSC study on the precipitation kinetics of cryorolled Al 6063 alloy

The microstructural evolution and precipitation behavior of cryorolled Al 6063 alloy were investigated. The Al 6063 alloy plates were solutionized and cryorolled with thickness reduction of 25% and 93%. The phase identification and microstructure of the cryorolled Al alloy sample were carried out by XRD, electron backscattered diffraction (EBSD) analysis and TEM. The cryorolled Al alloy upon 93% thickness reduction exhibits ultrafine grain structure. The DSC results of cryorolled Al 6063 alloy obtained at different heating rate are used to calculate activation energies for the evolution of precipitates. The influence of different reduction rates on activation energy of precipitate formation in the cryorolled Al 6063 alloy was analyzed. It was clear from the present study that an ultrafine-grained Al 6063 alloy exhibits a higher driving force for the precipitation formation when compared to bulk Al alloy.     

Mechanical and dry sliding wear behavior of ultrafine-grained AISI 1024 steel processed using multiaxial forging

AISI 1024 steel was severely deformed by using warm (500 °C) multiaxial forging (MAF) technique using up to nine forging passes in order obtain a composite ultrafine grained (UFG) microstructure consisting of fragmented cementite particles. Microstructural evolution is studied using optical and electron microscopy. After warm MAF, the hardness and strength properties improved significantly, although total elongation values decreased. The tribological properties of UFG low carbon steel produced by MAF have been investigated. Dry sliding was carried out using constant sliding speed. The wear test results showed that the strengthening of AISI 1024 steel by warm MAF processing did not lead to improvement of wear resistance. The results are explained on the basis of its microstructural features and lower pull-off work. Higher grain boundary density, presence of submicron-sized cementite particles, and lower pull-off work are found to be responsible for lower sliding wear resistance of UFG steel.     

Combined effect of shot peening,subcritical austenitic nitriding,and cryo-treatment on surface modification of AISI 4140 steel

Shot peening is a simple but effective severe plastic deformation process to synthesize ultrafine grains in micro- to nanometer range on metallic surfaces. In this work, shot peening on AISI 4140 steel specimens was done in a novel centrifugal air blast shot peening reactor with shot velocity of 5.8?m/s for 3?h. Characterization of the shot peened surface (XRD, micro-hardness, SEM, and TEM) showed that surface undergoes significant plastic deformation with marked increase in microstrain of lattice, dislocation density, and surface hardness. XRD profiles and TEM analysis confirmed formation of ultrafine grain structure in the nanometer range. These specimens were then subjected to austenitic nitriding at 610°C for 4?h followed by cryo-treatment at???185°C for 32?h. Characterization of pre-shot peened nitrided and cryo-treated surfaces showed that there was marked improvement in surface hardness (from 695 to 797 HV_0.05) and effective case depth (from 19 to 54?µm) in comparison with un-shot peened nitrided and cryo-treated specimens. It was demonstrated that presence of ultrafine grain structure and austenitic phase during nitriding plays synergetic role to improve content and diffusion kinetics of nitrogen in AISI 4140 steel surface.     

Effect of grain size on strain rate sensitivity of cryomilled Al–Mg alloy

Al–Mg alloy powder was cryomilled to achieve a nanocrystalline (NC) structure having an average grain size of 50 nm with high thermal stability, and then consolidated by quasi-isostatic forging. The consolidation resulted in a bulk material with ultrafine grains of about 250 nm, and the material exhibited enhanced strength compared to conventionally processed Al–Mg alloy. The hardness of as-cryomilled powder, the forged ultrafine-grained (UFG) material, and the conventional coarse-grained (CG) alloy were measured by nanoindentation using various loading rates, and the results were compared with strain rate sensitivity (SRS) from uniaxial compression tests. Negative SRS was observed in the cryomilled NC powder and the forged UFG material, while the conventional alloy was relatively insensitive to strain rate. The dependence on loading rate was stronger in the NC powders than in the UFG material.     

Effect of initial grain size on the joint properties of friction stir welded aluminum

In this study, 2 mm-thick commercial 1050-Al plates with an ultrafine grained (UFG) structure were obtained by the accumulative roll bonding (ARB) technique after a 5 cycle process and were subsequently joined by friction stir welding (FSW) at various revolution pitches (welding speed/rotation speed) of 1 mm/r, 1.67 mm/r and 2.5 mm/r. To understand the effect of the initial grain size on the welding properties, ARB processed samples followed by annealing under H24 conditions as well as the as-received samples in the fully annealed state were also applied to the FSW process. The microstructure evolution and Vickers hardness in the stir zone of all the samples were investigated. It was revealed that the annealed samples with an intermediate grain size finally obtained the most refined grain size and highest value of Vickers hardness in the stir zone. However, for the UFG samples, significant grain growth and corresponding decrease in hardness can be found in the stir zone.     

超细晶纯钛疲劳裂纹的扩展行为

对纯钛进行2道次室温等径弯曲通道变形(ECAP)、等径弯曲通道变形加旋锻复合变形(ECAP+RS)并在旋锻后在300℃和400℃退火1 h,制备出4种具有不同组织的超细晶纯钛。对这4种超细晶纯钛进行疲劳裂纹扩展实验并观察分析超细晶纯钛的显微组织和疲劳断口的形貌,研究了裂纹的扩展行为。结果表明：显微组织对超细晶纯钛的疲劳裂纹扩展门槛值和近门槛区有显著的影响;超细晶纯钛的疲劳裂纹扩展门槛值随着塑性变形量的增大而增大,随着旋锻后退火温度的提高而降低;疲劳裂纹扩展速率曲线因超细晶纯钛晶粒尺寸和强度的影响出现转折,转折前ECAP+RS复合变形纯钛的抗疲劳裂纹扩展能力比ECAP变形强,且随着退火温度的提高而降低;转折后4种超细晶纯钛的疲劳裂纹扩展速率相差较小,呈现出相反的结果。疲劳裂纹扩展寿命中转折前近门槛区裂纹扩展寿命占绝大部分,因而转折前的门槛值与近门槛区的扩展速率对抗裂纹扩展能力更为重要。     

Shape effect of ultrafine-grained structure on static fracture toughness in low-alloy steel

Abstract

A 0.4C-2Si-1Cr-1Mo steel with an ultrafine elongated grain (UFEG) structure and an ultrafine equiaxed grain (UFG) structure was fabricated by multipass caliber rolling at 773 K and subsequent annealing at 973 K. A static three-point bending test was conducted at ambient temperature and at 77 K. The strength–toughness balance of the developed steels was markedly better than that of conventionally quenched and tempered steel with a martensitic structure. In particular, the static fracture toughness of the UFEG steel, having a yield strength of 1.86 GPa at ambient temperature, was improved by more than 40 times compared with conventional steel having a yield strength of 1.51 GPa. Furthermore, even at 77 K, the fracture toughness of the UFEG steel was about eight times higher than that of the conventional and UFG steels, despite the high strength of the UFEG steel (2.26 GPa). The UFG steel exhibited brittle fracture behavior at 77 K, as did the conventional steel, and no dimple structure was observed on the fracture surface. Therefore, it is difficult to improve the low-temperature toughness of the UFG steel by grain refinement only. The shape of crystal grains plays an important role in delamination toughening, as do their refinement and orientation.     

Tensile and impact-toughness behaviour of cryorolled Al 7075 alloy

The effects of cryorolling and optimum heat treatment (short annealing + ageing) on tensile and impact-toughness behaviour of Al 7075 alloy have been investigated in the present work. The Al 7075 alloy was rolled for different thickness reductions (40% and 70%) at cryogenic (liquid nitrogen) temperature and its mechanical properties were studied by using tensile testing, hardness, and Charpy impact testing. The microstructural characterization of the alloy was carried out by using field emission scanning electron microscopy (FE-SEM). The cryorolled Al alloy after 70% thickness reduction exhibits ultrafine grain structure as observed from its FE-SEM micrographs. It is observed that the yield strength and impact toughness of the cryorolled material up to 70% thickness reduction have increased by 108% and 60% respectively compared to the starting material. The improved tensile strength and impact toughness of the cryorolled Al alloy is due to grain refinement, grain fragments with high angle boundaries, and ultrafine grain formation by multiple cryorolling passes. Scanning electron microscopy (SEM) analysis of the fracture surfaces of impact testing carried out on the samples in the temperature range of −200 to 100 °C exhibits ductile to brittle transition. cryorolled samples were subjected to short annealing for 5 min at, 170 °C, and 150 °C followed by ageing at 140 °C and 120 °C for both 40% and 70% reduced samples. The combined effect of short annealing and ageing, improved the strength and ductility of cryorolled samples, which is due to precipitation hardening and subgrain coarsening mechanism respectively. On the otherhand, impact strength of the cryorolled Al alloy has decreased due to high strain rate involved during impact loading.     

Annealing characteristics of nanostructured Cu-Fe-P alloy processed by accumulative roll-bonding

Annealing characteristics of a nanostructured copper alloy processed by accumulative roll-bonding (ARB) were studied. A nano-grained Cu-Fe-P alloy processed by 8 cycles of the ARB was annealed at various temperatures ranging from 100 to 400 degrees C for 0.6 ks. The sample still showed an ultrafine grained (UFG) structure up to 250 degrees C, however above 300 degrees C it began to replace by equiaxed and coarse grains due to an occurrence of the conventional static recrystallization. The hardness of the annealed copper decreased largely above 300 degrees C. These annealing characteristics of the UFG copper alloy were compared to those of a high purity copper.     

A study on the mechanical properties of cryorolled Al–Mg–Si alloy

The mechanical properties of a precipitation hardenable Al–Mg–Si alloy subjected to cryorolling and ageing treatments are reported in this present work. The severe strain induced during cryorolling of Al–Mg–Si alloys in the solid solutionised state produces ultrafine microstructures with improved mechanical properties such as strength and hardness. The improved strength and hardness of cryorolled alloys are due to the grain size effect and higher dislocation density. The ageing treatment of cryorolled Al–Mg–Si alloys has improved its strength and ductility significantly due to the precipitation hardening and grain coarsening mechanisms, respectively. The reduction in dimple size of cryorolled Al–Mg–Si alloy upon failure confirms the grain refinement and strain hardening mechanism operating in the severely deformed samples.     

Surface hardening of biocompatible ultrafine-grained niobium zirconium alloy by two-stage oxidation treatment

The present study reports on an optimized surface hardening process for biocompatible ultrafine-grained (UFG) niobium 2.3 wt% zirconium (NbZr) alloy, a promising candidate implant material. The as-received material of conventional grain size (CG) was processed using multipass equal channel angular processing at room temperature to obtain an UFG microstructure featuring high strength and ductility. Subsequent surface hardening was performed by a heat treatment leading to internal oxidation. Using a thermogravimetric system, the influence of temperatures, time, and partial pressure of oxygen ( $ p_{{\text{O}}_2} $ ) on the oxidation kinetics were investigated. Metallographic and microscopic analyses and hardness measurements were employed to evaluate maximum hardness, penetration-depth and scale formation under various conditions. Heat treatment at 620 °C for 6 h at a $ p_{{\text{O}}_2} $ of 0.2 hPa led to sufficiently rapid oxidation kinetics yielding a relatively high depth of penetration without formation of loose Nb₂O₅ on the surface, which was observed at higher $ p_{{\text{O}}_2} $ . As compared to CG material, improved hardness profiles were reached using the same heat treatment parameters, since the UFG structure significantly changes diffusion conditions and therefore oxidation kinetics. After a second heat treatment in high vacuum the high maximum hardness of 820 HV0.01 in the UFG material was reduced effectively and a less steep hardness gradient was achieved, both contributing to a less brittle behavior under mechanical loading. High-cycle fatigue tests performed on surface-hardened UFG NbZr samples showed a substantial improvement of fatigue life in tests conducted near the endurance limit. Especially when high fatigue and wear resistance are key issues for a given application, the internal oxidation process offers an effective way to further improve the properties of UFG NbZr.     

Sc元素对ZL205A合金组织和力学性能的影响EI北大核心CSCD

利用金相显微镜、扫描电镜、透射电镜等手段,研究Sc含量对砂型铸造ZL205A合金的组织和力学性能的影响规律。结果表明,Sc含量低于0.12%(质量分数,下同),未发现晶粒细化效果;Sc含量为0.06%,热处理态的合金晶界出现残留颗粒状W(AlCuSc)相,随Sc含量增加,W相由颗粒状转变为连续条带状;ZL205A合金热处理后弥散析出少量Al 3(Zr x,Ti 1-x)相,添加Sc后弥散相转变为Al 3(Zr x,Ti y,Sc 1-x-y)相,弥散相的数量随Sc含量的增加而增加;由于弥散相数量的增加,Sc含量为0.06%时,合金的时效响应速率和硬度峰值均略有增加,合金的屈服强度提高了4%;Sc含量为0.12%时,晶界残留相增加,Cu在α(Al)中的浓度降低,θ′相密度明显降低,合金的时效响应速率、硬度峰值以及力学性能各项指标均大幅下降;ZL205A合金中添加0.06%的Sc,即可明显地抑制θ′相的长大。     

Effect of annealing on precipitation, microstructural stability, and mechanical properties of cryorolled Al 6063 alloy

The effect of annealing on precipitation, microstructural stability, and mechanical properties of cryorolled Al 6063 alloy has been investigated in the present work employing hardness measurements, tensile test, XRD, DSC, EBSD, and TEM. The solution-treated bulk Al 6063 alloy was subjected to cryorolling to produce ultrafine grain structures and subsequently annealing treatment to investigate its thermal stability. The CR Al 6063 alloys with ultrafine-grained microstructure are thermally stable up to 250 °C as observed in the present work. Within the range of 150–225 °C, the size of small precipitate particles is <1 μm. These small precipitate particles pin the grain boundaries due to Zener drag effect, due to which the grain growth is retarded. The hardness and tensile strength of the cryorolled Al 6063 alloys have decreased upon subjecting it to annealing treatment (150–250 °C).     

Microstructural change of ultrafine-grained aluminum during high-speed plastic deformation

Effect of strain rate on microstructural change in deformation of the ultrafine grained (UFG) aluminum produced by severe plastic deformation (SPD) was studied. Commercial purity 1100 aluminum sheets were highly strained up to an equivalent strain of 4.8 by the Accumulative Roll-Bonding (ARB) process at ambient temperature. The ARB-processed sheets were found to be filled with pancake-shaped ultrafine grains surrounded by high-angle grain boundaries. The ultrafine grains had a mean grain thickness of 200 nm and a mean grain length of 1100 nm. The ultrafine-grained aluminum sheets were deformed at various strain rates ranging from 2 to 6.0×10⁴ s⁻¹ by conventional rolling, ultra-high-speed rolling, and impact compression. High-speed plastic deformation generates a large amount of heat, inducing coarsening of the ultrafine grains during and after deformation. On the other hand, it was also suggested that high-speed plastic deformation is effective for grain-subdivision, in other words, ultra-grain refinement, if the effect of heat generation is extracted.     

Fatigue Damage Evolution in Ultrafine‐Grained Interstitial‐Free Steel

The current work presents the crack propagation behavior in ultrafine‐grained (UFG) interstitial‐free (IF) steel, and in particular, focuses on the damage evolution in UFG IF steel under cyclic loading. The current results indicate that equal‐channel angular pressing (ECAP) has a major influence on the cyclic deformation response of the UFG IF steel, such that the failure and the crack path depend on the inclination plane during ECAP. Furthermore, the UFG IF steel demonstrates significant notch sensitivity in comparison to its coarse‐grained counterpart. This is attributed to the ultrafine grains with a large volume fraction of high‐angle grain boundaries, where glide of dislocations is hindered and the resulting internal stresses increase the stress concentration further in the presence of a pre‐existing notch.     

析出强化超细晶粒钢焊接热影响区粗晶区的组织和性能

为研究焊接对800 MPa级Ti、Nb复合微合金化析出强化超细晶粒钢组织性能的影响.运用Gleeble3500热模拟试验机,对实验钢进行单道次焊接热循环试验,并研究冷却速度、冷却时间t8/5对焊接热影响区粗晶区(CGHAZ)组织、性能的影响.结果表明:冷却速度5~15℃/s,CGHAZ的组织为贝氏体,冷却速度进一步增大,会出现马氏体.随着冷却时间t8/5的增加,原奥氏体晶粒尺寸逐渐增加,硬度值逐渐降低,冲击韧性先上升后下降.t8/5为20~120 s时,CGHAZ显微硬度(223~250.4 HV)均小于母材的显微硬度(270.6 HV),出现软化现象,t8/5为20 s时,冲击吸收功最高,为18.2 J,但仅有母材的25.3%.经历焊接热循环后,奥氏体晶粒粗化以及CGHAZ出现贝氏体组织是导致脆化的主要原因.     

Fabrication of large-bulk ultrafine grained 6061 aluminum alloy by rolling and low-heat-input friction stir welding

In this study, the ultrafine grained (UFG) 6061 Al alloys fabricated by cold rolling were friction stir welded (FSW) with different rotation rates under both air cooling and rapid cooling in water. Low-heat-input parameters of 400 rpm rotation rate in water (400-Water) could effectively inhibit the coarsening of recrystallized grains, reduce the precipitation rate, and retain more dislocations of the UFG 6061 Al parent metal. 400-Water joint showed high lowest-hardness value, narrow low-hardness zone, and high tensile strength, attributing to the effect of dislocation, grain boundary, solid-solution, and precipitation hardening. This work provides an effective strategy to fabricate large-sized bulk UFG Al alloy by cold rolling with large deformation and low-heat-input FSW.     

Grain size-dependent Mg/Si ratio effect on the microstructure and mechanical/electrical properties of Al-Mg-Si-Sc alloys

Al-Mg-Si-Sc alloys with different Mg/Si ratio (<1.73 in wt.% vs>1.73 in wt.%) and different grain size (coarse grains vs ultrafine grains) were prepared, which allowed to investigate the grain size-dependent Mg/Si ratio effect on the microstructural evolution and concomitantly on the hardness and electrical conductivity when subjected to aging at 200 °C. In the coarse-grained Al-Mg-Sc-Sc alloys, the β″ precipitation within the grain interior and also the precipitation hardening were highly dependent on the Mg/Si ratio, while the electrical conductivity was slightly affected by the Mg/Si ratio. A promoted β″ precipitation was found in the case of Si excess (Mg/Si ratio <1.73), much greater than in the case of Mg excess (Mg/Si ratio>1.73). While in the ultrafine-grained Al-Mg-Si-Sc alloys, the electrical conductivity rather than the hardness was more sensitive to the Mg/Si ratio. The alloy with Si excess displayed electrical conductivity much higher than its counterpart with Mg excess. This is rationalized by the grain boundary precipitation promoted by Si, which reduced the solute atoms and precipitates within the grain interior. Age softening was found in the ultrafine-grained alloy with Si excess, but the ultrafine-grained alloy with Mg excess held the hardness almost unchanged during the aging. The hardness-conductivity correlation is comprehensively discussed by considering the coupling effect of Mg/Si ratio and grain size. A strategy to simultaneously increase the hardness/strength and electrical conductivity is proposed for the Al-Mg-Si-Sc alloys, based on present understanding of the predominant factors on strengthening and conductivity, respectively.