中子辐照6H-SiC热力学及辐照缺陷高温回复动力学

doi:10.15541/jim20250216

无机材料学报 ›› 2026, Vol. 41 ›› Issue (3): 311-321.DOI: 10.15541/jim20250216 CSTR: 32189.14.jim20250216

中子辐照6H-SiC热力学及辐照缺陷高温回复动力学

朱飞¹(), 郝旭洁¹, 张全贵¹, 闫新越¹, 刘洪飞¹, 张博², 李欣³, 刘德峰³, 妥雅勇¹, 张守超¹()

1.天津城建大学理学院, 天津 300384
2.天津城建大学材料科学与工程学院, 天津 300384
3.北京长城航空测控技术研究所状态监测特种传感技术航空科技重点实验室, 北京 101111

收稿日期:2025-05-19 修回日期:2025-07-01 出版日期:2025-07-16 网络出版日期:2025-07-16
通讯作者: 张守超, 教授. E-mail: zhshch@tcu.edu.cn
作者简介:朱飞(1983-), 男, 实验师. E-mail: zhufei2012@tcu.edu.cn
基金资助:
国家级大学生创新创业训练计划(202510792019)

Irradiation Defects in Neutron-irradiated 6H-SiC: Thermodynamic and High-temperature Recovery Kinetics

ZHU Fei¹(), HAO Xujie¹, ZHANG Quangui¹, YAN Xinyue¹, LIU Hongfei¹, ZHANG Bo², LI Xin³, LIU Defeng³, TUO Yayong¹, ZHANG Shouchao¹()

1. School of Science, Tianjin Chengjian University, Tianjin 300384, China
2. School of Materials Science and Engineering, Tianjin Chengjian University, Tianjin 300384, China
3. Aviation Key Laboratory of Science and Technology on Special Condition Monitoring Sensor Technology, Beijing Changcheng Aeronautic Measurement and Control Technology Research Institute, Beijing 101111, China

Received:2025-05-19 Revised:2025-07-01 Published:2025-07-16 Online:2025-07-16
Contact: ZHANG Shouchao, professor. E-mail: zhshch@tcu.edu.cn
About author:ZHU Fei (1983-), male, engineer. E-mail: zhufei2012@tcu.edu.cn
Supported by:
National Undergraduate Training Program for Innovation and Entrepreneurship(202510792019)

摘要/Abstract

摘要：

碳化硅(SiC)是核反应堆结构的重要候选材料, 其辐照损伤行为与高温回复机制直接影响材料的服役性能与寿命。为阐明中子辐照对掺氮(氮掺杂浓度N_D≈3.0×10¹⁹ cm^-3)6H-SiC性能的影响及缺陷高温回复机制, 本研究系统探究了中子辐照(辐照温度约150 ℃, 辐照剂量2.58×10²⁰ n/cm²)和等时退火过程中的缺陷演化与热力学行为。结合不同表征技术和第一性原理计算, 深入解析了材料结构与性能的演变规律, 主要结果如下。(1) 辐照引发晶格显著肿胀(a、c轴及晶胞体积V的肿胀率分别为0.416%、0.430%和1.310%), 晶体保持单晶结构。(2) 辐照使比热增加14.7%, 并在100~500 ℃升温过程中释放375.4 J/g的辐照储能。(3) 基于晶胞参数回复与拉曼光谱演化, 揭示了缺陷高温回复的四阶段动力学(室温(RT)~600 ℃阶段以C-Frenkel近距复合为主, 迁移能E_a=0.14 eV; 600~850 ℃阶段涉及Si-Frenkel复合及碳间隙原子迁移, E_a=0.26 eV; 850~1200 ℃阶段为空位迁移驱动的晶格重构, E_a=0.65 eV; 1200~1500 ℃阶段为碳空位(V_C)长程扩散及N_CV_Si复合体解离, E_a=1.50 eV)。(4) 拉曼与荧光光谱结果确认氮掺杂形成N_CV_Si缺陷构型, 在785 nm激发下产生826 nm特征发光峰(对应634 cm^-1拉曼位移)。本研究揭示了中子辐照6H-SiC的缺陷回复路径与迁移能, 阐明了其热力学响应与高温回复动力学机制, 为核用SiC材料的辐照损伤评估、性能预测及退火工艺优化提供了重要依据。

关键词: 辐照储能, 比热, 拉曼光谱, 缺陷发光, 阿伦尼乌斯

Abstract:

Silicon carbide (SiC) is a promising material for nuclear reactor structures due to its excellent radiation resistance and high-temperature performance. The behavior of irradiation damage and the mechanisms of high-temperature recovery in SiC directly affect its service performance and longevity in nuclear environments. This study investigated effects of neutron irradiation on properties of 6H-SiC, with a particular focus on high-temperature recovery mechanisms of irradiation-induced defects. Specifically, defect evolution and thermodynamic responses in nitrogen-doped (N_D≈3.0×10¹⁹ cm^-3) 6H-SiC subjected to neutron irradiation at about 150 ℃ and a fluence of 2.58×10²⁰ n/cm² followed by isochronal annealing were examined. Integrated techniques and first-principles calculations were employed to comprehensively analyze its structural and property evolution. The key findings were as follows. (1) Significant lattice swelling was observed during the irradiation, with a swelling rate of 0.416% along the a-axis, 0.430% along the c-axis, and 1.310% in the unit cell volume, while all maintaining integrity of the single-crystalline structure. (2) A 14.7% increase in specific heat capacity was recorded, with 375.4 J/g of stored irradiation energy being released during heating from 100 ℃ to 500 ℃. (3) A four-stage defect recovery kinetic model was proposed based on the recovery of lattice parameters and the evolution of Raman spectra: Stage I (room temperature (RT)-600 ℃), primarily dominated by close-range recombination of carbon Frenkel pairs driven by migration energy (E_a) of 0.14 eV; Stage II (600-850 ℃), recombination of silicon Frenkel pairs and migration of carbon interstitials (E_a=0.26 eV); Stage III (850-1200 ℃), lattice reconstruction (E_a=0.65 eV); Stage IV (1200-1500 ℃), long-range diffusion of carbon vacancies (V_C) and dissociation of N_CV_Si complexes (E_a=1.50 eV). (4) The presence of nitrogen-stabilized N_CV_Si defect configurations was confirmed by a characteristic emission peak at 826 nm (634 cm^-1 Raman shift) when excited with 785 nm light. This study quantitatively reveals the defect recovery pathways and migration energies in neutron-irradiated 6H-SiC, providing a critical foundation for evaluating radiation damage, predicting performance, and optimizing annealing processes in nuclear-grade SiC materials.

Key words: irradiation-induced energy storage, specific heat, Raman spectroscopy, defect luminescence, Arrhenius

中图分类号:

朱飞, 郝旭洁, 张全贵, 闫新越, 刘洪飞, 张博, 李欣, 刘德峰, 妥雅勇, 张守超. 中子辐照6H-SiC热力学及辐照缺陷高温回复动力学[J]. 无机材料学报, 2026, 41(3): 311-321.

ZHU Fei, HAO Xujie, ZHANG Quangui, YAN Xinyue, LIU Hongfei, ZHANG Bo, LI Xin, LIU Defeng, TUO Yayong, ZHANG Shouchao. Irradiation Defects in Neutron-irradiated 6H-SiC: Thermodynamic and High-temperature Recovery Kinetics[J]. Journal of Inorganic Materials, 2026, 41(3): 311-321.

图/表 11

图1 (a, b) 6H-SiC晶胞参数和(c, d) (006)晶面衍射峰随退火温度的变化

Fig. 1 Variations of (a, b) 6H-SiC unit cell parameters and (c, d) (006) crystal plane diffraction peak with annealing temperature

图2 6H-SiC辐照损伤及退火回复的TEM照片与SAED图案

Fig. 2 TEM images and SAED patterns of 6H-SiC showing irradiation damage and annealing recovery (a) Unirradiated sample; (b) Irradiated sample; (c) 900 ℃ annealed sample after irradiation

图3 6H-SiC表面微观形貌SEM照片

Fig. 3 SEM images of 6H-SiC surface microstructures (a)Unirradiated sample; (b) Neutron-irradiated sample; (c-f) Annealed at (c) 600, (d) 900, (e) 1200 and (f) 1500 ℃

图4 6H-SiC的(a) TG和(b) DSC曲线

Fig. 4 (a) TG and (b) DSC curves of 6H-SiC

图5 辐照及不同温度退火后6H-SiC比热随温度的变化

Fig. 5 Temperature dependence of specific heat capacity for neutron-irradiated and annealed 6H-SiC at different temperatures (a) 100-300 ℃; (b) 600-1500 ℃

图6 空位、间隙原子对SiC晶格比热的影响

Fig. 6 Impact of vacancy and interstitial defects on lattice specific heat of SiC

图7 6H-SiC的(a1, b1, c1, d1) C1s、(a2, b2, c2, d2) Si2p及(a3, b3, c3, d3) O1s XPS谱图

Fig. 7 (a1, b1, c1, d1) C1s, (a2, b2, c2, d2) Si2p and (a3, b3, c3, d3) O1s XPS spectra of 6H-SiC (a1-a3) Unirradiated; (b1-b3) Irradiated; (c1-c3) Annealed at 600 ℃; (d1-d3) Annealed at 1500 ℃. Colorful figures are available on website

图8 6H-SiC的Raman光谱随退火温度的变化

Fig. 8 Temperature-dependent evolution of Raman spectra of 6H-SiC (a) Unirradiated, neutron-irradiated, and annealed below 900 ℃; (b) Annealed at 900-1500 ℃

图9 6H-SiC本征缺陷态密度及缺陷发光机理示意图

Fig. 9 Schematic diagrams of intrinsic defect states density and defect-induced photoluminescence mechanism in 6H-SiC (a) Total density of states with different intrinsic defects; (b) Defect-induced photoluminescence mechanism

图10 300~1500 ℃等温退火6H-SiC晶胞体积的自然对数变化量(lnV-lnV0)随退火时间的变化

Fig. 10 Variation of the natural logarithm change in unit cell volume (lnV-lnV0) of 6H-SiC with annealing time during isothermal annealing at 300-1500 ℃

图11 6H-SiC晶胞体积回复速率随退火温度变化的Arrhenius曲线

Fig. 11 Arrhenius plots of the unit cell volume recovery rate for 6H-SiC as a function of annealing temperature

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中子辐照6H-SiC热力学及辐照缺陷高温回复动力学

Irradiation Defects in Neutron-irradiated 6H-SiC: Thermodynamic and High-temperature Recovery Kinetics

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