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1.
The IR laser irradiation of a gaseous mixture of iron pentacarbonyl–methoxytrimethylsilane–ethene in argon induces ethene‐photosensitized decomposition of iron pentacarbonyl into elemental iron and decomposition of methyltrimethoxysilane into species that polymerize into methylmethoxysilicone. These two concurrent gas‐phase processes allow formation of iron–iron oxide/methylmethoxysilicone nanocomposite. Spectral analyses and electron microscopy reveal the nanocomposite as consisting of iron clusters oxidized in outer layers and covered with the organosilicon polymer. The procedure shows its potential for gas‐phase synthesis of iron‐based clusters embedded in a polymer matrix. Copyright © 2004 John Wiley & Sons, Ltd.  相似文献   

2.
A new type of hyperbranched polysilazane containing iron (PSZI) compound was synthesized by the polycondensation of silazane lithium salts with FeCl3, and the structure of the PSZIs was investigated by IR, NMR and elemental analyses. The PSZIs were pyrolyzed under nitrogen, argon or NH3, and magnetic ceramics could be obtained. The ceramic yields of the PSZIs were higher than those of their corresponding silazanes, and the PSZIs or silazanes with reactive groups containing Si? H, ? CH?CH2 or higher branched structures had higher yields. The magnetism of the ceramics could be controlled by a pyrolytic atmosphere and temperature: the saturation magnetization Ms ranged from 20 to 100 emu g?1 and coercivity Hc ranged from 463 to 50 Oe. The transformation of the magnetic loop of the PSZIs pyrolyzed at different temperatures under NH3 was quite different from those under nitrogen. It was shown by X‐ray diffraction measurements that the magnetic crystalline form could exist as Fe4N, Fe(0) or Fe3N depending on temperature under NH3, but under a nitrogen atmosphere Fe(0) was nearly the only magnetic crystalline form from 600 to 1100 °C. By dipping or spin‐coating of the PSZI solution, then through pyrolysis under nitrogen, argon or NH3, thin uniform magnetic ceramic films could be fabricated on the substrates. Copyright © 2003 John Wiley & Sons, Ltd.  相似文献   

3.
The electrodeposition of soft magnetic iron and iron–silicon alloys for magnetic measurements is presented. The preparation of these materials in 1‐butyl‐1‐methylpyrrolidinium trifluoromethylsulfonate, [Py1,4]TfO, at 100 °C with FeCl2 and FeCl2+SiCl4 was studied by using cyclic voltammetry. Constant‐potential electrolysis was carried out to deposit either Fe or FeSi, and deposits of approximately 10 μm thicknesses were obtained. By using scanning electron microscopy and X‐ray diffraction, the microstructure and crystallinity of the deposits were investigated. Grain sizes in the nanometer regime (50–80 nm) were found and the presence of iron–silicon alloys was verified. Frequency‐dependent magnetic polarizations, coercive forces, and power losses of some deposits were determined by using a digital hysteresis recorder. Corresponding to the small grain sizes, the coercive forces are around 950–1150 A m?1 and the power losses were at 6000 J m?3, which is much higher than in commercial Fe(3.2 wt %)Si electrical steel. Below a polarization of 1.8 T, the power losses are mainly caused by domain wall movements and, above 1.8 T, by rotation of magnetic moments as well as domain wall annihilation and recreation.  相似文献   

4.
Calcium carbonate (CaCO3)/polystyrene (PS) nanoparticles (<100 nm) with core–shell structure were synthesized by atomized microemulsion technique. The polymer chains were anchored onto the surface of nano‐CaCO3 through triethoxyvinyl silane (TEVS) as a coupling agent. Ammonium persulfate (APS), sodium dodecyl sulfate (SDS) and n‐pentanol were used as initiator, surfactant, and cosurfactant, respectively. Polymerization mechanism of core–shell latex particles was discussed. Encapsulation of nano‐CaCO3 by PS was confirmed by using transmission electron microscope (TEM). Grafting percentage of core–shell particles was investigated by Thermogravimetric Analyzer (TGA). Nano‐CaCO3/PS core–shell particles were characterized by Fourier transform infrared (FTIR) spectrophotometer and differential scanning calorimeter (DSC). The results of FTIR revealed existence of a strong interaction at the interface of nano‐CaCO3 particle and PS, which implies that the polymer chains were successfully grafted onto the surface of nano‐CaCO3 particle through the link of the coupling agent. In addition, TGA and DSC results indicated an enhancement of thermal stability of core–shell materials compared with the pure nano‐PS. Nano‐CaCO3/PS particles were blended with polypropylene (PP) matrix on Brabender Plastograph by melt process with different wt% of loading (i.e. 0.1–1 wt%). The interfacial adhesion between nano‐CaCO3 particles and PP matrix was significantly improved when the nano‐CaCO3 particles were grafted with PS, which led to increased thermal, rheological, and mechanical properties of (nano‐CaCO3/PS)/PP composites. Scanning electron microscope (SEM) and atomic force microscope (AFM) images showed a perfect dispersion of the nano‐CaCO3 particles in PP matrix. Copyright © 2011 John Wiley & Sons, Ltd.  相似文献   

5.
The dielectric and magnetic properties of carbonyl—iron (CI) and nickel zinc ferrite polymer composites were studied with respect to the ferrite particulate content and microwave frequency. From the experimental data and using empirical models that relate the composite dielectric and magnetic properties, the respective dielectric and magnetic properties of the neat fillers were estimated. The tensile properties of the particulate composites comprising CI were shown to follow qualitatively Mooney's equation for the elastic modulus. The tensile strength of an elastomeric polyurethane and PVC composites containing CI increased with particulate content, while the elongation to break decreased with filler content. SEM micrographs of tensile fracture surfaces indicated that somewhat better adhesion is obtained in the case of the polyurethane-based composites compared to the PVC ones.  相似文献   

6.
《先进技术聚合物》2018,29(2):896-905
The tribological characteristics of PEEK composites fretting against GCr 15 steel were investigated by a SRV‐IV oscillating reciprocating ball‐on‐disk tribometer. In order to clarify the effect of type and size of fillers on the properties of PEEK composites, nano‐sized and micro‐sized CF and PTFE fillers were added to the PEEK matrix. The thermal conductivity, hardness, and fretting wear properties of PEEK composites reinforced by CF or PTFE were comparatively studied. The results showed that the type and size of the fillers have an important effect on both the friction coefficient and wear rate, by affecting their thermal conductivity, hardness, as well as the surface areas of their transfer films. In comparison, the effect on improving the tribological properties of micro‐sized CF was superior to that of nano‐sized CF, while the effect of nano‐sized PTFE was superior to that of micro‐sized PTFE. Considering the acceptable friction coefficient and wear rate of the composite under the fretting wear test, it seemed that 4% nCF, 20% mCF, 2% nPTFE and 10% mPTFE were desired additive proportions. And it also can be found that during the fretting wear test, the abrasive and adhesive wear resulted in accumulative debris at the contacting surface. The transfer films made of debris were formed on the counterfaces.  相似文献   

7.
A novel and task‐specific nano‐magnetic Schiff base ligand with phosphate spacer using 2‐aminoethyl dihydrogen phosphate instead of usual coating agents, i.e. tetraethoxysilane and 3‐aminopropyltriethoxysilane, for coating of nano‐magnetic Fe3O4 is introduced. The nano‐magnetic Schiff base ligand with phosphate spacer as a novel catalyst was synthesized and fully characterized using infrared spectroscopy, X‐ray diffraction, scanning and transmission electron microscopies, thermogravimetry, derivative thermogravimetry, vibrating sample magnetometry, atomic force microscopy, X‐ray photoelectron spectroscopy and energy‐dispersive X‐ray spectroscopy. The resulting task‐specific nano‐magnetic Schiff base ligand with phosphate spacer was successfully employed as a magnetite Pd nanoparticle‐supported catalyst for Sonogashira and Mizoroki–Heck C–C coupling reactions. To the best of our knowledge, this is the first report of the synthesis and applications of magnetic nanoparticles of Fe3O4@O2PO2(CH2)2NH2 as a suitable spacer for the preparation of a designable Schiff base ligand and its corresponding Pd complex. So the present work can open up a new and promising insight in the course of rational design, synthesis and applications of various task‐specific magnetic nanoparticle complexes. Copyright © 2016 John Wiley & Sons, Ltd.  相似文献   

8.
Composites of (001)‐face‐exposed TiO2 ((001)‐TiO2) and CuO were synthesized in water vapor environment at 250°C with various Cu/Ti molar ratios (RCu/Ti). The resulting CuO/(001)‐TiO2 composites were characterized using a variety of techniques. The synthesis under high‐temperature vapor allows close contact between CuO and (001)‐TiO2, which results in the formation of heterojunctions, as evidenced by the shift of valence band maximum towards the forbidden band of TiO2. An appropriate ratio of CuO can enhance the absorption of visible light and promote the separation of photogenerated carriers, which improve the photocatalytic performance. The degradation rate constant Kapp increased from 5.5 × 10?2 to 8.1 × 10?2 min?1 for RCu/Ti = 0.5. Additionally, the results showed that superoxide radicals (?O2?) play a major role in the photocatalytic degradation of methylene blue.  相似文献   

9.
A density functional theory study is presented regarding the energetics and the Mulliken population analyses of a quantum mechanical/molecular mechanical (QM/MM) system including multiple iron–sulfur clusters in the QM region. The [FeFe]‐hydrogenase from Desulfovibrio desulfuricans was studied, and both the active site (an Fe6S6 assembly generally referred to as the H‐cluster) and an ancillary Fe4S4 site were treated at the BP86‐RI/TZVP level. The antiferromagnetic coupling that characterizes both sites was modeled using the broken‐symmetry (BS) approach. For such a QM system, 36 different BS couplings can be defined, depending on the localization of spin excess on the various spin centers. All the BS states were obtained by means of an effective and simple method for spin localization, that is here described and compared with more sophisticated approaches already available in literature. The variation of the QM/MM energy among the various geometry‐optimized protein models was found to be less than 25 kJ mol–1. This energy variation almost doubles if no geometry optimization is performed. A detailed analysis of the additive nature of these variations in QM/MM energy is reported. The Mulliken charges show very small variations among the 36 BS states, whereas the Mulliken spin populations were found to be somewhat more variable. The relevance of such variations is discussed in light of the available Mössbauer and Electron Paramagnetic Resonance (EPR) spectroscopic data for the enzyme. Finally, the influence of the basis set on the spin populations, charges, and structural parameters of the models was investigated, by means of QM/MM computations on the same system at the BP86‐RI/SVP level. © 2010 Wiley Periodicals, Inc. Int J Quantum Chem, 2011  相似文献   

10.
This paper describes the effect of nanofillers, such as nanographite, nickel–zinc ferrite (NiZnFerrite), and in‐house developed hybrid nanographite particles (i.e. iron‐coated nanographite [FeNG] and iron–nickel co‐deposited nanographite [FeNiNG] particles), on microwave‐absorption properties of thermoplastic polyurethane (TPU) based nanocomposite coatings on textile substrate. The flexible coatings were tested for various functional properties such as microwave absorbency, gas barrier property, impedance, and weather resistance. The comparison has also been made with other fillers such as bulk graphite (G) and iron powder (Fe) and carbon nanofiber (CNF) in coating form. The nanoparticles' dispersion was observed through optical microscope and phase image analysis on atomic force microscopy. The impedance behavior of such coated samples with 10 wt% nanofillers is frequency dependent except for CNF, which shows frequency‐independent behavior even at 2 wt% loading. The gas barrier property of the FeNG‐based and FeNiNG‐based coatings is better than that of pure TPU; however, G‐based, NG‐based, and NiZnFerrite‐based coatings show excellent barrier property. The coatings were evaluated for their microwave absorbency at low‐frequency (from 0.3 to 1.5 GHz) as well as high‐frequency (8–18 GHz) ranges. The FeNG‐based and FeNiNG‐based nanocomposite coatings showed good absorbency over a frequency range of 8 to 14 GHz as compared with those of others. The flexibility of the nanocomposite films is almost retained even at 10 wt% nanofiller loading. The weather resistance of the films was also evaluated, and the FeNiNG‐based coating outperformed the FeNG‐based coating as the latter is prone to oxidation on exposure to environment. Copyright © 2011 John Wiley & Sons, Ltd.  相似文献   

11.
Electrochemically co‐deposited sol–gel/Cu nanocomposites have been introduced as a novel, simple and single‐step technique for preparation of solid‐phase microextraction (SPME) coating to extract methadone (MDN) (a synthetic opioid) in urine samples. The porous surface structure of the sol–gel/Cu nanocomposite coating was revealed by scanning electron microscopy. Direct immersion SPME followed by HPLC‐UV determination was employed. The factors influencing the SPME procedure, such as the salt content, desorption solvent type, pH and equilibration time, were optimized. The best conditions were obtained with no salt content, acetonitrile as desorption solvent type, pH 9 and 10 min equilibration time. The calibration graphs for urine samples showed good linearity. The detection limit was about 0.2 ng mL−1. Also, the novel method for preparation of nanocomposite fiber was compared with previously reported techniques for MDN determination. The results show that the novel nanocomposite fiber has relatively high extraction efficiency.  相似文献   

12.
A magnetically separable NiFe2O4@GO–Pd composite (GO = graphene oxide) was successfully prepared by a facile one‐pot hydrothermal strategy. This new kind of hybrid material was fully characterized using powder X‐ray diffraction, Raman spectroscopy, X‐ray photoelectron spectroscopy, transmission electron microscopy and vibrating sample magnetometry. Structural characterizations confirmed the formation of NiFe2O4 and Pd nanocrystals, and the close anchoring between nanoparticles and GO sheets. Additionally, the as‐prepared NiFe2O4@GO–Pd nanocomposite was effectively employed in the palladium‐catalyzed Heck reaction in an ethanol–water system as a green solvent. The catalyst was completely recoverable with the simple application of an external magnetic field and with no obvious loss of catalytic activity even after six repeated cycles. Copyright © 2016 John Wiley & Sons, Ltd.  相似文献   

13.
Although selective laser sintering (SLS) has been widely applied in many fields, more research work is needed to develop proper polymer microspheres for SLS. Thermal‐induced phase separation (TIPS) is a facile way but rarely reported to prepare the polymer microspheres. The roles of liquid–liquid phase separation (LLPS) and crystallization in the TIPS process are not clear. In this study, proper polypropylene (PP) microspheres for SLS are successfully prepared via TIPS with xylene. The diameters and morphologies of these PP microspheres can be regulated easily by changing the PP concentration and the quench temperature. The large undercooling drives the solution into the metastable LLPS region and produces PP microspheres with smooth surfaces. The PP crystallization occurs both on the LLPS interface and inside the polymer‐rich phase when the solution is quenched to a temperature near the binodal line, and the tiny bent lamellae are formed on the microsphere surface. At higher temperature only PP crystallization occurs, which results in the formation of PP particles consisting of packed lamellae. The PP microspheres prepared here are suitable for SLS and promote the development of SLS potentially. © 2016 Wiley Periodicals, Inc. J. Polym. Sci., Part B: Polym. Phys. 2017 , 55, 320–329  相似文献   

14.
A novel heterogeneous magnetic palladium nano‐biocatalyst was designed by utilizing Irish moss, a family of sulfated polysaccharides extracted from algae, as a natural biopolymer. This magnetic Irish moss decorated with palladium (Pd–Fe3O4@IM) to form a biomagnetic catalytic system was synthesized and well characterized by FT–IR analysis, X‐ray powder diffraction, field emission scanning electron microscopy, energy‐dispersive X‐ray spectroscopy, atomic absorption spectroscopy and transmission electron microscopy. The catalyst was stable to air and moisture and displayed high catalytic activity in ligand‐free Suzuki–Miyaura cross‐coupling reactions conducted under green chemistry reaction conditions. The aromatic ketones are produced by the cross‐coupling reaction between acid chlorides and aryl boronic acid derivatives in high yields.  相似文献   

15.
In this study, the properties of polyethylene–octene elastomer/chitosan (POE/chitosan) and acrylic acid (AA)‐grafted‐polyethylene–octene elastomer/chitosan (POE‐g‐AA/chitosan) were examined using various characterizing instruments. Mechanical and thermal properties of POE deteriorated noticeably when it was blended with chitosan, due to the unsatisfactory compatibility between the two phases. The greater compatibility of POE‐g‐AA with chitosan, due to the formation of ester carbonyl and imide groups, led to a much better dispersion and homogeneity of chitosan in the POE‐g‐AA matrix and consequently to noticeably better mechanical properties. Furthermore, with a lower melting point temperature, the POE‐g‐AA/chitosan blend was more easily processed than POE/chitosan. POE‐g‐AA/chitosan had a higher water resistance than POE/chitosan. Both blends suffered weight loss when buried in soil, especially at high levels of chitosan substitution, indicating that both were biodegradable. The mechanical properties of both blends, such as tensile strength and elongation at break, also deteriorated after being buried in soil. © 2003 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 41: 3882–3891, 2003  相似文献   

16.
Various composites have been proposed in the literature for the fabrication of bioscaffolds for bone tissue engineering. These materials include poly(ε‐caprolactone) (PCL) with hydroxyapatite (HA). Since the biomaterial acts as the medium that transfers mechanical signals from the body to the cells, the fundamental properties of the biomaterials should be characterized. Furthermore, in order to control the processing of these materials into scaffolds, the characterization of the fundamental properties is also necessary. In this study, the physical, thermal, mechanical, and viscoelastic properties of the PCL‐HA micro‐ and nano‐composites were characterized. Although the addition of filler particles increased the compressive modulus by up to 450%, the thermal and viscoelastic properties were unaffected. Furthermore, although the presence of water plasticized the polymer, the viscoelastic behavior was only minimally affected. Testing the composites under various conditions showed that the addition of HA can strengthen PCL without changing its viscoelastic response. The results found in this study can be used to further understand and approximate the time‐dependent behavior of scaffolds for bone tissue engineering. Copyright © 2012 John Wiley & Sons, Ltd.  相似文献   

17.
Magnetic composite nanospheres (MCS) were first prepared via mini‐emulsion polymerization. Subsequently, the hybrid core–shell nanospheres were used as carriers to support gold nanoparticles. The as‐prepared gold‐loading magnetic composite nanospheres (Au‐MCS) had a hydrophobic core embed with γ‐Fe3O4 and a hydrophilic shell loaded by gold nanoparticles. Both the content of γ‐Fe3O4 and the size of gold nanoparticles could be controlled in our experiments, which resulted in fabricating various materials. On one hand, the Au‐MCS could be used as a T2 contrast agent with a relaxivity coefficient of 362 mg?1 ml S?1 for magnetic resonance imaging. On the other hand, the Au‐MCS exhibited tunable optical‐absorption property over a wavelength range from 530 nm to 800 nm, which attributed to a secondary growth of gold nanoparticles. In addition, dynamic light scattering results of particle sizing and Zeta potential measurements revealed that Au‐MCS had a good stability in an aqueous solution, which would be helpful for further applications. Finally, it showed that the Au‐MCS were efficient catalysts for reductions of hydrophobic nitrobenzene and hydrophilic 4‐nitrophenol that could be reused by a magnetic separation process. Copyright © 2014 John Wiley & Sons, Ltd.  相似文献   

18.
An effective one‐pot, convenient process for the synthesis of 1‐ and 5‐substituted 1H‐tetrazoles from nitriles and amines is described using1,4‐dihydroxyanthraquinone–copper(II) supported on Fe3O4@SiO2 magnetic porous nanospheres as a novel recyclable catalyst. The application of this catalyst allows the synthesis of a variety of tetrazoles in good to excellent yields. The preparation of the magnetic nanocatalyst with core–shell structure is presented by using nano‐Fe3O4 as the core, tetraethoxysilane as the silica source and poly(vinyl alcohol) as the surfactant, and then Fe3O4@SiO2 was coated with 1,4‐dihydroxyanthraquinone–copper(II) nanoparticles. The new catalyst was characterized using Fourier transform infrared spectroscopy, X‐ray diffraction, transmission electron microscopy, field emission scanning electron microscopy, dynamic light scattering, thermogravimetric analysis, vibration sample magnetometry, X‐ray photoelectron spectroscopy, nitrogen adsorption–desorption isotherm analysis and inductively coupled plasma analysis. This new procedure offers several advantages such as short reaction times, excellent yields, operational simplicity, practicability and applicability to various substrates and absence of any tedious workup or purification. In addition, the excellent catalytic performance, thermal stability and separation of the catalyst make it a good heterogeneous system and a useful alternative to other heterogeneous catalysts. Also, the catalyst could be magnetically separated and reused six times without significant loss of catalytic activity. Copyright © 2016 John Wiley & Sons, Ltd.  相似文献   

19.
A new fluorosilicone thermoplastic vulcanizate (TPV) composed of poly(vinylidene fluoride) (PVDF), silicone rubber (SR), and fluororubber (FKM) was successfully prepared through dynamic vulcanization. The morphological structure of the TPVs had core‐shell elastomer particles dispersed in a continuous PVDF matrix. Furthermore, the cross‐linking of core‐shell structure was controlled by adopting different curing agent. The effect of cross‐linking–controlled core‐shell structure on the morphology, crystallization behavior, stress relaxation test, solvent‐resistant properties of the obtained TPVs were investigated. It was found that the shell cross‐link had a significant influence on the crystallinity of the PVDF phase. The core‐shell bicross‐linked TPV was found to provide the lowest rate of relaxation. An obvious stress softening phenomenon was observed in the uniaxial loading‐unloading cycles in tension. The bicross‐linked TPV had good solvent resistant properties. The tensile strength of the bicross‐linked TPV was still 12 MPa even after immersed in butyl acetate for 48 hours.  相似文献   

20.
A new p‐phenylene–vinylene–thiophene‐based siloxane block copolymer has been synthesized. The copolymer consists of alternating rigid and flexible blocks. The rigid blocks are composed of phenylene–vinylene–thiophene‐based units, and the flexible blocks are derived from 1,3‐dialkyldisiloxane units. The former component acts as the chromophore, and allows fine tuning of band gap for blue‐light emission, while the latter imparts good solubility of the copolymer in organic solvents, and thus, should enhance processibility of the resulting copolymer. The thermal properties of the copolymer have been characterized by thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC). The photoluminescence (PL) of the copolymer in solution and in cast film has been studied. The effects of concentration on the PL intensity of the new copolymer in polymer blends with poly(methyl methacrylate) (PMMA) and poly(vinyl carbazole) (PVK) have also been described. Efficient energy transfer from PVK to the new block copolymer in the blended film was observed. © 2000 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 38: 1450–1456, 2000  相似文献   

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