In-situ TEM observation of the evolution of helium bubbles in Mo during He^(+)irradiation and post-irradiation annealing

The evolution of helium bubbles in purity Mo was investigated by in-situ transmission electron microscopy(TEM)during 30 keV He^(+)irradiation(at 673 K and 1173 K)and post-irradiation annealing(after 30 keV He^(+)irradiation with the fluence of 5.74×10^(16)He^(+)/cm^(2)at 673 K).Both He^(+)irradiation and subsequently annealing induced the initiation,aggregation,and growth of helium bubbles.Temperature had a significant effect on the initiation and evolution of helium bubbles.The higher the irradiation temperature was,the larger the bubble size at the same irradiation fluence would be.At 1173 K irradiation,helium bubbles nucleated and grew preferentially at grain boundaries and showed super large size,which would induce the formation of microcracks.At the same time,the geometry of helium bubbles changed from sphericity to polyhedron.The polyhedral bubbles preferred to grow in the shape bounded by{100}planes.After statistical analysis of the characteristic parameters of helium bubbles,the functions between the average size,number density of helium bubbles,swelling rate and irradiation damage were obtained.Meanwhile,an empirical formula for calculating the size of helium bubbles during the annealing was also provided.

Hollow glass microspheres/silicone rubber composite materials toward materials for high performance deep in-situ temperaturepreserved coring

Deep petroleum resources are stored under high temperature and pressure conditions,with the temperature having a significant influence on the properties of rocks.Deep in-situ temperature-preserved coring(ITP-coring)devices were developed to assess deep petroleum reserves accurately.Herein,hollow glass microspheres(HGMs)/silicone rubber(SR)composites that exhibit excellent thermal insulation properties were prepared as thermal insulation materials for deep ITP-coring devices.The mechanism and process of heat transfer in the composites were explored,as well as their other properties.The results show that the HGMs exhibit good compatibility with the SR matrix.When the volume fraction of the HGMs is increased to 50%,the density of the HGMs/SR composites is reduced from 0.97 to 0.56 g/cm^(3).The HGMs filler introduces large voids into the composites,reducing their thermal conductivity to 0.11 W/m·K.The addition of HGMs into the composites further enhances the thermal stability of the SR,wherein the higher the HGMs filler content,the better the thermal stability of the composites.HGMs significantly enhance the mechanical strength of the SR.HGMs increase the compressive strength of the composites by 828%and the tensile strength by 164%.Overall,HGMs improve the thermal insulation,pressure resistance,and thermal stability of HGMs/SR composites.

Research on properties of hollow glass microspheres/epoxy resin composites applied in deep rock in-situ temperature-preserved coring

Deep petroleum resources are in a high-temperature environment.However,the traditional deep rock coring method has no temperature preserved measures and ignores the effect of temperature on rock porosity and permeability,which will lead to the distortion of the petroleum resources reserves assessment.Therefore,the hollow glass microspheres/epoxy resin(HGM/EP)composites were innovatively proposed as temperature preserved materials for in-situ temperature-preserved coring(ITP-Coring),and the physical,mechanical,and temperature preserved properties were evaluated.The results indicated that:As the HGM content increased,the density and mechanical properties of the composites gradually decreased,while the water absorption was deficient without hydrostatic pressure.For composites with 50 vol%HGM,when the hydrostatic pressure reached 60 MPa,the water absorption was above 30.19%,and the physical and mechanical properties of composites were weakened.When the hydrostatic pressure was lower than 40 MPa,the mechanical properties and thermal conductivity of composites were almost unchanged.Therefore,the composites with 50 vol%HGM can be used for ITPCoring operations in deep environments with the highest hydrostatic pressure of 40 MPa.Finally,to further understand the temperature preserved performance of composites in practical applications,the temperature preserved properties were measured.An unsteady-state heat transfer model was established based on the test results,then the theoretical change of the core temperature during the coring process was obtained.The above tests results can provide a research basis for deep rock in-situ temperature preserved corer and support accurate assessment of deep petroleum reserves.

IN-SITU TEM OBSERVATION OF NANOSILICON FIBRE GROWTH

Nano silicon particles can be become nano fibre under low energy electron beam bombarding. The formation of the nano silicon fibre include two stages. At first, on the nano silicon particle surface many silicon atoms are gasified, then these silicon atoms deposit in the place where have more charge on account of the static electrical absorption and the point effect of the charge accumulation , these atoms grow into non crystalline silicon fibres. The second stage is the non crystalline silicon fibres crystallizing. Its crystallizing temperature is about 180℃. The growth mechanism of the nano silicon fibre is vapour solid mode.

Homogenization of twin-roll cast AA8079 aluminum alloy studied by in-situ TEM

AA8079 is a commonly used stock material for manufacturing thin packaging foils.The primary alloying elements Fe and Si can form binary and tertiary intermetallics.In-situ TEM simulating homogenization annealing process of the as-cast material was used to analyze the real-time changes of the shape,type,and distribution of these particles.They affect the mechanical properties of the final product and susceptibility of the material to the formation of pinholes and other macroscopic defects.Another set of as-cast samples were annealed in a regime simulating industrial treatment in combination with measurements of resistivity to validate the results of the in-situ experiment.The results show clear temperature intervals of recovery,matrix desaturation,and phase transformations occurring in several stages:spheroidization of the original particles above 450℃,nucleation of new particles at 475℃,particles coarsening above 525℃,and an entire dissolution of the original particles above 550℃.

Interaction of crack with twins in hot-rolling AZ31 magnesium alloys during in-situ TEM straining experiments

In-situ straining experiments in transmission electron microscopy were performed to investigate the propagation of crack,twinning and interaction of crack with twins. Lots of micro-twins were observed in the deformation band near the tip of crack. The stress is relaxed by the formation of micro-twins and the densely developed micro-twins prevent the growth of crack from the deformation band,subsequently the cracks extend into adjacent grains across grain boundaries,and grow along cleavage plane. Multiple twins are observed in hot-rolling AZ31 magnesium alloys,when cracks propagate into twins through twin grain boundaries(GBs),the direction of growth deviates. It is concluded that twins,especially multiple twins effectively baffle the development of crack.

An in-situ study of static recrystallization in Mg using high temperature EBSD

It has been a common method to improve the mechanical properties of metals by manipulating their microstructures via static recrystallization,i.e.,through heat treatment.Therefore,the knowledge of recrystallization and grain growth is critical to the success of the technique.In the present work,by using in-situ high temperature EBSD,the mechanisms that control recrystallization and grain growth of an extruded pure Mg were studied.The experimental results revealed that the grains of priority for dynamic recrystallization exhibit fading competitiveness under static recrystallization.It is also found that grain boundary movement or grain growth is likely to show an inverse energy gradient effect,i.e.,low energy grains tend to swallow or grow into high energy grains,and grain boundaries of close to 30°exhibit superior growth advantage to others.Another finding is that{10-12}tensile twin boundaries are sites of hardly observed for recrystallization,and are finally swallowed by adjacent recrystallized grains.The above findings may give comprehensive insights of static recrystallization and grain growth of Mg,and may guide the design of advanced materials processing in microstructural engineering.

A review of in-situ high-temperature characterizations for understanding the processes in metallurgical engineering

For the rational manipulation of the production quality of high-temperature metallurgical engineering,there are many challenges in understanding the processes involved because of the black box chemical/electrochemical reactors.To overcome this issue,various in-situ characterization methods have been recently developed to analyze the interactions between the composition,microstructure,and solid-liquid interface of high-temperature electrochemical electrodes and molten salts.In this review,recent progress of in-situ hightemperature characterization techniques is discussed to summarize the advances in understanding the processes in metallurgical engineering.In-situ high-temperature technologies and analytical methods mainly include synchrotron X-ray diffraction(s-XRD),laser scanning confocal microscopy,and X-ray computed microtomography(X-rayμ-CT),which are important platforms for analyzing the structure and morphology of the electrodes to reveal the complexity and variability of their interfaces.In addition,laser-induced breakdown spectroscopy,high-temperature Raman spectroscopy,and ultraviolet-visible absorption spectroscopy provide microscale characterizations of the composition and structure of molten salts.More importantly,the combination of X-rayμ-CT and s-XRD techniques enables the investigation of the chemical reaction mechanisms at the two-phase interface.Therefore,these in-situ methods are essential for analyzing the chemical/electrochemical kinetics of high-temperature reaction processes and establishing the theoretical principles for the efficient and stable operation of chemical/electrochemical metallurgical processes.

Oxidation of emerging organic contaminants by in-situ H_(2)O_(2) fenton system

The existence and risk of emerging organic contaminants(EOCs)have been under consideration and paid much effort to degrade these pollutants.Fenton system is one of the most widely used technologies to solve this problem.The original Fenton system relies on the hydroxyl radicals produced by Fe(Ⅱ)/H_(2)O_(2) to oxidize the organic contaminants.However,the application of the Fenton system is limited by its low iron cycling efficiency and the high risks of hydrogen peroxide transportation and storage.The introduction of external energy(including light and electricity etc.)can effectively promote the Fe(Ⅲ)/Fe(Ⅱ)cycle and the reduction of oxygen to produce hydrogen peroxide in situ.This review introduces three in-situ Fenton systems,which are electro-Fenton,Photo-Fenton,and chemical reaction.The mechanism,influencing factors,and catalysts of these three in-situ Fenton systems in degrading EOCs are discussed systematically.This review strengthens the understanding of Fenton and in-situ Fenton systems in degradation,offering further insight into the real application of the in-situ Fenton system in the removal of EOCs.

Effect of dose rate on the characteristics of dislocation loops in palladium:In-situ TEM analysis during 30 keV H_(2)^(+)irradiation

Ion irradiation is usually used to simulate neutron irradiation to accelerate the evaluation of the irradia-tion behavior of reactor materials.However,the validity of using a high damage rate of ion irradiation to simulate a low damage rate of neutron irradiation has always been a controversial topic.Here,the effect of two dose rates(2.94×10^(-6) and 7.35×10^(-5) dpa s^(-1))on the characteristics and evolution of dislo-cation loops in palladium was studied in situ during 30 keV H2+irradiation using transmission electron microscopy.The dose rate obviously affected the nucleation rate and growth rate of dislocation loops,the types(Frank loops or perfect loops)of dislocation loops,and the irradiation hardening and total damage obtained from the product of average loop size and loop density.At the same irradiation dose,a high dose rate would lead to high loop density,small average loop size,low loop growth rate,and low irra-diation hardening and damage induced by loops in pure Pd.Meanwhile,it was found for the first time that a high dose rate was beneficial to the generation of perfect dislocation loops.The effect of dose rate was attributed to the different dynamic equilibrium results between the effective generation rate of point defects and their absorption rate by existing sinks.The present results show that the effect of dose rate should be considered when using ion irradiation to simulate neutron irradiation to evaluate the irradiation damage to materials.

In-situ TEM investigation on the evolution of He bubbles and dislocation loops in Ni-based alloy irradiated by H_(2)^(+)&He^(+)dual-beam ions

The synergistic evolution mechanisms of He bubbles and dislocation loops under 30 keV H_(2)^(+)&He^(+)dual-beam ions irradiation at 650℃ in the Ni-based alloy GH3535,which is the most promising candidate structure material for molten salt reactors(MSRs),were revealed via in-situ TEM.The nucleation,merg-ing,and change in the size of the dislocation loops and He bubbles were characterized in detail to study the influences of irradiation fluence and pre-existing dislocation loops on their evolutions.The number density of both the He bubbles and dislocation loops increases rapidly and subsequently saturates,whereas their size continuously increases with the increasing ion fluence.Pre-existing dislocation loops with strong absorption characteristics grow preferentially and suppress the nucleation of dislocation loops during the dual-beam ions irradiation.Moreover,the bubbles tend to nucleate within the dislocation loops to form bubble-loop complexes,and then decrease in their number density.The details of the un-faulting processes of the Frank loops were discussed,where the energy difference between the two types of loops as well as the evolution of the inside Shockley dislocation loops dominates the unfaulting be-havior.The several evolution stages of the loop-punching mechanism are revealed,and the emitted loops can directly form perfect loops as well as unfault the neighboring Frank loops.The He bubbles inside the loops provide corresponding stress for the formation of rhombic loops,which can achieve rapid growth and sweep ability by merging with the neighboring loops.Additionally,its dissociation to Shockley dis-location can unfault the Frank loops along their slip direction.Among the four Frank loop variations,the edge-on Frank loop variations have the highest growth rate,followed by the perfect loop.The related mechanisms based on in-situ experimental observation are discussed in depth.

Phase/grain boundary assisted-3D static globularization mechanism of TC17 alloy based on the microstructure reconstruction and in-situ TEM observation

Lamellar globularization in the dual-phase titanium alloy is the key to improving plasticity and strength.However,the mechanism has not been fully elucidated so far.In this work,the role of phase/grain bound-ary in the static globularization of TC17 alloy was systematically studied by setting differentαphase con-tent before annealing through low-and high-temperature deformation.Isothermal compression causes the parallel distribution and fragmentation of 3Dαplates and few globularαparticles are formed at a strain rate of 1 s^(-1).Post-deformation annealing promotes the static globularization ofαphase while it is affected by initialαphase content.After 730°C deformation,the development ofα/αinterface by absorbing dislocations promotes the formation of globularαgrains based on the nucleation of sepa-ratedαparticles and pre-recoveryαsubgrain during subsequent annealing.Theα/α/βandα/β/βtriple junctions formed due to highαcontent with about 36%volume fraction are favorable for the further nucleation and growth of globularαgrains by reducing interface energy,forming a 3D irregularαplate.Then nucleation and growth of theβphase dominate the microstructure evolution during subsequent an-nealing,resulting in the local dissolution of the plate and formation ofαrods.After 850°C deformation,theαphase tends to nucleate at theβ/β/βtriple junctions and grow into a lamellar shape along the high energyβ/βgrain boundary due to lowαcontent with about 7%volume fraction.Theαnucleation that maintains the Burgers orientation relationship(BOR)with the surroundingβphase grows along the habit plane and thickens slowly,resulting in the formation of a precipitatedαplate with a flat surface and the suppression of static globularization.The comprehensive investigation of lamellar globularization provides guidance for optimizing the 3D microstructure and properties of dual-phase titanium alloy.

In situ TEM investigation of electron irradiation and aging-induced high-density nanoprecipitates in an Mg-10Gd-3Y-1Zn-0.5Zr alloy

In-situ electron irradiation and aging are applied to introduce high-density precipitates in an Mg-10Gd-3Y-1Zn-0.5Zr(GWZ1031K,wt.%)alloy to improve the hardness.The results show that the hardness of the Mg alloy after irradiation for 10 h and aging for 9 h at 250℃ is 1.64 GPa,which is approximately 64% higher than that of the samples before being treated.It is mainly attributed to γ'precipitates on the basal plane after irradiation and the high-density nanoscale β'precipitates on the prismatic plane after aging,which should be closely related to the irradiation-induced homogenous clusters.The latter plays a key role in precipitation hardening.This result paves a way to improve the mechanical properties of metallic materials by tailoring the precipitation through irradiation and aging.

一种新型可移动TEM喇叭辐射波模拟器的模拟优化

为改善基于TEM喇叭的辐射波模拟器的低频辐射特性从而展宽其辐射近场半高宽,首次提出了在指数型TEM喇叭上/下两个极板的端口加上2个金属直板、并通过倾斜金属板和并联电阻相连的新型可移动模拟器的设计方案。基于FDTD方法模拟分析了该新型模拟器的特性参数对其近场辐射性能的影响,并给出了优化后的模拟器及其阵列的辐射特性。计算结果表明:尺寸为6 m×6 m×6.24 m的优化后的新型模拟器在距离口面3 m的中心位置的辐射近场脉宽能达到18.95 ns,而达到相同低频辐射性能的常规模拟器尺寸为9 m×12 m×6.8 m。且与常规模拟器相比,优化后的模拟器的场峰值更大。与前人的研究相比,优化后的模拟器场在保持高峰值的同时,时域波形后延震荡的幅度与主峰的比值明显减小。优化后的模拟器2×2阵列模型的测试平面中心点场峰值最大,且在测试平面上满足6 dB均匀性要求的有效测试区最大;有效测试区在横向上范围最大的是2×2阵列模型,其次是2×1阵列模型;在纵向上范围最大的是2×2阵列模型及1×2阵列模型。

埋地钢质管线非开挖检测TEM技术新进展

主要介绍了埋地钢质管道非开挖检测TEM技术在实际应用中的最新进展情况,并根据最新国内外发表的文章、专利和论文,归纳了现阶段埋地管道TEM检测过程中出现主要问题及现在最新的应对手段,并对影响埋地管道TEM检测的技术原因进行了总结分析,提出了相应的建议和措施。

基于框架语义学的TEM8汉译英试题讲解策略新探

专业八级考试(简称TEM8)是本科英语专业高年级阶段最重要的等级考试之一,其汉译英部分既是考试的难点也是考生成绩的主要堵点。基于框架思想的TEM8真题讲解策略包括:教师借助通用概念框架引导学生建构原文认知图像;通过引入免费线上语料资源FrameNet中的框架信息指导学生在目标语中重构认知图像;引导学生利用FrameNet中的真实语料,特别是框架元素的句法构型,打磨并评估译文。

集成X射线、TEM和STM的晶体学教学尝试

以Si晶体为例,介绍了一种结合X-射线、电子显微学和扫描隧道显微技术进行晶体学教学的尝试。主要是从基本原理、实验技术、实验结果等方面建立不同方法之间的联系,也说明其区别。目的是使学生能依据基本的晶体学原理、概念和数据,理解不同的晶体结构分析和表征方法提供的晶体学信息之间的区别和联系,达到融会贯通的效果。

TSP结合TEM在风险围岩隧道超前地质预报中的应用

为了排查隧道施工过程中潜在的地质风险、指导隧道安全开挖掘进,针对某高速铁路风险围岩隧道浅埋段和可溶岩段,利用TSP和TEM两种方法开展超前地质预报。TSP预报可对掌子面前方围岩状况进行远距离宏观预测,能划定断层、破碎带、地下水等不良地质体的位置和大致规模;TEM预报可在掌子面附近开展多角度、多方位测量,能判定开挖面前方一定空间范围内不良围岩特征,特别是地下水、岩溶的分布及规模。研究表明,TSP震波对应的负反射和低速异常突出反映围岩岩性变化及岩体破碎程度,依据纵、横波速起伏特征可大致判定地下水发育情况;TEM低阻异常直观体现围岩富水状态,并可推测岩溶发育及分布状况,视电阻率阻值变化密集区对应了围岩岩体破碎。研究结果表明,采用两种或多种方法结合开展综合预报,可提升预报结论的准确度和可靠度,TSP结合TEM成功预报的应用实例可为类似风险围岩隧道的超前地质预报提供参考和借鉴。

In-situ interfacial passivation and self-adaptability synergistically stabilizing all-solid-state lithium metal batteries

The function of solid electrolytes and the composition of solid electrolyte interphase(SEI)are highly significant for inhibiting the growth of Li dendrites.Herein,we report an in-situ interfacial passivation combined with self-adaptability strategy to reinforce Li_(0.33)La_(0.557)TiO_(3)(LLTO)-based solid-state batteries.Specifically,a functional SEI enriched with LiF/Li_(3)PO_(4) is formed by in-situ electrochemical conversion,which is greatly beneficial to improving interface compatibility and enhancing ion transport.While the polarized dielectric BaTiO_(3)-polyamic acid(BTO-PAA,BP)film greatly improves the Li-ion transport kinetics and homogenizes the Li deposition.As expected,the resulting electrolyte offers considerable ionic conductivity at room temperature(4.3 x 10~(-4)S cm^(-1))and appreciable electrochemical decomposition voltage(5.23 V)after electrochemical passivation.For Li-LiFePO_(4) batteries,it shows a high specific capacity of 153 mA h g^(-1)at 0.2C after 100 cycles and a long-term durability of 115 mA h g^(-1)at 1.0 C after 800 cycles.Additionally,a stable Li plating/stripping can be achieved for more than 900 h at 0.5 mA cm^(-2).The stabilization mechanisms are elucidated by ex-situ XRD,ex-situ XPS,and ex-situ FTIR techniques,and the corresponding results reveal that the interfacial passivation combined with polarization effect is an effective strategy for improving the electrochemical performance.The present study provides a deeper insight into the dynamic adjustment of electrode-electrolyte interfacial for solid-state lithium batteries.

The effect of temperature on load partitioning evolution in magnesium metal matrix composite reinforced with Ti particles using in-situ synchrotron radiation diffraction experiments

The load partitioning between the magnesium and titanium phases in an extruded Mg-15%Ti(vol.%) composite from room temperature up to 300 ℃ using synchrotron radiation diffraction during in-situ compression tests. During compression, the magnesium matrix composite deforms mainly by the activation of the extension twinning system up to 200 ℃. The volume fraction of twins increases with the plastic strain but decrease with the compression temperature. Hard titanium particles bear an additional load transferred by the soft magnesium matrix from room temperature up to 300 ℃. This effect is amplified after yield stress during plastic deformation. Additionally, twins within magnesium grains behaves as an additional reinforcement at low temperature(below 200 ℃) inducing an increase in the work hardening of the composite.