CN109406593B - Electrochemical in-situ reaction X-ray testing device - Google Patents
Electrochemical in-situ reaction X-ray testing device Download PDFInfo
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- CN109406593B CN109406593B CN201811143429.0A CN201811143429A CN109406593B CN 109406593 B CN109406593 B CN 109406593B CN 201811143429 A CN201811143429 A CN 201811143429A CN 109406593 B CN109406593 B CN 109406593B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
- G01N27/301—Reference electrodes
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Abstract
The invention belongs to the technical field of electrochemistry, and relates to an electrochemistry in-situ reaction X-ray testing device which mainly comprises an electrochemistry reaction chamber and a working electrode cover; the working electrode cover is arranged at the upper end of the electrochemical reaction chamber; the electrochemical reaction chamber is internally provided with a working electrode, a counter electrode and a reference electrode, and a testing window and a pore canal are arranged on a working electrode cover. The active material to be tested is coated on the top end of the working electrode without using a metal current collector, so that the problems of X-ray absorption by the current collector, weak X-ray signals, low result accuracy and the like are avoided. The device has the characteristics of small volume, simple structure, convenient assembly, repeated use and the like. The invention can continuously test the same pole piece, the obtained map has high signal-to-noise ratio, uniform current density of the working electrode and accurate test potential, is suitable for testing a two-electrode system and a three-electrode system, and has extremely excellent accuracy and stability in water-based electrolyte.
Description
Technical Field
The invention belongs to the technical field of electrochemistry, and relates to an electrochemistry in-situ reaction X-ray testing device.
Background
With the increasing severity of global environmental pollution and energy crisis, the development of clean and efficient energy storage devices is urgent. Rechargeable batteries are considered to be the most potential energy storage systems due to their high energy storage, high safety, environmental friendliness, and the like. The electrode material, which is an important component of the battery, determines the overall performance of the rechargeable battery to a large extent.
During charge and discharge, the electrode material undergoes a series of physical and chemical changes, such as phase changes and structural cracking. These variations can affect the electrochemical performance of the rechargeable battery and even play a decisive role. As an important analysis means in the research of the current energy storage field, the in-situ XRD technology can not only exclude the influence of external factors on the electrode material and improve the authenticity and reliability of monitoring data, but also monitor the electrochemical process of the electrode material in real time and reveal the intrinsic reaction mechanism of the electrode material. In situ XRD (XRD, X-ray diffractometer) testing is currently one of the fastest growing X-ray testing techniques. In short, in situ XRD is to let a sample be stationary and measure the diffraction pattern of the same sample under different conditions (such as temperature, current voltage, atmosphere, etc.). The in-situ test has the advantages of monitoring the change of the sample under the condition change in real time and truly reflecting the actual change of the system under the given condition. Therefore, the in-situ XRD characterization technology can truly monitor the introduction of the internal structure of the sample along with the change of reaction conditions (temperature, current voltage and atmosphere), can promote the understanding of the intrinsic energy storage mechanism of the electrode material, and can rapidly promote the development of high-performance energy storage devices.
The in-situ XRD technique can be used for researching reaction mechanism, specific occurrence process of phase change, catalytic mechanism of catalyst and the like. Therefore, the development and expansion of the test function of the X-ray diffractometer and the increase of the in-situ XRD test technology have important significance for researching reaction dynamics, electrode processes, catalytic mechanisms and interface reactions.
For researching the structural change of the battery material in the charge-discharge process, the in-situ XRD method does not need to pause the charge-discharge and disassemble the battery, so that the potential can be accurately measured and the change of the crystal structure of the electrode material in the charge-discharge process can be continuously tested, and the in-situ XRD technology is a powerful means for confirming whether the material has phase change in the charge-discharge process of the electrode, thereby being beneficial to researching the mechanism of the electrode process.
For an in-situ XRD reaction chamber, an in-situ X-ray electrolytic cell testing instrument reaction chamber produced by Bruker company is commercialized at present, and is a reaction chamber specially designed for in-situ X-ray diffraction test, but is expensive, inconvenient to maintain, and more importantly, when the reaction chamber is used for testing a water-based battery, electrolyte is easy to react with an electrolytic cell under the condition of externally applied voltage, so that the accuracy of a testing result is influenced.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides an electrochemical in-situ reaction X-ray testing device. Particularly when it is tested for aqueous batteries or aqueous capacitors, it exhibits excellent uniformity and stability. The method can supplement the factors of the prior art that the test result is unreliable due to the inaccurate electrochemical signal of the water-based electrolyte. The invention is applicable to not only aqueous electrolyte but also organic electrolyte and ionic liquid.
The technical scheme of the invention is as follows:
an electrochemical in-situ reaction X-ray testing device mainly comprises an electrochemical reaction chamber 9 and a working electrode cover 1; the working electrode cover 1 is arranged at the upper end of the electrochemical reaction chamber 9;
the electrochemical reaction chamber 9 is of a hollow cylinder structure with an opening at the upper end, and three threaded through holes are formed in the bottom of the electrochemical reaction chamber and are used for installing the working electrode 4, the counter electrode 6 and the reference electrode 8; the lower ends of the working electrode 4, the counter electrode 6 and the reference electrode 8 are arranged in threaded through holes of the electrochemical reaction chamber 9, the bottom end of the working electrode, the counter electrode and the reference electrode is positioned outside the electrochemical reaction chamber 9, and the rest of the working electrode, the counter electrode and the reference electrode are positioned inside the electrochemical reaction chamber 9 and are in contact with electrolyte; the bottom of the working electrode 4 is connected with a working electrode binding post 5, the bottom of the counter electrode 6 is connected with a counter electrode binding post 7, the bottom of the reference electrode 8 is connected with a reference electrode binding post, and the working electrode binding post 5, the counter electrode binding post 7 and the reference electrode binding post are connected with an electrochemical workstation;
the working electrode cover 1 is disc-shaped and is in threaded connection with the upper end of the electrochemical reaction chamber 9; a testing window 2 is arranged in the center of the working electrode cover 1, the testing window 2 is positioned above the working electrode 4, a film is stuck on the testing window 2, the active material to be tested is coated at the top end of the working electrode 4, and no gap exists between the lower surface of the film and the top end of the working electrode 4; a pore canal 3 is arranged on the working electrode cover 1, and the pore canal 3 is positioned above the reference electrode 8 and is used for injecting electrolyte;
when performing in situ XRD testing of a three-electrode system, the working electrode 4, the counter electrode 6 and the reference electrode 8 all work; when in-situ XRD testing of the two-electrode system is carried out, the reference electrode 8 is disassembled, and the through hole for installing the reference electrode 8 is plugged at the bottom of the electrochemical reaction chamber 9 by using a sealing plug.
The electrochemical reaction chamber 9 and the working electrode cover 1 are made of polytetrafluoroethylene.
The membrane on the test window 2 is made of polyimide film.
When the electrolyte is aqueous, the working electrode 4 is a glassy carbon electrode.
And rubber rings are sleeved at the connection ports of the working electrode 4, the counter electrode 6 and the reference electrode 8 and the electrochemical reaction chamber 9, so that electrolyte loss is prevented.
The counter electrode 6 is a platinum electrode or a graphite electrode.
The counter electrode 6 and the reference electrode 8 are replaced according to the specific requirements of the experiment.
The invention has the beneficial effects that:
1. the invention has simple structure, small volume, easy assembly and disassembly, light weight, portability and low price, and the invention does not need to use a diaphragm and a current collector.
2. The invention is suitable for in-situ XRD test of two-electrode system and three-electrode system, and especially when testing aqueous electrolyte, the invention shows extremely excellent accuracy and stability. The invention is not only applicable to aqueous electrolyte, but also applicable to other types of electrolyte.
3. The invention can control the current and the voltage at the same time; x-rays are transmitted through the test window to the active substance to be tested, then reflected to the XRD detector, and the detector reflects the signal change of the XRD detector to the computer in the form of XRD spectrum, so that the micro change of the sample in the electrochemical process is accurately tested.
4. The invention can continuously test the same pole piece, the obtained map has high signal-to-noise ratio, the current density of the working electrode is uniform, and the test potential is accurate.
Drawings
FIG. 1 is a schematic view of the apparatus of the present invention;
FIG. 2 (a) is a schematic diagram showing CV data of an acidic electrolyte tested by an existing in-situ XRD electrolytic cell;
FIG. 2 (b) is a schematic diagram showing CV data of the device of the present invention under the same electrolyte and the same material;
FIG. 3 (a) is a schematic diagram of the device of the present invention for testing Ti 3 C 2 In situ XRD data for acidic electrolytes;
FIG. 3 (b) shows a test V of the device according to the invention 2 Schematic of in situ XRD data for C under acid electrolyte;
FIG. 4 (a) isThe inventive device tests V 2 Schematic of in situ XRD data for C under neutral electrolyte;
FIG. 4 (b) shows a test V of the device according to the invention 2 Schematic of in situ XRD data under alkaline electrolyte.
In the figure: 1 a working electrode cover; 2, testing a window; 3 pore channels; 4, working electrode; 5 working electrode binding post; 6 pairs of electrodes; 7 pairs of electrode binding posts; 8, a reference electrode; 9 electrochemical reaction chamber.
Detailed Description
The following describes the embodiments of the present invention further with reference to the drawings and technical schemes.
As shown in fig. 1, the electrochemical in-situ reaction X-ray testing device of the invention comprises an electrochemical reaction chamber 9 and a working electrode cover 1, wherein a working electrode 4, a counter electrode 6 and a reference electrode 8 are arranged in the electrochemical reaction chamber 9. The working electrode cover 1 is located at the upper end of the electrochemical reaction chamber 9.
The electrochemical reaction chamber 9 is hollow and cylindrical, and the upper surface is provided with threads required for connection with the working electrode cover 1.
The working electrode 4, the counter electrode 6 and the reference electrode 8 are connected with the bottom of the electrochemical reaction chamber 9 through threads, and preferably a rubber ring can be sleeved at a connecting port of the working electrode 4, the counter electrode 6 and the reference electrode to prevent electrolyte from losing.
The electrochemical reaction chamber 9 is connected with the electrode working cover 1 through threads, and a test window 2 is formed in the center of the electrode working cover 1. The working electrode 4 is arranged right below the test window 2, the active material to be tested is coated between the working electrode 4 and the test window 2, and no gap and no diaphragm are needed between the working electrode 4 and the test window 2.
The counter electrode 6 can be arbitrarily changed according to experiments, such as platinum with stable working voltage, a graphite rod with low price and the like. The reference electrode 8 is the same as the reference electrode 8, and can be changed randomly according to the experimental type.
The contact part of the electrochemical reaction chamber 9 and the electrolyte does not need a metal binding post, so that a series of side reactions between the water-based electrolyte and the electrolyte under the condition of externally applied voltage are avoided, and the measurement result is more accurate.
The working electrode cover 1 can be provided with a circular pore canal 3, and electrolyte required by the electrochemical process can be added by injection.
The polyimide film which has no impurity peak under X-ray diffraction and is low in cost is adhered to the test window 2.
The electrochemical reaction chamber 9 and the working electrode cover 1 are made of Polytetrafluoroethylene (PTEE) materials.
In the invention, a current collector is not needed, and the active material to be tested can be directly loaded on the working electrode 4 through coating or deposition and other modes; when a current collector is used, it absorbs a large amount of X-ray signals, so in existing in situ XRD electrolytic cells, expensive and extremely toxic metallic beryllium has to be used to enhance the X-ray signals.
The assembled chemical reaction chamber 9 is fixed in place on the sample stage of the X-ray diffractometer. Then, the X-ray diffractometer and the electrochemical workstation are started in sequence, and relevant parameters are set according to the test requirements to carry out the test.
CV data under acid electrolyte was tested using an existing in situ XRD cell as shown in fig. 2 (a); CV data for the same material and the same electrolyte were tested using the apparatus of the present invention as shown in FIG. 2 (b).
Testing Ti using the inventive apparatus 3 C 2 In situ XRD data under acidic electrolyte is shown in FIG. 3 (a); testing V using the inventive apparatus 2 The in situ XRD data for C under acid electrolyte is shown in FIG. 3 (b).
Testing V using the inventive apparatus 2 The in situ XRD data of C under neutral electrolyte is shown in fig. 4 (a); testing V using the inventive apparatus 2 The in situ XRD data for C under alkaline electrolyte is shown in FIG. 4 (b).
Claims (10)
1. An electrochemical in-situ reaction X-ray testing device is characterized by comprising an electrochemical reaction chamber (9) and a working electrode cover (1); the working electrode cover (1) is arranged at the upper end of the electrochemical reaction chamber (9);
the electrochemical reaction chamber (9) is of a hollow cylinder structure with an opening at the upper end, and three threaded through holes are formed in the bottom of the electrochemical reaction chamber and are used 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) are arranged in a threaded through hole of the electrochemical reaction chamber (9), the bottom end of the working electrode, the counter electrode and the reference electrode is positioned outside the electrochemical reaction chamber (9), and the rest of the working electrode, the counter electrode and the reference electrode are positioned inside the electrochemical reaction chamber (9) and are in contact with electrolyte; the bottom of the working electrode (4) is connected with a working electrode binding post (5), the bottom of the counter electrode (6) is connected with a counter electrode binding post (7), the bottom of the reference electrode (8) is connected with a reference electrode binding post, and the working electrode binding post (5), the counter electrode binding post (7) and the reference electrode binding post are connected with an electrochemical workstation;
the working electrode cover (1) is disc-shaped and is in threaded connection with the upper end of the electrochemical reaction chamber (9); a testing window (2) is arranged at the center of the working electrode cover (1), the testing window (2) is positioned above the working electrode (4), a polyimide film is stuck on the testing window (2), an active material to be tested is coated at the top end of the working electrode (4), and no gap exists between the lower surface of the film and the top end of the working electrode (4); a pore canal (3) is arranged on the working electrode cover (1), and the pore canal (3) is positioned above the reference electrode (8) and is used for injecting electrolyte;
when in-situ XRD testing of a three-electrode system is carried out, the working electrode (4), the counter electrode (6) and the reference electrode (8) all work; when in-situ XRD test of the two-electrode system is carried out, the reference electrode (8) is disassembled, and a through hole for installing the reference electrode (8) is formed in the bottom of the electrochemical reaction chamber (9) by using a sealing plug.
2. An electrochemical in-situ reaction X-ray testing device according to claim 1, characterized in that the electrochemical reaction chamber (9) and the working electrode cover (1) are made of polytetrafluoroethylene; the membrane on the test window (2) is made of polyimide film.
3. An electrochemical in situ reaction X-ray testing device according to claim 1 or 2, characterized in that the counter electrode (6) and the reference electrode (8) are replaced according to the specific requirements of the experiment.
4. An electrochemical in situ reaction X-ray testing device according to claim 1 or 2, characterized in that the counter electrode (6) is a platinum electrode or a graphite electrode.
5. An electrochemical in situ reaction X-ray testing device according to claim 3, characterized in that the counter electrode (6) is a platinum electrode or a graphite electrode.
6. An electrochemical in-situ reaction X-ray testing device according to claim 1, 2 or 5, characterized in that when the electrolyte is aqueous, the working electrode (4) is a glassy carbon electrode.
7. An electrochemical in-situ reaction X-ray testing device according to claim 3, characterized in that when the electrolyte is aqueous, the working electrode (4) is a glassy carbon electrode.
8. An electrochemical in-situ reaction X-ray testing device according to claim 4, characterized in that when the electrolyte is aqueous, the working electrode (4) is a glassy carbon electrode.
9. An electrochemical in-situ reaction X-ray testing device according to claim 1, 2, 5, 7 or 8, characterized in that the connection ports of the working electrode (4), the counter electrode (6) and the reference electrode (8) and the electrochemical reaction chamber (9) are sleeved with rubber rings to prevent electrolyte loss.
10. The electrochemical in-situ reaction X-ray testing device according to claim 6, wherein rubber rings are sleeved at the connection ports of the working electrode (4), the counter electrode (6) and the reference electrode (8) and the electrochemical reaction chamber (9) to prevent electrolyte loss.
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Families Citing this family (5)
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| CN111830071B (en) * | 2019-04-14 | 2024-07-05 | 南杰智汇(深圳)科技有限公司 | Sample stage for in-situ electrochemical X-ray diffraction analysis |
| CN110361403B (en) * | 2019-08-20 | 2024-02-20 | 南杰智汇(深圳)科技有限公司 | X-ray diffraction analysis sample table with three-electrode electrochemical test function |
| CN110687146B (en) * | 2019-10-14 | 2022-06-24 | 北京工业大学 | X-ray diffraction in-situ testing device for electrochromic film |
| CN113376188B (en) * | 2021-05-12 | 2022-11-01 | 中国科学院高能物理研究所 | In-situ X-ray absorption spectrum measuring system and measuring method |
| CN114235865A (en) * | 2021-11-19 | 2022-03-25 | 华南理工大学 | Temperature-controllable lithium battery in-situ X-ray diffraction spectrum testing device |
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| JP2017072530A (en) * | 2015-10-09 | 2017-04-13 | ソニー株式会社 | Analysis cell and analysis cell assembly |
| CN106645240A (en) * | 2016-10-27 | 2017-05-10 | 深圳市贝特瑞新能源材料股份有限公司 | An electrolytic bath reaction chamber used for in-situ XRD tests and a testing method |
| CN207571950U (en) * | 2017-10-11 | 2018-07-03 | 中国石油大学(北京) | A kind of diffraction experimental device of in-situ TiC particles test |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102435625A (en) * | 2011-12-27 | 2012-05-02 | 东莞新能源科技有限公司 | Method and sample shelf for X-ray diffraction in-situ test |
| CN104297274A (en) * | 2014-11-07 | 2015-01-21 | 广西师范大学 | In-situ XRD reaction chamber for testing electrochemical reaction process |
| JP2017072530A (en) * | 2015-10-09 | 2017-04-13 | ソニー株式会社 | Analysis cell and analysis cell assembly |
| CN106645240A (en) * | 2016-10-27 | 2017-05-10 | 深圳市贝特瑞新能源材料股份有限公司 | An electrolytic bath reaction chamber used for in-situ XRD tests and a testing method |
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