基于FIB-SEM双束系统制备TEM原位加热样品

聚焦离子束-扫描电子显微镜(FIB-SEM)双束系统因具有定位精准、加工精度高等优点,被广泛用于微纳尺度样品的高质量制备,如定点截面加工、纳米图形加工、透射电子显微镜(TEM)和三维原子探针样品等。然而,随着TEM原位表征技术的发展,对样品的制备提出了更高的要求。其中,TEM原位加热样品由于受加热芯片几何形状的限制,在样品的提取、转移和减薄等工序上具有较高的技术难度。利用FIB-SEM双束系统,在传统TEM样品制备工艺基础上,通过合理改进制备流程和参数,调整样品提取和减薄顺序,并配合低电压清扫工艺,成功制备了可用于原位加热和表征的TEM样品。

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。

聚集离子束扫描电镜(FIB-SEM)在页岩纳米级孔隙结构研究中的应用

页岩中大量发育的纳米级孔隙组成了页岩气储集的主要空间。聚集离子束扫描电镜(FIB-SEM)通过对页岩样品的连续切割和成像,能够在纳米尺度上三维重建页岩的空间分布。依据不同岩石组分灰度值的差异,可以将页岩内的孔隙、有机质、黄铁矿等分割提取出来,不仅可以三维展示其空间分布形态,还可以对孔隙的分布特征和孔隙度等参数进行定量计算。聚集离子束扫描电镜在页岩纳米孔隙中的应用,将给页岩微观结构的深入研究提供新的研究手段。

基于FIB-SEM双束系统的纳尺度真空间隙电学特性原位实验装置

纳米尺度真空电气击穿与绝缘特性研究是高电压与绝缘技术领域的前沿课题。一方面,随着微纳尺度加工技术的不断发展,电气部件和电子器件的特征物理尺寸已经逐步降低到微米、纳米甚至是分子原子尺度,并且在军事和民用领域得到越来越广泛的应用;另一方面,传统的放电击穿理论和绝缘性能评价方法无法用来解释和预估微纳尺度的放电特性和绝缘水平。因此,本文基于聚焦离子束和扫描电子显微镜(FIB-SEM)双束系统,借助纳米压电位移技术和微弱电流测量技术,建立了纳尺度真空间隙电学特性的原位研究系统。该系统不仅能够进行微纳尺度(曲率半径为15 nm^10μm)金属电极的原位加工,材料组成成分的定量分析,而且可以实现纳尺度真空间隙(>20 nm)的放电特性研究,为纳尺度击穿规律和绝缘特性的实验研究提供了有力的支撑。

FIB-SEM图像多策略层间配准与插值算法

聚焦离子束扫描电镜(FIB-SEM)生成的切片图层间距过大,导致重建后的三维微纳米孔隙图多存在断层现象。为解决此问题,提出一种基于非下采样轮廓波变换NSCT(Nonsubsampled Contourlet Transform)的多策略层间配准与插值算法。该方法利用NSCT捕捉切片图轮廓信息,生成相应NSCT系数;对NSCT低频系数利用基于自由形变FFD(Free-Form Deformation)配准的插值算法生成新插值图的低频子图概貌;对NSCT高频方向子带采用多项式拟合方法进行插值以获得精确的新插值图轮廓结构信息;通过逆NSCT,生成新层间图像,缩减切片纵向间距,提高三维微纳米孔隙图的质量。实验结果表明,该算法可有效提升新层间图像的质量与轮廓结构准确性,削弱噪声影响。相较于其他算法,该算法生成的新层间图像质量在主观与客观上均有所提升。

基于主动轮廓的岩心FIB-SEM序列图像孔隙提取方法

岩心FIB-SEM序列图像在孔隙提取过程中存在着灰度不均匀,孔隙内部出现高光等难点,目前尚没有一种统一的提取岩石孔隙的方法。提出一种基于主动轮廓的岩心FIB-SEM序列图像孔隙提取方法,其利用图像层间相关性,采用主动轮廓算法提取孔隙,同时给出一种自动寻找最优提取效果的算法。利用该方法所提取孔隙的效果优于对比算法,与人工识别出的孔隙区域十分接近。

FIB-SEM双束系统在PCB及IC载板缺陷检测中的应用

FIB-SEM(Focused Ion Beam-Scanning Electron Microscope)双束系统是集聚焦离子束和扫描电子显微镜与一体的系统,其最大的优势是可以实现离子束切割或微加工的同时用电子束实时观察的功能。主要介绍FIB-SEM双束系统在PCB及IC载板缺陷检测中的常见应用,如盲孔孔底分析、杂物失效分析和晶体结构分析。

HR-TEM and FIB-SEM characterization of formation of eutectic-like structure from amorphous GdAlO_3-Al_2O_3 system

The crystallization process of the eutectic composition of GdAlO_3-Al_2O_3 from the amorphous phase prepared by rapid-quenching of melt that leads to the formation of a cantaloupe skin-like microstructure was investigated using focused ion-beam scanning electron microscopy (FIB-SEM) and high-resolution transmission electron microscopy (HR-TEM).The amorphous films were heat-treated at temperatures between 1000 °C and 1500 °C for up to 30min to form the eutectic phases of GdAlO_3 and Al_2O_3.The GdAlO_3 and Al_2O_3 crystal phases that formed from the amorphous phase were identified by FIB-SEM and HR-TEM.Both components began to crystallize and grow from the amorphous phase separately at different temperatures.The formation process of these crystal phases was different from that of the ordinary eutectic microstructure solidified from the GdAlO_3-Al_2O_3 system.Therefore,the observed structure is termed "eutectic-like" for distinction.The microstructures formed from the amorphous phases at sufficiently high temperatures consisted of ultra-fine microstructures of individually crystallized components and were similar to ordinary eutectic microstructures.By heat-treating the amorphous films at 1500 °C for either 2 min,8min or 30min,the ultra-fine components of GdAlO_3 and Al_2O_3 were found to crystallize following a eutectic-like stage after 8min of heat treatment.

Microscale crack propagation in shale samples using focused ion beam scanning electron microscopy and three-dimensional numerical modeling

Reliable prediction of the shale fracturing process is a challenging problem in exploiting deep shale oil and gas resources.Complex fracture networks need to be artificially created to employ deep shale oil and gas reserves.Randomly distributed minerals and heterogeneities in shales significantly affect mechanical properties and fracturing behaviors in oil and gas exploitation.Describing the actual microstructure and associated heterogeneities in shales constitutes a significant challenge.The RFPA3D(rock failure process analysis parallel computing program)-based modeling approach is a promising numerical technique due to its unique capability to simulate the fracturing behavior of rocks.To improve traditional numerical technology and study crack propagation in shale on the microscopic scale,a combination of high-precision internal structure detection technology with the RFPA^(3D) numerical simulation method was developed to construct a real mineral structure-based modeling method.First,an improved digital image processing technique was developed to incorporate actual shale microstructures(focused ion beam scanning electron microscopy was used to capture shale microstructure images that reflect the distri-butions of different minerals)into the numerical model.Second,the effect of mineral inhomogeneity was considered by integrating the mineral statistical model obtained from the mineral nanoindentation experiments into the numerical model.By simulating a shale numerical model in which pyrite particles are wrapped by organic matter,the effects of shale microstructure and applied stress state on microcrack behavior and mechanical properties were investigated and analyzed.In this study,the effect of pyrite particles on fracture propagation was systematically analyzed and summarized for the first time.The results indicate that the distribution of minerals and initial defects dominated the fracture evolution and the failure mode.Cracks are generally initiated and propagated along the boundaries of hard mineral particles such as pyrite or in soft minerals such as organic matter.Locations with collections of hard minerals are more likely to produce complex fractures.This study provides a valuable method for un-derstanding the microfracture behavior of shales.

A dual-beam piezo-magneto-elastic wake-induced vibration energy harvesting system for high-performance wind energy harvesting

Wind-induced vibration energy harvesting has a great potential for utilizing wind energy to supply power for low-powered devices.To improve the working performance of energy harvesters effectively,a suitable structural design is crucial.This paper proposes a dual-beam piezo-magneto-elastic wake-induced vibration energy harvesting system to enhance the functional performance of aeroelastic energy harvesters in environments with variable wind speeds.The system contains two piezoelectric beams coupled by magnets(forming upstream and downstream energy harvesters),and each beam is attached with a foam cylinder.A corresponding dynamic model is provided,and output characteristics are obtained at different wind speeds.Results and experimental verification indicate that both upstream and downstream energy harvesters can realize efficient energy harvesting.When the wind speed exceeds a certain critical value,the amplitudes of the system’s displacement and voltage are high.The wind speed threshold value is approximately 1.25 m/s.When the wind speed and magnet spacing are 10.2 m/s and 20 mm,respectively,the output power of the system reaches 4.9×10^(−4)W.Moreover,the wind speed threshold value of the proposed system can be adjusted by an equivalent nonlinear restoring force.

High-precision alkali-atom density measurement and control methods using light absorption for dual-beam SERF magnetometers

The alkali-atom density measurement method based on light absorption is highly suitable for a spin-exchange relaxationfree(SERF)atomic magnetometer because of its high-precision measurement and complete nonmagnetic interference.In this study,the optical rotation angle detection system based on polarization balance detection is utilized to realize the alkali-atom density real-time measurement without affecting magnetic field measurement.We discovered that there exists an optimal frequency detuning of the probe light,which offers the highest sensitivity in alkali-atom density measurement and the lowest susceptibility to temperature fluctuations in terms of the scale factor.In contrast to conventional light absorption measurements based on pump light,this method demonstrated a threefold improvement in alkali-atom density measurement sensitivity while remaining immune to ambient magnetic fields and incident light intensity fluctuations.Furthermore,we utilized this method to achieve closed-loop temperature control with an accuracy of 0.04℃.

Structural and Chemical Characterization of the Ediacaran Embryo-Like Fossils via the Combination of 3D-XRM and FIB-SEM Approaches

The three-dimensional(3D)morphology,anatomy,and in-situ chemical composition analysis of fossils are crucial for systematic paleontology and determining their phylogenetic positions.Scanning electron microscopy(SEM)coupled with energy-dispersive X-ray spectroscopy(EDS),offers valuable structural and chemical information for the analysis of fossils.However,its primary limitation is the restriction to two-dimensional surface data,which limits the exploration of fossils’3D complexities.Conversely,3D X-ray microscopy(3D-XRM),also known as a novel form of micro-computed tomography(micro-CT)facilitates the non-destructive 3D reconstruction of fossil specimens.Nevertheless,it lacks the capability to provide in-situ compositional data.Acknowledging the constraints inherent in these individual techniques,and in response to the evolving requirements of paleontological research,this study introduces an integrated approach that combines 3D-XRM with EDS-coupled focused ion beam scanning electron microscopy(FIB-SEM).This innovative strategy is designed to synergize the advantages of both techniques,thereby addressing challenges that conventional methods cannot.It enables the rapid identification of regions of interest(ROI)within fossil specimens at micrometer resolution.Subsequently,this method collects detailed data on both 3D structures and chemical compositions at the nanometer scale for the identified ROI.This integrated approach represents a significant advancement in paleontological and geological research methodologies,promising to meet the increasing demands of these fields.

聚焦离子束扫描电镜研究微体化石的微观孔隙结构

聚焦离子束扫描电镜(FIB-SEM)是将聚焦离子束切割和扫描电镜结合起来的双束系统,可以在纳米尺度对样品进行切割加工与实时成像。文中用聚焦离子束扫描电镜对兰多维列统(志留系)龙马溪组黑色页岩内的几类微体化石进行了观察研究,并显示牙形刺、几丁石、疑源类均发育有亚微米至纳米级孔隙,这些孔隙可以为页岩气的储集提供有效空间,不同的微体化石孔隙发育的差异可以为页岩中有机质孔隙非均质性成因研究提供重要依据。

聚焦离子束电子束系统及其在生物学和医学上的应用

聚焦离子束电子束系统在材料失效分析、纳米材料结构表征与性能分析以及纳米器件研制等方面发挥着重要作用。近年来该系统在生物学和医学领域的应用日益受到人们的重视。本文介绍聚焦离子束电子束系统的组成、性能、相关功能及其在生物学和医学上的若干应用,包括透射电镜生物样品制备、细胞和组织内部结构观察与三维重构等。

基于FIB/SEM双束系统的原位、实时观测三点弯曲薄膜测试方法

目的需要直接测量薄膜的极限形变这一关键参数,来评价某种薄膜在一定服役载荷下的某种基体表面是否能胜任。方法借助聚焦离子束显微镜/扫描电子显微镜(FIB/SEM)双束显微分析测试系统,提出了一种在微米尺度下、原位进行三点弯曲薄膜测试的方法,同时可以进行实时观测与分析记录。之后,使用磁控溅射技术制备了具有强择优晶体生长取向的CrN薄膜和Cr/CrN多层薄膜,并使用上述三点弯曲测试方法对这两种薄膜进行了弯曲测试。结果CrN薄膜的极限形变量为(1.8±0.1)%,且其在原位三点弯曲试验中断裂前的变形类型为纯弹性形变,而不是塑性形变或者弹性/塑性混合形变。而Cr/CrN多层薄膜的极限形变达到了9.1%,是纯CrN薄膜的5倍,且对“预裂纹”等缺陷不敏感。结论将此测试方法与在微米尺度使用FIB测量薄膜残余应力的方法相结合,将可以有效地评估多种薄膜的形变能力及形变特性。所获得的薄膜相关性能数据,对于针对不同基体、不同使用工况(如不同的表面受力状态、变形状态等)的薄膜体系或结构的选择与设计,具有很好的指导意义。

Simulation and visualization of the displacement between CO2 and formation fluids at pore-scale levels and its application to the recovery of shale gas

This article reports recent developments and advances in the simulation of the CO2-formation fluid displacement behaviour at the pore scale of subsurface porous media. Roughly, there are three effective visualization approaches to detect and observe the CO2-formation fluid displacement mechanism at the micro-scale, namely, magnetic resonance imaging, X-ray computed tomography and fabricated micromodels, but they are not capable of investigating the dis- placement process at the nano-scale. Though a lab-on-chip approach for the direct visualization of the fluid flow behaviour in nanoscale channels has been developed using an advanced epi-fluorescence microscopy method combined with a nanofluidic chip, it is still a qualitative analysis method. The lattice Boltzmann method （LBM） can simulate the CO2 displacement processes in a two-dimensional or three-dimensional （3D） pore structure, but until now, the CO2 displace- ment mechanisms had not been thoroughly investigated and the 3D pore structure of real rock had not been directly taken into account in the simulation of the CO2 displacement process. The status of research on the applications of CO2 displacement to enhance shale gas recovery is also analyzed in this paper. The coupling of molecular dynamics and LBM in tandem is proposed to simulate the CO2-shale gas displacement process based on the 3D digital model of shale obtained from focused ion beams and scanning electron microscopy.

Characterization of 3D pore nanostructure and stress-dependent permeability of organic-rich shales in northern Guizhou Depression,China

The three-dimensional(3D)pore structures and permeability of shale are critical for forecasting gas production capacity and guiding pressure differential control in practical reservoir extraction.However,few investigations have analyzed the effects of microscopic organic matter(OM)morphology and 3D pore nanostructures on the stress sensitivity,which are precisely the most unique and controlling factors of reservoir quality in shales.In this study,ultra-high nanoscale-resolution imaging experiments,i.e.focused ion beam-scanning electron microscopy(FIB-SEMs),were conducted on two organic-rich shale samples from Longmaxi and Wufeng Formations in northern Guizhou Depression,China.Pore morphology,porosity of 3D pore nanostructures,pore size distribution,and connectivity of the six selected regions of interest(including clump-shaped OMs,interstitial OMs,framboidal pyrite,and microfractures)were qualitatively and quantitatively characterized.Pulse decay permeability(PDP)measurement was used to investigate the variation patterns of stress-dependent permeability and stress sensitivity of shales under different confining pressures and pore pressures,and the results were then used to calculate the Biot coefficients for the two shale formations.The results showed that the samples have high OM porosity and 85%of the OM pores have the radius of less than 40 nm.The OM morphology and pore structure characteristics of the Longmaxi and Wufeng Formations were distinctly different.In particular,the OM in the Wufeng Formation samples developed some OM pores with radius larger than500 nm,which significantly improved the connectivity.The macroscopic permeability strongly depends on the permeability of OM pores.The stress sensitivity of permeability of Wufeng Formation was significantly lower than that of Longmaxi Formation,due to the differences in OM morphology and pore structures.The Biot coefficients of 0.729 and 0.697 were obtained for the Longmaxi and Wufeng Formations,respectively.

Quantitative two/three-dimensional spatial characterization and fluid transport prediction of macro/micropores in Gaomiaozi bentonite

The sealing performance of a bentonite barrier is highly dependent on its seepage characteristics, which are directly related to the characteristics of its pore structure. Based on scanning electron microscopy(SEM) and focused ion beam-SEM(FIB-SEM), the pore structure of bentonite was characterized at different scales. First, a reasonable gray threshold was determined through back analysis, and the image was binarized based on the threshold. In addition, binary images were used to analyze bentonite’s pore structure(porosity and pore size distribution). Furthermore, the effects of different algorithms on the pore structure characterization were evaluated. Then, permeability calculations were performed based on the previous pore structure characteristics and a modified permeability prediction model. For permeability prediction based on the three-dimensional model, the effect of pore tortuosity was also considered. Finally, the accuracy of numerical calculations was verified by conducting macroscopic gas and alcohol permeability experiments. This approach provides a better understanding of the microscale mechanism of gas transport in bentonite and the importance of pore structures at different scales in determining its seepage characteristics.

冷冻双束扫描电镜的开放与管理

带冷冻传输系统的双束扫描电镜可实现样品原生态下的高分辨图像采集,以及冷冻含水样品的超薄切片制备,而被广泛应用于生命、医学、食品、化学、材料等领域,在相关科学研究中逐渐体现出不可取代的地位.介绍了带冷冻系统扫描电镜的基本配置,并重点从开放共享与成效、仪器常见故障及维护等方面详细阐述了仪器的科学管理,以提高仪器的使用效率,为同类型仪器的运行提供管理经验.

Bi-Function Multi-Beam Graphene Lens Antenna for Terahertz Applications

Bi-function Compact graphene lens antenna in terahertz (THz) band has been investigated. The array function is switched between two status, reflectarray and/or transmitarray. The tunability of graphene conductivity introduces the bi-function characteristics of a single array structure in the THz band. The design depends on changing the graphene DC biasing voltage to transform the transmitting antenna to reflecting antenna. The compact structure of the antenna array saves the cost and the allocation area for the terahertz communication applications. A 13 × 13 reflectarray/ transmitarray antenna covering an area of 364 × 364 μm2 is proposed. A dual-beams reflectarray/transmitarray antenna is achieved by rearranging the cell elements of the array successively. Finally, a single structure is used to work as reflectarray and transmitarray antenna at the same time by rearranging the applied voltages between the different pieces of the graphene sheet using chess board arrangement. The phases of the successive unit-cells are kept the same of their locations in the original full array. The radiation characteristics of the array are investigated using the CST Microwave Studio for the bi-function operation.