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

daftar isi yang tersedia di ScienceDirect

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 dan δ fase selalu menyebabkan perubahan komposisi lokal dan menyebabkan degradasi sifat
koheren diendapkan L1 2- struktur γ ' tahap. Sifat unik dari paduan ini sangat terkait dengan mekanik [15 - 17] . Selain kemungkinan pembentukan fase yang tidak diinginkan, jangka panjang
memerintahkan γ ' fase karena gerakan dislokasi dapat terhalang oleh γ ' fase selama deformasi plastik 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
[4 - 7] . Baru-baru ini, basis superalloy cor nikel baru terutama diperkuat oleh γ ' tahap [8] dikembangkan Orowan melewati di dasar nikel superalloy kaya Co sebagai peningkatan γ '
untuk aplikasi aero-mesin karena sifat mekanik yang sangat baik pada suhu sampai 750 ° C.

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

umumnya meningkat dengan waktu penuaan jangka panjang [21 - 23] . Oleh karena itu, eksperimen yang 3.2. Pengkasaran dari γ ' tahap
diinginkan secara sistematis menyelidiki di fl pengaruh dari γ '
Ukuran pada mekanisme deformasi paduan baru selama penuaan jangka panjang. Selain evolusi γ ' tahap, Selama penuaan jangka panjang, pengkasaran dari γ ' fase diamati dalam paduan baru. Gambar.
η fase ditemukan pada paduan baru setelah penuaan jangka panjang [8] . Hingga saat ini, ada sedikit 2 menunjukkan evolusi wakil dari γ ' Fase setelah jangka panjang penuaan pada 700 ° C, 750 ° C dan
literatur menyajikan karakteristik distribusi elemen paduan di η 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
fase melalui pengamatan eksperimental dan karakterisasi. Dalam tulisan ini, unsur-unsur paduan meningkatnya suhu penuaan dan waktu. setelah di ff jangka panjang erent penuaan perawatan, jari-jari
utama η fasa dan γ ' fase akan mengidentifikasikan fi ed jelas dengan menggunakan TEM / EDS. Selain rata-rata γ '
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 fase untuk semua spesimen diukur dengan software Ditambah Gambar-Pro. Setelah penuaan pada 700
antara evolusi struktur mikro dan sifat pecah stres dijelaskan. ° 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
2. Bahan-bahan dan metode-metode 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
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 [27] . Teori LSW dapat ditulis oleh Persamaan berikut. (1) .
dari paduan baru adalah (wt%) 19.44Cr,
rt3 - = r 03 kt (1)

5.06Fe, 4,35 (W + Mo), 4,39 (Ti + Al), 1.58Nb, ​0.12C, 0.006B, dan keseimbangan Ni. Dalam studi ini, dimana r 0 dan r t adalah radius partikel rata-rata γ ' fase sebelum penuaan dan setelah penuaan pada saat itu t, masing-masing.
tiga puluh bar disiapkan untuk tes stres pecah, dan enam belas spesimen yang diambil dari bar lain Tingkat pengasaran k adalah konstan dan tergantung pada beberapa parameter seperti yang diungkapkan
yang disiapkan untuk pengamatan struktur mikro. Semua bar dan spesimen solusi anil pada 1120 ° C dalam persamaan. (2) .
selama 4 jam dalam pendingin udara dan udara, dan kemudian berusia di 800 ° C selama 20 jam
8 γV DC
berikut dengan pendingin udara. Salah satu spesimen adalah fi rstly digunakan untuk pengamatan k =
9 RT
mm (2)
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 Dimana γ adalah energi antarmuka antara endapan dan matriks, V m adalah volume molar dari
800 ° C selama 300 jam, 500 jam, 1000 jam, 2000 h atau 3000 h. setelah di ff jangka panjang erent endapan, D adalah di dalam ff usion coe FFI efisien zat terlarut dalam matriks, C m adalah fraksi atom zat
perawatan penuaan, semua bar adalah mesin menjadi sampel stres pecah dengan diameter ukuran terlarut dalam kesetimbangan dengan endapan di fi Ukuran nite, R ( 8,314 amol - 1 K - 1) adalah gas
dari 5mm dan panjang ukuran 25mm. Dua stres sampel pecah diuji pada 750 ° C dan 430MPa, nilai konstan dan T adalah temperatur absolut. D di Persamaan. (3) adalah de fi didefinisikan sebagai
rata-rata digunakan untuk menentukan kehidupan stres pecah dan elongasi.

Q
DD= 0 exp ••- ••
RT (3)

setelah di ff jangka panjang erent perawatan penuaan, mikrostruktur paduan baru dianalisis dimana D 0 adalah faktor konstan dan Q adalah energi aktivasi untuk endapan pengkasaran. Dengan
dengan mikroskop elektron (SEM). spesimen SEM disiapkan melalui polishing mekanik dan kimia asumsi bahwa energi antarmuka γ, fraksi volume V m dan fraksi atom zat terlarut C m tidak berubah
etsa dalam larutan dengan 20 g CuSO 4, 150ml HCl dan 80ml H 2 O untuk pengamatan SEM umum. dalam paduan diberikan [28,29] , Rumus dapat dicapai berdasarkan Pers. (2) dan
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 (3) sebagai

ratus partikel dipilih untuk mengukur ukuran γ ' Fase oleh Gambar-Pro software Plus.
Q
ln ( kT ) konstan
= -
RT (4)

Eq. (1) diterapkan pada γ ' perilaku pengkasaran dari paduan baru pada 700 ° C, 750 ° C dan
Setelah tes stres pecah, semua sampel dipotong menjadi cakram sepanjang arah vertikal dari 800 ° C. Kubus rata-rata radius γ ' Fase setelah berbagai waktu penuaan pada tiga suhu diplot sebagai
stres garis aksial dan menipis ke 50 pM mekanis. Setelah penggilingan, foil TEM yang elektrokimia fungsi waktu penuaan di Gambar. 3 (Sebuah). Linier hubungan antara kubus γ '
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 Rata-rata radius dan waktu penuaan menunjukkan bahwa pengkasaran γ '
transmisi (TEM) dilengkapi dengan annular sudut tinggi gelap fi bidang (HAADF) detektor dan dispersi fase mengikuti teori LSW. Menurut kemiringan setiap baris di
spektrometer (EDS) sistem energi X-ray. dislokasi con- 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
fi gurations dihasilkan dari deformasi stres pecah diselidiki oleh Tecnai G 2 F20 TEM. dengan peningkatan temperatur penuaan. Hal ini terutama karena suhu tinggi lebih baik untuk di
dalam ff usion elemen.

3. Hasil dan Pembahasan Menurut Persamaan. (4) , Hubungan antara T suhu dan
tingkat pengasaran k diplot di Gambar. 3 (B). Energi aktivasi Q untuk
3.1. mikro awal 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 /
Setelah perlakuan panas standar, fase konstituen dari paduan baru termasuk γ matriks, kuning mol), dan baik dibandingkan dengan di dalam ff energi aktivasi usion Ni (287,0 kJ / mol), Al (270,0 kJ /
karbida MC, granular M 23 C 6 karbida dan fi ne bola γ ' fase, seperti yang ditunjukkan pada Gambar. 1 . mol) dan Ti (256,9 kJ / mol) di γ matriks
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 [29 - 32] . Energi aktivasi 279,98 kJ / mol, bersama-sama dengan kinetika pertumbuhan kubik γ ' fase,
dengan jari-jari rata-rata 13,5 nm. menunjukkan bahwa pengkasaran γ ' fase dalam paduan baru terutama dikendalikan oleh di dalam ff usion
Ni, Al dan Ti di γ
matriks.

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

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 fase dalam paduan baru, komposisi kimia γ matriks, γ ' fasa dan η fase diselidiki oleh TEM / EDS.

Setelah penuaan jangka panjang, morfologi MC dan M 23 C 6 Setelah penuaan pada 800 ° C selama 3000 jam, distribusi unsur-unsur γ
karbida tidak memiliki variasi yang jelas tetapi fase sekunder seperti jarum baru dibentuk dekat GBS matriks, γ ' fasa dan η fase dalam paduan baru diselidiki oleh TEM / EDS, hasil yang ditampilkan di Gambar.
dan sekitar karbida MC. Penelitian sebelumnya [8] memiliki con fi rmed bahwa fase seperti jarum baru η 6 . Kontras bervariasi diamati di kedua sisi antarmuka, sehingga elemen paduan dipisahkan di ff erently
fase dengan struktur-padat heksagonal dan parameter kisi dari ~ 5,25 Å dan c ~ 8.57 Å, yang η fase di γ matriks, γ ' fasa dan η tahap. Menurut peta elemental, Ni, Al, Ti, Nb dan Mo terutama diperkaya ke
memiliki hubungan orientasi koheren dengan γ matriks: ( 0001) η // (11 1) γ, [21 10] η // [011] γ. Hubungan kedua
orientasi yang jelas antara η fasa dan γ matriks menunjukkan bahwa η
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
fase diendapkan dari γ matriks. Gambar. 4 menunjukkan evolusi wakil dari η fase sekitar karbida MC distribusi unsur-unsur η
selama jangka panjang penuaan pada 700 ° C, 750 ° C dan 800 ° C. Serupa dengan evolusi η fase fase melalui karakterisasi eksperimental. Di sini, peta unsur unsur paduan utama, terutama Ni dan Ti
dekat GBS [8] , yang η fase sekitar karbida MC mulai diendapkan setelah penuaan pada 750 ° C elemen pemetaan ditampilkan dengan jelas di wilayah γ ' fasa dan η tahap.
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 Untuk jelas menampilkan variasi komposisi dari γ matriks, γ ' fasa dan η fase, analisis line-scan
lebih tinggi dan waktu penuaan lebih lama lebih membantu untuk curah hujan dan pertumbuhan η tahap. unsur diselidiki dengan cara TEM / EDS. Gambar. 7 menunjukkan perubahan komposisi unsur
Alasannya terkait erat dengan di dalam ff usion elemen paduan selama proses penuaan jangka paduan utama dari tiga fase setelah penuaan pada 800 ° C selama 3000 jam. Seperti bisa dilihat, γ matriks
panjang, yang akan dibahas oleh hasil TEM / EDS sebagai berikut. 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 '

Setelah menggunakan high-angle annular gelap fi bidang scanning gambar mikroskop transmisi
elektron (HAADF-STEM) modus, jarum-seperti η tahap. Khusus, isi Ni dan Ti di η fase sedikit lebih tinggi dari yang di γ ' fase, seperti yang ditunjukkan
fase dan daerah sekitarnya yang diamati dengan jelas, seperti yang ditunjukkan pada pada Gambar. 7 (B) dan (d).
Gambar. 5 . Setelah penuaan pada 800 ° C selama 3000 jam, η fase yang panjang dan lurus, Menurut identifikasi kuantitatif fi kasi TEM / EDS, komposisi kimia γ matriks adalah FFI rmed
γ ' endapan zona bebas (PFZ) diamati sekitar dewasa η berada, di di%, 66.97Ni,
fase, seperti yang ditandai dengan panah di Gambar. 5 (Sebuah). Tapi tidak ada yang jelas PFZ dekat 22.15Cr, 4.51Fe, 3.45Ti, 1.66Al, 0.21Nb, 0.67Mo dan 0.35W. Komposisi kimia γ ' fase itu, di di%,
tumbuh-up η fase atau di ujung η fase, seperti yang ditunjukkan oleh panah di Gambar. 5 (B) dan (c). 75.4Ni, 11.75Ti, 6.28Al,
Selain itu, γ ' fase jauh dari η 1.94Nb, 1.72Cr, 1.4Fe, 1.22Mo dan 0.25W. Komposisi kimia η fase itu, di di%, 76.59Ni, 12.12Ti,
fase terus bulat, sedangkan γ ' fase dekat η fase berubah menjadi belahan. Hasil di atas menunjukkan 5.31Al, 3.46Nb, 1.16Fe,
bahwa γ ' fase bisa diserap ke dalam η fase selama pertumbuhan η tahap. Oleh karena itu, 0.66Cr, 0.59Mo dan 0.06W. Hal ini dapat dilihat dengan jelas bahwa kedua γ ' fasa dan η fase
pertumbuhan mengandung sejumlah besar Ni dan Ti, dan isi Ni dan Ti di η fase sedikit lebih tinggi dari yang di γ ' tahap.
η fase melalui mengkonsumsi γ ' fase menyarankan bahwa satu atau beberapa dari γ '- Di atas semua, tumbuh dari η fase diserap dan dikonsumsi γ ' fase, yang membuat bola γ ' fase dekat η
unsur pembentuk harus bertindak sebagai elemen pembentukan η tahap. Untuk mendapatkan informasi fase berubah menjadi belahan dan kemudian
lebih lanjut untuk menjelaskan mekanisme pertumbuhan η

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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.

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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. was the lowest at 700 °C. Thus, the elements di ff usion rate was the largest at 800 °C, the second at
In the new alloy, needle-like η phase was precipitated preferentially near GBs and around MC 750 °C and the smallest at 700 °C. Higher temperature and longer time were more helpful to
carbide. Because, GBs acting as one of the main plan defects in metals promoted the elements di ff usion, accelerate the diffusion of elements. The higher elements di ff usion rate was more bene fi cial to the
MC carbide enriched Ti [8] , both of which were helpful to the precipitation of 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
η phase. Based on the morphological observations and the chemical compositions analysis about γ ′ and elements di ff usion rate was also more conductive to the precipitation of η phase, thus η phase started
η phases, the Ti and Ni elements of γ ′ to be precipitated after aging at 800 °C for 2000 h and at 750 °C for 3000 h but no η phase was found
phase were considered to be di ff used gradually to η phase during longterm aging, which caused the at 700 °C for 3000 h.
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.

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.

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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 level, all of them were larger than 8.0%. Specially, after aging at 700 °C and 750 °C, the stress
rst 500 h and then gradually decreased at 750 °C aging, while it sharply dropped at 800 °C aging, as rupture elongation fi rstly decreased and then slightly increased with prolonging the aging time. After
shown in Fig. 8 (a). In general, when the aging time was the same, the stress rupture life was the aging at 800 °C, the stress rupture elongation gradually increased when aging time increased from
greatest after aging at 700 °C, the second after aging at 750 °C, and the lowest after aging at 800 °C. 300 h to 2000 h, but it slightly decreased when the aging time prolonged to 3000 h.
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. 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,
The stress rupture elongation of all samples remained at a high

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.

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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 looping around γ ′ phase were still active, as shown in Fig. 9 (e) and (f). Based on the above results,
elongation with aging temperature and time may be concerned with the evolution of microstructure, after long-term aging treatments at 700 °C for 500 h, 1000 h and 3000 h, Orowan looping combining
including the coarsening of γ ′ phase and the formation of needle-like η phase. The following sections stacking fault shearing acted as the dominant deformation mechanism. Generally, Orowan loops
would focus on how microstructure a ff ected the stress rupture properties. 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.
3.5. The correlation between microstructure and the stress rupture properties

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

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

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

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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 revealed that the dominant deformation mechanism changed from Orowan bypassing to stacking fault
γ ′ particles with leaving Orowan loops and only a few γ ′ particles were sheared with forming SFs shearing as the increase of aging time at 800 °C. Therefore, the stress rupture life signi fi cantly
during deformation, as shown in Fig. 11 (a) and (b). Thus the stress rupture life remained at a 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.
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, Based on the above results, the strengthening e ff ect of new ally was controlled either by Orowan
as shown in Fig. 11 (c) –( f). The remarkable dislocation con fi gurations 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.

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

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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 stress rupture life at 750 °C/430MPa decreased to 45.77 h and 7.68 h after aging at 750 °C and
addition, the dislocation movement would be easier along the areas of PFZ because γ ′ phases acting 800 °C.
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 References
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