The corrosion of carbon steel is always a very serious issue, and the addition of corrosion inhibitors is an effective approach to prohibiting the corrosion of carbon steel. Because expired drugs are environmentally friendly, green, and non‐toxic; thus, this work provides a new idea for the treatment of expired drugs. The expired flunarizine hydrochloride (FH) is used as corrosion inhibitors for Q235 steel, investigating the corrosion inhibition efficiency of expired FH with different concentrations for carbon steel and illustrating the corrosion inhibition mechanism. Electrochemical impedance and Tafel curves are used to investigate the corrosion inhibition of carbon steel under 1 M HCl solution with different concentrations of the expired FH, and the corrosion efficiency is calculated according to the immersion tests, and the corrosion inhibition efficiency is more than 88.5%. Scanning electron microscopy (SEM), Fourier transform infrared spectrometer (FTIR), and Raman spectroscopy strongly support the results of the electrochemical experiment. Besides, the simulation results also provide the strong supports for the experimental results.
碳钢的腐蚀一直是一个非常严重的问题，添加缓蚀剂是抑制碳钢腐蚀的有效方法。因为过期药品是环保的、绿色的、无毒的；因此，这项工作为过期药品的治疗提供了新的思路。采用过期盐酸氟桂利嗪（FH）作为Q235钢的缓蚀剂，研究了不同浓度过期FH对碳钢的缓蚀效果，阐明了其缓蚀机理。用电化学阻抗和Tafel曲线研究了碳钢在1 M HCl溶液中不同浓度的失效FH，并根据浸泡试验计算腐蚀效率，缓蚀效率超过88.5%。扫描电子显微镜（SEM）、傅立叶变换红外光谱仪（FTIR）和拉曼光谱有力地支持了电化学实验的结果。仿真结果也为实验结果提供了有力的支持。
{"title":"Expired flunarizine hydrochloride as corrosion inhibitors for Q235 steel in hydrochloric acid medium: Experimental and computational investigation","authors":"Qiangwen Lin, Qiao Zhang, Yongbiao Huang, Yuzhou Luo, Renhui Zhang, Lei Guo","doi":"10.1002/sia.7245","DOIUrl":"https://doi.org/10.1002/sia.7245","url":null,"abstract":"The corrosion of carbon steel is always a very serious issue, and the addition of corrosion inhibitors is an effective approach to prohibiting the corrosion of carbon steel. Because expired drugs are environmentally friendly, green, and non‐toxic; thus, this work provides a new idea for the treatment of expired drugs. The expired flunarizine hydrochloride (FH) is used as corrosion inhibitors for Q235 steel, investigating the corrosion inhibition efficiency of expired FH with different concentrations for carbon steel and illustrating the corrosion inhibition mechanism. Electrochemical impedance and Tafel curves are used to investigate the corrosion inhibition of carbon steel under 1 M HCl solution with different concentrations of the expired FH, and the corrosion efficiency is calculated according to the immersion tests, and the corrosion inhibition efficiency is more than 88.5%. Scanning electron microscopy (SEM), Fourier transform infrared spectrometer (FTIR), and Raman spectroscopy strongly support the results of the electrochemical experiment. Besides, the simulation results also provide the strong supports for the experimental results.","PeriodicalId":22062,"journal":{"name":"Surface and Interface Analysis","volume":"55 1","pages":"774 - 786"},"PeriodicalIF":1.7,"publicationDate":"2023-06-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"48781433","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}
Xingguo Feng, Y. Zheng, Keliang Wang, Y. Zheng, Yanshuai Zhang, Hui Zhou
Diamond‐like carbon (DLC) films are prepared by pulsed laser‐induced cathodic vacuum arc technique with various arc voltages. The purpose of the research is to investigate the influence of the arc voltage on the structure, mechanical, and tribological properties of DLC films. The results from Raman spectra and XPS show that with increasing arc voltage from 180 to 280 V, the sp3 content in the DLC film increases from 43.2 to 56.9 at%, then follows by a significant decrease with further increasing arc voltage to 330 V. The trend in the mechanical properties of DLC films correlates well with the sp3 content in the films. The maximum hardness, modulus, and adhesion critical load (Lc) of the DLC film is obtained in the film deposited at 280 V; the values of that are 46.4 GPa, 380.6 GPa, and 620 mN, respectively. The friction coefficient of the films is between 0.1 and 0.2, and the film deposited at 280 V has the minimum wear rate with a value of 3.2 × 10−17 m3/m.N. It is concluded that the DLC films with high sp3 content (ta‐C, tetrahedral amorphous carbon) not only have good mechanical properties but also have excellent tribological properties, which provides a promising application for wear resistance parts.
{"title":"Structure and mechanical properties of diamond‐like carbon films prepared by pulsed laser‐induced cathodic vacuum arc technique","authors":"Xingguo Feng, Y. Zheng, Keliang Wang, Y. Zheng, Yanshuai Zhang, Hui Zhou","doi":"10.1002/sia.7244","DOIUrl":"https://doi.org/10.1002/sia.7244","url":null,"abstract":"Diamond‐like carbon (DLC) films are prepared by pulsed laser‐induced cathodic vacuum arc technique with various arc voltages. The purpose of the research is to investigate the influence of the arc voltage on the structure, mechanical, and tribological properties of DLC films. The results from Raman spectra and XPS show that with increasing arc voltage from 180 to 280 V, the sp3 content in the DLC film increases from 43.2 to 56.9 at%, then follows by a significant decrease with further increasing arc voltage to 330 V. The trend in the mechanical properties of DLC films correlates well with the sp3 content in the films. The maximum hardness, modulus, and adhesion critical load (Lc) of the DLC film is obtained in the film deposited at 280 V; the values of that are 46.4 GPa, 380.6 GPa, and 620 mN, respectively. The friction coefficient of the films is between 0.1 and 0.2, and the film deposited at 280 V has the minimum wear rate with a value of 3.2 × 10−17 m3/m.N. It is concluded that the DLC films with high sp3 content (ta‐C, tetrahedral amorphous carbon) not only have good mechanical properties but also have excellent tribological properties, which provides a promising application for wear resistance parts.","PeriodicalId":22062,"journal":{"name":"Surface and Interface Analysis","volume":"55 1","pages":"763 - 773"},"PeriodicalIF":1.7,"publicationDate":"2023-06-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43315807","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}
Zhiqiang Cheng, Xiaoli Wei, Kaixiong Gao, Chunyan Li
Although diamond‐like carbon (DLC) films are known for their low friction and wear properties in atmospheric environments, they commonly experience failure in vacuum environments. On the other hand, MoS2 exhibits a low friction coefficient under vacuum conditions, but its columnar structure limits its load‐bearing capacity and results in high wear rates. In this study, we prepared MoS2/DLC multilayer films using a high‐power impulse magnetron sputtering (HIPIMS) technique and examined the composition, bonding structure, mechanical properties, and frictional wear of the resulting films. The study findings revealed that the multilayer film exhibits a significantly low coefficient of friction (0.04), particularly in vacuum conditions (5 × 10−3 Pa). Remarkably, compared to the pure MoS2 film, the wear rate of the multilayer film is reduced by two orders of magnitude, wear rate as low as 3.6 × 10−9 mm3/Nm. Additionally, the DLC component enhances the hardness and reduces the wear rate of the multilayer film. Furthermore, the use of nanometer thickness (17 nm) allows for the incorporation of more MoS2 and DLC layers, which promotes the formation of graphene bands and further reduces the friction coefficient and wear rate. Our findings open new avenues for the application of MoS2 and DLC in vacuum environments.
{"title":"Molybdenum disulfide/carbon multilayer films achieve ultra‐low wear in vacuum","authors":"Zhiqiang Cheng, Xiaoli Wei, Kaixiong Gao, Chunyan Li","doi":"10.1002/sia.7241","DOIUrl":"https://doi.org/10.1002/sia.7241","url":null,"abstract":"Although diamond‐like carbon (DLC) films are known for their low friction and wear properties in atmospheric environments, they commonly experience failure in vacuum environments. On the other hand, MoS2 exhibits a low friction coefficient under vacuum conditions, but its columnar structure limits its load‐bearing capacity and results in high wear rates. In this study, we prepared MoS2/DLC multilayer films using a high‐power impulse magnetron sputtering (HIPIMS) technique and examined the composition, bonding structure, mechanical properties, and frictional wear of the resulting films. The study findings revealed that the multilayer film exhibits a significantly low coefficient of friction (0.04), particularly in vacuum conditions (5 × 10−3 Pa). Remarkably, compared to the pure MoS2 film, the wear rate of the multilayer film is reduced by two orders of magnitude, wear rate as low as 3.6 × 10−9 mm3/Nm. Additionally, the DLC component enhances the hardness and reduces the wear rate of the multilayer film. Furthermore, the use of nanometer thickness (17 nm) allows for the incorporation of more MoS2 and DLC layers, which promotes the formation of graphene bands and further reduces the friction coefficient and wear rate. Our findings open new avenues for the application of MoS2 and DLC in vacuum environments.","PeriodicalId":22062,"journal":{"name":"Surface and Interface Analysis","volume":"55 1","pages":"730 - 739"},"PeriodicalIF":1.7,"publicationDate":"2023-06-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43480008","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}
A. Biganeh, H. Rafi‐Kheiri, Mojtaba Badri, T. Kakavand, Alireza Jokar
Measuring hydrogen concentration and determining its depth profile in different substrates has always been a major challenge for material science. Proton–proton scattering is a nondestructive technique for hydrogen analysis in thin samples. In this paper, the development of a 2D coincidence proton–proton spectroscopy was performed using a 3 MeV Van de Graaff accelerator. In the presented technique, the coincidence recording of the proton–proton scattering events by a waveform digitizer provides the sum‐difference energy spectrum of the correlated events. By determining the proton energy loss in the sample, the hydrogen depth profile was extracted. To correct the error in the counting efficiency due to the multiple scattering, the Monte Carlo simulation was performed using the Corteo code. The performance of the technique was tested by measuring the concentration of hydrogen on both sides of a thin layer of aluminum. The results confirmed that the established technique is sensitive enough to separate the hydrogen peaks of these two thin layers.
{"title":"Development of a 2D digital proton–proton scattering technique for hydrogen depth profiling","authors":"A. Biganeh, H. Rafi‐Kheiri, Mojtaba Badri, T. Kakavand, Alireza Jokar","doi":"10.1002/sia.7242","DOIUrl":"https://doi.org/10.1002/sia.7242","url":null,"abstract":"Measuring hydrogen concentration and determining its depth profile in different substrates has always been a major challenge for material science. Proton–proton scattering is a nondestructive technique for hydrogen analysis in thin samples. In this paper, the development of a 2D coincidence proton–proton spectroscopy was performed using a 3 MeV Van de Graaff accelerator. In the presented technique, the coincidence recording of the proton–proton scattering events by a waveform digitizer provides the sum‐difference energy spectrum of the correlated events. By determining the proton energy loss in the sample, the hydrogen depth profile was extracted. To correct the error in the counting efficiency due to the multiple scattering, the Monte Carlo simulation was performed using the Corteo code. The performance of the technique was tested by measuring the concentration of hydrogen on both sides of a thin layer of aluminum. The results confirmed that the established technique is sensitive enough to separate the hydrogen peaks of these two thin layers.","PeriodicalId":22062,"journal":{"name":"Surface and Interface Analysis","volume":"55 1","pages":"740 - 748"},"PeriodicalIF":1.7,"publicationDate":"2023-06-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"42705007","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}
{"title":"Issue Information","authors":"","doi":"10.1002/sia.7220","DOIUrl":"https://doi.org/10.1002/sia.7220","url":null,"abstract":"No abstract is available for this article.","PeriodicalId":22062,"journal":{"name":"Surface and Interface Analysis","volume":" ","pages":""},"PeriodicalIF":1.7,"publicationDate":"2023-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46238502","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}
Angle‐resolved X‐ray photoelectron spectroscopy (ARXPS) is a technique used for depth‐dependent analysis in the near‐surface region of samples. Calculation of a concentration depth profile using ARXPS requires an inverse Laplace transform, which adds considerable complexity to the analysis. In this insight note, the Tikhonov regularization algorithm for depth profile reconstruction from ARXPS data is examined. The steps required to produce a concentration depth profile are provided. The discussion includes strategies that deal with elastic scattering, electron attenuation, choice of regularization terms and optimization of the regularization parameters. The method is implemented in a Microsoft Excel spreadsheet that allows users to calculate a depth profile for data collected at up to five angles for five different peak components.
{"title":"Surface analysis insight note: Straightforward concentration depth profiling by angle‐resolved X‐ray photoelectron spectroscopy using a Tikhonov regularization algorithm","authors":"B. Murdoch, D. McCulloch","doi":"10.1002/sia.7240","DOIUrl":"https://doi.org/10.1002/sia.7240","url":null,"abstract":"Angle‐resolved X‐ray photoelectron spectroscopy (ARXPS) is a technique used for depth‐dependent analysis in the near‐surface region of samples. Calculation of a concentration depth profile using ARXPS requires an inverse Laplace transform, which adds considerable complexity to the analysis. In this insight note, the Tikhonov regularization algorithm for depth profile reconstruction from ARXPS data is examined. The steps required to produce a concentration depth profile are provided. The discussion includes strategies that deal with elastic scattering, electron attenuation, choice of regularization terms and optimization of the regularization parameters. The method is implemented in a Microsoft Excel spreadsheet that allows users to calculate a depth profile for data collected at up to five angles for five different peak components.","PeriodicalId":22062,"journal":{"name":"Surface and Interface Analysis","volume":"55 1","pages":"658 - 664"},"PeriodicalIF":1.7,"publicationDate":"2023-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"44961428","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}
M. Zakir, T. Laiho, S. Granroth, E. Kukk, C. Chu, J. Tsoi, J. Matinlinna
The presence of Si on the Ti surface is quintessential for a strong, durable silane‐based adhesion utilized in several dental applications. Silica‐coating and silanization form durable ≡Si‐O‐Si≡ bonds, which might have a positive effect on resin‐Ti adhesion. This laboratory study studied the effect of strong acids, their blends, and silica‐coating on Ti and resin‐Ti bonding. One‐hundred sixty‐eight c.p. grade 2 polished Ti samples (10 mm × 10 mm × 1 mm), out of which 96 were etched with 9% and 12%HF, a blend of 35%HCl+85%H3PO4 and a blend of 69%HNO3+35%HCl at 60°C, each for 2 min. One half was silica‐coated (Rocatec™ Plus, 110 μm SiO2‐coated‐Al2O3). Sixty Ti samples were first silica‐coated, and then, 48 of them were etched with 9%HF, 12%HF, a blend of 35%HCl+85%H3PO4, and a blend of 69%HNO3+35%HCl at 60°C for 2 min. SEM, EDX, XPS, and Ra analyses were carried out. Polished Ti samples were controls. All silanizations were carried out with a blend of 0.3 vol% 1,2‐bis‐(triethoxysilyl)ethane+1.0 vol% 3‐acryloxypropyltrimethoxysilane. Multilink™ Automix self‐adhesive resin composite cement was used in adhesion testing, and the samples were artificially aged followed by enclosed‐mold micro‐shear test on day 1 and weeks 1, 4, and 8. Failure mode analysis and statistical analysis with one‐way/two‐way ANOVA (p < 0.05) were carried out. HF etching produced the highest surface roughness. XPS analysis identified after etching with HF a variety of Ti and Si ions: Ti4+, Ti3+, Ti2+, and Ti0 and, on the other hand, Si4+, Si3+, and Si2+. A gradual decrease in adhesion strength was observed after artificial aging. Adhesive and cohesive failures were observed.
{"title":"The effect of different strong acids and silica‐coating on resin Ti adhesion","authors":"M. Zakir, T. Laiho, S. Granroth, E. Kukk, C. Chu, J. Tsoi, J. Matinlinna","doi":"10.1002/sia.7239","DOIUrl":"https://doi.org/10.1002/sia.7239","url":null,"abstract":"The presence of Si on the Ti surface is quintessential for a strong, durable silane‐based adhesion utilized in several dental applications. Silica‐coating and silanization form durable ≡Si‐O‐Si≡ bonds, which might have a positive effect on resin‐Ti adhesion. This laboratory study studied the effect of strong acids, their blends, and silica‐coating on Ti and resin‐Ti bonding. One‐hundred sixty‐eight c.p. grade 2 polished Ti samples (10 mm × 10 mm × 1 mm), out of which 96 were etched with 9% and 12%HF, a blend of 35%HCl+85%H3PO4 and a blend of 69%HNO3+35%HCl at 60°C, each for 2 min. One half was silica‐coated (Rocatec™ Plus, 110 μm SiO2‐coated‐Al2O3). Sixty Ti samples were first silica‐coated, and then, 48 of them were etched with 9%HF, 12%HF, a blend of 35%HCl+85%H3PO4, and a blend of 69%HNO3+35%HCl at 60°C for 2 min. SEM, EDX, XPS, and Ra analyses were carried out. Polished Ti samples were controls. All silanizations were carried out with a blend of 0.3 vol% 1,2‐bis‐(triethoxysilyl)ethane+1.0 vol% 3‐acryloxypropyltrimethoxysilane. Multilink™ Automix self‐adhesive resin composite cement was used in adhesion testing, and the samples were artificially aged followed by enclosed‐mold micro‐shear test on day 1 and weeks 1, 4, and 8. Failure mode analysis and statistical analysis with one‐way/two‐way ANOVA (p < 0.05) were carried out. HF etching produced the highest surface roughness. XPS analysis identified after etching with HF a variety of Ti and Si ions: Ti4+, Ti3+, Ti2+, and Ti0 and, on the other hand, Si4+, Si3+, and Si2+. A gradual decrease in adhesion strength was observed after artificial aging. Adhesive and cohesive failures were observed.","PeriodicalId":22062,"journal":{"name":"Surface and Interface Analysis","volume":"55 1","pages":"701 - 711"},"PeriodicalIF":1.7,"publicationDate":"2023-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"45847231","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}
Alvaro J. Lizarbe, George H. Major, V. Fernandez, N. Fairley, M. Linford
X‐ray photoelectron spectroscopy (XPS) is the most widely used and important method for chemically analyzing and speciating surfaces. XPS has surface sensitivity (5–10 nm), is quantitative, and is able to probe the oxidation states of the elements at surfaces. However, during the past few years, a great deal of incorrect XPS data analysis has entered the scientific literature. Accordingly, efforts, including this Insight Note, are being made to provide tutorial information to the scientific community. Aluminum is a scientifically and technologically important element. Here we discuss approaches for fitting the Al 2p peak envelope from a sample of aluminum foil with a thin layer of oxide on it. Signals from the metal and oxide are present. We discuss methods for electrically isolating (or not isolating) the sample during data acquisition, the choice of the baseline, fitting the oxide peak with one or two synthetic peaks, and fitting the metal signal with two symmetric or two asymmetric peaks. The thickness of the oxide is calculated based on the areas of the oxide and metal signals.
{"title":"Insight note: X‐ray photoelectron spectroscopy (XPS) peak fitting of the Al 2p peak from electrically isolated aluminum foil with an oxide layer","authors":"Alvaro J. Lizarbe, George H. Major, V. Fernandez, N. Fairley, M. Linford","doi":"10.1002/sia.7238","DOIUrl":"https://doi.org/10.1002/sia.7238","url":null,"abstract":"X‐ray photoelectron spectroscopy (XPS) is the most widely used and important method for chemically analyzing and speciating surfaces. XPS has surface sensitivity (5–10 nm), is quantitative, and is able to probe the oxidation states of the elements at surfaces. However, during the past few years, a great deal of incorrect XPS data analysis has entered the scientific literature. Accordingly, efforts, including this Insight Note, are being made to provide tutorial information to the scientific community. Aluminum is a scientifically and technologically important element. Here we discuss approaches for fitting the Al 2p peak envelope from a sample of aluminum foil with a thin layer of oxide on it. Signals from the metal and oxide are present. We discuss methods for electrically isolating (or not isolating) the sample during data acquisition, the choice of the baseline, fitting the oxide peak with one or two synthetic peaks, and fitting the metal signal with two symmetric or two asymmetric peaks. The thickness of the oxide is calculated based on the areas of the oxide and metal signals.","PeriodicalId":22062,"journal":{"name":"Surface and Interface Analysis","volume":"55 1","pages":"651 - 657"},"PeriodicalIF":1.7,"publicationDate":"2023-05-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49060398","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}
L. Strange, M. Engelhard, C. Easton, Ju‐Myung Kim, D. Baer
X‐ray photoelectron spectroscopy (XPS) has become a highly important tool for the analysis of battery materials and components. However, both anecdotal and detailed analysis of selected parts of the literature indicate that many reports of XPS on battery electrodes have significant analysis or data flaws. In this paper, we highlight several of the common challenges that analysts face when using XPS for battery materials, pointing to recent literature that addresses many of the critical issues associated with sample preparation as well as data collection and analysis. A common error for battery materials (and other materials) involves ignoring peak overlaps and interferences. Specifically, when a “minor” peak associated with a component in relatively high concentration overlaps or contributes to the primary peak (or one recommended for quantitative analysis) from a different element in the material. Overlap issues apply to many battery electrodes composed of many elements with complex photoelectron peak structures, as well as those involving peaks with seemingly simpler spectral envelopes such as Li and F. Examples of issues associated with battery systems are highlighted by a discussion of challenges associated with XPS analysis of Li and nickel–manganese–cobalt (NMC) electrodes in battery systems. Lithium analysis has challenges associated with the preparation and an often‐unrecognized peak overlap with F. In our laboratory and in the literature, NMC electrodes are often examined and new XPS users do not always recognize interference of the Auger signal from FKLL (in or on the electrode) with Ni 2p photoelectron spectrum when generated with Al Kα X‐rays. The use of simulated spectra involving both F and NiO demonstrates the extent of F Auger contributions to the Ni 2p signal strength as a function of the F/Ni atom ratio in the material and suggests spectra information that can be used to identify how significant effects will be on the resultant spectra. Our analysis demonstrates that in many cases overlap issues are significant for real electrode materials.
{"title":"Surface analysis insight note: X‐ray photoelectron spectroscopy analysis of battery electrodes—Challenges with nickel–manganese–cobalt and Li examples using an Al Kα x‐ray source","authors":"L. Strange, M. Engelhard, C. Easton, Ju‐Myung Kim, D. Baer","doi":"10.1002/sia.7237","DOIUrl":"https://doi.org/10.1002/sia.7237","url":null,"abstract":"X‐ray photoelectron spectroscopy (XPS) has become a highly important tool for the analysis of battery materials and components. However, both anecdotal and detailed analysis of selected parts of the literature indicate that many reports of XPS on battery electrodes have significant analysis or data flaws. In this paper, we highlight several of the common challenges that analysts face when using XPS for battery materials, pointing to recent literature that addresses many of the critical issues associated with sample preparation as well as data collection and analysis. A common error for battery materials (and other materials) involves ignoring peak overlaps and interferences. Specifically, when a “minor” peak associated with a component in relatively high concentration overlaps or contributes to the primary peak (or one recommended for quantitative analysis) from a different element in the material. Overlap issues apply to many battery electrodes composed of many elements with complex photoelectron peak structures, as well as those involving peaks with seemingly simpler spectral envelopes such as Li and F. Examples of issues associated with battery systems are highlighted by a discussion of challenges associated with XPS analysis of Li and nickel–manganese–cobalt (NMC) electrodes in battery systems. Lithium analysis has challenges associated with the preparation and an often‐unrecognized peak overlap with F. In our laboratory and in the literature, NMC electrodes are often examined and new XPS users do not always recognize interference of the Auger signal from FKLL (in or on the electrode) with Ni 2p photoelectron spectrum when generated with Al Kα X‐rays. The use of simulated spectra involving both F and NiO demonstrates the extent of F Auger contributions to the Ni 2p signal strength as a function of the F/Ni atom ratio in the material and suggests spectra information that can be used to identify how significant effects will be on the resultant spectra. Our analysis demonstrates that in many cases overlap issues are significant for real electrode materials.","PeriodicalId":22062,"journal":{"name":"Surface and Interface Analysis","volume":"55 1","pages":"715 - 729"},"PeriodicalIF":1.7,"publicationDate":"2023-05-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"42500187","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}
Tielong Deng, Zekai Chen, Yaping Li, Biwen Zhang, Huiqiong Wang, Jia‐Ou Wang, Rui Wu, H. Zhan, Junyong Kang
(Mg,Zn)O films with various growth orientations were prepared on the MgO substrates with different surface structures using oxygen plasma‐assisted molecular beam epitaxy. X‐ray diffraction (XRD) revealed that the crystallographic orientation of (Mg,Zn)O thin films transforms from the polar c‐plane (0001) to a two‐fold‐symmetry inclined plane and then to the nonpolar m‐plane (10–10) as the substrate template changes from MgO(111) to MgO(011) and then to MgO(001). In addition, the surface topography and film roughness were monitored by atomic force microscopy. Interestingly, the electronic structures of the three films exhibited orientation‐dependent features, as revealed by synchrotron‐based X‐ray absorption spectroscopy. In addition, all of the (Mg,Zn)O thin films showed high optical transmittance (over 85%, 400–800 nm) and large energy gaps (around 3.33 eV). Our systematic study of the substrate‐influenced film characteristics demonstrates a method of tailoring thin films using the same substrate with different crystallographic orientations.
{"title":"Epitaxial growth of Zn‐rich (Mg,Zn)O thin films on MgO substrates with different surface orientations","authors":"Tielong Deng, Zekai Chen, Yaping Li, Biwen Zhang, Huiqiong Wang, Jia‐Ou Wang, Rui Wu, H. Zhan, Junyong Kang","doi":"10.1002/sia.7236","DOIUrl":"https://doi.org/10.1002/sia.7236","url":null,"abstract":"(Mg,Zn)O films with various growth orientations were prepared on the MgO substrates with different surface structures using oxygen plasma‐assisted molecular beam epitaxy. X‐ray diffraction (XRD) revealed that the crystallographic orientation of (Mg,Zn)O thin films transforms from the polar c‐plane (0001) to a two‐fold‐symmetry inclined plane and then to the nonpolar m‐plane (10–10) as the substrate template changes from MgO(111) to MgO(011) and then to MgO(001). In addition, the surface topography and film roughness were monitored by atomic force microscopy. Interestingly, the electronic structures of the three films exhibited orientation‐dependent features, as revealed by synchrotron‐based X‐ray absorption spectroscopy. In addition, all of the (Mg,Zn)O thin films showed high optical transmittance (over 85%, 400–800 nm) and large energy gaps (around 3.33 eV). Our systematic study of the substrate‐influenced film characteristics demonstrates a method of tailoring thin films using the same substrate with different crystallographic orientations.","PeriodicalId":22062,"journal":{"name":"Surface and Interface Analysis","volume":"55 1","pages":"694 - 700"},"PeriodicalIF":1.7,"publicationDate":"2023-05-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46255213","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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