CN111733441A - High-flux electrochemical synthesis and test all-in-one machine and use method thereof - Google Patents

High-flux electrochemical synthesis and test all-in-one machine and use method thereof Download PDF

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Publication number
CN111733441A
CN111733441A CN202010455333.9A CN202010455333A CN111733441A CN 111733441 A CN111733441 A CN 111733441A CN 202010455333 A CN202010455333 A CN 202010455333A CN 111733441 A CN111733441 A CN 111733441A
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anode
cathode
electrode
clamp
test
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魏永生
付文英
王茂森
刘妍
陈玲熙
吕怡梦
苏茂青
韦露
赵新生
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Jiangsu Normal University
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Jiangsu Normal University
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    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D17/00Constructional parts, or assemblies thereof, of cells for electrolytic coating
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D21/00Processes for servicing or operating cells for electrolytic coating
    • C25D21/12Process control or regulation
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00Electroplating characterised by the process; Pretreatment or after-treatment of workpieces

Abstract

The invention discloses a high-flux electrochemical synthesis and test integrated machine and a using method thereof, the integrated machine comprises an array liquid tank, an electric pump, an electromagnetic valve, a feed barrel, a discharge barrel, a magnetic stirrer, a 3D mounting frame, an anode clamp and a cathode clamp, wherein the array liquid tank is respectively communicated with the feed barrel and the discharge barrel through the feed pipe and the discharge pipe, the electric pump is arranged on the feed pipe, the electromagnetic valve is arranged 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 frame, the anode clamp and the cathode clamp well clamp an anode and a cathode, and the anode clamp and the cathode clamp are slidably arranged on the 3D mounting frame and are suspended above the array liquid tank, and the. The all-in-one electroplating bath is an array electroplating bath, can electroplate a plurality of samples at one time, has a plurality of using methods, unifies the synthesis and test processes, is convenient to operate, and has a local high-flux screening system, so that the screening process is accelerated, and the screening quality is improved.

Description

High-flux electrochemical synthesis and test all-in-one machine and use method thereof
Technical Field
The invention relates to an electrochemical synthesis and test all-in-one machine, in particular to a high-throughput electrochemical synthesis and test all-in-one machine and a using method thereof.
Background
The electroplating is a process of respectively carrying out oxidation and reduction reactions on an anode and a cathode under the action of an external power supply, is the basis of metal electrolytic smelting and electroplating processes, and becomes a very important modern processing technology in the aspects of traditional decoration, wear resistance, friction reduction, corrosion resistance, surface modification, development of new materials of electrical property coatings and optical property coatings and the like. The selection of the plating bath is particularly important in electroplating, the commonly used plating bath can only be used for preparing one sample at a time at present, a large amount of manpower and time are consumed, and the working efficiency is low; the distance between the cathode and the anode cannot be adjusted, so that the experimental result is single; and the material changing is complicated, and the electroplating efficiency is low.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to provide a high-throughput electrochemical synthesis and test all-in-one machine which can realize multi-sample synthesis, is adjustable in electrode distance and convenient in material change and has high electroplating efficiency.
The technical scheme is as follows: the high-flux electrochemical synthesis and test integrated machine comprises an array liquid tank, an electric pump, a solenoid valve, a feed barrel, a discharge barrel, a magnetic stirrer, a 3D mounting frame, an anode clamp and a cathode clamp, wherein the array liquid tank is respectively communicated with the feed barrel and the discharge barrel through a feed pipe and a discharge pipe; the electric pump and the electromagnetic valve are arranged on the feeding pipe and the discharging pipe and used for controlling the plating solution to flow in and out; magnetic stirrers sets up in array cistern bottom, and array cistern, magnetic stirrers set up on the 3D mounting bracket, and positive pole and negative pole have been held to positive pole anchor clamps, negative pole anchor clamps, and slidable mounting is on the 3D mounting bracket and hangs in array cistern top, is provided with the level gauge that links to each other with the electric pump in the array cistern.
The array liquid tank consists of n multiplied by m unit tanks, wherein n and m are more than or equal to 5, the unit tanks are connected with a feeding thin pipe and a discharging thin pipe, the feeding thin pipe and the discharging thin pipe in each unit tank are respectively provided with a liquid level meter and an electric pump, the feeding and discharging are controlled by switching on and off the electric pump, the discharging thin pipe is connected to a discharging pipe through an electromagnetic valve, the feeding thin pipe is connected with a feeding barrel which is provided with plating solutions with different components through a feeding pipe, the number of the feeding barrels is 1-10, the liquid level meters are used for sensing the position of the solutions and are connected with the electric pumps to control the volume of the plating; the magnetic stirrer is a heatable magnetic stirrer, the power is 400-1000W, the rotating speed range is 0-1500RPM, and the 3D mounting rack consists of a base, a support, a cathode clamp guide rail, an anode clamp guide rail, a motor and a motor switch; the motor is fixed on the base, the supports are perpendicular to the base and are installed on the motor, the cathode clamp guide rail and the anode clamp guide rail are fixed between the two supports, and the anode clamp and the cathode clamp are slidably installed on the anode clamp guide rail and the cathode clamp guide rail; the anode clamp and the cathode clamp are composed of stainless steel clamps welded on the lead; the all-in-one machine further comprises a cover plate, wherein electrode jacks are formed in the cover plate, the electrode jacks comprise cathode jacks, driving electrode jacks, first anode jacks and second anode jacks, the driving electrode jacks are symmetrically arranged, and the distances between the first anode jacks, the second anode jacks and the cathode jacks are 5-10 mm and 10-15 mm respectively; the anode is made of copper sheet, foam copper, foam nickel, nickel plate, carbon fiber cloth or stainless steel, and the cathode is made of Fe, Zn, Mn, Ni, Co, Cu, C, B, P, Ag, Au or Pd.
The use method of the high-flux electrochemical synthesis and test integrated machine comprises the following steps during high-flux electroplating:
(S1) placing a magnetic stirrer on a 3D mounting rack, wherein an array liquid tank is arranged on the magnetic stirrer, a feeding pipe and a discharging pipe are sequentially arranged on the array liquid tank, and an electric pump and an electromagnetic valve are arranged on the feeding pipe and the discharging pipe;
(S2) fixing a cathode and an anode on the anode clamp and the cathode clamp, opening the electric pump to introduce the plating solution into the array liquid tank, adjusting the positions of the anode clamp and the cathode clamp, and immersing the cathode, the anode and the carrier into the plating solution;
(S3) performing constant potential single pulse electroplating, selecting single pulse electroplating parameters, opening the electromagnetic valve to discharge the solution from the discharge pipe after the single pulse electroplating parameters are selected, and drying to obtain an electroplating product;
(S4) taking down the electroplating product, taking the electroplating product as a working electrode, forming a three-electrode system with a reference electrode and a counter electrode, connecting with an electrochemical workstation, and carrying out electrochemical test.
The use method of the high-flux electrochemical synthesis and test integrated machine comprises the following steps during double-electrode electroplating:
(S1) placing a magnetic stirrer on a 3D mounting rack, wherein an array liquid tank is arranged on the magnetic stirrer, a feeding pipe and a discharging pipe are sequentially arranged on the array liquid tank, and an electric pump and an electromagnetic valve are arranged on the feeding pipe and the discharging pipe;
(S2) fixing the dual-electrode cathode and two driving electrodes in the cathode insertion hole and the driving electrode insertion hole of the cover plate, fixing the driving electrodes with a cathode fixture, fixing the dual-electrode anode in the first anode insertion hole or the second anode insertion hole, and connecting the dual-electrode cathode and the dual-electrode anode with a wire;
(S3) introducing the plating solution into the array liquid tank by using the electric pump, judging the volume of the introduced plating solution according to the liquid level meter, and closing the electric pump; immersing the bipolar cathode and the bipolar anode in a plating solution;
(S4) providing a driving potential by using a direct current stabilized voltage supply, selecting a driving voltage and a deposition time for electroplating, opening an electromagnetic valve after the electroplating is finished, discharging the solution from a discharge pipe, and drying to obtain an electroplating product;
(S5) taking down the electroplating product, taking the electroplating product as a working electrode, forming a three-electrode system with a reference electrode and a counter electrode, connecting with an electrochemical workstation, and carrying out electrochemical test.
Has the advantages that: compared with the prior art, the invention has the following remarkable advantages: 1. the electroplating bath is an array electroplating bath, an electroplating mode can be freely selected, a plurality of samples can be electroplated at one time, and the integration of electroplating and testing is realized; 2. the high-flux screening system greatly reduces the consumption of reaction raw materials, remarkably accelerates the screening process and improves the screening quality; 3. the feeding and discharging can be automatically controlled, the position of the solution is judged by a liquid level meter and the flow and time of the electric pump, and the feeding and discharging are intelligently carried out; 4. can freely adjust the distance between the negative and positive poles, change the negative and positive poles of different materials, convenient to use is nimble.
Drawings
FIG. 1 is a schematic structural view of the present invention;
FIG. 2 is a top view of the present invention;
FIG. 3 is a front view of the present invention;
FIG. 4 is a schematic view showing the connection of parts of the array plating tank;
FIG. 5 is a top view of the array plating tank;
FIG. 6 is a schematic diagram of an array plating tank structure;
FIG. 7 is a cross-sectional view of a cell slot;
FIG. 8 is a schematic view of the anode and cathode clamps;
FIG. 9 is a schematic view of a cover plate configuration;
FIG. 10 is a schematic diagram of the use of dual-electrode plating to prepare a catalyst electrode;
FIG. 11 is a schematic representation of the electrode in use during testing;
FIG. 12 is a graph of LSV at different nickel chloride concentrations in example 1;
FIG. 13 is a graph comparing overpotentials for catalysts of different nickel chloride concentrations in example 1.
Detailed Description
Example 1
As shown in fig. 1 to 4, the 3D automatic control high flux electrochemical synthesis and test integrated machine comprises an array liquid tank 1, an electric pump 4, an electromagnetic valve 9, a feed tank 7, a discharge tank 8, a magnetic stirrer 10, a 3D mounting rack, an anode clamp 17 and a cathode clamp 18, as shown in fig. 5 to 7, the array liquid tank 1 has a tank length of 215mm, a width of 215mm and a tank depth of 40mm and consists of 5 × 5 unit tanks, two circular pore channels 2 communicated with the interior of the tank are respectively arranged on the edges of each unit tank, the unit tanks are connected with a feed tubule and a discharge tubule through the circular pore channels 2, the electric pump 4 is arranged on the feed tubule and the discharge tubule in each unit tank, the discharge tubule is connected to a discharge pipe 6 through the electromagnetic valve 9, the discharge pipe 6 and the discharge tank 8 of the discharge pipe 6 are communicated, the feed pipes 5 in the 5 unit tanks are connected to the respective feed tank 7 through the electromagnetic valve 9, the electric pump, the size is 42mm multiplied by 26mm multiplied by 39mm, the working voltage is direct current 10-15V, the rated current is 0.2-0.5A, the maximum lift is 0.8-1.5m, the electromagnetic valve 9 is arranged 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, the power is 400-1000W, the rotating speed range is 0-1500RPM, the array liquid tank 1 and the magnetic stirrer 10 are arranged on a 3D mounting rack, an anode clamp 17 and a cathode clamp 18 clamp an anode and a cathode, and the 3D mounting rack is composed of a base 11, a bracket 12, a cathode clamp guide rail 13, an anode clamp guide rail 14, a motor 15 and a motor switch 16; the motor 15 is fixed on the base 11, the support 12 is perpendicular to the base 11 and is installed on the motor 15, the cathode clamp guide rail 13 and the anode clamp guide rail 14 are fixed between the two support 12, the anode clamp 17 and the cathode clamp 18 are slidably installed on the anode clamp guide rail 14 and the cathode clamp guide rail 13, as shown in fig. 8, the anode clamp 17 and the cathode clamp 18 are composed of stainless steel chucks 20 welded on a lead 21, as shown in fig. 9, a cover plate 22 is further included during double-electrode electroplating, electrode jacks are formed in the cover plate 22, the electrode jacks include cathode jacks 30, symmetrically-arranged driving electrode jacks 29, first anode jacks 31 and second anode jacks 32, and distances between the first anode jacks 31, the second anode jacks 32 and the cathode jacks 30 are 8mm and 13mm respectively.
The high-flux electroplating is based on constant potential electroplating, a proper deposition potential is searched before electroplating, carrier carbon fiber cloth is pretreated firstly to remove surface oil stains, 5 carbon fiber cloth is put into ethanol solution to be ultrasonically vibrated for 5min, then the carrier carbon fiber cloth is ultrasonically vibrated for 2min in dilute hydrochloric acid solution with the concentration of 0.01mol/L, finally the carrier carbon fiber cloth is ultrasonically vibrated for 10min in deionized water, and the carrier carbon fiber cloth is dried and weighed for later use.
Iron chloride solution, sodium hypophosphite solution, boric acid, trisodium citrate and nickel chloride solution are respectively put into 5 feed barrels 7, wherein the concentration of the iron chloride solution is 0.05mol/L, the concentration of the sodium hypophosphite solution is 0.15mol/L, the concentration of the boric acid is 0.4mol/L, the concentration of the trisodium citrate is 37.5g/L, and the concentration of the nickel chloride solution is 1mol/L, the electric pump 4 is started to add the iron chloride solution, the sodium hypophosphite solution, the boric acid and the trisodium citrate into 5 unit tanks, and the electric pump 4 controls the concentrations of the nickel chloride solution in the 5 unit tanks to be 0.05, 0.08, 0.1, 0.12 and 0.15mol/L respectively by controlling the flow rate and the starting time; then, the volume of the plating solution is judged by using the liquid level meter 19, the electric pump 4 is closed, and when the plating solution is insufficient, the electric pump 4 continues to add the plating solution.
Selecting graphite plates as a cathode and an anode, fixing the cathode graphite plate on a cathode clamp 17, turning on a motor switch 16, controlling a motor 15 to adjust the distance between the cathode and the anode, adjusting the position in a unit tank, soaking the carbon fiber cloth in the solution, performing constant-potential single-pulse electroplating for 18min at the voltage of 6V, controlling the temperature of a magnetic stirrer 10 at 50 ℃, turning on an electromagnetic valve 9 to discharge the solution through a main discharge pipe 6 after the completion of the operation, repeatedly washing the solution for several times by using deionized water through ultrasonic oscillation, and drying to obtain 5 carbon fiber cloth loaded NiFeP alloy electro-catalytic hydrolysis catalysts with different nickel contents.
As shown in FIG. 11, a saturated calomel electrode is used as a reference electrode 24, graphite is used as a counter electrode 25, a NiFeP alloy supported carbon fiber cloth electrocatalytic hydrolysis hydrogen production catalyst is used as a working electrode 23, the three electrodes are fixed by a cathode clamp and an anode clamp, KOH solution with the concentration of 1mol/L is introduced into a unit cell, and N is introduced2And connecting with an electrochemical workstation, and performing electrochemical tests, wherein the results are shown in fig. 12-13, fig. 12 is an LSV (surface-to-surface voltage) graph under different nickel chloride concentrations, and fig. 13 is a comparative curve chart of overpotentials of catalysts under different nickel chloride concentrations.
Example 2
The difference between this example and example 1 is: pretreating 10 pieces of carbon fiber cloth, placing into a unit tank, selecting copper sheet as anode and graphite plate as cathode, turning on a motor switch 16, controlling a motor 15 to adjust the distance between the anode and the cathode, respectively placing plating solution comprising nickel chloride solution, sodium hypophosphite solution, boric acid, trisodium citrate and ferric chloride solution in 5 feed barrels 7, wherein the concentration of the nickel chloride solution is 0.08mol/L, the concentration of the sodium hypophosphite solution is 0.2mol/L, the concentration of boric acid is 0.3mol/L, the concentration of trisodium citrate is 25g/L, the concentration of the ferric chloride solution is 0.1mol/L, the electric pump 4 controls the concentrations of the ferric chloride solutions in 10 unit tanks to be 0.03, 0.04, 0.05, 0.06, 0.07, 0.08, 0.09, 0.1, 0.11 and 0.12mol/L respectively by controlling the flow rate and the opening time, the volume of the plating solution is judged to be introduced according to a liquid level meter 19, and then the electric pump is closed; constant potential single pulse electroplating is carried out for 15min, the voltage is 5V, and the temperature is controlled at 60 ℃. And after the reaction is finished, opening the electromagnetic valve 9 to discharge the solution through the main discharge pipe 6, repeatedly ultrasonically vibrating and washing the solution for several times by using deionized water, and drying the solution to obtain 10 carbon fiber cloth-loaded NiFeP alloy electrocatalytic hydrolysis hydrogen production catalysts with different iron contents.
Example 3
The difference between this example and example 1 is: pre-treating 25 pieces of carbon fiber cloth, placing the cloth into a unit tank, selecting a copper sheet as a cathode and a platinum sheet as an anode, adjusting the distance between the cathode and the anode, wherein a plating solution comprises a nickel chloride solution, an iron chloride solution, boric acid and trisodium citrate, wherein the concentration of the nickel chloride solution is 0.08mol/L, the concentration of the ferric chloride solution is 0.2mol/L, the concentration of boric acid is 0.3mol/L, the concentration of trisodium citrate is 25g/L, the concentration of the sodium hypophosphite solution is 1mol/L, the electric pump 4 controls the concentrations of the sodium hypophosphite solutions in 25 unit tanks 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 and 0.3mol/L respectively by controlling the flow rate and the turn-on time, the volume of the plating solution is judged according to a liquid level meter 19, and then the electric pump 4 is turned off; and (3) carrying out constant potential single pulse electroplating for 21min at the voltage of 4V and the temperature of 45 ℃, discharging the solution by using the electromagnetic valve 9 after finishing, repeatedly washing the solution by using deionized water through ultrasonic vibration for several times, and drying the solution to obtain 25 carbon fiber cloth-loaded NiFeP alloy electrocatalytic hydrolysis hydrogen production catalysts with different phosphorus contents.
Example 4
The difference between this example and example 1 is: double-electrode electroplating, namely selecting 10 copper sheets with the length, width and thickness of 50 multiplied by 3 multiplied by 0.5mm as a group, taking the 10 copper sheets as a group with two groups as a double-electrode cathode 27, soaking the double-electrode cathode 27 in acetone for oil removal and grease removal, soaking the double-electrode cathode 27 in chromic acid for 1min to remove surface oxides, marking the number on the copper sheets to be 1-10, ensuring that the ends of the 10 double-electrode cathodes 27 are positioned on one plane, winding each copper sheet by using a transparent adhesive tape to achieve an insulation effect, winding the 10 copper sheets for multiple circles by using the transparent adhesive tape to fix the copper sheets as a cathode whole consisting of 10 double-electrode cathodes 27, wherein a driving electrode 28 is a graphite sheet, the length, width and thickness are 40 multiplied by 3 multiplied by 2mm, a double-electrode anode 26 is a graphite; the plating solution comprises a nickel chloride solution with the concentration of 0.1mol/L, a ferric chloride solution with the concentration of 0.05mol/L, a sodium hypophosphite solution with the concentration of 0.15mol/L, boric acid with the concentration of 0.4mol/L and trisodium citrate with the concentration of 37.5g/L, which are respectively arranged in 5 feed barrels 7, a feed pipe 5 is led into the 5 feed barrels 7, an electric pump 4 is turned on to lead the plating solution into a unit cell, the volume of the plating solution is judged according to a liquid level meter 19, and the electric pump is turned off; covering the cover plate 22 as shown in fig. 9, and inserting the driving electrode 28, the two-electrode cathode 27, and the two-electrode anode 26, respectively; as shown in fig. 10, a double-electrode cathode 27, a driving electrode 28 and a double-electrode anode 26 are respectively fixed in a cathode jack 30, a driving electrode jack 29 and a first anode jack 31, wherein the number of the double-electrode cathodes 27 is 10, the thickness of the double-electrode cathodes 27 is 0.5mm, the distance between the double-electrode cathodes 27 and the double-electrode anode 26 is 8, 8.5, 9, 9.5, 10, 10.5, 11, 11.5, 12 and 12.5mm, a motor switch 16 is turned on, a motor 15 is controlled to select a proper height of a cathode clamp 18, the driving electrode 28 is fixed on the cathode clamp 18, the double-electrode cathodes 27 and the double-electrode anodes 26 are connected by leads, the driving electrode 28 is connected with a direct-current stabilized voltage power supply, the driving potential is set to be 6V, the electroplating time is 5min, after the electroplating is finished, the electroplating solution is discharged by using an electromagnetic valve 9, and the product is washed by.
Example 5
The difference between this example and example 4 is: the double-electrode anode 26 is fixed on the second anode jack 32, the distance between the 10 double-electrode cathodes 27 and the double-electrode anode 26 is 13mm, 13.5 mm, 14 mm, 14.5 mm, 15mm, 15.5 mm, 16 mm, 16.5 mm, 17 mm and 17.5mm, and the NiFeP catalysts with 10 different double-electrode distances are obtained after the test is finished.
Example 6
The difference between this example and example 4 is: the 5 feed barrels 7 are respectively filled with ferric chloride solution with the concentration of 0.05mol/L, sodium hypophosphite solution with the concentration of 0.15mol/L, boric acid with the concentration of 0.4mol/L, trisodium citrate with the concentration of 37.5g/L and nickel chloride solution with the concentration of 1mol/L, the volume of the plating solution is judged to be fed according to a liquid level meter 19, the electric pump 4 controls the concentration of the nickel chloride solution in 5 unit tanks to be 0.05, 0.08, 0.1, 0.12 and 0.15mol/L respectively by controlling the flow rate and the starting time, the volume of the plating solution is judged to be fed according to the liquid level meter 19, and the electric pump 4 is closed; the distance between the No. 1 sample and the No. 10 sample and the double-electrode anode is different, and the hydrogen evolution performance can be conveniently analyzed by sampling more samples. The bipolar cathode 27 and the bipolar anode 26 are connected by a lead, the driving electrode 28 is connected with a direct current stabilized power supply, the driving potential is set to be 8V, and the electroplating time is 6 min. After the electroplating is finished, the plating solution is discharged by using the electromagnetic valve 9, and the product is washed by deionized water, so that 50 NiFeP catalysts with different double-electrode distances and different nickel chloride concentrations shown in the table 1 are obtained.
Table 1 experimental samples in example 6
Figure BDA0002509149550000071

Claims (10)

1. The high-flux electrochemical synthesis and test integrated machine is characterized by comprising an array liquid tank (1), an electric pump (4), an electromagnetic valve (9), a feeding barrel (7), a discharging barrel (8), a magnetic stirrer (10), a 3D mounting frame, an anode clamp (17) and a cathode clamp (18), wherein the array liquid tank (1) is respectively communicated with the feeding barrel (7) and the discharging barrel (8) through a feeding pipe (5) and a discharging pipe (6); the electric pump (4) and the electromagnetic valve (9) are arranged on the feeding pipe (5) and the discharging pipe (6); magnetic stirrers (10) set up in array cistern (1) bottom, array cistern (1), magnetic stirrers (10) set up on the 3D mounting bracket, positive pole and negative pole have been good in positive pole anchor clamps (17), negative pole anchor clamps (18) centre gripping, and slidable mounting is on the 3D mounting bracket and hangs in array cistern (1) top, be provided with level gauge (19) that link to each other with electric pump (4) in array cistern (1).
2. The high-throughput electrochemical synthesis and test integrated machine according to claim 1, wherein the array liquid tank (1) is composed of n x m unit tanks, wherein n and m are larger than or equal to 5, the unit tanks are connected with a feeding tubule and a discharging tubule, liquid level meters (19) and electric pumps (4) are mounted on the feeding tubule and the discharging tubule in each unit tank, the discharging tubules are uniformly connected to a discharging pipe (6), the feeding tubules are connected with feeding barrels (7) which are connected with plating solutions containing different components through feeding pipes (5), and the number of the feeding barrels (7) is 1-10.
3. The integrated high-throughput electrochemical synthesis and test machine according to claim 1, wherein the magnetic stirrer (10) is a heatable magnetic stirrer with power of 400-1000W and rotation speed range of 0-1500 RPM.
4. The high-throughput electrochemical synthesis and test all-in-one machine is characterized in that the 3D mounting frame consists of a base (11), a support (12), a cathode clamp guide rail (13), an anode clamp guide rail (14), a motor (15) and a motor switch (16); the motor (15) is fixed on the base (11), the support (12) is perpendicular to the base (11) and is installed on the motor (15), the cathode clamp guide rail (13) and the anode clamp guide rail (14) are fixed between the two supports (12), the motor (15) controls the cathode clamp guide rail (13) and the anode clamp guide rail (14) to move, and the anode clamp (17) and the cathode clamp (18) are slidably installed on the anode clamp guide rail (14) and the cathode clamp guide rail (13).
5. The integrated high-throughput electrochemical synthesis and test machine according to claim 1, wherein the anode clamp (17) and the cathode clamp (18) are formed by stainless steel clamps (20) welded on lead wires (21).
6. The high-throughput electrochemical synthesis and test integrated machine according to claim 1, further comprising a cover plate (22), wherein electrode jacks are formed in the cover plate (22), the electrode jacks comprise cathode jacks (30), symmetrically-arranged driving electrode jacks (29), first anode jacks (31) and second anode jacks (32), and the distances between the first anode jacks (31), the second anode jacks (32) and the cathode jacks (30) are respectively 5-10 mm and 10-15 mm.
7. The high-throughput electrochemical synthesis and test all-in-one machine is characterized in that the anode is copper sheet, copper foam, nickel plate, carbon fiber cloth or stainless steel, and the cathode is Fe, Zn, Mn, Ni, Co, Cu, C, B, P, Ag, Au or Pd.
8. The use method of the high-throughput electrochemical synthesis and test all-in-one machine as claimed in claim 1, wherein the high-throughput electroplating comprises the following steps:
(S1) placing a magnetic stirrer (10) on a 3D mounting rack, installing an array liquid tank (1) on the magnetic stirrer (10), installing a feeding pipe (5) and a discharging pipe (6) on the array liquid tank (1), and installing an electric pump (4) and an electromagnetic valve (9) on the feeding pipe (6) and the discharging pipe (5);
(S2) fixing a cathode and an anode on the anode clamp (17) and the cathode clamp (18), opening the electric pump (4) to introduce the plating solution into the array liquid tank (1), adjusting the positions of the anode clamp (17) and the cathode clamp (18), and immersing the cathode, the anode and the carrier into the plating solution;
(S3) carrying out constant potential single pulse electroplating, selecting single pulse electroplating parameters, opening the electromagnetic valve (9) to discharge the solution from the discharge pipe after the single pulse electroplating parameters are selected, and drying to obtain an electroplating product;
(S4) taking off the electroplating product, taking the electroplating product as a working electrode (23), forming a three-electrode system with a reference electrode (24) and a counter electrode (25), connecting with an electrochemical workstation, and carrying out electrochemical test.
9. The use method of the high-throughput electrochemical synthesis and test all-in-one machine as claimed in claim 6, wherein the double-electrode electroplating comprises the following steps:
(S1) placing a magnetic stirrer (10) on a 3D mounting rack, installing an array liquid tank (1) on the magnetic stirrer (10), installing a feeding pipe (5) and a discharging pipe (6) on the array liquid tank (1), installing an electric pump (4) and an electromagnetic valve (9) on the feeding pipe (6) and the discharging pipe (5), and placing a liquid level meter (19) in the array liquid tank (1) and connecting the liquid level meter with the electric pump (4);
(S2) fixing the double-electrode cathode (27) and two driving electrodes (28) in a cathode jack (30) and a driving electrode jack (29) on the cover plate (22), fixing the driving electrodes (28) by a cathode clamp (18), fixing the double-electrode anode (26) at a first anode jack (31) or a second anode jack (32), and connecting the double-electrode cathode (27) and the double-electrode anode (26) by a lead;
(S3) introducing the plating solution into the array liquid tank (1) by using the electric pump (4), judging the volume of the introduced plating solution according to the liquid level meter (19), and closing the electric pump (4); immersing a bipolar cathode (27) and a bipolar anode (26) in a plating solution;
(S4) providing a driving potential by using a direct current stabilized voltage supply, selecting the driving voltage and the deposition time for electroplating, opening an electromagnetic valve (9) after the electroplating is finished, discharging the solution from a discharge pipe, and drying to obtain an electroplating product;
(S5) taking off the electroplating product, taking the electroplating product as a working electrode (23), forming a three-electrode system with a reference electrode (24) and a counter electrode (25), connecting with an electrochemical workstation, and carrying out electrochemical test.
10. The use method of the integrated machine for high throughput electrochemical synthesis and test according to claim 8 or 9, wherein the buffer solution used in the electrochemical test process is KOH solution.
CN202010455333.9A 2020-05-26 2020-05-26 High-flux electrochemical synthesis and test all-in-one machine and use method thereof Pending CN111733441A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
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CN114264708A (en) * 2021-12-22 2022-04-01 合肥工业大学 Method for rapidly analyzing potential influence in chemical deposition

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114264708A (en) * 2021-12-22 2022-04-01 合肥工业大学 Method for rapidly analyzing potential influence in chemical deposition

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