EFFECT OF HAFNIUM CONTENT ON MORPHOLOGY EVOLUTION OF γ PRECIPITATES IN P/M Ni BASED SUPERALLOY

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1 48 8 Vol.48 No ACTA METALLURGICA SINICA Aug pp Hf Ä Ì ÀÚÈÏ γ ß Ó Ð 1,2) 1) 3) 1) Ë² Å ², ) ± ² Â, ) Ë²² ² ², ¹ Hf ÍÆ Ð Ø ¾ γ Æ ¾Ä. Ý : Ð Ø ¾ γ «, Đ Õ «Ì³Æ, «Ì³Æ É Æ «, Í ÖÔ Æ. Hf ÈÓØ Đ Ä, γ ÌÊÃÄ ±ÃÆ «Ï Ã 2 ÛÚ, γ Á Ç Þ Ü Æ ÄÛ Ç. ÂÍ Æ Ð, Ni 3(Al, Ti), γ ÆÖÔ Æ TG ÜÞ½Ñ A ÜÅ¼Æ (2012) EFFECT OF HAFNIUM CONTENT ON MORPHOLOGY EVOLUTION OF γ PRECIPITATES IN P/M Ni BASED SUPERALLOY ZHANG Yiwen 1,2), WANG Fuming 1), HU Benfu 3) 1) School of Metallurgical and Ecological Engineering, University of Science and Technology Beijing, Beijing ) High Temperature Material Institute, Central Iron and Steel Research Institute, Beijing ) School of Materials Science and Engineering, University of Science and Technology Beijing, Beijing Correspondent: ZHANG Yiwen, professor, Tel: (010) , yiwen64@126.com Supported by National Key Basic Research Program of China (No.2010CB631204) and Sino Russian Intergovernmental Cooperation in Science and Technology Project (No.CR14 20) Manuscript received , in revised form ABSTRACT The cubic γ particle morphologyevolution wasstudied during long time agingprocess in a powder metallurgy (P/M) Ni based superalloy with Hf addition. The results show that, during long time aging process, the cubic γ particle splits into a doublet of plantes or an octet of cubes. The octet of cubes with low energy is a preferred shape, it splits no longer. The γ/γ lattice misfit varies with different Hf contents. The growth or coarsening process of γ precipitate can be roughly divided into interface controlling and strain controlling stages, the γ precipitate morphology is greatly influenced by the elastic interaction energy between γ particles. KEY WORDS powder metallurgy superalloy, Ni 3 (Al, Ti), γ phase morphology stability Î Ñ Æ ßÅ ÐÅ Û Ni 3 (Al, Ti) γ, Æ Á γ Æ Ý γ, ÌÊÀ ÑßÙ. γ Ý Í Ç Çß Ì ÆÅ, Á, º γ Ç Ú Å ½Ï, ßµÅ γ Ý Ê Ì,»³ º Øº * Í ¹ Ò Ã«2010CB ÐÐ «CR14 20 Ø : , Ø : Ñ : Õ Ó,, 1964, Ø µ, DOI: /SP.J ÐØË [1 3]. ¹ 70 Ï, º [4 7], Î Ñ ÆÎ Hf ß γ ÈÅÛÌ ÍÆ Å. Î Ñ B 1900 Alloy, 713 LC, Udimet700 M M246 ÆÎ 1.3% 2.0%(«, Ð ) Hf Æ Î MC ÈÅÛÆ, Hf ÈÅÛ ÎÈÅÛ±, ±, ÆÎ Hf ² MC ÈÅÛ Ç ß MC È ÅÛ, Ì ÎÆ»Ç ÕÌ Ó, Á Ê ÆÑßÙ [4,5]. ¹, Î Ñ ÆÎ 0.2% 0.8% Hf, Í± Hf γ γ ßÅ, Ê

2 1012 ± 48 γ ßÑÙ, γ/γ Ð Ô [8]. Æ Ä ¼ ÈÐ, Æ γ ² Ö (doublet of plantes) Í Ç (octet of cubes), γ Ç Í, Ç³ γ [9 11]. º Hf Ñ Ñ Ù± Æ γ Ç Í± Ç Õ, Á ¾ Ö Â È Ù ß¼. 1 Ð ³ È FGH97 Î Ñ, ÚÅ («, %) : Co 15.75, Cr 9.0, W 5.55, Mo 3.85, Al 5.05, Ti 1.8, Nb 2.6, C 0.04, B 0.012, Zr 0.015; ÆÎ Hf («, %) 0, 0.16, 0.3, , Ni Ï. µè ½ Ò Å, Ù µm, 5 Å. µè (HIP) ¼Þ, ÅÙ 1200, 4 h, AC+ ±, µ ± ÅÙ 700, h, AC. Ñ Ù± ÅÙ : ± ÑÙ 550, 650, , ± ±Ð 500, h. Hf FGH97 ¾ ( Ç 8 mm, 8 mm) Æ 1200, 2 h, AC ¼. ¼ ³ ±, ¾ 1200, Ñ 10 min, /s ¼ Å¼ 500 ³ ¼ ½Ñ. È JSM 6480Lu Ò (SEM) ZEISS Sup RA 55 ¼ Ò (FEG SEM) ¾º. SEM ¾ µèòßò Òß ²Å, Ò ßÒ ÅÙ : 20%H 2 SO 4 +80%CH 3 OH(Í ) Òß, Ò V, ±Ð s; Òß ²Å Ù 170 ml H 3 PO ml H 2 SO g CrO 3 Òß, Ò 3 5 V, ±Ð 3 5 s. γ ÇµÈ Image pro Plus 6.0 Ô. µèòå º γ, ÈÅ Ý Õ Hf FGH97 Æ γ, γ º 1%» +1% ÐÍ, ÑÙ 5, ÒÁÎÙ A/cm 2. ß ¾ ( Ç 10 mm, 1 mm), È D/max 2500H X ½ (XRD) ¹ Õ. È Origin8.0 Ô Î PEM ß Æ γ γ ½ ½, ¹À γ γ «¾, µè δ = 2(a γ aγ) a γ +a γ, À «ÉÔÙ (Ú Æ, δ ÉÔÙ, a γ a γ γ γ «¾ ). 2 Ð ÎÃ 2.1 FGH97 É Á Ê ÝÙ «1 ± 0.3%Hf FGH97 Æ 1200, Ø 1 0.3%Hf FGH97» ¾ γ É Fig.1 Morphology of γ precipitates in the FGH97 alloy with 0.3%Hf after solution treatment 4 h, AC ¼ γ Ê. ², Æ ¼, «Ý Í Ð γ ( Ç nm). 2.2 Ò Ö Hf Å FGH97 É γ 2 ± ¼ ÅÐ Hf FGH97 γ Ê. ²Ó, 3 /s ¼ Ð, Hf Æ²¾º ÎÙ γ, ( 2a); Î 0.3%Hf Æ, γ Ð Ñ, Ç Í ( 2c); 0.89%Hf Æ, Ñ γ ³, Ç ÌÃÑÍ ( 2e). Ù 3 /s ¼ Ð, Hf γ ÇÙ, Ù»Á Æ Í± γ ÇËÊ Ð Ç,, Æ Ã. ¼ Å 0.01 /s ±, Æ γ Ê Å. Hf Æ γ ÇÑÍ, Ð, Å Ö, À γ ÚÐÝ ( 2b); 0%Hf, 0.3%Hf γ ( 2d), ËÎ γ Æ À γ Í Å, Ð, ²»Á γ {100} 4 º µ; Hf 0.89% Æ, Í Ç γ, Ñ Í γ Ç, γ ( 2f). ²Ó, ¼ ÅÙ ±, Á Hf Ñ, Æ γ Í Ð Ç±, γ Í Ê Ç. 2.3 Ö Hf Å FGH97 É γ Ë Ç Æ¼ + À±, Hf 0, 0.3% 0.8% FGH97 Æ, γ Å (Ni Co ) 3 (Al Ti Nb ), (Ni Co ) 3 - (Al Ti Nb Hf ) (Ni Co ) 3 - (Al Ti Nb Hf ). 3 γ Æ Nb Ti ËÌ Å, Co Æ Ni, ²

$u Hf C Æ, γ A5l6 h, ^ 3a K+, γ +A =q mb., γ VuU, =Ou, bh 250 nm. \C Æ Hf ==h 0.3% %, γ =OuU, bh 450 nm, 2._ U=O6 γ B A, )! D S % 6 D, A mb6 6 U γ (^ 3b). ~ = 0.$

3 j8s pend : Hf ;;yit ka t!z << γ MaM 1013 B f!z/dl b Q 2 Hf FGH97 γ Fig.2 Morphologies of γ precipitates in the FGH97 alloys with different Hf contents at different cooling rates (a) 0%Hf, 3 /s (b) 0%Hf, 0.01 /s (c) 0.3%Hf, 3 /s (d) 0.3%Hf, 0.01 /s (e) 0.89%Hf, 3 /s (f) 0.89%Hf, 0.01 /s A P Ni Al Æ Ni. I!C Æ Hf ==mj, γ Æ Hf = = mj, Al = = n, [ Hf & P Al, Hf 7 _ γ Æ. ^ 3 %A?"[ Hf == FGH97 C Æ0 E3 `% G γ R. &A A, "[ Hf == C Æ γ RT[ "[. u Hf C Æ, γ A5l6 h, ^ 3a K+, γ +A =q mb., γ VuU, =Ou, bh 250 nm. \C Æ Hf ==h 0.3% %, γ =OuU, bh 450 nm, 2._ U=O6 γ B A, )! D S % 6 D, A mb6 6 U γ (^ 3b). ~ = 0.89%Hf C Æ, γ =O[ n, 6 γ B ia [,b,, ua[ γ 3? 6 D 8 6 U, p [12] 9A [? u= l. 3I Hf ==S 0 mj 0.89%, γ = >S 61.9% m 62.7%, Y γ = > mj "[, ^ γ D : ; " N γ = >. ;z8 [, e=\c Hf Vj[ M γ O"sq, ~ γ 'l # O. M 0.3%Hf = FGH97 QXY3rw>5hk R= γ p h?. "[% mu} γ DGNg OQ y, $P= 0.3%Hf C 550, }4 u% E3. ^ 4 %A? 0.3%Hf C Æ0 + `% "[mu}æ 5000 h 4u% γ R. ^ 4a h= 0.3%Hf C 0 + `% G γ 2.4

89%Hf (c) after solution and aging treatment t 4 < 0.3%Hf b FGH97 B 3t$ Fb γ Q Fig.

4 7 % 1014 j 48 t 3!Z Hf << FGH97 B D2Fb γ Q Fig.3 Morphologies of γ precipitates in the FGH97 alloys with 0%Hf (a), 0.3%Hf (b) and 0.89%Hf (c) after solution and aging treatment t 4 < 0.3%Hf b FGH97 B 3t$ Fb γ Q Fig.4 Morphologies of γ precipitates in the FGH97 alloy with 0.3%Hf after solution and tertiary aging treatment (a), and after 5000 h aging at 550 (b), 650 (c) and 750 (d)

5 8 Ô Ò : Hf Ý Ì γ Å Å 1015 Ç. ÞÃ, ± γ Ð, γ º, γ, ± γ Ñ. Æ 550 Ù ±, Í Ç γ ¼ {100}, γ Ç³ Ð, À γ Í Ý ÆÅ, γ Ç ( 4b). 650 ± Ð γ Í, γ, Ñ Í Ç γ {100}«( 4c). 750 ± γ, γ Ç Ê Ç (preferred shape) Â Í Ç µ LSW(Lifshitz Slyozov Wagher) ÄÅ [13], γ, Ç Ò, À γ ÄÅ ( 4d). 2.5 Ö Hf Å FGH97 É ĐÊ ÝÙ «5 ± Hf FGH97 Æ 850, 1000 h Ù± γ Ê. ²Ó, Ù Hf Æ γ, Í Ç, 100 Đ Ñ ( 5a); 0.3%Hf Æ γ Ç ÄÅ ( 5b), Ù Ù Hf, 0.3%Hf γ ±Ð³, LSW Ä Å ÇÜÛ [13] ; Hf Ñ 0.89%, Æ Ç γ Đ ÅË, Ù γ µ Ç γ ß Í Ç γ Í, γ ÇÒ, γ ßÍ Ú Ç, À γ ÄÅ ( 5c). Ë Þ ² : 850 Ù± Æ, Hf γ ±Ð, Á Hf Ñ ²Ù LSW ÄÅ ÇĐÔ. 1 ± 850, 1000 h ± Þ, Hf FGH97 Æ γ γ «¾ γ /γ ÐÜÉÔ Ù. ²Ó, ± ÞÁ Æ Hf Ñ, Hf γ Æ, «¾ Ñ, γ /γ ÉÔÙ ß ÕÒ, Æ 850 Ñ±, ÉÔÙ ß Å Ã, Ù Î γ /γ ÐÜÉÔÙ»Ë Å Õ,, Î± Æ TCP Ë À γ Ý ¾ 1 Hf FGH97 850, 1000 h Ý γ γ Å ½ γ /γ ÛÈÓØ Table 1 Lattice constants of γ and γ (a γ and a γ ) and lattice mismatch of γ and γ (δ) in the alloys with different Hf contents before and after 1000 h aging at 850 Hf content, % Condition a γ, nm a γ, nm δ, % 0 Before 1000 h aging After 1000 h aging Ø 5 Hf FGH97 850, 1000 h γ É Fig.5 Morphologies of γ precipitates in the FGH97 alloys with 0%Hf (a), 0.3%Hf (b) and 0.89%Hf (c) after 1000 h aging at 850

6 1016 ± 48 ¹ Ä ÑÍ, µ γ ÐÜ¾ ÑÍ. 3 Õ Á ³ Þ ², ßÎ Hf FGH97, γ ÄÅ ÆÊ Ð Ç±, γ. Hf, γ µ± Ð. γ, γ Í Ç Ê Ç. Á Ù± ±Ð», Ç Ê Ç, Ý Ð µå ÜÛ. ÜÛ, Â Í γ Ç ßÍ, γ ÄÅ Ã LSW ÄÅ Ç. 3.1 γ Ô (splitting) Ñ Ù± γ, ÐÁ FGH97 Æ Hf Ñ, γ. γ ÉÔÙÎ ½, Á Hf Ñ, ÉÔÙ ß δ Ö, 0.89%Hf, ËÎ γ ÐÜ¾ ÑÍ, 0.3%Hf δ Ò ( 1), Á, 0.89%Hf ³ [12]. ½Î γ, Ô [14 16] ÌÇ, ÆËÌÊ Ð¹ Ú ß¼ ÄÏ, ÌÔ γ»áý Æ µ Ó. ¹, Í ³, γ» Í γ {100}«4 º Æ, Ä ÆµÍ µ γ ÎÍ, Ã Æ ¾»Á ºÆÐ µ [17]. Qiu [18] Cha [19] ² À Đ«Æ¹ ÉÔÙÍ, Þ É Ò ½ ¼ Ú À : γ {100}«º ÆÐ Ä ¼µß, Ý, 110 «Å Ö ÙÍ, Ú Í Ù ßÚÄ«³, γ {100}«Ì ÅÆ (ËÅ ), γ 100 «º ÆÐ Å, Ä Æ, Å Å γ ß, ¼ 100 Õ γ. Á ÅÆ ÑÍ, γ Å Ó, Â γ Ü, 2, 4 Ë 8 Ö Ñ γ Ç. Ç Õ γ Ý Æ ÜµÐ. ³, Hf ß γ {100}«4 100 «º ÆÐ ±Å ÙÌ ÆÅ, Å» γ ÜÐ. Á Æ Hf Ñ, γ Å ÅÆ ÑÍ, Å Ä ¼ Ñß, «Â ÈÑÍ, Å Ù Ó, γ Ù. Ë ², Á Æ Hf Ñ, γ ÐÜ¾ ÑÍ ÐÜ Ä ¼Ñß, «γ, γ, Ù²» ÆÎ Hf Å γ ßÅ, Ä³ Ê Ç Á. 3.2 γ Ô (preferred shape) Miyazaki [20] Doi [21] º, Á Ý ÄÅ, Ý Ç ÅÆ Ê Ç Å, ¾º γ Ç»Ë 8 Í ( Ð){100}«, Ä»Ë 8 Í ( 3b). ÐÁ Æ Hf Ñ, Å Ê Ç Å ( 3b c). Á³ Þ ², ± Ù γ ÐÑ, ÎÍ ¹ ½Þ, Ä Ù. Á Ñ Ù± ±Ð», Í Ç γ, µ Í γ Ç, γ ÎÍÉÔÙÖ, Ò. Ù±, γ ÄÅ Ù ÇÈ, Õ Ç. ² Ô [14] À Ç γ ß Ä E Þ : 0.709, 0.558, Ñ Í 0.483, Í Ë À Þ ² : γ Á Ñ Í Í Å, Ä»ÐÖ, Ú»Ñ, Ã µ Ê ÇÄ» Ä µ ± Õ Ç. Æ, Ñ Ù±, ËÌ¾º Í Ç, Á, Í Ç»Æ ÜÛ µ Õ Ç, Ô [9] Æ Ê Ç²Ò ÎÍÐÜ. ÎÑ γ Ç» ßÍ Ç, ÎÝ Û Ç,» Ý ÄÅ Æ»Û. 3.3 Æ γ Ë (coarsening) ßÎ Ì ÕÉÔÙ Ñ, γ Ç ÕÎ Ä Þ Ó. ¼Ç Ý ¾ µ ÆÑ LSW ÄÅ Ç, Ñ Ù± ±, ÁÑÙ ±Ð», Ý É Í (ÄÅ), Ö Ú²Ð. ÄÅ» ß Í Í, Ý ²Í, ¹ Ý ÄÅÉ ßÙÖ. ³, γ Þ, γ Ê Õ Ç±, Á ± ÑÙ ±Ð», γ ÇÑ, ÎÙÒ. γ Ê Ð Ç, γ Í Ç±, Ù Ê ÇÁ Ñ± ±Ð», γ ÇÑ Å¾ÇÈ, Ð LSW ÄÅ Ç. Ã, ÄÈ LSW ÄÅ ±, ÂÝ Ç Õ, Ð Õ, LSW ÄÅ ÇËÌ ¹ Í Ç Ý Ë Í Ç ÄÅ (reverse coarsening). ³ ÄÅ ² 2 ÜÛ [14], Ý Ç ± (a r 0, r 0 = σ/e 1 ³ ÉÝ Ù, ÚÆ σ γ/γ

7 8 Ô Ò : Hf Ý Ì γ Å Å 1017 Ð, E 1 ³ ¾ ), ÄÅ»Ë Ö Ú Í, ÜĐÔ È», Ë Ð µå ÜÛ Ý Ì Ç, LSW Ç ºÄÈ. Ý Ç ³ ÉÝ Ù ± (a r 0 ), Ä Ð Ü È±, ÄÅ Ä µå ÜÛ, Ý ÄÅ, ³ Â Ç ( Ë Í Ç), Ù Ê Ç Ö (quasi equilibrium) Ç, Ý ÄÅÀ¾ÇÈ, Ñ ßÅ Õ, Ùß Ó Ñ Ì. 4 Î (1) Á FGH97 Æ Hf Ñ, Å Í Ç γ, Ç Í γ Ç, Ä γ Ê Ç, ÄÅ Å¾ÇÈ. (2) Á Æ Hf Ñ, γ ÐÜ¾ ÑÍ, ÐÜ Ä ¼Ñß, Ì Î «Î γ Å, γ, Ù» ÆÎ Hf ² Å γ Ê Ç Á. (3) Á Æ Hf Ñ, γ ÄÅ Ä µå ÜÛ, Å γ ÄÅ. ÜÞ [1] Maniar G N, Bridge J E. Metall Trans, 1971; 2: 95 [2] Muzyka D R. Met Eng Q, 1971; 11: 12 [3] Hu B F, Liu G Q, Wu K, Tian G F. Acta Metall Sin, 2012; 48: 257 (À ¹, À, Ú, Ï. ³, 2012; 48: 257) [4] Kotval P S, Venables J D, Calder R W. Metall Trans, 1972; 3: 453 [5] Duhl D N, Sullivan C P. J Met, 1971; 23: 38 [6] Dahl J M, Danesi W F, Dunn R G. Metall Trans, 1973; 4: 1087 [7] Maslenkov S B, Burova N N, Khangulov V V. Met Sci Heat Treat, 1980; 22: 283 [8] Miner R V. Metall Trans, 1977; 8A: 259 [9] Khachaturyan A G, Airapetyan V M. Phys Status Solidi, 1974; 26: 611 [10] Qiu Y Y. Acta Mater, 1996; 44: 4969 [11] Yoo Y S. Scr Mater, 2005; 53: 81 [12] Zhang Y W, Wang F M, Hu B F. Acta Metall Sin, 2012; 48: 187 (Õ Ó,, À ¹. ³, 2012; 48: 187) [13] Lifshitz I M, Slyozov V V. J Phys Chem Solids, 1961; 19: 35 [14] Khachaturyan A G, Semenovskaya S V, Morris Jr J W. Acta Metall, 1988; 36: 1563 [15] Kaufman M J, Voorhees P W, Johnson W C, Biancaniello F S. Metall Mater Trans, 1989; 20A: 2171 [16] Grosdidier T, Hazotte A, Simon A. Mater Sci Eng, 1998; A256: 183 [17] Banerjee D, Banerjee R, Wang Y. Scr Mater, 1999; 41: 1023 [18] Qiu Y Y. J Alloys Compd, 1998; 270: 145 [19] Cha P R, Yeon D H, Chung S H. Scr Mater, 2005; 52: 1241 [20] Miyazaki T, Imamura H, Kozakai T. Mater Sci Eng, 1982; 54: 9 [21] Doi M, Miyazaki T, Wakatsuki T. Mater Sci Eng, 1984; 67: 247 ( : )

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