Twin-twin geometric structure effect on the twinning behavior of an Mg-4Y-3Nd-2Sm-0.5Zr alloy traced by quasi-in-situ EBSD

We studied the microstructure evolution of Mg-4Y-3Nd-2Sm-0.5Zr alloy by quasi-in-situ electron backscatter diffraction(EBSD)along with several strains under compression tests,which provided direct evidence for the influence of different twin-twin geometric structure on the twinning behavior.The results showed that the mechanical properties of the alloy were higher than traditional magnesium alloys(the maximum compressive strength reaches 402.5 MPa)due to the strengthening effect of Sm and Nd elements addition on solution strengthening,precipitation strengthening,and grain refinement.Combined with the quasi-in-situ EBSD technique,two different twin-twin geometric structures,‘parallel structure’and‘cross structure’,were observed directly in the alloy.In the later stage of deformation,for‘parallel structure’,residual stress and a large number of dislocations mainly existed in the twin boundary and tip position.For the‘cross structure’,there was a lot of dislocation density in the interior of twins after fusion.The twin growth rate of‘parallel structure’was much faster than that of‘cross structure’because the stress of twins was mainly concentrated on the tip of twin.When the movement for the tip of twin was blocked,the growth rate of twin would be obviously decreased.Moreover,the‘cross structure’was easy to produce closed space.Due to the constraints of surrounding twins,the confined space was easy to stress concentration,thus inhibiting the growth of twins.At the same time,the‘cross structure’of twins needed a more external force to continue to deform,which also served as a strengthening structure.

材料变形过程中的原位电子背散射衍射(in-situ EBSD)分析

本文介绍一套既具备电子背散射衍射(EBSD),又具备应力加载功能的分析测试方法,简称原位EBSD。采用该系统能实现对拉伸、压缩、弯曲及剪切变形过程中材料的微观组织演变进行原位跟踪观察;可以分析材料在变形过程中的组织演变过程,获得组织演变的连续性信息,从而对研究材料变形过程中的机理及物理本质提供有力的实验依据。本文还以原位压缩过程中纯镁的微观组织演变的测试与分析为例,说明原位EBSD系统使用方法。

Quasi in-situ EBSD analysis of twinning-detwinning and slip behaviors in textured AZ31 magnesium alloy subjected to compressive-tensile loading

Twinning and detwinning behavior,together with slip behavior,are studied in a textured AZ31 magnesium alloy under compressive and tensile strains along the rolling direction(RD)after each interrupted mechanical test via quasi in-situ electron backscattered diffraction technique.The results show that twinning firstly takes place under the compressive strain along the RD.With the increasing compressive strain,{1012}tensile twins firstly nucleate,then propagate,and finally thicken.While under a reversed tensile strain along the RD,detwinning occurs.No nucleation happens during detwinning.Thus,tensile twins can detwin at lower tensile strain,followed by thinning,shortening,and vanishing.Slips are also activated to accommodate the plastic deformation.In the matrix,prismatic slip can only dominate at relatively high strains.Otherwise,basal slip dominates.While in the twins,prismatic slip can activate at lower strains,which is ascribed to the texture reorientation.

A review of in-situ EBSD experiments

Automated EBSD or Orientation Imaging Microscopy (OIM) systems are being used in combination with other equipment within the scanning electron microscope (SEM) to perform in-situ measurements. This paper briefly reviews OIM studies of in-situ experiments performed using tensile and heating stages as well as in-situ serial sectioning. In particular, in-situ OIM scan results on an aluminum alloy sample deformed in tension; phase transformations in a cobalt sample, recrystallization and grain growth in a copper sample and serial sectioning of a nickel super-alloy sample are reviewed.

An in-situ study of static recrystallization in Mg using high temperature EBSD

It has been a common method to improve the mechanical properties of metals by manipulating their microstructures via static recrystallization,i.e.,through heat treatment.Therefore,the knowledge of recrystallization and grain growth is critical to the success of the technique.In the present work,by using in-situ high temperature EBSD,the mechanisms that control recrystallization and grain growth of an extruded pure Mg were studied.The experimental results revealed that the grains of priority for dynamic recrystallization exhibit fading competitiveness under static recrystallization.It is also found that grain boundary movement or grain growth is likely to show an inverse energy gradient effect,i.e.,low energy grains tend to swallow or grow into high energy grains,and grain boundaries of close to 30°exhibit superior growth advantage to others.Another finding is that{10-12}tensile twin boundaries are sites of hardly observed for recrystallization,and are finally swallowed by adjacent recrystallized grains.The above findings may give comprehensive insights of static recrystallization and grain growth of Mg,and may guide the design of advanced materials processing in microstructural engineering.

含铜抗菌不锈钢拉伸过程中的微观组织演变EBSD分析

目的研究含铜抗菌不锈钢拉伸性能,为工业生产中的成形工艺优化提供一定的理论依据。方法在拉伸应变分别为5%、15%、30%、45%、60%、75%以及最后拉伸断裂时应变为81%条件下,采用岛津AGS-100KN万能拉伸试验机对含铜抗菌不锈钢进行拉伸试验。通过扫描电子显微镜(SEM)、电子背散射衍射仪(EBSD)和透射电子显微镜(TEM)表征分析含铜抗菌不锈钢拉伸断裂后的断口形貌以及拉伸过程中的微观组织演变。结果含铜抗菌不锈钢抗拉强度最大值为587.523 MPa,应变最大值为81%。拉伸断口与拉伸方向呈45°开裂,呈杯锥状,断裂模式是韧性断裂。结论随着应变的增大,低角度晶界逐渐增多,高角度晶界与孪晶逐渐减少,GOS值逐渐增大,Goss织构、S织构和R织构含量逐渐减少,Brass织构含量逐渐增加,拉伸断裂后的体积分数为23.3%。在拉伸后期,Copper织构和Brass织构含量较多,在拉伸过程中起到整体稳定协调微观组织作用的S织构不断减少,随应变的增大,组织内部协调变形加快,变形程度快速增大,从而导致S织构向Copper织构和Brass织构转变,出现板条状马氏体,存在应变诱发马氏体相变。位错滑移、形变孪晶和形变诱导马氏体等多种变形机制的共同作用使含铜抗菌不锈钢具有良好的塑性。

高强双相钢氩离子抛光EBSD制备研究

利用Gatan公司的685型多功能氩离子抛光镀膜仪对铁素体-马氏体高强双相钢EBSD样品进行制备。采用正交法研究了氩离子加速电压、抛光时间以及入射角度对高强双相钢EBSD衍射花样标定率的影响。结果表明,随着加速电压、抛光时间及氩离子入射角度的增加,可有效地降低砂纸打磨痕迹对EBSD衍射花样标定的影响,且花样标定率明显提高,试样表面平整度增加。

Z2CND18.12N奥氏体不锈钢低周疲劳损伤的EBSD分析

针对核电管道用Z2CND18.12N奥氏体不锈钢的低周疲劳损伤,研究电子背散射衍射(electron backscattered diffraction,EBSD)采集与后处理参数对局域取向差(local misorientation,ML)的影响,基于优选参数探讨特征取向晶粒的损伤规律。结果表明:测试步长、取向差平均范围(filter)及像素合并参数(binning)均影响ML测试结果,综合考虑晶粒尺寸、测试精度和效率等因素,优选确定binning 2×2,filter 11×11,测试步长为2μm或5μm。选取损伤程度不同的两个区域,〈111〉取向晶粒ΔM_(L)的峰值和平均值变化均高于〈101〉和〈001〉取向,〈101〉取向ΔM_(L)数值最小;同时,ML在小晶粒特别是晶界及交汇处数值较大。结合晶粒尺寸、晶界对变形分布的不均匀性进行了讨论。结果证实ML可以有效评价Z2CND18.12N钢的变形损伤,为发展基于多物理参量的材料以及结构损伤评价技术提供了参考和借鉴。

In-situ interfacial passivation and self-adaptability synergistically stabilizing all-solid-state lithium metal batteries

The function of solid electrolytes and the composition of solid electrolyte interphase(SEI)are highly significant for inhibiting the growth of Li dendrites.Herein,we report an in-situ interfacial passivation combined with self-adaptability strategy to reinforce Li_(0.33)La_(0.557)TiO_(3)(LLTO)-based solid-state batteries.Specifically,a functional SEI enriched with LiF/Li_(3)PO_(4) is formed by in-situ electrochemical conversion,which is greatly beneficial to improving interface compatibility and enhancing ion transport.While the polarized dielectric BaTiO_(3)-polyamic acid(BTO-PAA,BP)film greatly improves the Li-ion transport kinetics and homogenizes the Li deposition.As expected,the resulting electrolyte offers considerable ionic conductivity at room temperature(4.3 x 10~(-4)S cm^(-1))and appreciable electrochemical decomposition voltage(5.23 V)after electrochemical passivation.For Li-LiFePO_(4) batteries,it shows a high specific capacity of 153 mA h g^(-1)at 0.2C after 100 cycles and a long-term durability of 115 mA h g^(-1)at 1.0 C after 800 cycles.Additionally,a stable Li plating/stripping can be achieved for more than 900 h at 0.5 mA cm^(-2).The stabilization mechanisms are elucidated by ex-situ XRD,ex-situ XPS,and ex-situ FTIR techniques,and the corresponding results reveal that the interfacial passivation combined with polarization effect is an effective strategy for improving the electrochemical performance.The present study provides a deeper insight into the dynamic adjustment of electrode-electrolyte interfacial for solid-state lithium batteries.

Interplay of laser power and pore characteristics in selective laser melting of ZK60 magnesium alloys:A study based on in-situ monitoring and image analysis

This study offers significant insights into the multi-physics phenomena of the SLM process and the subsequent porosity characteristics of ZK60 Magnesium(Mg)alloys.High-speed in-situ monitoring was employed to visualise process signals in real-time,elucidating the dynamics of melt pools and vapour plumes under varying laser power conditions specifically between 40 W and 60 W.Detailed morphological analysis was performed using Scanning-Electron Microscopy(SEM),demonstrating a critical correlation between laser power and pore formation.Lower laser power led to increased pore coverage,whereas a denser structure was observed at higher laser power.This laser power influence on porosity was further confirmed via Optical Microscopy(OM)conducted on both top and cross-sectional surfaces of the samples.An increase in laser power resulted in a decrease in pore coverage and pore size,potentially leading to a denser printed part of Mg alloy.X-ray Computed Tomography(XCT)augmented these findings by providing a 3D volumetric representation of the sample internal structure,revealing an inverse relationship between laser power and overall pore volume.Lower laser power appeared to favour the formation of interconnected pores,while a reduction in interconnected pores and an increase in isolated pores were observed at higher power.The interplay between melt pool size,vapour plume effects,and laser power was found to significantly influence the resulting porosity,indicating a need for effective management of these factors to optimise the SLM process of Mg alloys.

In-situ X-ray computed tomography tensile tests and analysis of damage mechanism and mechanical properties in laser powder b e d fused Invar 36 alloy

Laser powder bed fusion(LPBF)is a potential additive manufacturing process to manufacture Invar 36 alloy components with complicated geometry.Whereas it inevitably introduces specific microstructures and pore defects,which will further influence the mechanical properties.Hence,aiming at exploring the LPBF process-related microstructures and pore defects,and especially their influences on the damage mechanism and mechanical properties,Invar 36 alloy was manufactured by LPBF under designed different laser scanning speeds.The microstructure observations reveal that higher scanning speeds lead to equiaxed and short columnar grains with higher dislocation density,while lower scanning speeds result in elongated columnar grains with lower dislocation density.The pore defects analyzed by X-ray computed tomography(XCT)suggest that the high laser scanning speed gives rise to numerous lamellar and large lack-of-fusion(LOF)pores,and the excessively low laser scanning speed produces relatively small keyhole pores with high sphericity.Moreover,the insitu XCT tensile tests were originally performed to evaluate the damage evolution and failure mechanism.Specifically,high laser scanning speed causes brittle fracture due to the rapid growth and coalescence of initial lamellar LOF pores along the scan-ning direction.Low laser scanning speed induces ductile fracture originating from unstable depressions in the surfaces,while metallurgical and keyhole pores have little impact on damage evolution.Eventually,the process-structure-property correlation is established.The presence of high volume fraction of lamel-lar LOF pores,resulting from high scanning speed,leads to inferior yield strength and ductility.Besides,specimens without LOF pores exhibit larger grain sizes and lower dislocation density at decreased scanning speeds,slightly reducing yield strength while slightly enhancing ductility.This understanding lays the foundation for widespread applications of LPBF-processed Invar 36 alloy.

电解铜箔截面微观组织的EBSD分析

目的通过树脂包埋结合离子截面抛光的制备方法,实现铜箔样品的截面EBSD分析,进而利用截面EBSD分析方法探究电流密度对铜箔组织性能的影响。方法通过使用热固性树脂对铜箔进行包埋,使用加热平台使胶体凝固,对得到的包埋好的铜箔试样在砂纸上进行截面打磨,放入截面离子抛光仪中进行离子切割,样品制备完成后,将样品取下。使用电子背散射(EBSD)作为电镜附件,进行晶体学取向的表征。结果结合截面微观组织的EBSD分析方法,分析了电流密度对铜箔组织性能的影响,结果表明,随着电流密度的增大,电解铜箔的晶粒尺寸呈现出先减小后增大的趋势,孪晶密度和位错密度呈现出先增大后减小的趋势,抗拉强度在45 A/dm^(2)时达到最大547.05 MPa。结论该方法可以利用EBSD分析软件自动分析铜箔截面的晶粒粒度分布、孪晶密度等,并将这些微观结构特征与力学性能结果进行详细对比分析,验证了电流密度对铜箔组织和性能的显著影响。

Ti60钛合金中等轴α相变形机理的原位EBSD研究

本文通过热处理得到了具有等轴状α相的Ti60钛合金,并用原位背散射电子衍射(in-situ EBSD)技术,系统研究了该合金单轴拉伸过程中的塑性变形机制。结果表明:该合金的塑性变形机制以滑移为主导,主要滑移系为{0001}<1ˉ2ˉ1ˉ0>和{011ˉ0}<112ˉ0>,且前者早于后者启动。值得注意的是,当拉伸应变超过10%时,{101ˉ2}<1ˉ011>孪晶开始启动,并进一步协调基体的变形。

In-situ coating and surface partial protonation co-promoting performance of single-crystal nickel-rich cathode in all-solid-state batteries

The poor electrochemical performance of all-solid-state batteries(ASSBs),which is assemblied by Ni-rich cathode and poly(ethylene oxide)(PEO)-based electrolytes,can be attributed to unstable cathodic interface and poor crystal structure stability of Ni-rich cathode.Several coating strategies are previously employed to enhance the stability of the cathodic interface and crystal structure for Ni-rich cathode.However,these methods can hardly achieve simplicity and high efficiency simultaneously.In this work,polyacrylic acid(PAA)replaced traditional PVDF as a binder for cathode,which can achieve a uniform PAA-Li(LixPAA(0<x≤1))coating layer on the surface of single-crystal LiNi_(0.83)Co_(0.12)Mn_(0.05)O_(2)(SC-NCM83)due to H^(+)/Li^(+)exchange reaction during the initial charging-discharging process.The formation of PAA-Li coating layer on cathode can promote interfacial Li^(+)transport and enhance the stability of the cathodic interface.Furthermore,the partially-protonated surface of SC-NCM83 casued by H^(+)/Li^(+)exchange reaction can restrict Ni ions transport to enhance the crystal structure stability.The proposed SC-NCM83-PAA exhibits superior cycling performance with a retention of 92%compared with that(57.3%)of SC-NCM83-polyvinylidene difluoride(PVDF)after 200 cycles.This work provides a practical strategy to construct high-performance cathodes for ASSBs.

Assessing the conservation impact of Chinese indigenous chicken populations between ex-situ and in-situ using genome-wide SNPs

Conservation programs require rigorous evaluation to ensure the preservation of genetic diversity and viability of conservation populations. In this study, we conducted a comparative analysis of two indigenous Chinese chicken breeds, Gushi and Xichuan black-bone, using whole-genome SNPs to understand their genetic diversity, track changes over time and population structure. The breeds were divided into five conservation populations(GS1, 2010, ex-situ;GS2, 2019, ex-situ;GS3, 2019, in-situ;XB1, 2010, in-situ;and XB2, 2019, in-situ) based on conservation methods and generations. The genetic diversity indices of three conservation populations of Gushi chicken showed consistent trends, with the GS3 population under in-situ strategy having the highest diversity and GS2 under ex-situ strategy having the lowest. The degree of inbreeding of GS2 was higher than that of GS1 and GS3. Conserved populations of Xichuan black-bone chicken showed no obvious changes in genetic diversity between XB1 and XB2. In terms of population structure, the GS3 population were stratified relative to GS1 and GS2. According to the conservation priority, GS3 had the highest contribution to the total gene and allelic diversity in GS breed, whereas the contribution of XB1 and XB2 were similar. We also observed that the genetic diversity of GS2 was lower than GS3, which were from the same generation but under different conservation programs(in-situ and ex-situ). While XB1 and XB2 had similar levels of genetic diversity. Overall, our findings suggested that the conservation programs performed in ex-situ could slow down the occurrence of inbreeding events, but could not entirely prevent the loss of genetic diversity when the conserved population size was small, while in-situ conservation populations with large population size could maintain a relative high level of genetic diversity.

In-situ AFM and quasi-in-situ studies for localized corrosion in Mg-9Al-1Fe-(Gd) alloys under 3.5 wt.% NaCl environment

Revealing the localized corrosion process of Mg alloy is considered as one of the most significant ways for improving its corrosion resistance.The reliable monitor should be high distinguishability and real-time in liquid environment.Herein,Mg-9Al-1Fe and Mg-9Al-1Fe-1Gd alloys were designed to highlight the impact of intermetallic on the corrosion behaviour.In-situ AFM with a special electrolyte circulation system and quasi-in-situ SEM observation were used to monitor the corrosion process of the designed alloys.SEM-EDS and TEM-SAED were applied to identify the intermetallic in the designed alloys,and their volta potentials were measured by SKPFM.According to the real-time and real-space in-situ AFM monitor,the corrosion process consisted of dissolution of anodicα-Mg phase,accumulation of corrosion products around cathodic phase and shedding of some fine cathodic phase.Then,the localized corrosion process of Mg alloy was revealed combined with the results of the monitor of corrosion process and Volta potential difference.

A continuous and long-term in-situ stress measuring method based on fiber optic. Part I: Theory of inverse differential strain analysis

A method for in-situ stress measurement via fiber optics was proposed. The method utilizes the relationship between rock mass elastic parameters and in-situ stress. The approach offers the advantage of long-term stress measurements with high spatial resolution and frequency, significantly enhancing the ability to measure in-situ stress. The sensing casing, spirally wrapped with fiber optic, is cemented into the formation to establish a formation sensing nerve. Injecting fluid into the casing generates strain disturbance, establishing the relationship between rock mass properties and treatment pressure.Moreover, an optimization algorithm is established to invert the elastic parameters of formation via fiber optic strains. In the first part of this paper series, we established the theoretical basis for the inverse differential strain analysis method for in-situ stress measurement, which was subsequently verified using an analytical model. This paper is the fundamental basis for the inverse differential strain analysis method.

An in-situ self-etching enabled high-power electrode for aqueous zinc-ion batteries

Sluggish storage kinetics is considered as the main bottleneck of cathode materials for fast-charging aqueous zinc-ion batteries(AZIBs).In this report,we propose a novel in-situ self-etching strategy to unlock the Palm tree-like vanadium oxide/carbon nanofiber membrane(P-VO/C)as a robust freestanding electrode.Comprehensive investigations including the finite element simulation,in-situ X-ray diffraction,and in-situ electrochemical impedance spectroscopy disclosed it an electrochemically induced phase transformation mechanism from VO to layered Zn_(x)V_(2)O_5·nH_(2)O,as well as superior storage kinetics with ultrahigh pseudocapacitive contribution.As demonstrated,such electrode can remain a specific capacity of 285 mA h g^(-1)after 100 cycles at 1 A g^(-1),144.4 mA h g^(-1)after 1500 cycles at 30 A g^(-1),and even 97 mA h g^(-1)after 3000 cycles at 60 A g^(-1),respectively.Unexpectedly,an impressive power density of 78.9 kW kg^(-1)at the super-high current density of 100 A g^(-1)also can be achieved.Such design concept of in-situ self-etching free-standing electrode can provide a brand-new insight into extending the pseudocapacitive storage limit,so as to promote the development of high-power energy storage devices including but not limited to AZIBs.

Microstructural characterization and mechanical properties of(TiC+TiB)/TA15 composites prepared by an in-situ synthesis method

Titanium matrix composites reinforced with ceramic particles are considered a promising engineering material due to their combination of high specific strength,low density,and high modulus.In this study,the TA15-based composites reinforced with a volume fraction of 10% to 25%(TiB+TiC)were prepared using powder metallurgy and casting technique.Microstructural characterization and phase constitution were examined using optical microscopy(OM),scanning electron microscopy(SEM),and X-ray diffraction(XRD).In addition,the microhardness,room temperature(RT)and high temperature(HT)tensile properties of the composites were evaluated.Results revealed that the reinforcements are distributed uniformly even in the composites with a high volume of TiB and TiC.However,as the volume fraction exceeds 15%,TiB and TiC particles become coarsening and exhibit rod-like and dendritic-like morphology.Microhardness increases gradually from 321.2 HV for the base alloy to a maximum of 473.3 HV as the reinforcement increases to 25vol.%.Tensile test results indicate that a reinforcement volume fraction above 20% is beneficial for enhancing tensile strength and yield strength at high temperatures,but it has an adverse effect on room temperature elongation.Conversely,if the reinforcement volume fraction is below 20%,it can improve high-temperature elongation when the temperature exceeds 600℃.

A review of in-situ high-temperature characterizations for understanding the processes in metallurgical engineering

For the rational manipulation of the production quality of high-temperature metallurgical engineering,there are many challenges in understanding the processes involved because of the black box chemical/electrochemical reactors.To overcome this issue,various in-situ characterization methods have been recently developed to analyze the interactions between the composition,microstructure,and solid-liquid interface of high-temperature electrochemical electrodes and molten salts.In this review,recent progress of in-situ hightemperature characterization techniques is discussed to summarize the advances in understanding the processes in metallurgical engineering.In-situ high-temperature technologies and analytical methods mainly include synchrotron X-ray diffraction(s-XRD),laser scanning confocal microscopy,and X-ray computed microtomography(X-rayμ-CT),which are important platforms for analyzing the structure and morphology of the electrodes to reveal the complexity and variability of their interfaces.In addition,laser-induced breakdown spectroscopy,high-temperature Raman spectroscopy,and ultraviolet-visible absorption spectroscopy provide microscale characterizations of the composition and structure of molten salts.More importantly,the combination of X-rayμ-CT and s-XRD techniques enables the investigation of the chemical reaction mechanisms at the two-phase interface.Therefore,these in-situ methods are essential for analyzing the chemical/electrochemical kinetics of high-temperature reaction processes and establishing the theoretical principles for the efficient and stable operation of chemical/electrochemical metallurgical processes.