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Network formation and differentiation of chitosan–acrylic acid hydrogels using X-ray absorption spectroscopy and multivariate analysis of Fourier transform infrared spectra 壳聚糖-丙烯酸水凝胶的x射线吸收光谱和傅立叶变换红外光谱多元分析
IF 1.9 4区 物理与天体物理 Q2 SPECTROSCOPY Pub Date : 2023-08-01 DOI: 10.1016/j.elspec.2023.147372
Kathrina Lois M. Taaca , Hideki Nakajima , Kanjana Thumanu , Eloise I. Prieto , Magdaleno R. Vasquez Jr.

Chitosan–acrylic acid (Cs–AA) hydrogels were prepared by blending different Cs concentrations and AA:Cs ratios. The Cs–AA hydrogel samples were analyzed using synchrotron radiation-induced near edge X-ray absorption fine structure (NEXAFS) and Fourier transform infrared (FTIR) spectroscopies. The characteristics of Cs were observed through the C, O, and N K edges in NEXAFS. Significant shifts in the Cs characteristic features were induced by the addition of AA. The NEXAFS findings confirmed the new covalent and ionic bridges to form the network of the Cs–AA hydrogel. Raw FTIR spectra were used to investigate the different functional groups of each of the macromolecules. The study attempted to discriminate the Cs–AA hydrogels prepared with different Cs wt% concentration and AA:Cs ratio using multivariate approaches. The preprocessed dataset was evaluated using principal component analysis (PCA) and hierarchical cluster analysis (HCA). The PCA and HCA methods showed the possibility of discriminating the Cs–AA hydrogel samples from the control samples and with each other. The approaches further confirmed that the CO groups found in the range of 1700–1800 cm−1 can be used as an identifier for Cs–AA hydrogel samples prepared using different solution parameters. The use of FTIR coupled with multivariate approaches provided a simple and reliable way to inspect the possible discrimination of Cs–AA hydrogels.

通过不同Cs浓度和AA:Cs比的复配制备了壳聚糖-丙烯酸(Cs - AA)水凝胶。采用同步辐射诱导近边x射线吸收精细结构(NEXAFS)和傅里叶变换红外光谱(FTIR)对Cs-AA水凝胶样品进行了分析。通过NEXAFS的C、O和N K边观察Cs的特征。AA的加入引起了Cs特征特征的显著变化。NEXAFS的研究结果证实了新的共价键和离子桥形成了Cs-AA水凝胶网络。利用原始FTIR光谱研究了每种大分子的不同官能团。本研究试图用多变量方法对不同Cs wt%浓度和AA:Cs比制备的Cs - AA水凝胶进行鉴别。采用主成分分析(PCA)和层次聚类分析(HCA)对预处理后的数据集进行评价。PCA和HCA方法均能将Cs-AA水凝胶样品与对照样品区分开来,并能相互区分。这些方法进一步证实了在1700-1800 cm−1范围内发现的CO基团可以作为不同溶液参数制备的Cs-AA水凝胶样品的标识符。FTIR结合多变量方法为Cs-AA水凝胶的鉴别提供了一种简单可靠的方法。
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引用次数: 1
Scanning transmission X-ray microscopy at the Advanced Light Source 先进光源的扫描透射X射线显微镜
IF 1.9 4区 物理与天体物理 Q2 SPECTROSCOPY Pub Date : 2023-08-01 DOI: 10.1016/j.elspec.2023.147381
Thomas Feggeler , Abraham Levitan , Matthew A. Marcus , Hendrik Ohldag , David A. Shapiro

Over 50 years of development, synchrotron based X-ray microscopy has become a routine and powerful tool for the analysis of nanoscale structure and chemistry in many areas of science. Scanning X-ray microscopy is particularly well suited to the study of chemical and magnetic states of matter and has become available at most synchrotron light sources using a variety of optical schemes, detectors and sample environments. The Advanced Light Source at Lawrence Berkeley National Laboratory has an extensive program of soft X-ray scanning microscopy which supports a broad range of scientific research using a suite of advanced tools for high spatio-temporal resolution and control of active materials. Instruments operating within an energy range between 200–2500 eV with spatial resolution down to 7 nm and sub 20 picosecond time resolution are available. These capabilities can be routinely used in combination with a variety of sample stimuli, including gas or fluid flow, temperature control from 100 to 1200 K, DC bias and pulsed or continuous microwave excitation. We present here a complete survey of our instruments, their most advanced capabilities and a perspective on how they complement each other to solve complex problems in energy, materials and environmental science.

经过50多年的发展,基于同步加速器的x射线显微镜已经成为在许多科学领域分析纳米结构和化学的常规和强大的工具。扫描x射线显微镜特别适合研究物质的化学和磁性状态,并且已经在大多数同步加速器光源中使用各种光学方案,探测器和样品环境。劳伦斯伯克利国家实验室的先进光源拥有广泛的软x射线扫描显微镜项目,该项目使用一套先进的工具来支持广泛的科学研究,以实现高时空分辨率和活性物质控制。仪器工作在200-2500 eV之间的能量范围内,空间分辨率低至7纳米,时间分辨率低于20皮秒。这些功能可以常规地与各种样品刺激结合使用,包括气体或流体流动,温度控制从100到1200 K,直流偏压和脉冲或连续微波激励。在这里,我们将全面介绍我们的仪器,它们最先进的功能,以及它们如何相互补充以解决能源,材料和环境科学中的复杂问题的观点。
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引用次数: 0
Electron scattering at high momentum transfer 高动量传递时的电子散射
IF 1.9 4区 物理与天体物理 Q2 SPECTROSCOPY Pub Date : 2023-08-01 DOI: 10.1016/j.elspec.2023.147382
Maarten Vos

Energetic (multiple keV) electrons scattering at high momentum transfer (i.e. scatter over a large angle (>20°)) interact with a single particle, either a nucleus or a target electron. Energy transfer is then determined by the incoming energy, scattering angle and the mass and velocity of the scattering particle. When scattering from a target electron a large fraction of the incoming energy is transferred and scattered and ejected electrons can be detected in coincidence. The experiment is then known as electron momentum spectroscopy or (e,2e) spectroscopy and information about the electronic structure is obtained. When scattering from a nucleus the transferred energy is much smaller, and only the scattered electron can be detected. Then the experiment is known as electron Rutherford backscattering and one can measure the sample composition and vibrational properties. In this review we give examples of experimental results for both cases to illustrate the unique information that can be obtained by electron spectroscopy at high-momentum transfer, a less-frequently utilised experimental condition.

高能(多keV)电子在高动量转移下散射(即在大角度(>20°)上散射)与单个粒子(原子核或目标电子)相互作用。能量传递由入射能量、散射角和散射粒子的质量和速度决定。当从目标电子散射时,入射能量的很大一部分被转移,散射和射出的电子可以重合地检测到。该实验被称为电子动量谱或(e,2e)谱,并获得有关电子结构的信息。当从原子核散射时,传递的能量要小得多,而且只能检测到散射的电子。该实验被称为电子卢瑟福后向散射,可以测量样品的组成和振动特性。在这篇综述中,我们给出了两种情况下的实验结果的例子,以说明在高动量转移(一种不太常用的实验条件)下电子能谱可以获得的独特信息。
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引用次数: 0
Present status and recent progress of research, using photoemission-electron microscopy at SPring-8 利用SPring-8光电子显微镜的研究现状及最新进展
IF 1.9 4区 物理与天体物理 Q2 SPECTROSCOPY Pub Date : 2023-08-01 DOI: 10.1016/j.elspec.2023.147371
T. Ohkochi , M. Tanaka , T. Ohtsuki , Z. Horita , F. Kitajima , A. Yamaguchi , M. Kotsugi , H. Ogawa , M. Oura

Photoemission electron microscopy (PEEM), particularly when combined with synchrotron radiation, exerts a powerful functionality in spectroscopy applications. The use of PEEM has steadily expanded the availed analysis objects at the SPring-8 synchrotron facility, such as magnetic materials, thin-film devices, semiconductors, monolayers, extraterrestrial matter, and multiferroics. Some special experimental settings such as time-resolved or operando measurements have also been developed according to user requests. In this paper, we present an overview on the achievements of PEEM studies so far and introduce some recent technical and scientific progress at SPring-8.

光电电子显微镜(PEEM),特别是当与同步辐射相结合时,在光谱学应用中具有强大的功能。PEEM的使用稳步扩大了SPring-8同步加速器设施的可用分析对象,如磁性材料、薄膜器件、半导体、单层、地外物质和多铁质。还根据用户要求开发了一些特殊的实验设置,如时间分辨或operando测量。在本文中,我们概述了迄今为止PEEM的研究成果,并介绍了SPring-8的一些最新技术和科学进展。
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引用次数: 0
Sample structure prediction from measured XPS data using Bayesian estimation and SESSA simulator 利用贝叶斯估计和SESSA模拟器对实测XPS数据进行样本结构预测
IF 1.9 4区 物理与天体物理 Q2 SPECTROSCOPY Pub Date : 2023-08-01 DOI: 10.1016/j.elspec.2023.147370
Hiroshi Shinotsuka , Kenji Nagata , Malinda Siriwardana , Hideki Yoshikawa , Hayaru Shouno , Masato Okada

We have developed a framework for solving the inverse problem of X-ray photoelectron spectroscopy (XPS) by incorporating an XPS simulator, Simulation of Electron Spectra for Surface Analysis (SESSA), into Bayesian estimation to obtain an overall picture of the distribution of plausible sample structures from the measured XPS data. The Bayesian estimation framework automated the very tedious task of adjusting the sample structure parameters manually in the simulator. As an example, we performed virtual experiments of angle-resolved XPS on a four-layered sample, and we estimated the sample structures based on the XPS intensity data obtained from experiments. We succeeded in not only obtaining an optimal solution, but also visualizing the distribution of the solution through the Bayesian posterior probability distribution.

我们开发了一个框架来解决x射线光电子能谱(XPS)的反问题,通过将XPS模拟器,模拟表面分析电子能谱(SESSA)纳入贝叶斯估计,从测量的XPS数据中获得合理样品结构分布的总体情况。贝叶斯估计框架自动完成了在模拟器中手动调整样本结构参数的繁琐任务。以四层样品为例,进行了角度分辨XPS的虚拟实验,并根据实验得到的XPS强度数据对样品结构进行了估计。我们不仅成功地获得了最优解,而且通过贝叶斯后验概率分布将解的分布可视化。
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引用次数: 0
Development of soft X-ray ptychography and fluorescence microscopy system using total-reflection wolter mirror and application to measurement of drug-treated mammalian cells 全反射镜软X射线ptychography和荧光显微镜系统的开发及其在药物治疗哺乳动物细胞测量中的应用
IF 1.9 4区 物理与天体物理 Q2 SPECTROSCOPY Pub Date : 2023-08-01 DOI: 10.1016/j.elspec.2023.147380
Yoko Takeo , Kai Sakurai , Noboru Furuya , Kyota Yoshinaga , Takenori Shimamura , Satoru Egawa , Hisao Kiuchi , Hidekazu Mimura , Haruhiko Ohashi , Yoshihisa Harada , Mari Shimura , Takashi Kimura

We developed a soft X-ray microscopic imaging system, CARROT, that combines ptychography and fluorescence X-ray microscopy using a total-reflection Wolter mirror illumination system. The system offers advantages such as achromaticity and long working distances, enabling seamless application to a wide wavelength range. We demonstrated high-resolution imaging of cellular structures and sub-micrometer-scale changes induced by drug administration in mammalian cells. We further showcased the capability to seamlessly switch from ptychography measurements to X-ray fluorescence measurements at different wavelengths to map elemental distributions within cells. Our findings suggest that this system can be used for investigating the correlation between intracellular structures and elemental distribution, as well as for multimodal measurements of visible light fluorescence, Raman scattering, and soft X-rays to provide valuable insights into understanding intracellular dynamics.

我们开发了一种软x射线显微成像系统,CARROT,它结合了平面摄影和荧光x射线显微镜,使用全反射Wolter镜照明系统。该系统具有消色差和长工作距离等优点,可以在宽波长范围内无缝应用。我们在哺乳动物细胞中展示了高分辨率的细胞结构成像和药物给药引起的亚微米级变化。我们进一步展示了从平面摄影测量无缝切换到不同波长的x射线荧光测量的能力,以映射细胞内的元素分布。我们的研究结果表明,该系统可用于研究细胞内结构和元素分布之间的相关性,以及可见光荧光、拉曼散射和软x射线的多模态测量,为理解细胞内动力学提供有价值的见解。
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引用次数: 0
magnetoARPES: Angle Resolved Photoemission Spectroscopy with magnetic field control 磁场控制的角度分辨光谱学
IF 1.9 4区 物理与天体物理 Q2 SPECTROSCOPY Pub Date : 2023-07-01 DOI: 10.1016/j.elspec.2023.147357
Sae Hee Ryu , Garett Reichenbach , Chris M. Jozwiak , Aaron Bostwick , Peter Richter , Thomas Seyller , Eli Rotenberg

Angle-Resolved Photoemission Spectroscopy (ARPES) is a premier technique for understanding the electronic excitations in conductive, crystalline matter, in which the induced photocurrent is collected and dispersed in energy and angle of emission to reveal the energy- and momentum-dependent single particle spectral function A(k,ω). So far, ARPES in a magnetic field has been precluded due to the need to preserve the electron paths between the sample and detector. In this paper we report progress towards “magnetoARPES”, a variant of ARPES that can be conducted in a magnetic field. It is achieved by applying a microscopic probe beam (10 μm) to a thinned sample mounted upon a special sample holder that generates magnetic field confined to a thin layer near the sample surface. In this geometry we could produce ARPES in magnetic fields up to around ±100 mT. The magnetic fields can be varied from purely in-plane to nearly purely out-of-plane, by scanning the probe beam across different parts of the device. We present experimental and simulated data for graphene to explore the aberrations induced by the magnetic field. These results demonstrate the viability of the magnetoARPES technique for exploring symmetry breaking effects in weak magnetic fields.

角分辨光发射光谱(ARPES)是了解导电晶体物质中电子激发的主要技术,其中感应光电流被收集并分散在能量和发射角度上,以揭示能量和动量依赖的单粒子光谱函数a (k,ω)。到目前为止,由于需要保持样品和探测器之间的电子路径,在磁场中的ARPES已经被排除在外。在本文中,我们报告了“磁ARPES”的进展,这是一种可以在磁场中进行的ARPES的变体。它是通过将微观探针束(小于10 μm)施加到安装在特殊样品支架上的薄样品上实现的,该支架产生的磁场限制在样品表面附近的薄层上。在这种几何结构中,我们可以在高达±100 mT的磁场中产生ARPES。通过扫描设备不同部分的探针束,磁场可以从纯粹的面内变化到几乎纯粹的面外变化。我们提出了石墨烯的实验和模拟数据,以探索磁场引起的像差。这些结果证明了磁arpes技术在弱磁场中探索对称性破缺效应的可行性。
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引用次数: 1
Theoretical spectral function of CH3NH3PbI3 hybrid perovskite around the Fermi level 费米能级附近CH3NH3PbI3杂化钙钛矿的理论光谱函数
IF 1.9 4区 物理与天体物理 Q2 SPECTROSCOPY Pub Date : 2023-07-01 DOI: 10.1016/j.elspec.2023.147345
Min-I Lee , S. Ayaz Khan , J. Minar , A. Tejeda

Methylammonium lead iodide CH3NH3PbI3 (MAPI) is one of the hybrid organic–inorganic perovskites (HOIPs) widely considered for photovoltaic devices. Since photoemission is possibly the best technique for the experimental determination of the bands, we have calculated photoemission spectra at the main photon energies available at conventional laboratories (He I - 21.2 eV, He II - 40.8 eV) by performing fully relativistic Spin-Polarized Relativistic Korringa–Kohn–Rostoker (SPRKKR) calculations. Similarly, we have studied how s- and p-polarization affect to the calculated spectra. These studies could help to reach a better understanding of photoemission measurements on MAPI.

甲基碘化铅铵CH3NH3PbI3 (MAPI)是一种广泛应用于光伏器件的有机-无机杂化钙钛矿。由于光发射可能是实验确定能带的最佳技术,我们通过执行完全相对论性自旋极化相对论性Korringa-Kohn-Rostoker (SPRKKR)计算,计算了传统实验室可用的主要光子能量(He I - 21.2 eV, He II - 40.8 eV)下的光发射光谱。同样,我们也研究了s极化和p极化对计算光谱的影响。这些研究有助于更好地理解MAPI的光发射测量。
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引用次数: 0
Scanning transmission soft X-ray spectromicroscopy of mouse kidney and liver 小鼠肾脏和肝脏的扫描透射软x射线光谱显微镜
IF 1.9 4区 物理与天体物理 Q2 SPECTROSCOPY Pub Date : 2023-07-01 DOI: 10.1016/j.elspec.2023.147368
Tuomas Mansikkala , Takuji Ohigashi , Miia H. Salo , Anniina E. Hiltunen , Reetta Vuolteenaho , Petra Sipilä , Satu Kuure , Marko Huttula , Johanna Uusimaa , Reetta Hinttala , Ilkka Miinalainen , Salla Kangas , Minna Patanen

Scanning transmission X-ray microscopy (STXM) in the soft X-ray range is well-suited to study ultrastructural features of mammalian soft tissues. Especially at the carbon 1s edge, the imaging contrast varies drastically across the edge due to rapid changes in the X-ray absorption cross-section of functional groups present in the tissue samples enabling label-free soft X-ray spectromicroscopic studies. We present STXM spectromicroscopic imaging of mouse kidney and liver tissues. We especially concentrate on ultrastructural abnormalities in genetically modified Slc17a5 mice. STXM is a promising technique to study storage diseases without chemical alteration due to staining agents, but sample preparation poses a challenge.

扫描透射x射线显微镜(STXM)在软x射线范围内非常适合研究哺乳动物软组织的超微结构特征。特别是在碳1s边缘,由于组织样品中存在的官能团的x射线吸收截面的快速变化,使得无标记软x射线光谱显微镜研究的成像对比度在边缘上变化很大。我们展示了小鼠肾脏和肝脏组织的STXM光谱显微镜成像。我们特别关注转基因Slc17a5小鼠的超微结构异常。STXM是一种很有前途的技术,可以在不受染色剂影响的情况下研究贮藏病,但样品制备存在挑战。
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引用次数: 0
Analysis of surface properties of Mg doped ZnS and ZnSe thin films through x-ray photoelectron spectroscopy Mg掺杂ZnS和ZnSe薄膜表面性质的x射线光电子能谱分析
IF 1.9 4区 物理与天体物理 Q2 SPECTROSCOPY Pub Date : 2023-07-01 DOI: 10.1016/j.elspec.2023.147341
V.S. Ganesha Krishna, M.G. Mahesha

The surface properties of the spray-deposited Mg-doped ZnS and ZnSe films were investigated using X-ray photoelectron spectroscopy (XPS). The energy levels of the core electrons in ZnMgS and ZnMgSe, their peak positions, area ratios, and full width at half maximum were determined. Chemical shifts in Auger peaks, which are highly sensitive to changes in the chemical environment were used in the analysis. Compositional analysis indicated selenium deficiency in the ZnMgSe films. XPS peak of magnesium 2p showed a shift from 50.46 eV for ZnMgSe film to 50.63 eV for ZnMgS film and Mg 2s peak shift from 86.56 eV for ZnMgSe to 87.64 eV for ZnMgS films. A careful justification for the formation of oxides in the ZnMgSe films is also given. Ionicity for both films is about 0.51. Peak shifts in the Auger and core-level peaks are used to analyze the material's bonding strength, oxidation states, and bonding types.

利用x射线光电子能谱(XPS)研究了喷镀mg掺杂ZnS和ZnSe薄膜的表面性质。测定了znmggs和ZnMgSe中核心电子的能级、峰位、面积比和半最大值时的全宽度。在分析中使用了对化学环境变化高度敏感的俄歇峰的化学位移。组分分析表明,ZnMgSe薄膜缺硒。镁2p的XPS峰由ZnMgSe膜的50.46 eV位移到znmggs膜的50.63 eV,镁2s的XPS峰由ZnMgSe膜的86.56 eV位移到znmggs膜的87.64 eV。对ZnMgSe薄膜中氧化物的形成进行了详细的论证。两种薄膜的离子度均约为0.51。螺旋钻和芯级峰的峰移用于分析材料的结合强度、氧化态和结合类型。
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引用次数: 1
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Journal of Electron Spectroscopy and Related Phenomena
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