Scanning transmission electron microscopy and atom probe tomography analysis of non-stoichiometry long-period-stacking-ordered structures in Mg-Ni-Y/Sm alloys

The long-period-stacking-ordered(LPSO)structure affects the mechanical,corrosion and hydrolysis properties of Mg alloys.The current work employs high angle annular dark field-scanning transmission electron microscopy(HAADF-STEM)and atom probe tomography(APT)to investigate the structural and local chemical information of LPSO phases formed in Mg-Ni-Y/Sm ternary alloys after extended isothermal annealing.Depending on the alloying elements and their concentrations,Mg-Ni-Y/Sm develops a two-phase LPSO+α-Mg structure in which the LPSO phase contains defects,hybrid LPSO structure,and Mg insertions.HAADF-STEM and APT indicate non-stoichiometric LPSO with incomplete Ni_(6)(Y/Sm)_(8) clusters.In addition,the APT quantitatively determines the local composition of LPSO and confirms the presence of Ni within the Mg bonding layers.These results provide insight into a better understanding of the structure and hydrolysis properties of LPSO-Mg alloys.

Experimental Investigation of the Early Stage of Precipitation on Binary Al-Li, Al-Cu Alloys and Ternary Al-Li-Cu Alloys by Means of Atom Probe Tomography

Aluminum-based alloys play a key role in modern engineering and are widely used in construction components in aircraft, automobiles and other means of transportation due to their light weight and superior mechanical properties. Introduction of different nano-structure features can improve the service and the physical properties of such alloys. An improvement of an Al-based alloy has been performed based on the understanding of the relationships among compositions, processing, microstructural characteristics and properties. Knowledge of the decomposition process of the microstructure during the precipitation reaction is particularly important for future technical developments. The objective of this study is to investigate the nano-scale chemical composition in the Al-Cu, Al-Li and Al-Li-Cu alloys during the early stage of the precipitation sequence and to describe whether this compositional difference correlates with variations in the observed precipitation kinetics. Investigation of the fine scale segregation effects of dilute solutes in aluminum alloys which were experienced different heat treatments by using atom probe tomography has been achieved. The results show that an Al-1.7 at.% Cu alloy requires a long ageing time of approximately 8 h at 160°C to allow the diffusion of Cu atoms into Al matrix. For the Al-8.2 at.% Li alloy, a combination of both the natural ageing condition (48 h at room temperature) and a short artificial ageing condition (5 min at 160°C) induces increasing on the number density of the Li clusters and hence increase number of precipitated particles. Applying this combination of natural ageing and short artificial ageing conditions onto the ternary Al-4 at.% Li-1.7 at.% Cu alloy induces the formation of a Cu-rich phase. Increasing the Li content in the ternary alloy up to 8 at.% and increasing the ageing time to 30 min resulted in the precipitation processes ending with δ' particles. Thus the results contribute to the understanding of Al-alloy design.

Crystallization and impact history of a meteoritic sample of early lunar crust(NWA 3163)refined by atom probe geochronology

Granulitic lunar meteorites offer rare insights into the timing and nature of igneous,metamorphic and impact processes in the lunar crust.Accurately dating the different events recorded by these materials is very challenging,however,due to low trace element abundances (e.g.Sm,Nd,Lu,Hf),rare micrometerscale U-Th-bearing accessory minerals,and disturbed Ar-Ar systematics following a multi-stage history of shock and thermal metamorphism.Here we report on micro-baddeleyite grains in granulitic mafic breccia NWA 3163 for the first time and show that targeted microstructural analysis (electron backscatter diffraction) and nanoscale geochronology (atom probe tomography) can overcome these barriers to lunar chronology.A twinned (-90°/<401>) baddeleyite domain yields a 232Th/208Pb age of 4328 ± 309 Ma,which overlaps with a robust secondary ion mass spectrometry (SIMS) 207Pb/206Pb age of 4308± 18.6 Ma and is interpreted here as the crystallization age for the igneous protolith of NWA 3163.A second microstructural domain,< 2 mm in width,contains patchy overprinting baddeleyite and yields a Th-Pb age of 2175± 143 Ma,interpreted as dating the last substantial impact event to affect the sample.This finding demonstrates the potential of combining microstructural characterization with nanoscale geochronology when resolving complex P-T-t histories in planetary materials,here yielding the oldest measured crystallization age for components of lunar granulite NWA 3163 and placing further constraints on the formation and evolution of lunar crust.

Atom Probe and Mssbauer Spectroscopy Investigations of Cementite Dissolution in a Cold Drawn Eutectoid Steel

Mssbauer spectrum and three dimensional atom probes（3DAP） were combined to investigate the mechanism of cementite dissolution in a cold-drawn eutectoid steel at a true strain of 2.89.The experimental results suggest that the dislocations play an important role in the dissolution of the cementite by sweeping across the nano-scaled cementite,and transferring carbon from cementite to ferrite inducing cementite decomposition.The mechanism of cementite dissolution in the steel is discussed in association with the investigation of nonstoichiometric cementite structure after heavy deformation.

Precise measurement of a weak radio frequency electric field using a resonant atomic probe

We present a precise measurement of a weak radio frequency electric field with a frequency of ■3 GHz employing a resonant atomic probe that is constituted with a Rydberg cascade three-level atom, including a cesium ground state |6S(1/2)〉,an excited state |6P(3/2)〉, and Rydberg state |nD(5/2)〉. Two radio frequency(RF) electric fields, noted as local and signal fields, couple the nearby Rydberg transition. The two-photon resonant Rydberg electromagnetically induced transparency(Rydberg-EIT) is employed to directly read out the weak signal field having hundreds of k Hz difference between the local and signal fields that is encoded in the resonant microwave-dressed Rydberg atoms. The minimum detectable signal fields of ESmin= 1.36 ± 0.04 mV/m for 2.18 GHz coupling |68D(5/2)〉→ |69P(3/2)〉 transition and 1.33 ± 0.02 mV/m for 1.32 GHz coupling |80D(5/2)〉→ |81P(3/2)〉 transition are obtained, respectively. The bandwidth dependence is also investigated by varying the signal field frequency and corresponding -3 dB bandwidth of 3 MHz is attained. This method can be employed to perform a rapid and precise measurement of the weak electric field, which is important for the atom-based microwave metrology.

Atom Probe Tomography Study of Fe Segregation at Phase Interface in Zr–2.5Nb Alloy

β-Nb is a typical second phase in Zr-Nb-based alloys used as fuel claddings in water-cooled nuclear reactors. The segregation of alloying element Fe may affect the corrosion resistance of Zr-Nb-based alloys. In this work, the Fe segregation at the interface between β-Nb phase and a-Zr matrix in Zr-2.5Nb alloy was studied using atom probe tomography and focused ion beam. The results suggested that the Fe concentration was much lower than Nb concentration in a-Zr matrix, while Fe selectively segregated at the β-Nb/a-Zr phase interface, leading to a Fe concentration peak at some interfaces. The peak Fe concentration varied from 0.4 to 1.2 at.% and appeared at the position where Zr concentration was approximately equal to Nb concentration. The selective segregation of Fe should be affected by the heat treatment and structure defects induced by cold rolling.

Solute Clusters/Enrichment at the Early Stage of Ageing in Mg-Zn-Gd Alloys Studied by Atom Probe Tomography

Three-dimensional distribution of solute elements in an Mg–Zn–Gd alloy during ageing process is quantitatively characterized by three-dimensional atom probe(3DAP) tomography. Based on the radius distribution function, it is found that Zn–Gd solute pairs in Mg matrix appear mainly at two peaks at early stage of ageing, and the separation distance between Zn and Gd atoms could be well rationalized by the first-principle calculation. Moreover, the fraction of Zn–Gd solute pairs increases first and then decreases due to the precipitation of long-period stacking ordered(LPSO) structures. Both the composition of the structural unit in LPSO structure and the solute enrichment around it are quantified. It is found that Zn and Gd elements are synchronized in the LPSO structure, and solute segregation of pure Zn or Gd is not observed at the transformation front of the LPSO structure in this alloy. In addition, the crystallography of transformation front is further determined by 3DAP data.

IMPROVED FABRICATION METHOD FOR CARBON NANOTUBE PROBE OF ATOMIC FORCE MICROSCOPY(AFM)

An improved arc discharge method is developed to fabricate carbon nanotube probe of atomic force microscopy （AFM） here. First, silicon probe and carbon nanotube are manipulated under an optical microscope by two high precision microtranslators. When silicon probe and carbon nanotube are very close, several tens voltage is applied between them. And carbon nanotube is divided and attached to the end of silicon probe, which mainly due to the arc welding function. Comparing with the arc discharge method before, the new method here needs no coat silicon probe with metal film in advance, which can greatly reduce the fabrication＇s difficulty. The fabricated carbon nanotube probe shows good property of higher aspect ratio and can more accurately reflect the true topography of silicon grating than silicon probe. Under the same image drive force, carbon nanotube probe had less indentation depth on soft triblock copolymer sample than silicon probe. This showed that carbon nanotube probe has lower spring constant and less damage to the scan sample than silicon probe.

Two-dimensional atom localization via probe absorption in a four-level atomic system

We have investigated the two-dimensional （2D） atom localization via probe absorption in a coherently driven four-level atomic system by means of a radio-frequency field driving a hyperfine transition. It is found that the detecting probability and precision of 2D atom localization can be significantly improved via adjusting the system parameters. As a result, our scheme may be helpful in laser cooling or the atom nano-lithography via atom localization.

High-precision two-dimensional atom localization via probe absorption in an M-scheme atomic system

In the present paper, we investigate the behavior of two-dimensional atom localization in a five-level M-scheme atomic system driven by two orthogonal standing-wave fields. We find that the precision and resolution of the atom localization depends on the probe field detuning significantly. And because of the effect of the microwave field, an atom can be located at a particular position via adjusting the system parameters.

THEORETICAL ANALYSIS AND EXPERIMENTAL STUDY OF CARBON NANOTUBE PROBE AND CONVENTIONAL ATOMIC FORCE MICROSCOPY PROBE ON SURFACE ROUGHNESS

In this paper, three different tips are employed, i.e., the carbon nanotube tip, monocrystalline silicon tip and silicon nitride tip. Resorting to atomic force microscope （AFM）, they are used for measuring the surface roughness of indium tin oxide （ITO） film and the immunoglobulin G （IgG） proteins within the scanning area of 10 μm×10 μm and 0.5 μm×0.5 μm, respectively. Subsequently, the scanned surface of the ITO film and IgG proteins are analyzed by using fractal dimension. The results show that the ffactal dimension measured by carbon nanotube tip is biggest with the highest frequency components and the most microscopic information. Therefore, the carbon nanotube tip is the ideal measuring tool for measuring super-smooth surface, which will play a more and more important role in the high-resolution imaging field.

三维原子探针的电场结构模拟研究

本文针对目前世界上被广泛使用的局部电极原子探针的样品及局部电极几何结构,通过有限元方法,结合多物理场仿真技术,研究了局部电极与针状样品的距离z、样品尖端曲率半径ρ、局部电极的入口直径φ、厚度w、开口角度α和入口长度h等参数对样品尖端附近的局部电场的影响。模拟结果表明:当z与φ的取值满足z/φ≥1时,既能在样品尖端得到较高的蒸发电场强度,又能降低局部电极对离子轨迹的影响;局部电极的厚度w和开口角度α的取值对样品尖端的电场影响较小;增大局部电极入口长度h的值有利于提高样品尖端电场强度;随着原子的蒸发(样品尖端曲率半径ρ增大),为维持原子蒸发所需的电场强度,施加在样品上的电压V与样品尖端的曲率半径ρ成正比,且所需维持的电场强度越高,施加的电压V越大。

基于大高宽比CD-AFM探针的设计与制备

针对传统原子力显微镜(AFM)探针和关键尺寸原子力显微镜(CD-AFM)探针受限于针尖有效扫描高度较低,无法对深沟槽和大悬垂侧壁结构进行精准扫描成像的问题,提出了一种大高宽比针尖结构的新型CDAFM探针设计与制备方案。开发的新型CD-AFM探针针尖有效高度为5.1~5.8μm,高宽比达到14,相较于传统硅基CD-AFM探针,其有效高度提升了约4倍。利用开发的探针完成了标称深度为2.3μm、深宽比为4.6的深沟槽样品测试。

基于光束偏转法的原子力显微镜探针一致性装配系统研究

为解决原子力显微镜(Atomic Force Microscope,AFM)系统更换探针后光路调整复杂耗时、精度不足的问题,本文首次提出通过精密控制探针与探针夹装配位置来实现更换的探针相对AFM系统原光路位置的一致,进而实现免去AFM系统换针后调整光路步骤。该系统的光路一致性组件采用光束偏转法对探针位置与偏转进行放大与监测,并使用高精度位移与角度调节平台进行探针相对于探针夹的方位调整。通过实物搭建对探针一致性效果进行了验证,并对紫外光(Ultraviolet,UV)胶水固化过程导致探针位置偏移影响;探针不同偏移量时产生的探测器噪音对AFM系统成像质量影响进行了系统分析。实验结果表明:经由该系统装配的探针平均位置精度接近1.1μm;并且在AFM系统中更换一致性探针仅需8 s。该系统实现了高精度且质量稳定的探针一致性装配,极大地简化了AFM系统重新校准光路的操作步骤,其与自动换针装置配合可有效提升工业计量型AFM的操作与测量性能。

含Benzo[a]azulene单元的锯齿状梯形共轭聚合物的表面在位合成

梯形共轭聚合物(CLPs)因其独特的光电性质而受到广泛关注。绝大多数CLPs是通过溶液方法合成的,但近年来,在超高真空环境中进行的表面原位合成策略逐渐崭露头角,成为CPL合成的新方法。表面原位合成方法能够克服传统溶液合成的限制,如随着聚合度增加而受限的溶解度和结构稳定性,从而实现复杂共轭结构的精确合成。Azulene衍生物是在表面合成非苯型CLPs的有吸引力的前体。与传统的只含六元环的CLPs相比,使用烷基取代的azulene作为前体分子,有望获得具有复杂骨架结构的CLPs,从而调控其电子性质,但目前很少有人探索这种策略。本文报道了3,3'-二溴-2,2’-二甲基-1,1’-联薁(DBMA)在Au(111)表面上的热化学反应。在室温的Au(111)衬底上,我们发现沉积的分子在重构表面的fcc(面心立方堆积)区域形成无定型的聚集体,并在100℃以下保持形貌不变。当退火温度高于150℃后,DBMA发生脱溴反应并与金原子络合形成具有复杂空间立体结构的2,2’-二甲基-1,1’-联薁有机金属聚合物,并展现出迥异的图像特征。随后在更高温度下退火,有机金属聚合物脱去金属原子并经历碳碳偶联反应。该过程伴随着甲基与相邻薁单元之间的分子内环化反应,形成了含有benzo[a]azulene单元的梯形共轭聚合物。有趣的是,我们发现当一侧甲基参与反应并在聚合物中形成六元环时,会显著地弯折聚合物链,使得另一侧甲基与薁单元之间的距离增加,并抑制预期的环化过程。我们通过键分辨扫描探针显微镜对反应过程中的相关结构进行了研究,发现反应结果与反应中间结构的应力关联紧密。我们的结果表明,烷基取代的azulene前体可应用于非苯型碳纳米结构的表面合成,并有望实现扩展的非苯型二维碳纳米结构。

先进表征技术在锆合金显微组织研究中的应用进展

锆合金具有良好的核性能、力学性能和加工性能,是一种重要的结构材料,在核工业、航空航天和医疗设备等领域中应用前景广泛。深入了解锆合金显微组织对于掌握其性能和性质至关重要,其显微组织(如第二相、氧化膜、氢化物等)在加工和服役过程中的演变规律及对性能影响正得到材料科学、核工程领域研究者的广泛关注。先进表征技术,如电子显微分析技术、电子探针显微技术、原位表征技术及原子探针分析技术等已被应用于锆合金显微组织研究。电子显微分析技术,可对锆合金包壳的第二相、氢化物和氧化膜的显微组织特征进行表征,为锆合金包壳材料性能的优化改进提供支持。电子探针显微技术(EPMA)是高分辨率显微技术,可对锆合金的微观结构及表面特征进行分析。原位表征技术,包括透射电子显微镜原位辐照技术、原位电化学阻抗谱技术、原位拉伸实验和原位拉曼光谱。透射电子显微镜原位辐照技术,可用于研究锆合金在辐照条件下的行为及辐照引起的微观结构变化;原位电化学阻抗谱技术,可用于研究锆合金在腐蚀过程中的阻抗模量及氧化膜厚度的变化;原位拉伸实验,可实时观察锆合金的变形行为;原位拉曼光谱,可用于检测锆合金成分及结构的变化。原子探针分析技术,可对锆合金中元素偏聚现象、氧化过程、氢的分布及纳米尺度下原子分布情况的表征。综述了先进表征技术在锆合金微观组织研究中的应用进展及存在的问题,展望了锆合金显微组织的未来研究方向。本研究为深入了解锆合金的微观结构提供了参考,深化了对锆合金组织结构及性能的认识。

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.

原子探针层析技术及其在矿床研究中的应用

原子探针层析技术(APT)是一种能够以亚纳米分辨率提供定量的三维元素和同位素分析的测试分析技术,具有极高的空间分辨率和低的检出限。虽然原子探针主要用于材料科学和半导体领域,但随着近年来在矿床研究中应用的不断增加,正逐渐成为矿床研究的有用手段。与传统的地质分析技术相比,原子探针具有独特的技术优势,可以测量体积<0.0007μm3的矿物的元素组成,能够在纳米尺度上揭示矿物成分的复杂性,为理解地质演化过程提供全新的认识。本文在简述原子探针层析技术的基本原理、样品的选择和处理以及针尖样品制备的基础上,重点从成矿元素赋存状态、纳米尺度包裹体和稳定同位素组成三个方面阐述了原子探针在矿床研究中的代表性应用成果。迄今为止,原子探针在矿床学中的应用主要集中在成矿元素赋存状态的分析上,尤其是与金矿相关的黄铁矿或其他化学组成相对简单的矿物。而在纳米尺度包裹体和稳定同位素组成方面,原子探针应用成果虽不如前者丰富,但也取得了一些重要的全新认识,表现出良好的应用前景。原子探针在矿床学领域迅速发展的同时,也存在一些亟需解决的问题,如复杂质谱峰的标定、三维重建失真等。尽管如此,相信随着技术的不断进步,原子探针将逐渐成为矿床研究的重要工具。

15-5PH不锈钢在580℃时效过程中的析出强化行为

对15-5PH不锈钢进行了1040℃×1 h水冷的固溶处理,随后于580℃时效不同时间。利用维氏硬度计、光学显微镜和原子探针层析技术(atom probe tomography,APT)研究了不锈钢时效过程中析出相演变规律及其对硬度的影响。结果表明:时效初期,15-5PH不锈钢的硬度迅速上升并在时效5 min后达到峰值411.0 HV0.5,随后快速下降。时效5 min的钢中富Cu相的数量密度大,强化作用明显,硬度达到峰值。随着时效时间的延长,富Cu相逐渐粗化,强化作用减弱,硬度迅速下降。时效过程中Nb(C,N)颗粒与富Cu相分布在相邻位置,且随着时效时间的延长,铌碳氮化物不断析出长大,元素富集程度不断提高。

718Plus合金时效初期强化相的析出规律

采用显微硬度计、扫描电子显微镜(SEM)、原子探针层析(APT)技术研究了在标准热处理过程中及720℃时效初期(时效至128 h)718Plus合金的显微组织以及成分的演变规律。结果表明:718Plus合金的硬度在788℃炉冷至704℃后明显上升,在720℃时效至64 h时达到最大值459.3HV±8.5HV,硬度变化与γ′相的析出长大有关。随着热处理的进行,Ti、Al、Nb元素的分配系数逐渐增大,球形γ′相的直径、体积分数逐渐增大。γ′相的析出长大由Ti、Al、Nb元素在基体中的扩散控制,扩散程度采用元素的分配系数进行表示。在整个热处理过程中,Ti、Al、Nb元素在γ′相与基体之间的分配行为造成γ′相的直径、体积分数的变化。此外,在基体中分散着纳米级γ′团簇,其尺寸和数量密度在热处理过程中基本不变。