模拟核芯FCM燃料的振荡烧结行为研究

doi:10.15541/jim20230492

无机材料学报 ›› 2024, Vol. 39 ›› Issue (5): 501-508.DOI: 10.15541/jim20230492 CSTR: 32189.14.10.15541/jim20230492

所属专题：【结构材料】核用陶瓷（202409）

模拟核芯FCM燃料的振荡烧结行为研究

何宗倍¹(), 陈放¹, 刘佃光²(), 李统业¹, 曾强¹

1.中国核动力研究设计院核燃料元件及材料研究所, 成都 610213
2.西南交通大学材料科学与工程学院, 成都 610031

收稿日期:2023-10-23 修回日期:2023-12-30 出版日期:2024-05-20 网络出版日期:2024-01-08
通讯作者: 刘佃光, 副教授. E-mail: dianguang@swjtu.edu.cn
作者简介:何宗倍(1985-), 男, 博士. E-mail: hezongbei@126.com
基金资助:
装备预研重点实验室基金项目(6142A06200108);中核集团基础研究项目(CNNC-JCYJ-202218)

Sintering Behavior of Simulating Core FCM Fuel via Hot Oscillatory Pressing

HE Zongbei¹(), CHEN Fang¹, LIU Dianguang²(), LI Tongye¹, ZENG Qiang¹

1. Nuclear Fuel and Material Institute, Nuclear Power Institute of China, Chengdu 610213, China
2. School of Materials Science and Engineering, Southwest Jiaotong University, Chengdu 610031, China

Received:2023-10-23 Revised:2023-12-30 Published:2024-05-20 Online:2024-01-08
Contact: LIU Dianguang, associate professor. E-mail: dianguang@swjtu.edu.cn
About author:HE Zongbei (1985-), male, PhD. E-mail: hezongbei@126.com
Supported by:
National Defense Key Laboratory Foundation(6142A06200108);China National Nuclear Corporation Basic Research Foundation(CNNC-JCYJ-202218)

摘要/Abstract

摘要：

全陶瓷微封装弥散(FCM)燃料以其较好的固有安全性而成为核能领域研究的重点。针对SiC基体难以烧结的问题, 本研究利用振荡烧结具有加速传质和降低烧结温度的优势, 开展了模拟核芯FCM燃料振荡烧结行为研究, 重点考察了振荡烧结温度、振荡时间与振荡压力等参数对基体致密化行为的影响, 并与热压烧结结果进行了对比。结果表明, 振荡烧结温度、保温时间以及中值压力对基体致密化有重要影响, 而振荡压力的振幅对基体致密化影响不大。相比于热压烧结, 振荡烧结可以提高材料的致密度, 振荡烧结试样的致密度更高, 1850 ℃振荡烧结试样的致密度为99.99%; 振荡烧结试样的晶粒尺寸更小, 1850 ℃振荡烧结试样的晶粒尺寸为(284±4) nm, 比同等温度下热压烧结试样的晶粒尺寸减小~27%; 振荡烧结试样的硬度更高, 1850 ℃振荡烧结试样的硬度为(26.7±0.4) GPa。借助改进的热压烧结本构方程, 计算得到试样在致密度为90%时的应力指数n=1, 活化能Q=430 kJ/mol, 致密化的主导机制为晶界扩散协调的晶界滑移。

关键词: FCM燃料, SiC基体, 振荡烧结, 致密化机理

Abstract:

Fully ceramic micro-encapsulated (FCM) fuel has become the focus of nuclear energy research because of its good inherent safety. In order to overcome the difficulty of SiC matrix densification, this study focused on the sintering behavior of simulating core FCM fuel via hot oscillatory pressing (HOP), taking the advantages of HOP to accelerate mass transfer and reduce sintering temperature. The influence of oscillatory sintering temperature, oscillatory time and oscillatory pressure on the matrix densification behavior was studied, and the results were compared with those of hot pressing (HP). The results indicate that the oscillatory sintering temperature, holding time, and median pressure have important effects on matrix densification, while the amplitude of oscillatory pressure has little effect. Compared with HP, the density of the samples is increased by HOP, and the density of sample sintered at 1850 ℃ via HOP is 99.99%. The grain size of the samples via HOP is smaller, and the grain size of the sample sintered via HOP at 1850 ℃ is (284±4) nm, which is ~27% less than that of the sample sintered via HP at the same temperature. The hardness of the samples sintered via HOP is higher, and the hardness of the sample sintered via HOP at 1850 ℃ is (26.7±0.4) GPa. When the density of sample is 90%, the stress exponent n=1 and activation energy Q=430 kJ/mol are obtained by using the modified constitutive equation of HP. The dominant mechanism of densification is grain boundary sliding, which is accommodated by the grain boundary diffusion.

Key words: fully ceramic micro-encapsulated fuel, SiC matrix, hot oscillatory pressing, densification mechanism

中图分类号:

TL352

何宗倍, 陈放, 刘佃光, 李统业, 曾强. 模拟核芯FCM燃料的振荡烧结行为研究[J]. 无机材料学报, 2024, 39(5): 501-508.

HE Zongbei, CHEN Fang, LIU Dianguang, LI Tongye, ZENG Qiang. Sintering Behavior of Simulating Core FCM Fuel via Hot Oscillatory Pressing[J]. Journal of Inorganic Materials, 2024, 39(5): 501-508.

图/表 14

图1 振荡烧结工艺示意图

Fig. 1 Schematic diagram of hot oscillatory pressing

表1 模拟核芯FCM燃料的振荡烧结和热压烧结参数

Table 1 Sintering parameters of simulated core FCM fuel via hot oscillatory pressing and hot pressing

No.	T/℃	t/h	σ_m/MPa	σ_a/MPa
HOP-1	1600	1	20	5
HOP-2	1600	2	20	5
HOP-3	1650	1	20	5
HOP-4	1650	2	20	5
HOP-5	1700	1	20	5
HOP-6	1700	2	20	5
HOP-7	1750	0	20	5
HOP-8	1750	1	20	5
HOP-9	1750	2	20	5
HOP-10	1750	2	10	5
HOP-11	1750	2	15	5
HOP-12	1750	2	20	1
HOP-13	1750	2	20	3
HOP-14	1800	2	20	5
HOP-15	1850	2	20	5
HP-1	1700	2	20	0
HP-2	1750	2	20	0
HP-3	1800	2	20	0
HP-4	1850	2	20	0

图2 不同烧结温度下振荡烧结试样的致密化曲线

Fig. 2 Densification curves of samples sintered via hot oscillatory pressing at different temperatures (a) Relative density-time curves; (b) Densification rate-relative density curves

表2 不同保温时间下试样致密度及开气孔率

Table 2 Densities and open porosities of samples under different holding time

No.	T/℃	t/h	ρ/(g·cm^-3)	Open porosity/%	ρ_m/(g·cm^-3)
HOP-7	1750	0	2.65	26.57	2.04
HOP-8	1750	1	3.63	3.68	3.00
HOP-9	1750	2	3.75	1.48	3.13

图3 不同中值压力下振荡烧结试样的致密化曲线

Fig. 3 Densification curves of samples sintered via hot oscillatory pressing under different median pressures

图4 不同压力振幅下振荡烧结试样的致密化曲线

Fig. 4 Densification curves of samples sintered via hot oscillatory pressing at different pressure amplitudes

图5 不同温度下振荡烧结试样的XRD图谱

Fig. 5 XRD patterns of samples sintered via hot oscillatory pressing at different temperatures

图6 不同温度下振荡烧结和热压烧结试样的致密化曲线

Fig. 6 Densification curves of samples sintered via hot oscillatory pressing and hot pressing at different temperatures

图7 振荡烧结和热压烧结试样的晶粒尺寸随(a)烧结温度和(b)相对密度的变化曲线

Fig. 7 Grain size of samples sintered via hot oscillatory pressing and hot pressing as function of (a) sintering temperature and (b) relative density

图8 1850 ℃烧结试样断面SEM照片及其晶粒尺寸分布图

Fig. 8 SEM images of fracture surface and grain size distributions of samples sintered at 1850 ℃ (a, c) Hot oscillatory pressing (2 h-(20±5) MPa); (b, d) Hot pressing (2 h-20 MPa)

图9 振荡烧结和热压烧结试样的硬度随(a)烧结温度和(b)气孔率的变化曲线

Fig. 9 Hardness of samples sintered via hot oscillatory pressing and hot pressing as function of (a) sintering temperature and (b) porosity

图10 当n=1时振荡烧结试样的致密化速率-有效应力曲线

Fig. 10 Densification rate-effective stress plots of samples sintered via hot oscillatory pressing by taking n=1

表3 不同应力指数(n)下致密化速率-有效应力的相似度

Table 3 Similarity between densification rate and effective stress at different stress exponents (n)

T/℃	n=1	n=2	n=3
1700	0.9994	0.9740	0.9476
1750	0.9773	0.9986	0.9874
1800	0.9904	0.9647	0.9528
1850	0.9858	0.9742	0.9695

图11 不同温度下振荡烧结试样的Arrhenius关系曲线

Fig. 11 Arrhenius relationship curve of samples sintered via hot oscillatory pressing at different temperatures

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模拟核芯FCM燃料的振荡烧结行为研究

Sintering Behavior of Simulating Core FCM Fuel via Hot Oscillatory Pressing

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