TSDC studies of the effects of plasticizer and water on the sub-T g relaxations of an epoxy resin system

The sub-glass-transition-temperature (sub-T _g relaxations of an epoxy resin system based on diglycidyl ether of bisphenol-A (DGEBA) and cured with triethylenetetramine (TETA) were investigated by means of the thermally stimulated depolarization current (TSDC) technique in the temperature range 77 K to 300 K. Three relaxation regions were observed: the γ relaxation at about 150 K, the β relaxation at 160 K to 200 K and the ω relaxation at 240 K to 270 K. The plasticization effect on the aforementioned relaxations of a plasticizer chemically connected to the epoxy resin network was investigated. The amount of plasticizer (commercial name THIOCOL LP3) was varied between 0% and 60% by weight of the epoxy. The broad range of the β relaxation reflects the heterogeneous structure of the material. The activation energies of the γ and β relaxations were calculated using the thermal sampling technique. Physical aging strongly influenced the TSDC thermogram of the ω relaxation, indicating phase separation during the aging procedure. Water effects were systematically investigated from dry samples to water-saturated samples (water content, 2.5%). In all specimens, water induced plasticization, which is expressed by the shifting of the β relaxation toward lower temperatures. The mode of water absorption (immersion in water or exposure to humid environment) also influenced the evolution of the ω relaxation.     

Electrical analysis of inter-growth structured Bi_4Ti_3O_(12)-Na_(0.5)Bi_(4.5)Ti_4O_(15) ceramics

Inter-growth bismuth layer-structured ferroelectrics(BLSFs), Bi_4Ti_3O_(12)-Na_(0.5)Bi_(4.5)Ti_4O_(15)(BIT-NBT), were successfully synthesized using the traditional solid-state reaction method. X-ray diffraction(XRD) Rietveld refinements were conducted using GSAS software. Good agreement and low residual are obtained. The XRD diffraction peaks can be well indexed into I2 cm space group. The inter-growth structure was further observed in the high-resolution TEM image. Dielectric and impedance properties were measured and systematically analyzed. At the temperature range 763-923 K(below T_c), doubly ionized oxygen vacancies(OVs) are localized and the short-range hopping leads to the relaxation processes with an activation energy of 0.79-1.01 eV. Above T_c, the doubly charged OVs are delocalized and become free ones, which contribute to the long-range dc conduction. The reduction in relaxation species gives rise to a higher relaxation activation energy ~ 1.6 eV.     

Monitoring of residual stresses in injection-molded plastics with holographic interferometry

Residual stresses are often trapped in injection-molded plastic parts due to the rapid cooling of the material in this manufacturing process. These stresses are a common source of failure in plastic components in automobiles, appliances and computers and are difficult to measure with conventional residual-stress experimental methods. Real-time holographic interferometry appears to be a viable technique to identify and monitor these stresses in plastic parts. In this investigation, holographic interferometry was used to monitor the relaxation of residual stresses in the plastic-molded actuator arm of a computer hard drive. In the first phase of this study, the relaxation of these residual stresses as a function of temperature was observed. In the second phase, the time to completely relax the residual stresses in the plastic part at an elevated temperature, the annealing temperature, was determined. In the third phase of this investigation, the rate of relaxation of these residual stresses as a function of time at various operating temperatures, was studied. Based on the results of this study, holographic interferometry appears to be a powerful research tool in the study of residual stresses in plastic parts. It also has the potential to be a practical tool for the inspection of manufactured plastic parts for the presence of residual stress.     

Residual stress relaxation in the core of optical fiber by CO(2) laser irradiation

We observed residual stress relaxation by CO(2) laser irradiation in the cores of optical fibers by direct stress measurement. It was demonstrated that the mechanical stress was fully relaxed by CO(2) laser irradiation and that the remaining stress in the core was thermal stress that was due to a mismatch of the thermal expansion coefficients of the fiber core and cladding. The net core stresses after relaxation were 17, 68, and 203 MPa in Ge-B-codoped fibers drawn at 0.53, 1.38, and 3.48 N, respectively. Changes in the refractive indices of the cores as a result of residual stress relaxation were also estimated.     

Relation between residual stresses and microstructure evolution in Al–Si alloys based on different casting parameters

Most designers take into consideration the stresses that act on a material but despite safety considerations, failure may occur due to other factors that were neglected in their design. These factors can be a pre-existing flaw, microstructure deficiency or the presence of residual stresses. Depending on the stress type, residual stresses combined with applied stresses can aid or hinder failures. Consequently, reducing the amount of residual stress can have a promising effect on the life of the component. Different casting parameters can change the microstructure and residual stresses of castings. In this research, the relation between residual stresses and microstructure evolution under the influence of different casting parameters was investigated, using both Al–Si–Mg (Al-356) and Al–Si–Mg–Cu (Al-319) alloys. Solidification rate, quenching rate, aging temperature and aging time were the main parameters considered for this study. The results indicate that the magnitude of the residual stresses increases with increasing solidification rate and quenching rate. Also, the residual stress relieving is proportional to the aging temperature     

Glass transition temperature and thermal stability of ZnS/PMMA nanocomposites

In this article, ZnS nanoparticles were prepared by wet chemical precipitation method using zinc sulphate (ZnSO₄), sodium sulphide (Na₂S) and thio-glycerol. These nanoparticles were characterized through X-ray diffraction (XRD) and transmission electron microscope (TEM) measurements. The solution-based processing was used to prepare Poly methyl methacrylate (PMMA) nanocomposites with different weight percents (0, 2, 4, 6 and 8) of ZnS nanoparticles. The obtained ZnS/PMMA nanocomposites were characterized through XRD, scanning electron microscope and TEM measurements. The dynamic mechanical analyzer was used to obtain the storage modulus and glass transition temperature (T _g) of the nanocomposites. The apparent activation energy of the glass transition region was also determined using the Vogel–Fulcher–Tammann equation. The results indicated that the thermal stability of ZnS/PMMA nanocomposites was higher than PMMA and 6 wt. % of ZnS nanoparticles in PMMA matrix showed the maximum activation energy, which indicated that this nanocomposite had higher thermal stability than other composites.     

Tb~(3+)掺杂含SrF_2纳米晶硅酸盐微晶玻璃的光谱性质

通过高温熔融法和后续热处理制得Tb~(3+)掺杂含SrF_2纳米晶的透明硅酸盐微晶玻璃。利用X射线衍射(XRD)、透射电子显微镜(TEM)、紫外可见透过光谱、荧光光谱、荧光寿命和X射线激发发光光谱(XEL)探讨了基础玻璃和微晶玻璃的结构和光谱特性。XRD结果表明,玻璃中析出晶体为SrF_2纳米晶,衍射峰随着热处理温度的升高和时间的延长而逐渐明显,晶粒也随热处理温度的升高和时间的延长越来越大。在376 nm紫外光和X射线激发下,与基础玻璃相比,微晶玻璃发光显著增强,且发光强度随热处理温度的升高和时间的延长而逐渐增强。     

Effect of Mg substitution on the magnetic properties of NiCuZn ferrite nanoparticles prepared through a novel method using egg white

Nanocrystalline Mg-substituted NiCuZn ferrites were successfully synthesized, for the first time, by using metal nitrates and freshly extracted egg white. The thermal decomposition process of the nitrate-egg white precursors was investigated by thermogravimetric (TG) technique. X-ray diffraction (XRD) revealed that, single-phase cubic ferrites with average particle size of 23.9-35.1 nm were directly formed after ignition at 500 °C. No noticeable variation of lattice parameters with increasing magnesium content was observed, while X-ray densities were found to decrease. This can be explained on the basis of ionic radii and atomic masses of the substituted cation. Transmission electron microscope (TEM) shows that, particles are permanently magnetized and get agglomerated. The saturation magnetization (M_s) and coercivity (H_c) as a function of Mg content were investigated using vibrating sample magnetometer (VSM). It has been found that the M_s increases firstly up to x=0.2 and then decreases, while H_c continuously decreases. Magnetic susceptibility measurements give results which agree well with those obtained by VSM. The obvious decrease in the Curie temperature (T_C) with increasing Mg indicates that the ferrimagnetic grains are widely separated and enclosed by non-magnetic magnesium ions.     

Synthesis and characterization of microwave processed PZT material

With a view to investigate the influence of microwave sintering on the structural and dielectric properties of lead zirconate titanate (PZT), the samples were prepared by citrate gel route. The well crystallized single phase perovskite PZT powders were obtained after calcination at 700 °C for 2 h. The X-ray diffraction (XRD) pattern clearly indicates the formation of PZT material with single phase. FTIR and TG-DTA studies also confirmed the formation of PZT along with the reaction process involved in the synthesis. The crystallite sizes of the samples calcined at different temperatures were calculated using Scherrer’s formula and were compared with those obtained by the transmission electron microscope (TEM) technique. The surface morphological features of all the samples were studied using a scanning electron microscope (SEM) while the chemical composition was obtained by an energy dispersive X-ray spectroscope (EDS). The variation of dielectric constant and loss tangent with temperature and frequency of both the type of samples was also investigated and the observed behavior is explained qualitatively.     

高压下制备的累托石/酚醛树脂复合材料微结构和热性能研究

 采用物理方法在高压下制备了酚醛树脂（PF）/累托石（REC）纳米复合材料,用X射线衍射（XRD）、透射电子显微镜（TEM）及热分析（DSC/TGA）等方法,研究了复合材料的物相、显微结构以及热学性能。结果表明,不通过层间高分子聚合反应,不预先对累托石进行有机化处理,在高压下,由聚合物分子插入粘土层间,可以形成剥离型树脂/粘土纳米复合材料,并且其热学性能发生了较大的改变。     

热蒸发YbF3薄膜的机械特性

 实验研究了热蒸发YbF₃薄膜在大气中的应力和附着力。利用Veeco干涉仪,测试了各种工艺条件下单层YbF₃薄膜的应力。结果发现:YbF₃薄膜的残余应力为张应力,热应力在残余应力中的比重较大;沉积方式对薄膜应力的影响不大;薄膜应力在大气中有一个释放的过程。热处理后,YbF₃薄膜应力增大。     

Laser bending of AISI 304 steel sheets: Thermal stress analysis

Laser induced bending of steel sheet is carried out and thermal stress developed in the heated region is examined. Temperature and stress fields are predicted using the finite element model. The microstructural changes in the melted region are investigated through scanning electron microscope, energy dispersive spectroscopy and X-ray diffraction. The residual stress developed at the surface vicinity of the laser treated region is measured using the X-ray diffraction technique, which is then compared with its counterpart predicted from the simulations. It is found that the residual stress at the surface vicinity is compressive and the prediction of the residual stress agrees well with that obtained from the X-ray diffraction technique. In addition, surface temperature predictions are in good agreement with the thermocouple data. The laser treated region is free from major cracks and large cavities.     

Synthesis of multi-wall carbon nanotubes by simple pyrolysis

A new pyrolysis technique has been developed for the synthesis of multi-walled carbon nanotubes (MWCNTs). In this simple method diethyl ether and nickelocene is pyrolysized in a reaction quartz tube without using carrier gas. The samples are prepared at pyrolysis temperatures of 650 and 950 ^°C and the effect of temperature on the tube morphology investigated. Purification has been done following the standard oxidation and acid bath treatment. The as-synthesized and purified nanotubes have been characterized by X-ray diffraction (XRD), Scanning electron microscope (SEM), transmission electron microscope (TEM), thermogravimetric analysis (TGA) and micro-Raman spectroscopy. The technique has great advantages such as low cost and easy operation for the production of CNTs.     

Characterization of martensite in Fe-25%Ni-15%Co-5%Mo alloy

Kinetic, morphological, crystallographical, magnetic and thermal characteristics of thermally induced martensite in Fe-25%Ni-15%Co-5%Mo alloy have been investigated by scanning electron microscope (SEM), transmission electron microscope (TEM), Mössbauer spectrometer, and differential scanning calorimeter (DSC). Kinetics of the transformation was found to be athermal. Also only lenticular martensite morphology was observed during microscope observations. In addition, martensite start temperature (M_s) was determined as −63 °C from differential scanning calorimeter. On the other hand, Mössbauer spectra revealed a paramagnetic character for the austenite phase and a ferromagnetic character for thermally induced martensite phase.     

Effect of Young's modulus evolution on residual stress measurement of thermal barrier coatings by X-ray diffraction

Subjected to thermal cycling, the apparent Young's modulus of air plasma-sprayed (APS) 8 wt.% Y₂O₃-stabilized ZrO₂ (8YSZ) thermal barrier coatings (TBCs) was measured by nanoindentation. Owing to the effects of sintering and porous microstructure, the apparent Young's modulus follows a Weibull distribution and changes from 50 to 93 GPa with an increase of thermal cycling. The evolution of residual stresses in the top coating of an 8YSZ TBC system was determined by X-ray diffraction (XRD). The residual stresses derived from the XRD data are well consistent with that obtained by the Vickers indention. It is shown that the evolution of Young's modulus plays an important role in improving the measurement precision of residual stresses in TBCs by XRD.     

Magnetic Properties of Iron-Based Amorphous Metal Wires

It has been studied how the conditions of machining and the elastic tensile stresses affect the magnetic properties of amorphous metal wires of composition Fe₇₅Si₁₀B₁₅ produced by drawing from a melt. The magnetic characteristics of wires subjected to both thermal treatment and treatment with a continuous electric current of different magnitude have been investigated. The residual induction of wires is their magnetic parameter most sensitive to the conditions of treatment. The dependences of the residual induction on temperature and on the magnitude of the treating electric current are qualitatively similar. The greatest changes in residual induction are observed in the range of treating electric currents from 0.5 to 0.8 A, which can be associated with the processes of structural relaxation and crystallization occurring in the wires. The run of the dependence of the residual induction on the magnitude of tensile stresses is nonmonotonic in character and is determined by the level of internal hardening stresses of the test wires.     

Grain boundary segregation and relaxation in nano-grained polycrystalline alloys

The present study carries out systematic thermodynamics analysis of Grain Boundary(GB)segregation and relaxation in NanoGrained(NG)polycrystalline alloys.GB segregation and relaxation is an internal process towards thermodynamic equilibrium,which occurs naturally in NG alloys without any applied loads,causes deformation and generates internal stresses.The analysis comprehensively investigates the multiple coupling effects among chemical concentrations and mechanical stresses in GBs and grains.A hybrid approach of eigenstress and eigenstrain is developed herein to solve the multiple coupling problem.The analysis results indicate that the GB stress and grain stress induced by GB segregation and relaxation can be extremely high in NG alloys,reaching the GPa level,which play an important role in the thermal stability of NG alloys,especially via the coupling terms between stress and concentration.The present theoretic analysis proposes a novel criterion of thermal stability for NG alloys,which is determined by the difference in molar free energy between a NG alloy and its reference single crystal with the same nominal chemical composition.If the difference at a temperature is negative or zero,the NG alloy is thermal stable at that temperature,otherwise unstable.     

Stress relaxation through ageing heat treatment – a comparison between in situ and ex situ neutron diffraction techniques

The effect of ageing heat treatment on the relaxation of residual stress in a water quenched polycrystalline nickel-base superalloy has been measured using neutron diffraction. Two separate experiments have been conducted; the first experiment was an ex situ study in which samples were individually processed with varying degrees of age time before measurement. The second experiment was an in situ heat treatment, which required heating and then holding the sample at ageing temperature while measuring strain using neutron diffraction. The in situ experiment was carried out twice using the same setup to assess the repeatability of the technique and found to be repeatable within experimental error. The agreement between in situ and ex situ experiments was found to be reasonable, particularly the manner in which the stresses relaxed with time. In both studies it was found that initial stress relaxation was rapid, approximately 200 MPa in 15–30 min, after this a slower linear relaxation remained for the rest of the ageing heat treatment. This behaviour suggests creep may be the means by which stress relaxation takes place in this material during ageing.     

Temperature dependence of proton relaxation times in vitro

Accurate measurement of tissue relaxation characteristics is dependent on many factors, including field strength and temperature. The purpose of this study was to evaluate the relationship between sample temperature, viscosity and proton spin-lattice relaxation time (T1) and spin-spin relaxation time (T2). A review of two basic models of relaxation the simple molecular motion model and the fast exchange two state model is given with reference to their thermal dependencies. The temperature dependence for both T1 and T2 was studied on a 0.15 Tesla whole body magnetic resonance imager. Thirteen samples comprising both simple and complex materials were investigated by using a standard spin-echo (SE) technique and a modified Carr-Purcell-Meiboom-Gill (CPMG) multi-echo sequence. A simple linear relationship between T1 and temperature was observed for all samples over the range of 20 degrees C to 50 degrees C. There is an inverse relationship between viscosity and T1 and T2. A quantity called the temperature dependence coefficient (TDC) is introduced and defined as the percent rate of change of the proton relaxation time referenced to a specific temperature. The large TDC found for T1 values, e.g. 2.37%/degrees C for CuSO4 solutions and 3.59%/degrees C for light vegetable oils at 22 degrees C, indicates that a temperature correction should be made when comparing in-vivo and in-vitro T1 times. The T2 temperature dependence is relatively small.     

Effects on the evolution of microstructure and properties of low-silicon cast aluminum alloys in service

ABSTRACT

The microstructure evolution and property change of four kinds of low silicon cast aluminum alloy exposed to heat for 0–50?h at 200°C were studied by means of Brinell hardness test, tensile property test, friction and wear property test and XRD analysis. The results show that with increasing thermal exposure time, the tensile strength of each group of samples decreased and the amount of wear increased. The tensile strength of samples with more Si content decreased slowly. When the time increased to 50?h, the increase of wear loss was the largest. The hardness of samples after thermal exposure increases compared with that before thermal exposure. The residual stress of (311) diffraction crystal surface of AlSi3.5Mg0.66 under different thermal exposure time was measured. The type of residual stress changed from residual tensile stress to residual compressive stress after thermal exposure. There is an abnormal phenomenon that the hardness of the sample increased and the amount of wear increased, and it is evident that the distribution of residual stress was inhomogeneous after thermal exposure. It is found that with increasing thermal exposure time to 50?h, the average lattice distortion ε of the low-index crystal plane and the high-index crystal plane in the aluminum alloys gradually increased.