胡小刚,董闯,陈宝清,杨红艳,张瑞谦,谷伟,陈大民.电弧离子镀制备耐事故包壳材料厚Cr涂层及高温抗氧化性能[J].表面技术,2019,48(2):207-219.
HU Xiao-gang,DONG Chuang,CHEN Bao-qing,YANG Hong-yan,ZHANG Rui-qian,GU Wei,CHEN Da-min.Preparation and High Temperature Oxidation Resistance of Thick Cr Coated on Zr-4 Alloy by Cathodic Arc Deposition for Accident Tolerant Fuel Claddings[J].Surface Technology,2019,48(2):207-219
电弧离子镀制备耐事故包壳材料厚Cr涂层及高温抗氧化性能
Preparation and High Temperature Oxidation Resistance of Thick Cr Coated on Zr-4 Alloy by Cathodic Arc Deposition for Accident Tolerant Fuel Claddings
投稿时间:2018-10-06  修订日期:2019-02-20
DOI:10.16490/j.cnki.issn.1001-3660.2019.02.030
中文关键词:  Cr涂层  厚膜  弧沉积  高温抗氧化  Zr-O通道  耐事故包壳材料
英文关键词:Cr  thick coating  high temperature oxidation  Zr-O channels  ATF
基金项目:
作者单位
胡小刚 1.大连理工大学 三束材料改性教育部重点实验室,辽宁 大连 116024 
董闯 1.大连理工大学 三束材料改性教育部重点实验室,辽宁 大连 116024 
陈宝清 1.大连理工大学 三束材料改性教育部重点实验室,辽宁 大连 116024 
杨红艳 2.中国核动力研究设计院 反应堆燃料及材料重点实验室,成都 610200 
张瑞谦 2.中国核动力研究设计院 反应堆燃料及材料重点实验室,成都 610200 
谷伟 3.大连纳晶科技有限公司,辽宁 大连 116600 
陈大民 3.大连纳晶科技有限公司,辽宁 大连 116600 
AuthorInstitution
HU Xiao-gang 1.Key Lab of Materials Modification by Laser, Ion, and Electron Beams (Ministry of Education), Dalian University of Tech-nology, Dalian 116024, China 
DONG Chuang 1.Key Lab of Materials Modification by Laser, Ion, and Electron Beams (Ministry of Education), Dalian University of Tech-nology, Dalian 116024, China 
CHEN Bao-qing 1.Key Lab of Materials Modification by Laser, Ion, and Electron Beams (Ministry of Education), Dalian University of Tech-nology, Dalian 116024, China 
YANG Hong-yan 2.Key Lab of Reactor Fuel and Materials, Nuclear Power Institute of China, Chengdu 610200, China 
ZHANG Rui-qian 2.Key Lab of Reactor Fuel and Materials, Nuclear Power Institute of China, Chengdu 610200, China 
GU Wei 3.Dalian Nano-Crystal Technology Co., Ltd, Dalian 116600, China 
CHEN Da-min 3.Dalian Nano-Crystal Technology Co., Ltd, Dalian 116600, China 
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中文摘要:
      目的 在Zr-4包壳材料表面制备具有耐事故高温性能的抗氧化厚Cr涂层,保护Zr基体,以防止与高温水蒸汽反应。方法 采用自主研发的φ155 mm大弧源电弧离子镀技术在Zr-4合金表面制备约20 μm的Cr涂层,通过X射线衍射仪(XRD)分析氧化前后的物相变化,通过扫描电子显微镜(SEM)和电子探针(EPMA)研究厚Cr涂层在不同温度下产生的多种缺陷,探究厚Cr涂层对Zr基体的防护机制。结果 当涂层沉积速率>3 μm/h,制备的Cr涂层均匀致密,结合力优异,具有柱状晶结构,可经受至少15.8%的形变量,其抗塑性形变能力优异。沉积Cr层样品经过1000、1100、1200 ℃氧化,保温1 h后快速冷却至室温,厚Cr涂层分化为CrOx层、Cr2O3层、残余Cr层和Cr-Zr扩散层。经受苛刻条件(1200 ℃/3600 s)测试,除保持连续性的氧化层外,在基体上仍残余良好结合的6.8 μm Cr层。氧化层两次开裂阻止基体被进一步破坏。Cr-Zr扩散层是由Zr元素向Cr涂层方向渗透生长的。1200 ℃时,在基体近表面处产生的大尺寸隆起,是由于在近表面处韧性β-Zr(O)相转变为脆性α-Zr相,以及Cr偏聚贫Sn造成的。残余Cr层的柱状晶结构会形成Zr-O扩散通道,对涂层最后失效将起关键作用。结论 Zr合金包壳材料镀覆20 μm的Cr涂层具有充分的耐事故能力,在严苛的事故条件测试下,各缺陷均未能使Zr-4合金基体暴露,涂层能够形成有效壁垒,防止锆合金基体暴露造成核事故,阻止基体进一步被破坏。
英文摘要:
      The work aims to prepare thick oxidation resistance Cr coating with high-temperature accident tolerance on Zr-4 fuel claddings (ATF), so as to protect Zr substrate from exposure to high temperature steam vapor. A 20 μm Cr was prepared by a home-made φ155 mm large arc-source on Zr-4 alloy substrate (>3 μm/h). Phase composition before and after oxidation was analyzed by X-ray diffraction (XRD) and defects generated at different temperature were analyzed by scanning electron microscope (SEM) and electron probe micro-analyzer (EPMA) to investigate the protective mechanism of Cr coating to Zr substrate. When deposition rate was >3 μm/h, the Cr coating was uniform and dense with excellent resultant force and columnar crystal structure and could withstand at least 15.8% of plastic deformation and had better plastic deformation ability. After coated samples were oxidized at 1000 °C, 1100 ℃, and 1200 ℃ for 1 h and cooled in air down to room temperature (RT), the thick Cr coating turned into four sublayers to protect the Zr-4 substrate: outer CrOx layer, inner Cr2O3 layer, residual Cr layer, and Cr-Zr diffusion layer. Even after the toughest test (1200 ℃/3600 s), except the outer oxide layer remaining continuous adhesion to the Zr-4 alloy, a 6.8 μm residual Cr layer still existed on the substrate. Twice oxide ruptures were formed to prevent the further damage. The Cr-Zr diffusion layer was formed by Zr element permeating to the Cr coating. The formation of sub-surface voids were clearly related to brittle α-Zr(O) turned by β-Zr(O) and Sn/Cr segregations near the surface. Zr-O channels formed by columnar crystal structure of residual Cr layer were the key factors of coatings failure. The ~20 μm Cr coating cladded on Zr alloy has sufficient accident tolerance. Zr-4 alloy substrate is not exposed under severe accident condition for all flaws. The thick Cr coating can create effective barriers to prevent the zirconium alloy substrate from causing nuclear accident and avoid further damage to the substrate.
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