Device and method for testing in-situ XRD (X-Ray Diffraction) data in metal electrodeposition

Abstract

The invention belongs to the technical field of metal electrodeposition, and particularly relates to a device and a method for testing in-situ XRD (X-Ray Diffraction) data in metal electrodeposition. Comprising a box body, the bottom of the box body is closed, an anode plate is placed at the bottom end in the box body, and the top of the box body is open; a pair of supporting rods is horizontally mounted in the box body, a diaphragm is placed above the supporting rods, a cathode screen plate is placed above the diaphragm, and electrolyte in the box body is in contact with the diaphragm but is not higher than the diaphragm; according to the invention, effective XRD diffraction data can be measured while electro-deposition and XRD testing are carried out at the same time; according to the invention, it can be ensured that the unit area density is large enough to obtain XRD data, electrolyte can be ensured to be fully distributed among meshes to facilitate electrodeposition, and the test error is comprehensively reduced; the device is simple to assemble, easy to operate and low in cost, and can realize rapid switching and connection between in-situ testing and common testing.

Description

Technical Field

[0001] The invention belongs to the technical field of metal electrodeposition, and in particular relates to a device and a method for testing in-situ XRD data in metal electrodeposition. Background Art

[0002] Electrodeposition is a technology based on the specific metal ions in the electrolyte receiving electrons under the action of an external electric field and reducing and depositing on the cathode surface to achieve material replication and formation. The entire process is carried out in a specific electrolyte solution. The electrode reaction equation is as follows:

[0003] Anode reaction: M-ne - →M n+ ;

[0004] Cathode reaction: M n+ +ne - →M;

[0005] Electrodeposition is the basis of metal electrorefining, electroplating and other technologies, including direct current electrodeposition, pulse electrodeposition, jet electrodeposition, composite electrodeposition, ultrasonic electrodeposition and other methods. The materials obtained by electrodeposition are widely used in catalysis, energy storage, corrosion-resistant coating and other aspects due to the unique structure of the deposited layer combined with the substrate. The difficulty of metal electrodeposition and the morphology of the deposit are related to the properties of the deposited metal, and also depend on factors such as the composition of the electrolyte, pH value, temperature, and current density. In the actual operation process, by adjusting the electrolyte composition, pH value, temperature and other conditions, deposits with different preferred orientations and different microscopic morphologies can be obtained. The preferred orientation of the electrodeposited sample has an important influence on the magnetism, elasticity and corrosion resistance of the material. Therefore, it is particularly important to study the changes in the orientation of the metal during the electrodeposition process. The real-time changes in the phase structure of the cathode surface during the electrodeposition process are studied by in-situ XRD technology. According to the results, the relationship between the electrodeposition parameters and the microstructure of the material is further explored to provide theoretical support for obtaining materials with specific properties.

[0006] However, since the electrodeposition process requires that the deposited surface of the cathode material is in full contact with the solution in order to be successfully deposited, and the XRD test needs to eliminate the interference of the solution layer in order to measure effective data, this brings challenges to the in-situ XRD test of electrodeposition; at the same time, how to overcome the error of in-situ XRD test data in electrodeposition is also an important factor affecting whether obvious orientation change data can be obtained in the end. Summary of the invention

[0007] In order to solve the shortcomings of the prior art, the present invention provides a device and method for testing in-situ XRD data in metal electrodeposition. The present invention ultimately realizes that effective XRD diffraction data can be measured while electrodeposition and XRD testing are carried out simultaneously; the present invention can ensure that the density per unit area is large enough to obtain XRD data, and can ensure that the electrolyte is fully distributed between the meshes to facilitate electrodeposition, thereby comprehensively reducing the test error; the present invention is simple to assemble, easy to operate, and low in cost, and can realize rapid switching and connection between in-situ testing and ordinary testing.

[0008] In order to achieve the above object, the present invention adopts the following technical solution:

[0009] A device for testing in-situ XRD data in metal electrodeposition, comprising a box, the bottom of which is closed and an anode plate is placed at the bottom of the box, and the top of the box is open; a pair of support rods are horizontally installed inside the box, a diaphragm is placed above the support rods, a cathode mesh plate is placed above the diaphragm, and an electrolyte in the box is in contact with the diaphragm but not higher than the height of the diaphragm;

[0010] The anode plate is fixedly connected with a wire, and a wire hole is opened below the side wall of the box body. The wire passes through the wire hole and is sealed and fixedly connected with the wire hole; the cathode mesh plate is also fixedly connected with a wire; the outer side wall of the box body is horizontally installed with a positioning card board, and the positioning card board is connected to the test card slot of the XRD instrument.

[0011] Furthermore, the positioning card plate is provided with an opening, and the outer side wall of the box body is correspondingly provided with a card slot, and the positioning card plate is inserted into the card slot of the outer side wall of the box body through the opening for installation.

[0012] Furthermore, one side of the positioning card plate is fixedly connected with a wire fixing mechanism, and the wire fixing mechanism includes an L-shaped bracket, one end of the L-shaped bracket is fixedly connected to one side of the positioning card plate; a sliding hole is opened on the L-shaped bracket, and a sliding rod is slidably connected to the sliding hole; a limit plate is fixedly provided at one end of the sliding rod close to the positioning card plate, and a limit block is fixedly provided at one end of the sliding rod away from the positioning card plate; a limit spring is sleeved on the sliding rod, and both ends of the limit spring are respectively fixedly connected to the limit plate and the L-shaped bracket; the wire connected to the cathode screen is located between the positioning card plate and the limit plate and is limited and fixed by the limit plate.

[0013] Furthermore, a rotating hole is provided through the upper side of one side of the box body, and a rotating groove is provided on the inner wall of the box body; one end of the support rod is located in the rotating groove and is rotatably connected to the rotating groove, and the other end of the support rod passes through the rotating hole and a knob is fixed on the end; the support rod and the rotating hole are connected by a rotating sealing ring.

[0014] Furthermore, the wire connected to the anode plate is connected to the positive electrode of the power supply, and the wire connected to the cathode mesh plate is connected to the negative electrode of the power supply.

[0015] Furthermore, the box body, support rods and positioning card plates are all made of polyethylene.

[0016] Furthermore, the material of the separator is multiple layers of dust-free paper.

[0017] Furthermore, the cathode mesh plate is a 200-mesh metal mesh plate structure.

[0018] Furthermore, the material of the anode plate is a crude copper plate, and the material of the cathode mesh plate is a titanium mesh or a stainless steel mesh.

[0019] A method for testing using the above device comprises the following steps:

[0020] S1. Clean the box, support rods, anode plate and cathode screen with deionized water and alcohol, and dry them in a drying oven;

[0021] S2, pouring electrolyte into the box, fitting the diaphragm and cathode mesh plate together, placing them on the support rod, so that the diaphragm is soaked and moistened by the electrolyte, and then fixing the wire connected to the cathode mesh plate by the wire fixing mechanism;

[0022] S3. Slowly turn the knobs of the two support rods in opposite directions to flatten the diaphragm;

[0023] S4. Connect the positioning card board to the test card slot of the XRD instrument, and then connect the wire to the constant current power supply to perform in-situ XRD data test of metal electrodeposition.

[0024] Compared with the prior art, the present invention has the following beneficial effects:

[0025] (1) The present invention adopts the structural design of the diaphragm and the cathode mesh plate. When the electrolyte in the box contacts the diaphragm but is not higher than the height of the diaphragm, the surface of the diaphragm remains flat after being soaked by the electrolyte. Since there is a small amount of electrolyte on the surface of the diaphragm but it is not enough to form an obvious liquid layer, the cathode mesh plate can fit well with it. The close contact between the two makes it difficult for the cathode to be displaced during the moving process of the device, and also ensures that the deposited surface of the cathode metal mesh is parallel to the sample table as a whole, which is convenient for XRD testing. At the same time, there will always be no obvious liquid layer on the top of the diaphragm. The diaphragm has good liquid absorption capacity, and it can ensure the smooth progress of electrodeposition even when there is no obvious liquid layer in contact with the cathode. The diaphragm realizes the smooth transmission of ions between the anode and the cathode through direct contact with the electrolyte, which can prevent the liquid layer from penetrating the top of the cathode mesh plate to interfere with the XRD test, and finally realizes that electrodeposition and XRD testing are carried out simultaneously and effective XRD diffraction data can be measured.

[0026] (2) The present invention can quickly fix the wires connected to the cathode mesh after the cathode mesh is placed through the wire fixing mechanism, insert the wires between the positioning card plate and the limit plate, and fix the wires by the rebound force of the limit spring, thereby preventing the wires from affecting the center of gravity of the cathode mesh, so that the cathode mesh can be completely parallel to the liquid surface. At the same time, the present invention keeps the surface of the cathode mesh flat by fully contacting the cathode mesh due to surface tension after being soaked, and completely flattens the diaphragm by rotating the knob of the support rod in the opposite direction, ultimately ensuring uniform deposition, which can ensure that the density per unit area is large enough to obtain XRD data, and can ensure that the electrolyte is fully distributed between the mesh holes to facilitate electrodeposition, thereby comprehensively reducing test errors.

[0027] (3) Compared with other commonly used in-situ XRD testing devices, the device of the present invention is simple to assemble, easy to operate, low in cost, can fully carry out ion transmission, and can easily realize the testing of in-situ XRD data of the electrodeposition process; the device does not require any changes to the accessories of the XRD instrument, and can be quickly positioned through the positioning card plate, so that the in-situ test and the ordinary test can be quickly switched. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] Figure 1 This is a schematic diagram of the overall structure of a device for testing in-situ XRD data in metal electrodeposition according to the present invention;

[0029] Figure 2 A schematic diagram of the cross-sectional structure of a device for testing in-situ XRD data in metal electrodeposition according to the present invention;

[0030] Figure 3 This is a schematic diagram of a wire fixing mechanism of a device for testing in-situ XRD data in metal electrodeposition according to the present invention;

[0031] Figure 4 A schematic diagram of the dispersed structure of a device for testing in-situ XRD data in metal electrodeposition according to the present invention;

[0032] Figure 5 This is the in-situ XRD pattern of copper electrodeposited on a titanium mesh obtained in Example 2 of the present invention;

[0033] Figure 6 This is the in-situ XRD pattern of copper electrodeposited on a stainless steel mesh obtained in Example 3 of the present invention.

[0034] The reference numerals are as follows:

[0035] Box body-1; wire hole-11; rotation hole-12; rotation groove-13; support rod-2; rotating seal ring-21; knob-22; diaphragm-3; positioning card plate-4; cathode mesh plate-5; wire-6; anode plate-7; wire fixing mechanism-8; L-shaped bracket-81; slide bar-82; limit block-83; limit spring-84; limit plate-85. DETAILED DESCRIPTION

[0036] In order to make the purpose, technical solution and advantages of the present invention clearer, the present invention is further described in detail below in conjunction with the embodiments. Of course, the specific embodiments described here are only used to explain the present invention and are not used to limit the present invention.

[0037] Although the steps in the present invention are arranged with numbers, they are not used to limit the order of the steps. Unless the order of the steps is clearly stated or the execution of a certain step requires other steps as a basis, the relative order of the steps can be adjusted. It is understood that the term "and / or" used in this article involves and covers any and all possible combinations of one or more of the associated listed items.

[0038] Example 1

[0039] like Figure 1 to Figure 6 As shown, a device for testing in-situ XRD data in metal electrodeposition comprises a box 1, the bottom of the box 1 is closed and an anode plate 7 is placed at the bottom of the box 1, and the top of the box 1 is open; a pair of support rods 2 are horizontally installed inside the box 1, a diaphragm 3 is placed above the support rods 2, a cathode mesh plate 5 is placed above the diaphragm 3, and the electrolyte in the box 1 is in contact with the diaphragm 3 but not higher than the height of the diaphragm 3;

[0040] The anode plate 7 is fixedly connected with a wire 6, and a wire hole 11 is opened at the bottom of the side wall of the box body 1. The wire 6 passes through the wire hole 11 and is sealed and fixedly connected to the wire hole 11; the cathode grid plate 5 is also fixedly connected with the wire 6; the outer side wall of the box body 1 is horizontally installed with a positioning card plate 4, and the positioning card plate 4 is clamped in the test card slot of the XRD instrument.

[0041] The present invention adopts the structural design of the diaphragm 3 and the cathode mesh plate 5. When the electrolyte in the box 1 contacts the diaphragm 3 but is not higher than the height of the diaphragm 3, the surface of the diaphragm 3 is still flat after being soaked by the electrolyte. Since there is a small amount of electrolyte on the surface of the diaphragm 3 but it is not enough to form an obvious liquid layer, the cathode mesh plate 5 can be well fitted therewith. The close contact between the two makes it difficult for the cathode to be displaced during the process of moving the device, and also ensures that the deposited surface of the cathode metal mesh is parallel to the sample table as a whole, which is convenient for XRD testing. At the same time, there will always be no obvious liquid layer on the top of the diaphragm 3. The diaphragm 3 has good liquid absorption capacity, and it can ensure the smooth progress of electrodeposition even when there is no obvious liquid layer in contact with the cathode. The diaphragm 3 realizes the smooth transmission of ions between the anode and the cathode through direct contact with the electrolyte, and can prevent the liquid layer from penetrating the top of the cathode mesh plate 5 to interfere with the XRD test, and finally realizes that the electrodeposition and XRD test are carried out simultaneously, and effective XRD diffraction data can be measured.

[0042] It is worth noting that the box body 1, the support rod 2 and the positioning card plate 4 of the present invention are all made of insulating materials.

[0043] Furthermore, the positioning card plate 4 is provided with an opening, and the outer side wall of the box body 1 is correspondingly provided with a card slot, and the positioning card plate 4 is installed by being inserted into the card slot of the outer side wall of the box body 1 through the opening.

[0044] It is worth noting that the present invention does not further limit the specific size of the positioning card plate 4, and can be conventionally adjusted according to different XRD instruments.

[0045] Furthermore, one side of the positioning card plate 4 is fixedly connected with a wire fixing mechanism 8, and the wire fixing mechanism 8 includes an L-shaped bracket 81, and one end of the L-shaped bracket 81 is fixedly connected to one side of the positioning card plate 4; a sliding hole is opened on the L-shaped bracket 81, and a sliding rod 82 is slidably connected to the sliding hole; the sliding rod 82 is fixedly provided with a limit plate 85 at one end close to the positioning card plate 4, and the sliding rod 82 is fixedly provided with a limit block 83 at one end away from the positioning card plate 4; a limit spring 84 is sleeved on the sliding rod 82, and the two ends of the limit spring 84 are respectively fixedly connected to the limit plate 85 and the L-shaped bracket 81; the wire 6 connected to the cathode screen plate 5 is located between the positioning card plate 4 and the limit plate 85 and is limited and fixed by the limit plate 85.

[0046] Through the resilience of the limit spring 84, the limit plate 85 presses the wire 6 to achieve temporary fixation of the wire 6, preventing the movement of the wire 6 from affecting the center of gravity and balance of the cathode screen 5, and facilitating the rapid disassembly and adjustment of the wire 6 by pulling the limit block 83.

[0047] Furthermore, a rotating hole 12 is formed through the upper side of one side of the box body 1, and a rotating groove 13 is formed on the inner wall of the box body 1; one end of the support rod 2 is located in the rotating groove 13 and is rotatably connected to the rotating groove 13, and the other end of the support rod 2 passes through the rotating hole 12 and a knob 22 is fixed on the end; the support rod 2 and the rotating hole 12 are connected by a rotating sealing ring 21.

[0048] The present invention can quickly fix the wire 6 connected to the cathode mesh plate 5 after the cathode mesh plate 5 is placed through the wire fixing mechanism 8, insert the wire 6 between the positioning card plate 4 and the limit plate 85, and limit and fix the wire 6 through the rebound force of the limit spring 84, so as to prevent the wire 6 from affecting the center of gravity of the cathode mesh plate 5, so that the cathode mesh plate 5 can be completely parallel to the liquid surface. At the same time, the present invention makes the surface of the cathode mesh plate 5 remain straight by fully contacting the cathode mesh plate 5 with the surface tension of the soaked diaphragm 3, and completely flattens the diaphragm 3 by rotating the knob 22 of the support rod 2 in the opposite direction, finally ensuring uniform deposition, which can ensure that the unit area density is large enough to obtain XRD data, and ensure that the electrolyte is fully distributed between the mesh holes to facilitate electrodeposition, thereby comprehensively reducing the test error.

[0049] Furthermore, the wire 6 connected to the anode plate 7 is connected to the positive electrode of the power supply, and the wire 6 connected to the cathode grid plate 5 is connected to the negative electrode of the power supply.

[0050] Furthermore, the box body 1, the support rod 2, and the positioning card plate 4 are all made of polyethylene. Polyethylene has good insulation properties, and its high toughness can also ensure load-bearing.

[0051] Furthermore, the material of the diaphragm 3 is a plurality of layers of dust-free paper, which has a strong liquid absorption capacity.

[0052] Furthermore, the cathode mesh plate 5 is a 200-mesh metal mesh plate structure.

[0053] Furthermore, the anode plate 7 is made of a crude copper plate, and the cathode mesh plate 5 is made of a titanium mesh or a stainless steel mesh.

[0054] A method for testing using the above device comprises the following steps:

[0055] S1. Clean the box 1, support rod 2, anode plate 7 and cathode screen 5 with deionized water and alcohol, and place them in a drying oven for drying;

[0056] S2, pour the electrolyte into the box 1, fit the diaphragm 3 and the cathode mesh plate 5 together, place them on the support rod 2, make the diaphragm 3 soaked and wetted by the electrolyte, and then fix the wire connected to the cathode mesh plate 5 by the wire fixing mechanism 8;

[0057] S3, slowly rotate the knobs 22 of the two support rods 2 in opposite directions to flatten the diaphragm 3;

[0058] S4, clamp the positioning card plate 4 into the test card slot of the XRD instrument, then connect the wire to the constant current power supply to perform in-situ XRD data test of metal electrodeposition.

[0059] Compared with other commonly used in-situ XRD testing devices, the device of the present invention is simple to assemble, easy to operate, low in cost, can fully carry out ion transmission, and can easily realize the testing of in-situ XRD data of the electrodeposition process; the device does not require any changes to the accessories of the XRD instrument, and can be quickly positioned through the positioning card plate 4, so as to realize the rapid switching and connection between the in-situ test and the ordinary test.

[0060] Example 2

[0061] An in-situ XRD testing method for electrodepositing copper on a titanium mesh comprises the following steps:

[0062] S1, clean the box 1, the support rod 2, the anode plate 7 made of a rough copper plate, and the cathode screen plate 5 made of a 200-mesh titanium screen with deionized water and alcohol, and place them in a drying oven for drying;

[0063] S2, pour the electrolyte into the box 1, fit the diaphragm 3 and the cathode mesh plate 5 together, place them on the support rod 2, make the diaphragm 3 soaked and wetted by the electrolyte, and then fix the wire connected to the cathode mesh plate 5 by the wire fixing mechanism 8;

[0064] S3, slowly rotate the knobs 22 of the two support rods 2 in opposite directions to flatten the diaphragm 3;

[0065] S4, clamp the positioning card plate 4 into the test card slot of the XRD instrument, then connect the wire to the constant current power supply to perform in-situ XRD data test of metal electrodeposition.

[0066] According to the actual working area of ​​the two electrodes, the working current is converted to 20mAcm -2 The XRD instrument scanning mode was set to timed stepping, sampling step width 0.05, timing 1.5s, measurement angle range 40°-80°, and in-situ XRD test was performed. The test results are shown in Figure 5 As shown in the figure, before the test started, the XRD instrument only detected the characteristic peak of titanium. 40 minutes after the start of electrodeposition, copper gradually deposited on the titanium mesh, and then the diffraction peak intensity of copper gradually increased, indicating that the electrodeposition continued and the amount of copper deposited gradually increased.

[0067] Example 3

[0068] An in-situ XRD testing method for electrodepositing copper on a stainless steel mesh comprises the following steps:

[0069] S1, clean the box 1, the support rod 2, the anode plate 7 made of a rough copper plate, and the cathode screen plate 5 made of a 200-mesh stainless steel screen with deionized water and alcohol, and place them in a drying oven for drying;

[0070] S2, pour the electrolyte into the box 1, fit the diaphragm 3 and the cathode mesh plate 5 together, place them on the support rod 2, make the diaphragm 3 soaked and wetted by the electrolyte, and then fix the wire connected to the cathode mesh plate 5 by the wire fixing mechanism 8;

[0071] S3, slowly rotate the knobs 22 of the two support rods 2 in opposite directions to flatten the diaphragm 3;

[0072] S4, clamp the positioning card plate 4 into the test card slot of the XRD instrument, then connect the wire to the constant current power supply to perform in-situ XRD data test of metal electrodeposition.

[0073] According to the actual working area of ​​the two electrodes, the working current is converted to 20mAcm -2 The XRD instrument scanning mode was set to timed stepping, sampling step width 0.05, timing 1.5s, measurement angle range 40°-80°, and in-situ XRD test was performed. The test results are shown in Figure 6 As shown in the figure, before the test, the XRD instrument only detected the characteristic peak of stainless steel. 40 minutes after the start of electrodeposition, copper gradually deposited on the stainless steel mesh, and then the diffraction peak intensity of copper gradually increased, the characteristic peak of stainless steel disappeared, the process of copper electrodeposition continued, and the amount of copper deposition gradually increased.

[0074] The above is only a preferred embodiment of the present invention. It should be pointed out that a person skilled in the art can make several improvements and changes without departing from the creative concept of the present invention, which all belong to the protection scope of the present invention.

Claims

1. A device for testing in-situ XRD data in metal electrodeposition, characterized in that: The invention comprises a box (1), the bottom of the box (1) is closed and an anode plate (7) is placed at the bottom of the box (1), and the top of the box (1) is open; a pair of support rods (2) are horizontally installed inside the box (1), a diaphragm (3) is placed above the support rods (2), a cathode mesh plate (5) is placed above the diaphragm (3), and the electrolyte in the box (1) is in contact with the diaphragm (3) but is not higher than the height of the diaphragm (3); The anode plate (7) is fixedly connected to a wire (6); a wire hole (11) is provided below the side wall of the box (1); the wire (6) passes through the wire hole (11) and is sealed and fixedly connected to the wire hole (11); the cathode mesh plate (5) is also fixedly connected to a wire (6); and a positioning card plate (4) is horizontally installed on the outer side wall of the box (1); the positioning card plate (4) is clamped in a test card slot of an XRD instrument.

2. The device for testing in-situ XRD data in metal electrodeposition according to claim 1, characterized in that: The positioning card plate (4) is provided with an opening, and the outer wall of the box body (1) is correspondingly provided with a card slot, and the positioning card plate (4) is installed by being inserted into the card slot of the outer wall of the box body (1) through the opening.

3. The device for testing in-situ XRD data in metal electrodeposition according to claim 1, characterized in that: A wire fixing mechanism (8) is fixedly connected to one side of the positioning card plate (4), and the wire fixing mechanism (8) comprises an L-shaped bracket (81), one end of which is fixedly connected to one side of the positioning card plate (4); a sliding hole is provided on the L-shaped bracket (81), and a sliding rod (82) is slidably connected to the sliding hole; a limiting plate (85) is fixedly provided at one end of the sliding rod (82) close to the positioning card plate (4), and a limiting block (83) is fixedly provided at one end of the sliding rod (82) away from the positioning card plate (4); a limiting spring (84) is sleeved on the sliding rod (82), and two ends of the limiting spring (84) are respectively fixedly connected to the limiting plate (85) and the L-shaped bracket (81); the wire (6) connected to the cathode screen plate (5) is located between the positioning card plate (4) and the limiting plate (85) and is limited and fixed by the limiting plate (85).

4. The device for testing in-situ XRD data in metal electrodeposition according to claim 1, characterized in that: A rotating hole (12) is provided through the upper side of one side of the box body (1), and a rotating groove (13) is provided on the inner wall of the box body (1); one end of the support rod (2) is located in the rotating groove (13) and is rotatably connected to the rotating groove (13), and the other end of the support rod (2) passes through the rotating hole (12) and is fixedly provided with a knob (22); the support rod (2) and the rotating hole (12) are connected via a rotating sealing ring (21).

5. The device for testing in-situ XRD data in metal electrodeposition according to claim 1, characterized in that: The lead (6) connected to the anode plate (7) is connected to the positive electrode of the power supply, and the lead (6) connected to the cathode mesh plate (5) is connected to the negative electrode of the power supply.

6. The device for testing in-situ XRD data in metal electrodeposition according to claim 1, characterized in that: The box body (1), the support rod (2) and the positioning card plate (4) are all made of polyethylene.

7. The device for testing in-situ XRD data in metal electrodeposition according to claim 1, characterized in that: The material of the diaphragm (3) is multiple layers of dust-free paper.

8. The device for testing in-situ XRD data in metal electrodeposition according to claim 1, characterized in that: The cathode mesh plate (5) is a 200-mesh metal mesh plate structure.

9. The device for testing in-situ XRD data in metal electrodeposition according to claim 1, characterized in that: The material of the anode plate (7) is a crude copper plate, and the material of the cathode mesh plate (5) is a titanium mesh or a stainless steel mesh.

10. A method for testing using the device according to any one of claims 1 to 9, characterized in that: The steps include: S1. Clean the box (1), support rod (2), anode plate (7) and cathode screen (5) thoroughly with deionized water and alcohol, and place them in a drying oven for drying; S2, pouring electrolyte into the box (1), fitting the diaphragm (3) and the cathode screen (5), placing them on the support rod (2), so that the diaphragm (3) is soaked and moistened by the electrolyte, and then fixing the wire connected to the cathode screen (5) by the wire fixing mechanism (8); S3, slowly turning the knobs (22) of the two support rods (2) in opposite directions to flatten the diaphragm (3); S4, clamping the positioning card plate (4) into the test card slot of the XRD instrument, and then connecting the wire to a constant current power supply to perform an in-situ XRD data test of metal electrodeposition.

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