High-Resolution Transmission Electron Microscopic Study of Various Borides Precipitated in Superalloys

doi:10.11900/0412.1961.2018.00342

Acta Metall Sin

2018, Vol. 54

Issue (11): 1503-1524 DOI: 10.11900/0412.1961.2018.00342

Microstructures

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High-Resolution Transmission Electron Microscopic Study of Various Borides Precipitated in Superalloys

Xiuliang MA(

), Xiaobing HU

Institute of Metal Research, Chinese Academy of Sciences, Shenyang 110016, China

Cite this article:

Xiuliang MA, Xiaobing HU. High-Resolution Transmission Electron Microscopic Study of Various Borides Precipitated in Superalloys. Acta Metall Sin, 2018, 54(11): 1503-1524.

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Abstract

Microelement B is widely added into almost all commercial superalloys because B contributes to strengthening grain boundaries at high temperature during service. Generally, B is present in two different forms. Besides the solute state in matrix, B tends to react with transition elements at high temperatures, giving rise to various borides including M₂B, M₃B₂ and M₅B₃ phases. An accurate knowledge of the microstructural characterizations of these borides is of great importance for a better understanding of the structure-property relationship and designing materials with improved properties. By means of various advanced techniques based on the aberration-corrected transmission electron microscopy (TEM), microstructural features of above borides have been systematically investigated. Various defect features which were controversial in the past have been clarified. In this paper, after a brief review on the studies of borides, the atomic-scale information on the microstructural features has been presented. Finally, some prospects for future studies have been proposed.

Key words: superalloy boride crystallographic feature polyhedral stacking transmission electron microscopy

Received: 23 July 2018

ZTFLH:

TG146.1

Fund: Supported by National Basic Research Program of China (Nos.2009CB623705 and 2010CB631206) and National Natural Science Foundation of China (No.11327901)

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https://www.ams.org.cn/EN/10.11900/0412.1961.2018.00342 OR https://www.ams.org.cn/EN/Y2018/V54/I11/1503

Table 1 Crystallographic data of W₂B, V₃B₂ and Cr₅B₃ phase^[32]

Fig.1 Structural configurations of M₃B₂ (a), M₅B₃ (b) and M₂B (c) (The basic polyhedral unit of trigonal prisms and anti-square prisms for each structure are shadowed)^[32]

Table 2 Crystallographic data of C16-, C_b- and C_a-Cr₂B phases^[33]

Fig.2 Pictorial diagram of square anti-prism (a), structural projection along fourfold axis (b) and twofold axis (c)

Fig.3 Schematic diagram showing the directional equivalence among C16-, C_b-, and C_a-Cr₂B in the conjunct plane of (110)_C₁₆,

(100) C b

and

(001) C a

(a), the structural projection of orthorhombic C_b-M₂B along

[011] C b

(b) and

[01 1 ?] C b

(c), tetragonal C16-Cr₂B along [001]_C₁₆ (d), and hexagonal C_a-Cr₂B along

[110] C a

(e),

[100] C a

(f) and

[010] C a

(g) directions showing the polyhedral configuration in each structure^[33]

Fig.4 Structural projection along

[100] C a

for C_a-Cr₂B (a) and the corresponding simplified description (b), structural simplification of [001]_C₁₆ (c),

[1 1 ? 1] C 16

(d),

[001] C b

(e),

[011] C b

(f) and [001]_N₂ (g) (The atomic fractional coordinates along the projected direction, and characteristic projected lengths for the basic structure units of A, A, B and B are indicated. The indicated a_o and b_o direction in Fig.4c is based on the basic unified orthorhombic lattice. The denoted 2d, 3d, 4d, 6d represent the periods along the stacking direction of a_o for C16-, C_b-, C_a- and N2-Cr₂B structure respectively, in which d is the lattice length of a_o. The denoted layer α₁, α₂, β₁, β₂ in Fig.4g represents four different stacking layers)^[33]

Fig.5 Structural derivation for the polytypic Cr₂B (N represents the number of stacking layers)^[33]

Fig.6 Dark (a) and bright (b) field TEM images showing the M₂B precipitates within the matrix (γ /γ’)

Fig.7 A series of electron diffraction patterns (EDPs) of a M₂B-type boride obtained by large-angle tilting with [001] (a), [102] (b), [101] (c), [100] (d), [113] (e), [111] (f), [110] (g) and [210] (h) zone axis (A C16-type M₂B with the space group of I4/mcm is determined according to the EDPs. The square-framed diffraction spots are proposed to result from double-diffraction)^[31]

Fig.8 A series of EDPs of a M₂B-type boride obtained by large-angle tilting with [100] (a), [101] (b), [103] (c), [001] (d), [310] (e), [110] (f), [010] (g), [011] (h) and [013] (i) zone axis (A C_b-type M₂B with the space group of Fddd is determined according to the EDPs. The square-framed diffraction spots are proposed to result from double-diffraction)^[31]

Fig.9 EDPs (a~c) obtained from highly defected regions within M₂B, schematics of the EDPs for C16 along

[001] C 16

(d) and

[1 1 ? 1] C 16

(e), and C_b along

[001] C b

(f) and

[011] C b

(g)

Fig.10 HAADF image (a), STEM-EDX spectrum (b) and TEM-EELS (c) showing the grain interior precipitation and chemical features of the lath-like M₂B-type boride

Fig.11 Schematic showing the crystallographic relationship of various orientations within (110)_C₁₆ and

(100) C b

(a), and schematics showing the distribution of reflections along

[010] C b

(b) and

[1 1 ? 3] C 16

(c), respectively

Fig.12 Dark field TEM image showing the 60° rotation twin within a M₂B grain (a), EDPs corresponding to area I can be indexed as [001]_C₁₆ (b),

[1 1 ? 3] C 16

[1 1 ? 1] C 16

(d) zone-axis, respectively. EDPs obtained from area II with the same tilt angles as Figs.12b~d corresponding to

[1 1 ? 1] C 16

(e),

[1 1 ? 0] C 16

(f) and

[1 1 ? 1 ?] C 16

(g) zone-axis, respectively^[31]

Fig.13 HRTEM image of a C16 structure including stacking fault along [001]_C₁₆ direction (a) and magnified image of rectangle in Fig.13a (b)^[31]

Fig.14 HRTEM image of a C16 structure including stacking fault along

[1 1 ? 0] C 16

direction (a) and magnified image of rectangle in Fig.14a (b)^[31]

Fig.15 HRTEM image taken along

[013] C b

direction showing details of a 60° rotation twin in C_b structure (a),

< 011 > C b

lattice image taken from the same area as in Fig.15a but with a 30° tilting angle along

[001] C b

direction (b),

[001] C b

HRTEM image of C_b structure with stacking fault indicated by the arrow (c) (The oblique lines in Figs.15a and c correspond to

(101) C b

and

(110) C b

, respectively)^[31]

Fig.16 Atomic resolution HAADF images (a~d) showing various kinds of structural intergrowth in M₂B-type boride^[33]

Fig.17 Atomic resolution HAADF image showing the long period stacking order (LPSO) structure with the uncertain period number of 6 or 12 or 18 or even bigger^[33]

Fig.18 A series of EDPs of a M₃B₂-type boride obtained by large-angle tilting with [001] (a), [101] (b), [201] (c), [100] (d), [112] (e), [111] (f), [110] (g) and [210] (h) zone axes

Fig.19 TEM bright filed image showing the M₃B₂ precipitates in grain interior (a) and EDX spectrum corresponding to M₃B₂ (b)

Fig.20 Atomic resolution HAADF images along [001] (a), [100] (b) and [110] (c) showing the ordered occupation of metal atoms M in M₃B₂ phase. Atomic configuration in the unit cell of the ordered M₃B₂ phase (d) and the corresponding projection along [001] (e), [100] (f), and [110] (g) showing the structural features of the ordered structure (The blue balls designated by L represent large metal atoms such as W and Mo. The green balls designated by S represent small metal atoms such as Cr, Co. The B atoms are indicates by red balls)^[32]

Fig.21 Direct determination of the chemical ordering within M₃B₂-type borides using element maps of Cr-K (a), Co-K (b), Ni-K (c), W-M (d), Mo-L (e), and composite map using Cr-K and W-M (f) edges^[35]

Fig.22 HRTEM image along [110] direction showing the planar defect in M₃B₂

Fig.23 Local intergrowth of polyhedral layer within M₃B₂ boride^[32]

Fig.24 A series of EDPs of a M₅B₃-type boride obtained by large-angle tilting with [001] (a), [101] (b), [301] (c), [100] (d), [111] (e), [221] (f), [110] (g), and [210] (h) zone axes (The square-framed reflections are resulted from double-diffraction)

Fig.25 BF-STEM image (a) and EDX spectrum (b) showing the grain interior precipitation and chemical composition of M₅B₃-type boride

Fig.26 Atomic resolution HAADF images taken along [001] (a), [100] (b) and [110] (c) direction showing the ordered occupation of metal atoms M in M₅B₃ phase. Atomic configuration in the unit cell of the ordered M₅B₃ phase (d) and the corresponding projection along [001] (e), [100] (f) and [110] (g) showing the structural features of the ordered structure (The blue balls designated by L represent large metal atoms such as W and Mo. The green balls designated by S represent small metal atoms such as Cr, Co. The B atoms are indicates by red balls)^[32]

Fig.27 Element maps using Cr-K (a), Co-K (b), Ni-K (c), W-M (d), Mo-L (e), and composite map using Cr-K and W-M (f) showing the chemical ordering within M₅B₃-type boride^[35]

Fig.28 HRTEM image along [110] direction showing the planar defect within M₅B₃ phase (The top right inset is a FFT image)

Fig.29 Atomic resolution HAADF images along [110] (a), and [100] (b) zone axes showing the local intergrowth of polyhedral layer within M₅B₃ boride^[32]

Fig.30 Low magnification HAADF image (a), the corresponding composite EDPs (b) and atomic resolution HAADF image (c) showing the large scale intergrowth between M₃B₂and M₅B₃ boride

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