This paper investigates the effect of fiber surface treatment on various properties of hair fiber reinforced composites. Human hair fiber reinforced modified epoxidized soybean oil based composites were prepared by compression molding technique. Acid treatment of hair fibers was carried out by using three different concentrations of HCl solution (0.25%, 0.75%, and 1%, respectively) in order to achieve improvement in adhesion between the fiber and the matrix. Epoxidized soybean oil was modified using methacrylic acid and methacrylic anhydride to form methacrylic anhydride modified epoxidized soybean oil. Rosin acid derivative (a rigid comonomer) was prepared and used as a crosslinker. Fourier‐transform infrared spectroscopy was carried out to study the interaction among the components of the composites. Various properties, namely, mechanical, thermal, flame resistance, and chemical resistance were checked. Scanning electron microscopy of the fractured surface of the composites was carried out to examine the morphologies. Hair fibers treated with 0.75% of HCl showed maximum improvement in all the properties and could be employed as reinforcement in various composites to be used for structural applications.
{"title":"Study on the physicochemical properties of human hair fiber‐reinforced modified epoxidized soybean oil‐based composites","authors":"Gitashree Gogoi, Pragya Banerjee, T. K. Maji","doi":"10.1002/sia.7312","DOIUrl":"https://doi.org/10.1002/sia.7312","url":null,"abstract":"This paper investigates the effect of fiber surface treatment on various properties of hair fiber reinforced composites. Human hair fiber reinforced modified epoxidized soybean oil based composites were prepared by compression molding technique. Acid treatment of hair fibers was carried out by using three different concentrations of HCl solution (0.25%, 0.75%, and 1%, respectively) in order to achieve improvement in adhesion between the fiber and the matrix. Epoxidized soybean oil was modified using methacrylic acid and methacrylic anhydride to form methacrylic anhydride modified epoxidized soybean oil. Rosin acid derivative (a rigid comonomer) was prepared and used as a crosslinker. Fourier‐transform infrared spectroscopy was carried out to study the interaction among the components of the composites. Various properties, namely, mechanical, thermal, flame resistance, and chemical resistance were checked. Scanning electron microscopy of the fractured surface of the composites was carried out to examine the morphologies. Hair fibers treated with 0.75% of HCl showed maximum improvement in all the properties and could be employed as reinforcement in various composites to be used for structural applications.","PeriodicalId":22062,"journal":{"name":"Surface and Interface Analysis","volume":null,"pages":null},"PeriodicalIF":1.7,"publicationDate":"2024-04-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140672955","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Marine biofouling poses a major challenge to ship navigation and hinders the development of the shipping industry. Urgent action is required to tackle this problem through the implementation of innovative strategies. Antimicrobial peptides have garnered considerable attention due to their outstanding effectiveness, wide range of activity, and eco-friendly characteristics. This study involved grafting the antibacterial peptide andricin 01 (AIGHCLGATL) onto the surface of an aluminum alloy, thereby creating a modified surface with antibacterial properties. In summary, amino groups were introduced onto the surface of aluminum alloys through the silanization process using (3-aminopropyl) triethoxysilane (APTES), and then the peptides were covalently immobilized on the treated surface using glutaraldehyde as a cross-linking agent. The successful modification of the peptide was confirmed by Fourier transform-infrared spectroscopy (FT-IR) and X-ray photoelectron spectroscopy (XPS) analysis. The antimicrobial peptide-modified aluminum alloy surfaces exhibited significant bactericidal activity, killing 75.3% of Bacillus sp. and 85.5% of Escherichia coli, while achieving antifouling efficiencies of 88.6% and 90.7% against Bacillus sp. and E. coli, respectively. Furthermore, molecular dynamics simulations showed that the inserted of the peptides into the phospholipid membrane caused a change in the local membrane curvature, which eventually led to membrane rupture. These results provide valuable information for the application of antimicrobial peptides in the field of antifouling and the elucidation of antifouling mechanisms.
{"title":"Experimental and molecular dynamics simulation study on antifouling performance of antimicrobial peptide-modified aluminum alloy surfaces","authors":"Wencheng Liu, Tong Lou, Xiuqin Bai, Xiaoyan He, Chengqing Yuan","doi":"10.1002/sia.7311","DOIUrl":"https://doi.org/10.1002/sia.7311","url":null,"abstract":"Marine biofouling poses a major challenge to ship navigation and hinders the development of the shipping industry. Urgent action is required to tackle this problem through the implementation of innovative strategies. Antimicrobial peptides have garnered considerable attention due to their outstanding effectiveness, wide range of activity, and eco-friendly characteristics. This study involved grafting the antibacterial peptide <i>andricin 01</i> (AIGHCLGATL) onto the surface of an aluminum alloy, thereby creating a modified surface with antibacterial properties. In summary, amino groups were introduced onto the surface of aluminum alloys through the silanization process using (3-aminopropyl) triethoxysilane (APTES), and then the peptides were covalently immobilized on the treated surface using glutaraldehyde as a cross-linking agent. The successful modification of the peptide was confirmed by Fourier transform-infrared spectroscopy (FT-IR) and X-ray photoelectron spectroscopy (XPS) analysis. The antimicrobial peptide-modified aluminum alloy surfaces exhibited significant bactericidal activity, killing 75.3% of <i>Bacillus</i> sp. and 85.5% of <i>Escherichia coli</i>, while achieving antifouling efficiencies of 88.6% and 90.7% against <i>Bacillus</i> sp. and <i>E. coli</i>, respectively. Furthermore, molecular dynamics simulations showed that the inserted of the peptides into the phospholipid membrane caused a change in the local membrane curvature, which eventually led to membrane rupture. These results provide valuable information for the application of antimicrobial peptides in the field of antifouling and the elucidation of antifouling mechanisms.","PeriodicalId":22062,"journal":{"name":"Surface and Interface Analysis","volume":null,"pages":null},"PeriodicalIF":1.7,"publicationDate":"2024-04-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140588307","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Beatriz Mendoza‐Sánchez, Vincent Fernandez, Pascal Bargiela, Neal Fairley, Jonas Baltrusaitis
Strategies to deal with sample charging effects on X‐ray photoelectron spectroscopy (XPS) spectra are presented. These strategies combine charge compensation (or lack of) via a flow of electrons and an electrical connection (or lack of) of samples to the ground. Practical examples involving samples with a range of different electrical properties, sample structure/composition and sensitivity to X‐rays, illustrate the correlation between sample properties, measurement strategies, and the resulting XPS data. The most appropriate measurement strategy for a particular sample is also recommended. We highlight the crucial importance of appropriate XPS data acquisition to obtain a correct data interpretation.
本文介绍了处理样品充电对 X 射线光电子能谱 (XPS) 光谱影响的策略。这些策略结合了通过电子流和样品与地面的电连接（或不连接）进行电荷补偿（或缺乏电荷补偿）的方法。实际示例涉及一系列具有不同电特性、样品结构/组成和对 X 射线敏感性的样品，说明了样品特性、测量策略和所得 XPS 数据之间的相互关系。此外，还推荐了最适合特定样品的测量策略。我们强调了适当的 XPS 数据采集对于获得正确的数据解释的重要性。
{"title":"Surface science insight note: Charge compensation and charge correction in X‐ray photoelectron spectroscopy","authors":"Beatriz Mendoza‐Sánchez, Vincent Fernandez, Pascal Bargiela, Neal Fairley, Jonas Baltrusaitis","doi":"10.1002/sia.7309","DOIUrl":"https://doi.org/10.1002/sia.7309","url":null,"abstract":"Strategies to deal with sample charging effects on X‐ray photoelectron spectroscopy (XPS) spectra are presented. These strategies combine charge compensation (or lack of) via a flow of electrons and an electrical connection (or lack of) of samples to the ground. Practical examples involving samples with a range of different electrical properties, sample structure/composition and sensitivity to X‐rays, illustrate the correlation between sample properties, measurement strategies, and the resulting XPS data. The most appropriate measurement strategy for a particular sample is also recommended. We highlight the crucial importance of appropriate XPS data acquisition to obtain a correct data interpretation.","PeriodicalId":22062,"journal":{"name":"Surface and Interface Analysis","volume":null,"pages":null},"PeriodicalIF":1.7,"publicationDate":"2024-04-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140588375","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Alloying elements segregating to grain boundaries (GBs) is vital in determining structural stability and mechanical properties of alloys, especially in high‐entropy alloys (HEAs) that consist of multiple elements. However, some details remain unclear, such as the process of varied atoms (Cr and Co) cosegregation to GBs in FeNiCrCo alloy. Therefore, the competition and cooperation between Fe, Ni, Cr, and Co atoms segregating to GBs of FeNiCrCo alloy were investigated via molecular dynamic (MD) simulation. Five [110] symmetric tilt GBs of FeNiCrCo were applied to study the relation between the tendency of atomic segregation especially Cr and Co and GB characters including GB energy and GB excess free volume (GB excess volume). A competitive segregation phenomenon between Cr and Co atoms was discovered, which could be dominated by GB excess volume and different atomic radii among components.
{"title":"Competitive segregation to grain boundaries between Cr and Co in FeNiCrCo alloy","authors":"Weiwei Zhang, Li Huang, Jing Liang, Yanchao Li, Wei Bai, Benqi Jiao, Dongxiao Kan, Jianfeng Li, Wen Zhang","doi":"10.1002/sia.7307","DOIUrl":"https://doi.org/10.1002/sia.7307","url":null,"abstract":"Alloying elements segregating to grain boundaries (GBs) is vital in determining structural stability and mechanical properties of alloys, especially in high‐entropy alloys (HEAs) that consist of multiple elements. However, some details remain unclear, such as the process of varied atoms (Cr and Co) cosegregation to GBs in FeNiCrCo alloy. Therefore, the competition and cooperation between Fe, Ni, Cr, and Co atoms segregating to GBs of FeNiCrCo alloy were investigated via molecular dynamic (MD) simulation. Five [110] symmetric tilt GBs of FeNiCrCo were applied to study the relation between the tendency of atomic segregation especially Cr and Co and GB characters including GB energy and GB excess free volume (GB excess volume). A competitive segregation phenomenon between Cr and Co atoms was discovered, which could be dominated by GB excess volume and different atomic radii among components.","PeriodicalId":22062,"journal":{"name":"Surface and Interface Analysis","volume":null,"pages":null},"PeriodicalIF":1.7,"publicationDate":"2024-04-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140588498","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Weijie Yu, Qiuping Mei, Weijiu Huang, Junjun Wang, Yongyao Su
The poor high‐temperature tribological performance of diamond‐like carbon (DLC) films severely limits their applications. To address this issue, silicon (Si) doped DLC films with Si content ranging from 0 to 11.52 at.% were synthesized utilizing the plasma‐assisted reactive magnetron sputtering technique. The influence of Si incorporation on the microstructure and mechanical properties was meticulously investigated by Raman spectroscopy, scanning electron microscope (SEM), X‐ray photoelectron spectroscopy (XPS), nanoindentation, and scratch testing. To ascertain the tribological behavior of the Si‐DLC films under elevated temperature conditions, in situ high‐temperature tests were conducted, spanning temperatures from ambient to 500°C. The findings indicated that distinct lubrication mechanisms prevail for Si‐DLC films with varying Si content across different temperature domains. As the test temperature and Si content increased, the lubrication mechanism exhibited a gradual transitions from high‐temperature induced graphitization to a particle wear regime dominated by SiC and formed SiO2 abrasive phases. The comprehensive performance of the films peaked at a Si content of 4.72 at.%, suggesting an optimal composition for high‐temperature applications. It is postulated that the in‐depth investigation presented herein holds considerable value for the design and fabrication of DLC films intended for use in high‐temperature settings, potentially unlocking their full potential in such demanding environments.
{"title":"Tailoring the mechanical and high‐temperature tribological properties of Si‐DLC films by controlling the Si content","authors":"Weijie Yu, Qiuping Mei, Weijiu Huang, Junjun Wang, Yongyao Su","doi":"10.1002/sia.7308","DOIUrl":"https://doi.org/10.1002/sia.7308","url":null,"abstract":"The poor high‐temperature tribological performance of diamond‐like carbon (DLC) films severely limits their applications. To address this issue, silicon (Si) doped DLC films with Si content ranging from 0 to 11.52 at.% were synthesized utilizing the plasma‐assisted reactive magnetron sputtering technique. The influence of Si incorporation on the microstructure and mechanical properties was meticulously investigated by Raman spectroscopy, scanning electron microscope (SEM), X‐ray photoelectron spectroscopy (XPS), nanoindentation, and scratch testing. To ascertain the tribological behavior of the Si‐DLC films under elevated temperature conditions, in situ high‐temperature tests were conducted, spanning temperatures from ambient to 500°C. The findings indicated that distinct lubrication mechanisms prevail for Si‐DLC films with varying Si content across different temperature domains. As the test temperature and Si content increased, the lubrication mechanism exhibited a gradual transitions from high‐temperature induced graphitization to a particle wear regime dominated by SiC and formed SiO<jats:sub>2</jats:sub> abrasive phases. The comprehensive performance of the films peaked at a Si content of 4.72 at.%, suggesting an optimal composition for high‐temperature applications. It is postulated that the in‐depth investigation presented herein holds considerable value for the design and fabrication of DLC films intended for use in high‐temperature settings, potentially unlocking their full potential in such demanding environments.","PeriodicalId":22062,"journal":{"name":"Surface and Interface Analysis","volume":null,"pages":null},"PeriodicalIF":1.7,"publicationDate":"2024-04-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140588501","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Chromium‐based coatings have been of interest to researchers for the last two decades because of their extraordinary properties like high hardness, high wear, and corrosion resistance properties. However, it is in practice and research to increase the properties of Cr‐based coatings for high‐temperature applications. Numerous dopants like silicon (Si), titanium (Ti), vanadium (V), aluminum (Al), and zirconium (Zr) have been used together with Cr to achieve enhanced properties. The plasma‐based sputtering process is one of the popular and reliable techniques to deposit thin film coatings. The substrate material, processed gas and pressure, substrate temperature, film thickness, and so on also play a significant role in varying the properties and microstructure of the deposited film. Several researchers have deposited Cr/CrN‐based thin films via the chemical vapor deposition technique (CVD) and physical vapor deposition technique (PVD) to study their properties and behavior at room temperature as well as for high‐temperature applications. This work reflects the review of work done to deposit Cr/CrN‐based coatings deposited via PVD: more specifically sputtering technique. The effect of doping in the CrN matrix and variation in sputtering parameters on the properties of CrN‐based coatings have also been studied.
{"title":"The effect of sputtering parameters and doping on the properties of CrN‐based coatings—A critical review","authors":"Sunil Kumar Tiwari, Akula Umamaheswara Rao, Archana Singh Kharb, Devesh Kumar Avasthi, Piyush Chandra Verma, Amit Kumar Chawla","doi":"10.1002/sia.7306","DOIUrl":"https://doi.org/10.1002/sia.7306","url":null,"abstract":"Chromium‐based coatings have been of interest to researchers for the last two decades because of their extraordinary properties like high hardness, high wear, and corrosion resistance properties. However, it is in practice and research to increase the properties of Cr‐based coatings for high‐temperature applications. Numerous dopants like silicon (Si), titanium (Ti), vanadium (V), aluminum (Al), and zirconium (Zr) have been used together with Cr to achieve enhanced properties. The plasma‐based sputtering process is one of the popular and reliable techniques to deposit thin film coatings. The substrate material, processed gas and pressure, substrate temperature, film thickness, and so on also play a significant role in varying the properties and microstructure of the deposited film. Several researchers have deposited Cr/CrN‐based thin films via the chemical vapor deposition technique (CVD) and physical vapor deposition technique (PVD) to study their properties and behavior at room temperature as well as for high‐temperature applications. This work reflects the review of work done to deposit Cr/CrN‐based coatings deposited via PVD: more specifically sputtering technique. The effect of doping in the CrN matrix and variation in sputtering parameters on the properties of CrN‐based coatings have also been studied.","PeriodicalId":22062,"journal":{"name":"Surface and Interface Analysis","volume":null,"pages":null},"PeriodicalIF":1.7,"publicationDate":"2024-03-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140323001","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Vincent Fernandez, Olivier Renault, Neal Fairley, Jonas Baltrusaitis
X‐ray photoelectron spectroscopy (XPS) provides quantitative information from photoemission peaks and shapes observed within the background due to the inelastic scattering of photoelectrons. To quantify the signal, both photoemission peaks and background in spectra must be adjusted for instrumental transmission variations that are a consequence of changes in efficiency when recording electrons with different kinetic energy. While it is generally assumed that correcting spectroscopic data for transmission is a necessary part of quantification by XPS, there are consequences for the quantification of spectra measured using an instrument for which transmission has significant curvature. In this Insight, the implications of curvature in transmission characteristics are discussed and a method based on XPS microscopy is proposed that ensures the transmission response of an instrument is free from significant curvature. An example of an instrument for which a flat transmission response is presented is achieved through collecting spectra using lens modes designed to measure stigmatic images.
X 射线光电子能谱（XPS）可从光电子非弹性散射造成的背景中观察到的光发射峰和形状提供定量信息。为了量化信号，必须对光谱中的光发射峰和背景进行调整，以适应仪器透射率的变化，这是记录不同动能电子时效率变化的结果。虽然人们普遍认为根据透射率校正光谱数据是 XPS 定量的必要部分，但使用透射率具有明显曲率的仪器测量光谱时，会产生一些量化后果。在本《洞察》中，讨论了透射特性中曲率的影响，并提出了一种基于 XPS 显微镜的方法，以确保仪器的透射响应没有明显的曲率。通过使用设计用于测量残像的透镜模式收集光谱，介绍了一个实现平坦透射响应的仪器示例。
{"title":"Surface science insight note: Optimizing XPS instrument performance for quantification of spectra","authors":"Vincent Fernandez, Olivier Renault, Neal Fairley, Jonas Baltrusaitis","doi":"10.1002/sia.7296","DOIUrl":"https://doi.org/10.1002/sia.7296","url":null,"abstract":"X‐ray photoelectron spectroscopy (XPS) provides quantitative information from photoemission peaks and shapes observed within the background due to the inelastic scattering of photoelectrons. To quantify the signal, both photoemission peaks and background in spectra must be adjusted for instrumental transmission variations that are a consequence of changes in efficiency when recording electrons with different kinetic energy. While it is generally assumed that correcting spectroscopic data for transmission is a necessary part of quantification by XPS, there are consequences for the quantification of spectra measured using an instrument for which transmission has significant curvature. In this <jats:italic>Insight</jats:italic>, the implications of curvature in transmission characteristics are discussed and a method based on XPS microscopy is proposed that ensures the transmission response of an instrument is free from significant curvature. An example of an instrument for which a flat transmission response is presented is achieved through collecting spectra using lens modes designed to measure stigmatic images.","PeriodicalId":22062,"journal":{"name":"Surface and Interface Analysis","volume":null,"pages":null},"PeriodicalIF":1.7,"publicationDate":"2024-03-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140147268","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
In recent years, instrument manufacturers have been providing laboratory-based HAXPES (hard X-ray photoelectron spectroscopy) instruments that have monochromated silver Lα, chromium Kα and gallium Kα X-ray sources. To be more than a qualitative tool, two things are required: calibration of the signal intensity as a function of kinetic energy (spectrometer response function) and relative sensitivity factors. This is now possible because of routines being available to generate the spectrometer response functions for dual Al Kα/Ag Lα X-ray sources and the availability of Cant average matrix relative sensitivity factors (AMRSFs). However, to improve accuracy when using the Cant AMRSF care needs to be taken in the definition of the peak areas being used. This is because they need to include the total intrinsic signal that often extends beyond the main peak. This is a particular challenge when quantifying using the Al 1s peak generated with Ag Lα X-rays as some of the intrinsic signal overlaps with the Al KLL Auger peak. When materials include both aluminium and silicon atoms, the Si 2s and 2p peaks sit upon extended signals coming from the Al 2s and 2s peaks, respectively. Thus, quantification should be limited to using the main peak area, which necessitates different relative sensitivity factors (RSFs). Using polydimethylsiloxane (PDMS) and sapphire (Al2O3) as model systems, experimental RSFs have been determined for use with the main peaks for O 1s, Al 1s, Al2s Al 2p, Si 1s, Si 2s and Si 2p subshells normalized to the RSF of the carbon 1s main peak.
近年来，仪器制造商一直在提供基于实验室的 HAXPES（硬 X 射线光电子能谱）仪器，这些仪器具有单色银 Lα、铬 Kα 和镓 Kα X 射线源。要使其不仅仅是一种定性工具，还需要两方面的条件：校准作为动能函数的信号强度（光谱仪响应函数）和相对灵敏度系数。由于有了可生成 Al Kα/Ag Lα 双 X 射线源光谱仪响应函数的例程，以及 Cant 平均矩阵相对灵敏度系数（AMRSF）的可用性，现在校准已经成为可能。不过，为了提高使用 Cant AMRSF 时的准确性，在定义使用的峰面积时需要注意。这是因为它们需要包括通常超出主峰范围的总内在信号。在使用 Ag Lα X 射线产生的 Al 1s 峰进行量化时，这是一个特殊的挑战，因为部分本征信号与 Al KLL 奥杰峰重叠。当材料同时包含铝原子和硅原子时，硅 2s 峰和 2p 峰分别位于来自铝 2s 峰和 2s 峰的扩展信号上。因此，定量应仅限于使用主峰面积，这就需要使用不同的相对灵敏度系数（RSF）。以聚二甲基硅氧烷 (PDMS) 和蓝宝石 (Al2O3) 为模型系统，确定了用于 O 1s、Al 1s、Al 2s、Al 2p、Si 1s、Si 2s 和 Si 2p 子壳主峰的实验 RSF，并将其归一化为碳 1s 主峰的 RSF。
{"title":"Quantification of aluminium and silicon-containing materials using Ag Lα X-rays","authors":"Stuart R. Leadley","doi":"10.1002/sia.7301","DOIUrl":"https://doi.org/10.1002/sia.7301","url":null,"abstract":"In recent years, instrument manufacturers have been providing laboratory-based HAXPES (hard X-ray photoelectron spectroscopy) instruments that have monochromated silver Lα, chromium Kα and gallium Kα X-ray sources. To be more than a qualitative tool, two things are required: calibration of the signal intensity as a function of kinetic energy (spectrometer response function) and relative sensitivity factors. This is now possible because of routines being available to generate the spectrometer response functions for dual Al Kα/Ag Lα X-ray sources and the availability of Cant average matrix relative sensitivity factors (AMRSFs). However, to improve accuracy when using the Cant AMRSF care needs to be taken in the definition of the peak areas being used. This is because they need to include the total <i>intrinsic</i> signal that often extends beyond the main peak. This is a particular challenge when quantifying using the Al 1s peak generated with Ag Lα X-rays as some of the <i>intrinsic</i> signal overlaps with the Al KLL Auger peak. When materials include both aluminium and silicon atoms, the Si 2s and 2p peaks sit upon extended signals coming from the Al 2s and 2s peaks, respectively. Thus, quantification should be limited to using the main peak area, which necessitates different relative sensitivity factors (RSFs). Using polydimethylsiloxane (PDMS) and sapphire (Al<sub>2</sub>O<sub>3</sub>) as model systems, experimental RSFs have been determined for use with the main peaks for O 1s, Al 1s, Al2s Al 2p, Si 1s, Si 2s and Si 2p subshells normalized to the RSF of the carbon 1s main peak.","PeriodicalId":22062,"journal":{"name":"Surface and Interface Analysis","volume":null,"pages":null},"PeriodicalIF":1.7,"publicationDate":"2024-03-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140147305","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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.
{"title":"The development of laboratory‐based high energy sources for XPS","authors":"John F. Watts, James E. Castle","doi":"10.1002/sia.7300","DOIUrl":"https://doi.org/10.1002/sia.7300","url":null,"abstract":"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 Fe<jats:italic>KLL</jats:italic> 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.","PeriodicalId":22062,"journal":{"name":"Surface and Interface Analysis","volume":null,"pages":null},"PeriodicalIF":1.7,"publicationDate":"2024-03-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140147267","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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.
{"title":"Challenges in quantifying Pt concentrations in Pd alloys by using secondary ion mass spectrometry: Strong grain orientation effects","authors":"Børge Holme, Silje Fosse Håkonsen, David Waller","doi":"10.1002/sia.7302","DOIUrl":"https://doi.org/10.1002/sia.7302","url":null,"abstract":"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.","PeriodicalId":22062,"journal":{"name":"Surface and Interface Analysis","volume":null,"pages":null},"PeriodicalIF":1.7,"publicationDate":"2024-03-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140147298","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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