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EXAFS study of the local environment of lead and iron sorbed onto volcanic ash 火山灰吸附铅和铁的局部环境EXAFS研究
IF 1.9 4区 物理与天体物理 Q2 Physics and Astronomy Pub Date : 2023-08-01 DOI: 10.1016/j.elspec.2023.147379
Bridinette Thiodjio Sendja , Duclair Tchana Kamgne , Rene Loredo Portales , Giuliana Aquilanti

This work focuses on the EXAFS investigation of the local environment of lead and iron sorbed onto volcanic ash materials previously studied using XANES technique. Different compounds found in the composition of volcanic ash were used as the models in the EXAFS fitting procedure of the experimental EXAFS spectra collected at the Fe K edge and Pb L3 edge in the Fe- and Pb-sorbed volcanic ash samples. The results showed two types of interactions involving in the adsorption process of both samples. The first is related to iron or lead absorber with oxygen atoms in the first coordination shell. The second interaction occurred between the absorbers (Fe or Pb) and the backscatters (Fe or Pb) in the second shell. The local environment of the iron-sorbed element may have a cubic geometry with different crystallographic sites related to oxygen and iron atoms. On the other hand, the lead-sorbed element may be in orthorhombic geometry with different sites related to oxygen atoms and lead atoms. The adsorption mechanisms involved in the process of iron and lead sorption are ion exchange with probable chemisorption for iron and microprecipitation for lead.

这项工作的重点是利用EXAFS对先前使用XANES技术研究的火山灰材料吸附铅和铁的局部环境进行调查。在EXAFS拟合过程中,采用火山灰成分中发现的不同化合物作为模型,对吸附铁和铅的火山灰样品中Fe K边缘和Pb L3边缘采集的EXAFS实验光谱进行拟合。结果表明,两种样品的吸附过程中存在两种类型的相互作用。第一种是在第一配位壳层中具有氧原子的铁或铅吸收体。第二次相互作用发生在吸收体(Fe或Pb)和后向散射体(Fe或Pb)之间。铁吸附元素的局部环境可能具有立方几何形状,具有与氧原子和铁原子相关的不同晶体学位点。另一方面,铅吸附元素可能呈正交几何,与氧原子和铅原子相关的位置不同。铁和铅的吸附机制主要是离子交换和可能的化学吸附和铅的微沉淀。
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引用次数: 0
Making chemical sense of phase in soft X-ray spectroptychography 软X射线光谱成像中相位的化学意义
IF 1.9 4区 物理与天体物理 Q2 Physics and Astronomy Pub Date : 2023-08-01 DOI: 10.1016/j.elspec.2023.147367
Joseph Stitsky , Jian Wang , Stephen Urquhart

Spectroptychography is being used to realize a significant improvement in the spatial resolution of x-ray spectromicroscopy, allowing chemical microanalysis at finer spatial scales. The chemical sensitivity of near edge X-ray absorption fine structure (NEXAFS) is familiar to most researchers who use x-ray spectromicroscopy for chemical microanalysis. However, the additional phase information available through ptychography provides additional and tantalizing data, and potentially additional chemical information. This paper explores the chemical information available in phase for a system of silicon dioxide nanospheres.

分光光度法被用于实现x射线光谱显微镜的空间分辨率的显着改进,允许在更细的空间尺度上进行化学微量分析。近边缘x射线吸收精细结构(NEXAFS)的化学灵敏度是大多数使用x射线光谱显微镜进行化学微量分析的研究人员所熟悉的。然而,通过压型图获得的额外相信息提供了额外的和诱人的数据,以及潜在的额外化学信息。本文探讨了二氧化硅纳米球体系的相化学信息。
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引用次数: 0
Soft X-ray microspectroscopic imaging studies of exfoliated surface between fluoropolymer and Cu plate directly bonded by plasma irradiation with ammonia gas 氨气等离子体辐照直接键合含氟聚合物与铜板剥离表面的软x射线显微成像研究
IF 1.9 4区 物理与天体物理 Q2 Physics and Astronomy Pub Date : 2023-08-01 DOI: 10.1016/j.elspec.2023.147385
A. Yamaguchi , S. Ikeda , M. Nakaya , Y. Kobayashi , Y. Haruyama , S. Suzuki , K. Kanda , Y. Utsumi , T. Ohkochi , H. Sumida , M. Oura

The F, C, O, and N elemental distribution maps at the exfoliated surfaces of Cu plate after peeling the fluoropolymers from Fluorinated ethylene propylene (FEP)/Cu and Perfluoroalkoxyalkane (PFA)/Cu pieces which were bonded by plasma treatment including amino acid were performed by microscopic synchrotron radiation (SR) spectroscopic imaging measurements. The spatial elemental distribution pattern of exfoliated Cu after peeling PFA/Cu piece was not detectable by scanning electron microscopy with energy dispersive X-ray spectroscopy imaging alone, was revealed by SR-based soft X-ray microspectroscopy. We also obtained the microprobe X-ray fluorescence spectra and microprobe near-edge X-ray absorption fine structure spectra. Based on these measurement results, it is considered that the delamination of FEP/Cu piece mainly caused by resin failure, while the delamination of PFA/Cu is caused by interfacial delamination in addition to resin failure. The Hard X-ray photoelectron spectroscopy was also performed to confirm that the bonding via nitrogen is formed. Our SR-based analyses provided confirmation that fluoropolymers and Cu plates are bonded by N-mediated chemical bonding. The present study insists that the technique and plasma bonding process reported are expected to contribute to the development of new devices and systems consisting of fluoropolymers and metals.

采用显微同步辐射(SR)光谱成像测量方法,对含氨基酸等离子体处理后的含氟乙烯丙烯(FEP)/Cu和全氟烷烷(PFA)/Cu片剥离后的含氟聚合物在Cu板剥离表面的F、C、O和N元素分布图进行了测量。PFA/Cu片剥离后,扫描电镜和x射线能谱成像无法检测到剥离后Cu的空间元素分布规律,而基于sr的软x射线显微光谱分析揭示了Cu的空间元素分布规律。获得了微探针x射线荧光光谱和微探针近边x射线吸收精细结构光谱。基于这些测量结果,认为FEP/Cu片的分层主要是由树脂失效引起的,而PFA/Cu片的分层除了树脂失效外,还由界面分层引起。硬x射线光电子能谱也证实了氮键的形成。我们基于sr的分析证实了含氟聚合物和Cu板是通过n介导的化学键结合的。本研究认为,所报道的技术和等离子键合过程有望为含氟聚合物和金属的新器件和系统的开发做出贡献。
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引用次数: 0
Soft X-rays radiation damage on plunge-frozen and freeze-dried maize roots evaluated by FTIR spectromicroscopy 用傅里叶红外光谱显微镜研究了软x射线辐射对浸冻和冻干玉米根系的损伤
IF 1.9 4区 物理与天体物理 Q2 Physics and Astronomy Pub Date : 2023-08-01 DOI: 10.1016/j.elspec.2023.147384
A. Gianoncelli , M. Žižić , V. Bonanni , G. Birarda , D.E. Bedolla , K. Vogel Mikuš

The radiation damage issue consequent to soft X-rays’ exposure is still an important aspect to be contemplated in soft X-ray microscopy. The work presented here is part of a more extended investigation on the topic and targets the effects of soft X-rays exposure on plant tissues.

The aftermaths of soft X-rays’ exposure were evaluated by FTIR spectromicroscopy by comparing irradiated and non-irradiated areas on similar plant structural features, one day and ten days after irradiation, to highlight also a possible time-dependent behavior consequent to air exposure.

Our results show partial degradation of lignocellulosic complex and oxidation of cellulose and most probably of hemicellulose; lignin moiety of cell walls in vascular tissue however remains stable.

Comparing the current study with our previous works it appears that, as expected, plant tissues seem less prone to soft X-rays radiation damage compared to mammalian cells or tissues.

软x射线暴露后的辐射损伤问题仍然是软x射线显微镜研究的一个重要方面。这里提出的工作是一个更广泛的调查课题的一部分,目标是软x射线暴露对植物组织的影响。通过FTIR光谱显微镜,比较辐照区和未辐照区在辐照后1天和10天的类似植物结构特征,评估软x射线暴露的后果,以强调空气暴露可能导致的时间依赖性行为。我们的结果表明,木质纤维素复合物的部分降解和氧化纤维素,很可能是半纤维素;然而,维管组织细胞壁的木质素部分保持稳定。将目前的研究与我们以前的工作进行比较,似乎正如预期的那样,与哺乳动物细胞或组织相比,植物组织似乎不太容易受到软x射线辐射的伤害。
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引用次数: 0
Quantitative mapping of calcium cell reservoirs in cyanobacteria at the submicrometer scale 亚微米级蓝藻钙细胞库的定量图谱
IF 1.9 4区 物理与天体物理 Q2 Physics and Astronomy Pub Date : 2023-08-01 DOI: 10.1016/j.elspec.2023.147369
Benzerara Karim , Görgen Sigrid , Khan Monis Athar , Chauvat Franck , March Katia , Menguy Nicolas , Mehta Neha , Skouri-Panet Fériel , Swaraj Sufal , Travert Cynthia , Cassier-Chauvat Corinne , Duprat Elodie

Calcium plays an important role in the physiology of bacterial cells and as a free soluble form inside the cells, it is tightly regulated at a low concentration. However, much higher amounts of stored calcium exist within cells and can be remobilized at diverse occasions. As a consequence, there has been a variety of techniques developed to quantitatively map the different forms of Ca in cells. Here we show how scanning transmission x-ray microscopy (STXM), a synchrotron-based microscopy technique, conducted in the soft x-ray range at the Ca L2,3 edges (340–360 eV) offers an original and informative quantitative view of different Ca reservoirs in bacterial cells at a spatial resolution better than 100 nm. To illustrate this, we analyzed mutants of the cyanobacterium Synechococcus elongatus PCC 7942, overexpressing different versions of a gene called ccyA from two phylogenetically distant cyanobacteria: Gloeomargarita lithophora and Synechococcus sp. PCC 6312. This gene is diagnostic of the capability of some cyanobacteria to form intracellular amorphous calcium carbonate (iACC) but its function remains unknown. Here we show that the overexpression of the ccyA gene in the iACC non-forming cyanobacterium S. elongatus PCC 7942 results in an increased Ca content, especially in some Ca-rich cells. Moreover, we show that STXM can discriminate four different reservoirs of Ca in cyanobacteria and provides quantitative assessment of their relative importance.

钙在细菌细胞的生理中起着重要的作用,作为细胞内的一种自由可溶性形式,它在低浓度下受到严格的调节。然而,细胞内储存了大量的钙,可以在不同的场合重新调动。因此,已经开发了各种技术来定量绘制细胞中不同形式的钙。在这里,我们展示了扫描透射x射线显微镜(STXM),一种基于同步加速器的显微镜技术,如何在Ca L2,3边缘(340-360 eV)的软x射线范围内进行,以优于100 nm的空间分辨率提供了细菌细胞中不同Ca库的原始和信息定量视图。为了说明这一点,我们分析了来自两个系统发育上遥远的蓝藻:Gloeomargarita lithophora和Synechococcus sp. PCC 6312的长聚球菌PCC 7942的突变体,这些突变体过表达了一种称为ccyA的基因的不同版本。该基因是一些蓝藻形成细胞内无定形碳酸钙(iACC)的诊断能力,但其功能尚不清楚。本研究表明,在iACC非形成蓝藻S. elongatus PCC 7942中,ccyA基因的过表达导致钙含量增加,特别是在一些富钙细胞中。此外,我们发现STXM可以区分蓝藻中四种不同的钙储集层,并提供了它们相对重要性的定量评估。
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引用次数: 1
Dissociative electron attachment to 1- and 9-chloroanthracene in the gas phase 气相中1-和9-氯蒽的离解电子附着
IF 1.9 4区 物理与天体物理 Q2 Physics and Astronomy Pub Date : 2023-08-01 DOI: 10.1016/j.elspec.2023.147383
Nail L. Asfandiarov, Mars V. Muftakhov, Stanislav A. Pshenichnyuk

Dissociative electron attachment (DEA) to 1-chloroanthracene and 9-chloroanthracene was investigated under gas-phase conditions. In both compounds, the elimination of the chlorine anion is the dominant channel for the dissociation of molecular negative ions (NIs). The second most intense channel leads to the formation of molecular anions (Mˉ). The autodetachment lifetime of Mˉ was measured to be about 170 μs for both compounds. The widths of the Mˉ peaks indicate that molecular anions are formed via two resonances: at thermal electron energies and through a shape resonance at the energy of ∼0.5 eV. Adiabatic electron affinities were estimated in the framework of the simple Arrhenius model to be 0.86 eV for both molecules, the values being close to the theoretical predictions by DFT method of 0.90 eV and 0.93 eV for 1-chloroanthracene and 9-chloroanthracene respectively. Metastable negative ions are observed in the DEA spectra of both molecules, which testifies that the elimination of chlorine anions from molecular NIs appears on a time scale of several microseconds.

在气相条件下研究了1-氯蒽和9-氯蒽的解离电子附着。在这两种化合物中,氯阴离子的消除是分子负离子(NIs)解离的主要通道。第二强通道导致分子阴离子(M - h)的形成。两种化合物的自脱离寿命均约为170 μs。M - h峰的宽度表明分子阴离子是通过两种共振形成的:热电子能共振和约0.5 eV的形状共振。在简单Arrhenius模型框架下,两种分子的绝热电子亲和值分别为0.86 eV,接近DFT方法对1-氯蒽和9-氯蒽的理论预测值0.90 eV和0.93 eV。在两种分子的DEA光谱中都观察到亚稳态负离子,这证明了氯阴离子在几微秒的时间尺度上从NIs分子中消除。
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引用次数: 0
Preface – Advances in photoelectron diffraction and photoelectron holograph 前言:光电子衍射和光电子全息术的研究进展
IF 1.9 4区 物理与天体物理 Q2 Physics and Astronomy Pub Date : 2023-08-01 DOI: 10.1016/j.elspec.2023.147339
Hiroshi Daimon , Michel A. Van Hove
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引用次数: 0
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 Physics and Astronomy 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 Physics and Astronomy 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 Physics and Astronomy 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
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Journal of Electron Spectroscopy and Related Phenomena
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