室溫注氫Fe-Cr合金在不同溫度退火后位錯環的表征

杜玉峰; 崔麗娟; 萬發榮

doi:10.13374/j.issn2095-9389.2019.08.007

室溫注氫Fe-Cr合金在不同溫度退火后位錯環的表征

doi: 10.13374/j.issn2095-9389.2019.08.007

北京科技大學材料科學與工程學院, 北京 100083

基金項目:

國家自然科學基金資助項目 51471026

詳細信息

通訊作者:
萬發榮, E-mail: wanfr@mater.ustb.edu.cn

中圖分類號: TL62⁺7
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出版歷程
- 收稿日期: 2018-07-16
- 刊出日期: 2019-08-01

Characterization of dislocation loops in hydrogen ion-implanted Fe-Cr alloy annealed at different temperatures

School of Materials Science and Engineering, University of Science and Technology Beijing, Beijing 100083, China

More Information

Corresponding author: WAN Fa-rong, E-mail: wanfr@mater.ustb.edu.cn

摘要

摘要: 利用透射電子顯微鏡, 通過構建位錯環在不同晶帶軸下的投影圖結合位錯環消光判據, 對室溫注氫后Fe-9%Cr模型合金在400、500及550℃退火形成的1/2 〈111〉和〈100〉兩種類型的位錯環進行了表征. 實驗結果表明, 室溫注氫Fe-9%Cr合金中柏氏矢量為〈100〉型位錯環的數量隨著退火溫度的升高而逐漸增加. 在400和500℃退火后, 〈100〉型位錯環所占比例分別為16.48%、92.78%;當退火溫度升高到550℃時, 位錯環全部轉變為〈100〉型位錯環. Fe-9%Cr合金中位錯環類型轉變溫度區間為400~500℃, 與純鐵相比, 添加Cr元素能夠使位錯環類型轉變溫度升高.
- Fe-Cr合金 /
- 氫離子輻照 /
- 退火溫度 /
- 位錯環類型 /
- 透射電鏡
Abstract: Reduced-activation ferritic/martensitic (RAFM) steels, based on Fe-Cr alloys, have been considered to be one of the most promising candidate structural materials for future fusion reactors. Dislocation loops, as one of the most common microstructures induced by radiation, are the key factors in the deterioration of material properties. Dislocation loops with different Burgers vectors have different effects on material properties. Currently, a consensus exists suggesting that there are two kinds of dislocation loops with Burgers vectors of 1/2 〈111〉 and 〈100〉 in bcc iron-based alloys. In this study, the Burgers vectors of dislocation loops formed at the annealing temperatures of 400, 500, and 550℃ in hydrogen-ion implanted Fe-9%Cr model alloy were examined based on dislocation loop maps and dislocation loop invisibility criteria. Dislocation loop maps manifest such that under the 〈100〉 or 〈110〉 zone axes, it is easy to distinguish 1/2 〈111〉 and 〈100〉 edge dislocation loops, while under the 〈111〉 zone axis, the loops cannot be distinguished. By direct comparison between loop maps and loop images obtained through transmission electron microscope (TEM), the dislocation loops with Burgers vectors of 1/2 〈111〉 and 〈100〉, formed at different annealing temperatures, were characterized. The results of the characterization show that with increasing annealing temperature, the size of the dislocation loops increases while density decreases. Furthermore, the proportion of dislocation loops with a Burgers vector of 〈100〉 increases with rising temperature. After annealing at 400℃ and 500℃, the percentages of 〈100〉 type dislocation loops are 16.48% and 92.78% respectively, in hydrogen-ion implanted Fe-9%Cr alloy. While the temperature is raised to 550℃, all the dislocation loops are of 〈100〉 type loops. This indicates that the transition temperature range of dislocation loops in Fe-9%Cr is 400℃-500℃. Compared with pure iron, the presence of Cr element promotes the transition temperature of dislocation loops from 1/2 〈111〉 type to 〈100〉 type.
- Fe-Cr alloy /
- hydrogen implantation /
- annealing temperature /
- dislocation loops /
- transmission electron microscope

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圖 1 由SRIM2008軟件模擬計算得到的注氫后Fe-9%Cr合金中的輻照損傷量及氫離子濃度分布

Figure 1. Displacement damage and hydrogen concentration profile in Fe-9%Cr model alloy after 30 keV hydrogen ion irradiation calculated using SRIM-2008

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圖 2 1/2 [111] (111)型位錯環在(001)面上的投影示意圖

Figure 2. Illustration of 1/2 [111] (111) loop projection on a (001) plane

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圖 3 1/2 〈111〉和〈100〉型位錯環在[001]晶帶軸下的投影示意圖

Figure 3. Schematic map of 1/2 〈111〉 and 〈100〉 loops projected along the [001] zone axis

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圖 4 1/2 〈111〉和〈100〉型位錯環在[011]晶帶軸下的投影示意圖

Figure 4. Schematic map of 1/2 〈111〉 and 〈100〉 loops projected along the [011] zone axis

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圖 5 1/2 〈111〉和〈100〉型位錯環在[111]晶帶軸下的投影示意圖

Figure 5. Schematic map of 1/2 〈111〉 and 〈100〉 loops projected along the [111] zone axis

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圖 6 氫離子輻照前后Fe-9%Cr合金顯微組織. (a) 輻照前; (b) 輻照后

Figure 6. Microstructures of Fe-9%Cr: (a) before hydrogen implantation; (b) after hydrogen implantation

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圖 7 注氫Fe-9%Cr合金在400 ℃退火后的相關圖像. (a) 衍射花樣; (b) 位錯環在[001]晶帶軸下，衍射矢量g =[200]的明場像; (c) 對應的位錯環投影示意圖(考慮g·b =0不可見判據)

Figure 7. Images of hydrogen ion implanted Fe-9%Cr alloy after annealing at 400 ℃: (a) the diffraction pattern; (b) the bright-field image with diffraction vector g =[200] under the [001] zone axis; (c) the corresponding dislocation loop map under the [001] zone axis (considering g·b =0 invisibility criterion)

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圖 8 注氫Fe-9%Cr合金在400 ℃退火后的相關圖像. (a) 衍射花樣; (b) 位錯環在[001]晶帶軸下，衍射矢量g =[020]的明場像; (c) 對應的位錯環投影示意圖(考慮g·b =0不可見判據)

Figure 8. Images of hydrogen ion implanted Fe-9%Cr alloy after annealing at 400 ℃: (a) the diffraction pattern; (b) the bright-field image with diffraction vector g =[020] under the [001] zone axis; (c) the corresponding dislocation loop map under the [001] zone axis (considering g·b =0 invisibility criterion)

下載: 全尺寸圖片幻燈片

圖 9 注氫Fe-9%Cr合金在400 ℃退火后的相關圖像. (a) 衍射花樣; (b) 位錯環在[001]晶帶軸下，衍射矢量g =[110]的明場像; (c) 對應的位錯環投影示意圖(考慮g·b =0不可見判據)

Figure 9. Images of hydrogen ion implanted Fe-9%Cr alloy after annealing at 400 ℃: (a) the diffraction pattern; (b) the bright-field image with diffraction vector g =[110] under the [001] zone axis; (c) the corresponding dislocation loop map under the [001] zone axis (considering g·b =0 invisibility criterion)

下載: 全尺寸圖片幻燈片

圖 10 注氫Fe-9%Cr合金在400 ℃退火后的相關圖像. (a) 衍射花樣; (b) 位錯環在[001]晶帶軸下，衍射矢量g =[110]的明場像; (c) 對應的位錯環投影示意圖(考慮g·b =0不可見判據)

Figure 10. Images of hydrogen ion implanted Fe-9%Cr alloy after annealing at 400 ℃: (a) the diffraction pattern; (b) the bright-field image with diffraction vector g =[110] under the [001] zone axis; (c) the corresponding dislocation loop map under the [001] zone axis (considering g·b =0 invisibility criterion)

下載: 全尺寸圖片幻燈片

圖 11 注氫Fe-9%Cr合金在500 ℃退火后的相關圖像. (a) 衍射花樣; (b) 位錯環在[011]晶帶軸下，衍射矢量g =[200]的明場像; (c) 對應的位錯環投影示意圖(考慮g·b =0不可見判據)

Figure 11. Images of hydrogen ion implanted Fe-9%Cr alloy after annealing at 500 ℃: (a) the diffraction pattern; (b) the bright-field image with diffraction vector g =[200]under the [011] zone axis; (c) the corresponding dislocation loop map under the [011] zone axis (considering g·b =0 invisibility criterion)

下載: 全尺寸圖片幻燈片

圖 12 注氫Fe-9%Cr合金在500 ℃退火后的相關圖像. (a) 衍射花樣; (b) 位錯環在[011]晶帶軸下，衍射矢量g =[011]的明場像; (c) 對應的位錯環投影示意圖(考慮g·b =0不可見判據)

Figure 12. Images of hydrogen ion implanted Fe-9%Cr alloy after annealing at 500 ℃: (a) the diffraction pattern; (b) the bright-field image with diffraction vector g =[011] under the [011] zone axis; (c) the corresponding dislocation loop map under the [011] zone axis (considering g·b =0 invisibility criterion)

下載: 全尺寸圖片幻燈片

圖 13 注氫Fe-9%Cr合金在550 ℃退火后的相關圖像. (a) 衍射花樣; (b) 位錯環在[001]晶帶軸下，衍射矢量g =[110]的明場像; (c) 對應的位錯環投影示意圖(考慮g·b =0不可見判據)

Figure 13. Images of hydrogen ion implanted Fe-9%Cr alloy after annealing at 550 ℃: (a) the diffraction pattern; (b) the bright-field image with diffraction vector g =[110] under the [001] zone axis; (c) the corresponding dislocation loop map under the [001] zone axis (considering g·b =0 invisibility criterion)

下載: 全尺寸圖片幻燈片

圖 14 注氫Fe-9% Cr合金在550 ℃退火后的相關圖像. (a) 衍射花樣; (b) 位錯環在[011]晶帶軸下，衍射矢量g =[011]的明場像; (c) 對應的位錯環投影示意圖(考慮g·b =0不可見判據)

Figure 14. Images of hydrogen ion implanted Fe-9%Cr alloy after annealing at 550 ℃: (a) the diffraction pattern; (b) the bright-field image with diffraction vector g =[011] under the [011] zone axis; (c) the corresponding dislocation loop map under the [011] zone axis (considering g·b =0 invisibility criterion)

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圖 15 注氫Fe-9%Cr合金在400，500，550 ℃退火后形成的1/2 〈111〉和〈100〉間隙型位錯環的數目以及〈100〉型位錯環所占比例

Figure 15. Number and proportion of 1/2 〈111〉 and 〈100〉 dislocation loops in hydrogen ion implanted Fe-9%Cr alloy after annealing at 400, 500 and 550 ℃

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表 1 Fe-Cr合金化學成分(質量分數)

Table 1. Chemical composition of Fe-Cr alloy ?%

Cr	C	N	Fe
9.43	0.013	0.008	余量

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表 2 〈100〉和1/2 〈111〉位錯環在[001]晶帶軸下觀察時位錯環的慣習面與投影面的晶體學信息

Table 2. Crystallographic information between dislocation-loop habit planes and the (100) plane when imaged under the [001] zone axis

位錯環柏氏矢量，b	慣習面	夾角，θ/(°)	cosθ	交線方向
[100]	(100)	90	0	[010]
[010]	(010)	90	0	[100]
[001]	(001)	0	1	平行
[111]	(111)	54.74	0.58	[110]
[111]	(111)	54.74	0.58	[110]
[111]	(111)	54.74	0.58	[110]
[111]	(111)	54.74	0.58	[110]

下載: 導出CSV

表 3 〈100〉和1/2 〈111〉位錯環在[011]晶帶軸下觀察時位錯環的慣習面與投影面的晶體學信息

Table 3. Crystallographic information between dislocation-loop habit planes and the (011) plane when imaged under the [011] zone axis

位錯環柏氏矢量，b	慣習面	夾角，θ/(°)	cosθ	交線方向
[100]	(100)	90	0	[011]
[010]	(010)	45	0.71	[100]
[001]	(001)	45	0.71	[100]
[111]	(111)	35.26	0.82	[011]
[111]	(111)	35.26	0.82	[011]
[111]	(111)	90	0	[211]
[111]	(111)	90	0	[211]

下載: 導出CSV

表 4 〈100〉和1/2 〈111〉位錯環在[111]晶帶軸下觀察時位錯環的慣習面與投影面的晶體學信息

Table 4. Crystallographic information between dislocation-loop habit planes and the (111) plane when imaged under the [111] zone axis

位錯環柏氏矢量，b	慣習面	夾角，θ/(°)	cosθ	交線方向
[100]	(100)	54.74	0.58	[011]
[010]	(010)	54.74	0.58	[101]
[001]	(001)	54.74	0.58	[110]
[111]	(111)	0	1	平行
[111]	(111)	70.53	0.33	[011]
[111]	(111)	70.53	0.33	[101]
[111]	(111)	70.53	0.33	[110]

下載: 導出CSV

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