Research progress in grain boundary serration in iron/nickel based austenitic polycrystalline alloys
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摘要: 對于在高溫環境服役的金屬材料，晶界作為組織結構上的薄弱環節常常引發晶界裂紋而造成合金失效，嚴重影響了材料的高溫力學性能表現。因而，如何改善晶界狀態、提高晶界強度，是提高合金高溫性能的關鍵。在鐵/鎳基奧氏體多晶合金中，采用晶界彎曲的方法強化晶界、改善合金性能一直受到國內外研究人員的廣泛關注。從彎曲晶界的獲得方法、形成機制及其對材料性能的影響3個方面概述了目前國內外的研究現狀。較為全面地總結了特殊熱處理與材料合金化等獲得彎曲晶界的方法；討論了不同合金中晶界第二相誘發晶界彎曲的驅動力和內在機理；介紹了彎曲晶界對材料力學性能、耐蝕性能及焊接性能的影響。最后，結合當前的研究現狀，圍繞彎曲晶界的形成條件和機制，以及彎曲晶界對性能的影響，提出了彎曲晶界未來的研究發展方向。Abstract: Grain boundaries of high-temperature metallic materials, such as alloys, are often considered weak. At elevated temperatures, the strength of the grain boundary is relatively lower than that of the intragranular areas, and cracks often initially form on the grain boundary and then develop along it, which leads to premature failure and significantly degrades the mechanical performance of the material at high temperature. Therefore, how to optimize the morphology and improve the strength of the grain boundary is key to improving the properties of alloys at high temperatures. A serrated grain boundary is a type of grain boundary with a wave shape evolving from the bending of the flat grain boundary during special heat treatments. For iron/nickel-based austenitic polycrystalline alloys, grain boundary serration has been viewed as an effective method for strengthening their grain boundaries and enhancing their properties. Here, the research progress of serrated grain boundaries was reviewed based on the aspects of formation method, formation mechanism, and their influence on the properties of materials. The methods of formation of serrated grain boundaries for different types of alloys, such as controlled cooling heat treatment, isothermal heat treatment, mechanical heat treatment, and alloying, were summarized. The interactions between the grain boundary and intergranular precipitates, such as M7C3 carbide, M23C6 carbide, and γ′ phase, were discussed in detail to understand the formation mechanism of the serrated grain boundary and how it improving the properties of materials and reveal the driving force of grain boundary migration. In addition, the influences of the serrated grain boundary on the mechanical (rupture, creep, fatigue, and tensile) properties, corrosion properties (hot and stress corrosion), and heat-affected-zone (HAZ) liquefying cracking behavior of different alloys were analyzed. Last, based on the abovementioned details, development directions for future work on serrated grain boundaries were outlined.
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圖 2 Ni–20Cr合金熱處理示意圖與對應的晶界SEM形貌。（a）控冷熱處理示意圖；（b）控冷熱處理的晶界形貌；（c）控冷熱處理同時進行5%應變壓縮示意圖；（d）控冷熱處理同時進行5%應變壓縮的晶界形貌[19]
Figure 2. Heat treatment regime and grain boundary SEM morphology of Ni–20Cr alloy: (a) schematic of controlled cooling heat treatment; (b) grain boundary morphology of the sample controlled cooled; (c) schematic of controlled cooling with a 5% compressive strain hold at the same time; (d) grain boundary morphology of the sample controlled cooled and 5% compressed [19]
圖 3 600合金熱處理制度示意圖與對應的晶界SEM形貌。（a）緩冷熱處理制度；（b）分步時效熱處理制度；（c）緩冷熱處理后的彎曲晶界；（d）等溫時效熱處理后的平直晶界[12]
Figure 3. Heat treatment regime and grain boundary SEM morphology of Alloy 600: (a) schematic of slow cooling heat treatment; (b) schematic of step aging heat-treatment; (c) grain boundary morphology of the sample slowly cooled; (d) grain boundary morphology of the sample step aged[12]
圖 4 690合金不同熱處理制度條件下的晶界和碳化物SEM形貌。（a）1080 ℃保溫10 min水淬后720 ℃保溫10 h；（b）1080 ℃保溫10 min后以0.5 ℃·min?1控冷[28]
Figure 4. SEM morphology of grain boundary and carbide in Alloy 690: (a) solution annealed at 1080 ℃ for 10 min before water quenching and aged at 720 ℃ for 10 h; (b) solution annealed at 1080 ℃ for 10 min and cooling at 0.5 ℃·min?1[28]
圖 7 采用三維原子探針觀察Ni?20Cr二元合金中彎曲晶界處的元素分布。（a）取樣位置；（b）柱狀樣品中的彎曲晶界；（c）元素分析區域；（d）Ni原子濃度分布; (e)Cr原子濃度分布；（f）Ni+Cr原子濃度分布；（g）Ni和Cr原子的濃度曲線[19]
Figure 7. APT elemental distribution at the serrated grain boundary in Ni?20Cr binary alloy: (a) sampling position; (b) the serrated grain boundary in cylindrical sample; (c) elemental analyzing area; (d) concentration distribution of Ni atoms; (e) concentration distribution of Cr atoms; (f) concentration distribution of Ni+Cr atoms; (g) concentration curve of Ni and Cr atoms[19]
圖 9 FGH98I合金固溶處理后緩冷過程中的γ′相與彎曲晶界。（a）γ′相長大誘發晶界彎曲；（b）γ′相長大誘發晶界彎曲示意圖；（c）樹枝狀γ′相生長誘發晶界彎曲；（d）樹枝狀γ′相生長誘發晶界彎曲示意圖；（e）γ′相移動誘發晶界彎曲；（f）γ′相移動誘發晶界彎曲示意圖；（g）晶界兩側γ′相密度不同誘發的彎曲晶界；（h）晶界兩側γ′相密度不同誘發的彎曲晶界示意圖[3]
Figure 9. γ′ phase and grain boundary serration in FGH98I alloy after solution annealing and slow cooling: (a) serration induced by γ′ phase growth; (b) schematic of the γ′ phase growth induced serration; (c) serration induced by dendritic γ′ phase formation; (d) schematic of the dendritic γ′ phase formation induced serration; (e) serration induced by γ′ phase movement; (f) schematic of the γ′ phase movement induced serration; (g) serration induced by particle density difference; (h) schematic of the particle density difference induced serration [3]
表 1 標準熱處理和控冷熱處理對晶界彎曲的影響
Table 1. Effects of standard and controlled-cooling heat treatments on the serration of grain boundary
Alloy Heat treatment type Heat treatment regime Grain boundary type Reference AISI304 Standard 1050 ℃×1 h+WQ，760 ℃×50 h+WQ Flat [14] Controlled cooling 1050 ℃×1 h+4 ℃·min?1→760 ℃×50 h+WQ Serrated Nimonic263 Standard 1150 ℃×30 min+WQ，800 ℃×8 h+AC Flat [15] Controlled cooling 1150 ℃×5 min+10 ℃·min?1→800 ℃×8 h+AC Serrated AISI316 Standard 1050 ℃×1 h+WQ，760 ℃×1 h+WQ Flat [16] (The mass fraction of
carbon is 0.044)Controlled cooling 1050 ℃×1 h+FC→760 ℃×1 h+WQ Serrated In718 Standard 1090 ℃×1 h+WQ，850 ℃×4 h+WQ Flat [17] Controlled cooling 1090 ℃×1 h+FC→850 ℃×4 h+WQ Serrated GH151 Standard 1250 ℃×5 h+AC，1000 ℃×5 h+AC，950 ℃×10 h+AC Flat [18] Controlled cooling 1250 ℃×5 h+0.5 ℃·min?1→1070 ℃×4 h+AC Serrated Note: WQ refers to water quenching, AC refers to air cooling and FC refers to furnace cooling. 
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表 2 固溶制度對晶界彎曲的影響
Table 2. Effect of solution heat treatment on the serration of grain boundary
Alloy Heat treatment regime Grain boundary type Average amplitude/
μmAverage wavelength/
μmReference In600 1100 ℃×2 h+0.25 ℃·min?1→900 ℃+WQ Flat — — [12] 1140 ℃×2 h+0.25 ℃·min?1→900 ℃+WQ Serrated 0.92 24.54 1120 ℃×2 h+3 ℃·min?1→900 ℃+WQ Serrated 0.75 21.6 1140 ℃×2 h+3 ℃·min?1→900 ℃+WQ Serrated 0.77 23.8 1000 ℃×2 h+12 ℃·min?1→900 ℃+WQ Flat — — 1100 ℃×2 h+12 ℃·min?1→900 ℃+WQ Serrated 0.64 19.02 1140 ℃×2 h+12 ℃·min?1→900 ℃+WQ Serrated 0.58 23.44 Ni?20Cr 1200 ℃×5 min+5 ℃·min?1→800 ℃+WQ Flat — — [19] 1250 ℃×5 min+5 ℃·min?1→800 ℃+WQ Serrated — —
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表 3 冷速對晶界彎曲的影響
Table 3. Effect of cooling rate on the serration of grain boundary
Alloy Heat treatment regime Grain boundary type Average amplitude/
μmAverage wavelength/
μmReference In600 1100℃×2 h+12 ℃·min?1→900 ℃+WQ Serrated 0.64 19.02 [12] 1100 ℃×2 h+30 ℃·min?1→900 ℃+WQ Serrated 0.62 13.7 1140 ℃×2 h+0.25 ℃·min?1→900 ℃+WQ Serrated 0.92 24.54 1140 ℃×2 h+3 ℃·min?1→900 ℃+WQ Serrated 0.77 23.8 1140 ℃×2 h+12 ℃·min?1→900 ℃+WQ Serrated 0.58 23.44 1140 ℃×2 h+60 ℃·min?1→900 ℃+WQ Serrated 0.47 21.83 FGH98I 1190 ℃×1 h+0.1 ℃·s?1→Room temperature Serrated 4.02 0.44 [3] 1190 ℃×1 h+0.4 ℃·s?1→Room temperature Serrated 2.61 0.86 1190 ℃×1 h+1.4 ℃·s?1→Room temperature Serrated 0.98 2.26 1190 ℃×1 h+4.3 ℃·s?1→Room temperature Serrated 0.64 6.41 1190 ℃×1 h+10.8 ℃·s?1→Room temperature Serrated 0.63 15.74
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表 4 控冷后直接等溫時效處理對晶界彎曲的影響
Table 4. Effect of direct isothermal aging treatment on the serration of grain boundary
Alloy Heat treatment regime Grain boundary type Average amplitude/
μmAverage wavelength/
μmReference In600 1140 ℃×2 h+12 ℃·min?1→900 ℃+WQ Serrated 0.58 23.44 [12] 1140 ℃×2 h+12 ℃·min?1→900 ℃×30 min+WQ Serrated 0.62 26.15 1140 ℃×2 h+12 ℃·min?1→1040 ℃× 30 min+WQ Flat — — 1140 ℃×2 h+12 ℃·min?1→1060 ℃× 30 min+WQ Flat — —
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表 5 標準熱處理和等溫熱處理對晶界彎曲的影響
Table 5. Effects of standard and isothermal heat treatments on the serration of grain boundary
Alloy Heat treatment type Heat treatment regime Grain boundary type Reference GH37 Standard 1180 ℃×2 h+AC，1150 ℃×4 h+AC，800 ℃×16 h+AC Flat [18] Isothermal 1180 ℃×2 h$ \stackrel{\mathrm{A}\mathrm{i}\mathrm{r}\mathrm{?}\mathrm{c}\mathrm{o}\mathrm{o}\mathrm{l}\mathrm{i}\mathrm{n}\mathrm{g}}{\to } $900 ℃×4 h+AC Serrated GH33 Standard 1080 ℃×8 h+AC，700 ℃×10 h+AC Flat Isothermal 1080 ℃×8 h$ \stackrel{\mathrm{A}\mathrm{i}\mathrm{r}\mathrm{?}\mathrm{c}\mathrm{o}\mathrm{o}\mathrm{l}\mathrm{i}\mathrm{n}\mathrm{g}}{\to } $900 ℃×4 h+AC Serrated GH36 Standard 1140 ℃×80 min+WQ，670 ℃×12 h+780×10 h+AC Flat Isothermal 1180 ℃×80 min$ \stackrel{\mathrm{A}\mathrm{i}\mathrm{r}\mathrm{?}\mathrm{c}\mathrm{o}\mathrm{o}\mathrm{l}\mathrm{i}\mathrm{n}\mathrm{g}}{\to } $800 ℃×16 h+AC Serrated Эи69 Standard 1140 ℃×80 min+AC，700 ℃×16 h+AC Flat Isothermal 1180 ℃×2 h$ \stackrel{\mathrm{A}\mathrm{i}\mathrm{r}\mathrm{?}\mathrm{c}\mathrm{o}\mathrm{o}\mathrm{l}\mathrm{i}\mathrm{n}\mathrm{g}}{\to } $900 ℃×4 h+AC Serrated GH220 Standard 1220 ℃×4 h+AC，1050 ℃×4 h+AC，950 ℃×2 h+AC Flat [23-25] Isothermal 1220 ℃×4 h$ \stackrel{\mathrm{A}\mathrm{i}\mathrm{r}\mathrm{?}\mathrm{?}\mathrm{?}\mathrm{?}\mathrm{?}\mathrm{?}\mathrm{?}\mathrm{?}\mathrm{c}\mathrm{o}\mathrm{o}\mathrm{l}\mathrm{i}\mathrm{n}}{\to } $1070 ℃×2.5 h+AC，950 ℃×2 h+AC Serrated
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表 6 不同合金中平直晶界與彎曲晶界對蠕變性能的影響
Table 6. Effects of flat and serrated grain boundaries on the creep properties of different alloys
Alloy (Temperature/°C)/
(Stress/MPa)Creep life/h Creep life
increase/%Fracture plasticity
increase /%Reference Flat grain boundary Serrated grain boundary Cr–15Co–Ni 850/343 150 183–193.5 22–29 [35] Ni–Cr–W–Mo 850/350 150 193 28.67 [36] GH49 850/350 94 120 27.66 73 [37-38] 21Cr–4Ni–9Mn 700/196 370 630 70.27 [39-40] 900/27.4 230 310 34.78 In718 650/625 1200 1600 33.33 [17] In600 700/170 29.8 30 0.67 5.7 [41] 815/70 40.7 59.8 46.93 9 900/40 46.1 63.9 38.61 5.3
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表 7 GH220合金彎曲晶界與平直晶界在950 ℃條件下的拉伸性能[2]
Table 7. Tensile properties of GH220 alloys with flat and serrated grain boundaries at 950 °C [2]
Grain boundary type Test temperature/
°CTensile
strength/
MPaElongation/
%Reduction
of area/
%Flat grain boundary 950 546.25 13.6 19.7 Serrated grain boundary 950 591.36 20.7 25.4 Percentage increase/% 0 8 50.7 28.9
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表 8 AISI304不銹鋼的彎曲晶界與平直晶界在600 ℃條件下的拉伸性能[14]
Table 8. Tensile properties of AISI304 steel with flat and serrated grain boundaries at 600 °C [14]
Grain boundary
typeTest temperature/
°CYield strength/
MPaTensile strength/
MPaElongation/
%Flat grain boundary 600 149 379 40.0 Serrated grain boundary 600 153 383 39.6
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表 9 Inconel751合金在大氣及熱腐蝕環境中的蠕變性能[2]
Table 9. Creep properties of Inconel751 alloy in air and in a corrosive environment [2]
Grain boundary type Creep strength /MPa In air Corrosive environment 100 h 1000 h 100 h Flat grain boundary 255 149 68 Serrated grain boundary 273 196 153
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