Transformation of long-period stacking ordered structures in Mg-Gd-Y-Zn alloys upon synergistic characterization of first-principles calculation and experiment and its effects on mechanical properties

Based on experiments and first-principles calculations,the microstructures and mechanical properties of as-cast and solution treated Mg-10Gd-4Y-xZn-0.6Zr(x=0,1,2,wt.%)alloys are investigated.The transformation process of long-period stacking ordered(LPSO)structure during solidification and heat treatment and its effect on the mechanical properties of experimental alloys are discussed.Results reveal that the stacking faults and 18R LPSO phases appear in the as-cast Mg-10Gd-4Y-1Zn-0.6Zr and Mg-10Gd-4Y-2Zn-0.6Zr alloys,respectively.After solution treatment,the stacking faults and 18R LPSO phase transform into 14H LPSO phase.The Enthalpies of formation and reaction energy of 14H and 18R LPSO are calculated based on first-principles.Results show that the alloying ability of 18R is stronger than that of 14H.The reaction energies show that the 14H LPSO phase is more stable than the 18R LPSO.The elastic properties of the 14H and 18R LPSO phases are also evaluated by first-principles calculations,and the results are in good agreement with the experimental results.The precipitation of LPSO phase improves the tensile strength,yield strength and elongation of the alloy.After solution treatment,the Mg-10Gd-4Y-2Zn-0.6Zr alloy has the best mechanical properties,and its ultimate tensile strength and yield strength are 278.7 MPa and 196.4 MPa,respectively.The elongation of Mg-10Gd-4Y-2Zn-0.6Zr reaches 15.1,which is higher than that of Mg-10Gd-4Y0.6Zr alloy.The improving mechanism of elastic modulus by the LPSO phases and the influence on the alloy mechanical properties are also analyzed.

Elucidating the evolution of long-period stacking ordered phase and its effect on deformation behavior in the as-cast Mg-6Gd-1Zn-0.6Zr alloy

Herein,the evolution of long-period stacking ordered(LPSO)phases in the as-cast Mg-6Gd-1Zn-0.6Zr(wt.%)alloy are investigated via transmission electron microscopy(TEM)and atom probe tomography(APT).The TEM results reveal that two types of LPSO phase(a bulky interdendritic phase and a plate-like matrix LPSO phase)are formed in the as-cast sample.Most of the LPSO phases are confirmed to be of the 14H type,with a smaller proportion being of the 18R LPSO.Further,the APT results reveal that the composition of the interdendritic LPSO phase is closer to that of the ideal 14H phase compared to the matrix LPSO phase,and both the interdendritic and matrix LPSO phases exhibit a Gd/Zn ratio of 2.5,thereby indicating a deficient Zn content compared to the ideal 14H phase(i.e.,1.3).In addition,the influence of the LPSO phases on the deformation behavior is investigated at different compressive plastic strains using electron backscatter diffraction(EBSD)analysis to reveal twinning and slip behavior during deformation.The results indicate that the LPSO phase induces additional work hardening in the late stage of deformation via the suppression of{1011}compressive twinning and the activation of non-basal slip systems.

Effect of long-period stacking ordered structure on very high cycle fatigue properties of Mg-Gd-Y-Zn-Zr alloys

Magnesium alloys with a long-period stacking ordered(LPSO)structure usually possess excellent static strength,but their fatigue behaviors are poorly understood.This work presents the effect of the LPSO structure on the crack behaviors of Mg alloys in a very high cycle fatigue(VHCF)regime.The LPSO lamellas lead to a facet-like cracking process along the basal planes at the crack initiation site and strongly prohibit the early crack propagation by deflecting the growth direction.The stress intensity factor at the periphery of the faceted area is much higher than the conventional LPSO-free Mg alloys,contributing higher fatigue crack propagation threshold of LPSO-containing Mg alloys.Microstructure observation at the facets reveals a layer of ultrafine grains at the fracture surface due to the cyclic contact of the crack surface,which supports the numerous cyclic pressing model describing the VHCF crack initiation behavior.

Microstructure and mechanical properties of Mg_(94)Zn_2Y_4 extruded alloy with long-period stacking ordered structure

The microstructure and mechanical properties of Mg94Zn2Y4 extruded alloy containing long-period stacking ordered structures were systematically investigated by SEM and TEM analyses. The results show that the 18R-LPSO structure and α-Mg phase are observed in cast Mg94Zn2Y4 alloy. After extrusion, the LPSO structures are delaminated and Mg-slices with width of 50-200 nm are generated. By ageing at 498 K for 36 h, the ageing peak is attained andβ′phase is precipitated. Due to this novel precipitation, the microhardness ofα-Mg matrix increases apparently from HV108.9 to HV129.7. While the microhardness for LPSO structure is stabilized at about HV145. TEM observations and SAED patterns indicate that the β′ phase has unique orientation relationships betweenα-Mg and LPSO structures, the direction in the close-packed planes ofβ′precipitates perpendicular to that ofα-Mg and LPSO structures. The ultimate tensile strength for the peak-aged alloy achieves 410.7 MPa and the significant strength originates from the coexistence ofβ′precipitates and 18R-LPSO structures.

Long-period stacking ordered structures in Mg-3Cu-1Mn-2Zn-1Y damping alloy

14H, 18R and 24R long-period stacking ordered （LPSO） structures were observed in the as-cast Mg-3Cu-1Mn-2Zn-1Y damping alloy using transmission electron microscopy （TEM）. These LPSO structures contained Mg, Y, Cu and Zn and thus they were quaternary phases. Sharp diffraction pattern of the 24R structure was obtained and the angle between and g10024R was measured to be 5.03°. During high resolution TEM observations, lattice fringes with two characteristic spacings were observed within the 24R structure. Based on the experimental results, 6H, 7H and three 8H are suggested as the building blocks of 18R, 14H and 24R structures, respectively. The 24R unit cell can be interpreted as the stacking of 8H building blocks in the same shear direction with a shear angle of about 5.03°. The imperfect 24R structures are in order or disorder arrangements of principal 8H and minor 6H blocks. This double-block structure model is also applicable to other reported defects in LPSO structures.

Review on long-period stacking-ordered structures in Mg-Zn-RE alloys

The recent development of high-strength magnesium alloys is focused on the role of the strengthening phases with a novel long-period stacking-ordered (LPSO) structure. This review detailed the main factors influencing the formation of LPSO phases, including alloying ele-ments, preparation methods, and heat treatments. Furthermore, process control in structure types, formation and transformation behavior, strengthening and toughening mechanisms of the LPSO phase were discussed. Finally, the current problems and development trends of high-strength Mg-Zn-RE alloys were also put forward.

Effect of long period stacking ordered phase on damping capacities of as-cast Mg-Zn-Y alloys

The microstructure and damping capacities of MgZnxYi.33x(x=l-4at.%)alloys were discussed and researched.The main phase composition of the alloys consists of a_Mg and long-period stacking ordered(LPSO)phase.Due to increasedLPSO phase,grain size was refined.LPSO phase was advantageous to the damping properties of the Mg-Zn-Y alloys.Mg-7%Zn-12.8%Y has the highest damping capacity up to0.04.Due to stacking fault probability,the LPSO phase in the Mg-Zn-Yalloys could be new damping source to dissipate energy so as to contribute to the improvement of damping capacities.

Dilute long period stacking/order(LPSO)-variant phases along the composition gradient in a Mg-Ho-Cu alloy

We have systematically investigated the microstructures of as-cast Mg_(97.49)Ho_(1.99)Cu_(0.43)Zr_(0.09)alloy by atomic resolution high-angle annular dark field scanning transmission electron microscopy(HAADF-STEM), revealing the coexistence of 18R, 14H and 24R long period stacking/order(LPSO) phases with fully coherent interfaces along step-like composition gradient in a blocky intermetallic compound distributed at grain boundary. The short-range order(SRO) L1_(2)-type Cu_(6)Ho_(8)clusters embedded across AB’C’A-stacking fault layers are directly revealed at atomic scale. Importantly, the order degree of SRO clusters in the present dilute alloy is significant lower than previous 6M and 7M in-plane order reported in ternary Mg-TM(transition metal)-RE(rare earth) alloys, which can be well matched by 9M in-plane order. This directly demonstrates that SRO in-plane L1_(2)-type clusters can be expanded into more dilute composition regions bounded along the definite TM/RE ratio of 3/4. In addition, the estimated chemical compositions of solute enriched stacking fault(SESF) in all LPSO variants are almost identical with the ideal SESF composition of 9M in-plane order, regardless of the type of LPSO phases. The results further support the viewpoint that robust L1_(2)-type TM_(6)RE_(8)clusters play an important role in governing LPSO phase formation.

Microstructure and mechanical properties of a compound reinforced Mg95Y2.5Zn2.5 alloy with long period stacking ordered phase and W phase

The microstructure evolution of Mg100-2xYxZnx （x=2, 2.5, 3, 3.5） alloys was investigated. Results show that the Mg100-2xYxZnx alloys are composed of a-Mg, long period stacking ordered （LPSO） phase and eutectic structure phase （W phase）, and the Mg95Y2.5Zn2.5 alloy has the best comprehensive mechanical properties. Subsequently, the microstructure evolution of the optimized alloy Mg95Y2.5Zn2.5 during solidification and heat treatment processes was analyzed and discussed by means of OM, SEM, TEM, XRD and DTA. After heat treatment, the lamellar phase 14H-LPSO precipitated in a-Mg and W phase transforms into particle phase （MgyZn2）. Due to the compound reinforcement effect of the particle phase and LPSO phase （18R＋14H）, the mechanical properties of the alloy are enhanced. The tensile strength and elongation of the Mg95Y2.5Zn2.5 alloy is improved by 9.1% and 31.3% to 215 MPa and 10.5%, respectively, after solid-solution treatment.

Effects of multimodal microstructure on fracture toughness and its anisotropy of LPSO-type extruded Mg-1Zn-2Y alloys

The fracture toughness of extruded Mg-1Zn-2Y(at.%)alloys,featuring a multimodal microstructure containing fine dynamically recrystallized(DRXed)grains with random crystallographic orientation and coarse-worked grains with a strong fiber texture,was investigated.The DRXed grains comprised randomly oriented equiaxedα-Mg grains.In contrast,the worked grains includedα-Mg and long-period stacking ordered(LPSO)phases that extended in the extrusion direction(ED).Both types displayed a strong texture,aligning the10.10direction parallel to the ED.The volume fractions of the DRXed and worked grains were controlled by adjusting the extrusion temperature.In the longitudinal-transverse(L-T)orientation,where the loading direction was aligned parallel to the ED,there was a tendency for the conditional fracture toughness,KQ,tended to increase as the volume fraction of the worked grains increased.However,the KQ values in the T-L orientation,where the loading direction was perpendicular to the ED,decreased with an increase in the volume fraction of the worked grains.This suggests strong anisotropy in the fracture toughness of the specimen with a high volume fraction of the worked grains,relative to the test direction.The worked grains,which included the LPSO phase and were elongated perpendicular to the initial crack plane,suppressed the straight crack extension,causing crack deflection,and generating secondary cracks.Thus,these worked grains significantly contributed to the fracture toughness of the extruded Mg-1Zn-2Y alloys in the L-T orientation.

Effect of Precipitated Phases on Corrosion of Mg95.8Gd3Zn1Zr0.2 Alloy with Long-Period Stacking Ordered Structure

The microstructure of the precipitated phases of Mg95.sGd3Zn1Zro.2 alloys with long-period stacking ordered structure before and after heat treatment is discussed. The corrosion properties of the as-cast （F）, solid-solution （T4） and aging-treated （T6） alloys in 1% NaC1 solution are studied. The hydrogen evolution and electrochemical measurements display that the as-cast Mg95.sGd3Zn1Zro.2 alloy with the continuous network eutectic phase exhibits the greatest corrosion resistance, while T6 sample with some needle-like phases and the particle phases is the worst among the three alloys. It is proposed to be mainly related to the amount, composition, microstructure and distribution of the precipitated phases.

Corrosion Behavior of Mg-Zn-Y Alloy with Long-period Stacking Ordered Structures

Mg-Zn-Y alloys with long-period stacking ordered structures were prepared by an ingot casting method. The corrosion performance of Mg-Zn-Y alloys was studied by combining gas-collecting test, immersion test and electrochemical measurements in order to determine the corrosion rate and mechanism of the alloys. The results showed that the volume fraction of Mg（12）YZn phase increased and the shape of the Mg（12）YZn phase changed from discontinuous to continuous net-like with increasing Zn and Y content. The corrosion rate of the alloys greatly depended on the distribution and volume fraction of the Mg（12）YZn phase. Corrosion products appeared at the junction of Mg phase and Mg（12）YZn phase, indicating that the Mg（12）YZn phase accelerated galvanic corrosion of Mg matrix. Mg（97）Zn1Y2 alloy shows the lowest corrosion rate due to the continuous distribution of Mg（12）YZn phase.

Guinier-Preston Zone,Quasicrystal and Long-period Stacking Ordered Structure in Mg-based Alloys,A Review

Both the solid solution and precipitation are mainly strengthening mechanism for the magnesium-based alloys. A great number of alloying elements can be dissolved into the Mg matrix to form the solutes and precipitates.Moreover, the type of precipitates varies with different alloying elements and heat treatments, which makes it quite difficult to understand the formation mechanism of the precipitates in Mg-based alloys in depth. Thus, it is very hard to give a systematical regularity in precipitation process for the Mg-based alloys. This review is mainly focused on the formation and microstructural evolution of the precipitates, as a hot topic for the past few years, including Guinier-Preston Zones, quasicrystals and long-period stacking ordered phases formed in a number of Mg-TM-RE alloy systems, where TM = Al, Zn, Zr and RE = Y,Gd, Hd, Ce and La.

Microstructure and tribological behavior of Mg-Gd-Zn-Zr alloy with LPSO structure

A Mg-14.28Gd-2.44Zn-0.54Zr （mass fraction, %） alloy was prepared by conventional ingot metallurgy （I/M）. The microstructure differences in as-cast and solution-treated alloys were investigated. Sliding tribological behaviors of the as-cast and solution-treated alloys were investigated under oil lubricant condition by pin-on-disc configuration. The wear loss and friction coefficients were measured at a load of 40 N and sliding speeds of 30-300 mm/s with a sliding distance of 5000 m at room temperature. The results show that the as-cast alloy is mainly composed ofα-Mg solid solution, the lamellar 14H-type long period stacking ordered （LPSO） structure within matrix, andβ-[（Mg,Zn）3Gd] phase. However, most of theβ-phase transforms to X-phase with 14H-type LPSO structure after solution heat treatment at 773 K for 35 h （T4）. The solution-treated alloy presents low wear-resistance, because the hard β-phase is converted into thermally-stable, ductile and soft X-Mg12GdZn phase with LPSO structure in the alloy.

Interfacial dislocations dominated lateral growth of long-period stacking ordered phase in Mg alloys

Understanding the interface between strengthening precipitates and matrix in alloys, especially at the atomic level, is a critical issue for tailoring the precipitate strengthening to achieve desired mechanical properties. Using high-resolution scanning transmission electron microscopy, we here clarify the semicoherent interfaces between the matrix and long-period stacking ordered(LPSO) phases, including 18 R and 14 H, in Mg–Zn–Y alloys. The LPSO/Mg interface features the unique configuration of the Shockley partial dislocations, which produces a near zero macroscopic strain because the net Burgers vectors equal zero. The 18 R/Mg interface characterizes a dissociated structure that can be described as a narrow slab of 54 R. There are two dislocation arrays accompanied to the 18 R/54 R and 54 R/Mg interface, resulting a slight deviation(about 2.3°). The 14 R/Mg interface exhibits the dislocation pairs associated with solute atoms. We further evaluate the stability and morphology of the corresponding interfaces based on elastic interaction, via calculating the mutual strong interactions between dislocation arrays, as well as that between the dislocations and solute atoms. The synchronized migration of interfacial dislocations and solute atoms, like move-drag behavior, dominates the lateral growth of LPSO phases in Mg alloys.

In-situ study of the microstructure evolution during tension of a Mg-Y-Zn-Al alloy processed by rapidly solidified ribbon consolidation technique

Mg-Y-Zn-Al alloys processed by rapidly solidified ribbon consolidation(RSRC)technique exhibit an exceptional mechanical performance indicating promising application potential.This material has a bimodal microstructure consisting of fine recrystallized and coarse non-recrystallized grains with solute-rich stacking faults forming cluster arranged layers(CALs)and nanoplates(CANaPs),or complete long period stacking ordered(LPSO)phase.In order to reveal the deformation mechanisms,in-situ synchrotron X-ray diffraction line profile analysis was employed for a detailed study of the dislocation arrangement created during tension in Mg-0.9%Zn-2.05%Y-0.15%Al(at%)alloy.For uncovering the effect of the initial microstructure on the mechanical performance,additional samples were obtained by annealing of the as-consolidated specimen at 300 and 400℃ for 2 h.The heat treatment at 300℃ had no significant effect on the initial microstructure,its evolution during tension and,thus,the overall deformation behavior under tensile loading.On the other hand,annealing at 400℃ resulted in a significant increase of the recrystallized grains fraction and a decrease of the dislocation density,leading to only minor degradation of the mechanical strength.The maximum dislocation density at the failure of the samples corresponding to the plastic strain of 10-25% was estimated to be about 16-20×10^(14)m^(-2).The diffraction profile analysis indicated that most dislocations formed during tension were of non-basal and pyramidal types,what was also in agreement with the Schmid factor values revealed independently from orientation maps.It was also shown that the dislocation-induced Taylor hardening was much lower below the plastic strain of 3% than above this value,which was explained by a model of the interaction between prismatic dislocations and CANaPs/LPSO plates.

Evolution of precipitates in Mg−7Gd−3Y−1Nd−1Zn−0.5Zr alloy with fine plate-like 14H-LPSO structures aged at 240℃

The morphology and crystal structure of the precipitates in Mg-7Gd-3Y-1Nd-1Zn-0.5Zr(wt.%)alloy with fine plate-like 14H-LPSO structures aged at 240℃were investigated using transmission electron microscopy(TEM)and high-angle annular dark-field scanning transmission electron microscopy(HAADF-STEM).Fine plate-like 14H-LPSO structures precipitate after heat treatment at 500℃for 2 h,andβ-type phases precipitate after the alloy is aged at 240℃.The long-period atomic stacking sequence of 14H-LPSO structures along the[0001]αdirection is ABABCACACACBABA.After being aged at 240℃for 2 h,theβ-type phases are the ordered solution clusters,zig-zag GP zones,and a small number ofβ′phases.The peak hardness is obtained at 240℃for 18 h with a Brinell hardness of 112,theβ-type phases areβ’phases and local RE-rich structures.After being aged at 240℃for 100 h,theβ-type phases areβ’,β1 andβ’F phases.β′phases nucleate from the zig-zag GP zones directly withoutβ″phases,and then transform intoβ1 phase byβ’→β’F→β1 transformations.The Zn not only can form LPSO structure,but also is the constituent element ofβ1 phases.LPSO structures have a certain hindrance to the coarsening ofβ’andβ1 along<0001>α.

The effect of the 18R-LPSO phase on the fatigue behavior of extruded Mg/LPSO two-phase alloy through a comparative experimental-numerical study

The fatigue behavior of four extruded Mg-Y-Zn alloys containing different volume fractions of long-period stacking ordered(LPSO)grains was investigated through a comparative study combining experiments and crystal plasticity finite element simulations.Strain controlled low-cycle fatigue experiments were conducted at different strain amplitudes and revealed a limited cyclic hardening in Mg_(89)Zn_(4)Y_(7)alloy or softening in Mg_(99.2)Zn_(0.2)Y_(0.6)and Mg_(97)Zn_(1)Y_(2)alloys.A decrease in the fatigue life against the plastic strain with the increase in LPSO phase volume fraction was observed and was related the limited ductility of extruded LPSO grains.Stress-strain hysteresis curves were used to calibrate and validate a crystal plasticity model taking into account twinning and detwinning.The interaction of the different phases on the distribution of local micro-mechanical fields at the grain scale was then analyzed on synthetic microstructures under strain-controlled conditions.Deformation twinning activity was predicted in coarse unrecrystallized grains and tended to disappear with the increase in the LPSO phase volume fraction.Cleavage-like facets observed in LPSO grains were related to high tensile stress,especially at the Mg/LPSO interface,due to the limited number of deformation mechanisms in LPSO crystal to accommodate out-of-basal plane strain.The increase of the fatigue limit with the increase in LPSO phase volume fraction was finally associated with the decreasing presence of coarse unrecrystallizedα-Mg grains due to a higher dynamic recrystallization activity during the extrusion process.

Formation of β' phase in LPSO structures in an Mg88Co5Y7 alloy

Formation of β’ phase in long-period stacking ordered(LPSO) structures in an Mg;Co;Y;(at.%) alloy after aging at 200 °C for 24 h or electron beam(EB) irradiation has been studied by high-angle annular dark-field scanning transmission electron microscopy(HAADFSTEM). β’ phase was precipitated only in the Mg matrix but not in LPSO structures after aging at 200 °C for 24 h. LPSO structure containing stacking defects transforms into the β’-long phase during EB irradiation, which plays a key role in accelerating solute atoms’ diffusion. New complex β’(LPSO) structures formed in the alloy after EB irradiation, such as β’(12 H) structure with an orthorhombic lattice(Mg;Y, Cmcm,a = 2 _(a0)= 0.642 nm, b=4√3_(a0), c = 6 _(c0)= 3.12 nm).

The role of melt cooling rate on the interface between 18R and Mg matrix in Mg_(97)Zn_(1)Y_(2) alloys

The role of melt cooling rate on the interface morphology and dislocation configuration between 18R long-period stacking ordered(LPSO)structure and Mg matrix in Mg_(97)Zn_(1)Y_(2)(at.%)alloys was investigated by atomic-scale HAADF-STEM imaging.The 18R/Mg interface is step-like both in the near-equilibrium alloy and non-equilibrium alloy.Lower cooling rate makes the step size more regular and larger.Only 54R structure can be observed at the interface in the near-equilibrium alloy,and the dislocations are highly ordered.54R and 54R′structure sandwiched by b1 and b2+b3 dislocation arrays,and new dislocation configuration can be detected at the interface in the non-equilibrium alloy,but the dislocations are less ordered.18R/Mg interface containing 54R or 54R′in equilibrium width,parallel to the(010)plane,should be most stable based on elastic calculation.The segregation of solute atoms and its strong interaction with dislocations dominate the LPSO/Mg interface via diffusion-displacive transformation.