CN108249927A - 一种fcm芯块无压致密化烧结方法 - Google Patents
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Abstract
本发明涉及核燃料芯块制备技术领域,具体公开了一种FCM芯块无压致密化烧结方法,包括步骤1,助烧剂添加;步骤2,FCM芯块生坯成型;步骤3,FCM芯块无压烧结。本发明与现有常规FCM烧结工艺相比,通过助烧剂的添加,实现了FCM芯块的无压致密化烧结,进而大大降低了FCM芯块的制备难度以及生产成本。同时,采用本发明方法能够大批量地进行FCM芯块的无压致密化烧结,且烧结完的芯块内部的TRISO颗粒结构保持完整,均匀分布于SiC基体内。
Description
技术领域
本发明属于核燃料芯块制备技术领域,具体涉及一种FCM芯块无压致密化烧结方法。
背景技术
FCM(Fully Ceramic Microencapsulated,全陶瓷微封装)燃料芯块作为一种重要的容错燃料,其概念由美国橡树岭国家实验室在2012年首先提出,是基于一种将三维结构同性TRISO(tri-structural isotropic)带涂层的颗粒嵌入SiC基体的燃料芯块。FCM芯块将TRISO颗粒封装在SiC基体中,TRISO颗粒为由内到外依次包覆疏松碳层、内致密碳层、SiC层和外致密碳层的UO2燃料颗粒。由于SiC基体兼具高稳定性和高热导率,同时与冷却剂有很好的兼容性,因此可很好地包容UO2燃料芯块释放出的裂变气体和腐蚀性裂变产物,加之TRISO颗粒本身即具有对裂解产物的多层防护,从而使整个核燃料元件适用于高燃耗反应堆,并在发生事故时容错性高,安全有保证。因而该燃料即是为轻水堆中使用的高燃耗铀所设计,优化反应堆通常及瞬时的操作性。
目前FCM芯块的烧结工艺一般为热压烧结,热压烧结只适用于小批量的实验室研究,不能进行大批量的应用,且烧结完的芯块表面会有石墨残留,不容易去除。
发明内容
本发明的目的在于提供一种FCM芯块无压致密化烧结方法,实现FCM芯块的无压致密化烧结。
本发明的技术方案如下:
一种FCM芯块无压致密化烧结方法,包括以下步骤:
步骤1,助烧剂添加;
步骤1.1,在SiC基体中添加助烧剂,添加量为6±0.5wt%,所述的助烧剂由几种稀土氧化物混合组成;
步骤1.2,进行湿法球磨,采用无水乙醇作为分散剂,不锈钢球作为研磨球,球料比为3~3.5:1,进行球磨2~3h,球磨后的粉末进行干燥处理,并对干燥后的粉末进行破碎、筛分,制得成型原料;
步骤2,FCM芯块生坯成型;
采用钢质模具进行双向成型,或者采用橡胶模具进行冷等静压成型;
步骤3,FCM芯块无压烧结;
通过高温烧结实现SiC收缩形成陶瓷,进而制备出全陶瓷封装芯块,烧结气氛为真空。
步骤3中,FCM芯块无压烧结的烧结制度如下:
(1)1~2小时由室温升至300~350℃,保温1~1.5小时;
(2)0.5~1小时升温至600~650℃,保温1~1.5小时;
(3)1.5~2小时升温至1400~1450℃,保温1~1.5小时;
(4)0.5~1小时升温至1700~1750℃,保温1~1.5小时;
(5)0.5~1小时升温至1950~2000℃,保温2~3小时;
(6)随炉冷却。
步骤2,采用钢质模具成型压力为2.0~3.0kN,升压速率为0.8~1.0KN/s,保压时间为10~15s。
步骤2,采用橡胶模具成型压强为160~250MPa,保压时间为10~15s。
步骤1.1中所述的助烧剂在高温下形成液相,从而促进碳化硅的烧结并实现材料的致密化。
步骤1.1,所述的助烧剂由Al2O3和Y2O3组成,其中Al2O3:Y2O3=1:1.5~4。
所得FCM芯块密度≥3.0g/cm3,FCM芯块内部的TRISO颗粒结构保持完整,均匀分布于SiC基体内。
本发明的显著效果在于:
(1)本发明与现有常规FCM烧结工艺相比,通过助烧剂的添加,实现了FCM芯块的无压致密化烧结,进而大大降低了FCM芯块的制备难度以及生产成本。
(2)采用本发明方法能够大批量地进行FCM芯块的无压致密化烧结,且烧结完的芯块内部的TRISO颗粒结构保持完整,均匀分布于SiC基体内。
具体实施方式
下面结合具体实施例对本发明作进一步详细说明。
一种FCM芯块无压致密化烧结方法,包括以下步骤:
步骤1,助烧剂添加。
步骤1.1,在SiC基体中添加助烧剂,添加量为6±0.5wt%,所述的助烧剂由几种稀土氧化物混合组成,例如由Al2O3和Y2O3组成,其中Al2O3:Y2O3=1:1.5~4。助烧剂在高温下很容易形成液相,从而促进碳化硅的烧结并实现材料的致密化。
步骤1.2,进行湿法球磨,采用无水乙醇作为分散剂,不锈钢球作为研磨球,球料比为3~3.5:1,进行球磨2~3h,球磨后的粉末进行干燥处理,并对干燥后的粉末进行破碎、筛分,制得成型原料。
步骤2,FCM芯块生坯成型
采用钢质模具进行双向成型,或者采用橡胶模具进行冷等静压成型。其中,采用钢质模具成型压力为2.0~3.0kN,升压速率为0.8~1.0KN/s,保压时间为10~15s;采用橡胶模具成型压强为160~250MPa,保压时间为10~15s。
步骤3,FCM芯块无压烧结
通过高温烧结实现SiC收缩形成陶瓷,进而制备出全陶瓷封装芯块,烧结气氛为真空,烧结制度如下:
(1)1~2小时由室温升至300~350℃,保温1~1.5小时;
(2)0.5~1小时升温至600~650℃,保温1~1.5小时;
(3)1.5~2小时升温至1400~1450℃,保温1~1.5小时;
(4)0.5~1小时升温至1700~1750℃,保温1~1.5小时;
(5)0.5~1小时升温至1950~2000℃,保温2~3小时;
(6)随炉冷却。
所得FCM芯块密度≥3.0g/cm3,FCM芯块内部的TRISO颗粒结构保持完整,均匀分布于SiC基体内。
实施例一
一种FCM芯块无压致密化烧结方法,包括以下步骤:
步骤1,助烧剂添加
步骤1.1,在SiC基体中添加Y2O3-Al2O3助烧剂,Y2O3与Al2O3的质量比为7:3,添加量为6±0.5wt%;
步骤1.2,进行湿法球磨,采用无水乙醇作为分散剂,不锈钢球作为研磨球,球料比为3:1,进行球磨2h,对球磨后的粉末进行干燥处理,并对干燥后的粉末进行破碎、筛分,制得成型原料;
步骤2,FCM生坯成型
采用钢质模具进行双向成型,成型压力为2.0kN,升压速率为0.8KN/s,保压时间为10s。
步骤3,FCM芯块的无压烧结
通过高温烧结实现SiC收缩形成陶瓷,进而制备出全陶瓷封装芯块,烧结气氛为真空,烧结制度如下所示:
(1)1小时由室温升至300℃,保温1小时;
(2)0.5小时升温至600℃,保温1小时;
(3)2小时升温至1400℃,保温1小时;
(4)0.5小时升温至1700℃,保温1小时;
(5)0.5小时升温至1950℃,保温2小时;
(6)随炉冷却。
所得FCM芯块密度≥3.0g/cm3,FCM芯块内部的TRISO颗粒结构保持完整,均匀分布于SiC基体内。
实施例二
一种FCM芯块无压致密化烧结方法,包括以下步骤:
步骤1,助烧剂添加
步骤1.1,在SiC基体中添加Y2O3-Al2O3助烧剂,Y2O3与Al2O3的质量比为4:1,添加量为6±0.5wt%;
步骤1.2,进行湿法球磨,采用无水乙醇作为分散剂,不锈钢球作为研磨球,球料比为3.5:1,进行球磨2.5h,对球磨后的粉末进行干燥处理,并对干燥后的粉末进行破碎、筛分,制得成型原料;
步骤2,FCM生坯成型
采用钢质模具进行双向成型,成型压力为2.6kN,升压速率为1.0KN/s,保压时间为13s。
步骤3,FCM芯块的无压烧结
通过高温烧结实现SiC收缩形成陶瓷,进而制备出全陶瓷封装芯块,烧结气氛为真空,烧结制度如下所示:
(1)1小时由室温升至320℃,保温1.5小时;
(2)1小时升温至650℃,保温1.5小时;
(3)1.5小时升温至1450℃,保温1小时;
(4)1小时升温至1750℃,保温1小时;
(5)1小时升温至2000℃,保温2.5小时;
(6)随炉冷却。
所得FCM芯块密度≥3.0g/cm3,FCM芯块内部的TRISO颗粒结构保持完整,均匀分布于SiC基体内。
实施例三
一种FCM芯块无压致密化烧结方法,包括以下步骤:
步骤1,助烧剂添加
步骤1.1,在SiC基体中添加Y2O3-Al2O3助烧剂,Y2O3与Al2O3的质量比为3:2,添加量为6±0.5wt%;
步骤1.2,进行湿法球磨,采用无水乙醇作为分散剂,不锈钢球作为研磨球,球料比为3:1,进行球磨3h,对球磨后的粉末进行干燥处理,并对干燥后的粉末进行破碎、筛分,制得成型原料;
步骤2,FCM生坯成型
采用橡胶模具进行冷等静压成型,成型压强为200MPa,保压时间为15s。
步骤3,FCM芯块的无压烧结
通过高温烧结实现SiC收缩形成陶瓷,进而制备出全陶瓷封装芯块,烧结气氛为真空,烧结制度如下所示:
(1)2小时由室温升至350℃,保温1.5小时;
(2)1小时升温至620℃,保温1.5小时;
(3)1.5小时升温至1400℃,保温1.5小时;
(4)1小时升温至1750℃,保温1小时;
(5)0.5小时升温至1950℃,保温3小时;
(6)随炉冷却。
所得FCM芯块密度≥3.0g/cm3,FCM芯块内部的TRISO颗粒结构保持完整,均匀分布于SiC基体内。上面对本发明的实施例作了详细说明,上述实施方式仅为本发明的最优实施例,但是本发明并不限于上述实施例,在本领域普通技术人员所具备的知识范围内,还可以在不脱离本发明宗旨的前提下作出各种变化。
Claims (7)
1.一种FCM芯块无压致密化烧结方法,其特征在于:包括以下步骤:
步骤1,助烧剂添加;
步骤1.1,在SiC基体中添加助烧剂,添加量为6±0.5wt%,所述的助烧剂由几种稀土氧化物混合组成;
步骤1.2,进行湿法球磨,采用无水乙醇作为分散剂,不锈钢球作为研磨球,球料比为3~3.5:1,进行球磨2~3h,球磨后的粉末进行干燥处理,并对干燥后的粉末进行破碎、筛分,制得成型原料;
步骤2,FCM芯块生坯成型;
采用钢质模具进行双向成型,或者采用橡胶模具进行冷等静压成型;
步骤3,FCM芯块无压烧结;
通过高温烧结实现SiC收缩形成陶瓷,进而制备出全陶瓷封装芯块,烧结气氛为真空。
2.如权利要求1所述的一种FCM芯块无压致密化烧结方法,其特征在于:步骤3中,FCM芯块无压烧结的烧结制度如下:
(1)1~2小时由室温升至300~350℃,保温1~1.5小时;
(2)0.5~1小时升温至600~650℃,保温1~1.5小时;
(3)1.5~2小时升温至1400~1450℃,保温1~1.5小时;
(4)0.5~1小时升温至1700~1750℃,保温1~1.5小时;
(5)0.5~1小时升温至1950~2000℃,保温2~3小时;
(6)随炉冷却。
3.如权利要求2所述的一种FCM芯块无压致密化烧结方法,其特征在于:步骤2,采用钢质模具成型压力为2.0~3.0kN,升压速率为0.8~1.0KN/s,保压时间为10~15s。
4.如权利要求2所述的一种FCM芯块无压致密化烧结方法,其特征在于:步骤2,采用橡胶模具成型压强为160~250MPa,保压时间为10~15s。
5.如权利要求1~4任一项所述的一种FCM芯块无压致密化烧结方法,其特征在于:步骤1.1中所述的助烧剂在高温下形成液相,从而促进碳化硅的烧结并实现材料的致密化。
6.如权利要求5所述的一种FCM芯块无压致密化烧结方法,其特征在于:步骤1.1,所述的助烧剂由Al2O3和Y2O3组成,其中Al2O3:Y2O3=1:1.5~4。
7.如权利要求6所述的一种FCM芯块无压致密化烧结方法,其特征在于:所得FCM芯块密度≥3.0g/cm3,FCM芯块内部的TRISO颗粒结构保持完整,均匀分布于SiC基体内。
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