An apparatus for measuring the current efficiency of electrochemical dissolution of a metal

Abstract

The application discloses a device for measuring metal electrochemical dissolution current efficiency, which comprises a reactor, a sample groove is formed on the upper surface of the reactor, liquid inlet holes and liquid outlet holes are respectively formed on the left and right sides of the reactor, the sample groove is communicated with the liquid inlet holes and the liquid outlet holes through liquid inlet auxiliary flow channels and liquid outlet auxiliary flow channels and forms a U-shaped channel, the liquid inlet holes and the liquid outlet holes are respectively connected with liquid inlet pipes and liquid outlet pipes, an anode hole which is communicated with the sample groove is formed on the front side of the reactor, an anode connecting post is arranged in the anode hole, a cover plate is arranged on the upper part of the reactor, a cathode hole which is corresponded to the sample groove is formed on the cover plate, and a cathode material is penetrated into the cathode hole. The device is compact in structure by arranging the reactor and designing the U-shaped channel in the reactor, a sealing ring is conveniently installed, the sealing effect of the reactor is enhanced, electrolyte leakage is avoided to cause corrosion to the equipment, and a process environment of electrolytic processing is simulated, so that the current efficiency test is realized quickly and with saved materials.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of current efficiency test, and particularly relates to a device for measuring current efficiency of metal electrochemical dissolution. BACKGROUND

[0002] The current efficiency of metal electrochemical dissolution is an important index for formulating electrolytic processing parameters. Wherein, η is the current efficiency, and the current efficiency can only be obtained through experiments, and no theoretical derivation formula is available, so obtaining accurate current efficiency value is an important guarantee for carrying out electrolytic processing.

[0003] At present, the current efficiency test basically adopts a flow cell device, a sample is installed in a designed square groove, the cathode feeding is controlled, a direct current is passed between the sample and the cathode in the device through the electrolyte, and the actual conditions of electrolytic processing are simulated.

[0004] The existing flow cell device design has the following defects: 1, when the test sample is small, the square cathode and the square hole matched therewith are difficult to process; 2, the upper cover of the device is connected and fastened with the main body by screws, and the operation is inconvenient; 3, in order to prevent the electrolyte flowing at high speed in the device from overflowing, a groove is further processed on the square cathode to place a sealing ring, the sealing ring is a standard part, and such design brings inconvenience to actual operation and reduces the service life of the sealing ring; 4, the opposite surfaces of the test sample and the cathode are usually designed to be the same size and shape, but in order to facilitate sample filling, the sample groove size is generally larger than the sample size, so that the sample and the cathode are not necessarily centered during sample filling, and the sample installation position offset will lead to uneven actual electrochemical dissolution, and there is a large error in the test data. SUMMARY

[0005] The technical problem to be solved by the application is to provide a device for measuring current efficiency of metal electrochemical dissolution in view of the defects of the prior art.

[0006] To solve the above technical problems, the technical scheme adopted by the present application is: a device for measuring the electrochemical dissolution current efficiency of metal, characterized in that the device comprises a reactor, a sample groove is formed on the upper surface of the reactor, liquid inlet holes and liquid outlet holes are respectively formed on the left and right sides of the reactor, the sample groove, the liquid inlet holes and the liquid outlet holes are respectively connected through liquid inlet auxiliary flow channels and liquid outlet auxiliary flow channels and form a Chinese character 'z', the liquid inlet holes and the liquid outlet holes are respectively connected with liquid inlet pipes and liquid outlet pipes, an anode hole is formed on the front side of the reactor and is connected with the sample groove, an anode terminal is arranged in the anode hole, a cover plate is arranged on the upper part of the reactor, a cathode hole corresponding to the sample groove is formed on the cover plate, and a cathode material is inserted into the cathode hole.

[0007] The device for measuring the electrochemical dissolution current efficiency of metal is characterized in that a recess is arranged on the upper surface of the reactor, and a protrusion is correspondingly arranged on the lower part of the cover plate.

[0008] The device for measuring the electrochemical dissolution current efficiency of metal is characterized in that a gasket groove is arranged on the outer side of the sample groove on the upper surface of the reactor, and a sealing ring is arranged in the gasket groove.

[0009] The device for measuring the electrochemical dissolution current efficiency of metal is characterized in that a base integrally formed with the reactor is arranged on the lower part of the reactor, and a plurality of recessed holes for bolt fixation are arranged on the base.

[0010] The device for measuring the electrochemical dissolution current efficiency of metal is characterized in that the anode material is a metal sample, the anode terminal is a metal screw, threads matched with the metal screw are arranged on the inner wall of the anode hole, a gasket and a baffle are sequentially fixed on the metal screw, the cathode material is a cylindrical brass, the cylindrical brass is installed on the Z-axis of a lathe and is fixed through a cathode terminal, a sealing ring sealed with the cover plate is installed on the cylindrical brass, and the cathode terminal and the anode terminal are respectively connected with the negative electrode and the positive electrode of a power supply.

[0011] The device for measuring the electrochemical dissolution current efficiency of metal is characterized in that a reactor quick release rod recess and a cover plate quick release rod recess are arranged on the corresponding positions of the reactor and the cover plate, and the reactor and the cover plate are connected through a quick release rod.

[0012] The device for measuring the electrochemical dissolution current efficiency of metal is characterized in that stainless steel pipes are arranged in the liquid inlet holes and the liquid outlet holes, and the stainless steel pipes are connected with an electrolyte conveyor.

[0013] The method for measuring the electrochemical dissolution current efficiency of metal by using the device comprises the following steps:

[0014] Step one, after the metal sample is ultrasonically cleaned in ethanol, it is blown dry, then weighed to obtain the weighed metal sample;

[0015] Step two, the concave hole of the base of the reactor is fixed by bolts, then the weighed metal sample obtained in step one is put into the sample groove, and the anode terminal is loaded into the anode hole to fix the metal sample, to obtain the reactor loaded with the sample;

[0016] Step three, the cathode material is installed on the Z-axis of the lathe and fixed by the cathode terminal, the position of the cathode material is adjusted by the lathe, the machining gap between the bottom surface of the cathode material and the metal sample of the reactor loaded with the sample obtained in step two is maintained, and the position of the cathode material is recorded, then the cathode material is lifted, the cover plate and the base are fixed with quick release rods, the cathode material is passed through the cathode hole, and is lowered to the recorded position to obtain the detection device; the machining gap is 0.1mm-0.4mm;

[0017] Step four, the liquid inlet hole of the detection device obtained in step three is connected to the electrolyte, and the cathode terminal and the anode terminal are connected to the negative electrode and the positive electrode of the direct current power supply respectively, to perform electrochemical dissolution of the metal sample, to obtain the dissolved metal sample;

[0018] Step five, the dissolved metal sample obtained in step four is ultrasonically cleaned in ethanol, then blown dry, then weighed, and the metal electrochemical dissolution current efficiency of the metal sample is calculated.

[0019] The metal sample is cleaned to prevent impurities from affecting, the mass of the metal sample before reaction is obtained by weighing, the concave hole of the base of the reactor is fixed by bolts, the reactor is fixed on the desktop or other plane to ensure the stability of the device, the metal sample is put into the sample groove, and the anode terminal is loaded into the anode hole to fix the metal sample, the cathode material is clamped by the Z-axis of the lathe and fixed by the cathode terminal, the cathode material is moved up and down, the machining gap between the bottom surface of the cathode material and the metal sample of the reactor loaded with the sample obtained in step two is maintained, and the position of the cathode material is recorded, a certain machining gap is maintained, a loop is formed by the electrolyte, electrochemical dissolution of the metal sample is performed, and finally the dissolved metal sample is cleaned to remove impurities, then weighed, and the metal electrochemical dissolution current efficiency of the metal sample is calculated.

[0020] The device for measuring the metal electrochemical dissolution current efficiency, characterized in that the calculation is performed by the following formula:

[0021]

[0022] In the formula, Δm is the mass loss, in g, obtained by subtracting the mass in step one from the mass in step five, K is the electrochemical equivalent, in g / C, I is the current of electrochemical dissolution, in A, t is the time of electrochemical dissolution, in min, and η is the current efficiency of metal electrochemical dissolution of the metal sample.

[0023] Compared with the prior art, the present application has the following advantages:

[0024] 1. The present application sets up a reactor and designs a few-shaped flow channel in the reactor to make the reactor structure compact, facilitate the installation of a sealing ring, strengthen the sealing effect of the reactor, avoid the corrosion of equipment caused by electrolyte leakage, simulate the process environment of electrolytic processing, realize the rapid and material-saving current efficiency test, and prevent the short circuit caused by the contact of the anode and the cathode due to the accumulation of products.

[0025] 2. The present application uses a metal sample as an anode material and is fixed by a metal screw, the metal screw is sequentially fixed with a gasket and a baffle to ensure the fixing effect, a cylindrical brass is clamped by the Z-axis of a lathe and is fixed by a cathode terminal post, the height of the cylindrical brass is adjusted by the lathe to make the cylindrical brass have a certain gap with the metal sample, the cathode terminal post and the anode terminal post are connected with the negative pole and the positive pole of a direct current power supply respectively, and electrolyte is introduced into the reactor to realize the electrochemical dissolution of the metal sample.

[0026] 3. The present application sets a recess on the upper surface of the reactor, sets a protrusion corresponding to the recess at the lower part of the cover plate, makes the recess and the protrusion cooperate with each other to ensure that the cover plate is combined with the reactor tightly and at the same time plays a positioning role for the cover plate, sets a base and a recess hole to facilitate the positioning and installation of the reactor, improves the accuracy of the test, and connects the reactor and the cover plate by a quick release rod to make the connection stable and convenient to disassemble.

[0027] The present application will be further described in detail below in combination with the drawings and examples. BRIEF DESCRIPTION OF DRAWINGS

[0028] Figure 1 is a structural schematic view of the reactor of the device for measuring the current efficiency of metal electrochemical dissolution.

[0029] Figure 2 is a top view of the reactor of the device for measuring the current efficiency of metal electrochemical dissolution.

[0030] Figure 3 is Figure 2 A-A sectional view of

[0031] Figure 4 yes Figure 2 BB cross-sectional view.

[0032] Figure 5 This is a schematic diagram of the cover plate of the device for measuring the efficiency of metal electrochemical dissolution current according to the present invention.

[0033] Figure 6 This is a schematic diagram showing the connection relationship between the cathode material of this invention and the Z-axis of the lathe.

[0034] Explanation of reference numerals in the attached figures:

[0035] 1—Reactor; 1-1—Sample tank; 1-2—Liquid inlet;

[0036] 1-3—Liquid outlet hole; 1-4—Liquid inlet auxiliary flow channel; 1-5—Liquid outlet auxiliary flow channel;

[0037] 1-6—Dent; 1-7—Washer groove; 1-8—Dent on reactor quick-release rod;

[0038] 2—Anode hole; 3—Cover plate; 3-1—Protrusion;

[0039] 3-2—Recessed quick-release lever on cover plate; 4—Cathode hole; 4-1—Cathode material;

[0040] 4-2—Sealing ring; 4-3—Cathode terminal; 5—Base;

[0041] 5-1—Concave hole; 6—Z-axis. Detailed Implementation

[0042] Example 1

[0043] like Figures 1-5 As shown, the device for measuring the electrochemical dissolution current efficiency of metals according to the present invention includes a reactor 1. A sample tank 1-1 is provided on the upper surface of the reactor 1. An inlet hole 1-2 and an outlet hole 1-3 are provided on the left and right sides of the reactor 1, respectively. The sample tank 1-1 is connected to the inlet hole 1-2 and the outlet hole 1-3 through an inlet auxiliary flow channel 1-4 and an outlet auxiliary flow channel 1-5, respectively, forming a U-shape. The inlet hole 1-2 and the outlet hole 1-3 are respectively connected to an inlet pipe and an outlet pipe. An anode hole 2 is provided on the front side of the reactor 1, which is connected to the sample tank 1-1. An anode terminal is installed in the anode hole 2. A cover plate 3 is provided on the upper part of the reactor 1. A cathode hole 4 corresponding to the sample tank 1 is provided on the cover plate 3. A cathode material 4-1 is inserted into the cathode hole 4.

[0044] It should be noted that by setting the sample groove 1-1 for containing the metal sample as the anode, by setting the liquid inlet hole 1-2 and the liquid outlet hole 1-3 and correspondingly setting the liquid inlet auxiliary flow channel 1-4 and the liquid outlet auxiliary flow channel 1-5, a few-shaped flow channel is formed, the few-shaped flow channel is adopted to make the reactor 1 compact in structure, and at the same time, it is convenient to add a sealing ring. If a straight-through type flow channel is not used, the flow channel will be very long, which will lead to the increase of the size of the reactor 1 and also cannot add a sealing ring, which is easy to cause liquid leakage at the gap between the upper cover and the lower cover. By setting the liquid inlet pipe and the liquid outlet pipe, the electrolyte can be conveniently introduced and discharged. By setting the cathode hole 4 and setting the cathode material 4-1, the cathode current is applied to the metal sample after the power is turned on. By setting the anode hole 2 and setting the anode connecting post, the anode current is applied to the metal sample after the power is turned on, so as to measure the metal electrochemical dissolution current efficiency.

[0045] It should be noted that the size of the sample groove 1-1 is 10mmx10mmx10mm (lengthxwidthxheight), the size of the metal sample is 10mmx10mmx10mm (lengthxwidthxheight) at most, the height of the metal sample is 7mm at least, the minimum size of the length and the width is 9mm, the size of the cathode material 4-1 is Φ15x70mm (diameterxlength), and the diameter of the cathode material 4-1 is greater than the diagonal length of the metal sample and the adjacent surface, so as to avoid the non-uniform electrochemical dissolution caused by the sample loading deviation.

[0046] As shown in Figures 1-5 In the embodiment, the upper surface of the reactor 1 is provided with a recess 1-6, and the lower part of the cover plate 3 is correspondingly provided with a protrusion 3-1. Through the cooperation of the recess 1-6 and the protrusion 3-1, the cover plate 3 is combined with the reactor 1 tightly, and at the same time, the cover plate 3 is positioned.

[0047] As shown in Figures 1-4 In the embodiment, the upper surface of the reactor 1 is provided with a recess 1-7 outside the sample groove 1-1, and the recess 1-7 is provided with a sealing ring. By setting the recess 1-7 and the sealing ring, the lateral liquid leakage is prevented, and the sealing effect is improved.

[0048] As shown in Figure 1 and Figure 2 In the embodiment, the lower part of the reactor 1 is provided with a base 5 which is integrally formed with the reactor 1, and the base 5 is provided with a plurality of concave holes 5-1 for bolt fixing. By setting the base 5 and the concave holes 5-1, the positioning installation of the reactor 1 is facilitated, and the accuracy of the test is improved.

[0049] As shown in Figure 1 , Figure 4 and Figure 6As shown, in this embodiment, the anode material is a metal sample, the anode terminal is a metal screw, the inner wall of the anode hole 2 is provided with threads that mate with the metal screw, a washer and a baffle are fixed on the metal screw in sequence, the cathode material 4-1 is a cylindrical brass, the cylindrical brass is mounted on the Z-axis 6 of the lathe and fixed by the cathode terminal 4-3, a sealing ring 4-2 that seals with the cover plate 3 is installed on the cylindrical brass, and the cathode terminal 4-3 and the anode terminal are connected to the negative and positive terminals of the power supply, respectively. A metal sample is used as the anode material and fixed with metal screws. A washer and a baffle are fixed to the metal screws in sequence, and the baffle presses the washer to prevent the washer from being pushed out, ensuring the fixing effect. A cylindrical brass is mounted on the Z-axis 6 of a lathe and fixed with the cathode terminal 4-3. The height of the cylindrical brass is adjusted by the lathe to make a certain gap between the cylindrical brass and the metal sample. The cathode terminal 4-3 and the anode terminal are connected to the negative and positive terminals of a DC power supply, respectively, and an electrolyte is introduced into reactor 1 to achieve electrochemical dissolution of the metal sample.

[0050] It should be noted that the lathe is a VMC650 high-speed CNC machine tool.

[0051] like Figure 1 , Figure 2 and Figure 5 As shown in this embodiment, reactor 1 and cover plate 3 are respectively provided with reactor quick-release rod recess 1-8 and cover plate quick-release rod recess 3-2 at corresponding positions. The reactor 1 and cover plate 3 are connected by quick-release rods. The quick-release rods connect reactor 1 and cover plate 3, making the connection stable and disassembly convenient.

[0052] In this embodiment, stainless steel pipes are installed in both the inlet hole 1-2 and the outlet hole 1-3, and the stainless steel pipes are connected to the electrolyte conveyor. By installing stainless steel pipes and connecting them to rubber pipes with clamps, and connecting them to the electrolyte conveyor, electrolyte is continuously supplied to reactor 1.

[0053] It should be noted that the electrolyte delivery device is a CDLF4-140 multistage pump from Shenzhou Pump Industry, which pumps the electrolyte from the water tank to the inlet hole 1-2, and then flows out from the outlet hole 1-3 and returns to the water tank to form a cycle.

[0054] Example 2

[0055] The method for measuring the efficiency of metal electrochemical dissolution current using the apparatus described in this invention includes the following steps:

[0056] Step 1: Clean the metal sample with ultrasonic in ethanol, dry it, and then weigh it to obtain the weighed metal sample.

[0057] Step two, the concave hole 5-1 of the base 5 of the reactor 1 is fixed by bolts, then the weighed metal sample obtained in step one is put into the sample groove 1-1, and the metal sample is fixed by loading the anode lug into the anode hole 2, to obtain the reactor loaded with the sample;

[0058] Step three, the cathode material 4-1 is installed on the Z-axis 6 of the lathe and fixed by the cathode lug 4-3, the position of the cathode material 4-1 is adjusted by the lathe, the machining gap between the bottom surface of the cathode material 4-1 and the metal sample of the reactor loaded with the sample obtained in step two is kept, and the position of the cathode material 4-1 is recorded, then the cathode material 4-1 is lifted, the cover plate 3 is fixed with the base 5 by quick release rods, the cathode material 4-1 is made to pass through the cathode hole 4, and is lowered to the recorded position, to obtain the device to be detected; the machining gap is 0.1mm-0.4mm, preferably 0.1mm, 0.2mm, 0.3mm and 0.4mm;

[0059] Step four, the liquid inlet hole 1-2 of the device to be detected obtained in step three is connected to an electrolyte, and the cathode lug 4-3 and the anode lug are connected to the negative electrode and the positive electrode of a direct current power supply respectively, to perform electrochemical dissolution of the metal sample, to obtain the dissolved metal sample; the electrolyte is a NaNO3 solution with a mass fraction of 10% or a NaCl solution with a mass fraction of 10%; the current of the direct current power supply is 5A-50A, preferably 5A, 10A, 25A, 40A and 50A;

[0060] Step five, the dissolved metal sample obtained in step four is ultrasonically cleaned in ethanol and then dried, and then weighed, to obtain the metal electrochemical dissolution current efficiency of the metal sample by calculation; the calculation is performed by the following formula:

[0061]

[0062] In the formula, Δm is the mass loss, in g, obtained by subtracting the mass weighed in step one from the mass weighed in step five, K is the electrochemical equivalent, in g / C, I is the current of electrochemical dissolution, in A, t is the time of electrochemical dissolution, in min, and η is the metal electrochemical dissolution current efficiency of the metal sample.

[0063] The above is only a preferred embodiment of the present application, and does not limit the present application. Any simple modification, change and equivalent change made according to the technical essence of the present application to the above embodiment are still within the protection scope of the technical solution of the present application.

Claims

1. An apparatus for measuring the current efficiency of electrochemical dissolution of a metal, characterized by, The device comprises a reactor (1), a sample groove (1-1) is formed on the upper surface of the reactor (1), liquid inlet holes (1-2) and liquid outlet holes (1-3) are formed on the left and right sides of the reactor (1) respectively, the sample groove (1-1) is communicated with the liquid inlet holes (1-2) and the liquid outlet holes (1-3) through liquid inlet auxiliary flow channels (1-4) and liquid outlet auxiliary flow channels (1-5) respectively and forms a U-shaped groove, the liquid inlet holes (1-2) and the liquid outlet holes (1-3) are connected with liquid inlet pipes and liquid outlet pipes respectively, an anode hole (2) is formed on the front side of the reactor (1) and communicated with the sample groove (1-1), an anode connecting post is arranged in the anode hole (2), a cover plate (3) is arranged on the upper part of the reactor (1), a cathode hole (4) corresponding to the sample groove (1-1) is formed on the cover plate (3), a cathode material (4-1) is penetrated into the cathode hole (4), the anode material is a metal sample, the anode connecting post is a metal screw, threads are arranged on the inner wall of the anode hole (2) and matched with the metal screw, a gasket and a baffle are fixed on the metal screw in sequence, the cathode material (4-1) is a cylindrical brass, the cylindrical brass is installed on a Z-axis (6) of a lathe and fixed through a cathode connecting post (4-3), a sealing ring (4-2) is installed on the cylindrical brass and sealed with the cover plate (3), the cathode connecting post (4-3) and the anode connecting post are connected with the negative electrode and the positive electrode of a power supply respectively.

2. The apparatus of claim 1, wherein the apparatus is characterized by: A recess (1-6) is arranged on the upper surface of the reactor (1), and a protrusion (3-1) is correspondingly arranged on the lower part of the cover plate (3).

3. The apparatus of claim 1, wherein the apparatus further comprises a current sensor configured to measure the current flowing through the metal sample. A gasket groove (1-7) is arranged on the outer side of the sample groove (1-1) on the upper surface of the reactor (1), and a sealing ring is arranged in the gasket groove (1-7).

4. The apparatus of claim 1, wherein the apparatus further comprises a current sensor. A base (5) is arranged on the lower part of the reactor (1) and integrally formed with the reactor (1), and a plurality of concave holes (5-1) for bolt fixing are arranged on the base (5).

5. The apparatus of claim 1, wherein the apparatus further comprises a current sensor. Reactor quick release rod recesses (1-8) and cover plate quick release rod recesses (3-2) are arranged on the corresponding positions of the reactor (1) and the cover plate (3), and the reactor (1) and the cover plate (3) are connected through quick release rods.

6. The apparatus of claim 1, wherein the apparatus is characterized by: Stainless steel pipes are arranged in the liquid inlet holes (1-2) and the liquid outlet holes (1-3), and the stainless steel pipes are connected with electrolyte conveyors.

7. The apparatus of claim 1, wherein the apparatus is characterized by: The method for measuring the metal electrochemical dissolution current efficiency by using the device comprises the following steps: Step one, the metal sample is ultrasonically cleaned in ethanol, dried, weighed, and the weighed metal sample is obtained; Step two, the concave holes (5-1) of the base (5) of the reactor (1) are fixed through bolts, then the weighed metal sample obtained in step one is put into the sample groove (1-1), and the metal sample is fixed by arranging the anode connecting post in the anode hole (2), so that the reactor containing the sample is obtained. Step three, install the cathode material (4-1) on the Z-axis (6) of the lathe and fix it through the cathode terminal post (4-3), adjust the position of the cathode material (4-1) through the lathe, keep the machining gap between the bottom surface of the cathode material (4-1) and the metal sample of the reactor with the sample obtained in step two, and record the position of the cathode material (4-1), then lift the cathode material (4-1), fix the cover plate (3) and the base (5) with quick release rods, make the cathode material (4-1) pass through the cathode hole (4), and lower it to the recorded position to obtain the device to be detected; the machining gap is 0.1mm~0.4mm; Step four, connect the liquid inlet hole (1-2) of the device to be detected obtained in step three to the electrolyte, and connect the cathode terminal post (4-3) and the anode terminal post to the negative and positive poles of the direct current power supply respectively, and carry out electrochemical dissolution of the metal sample to obtain the dissolved metal sample; Step five, after ultrasonic cleaning the dissolved metal sample obtained in step four in ethanol and blowing dry, then weighing, the metal electrochemical dissolution current efficiency of the metal sample is obtained by calculation.

8. A device for measuring the current efficiency of electrochemical dissolution of a metal according to claim 7, characterized in that The calculation uses the following formula: ； In the formula, △m is the mass loss, the unit is g, which is obtained by subtracting the mass in step one from the mass in step five, K is the electrochemical equivalent, the unit is g / C, I is the current of electrochemical dissolution, the unit is A, t is the time of electrochemical dissolution, the unit is min, and η is the metal electrochemical dissolution current efficiency of the metal sample.

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