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The development of laboratory‐based high energy sources for XPS 开发用于 XPS 的实验室高能源
IF 1.7 4区 化学 Q4 CHEMISTRY, PHYSICAL Pub Date : 2024-03-14 DOI: 10.1002/sia.7300
John F. Watts, James E. Castle
Over the last fifty years, a number of higher energy X‐ray sources have been suggested as alternatives for the usual AlKα source found in the first commercial XPS systems and still the standard anode material for XPS today. This paper reviews the development of a number of such sources, predominantly in the authors' laboratory, and the rationale behind the desire to extend the binding energy range of the technique. The achromatic sources SiKα, ZrLα and TiKα are described along with monochromatic sources AgLα and CrKβ, both based on the standard quartz monochromator geometry but taking higher orders of diffraction. The driving force for much of this development was the desire to probe deeper core levels and CCC Auger transitions. These could be combined into initial or final state Auger parameters as described in much of the work cited in this review. The highest energy source considered is the CuKα source based around an external X‐ray tube, which provides much insight into the electronic structure of steels by measurement of the Fe1s and FeKLL peaks. The last decade or so has seen a significant increase of interest in HAXPES, and all manufacturers of turn‐key XPS instruments offer HAXPES options of one form or another, there are three dedicated HAXPES systems commercially available, which are very briefly described.
在过去的五十年里,人们提出了许多能量更高的 X 射线源,以替代第一批商用 XPS 系统中的常见 AlKα 源,这种源至今仍是 XPS 的标准阳极材料。本文回顾了主要由作者实验室开发的一些此类源,以及希望扩大该技术结合能范围的理由。本文介绍了消色差源 SiKα、ZrLα 和 TiKα,以及单色源 AgLα 和 CrKβ,两者都基于标准的石英单色器几何结构,但采用了更高阶的衍射。推动这一发展的主要动力是探测更深核级和 CCC 奥杰跃迁的愿望。正如本综述中引用的大部分工作所描述的那样,这些可以结合到初始或最终状态的奥杰参数中。考虑的最高能量源是基于外部 X 射线管的 CuKα 源,通过测量 Fe1s 和 FeKLL 峰,可以深入了解钢的电子结构。在过去十年左右的时间里,人们对 HAXPES 的兴趣大大增加,所有整套 XPS 仪器的制造商都提供了这样或那样的 HAXPES 选项,目前市场上有三种专用的 HAXPES 系统,现对其进行简要介绍。
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引用次数: 0
Challenges in quantifying Pt concentrations in Pd alloys by using secondary ion mass spectrometry: Strong grain orientation effects 利用二次离子质谱法量化钯合金中铂浓度的挑战:强烈的晶粒取向效应
IF 1.7 4区 化学 Q4 CHEMISTRY, PHYSICAL Pub Date : 2024-03-14 DOI: 10.1002/sia.7302
Børge Holme, Silje Fosse Håkonsen, David Waller
Palladium–platinum alloys were analysed by dynamic secondary ion mass spectrometry (SIMS) to investigate grain orientation effects that gave differences of up to 400% in the Pt/Pd count rate ratios, even within the same grain upon small rotations of a Pd sample with 1 wt% Pt. The sample had been homogenized by annealing, and the homogeneity was confirmed by X‐ray analysis in scanning electron microscopy (SEM). Grain orientations were determined by electron backscatter diffraction (EBSD). Crater depths were measured by white light interferometry (WLI). SEM images from the bottom of SIMS craters made in the same grain after small rotations around the sample surface normally showed different patterns of microfaceting for some rotation angles, probably exposing low‐index crystallographic planes. A complete understanding of the observed grain orientation effect is still lacking. However, factors such as ion mass, sputter rate, ion channelling, ion focusing, preferential sputtering, surface height, crater microfaceting and/or angle‐dependent sputtering seem to play a role. For these Pd–Pt alloys, the strong grain orientation effect adds another level of complexity when attempting to quantify concentrations and obtain depth profiles by SIMS. Without proper sampling and/or averaging, one could reach very wrong conclusions when comparing results from different samples.
采用动态二次离子质谱法(SIMS)分析了钯铂合金,以研究晶粒取向效应,这种效应使铂/钯计数率比相差高达 400%,即使在含 1 wt% 铂的钯样品小幅旋转时的同一晶粒内也是如此。晶粒取向由电子反向散射衍射(EBSD)确定。凹坑深度通过白光干涉仪(WLI)进行测量。SIMS环形山底部的扫描电子显微镜图像显示,在样品表面进行小幅旋转后,同一晶粒在某些旋转角度下通常会出现不同的微切面,这可能是低指数晶面的暴露。对观察到的晶粒取向效应仍缺乏全面的了解。不过,离子质量、溅射速率、离子导流、离子聚焦、优先溅射、表面高度、陨石坑微尖化和/或与角度有关的溅射等因素似乎都在起作用。对于这些钯铂合金,当试图通过 SIMS 量化浓度和获得深度剖面图时,强烈的晶粒取向效应又增加了复杂性。如果没有适当的取样和/或平均,在比较不同样品的结果时可能会得出非常错误的结论。
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引用次数: 0
A study on functionalization process of silicon dioxide nanoparticles for hydrophobic coating applications 用于疏水涂层的二氧化硅纳米颗粒功能化工艺研究
IF 1.7 4区 化学 Q4 CHEMISTRY, PHYSICAL Pub Date : 2024-03-10 DOI: 10.1002/sia.7305
Avinash Kumar, Sushant Negi, Simanchal Kar
Functionalized nano-SiO2 is an inorganic compound that exhibits hydrophobic properties upon the addition of a silane group through a chemical reaction. This property is highly effective in surface modification for various substrates, including glass, metal, and ceramics. These surface modifications find applications in self-cleaning, anti-fogging coatings, and water-repellent materials. In this work, the role of nano-SiO2 and Hexadecyltrimethoxysilane (HDTMS) functionalized nano-SiO2 has been synthesized successfully by the sol–gel method for coating applications. The outcomes of water contact angle (WCA), analysis, Fourier transform infrared spectroscopy (FTIR), thermal gravimetric analysis (TGA), scanning electron microscope (SEM), and transmission electron microscope (TEM) observations revealed the successful grafting of hydrophobic long-chain alkyl groups from HDTMS onto the surface of SiO2 nanoparticles. Notably, when the ratio of SiO2 nanoparticles to HDTMS is 0.25:1, the WCA of the functionalized SiO2 nanoparticles is enhanced significantly. This value is 5.35 times greater than the initial angle of contact before the modification, leading to the achievement of a super hydrophobic property.
功能化纳米二氧化硅是一种无机化合物,在通过化学反应加入硅烷基团后会表现出疏水特性。这种特性对于玻璃、金属和陶瓷等各种基材的表面改性非常有效。这些表面改性可应用于自清洁、防雾涂层和憎水材料。在这项研究中,采用溶胶-凝胶法成功合成了纳米二氧化硅和十六烷基三甲氧基硅烷(HDTMS)功能化纳米二氧化硅,并将其应用于涂层。水接触角(WCA)分析、傅立叶变换红外光谱(FTIR)、热重分析(TGA)、扫描电子显微镜(SEM)和透射电子显微镜(TEM)观察结果表明,HDTMS 的疏水长链烷基成功接枝到了 SiO2 纳米粒子表面。值得注意的是,当 SiO2 纳米粒子与 HDTMS 的比例为 0.25:1 时,功能化 SiO2 纳米粒子的 WCA 显著提高。该值是改性前初始接触角的 5.35 倍,从而实现了超疏水特性。
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引用次数: 0
Effect of Al2O3 thickness and oxidant precursors on the interface composition and contamination in Al2O3/GaN structures Al2O3 厚度和氧化剂前驱体对 Al2O3/GaN 结构中界面成分和污染的影响
IF 1.7 4区 化学 Q4 CHEMISTRY, PHYSICAL Pub Date : 2024-03-04 DOI: 10.1002/sia.7299
Tarek Spelta, Eugénie Martinez, Marc Veillerot, Pedro Fernandes Paes Pinto Rocha, Laura Vauche, Bassem Salem, Bérangère Hyot
In this paper, we investigate the Al2O3/GaN critical buried interface of the next generation of gallium nitride (GaN)‐based transistors using time‐of‐flight secondary ion mass spectrometry (ToF‐SIMS) and hard X‐ray photoelectron spectroscopy (HAXPES). Results highlight that gallium oxidation at this interface is enhanced when increasing the Al2O3 thickness from 3 up to 20 nm. Gallium oxidation is reduced when using both O3 and H2O as oxidant precursors, compared with only H2O during the growth of Al2O3. In addition, the O3/H2O‐based Al2O3 favors a reduction of contaminants such as hydrogen and carbon but enhances the presence of halides (Cl and F) at this Al2O3/GaN interface.
本文采用飞行时间二次离子质谱法(ToF-SIMS)和硬 X 射线光电子能谱法(HAXPES)研究了下一代氮化镓(GaN)晶体管的 Al2O3/GaN 临界埋藏界面。结果表明,当 Al2O3 的厚度从 3 纳米增加到 20 纳米时,该界面上的镓氧化作用会增强。与 Al2O3 生长过程中仅使用 H2O 相比,同时使用 O3 和 H2O 作为氧化剂前驱体时,镓的氧化作用会减弱。此外,基于 O3/H2O 的 Al2O3 有利于减少氢和碳等污染物,但会增加 Al2O3/GaN 界面的卤化物(Cl- 和 F-)。
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引用次数: 0
Crater radius analysis after dual droplets successive oblique impact on liquid film 双液滴连续斜撞击液膜后的凹坑半径分析
IF 1.7 4区 化学 Q4 CHEMISTRY, PHYSICAL Pub Date : 2024-03-03 DOI: 10.1002/sia.7304
Minle Bao, Denghui Zhao, Luyuan Gong, Yali Guo, Shengqiang Shen
Droplet impact is a common occurrence in nature, agriculture, and industry. The research on the multi‐droplet impact is fundamental to understanding the tangled nature of reality. This paper numerically studies the successive oblique impact of dual droplets on the liquid film by building an effective three‐dimensional model. The leading and trailing droplets are set to pass a certain impact point with the same velocity. The main contribution of this paper is the investigation of the effects of Weber number, liquid film thickness, impact angle, and impact time interval on the interface morphology evolution after the droplet impact. Results show that splash pattern conversion of the primary or secondary crown occurs with the change of these factors. Besides, the variations of the maximum crater radius in upstream, lateral, and downstream directions with time are quantitatively analyzed. The crater radius analysis is carried out from three perspectives, the variation during the single droplet impact, the change during the dual droplets impact, and the comparison between them. It is found that the crater of dual droplets impact exhibits shape distortion in the deformation period and appears a marked dimensional increase in the secondary expansion period.
液滴撞击是自然界、农业和工业中经常发生的现象。对多液滴撞击的研究是理解现实纠结本质的基础。本文通过建立一个有效的三维模型,对双液滴对液膜的连续斜冲击进行了数值研究。设置前导液滴和后导液滴以相同的速度通过某一撞击点。本文的主要贡献在于研究了韦伯数、液膜厚度、撞击角度和撞击时间间隔对液滴撞击后界面形态演变的影响。结果表明,随着这些因素的变化,会发生主冠或次冠的飞溅形态转换。此外,还定量分析了最大弹坑半径在上游、横向和下游方向上随时间的变化。弹坑半径分析从三个角度进行:单液滴撞击时的变化、双液滴撞击时的变化以及它们之间的比较。结果发现,双液滴撞击的陨石坑在变形期表现出形状扭曲,在二次膨胀期出现明显的尺寸增大。
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引用次数: 0
Synthesis, characterization, and performance evaluation of polyamide‐Ag@SiO2 Raman substrate 聚酰胺-Ag@SiO2 拉曼衬底的合成、表征和性能评估
IF 1.7 4区 化学 Q4 CHEMISTRY, PHYSICAL Pub Date : 2024-03-01 DOI: 10.1002/sia.7303
Shiying Wu, Lan Zhang, Tingting Zhang, Lujie Li, Anqi Li, Lingling Wang, Chang Liu, Weihua Li, Jiansheng Li, Rui Lu
At present, Ag nanoparticles have been widely used as Raman substrates, but their easy oxidation and aggregation have limited practical applications. In order to address the above problems, firstly, tetraethyl orthosilicate as a precursor was applied to synthesis silver coated with silica dioxide nanoparticles (Ag@SiO2). As a result, the surface of Ag nanoparticles is uniformly coated with a thin layer of SiO2 in order to solve the easy oxidation problem without adversely affecting their surface‐enhanced Raman scattering (SERS) performance. Furthermore, Ag@SiO2 nanoparticles were electrostatically deposited onto polyamide (PA) films to form a two‐dimensional PA‐Ag@SiO2 film substrate, thus resolving nanoparticle agglomeration issues and further improving the repeatability of the entire system. As can been from the SERS detection results obtained from the probe molecules and pollutants, the Raman signal on the PA‐Ag@SiO2 thin film substrate has a good degree of sensitivity, stability, and repeatability.
目前,银纳米粒子已被广泛用作拉曼基底,但其易氧化和聚集的特性限制了其实际应用。为了解决上述问题,首先以正硅酸四乙酯为前驱体,合成了银包覆二氧化硅纳米粒子(Ag@SiO2)。这样,银纳米粒子的表面就均匀地镀上了一层薄薄的二氧化硅,从而解决了容易氧化的问题,同时又不会对其表面增强拉曼散射(SERS)性能产生不利影响。此外,将 Ag@SiO2 纳米粒子静电沉积到聚酰胺(PA)薄膜上,形成二维 PA-Ag@SiO2 薄膜基底,从而解决了纳米粒子的团聚问题,进一步提高了整个系统的重复性。从探针分子和污染物的 SERS 检测结果可以看出,PA-Ag@SiO2 薄膜基底上的拉曼信号具有良好的灵敏度、稳定性和可重复性。
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引用次数: 0
Quantification of secondary ion mass spectrometry measurements by using ion‐implanted metallic standards 利用离子注入金属标准品对二次离子质谱测量进行定量
IF 1.7 4区 化学 Q4 CHEMISTRY, PHYSICAL Pub Date : 2024-02-29 DOI: 10.1002/sia.7298
Guiomar Delgado Soria, María González, Miguel Luis Crespillo, Jesús Sánchez Prieto, Gastón García
This research addresses an analytical methodology to quantify elements of interest in fusion‐relevant materials using secondary ion mass spectrometry (SIMS). For this purpose, internal standards have been fabricated by ion implantation to avoid the well‐known matrix effect of this technique. In particular, chromium has been implanted at an energy of 12 MeV using two fluences in high‐purity iron and tungsten matrices together with Si control substrates. The latter were applied to determine the Cr concentration implanted through experimental and semiempirical methods. Specifically, the IBA technique Rutherford backscattering spectrometry (RBS) provided the quantitative results being 3.1 × 1019 at/cm3 and 1.6 × 1019 at/cm3 for the high and low dose, respectively. The SIMS depth profiles of Cr for the Fe and W matrices established an ion implantation depth close to 2 μm on both substrates in agreement with the calculations previously performed by Stopping and Range of Ions in Matter (SRIM) simulations. Correlation between the integration of SIMS profiles and known concentrations of the implanted ion resulted in the calibration curve for each matrix, obtaining the SIMS quantification approach by means of this relative sensitivity factor (RSF). Additionally, a cross‐check of the method by comparing commercial Fe‐Cr alloys with the Cr‐implanted Fe matrices of the present study pointed out the need to produce standards with higher chromium concentrations.
本研究采用二次离子质谱(SIMS)分析方法对核聚变相关材料中的相关元素进行定量分析。为此,通过离子注入法制作了内部标准,以避免该技术众所周知的基质效应。其中,铬是以 12 MeV 的能量植入高纯度的铁和钨基质以及硅控制基质中的。后者应用实验和半经验方法确定植入的铬浓度。具体来说,IBA 技术卢瑟福背散射光谱法(RBS)提供了定量结果,高剂量和低剂量分别为 3.1 × 1019 at/cm3 和 1.6 × 1019 at/cm3。铁基质和瓦基质中铬的 SIMS 深度剖面图显示,两种基质上的离子注入深度均接近 2 μm,这与之前通过物质中的离子停止和范围(SRIM)模拟进行的计算结果一致。SIMS 曲线的整合与植入离子的已知浓度之间的相关性导致了每种基质的校准曲线,通过这种相对灵敏度系数(RSF)获得了 SIMS 定量方法。此外,通过将商用铁铬合金与本研究中的铬植入铁基质进行比较,对该方法进行了交叉检验,结果表明需要生产铬浓度更高的标准物质。
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引用次数: 0
Tribological properties of Cetyltrimethyl ammonium bromide modified CS as lubrication additive 十六烷基三甲基溴化铵改性 CS 作为润滑添加剂的摩擦学特性
IF 1.7 4区 化学 Q4 CHEMISTRY, PHYSICAL Pub Date : 2024-02-26 DOI: 10.1002/sia.7297
Jing Li, Tianxia Liu, Jinyu Liu
The coal indirect liquefied diesel soot (Coal-to-liquids diesel soot, CS) was collected by a self-made soot trapper. CS was modified with cetyltrimethyl ammonium bromide (CTAB) and named as CS-CTAB. The tribological properties of CS and CS-CTAB in 10#white oil(10#WO) were tested on a WTM-2E controlled atmosphere miniature friction and wear testing machine. The morphology, composition, and tribological mechanism of CS and modified CS-CTAB were studied by using TEM, XPS, XRD, Raman, and other instruments. The results showed that CS modified by CTAB is wrapped and entangled in long chains. Their main structure components are all amorphous carbon with a small amount of graphite crystallites. The addition of CS-CTAB (0.8 wt%) significantly reduces both AFC and wear rate, with reductions of 32.9% for AFC, and 65.6% for wear rate compared to no additive. The anti-friction and anti-wear effect of CS is greatly improved after being modified by CTAB. Mechanism analysis shows that CS as a lubricant additive, acts as a micro-bearing in the friction process and falls off under the action of shear force to generate an independent graphite sheet, thus forming a graphite protective film on the surface of 304 stainless steel plate. However, CS has the defects of low graphitization degree, large particle size, and easy agglomeration. During friction, uneven adsorption of CS on the surface can worsen wear. However, CTAB modification can improve dispersion stability in 10#WO and effectively reduce wear on the friction surface.
煤间接液化柴油烟尘(Coal-to-liquids diesel soot,CS)由自制的烟尘捕集器收集。用十六烷基三甲基溴化铵(CTAB)对 CS 进行改性,命名为 CS-CTAB。在 WTM-2E 可控气氛微型摩擦磨损试验机上测试了 CS 和 CS-CTAB 在 10#白油(10#WO)中的摩擦学特性。利用 TEM、XPS、XRD、拉曼等仪器研究了 CS 和改性 CS-CTAB 的形貌、成分和摩擦学机理。结果表明,CTAB修饰的CS呈长链状缠绕。其主要结构成分均为无定形碳,并含有少量石墨结晶。添加 CS-CTAB(0.8 wt%)后,AFC 和磨损率均显著降低,与不添加相比,AFC 降低了 32.9%,磨损率降低了 65.6%。经 CTAB 改性后,CS 的抗摩擦和抗磨损效果大大提高。机理分析表明,CS 作为一种润滑添加剂,在摩擦过程中起到微轴承的作用,在剪切力的作用下脱落,生成独立的石墨片,从而在 304 不锈钢板表面形成石墨保护膜。但 CS 存在石墨化程度低、粒度大、易团聚等缺陷。在摩擦过程中,表面对 CS 的不均匀吸附会加剧磨损。然而,CTAB 改性可以提高 CS 在 10#WO 中的分散稳定性,并有效减少摩擦表面的磨损。
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引用次数: 0
Surface analysis insight note: Accounting for X-ray beam damage effects in positive electrode-electrolyte interphase investigations 表面分析见解说明:在正电极-电解质相间研究中考虑 X 射线束损伤效应
IF 1.7 4区 化学 Q4 CHEMISTRY, PHYSICAL Pub Date : 2024-02-20 DOI: 10.1002/sia.7294
Roberto Fantin, Ambroise Van Roekeghem, Jean-Pascal Rueff, Anass Benayad
We investigated the effects of X-ray beam damage during X-ray photoelectron spectroscopy measurement on LiNiO2 electrodes. The degree of damage induced by lab-based and synchrotron X-ray radiation has been compared between pristine and cycled electrodes, highlighting the role of positive solid electrode–electrolyte interphase to protect the cycled LiNiO2 surface from beam damage. The possible steps to avoid or at least reduce the beam-induced effects are outlined.
我们研究了在对 LiNiO2 电极进行 X 射线光电子能谱测量时 X 射线束损伤的影响。比较了原始电极和循环电极在实验室和同步辐射 X 射线辐射下的损伤程度,突出了正固态电极-电解质间相在保护循环 LiNiO2 表面免受光束损伤方面的作用。此外,还概述了避免或至少减少光束诱导效应的可能步骤。
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引用次数: 0
Multiple graphdiyne-like chains self-assemble into carbon nanotubes 多个类石墨二炔链自组装成碳纳米管
IF 1.7 4区 化学 Q4 CHEMISTRY, PHYSICAL Pub Date : 2024-02-16 DOI: 10.1002/sia.7295
Rui Wang, Houbo Yang, Danhui Zhang, Xuemei Sun, Dengbo Zhang, Jianhui Shi, Ruquan Liang, Anmin Liu
The formation process of core–shell structure from multiple graphdiyne-like chains and carbon nanotube is investigated by a molecular dynamics simulation. Multiple graphdiyne-like chains self-curl into helical structures located inside carbon nanotubes. The entire process involves two steps: sliding and twisting. A detailed analysis is conducted on the formation mechanism. Both the van der Waals potential well and the π–π stacking interaction between carbon nanotube and graphdiyne-like chains play a major role in the self-assemble process. Furthermore, the influence factors such as the number of graphdiyne-like chains, the diameter of carbon nanotube, the length of carbon nanotube, the length of graphdiyne-like chains, and the simulation temperature is also investigated. The research results are an important theoretical basis for manufacturing high-quality carbon nanomaterials and other novel nanostructures.
分子动力学模拟研究了由多条类石墨二炔链和碳纳米管形成核壳结构的过程。多条类石墨二炔链在碳纳米管内自卷曲成螺旋结构。整个过程包括两个步骤:滑动和扭曲。我们对形成机制进行了详细分析。在自组装过程中,碳纳米管与类石墨二乙烯链之间的范德华势阱和π-π堆积相互作用都发挥了重要作用。此外,还研究了类石墨二炔链的数量、碳纳米管的直径、碳纳米管的长度、类石墨二炔链的长度以及模拟温度等影响因素。研究成果为制造高质量碳纳米材料和其他新型纳米结构提供了重要的理论依据。
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引用次数: 0
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Surface and Interface Analysis
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