Claire Guyot, Jean-Paul Barnes, Olivier Renault, Tony Maindron
{"title":"Time-of-flight secondary ion mass spectrometry and X-ray photoelectron spectroscopy protocol for the analysis of organic multilayers","authors":"Claire Guyot, Jean-Paul Barnes, Olivier Renault, Tony Maindron","doi":"10.1002/sia.7277","DOIUrl":"https://doi.org/10.1002/sia.7277","url":null,"abstract":"With the development in the early 2000s of new cluster ion sputtering sources, a reliable analysis of organic multilayers and interfaces has become possible. Nowadays, time-of-flight secondary ion mass spectrometry (ToF-SIMS) and X-ray photoelectron spectroscopy (XPS) depth profiling are routinely used to investigate organic stacks. However, analysis beams can cause bond scission or beam-induced degradations that accumulate in buried layers. We developed a correlative protocol that minimises damages related to analysis beams. It uses a shallow angle bevel crater fabricated inside the ToF-SIMS analysis chamber. With this preparation method, the in-depth information is displayed over the surface of the bevel crater. XPS profiles and high-resolution spectra paired with ToF-SIMS images enable an easy identification of the organic layers and complete understanding of their chemistry. The reduction of beam-induced degradation is achieved by minimising the acquisition times, therefore beam exposure on materials. Finally, an important advantage of this preparation method is that the analysis can be performed on exactly the same spot by multiple techniques. Several ToF-SIMS and XPS acquisitions can be carried out with various parameters (investigation of backscattered Ar<sub>n</sub><sup>+</sup> cluster ion fragments, tandem MS imaging…) as well as analysis with other techniques that possess limitations in spatial resolution and/or inaptitude to probe buried layers such as Raman or AFM.","PeriodicalId":22062,"journal":{"name":"Surface and Interface Analysis","volume":"108 1","pages":""},"PeriodicalIF":1.7,"publicationDate":"2023-12-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"138568695","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":"Effect of substrate temperature and annealing on the growth of TiO2-x thin films deposited by using DC-magnetron sputtering technique","authors":"Swapan Jana, Anil Krishna Debnath, Veerender Putta, Jitendra Bahadur, Jugal Kishor, Anil Kumar Chauhan, Debarati Bhattacharya","doi":"10.1002/sia.7274","DOIUrl":"https://doi.org/10.1002/sia.7274","url":null,"abstract":"In this study, the effect of annealing on the structural, surface morphology and chemical structure of titanium suboxide (TiO<sub>2-x</sub>) thin films has been investigated. TiO<sub>2-x</sub> films had been grown on Si substrates by DC-magnetron sputtering with different sputter powers (75 and 100 W) at room temperature (RT) and 200°C substrate temperature (ST). The films were subsequently annealed for 1 h at 300, 400 and 500°C in vacuum. The impact of ST, post-annealing and sputter power on crystallinity, surface morphology and chemical state of the films were studied. Grazing incidence X-ray diffraction (GIXRD) data revealed that the films were amorphous or exhibited a very low crystalline structure while deposited at RT and even after annealing. Moreover, the films showed crystallinity while deposited at ST and exhibited an anatase-rutile (A-R) mix phase from anatase (A) annealed at 300°C (75 W at ST). X-ray reflectivity (XRR) data showed that the mass density of the films increased with the annealing temperature. Images obtained using atomic force microscopy (AFM) and field emission scanning electron microscopy (FESEM) revealed that post-annealing increased the surface roughness of the films. X-ray photoelectron spectroscopy (XPS) analysis indicated the films were sub stoichiometric. It was also indicated that Ti was in the form of Ti<sup>4+</sup> and Ti<sup>3+</sup> states in all films, and the proportion of Ti<sup>4+</sup> slightly increased after post-annealing at 500°C. The findings showed that post-annealing, ST and sputtering power can all affect the growth of TiO<sub>2-x</sub> films.","PeriodicalId":22062,"journal":{"name":"Surface and Interface Analysis","volume":"19 1","pages":""},"PeriodicalIF":1.7,"publicationDate":"2023-12-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"138569330","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":"Surface analysis insight note: Illustrating the effect of adventitious contamination on Pt photoemission peak intensities","authors":"Neal Fairley, Pascal Bargiela, Jonas Baltrusaitis","doi":"10.1002/sia.7276","DOIUrl":"https://doi.org/10.1002/sia.7276","url":null,"abstract":"Adventitious carbon contaminations are not only omnipresent and used for charge referencing of XPS spectra but also can alter the apparent presence of the element peaks that span over the large spectral window of binding energies. This <i>Insight</i> note describes the effect of an adventitious contamination layer on Pt and presents, in brief, the approach whereby the component spectra are derived for ion beam cleaned Pt samples that can then utilize linear mathematics to peak fit said spectra thus quantifying the amount of each component including that assigned to the contamination itself of Pt metal.","PeriodicalId":22062,"journal":{"name":"Surface and Interface Analysis","volume":"4 1","pages":""},"PeriodicalIF":1.7,"publicationDate":"2023-12-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"138536007","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":"HAXPES: Inelastic background for characterization of nanostructured materials","authors":"Sven Tougaard","doi":"10.1002/sia.7273","DOIUrl":"https://doi.org/10.1002/sia.7273","url":null,"abstract":"Analysis of the spectrum of inelastically scattered electrons in XPS has been used for decades to determine the structure of materials on the nanoscale. Using the higher photon energies available in HAXPES, the method was recently shown to determine structures rather accurately with a more than 100 nm probing depth. In this paper, these HAXPES applications are briefly reviewed. Only two parameters are required for the analysis, namely, the inelastic mean free path and the cross section for inelastic electron scattering. We also discuss in detail how these parameters are best selected.","PeriodicalId":22062,"journal":{"name":"Surface and Interface Analysis","volume":"56 1","pages":""},"PeriodicalIF":1.7,"publicationDate":"2023-11-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"138534738","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":"Selective removal of dolomite from rare earth element-bearing phosphorite by flotation and leaching and the adsorption mechanism of agents on mineral surfaces","authors":"Jun Xie","doi":"10.1002/sia.7271","DOIUrl":"https://doi.org/10.1002/sia.7271","url":null,"abstract":"The rare earth elements (REEs)-bearing phosphorite was a potential REE resource, which contained all REEs except polonium, among them lanthanide, cerium, neodymium, and yttrium were especially enriched. REEs mainly occurred in fluorapatite (Fap) and had a high positive correlation with phosphorus content. By adopting a new green environmental fatty acid collector GJBW and through one roughing and one refining reverse flotation process, all REEs were pre-enriched. The flotation concentrate was further leached with citric acid (CA), and all REEs were further enriched. The results of X-ray diffractometer (XRD), Fourier transform infrared spectroscopy (FT-IR), and X-ray photoelectron spectroscopy (XPS) showed that dolomite (Dolo) was removed and Fap was enriched in phosphorite, the selective enrichment of phosphorus and REEs was realized. Density functional theory (DFT) calculation revealed the mechanism of deep purification of REEs and phosphorus in phosphorite by CA at the micro-scale. The results showed that the number and strength of bonding between CA and Dolo (104) surface were greater than that between CA and Fap (001) surface, and CA was more easily adsorbed on Dolo (104) surface. Under the same conditions, Dolo in phosphorite was more easily leached by CA, while Fap was further enriched. This process provided a theoretical basis for the comprehensive recovery of REEs and phosphorus from phosphorite.","PeriodicalId":22062,"journal":{"name":"Surface and Interface Analysis","volume":"33 1","pages":""},"PeriodicalIF":1.7,"publicationDate":"2023-11-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"138534740","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}
Behnam Moeini, John M. Linford, Neal Gallagher, Matthew R. Linford
{"title":"Surface analysis insight note: An example of a cluster analysis of spectra from an X-ray photoelectron spectroscopy image","authors":"Behnam Moeini, John M. Linford, Neal Gallagher, Matthew R. Linford","doi":"10.1002/sia.7270","DOIUrl":"https://doi.org/10.1002/sia.7270","url":null,"abstract":"Identification of similar and dissimilar spectra is an important part of analyzing X-ray photoelectron spectroscopy (XPS) images. Cluster analysis (CA) is a commonly used exploratory data analysis (EDA) method that groups similar spectra in a data set. CA can be performed in either an agglomerative fashion, for example, using Ward's method, which involves successively linking together/clustering the most similar spectra in a data set, or in a divisive fashion, for example, using the K-means approach, which involves partitioning all the data into a specified number of clusters. In this note, we show the application of CA to an XPS image dataset. The use of Ward's method identified two major clusters in the image, where one of the clusters appeared as two subclusters. The K-means image based on two clusters agrees well with previous analyses of the same image. The average spectra corresponding to clusters helped confirm the assignments made by the CA algorithms, as did a multivariate curve resolution (MCR) analysis of the interior region identified in our cluster analysis. “Elbow” plots can help determine the number of clusters to keep in K-means clustering. The combination of the agglomerative and divisive forms of CA, where the first informs the second, can be effective in revealing the structures of XPS image datasets. The Procrustean bed is a metaphor for overfitting and underfitting in EDA.","PeriodicalId":22062,"journal":{"name":"Surface and Interface Analysis","volume":"105 1","pages":""},"PeriodicalIF":1.7,"publicationDate":"2023-11-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"138534748","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":"The effect of electrophoretic deposition of carbon nanotubes on carbon fiber on interfacial properties of the thermoplastic polyimide composite","authors":"Li Jian","doi":"10.1002/sia.7272","DOIUrl":"https://doi.org/10.1002/sia.7272","url":null,"abstract":"In order to improve the interfacial properties of carbon fiber/polyimide (CF/PI) composite, silanization reaction carbon nanotubes (CNTs) were introduced to the surface of carbon fiber by electrophoretic deposition to prepare CF/CNT/PI composite. The effects of carbon fiber surface treatment on the mechanical properties of the composites were studied. The results showed that the interlaminar shear strength and bending strength of the composite materials were increased by 11% and 9%, respectively. The scanning electron microscope and Atomic Force Microscope (AFM) was used to analyze the fine structure of composite interface phase. The results show that the introduction of CNTs creates an interface transition layer of CNTs reinforced PI resin between the fiber and the matrix.","PeriodicalId":22062,"journal":{"name":"Surface and Interface Analysis","volume":"13 7","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"2023-11-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135042704","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":"Comparing three strategies for surface treatment of Mg coated by hexamethylene diamine tetra methylene phosphonic acid for corrosion protection","authors":"Hanaa Soliman, Fatma Abdel Mouez, Hoda Hussien, Abdel Salam Makhlouf, Guojiang Wan","doi":"10.1002/sia.7269","DOIUrl":"https://doi.org/10.1002/sia.7269","url":null,"abstract":"Manufacturing Mg and Mg‐based alloys with controllable degradation rate has always been a challenge. Surface modification is one of the best ways to acquire protection against corrosion. Previously, many approaches such as phosphating (Na 3 PO 4 ), fluoridation (HF), and alkalization (NaOH) treatments have been used to regulate the corrosion rate. Here, we compare the corrosion rates of 3‐surface modified Mg samples coated with hexamethylene diamine tetra methylene phosphonic (HMDTMPA). The protection of those different layers was ranked in the order: phosphate > alkaline > fluoridation treatment. The chemistry of those chemical conversion layers was discussed in the light of scanning electron microscope (SEM), Fourier transform infrared spectroscopy (FTIR), and X‐ray photoelectron spectroscopy (XPS). The mechanism of tailoring a protective film of HMDTMPA on phosphated Mg was discussed according to the ability of P to bridge the substrate with the coating.","PeriodicalId":22062,"journal":{"name":"Surface and Interface Analysis","volume":"123 18","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"2023-11-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135136844","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":"Deep core level hard X‐ray photoelectron spectroscopy for catalyst characterization","authors":"Filippo Longo, Marin Nikolic, Andreas Borgschulte","doi":"10.1002/sia.7267","DOIUrl":"https://doi.org/10.1002/sia.7267","url":null,"abstract":"Abstract Heterogeneous catalysts are the crucial element for many catalytic processes. In most of the cases, the pivotal structure consists of catalytic metals/alloy particles supported by oxides. Knowledge of the interaction between metal and oxide is central to understand the structure–performance relationship of such systems. X‐ray photoelectron spectroscopy provides access to the chemical–physical properties of metal and oxide interface as well as polarization effects. The results are usually derived from changes of the measured binding energies based on initial state analysis. We propose to extend the analysis using photoelectron as well as Auger transition to include final state effects (Wagner/Hohlneichner plots). This gives additional information on the specific chemical neighborhood of the excited atom. Three archetypal systems are investigated by hard X‐ray photoelectron spectroscopy (HAXPES) to introduce two approaches to this analysis for the most common support elements Al and Si.","PeriodicalId":22062,"journal":{"name":"Surface and Interface Analysis","volume":"108 3","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"2023-11-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135476418","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":"Synthesis and characterization of iron sulfide immobilized on Algerian halloysite clay (HKDD3) with enhanced removal of methylene blue from aqueous medium","authors":"Asma Hayoune, Hocine Akkari, Marcello Marelli, Valeria Pappalardo, Jia Yang, Muhammad Zubair","doi":"10.1002/sia.7268","DOIUrl":"https://doi.org/10.1002/sia.7268","url":null,"abstract":"The aim of this study is to functionalize an Algerian halloysite clay (kaolin Djebel Debbagh, HKDD3) with FeS nanoparticles by employing a hydrothermal approach and exploring its ability to remove methylene blue under visible light irradiation. The FeS‐HKDD3 photocatalyst was synthesized successfully and exhibited good crystallinity. Different techniques were used to characterize the produced photocatalyst, including XRD, STEM/EDS, TEM, BET, and UV–vis DRS in order to investigate its structure, morphology, and optical performance. The HKDD3 is a natural halloysite having a tubular shape with a length ranging from 500 nm to several micrometers and a diameter that is estimated from 50 to 100 nm. The iron sulfide nanoparticles are immobilized as cube aggregates on the surface of the halloysite. The visible range displayed a strong absorption of the obtained photocatalyst, with an estimated bandgap of 1.60 eV, according to UV–vis DRS findings. The results exhibited a higher efficiency toward synergic adsorption‐photocatalytic degradation effect for methylene blue dye removal.","PeriodicalId":22062,"journal":{"name":"Surface and Interface Analysis","volume":"80 4","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"2023-11-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135539971","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}