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A Cylindrical Lens Spectrometer with Parallel Detection for Reflection Electron Energy Loss Spectroscopy. 用于反射电子能量损失光谱学的平行探测圆柱透镜光谱仪。
IF 2.9 4区 工程技术 Q3 MATERIALS SCIENCE, MULTIDISCIPLINARY Pub Date : 2025-02-17 DOI: 10.1093/mam/ozae118
Junhyeok Hwang, In-Yong Park, Takashi Ogawa

Reflection electron energy loss spectroscopy (REELS) has played a pivotal role in allowing researchers to explore the characteristics of various bulk materials. This study presents results for the low-loss region of REELS with a new cylindrical lens spectrometer integrated into a low-voltage scanning electron microscope. The operational principles and implementation of the spectrometer are explained through comparisons between electron optical simulations and experimental results. Notably, the analysis shows the ability to distinguish samples in film and bulk forms. Graphene and graphite, despite their identical elemental composition and crystalline structure, are found to have distinct energy spectra as indicated by plasmon peaks. Furthermore, the study explores the bandgap measurement of SiO2 at low-energy conditions of 2.5 keV, highlighting the proposed instrument's advantages in the measurement without the harmful effect of Cherenkov loss. Additionally, this method reaffirms the capability to measure multiple plasmon peaks from the energy spectra of bulk gold samples, thus introducing a pioneering avenue in energy spectrum measurement. Leveraging the compact size and simple experimental setup of the spectrometer for REELS, the method enables the measurement of energy spectra of both bulk- and film-formed samples under low electron energy conditions, marking a significant advancement in the field.

反射电子能量损失光谱(REELS)在研究人员探索各种块状材料的特性方面发挥了举足轻重的作用。本研究介绍了利用集成在低压扫描电子显微镜中的新型圆柱透镜光谱仪进行 REELS 低损耗区域分析的结果。通过比较电子光学模拟和实验结果,解释了光谱仪的工作原理和实施方法。值得注意的是,该分析表明了区分薄膜和块状样品的能力。尽管石墨烯和石墨的元素组成和晶体结构完全相同,但通过等离子峰可以发现它们具有不同的能谱。此外,该研究还探讨了在 2.5 keV 的低能量条件下测量二氧化硅带隙的问题,凸显了拟议仪器在测量中无切伦科夫损耗有害影响的优势。此外,该方法再次证实了从块状金样品的能谱中测量多个等离子峰的能力,从而为能谱测量开辟了一条先河。利用 REELS 光谱仪的紧凑尺寸和简单实验设置,该方法能够在低电子能量条件下测量块状和薄膜状样品的能谱,标志着该领域的重大进展。
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引用次数: 0
Large-Angle Rocking Beam Electron Diffraction of Large Unit Cell Crystals Using Direct Electron Detector. 使用直接电子探测器对大单元晶胞进行大角度摇摆光束电子衍射
IF 2.9 4区 工程技术 Q3 MATERIALS SCIENCE, MULTIDISCIPLINARY Pub Date : 2025-02-17 DOI: 10.1093/mam/ozae088
Robert Busch, Hsu-Chih Ni, Yu-Tsun Shao, Jian-Min Zuo

We report a large-angle rocking beam electron diffraction (LARBED) technique for electron diffraction analysis. Diffraction patterns are recorded in a scanning transmission electron microscope (STEM) using a direct electron detector with large dynamical range and fast readout. We use a nanobeam for diffraction and perform the beam double rocking by synchronizing the detector with the STEM scan coils for the recording. Using this approach, large-angle convergent beam electron diffraction (LACBED) patterns of different reflections are obtained simultaneously. By using a nanobeam, instead of a focused beam, the LARBED technique can be applied to beam-sensitive crystals as well as crystals with large unit cells. This paper describes the implementation of LARBED and evaluates the performance using silicon and gadolinium gallium garnet crystals as test samples. We demonstrate that our method provides an effective and robust way for recording LARBED patterns and paves the way for quantitative electron diffraction of large unit cell and beam-sensitive crystals.

我们报告了一种用于电子衍射分析的大角度摇臂电子衍射(LARBED)技术。衍射图样是在扫描透射电子显微镜(STEM)中使用动态范围大、读取速度快的直接电子探测器记录的。我们使用纳米光束进行衍射,并通过使探测器与 STEM 扫描线圈同步进行记录来实现光束双摇。利用这种方法,可以同时获得不同反射的大角度会聚束电子衍射(LACBED)图样。通过使用纳米光束而不是聚焦光束,LARBED 技术可以应用于光束敏感晶体以及具有大单元晶胞的晶体。本文介绍了 LARBED 的实现方法,并使用硅和钆镓石榴石晶体作为测试样本对其性能进行了评估。我们证明了我们的方法为记录 LARBED 图案提供了一种有效而稳健的方法,并为大单胞和光束敏感晶体的定量电子衍射铺平了道路。
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引用次数: 0
Ameliorative Potential of Carvedilol Versus Platelet-Rich Plasma Against Paclitaxel-Induced Femoral Neuropathy in Wistar Rats: A Light and Electron Microscopic Study.
IF 2.9 4区 工程技术 Q3 MATERIALS SCIENCE, MULTIDISCIPLINARY Pub Date : 2025-02-17 DOI: 10.1093/mam/ozaf002
Ereny Fekry, George Nagi Refaat, Sara Adel Hosny

Paclitaxel, a chemotherapeutic drug, induces sensorimotor peripheral neuropathy. Carvedilol, a nonselective β-adrenoreceptor blocker, has been shown to exert antioxidant activity. Platelet-rich plasma (PRP) has supra-physiological levels of growth factors (GFs), enhances biosynthesis of antioxidant enzymes, and suppresses oxidative stress. This study compared the ameliorative effects of carvedilol and PRP on paclitaxel-induced femoral neuropathy. Eighty-eight adult male albino rats were equally randomized into four groups: group I served as the control; group II received paclitaxel (16 mg/kg intraperitoneally, weekly); group III received carvedilol (10 mg/kg daily, orally) concomitant with paclitaxel; and group IV received PRP (0.5 mL/kg subcutaneously, twice weekly) concomitant with paclitaxel. After 5 weeks, femoral nerve conduction velocity was measured, and blood samples were collected to assess catalase and superoxide dismutase levels. All animals were sacrificed, and gene expression of miR-21 was quantified. Tissue sections were stained with hematoxylin and eosin and toluidine blue. Then, the ultrathin sections were examined by transmission electron microscopy. Both carvedilol and PRP reversed paclitaxel-induced changes in the peripheral nerve, but PRP demonstrated a stronger antioxidant effect and a more pronounced presence of GFs, as evidenced by electron microscopy. PRP may represent a promising therapeutic approach for paclitaxel-induced neuropathy.

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引用次数: 0
Exploring Structural Anisotropy in Amorphous Tb-Co via Changes in Medium-Range Ordering. 通过中程有序变化探索非晶态铍钴合金的结构各向异性
IF 2.9 4区 工程技术 Q3 MATERIALS SCIENCE, MULTIDISCIPLINARY Pub Date : 2025-02-17 DOI: 10.1093/mam/ozae113
Ellis Kennedy, Emily Hollingworth, Alejandro Ceballos, Daisy O'Mahoney, Colin Ophus, Frances Hellman, Mary Scott

Amorphous thin films grown by magnetron co-sputtering exhibit changes in atomic structure with varying growth and annealing temperatures. Structural variations influence the bulk properties of the films. Scanning nanodiffraction performed in a transmission electron microscope (TEM) is applied to amorphous Tb17Co83 (a-Tb-Co) films deposited over a range of temperatures to measure relative changes in medium-range ordering (MRO). These measurements reveal an increase in MRO with higher growth temperatures and a decrease in MRO with higher annealing temperatures. The trend in MRO indicates a relationship between the growth conditions and local atomic ordering. By tilting select films, the TEM measures variations in the local atomic structure as a function of orientation within the films. The findings support claims that preferential ordering along the growth direction results from temperature-mediated adatom configurations during deposition, and that oriented MRO correlates with increased structural anisotropy, explaining the strong growth-induced perpendicular magnetic anisotropy found in rare earth-transition metal films. Beyond magnetic films, we propose the tilted FEM workflow as a method of extracting anisotropic structural information in a variety of amorphous materials with directionally dependent bulk properties, such as films with inherent bonding asymmetry grown by physical vapor deposition.

通过磁控共溅射技术生长的无定形薄膜会随着生长和退火温度的变化而发生原子结构的变化。结构变化会影响薄膜的体积特性。在透射电子显微镜(TEM)中对在一定温度范围内沉积的非晶 Tb17Co83(a-Tb-Co)薄膜进行扫描纳米衍射,以测量中程有序性(MRO)的相对变化。这些测量结果表明,生长温度越高,MRO 越高;退火温度越高,MRO 越低。MRO 的变化趋势表明了生长条件与局部原子有序之间的关系。通过倾斜选定的薄膜,TEM 可以测量薄膜内局部原子结构的变化,这种变化是薄膜内取向的函数。研究结果支持以下说法,即沿生长方向的优先有序是沉积过程中温度介导的原子构型的结果,而取向 MRO 与结构各向异性的增加相关,从而解释了稀土过渡金属薄膜中由生长引起的强烈垂直磁各向异性。除了磁性薄膜之外,我们还提出了倾斜有限元工作流程作为一种方法,用于提取具有方向依赖性块体特性的各种非晶材料中的各向异性结构信息,例如通过物理气相沉积生长的具有固有键合不对称性的薄膜。
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引用次数: 0
Quantitative Particle Analysis of Neptunium-237 Oxides: Optimization of MAMA Analysis for Modified Direct Denitration Products. 镎237氧化物的定量粒子分析:针对改良直接脱硝产品的 MAMA 分析优化。
IF 2.9 4区 工程技术 Q3 MATERIALS SCIENCE, MULTIDISCIPLINARY Pub Date : 2025-02-17 DOI: 10.1093/mam/ozae112
Connor J Parker, Kathryn M Peruski, Samantha K Cary

The production of plutonium-238 through irradiation of neptunium-237 (237Np) target materials for the use in radioisotope thermoelectric generators is paramount for continued deep space exploration. This work employs scanning electron microscopy to analyze 237Np materials coupled with a well-developed image analysis framework (Morphological Analysis for Material Attribution, or MAMA) to determine the degree of micron-scale homogeneity in the materials. This work demonstrated how the quantification of particle characteristics can validate production materials and affirm the qualitative similarities observed in micrographs. The 237Np oxide particle analysis determined that the materials from five production runs were quantitatively homogenous (significant at α = 0.05) in particle area, circularity, equivalent circular diameter, and ellipse aspect ratio, with two of the sampling dates having statistically significant different means for one of the four characteristics. These metrics not only confirm general homogeneity of the material but also expand the application of MAMA workflows to 237Np materials, demonstrating the utility of MAMA analysis for a wider breadth of nuclear materials than previously reported. In the open literature, this study is the first time that these microanalytical techniques were applied to 237Np materials to this degree.

通过辐照镎237(237Np)目标材料来生产钚238,并将其用于放射性同位素热电发电机,这对于继续进行深空探测至关重要。这项工作利用扫描电子显微镜分析 237Np 材料,并结合完善的图像分析框架(材料归属形态分析,或 MAMA)来确定材料的微米级均匀程度。这项工作展示了颗粒特征的量化如何验证生产材料并确认显微照片中观察到的定性相似性。237Np 氧化物颗粒分析表明,来自五次生产运行的材料在颗粒面积、圆度、等效圆直径和椭圆长宽比方面具有定量同质性(α = 0.05 时显著),其中两个取样日期的四个特征之一的平均值差异具有统计学意义。这些指标不仅证实了材料的总体均匀性,还将 MAMA 工作流程的应用扩展到了 237Np 材料,证明了 MAMA 分析在比以往报告更广泛的核材料中的实用性。在公开文献中,这项研究是首次将这些微分析技术应用于 237Np 材料。
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引用次数: 0
Karyotype, Male Meiosis, and Pollen Features of Barleria (Acanthaceae): A Wild Ornamental From India. Barleria(刺桐科)的核型、雄性减数分裂和花粉特征:印度的一种野生观赏植物
IF 2.9 4区 工程技术 Q3 MATERIALS SCIENCE, MULTIDISCIPLINARY Pub Date : 2025-02-17 DOI: 10.1093/mam/ozae117
Suraj S Patil, Manoj M Lekhak

Barleria is a palaeotropical genus of herbs, shrubs, and rarely climbers or trees. We investigated the karyotypes and male meiosis of 12 and 13 species, respectively, for the first time. Mitotic metaphases revealed two chromosome counts, 2n = 40 and 2n = 44. Chromosomes had median (m), submedian (sm), and subterminal (st) region centromeres. The total haploid chromosome length (TCL) ranged from 78.95 µm (Barleria sahyadrica) to 37.80 µm (B. nitida). Dispersion index differentiated the species into two groups, one with lower (3.40-4.79) and the other with higher (6.63-12.87) values. Principal component analysis based on six karyological parameters, namely base number (x), 2n, TCL, coefficient of variation of chromosome length, coefficient of variation of centromeric index, and mean centromeric asymmetry, exhibited three clusters. Cluster I included species of the subgenus Barleria. Cluster III had species of the subgenus Prionitis section Somalia. Cluster II comprised species of the subgenus Barleria and the subgenus Prionitis section Prionitis (B. sahyadrica). Pollen grains were oblate spheroidal or distinctly three-lobed, tri-brevicolporate with honey-combed tectum. Our analyses revealed karyological relationships among the investigated species and also provide raw data to breeders interested in horticultural applications of Barleria for accomplishing interspecific hybridization.

巴勒亚属(Barleria)是古热带的草本、灌木属,很少有攀缘植物或乔木。我们首次分别对 12 和 13 个物种的核型和雄性减数分裂进行了研究。有丝分裂分裂相显示了两种染色体数目,分别为 2n = 40 和 2n = 44。染色体有中位(m)、亚中位(sm)和亚端(st)区中心粒。单倍体染色体总长度(TCL)从 78.95 微米(Barleria sahyadrica)到 37.80 微米(B. nitida)不等。分散指数将物种分为两组,一组的分散指数值较低(3.40-4.79),另一组的分散指数值较高(6.63-12.87)。基于碱基数(x)、2n、TCL、染色体长度变异系数、中心粒指数变异系数和平均中心粒不对称性这六个核学参数的主成分分析显示出三个聚类。群组 I 包括 Barleria 亚属的物种。第 III 组包括索马里 Prionitis 亚属的物种。第 II 组包括 Barleria 亚属和 Prionitis 亚属 Prionitis 部分的物种(B. sahyadrica)。花粉粒呈扁球形或明显的三裂,三苞片多孔,具有蜂窝状的花粉块。我们的分析揭示了所研究物种之间的核果关系,同时也为有兴趣在园艺中应用巴乐藻实现种间杂交的育种者提供了原始数据。
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引用次数: 0
Direct Evidence of Anomalous Peierls Transition-Induced Charge Density Wave Order at Room Temperature in Metallic NaRu2O4. 金属NaRu2O4在室温下异常peerls跃迁诱导电荷密度波序的直接证据。
IF 2.9 4区 工程技术 Q3 MATERIALS SCIENCE, MULTIDISCIPLINARY Pub Date : 2025-02-17 DOI: 10.1093/mam/ozae129
Anna Scheid, Isha, Arvind Kumar Yogi, Masahiko Isobe, Birgit Bußmann, Tobias Heil, Peter A van Aken

In the field of quantum materials, understanding anomalous behavior under charge degrees of freedom through bond formation is of fundamental importance, with two key concepts: Dimerization and charge order at different cation sites. The coexistence of both dimerization and charge ordering is unusually found in NaRu2O4, even in its metallic state at room temperature. Our work unveils the origin of the interplay of these effects within metallic single-crystalline NaRu2O4. Employing advanced transmission electron microscopy techniques, we probe the lattice order of NaRu2O4 as a function of temperature and provide direct microscopic evidence of a Peierls-type transition. This transition is accompanied by a pronounced dimerization of the ruthenium chains, resulting in a distinctive twofold superstructure along the b axis below the critical transition temperature of ∼535 K, coinciding with a charge order. In situ heating experiments confirm the reversibility of this first-order phase transition, and periodic lattice displacement maps depict atomic-scale displacements linked to dimerization.

在量子材料领域,通过键的形成来理解电荷自由度下的异常行为是至关重要的,其中有两个关键概念:二聚化和不同阳离子位置的电荷顺序。在常温下的金属态NaRu2O4中,二聚化现象和电荷有序现象同时存在。我们的工作揭示了金属单晶NaRu2O4中这些效应相互作用的起源。利用先进的透射电子显微镜技术,我们探测了NaRu2O4的晶格顺序随温度的变化,并提供了peerls型转变的直接显微证据。这种转变伴随着明显的钌链二聚化,导致在临界转变温度~ 535 K以下沿b轴形成独特的双重上层结构,与电荷顺序一致。原位加热实验证实了这种一阶相变的可逆性,周期性晶格位移图描述了与二聚化有关的原子尺度位移。
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引用次数: 0
Preparation of Small Extracellular Vesicles Using Sequential Ultrafiltration with Regenerated Cellulose Membranes of Different Molecular Weight Cutoffs: A Study of Morphology and Size by Electron Microscopy. 用不同分子量截留物的再生纤维素膜序贯超滤制备细胞外小泡:形貌和大小的电镜研究。
IF 2.9 4区 工程技术 Q3 MATERIALS SCIENCE, MULTIDISCIPLINARY Pub Date : 2025-02-17 DOI: 10.1093/mam/ozae133
Noriyuki Ishii, Hiroaki Tateno

There is still room for improvement in the isolation and purification techniques for extracellular vesicles (EVs), particularly in the separation of exosomes (small EVs) from other membrane vesicles such as microvesicles and apoptotic bodies. Furthermore, it is crucial to establish preparation methods that preserve the intrinsic properties of EVs in this context. In this study, we focus on the isolation and preparation of small EVs, exosomes, from the culture supernatant of a human cell line. We discuss the sequential use of regenerated cellulose membranes with different molecular weight cutoffs, based on direct evaluation by transmission electron microscopy, and examine the challenges of characterizing biological membrane vesicles, small EVs, identified during this process.

细胞外囊泡(EVs)的分离和纯化技术,特别是外泌体(小EVs)与其他膜囊泡(如微囊泡和凋亡小体)的分离仍有改进的空间。此外,在这种情况下,建立保持电动汽车固有特性的制备方法至关重要。在本研究中,我们着重于从人细胞系培养上清中分离和制备小ev,外泌体。基于透射电子显微镜的直接评价,我们讨论了具有不同分子量截止点的再生纤维素膜的顺序使用,并研究了在此过程中鉴定的生物膜囊泡(小ev)的挑战。
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引用次数: 0
Digital Dark Field-Higher Contrast and Greater Specificity Dark Field Imaging Using a 4DSTEM Approach. 数字暗场--使用 4DSTEM 方法进行对比度更高、特异性更强的暗场成像。
IF 2.9 4区 工程技术 Q3 MATERIALS SCIENCE, MULTIDISCIPLINARY Pub Date : 2025-02-17 DOI: 10.1093/mam/ozae104
Ian MacLaren, Andrew T Fraser, Matthew R Lipsett, Colin Ophus

A new method for dark field imaging is introduced, which uses scanned electron diffraction (or 4DSTEM-4-dimensional scanning transmission electron microscopy) datasets as its input. Instead of working on simple summation of intensity, it works on a sparse representation of the diffraction patterns in terms of a list of their diffraction peaks. This is tested on a thin perovskite film containing structural ordering resulting in additional superlattice spots that reveal details of domain structures, and is shown to give much better selectivity and contrast than conventional virtual dark field imaging. It is also shown to work well in polycrystalline aggregates of CuO nanoparticles. In view of the higher contrast and selectivity, and the complete exclusion of diffuse scattering from the image formation, it is expected to be of significant benefit for characterization of a wide variety of crystalline materials.

本文介绍了一种新的暗场成像方法,它使用扫描电子衍射(或 4DSTEM-4 维扫描透射电子显微镜)数据集作为输入。该方法不是简单的强度求和,而是根据衍射峰列表稀疏地表示衍射图样。该方法在含有结构有序化的过氧化物薄膜上进行了测试,结果显示,该薄膜上的额外超晶格斑点能揭示畴结构的细节,其选择性和对比度远远优于传统的虚拟暗场成像。此外,该方法还能在氧化铜纳米粒子的多晶聚集体中很好地发挥作用。由于对比度和选择性更高,而且图像形成过程中完全排除了漫散射,因此预计该技术将对各种晶体材料的表征大有裨益。
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引用次数: 0
Improved Three-Dimensional Reconstructions in Electron Ptychography through Defocus Series Measurements. 通过离焦系列测量改进电子乳排造影中的三维重建
IF 2.9 4区 工程技术 Q3 MATERIALS SCIENCE, MULTIDISCIPLINARY Pub Date : 2025-02-17 DOI: 10.1093/mam/ozae110
Marcel Schloz, Thomas C Pekin, Hamish G Brown, Dana O Byrne, Bryan D Esser, Emmanuel Terzoudis-Lumsden, Takashi Taniguchi, Kenji Watanabe, Scott D Findlay, Benedikt Haas, Jim Ciston, Christoph T Koch

A detailed analysis of ptychography for three-dimensional (3D) phase reconstructions of thick specimens is performed. We introduce multi-focus ptychography, which incorporates a 4D-STEM defocus series to enhance the quality of 3D reconstructions along the beam direction through a higher overdetermination ratio. This method is compared with established multi-slice ptychography techniques, such as conventional ptychography, regularized ptychography, and multi-mode ptychography. Additionally, we contrast multi-focus ptychography with an alternative method that uses virtual optical sectioning through a reconstructed scattering matrix (S-matrix), which offers more precise 3D structure information compared to conventional ptychography. Our findings from multiple 3D reconstructions based on simulated and experimental data demonstrate that multi-focus ptychography surpasses other techniques, particularly in accurately reconstructing the surfaces and interface regions of thick specimens.

我们详细分析了厚标本三维(3D)相位重建的分层摄影技术。我们引入了多焦点平片成像技术,该技术结合了 4D-STEM 去焦系列,通过更高的过确定比来提高沿光束方向的三维重建质量。我们将这种方法与已有的多切片层析技术(如传统层析技术、正则化层析技术和多模式层析技术)进行了比较。此外,我们还将多焦点断层扫描与另一种通过重建散射矩阵(S-matrix)进行虚拟光学切片的方法进行了对比,后者能提供比传统断层扫描更精确的三维结构信息。我们基于模拟和实验数据进行的多次三维重建结果表明,多焦点分层摄影超越了其他技术,尤其是在精确重建厚试样的表面和界面区域方面。
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引用次数: 0
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Microscopy and Microanalysis
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