In-situ pool for rapid and continuous synchrotron radiation X-ray absorption spectrum measurement

Abstract

The invention relates to the technical field of spectral measurement and analysis, and discloses an in-situ cell for rapid and continuous synchrotron radiation X-ray absorption spectrum measurement, the in-situ cell comprises a housing 1, one side of the housing 1 is provided with two through holes, and a counter electrode and a reference electrode are respectively fixed in the two through holes; the first shell and the second shell are correspondingly arranged, and square optical windows are arranged in the center of the second shell and the center of the first shell; the first shell and the second shell are each provided with a hole channel, the two hole channels are located on the two sides of the square optical window respectively, and a working electrode is fixedly arranged between the second shell and the first shell. The in-situ synchrotron radiation X-ray absorption spectrum measuring device is suitable for in-situ synchrotron radiation X-ray absorption spectrum measurement in a time-resolved energy dispersion / transmission mode, and through real-time supply and circular flow of the electrolyte on the surface of the working electrode, the uniformity of the X-ray penetrating through a solution layer is ensured, the elimination of product gas is accelerated, the influence of solution disturbance on a test signal is reduced, and the test stability is improved.

Description

TECHNICAL FIELD

[0001] The present application relates to the field of spectral measurement analysis, and particularly relates to an in-situ cell for rapid continuous synchrotron X-ray absorption spectrum measurement. BACKGROUND

[0002] Synchrotron X-ray absorption spectrum (XAS) technology is a powerful means to obtain information of atomic electronic structure and near-neighbor structure of a substance, and an electrochemical in-situ cell provides an in-situ dynamic research method for XAS technology.

[0003] The existing patent technology discloses a plurality of in-situ synchrotron electrochemical cells, which have a single application range. For example, the solution cavity of the existing synchrotron electrochemical in-situ cell is too thick, a large amount of electrolyte is needed, interference is strong, and the cell can only adapt to the traditional fluorescence mode back incidence X-ray absorption spectrum measurement means, which is time-consuming and difficult to real-time characterize the transient change and dynamic law of the local atomic and electronic structure of the material in a non-equilibrium state, resulting in a deviation between the experimental data and the actual situation, and seriously restricting the revelation of the whole picture of the real electrochemical reaction mechanism by the in-situ synchrotron spectrum technology.

[0004] Moreover, the distance between the electrodes of the existing in-situ cell is far, the mass transfer in the reaction process is limited, the upper limit of the voltage and current density is low, and the actual working condition demand cannot be met.

[0005] Although the in-situ synchrotron experiment in the energy dispersion / transmission mode greatly improves the test efficiency and time resolution, can continuously collect and real-time in-situ track the active structure, reaction intermediate evolution and electron transition, charge transfer behavior under the reaction working condition, and reveal the dynamic correlation between the material performance and the local structure, but the X-ray signal needs to penetrate the electrolyte to irradiate on the electrode in the collection mode, and the light signal will be severely interfered and strongly absorbed by the solution layer.

[0006] Therefore, it is necessary to design an in-situ cell for rapid continuous synchrotron X-ray absorption spectrum measurement. SUMMARY

[0007] The present application aims to provide an in-situ cell for rapid continuous synchrotron X-ray absorption spectrum measurement to solve the problems in the prior art.

[0008] The purpose of the present application can be achieved by the following technical solutions.

[0009] An in-situ cell for rapid continuous synchrotron X-ray absorption spectrum measurement, the in-situ cell comprises:

[0010] A first shell, one side of the first shell is provided with two through holes, and a counter electrode and a reference electrode are respectively fixed in the two through holes;

[0011] A second shell is arranged correspondingly to the first shell, and the second shell and the first shell are both provided with a square optical window at the center;

[0012] The first shell and the second shell are both provided with a hole, and the two holes are located on the two sides of the square optical window.

[0013] Further, the first shell is provided with a solution cavity on one side of the square optical window, and the solution cavity is composed of a trapezoidal liquid storage groove and a reaction chamber.

[0014] Further, the two holes are arranged oppositely.

[0015] Further, the first shell is provided with two through holes on the two sides, and the two through holes are respectively provided with a liquid inlet pipe and a liquid outlet pipe.

[0016] Further, the first shell and the second shell are both provided with a circular hole at the four corners, and the circular hole is connected with a fastening bolt for fixing the first shell and the second shell.

[0017] Further, a waterproof gasket is attached between the first shell and the second shell to improve the sealing performance of the reaction tank.

[0018] Further, the first shell and the second shell are both made of polyether ether ketone material.

[0019] Further, the square optical window is sealed with a Kapton film.

[0020] Further, the square optical window is closely attached to the working electrode, and the working electrode is fixedly provided with a conductive tape, and the conductive tape is clamped between the first shell and the second shell and is led out.

[0021] Further, the hole is a quadrangular frustum, and the included angle between the frustum and the horizontal is 45 degrees.

[0022] The beneficial effects of the present application are as follows:

[0023] 1. The present application is suitable for time-resolved energy dispersion / transmission mode in-situ synchrotron X-ray absorption spectrum measurement, and through real-time replenishment and circulation of the electrolyte on the surface of the working electrode, the uniformity of X-ray penetration through the solution layer is ensured, the product gas is removed quickly, the influence of solution disturbance on the test signal is reduced, and the test stability is improved.

[0024] 2、The in-situ cell structure of the application is compact, the shell is designed as a four-prism hole, and is highly adaptable to the light beam line station, and at the same time, has a thin liquid layer reaction microzone, which can reduce the loss of X-ray signals in the in-situ experiment process, so as to obtain high signal-to-noise ratio test signals, the compact three-electrode system has efficient mass transfer, and thus reliable reaction kinetic information of the local atomic and electronic structure of the sample under a non-equilibrium state is obtained;

[0025] 3、The X-ray solution of the application has less additional signal loss, reduces the absorption of the solution to the X-ray, the test stability of the in-situ cell is good, the signal strength is improved, and the subtle changes on the in-situ electrode are reflected in a faster time resolution. BRIEF DESCRIPTION OF DRAWINGS

[0026] The application will be further described below with reference to the drawings.

[0027] Figure 1 is an explosion structure schematic diagram of the in-situ cell of the application;

[0028] Figure 2 is a partial structure schematic diagram of the in-situ cell of the application;

[0029] Figure 3 is a side view of the in-situ cell structure of the application;

[0030] Figure 4 is a whole structure schematic diagram of the in-situ cell of the application.

[0031] The signs are explained as follows:

[0032] 1, outer shell one; 2, square optical window; 3, solution cavity; 4, outer shell two; 5, counter electrode; 6, reference electrode; 7, working electrode; 8, liquid inlet pipe; 9, liquid outlet pipe; 10, reaction chamber; 11, liquid storage groove; 12, bolt; 13, conductive tape; 14, hole; 15, Kapton film. DETAILED DESCRIPTION

[0033] The technical solutions in the embodiments of the application will be clearly and completely described below with reference to the drawings in the embodiments of the application. Obviously, the described embodiments are only part of the embodiments of the application, rather than all the embodiments of the application. Based on the embodiments in the application, all other embodiments obtained by those skilled in the art without creative labor fall within the protection scope of the application.

[0034] An in-situ cell for fast continuous synchrotron X-ray absorption spectrum measurement, like Figure 1 、 Figure 2As shown, it comprises a shell 1, a shell 1 is fixedly provided with a shell 2, a square optical window 2 is formed in the center of the shell 2, a hole 14 is formed in the shell 2, the hole 14 is located above the square optical window 2, and the square optical window 2 corresponds to the center of the shell 1.

[0035] A solution cavity 3 is formed in the shell 1 and located on one side of the square optical window 2, the solution cavity 3 is divided into a trapezoidal liquid storage groove 11 and a reaction chamber 10, the trapezoidal liquid storage groove 11 is located on one side of the reaction chamber 10, and the center of the shell 1 is also provided with a hole 14, and the two holes 14 are oppositely arranged.

[0036] Two through holes are formed in one side of the shell 1, and a counter electrode 5 and a reference electrode 6 are respectively placed in the two through holes, and through holes are formed on both sides of the shell 1, and a liquid inlet pipe 8 and a liquid outlet pipe 9 are respectively connected in the through holes.

[0037] Circular holes are formed at the four corners of the shell 1 for placing fastening bolts 12, and circular holes are also formed in the corresponding positions of the shell 2.

[0038] The shell 1 and the shell 2 are attached by waterproof gaskets, and then fixed by four bolts 12 passing through the circular holes, to ensure the tightness and stability between the components.

[0039] In this embodiment, the shell 1 and the shell 2 are both made of polyether ether ketone (PEEK) material.

[0040] Kapton films 15 are respectively placed in the square optical windows 2 in the centers of the shell 1 and the shell 2 for sealing, a working electrode 7 is fixedly arranged between the shell 1 and the shell 2, and the square optical window 2 is tightly attached to the working electrode 7.

[0041] The edge of the working electrode 7 is fixedly connected with a conductive tape 13, the conductive tape 13 is placed in the reaction chamber 10 of the shell 1, the working electrode 7 is located in the middle of the shell 1 and the shell 2 and is fixed by the conductive tape 13, and the conductive tape 13 is led out from between the shell 1 and the shell 2.

[0042] The depth of the trapezoidal liquid storage groove 11 in the solution cavity 3 is 10mm, the upper base and the lower base are 6mm*12mm, the depth of the reaction chamber 10 is 1mm, and the length and width are 20mm*20mm. The center of the shell 1 and the shell 2 is provided with a hole 14, which gradually shrinks in the direction of the square optical window 2, the hole 14 is a quadrangular frustum, the included angle between the frustum and the horizontal is 45 degrees, the outer diameter of the hole 14 is 40mm, and the inner diameter is 10mm.

[0043] In this embodiment, the reference electrode 6 is a silver-silver chloride electrode, a mercury-mercury oxide electrode or a standard hydrogen electrode, and the counter electrode 5 is a platinum wire or a carbon rod, which is inserted and fixed in the corresponding groove by a sealing ring.

[0044] In the in-situ test process, the shell one 1 and the shell two 4 are fixed by the bolt 12, then the electrolyte is injected into the reaction chamber 10 and the liquid storage groove 11 from the liquid inlet pipe 8 on both sides of the shell one 1, the liquid outlet pipe 9 is used for discharging the electrolyte, after the electrolyte circulation is stable, the counter electrode 5 and the reference electrode 6 are inserted into the corresponding counter electrode hole and the reference electrode hole above the shell one 1, a complete three-electrode electrochemical in-situ reaction cell system is constructed, and the time-resolved energy dispersive X-ray absorption spectroscopy synchronous acquisition experiment is started.

[0045] The communication liquid storage groove 11 above the reaction chamber 10 is arranged to realize the regulation and supply function of the thin liquid layer at the working electrode; the millimeter thick reaction chamber is designed, and the square optical window is closely attached to the working electrode to realize the micron level solution layer in the light path; the compact three-electrode arrangement and the solution circulation are arranged to achieve the current density closer to the actual working condition and reduce the influence of solution disturbance on the signal; the square optical window 2 selects the polyimide film (Kapton film) to reduce the loss of X-ray passing through the window; the four-prism incident and exit channels on the shell can increase the light flux.

[0046] The basic principle, main features and advantages of the present application are shown and described above. It should be understood by those skilled in the art that the present application is not limited by the above examples, and the above examples and descriptions in the specification are only to illustrate the principle of the present application, and various changes and improvements can be made without departing from the spirit and scope of the present application, and these changes and improvements all fall within the scope of the present application.

Claims

1. An in-situ cell for fast, continuous synchrotron X-ray absorption spectroscopy measurements, characterized in that, The in-situ cell comprises: a shell one (1), one side of which is provided with two through holes, in which a counter electrode (5) and a reference electrode (6) are respectively fixed; a shell two (4), which is correspondingly arranged with the shell one (1), and is provided with a square optical window (2) at the center of the shell two (4) and the shell one (1); the shell one (1) and the shell two (4) are both provided with a hole (14), and the two holes (14) are respectively located on the two sides of the square optical window (2), and a working electrode (7) is fixed between the shell two (4) and the shell one (1).

2. The in-situ cell for fast, sequential synchrotron X-ray absorption spectroscopy measurements according to claim 1, wherein, the shell one (1) is provided with a solution cavity (3) on one side of the square optical window (2), which is composed of a trapezoidal liquid storage groove (11) and a reaction chamber (10), and the trapezoidal liquid storage groove (11) is located on one side of the reaction chamber (10).

3. The in-situ cell for fast, sequential synchrotron X-ray absorption spectroscopy measurements according to claim 1, wherein, The two holes (14) are oppositely arranged.

4. The in-situ cell for fast, sequential synchrotron X-ray absorption spectroscopy measurements according to claim 2, wherein, The shell one (1) is provided with through holes on both sides, and the two through holes are respectively fixed with a liquid inlet pipe (8) and a liquid outlet pipe (9).

5. The in-situ cell for fast, sequential synchrotron X-ray absorption spectroscopy measurements according to claim 4, wherein, The shell one (1) and the shell two (4) are both provided with circular holes at the four corners, which are connected with fastening bolts (12) for fixing the shell one (1) and the shell two (4).

6. The in-situ cell for fast, sequential synchrotron X-ray absorption spectroscopy measurements according to claim 1, wherein, A waterproof gasket is attached between the shell one (1) and the shell two (4) to improve the sealing performance of the reaction cell.

7. The in-situ cell for fast, sequential synchrotron X-ray absorption spectroscopy measurements according to any one of claims 1 to 6, characterized in that, The shell one (1) and the shell two (4) are both made of polyether ether ketone material.

8. The in-situ cell for fast, sequential synchrotron X-ray absorption spectroscopy measurements according to claim 1, wherein, The square optical window (2) is sealed with a Kapton film (15).

9. The in-situ cell for fast, sequential synchrotron X-ray absorption spectroscopy measurements according to claim 2, wherein, The square optical window (2) is closely attached with the working electrode (7), and the working electrode (7) is fixed with a conductive adhesive tape (13) at the edge, which is clamped between the shell one (1) and the shell two (4) and led out.

10. The in-situ cell for fast, sequential synchrotron X-ray absorption spectroscopy measurements according to any one of claims 1 to 6, characterized in that, The hole (14) is a quadrangular frustum, and the included angle between the frustum and the horizontal is 45 degrees.

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