CN109406593B - Electrochemical in-situ reaction X-ray testing device - Google Patents
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Abstract
本发明属于电化学技术领域，涉及一种电化学原位反应X射线测试装置，主要由电化学反应室和工作电极盖组成；工作电极盖安装在电化学反应室的上端；电化学反应室内部安装有工作电极、对电极和参比电极，工作电极盖上设有测试窗口和孔道。待测试的活性材料涂覆在工作电极顶端，无需使用金属集流体，从而避免了集流体对X射线的吸收，X射线信号弱，结果准确性低等问题。本发明的装置具有体积小，结构简单，组装便捷，可重复利用等特点。本发明可对同一极片进行连续测试，所得图谱信噪比高，工作电极电流密度均匀，测试电位准确，适用于两电极体系以及三电极体系测试，且在水系电解液中表现出极其优异的准确性以及稳定性。
The invention belongs to the technical field of electrochemistry and relates to an electrochemical in-situ reaction X-ray testing device, which mainly consists of an electrochemical reaction chamber and a working electrode cover; the working electrode cover is installed at the upper end of the electrochemical reaction chamber; inside the electrochemical reaction chamber A working electrode, a counter electrode and a reference electrode are installed, and the working electrode cover is provided with a test window and a hole. The active material to be tested is coated on the top of the working electrode, eliminating the need to use a metal current collector, thereby avoiding problems such as absorption of X-rays by the current collector, weak X-ray signals, and low accuracy of results. The device of the invention has the characteristics of small size, simple structure, convenient assembly, and reusability. The invention can continuously test the same pole piece, and the resulting spectrum has a high signal-to-noise ratio, a uniform working electrode current density, and an accurate test potential. It is suitable for testing two-electrode systems and three-electrode systems, and exhibits extremely excellent performance in aqueous electrolytes. accuracy and stability.
Description
技术领域Technical field
本发明属于电化学技术领域，涉及一种电化学原位反应X射线测试装置。The invention belongs to the technical field of electrochemistry and relates to an electrochemical in-situ reaction X-ray testing device.
背景技术Background technique
随着全球环境污染和能源危机日益严峻，开发清洁高效储能装置迫在眉睫。可充电电池因具有高效能量储存，高安全性，环境友好性等特点，被认为是最具潜力的能量存储系统。电极材料作为电池的重要组成部分，在很大程度上决定了可充电电池的整体性能。As global environmental pollution and energy crisis become increasingly severe, the development of clean and efficient energy storage devices is urgent. Rechargeable batteries are considered to be the most potential energy storage system due to their high-efficiency energy storage, high safety, and environmental friendliness. As an important component of batteries, electrode materials determine the overall performance of rechargeable batteries to a large extent.
在充放电过程中，电极材料会发生一系列物理和化学变化，如相变和结构裂化等。这些变化会影响可充电电池的电化学性能，甚至起决定性作用。原位XRD技术作为当前储能领域研究中重要的分析手段，它不仅可排除外界因素对电极材料产生的影响，提高监测数据的真实性和可靠性，还可对电极材料的电化学过程进行实时监测，并揭示其本征反应机制。原位XRD(XRD即X射线衍射仪)测试技术是目前发展最快的一种X射线测试技术。简而言之，原位XRD是让样品不动，测量同一样品在不同的条件(如温度，电流电压、气氛等)下的衍射图谱。原位测试的优点在于能时时监控样品在条件改变时所发生的变化，能真实地反应体系在给定条件下的实际变化。因此，原位XRD表征技术能真实地监测样品内部结构随反应条件(温度、电流电压、气氛)的变化的引入，可提升我们对电极材料本征储能机制的理解，并将快速推动高性能储能器件的发展。During the charge and discharge process, electrode materials undergo a series of physical and chemical changes, such as phase changes and structural cracking. These changes can affect or even play a decisive role in the electrochemical performance of rechargeable batteries. In-situ XRD technology is an important analytical method in current research in the field of energy storage. It can not only eliminate the influence of external factors on electrode materials, improve the authenticity and reliability of monitoring data, but also conduct real-time analysis of the electrochemical process of electrode materials. Monitor and reveal its intrinsic reaction mechanism. In-situ XRD (XRD, X-ray diffractometer) testing technology is currently the fastest growing X-ray testing technology. In short, in-situ XRD keeps the sample motionless and measures the diffraction patterns of the same sample under different conditions (such as temperature, current, voltage, atmosphere, etc.). The advantage of in-situ testing is that it can constantly monitor the changes in the sample when conditions change, and can truly reflect the actual changes in the system under given conditions. Therefore, the introduction of in-situ XRD characterization technology that can truly monitor changes in the internal structure of samples with reaction conditions (temperature, current, voltage, and atmosphere) can improve our understanding of the intrinsic energy storage mechanism of electrode materials and will quickly promote high performance Development of energy storage devices.
原位XRD技术可以用于研究反应的机理、相变的具体发生过程以及催化剂的催化机理等。因此，开发扩展X射线衍射仪的测试功能，加大原位XRD测试技术对研究反应动力学、电极过程、催化机理以及界面反应具有重要的意义。In-situ XRD technology can be used to study the reaction mechanism, the specific occurrence process of phase change, and the catalytic mechanism of the catalyst. Therefore, it is of great significance to develop and expand the testing functions of X-ray diffractometers and increase in-situ XRD testing technology to study reaction kinetics, electrode processes, catalytic mechanisms and interface reactions.
对于研究电池材料在充放电过程中其结构变化，原位XRD方法无须暂停充放电和拆卸电池，因而可以精确测定电位并连续测试电极材料晶体结构在充放电过程中的变化，原位XRD技术是证实电极充放电过程中材料是否存在相变的有力手段，有利于研究电极过程的机理。For studying the structural changes of battery materials during the charge and discharge process, the in-situ XRD method does not require suspending charge and discharge and disassembling the battery, so it can accurately measure the potential and continuously test the changes in the crystal structure of the electrode material during the charge and discharge process. In-situ XRD technology is It is a powerful means to confirm whether there is a phase change in the material during the electrode charging and discharging process, and is conducive to studying the mechanism of the electrode process.
对于原位XRD反应室，目前已商品化的有Bruker公司生产的原位X射线电解池测试仪器反应室，它是专门设计用来进行原位X射线衍射试验的反应室，但是其价格昂贵，维修不方便，更重要的是，当其测试水系电池时，在外加电压条件下，其电解液易与其电解池发生反应，影响其测试结果的准确性。As for the in-situ XRD reaction chamber, the in-situ X-ray electrolytic cell test instrument reaction chamber produced by Bruker Company is currently commercialized. It is a reaction chamber specially designed to conduct in-situ X-ray diffraction tests, but it is expensive. Maintenance is inconvenient. More importantly, when it tests aqueous batteries, its electrolyte easily reacts with its electrolytic cell under external voltage conditions, affecting the accuracy of its test results.
发明内容Contents of the invention
针对现有技术的不足，本发明提供一种电化学原位反应X射线测试装置。尤其当其测试水系电池或水系电容器时，其展现出优异的均一性与稳定性。可补充现有技术在水系电解液下其电化学信号不准确导致测试结果不可信因素。本发明不仅适用于水系电解液同样也适用于有机电解液以及离子液体。In view of the shortcomings of the existing technology, the present invention provides an electrochemical in-situ reaction X-ray testing device. Especially when testing aqueous batteries or aqueous capacitors, it shows excellent uniformity and stability. It can supplement the existing technology's inaccurate electrochemical signals in aqueous electrolyte, leading to unreliable test results. The present invention is applicable not only to aqueous electrolytes but also to organic electrolytes and ionic liquids.
本发明的技术方案：Technical solution of the present invention:
一种电化学原位反应X射线测试装置，主要由电化学反应室9和工作电极盖1组成；所述的工作电极盖1安装在电化学反应室9的上端；An electrochemical in-situ reaction X-ray testing device mainly consists of an electrochemical reaction chamber 9 and a working electrode cover 1; the working electrode cover 1 is installed on the upper end of the electrochemical reaction chamber 9;
所述的电化学反应室9为上端开口的空心圆柱体结构，其底部设有三个带螺纹的通孔，用于安装工作电极4、对电极6和参比电极8；所述的工作电极4、对电极6和参比电极8，三者的下端安装在电化学反应室9的带螺纹的通孔中，且底端位于电化学反应室9外部，其余部分位于电化学反应室9的内部，与电解液相接触；所述的工作电极4的底部连接有工作电极接线柱5，所述的对电极6的底部连接有对电极接线柱7，所述的参比电极8的底部连接有参比电极接线柱，工作电极接线柱5、对电极接线柱7和参比电极接线柱与电化学工作站相连接；The electrochemical reaction chamber 9 is a hollow cylindrical structure with an open upper end, and three threaded through holes are provided at the bottom for installing the working electrode 4, the counter electrode 6 and the reference electrode 8; the working electrode 4 , the counter electrode 6 and the reference electrode 8, the lower ends of which are installed in the threaded through holes of the electrochemical reaction chamber 9, and the bottom ends are located outside the electrochemical reaction chamber 9, and the remaining parts are located inside the electrochemical reaction chamber 9 , in contact with the electrolyte; the bottom of the working electrode 4 is connected to the working electrode terminal 5, the bottom of the counter electrode 6 is connected to the counter electrode terminal 7, and the bottom of the reference electrode 8 is connected to The reference electrode terminal, working electrode terminal 5, counter electrode terminal 7 and reference electrode terminal are connected to the electrochemical workstation;
所述的工作电极盖1为圆盘状，与电化学反应室9的上端螺纹连接；工作电极盖1的中心处设有测试窗口2，测试窗口2位于工作电极4的上方，测试窗口2上贴有膜，待测试的活性材料涂覆在工作电极4顶端，且膜的下表面与工作电极4顶端之间无缝隙；工作电极盖1上设有孔道3，孔道3位于参比电极8上方，用于注入电解液；The working electrode cover 1 is disc-shaped and is threadedly connected to the upper end of the electrochemical reaction chamber 9; a test window 2 is provided at the center of the working electrode cover 1, and the test window 2 is located above the working electrode 4. A film is attached, and the active material to be tested is coated on the top of the working electrode 4, and there is no gap between the lower surface of the film and the top of the working electrode 4; the working electrode cover 1 is provided with a hole 3, and the hole 3 is located above the reference electrode 8 , used to inject electrolyte;
当进行三电极体系的原位XRD测试时，工作电极4、对电极6和参比电极8均工作；当进行两电极体系的原位XRD测试时，将参比电极8拆卸，并用密封塞封堵电化学反应室9底部用于安装参比电极8的通孔。When performing an in-situ XRD test of a three-electrode system, the working electrode 4, counter electrode 6 and reference electrode 8 are all working; when performing an in-situ XRD test of a two-electrode system, the reference electrode 8 is disassembled and sealed with a sealing plug. Plug the through hole at the bottom of the electrochemical reaction chamber 9 for installing the reference electrode 8 .
所述的电化学反应室9和工作电极盖1的材质为聚四氟乙烯。The material of the electrochemical reaction chamber 9 and the working electrode cover 1 is polytetrafluoroethylene.
所述的测试窗口2上的膜的材质为聚酰亚胺薄膜。The material of the film on the test window 2 is polyimide film.
当电解液为水系时，工作电极4为玻碳电极。When the electrolyte is aqueous, the working electrode 4 is a glassy carbon electrode.
所述的工作电极4、对电极6和参比电极8与电化学反应室9的连接口处套有橡胶圈，防止电解液流失。The connection ports of the working electrode 4, the counter electrode 6 and the reference electrode 8 and the electrochemical reaction chamber 9 are covered with rubber rings to prevent electrolyte loss.
所述的对电极6为铂金电极或石墨电极。The counter electrode 6 is a platinum electrode or a graphite electrode.
所述的对电极6和参比电极8根据实验的具体要求进行更换。The counter electrode 6 and reference electrode 8 are replaced according to the specific requirements of the experiment.
本发明的有益效果：Beneficial effects of the present invention:
1、本发明结构简单、体积小、易于组装和拆卸、质轻便于携带、价格低廉，且本发明中无需使用隔膜以及集流体。1. The present invention has a simple structure, small volume, easy assembly and disassembly, light weight and portability, and low price. There is no need to use a diaphragm or a current collector in the present invention.
2、本发明适用于两电极体系以及三电极体系的原位XRD测试，尤其当测试水系电解液时，其表现出极其优异的准确性与稳定性。本发明不仅仅适用于水系电解液，同样适用于其它种类电解液。2. The present invention is suitable for in-situ XRD testing of two-electrode systems and three-electrode systems. Especially when testing aqueous electrolytes, it shows extremely excellent accuracy and stability. The present invention is not only applicable to aqueous electrolytes, but is also applicable to other types of electrolytes.
3、本发明可以同时控制电流和电压；X射线透过测试窗口射到待测的活性物质上，然后反射到XRD的探测器上，探测器再以XRD谱的形式将其信号变化反映到计算机上，从而精确测试出样品在电化学过程发生的微小变化。3. The present invention can control current and voltage at the same time; to accurately measure the tiny changes that occur in the electrochemical process of the sample.
4、本发明可对同一极片进行连续测试，所得图谱信噪比高，工作电极电流密度均匀，测试电位准确。4. The present invention can continuously test the same pole piece, and the obtained spectrum has a high signal-to-noise ratio, a uniform working electrode current density, and an accurate test potential.
附图说明Description of drawings
图1为本发明装置的示意图；Figure 1 is a schematic diagram of the device of the present invention;
图2(a)为现有原位XRD电解池测试酸性电解液CV数据示意图；Figure 2(a) is a schematic diagram of the CV data of the acidic electrolyte tested by the existing in-situ XRD electrolytic cell;
图2(b)为本发明装置测试同一材料同一电解液下的CV数据示意图；Figure 2(b) is a schematic diagram of CV data tested by the device of the present invention under the same material and the same electrolyte;
图3(a)为本发明装置测试Ti3C2在酸性电解液下的原位XRD数据示意图；Figure 3(a) is a schematic diagram of the in-situ XRD data of the device of the present invention testing Ti 3 C 2 under acidic electrolyte;
图3(b)为本发明装置测试V2C在酸性电解液下的原位XRD数据示意图；Figure 3(b) is a schematic diagram of the in-situ XRD data of the device of the present invention testing V 2 C under acidic electrolyte;
图4(a)为本发明装置测试V2C在中性电解液下的原位XRD数据示意图；Figure 4(a) is a schematic diagram of the in-situ XRD data of the device of the present invention testing V 2 C under neutral electrolyte;
图4(b)为本发明装置测试V2C在碱性电解液下的原位XRD数据示意图。Figure 4(b) is a schematic diagram of the in-situ XRD data of V 2 C tested in alkaline electrolyte by the device of the present invention.
图中：1工作电极盖；2测试窗口；3孔道；4工作电极；5工作电极接线柱；6对电极；7对电极接线柱；8参比电极；9电化学反应室。In the picture: 1 working electrode cover; 2 test window; 3 holes; 4 working electrodes; 5 working electrode terminals; 6 pairs of electrodes; 7 pairs of electrode terminals; 8 reference electrode; 9 electrochemical reaction chamber.
具体实施方式Detailed ways
以下结合附图和技术方案，进一步说明本发明的具体实施方式。The specific embodiments of the present invention will be further described below in conjunction with the accompanying drawings and technical solutions.
如图1所示，本发明所述的一种电化学原位反应X射线测试装置，包括电化学反应室9和工作电极盖1，电化学反应室9的内部设置工作电极4、对电极6和参比电极8。工作电极盖1位于电化学反应室9的上端。As shown in Figure 1, an electrochemical in-situ reaction X-ray testing device according to the present invention includes an electrochemical reaction chamber 9 and a working electrode cover 1. The electrochemical reaction chamber 9 is provided with a working electrode 4 and a counter electrode 6 inside. and reference electrode 8. The working electrode cover 1 is located at the upper end of the electrochemical reaction chamber 9 .
所述的电化学反应室9呈中空圆柱形，上表面设有与工作电极盖1连接所需的螺纹。The electrochemical reaction chamber 9 is in the shape of a hollow cylinder, and the upper surface is provided with threads required for connection with the working electrode cover 1 .
所述的工作电极4、对电极6和参比电极8，通过螺纹与电化学反应室9的底部相连接，优选地可在其连接口处套有橡胶圈防止电解液流失。The working electrode 4, the counter electrode 6 and the reference electrode 8 are connected to the bottom of the electrochemical reaction chamber 9 through threads. Preferably, a rubber ring can be placed at the connection port to prevent the loss of electrolyte.
所述的电化学反应室9与电极工作盖1两者通过螺纹相连接，在电极工作盖1的中心处开有测试窗口2。测试窗口2的正下方即为工作电极4，工作电极4与测试窗口2之间涂有待测的活性材料，工作电极4与测试窗口2之间无需缝隙且无需隔膜。The electrochemical reaction chamber 9 and the electrode working cover 1 are connected through threads, and a test window 2 is opened in the center of the electrode working cover 1 . Directly below the test window 2 is the working electrode 4. The active material to be tested is coated between the working electrode 4 and the test window 2. There is no gap or separator between the working electrode 4 and the test window 2.
所述的对电极6可根据实验进行任意更改，例如可选工作电压稳定的铂金以及价格低廉的石墨棒等。其参比电极8同理，可根据实验类型，进行任意更改。The counter electrode 6 can be changed arbitrarily according to the experiment, for example, platinum with stable working voltage and low-price graphite rod can be selected. The reference electrode 8 is the same and can be changed arbitrarily according to the type of experiment.
所述的电化学反应室9与电解液接触部分，无需金属接线柱，避免了水系电解液在外加电压的条件下与电解液发生一系列的副反应，使测量结果更为准确。The part of the electrochemical reaction chamber 9 that is in contact with the electrolyte does not require metal terminals, which avoids a series of side reactions between the aqueous electrolyte and the electrolyte under the condition of external voltage, making the measurement results more accurate.
所述的工作电极盖1上可开一圆形的孔道3，可使用注射方式加入电化学过程所需电解液。A circular hole 3 can be opened on the working electrode cover 1, and the electrolyte required for the electrochemical process can be added by injection.
所述的测试窗口2上贴有为X射线衍射下无杂相峰且价格低廉的聚酰亚胺膜。The test window 2 is pasted with a low-price polyimide film that has no impurity peaks under X-ray diffraction.
所述的电化学反应室9和工作电极盖1均以聚四氟乙烯(PTEE)材质制成。The electrochemical reaction chamber 9 and the working electrode cover 1 are both made of polytetrafluoroethylene (PTEE).
在本发明中无需使用集流体，可直接将待测活性材料可通过涂覆或沉积等方式负载到工作电极4上；当使用集流体时，其集流体会吸收大量的X射线信号，所以在现有的原位XRD电解池中，不得不使用价格高昂且毒性极强的金属铍，以增强X射线信号。In the present invention, there is no need to use a current collector, and the active material to be measured can be directly loaded onto the working electrode 4 through coating or deposition. When a current collector is used, the current collector will absorb a large amount of X-ray signals, so in In existing in-situ XRD electrolytic cells, the expensive and highly toxic metal beryllium has to be used to enhance the X-ray signal.
将组装好的化学反应室9固定在X射线衍射仪的样品台位置。然后依次启动X射线衍射仪和电化学工作站，并按测试要求设定相关参数，进行测试。Fix the assembled chemical reaction chamber 9 on the sample stage of the X-ray diffractometer. Then start the X-ray diffractometer and electrochemical workstation in sequence, set the relevant parameters according to the test requirements, and conduct the test.
使用现有原位XRD电解池测试酸性电解液下的CV数据如图2(a)所示；使用本发明装置测试同一材料同一电解液下的CV数据如图2(b)所示。The CV data using the existing in-situ XRD electrolytic cell to test the acidic electrolyte is shown in Figure 2(a); the CV data using the device of the present invention to test the same material and the same electrolyte is shown in Figure 2(b).
使用本发明装置测试Ti3C2在酸性电解液下的原位XRD数据如图3(a)所示；使用本发明装置测试V2C在酸性电解液下的原位XRD数据如图3(b)所示。The in-situ XRD data of Ti 3 C 2 under acidic electrolyte tested using the device of the present invention is shown in Figure 3(a); the in-situ XRD data of V 2 C tested under acidic electrolyte using the device of the present invention is shown in Figure 3( b) shown.
使用本发明装置测试V2C在中性电解液下的原位XRD数据如图4(a)所示；使用本发明装置测试V2C在碱性电解液下的原位XRD数据如图4(b)所示。The in-situ XRD data of V 2 C under neutral electrolyte tested using the device of the present invention is shown in Figure 4(a); the in-situ XRD data of V 2 C tested under alkaline electrolyte using the device of the present invention is shown in Figure 4 (b) is shown.
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