核石墨热解炭涂层的辐照损伤及熔盐浸渗特性的研究
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摘要
熔盐反应堆是第四代核能系统中六种反应堆型之一，具有固有安全性、核资源有效利用、防止核扩散、燃料循环、经济性等优点。核石墨具有低原子序数、高慢化比、高热导率和优良的机械性能等优势，可作为熔盐堆的中子慢化剂、反射体和堆芯支撑结构。在熔盐堆中，熔盐在核石墨通道内流通。核石墨是多孔材料，高温熔盐及裂变产物气体会扩散渗透到核石墨中，并影响其力学性能、热学性能及辐照寿命等。为了阻隔熔盐及裂变产物气体的扩散与渗透，我们与中国科学院金属研究所合作在核石墨表面沉积热解炭涂层。本论文研究了热解炭涂层的结构及性能、热解炭涂层前后核石墨与熔盐相容性、辐照缺陷对热解炭涂层与熔盐相容性的影响。
本论文利用同步辐射掠入射X射线衍射（GI-XRD）、场发射扫描电子显微镜（FE-SEM）、偏光显微镜（PLM）、高分辨的透射电子显微镜（HRTEM）研究了热解炭涂层的结构、石墨化度、孔径分布，同时采用透气性测试仪研究了热解炭涂层前后氦气渗透性，进行了静态熔盐实验来检验涂层前后核石墨与熔盐的相容性。实验结果揭示采用化学气相沉积技术在IG-110核石墨基底上沉积的热解炭涂层具有各向异性石墨化结构，结构致密、无裂纹，内部孔洞的孔径仅在纳米级别。热解炭涂层后核石墨的氦气渗透性降低至10-8cm2/s以下，能有效阻隔熔盐向核石墨中的渗透。
在熔盐堆堆芯中，热解炭涂层需承受辐照与熔盐的协同作用。本论文采用离子束辐照热解炭涂层，并采用FE-SEM、GI-XRD、TEM、拉曼和X射线光电子能谱（XPS）研究了辐照对热解炭结构的影响。实验结果揭示300keVAr+离子辐照使热解炭涂层中沿C轴方向的石墨相堆垛结构退化、石墨层间距变大。随着离子辐照剂量增加，热解炭涂层中的辐照损伤深度增加，在峰值剂量为0.26DPA时辐照损伤深度达到最大值，在辐照损伤区热解炭的晶体结构趋于无序，并在峰值剂量为1.58DPA时完全非晶。
对辐照后的热解炭涂层进行了静态熔盐实验，采用FE-SEM、拉曼、同步辐射近边X射线吸收精细结构（NEXAFS）和XPS研究了辐照缺陷对热解炭涂层与熔盐相容性的影响。实验结果揭示熔盐使热解炭涂层表面形成C-F键，辐照产生的缺陷进一步促进了热解炭涂层在熔盐中的氟化。
The Molten Salt Reactor (MSR) is one of the six reactors proposed by the Generation IVNuclear Energy System, with advantages of inherent safety, effective utilization of nuclearpower and nuclear nonproliferation, unique fuel cycle capabilities, economics, and so on.Nuclear graphite has been used as neutron moderator and structural material in MSR due to itslow Z, high moderating ratio, high thermal conductivity, mechanical strength and etc. Nucleargraphite is porous material. In MSR, molten salt flows through the nuclear graphite channels.Molten salt and gas fission product (primary, Xe-135) maybe diffuse into nuclear graphite, whichmaybe effect mechanical, thermal and irradiation properties of nuclear graphite, and so on.Therefore, we cooperated with the Institute of Metal Research (IMR), Chinese Academy ofSciences (CAS) to prepare pyrolytic carbon (PyC) coating to seal nuclear graphite. In this thesis,the structures and properties of PyC coating have been studied before and after ion irradiationand static FLiNaK molten salt experiments.
In this thesis, synchrotron-based grazing incidence X-ray diffraction (GI-XRD),field-emission scanning electron microscopy (FE-SEM), polarized light microscopy(PLM) andhigh resolution transmission electron microscopy (HRTEM) were used to study themicrotopography, degree of graphitization, distribution of pore diameter in PyC coating.Meanwhile, static FLiNaK molten salt experiments and helium gas permeability were performed.Results show that PyC coating prepared by thermal chemical vapor deposition (CVD) exhibitsanisotropic with nano pores. There is no obvious crack in PyC coating, which make the gaspermeability of IG-110nuclear graphite decreased to less than10-8cm2/s. Therefore, it’s possiblefor PyC coating to decrease the diffusion of gases into nuclear graphite.
In the core of MSR, nuclear graphite with PyC coating is irradiated by neutron and fissionproducts in molten salt. In this thesis, ion beam irradiation was used to induce defects in PyCcoating. FE-SEM, synchrotron-based GI-XRD, Raman, XPS and TEM were employed to studythe microstructure of PyC before and after ion irradiation. Results reveal that300keV Ar+ionirradiation leads to the structural deterioration along c axis and the increase of interlayerspacing of graphite. The damage depth in PyC coating increases with the increase of irradiationdose and reaches the maximum at the peak damage dose of0.26DPA. The surface crystalstructure in the irradiation damage zone of PyC coating tends to disorder with the increase ofirradiation dose and amorphous at the peak damage dose of1.58DPA.
Static FLiNaK molten salt experiments, FE-SEM, Raman spectroscopy, near-edge X-rayabsorption fine structure (NEXAFS) spectroscopy and XPS were performed to study the effect ofirradiation defect on the compatibility of PyC coating with FLiNaK salt. Results reveal that thereare C-F bond forming in the PyC coating after FLiNaK experiment. And results suggest thatirradiation defects maybe increase the fluorination of PyC coating in FLiNaK salt.
本论文利用同步辐射掠入射X射线衍射（GI-XRD）、场发射扫描电子显微镜（FE-SEM）、偏光显微镜（PLM）、高分辨的透射电子显微镜（HRTEM）研究了热解炭涂层的结构、石墨化度、孔径分布，同时采用透气性测试仪研究了热解炭涂层前后氦气渗透性，进行了静态熔盐实验来检验涂层前后核石墨与熔盐的相容性。实验结果揭示采用化学气相沉积技术在IG-110核石墨基底上沉积的热解炭涂层具有各向异性石墨化结构，结构致密、无裂纹，内部孔洞的孔径仅在纳米级别。热解炭涂层后核石墨的氦气渗透性降低至10-8cm2/s以下，能有效阻隔熔盐向核石墨中的渗透。
在熔盐堆堆芯中，热解炭涂层需承受辐照与熔盐的协同作用。本论文采用离子束辐照热解炭涂层，并采用FE-SEM、GI-XRD、TEM、拉曼和X射线光电子能谱（XPS）研究了辐照对热解炭结构的影响。实验结果揭示300keVAr+离子辐照使热解炭涂层中沿C轴方向的石墨相堆垛结构退化、石墨层间距变大。随着离子辐照剂量增加，热解炭涂层中的辐照损伤深度增加，在峰值剂量为0.26DPA时辐照损伤深度达到最大值，在辐照损伤区热解炭的晶体结构趋于无序，并在峰值剂量为1.58DPA时完全非晶。
对辐照后的热解炭涂层进行了静态熔盐实验，采用FE-SEM、拉曼、同步辐射近边X射线吸收精细结构（NEXAFS）和XPS研究了辐照缺陷对热解炭涂层与熔盐相容性的影响。实验结果揭示熔盐使热解炭涂层表面形成C-F键，辐照产生的缺陷进一步促进了热解炭涂层在熔盐中的氟化。
The Molten Salt Reactor (MSR) is one of the six reactors proposed by the Generation IVNuclear Energy System, with advantages of inherent safety, effective utilization of nuclearpower and nuclear nonproliferation, unique fuel cycle capabilities, economics, and so on.Nuclear graphite has been used as neutron moderator and structural material in MSR due to itslow Z, high moderating ratio, high thermal conductivity, mechanical strength and etc. Nucleargraphite is porous material. In MSR, molten salt flows through the nuclear graphite channels.Molten salt and gas fission product (primary, Xe-135) maybe diffuse into nuclear graphite, whichmaybe effect mechanical, thermal and irradiation properties of nuclear graphite, and so on.Therefore, we cooperated with the Institute of Metal Research (IMR), Chinese Academy ofSciences (CAS) to prepare pyrolytic carbon (PyC) coating to seal nuclear graphite. In this thesis,the structures and properties of PyC coating have been studied before and after ion irradiationand static FLiNaK molten salt experiments.
In this thesis, synchrotron-based grazing incidence X-ray diffraction (GI-XRD),field-emission scanning electron microscopy (FE-SEM), polarized light microscopy(PLM) andhigh resolution transmission electron microscopy (HRTEM) were used to study themicrotopography, degree of graphitization, distribution of pore diameter in PyC coating.Meanwhile, static FLiNaK molten salt experiments and helium gas permeability were performed.Results show that PyC coating prepared by thermal chemical vapor deposition (CVD) exhibitsanisotropic with nano pores. There is no obvious crack in PyC coating, which make the gaspermeability of IG-110nuclear graphite decreased to less than10-8cm2/s. Therefore, it’s possiblefor PyC coating to decrease the diffusion of gases into nuclear graphite.
In the core of MSR, nuclear graphite with PyC coating is irradiated by neutron and fissionproducts in molten salt. In this thesis, ion beam irradiation was used to induce defects in PyCcoating. FE-SEM, synchrotron-based GI-XRD, Raman, XPS and TEM were employed to studythe microstructure of PyC before and after ion irradiation. Results reveal that300keV Ar+ionirradiation leads to the structural deterioration along c axis and the increase of interlayerspacing of graphite. The damage depth in PyC coating increases with the increase of irradiationdose and reaches the maximum at the peak damage dose of0.26DPA. The surface crystalstructure in the irradiation damage zone of PyC coating tends to disorder with the increase ofirradiation dose and amorphous at the peak damage dose of1.58DPA.
Static FLiNaK molten salt experiments, FE-SEM, Raman spectroscopy, near-edge X-rayabsorption fine structure (NEXAFS) spectroscopy and XPS were performed to study the effect ofirradiation defect on the compatibility of PyC coating with FLiNaK salt. Results reveal that thereare C-F bond forming in the PyC coating after FLiNaK experiment. And results suggest thatirradiation defects maybe increase the fluorination of PyC coating in FLiNaK salt.
引文
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