Observation and formation mechanism of individual graphene foils inside multi-walled carbon nanotubes

The formation of individual graphene foils (GF) has been evidenced in the present study inside multi-walled carbon nanotubes. The graphene foils are attached on one side to a catalyst nanoparticle and on the other side to the internal walls of the nanotube. Moreover, results suggest that a necking process occurs in which internal carbon walls are deformed until formation of the graphene foil. A possible mechanism for the GF formation is then proposed.     

Synthesis of zirconium tungstate–zirconia core–shell composite particles

In this work, ZrW₂O₈–ZrO₂ core–shell composite particles were synthesized. ZrW₂O₈ that was used in the core is a material with negative coefficient of thermal expansion, and it was synthesized from a high-pH precursor based on use of tungstic acid and zirconium acetate. Shell layer was composed of ZrO₂ nanocrystallites and precipitated from an aqueous solution by urea hydrolysis. While volume of the shell was effectively controlled by the initial zirconium ion concentration in the solutions, the rate of precipitation was a function of the ratio of initial concentrations of urea to zirconium ions. It is hypothesized that isolation of the ZrW₂O₈ within a layer of ZrO₂, will be a key element in solving problems associated with reactivity of ZrW₂O₈ towards other components in sintering of ceramic–ceramic composites with tuned or zero thermal expansion coefficient.     

Spatially resolved X-ray spectroscopy using a flat HOPG crystal

A novel design of a 1-D imaging X-ray spectrometer is implemented, using a high efficiency HOPG (highly oriented pyrolitic graphite) Bragg crystal and a double-entrance-slit. The double slit provides self-calibration of the imaging magnification. The spatial and spectral resolutions and dispersion are characterised both analytically and by ray tracing simulations. A key feature of this approach is that it enables the X-ray spectrum to be measured over different regions of the plasma source. The application of this instrument is demonstrated in high intensity laser-foil interaction experiments.     

Study on conductivity and redox stability of iron orthovanadate

FeVO₄ was synthesised by conventional solid state technique. Impedance measurements using a silver electrode were unsuccessful due to a solid state reaction between FeVO₄ and Ag, forming α-AgVO₃ and α-Fe₂O₃ at the interface. Impedance measurements, with a platinum electrode, reaffirmed that FeVO₄ exhibits semiconductor behaviour in air. In a reducing atmosphere, 5% H₂/Ar, high electronic conductivity, from 1 S cm⁻¹ at 300 °C to 2 S cm⁻¹ at 700 °C, was observed with an activation energy of 0.13(1) eV. X-ray diffraction, thermogravimetric analysis and differential scanning calorimetry data determined that the change in electronic conductivity was due to the degradation of the material into FeV₂O₄ and α-Fe₂O₃. It is believed that the conduction was due to electron hopping between vanadium d-orbitals. Neither FeVO₄ nor FeV₂O₄ are deemed suitable as anode materials for solid oxide fuel cells, due to redox instability.     

Template-free mechanochemical route to prepare crystalline and electroactive polydiphenylamine nanostructures

A facile and sustainable mechanochemical route for the synthesis of undoped polydiphenylamine (PDPA) and inorganic acid doped nanostructures are reported. Field emission scanning electron microscopic (FESEM) images highlighted the formation of distinctly different nanostructures for each of the inorganic acid doped PDPA. Elemental analysis carried out for the polymers revealed the presence of more repeating units in their backbone. The X-ray diffraction (XRD) results of the as-prepared PDPA nanostructures indicated the high degree of crystallinity ever reported for PDPA. Spectroscopic profile of the polymers showed that the prepared PDPA is in a doped conducting form. Electrochemical studies performed for the polymeric particles ascertained the redox behaviour and the good electrochemical activity of obtained PDPA samples. The probable mechanistic aspect behind the formation of PDPA nanostructures through this simple and efficient route is discussed.     

Grain boundary microstructure and fatigue crack growth in Allvac 718Plus superalloy

The correlation between grain boundary microstructure and fatigue crack growth with hold-times was investigated for two conditions of the superalloy Allvac 718Plus; a Standard condition with the recommended distribution of grain boundary phases and a Clean condition with virtually no grain boundary phases. Fatigue testing was performed at 704 °C using 10 Hz cyclic load with intermittent hold-times of 100 s at maximum tensile load. Microstructural characterization and fractography were conducted using scanning- and transmission electron microscopy techniques. Auger electron- and X-ray photoelectron spectroscopy techniques were used for oxide analyses on fracture surfaces. It was found that in the Standard condition crack growth is mostly transgranular for 10 Hz loading and intergranular for hold-times, while for the Clean condition crack growth is intergranular in both load modes. The lower hold-time crack growth rates in the Standard condition are attributed to grain boundary δ-phase precipitates. No effect of δ-phase was observed for 10 Hz cyclic loading crack growth rates. Two different types of oxides and oxide colours were found on the fracture surfaces in the Standard condition and could be correlated to the different loading modes. For cyclic loading a bright thin Cr-enriched oxide was dominate and for hold-times a dark and slightly thicker Nb-enriched oxide was dominant These oxide types could be related to the oxidation of δ-phase and the matrix respectively. The influence of δ-phase precipitates on crack propagation is discussed.     

Structure and water-barrier properties of vanadate-based corrosion inhibitor films

Uniform, crack-free vanadium-based corrosion inhibitor films were grown on aluminum alloy 2024. Neutron and X-ray reflectivity were utilized to investigate the structure, water-barrier properties and speciation of the inhibitor film. The top part of the alloy participates in the formation of vanadate film. The similarity of films prepared from H₂O and D₂O implies the vanadate film is not hydrated. The film has a layered structure with vanadium enriched at the alloy interface. The film behaves as an effective water barrier when the thickness is greater than 800 Å. Films grown without K₃Fe[CN]₆ accelerator are found to be extremely thin.     

The corrosion behaviour of WC-VC-Co hardmetals in acidic media

The effect of increasing vanadium carbide (VC) content on the corrosion behaviour of tungsten carbide - 10 wt% cobalt hardmetals was investigated in 1 M hydrochloric (HCl), and sulphuric (H₂SO₄) acids solutions. Increasing VC content makes the open circuit potential (OCP) in the test solutions more negative than the base alloy. Specimens exhibited pseudo passivation in all the test solutions. Increasing VC led to decreasing corrosion current density. However, the corrosion current densities during chronoamperometric tests were lower for 0 wt% VC. XRD and Raman spectroscopy showed that hydrated WO₃ formed in the surface films of all specimens in hydrochloric acid (HCl), while hydrated vanadyl sulphate also formed for higher VC content specimens in sulphuric acid (H₂SO₄).     

绿色路线制备金纳米

从绿色化学的观点出发,选择无毒、无害的水作溶剂,环境友好、无毒的葡萄糖同时作还原剂和稳定剂,在加热条件下还原HAuCl4制备金纳米粒子。实验中通过加入不同量的NaOH和葡萄糖,合成出了不同尺寸、形貌的金纳米粒子。当n(NaOH)∶n(HAuCl4)∶n(葡萄糖)=3∶1∶10时,得到了分散较好的直径10~20 nm、长度可达2μm的多晶结构的金纳米线。根据透射电镜、X-射线衍射的测试结果对纳米线的生长机理进行了分析认为,首先纳米金进行定向排列,然后由于金属键的作用导致金纳米线的生成。     

热疲劳载荷作用下不同成分BGA焊点可靠性

针对微电子组装中常见的BGA封装形式,对比采用3种不同成分的BGA焊球和焊膏组合(锡铅共晶焊球和锡铅共晶焊膏Sn63Pb37、Sn3Ag0.5Cu焊球和锡铅共晶焊膏以及Sn3Ag0.5Cu焊球和Sn3Ag0.5Cu焊膏)焊接得到的BGA焊接界面。经过不同周期的热疲劳试验后,在金相显微镜和电子背散射衍射下观察,发现Sn3Ag0.5Cu焊球和锡铅共晶焊膏混装形成的BGA焊点中黑色的富锡相均匀弥散分布在焊球内,在热循环载荷作用下极难形成再结晶,抗热疲劳性能最好。