Carbon Black Surface Characterization by TOF-SIMS and XPS

1999 ◽  
Vol 72 (2) ◽  
pp. 384-397 ◽  
Author(s):  
P. Bertrand ◽  
L. T. Weng
Keyword(s):  
Carbon Black ◽  
Functional Groups ◽  
Surface Characterization ◽  
Secondary Ion Mass Spectrometry ◽  
Structural Information ◽  
Chemical Shifts ◽  
Molecular Ions ◽  
Chemical Information ◽  
Trace Detection ◽  
Tof Sims

Abstract The functional groups present at the carbon black (CB) surface contribute, along with the surface microstructure, to the CB surface activity which is known to be an important parameter for the rubber reinforcing properties. A direct detection of the foreign elements (H, N, O, S, Cl, …) present at the CB surface can be achieved with surface analytical techniques such as Time-of-Flight Secondary Ion Mass Spectrometry (TOF-SIMS) and X-ray Photoelectron Spectoscopy (XPS). The combination of these two techniques is found to be very fruitful. Indeed, although the TOF-SIMS sensitivity is much higher than for XPS, allowing trace detection, this technique suffers from a lack of quantification which can be fulfilled by XPS. The chemical information on the functional groups obtained by both methods is complementary. In XPS, this information is deduced from the electron core level chemical shifts which are mainly influenced by the first neighboring atoms; whereas, in TOF-SIMS, the full molecular environment can be detected. Not only information on the surface groups, but also some structural information can be obtained. Indeed, the TOF-SIMS spectra of carbon black exhibit molecular ions which are characteristic of the surface aromaticity (graphene structure) and also specific clusters at high masses which seem to be related to the basic building block of carbon black particles.

Applications of Time-OF-Flight Secondary Ion Mass Spectrometry (TOF-SIMS)

1990 ◽  
Vol 48 (2) ◽  
pp. 308-309
Author(s):  
Bruno Schueler ◽  
Robert W. Odom
Keyword(s):  
Mass Spectrometry ◽  
Secondary Ion Mass Spectrometry ◽  
Structural Information ◽  
Time Of Flight ◽  
Biological Tissues ◽  
Polymer Surfaces ◽  
Tof Sims ◽  
Secondary Ions ◽  
Ion Mass Spectrometry ◽  
Secondary Ion

Time-of-flight secondary ion mass spectrometry (TOF-SIMS) provides unique capabilities for elemental and molecular compositional analysis of a wide variety of surfaces. This relatively new technique is finding increasing applications in analyses concerned with determining the chemical composition of various polymer surfaces, identifying the composition of organic and inorganic residues on surfaces and the localization of molecular or structurally significant secondary ions signals from biological tissues. TOF-SIMS analyses are typically performed under low primary ion dose (static SIMS) conditions and hence the secondary ions formed often contain significant structural information.This paper will present an overview of current TOF-SIMS instrumentation with particular emphasis on the stigmatic imaging ion microscope developed in the authors’ laboratory. This discussion will be followed by a presentation of several useful applications of the technique for the characterization of polymer surfaces and biological tissues specimens. Particular attention in these applications will focus on how the analytical problem impacts the performance requirements of the mass spectrometer and vice-versa.

scholarly journals Exploring the geochemical distribution of organic carbon in early land plants: a novel approach

2017 ◽  
Vol 373 (1739) ◽  
pp. 20160499 ◽  
Author(s):  
Geoffrey D. Abbott ◽  
Ian W. Fletcher ◽  
Sabrina Tardio ◽  
Ethan Hack
Keyword(s):  
Mass Spectrometry ◽  
Photoelectron Spectroscopy ◽  
Plant Cell Wall ◽  
Secondary Ion Mass Spectrometry ◽  
Structural Information ◽  
Terrestrial Ecosystem ◽  
Gas Chromatography Mass Spectrometry ◽  
Fossil Plants ◽  
Tof Sims ◽  
Chromatography Mass Spectrometry

Terrestrialization depended on the evolution of biosynthetic pathways for biopolymers including lignin, cutin and suberin, which were concentrated in specific tissues, layers or organs such as the xylem, cuticle and roots on the submillimetre scale. However, it is often difficult, or even impossible especially for individual cells, to resolve the biomolecular composition of the different components of fossil plants on such a scale using the well-established coupled techniques of gas chromatography/mass spectrometry and liquid chromatography/mass spectrometry. Here, we report the application of techniques for surface analysis to investigate the composition of Rhynia gwynne-vaughanii . X-ray photoelectron spectroscopy of two different spots (both 300 µm × 600 µm) confirmed the presence of carbon. Time-of-flight secondary ion mass spectrometry (ToF-SIMS) revealed ‘chemical maps’ (imaging mode with 300 nm resolution) of aliphatic and aromatic carbon in the intact fossil that correlate with the vascular structures observed in high-resolution optical images. This study shows that imaging ToF-SIMS has value for determining the location of the molecular components of fossil embryophytes while retaining structural information that will help elucidate how terrestrialization shaped the early evolution of land plant cell wall biochemistry. This article is part of a discussion meeting issue ‘The Rhynie cherts: our earliest terrestrial ecosystem revisited’.

scholarly journals Revealing the planar chemistry of two-dimensional heterostructures at the atomic level

2015 ◽  
Vol 6 (1) ◽  
Author(s):  
Harry Chou ◽  
Ariel Ismach ◽  
Rudresh Ghosh ◽  
Rodney S. Ruoff ◽  
Andrei Dolocan
Keyword(s):  
Secondary Ion Mass Spectrometry ◽  
Structural Information ◽  
Layer Structure ◽  
Atomic Level ◽  
Chemical Information ◽  
Two Dimensional ◽  
Force Microscopy ◽  
System A ◽  
Atomic Force

Abstract Two-dimensional (2D) atomic crystals and their heterostructures are an intense area of study owing to their unique properties that result from structural planar confinement. Intrinsically, the performance of a planar vertical device is linked to the quality of its 2D components and their interfaces, therefore requiring characterization tools that can reveal both its planar chemistry and morphology. Here, we propose a characterization methodology combining (micro-) Raman spectroscopy, atomic force microscopy and time-of-flight secondary ion mass spectrometry to provide structural information, morphology and planar chemical composition at virtually the atomic level, aimed specifically at studying 2D vertical heterostructures. As an example system, a graphene-on-h-BN heterostructure is analysed to reveal, with an unprecedented level of detail, the subtle chemistry and interactions within its layer structure that can be assigned to specific fabrication steps. Such detailed chemical information is of crucial importance for the complete integration of 2D heterostructures into functional devices.

Molecular surface analysis by TOF-SIMS

1992 ◽  
Vol 50 (2) ◽  
pp. 1556-1557
Author(s):  
Robert W. Odom
Keyword(s):  
Mass Spectrometry ◽  
Surface Analysis ◽  
Secondary Ion Mass Spectrometry ◽  
Molecular Ions ◽  
Molecular Surface ◽  
Tof Sims ◽  
Ion Mass Spectrometry ◽  
Static Conditions ◽  
Primary Ions ◽  
Secondary Ion

Time-of-flight secondary ion mass spectrometry (TOF-SIMS) performs surface sensitive analysis of the elemental and molecular composition of solids. TOFSIMS is a relatively new embodiment of static secondary ion mass spectrometry (SSIMS) in which the dose of primary ions incident on the surface is typically less than 1012 ions/cm2. Since typical solid surfaces have an atomic density of 1015 atoms/cm2, this primary ion dose nominally removes less than 0.1% of a monolayer. Hence, SIMS analyses performed under these static conditions represent near surface analysis in which secondary ions are produced from the top few monolayers of the surface. The actual sampling depth is determined by the primary ion momentum, angle of incidence and chemistry of the surface. Since low dose primary ions cause minimal perturbation of the chemistry of the solid surface, SSIMS analyses often produce molecular or pseudo-molecular ions characteristic of the chemical composition of the surface. Thus, molecular ions or structurally significant fragment ions are often observed in SSIMS analyses of surfaces containing inorganic and organic residues, polymers surfaces, coatings, and biological materials such as tissues and membranes.

Surface Characterization of Rubber by Secondary Ion Mass Spectrometry

1989 ◽  
Vol 62 (4) ◽  
pp. 656-682 ◽  
Author(s):  
W. J. van Ooli ◽  
M. Nahmias
Keyword(s):  
Surface Characterization ◽  
Structural Changes ◽  
Secondary Ion Mass Spectrometry ◽  
Structural Information ◽  
Great Promise ◽  
Related Data ◽  
Organic Sulfides ◽  
Secondary Ion ◽  
Oxidation Wear

Abstract It has been demonstrated that static SIMS is potentially a very useful technique for the characterization of rubber surfaces. Its major capability is to provide molecular structural information of the polymer in addition to elemental analysis, which would also be possible with other surface techniques such as XPS or AES. The SIMS spectra are in many cases highly characteristic, and they can be used to identify the type and structure of the hydrocarbon polymer. In addition, structural changes in the rubber surface can be detected, and very useful information on the types and amounts of sulfur crosslinks can be obtained as well, as has been published elsewhere. Therefore, the technique shows great promise as a tool for the study of surface-related rubber phenomena, such as oxidation, wear, tack, antiozonant and antioxidant performance and mechanisms, and also for the study of the adhesion between dissimilar rubbers or between rubbers and other materials, such as metals. Before SIMS can be routinely used in rubber laboratories, a considerable amount of basic and fundamental work will have to be done because the spectra of many materials are not known, and they cannot always be predicted either. Therefore, a rubber-related data base will have to be built up with well-characterized polymers but also using clean films of various rubber additives. Crosslinking studies will have to be confirmed with compounds of known crosslink structures, e.g., by using different polymers, different types of accelerators, and a series of model compounds of organic sulfides.

scholarly journals The Interface Characterization of 2-Mercapto-1-methylimidazole Corrosion Inhibitor on Brass

Coatings ◽  
2021 ◽  
Vol 11 (3) ◽  
pp. 295
Author(s):  
Matjaž Finšgar
Keyword(s):  
Surface Layer ◽  
Corrosion Inhibitor ◽  
Photoelectron Spectroscopy ◽  
Related Species ◽  
Surface Characterization ◽  
Secondary Ion Mass Spectrometry ◽  
Ion Beam ◽  
Xps Analysis ◽  
Spectral Interferences ◽  
Tof Sims

This work presents a detailed surface analytical study and surface characterization, with an emphasis on the X-ray photoelectron spectroscopy (XPS) and time-of-flight secondary ion mass spectrometry (ToF-SIMS) analyses of 2‑mercapto‑1‑methylimidazole (MMI) as a corrosion inhibitor for brass. First, the electrochemical measurements demonstrated a corrosion inhibition effect of MMI in a 3 wt.% NaCl solution. Next, the formation of the MMI surface layer and its properties after 1 month of immersion was analyzed with attenuated total reflectance–Fourier-transform infrared spectroscopy, atomic force microscopy, field-emission scanning electron microscopy, and contact angle analysis. Moreover, to gradually remove the organic surface layer, a gas cluster ion beam (GCIB) sputtering source at different accelerated voltages and cluster sizes was employed. After each sputtering cycle, a high-resolution XPS analysis was performed. Moreover, an angle‑resolved XPS analysis was carried out for the MMI-treated brass sample to analyze the heterogeneous layered structure (the interface of the MMI organic/inorganic brass substrate). The interface properties were also investigated in detail using ToF-SIMS for spectra measurements and 2D imaging. Special attention was devoted to the possible spectral interferences for MMI‑related species. The thermal stability of different MMI-related species using molecular-specific signals without possible spectral interferences was determined by performing a cooling/heating experiment associated with ToF-SIMS measurements. It was shown that these species desorbed from the brass surface in the temperature range of 310–370 °C.

scholarly journals Chemical Separation on Silver Nanorods Surface Monitored by TOF-SIMS

2017 ◽  
Vol 2017 ◽  
pp. 1-6
Author(s):  
Ondrej Petruš ◽  
Andrej Oriňak ◽  
Renáta Oriňaková ◽  
Christian Muhmann ◽  
Ján Macko ◽  
...  
Keyword(s):  
Secondary Ion Mass Spectrometry ◽  
Rhodamine 6G ◽  
Chemical Separation ◽  
Molecular Ions ◽  
Chemical Components ◽  
Sampling Point ◽  
Self Assembled Monolayer ◽  
Component Mixture ◽  
Silver Nanorods ◽  
Tof Sims

The article introduces a possible chemical separation of a mixture of two compounds on the metal nanorods surface. A silver nanorods surface has been prepared by controlled electrochemical deposition in anodic alumina oxide (AAO) template. Rhodamine 6G and 4-aminothiophenol have been directly applied to the sampling point on a silver nanorods surface in an aliquot mixture. The position of the resolved compounds was analysed by time-of-flight secondary ion mass spectrometry (TOF-SIMS) which measured the fragments and the molecular ions of the two compounds separated on the silver nanorods surface. Rhodamine 6G has been preconcentrated as 1.5 mm radial from the sampling point while 4-aminothiophenol formed a continuous self-assembled monolayer on the silver nanorods surface with a maximum molecular ion intensity at a distance of 0.5 mm from the sampling point. The separation of the single chemical components from the two-component mixture over the examined silver nanostructured films could clearly be shown. A fast separation on the mentioned nanotextured films was observed (within 50 s). This procedure can be easily integrated into the micro/nanofluidic systems or chips and different detection systems can be applied.

scholarly journals Quantitative Analysis of Blended Asian Lacquers Using ToF–SIMS, Py–GC/MS and HPLC

Polymers ◽  
2020 ◽  
Vol 13 (1) ◽  
pp. 97
Author(s):  
Hye Hyun Yu ◽  
Jung-Ah Lim ◽  
Seung Wook Ham ◽  
Kang-Bong Lee ◽  
Yeonhee Lee
Keyword(s):  
Mass Spectrometry ◽  
High Performance ◽  
Quantitative Methods ◽  
Secondary Ion Mass Spectrometry ◽  
Structural Information ◽  
Complex Mixture ◽  
Gas Chromatography Mass Spectrometry ◽  
Linear Calibration ◽  
Pyrolysis Gas ◽  
Tof Sims

Asian lacquer is a special polymeric material tapped from lacquer trees. The tree’s sap is a complex mixture of compounds, such as catechol lipids, polysaccharides, glycoproteins, enzymes, and water. Researchers have not yet quantitatively analyzed blended lacquers. We evaluated the compositions of Japanese and Vietnamese lacquers, and blends of the two, using time-of-flight secondary ion mass spectrometry (ToF–SIMS), pyrolysis–gas chromatography/mass spectrometry (Py–GC/MS), and high-performance liquid chromatography (HPLC). ToF–SIMS provided quantitative results for blended lacquers; provided structural information on polymeric lacquer films; and indicated the presence of dimers of urushiol–urushiol, urushiol–laccol, and laccol–laccol derivatives. We used Py–GC/MS and HPLC to obtain linear calibration curves. The specific peak intensity was a linear function of the ratio of Japanese to Vietnamese lacquer in the blends. For an unknown mixture, all three techniques gave essentially the same results. These quantitative methods will be useful for improving the physical properties of polymeric lacquer films, and evaluating the lacquer quality in industry and historic conservation.

Surface characterization of a rosin sizing agent in paper by means of EPMA, ESCA and TOF-SIMS

1997 ◽  
Vol 12 (4) ◽  
pp. 260-266 ◽  
Author(s):  
Yasushi Ozaki ◽  
Atsushi Sawatari
Keyword(s):  
Surface Layer ◽  
Surface Characterization ◽  
Osmium Tetroxide ◽  
Secondary Ion Mass Spectrometry ◽  
Pulp Fiber ◽  
Fragment Ions ◽  
Tof Sims ◽  
Micro Analysis ◽  
Secondary Ion

Abstract EPMA(e1ectronprobe micro analysis), ESCA (electron spectroscopy for chemical analysis) and TOF-SIMS (time of flight type secondary ion mass spectrometry) were used to detect the distribution of a rosin sizing agent in paper. For EPMA we labelled paper samples with osmium tetroxide which enabled the detection of rosin in the XY direction of the paper sheet. For ESCA we labelled paper samples with fluorine which also enabled the detection of rosin. At the same time, the ESCA angle-dependent technique was used to obtain depth profiles of the rosin. Also, distribution images of rosin on an extremely thin ( 1 nm) surface layer were made observable by monitoring fragment ions from the rosin with TOF-SIMS. By using EPMA, a notable difference in rosin distribution was shown on the pulp fiber. However, according to the TOF-SIMS examination, the rosin was shown to be distributed relatively even in an extremely thin surface layer. The ESCA angle- dependent technique showed that rosin was present mainly on the outer surface layer.

Determination of chemical composition in multilayer polymer film using ToF-SIMS

2018 ◽  
Vol 10 (21) ◽  
pp. 2444-2449 ◽  
Author(s):  
Chuanzhen Zhou ◽  
Dayong Sun ◽  
Roberto Garcia ◽  
Fred A. Stevie
Keyword(s):  
Mass Spectrometry ◽  
Chemical Composition ◽  
Polymer Film ◽  
Secondary Ion Mass Spectrometry ◽  
Chemical Information ◽  
Analytical Technique ◽  
Tof Sims ◽  
Surface Analytical Technique ◽  
Secondary Ion

Time-of-flight secondary ion mass spectrometry is a widely used surface analytical technique, which can provide chemical information from both the uppermost surface and underneath the surface for various materials.

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