Morphology and thermal properties of polyhedral oligomeric silsesquioxane/polybutadiene nanocomposites prepared by anionic polymerization

The morphology and thermal properties of Allylisobutyl Polyhedral Oligomeric Silsesquioxane (POSS)/Polybutadiene (PB) nanocomposites prepared through anionic polymerization technique were investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA). The results of XRD, SEM and TEM showed that the aggregation of POSS in PB matrix occurred obviously, forming crystalline domains and the size of POSS particles increased with increasing POSS content. The DSC and TGA results indicated that the glass transition temperature (T _g) of the nanocomposites was significantly increased and the maximum degradation temperature (T _dmax) of nanocomposites was slightly increased compared with pure PB, implying an increase in thermal stability.     

Preparation and characterization of polyoxymethylene‐copolymer/hydroxyapatite nanocomposites for long‐term bone implants

In this work, new polyoxymethylene (POM)/hydroxyapatite (HAp) nanocomposites for long‐term bone implants have been obtained via extrusion and injection molding processes and characterized by differential scanning calorimetry (DSC), temperature‐modulated DSC (TMDSC), scanning electron microscopy (SEM), transmission electron microscopy (TEM), wide‐angle X‐ray diffraction (WAXD), Fourier transform infrared spectroscopy (FTIR), thermogravimetry (TG), and tensile mechanical and in vitro stability tests. Based on the DSC results, it was found that the degree of crystallinity increases for POM/0.5% HAp sample and decreases for POM/1.0% HAp and POM/2.5% HAp. SEM and TEM observations for POM/HAp nanocomposites indicated that the dispersion of HAp in the polymer matrix was uniform and the diameter of the HAp particles was less than 100 nm for most of them. Young's modulus increases with increasing HAp concentration, whereby elongation at break decreases. On the contrary, HAp concentration does not have a significant influence on the tensile strength. TG results show that for POM/0.5% HAp, POM/1.0% HAp, and POM/2.5% HAp, thermal stability slightly increases in comparison to pure POM, whereas for POM/5.0 HAp and POM/10.0% HAp, lower thermal stability was observed. In vitro data reveal that with an increase of HAp content, bioactivity of nanocomposites increases; a good in vitro chemical stability of POM and POM nanocomposites was confirmed. Copyright © 2011 John Wiley & Sons, Ltd.     

TiO2@MWNTs纳米复合材料的制备及其储锂性能

以TiOSO4为钛源,多壁碳纳米管(MWNTs)为载体,溶剂热法制备了多壁碳纳米管/二氧化钛纳米复合材料(TiO2@MWNTs),并利用XRD,SEM,TEM,N2吸附-脱附和TG-DSC等测试手段对合成产物的结构和形貌进行表征,用恒流充放电测试研究TiO2@MWNTs纳米复合材料的储锂性能.N2吸附-脱附曲线和孔径分布曲线证实TiO2@MWNTs存在多级孔道结构以及较大的比表面积.电化学测试结果表明,与纯TiO2颗粒相比,TiO2@MWNTs纳米复合材料具有更好的容量保持率和倍率性能.在1 C倍率下,复合材料的可逆容量为200 mAh?g-1,循环100圈后容量仍达182 mAh?g-1,即使在10 C大倍率下,容量约为100 mAh?g-1左右.     

Synergistic effects of layered double hydroxide with phosphorus-nitrogen intumescent flame retardant in PP/EPDM/IFR/LDH nanocomposites

<正>Synergistic effects of layered double hydroxide(LDH) with intumescent flame retardanct(IFR) of phosphorus-nitrogen (NP) compound in the polypropylene/ethylene-propylene-diene/IFR/LDH(PP/EPDM/IFR/LDH) nanocomposites and related properties were studied by X-ray diffraction(XRD),transmission electron microscopy(TEM),scanning electron microscopy(SEM),limiting oxygen index(LOI),UL-94 test,cone calorimeter test(CCT) and thermo-gravimetric analysis (TGA).The XRD and TEM results show that the intercalated and/or exfoliated nanocomposites can be obtained by direct melt-intercalation of PP/EPDM into modified LDH and that LDH can promote the IFR additive NP to disperse more homogeneously in the polymer matrix.The SEM results provide positive evidence that more compact charred layers can be obtained from the PP/EPDM/NP/LDH sample than those from the PP/EPDM/LDH and PP/EPDM/NP samples during burning.The LOI and UL-94 rating tests show that the synergetic effects of LDH with NP can effectively increase the flame retardant properties of the PP/EPDM/NP/LDH samples.The data from the CCT and TGA tests indicate that the PP/EPDM/NP/LDH samples apparently decrease the HRR and MLR values and thus enhance the flame retardant properties and have better thermal stability than the PP/EPDM/LDH and PP/EPDM/NP samples.     

乳液聚合法制备聚苯乙烯/Mg-Al层状双氢氧化物纳米复合材料

采用乳液聚合法制备阻燃性聚苯乙烯MgAl层状双氢氧化物(LDHs)纳米复合材料.通过对不同合成条件下复合材料的XRD谱,讨论了纳米复合材料的形成过程;经SEM图证实了LDHs是以剥离的纳米级层片分散在基体中的;TG和DSC谱图揭示了LDHs纳米层板可有效提高PS的热稳定性,并可使PS的玻璃化转化温度明显提高;当层状双氢氧化物在插层复合材料中含量为14.92%时,纳米复合材料的氧指数可达23.5%,其用量比在PS中直接添加纳米LDHs时要少约一倍.文中还分析了纳米复合材料的形成过程.     

The disorderly exfoliated LDHs/PMMA nanocomposites synthesized by in situ bulk polymerization: The effects of LDH-U on thermal and mechanical properties

The disorderly exfoliated layered double hydroxides/poly(methyl methacrylate) (LDHs/PMMA) nanocomposites were obtained in a two-stage process by the in situ bulk polymerization of methyl methacrylate (MMA) in the presence of 10-undecenoate intercalated LDH (LDH-U). The dispersed behavior of the LDH-U in the PMMA matrix was identified by using X-ray diffraction (XRD), transmission electron microscopy (TEM), and UV/visible transmission spectroscopy. All these nanocomposites showed significantly enhancement of glass transition temperature (T_g) and the decomposition temperatures compared to pristine PMMA, as identified in differential scanning calorimetry (DSC) and thermogravimetric (TGA) analysis. The tensile modulus of these nanocomposites was also enhanced by incorporating the LDH-U into the PMMA matrix and increased as the amount of LDH-U increased. According to the analytical method of Ozawa-Flynn, the degradation activation energies of these nanocomposites are higher than that of pristine PMMA.     

Thermal properties and combustion characterization of nylon 6/MgAl-LDH nanocomposites via organic modification and melt intercalation

The nylon 6/MgAl layered double hydroxide (MgAl-LDH) nanocomposites have been prepared by melt intercalation of nylon 6 into the part organic dodecyl sulfate (DS) anion-modified MgAl(H-DS) interlayers. The structures and properties of MgAl(H-DS) and corresponding nanocomposites were characterized by ion chromotography, X-ray diffraction (XRD), transmission electron microscopy (TEM), differential scanning calorimetry (DSC), thermogravimetry analysis (TGA), and cone calorimeter test (CCT). The nanoscale dispersion of MgAl(H-DS) layers in the nylon 6 matrix has been verified by the disappearance of d₀₀₁ XRD diffraction peak of MgAl(H-DS) and the observation of TEM image. DSC tests evince that these exfoliated MgAl(H-DS) layers play the role of nucleating agents with strong heterogeneous nucleation effect on the crystallization of nylon 6 and increase its crystallization temperature over 12 °C with only 5 wt% MgAl(H-DS). TGA tests show that the effect of alkaline catalysis degradation from LDH on nylon 6 decreases the thermal stability of nylon 6/MgAl-LDH nanocomposites. The data from the cone calorimeter tests show that the HRR and MLR values of the sample with 5 wt% MgAl(H-DS) decrease considerably to 664 kW/m² and 0.161 g/m² s from 1064 kW/m² and 0.252 g/m² s of pure nylon 6, respectively. This kind of exfoliated nanocomposite is promising for the application of flame-retardant polymeric materials.     

Investigation of structural and thermal characteristics of PVDF/ZnO nanocomposites

The structural and thermal behavior of PVDF/ZnO nanocomposites have been investigated by employing scanning electron microscopy (SEM),TEM, DSC, powder X-ray diffraction (XRD), thermally stimulated discharge current (TSDC), and transient current techniques. SEM/TEM observation indicated the homogeneous dispersion of functionalized ZnO nanoparticles throughout PVDF matrix. DSC shows that the crystallinity is influenced by the presence of ZnO nanoparticles in the PVDF matrix because the filler acts as efficient nucleating agent to facilitate PVDF crystallization. DSC results indicated the enhancement of the glass transition temperature (T _g), melting temperature (T _m) and crystallization temperature (T _c) of nanocomposites compared to pristine PVDF. XRD shows that the full-width at half maximum decreases with increasing ZnO content, which is attributed to the improvement in crystallinity. The incorporation of ZnO nanoparticles influences the modification of polarization process in PVDF as observed by means of TSDC and transient current study.     

The role of interfacial compatibilization upon the microstructure and electrical conductivity threshold in polypropylene/expanded graphite nanocomposites

Attempts have been made to evaluate the effect of interface and degree of interfacial interaction upon electrical conductivity threshold in polypropylene/expanded graphite (PP/EG) nanocomposites, and dispersion state of graphite nanosheets. For this purpose, maleic anhydride grafted polypropylene (PPgMA) and maleic anhydride grafted EPDM (EPDMgMA) were used as compatibilizer. Nanocomposite samples containing 1–5 vol% of EG were prepared by melt mixing method using laboratory scale internal mixer. Characterization was carried out by using X‐ray diffraction (XRD), differential scanning calorimeter (DSC), thermo‐gravimetric analysis (TGA), scanning electron microscope (SEM), transmission electron microscope (TEM), and rheo‐mechanical spectroscopy (RMS). The conductivity measurements were carried out by using four point probe method according to ASTM D991. Results showed that the conductivity threshold is controlled by the extent of interfacial interaction between PP and EG. So, better conductivity was obtained using PPgMA as compatibilizer which causes higher level of interaction between PP and EG, and therefore better dispersion of the EG nanolayers in the polymer matrix. On the other hand, high levels of compatibilizers, especially EPDMgMA, caused formation of separated aggregates of EG shelled with the compatibilizer, which results in the reduction of conductivity of the nanocomposites. This finding has been verified by SEM, RMS, and conductivity measurements. Effects of EG nanolayers on crystalline structure and thermal decomposition temperature of the nanocomposites have also been investigated by DSC and TGA, respectively. Copyright © 2009 John Wiley & Sons, Ltd.     

Synthesis and physical properties of new layered double hydroxides based on ionic liquids: Application to a polylactide matrix

Ionic liquids based on tetraalkylphosphonium salts combined with different anions (decanoate and dodecylsulfonate) have been used as intercalating agents of layered double hydroxides (LDHs) by ion exchange. The synthesized phosphonium-treated LDHs display a dramatically improved thermal degradation and a significant increase in the interlayer distance as confirmed by thermogravimetric analysis (TGA) and X-ray Diffraction (XRD), respectively. To highlight the effect of thermostable ionic liquids, a very low amount of LDHs has been introduced within a polylactide (PLA) matrix and PLA/LDHs nanocomposites have been processed in melt by twin-screw extrusion. Then, transmission electron microscopy (TEM) analysis has been used to investigate the influence of ILs on the different morphologies of these nanocomposites. Even though the thermal stability of PLA matrix decreased, an excellent stiffness-toughness compromise has been obtained.     

Preparation, Characterization and Magnetic Properties of PANI/La-substituted LiNi Ferrite Nanocomposites

Magnetic nanocomposites containing polyaniline （PANI）-coated La-substituted LiNi ferrite （LiNi0.5La0.02Fe1.98O4） were synthesized by in situ polymerization in aqueous solution of hydrochloric acid. The nanocomposites exhibited the magnetic hysteresis nature under applied magnetic field. The saturation magnetization （Ms） and coercivity （Hc） varied with the ferrite content. The obtained nanocomposites were characterized by X-ray diffraction （XRD）, transmission electron microscopy （TEM）, scanning electron microscopy （SEM）, Fourier transform infrared spectroscopy （FT-IR）, UV-Visible spectroscopy and vibrating sample magnetometer （VSM）. TEM and SEM studies showed that the nanocomposites present the core-shell structure. The results of XRD patterns, FT-IR and UV-Visible spectra indicated the formation of PANI-LiNi0.5La0.002Fe1.98O4 nanocomposites and showed that the interaction existed between PANI backbone and ferrite particles in the nanocomposites. The bonding mechanism in the nanocomposites has been proposed.     

Metal‐organic framework MIL‐53 (Fe)@C/graphite carbon nitride hybrids with enhanced thermal stability,flame retardancy,and smoke suppression for unsaturated polyester resin

Metal‐organic framework MIL‐53 (Fe)@C/graphite carbon nitride hybrid (MFeCN), a novel flame retardant, was synthesized by hydrothermal reaction and subsequently added into unsaturated polyester resin (UPR). The structure, morphology, and thermal stability of MFeCN were characterized by Fourier transform infrared spectroscopy (FTIR), X‐ray diffraction (XRD), X‐ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy‐dispersive X‐ray spectroscopy (EDS), and thermogravimetric analysis (TG). The thermal stability and flammability of the UPR composites were characterized by TG and cone calorimeter tests (CCT). The results of CCT demonstrated that the peak heat release rate (pHRR), total heat release (THR), peak smoke production rate (pSPR), and total smoke production (TSP) of UPR/MFeCN‐4 were reduced by 39.8%, 10.2%, 33.3%, and 14.5%, respectively, comparing with UPR. The results of TG and CCT indicated that MFeCN could improve the thermal stability, flame retardancy, and smoke suppression properties of the UPR composites. The residues after CCT were then characterized by laser Raman spectroscopy (LRS), XPS, and SEM. Finally, based on the above experimental results and analysis, the flame retardancy mechanism of MFeCN was proposed.     

Fabrication of a novel nonenzymatic hydrogen peroxide sensor based on Se/Pt nanocomposites

A novel nonenzymatic hydrogen peroxide sensor was successfully fabricated based on the Se/Pt nanocomposites. The nanocomposites were constructed via a simple solvethermal method, and were confirmed by X-ray diffraction (XRD), energy-dispersive X-ray spectrometry (EDS), transmission electron microscopy (TEM) and scanning electron microscopy (SEM). Cyclic voltammetry (CV) was used to evaluate the electrochemical performance of the nanocomposites at glassy carbon electrode (GCE). The results indicated that the Se/Pt nanocomposites exhibited excellent electrocatalytic activity to the reduction of H₂O₂ and could be used to construct a hydrogen peroxide amperometric sensor with a low detection limit and wide responding range.     

Flame retardancy and thermal degradation mechanism of calcium alginate/CaCO<Subscript>3</Subscript> composites prepared via in situ method

The calcium alginate/CaCO₃ composites were prepared via in situ method, and their flame retardancy and thermal degradation mechanism were investigated. The composites as-prepared were analyzed by the scanning electron microscopy (SEM), Fourier transform infrared spectroscopy, thermogravimetric analysis (TG), vertical burning (UL-94), cone calorimeter (CONE) and X-ray diffraction (XRD). The SEM demonstrated that the inorganic calcium salt in the composites had great influence on the morphology of materials. The TG results indicated the thermal stability of the composites was remarkably improved by 70 °C, compared with that of the calcium alginate. The combustion behaviors of the materials were assessed by CONE. In comparison with those of the calcium alginate, the peak heat release rate and total heat release of the composites decreased by 40.42 and 62.59%, respectively. The different degradation mechanisms of the calcium alginate and the composites were first proposed in detail based on the TG, XRD and SEM results. The composites exhibited excellent thermal stability and flame retardancy, which is promising to be developed for the application as flame-retardant materials in the future.     

The effects of intralayer metal composition of layered double hydroxides on glass transition, dispersion, thermal and fire properties of their PMMA nanocomposites

A series of aluminum-containing layered double hydroxides (LDHs), containing Mg, Ca, Co, Ni, Cu and Zn as the divalent metals, have been prepared by the co-precipitation method and used to prepare nanocomposites of PMMA by in situ bulk polymerization. The additives were characterized by Fourier transform infrared spectroscopy, X-ray diffraction spectroscopy (XRD) and thermogravimetric analysis while the polymer composites were characterized by XRD, transmission electron microscopy, differential scanning calorimetry and cone calorimetry. Polymerization of methyl methacrylate in the presence of these undecenoate LDHs results in composites with enhanced thermal stability. The glass transition temperatures of the composites and the pristine polymers are found to be around 110 °C; this suggests that the presence of these additives has little effect on the polymer. It is found that the additive composition and the dispersion state of LDHs agglomerates in the polymer matrix influence the fire properties of composites as measured by cone calorimetry.     

本质阻燃聚苯乙烯/蒙脱土纳米复合物的制备及性能

通过原位聚合法制备了本质阻燃聚苯乙烯[P(St-co-AEPPA)]/有机改性蒙脱土(OMMT)纳米复合物[P(St-co-AEPPA)/OMMT], 并用普通聚苯乙烯/有机改性蒙脱土(PS/OMMT)复合物作为对比实验, 研究了含磷、氮单体丙烯酸羟乙基-苯氧基-二乙基磷酰胺(AEPPA)和OMMT等添加物对本质阻燃聚苯乙烯性能的影响.用X射线衍射仪(XRD)和透射电子显微镜(TEM)分析了复合材料的结构与形貌, 并对OMMT在基体中的分散机理进行了讨论.用差示扫描量热仪(DSC)、热重分析(TGA)和微型量热仪(MCC)研究了材料的热性能和燃烧性能.结果表明, AEPPA和OMMT能够显著提高基体的热稳定性和阻燃性.     

Facile Electrospinning of CeO2/Bi2WO6 Heterostructured Nanofibers with Excellent Visible‐light‐driven Photocatalytic Performance

One‐dimensional (1D) CeO₂/Bi₂WO₆ heterostructured nanofibers with a diameter of about 300 nm were successfully synthesized by using a straightforward strategy combining an electrospinning technique with a sintering process. The acquired products were characterized by thermogravimetric and differential scanning calorimetric (TG‐DSC), Fourier transform infrared (FT‐IR) spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), X‐ray diffraction (XRD), X‐ray photoelectron spectroscopy (XPS), Brunauer–Emmett–Teller (BET) surface area measurements, and UV/Vis spectroscopy. The obtained CeO₂/Bi₂WO₆ heterostructured nanofibers exhibited an excellent photocatalytic property for the degradation of Rhodamine B (RhB) dye driven by visible light due to the promoted separation of photoelectrons and holes and the large contact area between the photocatalyst and organic pollutant.     

溶胶-凝胶法制备聚醚砜-二氧化硅复合材料

以聚醚砜(PES)为基体,通过溶胶-凝胶过程,得到了分散均匀的PES/SiO₂杂化材料,用扫描电镜、透射电镜、傅里叶红外及差示扫描量热法研究不同SiO₂含量的PES/SiO₂杂化材料材料性能.结果表明,当PES/SiO₂杂化材料中SiO₂的质量分数大于10%时可获得有机聚合物链段与无机网络互穿的均匀分散的复合材料.此材料的玻璃化转变温度(Tg)明显提高.     

ZnO-CNTs纳米复合材料的制备及性能表征

以醋酸锌(Zn(CH3COO)2•2H2O)和经硝酸处理过的碳纳米管(CNTs)为原料, 一缩二乙二醇(DEG)为溶剂, 采用溶胶法制备得到ZnO-CNTs纳米复合材料, 并通过XRD、TEM、SEM、IR、PL等手段对样品进行了表征, TEM及SEM结果显示, 负载在碳纳米管上的氧化锌纳米颗粒的尺寸小于25 nm. 讨论了反应时间、反应温度等因素对产品形貌的影响, 并对复合材料的光致发光效应及其形成机理进行了初步的探讨. PL结果表明, 相对于纯ZnO, ZnO-CNTs纳米复合材料的近紫外发射峰峰位发生了明显的蓝移.     

Crystallization Behavior and Thermal Properties of PP/MgAl LDH Nanocomposites Prepared in Non-polar Solution

Polypropylene(PP)/MgAl layered double hydroxide(MgAl LDH) nanocomposites were synthesized by refluxing PP and dodecyl sulfate-intercalated MgAl LDH[MgAl(DS)] in non-polar xylene. Their structure, thermal and crystallization properties were studied via X-ray diffraction(XRD), transmission electron microscopy(TEM), thermogravimetric analysis(TGA), differential scanning calorimetry(DSC), and polarized light microscopy(PLM). The nanoscaled dispersion of MgAl(DS) nanolayeres in the PP matrix was verified by the disappearance of the d(003) XRD diffraction peak of MgAl(DS) and observation of TEM image. The DSC data show that the SDS/LDH inorganic components negatively affect the crystallization properties of PP and decrease the size of PP spherulites because the inorganic components act as additional nuclei. The PP/MgAl LDH nanocomposites have a faster charring progress in a temperature range of 250―430 °C and a better thermal stability above 320 °C than pure PP.