Direct visualization of the nanoscopic three‐phase structure and stiffness of NBR/PVC blends by AFM nanomechanical mapping

The PeakForce Quantitative Nanomechanical Mapping based on atomic force microscope (AFM) is employed to first visualize and then quantify the elastic properties of a model nitrile rubber/poly(vinyl chloride) (NBR/PVC) blend at the nanoscale. This method allows us to consistently observe the changes in mechanical properties of each phase in polymer blends. Beyond measuring and discriminating elastic modulus and adhesion forces of each phase, we tune the AFM tips and the peak force parameters in order to reliably image samples. In view of viscoelastic difference in each phase, a three‐phase coexistence of an unmixed NBR phase, the mixed phase, and PVC microcrystallites is directly visualized in NBR/PVC blends. The nanomechanical investigation is also capable of recognizing the crosslinked rubber phase in cured rubber. The contribution of the mixed phase was quantified and it was found that the mechanical properties of blends are mainly determined by the homogeneity and stiffness of the mixed phase. This study furthers our understanding the structure–mechanical property relationship of thermoplastic elastomers, which is important for their potential design and applications. © 2019 Wiley Periodicals, Inc. J. Polym. Sci., Part B: Polym. Phys. 2019 , 57, 662–669     

Microstructural stability and age-hardening behavior of Re-added dual two-phase Ni3Al and Ni3V intermetallic alloys

The effect of Re addition on the microstructure and hardening behaviour of the dual two-phase Ni₃Al (L1₂) and Ni₃V (D0₂₂) intermetallic alloy was investigated by scanning electron microscopy, transmission electron microscopy and Vickers hardness test. The two-phase eutectoid microstructure accompanying the Re-rich precipitates were observed in the channel region of the alloys in which Re substituted for Ni but not in those in which Re substituted for Al and V. The concomitant addition of Nb (or Ta) with Re more stabilized the two-phase eutectoid microstructure and consequently more induced the fine precipitates in the channel region. The annealing at temperatures below the eutectoid temperature was necessary to induce the fine precipitates in the channel region and thereby result in the precipitation hardening. The fine precipitation in the channel region and related hardening was attributed to the alloying feature so that Re is soluble in the A1 (fcc) phase at high temperatures and becomes less soluble in the two intermetallic phases decomposed from the A1 phase at low temperatures.     

铝互连线的电迁移问题及超深亚微米技术下的挑战

铝互连线的电迁移问题历来是微电子产业的研究热点，其面临的电迁移可靠性挑战也是芯片制造业最持久和最重要的挑战之一.从20世纪90年代开始，超深亚微米(特征尺寸≤0.18 μm)铝互连技术面临了更加复杂的电迁移可靠性问题.从电迁移理论出发，分析概括了铝互连电迁移问题的研究方法，总结了上世纪至今关于铝互连电迁移问题的主要经验；最后结合已知的结论和目前芯片制造业现状，分析了当前超深亚微米铝互连线电迁移可靠性挑战的原因和表现形式，提出了解决这些问题的总方向. 关键词： 电迁移 铝互连 微结构     

Diffusion Structural Analysis Study of Titania Films Deposited by Sol-Gel Technique on Silica Glass

The diffusion structural analysis (DSA) was used to characterize microstructure changes of hydrous titania gel films under in situ conditions of heating. TG and DTA were used in order to elucidate the processes controlling the formation of anatase film during heating of hydrous titania gel film. The annealing of porosity and near surface structure defects of the dehydrated titania films was indicated by DSA in the temperature range 255–700°C as the decrease of radon release rate. It was demonstrated that the annealing was enhanced on heating in oxygen in comparison with heating in argon. The DSA experimental results were compared with model curves describing the radon diffusion mobility and the annealing of radon diffusion paths.     

Polymerization of 1,3‐dienes with functional groups. III. Free‐radical polymerization of N,N‐diethyl‐2‐methylene‐3‐butenamide

Free‐radical homo‐ and copolymerization behavior of N,N‐diethyl‐2‐methylene‐3‐butenamide (DEA) was investigated. When the monomer was heated in bulk at 60 °C for 25 h without initiator, rubbery, solid gel was formed by the thermal polymerization. No such reaction was observed when the polymerization was carried out in 2 mol/L of benzene solution with with 1 mol % of azobisisobutyronitrile (AIBN) as an initiator. The polymerization rate (R_p) equation was R_p ∝ [DEA]^1.1[AIBN]^0.51, and the overall activation energy of polymerization was calculated 84.1 kJ/mol. The microstructure of the resulting polymer was exclusively a 1,4‐structure where both 1,4‐E and 1,4‐Z structures were included. From the product analysis of the telomerization with tert‐butylmercaptan as a telogen, the modes of monomer addition were estimated to be both 1,4‐ and 4,1‐addition. The copolymerizations of this monomer with styrene and/or chloroprene as comonomers were also carried out in benzene solution at 60 °C. In the copolymerization with styrene, the monomer reactivity ratios obtained were r₁ = 5.83 and r₂ = 0.05, and the Q and e values were Q = 8.4 and e = 0.33, respectively. © 2004 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 42: 999–1007, 2004     

Radiolytic unsaturation decay in polyethylene. Part III—the effect of certain chain transfer agents

Small amounts of certain halogenated compounds are found to have, at most, only a slight enhancing effect on the radiolytic decay rates of added poly-unsaturated compounds in polyethylene, but significantly increase the elastic modulus at 433 K (melt modulus) obtained thereby. Experiments with model chlorine-containing additives suggest that this increase is due to a more random distribution of polymer and monomer mediated crosslinks in the polymer, that it does not result from a significant increase in crosslinking and that it is mediated by chlorine atoms, in a similar manner to radiolytic hydrogen atoms, through facilitation of long range free radical migration. Although low molecular weight chloro-paraffins inhibit radiolytically induced growth of melt modulus in monomer containing polyethylenes, even very small additions of chlorinated polyethylenes, which form a separate phase, increase the melt modulus. This again indicates that the active species is the chlorine radical.     

晶体微观结构的数值计算

晶体微观结构是晶体材料在特定物理条件下其多个能量极小平衔态在空间形成的某种微尺度的规则分布．几何非线性的连续介质力学理论可以用能量极小化原理来解释晶体微观结构的形成，并用Young测度来刻画平衡态各变体在空间的概率分布．定性的理解与定量地分析和计算晶体材料的微观结构对于发展和改进高级晶体功能材料，如形状记忆合金、铁电体、磁至伸缩材料等，有重要的意义．本文回顾了近年来晶体微观结构数值计算方面的最新进展．介绍了计算晶体微观结构的几种数值方法及有关的数值分析结果。     

The role of alkali content in the devitrification mechanisms of SiO2–Fe2O3–Na2O–PbO SYSTEM

Three batch compositions of pure oxides (SiO₂, Fe₂O₃, PbO, Na₂O) with equivalent SiO₂, Fe₂O₃ and PbO contents and a gradually increased Na₂O content were vitrified through heating in a high temperature electric furnace and subsequent quenching. The resulting vitreous products were thermally treated in order to study the devitrification behaviour, under conditions designated from differential thermal analysis experiments. Depending on the Na₂O content, crystal phase separation gave rise to the growth of acmite and hematite or maghemite. A uniformly phase separated glass-ceramic material, with crystallites of similar size and population density, was produced from devitrification of the vitreous product with the higher Na₂O content.     

Convergence rates for Markov chain order estimates using EDC criterion

The Efficient Determination Criterion (EDC) generalizes the AIC and BIC criteria and provides a class of consistent estimators for the order of a Markov chain with finite state space. In this note, we derive rates of convergence for the EDC estimates. *Partially supported by CNPq, CAPES/PROCAD, FAPDF/PRONEX, FINATEC and FUNPE/UnB. **Partially supported by CAPES.     

轻型汽车后桥半轴断裂件的组织及断口特征

采用光学显微镜和扫描电子显微镜等手段，对某轻型汽车40Cr后桥半轴断裂件的组织及断口特征进行了分析结果表明：半轴在调质处理时的淬火温度不够高，使其表层和心部组织中存在较多的铁素体相，造成了工件最终的硬度和疲劳强度不足，导致半轴在使用中发生扭转疲劳断裂．