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摘要: 以易控的工藝條件為基礎，通過設計簡易實驗裝置來模擬鋯合金在實際生產中的張力退火過程。采用X射線衍射（XRD）和電子背散射（EBSD）技術，對不同溫度和不同張力下退火處理后的Zr–4合金織構和再結晶行為進行研究。結果表明，施加外加應力和提高退火溫度可顯著改變再結晶織構演化過程。隨著外加應力值的增加以及退火溫度的升高，鋯合金的主要織構(
$\overline 1 2\overline 1 5$ )[$ 10 \overline 1 0$ ]總量減少，極密度減弱，從而導致材料各向異性減小；外加應力和退火溫度對材料再結晶過程中小角度晶界數量以及再結晶比例產生了顯著影響，隨著外加應力的增加以及退火溫度的升高，材料內部發生動態回復和再結晶，位錯和亞結構逐漸消失，材料再結晶過程中的小角度晶界數量明顯減少，材料的再結晶過程加快，材料的再結晶比例顯著提高。外加應力的施加以及退火溫度的升高均有利于材料內部再結晶過程的加速進行。研究結果對Zr–4合金退火處理優化有指導作用，為解決鋯合金在工程應用中所遇到的問題提供了科學基礎。Abstract: The texture of Zr–4 alloy not only affects its irradiation growth performance, but also affects mechanical properties, stress corrosion cracking, and water-side corrosion. Therefore, it is important to control the texture of Zr–4 alloy during processing. The effect of the applied external stress, annealing temperature, and annealing time on texture evolution and recrystallization of Zr–4 alloy is still unclear. Based on controllable process conditions, the stress annealing process of zirconium alloy in practical production was simulated by designing a simple experimental device. The texture and recrystallization behavior of Zr–4 alloy after annealing at different temperatures and stresses were studied by X-ray diffraction (XRD) and electron backscatter diffraction (EBSD) techniques. The results show that applying external stress and increasing annealing temperature significantly change the evolution of recrystallized texture. With an increase in stress and annealing temperature, the texture of the zirconium alloy ($\overline 1 2\overline 1 5$ )[$10 \overline 1 0$ ], and the polar density decreases, thereby resulting in a decrease in material anisotropy. The annealing temperature has a significant effect on the amount of small-angle grain boundary and recrystallization ratio during material recrystallization. With an increase in applied stress and annealing temperature, dynamic recovery and recrystallization occur inside the material. The sub-structures in dynamic recovery and the dislocation sub-structures in the grains that undergo dynamic recrystallization gradually disappear. The small-angle grain boundary in the material recrystallization process is reduced significantly. The process is accelerated and the recrystallization ratio of the material is significantly increased. The application of applied external stress and the increase of annealing temperature are beneficial to the acceleration of the internal recrystallization process of the material. The main results from this paper can guide the optimization of annealing treatment of Zr–4 alloy, and provide a scientific basis for solving the problems encountered in the engineering application of Zr–4 alloy.-
Key words:
- Zr–4 alloy /
- annealing /
- stress /
- texture /
- recrystallization
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圖 3 應力退火處理后Zr–4板材取向分布函數。（a）冷軋態；（b）580 ℃，0 MPa；（c）580 ℃，3 MPa；（d）580 ℃，9 MPa；（e）610 ℃，0 MPa；（f）610 ℃，3 MPa；（g）610 ℃，9 MPa；（h）640 ℃，0 MPa；（i）640 ℃，3 MPa；（j）640 ℃，9 MPa；（k）重要取向
Figure 3. Orientation distribution function of Zr–4 sheet after stress annealing: (a) cold rolled sheet; (b) 580 ℃, 0 MPa; (c) 580 ℃, 3 MPa; (d) 580 ℃, 9 MPa; (e) 610 ℃, 0 MPa; (f) 610 ℃, 3 MPa; (g) 610 ℃, 9 MPa; (h) 640 ℃, 0 MPa; (i) 640 ℃, 3 MPa;（j）640 ℃, 9 MPa; (k) important orientation position
圖 4 不同溫度下應力退火后Zr–4合金主要織構組分極密度變化
Figure 4. Polar density variation of main texture components of Zr–4 alloy after stress annealing at different temperatures
圖 5 580 ℃條件下不同保溫時間退火處理后Zr–4板材取向分布函數。（a）保溫3 min；（b）保溫9 min
Figure 5. Orientation distribution function of the Zr–4 sheet after annealing at different holding times at 580 °C: (a) holding 3 min；(b) holding 9 min
圖 6 不同應力退火處理后Zr–4板材取向成像圖。（a） 冷軋態；（b） 580 ℃，0 MPa；（c） 580 ℃，3 MPa；（d） 580 ℃，9 MPa；（e） 610 ℃，0 MPa；（f） 610 ℃，3 MPa；（g） 610 ℃，9 MPa；（h） 640 ℃，0 MPa；（i） 640 ℃，3 MPa；（j）640 ℃，9 MPa
Figure 6. Orientation imaging of the Zr–4 sheet after different stress annealing treatments: (a) cold rolled sheet; (b) 580 ℃, 0 MPa；(c) 580 ℃, 3 MPa; (d) 580 ℃, 9 MPa; (e) 610 ℃, 0 MPa; (f) 610 ℃, 3 MPa; (g) 610 ℃, 9 MPa；(h) 640 ℃, 0 MPa; (i) 640 ℃, 3 MPa; (j) 640 ℃, 9 MPa
圖 7 不同應力退火處理后Zr–4板材再結晶晶粒尺寸分布圖。（a）冷軋態；（b）580 ℃，0 MPa；（c）580 ℃，3 MPa；（d）580 ℃，9 MPa；（e）610 ℃，0 MPa；（f）610 ℃，3 MPa；（g）610 ℃，9 MPa；（h）640 ℃，0 MPa；（i）640 ℃，3 MPa；（j）640 ℃，9 MPa
Figure 7. Recrystallization grain size distribution of Zr–4 plate after different stress annealing treatments: (a) cold rolled sheet; (b) 580 ℃, 0 MPa; (c) 580 ℃, 3 MPa; (d) 580 ℃, 9 MPa; (e) 610 ℃, 0 MPa; (f) 610 ℃, 3 MPa; (g) 610 ℃, 9 MPa; (h) 640 ℃, 0 MPa; (i) 640 ℃, 3 MPa; (j) 640 ℃, 9 MPa
圖 8 不同應力退火處理后Zr–4板材取向差分布圖。（a）冷軋態；（b） 580 ℃，0 MPa；（c） 580 ℃，3 MPa；（d） 580 ℃，9 MPa；（e） 610 ℃，0 MPa；（f）610 ℃，3 MPa；（g） 610 ℃，9 MPa；（h） 640 ℃，0 MPa；（i） 640 ℃，3 MPa；（j） 640 ℃，9 MPa
Figure 8. Zr–4 plate orientation difference distributions after different stress annealing treatments: (a) cold rolled sheet; (b) 580 ℃, 0 MPa; (c) 580 ℃, 3 MPa; (d) 580 ℃, 9 MPa; (e) 610 ℃, 0 MPa; (f) 610 ℃, 3 MPa; (g) 610 ℃, 9 MPa; (h) 640 ℃, 0 MPa; (i) 640 ℃, 3 MPa; (j) 640 ℃, 9 MPa
圖 9 不同應力退火處理后Zr–4板材再結晶比例統計圖
Figure 9. Statistical diagram denoting the recrystallization ratio of the Zr–4 sheet after different stress annealing treatments
表 1 實驗參數
Table 1. Experimental parameters
Annealing temperature/℃ Holding time/min External stress/MPa 580 3 0 580 3 3 580 6 3 580 3 9 610 3 0 610 3 3 610 3 9 640 3 0 640 3 3 640 3 9 
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表 2 不同應力退火處理后其小角度晶界比例統計結果
Table 2. Statistics of the proportion of small-angle grain boundaries after different stress annealing treatments
Annealing temperature/℃ External stress/MPa Small angle grain boundary ratio/% Rolled sheet 0 68 580 3 49 580 3 46 580 6 38 610 3 40 610 3 31 610 3 17 640 3 22 640 3 21 640 3 14
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