核级锆的熔盐制备与回收研究进展

doi:10.6023/A25110360

化学学报 ›› 2026, Vol. 84 ›› Issue (3): 425-447.DOI: 10.6023/A25110360 上一篇下一篇

综述

核级锆的熔盐制备与回收研究进展

周铭宇^a^,^c, 刘乐彬^a^,^c, 梅雷^a, 刘雅兰^a^,^*(), 石伟群^b^,^*()

^a 中国科学院高能物理研究所核能放射化学实验室北京 100049
^b 上海交通大学机械与动力工程学院核燃料循环与核材料研究所上海 200030
^c 中国科学院大学化学科学学院北京 100049

投稿日期:2025-11-06 发布日期:2025-12-31
通讯作者: 刘雅兰, 石伟群

作者简介:

周铭宇, 中国科学院高能物理研究所博士研究生, 主要从事金属锆的熔盐电化学研究.

刘乐彬, 中国科学院高能物理研究所硕士研究生, 主要从事干法后处理研究.

梅雷, 中国科学院高能物理研究所, 研究员. 主要研究方向为锕系元素化学与分离材料, 致力于将超分子识别与组装的理念和方法应用于锕系固体化学和放射性核素分离化学研究, 在锕系超分子配合物及其配位化学基础、基于协同识别的放射性核素分离新方法、新型锕系固相材料开发等方面开展了系列原创性工作, 为解决乏燃料后处理、环境放射性污染控制与资源回用研究等领域中的关键问题提供了新思路. 以通讯/第一作者身份在Nature Commun., J. Am. Chem. Soc., Angew. Chem. Int. Ed., Adv. Funct. Mater.等国际知名期刊发表研究论文130余篇. 目前担任中国化学会青年化学工作者委员会委员, 中科院青促会化学与材料分会委员, 中国核学会锕系化学与物理分会理事, 并担任《核化学与放射化学》期刊编委, SmartMat、Materials Research Letters、《结构化学》等学术期刊青年编委.

刘雅兰, 副研究员, 中国科学院高能物理研究所. 多年来致力于氧化物乏燃料干法后处理领域, 聚焦于锕-镧分离研究. 首先开展了锕、镧系氧化物在熔盐中的溶解及其电化学行为研究, 随后在固态活性铝阴极上进行了锕-镧的电化学分离, 并采用原位光谱技术监测了分离过程中锕、镧元素的化学种态变化, 发现了铀的循环电解并将其消除, 提高了电流效率. 最终成功实现了锕-镧元素的有效分离, 与传统的液态Cd阴极相比将分离因子提高了两个数量级. 在此基础上, 进一步总结了锕、镧氧化物在氯化物熔盐中的溶解规律, 提出了利用其溶解性差异实现一步分离的新方法. 基于相关工作, 在电化学领域与核能领域著名期刊Electrochim. Acta, J. Electrochem. Soc., Electrochem. Commun.和 J. Nucl. Mater.等上共发表论文40余篇, 其中第一作者及通讯作者论文20篇.

石伟群, 上海交通大学特聘教授, 核燃料循环与核材料研究所所长, 国家杰出青年科学基金获得者. 2007年1月在清华大学化学系获博士学位. 长期致力于核燃料循环化学相关基础研究, 在JACS、Angew. Chem、Chem.、CCS Chem.、Nat. Commun、Adv. Mater.等国际知名期刊发表SCI论文400余篇, 成果被国内外同行广泛关注和引用, 文章总引两万余次, H因子71 (Google Scholar), 2020~2024年连续入选Elsevier中国高被引学者榜单(核科学技术). 分别担任期刊《Supramolecular Materials》副主编, 《Industrial Chemistry & Materials》、《Chinese Chemical Letters》、《Journal of Nuclear Fuel Cycle and Waste Technology》、《International Journal of Advanced Nuclear Reactor Design and Technology》和《Journal of Nuclear Science and Technology》的编委与国际顾问编委, 中文期刊《化学学报》、《高等学校化学学报》、《核化学与放射化学》、《核动力》编委. 现为中国核工业教育学会副理事长、中国核学会锕系物理与化学分会副理事长、中国有色金属学会熔盐化学与技术专业委员会副主任委员、中国化学会核化学与放射化学专业委员会委员、中国核学会核化工分会常务理事兼副秘书长.

Research Progress on the Preparation and Recovery of Nuclear-Grade Zirconium Using Molten Salts

Zhou Mingyu^a^,^c, Liu Lebin^a^,^c, Mei Lei^a, Liu Yalan^a^,^*(), Shi Weiqun^b^,^*()

^a Laboratory of Nuclear Energy Chemistry, Institute of High Energy Physics, Chinese Academy of Sciences, Beijing 100049, China
^b Institute of Nuclear Fuel Cycle and Materials, School of Mechanical Engineering, Shanghai Jiao Tong University, Shanghai 200030, China
^c School of Chemical Sciences, University of Chinese Academy of Sciences, Beijing 100049, China

Received:2025-11-06 Published:2025-12-31
Contact: Liu Yalan, Shi Weiqun

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摘要/Abstract

核级锆是核电站反应堆的必备金属材料, 具有普通商用锆材无法企及的低中子吸收截面与耐腐蚀性, 兼具高经济价值与战略意义, 是关乎国家能源安全的储备性资源. 因此, 高效经济地制备和回收核级锆受到核科学工作者们的重视. 熔盐技术作为实现锆铪分离、金属锆制备及退役锆回收的重要途径, 具有流程简洁、适应性强等优势. 此综述概括了熔盐在核级锆全流程管理中的关键作用, 包括不同熔盐体系(氟化物、氯化物及氟氯混合盐体系)在金属锆制备和回收中的应用特性分析和对比. 此外, 重点对熔盐中锆离子的电还原行为进行了系统的梳理, 以推动核级锆的绿色冶金与循环利用.

关键词: 核级锆, 熔盐, 电沉积, 电精炼

Nuclear-grade zirconium is a critical metallic material for nuclear power plants. It boasts a low neutron absorption cross-section and corrosion resistance that are far superior to those of ordinary commercial zirconium materials. With high economic value and vital strategic significance, it serves as a strategic reserve resource critical to national energy security. Consequently, the efficient and economical preparation and recovery of nuclear-grade zirconium have garnered increasing attention. Molten salt technology serves as a crucial pathway for the separation of zirconium and hafnium, the preparation of metallic zirconium, and the recycling of the used zirconium, offering advantages such as a simplified process and strong adaptability. This review outlines the key role of molten salts in the life cycle management of nuclear-grade zirconium, including the analysis and comparison of the application characteristics of different molten salt systems (fluoride, chloride, and fluorine-chloride mixed salt systems) in the preparation and recovery of metallic zirconium. In addition, it focuses on systematically sorting out and summarizing the electroreduction behavior of zirconium ions in molten salts, aiming to promote the green metallurgy and recycling of nuclear-grade zirconium.

Key words: nuclear-grade zirconium, molten salts, electrowinning, electrorefining

引用此文

周铭宇, 刘乐彬, 梅雷, 刘雅兰, 石伟群. 核级锆的熔盐制备与回收研究进展[J]. 化学学报, 2026, 84(3): 425-447.

Zhou Mingyu, Liu Lebin, Mei Lei, Liu Yalan, Shi Weiqun. Research Progress on the Preparation and Recovery of Nuclear-Grade Zirconium Using Molten Salts[J]. Acta Chimica Sinica, 2026, 84(3): 425-447.

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图/表 18

图1. 典型的(a)商业纯锆(Zr-207)和(b)核工业用锆(Zircaloy-2)的化学组成

Figure 1. The chemical compositions of typical (a) commercial pure zirconium (Zr-207) and (b) zirconium for the nuclear industry (Zircaloy-2)

图2. 相对成熟的Zr/Hf分离工艺, 分级结晶中的(a) K2ZrF6晶体单胞结构[42], (b)固溶体晶体单胞结构[42]; (c)溶剂萃取法中代表性的萃取剂[48]; (d)熔盐精馏法的精馏塔结构示意图[52]; 固相吸附法中的代表性材料(e)接枝树脂[49], (f)修饰硅胶[50], (g) MOF吸附剂[51]

Figure 2. Established Zr/Hf separation technologies: (a) Crystal structure of the K2ZrF6 unit cell[42]; (b) Crystal structure of a solid solution unit cell[42]; (c) Representative extractants used in solvent extraction methods[48]; (d) Schematic diagram of the distillation column structure in molten salt distillation method[52]; Representative materials in solid phase extraction methods: (e) Grafted resin[49], (f) Modified silica gel[50], (g) MOF adsorbent[51]

Methods	Advantage	Challenges
Fractional Crystallization	Simplicity principle; Mild operating conditions	Low separation factor; Low productivity; Intermittent operation
Solvent Extraction	Large-scale production; Mature process; Separation efficiency	High consumption; High waste generation; Process complexity
Solid-phase Extraction	Eco-Friendly; Highly efficient	Adsorbent cost; Low stability
Molten Salt Distillation	Process simplicity; Simplifies downstream; Waste minimization	High temperature; Corrosivity; High energy consumption

表1. 四种Zr/Hf分离工艺的优缺点

Table 1. Advantages and disadvantages of Zr-Hf separation methods

图3. 熔盐在Zr/Hf分离中承担的角色

Figure 3. The function of molten salt in Zr/Hf separation

图4. 不同熔盐电解工艺的原理示意图: (a)传统的电沉积法; (b)阴极氧化物电脱氧法(The FFC process); (c)可溶性阳极电解法(The USTB process)

Figure 4. Schematic diagrams of the principles of different molten salt electrolysis processes: (a) Traditional electrowinning method; (b) Cathodic oxide electro-deoxidation method (The FFC process); (c) Soluble anode electrolysis method (The USTB process)

图5. FFC还原过程图示: (a)电脱氧的微观机制[91]; (b)电脱氧的宏观3PIs迁移模型[92]

Figure 5. Schematic diagram of the mechanism of the FFC reduction process: (a) Microscopic mechanism[91]; (b) Macroscopic 3PIs migration model[92]

图6. (a) Zr-O相图[97]; (b)特殊阴极的FFC工艺装置图[99]; (c)二合一的双电池装置示意图[103]; (d) FFC工艺制备的锆金属管[100]; (e) MCE电极和氧化锆在熔融CaCl2中的CV曲线[102]

Figure 6. (a) Zr-O phase diagram[97]; (b) Diagram of the FFC process device with special cathode[99]; (c) Schematic diagram of the dual-cell device[103]; (d) Zirconium metal tube prepared by FFC process[100]; (e) CV curves of MCE electrode and zirconia in molten CaCl2[102]

图7. (a)石墨坩埚作为阴极的电解池设计图[113]; (b)耦合碳捕集的USTB工艺设计图[116]; (c)电解ZrO2-C混合物的I-t曲线[117]; (d)熔体中锆离子(来源于ZrCxOyNz氧化溶解)的CV曲线[114]; (e)以ZrCxOy为工作电极的CV曲线[115]

Figure 7. (a) Design diagram of an electrolytic cell with a graphite crucible as the cathode[113]; (b) Design diagram of the USTB process coupled with carbon capture[116]; (c) I-t curve of the electrolytic ZrO2-C mixture[117]; (d) CV curve of zirconium ions (from the oxidative dissolution of ZrCxOyNz)[114]; (e) CV curve with ZrCxOy as the working electrode[115]

图8. 金属锆回收方法流程简图: (a)碘化法流程简图; (b)氯气氯化法流程简图; (c)氯化氢氯化法流程简图; (d) S2Cl2氯化法流程简图

Figure 8. Methods for recovering metallic zirconium: Schematic diagram of (a) The iodination method; (b) The chlorination method using chlorine gas; (c) The chlorination method using hydrogen chloride; (d) The chlorination method using disulfur dichloride

图9. 熔盐电精炼回收金属锆示意图

Figure 9. Diagram of molten salt electrorefining for the recovery of metallic zirconium

Components	Melting/Eutectic Temp. (℃)	Characteristics/Properties	Primary Applications in Zr Industry
NaCl	801	Wide electrochemical window; High Zr-salt solubility; Low cost; Formation of dense, adherent Zr deposits.	Molten Salt Distillation; Molten Salt Electrolysis for Zr/Hf Separation; Electrowinning for Zirconium Production.
MgCl₂	714	Denser Kroll byproduct than molten Mg; Electrolytically regeneratable.	Kroll Process for Zirconium Production.
CaCl₂	772	High O²⁻ affinity/solubility; Efficient O²⁻ transport.	FFC Process for Zirconium Production.
NaCl-KCl	657	Powdery, non-adherent zirconium deposits; Favorable solubility for ZrC_xO_y anodes.	Molten Salt Distillation; Molten Salt Extraction for Zr/Hf Separation; Molten Salt Electrolysis for Zr/Hf Separation; Electrowinning for Zirconium Production; USTB Process for Zirconium Production.
LiCl-KCl	352	Multi-metallic processing capability; Highly purifiable; Wide/stable electrochemical window.	Molten Salt Electrolysis for Zr/Hf Separation; Electrowinning for Zirconium Production; Electrorefining for Zirconium Recovery.
LiF-KF	492	High Zr(IV) reduction efficiency; Dense Zr deposition; Fluoride-induced anode passivation; High viscosity and corrosivity.	Electrorefining for Zirconium Recovery.
LiF-NaF	649
LiF-NaF-KF	460

表2. 适用于核级锆冶金关键环节的熔盐体系特性

Table 2. Characteristics of molten salt systems applicable to critical processes in nuclear-grade zirconium metallurgy

Technique	Description/Formula Name	Equation	Applicable System & Notes
EFM^a	Nernst Equation	${-E}_{\mathrm{c}\mathrm{e}\mathrm{l}\mathrm{l}}^{\mathrm{\text{'}}}={E}_{\mathrm{Z}\mathrm{r}\left(n\right)/\mathrm{Z}\mathrm{r}\left(0\right)}^{{0}^{\mathrm{\text{'}}}}+$ $\frac{2.303RT}{nF}\mathrm{l}\mathrm{o}\mathrm{g}C$	E_cell: Measured potential (V) ${E}_{\mathrm{Z}\mathrm{r}\left(n\right)/\mathrm{Z}\mathrm{r}\left(0\right)}^{{0}^{\text{'}}}$: Formal potential (V) C: Concentration of the electroactive species (mol/L)
LSV/CV	Reversible System Half-Wave Potential	${E}_{P/2}={E}_{P}+2.2\left(\frac{RT}{nF}\right)$	Reversible System: Fast electron transfer. E_P/2: Half-wave potential (V) E_P: Peak potential (V) Constant 2.2 is characteristic of a reversible process.
LSV/CV	Irreversible System Half-Wave Potential	${E}_{P/2}={E}_{P}+1.85\left(\frac{RT}{nF}\right)$	Totally Irreversible System: Slow electron transfer. Constant 1.85 is characteristic of an irreversible process.
SWV	Peak Width at Half Height	${W}_{1/2}=\frac{3.52RT}{nF}$	W_1/2: Peak width at half height (V) Applicable when electron transfer is sufficiently fast.
CP	Sand's Equation	$i{\tau }^{1/2}=0.5nFCA{\left(\pi \nu \right)}^{1/2}$	Used to calculate the diffusion coefficient D or n. $\tau $: Transition time (s) i: Applied constant current (A) A: Electrode area (cm²) C: Bulk concentration (mol/cm³)
Calculation	Randles-Sevcik Equation	${i}_{\mathrm{p}}=0.4463nFAC{\left(\frac{nF\nu D}{RT}\right)}^{1/2}$	Primarily used in LSV/CV to calculate the diffusion coefficient D from the peak current i_p. i_p: Peak current (A) ν: Scan rate (V/s)

表3. 熔盐电化学测试中使用到的电化学计算公式

Table 3. Summary of electrochemical calculation formulas used in molten salt electrochemical testing

FLiNaK (LiF:NaF:KF)
Author	Time	Zr(IV) Ion Source	Electrode	Electroreduction behavior of Zr(IV)	D_(Zr4+)/(cm²•s⁻¹)
Mellors^[77]	1966	ZrF₄ & K₂ZrF₆	Mo	Zr(IV)→Zr	—
Li^[135]	2023	K₂ZrF₆	Cu	${\mathrm{Z}\mathrm{r}\mathrm{F}}_{x}^{4-x}$→Zr	—
Zuo^[140]	2025	ZrF₄	W	${\mathrm{Z}\mathrm{r}\mathrm{F}}_{8}^{4-}$→Zr	3.85×10⁻⁶ (600 ℃)
LiF-CaF₂
Gibilaro^[134]	2013	ZrF₄	Ta, Cu, Ni	Zr(IV)→Zr	9.96×10⁻⁶ (840 ℃)
Fabian^[139]	2022	ZrF₄	Mo, Ni	Zr(IV)→Zr0(sol)→Zr	2.6×10⁻⁵ (840 ℃)
LiF-KF
Mellors^[77]	1966	ZrF₄ & K₂ZrF₆	Mo	Zr(IV)→Zr	—
Park^[136]	2013	ZrF₄	Mo	Zr(IV)→Zr	—
Xu^[152]	2016	ZrF₄	Mo	Step 1: Zr⁴⁺→Zr²⁺ Step 2: Zr⁴⁺, Zr²⁺→Zr⁺ Step 3: Zr⁺, Zr²⁺, Zr⁴⁺→Zr	1.32×10⁻⁶~1.53×10⁻⁵ (600 ℃)
LiF-NaF
Groult^[153]	2007	ZrF₄	W, Mo, C, Ni	Zr(IV)→Zr	1.19×10⁻⁵ (694 ℃) 2.59×10⁻⁵ (730 ℃) 3.19×10⁻⁵ (762 ℃)
Groult^[154]	2011	n(LiF):n(KF):n(ZrF₄)= (26:37:37)	C	Zr(IV)→ZrC	—
Xu^[155]	2017	K₂ZrF₆	Mo	Zr(IV)→Zr(II) Zr(IV)/Zr(II)→Zr	8.14×10⁻⁶~1.91×10⁻⁵(750 ℃)
Quaranta^[87]	2018	ZrF₄	Ag	Zr(IV)→Zr	1.21×10⁻⁵~1.35×10⁻⁵ (750 ℃)

表4. 氟化物熔体中锆离子的电还原行为研究: 文献综述

Table 4. Electroreduction analysis of zirconium in fluoride melts: a literature review

图10. (a) LiF-CaF2熔体中氧离子对Zr(IV)离子电化学行为的影响[134]; (b) LiF-KF熔体中ZrF4还原的SWV曲线[152]; (c) LiF-NaF熔体中Ag电极上锆成核行为表征的I-t曲线[87]; (d)石墨电极作为阴极在LiF-NaF-ZrF4熔体中沉积金属锆后的SEM形貌图[154]

Figure 10. (a) Influence of oxygen ions on the electrochemical behavior of Zr(IV) ions in LiF-CaF2 melts[134]; (b) SWV curve of ZrF4 reduction in LiF-KF melts[152]; (c) Chronoamperometric curve characterizing zirconium nucleation behavior on Ag electrode in LiF-NaF melts[87]; (d) SEM morphology of metallic zirconium deposited on graphite electrode in LiF-NaF-ZrF4 melts[154]

图11. LiCl-KCl熔体中Zr(IV)的还原机制: (a) Inman[146]和Basile[157]等; (b) Sakamura[158]; (c) Ghosh等[166]; (d) Lee等[130]

Figure 11. Proposed Zr(IV) reduction mechanisms in LiCl-KCl melt: (a) By Inman[146] and Basile[157] et al.; (b) By Sakamura[158]; (c) By Ghosh et al.[166]; (d) By Lee et al.[130]

图12. (a)不同浓度和扫描速率下LiCl-KCl-ZrCl4体系的CV曲线, 图中氧化还原峰对应的氧化还原电对: Zr(IV)/Zr(II) (A)、Zr(IV)/Zr(0)与Zr(IV)/ZrCl (B)、ZrCl/Zr(IV) (D)和Zr(0)/Zr(IV) (E)[158]; (b)利用电还原回收Zr(IV)离子和Cd(II)离子的示意图[169]; (c)原始CV曲线与其对应的卷积伏安图对比[166]; (d) LiCl-KCl-ZrCl4熔体的XPS测试图[172]

Figure 12. (a) CV curves of the LiCl-KCl-ZrCl4 system at different concentrations and scan rates, with the peaks corresponding to the redox couples: Zr(IV)/Zr(II) (A), Zr(IV)/Zr(0) and Zr(IV)/ZrCl (B), ZrCl/Zr(IV) (D), and Zr(0)/Zr(IV) (E)[158]; (b) Schematic diagram of the electrochemical recovery of Zr(IV) and Cd(II) ions[169]; (c) Comparison of the original CV curve and its corresponding convolution voltammogram[166]; (d) XPS test results of LiCl-KCl-ZrCl4 melt[172]

Author	Year	Technique/Method	Electrolyte	Electroreduction behavior of Zr(IV)	Temp.^a/℃
Mellors^[77]	1966	ED ^b	NaCl-KCl-ZrCl₄ NaCl-KCl-K₂ZrF₆	ZrCl₂ forms in electroreduction	600~900
Swaroop^[176]	1966	EFM	NaCl-KCl-ZrCl₂ NaCl-KCl-ZrCl₂-ZrCl₃ NaCl-KCl-ZrCl₃-ZrCl₄	Zr(IV)→Zr(III)→Zr(II)→Zr(0)	670~740
Sakakura^[177]	1976	CP	NaCl-KCl-ZrCl₂ NaCl-KCl-ZrCl₄	Zr(IV)→Low Valency→Zr(0)	700~900
Polyakova^[80]	1982	LSV	NaCl-KCl-ZrCl₄	Zr(IV)→Zr(II)→Zr(0)	735
Polyakova^[80]	1982	LSV	NaCl-KCl-K₂ZrF₆	${\mathrm{Z}\mathrm{r}\mathrm{F}}_{6}^{2-}$→Zr(0)	805
Guang-Sen^[68]	1990	LSV and CV	NaCl-KCl-ZrCl₄	${\mathrm{Z}\mathrm{r}\mathrm{F}}_{6}^{2-}$→Zr(II)→Zr(0)	760
Wu^[81]	2011	CV and SWV	NaCl-KCl-K₂ZrF₆	Zr(IV)→Zr(II)→Zr(0)	750
Ueda^[88]	2015	CV	AlCl₃-NaCl-KCl-ZrCl₄	Zr(IV)→Zr(II)→Zr(0)	175
Wang^[82]	2016	CV, CP and ED ^b	NaCl-KCl-K₂ZrF₆	Pathway 1: Zr(IV)→Zr(III)→Zr(II)→Zr(0) Pathway 2: Zr(IV)→Zr(0)	750
Tekeda^[111]	2018	CV and SWV	NaCl-KCl-ZrCl₄	Pathway 1: Zr(IV)→Zr(II)→Zr(0) Pathway 2: Zr(IV)→Zr(0)	800
Tekeda^[111]	2018	CV and SWV	NaCl-KCl-K₂ZrF₆	${\mathrm{Z}\mathrm{r}\mathrm{F}}_{6}^{2-}$→Zr(0)	800
Zhang^[83]	2022	CV	NaCl-KCl-K₂ZrF₆	Zr(IV)→Zr(II)→Zr(0)	750
Wang^[89]	2023	CV	NaCl-KCl-K₂ZrF₆	Pathway 1: Zr(IV)→Zr(III)→Zr(II)→Zr(0) Pathway 2: Zr(IV)→Zr(0)	750

表5. NaCl-KCl熔体中锆电还原行为的研究: 文献综述

Table 5. Electrochemical analysis of zirconium in NaCl-KCl molten salts: a literature review

图13. (a)温度对拉曼测试的影响[180]; (b)氟离子对NaCl-KCl熔体中锆配位形式的影响[184]

Figure 13. (a) Effect of temperature on Raman testing[180]; (b) Effect of fluoride ion concentration on zirconium coordination forms in NaCl-KCl melt[184]

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核级锆的熔盐制备与回收研究进展

Research Progress on the Preparation and Recovery of Nuclear-Grade Zirconium Using Molten Salts

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