Please wait a minute...
Acta Metall Sin  2024, Vol. 60 Issue (8): 1109-1118    DOI: 10.11900/0412.1961.2024.00062
Research paper Current Issue | Archive | Adv Search |
Morphology and Chemical Composition of Nanoprecipitate in AerMet100 Steel by Separation of the Nuclear and Magnetic Small-Angle Neutron Scattering Data
KE Yubin1,2(), LI Bin3, DUAN Huiping3()
1 Spallation Neutron Source Science Center, Dongguan 523803, China
2 Institute of High Energy Physics, Chinese Academy of Sciences, Beijing 100049, China
3 School of Materials Science and Engineering, Beihang University, Beijing 100191, China
Cite this article: 

KE Yubin, LI Bin, DUAN Huiping. Morphology and Chemical Composition of Nanoprecipitate in AerMet100 Steel by Separation of the Nuclear and Magnetic Small-Angle Neutron Scattering Data. Acta Metall Sin, 2024, 60(8): 1109-1118.

Download:  HTML  PDF(2222KB) 
Export:  BibTeX | EndNote (RIS)      
Abstract  

AerMet100 ultrahigh-strength steel is widely used in aircraft landing gears because of its excellent mechanical properties. Its high strength mainly results from the secondary hardening effect of a large amount of needle-shaped M2C-type precipitates generated during the alloy tempering process. Given the nanoscale size and coherency with the martensitic matrix, the size and composition of the precipitates in the AerMet100 steel are difficult to extract and accurately characterize by using traditional imaging techniques. In this study, the size, distribution, and composition of M2C-type needle-like precipitates in AerMet100 steel tempered for 5 h at 454, 482, 486, and 498oC were quantitatively characterized by combining TEM, XRD, and small-angle neutron scattering (SANS) techniques. By applying a transverse magnetic field of 1.1 T during the SANS experiment and reducing the data along the parallel and perpendicular magnetic field directions, the separation of nuclear and magnetic scattering data was achieved. Model fitting of the nuclear scattering curves revealed an average length of 6-16 nm and an average diameter of 1-2 nm for the needle-like precipitates in the alloy. The volume fraction of the needle-like phase increases with the tempering temperature ranging from 0.54% to 5.19%. Given the nanodomains between the precipitates and matrix phase with spin misalignment, the structural parameters obtained from magnetic scattering data are much bigger than the nuclear ones. Furthermore, by comparing the neutron scattering length densities of the carbides and matrix phases, the possible chemical composition and physical density of the needle-like precipitates within are (Cr0.4Mo1.6)C and 8.55 g/cm3, respectively. This study demonstrates nondestructive quantitative neutron scattering analysis of the nanoscale morphology and chemical composition of nanophases in ferromagnetic alloys.

Key words:  AerMet100 steel      nanoscale precipitate      small-angle neutron scattering      separation of nuclear and magnetic scattering      chemical composition of nanophase     
Received:  01 March 2024     
ZTFLH:  TG142  
Fund: National Key Research and Development Program of China(2021YFB3501201);National Natural Science Foundation of China(12275154);Guangdong Basic and Applied Basic Research Foundation(2021B1515140028);Youth Innovation Promotion Association, CAS(2020010)
Corresponding Authors:  KE Yubin, associate professor, Tel: (0769)88931334, E-mail: keyb@ihep.ac.cnDUAN Huiping, professor, Tel: (010)82339822, E-mail: hpduan@buaa.edu.cn

URL: 

https://www.ams.org.cn/EN/10.11900/0412.1961.2024.00062     OR     https://www.ams.org.cn/EN/Y2024/V60/I8/1109

Fig.1  Transmission curve and Bragg-edge feature of CoNi_454 sample (a), integration and normalization within 10° azimuth angle along the 0° and 90° orientations (b) (Qx, Qy —scattering vector moduli in x and y axes, repectively)
Fig.2  TEM images and SAED patterns (insets) of AerMet100 steel samples tempered at 486oC (a) and 498oC (b) for 5 h (White and black arrows indicate precipitates and reverted austenite films (RAFs), respectively)
Fig.3  XRD spectra of the AerMet100 steel tempered at different temperatures
Fig.4  TEM images and SAED patterns (insets) of the needle-like M2C precipitates in tempered AerMet100 steel along different crystallographic orientations of the matrix phase (White arrows indicate the needle-like precipitates)
(a) 486oC, [001] α (b) 486oC, [011] α (c) 498oC, [001] α (d) 498oC, [011] α
Fig.5  Magnetic hysteresis curves (a) and the 1D SANS scattering curves measured under no field application (5 mT remanence) and 1.1 T magnetic field of AerMet100 steel tempered at different temperatures (b) (SANS—small-angle neutron scattering; Q—scattering vector modulus)
PhaseChemical compositionDensity / (g·cm-3)ρN / (1010 cm-2)ρM / (1010 cm-2)
Martensite lath matrixFe70.92Co13.4Ni11.1Cr3.1Mo1.2C0.23Ti0.057.626.844.43
Reverse austenite filmFe70.92Co13.4Ni11.1Cr3.1Mo1.2C0.23Ti0.057.596.740
Needle-like carbide(Cr x Mo y )CUnknown5.210
Tempered particleFe3Mo3C9.176.52-
Table 1  Chemical compositions, densities and neutron scattering length densities of phases in AerMet100 steel
Fig.6  2D SANS patterns of 498oC-tempered AerMet100 steel under different magnetic field strengths (I—integral intensity)
(a) no field application (5 mT) (b) 50 mT (c) 0.1 T (d) 1.1 T
Fig.7  SANS results of AerMet100 tempered steel under magnetic field application
(a) total SANS 1D scattering data
(b, c) experimental and fitted nuclear (b) and magnetic (c) SANS results
(d) observed ratio between SANS nuclear scattering intensity (IN) and magnetic scattering intensity (IM)
SampleD / nmL / nmRHS / nmfV / %
CoNi_4541.15 ± 0.766.00 ± 1.275.95 ± 1.050.54 ± 0.15
CoNi_4822.02 ± 1.049.63 ± 0.876.68 ± 0.922.47 ± 0.34
CoNi_4862.37 ± 0.7510.6 ± 1.726.75 ± 0.783.25 ± 0.38
CoNi_4982.48 ± 0.9915.9 ± 2.947.07 ± 0.935.19 ± 0.68
Table 2  Fitted structural parameters of nanoprecipitates from the nuclear SANS data of AerMet100 steel
SampleDLRHSt
CoNi_4541.80 ± 0.746.51 ± 0.425.01 ± 0.470
CoNi_4822.46 ± 0.7513.70 ± 1.2418.50 ± 0.412.59 ± 0.47
CoNi_4862.60 ± 0.8613.40 ± 1.5018.00 ± 0.355.56 ± 1.60
CoNi_4982.62 ± 0.4019.07 ± 1.6118.57 ± 0.465.57 ± 1.56
Table 3  Fitted structural parameters of nanodomains from the magnetic SANS data of AerMet100 steel
1 Ayer R, Machmeier P M. Transmission electron microscopy examination of hardening and toughening phenomena in AerMet 100 [J]. Metall. Trans., 1993, 24A: 1943
2 Figueroa D, Robinson M J. Hydrogen transport and embrittlement in 300 M and AerMet100 ultra high strength steels [J]. Corros. Sci., 2010, 52: 1593
3 Oehlert A, Atrens A. Room temperature creep and the initiation of stress corrosion cracking in AerMet 100 [J]. Mater. Forum, 1993, 17: 415
4 Novotny P, McCaffrey T. An advanced alloy for landing gear and aircraft structural applications—Aerometr® 100 Alloy [R]. SAE Technical Paper 922040, 1992, https://doi.org/10.4271/922040
5 Shi X H, Zeng W D, Zhao Q Y, et al. Study on the microstructure and mechanical properties of Aermet 100 steel at the tempering temperature around 482°C [J]. J. Alloys Compd., 2016, 679: 184
6 Duan H, Liu X, Ran X Z, et al. Effect of ordered domains on the fracture toughness of high Co-Ni secondary hardening steel [J]. Mater. Sci. Eng., 2017, A704: 32
7 Zhang Y P, Zhan D P, Qi X W, et al. Effect of tempering temperature on the microstructure and properties of ultrahigh-strength stainless steel [J]. J. Mater. Sci. Technol., 2019, 35: 1240
doi: 10.1016/j.jmst.2019.01.009
8 Zhong P. Microstructure and mechanical properties in isothermal tempering of high Co-Ni secondary hardening ultrahigh strength steel [J]. J. Iron Steel Res. Int., 2007, 14: 292
9 Xue C P, Zhang Y X, Wang S, et al. Achieving highest Young's modulus in Al-Li by tracing the size and bonding evolution of Li-rich precipitates [J]. J. Mater. Sci. Technol., 2023, 145: 125
doi: 10.1016/j.jmst.2022.10.052
10 He S M, van Dijk N H, Paladugu M, et al. In situ determination of aging precipitation in deformed Fe-Cu and Fe-Cu-B-N alloys by time-resolved small-angle neutron scattering [J]. Phys. Rev., 2010, 82B: 174111
11 Wang W J, Gong D L, Wang H L, et al. Spinodal decomposition coupled with a continuous crystal ordering in a titanium alloy [J]. Acta Mater., 2022, 233: 117969
12 Staron P, Jamnig B, Leitner H, et al. Small-angle neutron scattering analysis of the precipitation behaviour in a maraging steel [J]. J. Appl. Cryst., 2003, 36: 415
13 Yan S B, Wang Z J, Li T F, et al. In situ characterization of 17-4PH stainless steel by small-angle neutron scattering [J]. Materials, 2023, 16: 5583
14 Rogozhkin S V, Klauz A V, Ke Y B, et al. Study of precipitates in oxide dispersion-strengthened steels by SANS, TEM, and APT [J]. Nanomaterials, 2024, 14: 194
15 Yuan Y, Yuan S, Wang Y F, et al. Nanostructure, mechanical properties, and corrosion resistance of super duplex stainless steel 2507 aged at 500oC [J]. Crystals, 2023, 13: 243
16 Ge J C, Gu Y, Yao Z Z, et al. Evolution of medium-range order and its correlation with magnetic nanodomains in Fe-Dy-B-Nb bulk metallic glasses [J]. J. Mater. Sci. Technol., 2024, 176: 224
doi: 10.1016/j.jmst.2023.07.066
17 Lifshitz I M, Slyozov V V. The kinetics of precipitation from supersaturated solid solutions [J]. J. Phys. Chem. Solids, 1961, 19: 35
18 Große M, Gokhman A, Böhmert J. Dependence of the ratio between magnetic and nuclear small angle neutron scattering on the size of the heterogeneities [J]. Nucl. Instrum. Methods Phys. Res., 2000, 160B: 515
19 Ke Y B, He C Y, Zheng H B, et al. The time-of-flight small-angle neutron spectrometer at China spallation neutron source [J]. Neutron News, 2018, 29: 14
20 Griffith W L, Triolo R, Compere A L. Analytical scattering function of a polydisperse Percus-Yevick fluid with Schulz- (Γ-) distributed diameters [J]. Phys. Rev., 1987, 35A: 2200
21 Beaucage G. Approximations leading to a unified exponential/power-law approach to small-angle scattering [J]. J. Appl. Cryst., 1995, 28: 717
22 Beaucage G. Small-angle scattering from polymeric mass fractals of arbitrary mass-fractal dimension [J]. J. Appl. Cryst., 1996, 29: 134
23 Feigin L A, Svergun D I. Structure Analysis by Small-Angle X-Ray and Neutron Scattering [M]. New York: Springer, 1987: 224
24 Pedersen J S. Analysis of small-angle scattering data from colloids and polymer solutions: modeling and least-squares fitting [J]. Adv. Colloid Interface Sci., 1997, 70: 171
25 Goll D. Micromagnetism-microstructure relations and the hysteresis Loop [A]. Handbook of Magnetism and Advanced Magnetic Materials [M]. Hoboken: Wiley InterScience, 2007: 1023
26 Vivas L G, Yanes R, Berkov D, et al. Toward understanding complex spin textures in nanoparticles by magnetic neutron scattering [J]. Phys. Rev. Lett., 2020, 125: 117201
27 Mühlbauer S, Honecker D, Périgo É A, et al. Magnetic small-angle neutron scattering [J]. Rev. Mod. Phys., 2019, 91: 015004
28 Leitner H, Staron P, Clemens H, et al. Analysis of the precipitation behaviour in a high-speed steel by means of small-angle neutron scattering [J]. Mater. Sci. Eng., 2005, A398: 323
29 Han Y S, Mao X D, Jang J, et al. Characterization of nano-sized oxides in Fe-12Cr oxide-dispersion-strengthened ferritic steel using small-angle neutron scattering [J]. Appl. Phys., 2015, 119A: 249
[1] LI Yawei, XIE Guang, KE Yubin, LU Yuzhang, HUANG Yaqi, ZHANG Jian. In Situ Small-Angle Neutron Scattering Study of Precipitation and Evolution Behavior of Secondary Phases in Ni-Based Superalloys[J]. 金属学报, 2024, 60(8): 1100-1108.
No Suggested Reading articles found!