A two-step Sol-Gel method to synthesize a ladder polymethylsilsesquioxane nanoparticles

Baatti, Abdessamad; Erchiqui, Fouad; Bébin, Philippe; Guilhot, François; Bussières, Denis

doi:10.1016/j.apt.2017.01.009

Cited by 23 publications

(26 citation statements)

References 46 publications

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“…FTIR spectra of unmodified CNCs, CNC‐1 % and CNC‐3 %, are shown in Figures a and b, while Table summarizes the characteristic FTIR's absorption bands of the samples and their related assignments. The presence of the PMSQ coating on the CNCs is evidenced from the FTIR spectra by the appearance of six characteristic absorption bands of PMSQ nanostructures . Indeed, the bands at ∼2071, 1271, 1013, 897, and 777 cm −1 can be attributed, respectively, to the stretching vibrations of CH in −Si–CH 3 , −CH 3 deformation vibrations in −Si–CH 3 , the asymmetric stretching vibration of Si–O–Si, the symmetric stretching vibration of Si–O–Si and the out‐of‐plane wagging of methyl groups in Si–CH 3 (897 and 777 cm −1 ) .…”

Section: Resultsmentioning

confidence: 99%

“…The presence of the PMSQ coating on the CNCs is evidenced from the FTIR spectra by the appearance of six characteristic absorption bands of PMSQ nanostructures . Indeed, the bands at ∼2071, 1271, 1013, 897, and 777 cm −1 can be attributed, respectively, to the stretching vibrations of CH in −Si–CH 3 , −CH 3 deformation vibrations in −Si–CH 3 , the asymmetric stretching vibration of Si–O–Si, the symmetric stretching vibration of Si–O–Si and the out‐of‐plane wagging of methyl groups in Si–CH 3 (897 and 777 cm −1 ) . The typical absorption bands of C–O cellulose bonds located at 1033 cm −1 may be substituted by the intense Si–O–cellulose band observed at 1032 cm −1 , which confirms the covalent bonding of MTMS on the surface of the CNCs.…”

Section: Resultsmentioning

confidence: 99%

“…This field of study could benefit from the development capacity of nanostructures through surfaces hydrophobization. In fact, Baatti et al have recently developed a process for the synthesis of nanostructured particles with a 15 nm diameter and from methyltrimethoxysilane (MTM) based on the sol‐gel process. Thus, MTM was hydrolyzed to form silanol groups, which condensed to form 3‐dimentional units whose structure further grew into nanoparticles of polymethylsilsesquioxane (PMSQ).…”

Section: Introductionmentioning

confidence: 99%

“…Thus, MTM was hydrolyzed to form silanol groups, which condensed to form 3‐dimentional units whose structure further grew into nanoparticles of polymethylsilsesquioxane (PMSQ). PMSQ is a ladder structure in which two chains of Si–O–Si are connected by oxane bridges . Due to this structure, PMSQ have a high thermal stability with a decomposition temperature of 380 °C.…”

Section: Introductionmentioning

confidence: 99%

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Fabrication of hydrophobic cellulose nanocrystals

Baatti

Erchiqui

Bébin³

et al. 2019

Can J Chem Eng

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An environmentally friendly procedure for the chemical modification of cellulose nanocrystals (CNCs), obtained from pine wood, was developed to manufacture hydrophobic CNCs. In comparison to other methods, this procedure has the particularity of producing a hydrophobic CNC in a single step, without using organic solvents while using MTMS as a precursor. CNCs were successfully dispersed in water, and the NMR technique was used to study the hydrolysis reaction of the MTMS in water before the surface modification of the CNCs. After 24 h of the modification reaction, the spray-drying method was used to produce a dry powder of modified CNCs. The obtained hydrophobic CNCs were characterized by several techniques. FTIR spectroscopy confirmed the covalent bonds between the MTMS and CNCs as well as the formation of nanostructured polymethylsilsesquioxane (PMSQ) on the surface of the CNCs. XPS spectroscopy examined the presence of Si atoms of the MTMS on the surface of the CNCs. XRD detected the presence of a crystalline structure of PMSQ on the surface of the CNCs and confirmed the preservation of the CNCs crystal after the modification operation. The morphology study using SEM, AFM, and TEM techniques confirmed the presence of nanostructured PMSQ on the surfaces of modified CNCs. The hydrophobic CNCs showed a significant increase in water contact angle (1108) compared to that of unmodified CNCs (438). This new way of modifying CNCs can produce hydrophobic CNCs with potential for dispersion in non-polar polymers for the formulation of new nanocomposites. Figure 15. (a) Thermogravimetric curves; and (b) DTG curves of CNC and CNC-1 % samples.

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Section: Resultsmentioning

confidence: 99%

Section: Resultsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Fabrication of hydrophobic cellulose nanocrystals

Baatti

Erchiqui

Bébin³

et al. 2019

Can J Chem Eng

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“…This work is part of the work carried out on the development of a nanocomposite family based on polymethylsilsesquioxane (PMSQ, synthetized in our previous work [ 18 ]) and a high-density polyethylene (HDPE Hival-500354 with a melt flow index of 0.03 g min-1 (ASTM D1505) and a density of 0.954 g cm-3 (ASTM D1238) was supplied by IDES Prospector North America) matrix [ 19 ]. The method for the development of HDPE–PMSQ nanocomposites is based on a fusion mixing process.…”

Section: Methodsmentioning

confidence: 99%

Reliability of Free Inflation and Dynamic Mechanics Tests on the Prediction of the Behavior of the Polymethylsilsesquioxane–High-Density Polyethylene Nanocomposite for Thermoforming Applications

et al. 2020

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Numerical modeling of the thermoforming process of polymeric sheets requires precise knowledge of the viscoelastic behavior under conjugate effect pressure and temperature. Using two different experiments, bubble inflation and dynamic mechanical testing on a high-density polyethylene (HDPE) nanocomposite reinforced with polymethylsilsesquioxane HDPE (PMSQ–HDPE) nanoparticles, material constants for Christensen’s model were determined by the least squares optimization. The viscoelastic identification relative to the inflation test seemed to be the most appropriate for the numerical study of thermoforming of a thin PMSQ–HDPE part. For this purpose, the finite element method was considered.

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Surfactant Assisted In Situ Synthesis of Nanofibrillated Cellulose/Polymethylsilsesquioxane Aerogel for Tuning Its Thermal Performance

Gupta

Sathwane

Chhajed

et al. 2022

Macromol. Rapid Commun.

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Nanofibrillated cellulose (NFC) and polymethylsilsesquioxane (PMSQ) based aerogel are prepared by the sol-gel method. The objective of this work is to study the impact of surfactant and base catalyst on the thermal and mechanical performance of the corresponding aerogel. The rheological premonitory assists in predicting the bulk properties of the aerogel. The chemical structure of the aerogel is studied by Fourier-transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and solid-state nuclear magnetic resonance (NMR). X-ray microtomographic (XMT) analysis confirms the homogeneous and monolithic structure of the aerogel. The lowest thermal conductivity is achieved as 23.21 mW m −1 K −1 with V-0 and HBF rating through UL-94 test. Thermal performance of aerogels is cross-verified through modeling and simulation in COMSOL multiphysics platform. The mechanical properties of aerogel are evaluated by monolithic compression test in axial and radial compression test up to 90% strain, cyclic compression loading-unloading, and reloading test, flexural test, and dynamic mechanical analysis. The time-temperature analysis has shown around 5 °C temperature difference in the middle of the room after using the aerogel panel at the exposed surface, which assists in the practical application of the synthesized aerogel panel.

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A two-step Sol-Gel method to synthesize a ladder polymethylsilsesquioxane nanoparticles

Cited by 23 publications

References 46 publications

Fabrication of hydrophobic cellulose nanocrystals

Fabrication of hydrophobic cellulose nanocrystals

Reliability of Free Inflation and Dynamic Mechanics Tests on the Prediction of the Behavior of the Polymethylsilsesquioxane–High-Density Polyethylene Nanocomposite for Thermoforming Applications

Surfactant Assisted In Situ Synthesis of Nanofibrillated Cellulose/Polymethylsilsesquioxane Aerogel for Tuning Its Thermal Performance

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