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High energy-resolution soft X-ray emission spectrometer using a back-thinned CMOS detector for chemical bonding state analysis. 高能量分辨率软x射线发射光谱仪,采用后薄型CMOS探测器,用于化学键态分析。
IF 1.9 Pub Date : 2025-12-01 DOI: 10.1093/jmicro/dfaf021
Shogo Koshiya, Takanori Murano, Masami Terauchi

Improvement of a commercially available soft X-ray emission spectrometer was tested by introducing a fine-pixel-sized CMOS detector. The peak width of Mg Kα-emission was reduced to one-fourth of that obtained by the CCD detector presently used. Furthermore, the differences in the energy positions of satellite lines of Mg Kα- and also Kβ-emission profiles of Mg and MgO were observed. O K-emission profile of MgO exhibited a few structures reflecting the chemical bonding state. This spectrometer easily discriminated the intensity profiles of Fe Lα,β-emission reflecting the chemical bonding states of Fe atoms in Fe, FeO, Fe3O4 and Fe2O3.

通过引入细像素级CMOS探测器,测试了商用软x射线发射光谱仪的改进。Mg - k - α-发射峰宽减小到现有CCD探测器的1/4。此外,还观察到Mg和MgO的Kα-和k β-发射谱线能量位置的差异。MgO的O - k发射谱显示出一些反映化学键态的结构。该光谱仪可以很容易地分辨出Fe、FeO、Fe3O4和Fe2O3中Fe原子的化学键态的Lα、β-发射强度谱。
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引用次数: 0
Local Strain Effects on Bandgap Energy in Flexible h-WO3 Nanowires. 局部应变对柔性h-WO3纳米线带隙能的影响。
IF 1.9 Pub Date : 2025-10-31 DOI: 10.1093/jmicro/dfaf050
Sho Nekita, Naomu Sekiguchi, Yuya Kasamura, Itsuki Misono, Yusuke Shimada, Satoshi Iikubo, Tetsuya Okuyama, Satoshi Hata

According to theoretical predictions, local strain in the bent regions of flexible nanowires can alter their electronic structure. However, the experimental validation of such strain-induced effects remains elusive. In this study, we established a clear correlation between local structural deformation and electronic properties in bent hexagonal-WO3 nanowires using four-dimensional scanning transmission electron microscopy and electron energy loss spectroscopy. Although a simple geometric bending model predicts an expansion of the (0001) lattice spacing on the outer side of the bend, our direct observations revealed a larger expansion than predicted. This lattice expansion was accompanied by a significant reduction in bandgap energy. We employed density functional theory calculations and crystal orbital Hamilton population analyses to provide a theoretical framework for these findings. These results provide direct experimental evidence of strain-induced modulation of the electronic structure in metal oxide nanowires.

根据理论预测,柔性纳米线弯曲区域的局部应变可以改变其电子结构。然而,这种菌株诱导效应的实验验证仍然难以捉摸。在这项研究中,我们利用四维扫描透射电子显微镜和电子能量损失谱建立了弯曲六边形wo3纳米线的局部结构变形与电子性能之间的明确相关性。尽管一个简单的几何弯曲模型预测了弯曲外侧(0001)晶格间距的膨胀,但我们的直接观察显示了比预测更大的膨胀。这种晶格膨胀伴随着带隙能量的显著降低。我们采用密度泛函理论计算和晶体轨道汉密尔顿居群分析为这些发现提供了理论框架。这些结果为金属氧化物纳米线中电子结构的应变诱导调制提供了直接的实验证据。
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引用次数: 0
Cathodoluminescence, light injection and EELS in STEM: From comparative to coincidence experiments. STEM中的阴极发光、光注入与EELS:从比较实验到重合实验。
IF 1.9 Pub Date : 2025-10-27 DOI: 10.1093/jmicro/dfaf047
Luiz H G Tizei, Yves M Auad, Florian Castioni, Mathieu Kociak

Electron spectroscopy implemented in electron microscopes provides high spatial resolution, down to the atomic scale, of the chemical, electronic, vibrational and optical properties of materials. In this review, we will describe how temporal coincidence experiments in the nanosecond to femtosecond range between different electron spectroscopies involving photons, inelastic electrons and secondary electrons can provide information bits not accessible to independent spectroscopies. In particular, we will focus on nano-optics applications. The instrumental modifications necessary for these experiments are discussed, as well as the perspectives for these coincidence techniques.

在电子显微镜中实现的电子能谱提供了高空间分辨率,低到原子尺度,材料的化学,电子,振动和光学性质。在这篇综述中,我们将描述在纳秒到飞秒范围内,涉及光子、非弹性电子和二次电子的不同电子能谱之间的时间重合实验如何提供独立能谱无法获得的信息位。我们将特别关注纳米光学的应用。讨论了这些实验所需的仪器修改,以及这些符合技术的前景。
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引用次数: 0
Domain-Specific Simulated Data Enhances Knife-Mark Noise Suppression in Microscopy Images of Materials. 特定领域的模拟数据增强了材料显微图像中的刀痕噪声抑制。
IF 1.9 Pub Date : 2025-10-24 DOI: 10.1093/jmicro/dfaf049
Masato Suzuki, Yasuhiko Igarashi

Knife-mark noise often arises in microscopy of materials. Leveraging their simple textures relative to natural images, we simulate knife-marked micrographs and train a deep network without labeled real data. The resulting model surpasses conventional methods, removing artifacts while preserving structure, demonstrating simulation-driven learning as a practical materials-science solution in research. Accurate quantitative analysis of material microstructures from images is often hindered by noise and artifacts generated during sample preparation. While deep learning is a promising approach for this challenge, preparing the large amount of "supervised data" (labeled real images) required for training poses a significant barrier in material science. This study proposes and validates a simulation-driven learning paradigm where a deep learning model is trained exclusively on simulated images that mimic the key features of target structures and noise, serving as a powerful solution to this data scarcity problem. As a specific case study, we applied this paradigm to the removal of "knife-mark noise" from cross-sectional images of rubber materials to enable accurate filler region segmentation. In evaluations using simulated data, the proposed method showed superior performance across all the metrics (PSNR, SSIM, and MAE) compared with conventional methods such as the median filter and TV reconstruction, as well as a U-Net model trained on general-purpose Gaussian noise. More importantly, the model also performed effectively on real images, despite being trained solely on simulated data. It successfully removed both knife-marks and material-derived background textures, which demonstrates the viability of simulation-driven learning to overcome the need for manually annotated datasets. This work highlights the power of task-specific simulations as a practical alternative to manual data annotation in quantitative materials analysis.

在显微镜下观察材料时,经常会出现刀痕噪声。利用它们相对于自然图像的简单纹理,我们模拟了刀标记的显微照片,并在没有标记真实数据的情况下训练了一个深度网络。由此产生的模型超越了传统方法,在保留结构的同时去除了人工制品,展示了模拟驱动的学习作为研究中实用的材料科学解决方案。从图像中对材料微观结构进行精确的定量分析常常受到样品制备过程中产生的噪声和伪影的阻碍。虽然深度学习是应对这一挑战的一种很有前途的方法,但准备训练所需的大量“监督数据”(标记的真实图像)对材料科学构成了重大障碍。本研究提出并验证了一种模拟驱动的学习范式,其中深度学习模型专门针对模拟目标结构和噪声的关键特征的模拟图像进行训练,作为该数据稀缺问题的有力解决方案。作为一个具体的案例研究,我们将这种范式应用于从橡胶材料的横截面图像中去除“刀痕噪声”,以实现准确的填充区域分割。在使用模拟数据的评估中,与传统方法(如中值滤波和电视重构)以及基于通用高斯噪声训练的U-Net模型相比,所提出的方法在所有指标(PSNR、SSIM和MAE)上都表现出优越的性能。更重要的是,尽管只在模拟数据上训练,该模型在真实图像上的表现也很有效。它成功地去除了刀痕和材料衍生的背景纹理,这证明了模拟驱动学习的可行性,以克服对手动注释数据集的需求。这项工作突出了任务特定模拟的力量,作为定量材料分析中手动数据注释的实际替代方案。
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引用次数: 0
Relaxation Time Measurement: Correlating Diffraction Patterns. 弛豫时间测量:相关衍射图样。
IF 1.9 Pub Date : 2025-10-21 DOI: 10.1093/jmicro/dfaf048
Katsuaki Nakazawa, Kazutaka Mitsuishi

Dynamics in liquids and glasses can be assessed using X-ray photon correlation spectroscopy or electron correlation microscopy, which involves measuring the temporal changes in diffraction patterns. Two methods are commonly used to evaluate these temporal changes: one-time correlation function or two-time correlation function. However, the specific characteristics of these methods have not been thoroughly studied. In this study, we investigated the differences between these methods and found that the two-time correlation function can measure dynamics for longer periods than the method relying on the one-time correlation function. Additionally, we demonstrated that the two-time correlation function exhibits a weak dependence on the amount of dose applied.

液体和玻璃中的动力学可以用x射线光子相关光谱或电子相关显微镜来评估,这涉及到测量衍射图样的时间变化。通常用两种方法来评价这些时间变化:一次相关函数或两次相关函数。然而,这些方法的具体特点还没有得到深入的研究。在本研究中,我们研究了这些方法之间的差异,发现两次相关函数比依赖一次相关函数的方法可以测量更长时间的动态。此外,我们还证明了两次相关函数对剂量的依赖性较弱。
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引用次数: 0
Development of atomic force microscopy for investigations on molten metal/solid interfaces. 原子力显微镜研究熔融金属/固体界面的进展。
IF 1.9 Pub Date : 2025-10-17 DOI: 10.1093/jmicro/dfaf043
Takashi Ichii

Atomic force microscopy (AFM) has developed remarkably in recent years, and its measurement environment has been extended not only to ultrahigh vacuum and air, but also to liquids. Since the solid-liquid interface is the site of various reactions, such as crystal growth and catalytic reactions, its atomic-scale analysis is crucially important. Although AFM analyses in various liquids, such as aqueous solutions, organic solvents, and ionic liquids, have been reported, there have been no studies of AFM analysis in molten metals. One of the reasons for this is the opacity of molten metals. Achieving AFM analysis in molten metal is expected to provide new insights into metallurgy. In this review, AFM that can analyze in molten metal is presented. The key innovation is the utilization of an AFM sensor employing a quartz tuning fork, the so-called qPlus sensor, instead of a silicon cantilever. In addition to the technical fundamentals of AFM in molten metal, we present two applications: in-situ and atomic-resolution analysis of alloy crystal growth processes and measurements of two-body interaction forces.

原子力显微镜(AFM)近年来发展迅速,其测量环境已从超高真空和空气扩展到液体。由于固液界面是各种反应的场所,如晶体生长和催化反应,其原子尺度的分析是至关重要的。虽然AFM分析在各种液体,如水溶液,有机溶剂和离子液体,已经有报道,还没有研究AFM分析在熔融金属。其中一个原因是熔融金属的不透明性。在熔融金属中实现AFM分析有望为冶金学提供新的见解。本文介绍了原子力显微镜在分析熔融金属中的应用。关键的创新是AFM传感器采用石英音叉,即所谓的qPlus传感器,而不是硅悬臂。除了熔融金属中AFM的技术基础外,我们还介绍了两种应用:合金晶体生长过程的原位和原子分辨率分析以及两体相互作用力的测量。
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引用次数: 0
Establishment of artificial intelligence-driven fluorescence morphometry reveals involvement of osteocyte perilacunar remodeling specifically in mandibular bone of ovariectomized rats. 人工智能驱动的荧光形态测定法的建立揭示了骨细胞在去卵巢大鼠下颌骨的骨腔周围重构。
IF 1.9 Pub Date : 2025-10-17 DOI: 10.1093/jmicro/dfaf046
Atsuko Nakanishi-Kimura, Haruhisa Watanabe, Marie Hoshi-Numahata, Masae Goseki-Sone, Tadahiro Iimura

Bone dynamically changes its shape and structure in response to extra-tissue environments, so that bone morphometry has been a substantial method to evaluate pathophysiology of bone. Osteocytes embedded in mineralized bone matrix play key roles in systemic bone metabolism and characterize distinct bone sites. The jawbone has been described as a unique bone in the context of vertebrate evolution and function. Bone loss in the mandibular bone is less obvious in osteoporotic conditions than in other bones, such as vertebral and limb long bones, both in animal models and in clinical studies. Since osteocyte lacunae are complex and small (-10µm in length) in shape and size, respectively, comprehensive and unbiased morphometrical analysis of changes in the size of osteocyte lacunae was still an obstacle. This study established an artificial intelligence-driven morphometry with wide-field microscopy-based imaging of osteocyte lacunae. Successive comparative analyses demonstrated active perilacunar bone remodeling in the mandibular bone than in the parietal bone. This approach enabled us to statistically compare morphometric parameters in a more comprehensive and unbiased manner. We further discuss the possible unique contribution of the mandibular bone to the pathophysiology of osteoporosis. This study established an artificial intelligence-driven morphometry with wide-field microscopy-based imaging of osteocyte lacunae. Successive comparative analyses demonstrated active perilacunar bone remodeling in the mandibular bone than in the parietal bone. This approach enabled us to statistically compare morphometric parameters in a more comprehensive and unbiased manner.

骨的形状和结构会随着组织外环境的变化而发生动态变化,因此骨形态测量学已成为评价骨病理生理的重要方法。嵌入矿化骨基质中的骨细胞在全身骨代谢中发挥关键作用,并表征不同的骨部位。在脊椎动物的进化和功能中,颚骨被描述为一种独特的骨骼。在动物模型和临床研究中,与其他骨骼(如椎体和肢体长骨)相比,在骨质疏松症条件下,下颌骨的骨质流失不那么明显。由于骨细胞腔隙的形状和大小分别复杂而小(长度为-10µm),因此对骨细胞腔隙大小变化的全面、公正的形态计量学分析仍然是一个障碍。本研究建立了人工智能驱动的骨细胞腔隙宽视场显微镜成像形态学。连续的比较分析表明活跃的骨重构在下颌骨的棘突周围比在顶骨。这种方法使我们能够以更全面和无偏的方式统计比较形态计量参数。我们进一步讨论可能的独特贡献下颌骨骨质疏松症的病理生理。本研究建立了人工智能驱动的骨细胞腔隙宽视场显微镜成像形态学。连续的比较分析表明活跃的骨重构在下颌骨的棘突周围比在顶骨。这种方法使我们能够以更全面和无偏的方式统计比较形态计量参数。
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引用次数: 0
Cryo-FIB-SEM visualization and radiation damage of a water-THF phase-separated mixture and in situ formed organic nanoparticles. 水- thf相分离混合物和原位形成的有机纳米颗粒的冷冻fib - sem可视化和辐射损伤。
IF 1.9 Pub Date : 2025-10-11 DOI: 10.1093/jmicro/dfaf044
Satoshi Okada, Hayato Tsuji

Cryoelectron microscopy is a powerful technique for high-resolution imaging of nonaqueous liquids, but challenges remain regarding imaging and data interpretation. Recent advancements in estimating the physicochemical properties of pure organic liquids at cryogenic temperatures have enhanced the selection of imaging and pre-treatment conditions. However, whether binary mixtures behave similarly to pure substances is still unclear. Furthermore, focused ion beam (FIB) milling facilitates site-specific cross-sectioning, but its effects on the microscopic morphology of frozen organic liquids are not well understood. In this study, we investigated water-tetrahydrofuran (THF) binary mixtures as a model to explore their phase behavior and radiation damage under cryogenic conditions. Spectroscopic analyses indicated microscopic phase separation within the seemingly miscible water-THF mixtures, but their detailed structure has been a subject of ongoing debate. Using cryo-scanning electron microscopy with FIB (cryo-FIB-SEM), we visualized bicontinuous phase-separation. The domain sizes were consistent across spectroscopic data, thermally sublimed surfaces, and FIB cross-sections. Notably, FIB milling caused a significant loss of THF-rich regions, likely due to localized temperature increases of approximately 178 K, which is an order of magnitude greater than that in water-rich domains. We also noted the nanoparticles of electron-resistant carbazole-terminated carbon-bridged oligo(para-phenylenevinylene) (COPV2-G1) formed within the THF-rich phase. Extended electron irradiation led to morphological changes and shrinkage, suggesting THF was incorporated into COPV2-G1 aggregates along with THF decomposition induced by the electron beam. These findings underscore critical considerations in cryo-FIB-SEM imaging of binary organic liquids and solvated particles, providing practical insights for reducing or leveraging ion/electron beam-induced artifacts.

低温电子显微镜是一种强大的非水液体高分辨率成像技术,但在成像和数据解释方面仍然存在挑战。在估计纯有机液体在低温下的物理化学性质方面的最新进展,提高了成像和预处理条件的选择。然而,二元混合物的行为是否与纯物质相似尚不清楚。此外,聚焦离子束(FIB)铣削有利于特定位置的横截面,但其对冷冻有机液体微观形貌的影响尚不清楚。在这项研究中,我们以水-四氢呋喃(THF)二元混合物为模型,探讨了它们在低温条件下的相行为和辐射损伤。光谱分析表明,在看似可混溶的水-四氢呋喃混合物中存在微观相分离,但其详细结构一直是争论的主题。利用FIB冷冻扫描电镜(cro -FIB- sem),我们看到了双连续相分离。光谱数据、热升华表面和FIB截面上的畴尺寸是一致的。值得注意的是,FIB铣削导致了富thf区域的显著损失,可能是由于局部温度升高了约178 K,这比富水区域的温度升高了一个数量级。我们还注意到在富thf相中形成了抗电子咔唑端碳桥低聚物(对苯基乙烯)(COPV2-G1)纳米颗粒。长时间的电子照射导致了COPV2-G1的形态变化和收缩,表明随着电子束诱导THF分解,THF被纳入COPV2-G1聚集体。这些发现强调了二元有机液体和溶剂化颗粒的低温fib - sem成像的关键考虑因素,为减少或利用离子/电子束诱导的伪影提供了实用的见解。
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引用次数: 0
Accumulation of 13C-Labeled Phosphatidylethanolamine in the Termite Abdomen Revealed by Correlative Isotope Microscopy and Mass Microscopy. 用相关同位素显微镜和质显微镜观察白蚁腹部13c标记的磷脂酰乙醇胺的积累。
IF 1.9 Pub Date : 2025-10-11 DOI: 10.1093/jmicro/dfaf045
Rafia Ferdous, Md Muedur Rahman, Takumi Sakamoto, Md Shoriful Islam, Md Maniruzzaman, Md Monirul Islam, Md Foyzur Rahman, Ryo Omagari, Md Al Mamun, Ariful Islam, Shuhei Aramaki, Shoshiro Hirayama, Tomohito Sato, Yutaka Takahashi, Tomoaki Kahyo, Naoya Sakamoto, Hisayoshi Yurimoto, Kenji Matsuura, Mitsutoshi Setou

Isotope microscopic imaging and atmospheric pressure matrix-assisted laser desorption/ionization mass spectrometry imaging (AP-MALDI-MSI) provide powerful, complementary approaches for visualizing metabolic dynamics in biological tissues. This study applied these techniques to termite workers fed with 13C-labeled cellulose for one week. Termites are classified as eusocial insects because of their colonies' clear division of labor. The two primary castes in their life cycle are reproductive (king and queen), responsible for reproduction, and non-reproductive (workers and soldiers), who handle tasks such as defense, brood care, and foraging. Although various techniques have been developed to detect 13C-labeled biomolecules in samples, it remains unclear whether the iMScopeTM prototype can visualize these molecules with high spatial resolution. Advanced isotope microscopic imaging technique with high spatial resolution (200-300 nm) offered ultra-high-resolution visualization of the relative abundance of the 13C/12C distribution, suggesting precise localization of isotope enrichment in the abdomen. AP-MALDI-MSI performed in the iMScopeTM prototype enabled spatial mapping of 13C-labeled and unlabeled metabolites, such as acetyl-L-carnitine (ALC) and phosphatidylethanolamine (PE), by detecting characteristic mass shifts due to 13C incorporation. The accumulation of PE in the termite abdomen represents an adaptive strategy to optimize nutrient allocation and promote social cohesion, thereby highlighting its potential role in maintaining colony fitness. Our study shows that the iMScopeTM prototype is a novel AP-MALDI-MSI technique to detect 13C-integrated metabolites in the 13C-labeled sample. This study also demonstrated that this technique can detect 13C-integrated PE, which is abundant mainly in termite abdomen.

同位素显微成像和大气压基质辅助激光解吸/电离质谱成像(AP-MALDI-MSI)为可视化生物组织中的代谢动力学提供了强大的互补方法。本研究将这些技术应用于喂食13c标记纤维素的白蚁工蚁一周。由于蚁群分工明确,白蚁被归类为真群居昆虫。它们生命周期中的两个主要种姓是负责繁殖的生殖阶层(国王和王后)和负责繁殖的非生殖阶层(工人和士兵),他们负责防御、照顾后代和觅食等任务。尽管已经开发了各种技术来检测样品中13c标记的生物分子,但iMScopeTM原型是否能够以高空间分辨率可视化这些分子仍不清楚。高空间分辨率(200-300 nm)的先进同位素显微成像技术提供了13C/12C分布相对丰度的超高分辨率可视化,提示了腹部同位素富集的精确定位。在iMScopeTM原型中执行的AP-MALDI-MSI通过检测由于13C掺入引起的特征质量变化,实现了13C标记和未标记代谢物(如乙酰左旋肉碱(ALC)和磷脂酰乙醇胺(PE))的空间映射。PE在白蚁腹部的积累代表了一种优化营养分配和促进社会凝聚力的适应性策略,从而突出了其在维持群体健康方面的潜在作用。我们的研究表明,iMScopeTM原型是一种新的AP-MALDI-MSI技术,用于检测13c标记样品中的13c整合代谢物。本研究还表明,该技术可以检测到主要存在于白蚁腹部的13c -整合PE。
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引用次数: 0
Impact of Atomic Thermal Motion on the Ti L2,3-edge Fine Structure. 原子热运动对Ti L2三棱精细结构的影响
IF 1.9 Pub Date : 2025-10-07 DOI: 10.1093/jmicro/dfaf042
Mitsutaka Haruta, I-Ching Lin, Takashi Nemoto, Hiroki Kurata

This review examines the effects of thermal vibrations on core-level excitation spectra, with a particular emphasis on the Ti L  2,3-edge spectra of cubic perovskite-type titanium oxides (SrTiO3 and PbTiO3). Based on combining scanning transmission electron microscopy energy-loss near-edge structure analyses with cluster-type crystal-field multiplet calculations, the influence of atomic thermal vibrations on the fine structure of the Ti L  2,3-edge is investigated, and it is demonstrated that the thermal vibration of oxygen atoms in cubic SrTiO3 can be estimated from the spectrum by fitting experimental and theoretical results. The same approach was extended to cubic PbTiO3 such that isotropic thermal vibrations were identified that relate to the difference in the transition to a low-temperature tetragonal phase. Although the present technique does not directly resolve phonon modes, it treats thermal factors as adjustable parameters, enabling the identification of subtle vibrational features even in materials already widely studied. Further investigation of the relationship between thermal vibrations and the fine structure of core-loss spectra could assist in elucidating certain material properties. This review explores the effects of thermal vibrations on Ti L  2,3-edge spectra of cubic perovskite oxides (SrTiO3, PbTiO3). Combining STEM-ELNES with crystal-field multiplet calculations, it shows that oxygen thermal vibrations can be estimated from spectral fitting, revealing subtle vibrational features and their relation to phase transitions.

本文研究了热振动对核心能级激发光谱的影响,特别强调了立方钙钛矿型钛氧化物(SrTiO3和PbTiO3)的Ti l2,3边光谱。基于扫描透射电子显微镜能量损失近边结构分析和簇型晶体场多重计算相结合的方法,研究了原子热振动对til2,3边缘精细结构的影响,并通过拟合实验和理论结果证明,可以从光谱上估计立方SrTiO3中氧原子的热振动。同样的方法被扩展到立方PbTiO3,这样就确定了各向同性热振动,这与向低温四方相转变的差异有关。虽然目前的技术不能直接解决声子模式,但它将热因素作为可调参数,即使在已经广泛研究的材料中也能识别细微的振动特征。进一步研究热振动与芯损谱精细结构之间的关系有助于阐明材料的某些特性。本文研究了热振动对立方钙钛矿氧化物(SrTiO3, PbTiO3)的til2,3边光谱的影响。结合STEM-ELNES和晶体场多重计算,表明氧的热振动可以从光谱拟合中估计出来,揭示了微妙的振动特征及其与相变的关系。
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引用次数: 0
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Microscopy (Oxford, England)
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