Silane-modified MWCNT/PMMA composites – Preparation, electrical resistivity, thermal conductivity and thermal stability

Multiwalled carbon nanotubes (MWCNT) were modified using 3-isocyanato- propyltriethoxysilane (IPTES). Crosslinkable PMMA was prepared from MMA monomer and Vinyltriethoxysilane (VTES) (PMMA–VTES). The IPTES-modified MWCNT (Si-MWCNT) was mixed with the PMMA–VTES copolymer and crosslinked with catalyst to form Si-MWCNT/PMMA–VTES composites. The degree of condensation of tri-distribution structure of the Si-MWCNT/PMMA–VTES composites decreases as the Si-MWCNT content increases. The morphology of the Si-MWCNT/PMMA–VTES composites was analyzed by SEM and TEM. The MWCNTs were well dispersed in the PMMA–VTES matrix. Surface and volume electrical resistivity decreased as the MWCNT content increased. The thermal conductivity of the PMMA–VTES composites increased by 87.5% when 0.99 wt% Si-MWCNT content was added to neat PMMA–VTES. The thermal stability of the PMMA–VTES in nitrogen and air increased significantly even when a small quantity (0.5 wt%) of Si-MWCNT was added.     

二甲基硅油结构及热稳定性

采用红外(IR)光谱开展了二甲基硅油的结构研究。实验发现:二甲基硅油主要存在着νasCH3-二甲基硅油、νsCH3-二甲基硅油、δCH3-二甲基硅油、νSi-O-二甲基硅油、ρCH3-二甲基硅油和νSi-C-二甲基硅油等六种红外吸收模式。采用变温红外(TD-IR)光谱进一步开展了二甲基硅油的热稳定性研究。实验发现:在303~523 K温度范围内,随着测定温度的升高,二甲基硅油主要官能团对应的吸收频率及强度均有明显的改变,并进一步研究了其热变机理。     

Structure and thermal stability of nanocrystalline materials

Nanocrystalline materials, which are expected to play a key role in the next generation of human civilization, are assembled with nanometre-sized “building blocks” consisting of the crystalline and large volume fractions of intercrystalline components. In order to predict the unique properties of nanocrystalline materials, which are a combination of the properties of the crystalline and intercrystalline regions, it is essential to understand precisely how the structures of crystalline and intercrystalline regions vary with decrease in crystallite size. In addition, study of the thermal stability of nanocrystalline materials against significant grain growth is both scientific and technological interest. A sharp increase in grain size (to micron levels) during consolidation of nanocrystalline powders to obtain fully dense materials may consequently result in the loss of some unique properties of nanocrystalline materials. Therefore, extensive interest has been generated in exploring the size effects on the structure of crystalline and intercrystalline region of nanocrystalline materials, and the thermal stability of nanocrystalline materials against significant grain growth. The present article is aimed at understanding the structure and stability of nanocrystalline materials.     

Structure refinement and thermal stability of creedite

The crystal structure of the mineral creedite (hydrous calcium aluminum sulfate fluoride, Ca₃Al₂(F,OH)₁₀(SO₄) · 2H₂O) has been determined by Rietveld powder diffraction analysis. X-ray diffraction data obtained in the temperature range from 25 to 470°C indicate that the crystal structure of creedite is stable up to 390°C. We have measured the unit-cell parameters of creedite as functions of temperature and determined its thermal expansion coefficients. Above 390°C, the mineral decomposes.     

Structure refinement and thermal stability of gibbsite

The crystal structure of gibbsite (aluminum hydroxide) has been refined by Rietveld powder diffraction analysis, and the thermal stability of the crystal structure of the mineral has been studied in detail by high-temperature X-ray diffraction. The X-ray diffraction data obtained in the temperature range from 25 to 300°C indicate that the crystal structure of gibbsite is stable up to 200–250°C. The unit-cell parameters of gibbsite increase with temperature. Above 200°C, the gibbsite to boehmite (AlO(OH)) phase transformation begins.     

Correlation between electrical properties and thermal stability in Ni-Si-B metallic glasses

The temperature coefficient of resistivity (TCR), specific resistivity _{3000 K}, crystallization temperatureT _x and activation energyE _a for crystallization in various Ni-Si-B metallic glasses were measured and relationships among them were examined. It was found that the values of TCR decreased with increasing metalloid (Si, B) contents and by substituting silicon atoms for boron atoms, but conversely the values of _{300 K},T _x andE _a increased. A very close correlation was observed between TCR andT _x orE _a. The compositional dependences of TCR, _300K,T _x andE _a and good correlations among them can be explained qualitatively by considering the short-range structure and the directional chemical bonding between nickel and silicon or boron atoms.     

Formation,thermal stability and electrical resistivity of quasicrystalline phase in rapidly quenched Al-Cr alloys

The icosahedral quasicrystal has been found to appear in a wide composition range from about 5 to 16 at % Cr in rapidly quenched Al-Cr alloys, but the formation of the quasicrystal line single phase was limited only in the vicinity of about 15.5at% Cr. Analytical solute concentrations in the quasicrystalline phase are not always constant and increase continuously from 9.0 to 15.4 at% Cr with increasing nominal solute concentration from 6 to 15.4%. The quasicrystal can be approximately formulated to be Al₁₁ Cr₂ with a maximum deviation of about 6% Cr from the stoichiometric ratio to lower concentration side. Vickers hardness and electrical resistivity increase gradually with increasing chromium content and rapidly at about 14.5% Cr, and their values of Al_84.6Cr_15.4 quasicrystal are 710 DPN, 2.38m at 4.2 K, and 2.72m at 293 K. On the other hand, the onset transformation temperature of quasicrystal to crystalline phase,T _t, and the heat of transformation, H _t show maximum values of 644 K and 1805 J mol^–1 at 14.5% Cr and decrease to 625 K and 550 J mol^–1 at 15.4% Cr. Al_84.6Cr_15.4 quasicrystal trans forms at two stages to a stable orthorhombic Al₁₁Cr₂ compound through a metastable intermediate phase with unidentified structure, while the quasicrystal + Al structure in Al-Cr alloys containing less than 15% Cr changes directly to stable phases of compounds and aluminium. The distinct difference in transformation behaviour of the quasicrystal is thought to be the reason for the abrupt changes inT _t and H _t at a composition between 14.5 and 15.4% Cr.     

Structure and thermal stability of vapour-deposited Fe-Cu alloys

The structure of vapour-deposited Fe-Cu alloys was analysed and compared with that obtained by quenching from the liquid and solid state. Transmission electron microscopy was used to observe grain size at room temperature and precipitation at elevated temperatures. A discussion of thermal stability of metastable phases is based on nucleation mechanisms and diffusion coefficients in the highly defect or glassy state and the crystalline state.     

Structure, properties, and thermal stability of nanocrystallite Fe-Ti-N soft magnetic films

We deposited Fe-Ti-N magnetic films with a high sputtering power of 7 W/cm/sup 2/. When the composition of the films was in the range of Fe-Ti(3.9 at.%)-N(8.8 at.%) to Fe-Ti(3.3 at.%)-N(13.5 at.%), the films were composed of /spl alpha/' and Ti/sub 2/N precipitates. With the addition of nitrogen, 4/spl pi/M/sub s/ became higher than that of pure iron, reaching a maximum of 23.8 kG. At the same time, H/sub c/ was reduced to a minimum of 1.12 Oe. The best films can meet the needs of the recording head in dual-element giant magnetoresistive/inductive heads, yielding high storage density (10 Gb/in/sup 2/). The incorporation of N in /spl alpha/-Fe brought about the /spl alpha/' phase with its higher saturation magnetization. Ti additions inhibited the equilibrium decomposition /spl alpha/'/spl rarr//spl alpha/+/spl gamma/'. Because H/sub C//sup D//spl prop/D/sup 6/, where D is average grain diameter, grain size control is very important. The nitrogen induces severe distortion of the /spl alpha/' lattice, which can cause the grains to break into pieces and reduce the grain size. High sputtering power also led to the formation of fine grains, with diameter in the order of 14 nm. Probably Ti/sub 2/N is preferentially precipitated on the grain boundary, pinning the grain boundary and stabilizing the grain size during high-temperature heat treatment. The temperature limit for stability of the structure and its associated low coercivity was not less than 520/spl deg/C.     

Morphology, thermal, electrical and electrochemical stability of nano aluminium-oxide-filled polyvinyl alcohol composite gel electrolyte

In the present work, an attempt has been made to develop nano aluminium oxide (Al₂O₃)-filled polyvinyl alcohol (PVA) composite gel electrolytes. Surface morphological studies, thermal behaviour, electrochemical stability and electrical characterization of these composite gel electrolytes have been performed. An increase in the concentration of Al₂O₃ in composite gel electrolytes increases the amorphous characteristics of pure PVA. Bulk conductivity of composite gel electrolytes increases by an order of magnitude on addition of a nano filler. Maximum conductivity of 5·81 × 10^?2 S/cm is observed for 6 wt% Al₂O₃-filled polymer gel composite electrolytes. Temperature dependence of electrical conductivity shows a combination of Arrhenius and Vogel-Tamman-Fulcher (VTF) nature. Maximum current stability during oxidation and reduction cycle is noticed for 6 wt% Al₂O₃-filled PVA composite electrolyte, viz. ±1·65 V.     

Structure, hardness and thermal stability of nanolayered TiN/CrN multilayer coatings

Nanolayered TiN/CrN multilayer coatings were deposited on silicon substrates using a reactive DC magnetron sputtering process at various modulation wavelengths (Λ), substrate biases (V_B) and substrate temperatures (T_S). X-ray diffraction (XRD), nanoindentation and atomic force microscopy (AFM) were used to characterize the coatings. The XRD confirmed the formation of superlattice structure at low modulation wavelengths. The maximum hardness of the TiN/CrN multilayers was 3800 kg/mm² at Λ=80  Å, V_B=−150 V and T_S=400°C. Thermal stability of TiN, CrN and TiN/CrN multilayer coatings was studied by heating the coatings in air in the temperature range (T_A) of 400-800°C. The XRD data revealed that TiN/CrN multilayers retained superlattice structure even up to 700°C and oxides were detected only after T_A?750°C, whereas for single layer TiN and CrN coatings oxides were detected even at 550°C and 600°C, respectively. Nanoindentation measurements showed that TiN/CrN multilayers retained a hardness of 2800 kg/mm² upon annealing at 700°C, and this decrease in the hardness was attributed to interdiffusion at the interfaces.     

Investigation of thermal stability, phase formation, electrical, and microstructural properties of sputter-deposited titanium aluminide thin films

Titanium aluminide thin films are being considered as coating materials for high temperature applications due to their high melting points and high oxidation resistance. In this study, Ti₃₇Al₆₃ and Ti₅₃Al₄₇ thin films are deposited onto SiO₂ substrates by RF magnetron sputtering using compound targets and then annealed in vacuum to investigate the properties of the films. Rutherford backscattering spectrometry, X-ray diffractometry, transmission electron microscopy, and four-point probe measurements are used to analyze the characteristics of Ti₃₇Al₆₃ and Ti₅₃Al₄₇ thin films for high temperature electronics applications. The films show good thermal stability up to 700 °C for 1 h in vacuum. Reasonable resistivity is obtained when appropriate compositions and anneal conditions are used.     

Structure, hardness and thermal stability of TiAlN and nanolayered TiAlN/CrN multilayer films

TiAlN films were deposited on silicon (1 1 1) substrates from a TiAl target using a reactive DC magnetron sputtering process in Ar+N₂ plasma. Films were prepared at various nitrogen flow rates and TiAl target compositions. Similarly, CrN films were prepared from the reactive sputtering of Cr target. Subsequently, nanolayered TiAlN/CrN multilayer films were deposited at various modulation wavelengths (Λ). X-ray diffraction (XRD), energy dispersive X-ray analysis, nanoindentation and atomic force microscopy were used to characterize the films. The XRD confirmed the formation of superlattice structure at low modulation wavelengths. The maximum hardness of TiAlN/CrN multilayers was 3900 kg/mm², whereas TiAlN and CrN films exhibited maximum hardnesses of 3850 and 1000 kg/mm², respectively. Thermal stability of TiAlN and TiAlN/CrN multilayer films was studied by heating the films in air in the temperature range (T_A) of 500-900 °C for 30 min. The XRD spectra revealed that TiAlN/CrN multilayers were stable up to 800 °C and got oxidized substantially at 900 °C. On the other hand, the TiAlN films were stable up to 700 °C and got completely oxidized at 800 °C. Nanoindentation measurements performed on the films after heat treatment showed that TiAlN retained a hardness of 2200 kg/mm² at T_A=700 °C and TiAlN/CrN multilayers retained hardness as high as 2600 kg/mm² upon annealing at 800° C.     

Structure and thermal stability of supercooled Li2SO4 melts

Journal of Materials Science Letters -     

Poly(3-hexylthiophene)/hexamine modified ZnO hybrid nanocomposite: structural,optical, thermal and electrical transport studies

This paper reports the synthesis of poly(3-hexylthiophene) (P3HT)/HA@ZnO nanocomposite by in situ polymerization and demonstrates their thermal, morphological and optoelectronic properties. Zinc oxide (ZnO) nanoparticles were prepared by the simple approach of co- precipitation method using zinc acetate dihydrate as precursor modified by hexamine (HA) acting as a capping agent. Structural and photo physical studies shows that conjugated polymer chains intimately contact with the inorganic semiconductor. ZnO has wurtzite structure with average crystallite size of 40 nm. The emission spectra indicate that modified ZnO nanoparticles results in more efficient photo induced charge transfer than that of the simple nanocomposite of P3HT/ZnO. The morphological studies revealed that the transformation of granular morphology of P3HT to the clusters in P3HT/HA@ZnO hybrid nanocomposites. Cyclic voltammeter elucidates the electrochemical behavior and the HOMO–LUMO energy levels of the nanocomposites. The results indicate that the P3HT/HA@ZnO nanocomposite has energy gap of 0.72 eV, indicating this composite has potential for the fabricating hybrid organic–inorganic solid state solar cells. A solar to electric energy conversion efficiency of 0.1238 % was attained with the system.     

Large thermoelectric figure-of-merits from SiGe nanowires by simultaneously measuring electrical and thermal transport properties

The strongly correlated thermoelectric properties have been a major hurdle for high-performance thermoelectric energy conversion. One possible approach to avoid such correlation is to suppress phonon transport by scattering at the surface of confined nanowire structures. However, phonon characteristic lengths are broad in crystalline solids, which makes nanowires insufficient to fully suppress heat transport. Here, we employed Si-Ge alloy as well as nanowire structures to maximize the depletion of heat-carrying phonons. This results in a thermal conductivity as low as ～1.2 W/m-K at 450 K, showing a large thermoelectric figure-of-merit (ZT) of ～0.46 compared with those of SiGe bulks and even ZT over 2 at 800 K theoretically. All thermoelectric properties were "simultaneously" measured from the same nanowires to facilitate accurate ZT measurements. The surface-boundary scattering is prominent when the nanowire diameter is over ～100 nm, whereas alloying plays a more important role in suppressing phonon transport for smaller ones.     

微米、亚微米高铬铁基纤维的结构和热稳定性

研究了热处理对高铬铁基纤维样品的结构和磁性的影响.微米级、亚微米级高铬铁基纤维由Cu-11Fe-4Cr原位复合丝材硝酸法萃取得到.采用X-射线衍射和扫描电镜观察分析了样品的结构和形貌,采用振动样品磁强计测试了样品的磁性,利用热重-差热分析比较了不同变形量的高铬铁基纤维在空气中的热稳定性.结果表明,在空气中低于400 ℃加热1 h后,高铬铁基纤维保持BCC结构不变,样品的饱和磁化强度均大于103 A·m2·kg-1;经800 ℃加热1 h后,由铁磁性的α-(Fe,Cr)固溶体转变为顺磁性的(Fe,Cr)2O3,样品的饱和磁化强度显著下降.随着变形量增大,较细的高铬铁基纤维的热稳定性较差.微米级、亚微米级高铬铁基纤维的热稳定性显著高于微米级多晶铁纤维.     

Effect of P addition on the thermal stability and electrical characteristics of NiSi films

Immersion Ni-P deposition is undoubtedly one of the most important catalytic deposition process, due to its simplicity in operation and low equipment cost. In this study, immersion deposited Ni-P films were used to form Ni-silicide films. Ni-P films with a thickness of 100 nm were fabricated by immersing Si(100) substrates in an aqueous deposition solution. Ni-silicide films were then formed by annealing the samples in a furnace at temperatures ranging from 400 °C to 900 °C for 1 h in an argon ambient. Experimental results indicate that a phosphor addition in Ni films increased the transformation temperature of NiSi to NiSi₂ to 900 °C. Moreover, the feasibility of enhancing the thermal stability of NiSi by varying the interface energy at the NiSi₂/Si interface and the surface energy of a Ni-P-Si capping layer on the NiSi surface is discussed.