Method for rapidly preparing electroplated diamond fretsaw

Abstract

The invention belongs to the technical field of superhard material products, and particularly discloses a method for quickly preparing an electroplated diamond fretsaw, which comprises the following steps of: firstly, carrying out surface nickel plating on diamond micro powder with the granularity of 22-36 microns by using a pre-prepared chemical plating solution, and then carrying out oil removal, erosion, drying and magnetization treatment on a metal matrix, thereby obtaining the electroplated diamond fretsaw. The method comprises the steps that firstly, a metal substrate is placed in a prepared electroplating bath containing cobalt sulfate hexahydrate and 1, 4-butynediol, current of 5 A / dm < 2 > is introduced, preplating is conducted for 2 min, then sand feeding and nickel plating are conducted on the metal substrate, current of 5 A / dm < 2 > is introduced in the sand feeding and nickel plating link, sand feeding is conducted for 30 s, the current density is increased to 14 A / dm < 2 >, thickening treatment is conducted for 10 min, and finally packaging is conducted after drying and quality inspection. The electroplating efficiency of the diamond fretsaw can be effectively improved.

Description

Technical Field

[0001] This invention belongs to the field of superhard material products technology, specifically a method for rapidly preparing electroplated diamond wire saws. Background Technology

[0002] With the large-scale development and utilization of clean energy globally, the photovoltaic industry has experienced rapid growth. Human demand for the smelting and processing of monocrystalline and polycrystalline silicon, key components for photoelectric conversion, is increasing. Electroplated diamond wire saws have seen significant development due to their advantages in cutting precious, hard, and brittle materials such as monocrystalline silicon and sapphire, including narrow kerfs, low wear, and high processing efficiency. However, the manufacturing process of wire saws has always suffered from drawbacks such as low electroplating efficiency and high production costs. Firstly, research should be conducted on the effects of various components and additives in the plating solution on current limits, current efficiency, and coating performance, aiming to obtain a plating solution with the maximum allowable current density while ensuring optimal performance and quality. Secondly, the parameters of the preparation process, especially the abrasive coating process, should be studied to achieve the highest preparation efficiency and performance. Currently, the cutting performance of diamond wire saws on the market is not ideal. Although it can be improved by controlling parameters such as cutting direction, feed rate, and wire speed, the distribution of abrasive cannot be well controlled.

[0003] For example, Chinese invention patent application CN109290970A discloses an electroplated diamond abrasive belt with mixed abrasive particles, comprising a metal substrate, a metal coating on the metal substrate, and diamond abrasive particles embedded in the metal coating. The metal coating includes a thin nickel layer disposed on the metal substrate and a thickened metal layer covering the thin nickel layer. The diamond abrasive particles include coarse and fine abrasive particles uniformly distributed in the metal coating, with the particle size relationship between the coarse and fine abrasive particles being y≤x≤7y / 5, where x represents the particle size of the larger abrasive particle and y represents the particle size of the smaller abrasive particle. The embedding depth of the coating into the fine diamond abrasive particles is 50%–70% of the particle size. However, in the technical solution provided by this invention, the current is controlled at 0.3–0.8 A / dm during the pre-nickel plating stage. 2 The time is 30-50 minutes; during the nickel plating process, the flux is 0.2-0.6 A / dm. 2 The current is maintained for 15-60 minutes; during the thickening nickel plating process, the current is controlled at 0.3-0.8 A / dm. 2 The thickening time is no less than 1 hour; the maximum current density of this technical solution in the entire preparation process is 2A / dm³. 2 Furthermore, the preparation process is time-consuming. Summary of the Invention

[0004] To address the shortcomings of existing technologies, this invention provides a method for rapidly preparing electroplated diamond wire saws, thus solving the problems mentioned in the background section.

[0005] The technical solution of this invention is as follows:

[0006] As a technical solution of the present invention, the present invention provides a method for rapidly preparing electroplated diamond wire saws, comprising the following steps:

[0007] Step S1: Electroless nickel plating on the surface of diamond micro powder. After pretreatment, diamond micro powder with a particle size of 22-36μm is electroless nickel plating on the surface using a pre-prepared electroless plating solution.

[0008] Step S2: Metal substrate treatment. After the metal substrate is degreased with organic solvent, degreased with electrochemical solvent, subjected to strong etching, weak etching and drying, it is magnetized with a metal substrate magnetization device.

[0009] Step S3: Pre-plating the metal substrate with nickel. Using the metal substrate treated in step S2 as the cathode and the nickel block as the anode, after connecting the wires, place it in an electroplating tank containing a prepared electroplating solution containing cobalt sulfate hexahydrate and 1,4-butynediol, and introduce 5A / dm³ of flux. 2 The current is applied for pre-plating for 2 minutes;

[0010] Step S4, Abrasive Plating: The metal substrate pre-plated with nickel in Step S3 is placed into the electroplating solution containing the abrasive plating tank. Diamond micro powder treated in Step S1 is applied at a mass concentration of 15-20 g / L, and a flow rate of 5 A / dm³ is introduced. 2 The current was applied, the sand was applied for 30 seconds, the temperature of the electroplating solution was kept at 45℃, and the mixture was stirred at a stirring speed of 100r / min.

[0011] Step S5: Thickening. After completing step S5, the current density is increased to 14 A / dm. 2 Thickening treatment for 10 minutes;

[0012] Step S6: After heat-treating the metal substrate treated in step S5 at 180°C for 2 hours, it is dried, inspected, and then packaged.

[0013] Furthermore, the chemical plating solution in step S1 is prepared from nickel sulfate hexahydrate with a concentration of 25 g / L, sodium hypophosphite with a concentration of 25-35 g / L, ammonia with a concentration of 15-35 ml / L, lactic acid with a concentration of 10-20 ml / L, sodium acetate with a concentration of 15 g / L, and thiourea with a concentration of 20 mg / L.

[0014] Furthermore, the preparation process of the chemical plating solution is as follows:

[0015] First, weigh out the following raw materials according to the following concentrations: 25 g / L nickel sulfate hexahydrate, 25-35 g / L sodium hypophosphite, 15-35 ml / L ammonia, 10-20 ml / L lactic acid, 15 g / L sodium acetate, and 20 mg / L thiourea.

[0016] Next, dissolve the weighed sodium acetate, nickel sulfate, thiourea and sodium hypophosphite in an appropriate amount of deionized water to obtain the first solution;

[0017] Then, while stirring the first solution, lactic acid, nickel sulfate, thiourea, ammonia, and sodium hypophosphite solution were added in sequence, and after continuous stirring, a light blue chemical plating solution was obtained.

[0018] Furthermore, the electroplating solution is prepared from nickel aminosulfonate (300-500 g / L), cobalt sulfate hexahydrate (15-30 g / L), nickel chloride (20-30 g / L), boric acid (30-40 g / L), saccharin (0-1 g / L), 1,4-butynediol (0-1 g / L), and sodium dodecyl sulfate (0-0.2 g / L) at a mass concentration of 300-500 g / L.

[0019] Furthermore, the preparation process of the electroplating solution is as follows:

[0020] Step S41: Weigh the following raw materials according to their mass concentrations: 300-500 g / L nickel aminosulfonate, 15-30 g / L cobalt sulfate hexahydrate, 20-30 g / L nickel chloride, 30-40 g / L boric acid, 0-1 g / L saccharin, 0-1 g / L 1,4-butynediol and 0-0.2 g / L sodium dodecyl sulfate;

[0021] Step S42: Dissolve the nickel aminosulfonate and cobalt sulfate hexahydrate weighed in step S41 separately in deionized water. After the nickel aminosulfonate and cobalt sulfate hexahydrate are fully dissolved, pour them into the electroplating tank.

[0022] Step S43: Dissolve the boric acid weighed in step S41 in heated deionized water, then add the dissolved boric acid to the electroplating tank while stirring the liquid in the electroplating tank.

[0023] Step S44: Mix the sodium dodecyl sulfate weighed in step S41 with deionized water to form a paste, then add 100 times the mass of the sodium dodecyl sulfate paste to deionized water and boil until the sodium dodecyl sulfate is completely dissolved. Then add the solution to the electroplating tank while stirring the liquid in the electroplating tank.

[0024] Step S45: Add the plating solution obtained in step S44 to a certain volume using deionized water, and finally add the saccharin and 1,4-butynediol that have been fully dissolved in hot deionized water according to step S41 to obtain the prepared electroplating solution.

[0025] The organic solvent in step S2 is alcohol;

[0026] The intense etching process involves placing the metal substrate in 15% sulfuric acid, using the metal substrate as both the anode and cathode sequentially, and then introducing a 5A / dm³ flow. 2The current is applied for 1 minute when the metal substrate is used as the anode and for 3 minutes when the metal substrate is used as the cathode.

[0027] The weak etching process involves placing the metal substrate in 5% sulfuric acid, using the metal substrate as the anode, and then introducing a 5A / dm³ flow. 2 The current was applied for 1 minute.

[0028] Furthermore, the diamond micron powder pretreatment process in step S1 is as follows:

[0029] Step S71, surface degreasing: Diamond micro powder with a particle size of 22-36μm is boiled in 10% NaOH solution for 0.5h to remove surface oil.

[0030] Step S72, roughening treatment: After completing step S71, the diamond micro powder is boiled in a 30% nitric acid solution for 0.5 hours for roughening treatment.

[0031] Step S73, Sensitization treatment: After completing step S72, the diamond micro powder is placed in a sensitization solution containing 16 g / L stannous chloride and sensitized at 60°C for 0.5 h.

[0032] Step S74, activation treatment: After completing step S73, the diamond micro powder is placed in an activation solution containing 0.4 g / L palladium chloride and activated at 60°C for 0.5 h.

[0033] Step S75, reduction: After completing step S74, the diamond micro powder is placed in a reducing solution containing 6 g / L sodium hypophosphite and reduced at room temperature for 15 min.

[0034] As one technical solution of the present invention, the present invention provides a rapid preparation of an electroplating solution for electroplating diamond wire saws. The electroplating solution is prepared from nickel aminosulfonate (300-500 g / L), cobalt sulfate hexahydrate (15-30 g / L), nickel chloride (20-30 g / L), boric acid (30-40 g / L), saccharin (0-1 g / L), 1,4-butynediol (0-1 g / L), and sodium dodecyl sulfate (0-0.2 g / L).

[0035] As one technical solution of the present invention, the present invention provides a chemical plating solution for electroless nickel plating on the surface of diamond micro powder. The chemical plating solution is prepared from nickel sulfate hexahydrate with a concentration of 25 g / L, sodium hypophosphite with a concentration of 25-35 g / L, ammonia with a concentration of 15-35 ml / L, lactic acid with a concentration of 10-20 ml / L, sodium acetate with a concentration of 15 g / L and thiourea with a concentration of 20 mg / L.

[0036] Beneficial effects

[0037] 1. Compared with existing technologies, the beneficial effects of the method for rapidly preparing electroplated diamond wire saws provided by this invention are as follows:

[0038] 1) The method for rapid preparation of electroplated diamond wire saws provided by this invention involves applying a current density of 5 A / dm during the electroplating of metallic nickel. 2 With the current, the pre-plating nickel time is only 2 minutes, the sand plating nickel time is only 30 seconds, and the thickening nickel plating time is only 10 minutes, which effectively shortens the nickel plating time of the metal substrate and can effectively improve the efficiency of pre-plating nickel, sand plating nickel and thickening nickel plating of the metal substrate.

[0039] 2) The method for rapidly preparing electroplated diamond wire saws provided by this invention can effectively prevent the formation of nickel ions and precipitate by adding a pre-prepared chemical plating solution during the chemical nickel plating process on the surface of diamond micro powder, which can improve the speed of chemical nickel plating on the surface of diamond micro powder to a certain extent.

[0040] 3) The rapid preparation method for electroplated diamond wire saws provided by this invention utilizes an electroplating solution that significantly improves the mechanical properties of the final diamond wire saw during the pre-plating, abrasive plating, and thickening of the nickel plating process on the metal substrate, while ensuring a current density of 5 A / dm³. 2 High current is used for rapid nickel plating.

[0041] 2. Compared with existing technologies, the beneficial effects of the rapid preparation of electroplating solution for electroplated diamond wire saws provided by this invention are as follows:

[0042] 1) The electroplating solution for rapidly preparing electroplated diamond wire saws provided in this invention contains cobalt sulfate hexahydrate, which itself acts as a luminescent agent. Furthermore, by controlling the concentration of cobalt sulfate hexahydrate at 15-30 g / L, the hardness and brittleness of the nickel plating layer can be effectively improved.

[0043] 2) The electroplating solution for rapidly preparing electroplated diamond wire saws provided in this invention contains 1,4-butynediol, which can appropriately increase the polarization of the cathode and refine the crystals, thereby improving the performance of the coating and making it smooth and wear-resistant. The concentration of 1,4-butynediol has a great influence on the hardness, tensile strength, bonding ability with the substrate, and wear of the coating. When the mass fraction of 1,4-butynediol is 0.3 g / L, the nickel coating has the best bonding ability with the metal substrate, and the coating microhardness is the highest at 427 MPa.

[0044] 3) The rapid preparation solution for electroplating diamond wire saws provided in this invention can achieve an applied current density of 5 A / dm². 2 The high current ensures rapid nickel plating on the surface of the metal substrate.

[0045] 3. Compared with the prior art, the chemical plating solution for electroless nickel plating on the surface of diamond micropowder provided by the present invention has the following beneficial effects:

[0046] 1) The chemical plating solution of the present invention contains 15-35 ml / L of ammonia water, which can effectively improve the efficiency of nickel plating on the surface of diamond micro powder; when the concentration of ammonia water is greater than or equal to 15 ml / L, it can significantly improve the efficiency of chemical nickel plating on the surface of diamond micro powder, and as the concentration of ammonia water increases, the speed of chemical nickel plating on the surface of diamond micro powder continuously increases.

[0047] 2) The ammonia in the chemical plating solution provided in this invention can form a complex with nickel ions in the chemical plating solution, thereby effectively preventing nickel ions from precipitating, ensuring the degree of free nickel ions in the chemical plating solution, and thus improving the efficiency of chemical nickel plating on the surface of diamond micro powder to a certain extent.

[0048] 3) The ammonia water in the chemical plating solution provided in this invention has weak alkalinity and can adjust the pH value of the plating solution. The concentration of hydrogen ions in the plating solution decreases as the alkalinity increases, and the reducing power of H2PO2- is improved, thus improving the plating efficiency. Attached Figure Description

[0049] Figure 1 The current limits of the electroplating solutions in Examples 1-3 at different temperatures are shown. Detailed Implementation

[0050] The technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings of the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments.

[0051] Example 1

[0052] A method for rapidly preparing electroplated diamond wire saws includes the following steps:

[0053] Step S1: Electroless nickel plating on the surface of diamond micro powder. After pretreatment, diamond micro powder with a particle size of 22-36μm is electroless nickel plating on the surface using a pre-prepared electroless plating solution.

[0054] Step S2: Metal substrate treatment. After the metal substrate is degreased with organic solvent, degreased with electrochemical solvent, subjected to strong etching, weak etching and drying, it is magnetized with a metal substrate magnetization device.

[0055] Step S3: Pre-plating the metal substrate with nickel. Using the metal substrate treated in step S2 as the cathode and the nickel block as the anode, after connecting the wires, place it in an electroplating tank containing a prepared electroplating solution containing cobalt sulfate hexahydrate and 1,4-butynediol, and introduce 5A / dm³ of flux. 2 The current is applied for pre-plating for 2 minutes;

[0056] Step S4, Abrasive Plating: The metal substrate pre-plated with nickel in Step S3 is placed into the electroplating solution containing the abrasive plating tank. Diamond micro powder treated in Step S1 is applied at a mass concentration of 15 g / L, and a flow rate of 5 A / dm³ is introduced. 2 The current was applied, the sand was applied for 30 seconds, the temperature of the electroplating solution was kept at 45℃, and the mixture was stirred at a stirring speed of 100r / min.

[0057] Step S5: Thickening. After completing step S5, the current density is increased to 14 A / dm. 2 Thickening treatment for 10 minutes;

[0058] Step S6: After heat-treating the metal substrate treated in step S5 at 180°C for 2 hours, it is dried, inspected, and then packaged.

[0059] In this embodiment, the chemical plating solution in step S1 is prepared from nickel sulfate hexahydrate with a concentration of 25 g / L, sodium hypophosphite with a concentration of 25 g / L, ammonia with a concentration of 35 ml / L, lactic acid with a concentration of 10 ml / L, sodium acetate with a concentration of 15 g / L, and thiourea with a concentration of 20 mg / L.

[0060] In this embodiment, the preparation process of the chemical plating solution is as follows:

[0061] First, weigh out the following raw materials according to the following concentrations: 25 g / L nickel sulfate hexahydrate, 25 g / L sodium hypophosphite, 35 ml / L ammonia, 10 ml / L lactic acid, 15 g / L sodium acetate, and 20 mg / L sodium acetate.

[0062] Next, dissolve the weighed sodium acetate, nickel sulfate, thiourea and sodium hypophosphite in an appropriate amount of deionized water to obtain the first solution;

[0063] Then, while stirring the first solution, lactic acid, nickel sulfate, thiourea, ammonia, and sodium hypophosphite solution were added in sequence, and after continuous stirring, a light blue chemical plating solution was obtained.

[0064] In this embodiment, the electroplating solution is prepared from nickel aminosulfonate (300 g / L), cobalt sulfate hexahydrate (15 g / L), nickel chloride (20 g / L), boric acid (40 g / L), saccharin (0.3 g / L), 1,4-butynediol (0.5 g / L), and sodium dodecyl sulfate (0.1 g / L).

[0065] In this embodiment, the preparation process of the electroplating solution is as follows:

[0066] Step S41: Weigh the following raw materials according to their mass concentrations: 300 g / L nickel aminosulfonate, 15 g / L cobalt sulfate hexahydrate, 20 g / L nickel chloride, 40 g / L boric acid, 0.3 g / L saccharin, 0.5 g / L 1,4-butynediol and 0.1 g / L sodium dodecyl sulfate.

[0067] Step S42: Dissolve the nickel aminosulfonate and cobalt sulfate hexahydrate weighed in step S41 separately in deionized water. After the nickel aminosulfonate and cobalt sulfate hexahydrate are fully dissolved, pour them into the electroplating tank.

[0068] Step S43: Dissolve the boric acid weighed in step S41 in heated deionized water, then add the dissolved boric acid to the electroplating tank while stirring the liquid in the electroplating tank.

[0069] Step S44: Mix the sodium dodecyl sulfate weighed in step S41 with deionized water to form a paste, then add 100 times the mass of the sodium dodecyl sulfate paste to deionized water and boil until the sodium dodecyl sulfate is completely dissolved. Then add the solution to the electroplating tank while stirring the liquid in the electroplating tank.

[0070] Step S45: Add the plating solution obtained in step S44 to a certain volume using deionized water, and finally add the saccharin and 1,4-butynediol that have been fully dissolved in hot deionized water according to step S41 to obtain the prepared electroplating solution.

[0071] The organic solvent in step S2 is alcohol;

[0072] The intense etching process involves placing the metal substrate in 15% sulfuric acid, using the metal substrate as both the anode and cathode sequentially, and then introducing a 5A / dm³ flow. 2 The current is applied for 1 minute when the metal substrate is used as the anode and for 3 minutes when the metal substrate is used as the cathode.

[0073] The weak etching process involves placing the metal substrate in 5% sulfuric acid, using the metal substrate as the anode, and then introducing a 5A / dm³ flow. 2 The current was applied for 1 minute.

[0074] In this embodiment, the diamond micro powder pretreatment process in step S1 is as follows:

[0075] Step S71, surface degreasing: Diamond micro powder with a particle size of 22-36μm is boiled in 10% NaOH solution for 0.5h to remove surface oil.

[0076] Step S72, roughening treatment: After completing step S71, the diamond micro powder is boiled in a 30% nitric acid solution for 0.5 hours for roughening treatment.

[0077] Step S73, Sensitization treatment: After completing step S72, the diamond micro powder is placed in a sensitization solution containing 16 g / L stannous chloride and sensitized at 60°C for 0.5 h.

[0078] Step S74, activation treatment: After completing step S73, the diamond micro powder is placed in an activation solution containing 0.4 g / L palladium chloride and activated at 60°C for 0.5 h.

[0079] Step S75, reduction: After completing step S74, the diamond micro powder is placed in a reducing solution containing 6 g / L sodium hypophosphite and reduced at room temperature for 15 min.

[0080] Example 2

[0081] A method for rapidly preparing electroplated diamond wire saws includes the following steps:

[0082] Step S1: Electroless nickel plating on the surface of diamond micro powder. After pretreatment, diamond micro powder with a particle size of 22-36μm is electroless nickel plating on the surface using a pre-prepared electroless plating solution.

[0083] Step S2: Metal substrate treatment. After the metal substrate is degreased with organic solvent, degreased with electrochemical solvent, subjected to strong etching, weak etching and drying, it is magnetized with a metal substrate magnetization device.

[0084] Step S3: Pre-plating the metal substrate with nickel. Using the metal substrate treated in step S2 as the cathode and the nickel block as the anode, after connecting the wires, place it in an electroplating tank containing a prepared electroplating solution containing cobalt sulfate hexahydrate and 1,4-butynediol, and introduce 5A / dm³ of flux. 2 The current is applied for pre-plating for 2 minutes;

[0085] Step S4, Abrasive Plating: The metal substrate, after pre-plating nickel in Step S3, is placed into the electroplating solution containing the abrasive plating tank. Diamond micro powder treated in Step S1 is applied at a concentration of 20 g / L, and a flow rate of 5 A / dm³ is introduced. 2 The current was applied, the sand was applied for 30 seconds, the temperature of the electroplating solution was kept at 45℃, and the mixture was stirred at a stirring speed of 100r / min.

[0086] Step S5: Thickening. After completing step S5, the current density is increased to 14 A / dm. 2 Thickening treatment for 10 minutes;

[0087] Step S6: After heat-treating the metal substrate treated in step S5 at 180°C for 2 hours, it is dried, inspected, and then packaged.

[0088] In this embodiment, the chemical plating solution in step S1 is prepared from nickel sulfate hexahydrate with a concentration of 25 g / L, sodium hypophosphite with a concentration of 30 g / L, ammonia with a concentration of 15 ml / L, lactic acid with a concentration of 20 ml / L, sodium acetate with a concentration of 15 g / L, and thiourea with a concentration of 20 mg / L.

[0089] In this embodiment, the preparation process of the chemical plating solution is as follows:

[0090] First, weigh out the following raw materials according to the following concentrations: 25 g / L nickel sulfate hexahydrate, 30 g / L sodium hypophosphite, 15 ml / L ammonia, 20 ml / L lactic acid, 15 g / L sodium acetate, and 20 mg / L thiourea.

[0091] Next, dissolve the weighed sodium acetate, nickel sulfate, thiourea and sodium hypophosphite in an appropriate amount of deionized water to obtain the first solution;

[0092] Then, while stirring the first solution, lactic acid, nickel sulfate, thiourea, ammonia, and sodium hypophosphite solution were added in sequence, and after continuous stirring, a light blue chemical plating solution was obtained.

[0093] In this embodiment, the electroplating solution is prepared from nickel aminosulfonate (400 g / L), cobalt sulfate hexahydrate (30 g / L), nickel chloride (25 g / L), boric acid (30 g / L), saccharin (1 g / L), 1,4-butynediol (0.8 g / L), and sodium dodecyl sulfate (0.2 g / L).

[0094] In this embodiment, the preparation process of the electroplating solution is as follows:

[0095] Step S41: Weigh the following raw materials according to their mass concentrations: 400 g / L nickel aminosulfonate, 30 g / L cobalt sulfate hexahydrate, 25 g / L nickel chloride, 30 g / L boric acid, 1 g / L saccharin, 0.8 g / L 1,4-butynediol and 0.2 g / L sodium dodecyl sulfate.

[0096] Step S42: Dissolve the nickel aminosulfonate and cobalt sulfate hexahydrate weighed in step S41 separately in deionized water. After the nickel aminosulfonate and cobalt sulfate hexahydrate are fully dissolved, pour them into the electroplating tank.

[0097] Step S43: Dissolve the boric acid weighed in step S41 in heated deionized water, then add the dissolved boric acid to the electroplating tank while stirring the liquid in the electroplating tank.

[0098] Step S44: Mix the sodium dodecyl sulfate weighed in step S41 with deionized water to form a paste, then add 100 times the mass of the sodium dodecyl sulfate paste to deionized water and boil until the sodium dodecyl sulfate is completely dissolved. Then add the solution to the electroplating tank while stirring the liquid in the electroplating tank.

[0099] Step S45: Add the plating solution obtained in step S44 to a certain volume using deionized water, and finally add the saccharin and 1,4-butynediol that have been fully dissolved in hot deionized water according to step S41 to obtain the prepared electroplating solution.

[0100] The organic solvent in step S2 is alcohol;

[0101] The intense etching process involves placing the metal substrate in 15% sulfuric acid, using the metal substrate as both the anode and cathode sequentially, and then introducing a 5A / dm³ flow. 2 The current is applied for 1 minute when the metal substrate is used as the anode and for 3 minutes when the metal substrate is used as the cathode.

[0102] The weak etching process involves placing the metal substrate in 5% sulfuric acid, using the metal substrate as the anode, and then introducing a 5A / dm³ flow. 2 The current was applied for 1 minute.

[0103] In this embodiment, the diamond micro powder pretreatment process in step S1 is as follows:

[0104] Step S71, surface degreasing: Diamond micro powder with a particle size of 22-36μm is boiled in 10% NaOH solution for 0.5h to remove surface oil.

[0105] Step S72, roughening treatment: After completing step S71, the diamond micro powder is boiled in a 30% nitric acid solution for 0.5 hours for roughening treatment.

[0106] Step S73, Sensitization treatment: After completing step S72, the diamond micro powder is placed in a sensitization solution containing 16 g / L stannous chloride and sensitized at 60°C for 0.5 h.

[0107] Step S74, activation treatment: After completing step S73, the diamond micro powder is placed in an activation solution containing 0.4 g / L palladium chloride and activated at 60°C for 0.5 h.

[0108] Step S75, reduction: After completing step S74, the diamond micro powder is placed in a reducing solution containing 6 g / L sodium hypophosphite and reduced at room temperature for 15 min.

[0109] Example 3

[0110] A method for rapidly preparing electroplated diamond wire saws includes the following steps:

[0111] Step S1: Electroless nickel plating on the surface of diamond micro powder. After pretreatment, diamond micro powder with a particle size of 22-36μm is electroless nickel plating on the surface using a pre-prepared electroless plating solution.

[0112] Step S2: Metal substrate treatment. After the metal substrate is degreased with organic solvent, degreased with electrochemical solvent, subjected to strong etching, weak etching and drying, it is magnetized with a metal substrate magnetization device.

[0113] Step S3: Pre-plating the metal substrate with nickel. Using the metal substrate treated in step S2 as the cathode and the nickel block as the anode, after connecting the wires, place it in an electroplating tank containing a prepared electroplating solution containing cobalt sulfate hexahydrate and 1,4-butynediol, and introduce 5A / dm³ of flux. 2 The current is applied for pre-plating for 2 minutes;

[0114] Step S4, Abrasive Plating: The metal substrate pre-plated with nickel in Step S3 is placed into the electroplating solution containing the abrasive plating tank. Diamond micro powder treated in Step S1 is applied at a mass concentration of 15-20 g / L, and a flow rate of 5 A / dm³ is introduced. 2 The current was applied, the sand was applied for 30 seconds, the temperature of the electroplating solution was kept at 45℃, and the mixture was stirred at a stirring speed of 100r / min.

[0115] Step S5: Thickening. After completing step S5, the current density is increased to 14 A / dm. 2 Thickening treatment for 10 minutes;

[0116] Step S6: After heat-treating the metal substrate treated in step S5 at 180°C for 2 hours, it is dried, inspected, and then packaged.

[0117] In this embodiment, the chemical plating solution in step S1 is prepared from nickel sulfate hexahydrate with a concentration of 25 g / L, sodium hypophosphite with a concentration of 35 g / L, ammonia with a concentration of 30 ml / L, lactic acid with a concentration of 15 ml / L, sodium acetate with a concentration of 15 g / L, and thiourea with a concentration of 20 mg / L.

[0118] In this embodiment, the preparation process of the chemical plating solution is as follows:

[0119] First, weigh out the following raw materials according to the following concentrations: 25 g / L nickel sulfate hexahydrate, 35 g / L sodium hypophosphite, 30 ml / L ammonia, 15 ml / L lactic acid, 15 g / L sodium acetate, and 20 mg / L thiourea.

[0120] Next, dissolve the weighed sodium acetate, nickel sulfate, thiourea and sodium hypophosphite in an appropriate amount of deionized water to obtain the first solution;

[0121] Then, while stirring the first solution, lactic acid, nickel sulfate, thiourea, ammonia, and sodium hypophosphite solution were added in sequence, and after continuous stirring, a light blue chemical plating solution was obtained.

[0122] In this embodiment, the electroplating solution is prepared from nickel aminosulfonate (500 g / L), cobalt sulfate hexahydrate (20 g / L), nickel chloride (25 g / L), boric acid (35 g / L), saccharin (0.2 g / L), 1,4-butynediol (0.3 g / L), and sodium dodecyl sulfate (0.1 g / L).

[0123] In this embodiment, the preparation process of the electroplating solution is as follows:

[0124] Step S41: Weigh the following raw materials according to their mass concentrations: 500 g / L nickel aminosulfonate, 20 g / L cobalt sulfate hexahydrate, 25 g / L nickel chloride, 35 g / L boric acid, 0.2 g / L saccharin, 0.3 g / L 1,4-butynediol and 0.1 g / L sodium dodecyl sulfate.

[0125] Step S42: Dissolve the nickel aminosulfonate and cobalt sulfate hexahydrate weighed in step S41 separately in deionized water. After the nickel aminosulfonate and cobalt sulfate hexahydrate are fully dissolved, pour them into the electroplating tank.

[0126] Step S43: Dissolve the boric acid weighed in step S41 in heated deionized water, then add the dissolved boric acid to the electroplating tank while stirring the liquid in the electroplating tank.

[0127] Step S44: Mix the sodium dodecyl sulfate weighed in step S41 with deionized water to form a paste, then add 100 times the mass of the sodium dodecyl sulfate paste to deionized water and boil until the sodium dodecyl sulfate is completely dissolved. Then add the solution to the electroplating tank while stirring the liquid in the electroplating tank.

[0128] Step S45: Add the plating solution obtained in step S44 to a certain volume using deionized water, and finally add the saccharin and 1,4-butynediol that have been fully dissolved in hot deionized water according to step S41 to obtain the prepared electroplating solution.

[0129] The organic solvent in step S2 is alcohol;

[0130] The intense etching process involves placing the metal substrate in 15% sulfuric acid, using the metal substrate as both the anode and cathode sequentially, and then introducing a 5A / dm³ flow. 2 The current is applied for 1 minute when the metal substrate is used as the anode and for 3 minutes when the metal substrate is used as the cathode.

[0131] The weak etching process involves placing the metal substrate in 5% sulfuric acid, using the metal substrate as the anode, and then introducing a 5A / dm³ flow. 2 The current was applied for 1 minute.

[0132] In this embodiment, the diamond micro powder pretreatment process in step S1 is as follows:

[0133] Step S71, surface degreasing: Diamond micro powder with a particle size of 22-36μm is boiled in 10% NaOH solution for 0.5h to remove surface oil.

[0134] Step S72, roughening treatment: After completing step S71, the diamond micro powder is boiled in a 30% nitric acid solution for 0.5 hours for roughening treatment.

[0135] Step S73, Sensitization treatment: After completing step S72, the diamond micro powder is placed in a sensitization solution containing 16 g / L stannous chloride and sensitized at 60°C for 0.5 h.

[0136] Step S74, activation treatment: After completing step S73, the diamond micro powder is placed in an activation solution containing 0.4 g / L palladium chloride and activated at 60°C for 0.5 h.

[0137] Step S75, reduction: After completing step S74, the diamond micro powder is placed in a reducing solution containing 6 g / L sodium hypophosphite and reduced at room temperature for 15 min.

[0138] The current limit of each electroplating solution prepared in Examples 1 to 3 was tested at different temperatures, and the results are as follows: Figure 1 As shown, the minimum current limit of the electroplating solution provided by this invention is 5A / dm. 2 As the temperature increases, the current limit of the electroplating solution continuously increases. Therefore, the method for rapidly preparing electroplated diamond wire saws provided by this invention can pass a large current to achieve rapid nickel plating of diamond wire saws.

[0139] In addition, the present invention provides a method for rapidly preparing electroplated diamond wire saws, wherein the pre-plating current is 5A / dm in the pre-plating nickel stage. 2 The pre-plating time is 2 minutes, during which a layer of metallic nickel is pre-plated onto the substrate surface to facilitate the subsequent sandblasting process. In the post-treatment stage, the electroplating bath temperature is maintained at 180°C, effectively eliminating defects such as hydrogen embrittlement generated during wire saw manufacturing. Furthermore, through the flow of the plating bath, the movement of the diamond itself, and the attraction of the substrate to the nickel-plated diamond, the nickel-plated diamond is adsorbed onto the substrate and firmly bonded to it through continuous nickel deposition. In the thickening nickel plating stage, the current is controlled at 14 A / dm². 2 The thickening time is 10 minutes, which allows for the rapid deposition of metallic nickel on the substrate and diamond surface, further increasing the bonding ability of the coating to the diamond.

[0140] The above description is only a preferred embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any equivalent substitutions or modifications made by those skilled in the art within the scope of the technology disclosed in the present invention, based on the technical solution and inventive concept of the present invention, should be covered within the scope of protection of the present invention.

Claims

1. A method for rapidly preparing electroplated diamond wire saws, characterized in that, Includes the following steps: Step S1: Electroless nickel plating on the surface of diamond micro powder. After pretreatment, diamond micro powder with a particle size of 22-36μm is electroless nickel plating on the surface using a pre-prepared electroless plating solution. Step S2: Metal substrate treatment. After the metal substrate is degreased with organic solvent, degreased with electrochemical solvent, subjected to strong etching, weak etching and drying, it is magnetized with a metal substrate magnetization device. Step S3: Pre-plating of nickel on the metal substrate. The metal substrate treated in step S2 is used as the cathode and the nickel block is used as the anode. After connecting the wires, it is placed in an electroplating tank containing a prepared electroplating solution containing cobalt sulfate hexahydrate and 1,4-butynediol. A current of 5A / dm2 is passed through for pre-plating for 2 minutes. Step S4, Abrasive Plating: The metal substrate pre-plated with nickel in Step S3 is placed into the electroplating solution containing the abrasive plating tank. Diamond micro powder treated in Step S1 is applied at a mass concentration of 15-20 g / L, and a flow rate of 5 A / dm³ is introduced. 2 The current was applied, the sand was applied for 30 seconds, the temperature of the electroplating solution was kept at 45℃, and the mixture was stirred at a stirring speed of 100r / min. Step S5: Thickening. After completing step S5, the current density is increased to 14 A / dm. 2 Thickening treatment for 10 minutes; Step S6: After heat-treating the metal substrate treated in step S5 at 180°C for 2 hours, it is dried, inspected, and then packaged.

2. The method for rapidly preparing electroplated diamond wire saws according to claim 1, characterized in that: The chemical plating solution in step S1 is prepared from nickel sulfate hexahydrate with a concentration of 25 g / L, sodium hypophosphite with a concentration of 25-35 g / L, ammonia with a concentration of 15-35 ml / L, lactic acid with a concentration of 10-20 ml / L, sodium acetate with a concentration of 15 g / L, and thiourea with a concentration of 20 mg / L.

3. The method for rapidly preparing electroplated diamond wire saws according to claim 2, characterized in that, The preparation process of the chemical plating solution is as follows: First, weigh out the following raw materials according to the following concentrations: 25 g / L nickel sulfate hexahydrate, 25-35 g / L sodium hypophosphite, 15-35 ml / L ammonia, 10-20 ml / L lactic acid, 15 g / L sodium acetate, and 20 mg / L thiourea. Next, dissolve the weighed sodium acetate, nickel sulfate, thiourea and sodium hypophosphite in an appropriate amount of deionized water to obtain the first solution; Then, while stirring the first solution, lactic acid, nickel sulfate, thiourea, ammonia, and sodium hypophosphite solution were added in sequence, and after continuous stirring, a light blue chemical plating solution was obtained.

4. The method for rapidly preparing electroplated diamond wire saws according to claim 1, characterized in that: The electroplating solution is prepared from nickel aminosulfonate (300-500 g / L), cobalt sulfate hexahydrate (15-30 g / L), nickel chloride (20-30 g / L), boric acid (30-40 g / L), saccharin (0-1 g / L), 1,4-butynediol (0-1 g / L), and sodium dodecyl sulfate (0-0.2 g / L).

5. The method for rapidly preparing electroplated diamond wire saws according to claim 4, characterized in that, The preparation process of the electroplating solution is as follows: Step S41: Weigh the following raw materials according to their mass concentrations: 300-500 g / L nickel aminosulfonate, 15-30 g / L cobalt sulfate hexahydrate, 20-30 g / L nickel chloride, 30-40 g / L boric acid, 0-1 g / L saccharin, 0-1 g / L 1,4-butynediol and 0-0.2 g / L sodium dodecyl sulfate; Step S42: Dissolve the nickel aminosulfonate and cobalt sulfate hexahydrate weighed in step S41 separately in deionized water. After the nickel aminosulfonate and cobalt sulfate hexahydrate are fully dissolved, pour them into the electroplating tank. Step S43: Dissolve the boric acid weighed in step S41 in heated deionized water, then add the dissolved boric acid to the electroplating tank while stirring the liquid in the electroplating tank. Step S44: Mix the sodium dodecyl sulfate weighed in step S41 with deionized water to form a paste, then add 100 times the mass of the sodium dodecyl sulfate paste to deionized water and boil until the sodium dodecyl sulfate is completely dissolved. Then add the solution to the electroplating tank while stirring the liquid in the electroplating tank. Step S45: Add the plating solution obtained in step S44 to a certain volume using deionized water, and finally add the saccharin and 1,4-butynediol that have been fully dissolved in hot deionized water according to step S41 to obtain the prepared electroplating solution.

6. The method for rapidly preparing electroplated diamond wire saws according to claim 1, characterized in that: The organic solvent in step S2 is alcohol; The intense etching process involves placing the metal substrate in 15% sulfuric acid, using the metal substrate as both the anode and cathode sequentially, and then introducing a 5A / dm³ flow. 2 The current is applied for 1 minute when the metal substrate is used as the anode and for 3 minutes when the metal substrate is used as the cathode. The weak etching process involves placing the metal substrate in 5% sulfuric acid, using the metal substrate as the anode, and then introducing a 5A / dm³ flow. 2 The current was applied for 1 minute.

7. The method for rapidly preparing electroplated diamond wire saws according to claim 1, characterized in that, The diamond micro powder pretreatment process in step S1 is as follows: Step S71, surface degreasing: Diamond micro powder with a particle size of 22-36μm is boiled in 10% NaOH solution for 0.5h to remove surface oil. Step S72, roughening treatment: After completing step S71, the diamond micro powder is boiled in a 30% nitric acid solution for 0.5 hours for roughening treatment. Step S73, Sensitization treatment: After completing step S72, the diamond micro powder is placed in a sensitization solution containing 16 g / L stannous chloride and sensitized at 60°C for 0.5 h. Step S74, activation treatment: After completing step S73, the diamond micro powder is placed in an activation solution containing 0.4 g / L palladium chloride and activated at 60°C for 0.5 h. Step S75, reduction: After completing step S74, the diamond micro powder is placed in a reducing solution containing 6 g / L sodium hypophosphite and reduced at room temperature for 15 min.

8. A rapid preparation solution for electroplating diamond wire saws, characterized in that: The electroplating solution is prepared from nickel aminosulfonate (300-500 g / L), cobalt sulfate hexahydrate (15-30 g / L), nickel chloride (20-30 g / L), boric acid (30-40 g / L), saccharin (0-1 g / L), 1,4-butynediol (0-1 g / L), and sodium dodecyl sulfate (0-0.2 g / L).

9. A chemical plating solution for electroless nickel plating on the surface of diamond micropowder, characterized in that: The electroless plating solution is prepared from nickel sulfate hexahydrate with a concentration of 25 g / L, sodium hypophosphite with a concentration of 25-35 g / L, ammonia with a concentration of 15-35 ml / L, lactic acid with a concentration of 10-20 ml / L, sodium acetate with a concentration of 15 g / L, and thiourea with a concentration of 20 mg / L.

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