氟硅氧烷共聚低表面能杂化材料的研究

通过溶液聚合和溶胶-凝胶法复合工艺,采用甲基丙烯酸十二氟庚酯(FA)为含氟单体、乙烯基三乙氧基硅烷(VTES)为硅单体和正硅酸乙酯(TEOS)为无机相前驱体直接合成了一种分子级复合,最外层含氟侧链定向于空气,中间层是碳碳主链,底层为硅氧网络结构的氟硅氧烷共聚低表面能杂化材料.结果表明,溶剂含量对含氟侧链向表面的迁移速度以及材料疏水性能有着非常重要的影响.     

凝胶型LED封装材料基础聚合物的制备及性能

过开环聚合制备了透明的聚(二甲基-甲基苯基-甲基乙烯基)硅氧烷共聚物,考察了聚合条件对产物结构与性能的影响.以该共聚物为基础聚合物,含氢硅油为交联剂,在Karstedt催化剂作用下硅氢加成硫化成型,获得折射率n<'25><,D>>1.5000,透光率大于90%(400 nm～800 nm,10 mm)的凝胶型发光二级管...     

由多聚硅氧烷制备二氧化硅气凝胶

SiO2 气凝胶是一种新型轻质纳米多孔材料。本工作以多聚硅氧烷 (E -4 0 )为硅源 ,用溶胶 -凝胶法制备出了SiO2气凝胶。研究了催化剂、温度、水等因素对其溶胶 -凝胶过程的影响 ;讨论了F离子以及水对E -4 0水解 -缩聚反应的作用机理 ;并用孔径分布测定仪、TEM等方法对其微结构进行了研究。结果表明 :由E -4 0为硅源制备的SiO2 气凝胶骨架颗粒为十几nm ;孔径分布较广 ,其峰值在 3 0nm附近 ,此外 ,还存在几nm的微孔。     

乙烯基取代聚苯撑硅氧烷的热性质

以1,4-双(二甲基硅基)苯、二甲基二甲氧基硅烷和甲基乙烯基二甲氧基硅烷为原料,用Si-H/Si-OR缩聚的方法制备了一系列聚(四甲基对硅亚苯基-二甲基-甲基乙烯基)硅氧烷三元共聚物(PTMPS/DMS/VMS),并用TG与DSC对共聚物的热性质进行了表征.结果表明,乙烯基能显著提高PTMPS/DMS/VMS在氮气中的热稳定性,且当DMS/VMS为50:50(摩尔比)时热稳定性最好.在空气中,引入乙烯基同样能提高PTMPS/DMS/VMS的热稳定性,但其影响比氮气中小得多.PTMPS/DMS/VMS的Tg与VMS链节含量的关系为:Tg=-56.1-0.04[VMS%],Tg随共聚物中VMS链节含量的增加而线性降低,但降低的幅度很小(不超过4.3℃).     

1,3,5-三甲基-1,3,5-三(3′,3′,3′-三氟丙基)环三硅氧烷的阴离子开环(共)聚合研究进展

1,3,5-三甲基-1,3,5-三(3′,3′,3′-三氟丙基)环三硅氧烷(F3)的阴离子开环聚合可以合成优越耐油耐溶剂性能的聚甲基三氟丙基硅氧烷(PMTFPS),但在开环聚合过程中“反咬”与再分布副反应严重,要得到高分子量、高产率的氟硅聚合物材料,必须严格控制聚合反应条件。文中总结了本体、溶液、细乳液中F3的阴离子开环聚合影响因素、机理与动力学,以及F3与其它单体共聚合反应等方面的研究进展。     

一种新型含硅脂环族四酸的合成研究

以1,3二甲基-1,3-二苯基二硅氧烷与降冰片烯单酐为反应物,通过酯化、硅氢加成和酸化3个步骤合成了一种新型含硅脂环族四酸,并对其进行了结构表征和溶解性研究.红外光谱(FTIR)与核磁共振(1 H NMR和13C-NMR)证实了目标产物含硅脂环族四酸被成功合成,且该四酸在常规有机溶剂中具有良好的溶解性.同时,研究表明:这是一条可以在一定程度上提高某些高位阻反应物之间硅氢加成反应活性的合成路线.     

氟硅聚合物/纳米SiO2杂化材料的制备与应用性能

通过本体聚合、溶胶-凝胶和接枝共聚等方法,以三氟丙基甲基-co-一甲基氢硅氧烷(PFHMS)、烯丙基缩水甘油醚(AGE)和全氟辛基乙烯(PFOE)间的硅氢化加成反应制得侧链含有全氟烷基、反应性环氧基的氟硅聚合物(PFAMS),并利用其与氨丙基三乙氧基硅烷(KH550)溶胶-凝胶改性纳米SiO2间的接枝共聚反应制备了一种...     

有机磷毒剂压电传感器敏感材料的制备及性能研究

以邻氟苯酚、3-溴丙烯与含氢硅油为原料,合成有机磷毒剂压电传感器敏感材料聚甲基[3-(2-羟基-3-氟)苯基]丙基硅氧烷.将聚甲基[3-(2-羟基-3-氟)苯基]丙基硅氧烷料涂覆在QCM传感器上,研究其对有机磷毒剂模拟剂甲基膦酸二甲酯(DMMP)和其它干扰气体的响应.结果表明,在13.2×10-6～65.8×10-6范围内,传感器对DMMP的响应成呈好的线性关系,灵敏度为9.369×106 Hz,最低检测极限为0.323×10-6(S/N=3),对DMMP的响应远高于其它干扰气体.     

气凝胶骨架结构的有机-无机交联度对其力学、热学性能的影响

硅系气凝胶是目前研究理论最为完善、合成技术最为成熟的气凝胶材料。本工作分别以四乙氧基硅烷(TEOS)、甲基三甲氧基硅烷(MTMS)、MTMS与二甲基二甲氧基硅烷(DMDMS)混合硅源、乙烯基甲基二甲氧基硅烷(VMDMS)为前驱体, 制备了不同种类的硅系气凝胶。所制得的硅系气凝胶具有较高的比表面积, 并呈现出纳米多孔的网络结构。本研究详细探讨了前驱体结构对气凝胶的力学及热学性能的影响。结果表明, 硅系气凝胶的骨架结构交联度越低, 弹性性能越好; 同时, 引入有机碳氢链会进一步提升气凝胶的弹性性能。所制备的硅系气凝胶兼具良好的保温隔热性能, 常温热导率在0.032~0.041 W/(m·K)范围内, 热重损失随着骨架结构内有机组分的增多而增大。这些优良的力学及热学性能使硅系气凝胶在保温隔热、储能等领域均具有广阔的应用前景。     

新型可降解聚硅基酯的合成及性质研究

主链中含有不稳定的硅酯键的聚硅基酯是一种新型的可降解聚合物.合成并研究了新型聚硅基酯即聚(己二酸四甲基二硅氧烷基硅基酯):首次利用熔融缩聚法使己二酸与1,1,3,3-四甲基二硅氧烷为单体合成了聚硅基酯,并用1H-NMR对该聚合物进行了结构表征,利用差示扫描量热(DSC)、热重分析(TGA)对其热力学性质进行了研究,利用凝胶渗透色谱(GPC)就分子量分布及降解性质进行了研究.     

Synthesis of soluble polyimide/silica–titania core–shell nanoparticle hybrid thin films for anti-reflective coatings

In this study, researchers prepared polyimide/silica–titania core–shell nanoparticle hybrid thin films (PI/SiO₂–TiO₂) from soluble fluorine-containing polyimide, colloidal silica, and titanium butoxide. The soluble polyimide with carboxylic acid end groups (6FDA–6FpDA–4ABA–COOH) could condense with titanium butoxide to provide organic–inorganic bonding, and thus prevent macrophase separation. TGA and DSC analysis showed that the decomposition temperature of hybrid materials increased with an increase in the content of silica–titania nanoparticles within the hybrid films. FTIR spectra indicated that the imidization was complete and the cross-linking Ti–O–Ti network formed. HRTEM and HRSEM images showed that the size of the core–shell nanoparticles were 18–20 nm. The thickness of titania shell on the silica is about 2.5 nm. The n&k and UV–Vis analysis showed that the prepared hybrid films had good optical properties and a high refractive index of 1.735. Researchers applied the prepared PI/SiO₂–TiO₂ hybrid thin films to develop a three layer antireflective (AR) coating on the glass and PMMA substrate. Results showed that the reflectance of the AR coating on the glass and PMMA substrate at 550 nm was 0.356 and 0.495%, respectively. The transparency was greater than 90% for both AR coatings on the glass and PMMA substrates.     

Highly transparent polyimide/nanocrystalline-titania hybrid optical materials for antireflective applications

This study prepared polyimide/titania hybrid thin films of, poly(3,3′,4,4′-Benzophenone tetra carboxylic dianhydride)–(4,4-Diaminodiphenyl Ether)/nanocrystalline titania (BTDA-ODA/TiO₂), with a high refractive index. FTIR analysis confirmed the formation of a polyimide and titania matrix. TGA and DSC analysis gauged the decomposition temperature in the range of 455–532 °C, indicating that the addition of titania could increase the glass transition temperature of hybrid films. XRD results indicate the formation of nanocrystalline titania domains of approximately 8–11 nm in the hybrid films. AFM, SEM, TEM, and XRD results show the formation of well-dispersed nanocrystalline titania. The refractive index was measured by ellipsometry, demonstrating an increase in the refractive index of the prepared hybrid thin films from 1.657 to 1.958, when the titania content was increased from 0 to 90 wt.%. UV–vis analysis gauged the cutoff wavelength in the range of 288–357 nm. The prepared polyimide/titania hybrid thin films were used to develop a three layer antireflective (AR) coating on a glass substrate. The average reflectance of the AR was 0.5% for the PT20/PT90/F-siloxane layer and 0.6% for the PT20/PT90/porous silica. Transparency at 550 nm exceeded 90% for both AR coatings.     

Titanium dioxide–cellulose hybrid nanocomposite and its glucose biosensor application

This paper investigates the fabrication of titanium dioxide (TiO₂)–cellulose hybrid nanocomposite and its possibility for a conductometric glucose biosensor. TiO₂ nanoparticles were blended with cellulose solution prepared by dissolving cotton pulp with lithium chloride/N,N-dimethylacetamide solvent to fabricate TiO₂–cellulose hybrid nanocomposite. The enzyme, glucose oxidase (GOx) was immobilized into this hybrid nanocomposite by physical adsorption method. The successful immobilization of glucose oxidase into TiO₂–cellulose hybrid nanocomposite via covalent bonding between TiO₂ and GOx was confirmed by X-ray photoelectron analysis. The linear response of the glucose biosensor is obtained in the range of 1–10 mM. This study demonstrates that TiO₂–cellulose hybrid nanocomposite can be a potential candidate for an inexpensive, flexible and disposable glucose biosensor.     

Preparation of the BaTiO3–SiO2 hybrid particles for the catalyst of methane steam reforming process

BaTiO₃ nano-coated SiO₂ (BaTiO₃–SiO₂) hybrid particles were prepared by liquid phase deposition and sol–gel process. The obtained BaTiO₃–SiO₂ hybrid particles have relatively high surface area (20 m² g⁻¹) at 600 °C annealing temperature. Ni component was impregnated to the obtained BaTiO₃–SiO₂ hybrid particles, and the obtained catalyst was used for the methane steam reforming process to consider the effect of the surface area on the catalytic activity. The catalytic activity of the Ni/BaTiO₃–SiO₂ catalyst was approximately three times as large as that of the reported Ni/BaTiO₃ catalyst, even in the lower process temperature. However, the limitation temperature for methane steam reforming process of this hybrid material was 600 °C, because of the diffusion of the Ba component.     

Synthesis,properties, and anti-reflective applications of new colorless polyimide-inorganic hybrid optical materials

We report the synthesis, properties and anti-reflective applications of new colorless polyimide-inorganic hybrid thin films prepared from 1,4-bis(3,4-dicarboxyphenoxy)-2,5-di-tert-butylbenzene dianhydride (DDBBDA)/oxydianiline (ODA) with silica or titania precursors. The experimental results suggest that the prepared hybrid films have good thermomechanical properties, excellent transparence, tunable refractive indices of 1.550–1.847, and low optical birefringence. The nanocrystalline titania domain size analyzed form TEM and XRD is in the range of 10–20 nm in the hybrid materials. Three-layer anti-reflective films on glass or polymer substrates processed from the hybrid precursors have a relatively low reflection of less than 0.5% in the visible range. These results indicate that the newly prepared colorless polyimide-inorganic hybrid materials have potential applications for optical devices.     

PMMA–SiO2 hybrid films as gate dielectric for ZnO based thin-film transistors

In this paper we report a low temperature sol–gel deposition process of PMMA–SiO₂ hybrid films, with variable dielectric properties depending on the composition of the precursor solution, for applications to gate dielectric layers in field-effect thin film transistors (FE-TFT). The hybrid layers were processed by a modified sol–gel route using as precursors Tetraethyl orthosilicate (TEOS) and Methyl methacrylate (MMA), and 3-(Trimethoxysilyl)propyl methacrylate (TMSPM) as the coupling agent. Three types of hybrid films were processed with molar ratios of the precursors in the initial solution 1.0: 0.25, 0.50, 0.75: 1.0 for TEOS: TMSPM: MMA, respectively. The hybrid films were deposited by spin coating of the hybrid precursor solutions onto p-type Si (100) substrates and heat-treated at 90 °C for 24 h. The chemical bonding in the hybrid films was analyzed by Fourier Transform Infrared Spectroscopy to confirm their hybrid nature. The refractive index of the hybrid films as a function of the TMSPM coupling agent concentration, were determined from a simultaneous analysis of optical reflectance and spectroscopic ellipsometry experimental data. The PMMA–SiO₂ hybrid films were studied as dielectric films using metal-insulator-metal structures. Capacitance–Voltage (C–V) and current–voltage (I–V) electrical methods were used to extract the dielectric properties of the different hybrid layers. The three types of hybrid films were tested as gate dielectric layers in thin film transistors with structure ZnO/PMMA–SiO₂/p-Si with a common bottom gate and patterned Al source/drain contacts, with different channel lengths. We analyzed the output electrical responses of the ZnO-based TFTs to determine their performance parameters as a function of channel length and hybrid gate dielectric layer.     

Graphene/MnO2 hybrid nanosheets as high performance electrode materials for supercapacitors

Graphene/MnO₂ hybrid nanosheets were prepared by incorporating graphene and MnO₂ nanosheets in ethylene glycol. Scanning electron microscopy and transmission electron microscopy analyses confirmed nanosheet morphology of the hybrid materials. Graphene/MnO₂ hybrid nanosheets with different ratios were investigated as electrode materials for supercapacitors by cyclic voltammetry (CV) and galvanostatic charge–discharge in 1 M Na₂SO₄ electrolyte. We found that the graphene/MnO₂ hybrid nanosheets with a weight ratio of 1:4 (graphene:MnO₂) delivered the highest specific capacitance of 320 F g⁻¹. Graphene/MnO₂ hybrid nanosheets also exhibited good capacitance retention on 2000 cycles.     

Wear characteristics of hybrid aluminium matrix composites reinforced with graphite and silicon carbide particulates

This investigation studies the dry sliding wear behaviour of Al matrix composites reinforced with Gr and SiC particulate up to 10%, to study the effect of % reinforcement, load, sliding speed and sliding distance on stir cast Al–SiC–Gr hybrid composites, Al–Gr and Al–SiC composites. Parametric studies indicate that the wear of hybrid composites has a tendency to increase beyond% reinforcement of 7.5% as its values are 0.0242 g, 0.0228 g and 0.0234 g respectively at 3%, 7.5% and 10% reinforcement. The corresponding values are 0.0254 g, 0.0240 g and 0.0242 g in Al–Gr composites and 0.0307 g, 0.0254 g and 0.0221 g in Al–SiC composites, clearly indicating that hybrid composites exhibit better wear characteristics. Increase of speed reduces wear and increase of either load or sliding distance or both increases wear. Statistical analysis has revealed interactions among load, sliding speed and sliding distance in composites with Gr particulates.     

Corrosion resistance enhancement of Ni–P electroless coatings by incorporation of nano-SiO2 particles

Composite coatings were prepared using hypophosphite reduced electroless nickel bath containing 7 g/L SiO₂ nano-particles at pH 4.6 ± 0.2 and temperature 90 ± 2 °C. Deposition rate for SiO₂ nano-composite coatings was 10–12 μm/h. The amount of SiO₂ nano-particles co-deposited in the Ni–P matrix was around 2 wt.%. The analyzes of coating compositions, carried out by Energy Dispersive Analysis of X-ray (EDAX), showed that plain Ni–P and Ni–P/nano-SiO₂ deposits contained around 8 wt.% phosphorus. The X-ray diffraction (XRD) pattern of Ni–P/nano-SiO₂ coating was very similar to that of plain electroless Ni–P coating, whose structure was also amorphous.     

Photovoltaic performance of dye-sensitized solar cells fabricated with polyvinylidene fluoride–polyacrylonitrile–silicondioxide hybrid composite membrane

Electrospun fibrous membranes of hybrid composites of polyvinylidene fluoride (PVdF), polyacrylonitrile (PAN) and silicon dioxide (SiO₂) (PVdF–PAN–SiO₂) are prepared with different proportions of SiO₂ (3, 5 and 7% w/w). The field emission scanning electron microscopy (FE-SEM) reveals that these membranes have three-dimensional, fully interconnected network structures, which are combined with micropores of fine SiO₂ distribution. The surface roughness of the membranes increases with increasing the SiO₂ content. It is found that 7 wt% SiO₂/PVdF–PAN electrolyte membrane has the highest ionic conductivity (6.96 × 10⁻² S cm⁻¹) due to the large liquid electrolyte uptake (about 570%). As the concentration of SiO₂ nanoparticles increase, the contact angle value also increases, ranging from 135.70° to 140.60° which indicates that the membrane has higher hydrophobicity. The dye sensitized solar cells (DSSCs) are fabricated using the hybrid composite membrane with PVdF–PAN with 7 wt % SiO₂. Its photovoltaic performance exhibits an open circuit voltage (V_oc) of 0.79 V and a short circuit current 11.6 mA cm⁻² at an incident light intensity of 100 mW cm⁻², producing an efficiency of 5.61%. DSSC, using the hybrid composite electrospun membrane which shows more stable photovoltaic performance than other assembled DSSCs.