A Quantitative and Statistical Method of γ' Precipitates in Superalloy Based on the High-Throughput Field Emission Scanning Eelectron Microscope

doi:10.11900/0412.1961.2021.00376

Acta Metall Sin

2023, Vol. 59

Issue (7): 841-854 DOI: 10.11900/0412.1961.2021.00376

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A Quantitative and Statistical Method of γ' Precipitates in Superalloy Based on the High-Throughput Field Emission Scanning Eelectron Microscope

LU Yuhua¹^,², WANG Haizhou¹^,²(

), LI Dongling¹^,², FU Rui³, LI Fulin³, SHI Hui¹^,²

¹Beijing Advanced Innovation Center for Materials Genome Engineering, Central Iron and Steel Research Institute, Beijing 100081, China
²Beijing Key Laboratory of Metal Materials Characterization, NCS Testing Technology Co., Ltd., Beijing 100081, China
³High Temperature Material Research Institute, Center Iron and Steel Research Institute, Beijing 100081, China

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LU Yuhua, WANG Haizhou, LI Dongling, FU Rui, LI Fulin, SHI Hui. A Quantitative and Statistical Method of γ' Precipitates in Superalloy Based on the High-Throughput Field Emission Scanning Eelectron Microscope. Acta Metall Sin, 2023, 59(7): 841-854.

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Abstract

Superalloys are used widely in national defense, energy, maritime, aviation, and other vital areas requiring stable and reliable materials owing to their excellent oxidation and heat corrosion resistance, high-temperature strength, good fatigue performance, and fracture toughness. The presence of a coherent gamma prime (γ') precipitate is the main factor affecting the high-temperature mechanical properties. Therefore, obtaining the quantitative and statistical γ' precipitate data is indispensable for examining and developing new superalloys. On the other hand, conventional instruments and methods barely achieve this goal. In this study, high-throughput field emission scanning electron microscope (high-throughput SEM) was introduced because of its high-speed imaging and original position visualization. Based on the high-throughput SEM, an innovative deformation GH4096 superalloy prepared at five different solution cooling rates were used as an object to establish a quantitative and statistical method for characterizing the primary, secondary, and tertiary γ' precipitates. Many images of γ' precipitates with magnifications of ×57000 and ×3000 were obtained rapidly, and methodologies for recognizing the γ' precipitates were developed using MIPAR software. Matrices of images of different amounts were formed. Through these methodologies, information on these matrices was obtained, including the ratio of the primary γ' precipitates area fractions between images with magnifications of ×57000 and ×3000. The ratio between the amounts of secondary and tertiary γ' precipitates and the area fraction of the secondary and tertiary γ' precipitates varied with the number of images investigated, respectively. By comparing the tendencies of these three results, the minimum field of view that could represent the actual distribution of γ' precipitates was set to a matrix of 13 × 13 images with a magnification of ×57000 and a pixels square of 2048 × 2048. Considering the consistency between the results of the standardized small-angle X-ray scattering (SAXS) and γ' precipitates in the 13 × 13 images, the established method was quantitative in characterizing the primary, secondary, and tertiary γ' precipitates of GH4096 superalloy. The results of the samples with five different solution cooling rates showed that the solution cooling rates strongly influenced the morphology and quantitative results of the γ' precipitates. Moreover, the behavior of the precipitates corresponded to the classical nucleation growth mechanism and Ostwald Ripening. The solution cooling rates influenced the tensile strength of the samples. The samples exhibited excellent tensile strengths at relatively faster cooling rates, more secondary γ' precipitates, and a higher total area fraction of secondary and tertiary γ' precipitates. Overall, a GH4096 superalloy was prepared using the established method. The statistical and quantitative results of the γ' precipitates highlight a novel way of studying the impact of the solution cooling process on γ' precipitates that can predict the performance of GH4096 superalloys.

Key words: GH4096 superalloy nanoparticle γ' precipitate high-throughput field emission SEM image analysis characterization region

Received: 07 September 2021

ZTFLH:

TG146.1

Fund: National Key Research and Development Program of China(2016YFB0701401)

Corresponding Authors: WANG Haizhou, professor, Tel: (010)62181950, E-mail: wanghaizhou@ncschina.com

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	LU Yuhua
	WANG Haizhou
	LI Dongling
	FU Rui
	LI Fulin
	SHI Hui

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https://www.ams.org.cn/EN/10.11900/0412.1961.2021.00376 OR https://www.ams.org.cn/EN/Y2023/V59/I7/841

Fig.1 Main procedures on building the Recipe-1 for characterizing primary γ' precipitates in SEM images with magnification of 3000

Fig.2 Original SEM images with a magnification of 3000, in which the black particles were primary γ' precipitates (a-c) and corresponding pseudo-colorized images by Recipe-1 according to the diameter of primary γ' precipitates (d-f) in sample CR-1

Table 1 Statistical area fractions of primary γ' precipitates in 5 pseudo-colorized images with magnification of 3000 in samples CR-1-CR-5

Fig.3 Main procedures on building the Recipe-2 for characterizing primary, secondary, and tertiary γ' precipitates in SEM images with magnification of 57000

Fig.4 Original SEM images with a magnification of 57000 (a-e) and corresponding pseudo-colorized images by Recipe-2 according to the diameter of secondary and tertiary γ' precipitates (f-j) and primary γ' precipitates (k-o) for samples CR-1 (a, f, k), CR-2 (b, g, l), CR-3 (c, h, m), CR-4 (d, i, n), and CR-5 (e, j, o)

Fig.5 Stitched image by 484 original SEM images with magnification of 57000 of sample CR-1 (The scanning matrix of images was 22 × 22)

Table 2 Statistical area fractions of primary γ' precipitates in a series of different amounts of pseudo-colorized images with magnification of 57000 in samples CR-1-CR-5

Fig.6 Tendency of primary γ' precipitates area fractions ratio between images with magnification of 57000 and 3000 in all samples varied with the amount of image

Fig.7 Tendencies of the amount of secondary (a) and tertiary (b) γ' precipitates with magnification of 57000 in samples CR-1-CR-5 varied with the amount of image

Fig.8 Tendencies of the ratio between the amounts of secondary and tertiary γ' precipitates with magnification of 57000 in all samples varied with the investigated amount of image

Table 3 Statistical area fractions of secondary γ' precipitates in a series of different amounts of pseudo-colorized images with magnification of 57000 in samples CR-1-CR-5

Table 4 Statistical area fractions of tertiary γ' precipitates in a series of different amounts of pseudo-colorized images with magnification of 57000 in samples CR-1-CR-5

Fig.9 Original SEM image of CR-4 (a) and corresponding pseudo-colored recognitions only colored by Recipe-2 (b), and colored by Recipe-2 and manual work (c)

Fig.10 Comparisons of total amount (a), average diameter (b), and the median diameter (c) of secondary and tertiary γ' precipitates in 169 images with magnification of 57000 in samples CR-4 between Recipe-2 and Recipe-2 & manual, two ways to recognized γ' precipitates

Fig.11 Comparisons of mass fraction of γ' precipitates by using electrochemical extraction method & small-angle X-ray scattering (SAXS) (a, c, e, g, i) and area fraction of γ' precipitates by using the way in this work (b, d, f, h, j) in samples CR-1 (a, b), CR-2 (c, d), CR-3 (e, f), CR-4 (g, h), and CR-5 (i, j)

Fig.12 Mechanical properties of samples CR-1-CR-5 tensiled at 400^oC (R_m—tensile strength, R_p0.2—yield strength (plastic deformation at 0.2%))

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