热室内样品制备技术研究

核电站能否安全高效运行取决于材料的可靠性。辐照后检验工作主要用于研究反应堆材料辐照性能。由于反应堆材料的高放射性,这类检验工作往往在热室内开展,检验人员远程操作存在着很多困难,尤其在燃料棒破坏性检验阶段,涉及燃料棒的的切割、微观分析样品和力学性能测试等一系列样品的制备工作。该文介绍了热室辐照后检验涉及了样品类型以及样品制备的主要困难,开展了热室内燃料芯块样品和包壳样品制备技术的研究,重点研究了热室内燃料芯块金相样品的制备和包壳透射电镜(TEM)样品的制备技术,以掌握热室内样品制备工艺和流程,建立热室内样品制备技术。

锆钛酸铅陶瓷在力电耦合场下疲劳性能的评价

小样品力学性能试验方法(Modified Small Punch Tests,简称MSP)是评价陶瓷材料力学性能的一种有效方法.采用改进型多场耦合小冲压(MSP)试验法评价了Pb(Zr,Ti)O3陶瓷(PZT)在力电耦合和纯力场下的疲劳性能.通过对比在纯力场和力电耦合下的力学性能可以看出:与纯力场下相比,PZT陶瓷在力电耦合下的断裂强度会降低.在力场和电场的同时作用下,疲劳寿命显著缩短,压电陶瓷材料内部易出现沿晶断裂.

FIB-SEM双束技术简介及其部分应用介绍

聚焦离子束(FIB)与扫描电子显微镜(SEM)耦合成为FIB-SEM双束系统后,通过结合相应的气体沉积装置,纳米操纵仪,各种探测器及可控的样品台等附件成为一个集微区成像、加工、分析、操纵于一体的分析仪器。其应用范围也已经从半导体行业拓展至材料科学、生命科学和地质学等众多领域。本文介绍了双束系统中的一些关键概念及基本原理并综述了其在材料科学领域的一些典型应用,包括透射电镜(TEM)样品制备,微纳尺度力学测试样品制备以及材料三维成像及分析。

MSP试验法评价PZT陶瓷的循环疲劳寿命

采用小样品力学性能试验方法(Modified Small Punch Tests,简称MSP)对Pb(Zr,Ti)O3陶瓷(PZT)实施了不同大小应力下的循环疲劳实验,循环应力越大,样品的残余强度和压电常数衰减越快,这是由应力循环过程中大量微裂纹的产生和扩展所致.通过最大强度值与疲劳寿命的对应关系求得100 Hz循环疲劳下该样品的裂纹扩展指数n为395,由此推测了PZT陶瓷样品的使用寿命,在循环应力的最大值不超过79.1 MPa的条件下,该样品的连续使用寿命可达5年以上.

Experimental investigation on the relevance of mechanical properties and porosity of sandstone after hydrochemical erosion

Under the effect of chemical etching,the macroscopic mechanical properties,mesoscopic structure,mineral content,and porosity of rocks undergo significant changes,which can lead to the geological disasters; thus,an understanding of changes in the microscopic and macroscopic structure of rocks after chemical etching is crucial.In this study,uniaxial mechanical tests and nuclear magnetic resonance(NMR) spectroscopy were carried out on sandstone samples that had been previously subjected to chemical erosion under different p H values.The aim was to study changes in properties and mechanical characteristics,including deformation and strength characteristics,of the rock,and microscopic pore variation characteristics,and to perform preliminary studies of the chemical corrosion mechanism.Results show that different chemical solutions have a significant influence on the uniaxial compressive strength,the axial strain corresponding to the peak axial stress,elastic modulus,etc.With the passage of time,porosity increases gradually with exposure to different chemical solutions,and exposure to chemical solutions results in large changes in the NMR T2 curve and T2 spectrum area.Sandstone exposed to different chemical solutions exhibits different corrosion mechanisms; the root cause is the change of mineral.

Mechanical behavior and failure analysis of brittle sandstone specimens containing combined flaws under uniaxial compression

Based on the axial stress-axial strain curves,the effect of fissure angle on the strength and deformation behavior of sandstone specimens containing combined flaws is analyzed.The mechanical parameters of sandstone specimens containing combined flaws are all lower than that of intact specimen,but the reduction extent is distinctly related to the fissure angle.The results of sandstone specimens containing combined flaws are obtained by the acoustic emission,which can be used to monitor the crack initiation and propagation.The ultimate failure mode and crack coalescence behavior are evaluated for brittle sandstone specimens containing combined flaws.Nine different crack types are identified on the basis of their geometry and crack coalescence mechanism(tensile crack,hole collapse,far-field crack and surface spalling)for combined flaws.The photographic monitoring was also adopted for uniaxial compression test in order to confirm the sequence of crack coalescence in brittle sandstone specimens containing combined flaws,which recorded the real-time crack coalescence process during entire deformation.According to the monitored results,the effect of crack coalescence process on the strength and deformation behavior is investigated based on a detailed analysis for brittle sandstone specimens containing combined flaws by using digital photogrammetry.

Al_2O_3对R_2O-CaO-SiO_2-F系废渣微晶玻璃析晶与性能的影响

以花岗岩废渣为主要原料,用熔融法制备了R_2O-CaO-SiO_2-F系微晶玻璃。采用差示扫描量热法、X射线衍射、扫描电子显微镜等测试方法研究了Al_2O_3含量对RO-CaO-SiO_2-F系微晶玻璃的析晶与性能的影响。结果表明:随着Al_2O_3含量的增加,硅碱钙石与硬硅钙石晶体细化;Al_2O_3含量(质量分数)为6.0%的基础玻璃经560℃核化2 h、910℃晶化2 h后的主晶相为硅碱钙石,其抗弯强度和断裂韧性分别为(154±20)MPa、(2.37±0.12)MPa·m^(-1/2);当Al_2O_3含量增加至6.5%时,硅碱钙石减少、氟化钙增多,力学性能降低。

Determination of Trace Vanadium (Ⅴ) in Seawater and Fresh Water by the Catalytic Kinetic Spectrophotometric Method

A new kinetic spectrophotometric method has been developed for the determination of vanadium（V）.The method is based on the catalytic effect of vanadium（V）on the oxidation of weak acid brilliant blue dye（RAWL）by KBrO3 using the citric acid as activation reagent.The obtained optimum conditions are：c（RAWL）= 1×10-4 molL-1,c（KBrO3）= 3×10-2 molL-1,c（citric acid）=9×10-3 molL-1,pH = 2.50,the reaction time being 7.0min and the temperature being 25.0℃.Under the optimum conditions,the proposed method allows the determination of vanadium（V）in the range of 0-70.0ng mL-1 and the detection limit is down to 0.407 ng mL-1.For standard vanadium（V）solution determination,the recovery efficiency is in the range of 98.5%-102% and the RSD ranges from 0.76%-1.25%.Moreover,it is demonstrated that most cations and anions do not interfere with the determination of vanadium（V）under the analytical condition.The new method was successfully applied in the determination of vanadium（V）in fresh water and seawater samples with satisfactory results.Vanadium（V）in the seawater samples from Qingdao offshore was determined using the method and the distribution of vanadium（V）was mapped.Compared with other instrumental analytical methods,the proposed method shows good selectivity,sensitivity,simplicity,lower cost and rapidity.It can be employed on shipboard easily.

Nonlinear characteristics of induced spontaneous combustion process of sulfide ores

To investigate the relationship between nonlinear parameters and spontaneous combustion tendency of sulfide ores, nine different sulfide ore samples were taken from a pyrite mine in China, and induced spontaneous combustion experiment was carried out in the laboratory. Different stages of the induced spontaneous combustion process were studied by integrating wavelet technology and nonlinear dynamics theory. The results show that ignition points of all the ore samples are above 330 ℃, indicating that sulfide ores of the pyrite mine are difficult to combust spontaneously under normal mining conditions. Spontaneous combustion process includes three stages： incubation stage, development stage and approaching stage. The average temperature rising rate of the three stages are 1.0 ~C/min, 2.0 ~C/min and 4.2 ~C/min, respectively. During the spontaneous combustion process, mean values of approximate entropy and correlation dimension increase at first, and then decrease in the following stage. The mean value of the maximum Lyapunov exponent increases with the passage of reaction time. In a whole, correlation among the three nonlinear parameters firstly weakens, then enhances, and the best correlation period is at approaching stage. As ignition point increases, the maximum Lyapunov exponent of approaching stage decreases. Therefore, combustible tendency of sulfide ores could be qualitatively evaluated based on the maximum Lyapunov exponent of this stage.

Investigations on the Thermodynamic Stability and Availability of Nutrients for Plants by Humic Substances Extracted from Peat Samples

This work evaluated the complexation capacity, exchange constants and availability of micronutrients for plants and humic substances extracted from peat samples. Samples of humic substances extracted from two tropical peats （HS-P1 and HS-P2） were enriched with the micronutrients Cu（II）, Co（II）, Fe（II）, Mn（II）, Ni（II） and Zn（II） and the parameters for formation of the complexes （HS-N） were evaluated at different pH. The Scatchard model was used to calculate the maximum complexation capacity and the nutrient availability was studied using exchange capacity experiments based on ultrafiltration procedure. The optimum pH for complexation was 4.5 and the order of affinity was： Fe（II） 〉 Cu（II） 〉 Co（II） 〉 Mn（II） = Ni（II） 〉 Zn（II）. The maximum complexation capacity reached 56.8 mg·g-1 Fe of HS-P1 （the highest） and 1.7 mg.g1 Zn of HS-P2 （the slightest）. The exchange experiments showed that HS-P-Fe complexes were formed preferentially. The least stable complex was formed with Zn, which was therefore, more easily available. The results contribute to understand the behavior and availability of some nutrients in soils.

The Kinetic Study of Adsorption of Copper Metal Ion in Selected Contaminated Red Soil Samples in Palestine

Heavy metals are persistent pollutants in the environment. Problems associated with the cleanup of sites contaminated by metals have demonstrated the need to develop remediation technologies that are feasible, quick, and effective in a wide range of physical settings. In this study we have investigated the adsorption of Cu（lI）, onto red soil in single and multi-element systems as a function of soil and heavy metal concentrations. Before contamination, soils were characterized to determine particle size, pH, organic matter content and heavy metal contents. The results of experimental sorption data fitted very well the Freundlich isotherm model with n = 1.4 and k = 1.25 and first order kinetics model. The best pH for adsorption of Cu^2＋ on red soil was found to be 4.0. Adsorption of metals on soil increased in the order Cu 〉 Pb 〉 Zn ≈ Cd. This trend might be related to the increase in the electronegativity of the metal ion.