CN114293242B - Polishing solution for side duplex silver-copper composite electrolytic polishing and electrolytic polishing method - Google Patents
Polishing solution for side duplex silver-copper composite electrolytic polishing and electrolytic polishing method Download PDFInfo
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- CN114293242B CN114293242B CN202210010381.6A CN202210010381A CN114293242B CN 114293242 B CN114293242 B CN 114293242B CN 202210010381 A CN202210010381 A CN 202210010381A CN 114293242 B CN114293242 B CN 114293242B
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- C25F3/00—Electrolytic etching or polishing
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Abstract
The invention relates to polishing solution for side duplex silver-copper composite belt electrolytic polishing and an electrolytic polishing method, and belongs to the technical field of electrolytic polishing. The polishing solution for side duplex silver-copper composite belt electrolytic polishing comprises the following components in percentage by mass: 5 to 8 percent of citric acid, 3 to 5 percent of sulfamic acid, 0.5 to 1 percent of sodium chloride, 0.2 to 0.5 percent of urea and the balance of water. When the polishing solution for electrolytic polishing of the side compound silver-copper composite belt is adopted for electrolytic polishing of the side compound silver-copper composite belt, the surface of the treated electrolytic polishing side compound silver-copper composite belt can be ensured to have smaller roughness, and the loss of noble metal can be avoided.
Description
Technical Field
The invention relates to polishing solution for side duplex silver-copper composite belt electrolytic polishing and an electrolytic polishing method, and belongs to the technical field of electrolytic polishing.
Background
As a substitute material of the pure silver belt, the side duplex silver-copper composite belt is a novel composite material currently applied to the manufacture of melt materials in low-voltage fuses, and can well save silver materials and reduce cost by replacing silver with copper, and has good electrical performance. Along with the development of industries such as electric power, metallurgy, chemical industry, petrochemical industry and the like, the side duplex silver-copper composite belt is rapidly developed.
However, the copper material part used for compounding in the silver-copper compound belt is extremely easy to oxidize in the production circulation and intermediate storage process to cause the surface quality to be reduced, and the adverse effect is generated on the subsequent cold rolling and annealing procedures, and meanwhile, the surface finish of the final finished product is influenced and the electrical performance of the product is influenced. Therefore, the silver-copper composite belt needs to be subjected to surface treatment, and a common surface treatment process is mechanical polishing and grinding after pickling, so that the process is complicated, environmental pollution is easy to cause, and the occupational health of operators is endangered.
The electrolytic polishing is a special anode electrochemical machining mode, in the process, a polished workpiece is used as an anode, insoluble metal is used as a cathode, and the effects of removing scratches, burrs and the like on the surface of a workpiece are achieved through electrochemical anode dissolution, so that the surface of the workpiece is smooth and bright. However, when the surface treatment is carried out by adopting the traditional mechanical polishing method or the polishing solution of the traditional components, the pure silver part in the composite belt is softer, the mechanical polishing abrasion consumption is higher, the reaction speed of silver and the medium-strength inorganic acid such as nitric acid, phosphoric acid and the like is higher, and the loss of noble metal is easy to cause.
Disclosure of Invention
The invention aims to provide polishing solution for electrolytic polishing of side duplex silver-copper composite strips, which is used for solving the problem of larger noble metal loss when the conventional inorganic medium-strong acid polishing solution is adopted for electrolytic polishing of the side duplex silver-copper composite strips at present.
Another object of the present invention is to provide a method for electropolishing a side-duplex silver-copper composite strip.
In order to achieve the above purpose, the technical scheme adopted by the polishing solution for side duplex silver-copper composite electrolytic polishing of the invention is as follows:
the polishing solution for side duplex silver-copper composite electrolytic polishing consists of the following components in percentage by mass: 5 to 8 percent of citric acid, 3 to 5 percent of sulfamic acid, 0.5 to 1 percent of sodium chloride, 0.2 to 0.5 percent of urea and the balance of water.
The polishing solution for side duplex silver-copper composite electrolytic polishing has a good electrolytic polishing effect. Wherein, the citric acid has the function of providing ions for the electrolyte, the sulfamic acid has the function of adjusting the ion concentration, the sodium chloride has the functions of improving the stripping speed and the strip smoothness, and the urea has the function of adjusting acid and alkali; when the raw materials are combined, the method has the beneficial effects of improving the synergistic effect of the electrolyte in the electrolyte and reducing the energy consumption. When the polishing solution for electrolytic polishing of the side compound silver-copper composite belt is adopted for electrolytic polishing of the side compound silver-copper composite belt, the surface of the treated electrolytic polishing side compound silver-copper composite belt can be ensured to have smaller roughness, and the loss of noble metal can be avoided.
In order to avoid corrosion of the metal under the oxide layer by the polishing solution and reduce the thickness of the side compound silver-copper compound belt, the polishing solution for the side compound silver-copper compound belt is preferably composed of the following components in percentage by mass: 5 to 7 percent of citric acid, 3 to 4.5 percent of sulfamic acid, 0.5 to 0.75 percent of sodium chloride, 0.2 to 0.4 percent of urea and the balance of water.
In order to improve the flatness and reduce the roughness of the surface of the side duplex silver-copper composite belt, the polishing solution for the side duplex silver-copper composite belt electrolytic polishing is preferably composed of the following components in percentage by mass: 6.5 to 7 percent of citric acid, 4 to 4.5 percent of sulfamic acid, 0.75 percent of sodium chloride, 0.35 to 0.4 percent of urea and the balance of water.
The electrolytic polishing method of the side duplex silver-copper composite belt adopts the following technical scheme:
an electrolytic polishing method of a side duplex silver-copper composite belt comprises the following steps: immersing the side compound silver-copper composite belt into polishing solution for electrolytic polishing, and cleaning and drying the side compound silver-copper composite belt after the polishing solution is discharged; the polishing solution is the polishing solution for side duplex silver-copper composite electrolytic polishing; in the electrolytic polishing process, the temperature of the polishing solution is 35-45 ℃ and the current density is 6-8 mA/cm 2 The method comprises the steps of carrying out a first treatment on the surface of the The electrolytic polishing time is 2-3 min.
The electrolytic polishing method of the side compound silver-copper composite belt avoids dust pollution generated by traditional mechanical polishing, improves the production efficiency, improves the surface quality of products, and provides guarantee for occupational safety and health of operators. The side compound silver-copper composite belt after electrolytic polishing has the advantages of bright and smooth surface and smaller roughness.
In order to facilitate adjustment of current density and electrolysis rate in the electrolytic polishing process, the temperature of the polishing solution is controlled to be 35-45 ℃. Further preferably, in the electrolytic polishing, the temperature of the polishing liquid is 40 ℃.
The electrolytic polishing time is 2-3 min, so that the oxide layer on the surface of the side compound silver-copper composite belt can be effectively removed, and corrosion of acid liquor to a metal layer below the oxide layer can be avoided, and the thickness of the side compound silver-copper composite belt is reduced.
In the present invention, the current density means the current intensity (a) distributed over the anode per unit area in the electrolytic polishing. The current density is controlled to be 6-8 mA/cm in the electrolytic polishing process 2 The electrolytic rates of the silver strip part and the copper strip part in the side compound silver-copper compound belt in electrolytic polishing can be made to be consistent.
Preferably, in the electrolytic polishing, the DC power supply voltage is set to 25 to 30V.
Preferably, in the electrolytic polishing, the cathode is a nickel plate; the distance between the cathode and the anode is 10-15 cm. For example, the cathode-anode spacing is 10cm. Preferably, in the electrolytic polishing, the width of the nickel plate is 2 times of the width of the lateral compound silver-copper compound belt and is symmetrically arranged in the width direction.
Preferably, the side compound silver-copper compound is carried out of the polishing solution, sequentially enters water for ultrasonic cleaning, enters alcohol for cleaning, and is dried. The residual electrolyte and other impurities on the surface of the side duplex silver-copper composite belt can be removed by ultrasonic cleaning with water. The alcohol can be used for carrying out water and oil removal cleaning on the side duplex silver-copper composite belt.
Drawings
FIG. 1 is a schematic view of a polishing apparatus used in the electrolytic polishing method of the side duplex silver-copper composite tape of example 5; wherein, the reference numerals are as follows: the device comprises a 1-electrolytic cell, a 2-polishing solution, a 3-cathode nickel plate, a 4-anode guide wheel, a 5-insulating guide wheel, a 6-liquid storage tank, a 7-liquid guide pipe, an 8-circulating pump, a 9-controller, a 10-anticorrosion thermocouple and an 11-heating coil.
Detailed Description
The technical scheme of the invention is further described below with reference to specific embodiments.
1. The specific examples of the polishing solution for side duplex silver-copper composite electrolytic polishing of the invention are as follows:
example 1
The polishing solution for side duplex silver-copper composite belt electrolytic polishing in the embodiment comprises the following components in percentage by mass: 5% of citric acid, 3% of sulfamic acid, 0.5% of sodium chloride, 0.2% of urea and the balance of water.
Example 2
The polishing solution for side duplex silver-copper composite belt electrolytic polishing in the embodiment comprises the following components in percentage by mass: 6.5% of citric acid, 4% of sulfamic acid, 0.75% of sodium chloride, 0.35% of urea and the balance of water.
Example 3
The polishing solution for side duplex silver-copper composite belt electrolytic polishing in the embodiment comprises the following components in percentage by mass: 8% of citric acid, 5% of sulfamic acid, 1% of sodium chloride, 0.5% of urea and the balance of water.
Example 4
The polishing solution for side duplex silver-copper composite belt electrolytic polishing in the embodiment comprises the following components in percentage by mass: 7% of citric acid, 4.5% of sulfamic acid, 0.75% of sodium chloride, 0.4% of urea and the balance of water.
Comparative example 1
The polishing solution for side duplex silver-copper composite belt electrolytic polishing of the comparative example comprises the following components in percentage by mass: 7% of citric acid, 4.5% of sulfamic acid, 0.4% of urea and the balance of water.
Comparative example 2
The polishing solution for side duplex silver-copper composite belt electrolytic polishing of the comparative example comprises the following components in percentage by mass: 7% of citric acid, 4.5% of sulfamic acid, 0.75% of sodium chloride and the balance of water.
Comparative example 3
The polishing solution for side duplex silver-copper composite belt electrolytic polishing of the comparative example comprises the following components in percentage by mass: 4% of citric acid, 2.5% of sulfamic acid, 0.5% of sodium chloride, 0.2% of urea and the balance of water.
Comparative example 4
The polishing solution for side duplex silver-copper composite belt electrolytic polishing of the comparative example comprises the following components in percentage by mass: 10% of citric acid, 6% of sulfamic acid, 1% of sodium chloride, 0.5% of urea and the balance of water.
Comparative example 5
The polishing solution for side duplex silver-copper composite belt electrolytic polishing of the comparative example comprises the following components in percentage by mass: 4% of nitric acid, 2.5% of sulfamic acid, 0.5% of sodium chloride, 0.2% of urea and the balance of water.
Comparative example 6
The polishing solution for side duplex silver-copper composite belt electrolytic polishing of the comparative example comprises the following components in percentage by mass: 4% of nitric acid, 2.5% of phosphoric acid, 0.5% of sodium chloride, 0.2% of urea and the balance of water.
2. The specific embodiment of the electrolytic polishing method of the side duplex silver-copper composite belt is as follows:
example 5
The polishing equipment adopted by the electrolytic polishing method of the side compound silver-copper composite belt in the embodiment is shown in fig. 1, and comprises an electrolytic cell 1, wherein the electrolytic cell 1 is used for containing polishing liquid 2 in use, anode guide wheel assemblies are respectively arranged on two sides of the electrolytic cell 1, each anode guide wheel assembly comprises two oppositely arranged anode guide wheels 4, the anode guide wheels are anode graphite guide wheels, and the anode guide wheels 4 are connected with a direct current power supply in use. A channel is formed between two anode guide wheels 4 in the same anode guide wheel assembly, and a side compound silver-copper composite belt passes through during electrolytic polishing. During electrolytic polishing, the side compound silver-copper composite belt enters between the two anode guide wheels 4 and penetrates out of the other two anode guide wheels 4 after electrolytic polishing, and the side compound silver-copper composite belt is in contact with the anode guide wheels 4 to conduct electricity, so that the side compound silver-copper composite belt forms an anode.
The bottom and the intermediate position of the electrolytic cell 1 are respectively fixed with cathode plates, wherein the cathode plates are cathode nickel plates 3, the two cathode nickel plates 3 are arranged along the up-down direction and are arranged in parallel, and during electrolytic polishing, the two cathode nickel plates 3 are all positioned below the liquid level (the dotted line in fig. 1) of the electrolyte 2. When the double-sided silver-copper composite belt is used, the middle of the two cathode nickel plates 3 is penetrated, the distance between the double-sided silver-copper composite belt and the two cathode nickel plates 3 is equal, the width of the cathode nickel plates 3 is 2 times of the width of the double-sided silver-copper composite belt, and the double-sided silver-copper composite belt is symmetrically placed in the width direction, so that the electrolytic polishing effect of the two sides of the double-sided silver-copper composite belt is consistent. In order to guide the side compound silver-copper composite belt to the position below the liquid level (broken line in fig. 1) of the electrolyte 2 and keep the side compound silver-copper composite belt at the position with equal distance from the two cathode nickel plates 3, as shown in fig. 1, insulating guide wheels 5 are arranged at each anode guide wheel assembly, the insulating guide wheels 5 are made of insulating materials, the lower edge of the insulating guide wheels 5 is immersed below the liquid level (broken line in fig. 1) of the electrolyte 2 when in use, the side compound silver-copper composite belt can be guided into the electrolyte 2, and the mirror surfaces between the lower edge of the insulating guide wheels 5 and the two cathode nickel plates 3 are positioned on the same plane, so that the side compound silver-copper composite belt can be kept at the position with equal distance from the two cathode nickel plates 3.
The lower part of the electrolytic cell 1 is also provided with a liquid storage tank 6, the liquid storage tank 6 is used for storing polishing liquid, a liquid guide pipe 7 is connected between the liquid storage tank 6 and the electrolytic cell 1, the liquid guide pipe 7 is an acid-resistant pipe, a circulating pump 8 is arranged on the liquid guide pipe 7, and the circulating flow of the polishing liquid 2 in the electrolytic cell 1 and the liquid storage tank 6 is realized in the electrolytic polishing process. In order to control the temperature of the polishing solution 2, the electrolytic polishing device further comprises a temperature control system, the temperature control system comprises a heating coil 11 arranged in the liquid storage tank 6, the heating coil 11 is a teflon acid and alkali resistant heating coil, and the heating coil 11 is connected with a heating power supply; the device also comprises a corrosion-resistant thermocouple 10 arranged in the electrolytic cell 1, wherein the corrosion-resistant thermocouple 10 is sleeved outside the corrosion-resistant thermocouple 10, and the corrosion-resistant thermocouple 10 can measure the temperature of the polishing solution 2 in the electrolytic cell 1. The temperature control system further comprises a controller 9, wherein the controller 9 can collect the temperature value of the anti-corrosion thermocouple 10 and determine whether the heating power supply is started or not and the current according to the temperature value, so that the polishing solution 2 in the electrolytic cell 1 is kept at the set temperature.
The electrolytic polishing method of the side compound silver-copper composite belt of the embodiment comprises the following steps:
(1) The side duplex silver-copper composite belt is used as an anode, a nickel plate is used as a cathode, the distance between the cathode and the anode is 10cm,the side compound silver-copper compound belt passes through the anode guide wheel and then is guided into polishing solution in the electrolytic cell through the insulating guide wheel to pass through the middle of the two cathode nickel plates, and then is guided into the anode guide wheel through the insulating guide wheel to obtain polishing solution; setting the DC power supply voltage to 25V and the current density to 6mA/cm in the process 2 And controlling the temperature of the polishing solution to be 40 ℃, and simultaneously controlling the advancing speed of the side compound silver-copper composite belt in the polishing solution to be 0.6m/min, so that the electrolytic polishing time of the side compound silver-copper composite belt in the polishing solution is 3min. The polishing liquid used for the electrolytic polishing was the polishing liquid for the side duplex silver-copper composite belt electrolytic polishing of example 4.
(2) After the side compound silver-copper compound is brought out of the polishing solution, the polishing solution is firstly put into water for ultrasonic cleaning, then put into alcohol for water and oil removal cleaning, and finally the surface is dried by air drying equipment.
Example 6
The electrolytic polishing method of the side duplex silver-copper composite tape of this embodiment differs from that of embodiment 7 only in that in the electrolytic polishing process, the DC power supply voltage is set to 27V, and the current density is 7mA/cm 2 。
Example 7
The electrolytic polishing method of the side duplex silver-copper composite tape of this embodiment differs from that of embodiment 7 only in that in the electrolytic polishing process, the DC power supply voltage is set to 27V, and the current density is 7mA/cm 2 The advancing speed of the side compound silver-copper composite belt in the polishing solution is controlled to be 0.8m/min, so that the electrolytic polishing time of the side compound silver-copper composite belt in the polishing solution is 2.5min.
Example 8
The electrolytic polishing method of the side duplex silver-copper composite tape of this embodiment differs from that of embodiment 7 only in that in the electrolytic polishing process, the DC power supply voltage is set to be 30V, and the current density is set to be 8mA/cm 2 The advancing speed of the side compound silver-copper composite belt in the polishing solution is controlled to be 1.0m/min, so that the electrolytic polishing time of the side compound silver-copper composite belt in the polishing solution is 2min.
Comparative example 7
The electrolytic polishing method of the side double silver-copper composite tape of the present comparative example was different from example 8 only in that the traveling speed of the side double silver-copper composite tape in the polishing liquid was controlled to be 2m/min during the electrolytic polishing, so that the time of electrolytic polishing of the side double silver-copper composite tape in the polishing liquid was 1min.
Comparative example 8
The electrolytic polishing method of the side double silver-copper composite tape of the present comparative example was different from example 8 only in that the traveling speed of the side double silver-copper composite tape in the polishing liquid was controlled to be 0.2m/min during the electrolytic polishing, so that the time of electrolytic polishing of the side double silver-copper composite tape in the polishing liquid was 10min.
Experimental example 1
In order to examine the influence of the process parameters adopted in the electrolytic polishing on the polishing of the side double silver-copper composite tape, the same batch of side double silver-copper composite tape was subjected to electrolytic polishing treatment by the electrolytic polishing methods of examples 5 to 8 and comparative examples 7 to 8, respectively (the polishing solutions used in the electrolytic polishing treatment process were the polishing solutions for electrolytic polishing of the side double silver-copper composite tape of example 4), to obtain the test sample of the side double silver-copper composite tape subjected to electrolytic polishing treatment. The surface appearance of the test specimen was observed again, and then the surface roughness of the test specimen was measured by a surface roughness meter, and the test results are shown in table 1.
TABLE 1 surface appearance and surface roughness of side double silver-copper composite strips after electropolishing treatment by electropolishing method of side double silver-copper composite strips of examples 5-8 and comparative examples 7-8
Note that: negligible means that the thickness reduction is less than 0.002mm, ra representing the arithmetic mean of the absolute value of the profile offset within the sampling length L; rz represents the sum of the average of 5 largest profile peak heights and the average of 5 largest profile valley depths over the sample length.
As can be seen from table 1, the electrolytic polishing effect of the side duplex silver-copper composite tape is affected by various factors such as current density and electrolytic time. The electrolytic polishing method of the side compound silver-copper composite belt of the embodiment 8 adopts higher current density, which causes slight corrosion on the surface of the copper strip and slightly reduces the thickness of the side compound silver-copper composite belt; the electrolytic polishing method of the side compound silver-copper composite belt of the comparative example 7 has the advantages that the electrolytic polishing time is short, and the polishing effect is not ideal; the electrolytic polishing method of the side compound silver-copper composite belt of comparative example 8 adopts a longer electrolytic polishing time, so that the copper bar is corroded. Therefore, when the current density is high and the electrolysis time is long, corrosion of the metal substrate is liable to occur.
Experimental example 2
The same batch of side compound silver-copper composite belts are subjected to electrolytic polishing treatment by adopting polishing solutions of examples 1-4 and comparative examples 1-6 according to an electrolytic polishing method of the side compound silver-copper composite belt of example 6, so as to obtain an electrolytic polishing treated side compound silver-copper composite belt test sample. The surface appearance of the test specimen was observed again, and then the surface roughness of the test specimen was measured by a surface roughness meter, and the test results are shown in table 1.
TABLE 2 surface appearance and surface roughness of side Duplex silver-copper composite strips treated by electropolishing with the polishing solutions of examples 1-4 and comparative examples 1-2
Note that: negligible means that the thickness reduction is less than 0.002mm, ra representing the arithmetic mean of the absolute value of the profile offset within the sampling length L; rz represents the sum of the average of 5 largest profile peak heights and the average of 5 largest profile valley depths over the sample length.
As is clear from Table 2, the polishing solutions of comparative examples 1 and 2 had low ion concentrations, resulting in unsatisfactory polishing effects, since sodium chloride or urea was not added; the polishing solution of comparative example 3 has lower concentrations of citric acid and sulfamic acid, and the polishing effect is not ideal; the polishing solution in the comparative example 4 has higher concentration of citric acid and sulfamic acid, and has ideal polishing effect, but the thickness of the lateral compound silver-copper composite belt is slightly reduced; because of the strong acidity of nitric acid and phosphoric acid, copper strips in the lateral compound silver-copper composite belt can be corroded when the polishing solution of comparative examples 4-5 is adopted for electrolytic polishing.
Claims (5)
1. The polishing solution for side duplex silver-copper composite electrolytic polishing is characterized by comprising the following components in percentage by mass: 5 to 8 percent of citric acid, 3 to 5 percent of sulfamic acid, 0.5 to 1 percent of sodium chloride, 0.2 to 0.5 percent of urea and the balance of water.
2. The polishing solution for side duplex silver-copper composite electrolytic polishing as claimed in claim 1, which is characterized by comprising the following components in percentage by mass: 5 to 7 percent of citric acid, 3 to 4.5 percent of sulfamic acid, 0.5 to 0.75 percent of sodium chloride, 0.2 to 0.4 percent of urea and the balance of water.
3. The polishing solution for side duplex silver-copper composite electrolytic polishing as claimed in claim 2, which is characterized by comprising the following components in percentage by mass: 6.5 to 7 percent of citric acid, 4 to 4.5 percent of sulfamic acid, 0.75 percent of sodium chloride, 0.35 to 0.4 percent of urea and the balance of water.
4. The electrolytic polishing method of the side duplex silver-copper composite belt is characterized by comprising the following steps of: immersing the side compound silver-copper composite belt into polishing solution for electrolytic polishing, and cleaning and drying the side compound silver-copper composite belt after the polishing solution is discharged; the polishing solution is the polishing solution for side duplex silver-copper composite electrolytic polishing according to any one of claims 1 to 3; in the electrolytic polishing process, the temperature of the polishing solution is 35-45 ℃ and the current density is 6-8 mA/cm 2 The method comprises the steps of carrying out a first treatment on the surface of the The electrolytic polishing time is 2-3 min.
5. The electropolishing method of side-duplex silver-copper composite tape of claim 4, wherein during electropolishing, the cathode is a nickel plate; the distance between the cathode and the anode is 10-15 cm.
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