Synergetic effect of thermal conductive properties of epoxy composites containing functionalized multi-walled carbon nanotubes and aluminum nitride

This study investigates the thermal conductivity of epoxy composites containing two hybrid fillers which are multi-walled carbon nanotubes (MWCNTs) and aluminum nitride (AlN). To form a covalent bonds between the fillers and the epoxy resin, poly(glycidyl methacrylate) (PGMA) were grafted onto the surface of nano-sized MWCNTs via free radical polymerization and micro-sized AlN was modified by zirconate coupling agent. Results show that functionalized fillers improve thermal conductivity of epoxy composites, due to the good dispersion and interfacial adhesion, which is confirmed by scanning electron microscope. Furthermore, the hybrid fillers provide synergetic effect on heat conductive networks. The thermal conductivity of epoxy composites containing 25 vol.% modified AlN and 1 vol.% functionalized MWCNTs is 1.21 W/mK, comparable to that of epoxy composites containing 50 vol.% untreated AlN (1.25 W/mK), which can reduce the half quantity of AlN filler used.     

Electrical and humidity sensing properties of lead(II) tungstate–tungsten(VI) oxide and zinc(II) tungstate–tungsten(VI) oxide composites

Lead(II) tungstate and zinc(II) tungstate were prepared by a solution route and sintered at 973 K in the form of cylindrical discs. Experimental results on PbWO₄ (PW) and WO₃ (WO) composites for humidity sensing are described. Sintered polycrystalline discs of PbWO₄ (PWWO-10), WO₃ (PWWO-01), ZnWO₄ (ZWWO-10) and composites of PW or ZW and WO in the mole ratios 8:2, 6:4, 4:6, 2:8 designated as PWWO and ZWWO-82, 64, 46 and 28, respectively and doped with 2 mol% of Li⁺ were studied. The composites were subjected to dc conductance measurements over the temperature range 373–673 K in air atmosphere from which activation energies were determined. The activation energy values for dc conductance were found to be in the range of 1.09–1.30 eV. The composites were identified by powder XRD data. The scanning electron microscopy (SEM) studies were carried out to study the surface and pores structure of the sensor materials. The composites were subjected to dc resistance measurements as a function of relative humidity in the range of 5–98% RH, achieved by different water vapor buffers thermostated at room temperature. The sensitivity factor (S_f=R_5%/R_98%) measured at 298 K revealed that PWWO-28 and ZWWO-46 composites have the highest humidity sensitivity factor of 17 615±3000 and 2666±550, respectively. The response and recovery time for these humidity sensing composites were good.     

Crystal growth and scintillation properties of potassium strontium bromide

In this work, potassium strontium bromide activated with divalent europium, (KSr₂Br₅:Eu) has been studied. It has a monoclinic crystal structure and a density of 3.98 g/cm³. Two single crystals of KSr₂Br₅ doped with 5% Eu²⁺, with diameters of 13 mm and 22 mm, were grown in a two zone transparent furnace via the Bridgman technique. The X-ray excited emission spectrum consisted of a single peak at ∼427 nm due to the 5d–4f transition in Eu²⁺. The measured light yield and energy resolution at 662 keV was 75,000 ph/MeV and 3.5%. At low energies KSr₂Br₅:Eu 5% also displays good energy resolution, 6.7% at 122 keV and 7.9% at 59.5 keV.     

Low energy implantation to inhibit wear in N+ ions implanted WC–Co composite

This work discusses the influence of nitrogen ion (N⁺) implantation on wear resistance of WC–Co composite. The WC–Co samples were bombarded at low N⁺ ions energies of 20 and 30 keV and doses of 10¹⁷ and 2 × 10¹⁷ ions cm⁻². Tribological tests were conducted against cylindrical 100Cr6 pin at 200 N load and 180 mm s⁻¹ speed. The tests use water lubrication and four sample types with Co binder content ranging in 6.5–25%. The X-ray spectra reveal that implantation is able to transform the original [CFC] Co structure of virgin surface to harder amorphous phase. However, it was found that excessive low binder content alters the wear behavior on non-implanted samples since it causes wear rate transition from 0.59 × 10⁻⁷ to 2.1 × 10⁻⁷ mm³/(mm² s) imposing hence instable wear regime. The SEM micrographs confirm the formation of transferred film within the implanted worn surface owing to (i) an enhancement in Co flow and (ii) a generation of oxides (Fe₂O₃, Fe₃O₄, Co₂O₃, WO₂). While the formed film acts to inhibit severe abrasion, the material removal process combining cobalt flow and carbide grains pull-out seems to be associated with oxidation mechanisms to be accentuated with energy increase. The most improvements in wear resistance were observed on samples with the highest Co content and the results were found more sensitive to N⁺ ions implantation energy than dose.     

Effect of hydrothermal temperature on structure and photochromic properties of WO3 powder

Tungsten trioxide (WO₃) powders were prepared via a simple hydrothermal method. The morphology, structure and photochromic activity of the synthesized WO₃ powders were studied by X-ray diffraction, scanning electron microscopy and UV–vis spectrophotometer combined with color difference meter. The results showed the synthesized WO₃ powders with hexagonal phase got much better photochromic properties than the WO₃ powders with cubic phase, the ones not appear until about 160 °C. Besides, the WO₃ powder synthesized at 120 °C exhibited the best photochromic properties of the samples prepared below 160 °C, the particles of which formed a shape of clusters of cactus with uniform size and good dispersion.     

Effects of WO3 addition on the structure and electrical properties of Pb3O4 modified PZT–PFW–PMN piezoelectric ceramics

The ceramics were prepared successfully by Pb₃O₄ and WO₃ additions to 0.90Pb(Zr,Ti)O₃–0.03Pb(Fe_2/3W_1/3)O₃–0.07Pb(Mn_1/3Nb_2/3)O₃ (0.90PZT–0.03PFW–0.07PMN). Effects of the additions on the structure, bulk density and electrical properties of ceramics were investigated. The results revealed that the proper additions of WO₃ with 2.0 wt.% Pb₃O₄ excess could form liquid phase that promoted the densification of the ceramics. The fracture mode changed from transgranular to intergranular as increasing WO₃ with 2.0 wt.% Pb₃O₄ excess. The piezoelectric and dielectric properties were also promoted by excess of Pb₃O₄ and WO₃ additions. The optimized electrical properties were obtained at excess of 2.0 wt.% Pb₃O₄ and 0.15 wt.% WO₃. The parameters were as follows: d₃₃ = 351 pC/N, K_p = 0.64, Q_m = 1882, ɛ_r = 1798, tan δ = 0.0052, P_r = 19.94 μC/cm² and E_c = 11.98 kV/cm, which shows high K_p, Q_m, d₃₃ and low tan δ can be obtained simultaneously by adding WO₃ addition to Pb₃O₄ modified PZT–PFW–PMN system.     

Fabrication of WO3 nanofibers by high voltage electrospinning

Mixtures of 0.1, 0.3, and 0.5 mmol ammonium metatungstate hydrate (AMH), and poly (vinyl alcohol) (PVA) were electrospun by a + 20 kV direct voltage to synthesize fibers. Those of 0.5 mmol AMH were further calcined to have PVA removed and crystalline degree improved. At 500 °C and 2 h calcination, WO₃ nanofibers, including two main stretching modes, 3.24 eV direct energy gap, and 378 nm wavelength violet emission were detected. A possible formation mechanism of WO₃ nanofibers was proposed according to the experimental results.     

Structural and microstructural behaviour of SnO2 dense ceramics doped with ZnO and WO3

SnO₂-based varistors doped with ZnO and WO₃ were prepared by mixed oxide method. Experimental evidence shows that the increase in ZnO amount increases the volume and microstrain of unit cell while the WO₃ promotes a decrease. The effect of ZnO and WO₃ additives could be explained by the substitution of Sn^4 +  by Zn^2 +  and W^6 + . The addition of WO₃ inhibits the grain growth due to the segregation in the grain boundary without influence in the densification of the samples. Besides that, an increase in the electrical resistance of the SnO₂–ZnO–WO₃ system was observed independent of the WO₃ concentration.     

Crystal structure and electrical properties of CaxWO3 (0.01 ≤ x ≤ 0.15) prepared by hybrid microwave synthesis

Calcium tungsten bronzes Ca_xWO₃ (0.01 ≤ x ≤ 0.15) were synthesized by hybrid microwave method from mixtures of CaO, WO₃ and tungsten powder. Single-phased samples can be obtained by microwave heating within 40 min. With the increase of calcium content, the crystal structure of Ca_xWO₃ transforms from orthorhombic (0.01 ≤ x ≤ 0.02) to tetragonal (0.03 ≤ x ≤ 0.11) and then to cubic (0.12 ≤ x ≤ 0.15). The average size of crystallites is in the range 1–5 μm. All samples show semiconductor behaviour in their temperature dependence of resistivity. The electrical conduction mechanism changes from variable-range hopping to the thermally activated mechanism when x > 0.12.     

Synthesis and electrochemical properties of nanosized LiFeO2 particles with a layered rocksalt structure for lithium batteries

Layered rocksalt-type LiFeO₂ particles (O3-LiFeO₂) with average particle sizes of ca. 40 and 400 nm were synthesized by an ion exchange reaction from α-NaFeO₂ precursors. X-ray diffraction (XRD) patterns and scanning electron microscopy (SEM) images confirmed the formation of nanosized O3-LiFeO₂. 40-nm LiFeO₂ exhibited a higher discharge capacity (115 mAh g^?1) than 400-nm LiFeO₂ (80 mAh g^?1), and also had better rate characteristics. The downsizing effect and cation disorder between the lithium and iron layers may have improved the electrochemical activity of the LiFeO₂ particles. Transmission electron microscopy (TEM) observation indicated a phase transition from O3-LiFeO₂ to a cubic lattice system during the electrochemical process. The cubic lithium iron oxide exhibited stable electrochemical reactions based on the Fe²⁺/Fe³⁺ and Fe²⁺/Fe⁰ redox couples at voltages between 4.5 and 1.0 V. The discharge capacities of 40-nm LiFeO₂ were ca. 115, 210, and 390 mAh g^?1 under cutoff voltages of 4.5–2.0 V, 4.5–1.5 V, and 4.5–1.0 V, respectively.     

Sintering and technological properties of alumina/zirconia/nano-TiO2 ceramic composites

The present work focuses on studying the effect of nano TiO₂ (0.0–25 mass%) on the sintering behavior and mechanical properties of alumina/zirconia ceramic composites. Al₂O₃–ZrO₂–TiO₂ oxides mixture was sintered at 1600 °C to obtain the desired composites. The sinterability and the technological properties of these ceramic composites, i.e. the sintering parameters and microhardness as well as thermal shock resistance were investigated. Moreover, phase composition and microstructure of the sintered bodies were examined using X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersive spectrometer (EDS). The results revealed that nano TiO₂ is a beneficial component for alumina/zirconia ceramic composites. The batch containing 20 mass% TiO₂ exhibited the highest sintering and mechanical properties as well as resistance to thermal shock. The obtained microstructure exhibited high compacted ceramic matrix composites.     

Structural,electrical and electrochemical parameters of PEO–NaClO3 composite for battery applications

Polyethylene oxide–NaClO₃ composite have been prepared by solution casting technique with different weight percentages as a polymer electrolyte for battery application. The prepared composites were characterized by various tools like XRD, FTIR and SEM. The X-ray diffraction analysis shows the complexation of polymer with salt and existence of both crystalline and amorphous phases. From FTIR spectra confirms the formation of PEO–NaClO₃ composites. SEM images shows the grains are highly agglomerated and its average size increases with increase in salt ratio. Frequency dependence of dielectric property and ac electrical conductivity of polymer electrolytes were studied within the frequency range of 50 Hz to 5 MHz using complex impedance analysis technique. Ionic conductivity follows Arrhenius type behavior as a function of temperature. The fabricated cell of 25 wt.% of PEO–NaClO₃ composites generated high current of 1.79 A.     

Mechanical behavior of nickel + aluminum powder-reinforced epoxy composites

The mechanical behavior of composites containing micro-sized Ni particles and micro- or nano-sized Al particles, fabricated by casting/curing with epoxy, were studied to investigate their mechanical behavior for potential application as structural energetic materials. Reverse Taylor anvil-on-rod impact tests combined with high-speed digital photography provided information about the high-strain-rate transient deformation and failure response. The nano Al-containing composite exhibited a higher elastic modulus and static and dynamic compressive strengths than pure epoxy and micro Al-containing composite due to increased cross-link density, as revealed by dynamic mechanical analysis. Microstructural characterization of the cast composites revealed that micro-sized Ni and Al remained homogeneously and intimately mixed within the epoxy matrix. In contrast, the composites containing micro Ni and nano Al showed separation of the nano Al particles, effectively forming a nano Al + epoxy matrix surrounding the Ni particles and consequently altering the physical response and enhancing the mechanical properties of the composite.     

Nanocrystalline matrix TiC–Al3Ti and TiC–Al3Ti–Al composites produced by reactive hot-pressing of milled powders

Mechanically alloyed nanocrystalline TiC powder was short-term milled with 40 vol.% of Al powder. The powders mixture was consolidated at 1200 °C under the pressure of 4.8 GPa for 15 s and at 1000 °C under the pressure of 7.7 GPa for 180 s. The bulk materials were characterised by X-ray diffraction, light and scanning electron microscopy, energy dispersive spectroscopy, hardness, density and open porosity measurements. During the consolidation a reaction between TiC and Al occurred, yielding an Al₃Ti intermetallic. The microstructure of the produced composites consists of TiC areas surrounded by lamellae-like regions of Al₃Ti intermetallic (after consolidation at 1200 °C) or Al₃Ti and Al (after consolidation at 1000 °C). The mean crystallite size of TiC is 38 nm. The hardness of the TiC–Al₃Ti and TiC–Al₃Ti–Al composites is 13.28 GPa (1354 HV1) and 10.22 GPa (1041 HV1) respectively. The produced composites possess relatively high hardness and low density. The results obtained confirmed satisfactory quality of the consolidation with keeping a nanocrystalline structure of TiC.     

Sodium gluconate-assisted hydrothermal synthesis,characterization and electrochemical performance of LiFePO4 powders

Nano- and micro-sized LiFePO₄ powders were synthesized by a sodium gluconate (C₆H₁₁NaO₇)-assisted hydrothermal synthesis method at 220 °C for 10 h with pH = 2–7. The resulting powders were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), and energy-dispersive X-ray spectrometer (EDS). The obtained data showed that the pH of synthesis solution played a key role in the formation of the LiFePO₄ powders with different morphologies, such as ball-like microspheres, irregular microspheres with the agglomerated rods and particles, sphere-like nanoparticles and nano-ellipsoids. The results from electrochemical performance measurements revealed that the charge–discharge cycling characteristics of the samples were strongly dependent on their morphologies. In particular, the ellipsoidal LiFePO₄ nanoparticles with the average size of 70–90 nm showed the highest initial discharge capacity of 150 mA h g⁻¹ at 0.1 C rate, and cycling stability of the ellipsoidal LiFePO₄ nanoparticles was optimum among all the samples prepared due to their dual advantages of high tap density and good diffusion property. The present study offers a simple morphology-controllable route, without carbon coating or doping with supervalent cations, to synthesize and to design high performance cathode materials for lithium-ion batteries.     

High-temperature dielectric and electromagnetic interference shielding properties of SiCf/SiC composites using Ti3SiC2 as inert filler

Ti₃SiC₂ filler has been introduced into SiC_f/SiC composites by precursor infiltration and pyrolysis (PIP) process to optimize the dielectric properties for electromagnetic interference (EMI) shielding applications in the temperatures of 25–600 °C at 8.2–12.4 GHz. Results indicate that the flexural strength of SiC_f/SiC composites is improved from 217 MPa to 295 MPa after incorporating the filler. Both the complex permittivity and tan δ of the composites show obvious temperature-dependent behavior and increase with the increasing temperatures. The absorption, reflection and total shielding effectiveness of the composites with Ti₃SiC₂ filler are enhanced from 13 dB, 7 dB and 20 dB to 24 dB, 21 dB and 45 dB respectively with the temperatures increase from 25 °C to 600 °C. The mechanisms for the corresponding enhancements are also proposed. The superior absorption shielding effectiveness is the dominant EMI shielding mechanism. The optimized EMI shielding properties suggest their potentials for the future shielding applications at temperatures from 25 °C to 600 °C.     

Microstructure and mechanical properties of in situ TiC and Nd2O3 particles reinforced Ti–4.5 wt.%Si alloy composites

(TiC + Nd₂O₃)/Ti–4.5 wt.%Si composites were in situ synthesized by a non-consumable arc-melting technology. The phases in the composites were identified by X-ray diffraction. Microstructures of the composites were observed by optical microscope and scanning electron microscope. The composite contains four phases: TiC, Nd₂O₃, Ti₅Si₃ and Ti. The TiC and Nd₂O₃ particles with dendritic and near-equiaxed shapes are well distributed in Ti–4.5 wt.%Si alloy matrix, and the fine Nd₂O₃ particles exist in the network Ti + Ti₅Si₃ eutectic cells and Ti matrix of the composites. The hardness and compressive strength of the composites are markedly higher than that of Ti–4.5 wt.%Si alloy. When the TiC content is fixed as 10 wt.% in the composites, the hardness is enhanced as the Nd₂O₃ content increases from 8 wt.% to 13 wt.%, but the compressive strength peaks at the Nd₂O₃ content of 8 wt.%.     

Fabrication of Yb3+/Er3+ codoped Bi2O3–WO3–TeO2 pedestal type waveguide for optical amplifiers

We report, for the first time to our knowledge, experimental results on pedestal waveguides produced with Yb³⁺/Er³⁺ codoped Bi₂O₃–WO₃–TeO₂ thin films deposited by RF Sputtering for photonic applications. Thin films were deposited using Ar/O₂ plasma at 5 mTorr pressure and RF power of 40 W on substrates of silicon wafers. The definition of the pedestal waveguide structure was made using conventional optical lithography followed by plasma etching. Propagation losses around 2.0 dB/cm and 2.5 dB/cm were obtained at 633 and 1050 nm, respectively, for waveguides in the 20–100 μm width range. Single-mode propagation was measured for waveguides width up to 10 μm and 12 μm, at 633 nm and 1050 nm, respectively; for larger waveguides widths multi-mode propagation was obtained. Internal gain of 5.6 dB at 1530 nm, under 980 nm excitation, was measured for 1.5 cm waveguide length (∼3.7 dB/cm). The present results show the possibility of using Yb³⁺/Er³⁺ codoped Bi₂O₃–WO₃–TeO₂ pedestal waveguide for optical amplifiers.     

Al3Ni2–Al composites with nanocrystalline intermetallic matrix produced by consolidation of milled powders

Mechanically alloyed nanocrystalline Al₆₃Ni₃₇ powder with a metastable structure of NiAl phase was mixed with 20, 30 and 40 vol.% of Al powder. The powder mixtures as well as pure powder of Al₆₃Ni₃₇ alloy were consolidated at 600 °C under the pressure of 7.7 GPa. The bulk materials were characterised by structural investigations (X-ray diffraction, light and scanning electron microscopy, energy dispersive spectroscopy), compression and hardness tests and measurements of density and open porosity. During the consolidation, the metastable NiAl phase transformed into the equilibrium Al₃Ni₂ intermetallic. The mean crystallite size of the Al₃Ni₂ intermetallic in the bulk materials is below 40 nm. The microstructure of the composite samples consists of Al₃Ni₂ intermetallic areas surrounded by lamellae-like Al regions. The hardness of the produced Al₃Ni₂–Al composites is in the range of 5–6.5 GPa (514–663 HV1), while that of the Al₃Ni₂ intermetallic is 9.18 GPa (936 HV1). The compressive strength of the composites increases with the decrease of Al content, ranging from 567 MPa to 876 MPa. The plastic elongation of the composites was increasing with the increase of Al content, while the Al₃Ni₂ intermetallic failed in the elastic region.     

New developments at the INE-Beamline for actinide research at ANKA

The INE-Beamline for actinide research at the synchrotron source Ångströmquelle Karlsruhe (ANKA) completed its first year of operation in October 2006. Experiments on radioactive samples with activities up to 10⁶ times the limit of exemption at X-ray energies from around 2.1 keV (P K-edge) to 25 keV (Pd K-edge) are possible. Three recent instrumental developments at the Nuclear Waste Disposal (INE)-Beamline are presented: a Quick-XAFS mode of operating the Lemonnier-type monochromator in fixed exit for time-resolved experiments, total electron yield detection, and the use of one-dimensional compound refractive lenses, fabricated at the Institut für Mikrostrukturtechnik (IMT) at Forschungszentrum Karlsruhe (FZK), as a virtual slit for surface sensitive X-ray studies. Future upgrades for lowering the attainable energy, installing a microfocus option, and commissioning a cryostat for radioactive samples are planned.