上海光源BL14W1线站高分辨XAFS方法的实现及其应用研究
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摘要
自同步辐射光源发现以来，同步辐射实验方法已成为科学研究中一种越来越重要的实验技术。伴随着同步辐射技术的发展，X射线吸收精细结构谱（XAFS）方法也得到了快速的发展，新的实验技术如快速扫描XAFS、掠入射XAFS等相继出现。发展并利用新的实验技术，已经成为XAFS领域的重要方向之一。
上海光源BL14W1线站是一条硬X射线通用谱学线站，主要进行X射线吸收精细结构谱的研究。现在已有多种吸收谱的测试手段如透射法，lytle荧光法、32元固探荧光法、掠入射XAFS方法，并可以在高低温等环境下进行XAFS谱的测试。高分辨XAFS方法的发展不仅可以拓展线站的实验技术，还可以解决一些常规XAFS方法无法解决的问题。
高分辨XAFS谱仪是利用高能量分辨的分析晶体的谱仪，使样品、分析晶体、探测器三者采取罗兰圆几何结构。可以研究电子跃迁发出的更精细的光谱，一般主要是观测元素的Kβ1,3及其附近的各种卫星谱线，这些谱线往往需要几个eV或更高能量分辨的探测方法才能实现，常规探测方法的能量分辨率一般不好于120eV，难以或无法区分Kβ1,3及其附近的卫星谱线，而正是Kβ1,3及其附近的卫星谱线包含了重要的结构信息，如电子自旋与轨道耦合等，通过研究这种高分辨的发射谱及吸收谱可以获得常规XAFS吸收谱得不到的结构和信息。
论文第一部分主要是在上海光源BL14W1线站成功发展并实现了高分辨XAFS方法，获得了高分辨的发射谱和吸收谱，本部分主要包括以下内容：
1、对高分辨XAFS方法在上海光源BL14W1线站的实现进行了可行性讨论；
2、介绍了高分辨XAFS方法的硬件系统，其主要由样品架系统、球面晶体系统和探测器系统三部分组成；
3、对高分辨XAFS方法的软件系统的介绍，其软件系统主要是基于线站现有的编程软件Lab-View；
4、安装调试了高分辨XAFS谱仪，并研究了Mn的各个价态的标准化合物样品，获得了高分辨的发射谱和吸收谱，测试了高分辨谱仪的性能；
5、解决并优化了存在的问题，主要是对谱仪的分辨率、探测器参数和信噪比等加以优化。
最终通过优化获得了分辨率在3eV左右的高分辨发射谱，已达到国际同类仪器的水平，证明了高分辨谱仪具有优越的性能，为今后XAFS线站进行相关的实验奠定了重要基础。
论文第二部分主要是将高分辨XAFS方法应用在环境领域，结合静态法和高分辨XAFS方法，对不同pH值下Eu(III)在γ-MnOOH的表面的吸附机理和微观结构进行了研究，在对放射性核废料的存放存储以及放射性核素的寿命和迁移评估中，放射性核素与水体和土壤环境的迁移和吸附过程被认为是评估放射性核素与水体和土壤的相互作用的重要因素，自然界水体和土壤中的材料对放射性核素的吸附性能决定了放射性核素在水体和土壤等环境中的扩散和迁移能力。通过对Eu(III)与环境中材料的相互作用的研究，来获得镧系、锕系等有相似化学性质的元素的处理方式。本部分的主要研究内容有：
1、配备了实验所需的化学试剂，并对合成的材料进行表征测试，结果表明所制备的Eu的溶液和碱式氧化锰符合实验要求。
2、通过静态批式法对制备的Eu在碱式氧化锰表明进行吸附实验，并对吸附结果进行分析，结果表明随着pH值的增大，吸附效果变好，但当pH值达到一定值后吸附效果趋于稳定，分析发现这是由γ-MnOOH的表面的基团浓度影响的。进一步分析发现，Eu(III)在γ-MnOOH的表面的吸附源自于Eu(III)在γ-MnOOH的表面形成的内层表面络合物。
3、对吸附样品和标样参照样品进行了吸收谱研究，吸收谱数据显示所有样品中的Eu均为三价，通过对吸附样品吸收谱数据的拟合发现，Eu(III)在γ-MnOOH的表面的相互作用，除在第一配位层有Eu与O的配位外，在第二配位层有Eu与Mn的配位存在，这也表明Eu(III)与γ-MnOOH相互作用形成的内层表面络合物，这与宏观吸附结果相吻合。
实验中因为Mn的Kα荧光峰和Eu的Lα1荧光峰相互干扰，常规吸收谱实验无法正常进行，基于高分辨XAFS方法，成功将上述荧光峰区分开来，使实验得以成功进行，为以后此类复杂体系（基底元素的荧光信号与目标元素的荧光信号相互干扰）的研究奠定了基础。
此研究不仅从宏观上发现了放射性核素Eu(III)与碱式氧化锰表面的作用机理，还从微观上印证了这种相互作用机理，这对于揭示放射性核素Eu(III)等放射性核素与自然界中的氧化物等天然矿物的作用机理有一定的参考价值，对于阐明放射性核素在界面表面的吸附作用过程也有一定的意义。
Since the appearance of the synchrotron radiation, synchrotron radiation techniquesare becoming important experimental techniques of scientific researches gradually.XAFS technique is one of the most important synchrotron radiation techniques andhas been developed rapidly. New experimental techniques, such as QXAFS, GIXAFSand so on, have emerged. The development of new methods of XAFS technique isimportant for scientific researches.
XAFS beamline (BL14W1) at Shanghai Synchrotron Radiation Facility (SSRF) is ageneral purpose XAFS beamline. It is mainly used for XAFS tests. Now XAFSbeamline have a variety of testing methods for XAFS, such as transmission mode,lytle fluorescence mode，SDD detector mode etc.. The development of high-resolutionXAFS method can not only expand the experimental techniques of beamline, but alsosolve some questions that conventional XAFS methods cannot solve.
The high-resolution XAFS spectrometer is composed of a spherically curvedsilicon crystal, a detector and a sample. The analyzing plane is horizontal. The bentcrystal, the sample and the detector are located on the Rowland circle. It is used tostudy the spectrum from the electronic transitions. Generally it is mainly used toobtain the Kβ1,3and its satellite spectrum. The obtainment of these spectra can beachieved by using high energy resolution method. Generally speaking, the energyresolution of conventional XAFS method is not more than120eV. It is difficult (evenimpossible) to distinguish these spectra. But these spectra contain important structuralinformation such as spin state and orbit coupling. We can get some information thatconventional XAFS method cannot obtain through high-resolution emission spectraand absorption spectra.
The first part of this thesis discussed high-resolution XAFS method at Bl14W1beamline. High-resolution XES and XAFS spectra were obtained. The following isthe main content of this part:
1. Design of high-resolution XAFS method at BL14W1beamline;
2. Introduction of hardware of high-resolution XAFS spectrometer;
3. Introduction of software of high-resolution XAFS spectrometer. It is based on theexisting software Labview;
4. Installation and test of high-resolution XAFS spectrometer. Test of theperformance of the spectrometer through the emission spectra of Mn compounds;
5. Optimization of the resolution and signal-to-noise ratio for high-resolutionXAFS method.
The resolution of the emission spectrum about3eV can be obtained through theoptimization. The testing results indicated that high-resolution XAFS method hadbeen achieved at BL14W1beamline in SSRF. It reached the international level ofsimilar instruments.
The second part of this thesis discussed the high-resolution XAFS method appliedto the field of environment. Mechanism and microstructure of Eu(III) interaction withγ-MnOOH by a combination of batch and high resolution EXAFS. In the context ofsafety of nuclear waste repositories and for the assessment of radionuclide fate andmobility in the natural environment, understanding of the interaction mechanism andmicrostructure of radionuclides at the interface is of great importance to assess theinterfacial behavior of radionuclides in the natural environment. The chemicalproperty of Eu(III) is very similar to other lanthanides and actinides, thus we canunderstand other lanthanides and actinides interfacial behavior through Eu(III). Thework is listed in the following part:
Preparation and characterization of chemicals was carried out. The results showedthat the prepared solution of Eu and γ-MnOOH met experimental requirements.
Adsorption experiments about Eu(III) interaction with γ-MnOOH. The resultsindicated that Eu(III) interaction with γ-MnOOH by sorption process was mainly dueto inner-sphere surface complexation.
XAFS investigation of interaction mechanism and microstructure about Eu(III)interaction with γ-MnOOH through high-resolution XAFS method. This result wasconsistent with the macroscopic adsorption results.
In this experiment, the fluorescence peak Lα of Eu(III) and Mn which is difficult tobe discriminated using conventional XAFS technique was discriminated. It formedthe basis of the studies on such complex systems.
The utility of high-resolution EXAFS technique has been well-demonstrated in thepresent study. The results of this work are important to understand thephysicochemical behavior of the interested radionuclides in the natural environment.
上海光源BL14W1线站是一条硬X射线通用谱学线站，主要进行X射线吸收精细结构谱的研究。现在已有多种吸收谱的测试手段如透射法，lytle荧光法、32元固探荧光法、掠入射XAFS方法，并可以在高低温等环境下进行XAFS谱的测试。高分辨XAFS方法的发展不仅可以拓展线站的实验技术，还可以解决一些常规XAFS方法无法解决的问题。
高分辨XAFS谱仪是利用高能量分辨的分析晶体的谱仪，使样品、分析晶体、探测器三者采取罗兰圆几何结构。可以研究电子跃迁发出的更精细的光谱，一般主要是观测元素的Kβ1,3及其附近的各种卫星谱线，这些谱线往往需要几个eV或更高能量分辨的探测方法才能实现，常规探测方法的能量分辨率一般不好于120eV，难以或无法区分Kβ1,3及其附近的卫星谱线，而正是Kβ1,3及其附近的卫星谱线包含了重要的结构信息，如电子自旋与轨道耦合等，通过研究这种高分辨的发射谱及吸收谱可以获得常规XAFS吸收谱得不到的结构和信息。
论文第一部分主要是在上海光源BL14W1线站成功发展并实现了高分辨XAFS方法，获得了高分辨的发射谱和吸收谱，本部分主要包括以下内容：
1、对高分辨XAFS方法在上海光源BL14W1线站的实现进行了可行性讨论；
2、介绍了高分辨XAFS方法的硬件系统，其主要由样品架系统、球面晶体系统和探测器系统三部分组成；
3、对高分辨XAFS方法的软件系统的介绍，其软件系统主要是基于线站现有的编程软件Lab-View；
4、安装调试了高分辨XAFS谱仪，并研究了Mn的各个价态的标准化合物样品，获得了高分辨的发射谱和吸收谱，测试了高分辨谱仪的性能；
5、解决并优化了存在的问题，主要是对谱仪的分辨率、探测器参数和信噪比等加以优化。
最终通过优化获得了分辨率在3eV左右的高分辨发射谱，已达到国际同类仪器的水平，证明了高分辨谱仪具有优越的性能，为今后XAFS线站进行相关的实验奠定了重要基础。
论文第二部分主要是将高分辨XAFS方法应用在环境领域，结合静态法和高分辨XAFS方法，对不同pH值下Eu(III)在γ-MnOOH的表面的吸附机理和微观结构进行了研究，在对放射性核废料的存放存储以及放射性核素的寿命和迁移评估中，放射性核素与水体和土壤环境的迁移和吸附过程被认为是评估放射性核素与水体和土壤的相互作用的重要因素，自然界水体和土壤中的材料对放射性核素的吸附性能决定了放射性核素在水体和土壤等环境中的扩散和迁移能力。通过对Eu(III)与环境中材料的相互作用的研究，来获得镧系、锕系等有相似化学性质的元素的处理方式。本部分的主要研究内容有：
1、配备了实验所需的化学试剂，并对合成的材料进行表征测试，结果表明所制备的Eu的溶液和碱式氧化锰符合实验要求。
2、通过静态批式法对制备的Eu在碱式氧化锰表明进行吸附实验，并对吸附结果进行分析，结果表明随着pH值的增大，吸附效果变好，但当pH值达到一定值后吸附效果趋于稳定，分析发现这是由γ-MnOOH的表面的基团浓度影响的。进一步分析发现，Eu(III)在γ-MnOOH的表面的吸附源自于Eu(III)在γ-MnOOH的表面形成的内层表面络合物。
3、对吸附样品和标样参照样品进行了吸收谱研究，吸收谱数据显示所有样品中的Eu均为三价，通过对吸附样品吸收谱数据的拟合发现，Eu(III)在γ-MnOOH的表面的相互作用，除在第一配位层有Eu与O的配位外，在第二配位层有Eu与Mn的配位存在，这也表明Eu(III)与γ-MnOOH相互作用形成的内层表面络合物，这与宏观吸附结果相吻合。
实验中因为Mn的Kα荧光峰和Eu的Lα1荧光峰相互干扰，常规吸收谱实验无法正常进行，基于高分辨XAFS方法，成功将上述荧光峰区分开来，使实验得以成功进行，为以后此类复杂体系（基底元素的荧光信号与目标元素的荧光信号相互干扰）的研究奠定了基础。
此研究不仅从宏观上发现了放射性核素Eu(III)与碱式氧化锰表面的作用机理，还从微观上印证了这种相互作用机理，这对于揭示放射性核素Eu(III)等放射性核素与自然界中的氧化物等天然矿物的作用机理有一定的参考价值，对于阐明放射性核素在界面表面的吸附作用过程也有一定的意义。
Since the appearance of the synchrotron radiation, synchrotron radiation techniquesare becoming important experimental techniques of scientific researches gradually.XAFS technique is one of the most important synchrotron radiation techniques andhas been developed rapidly. New experimental techniques, such as QXAFS, GIXAFSand so on, have emerged. The development of new methods of XAFS technique isimportant for scientific researches.
XAFS beamline (BL14W1) at Shanghai Synchrotron Radiation Facility (SSRF) is ageneral purpose XAFS beamline. It is mainly used for XAFS tests. Now XAFSbeamline have a variety of testing methods for XAFS, such as transmission mode,lytle fluorescence mode，SDD detector mode etc.. The development of high-resolutionXAFS method can not only expand the experimental techniques of beamline, but alsosolve some questions that conventional XAFS methods cannot solve.
The high-resolution XAFS spectrometer is composed of a spherically curvedsilicon crystal, a detector and a sample. The analyzing plane is horizontal. The bentcrystal, the sample and the detector are located on the Rowland circle. It is used tostudy the spectrum from the electronic transitions. Generally it is mainly used toobtain the Kβ1,3and its satellite spectrum. The obtainment of these spectra can beachieved by using high energy resolution method. Generally speaking, the energyresolution of conventional XAFS method is not more than120eV. It is difficult (evenimpossible) to distinguish these spectra. But these spectra contain important structuralinformation such as spin state and orbit coupling. We can get some information thatconventional XAFS method cannot obtain through high-resolution emission spectraand absorption spectra.
The first part of this thesis discussed high-resolution XAFS method at Bl14W1beamline. High-resolution XES and XAFS spectra were obtained. The following isthe main content of this part:
1. Design of high-resolution XAFS method at BL14W1beamline;
2. Introduction of hardware of high-resolution XAFS spectrometer;
3. Introduction of software of high-resolution XAFS spectrometer. It is based on theexisting software Labview;
4. Installation and test of high-resolution XAFS spectrometer. Test of theperformance of the spectrometer through the emission spectra of Mn compounds;
5. Optimization of the resolution and signal-to-noise ratio for high-resolutionXAFS method.
The resolution of the emission spectrum about3eV can be obtained through theoptimization. The testing results indicated that high-resolution XAFS method hadbeen achieved at BL14W1beamline in SSRF. It reached the international level ofsimilar instruments.
The second part of this thesis discussed the high-resolution XAFS method appliedto the field of environment. Mechanism and microstructure of Eu(III) interaction withγ-MnOOH by a combination of batch and high resolution EXAFS. In the context ofsafety of nuclear waste repositories and for the assessment of radionuclide fate andmobility in the natural environment, understanding of the interaction mechanism andmicrostructure of radionuclides at the interface is of great importance to assess theinterfacial behavior of radionuclides in the natural environment. The chemicalproperty of Eu(III) is very similar to other lanthanides and actinides, thus we canunderstand other lanthanides and actinides interfacial behavior through Eu(III). Thework is listed in the following part:
Preparation and characterization of chemicals was carried out. The results showedthat the prepared solution of Eu and γ-MnOOH met experimental requirements.
Adsorption experiments about Eu(III) interaction with γ-MnOOH. The resultsindicated that Eu(III) interaction with γ-MnOOH by sorption process was mainly dueto inner-sphere surface complexation.
XAFS investigation of interaction mechanism and microstructure about Eu(III)interaction with γ-MnOOH through high-resolution XAFS method. This result wasconsistent with the macroscopic adsorption results.
In this experiment, the fluorescence peak Lα of Eu(III) and Mn which is difficult tobe discriminated using conventional XAFS technique was discriminated. It formedthe basis of the studies on such complex systems.
The utility of high-resolution EXAFS technique has been well-demonstrated in thepresent study. The results of this work are important to understand thephysicochemical behavior of the interested radionuclides in the natural environment.
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