Comparison of techniques for determining crosslinking in silane-water crosslinked materials

Sirisinha, Kalyanee; Chimdist, Sirinya

doi:10.1016/j.polymertesting.2006.01.015

Cited by 53 publications

(43 citation statements)

References 16 publications

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“…After extraction, samples were weighted before and after drying in a vacuum oven at 60 ºC until constant weight. Equation 1 shows the calculation of gel content of crosslinked samples 22 .…”

Section: Gel Contentmentioning

confidence: 99%

Silane Crosslinked Polyethylene from Different Commercial PE’s: Influence of Comonomer, Catalyst Type and Evaluation of HLPB as Crosslinking Coagent

2015

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Section: Gel Contentmentioning

confidence: 99%

Silane Crosslinked Polyethylene from Different Commercial PE’s: Influence of Comonomer, Catalyst Type and Evaluation of HLPB as Crosslinking Coagent

2015

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“…According to the literature procedure [26,27], the gel content measurements were carried out to evaluate the overall water-crosslinking reaction in EPR-g-VTMS system. Water-crosslinked EPR-g-VTMS samples in a glass wool filter were put into boiling xylene for 12 hours in a Soxhlet extractor apparatus.…”

Section: 1mentioning

confidence: 99%

The utility of sulfonic acid catalysts for silane water-crosslinked network formation in the ethylene–propylene copolymer system

Adachi

Hirano²

2008

J Sol-Gel Sci Technol

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Catalytic effects of Brönsted acid on the early kinetics of water-crosslinking reaction in the vinyltrimethoxysilane-grafted ethylene-propylene copolymer (EPR-g-VTMS) system were investigated by means of an attenuated total reflectance-Fourier transform infrared (ATR-FTIR) technique and gel fraction measurements. Four sulfonic acids with different substituent, including methanesulfonic acid (C1SO 3 H), 1-propanesulfonic acid (C3SO 3 H), 1-pentanesulfonic acid (C5SO 3 H), and dodecylbenzenesulfonic acid (C12PhSO 3 H), were selected to examine the progress and effect of progressive changes in the silane watercrosslinked network structure in comparison with a primary amine (n-octadecylamine, Lewis base). From the kinetic analysis using Arrhenius equation, we found that the frequency factors for both hydrolysis (ATR-FTIR) and condensation step (gel content) of EPR-g-VTMS decreased in the order of C1SO 3 H > C3SO 3 H > C5SO 3 H > C12PhSO 3 H, while the activation energy values for each reaction did not differ significantly.These relationships can be explained mainly on the basis of the diffusion factors of the sulfonic acids in EPRg-VTMS system. Moreover, the stress-strain curve comparison between water-crosslinked EPR-g-VTMS samples containing sulfonic acid and amine compound clearly indicated the difference in their tensile properties as a result of the catalyst variation; the use of sulfonic acid as water-crosslinking catalyst eventually achieves to the soft and tough water-crosslinked EPR-g-VTMS, while the hard and strong one was produced using amine catalyst. Not only the catalytic activity but also the type of the catalyst has eventually significant effects upon the physical properties of the water-crosslinked EPR-g-VTMS.3/32

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“…Heat treatment and rinsing at 80°C water improved bond strength between organic to inorganic elements after water storage or thermocycling compared to those groups that did not receive any postheat treatment [6,7,9,15,22,24,25]. The curing temperature and the boiling point of the silanes may vary between silanes.…”

Section: Discussionmentioning

confidence: 98%

“…FT-IR spectra can be used to provide useful information about the presence or absence of functional groups [4,7,21,23,24].…”

Section: Discussionmentioning

confidence: 99%

Surface characterization of feldspathic ceramic using ATR FT-IR and ellipsometry after various silanization protocols

et al. 2012

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OBJECTIVES: This study characterized the feldspathic ceramic surfaces after various silanization protocols. METHODS: Ceramic bars (2 mm × 4 mm × 10 mm) (N = 18) of feldpathic ceramic (VM7, VITA Zahnfabrik) were manufactured and finished. Before silane application, the specimens were ultrasonically cleaned in distilled water for 10 min. The ceramic specimens were randomly divided into nine groups (N = 2 per group) and were treated with different silane protocols. MPS silane (ESPE-Sil, 3M ESPE) was applied to all specimens and left to react at 20°C for 2 min (G20). After drying, the specimens were subjected to heat treatment in an oven at 38°C (G38), 79°C (G79) or 100°C (G100) for 1 min. Half of the specimens of each group were rinsed with water at 80°C for 15s (G20B, G38B, G79B, G100B). The control group (GC) received no silane. Attenuated total reflection infrared Fourier transform analysis (ATR FT-IR) was performed using a spectrometer. Thickness of silane layer was measured using a spectroscopic ellipsometer working in the = 632.8 nm (He-Ne laser) at 70°incidence angle. Surface roughness was evaluated using an optical profilometer. Specimens were further analyzed under the Scanning Electron Microscopy (SEM) to observe the topographic patterns. RESULTS: ATR FT-IR analysis showed changes in Si-O peaks with enlarged bands around 940 cm(-1). Ellipsometry measurements showed that all post-heat treatment actions reduced the silane film thickness (30.8-33.5 nm) compared to G20 (40 nm). The groups submitted to rinsing in hot water (B groups) showed thinner silane films (9.8-14.4 nm) than those of their corresponding groups (without washing) (30.8-40 nm). Profilometer analysis showed that heat treatments (Ra 0.10-0.19 m; Rq 0.15-0.26 m) provided a smoother surface than the control group (Ra 0.48 m; Rq 0.65 m). Similar patterns were also observed in SEM images. SIGNIFICANCE: Heat treatment after MPS silane application improved the silane layer network. Rinsing with boiling water eliminated the outmost unreacted regions of the silane yielding to thinner film thicknesses. ABSTRACTObjectives. This study characterized the feldspathic ceramic surfaces after various silanization protocols.Methods. Ceramic bars (2 mm x 4 mm x 10 mm) (N=18) of feldpathic ceramic (VM7, VITA Zahnfabrik) were manufactured and finished. Before silane application, the specimens were ultrasonically cleaned in distilled water for 10 min. The ceramic specimens were randomly divided into nine groups (n=2 per group) and were treated with different silane protocols. MPS silane (ESPE-Sil, 3M ESPE) was applied to all specimens and left to react at 20°C for 1 min (G20). After drying, the specimens were subjected to heat treatment in an oven at 38°C (G38), 79°C (G79) or 100°C (G100) for 1 min. Half of the specimens of each group were rinsed with water at 38°C, 79°C, 100°C for 15 s (G38B, G79B, G100B). The control group (GC) received no silane. Attenuated total reflection infrared Fourier transform analysis (ATR FT-IR) was performed using a spectrom...

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Comparison of techniques for determining crosslinking in silane-water crosslinked materials

Cited by 53 publications

References 16 publications

Silane Crosslinked Polyethylene from Different Commercial PE’s: Influence of Comonomer, Catalyst Type and Evaluation of HLPB as Crosslinking Coagent

Silane Crosslinked Polyethylene from Different Commercial PE’s: Influence of Comonomer, Catalyst Type and Evaluation of HLPB as Crosslinking Coagent

The utility of sulfonic acid catalysts for silane water-crosslinked network formation in the ethylene–propylene copolymer system

Surface characterization of feldspathic ceramic using ATR FT-IR and ellipsometry after various silanization protocols

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