Quantitative ToF‐SIMS analysis of monomers, oxidation and trace elements in EPDM gels

Galuska, A. A.

doi:10.1002/sia.954

Cited by 12 publications

(7 citation statements)

References 17 publications

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“…The positive ion spectra of the studied sample surfaces are shown in Figure . As expected, the spectrum of the untreated EPDM surface shows mainly hydrocarbon ion fragments related to ethylene, propylene, and ENB, such as C 2 H 3 + (27 m / z ), C 3 H 5 + (41 m / z ), C 4 H 7 + (55 m / z ), and C 7 H 4 + (88 m / z ) . In addition, a small amount of zinc (Zn + , 64 m / z ) was detected, which is related to the used catalyst ZnO.…”

Section: Resultssupporting

confidence: 68%

“…As expected, the spectrum of the untreated EPDM (88 m/z). 37 In addition, a small amount of zinc (Zn + , 64 m/z) was detected, which is related to the used catalyst ZnO. The positive ion spectrum of EPDM−TEOS looks very similar to the spectrum of the uncoated sample and shows many ion fragments that are associated with EPDM-related hydrocarbons.…”

Section: ■ Results and Discussionmentioning

confidence: 92%

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Surface Modification of Ethylene Propylene Diene Terpolymer Rubber by Plasma Polymerization Using Organosilicon Precursors

Karl

Rahimi

Kubowicz

et al. 2020

ACS Appl. Polym. Mater.

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The effect of atmospheric pressure plasma-enhanced chemical vapor deposition on ethylene propylene diene terpolymer (EPDM) with the precursors hexamethyldisiloxane (HMDSO) and tetraethyl orthosilicate (TEOS) on roughness, chemical composition, as well as wetting and friction properties has been investigated. For the first time, topography analyses like scanning electron microscopy, white light interferometry, digital microscopy, as well as surface analytical methods by using X-ray photoelectron spectroscopy (XPS) and time-of-flight secondary ion mass spectrometry (ToF-SIMS) were combined with contact angle and friction experiments to obtain a detailed analysis of plasma polymer surfaces. This work shows that different plasma coatings can be utilized to tailor wettability and surface energies and reduce friction of EPDM rubber, which are important for various applications. Wettability investigations have shown that both coatings are more polar compared to the untreated surface but less polar than the surface-activated EPDM without precursors. The carbon content decreased, and the content of oxygen and silicon increased after plasma polymerization, as shown by XPS investigations. ToF-SIMS investigations have revealed that the ion spectra of both coatings are very similar with a comparable surface chemistry. A lower penetration depth is considered for the contact angle measurements in contrast to the other surface-sensitive methods. The surface energy of the activated EPDM surface without precursors increases significantly compared to the untreated EPDM because of the incorporation of polar groups in the elastomer surface. Both coatings with the corresponding precursors also have a higher surface energy compared to the uncoated EPDM, whereas the TEOS coating reveals a higher surface energy than the HMDSO coating. However, both coatings have lower surface energies than the activated EPDM. The coefficient of friction and the stick−slip phenomenon can be significantly reduced using plasma polymer coatings based on organosilicon precursors sliding on glass substrates. The lowest friction values with the absence of stick−slip on EPDM were achieved by using the precursor TEOS as the friction partner.

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Section: Resultssupporting

confidence: 68%

Section: ■ Results and Discussionmentioning

confidence: 92%

Surface Modification of Ethylene Propylene Diene Terpolymer Rubber by Plasma Polymerization Using Organosilicon Precursors

Karl

Rahimi

Kubowicz

et al. 2020

ACS Appl. Polym. Mater.

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“…TOF‐SIMS is a technique based on mass spectrometry and is therefore said not to be a quantitative technique. However, in spite of TOF‐SIMS not being a quantitative technique in principle, many workers have made extensive efforts to find ways to use TOF‐SIMS quantitatively 12–62. Whether or not TOF‐SIMS can be said to be quantitative is still debated.…”

Section: Introductionmentioning

confidence: 99%

Quantification of grafted poly(ethylene glycol)‐silanes on silicon by time‐of‐flight secondary ion mass spectrometry

et al. 2002

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Silicon grafted monodisperse poly(ethylene glycol) (PEG) silanes with various PEG chain lengths and mixtures of these were systematically analyzed with static time-of-flight secondary ion mass spectrometry (TOF-SIMS). The mass spectra show differences in the various relative signal intensities, an observation that was used to elucidate important aspects of the grafting process. The relationship between PEG-silane fragment ion abundances and Si(+) ion abundances were used to (i) qualitatively describe layer thicknesses of grafted mixtures of PEG-silanes on silicon, (ii) construct a calibration curve from which PEG chain length (or molecular mass) can be determined and (iii) quantitatively determine surface mixture compositions of grafted monodisperse PEG-silanes of different chain lengths (3, 7 and 11 PEG units). The results suggest that discrimination does take place in the adsorption process. The PEG-silane with the shorter PEG chain is discriminated for mixtures containing PEG3-silane, whereas the PEG-silane with the longer PEG chain is discriminated in PEG7/PEG11-silane mixtures. The origin of this difference in adsorption behavior is not well understood. Aspects of the grafting process and the TOF-SIMS analyses are discussed.

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“…Many of these multicomponent/multiphase systems have interfaces between chemically distinct phases that need to be probed structurally and chemically at the relevant length scales to develop strategies for enhancement and eventual deconstruction of the interfaces. Currently, time-of-flight secondary ion mass spectrometry (ToF-SIMS) that offers excellent surface sensitivity, high mass resolution, and breadth of mass and fragment detection is the primary tool for chemical visualization of polymeric interfaces. − As such, research has primarily been focused on characterization of copolymers and polymer blends using ToF-SIMS. − ToF-SIMS has been used to investigate surface chemistry, interfaces, and microscopic phases and to quantitatively map surface-specific polymers in blends including styrene-methyl methacrylate random copolymers, ethylene–propylene–diene terpolymers, and polypropylene/ethylene–propylene copolymer blends − as well as to determine the molecular weight for a variety of polymers including PE, PP, and polystyrene (PS) …”

Section: Introductionmentioning

confidence: 99%

Helium Ion Microscopy with Secondary Ion Mass Spectrometry for Nanoscale Chemical Imaging and Analysis of Polyolefins

Ovchinnikova

Borodinov

Trofimov

et al. 2021

ACS Appl. Polym. Mater.

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To date, chemical imaging of polymers and polymer blends has been primarily accomplished using time-of-flight secondary ion mass spectrometry (ToF-SIMS) to directly visualize the distribution of components in a complex material with spatial resolution ranging from 100 nm to 5 μm. However, in many cases, this resolution falls far short of visualizing interfaces directly. To overcome these limitations, recent work has focused on developing a SIMS detection system based on a helium ion microscope (HIM) enabling chemical imaging with a demonstrated ∼14 nm spatial resolution. Here, we utilize HIM-SIMS for differentiation between the olefin-based polymers of polyethylene (PE) and polypropylene (PP). We illustrate both analyses for separating PE and PP using specific mass fragment ratios as well as demonstrate spatially resolved imaging of phase-separated domains within PE. Overall, we demonstrate the abilities of HIM-SIMS as a multimodal chemical technique for imaging and quantification of polyolefin interfaces, which could be more broadly applied to the analysis of more complex polymeric systems.

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Quantitative ToF‐SIMS analysis of monomers, oxidation and trace elements in EPDM gels

Cited by 12 publications

References 17 publications

Surface Modification of Ethylene Propylene Diene Terpolymer Rubber by Plasma Polymerization Using Organosilicon Precursors

Surface Modification of Ethylene Propylene Diene Terpolymer Rubber by Plasma Polymerization Using Organosilicon Precursors

Quantification of grafted poly(ethylene glycol)‐silanes on silicon by time‐of‐flight secondary ion mass spectrometry

Helium Ion Microscopy with Secondary Ion Mass Spectrometry for Nanoscale Chemical Imaging and Analysis of Polyolefins

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