Application of BIB polishing technology in cross-section preparation of porous, layered and powder materials: A review

doi:10.1007/s11706-019-0457-0

Front. Mater. Sci.

2019, Vol. 13

Issue (2) : 107-125 https://doi.org/10.1007/s11706-019-0457-0

REVIEW ARTICLE

Application of BIB polishing technology in cross-section preparation of porous, layered and powder materials: A review

Rongrong JIANG¹, Ming LI^1,², Yirong YAO¹, Jianmin GUAN¹, Huanming LU¹(

)

¹. Test Center, Ningbo Institute of Materials Technology and Engineering, Chinese Academy of Sciences, Ningbo 315201, China
². University of Chinese Academy of Sciences, Beijing 100049, China

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Abstract

For the accuracy of experimental results, preparing a high quality polished surface and cross-section of the materials for further analysis using electron backscattered diffraction (EBSD), electron probe microanalysis (EPMA), and scanning probe microscopy (SPM) is extremely important. Broad ion beam (BIB) polishing, a method based on the principle of ion bombardment, has irreplaceable advantages. It makes up for the drawbacks and limitations of traditional polishing methods such as mechanical polishing, electrochemical polishing, and chemical polishing. The ions will not leave the bombardment area during polishing, which makes the BIB method suitable for porous materials. The energy of the ion beam can be adjusted according to the sample to reduce the deformation and strain of the polishing area, especially for fragile, soft, and hard materials. The conditions that need to be controlled during BIB polishing are simple. This paper demonstrated the unique advantages of BIB polishing technology in porous, layered and powder materials characterization through some typical application examples, and guided more researchers to understand and utilize BIB polishing technology in the development of new applications.

Keywords broad ion beam polishing layered material powder cross-section porous material

Corresponding Author(s): Huanming LU

Online First Date: 06 May 2019 Issue Date: 19 June 2019

Cite this article:

Rongrong JIANG,Ming LI,Yirong YAO, et al. Application of BIB polishing technology in cross-section preparation of porous, layered and powder materials: A review[J]. Front. Mater. Sci., 2019, 13(2): 107-125.

URL:

https://academic.hep.com.cn/foms/EN/10.1007/s11706-019-0457-0
https://academic.hep.com.cn/foms/EN/Y2019/V13/I2/107

Tab.1 Comparison of typical beam conditions for FIB milling and conventional BIB thinning (Reproduced with permission from Ref. [²³])

Fig.1 Schematic of general instrument operation. Reproduced with permission from Ref. [¹²].

Fig.2 Schematic illustration of the preparation for smooth cross-section by cross-section polisher. Reproduced with permission from Ref. [¹⁵].

Fig.3 The final shape of the BIB polishing area: (a) diagram of polishing area; (b) typical cross-section performed by BIB. Reproduced with permission from Ref. [²⁴].

Tab.2 Advantages and obtained information by BIB polishing for porous, layered and powder materials

Fig.4 Qualitative and quantitative analysis of nanopore morphology observation: (a) secondary electron images showing variations in nanopore morphology; (b) histograms of pore-throat diameters calculated from four capillary-pressure sample. Reproduced with permission from Ref. [¹⁴].

Fig.5 Conventional second electron detector (SE2) microstructural overview of pores. Reproduced with permission from Ref. [⁴⁰].

Fig.6 Comparison of pore dimensions for each analyzed sample. Reproduced with permission from Ref. [²⁹].

Fig.7 BIB serial cross-sectioning experiment: (a) fabric and porosity 3D-model; (b) series of BSE micrographs from top view after the five successive cross-sections. Reproduced with permission from Ref. [²⁴].

Fig.8 Conceptual view of double cross-sectioning in grain boundary. Reproduced with permission from Ref. [³⁴].

Fig.9 Typical grain boundary microstructures from single BIB cross-sections at room temperature: (a) straight and gently curved grain boundaries (H_nH_n) with void inclusions (H_nVH_n); (b) solid inclusions located initially prefer steps in grain–grain interfaces (H_f(h)H_f); (c) trapezoid-shaped second phase inclusions; (d) internal edges of voids are usually coated with fine-grained halite aggregates. Reproduced with permission from Ref. [³⁴].

Fig.10 Sublimation test after BIB cross-sectioning at cryo-temperature: (a) after BIB milling and before sublimation; (b) after sublimation of the same region shown in (a). Reproduced with permission from Ref. [³⁹].

Fig.11 Schematic drawing of the technical BIB-cryo-SEM principle: (a) the sample mount on a stub; (b) the system is in milling position; (c) for serial cross-sectioning. Reproduced with permission from Ref. [³⁹].

Fig.12 Cross-section polished hierarchical material: (a) where the silica walls are thick; (b) where the silica walls are thin; (c) a defect in the shape of a missing PS sphere during synthesis; (d) an unpolished sample displaying defects in the form of connected silica rings. Reproduced with permission from Ref. [⁴⁴].

Fig.13 SEM images of the surface and the vertical cross-section of specimens anodized in different concentrations of 1.0 mol·L⁻¹ NH₄NO₃/EG solution containing (a) 1.0 vol.%, (b) 5.0 vol.%, and (c) 15 vol.% H₂O for 360 min. Reproduced with permission from Ref. [⁴³].

Fig.14 Sn inverse pole figure orientation maps of the bumps in test samples: (a)(b)(c)(d) test sample 5; (e)(f)(g)(h) test sample 2; (i)(j)(k)(l) test sample 4. Reproduced with permission from Ref. [⁵⁴].

Fig.15 Backscattered electron images, concentration mappings of Zn and concentration profiles of Au, Si, O and Zn obtained from line scan on the gray horizontal lines across the interface: (a) Bio Herador SG joint with peroxidation; (b) Bio Herador SG joint without peroxidation. Reproduced with permission from Ref. [⁵⁸].

Fig.16 Morphology of multilayered materials: (a) cross-section micrograph of composite polyacrylonitrile (PAN) support poly(1-trimethylsilyl-1-propyne) (PTMSP)–silica membranes; (b) cross-section micrograph of composite polyvinylidenefluoride (PVDF) support PTMSP–silica membranes; (c) SEM image of the cross-section of the membrane by mechanically broken; (d) SEM image of the cross-section of the membrane prepared by BIB. Reproduced with permission from Ref. [⁶³,⁶⁵].

Fig.17 Crack pattern and morphology obtained after 200, 400, and 800 thermal cycles for samples with a large thermally grown oxide irregularity. Reproduced with permission from Ref. [⁸⁸].

Fig.18 Protective BIB polishing: (a) schematic of protective BIB milling; (b) ion milled area, the zoomed in microscope image shows the milled area over three phases. Reproduced with permission from Ref. [⁸⁴].

Fig.19 AFM indentation results: (a) the topography, adhesion, and modulus maps over the same area on a polymethyl methacrylate (PMMA)/silica sample; (b) a group of typical scan lines of topography, adhesion, and modulus. Reproduced with permission from Ref. [⁸⁴].

Fig.20 The EDS mapping of cross-sectional Si–C composites: (a) cross-sectional FE-SEM image of type A; (b) cross-sectional FE-SEM image of type B; (c) C element EDS mapping in type A; (d) C element EDS mapping in type B; (e) Si element EDS mapping in type A; (f) Si element EDS mapping in type B. Reproduced with permission from Ref. [⁸⁹].

Fig.21 SEM images of powder cross-sections of the LiNi_0.88Co_0.09Mn_0.03O₂ cathode after 1, 100, 200, and 300 cycles in full cells: (a)(b)(c)(d) low-magnification; (e)(f)(g)(h) high-magnification. Reproduced with permission from Ref. [⁹²].

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