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Analysis of LePera's etching of the heat affected zone of a microalloyed steel. 微合金钢热影响区的LePera蚀刻分析。
IF 2.2 3区 工程技术 Q1 MICROSCOPY Pub Date : 2025-12-11 DOI: 10.1016/j.micron.2025.103982
Douglas G Ivey, Peter Schamuhn Kirk, Tailin Ren, Junfang Lu

LePera's etching combined with optical microscopy is an effective way to distinguish various microstructures that can form in microalloyed steels, especially within the heat affected zone (HAZ) of steels that have been welded. Ferritic and bainitic constituents tend to be tinted by the etchant and show up as various shades of tan, while martensite-austenite (M-A) regions are not tinted and exhibit a white color or bright contrast. This paper reveals that LePera's etchant also provides a similar contrast effect, as that for M-A, for any cementite particles in the microstructure. In addition, it is shown that heat tinting of the steel, which is a common imaging aid after fracture toughness testing (including the crack tip opening displacement (CTOD) method), can alter the steel microstructure. These effects can be important when trying to correlate microstructure with mechanical properties.

LePera蚀刻与光学显微镜相结合是一种有效的方法,可以区分微合金钢中可能形成的各种微观结构,特别是在焊接钢的热影响区(HAZ)内。铁素体和贝氏体成分往往被蚀蚀剂着色,呈现各种深浅的褐色,而马氏体-奥氏体(M-A)区域没有着色,呈现白色或明亮的对比。研究表明,LePera蚀刻剂对微观结构中的渗碳体颗粒也提供了类似于M-A的对比效果。此外,热着色是断裂韧性测试(包括裂纹尖端张开位移(CTOD)法)后常见的成像辅助手段,可以改变钢的显微组织。当试图将微观结构与机械性能联系起来时,这些效应可能很重要。
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引用次数: 0
Morphometric analysis of axonal ultrastructure: Coordinated scaling of organelles and myelin 轴突超微结构的形态计量学分析:细胞器和髓鞘的协调缩放。
IF 2.2 3区 工程技术 Q1 MICROSCOPY Pub Date : 2025-12-08 DOI: 10.1016/j.micron.2025.103981
Vitalijs Borisovs , Mario Bossi , Guido Cavaletti
The endoplasmic reticulum (ER) is a crucial neuronal organelle involved in protein synthesis, calcium homeostasis, and metabolic support, essential for neuronal function and plasticity. Understanding its three-dimensional (3D) architecture is key to elucidating functional organization. Using SBF-SEM and AI-assisted segmentation, we established a quantitative framework to characterize ER and mitochondrial scaling within 35 peripheral nervous system (PNS) myelinated axons. Analysis of individual organelle morphometrics revealed a strong power-law relationship between surface area and volume for both mitochondria (R2 = 0.949) and ER (R2 = 0.949). The resulting exponents were super-isometric (kMito = 0.85, kER = 0.73), suggesting structural plasticity that prioritizes membrane surface expansion. A key finding was the distinction between size and number regulation: mitochondrial and ER volumes were negligibly correlated (r ≈ 0.03), implying independent size regulation. However, organelle abundance (counts) showed a strong positive correlation (r = 0.79), maintaining an extremely low Bonferroni-adjusted Q value (8.1 ×10−9), suggesting coordinated control of organelle number in response to axonal size. Axonal populations were heterogeneous, with larger axons consistently containing more ER elements (r = 0.59) and mitochondria (r = 0.69). Furthermore, a low correlation of axon length with organelle content supports the idea that regulation is primarily a local phenomenon tied to cross-sectional size. These findings provide a quantitative basis for understanding how ER and mitochondria structurally adapt to axonal size, laying the groundwork for future research into how these scaling relationships influence neuronal metabolic health and contribute to neurological disease.
内质网是一个重要的神经元细胞器,参与蛋白质合成、钙稳态和代谢支持,对神经元的功能和可塑性至关重要。了解其三维(3D)架构是阐明功能组织的关键。使用SBF-SEM和ai辅助分割,我们建立了定量框架来表征35个外周神经系统(PNS)髓鞘轴突内的ER和线粒体缩放。单个细胞器形态计量学分析显示,线粒体和ER的表面积与体积呈幂律关系(R2 = 0.949)。得到的指数是超等距的(kMito = 0.85, kER = 0.73),表明结构可塑性优先于膜表面的膨胀。一个关键的发现是大小和数量调节之间的区别:线粒体和内质网体积是可忽略的相关(r ≈ 0.03),这意味着独立的大小调节。然而,细胞器丰度(计数)呈强正相关(r = 0.79),保持极低的bonferroni调整Q值(8.1 ×10-9),提示细胞器数量响应轴突大小而协调控制。轴突种群具有异质性,较大的轴突始终含有较多的ER元素(r = 0.59)和线粒体(r = 0.69)。此外,轴突长度与细胞器含量的低相关性支持了调节主要是与横截面大小相关的局部现象的观点。这些发现为理解内质网和线粒体如何在结构上适应轴突大小提供了定量基础,为未来研究这些缩放关系如何影响神经元代谢健康和促进神经系统疾病奠定了基础。
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引用次数: 0
Development and validation of an interface for automated image acquisition during high-temperature environmental scanning electron microscopy experiments 高温环境扫描电子显微镜实验中自动图像采集接口的开发和验证。
IF 2.2 3区 工程技术 Q1 MICROSCOPY Pub Date : 2025-12-05 DOI: 10.1016/j.micron.2025.103980
J. Lautru, R. Podor
An interface that enables automatic image acquisition during high-temperature experiments in an environmental SEM is developed. It is optimized to work on multiple regions of interest at multiple magnifications, performing image focusing (focus and astigmatism) and automatic re-centering of regions of interest. Its operation has been validated by monitoring two regions of interest of a nickel-based superalloy undergoing oxidation at 950 °C at different magnifications. Recording series of images at different magnifications on different regions of interest makes it possible to qualify the behavior of different areas of the sample in a single operation and/or to validate the reproducibility of the observations.
开发了一种在环境扫描电镜中进行高温实验时自动图像采集的接口。它被优化为在多个放大倍数下对多个感兴趣的区域工作,执行图像聚焦(聚焦和散光)和自动重新定心感兴趣的区域。通过监测在950°C下以不同倍率氧化的镍基高温合金的两个感兴趣区域,验证了其操作。以不同倍率记录不同感兴趣区域的一系列图像,可以在一次操作中确定样品不同区域的行为和/或验证观察结果的可重复性。
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引用次数: 0
A combined hardware and software method for the projection center calibration of the diffraction pattern 一种结合硬件和软件的衍射图样投影中心标定方法。
IF 2.2 3区 工程技术 Q1 MICROSCOPY Pub Date : 2025-12-04 DOI: 10.1016/j.micron.2025.103977
Liting Zhang , Qiwei Shi , Dominique Loisnard , Maxime Mollens , Haowei Wang , Stéphane Roux
The precise knowledge of the projection center (PC) coordinates is vital for diffraction techniques, especially for electron backscatter diffraction (EBSD) and transmission Kikuchi diffraction (TKD). Numerous techniques have been proposed for PC calibration, involving both hardware maneuver and algorithm developments. Hardware calibration is straightforward 1, while software calibration generally displays small uncertainties yet possible biases. A novel method is proposed herein for PC calibration, associating a moving screen 1 image correlation, thus combining the strengths of both techniques. Multiple sets of diffraction patterns of the same sample area are acquired at different positions of the detector along its track. Exploiting the geometrical relationship between them through a dedicated integrated digital image correlation framework (IDIC-M) that also associates a simulated master pattern, the PC coordinates are obtained. A unique crystal orientation and varying PC values are sought relating the different diffraction patterns to fully benefit from their consistency. This hybrid method improves the precision of PC calibration by 74.0% and 21.8% as compared to pure (hardware) moving-screen method and (software) image correlation method, respectively. Besides, the present work further validates the gradient-based version of pattern correlation, free of perceivable systematic errors, and hence deemed efficient and reliable in EBSD practices.
准确的投影中心坐标对于衍射技术,特别是电子背散射衍射(EBSD)和透射菊池衍射(TKD)至关重要。已经提出了许多用于PC校准的技术,包括硬件操作和算法开发。硬件校准很简单,而软件校准通常显示出很小的不确定性,但可能存在偏差。本文提出了一种新的PC校准方法,将移动屏幕与图像相关相关联,从而结合了两种技术的优点。在探测器沿轨迹的不同位置获得了同一样品区域的多组衍射图。利用它们之间的几何关系,通过一个专用的集成数字图像相关框架(dic - m),也关联一个模拟的主模式,得到PC坐标。在不同的衍射模式中寻求独特的晶体取向和不同的PC值,以充分受益于它们的一致性。与纯(硬件)动屏法和(软件)图像相关法相比,该混合方法的PC标定精度分别提高了74.0%和21.8%。此外,本工作进一步验证了基于梯度的模式相关版本,没有可感知的系统误差,因此在EBSD实践中被认为是有效和可靠的。
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引用次数: 0
Molecular dynamic simulation of multi-frequency electrostatic force microscopy 多频静电力显微镜的分子动力学模拟
IF 2.2 3区 工程技术 Q1 MICROSCOPY Pub Date : 2025-12-04 DOI: 10.1016/j.micron.2025.103979
Quan Yuan, Jianqiang Qian, Yingzi Li, Minghao Wang, Rui Lin, Yifan Hu, Duo Feng, Peng Cheng, Yanan Chen, Haowei Sun
Multifrequency electrostatic force microscopy (MF-EFM) is a critical tool for the electrical characterization of nanomaterial surfaces, and the quality is closely related to parameters. Molecular simulations have successfully explained the motion process in bimodal AFM. However, additional considerations are required for implementing electrostatic interactions in molecular simulations for MF-EFM. We use COMSOL to model the tip-sample system in MF-EFM, derive the fitting formula for the electrostatic forces between tip and sample, and applied it in LAMMPS. The tip response amplitude variations obtained by simulations are analyzed, and the effect of different parameters on the amplitudes of the two modes is examined. This approach successfully explained the scan process of MF-EFM, and the results are validated by experiments. We provide a reliable method for simulating atomic-scale vibration responses during MF-EFM scan.
多频静电力显微镜(MF-EFM)是纳米材料表面电学表征的重要工具,其质量与参数密切相关。分子模拟已经成功地解释了双峰AFM的运动过程。然而,在MF-EFM的分子模拟中实现静电相互作用需要额外的考虑。利用COMSOL软件对MF-EFM中针尖-样品系统进行建模,推导出针尖-样品间静电力的拟合公式,并将其应用于LAMMPS中。分析了仿真得到的叶尖响应幅值变化规律,并考察了不同参数对两种模态幅值的影响。该方法成功地解释了微波efm的扫描过程,并通过实验验证了结果。我们提供了一种可靠的模拟原子尺度振动响应的方法。
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引用次数: 0
A study of in-the-column detector micrograph contrast in low-voltage scanning electron microscopy 低压扫描电镜中柱内检测器显微图像对比的研究。
IF 2.2 3区 工程技术 Q1 MICROSCOPY Pub Date : 2025-11-30 DOI: 10.1016/j.micron.2025.103978
Asia Matatyaho Ya'akobi, Irina Davidovich, Yeshayahu Talmon
Scanning electron microscopy (SEM) is a widely used technique in science and engineering, traditionally performed at electron beam acceleration voltages (BAVs) above 5 kV. However, progress in field emission guns and SEM technology have made low-voltage SEM imaging more available. Low-voltage SEM offers significant advantages, such as high-resolution imaging and the imaging of non-coated insulating specimens without charging artifacts. Nevertheless, there is limited research on electron-specimen interactions and the influence of SEM operational parameters on the obtained micrograph at the low-voltage range. This study focuses on low-voltage SEM imaging, below 2 kV, using a high-resolution in-the-lens detector. We investigated the effects of BAV and working distance (WD) on micrograph contrast and resolution. Carbon nanotubes and boron nitride nanotubes, two very important advanced materials, were used as model specimens of conductive and non-conductive materials, respectively, and silicon wafers and glass slides were used as model conductive and non-conductive substrates. We found that optimal imaging conditions differ with specimen properties; optimal results were typically obtained at low BAV (0.8–1.2 kV) and short WD (below 3 mm). Additionally, we show that substrate conductivity affects micrograph quality. Counterintuitively, insulating substrates provide better results in some cases. These findings emphasize the importance of optimizing SEM imaging parameters, and choosing the substrate according to sample properties for optimal imaging at low-voltage conditions.
扫描电子显微镜(SEM)是一种广泛应用于科学和工程的技术,传统上是在5 kV以上的电子束加速电压(BAVs)下进行的。然而,场发射枪和扫描电镜技术的进步使得低压扫描电镜成像变得更加可行。低压扫描电镜具有显著的优势,如高分辨率成像和无电荷伪影的无涂层绝缘样品的成像。然而,在低电压范围内,电子与样品的相互作用以及SEM操作参数对所获得的显微图的影响的研究有限。这项研究的重点是低压扫描电镜成像,低于2 千伏,使用高分辨率镜头内探测器。我们研究了BAV和工作距离(WD)对显微照片对比度和分辨率的影响。以碳纳米管和氮化硼纳米管这两种非常重要的先进材料分别作为导电和非导电材料的模型试样,以硅片和玻片作为导电和非导电基片的模型试样。我们发现最佳成像条件随样品性质不同而不同;在低BAV(0.8-1.2 kV)和短WD(小于3 mm)条件下获得最佳效果。此外,我们表明衬底电导率影响显微照片的质量。与直觉相反,绝缘基板在某些情况下提供更好的结果。这些发现强调了优化SEM成像参数的重要性,以及根据样品性质选择衬底以实现低压条件下的最佳成像。
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引用次数: 0
Effect of interlayer deposition strategy on thermal characteristics and multiphase synergistic strengthening of HEAs prepared by LPBF 层间沉积策略对LPBF制备HEAs热特性及多相协同强化的影响
IF 2.2 3区 工程技术 Q1 MICROSCOPY Pub Date : 2025-11-30 DOI: 10.1016/j.micron.2025.103975
Yaqiong Ge, Yan Yin, Yue Song, Lina Wang, Qingling Hou, Zexin Chang, Wen Yang
Laser powder bed fusion (LPBF) technology provides a new approach for microstructure control of high entropy alloys (HEAs) through layer-by-layer stacking and rapid solidification characteristics. This study focuses on the Al0.5CoCrFeNi HEAs and systematically investigates the effects of different interlayer rotation angles (0°, 67°, 90°) on the porosity, grain orientation, phase distribution, and mechanical properties of LPBF formed HEAs. The results showed that the interlayer rotation angle significantly controlled the grain morphology and grain boundary characteristics by changing the thermal accumulation and gradient direction of the melt pool. At a rotation angle of 67°, the melt pool size increased, the porosity decreased to 2.05 %, and the proportion of high angle grain boundaries (HAGB) increased to 31.34 %. Combining EBSD and TEM analysis, it was found that at the rotation angle of 67°, the BCC phase content increased to 8.36 %, the preferred grain orientation weakened, the degree of recrystallization increased to 7.69 %, and the dislocation network density decreased to 1.18 × 1014m−2. These promoted the tensile strength to 733.53 MPa, an increase of 36.9 % compared to the 0° sample and 6.4 % compared to the 90° sample. This study reveals the coupling mechanism of interlayer rotation angle on the ‘thermal-mechanical-microstructure’ of LPBF formed HEAs, providing theoretical support for the optimization of additive manufacturing processes for high-performance complex structural alloys.
激光粉末床熔合技术通过对高熵合金的逐层堆焊和快速凝固特性,为高熵合金的微观组织控制提供了新的途径。本研究以Al0.5CoCrFeNi HEAs为研究对象,系统研究了不同层间旋转角度(0°、67°、90°)对LPBF形成HEAs孔隙度、晶粒取向、相分布和力学性能的影响。结果表明,层间旋转角度通过改变熔池的热积累和梯度方向,对晶粒形貌和晶界特征有明显的控制作用。当旋转角度为67°时,熔池尺寸增大,孔隙率减小至2.05 %,高角晶界(HAGB)比例增大至31.34 %。结合EBSD和TEM分析发现,当旋转角度为67°时,BCC相含量增加到8.36 %,晶粒择优取向减弱,再结晶程度增加到7.69 %,位错网络密度降低到1.18 × 1014m−2。拉伸强度达到733.53 MPa,比0°试样提高36.9 %,比90°试样提高6.4 %。本研究揭示了层间旋转角度对LPBF成形HEAs“热-力学-微观结构”的耦合机理,为高性能复杂结构合金增材制造工艺的优化提供了理论支持。
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引用次数: 0
In-depth analysis of grain structure of heavily-deformed multilayered composites by electron backscattered diffraction 电子背散射衍射对大变形多层复合材料晶粒结构的深入分析。
IF 2.2 3区 工程技术 Q1 MICROSCOPY Pub Date : 2025-11-30 DOI: 10.1016/j.micron.2025.103976
Luo Sung Hong , Fu-ming Xiaoyu
The variation of texture, grain size, grain boundaries, and hardness of the composite layers has been examined at different deformation passes and regions of the Cu (matrix)–Mg (reinforcement) composite and the Mg (matrix)–Cu (reinforcement) composite. The multilayered composites were processed by the accumulative roll bonding (ARB) method. With the rise of ARB passes, the layers became wavy, then necked, and were finally broken into smaller layers. Rolling texture and shear texture were the predominant textures in the rolled composites. The rolling texture grew with increasing ARB pass. Also, the intensity of the shear texture increased in regions closer to the surfaces. Furthermore, a grain size decrement was observed in all layers, even though the Cu layer in the Cu/Mg/Cu and the Mg layer in the Mg/Cu/Mg showed finer grains than when these layers were used as inner layers. Additionally, the grain sizes gradually increased from near-surface regions to near-center regions. Based on kernel average misorientation (KAM) images, more evident strain was accumulated near boundaries in regions closer to the surfaces. Furthermore, the hardness measurements showed a reduction from the composite’s surface to the composite’s center, although all matrix and reinforcing layers showed an increase in hardness with increasing ARB pass.
研究了Cu(基体)-Mg(增强)复合材料和Mg(基体)-Cu(增强)复合材料在不同变形道和变形区域的织构、晶粒尺寸、晶界和硬度的变化。采用累积辊焊(ARB)方法制备了多层复合材料。随着ARB通道的增加,这些层变得波浪状,然后呈颈状,最后被分解成更小的层。轧制复合材料的主要织构是轧制织构和剪切织构。随着ARB道次的增加,轧制织构逐渐增大。此外,在靠近表面的区域,剪切织构的强度增加。此外,尽管Cu/Mg/Cu中的Cu层和Mg/Cu/Mg中的Mg层的晶粒比用作内层时细,但所有层的晶粒尺寸都有所减小。晶粒尺寸从近地表向近中心逐渐增大。基于核平均错误取向(KAM)图像,在靠近表面的区域,边界附近积累了更明显的应变。此外,硬度测量显示,从复合材料的表面到复合材料的中心都有降低,尽管所有的基体和增强层的硬度都随着ARB次数的增加而增加。
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引用次数: 0
Feasibility and strategies for direct atomic force microscopy on standard transmission electron microscopy specimens 直接原子力显微镜在标准透射电镜样品上的可行性和策略。
IF 2.2 3区 工程技术 Q1 MICROSCOPY Pub Date : 2025-11-28 DOI: 10.1016/j.micron.2025.103965
Michéle Brugger-Hatzl , Verena Reisecker , Anas Alatrash , Martina Dienstleder , Evelin Fisslthaler , Daniel Knez , Gerald Kothleitner
Correlative microscopy has gained increasing importance across a range of research disciplines. Combining different microscopy techniques broadens knowledge about a sample by providing more comprehensive insights. In particular, the correlation of atomic force microscopy (AFM) and transmission electron microscopy (TEM) offers a powerful complementary approach for investigating materials, as both surface and subsurface information can be obtained. The fundamental motivation of this study is to establish a direct correlation between measurements obtained from the same specimen region by both methods. Such correlation is not always straightforward, as each technique requires different sample preparation. Consequently, performing AFM measurements on TEM samples inevitably gives rise to several challenges, including, but not limited to, surface distortion and limited accessibility. In this study, we propose a range of AFM measurement strategies tailored to two typical TEM sample types: a 3 nm thin membrane on lacey carbon and a TEM lamella mounted on a lift-out grid. We compare the influence of different cantilever dimensions and AFM modes on image quality, and explore the fabrication of AFM tips positioned at the very front of a cantilever via focused electron beam induced deposition to improve accessibility of regions of interest. With the strategies developed here, we successfully demonstrate the feasibility of AFM measurements on TEM samples without the need for additional sample preparation, enabling direct correlation. The results highlight the practical viability of this combined approach, and expand the scope of correlative microscopy for advanced materials characterization.
相关显微镜在一系列研究学科中越来越重要。结合不同的显微镜技术,通过提供更全面的见解,拓宽了对样品的了解。特别是,原子力显微镜(AFM)和透射电子显微镜(TEM)的相关性为研究材料提供了一种强大的互补方法,因为可以获得表面和次表面信息。本研究的基本动机是通过两种方法在同一标本区域获得的测量结果之间建立直接相关性。这种相关性并不总是直截了当的,因为每种技术需要不同的样品制备。因此,对TEM样品进行AFM测量不可避免地会产生一些挑战,包括但不限于表面畸变和有限的可及性。在这项研究中,我们提出了一系列针对两种典型TEM样品类型的AFM测量策略:在蕾丝碳上的3 nm薄膜和安装在提升网格上的TEM片层。我们比较了不同悬臂尺寸和AFM模式对图像质量的影响,并探索了通过聚焦电子束诱导沉积在悬臂最前面的AFM尖端的制造,以提高感兴趣区域的可达性。利用本文开发的策略,我们成功地证明了在TEM样品上进行AFM测量的可行性,而无需额外的样品制备,从而实现了直接相关。结果突出了这种组合方法的实际可行性,并扩大了相关显微镜用于高级材料表征的范围。
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引用次数: 0
Loss of coherence in a magnetic electron lens due to spin rotation 自旋引起的磁性电子透镜中相干性的丧失
IF 2.2 3区 工程技术 Q1 MICROSCOPY Pub Date : 2025-11-22 DOI: 10.1016/j.micron.2025.103964
Hiroshi Okamoto
Rotation of the electron spin in an inhomogeneous magnetic field in the magnetic electron lens causes a partial loss of coherence. Such incoherence entails non-ideal focusing properties of an electron lens. Although this effect should be small in the current electron-optical systems, we show that the effect could be a non-negligible factor in an aberration-corrected system with an electron probe with a large half angle in the future. A semiclassical framework for evaluating the effect is described. We emphasize that the incoherence effect manifests itself for the spin unpolarized electron beam as well.
在磁电子透镜的非均匀磁场中,电子自旋的旋转导致部分相干性的损失。这种不相干导致了电子透镜的非理想聚焦特性。虽然这种影响在当前的电子光学系统中应该很小,但我们表明,在未来具有大半角电子探针的像差校正系统中,这种影响可能是一个不可忽略的因素。描述了一个半经典的评价框架。我们强调非相干效应在自旋非极化电子束中也表现出来。
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引用次数: 0
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Micron
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