Material Science & Engineering A 736 (2018) 76-86

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Material Science & Engineering A

jurnal homepage: www.elsevier.com/locate/msea

E ff dll penuaan jangka panjang pada struktur mikro, sifat stres pecah dan mekanisme deformasi
dasar superalloy cor nikel baru

Meiqiong Ou Sebuah . Yingche Ma Sebuah . • . Hualong Ge b . c . bo Chen Sebuah . Shijian Zheng b . Kui Liu Sebuah . •
Sebuah Institute of Logam Penelitian, Chinese Academy of Sciences, Shenyang 110.016, Cina
b Shenyang National Laboratory untuk Materials Science, Institut Logam Penelitian, Chinese Academy of Sciences, Shenyang 110.016, Cina
c Sekolah Ilmu dan Teknik Material, Universitas Sains dan Teknologi Cina, Hefei 230.026, Cina

ARTICLEINFO ABSTRAK

Kata kunci: Mikro, sifat stres pecah dan mekanisme deformasi paduan baru selama penuaan jangka panjang diselidiki. Mikro evolusi terutama termasuk
Nikel superalloy berbasis penuaan pengkasaran dari γ ' fase dan pengendapan η tahap. Selama penuaan pada 700 ° C, 750 ° C dan 800 ° C, tingkat pengasaran k dari γ ' fase
jangka panjang adalah tentang
γ ' tahap
7,818 nm 3 / h, 42,927 nm 3 / h dan 178,226 nm 3 / h, masing-masing. Energi aktivasi Q untuk γ ' pengasaran adalah sekitar 279,98 kJ / mol, yang berarti
η fase
bahwa elemen di ff usion menguasai pengkasaran γ ' tahap. Setelah penuaan pada 750 ° C selama 3000 jam dan 800 ° C untuk tahun 2000 h, baru
Dislokasi
seperti jarum η fase diendapkan dekat GBS dan sekitar karbida MC, kemudian tumbuh menjadi interior gandum. Kuantitas η fase meningkat dengan
sifat stres pecah
meningkatnya waktu penuaan. Dengan pertumbuhan η tahap, γ ' zona habis ditemukan di sekitar η tahap. Hal ini terutama karena kedua γ '

fasa dan η fase yang diperkaya dengan Ni dan Ti, dan tumbuh dari η fase diserap γ ' tahap. Setelah penuaan pada 700 ° C selama 300 - 3000 h dan
750 ° C selama 300 - 2000 h, kehidupan pecah stres pada 750 ° C / 430MPa tetap pada tingkat tinggi dan kebanyakan dari mereka lebih tinggi dari 100
h. Itu karena sedikit dewasa γ ' fase bertindak rintangan yang kuat untuk gerakan dislokasi, Orowan bypassing menyisir susun geser kesalahan
bertindak sebagai mekanisme yang dominan selama deformasi stres pecah. Setelah penuaan pada 750 ° C dan 800 ° C selama 3000 jam, kehidupan
stres pecah menurun menjadi 45,7 jam dan 7,68 jam, masing-masing. Salah satu alasannya adalah bahwa serius dewasa γ ' fase itu sangat sulit untuk
menghambat gerak dislokasi, hampir semua γ ' fase dipotong oleh dislokasi dengan meninggalkan kesalahan susun di dalamnya selama deformasi
stres pecah. Alasan lain adalah bahwa seperti jarum η fase dipromosikan dislokasi tumpukan-up dan berkontribusi pada nukleasi mikro-retak,
sedangkan γ ' zona habis bisa menjadi konduktif untuk penyebaran mikro-retak.

1. Perkenalan untuk menjaga sifat mekanik yang baik selama jangka panjang layanan [9 - 11] . Karena banyak unsur
paduan seperti Al, Ti, Nb Cr, W, Mo dan Co dll ditambahkan ke dalam superalloy dasar nikel,
superalloy dasar nikel adalah bahan yang paling penting bagi banyak aplikasi suhu tinggi karena beberapa tahapan yang tidak diinginkan yang mungkin akan diendapkan selama jangka
sifat mekanik yang baik mereka, korosi dan ketahanan oksidasi pada suhu tinggi panjang-penuaan pada suhu tinggi [12 - 14] . Pembentukan fase yang tidak diinginkan seperti σ, η,

[1 - 3] . Mikro superalloy dasar nikel terutama terdiri dari teratur wajah berpusat kubik γ matriks dan
koheren diendapkan L1 2- struktur γ ' tahap. Sifat unik dari paduan ini sangat terkait dengan
memerintahkan γ ' fase karena gerakan dislokasi dapat terhalang oleh γ ' fase selama deformasi plastik
[4 - 7] . Baru-baru ini, basis superalloy cor nikel baru terutama diperkuat oleh γ ' tahap [8] dikembangkan
untuk aplikasi aero-mesin karena sifat mekanik yang sangat baik pada suhu sampai 750 ° C.
dan δ fase selalu menyebabkan perubahan komposisi lokal dan menyebabkan degradasi sifat
mekanik [15 - 17] . Selain kemungkinan pembentukan fase yang tidak diinginkan, jangka panjang
penuaan juga di fl uences ukuran, bentuk dan volume fraksi γ ' tahap. Itu γ ' ukuran memiliki signi fi tidak
bisa e ff dll pada mekanisme deformasi superalloy dasar nikel. Fu et al. [18] telah melaporkan bahwa
perubahan mekanisme deformasi dari batas anti-fase (APB) geser ke susun kesalahan geser ke
Orowan melewati di dasar nikel superalloy kaya Co sebagai peningkatan γ '

ukuran. Transisi dari mekanisme deformasi juga ditemukan dalam paduan Nimonic [19] dan paduan
Stabilitas mikrostruktur superalloy dasar nikel penting TMW [20] . Itu γ' ukuran superalloy dasar nikel

• penulis yang sesuai.

Alamat email: ycma@imr.ac.cn (Y. Ma), kliu@imr.ac.cn (K. Liu).

https://doi.org/10.1016/j.msea.2018.08.096
Menerima 6 Juli 2018; Diterima dalam bentuk direvisi 25 Agustus 2018; Diterima Agustus 2018 27
Tersedia online 29 Agustus 2018
0921-5093 / © 2018 Diterbitkan oleh Elsevier
M. Ou et al.
umumnya meningkat dengan waktu penuaan jangka panjang [21 - 23] . Oleh karena itu, eksperimen yang
diinginkan secara sistematis menyelidiki di fl pengaruh dari γ '
Ukuran pada mekanisme deformasi paduan baru selama penuaan jangka panjang. Selain evolusi γ ' tahap,
η fase ditemukan pada paduan baru setelah penuaan jangka panjang [8] . Hingga saat ini, ada sedikit
literatur menyajikan karakteristik distribusi elemen paduan di η
fase melalui pengamatan eksperimental dan karakterisasi. Dalam tulisan ini, unsur-unsur paduan
utama η fasa dan γ ' fase akan mengidentifikasikan fi ed jelas dengan menggunakan TEM / EDS. Selain
itu, di fl pengaruh evolusi mikro selama proses penuaan jangka panjang pada sifat stres pecahnya
alloy baru dipelajari. Setelah deformasi stres pecah, dislokasi con fi gurations diamati, dan korelasi
antara evolusi struktur mikro dan sifat pecah stres dijelaskan.
2. Bahan-bahan dan metode-metode
Ingot cor paduan baru disiapkan melalui leleh vakum induksi, dan kemudian bar mekanik dicor.
Menurut hasil induktif Ditambah Plasma Atomic Emission Spectrometer (ICP-AES), komposisi kimia
dari paduan baru adalah (wt%) 19.44Cr,
5.06Fe, 4,35 (W + Mo), 4,39 (Ti + Al), 1.58Nb, ​0.12C, 0.006B, dan keseimbangan Ni. Dalam studi ini,
tiga puluh bar disiapkan untuk tes stres pecah, dan enam belas spesimen yang diambil dari bar lain
yang disiapkan untuk pengamatan struktur mikro. Semua bar dan spesimen solusi anil pada 1120 ° C
selama 4 jam dalam pendingin udara dan udara, dan kemudian berusia di 800 ° C selama 20 jam
berikut dengan pendingin udara. Salah satu spesimen adalah fi rstly digunakan untuk pengamatan
struktur mikro. Setelah itu, dua bar dan satu spesimen yang bertindak sebagai sebuah kelompok,
masing-masing kelompok dilakukan perawatan jangka panjang-penuaan pada 700 ° C, 750 ° C atau
800 ° C selama 300 jam, 500 jam, 1000 jam, 2000 h atau 3000 h. setelah di ff jangka panjang erent
perawatan penuaan, semua bar adalah mesin menjadi sampel stres pecah dengan diameter ukuran
dari 5mm dan panjang ukuran 25mm. Dua stres sampel pecah diuji pada 750 ° C dan 430MPa, nilai
rata-rata digunakan untuk menentukan kehidupan stres pecah dan elongasi.
setelah di ff jangka panjang erent perawatan penuaan, mikrostruktur paduan baru dianalisis
dengan mikroskop elektron (SEM). spesimen SEM disiapkan melalui polishing mekanik dan kimia
etsa dalam larutan dengan 20 g CuSO 4, 150ml HCl dan 80ml H 2 O untuk pengamatan SEM umum.
Dalam metode elektrokimia-etsa dengan larutan 13ml H 3 PO 4, 42ml H 2 BEGITU 4 dan HNO 45ml 3, yang
dilucuti γ matriks, dipekerjakan untuk pengamatan γ ' tahap. Untuk meminimalkan kesalahan, dua
ratus partikel dipilih untuk mengukur ukuran γ ' Fase oleh Gambar-Pro software Plus.
Setelah tes stres pecah, semua sampel dipotong menjadi cakram sepanjang arah vertikal dari
stres garis aksial dan menipis ke 50 pM mekanis. Setelah penggilingan, foil TEM yang elektrokimia
menipis dalam larutan 10 vol% HClO 4 dan 90 vol% C 2 H 5 OH di - 20 ° C dan pada tegangan 24 V.
Struktural dan analisis komposisi kimia yang dilakukan pada Tecnai G 2 F30 mikroskop elektron
transmisi (TEM) dilengkapi dengan annular sudut tinggi gelap fi bidang (HAADF) detektor dan dispersi
spektrometer (EDS) sistem energi X-ray. dislokasi con-
fi gurations dihasilkan dari deformasi stres pecah diselidiki oleh Tecnai G 2 F20 TEM.
3. Hasil dan Pembahasan
3.1. mikro awal
Setelah perlakuan panas standar, fase konstituen dari paduan baru termasuk γ matriks, kuning
karbida MC, granular M 23 C 6 karbida dan fi ne bola γ ' fase, seperti yang ditunjukkan pada Gambar. 1 .
Gumpal MC karbida dibagikan secara acak di interior butir atau pada batas butir (GBS), granular M 23 C
6 karbida hanya diendapkan di GBS, dan fi ne bola γ ' fase yang terdistribusi secara merata di γ matriks
dengan jari-jari rata-rata 13,5 nm.
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Material Science & Engineering A 736 (2018) 76-86
3.2. Pengkasaran dari γ ' tahap
Selama penuaan jangka panjang, pengkasaran dari γ ' fase diamati dalam paduan baru. Gambar.
2 menunjukkan evolusi wakil dari γ ' Fase setelah jangka panjang penuaan pada 700 ° C, 750 ° C dan
800 ° C selama 500 jam, 1000 jam dan 3000 jam. Sudah jelas bahwa γ ' fase pada dasarnya terus
morfologi bulat dan terdistribusi secara merata di γ matriks, tetapi γ ' Ukuran meningkat jelas dengan
meningkatnya suhu penuaan dan waktu. setelah di ff jangka panjang erent penuaan perawatan, jari-jari
rata-rata γ '
fase untuk semua spesimen diukur dengan software Ditambah Gambar-Pro. Setelah penuaan pada 700
° C, 750 ° C dan 800 ° C selama 300 jam, jari-jari rata-rata γ '
fase adalah sekitar 21,6 nm, 27,8 nm dan 34,1 nm, masing-masing. Dengan penuaan waktu
meningkat menjadi 3000 h, jari-jari rata-rata γ ' fase meningkat menjadi 31,5 nm, 51,6 nm dan 80,5 nm,
masing-masing.
Hal ini juga diketahui bahwa pengkasaran γ ' fase dalam superalloy dasar nikel terjadi melalui
Ostwald proses pematangan, yang di suatu ff proses usioncontrolled [24,25] . di The ff Sifat usion dari
Ostwald pematangan adalah teori LSW disajikan oleh Lifshitz dan Slyozov [26] , Dan Wagner
[27] . Teori LSW dapat ditulis oleh Persamaan berikut. (1) .
rt3 - = r 03 kt (1)
dimana r 0 dan r t adalah radius partikel rata-rata γ ' fase sebelum penuaan dan setelah penuaan pada saat itu t, masing-masing.
Tingkat pengasaran k adalah konstan dan tergantung pada beberapa parameter seperti yang diungkapkan
dalam persamaan. (2) .
8 γV DC
k =
9 RT
mm (2)
Dimana γ adalah energi antarmuka antara endapan dan matriks, V m adalah volume molar dari
endapan, D adalah di dalam ff usion coe FFI efisien zat terlarut dalam matriks, C m adalah fraksi atom zat
terlarut dalam kesetimbangan dengan endapan di fi Ukuran nite, R ( 8,314 amol - 1 K - 1) adalah gas
konstan dan T adalah temperatur absolut. D di Persamaan. (3) adalah de fi didefinisikan sebagai
Q
DD= 0 exp ••- ••
RT (3)
dimana D 0 adalah faktor konstan dan Q adalah energi aktivasi untuk endapan pengkasaran. Dengan
asumsi bahwa energi antarmuka γ, fraksi volume V m dan fraksi atom zat terlarut C m tidak berubah
dalam paduan diberikan [28,29] , Rumus dapat dicapai berdasarkan Pers. (2) dan
(3) sebagai
Q
ln ( kT ) konstan
= -
RT (4)
Eq. (1) diterapkan pada γ ' perilaku pengkasaran dari paduan baru pada 700 ° C, 750 ° C dan
800 ° C. Kubus rata-rata radius γ ' Fase setelah berbagai waktu penuaan pada tiga suhu diplot sebagai
fungsi waktu penuaan di Gambar. 3 (Sebuah). Linier hubungan antara kubus γ '
Rata-rata radius dan waktu penuaan menunjukkan bahwa pengkasaran γ '
fase mengikuti teori LSW. Menurut kemiringan setiap baris di
Gambar. 3 (A), nilai-nilai dari tingkat pengasaran k pada 700 ° C, 750 ° C dan 800 ° C sekitar 7,818
nm 3 / h, 42,927 nm 3 / h dan 178,226 nm 3 / h. Penuaan tinggi suhu, semakin besar tingkat pengkasaran γ '
tahap. Nilai-nilai tingkat pengasaran konstan k Menyarankan bahwa γ ' fase mengasarkan lebih cepat
dengan peningkatan temperatur penuaan. Hal ini terutama karena suhu tinggi lebih baik untuk di
dalam ff usion elemen.
Menurut Persamaan. (4) , Hubungan antara T suhu dan
tingkat pengasaran k diplot di Gambar. 3 (B). Energi aktivasi Q untuk
γ ' pengasaran ditentukan sebagai 279,98 kJ / mol dari kemiringan plot ln (KT) vs 1 / T. dihitung Q dalam
paduan baru konsisten baik dengan yang di superalloy dasar nikel lainnya (di kisaran 250 - 290 kJ /
mol), dan baik dibandingkan dengan di dalam ff energi aktivasi usion Ni (287,0 kJ / mol), Al (270,0 kJ /
mol) dan Ti (256,9 kJ / mol) di γ matriks
[29 - 32] . Energi aktivasi 279,98 kJ / mol, bersama-sama dengan kinetika pertumbuhan kubik γ ' fase,
menunjukkan bahwa pengkasaran γ ' fase dalam paduan baru terutama dikendalikan oleh di dalam ff usion
Ni, Al dan Ti di γ
matriks.
M. Ou et al.
Gambar. 1. The microstructure of new alloy after standard heat treatment: SEM images showing (a) the distribution of MC carbides, (b) the morphology of MC carbides in grain interiors, (c) granular M 23 C 6 carbides
at GBs and (d) fi ne spherical γ' phase in γ matrix.
3.3. Pengendapan η tahap
Setelah penuaan jangka panjang, morfologi MC dan M 23 C 6
karbida tidak memiliki variasi yang jelas tetapi fase sekunder seperti jarum baru dibentuk dekat GBS
dan sekitar karbida MC. Penelitian sebelumnya [8] memiliki con fi rmed bahwa fase seperti jarum baru η
fase dengan struktur-padat heksagonal dan parameter kisi dari ~ 5,25 Å dan c ~ 8.57 Å, yang η fase
memiliki hubungan orientasi koheren dengan γ matriks: ( 0001) η // (11 1) γ, [21 10] η // [011] γ. Hubungan
orientasi yang jelas antara η fasa dan γ matriks menunjukkan bahwa η
fase diendapkan dari γ matriks. Gambar. 4 menunjukkan evolusi wakil dari η fase sekitar karbida MC
selama jangka panjang penuaan pada 700 ° C, 750 ° C dan 800 ° C. Serupa dengan evolusi η fase
dekat GBS [8] , yang η fase sekitar karbida MC mulai diendapkan setelah penuaan pada 750 ° C
selama 3000 jam dan 800 ° C untuk tahun 2000 h. Kuantitas seperti jarum η fase meningkat setelah
penuaan pada 800 ° C selama 3000 jam. Hasil penelitian menunjukkan bahwa suhu penuaan yang
lebih tinggi dan waktu penuaan lebih lama lebih membantu untuk curah hujan dan pertumbuhan η tahap.
Alasannya terkait erat dengan di dalam ff usion elemen paduan selama proses penuaan jangka
panjang, yang akan dibahas oleh hasil TEM / EDS sebagai berikut.
Setelah menggunakan high-angle annular gelap fi bidang scanning gambar mikroskop transmisi
elektron (HAADF-STEM) modus, jarum-seperti η
fase dan daerah sekitarnya yang diamati dengan jelas, seperti yang ditunjukkan pada
Gambar. 5 . Setelah penuaan pada 800 ° C selama 3000 jam, η fase yang panjang dan lurus,
γ ' endapan zona bebas (PFZ) diamati sekitar dewasa η
fase, seperti yang ditandai dengan panah di Gambar. 5 (Sebuah). Tapi tidak ada yang jelas PFZ dekat
tumbuh-up η fase atau di ujung η fase, seperti yang ditunjukkan oleh panah di Gambar. 5 (B) dan (c).
Selain itu, γ ' fase jauh dari η
fase terus bulat, sedangkan γ ' fase dekat η fase berubah menjadi belahan. Hasil di atas menunjukkan
bahwa γ ' fase bisa diserap ke dalam η fase selama pertumbuhan η tahap. Oleh karena itu,
pertumbuhan
η fase melalui mengkonsumsi γ ' fase menyarankan bahwa satu atau beberapa dari γ '-
unsur pembentuk harus bertindak sebagai elemen pembentukan η tahap. Untuk mendapatkan informasi
lebih lanjut untuk menjelaskan mekanisme pertumbuhan η
78
Materials Science & Engineering A 736 (2018) 76–86
fase dalam paduan baru, komposisi kimia γ matriks, γ ' fasa dan η fase diselidiki oleh TEM / EDS.
Setelah penuaan pada 800 ° C selama 3000 jam, distribusi unsur-unsur γ
matriks, γ ' fasa dan η fase dalam paduan baru diselidiki oleh TEM / EDS, hasil yang ditampilkan di Gambar.
6 . Kontras bervariasi diamati di kedua sisi antarmuka, sehingga elemen paduan dipisahkan di ff erently
di γ matriks, γ ' fasa dan η tahap. Menurut peta elemental, Ni, Al, Ti, Nb dan Mo terutama diperkaya ke
kedua
γ ' fasa dan η fase, sedangkan Cr dan Fe yang jelas diperkaya ke γ
matriks. Distribusi W adalah homogen dalam γ matriks dan γ ' tahap. Ada sedikit literatur menyajikan
distribusi unsur-unsur η
fase melalui karakterisasi eksperimental. Di sini, peta unsur unsur paduan utama, terutama Ni dan Ti
elemen pemetaan ditampilkan dengan jelas di wilayah γ ' fasa dan η tahap.
Untuk jelas menampilkan variasi komposisi dari γ matriks, γ ' fasa dan η fase, analisis line-scan
unsur diselidiki dengan cara TEM / EDS. Gambar. 7 menunjukkan perubahan komposisi unsur
paduan utama dari tiga fase setelah penuaan pada 800 ° C selama 3000 jam. Seperti bisa dilihat, γ matriks
diperkaya dalam Cr dan Fe, namun lowed di Ni, Al, Ti dll Komposisi kimia dewasa η fase dalam Gambar.
7 (A) adalah sesuai dengan yang tumbuh-up η fase dalam Gambar. 7 (C). η fase berisi banyak Ni, Ti
dan sejumlah kecil Al, Nb dll, serta γ '
tahap. Khusus, isi Ni dan Ti di η fase sedikit lebih tinggi dari yang di γ ' fase, seperti yang ditunjukkan
pada Gambar. 7 (B) dan (d).
Menurut identifikasi kuantitatif fi kasi TEM / EDS, komposisi kimia γ matriks adalah FFI rmed
berada, di di%, 66.97Ni,
22.15Cr, 4.51Fe, 3.45Ti, 1.66Al, 0.21Nb, 0.67Mo dan 0.35W. Komposisi kimia γ ' fase itu, di di%,
75.4Ni, 11.75Ti, 6.28Al,
1.94Nb, 1.72Cr, 1.4Fe, 1.22Mo dan 0.25W. Komposisi kimia η fase itu, di di%, 76.59Ni, 12.12Ti,
5.31Al, 3.46Nb, 1.16Fe,
0.66Cr, 0.59Mo dan 0.06W. Hal ini dapat dilihat dengan jelas bahwa kedua γ ' fasa dan η fase
mengandung sejumlah besar Ni dan Ti, dan isi Ni dan Ti di η fase sedikit lebih tinggi dari yang di γ ' tahap.
Di atas semua, tumbuh dari η fase diserap dan dikonsumsi γ ' fase, yang membuat bola γ ' fase dekat η
fase berubah menjadi belahan dan kemudian
M. Ou et al. Materials Science & Engineering A 736 (2018) 76–86

Fig. 2. High magni fi cation SEM images show the evolution of γ ′ phase after long-term aging at (a) 700 °C for 500 h, (b) 700 °C for 1000 h, (c) 700 °C for 3000 h, (d) 750 °C for 500 h, (e) 750 °C for 1000 h, (f) 750
°C for 3000 h, (g) 800 °C for 500 h, (h) 800 °C for 1000 h and (i) 800 °C for 3000 h.

Fig. 3. ( a) The variation of the cube of γ ′ average radius in the new alloy with aging time at di ff erent temperatures, (b) the relationship between aging temperature and the coarsening rate.

79
M. Ou et al. Materials Science & Engineering A 736 (2018) 76–86

Fig. 4. Backscattered electron (BSE) images show needle-like η phase around MC carbides after long-term aging at (a) 700 °C for 3000 h, (b) 750 °C for 2000 h, (c) 750 °C for 3000 h, (d) 800 °C for 1000 h, (e)
800 °C for 2000 h, (f) 800 °C for 3000 h.

led to the formation of γ ′ depleted zones.
In the new alloy, needle-like η phase was precipitated preferentially near GBs and around MC
carbide. Because, GBs acting as one of the main plan defects in metals promoted the elements di ff usion,
MC carbide enriched Ti [8] , both of which were helpful to the precipitation of
η phase. Based on the morphological observations and the chemical compositions analysis about γ ′ and
η phases, the Ti and Ni elements of γ ′
phase were considered to be di ff used gradually to η phase during longterm aging, which caused the
disappearance of γ ′ phase and the formation of PFZ around η phase. Many spherical γ ′ phases were
distributed uniformly in grain interiors, so the needle-like η phase was able to extend from GBs or MC
carbides into the grain interiors through absorbing and consuming γ ′ phase. Hence, the precipitation
and growth of η phase was signi fi cantly impacted by the elements di ff usion.
was the lowest at 700 °C. Thus, the elements di ff usion rate was the largest at 800 °C, the second at
750 °C and the smallest at 700 °C. Higher temperature and longer time were more helpful to
accelerate the diffusion of elements. The higher elements di ff usion rate was more bene fi cial to the
coarsening of γ ′ phase, so the average radius of γ ′ phase was beyond 50 nm after aging at 800 °C for
1000 h and at 750 °C for 3000 h, but it was only 31.5 nm after aging at 700 °C for 3000 h. The higher
elements di ff usion rate was also more conductive to the precipitation of η phase, thus η phase started
to be precipitated after aging at 800 °C for 2000 h and at 750 °C for 3000 h but no η phase was found
at 700 °C for 3000 h.

3.4. The stress rupture properties after long-term aging

Besides, the coarsening of γ ′ phase was a ff ected by the elements di ff usion, and mainly
controlled by the di ff usion of Ni, Al and Ti. The coarsening rate k of γ ′ phase at 800 °C was higher After long-term aging at 700 °C, 750 °C and 800 °C for di ff erent times, the stress rupture
than that at 750 °C, it properties at 750 °C and 430MPa were plotted in Fig. 8 . As the increase of aging time, the stress
rupture life increased

Fig. 5. HAADF images show the needle-like η phase and the surrounding area in the new alloy after aging at 800 °C for 3000 h.

80
M. Ou et al. Materials Science & Engineering A 736 (2018) 76–86

Fig. 6. EDS maps show the elements distribution of γ matrix, γ ′ phase and η phase after aging at 800 °C for 3000 h: (a) Ni; (b) Al; (c) Ti; (d) Nb; (e) Cr; (f) W; (g) Mo and (h) Fe.

at the fi rst 500 h and kept stable to 1000 h then slowly decreased at 700 °C aging, it increased at the fi
rst 500 h and then gradually decreased at 750 °C aging, while it sharply dropped at 800 °C aging, as
shown in Fig. 8 (a). In general, when the aging time was the same, the stress rupture life was the
greatest after aging at 700 °C, the second after aging at 750 °C, and the lowest after aging at 800 °C.
Thereinto, after aging for the same 3000 h, the stress rupture life was rapidly dropped from 121.73 h
to 45.77 h and fi nally to 7.68 h as the aging temperature increasing from 700 °C to 750 °C and fi nally
to 800 °C.
The stress rupture elongation of all samples remained at a high
level, all of them were larger than 8.0%. Specially, after aging at 700 °C and 750 °C, the stress
rupture elongation fi rstly decreased and then slightly increased with prolonging the aging time. After
aging at 800 °C, the stress rupture elongation gradually increased when aging time increased from
300 h to 2000 h, but it slightly decreased when the aging time prolonged to 3000 h.
Based on the above results, the new alloy maintained a long stress rupture life and displayed
good ductility after aging at 700 °C for 300 – 3000 h and 750 °C for 300 – 2000 h. However, its stress
rupture properties dropped after aging at 750 °C and 800 °C for 3000 h. Hence,

Fig. 7. After aging at 800 °C for 3000 h, (a) HAADF images of γ ′ phase and grown-up η phase and (b) the corresponding EDS spectra of them, (c) HAADF images of γ ′
phase and growing-up η phase and (d) the corresponding EDS spectra of them.

81
M. Ou et al. Materials Science & Engineering A 736 (2018) 76–86

Fig. 8. ( a) The stress rupture life and (b) the elongation of new alloy at 750 °C/430MPa after aging at 700 °C, 750 °C and 800 °C for various times.

the new alloy could be used at temperatures up to 750 °C. The changes of stress rupture life and
elongation with aging temperature and time may be concerned with the evolution of microstructure,
including the coarsening of γ ′ phase and the formation of needle-like η phase. The following sections
would focus on how microstructure a ff ected the stress rupture properties.
3.5. The correlation between microstructure and the stress rupture properties
looping around γ ′ phase were still active, as shown in Fig. 9 (e) and (f). Based on the above results,
after long-term aging treatments at 700 °C for 500 h, 1000 h and 3000 h, Orowan looping combining
stacking fault shearing acted as the dominant deformation mechanism. Generally, Orowan loops
surrounding γ ′ phases had the characters of perfect dislocations. In other words, γ ′ phases e ff ectively
impeded the dislocation motion although the size of γ ′ phase slightly increased after aging at 700 °C.
As aging time increasing from 500 h to 3000 h, an increasing number of γ ′ phases were sheared by
dislocations, so the stress rupture life gradually decreased. Anyhow, the stress rupture life maintained
a high level and was higher than 120 h.

In nickel base superalloys, dislocations in γ matrix are di ffi cult to penetrate γ ′ phase, partly
because the γ ′ phase is an atomically ordered phase, which can act as e ff ective obstacles for
preventing dislocation motion [33 – 35] . When dislocations pile up in the areas of γ/γ ′ interface during
deformation, the interactions between dislocations and γ ′ phase, including Orowan bypassing,
stacking faults shearing and cooperative climbing etc., are conducive to impede the dislocations move
forward
After aging at 750 °C for 500 h, 1000 h, 2000 h and 3000 h, similar observations were applied to
study the dislocation con fi gurations of 750 °C/430MPa stress rupture specimens, as shown in Fig. 10 .
After aging at 750 °C for 500 h, γ ′ phase was small and the average radius was about 28.2 nm.
Subsequently, Orowan looping acted as the dominant deformation mechanism. Specially, some
dislocations bypassed some γ ′

phases which had been surrounded by Orowan loop before, namely forming double loops, as shown
[7,18,36] . Especially, the size of γ ′ phase has a signi fi cant impact on the dislocation motion [18,35] . In in Fig. 10 (a) and (b). These double loops were helpful for promoting dislocation tangle and preventing
this paper, all stress rupture samples were fi rstly performed the long-term aging treatment, the size of γ the dislocation motion. In addition, stacking fault shearing stared to be found. As aging time
′ increasing to 1000 h at 750 °C, the average radius of γ ′ phase gradually increased to 37.7 nm. In the
phase was di ff erent before stress rupture testing. The increase of γ ′ size was likely to change the process of deformation, Orowan bypassing was still active, but increasing γ ′ particles were sheared
stress rupture deformation mechanism, and then a ff ected the stress rupture life. Therefore, the by dislocations and SFs were left inside them. In this situation, the new alloy had a high stress rupture
observation of dislocation con fi gurations after stress rupture deformation had been performed life, which was higher than 100 h. After aging at 750 °C for 2000 h, the average radius of γ ′ phase
carefully. further increased to 45.8 nm. During deformation, a few Orowan loops were observed around some γ ′
particles, but much more γ ′ particles were sheared and SFs were formed inside those γ ′ particles, so
After long-term aging treatments at 700 °C for 500 h, 1000 h and 3000 h, the dislocation con fi gurationsthe stress rupture life decreased to 80.5 h. Most noteworthy, after aging at 750 °C for 3000 h, γ ′ phase
of 750 °C/430MPa stress rupture specimens are shown in Fig. 9 . Two types of main dislocation con fi gurations,
was continued to coarsen, the average radius of γ ′
including Orowan looping and stacking fault shearing, were observed in these stress rupture
specimens. After aging at 700 °C for 500 h, γ ′ phase was very small and the average radius was only
about

24.3 nm. After that, dislocations bypassed γ ′ phase and some Orowan loops were formed around
these γ ′ phase during deformation, as shown in Fig. 9 (a) and (b). Specially, some dislocations bowed
out and tended to form large loops around two or more γ ′ particles, as marked by yellow arrows in Fig.
9 (b). It would be very di ffi cult if these larger loops wanted to bow out and then form an individual
Orowan loop around single γ ′ phase. In addition, a few γ ′ phases started to be cut by dislocations, and
stacking faults (SF) were left inside these γ ′ phase, as denoted by red arrows in Fig. 9 (b). Similar
dislocation con fi gurations had been observed in the stress rupture specimens after aging at 700 °C
for 1000 h, as shown in Fig. 9 (c) and (d). After aging time increasing to 3000 h, the average radius of γ
′ phase slightly increased to 31.5 nm. Subsequently, more and more γ ′ phases were cut by
dislocations during stress rupture deformation, and SFs were obviously found inside some
phase was about 51.6 nm. Subsequently, nearly all γ ′ particles were sheared by dislocations with
creation of SFs inside them during deformation. Nonetheless, few Orowan loops could be seen and
some dislocations were still piled up at γ/γ ′ interface, which could play a certain role for impeding the
dislocation motion. In this condition, the stress rupture life quickly decreased to 45.7 h. The above
results indicated that the aging time in fl uenced the stress rupture deformation mechanism of new
alloy. With aging time increasing from 500 h to 3000 h at 750 °C, the size of γ ′ phase increased
gradually, the dominant deformation mechanism transferred from Orowan looping to stacking fault
shearing, so the stress rupture life decreased.

Fig. 11 shows the dislocation con fi gurations of 750 °C /430MPa stress rupture specimens after
aging at 800 °C. After aging at 800 °C for 300 h, γ ′ phase was slightly growing, the average radius of γ
′ phase was
γ ′ phases. Meanwhile, dislocations bypassing γ ′ phase and Orowan

82
M. Ou et al. Materials Science & Engineering A 736 (2018) 76–86

Fig. 9. The dislocation con fi gurations of stress rupture specimens after long-term aging at 700 °C for (a, b) 500 h, (c,d) 1000 h and (e, f) 3000 h.

about 33.3 nm. Subsequently, a great amount of dislocations bypassed
γ ′ particles with leaving Orowan loops and only a few γ ′ particles were sheared with forming SFs
during deformation, as shown in Fig. 11 (a) and (b). Thus the stress rupture life remained at a
relatively high level and was 103.0 h. After aging at 800 °C for 1000 and 3000 h, γ ′ phase was
obviously coarsening, the average radius of γ ′ phase was beyond 50 nm. After that, all γ ′ phases were
sheared seriously by dislocations with leaving many dense SFs inside γ ′ phases during deformation,
as shown in Fig. 11 (c) –( f). The remarkable dislocation con fi gurations
revealed that the dominant deformation mechanism changed from Orowan bypassing to stacking fault
shearing as the increase of aging time at 800 °C. Therefore, the stress rupture life signi fi cantly
decreased to 19.3 h, 7.95 h and 7.68 h after aging at 800 °C for 1000 h, 2000 h and 3000 h.
Based on the above results, the strengthening e ff ect of new ally was controlled either by Orowan
looping mechanism or stacking fault shearing mechanism. Strengthen initially increased with
increasing γ ′
size owing to Orowan looping was the dominant mechanism. As the γ ′

Fig. 10. Dislocation con fi gurations of 750 °C /430MPa stress rupture specimens after subjecting to aging at 750 °C for (a, b) 500 h, (c) 1000 h, (d,e) 2000 h, (f) 3000 h.

83
M. Ou et al. Materials Science & Engineering A 736 (2018) 76–86

Fig. 11. Dislocation con fi gurations of 750 °C /430MPa stress rupture specimens after subjecting to aging at 800 °C for (a, b) 300 h, (c,d) 1000 h, (e,f) 3000 h.

size continued to increase, strengthen decreased owing to stacking fault shearing was the dominant
mechanism. The maximum strengthen e ff ect occurred at the critical γ ′ size [34] where the mechanism
started to transition from looping to shearing. In other words, the average radius of γ ′ phase was
around 24 – 28 nm after aging at 700 °C for 500 – 1000 h and 750 °C for 500 h, the deformation
mechanism started to transitioned, so the new alloy obtained the maximum value of stress rupture
life. However, when the average radius of γ ′ phase was beyond 50 nm after aging at 750 °C for 3000
h and at 800 °C for 1000 – 3000 h, the dominant deformation mechanism was stacking fault shearing,
thus the
stress rupture lives were reduced to half or lower.
After long-term aging at 750 °C for 3000 h and 800 °C for 2000 – 3000 h, needle-like η phase was
found and then grew into the grain interiors, η phase absorbed γ ′ phase and caused the formation of
PFZ (See Figs. 5 and 7 ). To study the in fl uence of η phase on the stress rupture properties of new
alloy, after aging at 800 °C for 3000 h, the dislocation distribution of stress rupture specimen around η
phase was observed by TEM, as shown in Fig. 12 . In TEM images, needle-like η
phases were long and straight, they obviously impeded the gliding of dislocations, so many
dislocations piled up and netted at the edges of η

Fig. 12. Dislocation distributions around the η phase of stress rupture specimen after aging at 800 °C for 3000 h.

84
M. Ou et al.
phases. Accordingly, the existence of dislocation pile-up would induce the stress concentration at η phase/matrix zones around η phases were conductive to the propagation of microcracks. Therefore, the
interface, which was able to promote the nucleation of micro-cavities and micro-cracks [37,38] . In
addition, the dislocation movement would be easier along the areas of PFZ because γ ′ phases acting
as obstacles were missing. Once microcracks were nucleated around η phases, PFZ acting as
strength-weakening regions would attribute to the extension and link-up of microcracks [38 – 40] . The
needle-like η phases in new alloy were preferentially located near GBs or around MC carbides, where
micro-cracks were also easy to be produced, because micro-cracks could extend along GBs, η phase/matrix [1] R.C. Reed, The Superalloys: Fundamentals and applications, Cambridge University Press, New York, 2006 .
interface or carbides/matrix interface [40 – 42] . Some articles [43 – 45] have reported that amounts of
coarse η phases are detrimental to the mechanical properties due to the depletion of γ ′
phase. Above all, η phase would cause the nucleation of micro-cracks, the appearance of PFZ around
η phases would be conductive to the propagation of micro-cracks, both of which helped to further
reduce the stress rupture properties.
After di ff erent long-term aging, the position of micro-viods and micro-cracks in the new alloy was
similar. Some micro-viods and microcracks were found at grain boundaries, some others were
observed in the grain interior especially around MC carbides. After the formation of
η phase, the position of micro-viods and micro-cracks basically unchanged because η phase was
formed near GBs and around MC carbides. Nevertheless, η phase promoted dislocation pile-up which
would accelerate the nucleation of micro-cracks, the formation of γ ′ depleted zones around η phases
would be conductive to the propagation of micro-cracks. Therefore, compared with the specimens
without η phase, the stress rupture life of specimens containing η phase further decreased.
Accordingly, the stress rupture elongation decreased after aging at 750 °C and 800 °C for 3000 h
because of the formation of η
phase.
4. Conclusions
In this study, the e ff ect of long-term aging on the microstructure of new alloy was studied in
detail. The relationship among microstructure, deformation mechanism and stress rupture properties
was discussed. The following conclusions were made.
(1) The coarsening of γ ′ phase in new alloy was agree well with LSW
theory. During long-term aging at 700 °C, 750 °C and 800 °C, the coarsening rate k of γ ′ phase
was about 7.818 nm 3/ h, 42.927 nm 3/ h and 178.226 nm 3/ h, respectively. The activation energy Q for [17] C.S. Wang, T.T. Wang, M.L. Tan, Y.G. Guo, J.T. Guo, L.Z. Zhou, Thermal stability of a new Ni-Fe-Cr base alloy
γ′
coarsening was about 279.98 kJ/mol, the γ ′ coarsening was controlled mainly by the element di ff usion
of Ni, Al and Ti. (2) After aging at 750 °C for 3000 h and at 800 °C for 2000 h, needle-
like η phase was precipitated preferentially around MC carbides and near GBs. Both γ ′ phase
and η phase were enriched in Ni and Ti, so η
phase was able to absorb γ ′ phase, which made η phase extend from GBs or MC carbides into
the grain interiors. As aging time prolonging, the spherical γ ′ phase near η phase gradually turned
into hemisphere and then disappeared, which led to the appearance of γ ′ depleted zones around η
phase. (3) After aging at 700 °C for 300 – 3000 h and 750 °C for 300 – 2000 h, γ ′
phase grew slightly, the average radius of γ ′ phase was below 50 nm. Subsequently, Orowan
looping combing stacking fault shearing acted as the dominant deformation mechanism at 750 °C
and 430MPa. In these situations, γ ′ phases acted as strong obstacles for the dislocation motion,
so the stress rupture life maintained a high level and most of them were higher than 100 h. (4)
After aging at 750 °C for 3000 h and 800 °C for 2000 – 3000 h, γ ′
phase coarsened obviously, the average radius of γ ′ phase was greater than 50 nm. After that,
stacking fault shearing acted as the dominant deformation mechanism, γ ′ phase was very hard
to impede the dislocation motion. Besides, η phase promoted dislocation pile-up and helped to
the nucleation of micro-cracks, the γ ′ depleted
85
Materials Science & Engineering A 736 (2018) 76–86
stress rupture life at 750 °C/430MPa decreased to 45.77 h and 7.68 h after aging at 750 °C and
800 °C.
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