28 January 2026, Volume 46 Issue 1
    

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  • Focused ion beam technology in materials science: From micro/nanofabrication to multimodal correlative characterization
    QIAO Yi, LI Shilei, WANG Yanhua
    Metallurgical Analysis. 2026, 46(1): 1-23. https://doi.org/10.13228/j.boyuan.issn1000-7571.013177
    Abstract ( ) Download PDF ( )   Knowledge map   Save
    Since the advent of focused ion beam(FIB) technology,it has developed from a micro/nanofabrication tool in the semiconductor industry into an indispensable platform for multimodal characterization in materials science.This paper systematically summarizes the fundamental principles and equipment configuration FIB technology as well as the key applications in micro/nanofabrication.The combination characterization strategies of FIB with scanning electron microscope(SEM),energy-dispersive X-ray spectroscopy(EDS),electron backscatter diffraction(EBSD),transmission electron microscope(TEM),and atom probe tomography(APT) are emphasized.The correlative characterization is classified into two categories,i.e.,in situ integration and offline correlative analysis.The advantages of two categories in dynamic process observation and cross-scale information association are discussed,respectively.In addition,the possible irradiation damage mechanisms in FIB fabrication and the mitigation strategy are analyzed in depth.The latest developments in FIB-related standardization efforts at home and abroad are introduced.Finally,the development trend of FIB technology toward higher performance,intelligent operation and deeper integration are prospected.The key roles of FIB technology in constructing material genome map and promoting materials design and property optimization are highlighted.
  • Application of focused ion beam-scanning electron microscope in shale oil and gas research
    ZHANG Lin, WANG Xiaoqi, JIN Xu, FANG Zhengwei WANG Mingwei, BAO Fang, GAO Huanxiang, GAO Haifeng
    Metallurgical Analysis. 2026, 46(1): 24-36. https://doi.org/10.13228/j.boyuan.issn1000-7571.013135
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    Focused ion beam-scanning electron microscope(FIB-SEM) has become a crucial tool in shale oil and gas research due to its ability in nanoscale precision in micro-nano fabrication,high-resolution imaging capability,and extensive range of accessory functions.Particularly,it demonstrates unique advantages in characterizations of shale reservoirs microstructure,pore characteristics,and organic matter distribution.The technical advancements and comprehensive applications of FIB-SEM in shale oil and gas research in recent years were systematically reviewed in this article,which covered multiple aspects such as the three-dimensional quantitative characterization of nanopore systems,microscopic distribution analysis of organic and inorganic matters,analysis of residual oil distribution,mineral identification and analysis,and the construction of digital rock core models based on serial sectioning-imaging.Furthermore,as a vital component in shale characterization,FIB-SEM could be integrated with other advanced techniques,which enabled the comprehensive characterizations that spanned from the nanoscale to the macroscale,encompassed multiple dimensions from chemical composition to physical structure,and covered multiple temporal domains from static imaging to dynamic evolution.The evolutionary behavior of shale under subsurface conditions or extreme environments could be revealed.The multi-scale and multi-dimensional comprehensive analysis platform built based FIB-SEM as the core,combined with the automation of equipment and the application of artificial intelligence(AI) technology,could provide unprecedented integrated research solutions for addressing complex systemic challenges in shale oil and gas,which willprovide critical technical support for research on microscopic mechanisms and the construction of macro-scale cognition in the field of petroleum geology.
    • Ferrous Metallurgy
  • Application of focused ion beam scanning electron microscope in failure analysis of anode cap pickling for glow discharge mass spectrometry
    CUI Siyu, YU Xing, LIU Suran, SHEN Yixuan, ZHAO Lei, WANG Haizhou
    Metallurgical Analysis. 2026, 46(1): 37-45. https://doi.org/10.13228/j.boyuan.issn1000-7571.013111
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    The corrosion failure causes of anode caps for glow discharge mass spectrometry(GDMS) after acid pickling were investigated by focused ion beam scanning electron microscope(FIB-SEM).Additionally,electron backscatter diffraction(EBSD) and time-of-flight secondary ion mass spectrometry(TOFSIMS) were employed to conducted the comparative characterizations of 304 stainless steel anode caps with different processing technologies(designated as CN and IM,respectively) for GDMS.The results of SEM morphology analysis revealed that the passive film of CN anode cap had defects,and a large number of pitting corrosion pits appeared after acid pickling.In contrast,the passive film of IM anode cap was dense with no corrosion traces on its surface after acid pickling.Energy dispersive spectroscopy(EDS) compositional analysis showed that the CN anode cap contained 0.3%(mass fraction,the same below) S and 1.8% Mn,leading to the formation of sulfide inclusions.On the contrary,S was not detected from the IM anode cap;the content of Mn was 0.8%;the distribution of 0.4% Cu was uniform,which could enhance the corrosion resistance.The crystal structure characterization by EBSD indicated that the grains in IM anode cap was finer,and there was a work-hardened layer with a grain gradient near its surface.Conversely,the size of grains in CN anode cap was larger,and there was no work-hardened layer in the near-surface region.TOFSIMS results demonstrated that the passive film of the CN anode cap had a thickness of 90 nm.For the IM anode cap,the nanocrystals near its surface exhibited stronger resistance to plasma,and its passive film thickness was 40 nm.
  • Discussion on the effect of inclusion characteristics in silicon-manganese killed high-carbon steel on the casting performance of molten steel
    WU Yuanyuan, JIN Chuanwei, ZHANG Jiming, ZHAO Jiaqi
    Metallurgical Analysis. 2026, 46(1): 46-54. https://doi.org/10.13228/j.boyuan.issn1000-7571.012842
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    During the smelting of silicon-manganese killed high-carbon steel wire rods using a high-basicity refining slag system,the phenomenon of nodulation frequently occurs in the continuous casting process of molten steel.Calcium treatment is usually employed for the modification of inclusion types to reduce the nozzle clogging.However,the clogging issues persist during production even after calcium treatment.Therefore,it has significant importance to study the effect of inclusion characteristics in silicon-manganese killed high-carbon steel on the casting performance of molten steel.In this study,the high-strength cable steel was selected as the research subject.Some advanced analytical tools,including focused ion beam-scanning electron microscope(FIB-SEM),transmission electron microscope(TEM),inclusion analyzer,and three-dimensional reconstruction software,were used to conduct detailed analyses of inclusions in two batches of samples:one with poor casting performance and another with significantly improved casting performance.The results showed that the casting performance of molten steel was directly related to the proportion of high-melting-point inclusions.In the batch with poor casting performance,the proportion of high-melting-point inclusions increased from 59% to 82% after calcium treatment.Conversely,in the batch with improved casting performance,the proportion of high-melting-point inclusions decreased from 76% to 53% after calcium treatment.Additionally,the structural morphology of inclusions also affected the casting performance of molten steel.Since the high-melting-point phases in inclusions were exposed outside,they were tended to adhere to the submerged entry nozzle during casting,leading to the nozzle clogging and deteriorating the steel fluidity.In contrast,the encapsulating of high-melting-point phases by low-melting-point phases in inclusions would exhibit better encapsulation.Such inclusions maintained closer contact with the molten steel,which could increase the wetting angle between inclusions and refractory materials,thus reducing the clogging risks and thereby enhancing the castability of molten steel.
  • Characterization of macroscopic distribution and microstructure of inclusions in continuous casting billet of 82A tire cord steel
    JIN Chuanwei, ZHANG Jiming, WU Yuanyuan, ZHAO Jiaqi
    Metallurgical Analysis. 2026, 46(1): 55-62. https://doi.org/10.13228/j.boyuan.issn1000-7571.012946
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    The macroscopic distribution,microstructure,and formation mechanisms of inclusions in continuous casting billets of 82A tire cord steel were investigated in this study.The tests by inclusion analyzer,focused ion beam-scanning electron microscope(FIB-SEM) and transmission electron microscope(TEM) indicated that the inclusions in casting billets were mainly categorized into three types:MnS,MnS-SiO2 composite,and MnS/SiO2-MgAlSiCaMnO composite.Specifically, MnS type inclusions with sizes of [5,15] μm were predominantly aggregated within 14 mm from the edge of casting billet,while larger MnS type inclusions (equivalent spherical diameter d≥15 μm) were uniformly distributed from 14 mm to the core.MnS-SiO2 type composite inclusions are mainly distributed within the range of (0,17] mm from the edge of casting billet,with a dominant size of [5,15] μm,and exhibit local aggregation in the interval of (14,17] mm. In contrast,MnS/SiO2-MgAlSiCaMnO type composite inclusions were uniformly distributed without any localized clustering.The detailed microstructures and three-dimensional morphologies of these inclusions were revealed by TEM and three-dimensional reconstruction.MnS type inclusions were rod-like in shape with through-hole defects inside.The edges of these defects were enriched with Fe and C particles,and the outer surface was coated with small SiO2 particles.In the MnS-SiO2 type composite inclusions,SiO2 were in the core and MnS were located on outer surface,forming a core-shell encapsulated near-spherical structure.The MnS/SiO2-MgAlSiCaMnO type composite inclusions contained Fe-rich particles and hole defects internally.The formation mechanisms of MnS type and MnS-SiO2 type composite inclusions were closely related to the temperature distribution and crystal dendrite aggregation during the cooling process of the casting billet.MnS was preferentially nucleated and aggregated within the rapid solidification region with depth of 14 mm from the surface of the casting billet.MnS-SiO2 type composite inclusions were locally aggregated in the semi-solid region of (14,17] mm.MnS/SiO2-MgAlSiCaMnO type composite inclusions were uniformly distributed throughout the billet.
  • Application of focused ion beam dual-beam scanning electron microscope in fracture crack analysis
    ZOU Yongchun, SUN Jiashuo, SHAO Dihua, DI Yue, WANG Shuqi CHEN Guoliang, YE Zhiyun, WANG Yaming
    Metallurgical Analysis. 2026, 46(1): 63-71. https://doi.org/10.13228/j.boyuan.issn1000-7571.013163
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    Due to the high-resolution imaging ability and site-specific nanoscale processing capacity,the focused ion beam dual-beam scanning electron microscope(FIB-SEM dual-beam system) has become an important approach for material information analysis such as microscopic morphology and structure of fracture crack as well as the internal cracks and porosity distribution.The micron-to-nanometer scale site-specific processing at targeted regions such as crack tips by FIB-SEM dual-beam system was systematically introduced in this paper.The in-situ analysis technique was employed to expose and observe the crack propagation paths and tip microstructure.In addition,the three-dimensional morphological reconstruction inside the material was realized by combining with serial sectioning.The distribution of internal cracks and pores were deeply analyzed.On this basis,a comprehensive and standardized FIB-based specimen preparation method for site-specific analysis was established.This method delineated the operation specifications and parameter instructions of key steps such as protective layer deposition,coarse milling,fine polishing,specimen lift-out and transfer.The proposed method effectively solved the longstanding limitations of conventional techniques in fractography,namely imprecise localization,introduction of mechanical damage,and limited structural information,thereby providing method reference and technical support for crack analysis and lift-out from fracture.
    • Semiconductor Fabrication
  • Application of focused ion beam in semiconductor device processing and elemental analysis coupled with time-of-flight secondary ion mass spectrometry
    WANG Linjun
    Metallurgical Analysis. 2026, 46(1): 72-79. https://doi.org/10.13228/j.boyuan.issn1000-7571.013162
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    Focused ion beam(FIB) technology demonstrates significant value in semiconductor device research due to its high-precision micro/nano fabrication and in-situ analysis capabilities.This paper aimed to provide an in-depth exploration in typical applications of FIB in semiconductor device processing and elemental analysis.The FIB system was employed to realize the microelectrode fabrication for two-dimensional materials and one-dimensional nanowires,as well as to precisely process optical microstructures such as solid immersion lens(SIL) and two-dimensional photonic crystals.Furthermore,by combining FIB with time-of-flight secondary ion mass spectrometry(ToF-SIMS),a high-resolution analysis of elemental depth distribution in semiconductor multilayer film structures was achieved.The experimental results indicated that FIB enabled precise control of fabrication scales down to the 10-nanometer level,which significantly enhanced the device integration and performance.The combined FIB-ToF-SIMS technique effectively revealed the doping element and interface diffusion behavior.The study demonstrated that FIB was not only an efficient micro/nano fabrication tool,but also could synergize with characterization techniques such as ToF-SIMS to highlight its critical role as an advanced tool in the semiconductor field.It could provide essential technical support for the design,processing,and failure analysis of advanced semiconductor devices.
  • Application of focused ion beam dual-beam scanning electron microscope in defect and failure analysis of silicon-based chip
    LIU Chen, CHEN Zhen, LU Yudong, LÜ Jinhao JIANG Liang, ZHANG Cuiyuan, PAN Jing
    Metallurgical Analysis. 2026, 46(1): 80-86. https://doi.org/10.13228/j.boyuan.issn1000-7571.013164
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    The unique advantage of the focused ion beam-dual beam scanning electron microscope(FIB-SEM dual-beam system) lies in its simultaneous capability for high-resolution imaging and nanoscale micro-area processing precision.In this paper,the fundamental functions of FIB-SEM dual-beam system and the conventional procedures of chip failure analysis are first briefly introduced.Then the application cases of FIB-SEM dual-beam system in defect and failure analysis of different types of chips are discussed,including three-dimensional failure analysis of silicon-based integrated circuits and hot spot cross-sectional analysis of power devices.In the case of three-dimensional failure analysis of silicon-based integrated circuits,a novel three-dimensional failure analysis method is introduced,which is more time-efficient and high-effective compared with the traditional FIB-SEM three-dimensional reconstruction method.In this method a planar transmission electron microscope(TEM) sample which covers the hot spot area is prepared in the X-Y direction,i.e.,the direction parallel to the chip surface.Subsequently,the planar-to-cross-sectional sample preparation method is adopted to convert the planar sample into a cross-sectional sample perpendicular to the chip surface.This three-dimensional analysis confirms that the abnormal point is indeed an abnormal overlap of tungsten(W).In another case of hot spot cross-sectional analysis of power devices,the silicon-based insulated gate bipolar transistors(Si-IGBT) is used as an example.The key steps and parameter selections for failure analysis of power devices using FIB-SEM are introduced in detail,including the selection of currents for ion beam cutting and protective layer deposition.Finally,the development prospect of FIB-SEM technology in this area is summarized.
  • Research on detection method for chip packaging process
    ZHANG Cuiyuan
    Metallurgical Analysis. 2026, 46(1): 87-94. https://doi.org/10.13228/j.boyuan.issn1000-7571.013161
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    With the miniaturization and high density of chip packaging,as well as the continuous emergence of various new packaging technologies,the detection requirements for chip packaging process are becoming increasingly higher.This paper mainly expounds the detection methods for chip packaging processes,including non-destructive analysis methods and destructive analysis methods.Among them,the focused ion beam(FIB) analysis method is introduced in detail,including its principle and related applications.In addition,the typical applications,advantages and disadvantages of several detection methods for chip packaging processes are compared.These methods are of great significance for the quality evaluation and defect detection of chip packaging processes.
  • Geometric prior enhanced edge detection algorithm for regular pattern measurement in FIB-SEM nanostructure
    WANG Xuxing, CAO Zhenfeng, SUN Wei, QIU Tingting, WANG Xianhao ZHANG Xiaohui, YANG Minglai, WANG Ying
    Metallurgical Analysis. 2026, 46(1): 95-106. https://doi.org/10.13228/j.boyuan.issn1000-7571.013159
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    This paper proposed a geometric prior enhanced edge detection algorithm for the focused ion beam-scanning electron microscope(FIB-SEM) nanostructure measurement,aiming to address the insufficient detection accuracy of traditional edge detection methods for regular nanopatterns in scanning electron microscope images.The core innovation lied in the geometric prior enhanced pixel difference convolution network(PiDiNet-GP),which explicitly constructed the specialized convolution kernels that preferentially respond to specific geometric structures through direction-enhanced pixel difference convolution(PDC) and curvature-aware PDC.The direction-enhanced PDC module specifically targeted the structures with obvious directionality such as rectangles,constructing differential kernels in multiple fundamental directions to significantly improve the detection accuracy of straight edges.The curvature-aware PDC module mainly targeted the curved structures such as circles,constructing radial differential kernels at multiple radius scales to enhance the detection capability of circular contours,thus enabling the network to possess geometric structure perception capability from shallow layers.The algorithm adopted a two-stage pipeline architecture:the first stage used the PiDiNet-GP model for high-quality edge detection,while the second stage performed contour classification and parameter fitting based on traditional image processing and machine learning methods.The experimental results demonstrated that the proposed method achieved higher precision and robustness in detecting circular and rectangular nanostructures in FIB-SEM images,showing significant advantages particularly in the detection of regular geometric patterns.The accurate detection of regular patterns was crucial for defect detection and quality control in nanomanufacturing.It could effectively identify the shape anomalies,dimensional deviations,and geometric deformations in nanostructures,which provided key evidence for the early detection of process defects.The quantification of dimensional consistency,positional precision,and shape integrity of nanostructures through high-precision geometric parameter measurement provided reliable data support for objective evaluation of product quality,and offered powerful technical support for the quality control and process optimization in nanomanufacturing processes.
  • Development of quality control sample of length measurement for electron microscope
    PENG Kaiwu, CHANG Huaiqiu, BAI Lu, GUO Yanjun
    Metallurgical Analysis. 2026, 46(1): 107-113. https://doi.org/10.13228/j.boyuan.issn1000-7571.013179
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    In order to ensure the stability of results of nanoscale length measurement obtained with scanning electron microscope(SEM) and transmission electron microscope(TEM) in scientific research laboratories,a universal quality control sample for two types of electron microscopes was developed.The sample is not only suitable for the high magnification length calibration of SEM,but also suitable for the medium magnification length calibration of TEM.In this paper,the development process of quality control sample was introduced in detail,including the substrate selection and periodic structure fabrication.Wherein the structure fabrication was achieved with focused ion beam(FIB) instrument,which could fabricate the target sample with positive or negative structures in nanoscale.Subsequently,the target sample was loaded into SEM and TEM for imaging tests.To address the issue of insufficient contrast in TEM imaging,the structural parameters were continuously optimized.Finally,the uniformity and stability tests of the developed sample were conducted,and the results indicated that the quality control sample could meet the requirements of flexible usage in scientific research laboratories.
  • Research on deep learning recognition method for focused ion beam-based chip defect detection images
    LIU Hongxuan, CAO Zhenfeng, SUN Wei, QIU Tingting, WANG Xianhao ZHANG Xiaohui, YANG Minglai, WANG Ying
    Metallurgical Analysis. 2026, 46(1): 114-121. https://doi.org/10.13228/j.boyuan.issn1000-7571.013160
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    As the chip structures continue to scale down,the surface defects generated during focused ion beam(FIB) sample preparation significantly affect the subsequent cross-section exposure and failure analysis results.However,the traditional manual evaluation of scanning electron microscope(SEM) images is increasingly unable to meet the efficiency and stability required by current sample preparation workflows.To address this issue,this study constructed an SEM image dataset covering 15 typical FIB-related defects and proposed a lightweight YOLOv5s-based deep learning detection method,which enabled the high-precision identification of defects under weak contrast,small target size,and complex texture backgrounds.Combined with batch detection and comma-separated value(CSV) based structured output modules,the system could automatically generate the defect categories and statistical summaries,which provided data-driven support for quality assessment and process monitoring.The experimental results demonstrated that the proposed method achieved good detection performance,robustness,and engineering applicability,which could effectively improve the automation and standardization of FIB sample quality inspection,thus offering a feasible approach for the intelligentization of microscopy analysis workflows.
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