When measuring the thickness of ultrathin overlayer films using X-ray photoelectron spectroscopy (XPS), accurate values of the reference intensity ratio (R0) and the effective attenuation length (L) are essential. By definition, R0 is the peak intensity ratio for an overlayer and the substrate in “bulk” phases. Two issues need to be addressed in experimental determining R0 for ultrathin films: (i) How might a contamination layer on the sample used for measuring peak intensities impact R0? And (ii) do differences in the structure or chemistry of an ultrathin film make it inappropriate to determine R0 using bulk forms of the overlayer? In this study, we demonstrate the experimental determination of the R0 for an ultrathin HfO2 film on a Si(100) substrate with a 2 nm SiO2 layer. The values of R0 were determined using (i) the bulk materials of the HfO2 film and substrate and (ii) the ultrathin HfO2 films after different cleaning treatments. The results show that the R0 determined by the ultrathin films is higher than that determined by the bulk materials. Also, keeping the same level of carbonaceous contamination on the sample surface by cleaning as much as possible is essential for an accurate experimental determination of R0. In addition, the effective attenuation length was obtained using samples with known thicknesses measured by X-ray reflectometry. The thicknesses and uncertainty budget of the ultrathin HfO2 films were then evaluated.
{"title":"Experimental determination of reference intensity ratio essential for accurate thickness measurement of HfO2 ultrathin films by XPS","authors":"Lulu Zhang, Yasushi Azuma, Akira Kurokawa, Hiroyuki Matsuzaki","doi":"10.1002/sia.7293","DOIUrl":"https://doi.org/10.1002/sia.7293","url":null,"abstract":"When measuring the thickness of ultrathin overlayer films using X-ray photoelectron spectroscopy (XPS), accurate values of the reference intensity ratio (<i>R</i><sub>0</sub>) and the effective attenuation length (<i>L</i>) are essential. By definition, <i>R</i><sub>0</sub> is the peak intensity ratio for an overlayer and the substrate in “bulk” phases. Two issues need to be addressed in experimental determining <i>R</i><sub>0</sub> for ultrathin films: (i) How might a contamination layer on the sample used for measuring peak intensities impact <i>R</i><sub>0</sub>? And (ii) do differences in the structure or chemistry of an ultrathin film make it inappropriate to determine <i>R</i><sub>0</sub> using bulk forms of the overlayer? In this study, we demonstrate the experimental determination of the <i>R</i><sub>0</sub> for an ultrathin HfO<sub>2</sub> film on a Si(100) substrate with a 2 nm SiO<sub>2</sub> layer. The values of <i>R</i><sub>0</sub> were determined using (i) the bulk materials of the HfO<sub>2</sub> film and substrate and (ii) the ultrathin HfO<sub>2</sub> films after different cleaning treatments. The results show that the <i>R</i><sub>0</sub> determined by the ultrathin films is higher than that determined by the bulk materials. Also, keeping the same level of carbonaceous contamination on the sample surface by cleaning as much as possible is essential for an accurate experimental determination of <i>R</i><sub>0</sub>. In addition, the effective attenuation length was obtained using samples with known thicknesses measured by X-ray reflectometry. The thicknesses and uncertainty budget of the ultrathin HfO<sub>2</sub> films were then evaluated.","PeriodicalId":22062,"journal":{"name":"Surface and Interface Analysis","volume":"45 1","pages":""},"PeriodicalIF":1.7,"publicationDate":"2024-02-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139923919","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}
Stefan Makowski, Martin Zawischa, Dieter Schneider, Stephan Barth, Sebastian Schettler, Thanh-Tung Hoang, Hagen Bartzsch, Martina Zimmermann
Surface acoustic wave spectroscopy has been established as non-destructive and fast method for characterization of mechanical properties of surfaces and bulk materials in both research and industry. The present work shows that by application of a novel and robust aluminum nitride (AlN) coated piezoelectric contact sensor the advantages of the method can be extended from room temperature to at least 600°C. An overview of sensor concepts and applications of the method is discussed first, followed by theoretical and practical considerations for design and coating of a novel temperature stable contact sensor. After fabrication of such a sensor using magnetron sputtering, it was tested in a modified surface acoustic wave spectroscopy setup with an incorporated heating table concerning signal amplitude and frequency range. The AlN coated sensor was found to perform well up to 600°C, with temperature limited by the specification of the heating table. At room temperature, performance was acceptable when compared with a conventional contact sensor using a PVDF piezoelectric foil. Application of the high temperature capabilities of the setup was demonstrated by measuring temperature stability of hydrogen-free amorphous carbon coatings (a-C and ta-C) depending on their sp3 carbon ratio. In another example, high precision temperature dependent measurement of Young's modulus for ultrasonic fatigue test specimen was taken, achieving an accuracy better than 1%. Use of the developed sensor opens up new possibilities in material science for in situ study of temperature depending mechanical properties for coatings and surfaces.
{"title":"Surface acoustic wave spectroscopy for non-destructive coating and bulk characterization at temperatures up to 600°C enabled by piezoelectric aluminum nitride coated sensor","authors":"Stefan Makowski, Martin Zawischa, Dieter Schneider, Stephan Barth, Sebastian Schettler, Thanh-Tung Hoang, Hagen Bartzsch, Martina Zimmermann","doi":"10.1002/sia.7291","DOIUrl":"https://doi.org/10.1002/sia.7291","url":null,"abstract":"Surface acoustic wave spectroscopy has been established as non-destructive and fast method for characterization of mechanical properties of surfaces and bulk materials in both research and industry. The present work shows that by application of a novel and robust aluminum nitride (AlN) coated piezoelectric contact sensor the advantages of the method can be extended from room temperature to at least 600°C. An overview of sensor concepts and applications of the method is discussed first, followed by theoretical and practical considerations for design and coating of a novel temperature stable contact sensor. After fabrication of such a sensor using magnetron sputtering, it was tested in a modified surface acoustic wave spectroscopy setup with an incorporated heating table concerning signal amplitude and frequency range. The AlN coated sensor was found to perform well up to 600°C, with temperature limited by the specification of the heating table. At room temperature, performance was acceptable when compared with a conventional contact sensor using a PVDF piezoelectric foil. Application of the high temperature capabilities of the setup was demonstrated by measuring temperature stability of hydrogen-free amorphous carbon coatings (a-C and ta-C) depending on their sp<sup>3</sup> carbon ratio. In another example, high precision temperature dependent measurement of Young's modulus for ultrasonic fatigue test specimen was taken, achieving an accuracy better than 1%. Use of the developed sensor opens up new possibilities in material science for in situ study of temperature depending mechanical properties for coatings and surfaces.","PeriodicalId":22062,"journal":{"name":"Surface and Interface Analysis","volume":"15 1","pages":""},"PeriodicalIF":1.7,"publicationDate":"2024-02-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139768791","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}
Among the nondestructive carbon material characterization tools, the prominence of visible Raman spectroscopy has surged remarkably for many years due to its ability to explore a diverse array of carbon bonding configurations. However, to fully unlock the distinctive features concealed within carbon composite materials, additional specimen treatments or precise spectroscope calibrations are necessary. In the same regard, the tiny diamond grain size (5–10 nm) and the pronounced amount of sp2 carbon in the ultrananocrystalline diamond film represent major challenges in visible light excitation. In this work, we employ calibrated oxygen plasma reactive ion etching conditions to manifest the nanodiamond visible Raman signature from ultrananocrystalline diamond/amorphous carbon composite (UNCD/a-C) films fabricated by coaxial arc plasma deposition. Upon plasma etching, the broad defect band in the visible Raman spectra converged toward the diamond characteristic Raman peak at 1332 cm−1. A detailed explanation of band components of the Raman spectra is extracted through peak fitting procedures. The results of Raman spectroscopy are further correlated with the electrical characteristics of the nitrogen-doped UNCD/a-C films due to the optimized oxygen plasma etching processes.
{"title":"Maximizing visible Raman resolution of nanodiamond grains fabricated by coaxial arc plasma deposition through oxygen plasma etching optimization","authors":"Sreenath Mylo Valappil, Abdelrahman Zkria, Phongsaphak Sittimart, Shinya Ohmagari, Tsuyoshi Yoshitake","doi":"10.1002/sia.7289","DOIUrl":"https://doi.org/10.1002/sia.7289","url":null,"abstract":"Among the nondestructive carbon material characterization tools, the prominence of visible Raman spectroscopy has surged remarkably for many years due to its ability to explore a diverse array of carbon bonding configurations. However, to fully unlock the distinctive features concealed within carbon composite materials, additional specimen treatments or precise spectroscope calibrations are necessary. In the same regard, the tiny diamond grain size (5–10 nm) and the pronounced amount of <i>sp</i><sup><i>2</i></sup> carbon in the ultrananocrystalline diamond film represent major challenges in visible light excitation. In this work, we employ calibrated oxygen plasma reactive ion etching conditions to manifest the nanodiamond visible Raman signature from ultrananocrystalline diamond/amorphous carbon composite (UNCD/a-C) films fabricated by coaxial arc plasma deposition. Upon plasma etching, the broad defect band in the visible Raman spectra converged toward the diamond characteristic Raman peak at 1332 cm<sup>−1</sup>. A detailed explanation of band components of the Raman spectra is extracted through peak fitting procedures. The results of Raman spectroscopy are further correlated with the electrical characteristics of the nitrogen-doped UNCD/a-C films due to the optimized oxygen plasma etching processes.","PeriodicalId":22062,"journal":{"name":"Surface and Interface Analysis","volume":"2 1","pages":""},"PeriodicalIF":1.7,"publicationDate":"2024-01-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139657453","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}
Pascal Bargiela, Vincent Fernandez, David Morgan, Neal Fairley, Jonas Baltrusaitis
Standard materials are often used to obtain spectra that can be compared to those from unknown samples. Spectra measured from these known substances are also used as a means of computing sensitivity factors to allow quantification by X-ray photoelectron spectroscopy (XPS) of less well-defined materials. Spectra from known materials also provide line shapes suitable for inclusion in spectral models which, when fitted to spectra, permit the chemical state for a sample to be assessed. Both types of information depend on isolating photoemission signals from the inelastically scattered signal. In this Insight note, technical issues associated with the use of XPS of as received Fe3O4 powder sample surface are discussed. The Insight note is designed to show how linear algebraic techniques applied to data collected from a sample marketed as pure Fe3O4 powder are used to verify that XPS has been performed on chemistry representative of the sample. The methods described in this Insight note can further be utilized in elucidating complex XPS data obtained from thin films formed or evolved during cyclic/non-steady use of complex (electro)catalyst surfaces, especially in the presence of contaminants.
{"title":"Surface science insight note: A linear algebraic approach to elucidate native films on Fe3O4 surface","authors":"Pascal Bargiela, Vincent Fernandez, David Morgan, Neal Fairley, Jonas Baltrusaitis","doi":"10.1002/sia.7290","DOIUrl":"https://doi.org/10.1002/sia.7290","url":null,"abstract":"Standard materials are often used to obtain spectra that can be compared to those from unknown samples. Spectra measured from these known substances are also used as a means of computing sensitivity factors to allow quantification by X-ray photoelectron spectroscopy (XPS) of less well-defined materials. Spectra from known materials also provide line shapes suitable for inclusion in spectral models which, when fitted to spectra, permit the chemical state for a sample to be assessed. Both types of information depend on isolating photoemission signals from the inelastically scattered signal. In this <i>Insight</i> note, technical issues associated with the use of XPS of as received Fe<sub>3</sub>O<sub>4</sub> powder sample surface are discussed. The <i>Insight</i> note is designed to show how linear algebraic techniques applied to data collected from a sample marketed as pure Fe<sub>3</sub>O<sub>4</sub> powder are used to verify that XPS has been performed on chemistry representative of the sample. The methods described in this <i>Insight</i> note can further be utilized in elucidating complex XPS data obtained from thin films formed or evolved during cyclic/non-steady use of complex (electro)catalyst surfaces, especially in the presence of contaminants.","PeriodicalId":22062,"journal":{"name":"Surface and Interface Analysis","volume":"281 1","pages":""},"PeriodicalIF":1.7,"publicationDate":"2024-01-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139658081","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}
Sangmin Han, Hee-Seung Yoon, Juyun Park, Jin-Woo Oh, Yong-Cheol Kang
In this work, RF magnetron co-sputtering was used to fabricate molybdenum oxytelluride thin films with different atomic ratios. Scanning electron micrographs and atomic force micrographs revealed that pure Mo thin films were segregated. Thin films with 40% Te content portrayed needle-like structures and thus had the largest Rq value of 2.48 nm. Contact angle measurements further supported the findings as the thin films with 40% Te content were the most hydrophobic. X-ray photoelectron spectroscopy results revealed that the major oxidation states of Mo from Te-poor to Te-rich TFs were changed from high (+6) to low (+4 and/or +2). X-ray diffraction data showed that peaks pertaining to molybdenum oxide species appeared, notably at 33.048° and 33.115°. Ultraviolet photoelectron spectroscopy and Kelvin probe measurements evinced that the work function increases with increasing Te content. Four-point probe measurements revealed that molybdenum oxytelluride thin films tend to have higher electrical conductivity than pure Mo and Te thin films.
在这项工作中，采用射频磁控共溅射技术制造了不同原子比的钼氧碲薄膜。扫描电子显微镜和原子力显微镜显示，纯钼薄膜呈离析状。含 40% Te 的薄膜呈现针状结构，因此 Rq 值最大，为 2.48 nm。接触角测量进一步证实了这一发现，因为含 40% Te 的薄膜疏水性最强。X 射线光电子能谱结果表明，从贫钛到富钛 TF 中，钼的主要氧化态由高（+6）变为低（+4 和/或 +2）。X 射线衍射数据显示，出现了与氧化钼物种有关的峰值，特别是在 33.048°和 33.115°。紫外光电子能谱和开尔文探针测量表明，功函数随 Te 含量的增加而增加。四点探针测量显示，碲化钼薄膜的导电率往往高于纯 Mo 和 Te 薄膜。
{"title":"Tailoring the surface properties of molybdenum oxytelluride thin films by its compositional ratio","authors":"Sangmin Han, Hee-Seung Yoon, Juyun Park, Jin-Woo Oh, Yong-Cheol Kang","doi":"10.1002/sia.7288","DOIUrl":"https://doi.org/10.1002/sia.7288","url":null,"abstract":"In this work, RF magnetron co-sputtering was used to fabricate molybdenum oxytelluride thin films with different atomic ratios. Scanning electron micrographs and atomic force micrographs revealed that pure Mo thin films were segregated. Thin films with 40% Te content portrayed needle-like structures and thus had the largest <i>R</i><sub><i>q</i></sub> value of 2.48 nm. Contact angle measurements further supported the findings as the thin films with 40% Te content were the most hydrophobic. X-ray photoelectron spectroscopy results revealed that the major oxidation states of Mo from Te-poor to Te-rich TFs were changed from high (+6) to low (+4 and/or +2). X-ray diffraction data showed that peaks pertaining to molybdenum oxide species appeared, notably at 33.048° and 33.115°. Ultraviolet photoelectron spectroscopy and Kelvin probe measurements evinced that the work function increases with increasing Te content. Four-point probe measurements revealed that molybdenum oxytelluride thin films tend to have higher electrical conductivity than pure Mo and Te thin films.","PeriodicalId":22062,"journal":{"name":"Surface and Interface Analysis","volume":"10 1","pages":""},"PeriodicalIF":1.7,"publicationDate":"2024-01-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139648745","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}
Pengjie Wang, Lin Fan, Yuhao Song, Kuaihai Deng, Lei Guo, Zhonghui Li, Yuanhua Lin
In order to reduce the investment of corrosion inhibitors, based on experimental and theoretical studies, the corrosion inhibition and mechanism of new imidazoline derivatives (SMIS) and 2-aminopyridine (AMP) were investigated carefully. The best corrosion inhibition effect was at 0.7-g/L SMIS and 0.3-g/L AMP, the corrosion inhibition efficiency of weight loss, electrochemical impedance spectroscopy, and potentiodynamic polarization (Tafel) were 90.54%, 98.56% and 97.68%, respectively. Electrochemical research shows that SMIS& belongs to cathodic corrosion inhibition. SMIS& mainly increased the film resistance and charge transfer resistance in 1-M HCl, thus playing a certain role in corrosion inhibition. X-ray photoelectron spectroscopy and energy dispersive spectrometer proved that SMIS& can be adsorbed on the surface of Q235, molecular dynamics showed that there was a certain synergy between SMIS and AMP. This study confirmed that SMIS and AMP have a good synergistic effect, improve the corrosion inhibition efficiency, reduce the synthesis cost of SMIS, and have a certain guiding significance for synergistic corrosion inhibition.
{"title":"Synergistic effect of new imidazoline derivative and 2-aminopyridine as corrosion inhibitors for Q235: Experimental and theoretical study","authors":"Pengjie Wang, Lin Fan, Yuhao Song, Kuaihai Deng, Lei Guo, Zhonghui Li, Yuanhua Lin","doi":"10.1002/sia.7286","DOIUrl":"https://doi.org/10.1002/sia.7286","url":null,"abstract":"In order to reduce the investment of corrosion inhibitors, based on experimental and theoretical studies, the corrosion inhibition and mechanism of new imidazoline derivatives (SMIS) and 2-aminopyridine (AMP) were investigated carefully. The best corrosion inhibition effect was at 0.7-g/L SMIS and 0.3-g/L AMP, the corrosion inhibition efficiency of weight loss, electrochemical impedance spectroscopy, and potentiodynamic polarization (Tafel) were 90.54%, 98.56% and 97.68%, respectively. Electrochemical research shows that SMIS& belongs to cathodic corrosion inhibition. SMIS& mainly increased the film resistance and charge transfer resistance in 1-M HCl, thus playing a certain role in corrosion inhibition. X-ray photoelectron spectroscopy and energy dispersive spectrometer proved that SMIS& can be adsorbed on the surface of Q235, molecular dynamics showed that there was a certain synergy between SMIS and AMP. This study confirmed that SMIS and AMP have a good synergistic effect, improve the corrosion inhibition efficiency, reduce the synthesis cost of SMIS, and have a certain guiding significance for synergistic corrosion inhibition.","PeriodicalId":22062,"journal":{"name":"Surface and Interface Analysis","volume":"179 1","pages":""},"PeriodicalIF":1.7,"publicationDate":"2024-01-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139581410","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}
Marius Behnecke, Eva Berghaus, Alina Wildeis, Eva Brandes, Svea Petersen
The growing significance of surface properties in modern materials, particularly in medical technology, drives the need for accurate characterization techniques. Traditional contact angle measurements face challenges when applied to intricate surfaces like dental implants. Here, tensiometry applying the Wilhelmy plate method has been described in the last decade to offer one solution for the evaluation of complex surface geometries by quantifying apparent contact angles based on wetting forces. This study evaluates a simple setup employing the Wilhelmy balance concept for immersion angle determination. Instead of using a force sensor as in tensiometers, the wetting force is determined via changes in mass signal by means of an analytical balance available in standard laboratories. The force is thus recorded inverse to conventional tensiometry. The approach was validated on diverse geometries and extended to intricate structures, including plasma-treated dental implants. Results were compared to conventional contact angle analysis systems underlining the reliability of the method in characterizing non-planar and complex surfaces. Additionally, the method was successfully extended to the evaluation of surface energies on planar and non-planar surfaces using various solvent sets. However, results evidenced that specimen geometry can influence the measurements to such an extent that immersion contact angles can no longer be calculated due to capillary effects. An outlook suggests further exploration with a wider range of test liquids to enhance accuracy in surface energy determination.
{"title":"Wilhelmy balance—A simple and reliable method for determining immersion angles and surface energies even on non-planar and complex geometries?","authors":"Marius Behnecke, Eva Berghaus, Alina Wildeis, Eva Brandes, Svea Petersen","doi":"10.1002/sia.7287","DOIUrl":"https://doi.org/10.1002/sia.7287","url":null,"abstract":"The growing significance of surface properties in modern materials, particularly in medical technology, drives the need for accurate characterization techniques. Traditional contact angle measurements face challenges when applied to intricate surfaces like dental implants. Here, tensiometry applying the Wilhelmy plate method has been described in the last decade to offer one solution for the evaluation of complex surface geometries by quantifying apparent contact angles based on wetting forces. This study evaluates a simple setup employing the Wilhelmy balance concept for immersion angle determination. Instead of using a force sensor as in tensiometers, the wetting force is determined via changes in mass signal by means of an analytical balance available in standard laboratories. The force is thus recorded inverse to conventional tensiometry. The approach was validated on diverse geometries and extended to intricate structures, including plasma-treated dental implants. Results were compared to conventional contact angle analysis systems underlining the reliability of the method in characterizing non-planar and complex surfaces. Additionally, the method was successfully extended to the evaluation of surface energies on planar and non-planar surfaces using various solvent sets. However, results evidenced that specimen geometry can influence the measurements to such an extent that immersion contact angles can no longer be calculated due to capillary effects. An outlook suggests further exploration with a wider range of test liquids to enhance accuracy in surface energy determination.","PeriodicalId":22062,"journal":{"name":"Surface and Interface Analysis","volume":"62 1","pages":""},"PeriodicalIF":1.7,"publicationDate":"2024-01-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139581407","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}
Liqiang Chai, Pengxiang Ma, Chengyan Jiang, L. Qiao, Peng Wang
Polytetrafluoroethylene (PTFE) solid self‐lubricating materials exhibit inferior tribological properties in the gamma‐irradiated environment. In this paper, amorphous hydrogen‐free carbon (a‐C) film was deposited on the PTFE polymer surface by magnetron sputtering, and the a‐C/PTFE samples were irradiated with gamma ray at a maximum dose of up to 5 MGy. The evolution of the structure and nanomechanical and tribological properties of a‐C/PTFE with different irradiation doses were investigated. The structural analyses reveal that the microstructure of a‐C films irradiated at 5 MGy doses is stable. Due to the covering of the a‐C film, significant cracks appear at the surface of the a‐C/PTFE sample only when the irradiation dose reaches 5 MGy. Before and after irradiation, the nanohardness and Young's modulus of the a‐C/PTFE are significantly higher than those of PTFE. The mechanical properties of PTFE are improved by a‐C film surface treatment. The friction experiments show that the average friction coefficients of both a‐C/PTFE and PTFE remain stable around 0.175 with increasing irradiation dose. When the irradiation dose is within 1 MGy, frictional behaviors occur only on the surface of a‐C films, and the wear rate of a‐C/PTFE is as low as 9.3 × 10−5 mm3/N.m, which is significantly lower than that of PTFE. The method of a‐C film treatment on the PTFE surface can dramatically improve the irradiation resistance of PTFE.
{"title":"Enhancing gamma irradiation resistance by a‐C film treatment on polytetrafluoroethylene (PTFE) surface","authors":"Liqiang Chai, Pengxiang Ma, Chengyan Jiang, L. Qiao, Peng Wang","doi":"10.1002/sia.7285","DOIUrl":"https://doi.org/10.1002/sia.7285","url":null,"abstract":"Polytetrafluoroethylene (PTFE) solid self‐lubricating materials exhibit inferior tribological properties in the gamma‐irradiated environment. In this paper, amorphous hydrogen‐free carbon (a‐C) film was deposited on the PTFE polymer surface by magnetron sputtering, and the a‐C/PTFE samples were irradiated with gamma ray at a maximum dose of up to 5 MGy. The evolution of the structure and nanomechanical and tribological properties of a‐C/PTFE with different irradiation doses were investigated. The structural analyses reveal that the microstructure of a‐C films irradiated at 5 MGy doses is stable. Due to the covering of the a‐C film, significant cracks appear at the surface of the a‐C/PTFE sample only when the irradiation dose reaches 5 MGy. Before and after irradiation, the nanohardness and Young's modulus of the a‐C/PTFE are significantly higher than those of PTFE. The mechanical properties of PTFE are improved by a‐C film surface treatment. The friction experiments show that the average friction coefficients of both a‐C/PTFE and PTFE remain stable around 0.175 with increasing irradiation dose. When the irradiation dose is within 1 MGy, frictional behaviors occur only on the surface of a‐C films, and the wear rate of a‐C/PTFE is as low as 9.3 × 10−5 mm3/N.m, which is significantly lower than that of PTFE. The method of a‐C film treatment on the PTFE surface can dramatically improve the irradiation resistance of PTFE.","PeriodicalId":22062,"journal":{"name":"Surface and Interface Analysis","volume":"72 2","pages":""},"PeriodicalIF":1.7,"publicationDate":"2024-01-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139440626","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}
Alexander G. Shard, Donald R. Baer, Charles A. Clifford
The International Standard ISO 18115-1 on terminology in surface chemical analysis has been revised with clarifications, modifications, and deletions to more than 70 terms and with the addition of more than 50 terms in response to trends, issues, and needs identified by the surface analysis community. This revision adds terminology and concepts associated with emerging methods such as atom probe tomography, near ambient pressure XPS, and hard X-ray photoelectron spectroscopy. It includes 25 new and revised terms to ensure that the description of resolution is consistent across all surface analysis methods. The 630 terms in the document cover words or phrases used in describing the samples, instruments, and concepts involved in surface chemical analysis. The terms have been collated into subject specific sections to ensure that related terms can be found easily.
国际标准 ISO 18115-1 对表面化学分析术语进行了修订，澄清、修改和删除了 70 多个术语，并根据表面分析界确定的趋势、问题和需求增加了 50 多个术语。本次修订增加了与原子探针层析成像、近环境压力 XPS 和硬 X 射线光电子能谱等新兴方法相关的术语和概念。它包括 25 个新术语和修订术语，以确保所有表面分析方法对分辨率的描述保持一致。文件中的 630 个术语涵盖了用于描述样品、仪器和表面化学分析相关概念的单词或短语。这些术语已按主题分类整理，以确保相关术语易于查找。
{"title":"Importance of standard terminology in surface chemical analysis: ISO 18115-1:2023, general terms and terms used in spectroscopy","authors":"Alexander G. Shard, Donald R. Baer, Charles A. Clifford","doi":"10.1002/sia.7284","DOIUrl":"https://doi.org/10.1002/sia.7284","url":null,"abstract":"The International Standard ISO 18115-1 on terminology in surface chemical analysis has been revised with clarifications, modifications, and deletions to more than 70 terms and with the addition of more than 50 terms in response to trends, issues, and needs identified by the surface analysis community. This revision adds terminology and concepts associated with emerging methods such as atom probe tomography, near ambient pressure XPS, and hard X-ray photoelectron spectroscopy. It includes 25 new and revised terms to ensure that the description of resolution is consistent across all surface analysis methods. The 630 terms in the document cover words or phrases used in describing the samples, instruments, and concepts involved in surface chemical analysis. The terms have been collated into subject specific sections to ensure that related terms can be found easily.","PeriodicalId":22062,"journal":{"name":"Surface and Interface Analysis","volume":"54 1","pages":""},"PeriodicalIF":1.7,"publicationDate":"2024-01-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139415194","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}
Claudia Cancellieri, Simon Gramatte, Olivier Politano, Léo Lapeyre, Fedor Klimashin, Krzysztof Mackosz, Ivo Utke, Zbynek Novotny, Arnold M. Müller, Christof Vockenhuber, Vladyslav Turlo, Lars P. H. Jeurgens
Amorphous oxide thin films grown by thermal atomic layer deposition (ALD) typically contain high impurity concentrations of hydrogen, which affects both chemistry and structure and thereby the functional properties, such as the barrier properties in, for example, microelectronic and photovoltaic devices. This study discloses the effect of H incorporation in amorphous Al2O3 ALD oxide films on the local chemical binding states of Al, O and H, as well as the oxide density and stoichiometry, by a combined analytical approach using elastic recoil detection analysis, Rutherford backscattering spectroscopy and full chemical state analysis by dual-source X-ray photoelectron spectroscopy (XPS)/hard X-ray photoelectron spectroscopy (HAXPES). The experimental findings are compared with crystalline anhydrous α-Al2O3 and hydroxide α-Al (OH)3 reference phases and further supported by molecular dynamic simulations. It is shown that H preferably forms covalent –OH hydroxyl bonds with O in the nearest-neighbour coordination spheres of interstitial Al cations, which affects both the ligand electronic polarizability and the bond length of the randomly interconnected [AlOn] polyhedral building blocks in the amorphous ALD oxide films.
通过热原子层沉积（ALD）技术生长的非晶氧化物薄膜通常含有高浓度的氢杂质，这会影响其化学性质和结构，从而影响其功能特性，例如微电子和光伏设备的阻隔特性。本研究采用弹性反冲探测分析、卢瑟福反向散射光谱和双源 X 射线光电子能谱（XPS）/硬 X 射线光电子能谱（HAXPES）全化学态分析相结合的分析方法，揭示了非晶态 Al2O3 ALD 氧化物薄膜中加入氢对 Al、O 和 H 的局部化学结合态以及氧化物密度和化学计量学的影响。实验结果与结晶无水 α-Al2O3 和氢氧化物 α-Al (OH)3 参考相进行了比较，并得到了分子动力学模拟的进一步支持。实验结果表明，在间隙铝阳离子的近邻配位圈中，H 优先与 O 形成共价 -OH 羟基键，这既影响了配体的电子极化性，也影响了无定形 ALD 氧化物薄膜中随机互连的 [AlOn] 多面体结构单元的键长。
{"title":"Effect of hydrogen on the chemical state, stoichiometry and density of amorphous Al2O3 films grown by thermal atomic layer deposition","authors":"Claudia Cancellieri, Simon Gramatte, Olivier Politano, Léo Lapeyre, Fedor Klimashin, Krzysztof Mackosz, Ivo Utke, Zbynek Novotny, Arnold M. Müller, Christof Vockenhuber, Vladyslav Turlo, Lars P. H. Jeurgens","doi":"10.1002/sia.7282","DOIUrl":"https://doi.org/10.1002/sia.7282","url":null,"abstract":"Amorphous oxide thin films grown by thermal atomic layer deposition (ALD) typically contain high impurity concentrations of hydrogen, which affects both chemistry and structure and thereby the functional properties, such as the barrier properties in, for example, microelectronic and photovoltaic devices. This study discloses the effect of H incorporation in amorphous Al<sub>2</sub>O<sub>3</sub> ALD oxide films on the local chemical binding states of Al, O and H, as well as the oxide density and stoichiometry, by a combined analytical approach using elastic recoil detection analysis, Rutherford backscattering spectroscopy and full chemical state analysis by dual-source X-ray photoelectron spectroscopy (XPS)/hard X-ray photoelectron spectroscopy (HAXPES). The experimental findings are compared with crystalline anhydrous α-Al<sub>2</sub>O<sub>3</sub> and hydroxide α-Al (OH)<sub>3</sub> reference phases and further supported by molecular dynamic simulations. It is shown that H preferably forms covalent –OH hydroxyl bonds with O in the nearest-neighbour coordination spheres of interstitial Al cations, which affects both the ligand electronic polarizability and the bond length of the randomly interconnected [AlO<sub>n</sub>] polyhedral building blocks in the amorphous ALD oxide films.","PeriodicalId":22062,"journal":{"name":"Surface and Interface Analysis","volume":"216 4 1","pages":""},"PeriodicalIF":1.7,"publicationDate":"2024-01-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139408690","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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