A high-throughput electrochemical synthesis and testing integrated machine and its usage method

By designing a high-throughput electrochemical synthesis and testing machine, the problems of low plating tank efficiency and single sample preparation in the existing electroplating technology are solved, and the synthesis of multiple samples is achieved, adjustable electrode distance and convenient material replacement are achieved, which significantly improves the electroplating efficiency and diversity of experimental results.

CN111733441BActive Publication Date: 2025-06-10JIANGSU YUNTIAN HYDROGEN ENERGY TECHNOLOGY CO LTD
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Patent Information

Application Number
CN202010455333.9
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2020-05-26
Publication Date
2025-06-10
Estimated Expiration
2040-05-26

AI Technical Summary

Technical Problem

The existing electroplating technology has the ability to make one sample at a time, which consumes a lot of manpower and time, has low working efficiency, and cannot adjust the distance between the cathode and anode, resulting in a single experimental result, cumbersome material replacement, and low electroplating efficiency.

Method used

A high-throughput electrochemical synthesis and testing integrated machine is designed, including array liquid tanks, electric pumps, solenoid valves, magnetic stirrers and 3D mounting frames, which can realize multi-sample synthesis, adjustable electrode distances, easy material replacement, and improve electroplating efficiency.

Benefits of technology

It is possible to make multiple samples at one time, which improves working efficiency and can freely adjust the distance of the cathode and anode, enhances the diversity and accuracy of the experimental results, simplifies the material change process, and significantly improves the electroplating efficiency.

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Abstract

The present invention discloses a high-throughput electrochemical synthesis and testing integrated machine and its usage method. The integrated machine includes an array liquid tank, an electric pump, a solenoid valve, a feed barrel, a discharge barrel, a magnetic stirrer, a 3D mounting rack, an anode fixture, and a cathode fixture. The array liquid tank communicates with the feed barrel and the discharge barrel through a feed pipe and a discharge pipe respectively. The electric pump is installed on the feed pipe, and the solenoid valve is installed on the discharge pipe. The magnetic stirrer is arranged at the bottom of the array liquid tank. The array liquid tank and the magnetic stirrer are arranged on the 3D mounting rack. The anode fixture and the cathode fixture hold the anode and the cathode well, are slidably installed on the 3D mounting rack and suspended above the array liquid tank. The integrated machine includes usage methods for high-throughput electroplating and two-electrode electroplating. The electroplating tank of the integrated machine is an array electroplating tank, which can electroplate multiple samples at one time, has multiple usage methods, unifies the synthesis and testing processes, is convenient to operate, is a local high-throughput screening system, speeds up the screening process, and improves the screening quality.
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Description

Technical Field

[0001] The present invention relates to an integrated machine for electrochemical synthesis and testing, and more specifically, to a high-throughput integrated machine for electrochemical synthesis and testing and a method for using the same. Background Art

[0002] Electroplating is a process in which oxidation and reduction reactions occur on two electrodes, namely the anode and the cathode, under the action of an external power source. It is the basis of metal electrolytic smelting and electroplating processes and has become a very important modern processing technology in traditional aspects such as decoration, wear resistance, friction reduction, corrosion prevention and surface modification, development of new materials for electroplating layers with electrical properties and optical properties. The selection of the plating bath is particularly important in electroplating. Currently, the commonly used plating bath can only produce one sample at a time, consuming a large amount of manpower and time, with low work efficiency; and the distance between the anode and the cathode cannot be adjusted, resulting in a single experimental result; moreover, the material replacement is cumbersome and the electroplating efficiency is low. Summary of the Invention

[0003] Object of the Invention: The object of the present invention is to provide a high-throughput integrated machine for electrochemical synthesis and testing that can achieve multi-sample synthesis, adjustable electrode distance, convenient material replacement and high electroplating efficiency. Another object of the present invention is to provide a method for using the integrated machine.

[0004] Technical Solution: The high-throughput integrated machine for electrochemical synthesis and testing according to the present invention includes an array liquid tank, an electric pump, a solenoid valve, a feed barrel, a discharge barrel, a magnetic stirrer, a 3D mounting rack, an anode clamp and a cathode clamp. The array liquid tank communicates with the feed barrel and the discharge barrel through a feed pipe and a discharge pipe respectively; the electric pump and the solenoid valve are installed on the feed pipe and the discharge pipe to control the inflow and outflow of the plating solution; the magnetic stirrer is arranged at the bottom of the array liquid tank, and the array liquid tank and the magnetic stirrer are arranged on the 3D mounting rack. The anode clamp and the cathode clamp hold the anode and the cathode, are slidably installed on the 3D mounting rack and are suspended above the array liquid tank. A liquid level gauge connected to the electric pump is arranged in the array liquid tank.

[0005] Among them, the array liquid tank is composed of n×m unit tanks, where n, m≥5. The unit tank is connected with a feed capillary and a discharge capillary. A liquid level gauge and an electric pump are installed on the feed capillary and the discharge capillary in each unit tank. The feed and discharge are controlled by switching on and off the electric pump. The discharge capillary is connected to the discharge pipe through a solenoid valve. The feed capillary is connected to a feed bucket containing plating solutions with different compositions through a feed pipe. The number of feed buckets is 1 to 10. The liquid level gauge is used to sense the position of the solution and is connected with the electric pump to cooperate in controlling the volume of the plating solution introduced. The magnetic stirrer is a heatable magnetic stirrer with a power of 400 - 1000W and a rotation speed range of 0 - 1500 RPM. The 3D mounting rack consists of a base, a bracket, a cathode fixture guide rail, an anode fixture guide rail, a motor, and a motor switch. The motor is fixed on the base, the bracket is vertically installed on the motor, the cathode fixture guide rail and the anode fixture guide rail are fixed between the two brackets, and the anode fixture and the cathode fixture are slidably installed on the anode fixture guide rail and the cathode fixture guide rail. The anode fixture and the cathode fixture are composed of stainless steel chucks welded to the wires. The all-in-one machine further includes a cover plate, and electrode jacks are opened on the cover plate. The electrode jacks include a cathode jack, symmetrically arranged drive electrode jacks, a first anode jack, and a second anode jack. The distances between the first anode jack, the second anode jack, and the cathode jack are 5 - 10mm and 10 - 15mm respectively. The anode is a copper sheet, copper foam, nickel foam, nickel plate, carbon fiber cloth, or stainless steel, and the cathode is Fe, Zn, Mn, Ni, Co, Cu, C, B, P, Ag, Au, Pd.

[0006] The usage method of the high-throughput electrochemical synthesis and testing all-in-one machine described in the present invention includes the following steps during high-throughput electroplating:

[0007] (S1) Place the magnetic stirrer on the 3D mounting rack, install the array liquid tank on the magnetic stirrer, sequentially install the feed pipe and the discharge pipe on the array liquid tank, and install the electric pump and the solenoid valve on the feed pipe and the discharge pipe.

[0008] (S2) Fix the cathode and the anode on the anode fixture and the cathode fixture, turn on the electric pump to introduce the plating solution into the array liquid tank, adjust the positions of the anode fixture and the cathode fixture, and immerse the cathode, the anode, and the carrier in the plating solution.

[0009] (S3) Perform potentiostatic single-pulse electroplating, select the single-pulse electroplating parameters, after completion, open the solenoid valve to discharge the solution from the discharge pipe, and obtain the electroplated product after drying.

[0010] (S4) Remove the electroplated product, use the electroplated product as the working electrode, form a three-electrode system with the reference electrode and the counter electrode, connect it to the electrochemical workstation, and perform electrochemical testing.

[0011] The usage method of the high-throughput electrochemical synthesis and testing all-in-one machine described in the present invention includes the following steps during two-electrode electroplating:

[0012] (S1) Place the magnetic stirrer on the 3D mounting bracket, install the array liquid tank on the magnetic stirrer, and sequentially install the feed pipe and the discharge pipe on the array liquid tank. Install the electric pump and the solenoid valve on the feed pipe and the discharge pipe;

[0013] (S2) Fix the double-electrode cathode and the two driving electrodes in the cathode jack and the driving electrode jack on the cover plate, fix the driving electrode with the cathode clamp, fix the double-electrode anode at the first anode jack or the second anode jack, and connect the double-electrode cathode and the double-electrode anode together with wires;

[0014] (S3) Use the electric pump to introduce the plating solution into the array liquid tank, judge the volume of the introduced plating solution according to the liquid level gauge, and turn off the electric pump; Immerse the double-electrode cathode and the bipolar electrode anode in the plating solution;

[0015] (S4) Use a DC regulated power supply to provide a driving potential, select the driving voltage and the deposition time for electroplating. After completion, open the solenoid valve to discharge the solution from the discharge pipe. After drying, the electroplated product is obtained;

[0016] (S5) Remove the electroplated product, use the electroplated product as the working electrode, form a three-electrode system with the reference electrode and the counter electrode, connect it to the electrochemical workstation, and perform electrochemical tests.

[0017] Advantageous effects: Compared with the prior art, the present invention has the following remarkable advantages: 1. The electroplating tank is an array electroplating tank, which can freely select the electroplating method, electroplate multiple samples at one time, and realizes the integration of electroplating and testing; 2. The high-throughput screening system greatly reduces the consumption of reaction raw materials, significantly speeds up the screening process, and improves the screening quality; 3. It can automatically control the feeding and discharging, judge the position of the solution through the liquid level gauge and calculate the flow rate and time of the electric pump, and realize intelligent feeding and discharging; 4. It can freely adjust the distance between the anode and the cathode, exchange the anode and cathode of different materials, and is convenient and flexible to use. Description of the Drawings

[0018] Figure 1 is a schematic structural diagram of the present invention;

[0019] Figure 2 is a top view of the present invention;

[0020] Figure 3 is a front view of the present invention;

[0021] Figure 4 is a schematic connection diagram of some components of the array electroplating tank;

[0022] Figure 5 is a top view of the array electroplating tank;

[0023] Figure 6 is a schematic structural diagram of the array electroplating tank;

[0024] Figure 7 is a sectional view of a unit cell;

[0025] Figure 8 is a schematic structural diagram of an anode fixture and a cathode fixture;

[0026] Figure 9 is a schematic structural diagram of a cover plate;

[0027] Figure 10 is a schematic diagram of the use of a dual - electrode electroplating for preparing a catalyst electrode;

[0028] Figure 11 is a schematic diagram of the use of an electrode during testing;

[0029] Figure 12 is an LSV graph at different nickel chloride concentrations in Example 1;

[0030] Figure 13 is a comparative curve graph of the over - potential of the catalyst at different nickel chloride concentrations in Example 1. Detailed implementation manners

[0031] Example 1

[0032] As Figures 1 to 4 shown, the 3D automatic control high - throughput electrochemical synthesis and testing integrated machine includes an array liquid tank 1, an electric pump 4, a solenoid valve 9, a feed bucket 7, a discharge bucket 8, a magnetic stirrer 10, a 3D mounting rack, an anode fixture 17, and a cathode fixture 18. As Figures 5 to 7As shown, the array liquid tank 1 has a length of 215 mm, a width of 215 mm, and a depth of 40 mm. It consists of 5×5 unit cells. There are two circular channels 2 on each side of each unit cell that communicate with the inside of the tank. The unit cells are connected to the feed capillary and the discharge capillary through the circular channels 2. Electric pumps 4 are installed on the feed capillary and the discharge capillary in each unit cell. The discharge capillary is connected to the discharge pipe 6 through a solenoid valve 9, and the discharge pipe 6 communicates with the discharge bucket 8. The feed pipes 5 in the 5 unit cells are connected to their respective feed buckets 7 through solenoid valves 9. The electric pump 4 is made of corrosion-resistant plastic material and a ceramic shaft core, with dimensions of 42 mm×26 mm×39 mm, a working voltage of DC 10 - 15 V, a rated current of 0.2 - 0.5 A, and a maximum lift of 0.8 - 1.5 m. The solenoid valve 9 is installed on the discharge pipe. The magnetic stirrer 10 is arranged at the bottom of the array liquid tank 1. The magnetic stirrer 10 is a heatable magnetic stirrer with a power of 400 - 1000 W and a rotation speed range of 0 - 1500 RPM. The array liquid tank 1 and the magnetic stirrer 10 are arranged on a 3D mounting frame. The anode fixture 17 and the cathode fixture 18 hold the anode and the cathode well. The 3D mounting frame consists of a base 11, a bracket 12, a cathode fixture guide rail 13, an anode fixture guide rail 14, a motor 15, and a motor switch 16; the motor 15 is fixed on the base 11, the bracket 12 is perpendicularly installed on the motor 15, the cathode fixture guide rail 13 and the anode fixture guide rail 14 are fixed between the two brackets 12, and the anode fixture 17 and the cathode fixture 18 are slidably installed on the anode fixture guide rail 14 and the cathode fixture guide rail 13, as Figure 8 shown, the anode fixture 17 and the cathode fixture 18 are composed of stainless steel chucks 20 welded to the wire 21, as Figure 9 shown, during double - electrode electroplating, it also includes a cover plate 22. The cover plate 22 is provided with electrode jacks. The electrode jacks include a cathode jack 30, symmetrically arranged drive electrode jacks 29, a first anode jack 31, and a second anode jack 32. The distances between the first anode jack 31, the second anode jack 32 and the cathode jack 30 are 8 mm and 13 mm respectively.

[0033] High - throughput electroplating is based on potentiostatic electroplating. Before electroplating, a suitable deposition potential should be found first. First, the carrier carbon fiber cloth is pretreated to remove surface oil stains. Five carbon fiber cloths are put into an ethanol solution and ultrasonically vibrated for 5 min, then ultrasonically vibrated in a 0.01 mol / L dilute hydrochloric acid solution for 2 min, and finally ultrasonically vibrated in deionized water for 10 min, and then dried and weighed for standby.

[0034] Put ferric chloride solution, sodium hypophosphite solution, boric acid, trisodium citrate, and nickel chloride solution into 5 feed barrels 7 respectively. The concentration of the ferric chloride solution is 0.05 mol / L, the concentration of the sodium hypophosphite solution is 0.15 mol / L, the concentration of boric acid is 0.4 mol / L, the concentration of trisodium citrate is 37.5 g / L, and the concentration of the nickel chloride solution is 1 mol / L. Open the electric pump 4 to add the ferric chloride solution, sodium hypophosphite solution, boric acid, and trisodium citrate into 5 unit cells. The electric pump 4 controls the nickel chloride solution concentrations in the 5 unit cells to be 0.05, 0.08, 0.1, 0.12, and 0.15 mol / L respectively by controlling the flow rate and opening time. Then use the liquid level gauge 19 to judge the volume of the plating solution introduced. Close the electric pump 4. When the plating solution is insufficient, the electric pump 4 continues to add the plating solution.

[0035] Select graphite plates as the cathode and anode. Fix the cathode graphite plate on the cathode fixture 17. Turn on the motor switch 16, control the motor 15 to adjust the distance between the cathode and the anode, and adjust the position in the unit cell so that the carbon fiber cloth is immersed in the solution. Perform potentiostatic single-pulse electroplating for 18 min at a voltage of 6 V. Control the temperature of the magnetic stirrer 10 at 50 °C. After completion, open the solenoid valve 9 to drain the solution through the total discharge pipe 6. Rinse it several times with deionized water by ultrasonic oscillation. After drying, 5 carbon fiber cloth-supported NiFeP alloy electrocatalytic hydrolysis hydrogen production catalysts with different nickel contents are obtained.

[0036] As Figure 11 shown, use the saturated calomel electrode as the reference electrode 24, graphite as the counter electrode 25, and the carbon fiber cloth-supported NiFeP alloy electrocatalytic hydrolysis hydrogen production catalyst as the working electrode 23. Fix the three electrodes with the cathode fixture and the anode fixture. Introduce a 1 mol / L KOH solution into the unit cell, introduce N 2 , connect it to the electrochemical workstation, and conduct electrochemical tests. The results are as Figures 12 to 13 shown, Figure 12 is the LSV diagram under different nickel chloride concentrations, Figure 13 is the comparative curve diagram of the overpotential of the catalyst under different nickel chloride concentrations.

[0037] Example 2

[0038] The differences between this embodiment and Embodiment 1 are as follows: After pretreating 10 carbon fiber cloths and putting them into the unit cell, a copper sheet is selected as the anode and a graphite plate is selected as the cathode. The motor switch 16 is turned on, and the motor 15 is controlled to adjust the distance between the anode and the cathode. The plating solution includes nickel chloride solution, sodium hypophosphite solution, boric acid, trisodium citrate, and iron chloride solution, which are respectively filled in 5 feed barrels 7. Among them, the concentration of nickel chloride solution is 0.08 mol / L, the concentration of sodium hypophosphite solution is 0.2 mol / L, the concentration of boric acid is 0.3 mol / L, the concentration of trisodium citrate is 25 g / L, and the concentration of iron chloride solution is 0.1 mol / L. The electric pump 4 controls the concentration of iron chloride solution in 10 unit cells to be 0.03, 0.04, 0.05, 0.06, 0.07, 0.08, 0.09, 0.1, 0.11, 0.12 mol / L respectively by controlling the flow rate and opening time. The volume of the plating solution introduced is judged according to the liquid level gauge 19, and then the electric pump is turned off; constant potential single pulse electroplating is carried out for 15 min at a voltage of 5 V, and the temperature is controlled at 60 °C. After completion, the solenoid valve 9 is opened to discharge the solution through the total discharge pipe 6, and it is repeatedly ultrasonically oscillated and rinsed several times with deionized water. After drying, 10 carbon fiber cloths loaded with NiFeP alloy electrocatalytic hydrolysis hydrogen production catalysts with different iron contents are obtained.

[0039] Embodiment 3

[0040] The differences between this embodiment and Embodiment 1 are as follows: After pretreating 25 carbon fiber cloths and putting them into the unit cell, a copper sheet is selected as the cathode and a platinum sheet is selected as the anode, and the distance between the cathode and the anode is adjusted. The plating solution includes nickel chloride solution, iron chloride solution, boric acid, and trisodium citrate. Among them, the concentration of nickel chloride solution is 0.08 mol / L, the concentration of iron chloride solution is 0.2 mol / L, the concentration of boric acid is 0.3 mol / L, the concentration of trisodium citrate is 25 g / L, and the concentration of sodium hypophosphite solution is 1 mol / L. The electric pump 4 controls the concentration of sodium hypophosphite solution in 25 unit cells to be 0.06, 0.07, 0.08, 0.09, 0.1, 0.11, 0.12, 0.13, 0.14, 0.15, 0.16, 0.17, 0.18, 0.19, 0.2, 0.21, 0.22, 0.23, 0.24, 0.25, 0.26, 0.27, 0.28, 0.29, 0.3 mol / L respectively by controlling the flow rate and opening time. The volume of the plating solution introduced is judged according to the liquid level gauge 19, and then the electric pump 4 is turned off; constant potential single pulse electroplating is carried out for 21 min at a voltage of 4 V, and the temperature is controlled at 45 °C. After completion, the solution is discharged by using the solenoid valve 9, and it is repeatedly ultrasonically oscillated and rinsed several times with deionized water. After drying, 25 carbon fiber cloths loaded with NiFeP alloy electrocatalytic hydrolysis hydrogen production catalysts with different phosphorus contents are obtained.

[0041] Embodiment 4

[0042] The differences between this embodiment and Embodiment 1 are as follows: For double-electrode electroplating, ten copper sheets with a length, width, and thickness of 50×3×0.5 mm are selected as a group, and there are two groups in total, which serve as the double-electrode cathode 27. They are degreased and defatted by soaking in acetone, and then soaked in chromic acid for 1 minute to remove surface oxides. Numbers 1 to 10 are marked on the copper sheets. Then, the ten double-electrode cathodes 27 are ensured that their ends are on the same plane, and each copper sheet is wrapped with transparent tape to achieve an insulating effect. Then, the ten copper sheets are wrapped with transparent tape multiple times to fix them into an integral cathode composed of ten double-electrode cathodes 27. The driving electrode 28 is a graphite sheet with a length, width, and thickness of 40×3×2 mm, and the double-electrode anode 26 is a graphite sheet with a length, width, and thickness of 35×3×2 mm; The plating solution includes a nickel chloride solution with a concentration of 0.1 mol / L, a ferric chloride solution with a concentration of 0.05 mol / L, a sodium hypophosphite solution with a concentration of 0.15 mol / L, boric acid with a concentration of 0.4 mol / L, and trisodium citrate with a concentration of 37.5 g / L. They are respectively filled in five feed barrels 7. The feed pipe 5 is led into the five feed barrels 7, and the electro-pump 4 is turned on to introduce the plating solution into the unit cell. The volume of the plating solution introduced is judged according to the liquid level gauge 19, and then the electro-pump is turned off; The cover plate 22 as shown in Figure 9 is covered, and the driving electrode 28, the double-electrode cathode 27, and the double-electrode anode 26 are respectively inserted; As shown in Figure 10 , the double-electrode cathode 27, the driving electrode 28, and the double-electrode anode 26 are respectively fixed in the cathode jack 30, the driving electrode jack 29, and the first anode jack 31. There are ten double-electrode cathodes 27 with a thickness of 0.5 mm, and the distances from the double-electrode anode 26 are 8, 8.5, 9, 9.5, 10, 10.5, 11, 11.5, 12, and 12.5 mm. The motor switch 16 is turned on, and the motor 15 is controlled to select an appropriate height of the cathode fixture 18. The driving electrode 28 is fixed on the cathode fixture 18. The double-electrode cathode 27 and the double-electrode anode 26 are connected with wires, and the driving electrode 28 is connected to the DC regulated power supply. The driving potential is set to 6 V, and the electroplating time is 5 minutes. After the electroplating is completed, the plating solution is discharged by using the solenoid valve 9, and the product is rinsed with deionized water, thus obtaining ten NiFeP catalysts with different double-electrode distances.

[0043] Embodiment 5

[0044] The differences between this embodiment and Embodiment 4 are as follows: The double-electrode anode 26 is fixed on the second anode jack 32, and the distances formed by the ten double-electrode cathodes 27 and the double-electrode anode 26 are 13, 13.5, 14, 14.5, 15, 15.5, 16, 16.5, 17, and 17.5 mm. After the test is completed, ten NiFeP catalysts with different double-electrode distances are obtained.

[0045] Embodiment 6

[0046] The differences between this embodiment and Embodiment 4 are as follows: The five feed barrels 7 are respectively filled with ferric chloride solution with a concentration of 0.05 mol / L, sodium hypophosphite solution with a concentration of 0.15 mol / L, boric acid with a concentration of 0.4 mol / L, trisodium citrate with a concentration of 37.5 g / L, and nickel chloride solution with a concentration of 1 mol / L. The volume of the plating solution introduced is judged according to the liquid level gauge 19. The electric pump 4 controls the concentrations of the nickel chloride solutions in the five unit cells to be 0.05, 0.08, 0.1, 0.12, and 0.15 mol / L respectively by controlling the flow rate and the opening time. The volume of the plating solution introduced is judged according to the liquid level gauge 19, and the electric pump 4 is turned off; The distances between the samples numbered 1 to 10 and the double-electrode anode are different, and multiple samplings are convenient for analyzing the hydrogen evolution performance. Connect the double-electrode cathode 27 and the double-electrode anode 26 with wires, connect the driving electrode 28 to the DC regulated power supply, set the driving potential to 8 V, and the electroplating time to 6 min. After the electroplating is completed, the plating solution is discharged by using the solenoid valve 9, and the product is rinsed with deionized water to obtain 50 NiFeP catalysts with different double-electrode distances and different nickel chloride concentrations as shown in Table 1.

[0047] Table 1 Experimental samples in Embodiment 6

[0048]

Claims

1. A method for high-throughput electroplating using a high-throughput electrochemical synthesis and testing integrated machine, characterized in that, the integrated machine includes an array liquid tank, an electric pump, a solenoid valve, a feed bucket, a discharge bucket, a magnetic stirrer, a 3D mounting rack, an anode clamp, and a cathode clamp. The array liquid tank is communicated with the feed bucket and the discharge bucket through a feed pipe and a discharge pipe respectively; the electric pump and the solenoid valve are installed on the feed pipe and the discharge pipe; the magnetic stirrer is arranged at the bottom of the array liquid tank, and the array liquid tank and the magnetic stirrer are arranged on the 3D mounting rack. The anode clamp and the cathode clamp hold the anode and the cathode well, are slidably installed on the 3D mounting rack and suspended above the array liquid tank, and a liquid level gauge connected to the electric pump is arranged in the array liquid tank; the array liquid tank is composed of 5×5 unit cells; ferric chloride solution, sodium hypophosphite solution, boric acid, trisodium citrate, and nickel chloride solution are respectively placed in 5 feed buckets; the method includes the following steps: (S1) Place the magnetic stirrer on the 3D mounting rack, install the array liquid tank on the magnetic stirrer, install the feed pipe and the discharge pipe on the array liquid tank, and install the electric pump and the solenoid valve on the feed pipe and the discharge pipe; (S2) Fix the cathode and the anode on the anode clamp and the cathode clamp, turn on the electric pump to feed the plating solution into the array liquid tank, adjust the positions of the anode clamp and the cathode clamp, and immerse the cathode, the anode, and the carrier in the plating solution; (S3) Perform potentiostatic single-pulse electroplating, select the single-pulse electroplating parameters, after completion, open the solenoid valve to discharge the solution from the discharge pipe, and obtain the electroplated product after drying; (S4) Remove the electroplated product, use the electroplated product as a working electrode, form a three-electrode system with a reference electrode and a counter electrode, connect it to an electrochemical workstation, and perform electrochemical testing.

2. A method for two-electrode electroplating using a high-throughput electrochemical synthesis and testing integrated machine, characterized in that, the integrated machine is the integrated machine of claim 1, and further includes a cover plate. An electrode jack is opened on the cover plate. The electrode jack includes a cathode jack, symmetrically arranged driving electrode jacks, a first anode jack, and a second anode jack. The distances between the first anode jack, the second anode jack, and the cathode jack are 5-8 mm and 13-15 mm respectively; the method includes the following steps: (S1) Place the magnetic stirrer on the 3D mounting rack, install the array liquid tank on the magnetic stirrer, install the feed pipe and the discharge pipe on the array liquid tank, install the electric pump and the solenoid valve on the feed pipe and the discharge pipe, and place the liquid level gauge in the array liquid tank and connect it to the electric pump; (S2) Fix the two-electrode cathode and two driving electrodes in the cathode jack and the driving electrode jacks on the cover plate, fix the driving electrodes with the cathode clamp, fix the two-electrode anode at the first anode jack or the second anode jack, and connect the two-electrode cathode and the two-electrode anode together with a wire; (S3) Use the electric pump to feed the plating solution into the array liquid tank, judge the volume of the fed plating solution according to the liquid level gauge, and turn off the electric pump; immerse the two-electrode cathode and the two-electrode anode in the plating solution; (S4) Use a DC regulated power supply to provide a driving potential, select the driving voltage and deposition time for electroplating. After completion, open the solenoid valve to discharge the solution from the discharge pipe. After drying, the electroplated product is obtained. (S5) Remove the electroplated product. Using the electroplated product as the working electrode, form a three-electrode system with the reference electrode and the counter electrode, connect it to an electrochemical workstation, and conduct electrochemical tests.

3. The method according to claim 2, characterized in that, the array liquid tank is composed of n×m unit tanks, where n, m≥5. The unit tanks are connected with feed capillary tubes and discharge capillary tubes. Level gauges and electric pumps are installed on the feed capillary tubes and discharge capillary tubes in each unit tank, and the discharge capillary tubes are uniformly connected to the discharge pipe.

4. The method according to claim 1 or 2, characterized in that, the magnetic stirrer is a heatable magnetic stirrer with a power of 400 - 1000 W and a rotation speed range of 0 - 1500 RPM.

5. The method according to claim 1 or 2, characterized in that, the 3D mounting rack is composed of a base, a bracket, a cathode fixture guide rail, an anode fixture guide rail, a motor, and a motor switch; the motor is fixed on the base, the bracket is perpendicularly mounted on the motor with respect to the base, the cathode fixture guide rail and the anode fixture guide rail are fixed between the two brackets, the motor controls the movement of the cathode fixture guide rail and the anode fixture guide rail, and the anode fixture and the cathode fixture are slidably mounted on the anode fixture guide rail and the cathode fixture guide rail.

6. The method according to claim 1 or 2, characterized in that, the anode fixture and the cathode fixture are composed of stainless steel chucks welded to wires.

7. The method according to claim 1 or 2, characterized in that, the anode is a copper sheet, copper foam, nickel foam, nickel plate, carbon fiber cloth or stainless steel, and the cathode is Fe, Zn, Mn, Ni, Co, Cu, C, B, P, Ag, Au, Pd.

Citation Information

Patent Citations

  • High-flux electrochemical synthesis and test integrated machine

    CN212688224U