scholarly journals Preparation and Characterization of Transparent Polyimide–Silica Composite Films Using Polyimide with Carboxylic Acid Groups

Polymers ◽  
2019 ◽  
Vol 11 (3) ◽  
pp. 489 ◽  
Author(s):  
Kwan Moon ◽  
Boknam Chae ◽  
Ki Kim ◽  
Seung Lee ◽  
Young Jung
Keyword(s):  
Thermal Stability ◽  
Carboxylic Acid ◽  
Coefficient Of Thermal Expansion ◽  
Condensation Reaction ◽  
Sol Gel ◽  
Composite Films ◽  
Amic Acid ◽  
Good Thermal Stability ◽  
Silica Composite ◽  
Sol Gel Process

Polyimide (PI) composite films with thicknesses of approximately 100 µm were prepared via a sol–gel reaction of 3-aminopropyltrimethoxysilane (APTMS) with poly(amic acid) (PAA) composite solutions using a thermal imidization process. PAA was synthesized by a conventional condensation reaction of two diamines, 3,5-diaminobenzoic acid (DABA), which has a carboxylic acid side group, and 2,2′-bis(trifluoromethyl)benzidine (TFMB), with 4,4′-(hexafluoroisopropylidene)diphthalic anhydride (6FDA) in N,N-dimethylacetamide (DMAc). The PAA–silica composite solutions were prepared by mixing PAA with carboxylic acid side groups and various amounts of APTMS in a sol–gel process in DMAc using hydrochloric acid as a catalyst. The obtained PI–silica composite films showed relatively good thermal stability, and the thermal stability increased with increasing APTMS content. The optical properties and in-plane coefficient of thermal expansion (CTE) values of the PI–silica composite films were investigated. The CTE of the PI–silica composite films changed from 52.0 to 42.1 ppm/°C as the initial content of APTMS varied. The haze values and yellowness indices of the composite films increased as a function of the APTMS content.

scholarly journals Facile Synthesis of Methylsilsesquioxane Aerogels with Uniform Mesopores by Microwave Drying

2019 ◽  
Author(s):  
Xingzhong Guo ◽  
Jiaqi Shan ◽  
Wei Lei ◽  
Ronghua Ding ◽  
Yun Zhang ◽  
...  
Keyword(s):  
Thermal Stability ◽  
Production Efficiency ◽  
Sol Gel ◽  
Microwave Drying ◽  
Remarkable Effect ◽  
Good Thermal Stability ◽  
Pore Structures ◽  
Sol Gel Process ◽  
20 Nm ◽  
Uniform Mesopores

Methylsilsesquioxane aerogels with uniform mesopores have been facilely prepared via a sol–gel process followed by microwave drying with methyltrimethoxysilane (MTMS) as precursor, hydrochloric acid (HCl) as catalyst, water and methanol as solvents, hexadecyltrimethylammonium chloride (CTAC) as surfactant and template and propylene oxide (PO) as gelation agent. The microstructure, chemical composition and pore structures of the resultant MSQ aerogels were investigated in detail to achieve controllable preparation of MSQ aerogels, and the thermal stability of MSQ aerogels was also analyzed. The gelation agent, catalyst, solvent and microwave power have important roles on pore structures of MSQ aerogels. Meanwhile, microwave drying method is found to not only have a remarkable effect on improving production efficiency, but also be conducive to avoid the collapse of pore structure especially micropores during drying. The resulting MSQ aerogel microwave-dried at 500 W possesses a specific surface area up to 821 m2/g and a mesopore size of 20 nm, and displays good thermal stability.

scholarly journals Facile Synthesis of Methylsilsesquioxane Aerogels with Uniform Mesopores by Microwave Drying

Polymers ◽  
2019 ◽  
Vol 11 (2) ◽  
pp. 375 ◽  
Author(s):  
Xingzhong Guo ◽  
Jiaqi Shan ◽  
Wei Lei ◽  
Ronghua Ding ◽  
Yun Zhang ◽  
...  
Keyword(s):  
Thermal Stability ◽  
Production Efficiency ◽  
Sol Gel ◽  
Microwave Drying ◽  
Remarkable Effect ◽  
Good Thermal Stability ◽  
Pore Structures ◽  
Sol Gel Process ◽  
20 Nm ◽  
Uniform Mesopores

Methylsilsesquioxane (MSQ) aerogels with uniform mesopores were facilely prepared via a sol–gel process followed by microwave drying with methyltrimethoxysilane (MTMS) as a precursor, hydrochloric acid (HCl) as a catalyst, water and methanol as solvents, hexadecyltrimethylammonium chloride (CTAC) as a surfactant and template, and propylene oxide (PO) as a gelation agent. The microstructure, chemical composition, and pore structures of the resultant MSQ aerogels were investigated in detail to achieve controllable preparation of MSQ aerogels, and the thermal stability of MSQ aerogels was also analyzed. The gelation agent, catalyst, solvent, and microwave power have important roles related to the pore structures of MSQ aerogels. Meanwhile, the microwave drying method was found to not only have a remarkable effect on improving production efficiency, but also to be conducive to avoiding the collapse of pore structure (especially micropores) during drying. The resulting MSQ aerogel microwave-dried at 500 W possessed a specific surface area up to 821 m2/g and a mesopore size of 20 nm, and displayed good thermal stability.

AO-resistant shape memory polyimide/silica composites with excellent thermal stability and mechanical properties

RSC Advances ◽  
2015 ◽  
Vol 5 (89) ◽  
pp. 72971-72980 ◽  
Author(s):  
Zenghui Yang ◽  
Qihua Wang ◽  
Yongkang Bai ◽  
Tingmei Wang
Keyword(s):  
Mechanical Properties ◽  
Thermal Stability ◽  
Shape Memory ◽  
Composite Films ◽  
Excellent Thermal Stability ◽  
Good Thermal Stability ◽  
Silica Composite

Shape memory polyimide/silica composite films show AO-resistant performance, good thermal stability and mechanical properties.

The Preparation and Photocatalytic Activity of SWNTs Doped ZnO/TiO2 Compound Films

2010 ◽  
Vol 97-101 ◽  
pp. 1611-1615 ◽  
Author(s):  
Qing Wang ◽  
Xin Li Li ◽  
Wei Nie ◽  
Yong Mei Xia ◽  
Jian Feng Dai
Keyword(s):  
Photocatalytic Activity ◽  
Absorption Spectra ◽  
Sol Gel ◽  
Composite Films ◽  
Wavelength Region ◽  
Tio2 Films ◽  
X Ray Diffraction ◽  
Sol Gel Process ◽  
Doped Zno ◽  
Walled Carbon Nanotubes

The ZnO/TiO2 composite films were deposited over glass using spin coating technique by sol-gel process. Single-walled carbon nanotubes (SWNTs) were used to modify the ZnO/TiO2 films successfully in this paper. The structure and composition of the ZnO/TiO2 composite and SWNTs doped ZnO/TiO2 composite were characterized by X-ray diffraction (XRD). The morphology of samples was characterized by scanning electron microscopy (SEM). The photocatalytic activity was investigated by photocatalytic degradation of aqueous methyl orange under ultraviolet (UV) radiation. The UV-vis absorption spectra of the ZnO/TiO2 films and SWNTs doped ZnO/TiO2 films in the wavelength region 200~800 nm were obtained. The results indicate that the SWNTs addition can decrease the grain size of ZnO/TiO2, which can enhance the photocatalytic activity. UV-vis absorption spectra of SWNTs-ZnO/TiO2 showed obvious blue shifts compared with ZnO/TiO2. The optimal amount of doping SWNTs is 1% according to this research. The enhanced mechanism of the SWNTs for the photocatalytic activity in ZnO/TiO2 films was analyzed in this article.

scholarly journals Preparation and Characteristics of an Environmentally Friendly Hyperbranched Flame-Retardant Polyurethane Hybrid Containing Nitrogen, Phosphorus, and Silicon

Polymers ◽  
2019 ◽  
Vol 11 (4) ◽  
pp. 720 ◽  
Author(s):  
Chen ◽  
Chiang
Keyword(s):  
Thermal Stability ◽  
Flame Retardant ◽  
Hybrid Material ◽  
Functional Group ◽  
Condensation Reaction ◽  
Sol Gel ◽  
Decomposition Temperature ◽  
Limiting Oxygen Index ◽  
Raman Analysis ◽  
Ring Opening Reaction

The NCO functional group of 3-isocyanatoproplytriethoxysilane (IPTS) and the OH functional group of 10-(2,5-dihydroxyphenyl)-10H-9-oxa-10-phospha-phenantbrene-10-oxide (DOPO-BQ) were used to conduct an addition reaction. Following completion of the reaction, triglycidyl isocyanurate (TGIC) was introduced to conduct a ring-opening reaction. Subsequently, a sol–gel method was used to initiate a hydrolysis–condensation reaction on TGIC–IPTS–DOPO-BQ to form a hyperbranched nitrogen–phosphorous–silicon (HBNPSi) flame retardant. This flame retardant was incorporated into a polyurethane (PU) matrix to prepare a hybrid material. Fourier-transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), limiting oxygen index (LOI), UV-VIS spectrophotometry, and Raman analysis were conducted to characterize the structure and analyze the transparency, thermal stability, flame retardancy, and residual char to understand the flame retardant mechanism of the prepared hybrid material. After the flame retardant was added, the maximum degradation rate decreased from −36 to −17 wt.%/min, the integral procedural decomposition temperature (IPDT) increased from 348 to 488 °C, and the char yield increased from 0.7 to 8.1 wt.%. The aforementioned results verified that the thermal stability of PU can be improved after adding HBNPSi. The LOI analysis indicated that the pristine PU was flammable because the LOI of pristine PU was only 19. When the content of added HBNPSi was 40%, the LOI value was 26; thus the PU hybrid became nonflammable.

Synthesis and properties of low coefficient of thermal expansion copolyimides derived from biphenyltetracarboxylic dianhydride with p-phenylenediamine and 4,4′-oxydialinine

e-Polymers ◽  
2016 ◽  
Vol 16 (4) ◽  
pp. 295-302 ◽  
Author(s):  
Yonglin Lei ◽  
Yuanjie Shu ◽  
Jinhua Peng ◽  
Yongjian Tang ◽  
Jichuan Huo
Keyword(s):  
Thermal Stability ◽  
Thermal Expansion ◽  
Coefficient Of Thermal Expansion ◽  
Thermomechanical Analysis ◽  
Amic Acid ◽  
Molar Ratio ◽  
Structure And Property ◽  
Property Relations ◽  
Ft Ir ◽  
Biphenyltetracarboxylic Dianhydride

AbstractA series of copolyimides were prepared by thermal imidization of poly(amic acid)s (PAAs) derived from 3,3′,4,4′-biphenyltetracarboxylic dianhydride (s-BPDA), 2,3′,3,4′-biphenyltetracarboxylic dianhydride (a-BPDA), p-phenylenediamine (PDA) and 4,4′-oxydialinine (4,4′-ODA) commonly used for the production of commercial polyimides. The flexible copolyimide films were obtained from that the molar ratio of s-BPDA, a-BPDA, PDA and 4,4′-ODA was 9:1:8:2 (Co-PIs-3), 8:2:9:1 (Co-PIs-5) and 8:2:8:2 (Co-PIs-6). These obtained copolyimide films were characterized by Fourier transform-infrared spectroscopy(FT-IR), wide angle X-ray (WAXD), Thermogravimetric (TG), dynamic mechanical thermal analysis (DMA), thermomechanical analysis (TMA), field-emission scanning electron microscopy (FE-SEM) and mechanical properties measurement. The results showed that three copolyimides remained semi-crystalline and exhibited high glass transition temperature (Tg), high thermal stability, great ultimate tensile strength and low coefficient of thermal expansion (CTE). The Co-PIs-5 had lower crystallinity, lower CTE, greater elongation at break, higher Tg and thermal stability and the greater dense extent, compared with Co-PIs-3 and Co-PIs-6. Structure and property relations of the prepared polyimides were also briefly discussed. The results revealed that the copolymerization of s-BPDA/PDA with a small number of 4,4′-ODA/a-BPDA was a useful means for enhancing flexibility without sacrificing low CTE.

Zirconium oxide nanoparticles coated on sepiolite by sol–gel process — Their application as a solvent-free catalyst for condensation reactions

2011 ◽  
Vol 89 (3) ◽  
pp. 280-288 ◽  
Author(s):  
Sadok Letaief ◽  
Yun Liu ◽  
Christian Detellier
Keyword(s):  
Clay Mineral ◽  
Zirconium Oxide ◽  
Condensation Reaction ◽  
Sol Gel ◽  
Magic Angle Spinning ◽  
Solvent Free ◽  
Cubic Phase ◽  
Magic Angle ◽  
Solvent Free Conditions ◽  
Sol Gel Process

An inorganic nanocomposite made of zirconia nanoparticles coated on the external surfaces of the fibrous clay mineral sepiolite was prepared by using the sol–gel process under soft conditions using zirconium(IV) propoxide in 1-propanol as the precursor. The resulting materials were characterized by X-ray diffraction (XRD), thermal gravimetric analyses (TGA) and differential thermal analyses (DTA), microporosimetry, 29Si magic-angle spinning (MAS) nuclear magnetic resonance (NMR), and high-resolution transmission electron microscopy (HR-TEM). The organic material from the precursor was fully removed after calcination at 450 °C, concurrently with the crystallization of the cubic phase of zirconium oxide. The coordinated water molecules of sepiolite were fully removed and its symmetrical layered structure was folded after calcination at 650 °C, as observed by XRD and 29Si cross-polarization (CP) / MAS NMR. The arrangement of the nanoparticles of zirconium oxide on the sepiolite external surfaces maintains a fibrous morphology for the nanocomposite. This material was applied as a catalyst for the Knoevenagel condensation reaction of benzaldehyde and malononitrile under solvent-free conditions. Strongly improved yields of reaction, attributed to larger catalytically active surfaces, were obtained compared with either the sepiolite clay mineral or the zirconium oxide tested individually.

Research of Aluminum Sheet Encapsulated by Organic Silane Acrylate Resin and Tetraethyl Orthosilicate

2011 ◽  
Vol 399-401 ◽  
pp. 390-393
Author(s):  
Ai Huan Gao ◽  
Pi Hui Pi ◽  
Jiang Cheng ◽  
Zhuo Ru Yang
Keyword(s):  
Hybrid Film ◽  
Condensation Reaction ◽  
Sol Gel ◽  
Tetraethyl Orthosilicate ◽  
Aluminum Sheet ◽  
Aluminum Surface ◽  
Hydroxyl Groups ◽  
Organic Hybrid ◽  
Sol Gel Process ◽  
Acrylate Resin

Aluminum sheet was encapsulated by inorganic-organic hybrid film through a base catalyzed sol-gel method using organic acrylate silane resin PMBV and TEOS as precursors. FTIR and AFM characterizations prove that PMBV and TEOS have hydrolyzed and co-condensed with each other in the sol-gel process to form an uniform film on the surface of aluminum sheet. XPS result shows hydroxyl groups on aluminum surface have taken part in the co-condensation reaction.

The optical waveguiding properties of TiO2–SiO2 composite films prepared by the sol–gel process

1999 ◽  
Vol 25 (7) ◽  
pp. 667-670 ◽  
Author(s):  
Zhai Jiwei ◽  
Yang Tao ◽  
Zhang Liangying ◽  
Yao Xi
Keyword(s):  
Sol Gel ◽  
Composite Films ◽  
Sol Gel Process ◽  
Optical Waveguiding

Pd/SiO2 Organic-Inorganic Hybrid Materials by Sol-Gel Method: Preparation and Thermal Stability under H2 Atmosphere

2015 ◽  
Vol 1118 ◽  
pp. 20-27
Author(s):  
Jing Yang ◽  
Bao Song Li ◽  
Xiang Huo ◽  
Hao Xu ◽  
Hai Yun Hou
Keyword(s):  
Thermal Stability ◽  
Calcination Temperature ◽  
Hybrid Materials ◽  
Photoelectron Spectroscopy ◽  
Sol Gel ◽  
X Ray Diffraction ◽  
Inorganic Hybrid ◽  
X Ray ◽  
Good Thermal Stability ◽  
Pd Doping

Pd/SiO2 organic-inorganic hybrid materials were prepared by adding PdCl2 into methyl-modified silica sol. The Pd/SiO2 hybrid materials were characterized by X-ray diffraction (XRD), fourier transform infrared (FTIR) and X-ray photoelectron spectroscopy (XPS). The effects of calcination temperature and Pd-doping on the phase transition of Pd element and the thermal stability of CH3 group in the Pd/SiO2 organic-inorganic hybrid materials were investigated. The results showed that the reduced metallic Pd0 exhibits good thermal stability under H2 atmosphere in the calcination process. Pd element in noncalcined Pd/SiO2 materials exists in PdCl2 form, calcination at 200 °C in a H2 atmosphere produces some metallic Pd0 and calcinations at 350 °C results in the complete transformation of Pd2+ to metallic Pd0. With the increase of calcination temperature, the Pd0 particle sizes increase and the hydrophobic Si−CH3 bands decrease in intensity. As the calcination temperature is greater than or equal to 350 °C, the loading of metallic Pd0 nearly has no influence on the chemical structure but, with the increase of Pd content, the formed Pd0 particle size increases. To keep the hydrophobicity of Pd/SiO2 membrane materials, the optimal calcination temperature is about 350 °C under H2 atmosphere.

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