Iron plating solution, method for preparing same, and electroplating process and application thereof

Abstract

This invention relates to an iron plating solution for manufacturing polishing pad dressing devices, comprising: an oxalic acid complex of ferric ions, a pH buffer, a chloride salt auxiliary reagent, a stress reliever, and a wetting agent; the pH of the iron plating solution is 3.0-3.8. This invention provides a method for preparing the iron plating solution for manufacturing polishing pad dressing devices. This invention provides an electroplating process for the iron plating solution for manufacturing polishing pad dressing devices. This invention also provides a polishing pad dressing device obtained by the electroplating process of the iron plating solution for manufacturing polishing pad dressing devices. The iron plating solution of this invention uses ferric ions as the main salt, and uses ammonium oxalate to complex with ferric ions to form a stable soluble iron salt, eliminating the oxidation problem of commonly used divalent ferric ion main salts in the plating solution, preventing the formation and precipitation of ferric hydroxide, and solving the stability problem of the iron plating solution.

Description

TECHNICAL FIELD

[0001] The present application relates to the field of electroplating, in particular to a plating iron solution, a preparation method thereof, an electroplating process and application. BACKGROUND

[0002] The plating iron process has a wide application in repairing crankshafts, camshafts, transmission shafts and worn, corroded and machined parts. The early chloride plating solution produces a hard and brittle plating iron layer at room temperature, which has poor adhesion to the substrate and large internal stress. The improved high-temperature (85-105℃) chloride direct current plating iron process has been widely used in repairing worn devices. However, the plating solution evaporates a lot in the high-temperature plating process, causing serious environmental pollution, and the plating layer has poor hardness and wear resistance.

[0003] A conditioner is a necessary consumable for chemical mechanical planarization, which functions to condition a polishing pad, including cutting the surface of the polishing pad appropriately to maintain a suitable roughness of the polishing pad surface, and cleaning the swarf in the polishing process to prevent the surface of the polishing pad from glazing, thereby prolonging the service life of the polishing pad and improving the polishing efficiency. The fixation of diamonds in the conditioner includes electroplating, brazing and metal sintering methods. In the process of fixing diamonds in the plating layer by using the electroplating process, manual operations such as sanding and unsanding on the diamonds are involved, and the high-temperature plating iron solution makes these operations extremely difficult, so the high-temperature plating iron process is not suitable for the manufacture of electroplated diamond conditioners.

[0004] Another outstanding problem existing in the current plating iron solution formula and process is that the divalent iron ions in the plating iron solution are easily oxidized into trivalent iron ions. On the one hand, this oxidation reaction reduces the concentration of divalent iron ions in the plating iron solution, causing instability of the composition of the plating iron solution; on the other hand, the trivalent iron ions are easily combined with hydroxyl ions to precipitate in the form of iron hydroxide in the plating iron solution with a pH value higher than 3, and the adsorption of iron hydroxide on the surface of the cathode will cause roughness and deterioration of the mechanical properties of the plating iron layer. In order to solve the key problem of oxidation of divalent iron ions into trivalent iron ions and formation of iron hydroxide precipitate, the current main technical approach is to use slightly higher anti-oxidation ferrous sulfate as the main salt, and use ascorbic acid, hydroxyacetic acid, gluconic acid, ethylenediaminetetraacetic acid, monoethanolamine sulfamic acid, ammonium fluoroborate, ammonium bifluoride, etc. as reducing agents or complexing agents for trivalent iron. Among them, fluorides have good effects, but plating solutions containing fluoride ions are harmful to workers and difficult to treat in electroplating wastewater. Moreover, with the consumption of these reducing agents or complexing agents, the precipitation of iron hydroxide is inevitable even under continuous electroplating conditions. Therefore, the above methods do not fundamentally solve the stability problem of the plating iron solution. SUMMARY

[0005] In order to overcome the shortcomings and deficiencies of the above existing iron plating technology, solve the harm of trivalent iron ions in the divalent iron plating solution to the stability of the iron plating solution and the performance of the plated layer, and the primary purpose of the present application is to provide a stable iron plating solution for manufacturing a polishing pad trimmer. The iron plating solution of the present application can be used to electrodeposit a pure iron plated layer on the base body of the trimmer, and the prepared pure iron plated layer is dense and uniform, has high hardness, good bonding strength with the base body, and easy diamond sanding, thereby solving the problem of unstable plating solution caused by the oxidation of divalent iron ions in the iron plating solution.

[0006] An object of the present application is to solve at least the above problems and to provide at least the advantages to be described later.

[0007] In order to achieve these objects and other advantages according to the present application, an iron plating solution for manufacturing a polishing pad trimmer is provided, comprising: an oxalate complex of trivalent iron ions, a pH buffer, a chlorinated salt auxiliary agent, a stress reliever, and a wetting agent; the pH of the iron plating solution is 3.0-3.8.

[0008] Specifically, the iron concentration in the iron plating solution is 0.3-0.5 mol / L;

[0009] The concentration of the pH buffer is 0.4-0.7 mol / L;

[0010] The concentration of the chlorinated salt auxiliary agent is 0.2-0.7 mol / L;

[0011] The concentration of the stress reliever is 0.01-0.025 mol / L;

[0012] The concentration of the wetting agent is 0.35-1.4 mmol / L.

[0013] Specifically, the oxalate complex of trivalent iron ions is one or more of a complex formed by ammonium ferric oxalate, a complex formed by a soluble trivalent iron salt and ammonium oxalate.

[0014] Specifically, the soluble trivalent iron salt is one or more of ferric chloride, ferric sulfate, and ferric sulfamate.

[0015] Specifically, the molar ratio of the complexing agent to the soluble trivalent iron salt is at least 3.1:1.

[0016] Specifically, the pH buffer is boric acid;

[0017] The chlorinated salt auxiliary agent is one or more of ammonium chloride, manganese chloride, and sodium chloride;

[0018] The stress reliever is one or more of sodium o-benzoylsulfonamide, sodium p-toluenesulfonamide, and sodium p-toluenesulfinate;

[0019] The wetting agent is one or more of sodium dodecyl sulfate and sodium methylene bisnaphthalene sulfonate.

[0020] The application also provides a preparation method of a plating iron solution for manufacturing a polishing pad trimmer, comprising the following steps:

[0021] S1, adding a pH buffer and a chlorinated salt auxiliary agent into deionized water, heating to 60-80 DEG C, stirring until completely dissolved, adjusting the pH to 3 to obtain a first solution;

[0022] S2, adding an oxalate complex of trivalent iron ions into the first solution, stirring until completely dissolved to obtain a second solution;

[0023] S3, adding a stress reliever and a wetting agent into the second solution, then supplementing deionized water to a preset volume, adjusting the pH value range to 3.0-3.8 to obtain a plating iron solution;

[0024] The volume of the deionized water added in step S1 is 2 / 3 of the preset volume.

[0025] The application also provides an electroplating process of a plating iron solution, comprising the following steps: taking the base body of the trimmer as a cathode, taking a pure iron plate as an anode, the electroplating temperature is 30-40 DEG C, the pH of the plating iron solution is 3.0-3.8, the current density is 0.5-2.0 A / dm 2 .

[0026] Specifically, the current waveform can be one of direct current, single pulse current or double pulse current;

[0027] When pulse electroplating is adopted, the duty cycle of the pulse current is 5%-50%, and the peak current is 1.0-4.0 A / dm 2 .

[0028] The application also provides a polishing pad trimmer, the roughness Ra of the plating layer of the trimmer is 0.3-0.5 μm.

[0029] The application at least has the following beneficial effects:

[0030] 1. The plating iron solution adopts trivalent iron ions as a main salt, and ammonium oxalate and trivalent iron ions are combined to form a stable soluble iron salt, so that the oxidation problem of the commonly used divalent iron ion main salt in the plating solution is eliminated, the generation and precipitation of iron hydroxide are prevented, and the stability problem of the plating iron solution is solved;

[0031] 2. By changing the electroplating temperature and current parameters, the surface morphology of the plating iron layer can be adjusted and controlled, the roughness of the trimmer plating layer is controlled, and the obtained pure iron plating layer has strong adhesion with the base body and dense plating layer structure;

[0032] 3. Compared with the plating solution for preventing iron hydroxide from precipitating by using fluoride, fluoroborate and the like, the iron plating solution composition of the present application is more green and environmentally friendly, and the electroplating solution has low cost and simple manufacturing process.

[0033] Other advantages, objects, and features of the present application will be understood by those skilled in the art from the following description, taken in conjunction with the accompanying drawings. BRIEF DESCRIPTION OF DRAWINGS

[0034] Figure 1 Microphotograph of the working surface of the dresser base body after electroplating. DETAILED DESCRIPTION

[0035] The following discussion will focus on specific implementations and examples of the present content. This detailed description is provided to help describe certain embodiments and is not intended to limit or restrict the scope or applicability of the disclosure. It will be appreciated that other embodiments can be used based on the disclosure.

[0036] The terms used in the present application are used only to explain specific embodiments and are not intended to limit the present application.

[0037] Unless defined differently, all terms used herein, including technical or scientific terms, have the same meanings as those commonly understood by those skilled in the art to which the present application pertains. Terms such as terms defined in generally used dictionaries should be interpreted as having meanings consistent with the context in the relevant technology, and should not be interpreted in an ideal or overly formal sense unless explicitly defined in the present application.

[0038] The polishing pad is one of the main consumables in the chemical mechanical polishing system, and the structure and surface roughness of the polishing pad have a great influence on the wafer material removal rate and surface roughness in the CMP process. The chemical mechanical polishing pad dresser can regenerate the polishing pad surface to the best state, correct the shape of the polishing pad, and maintain the wafer polishing rate. The dresser mainly uses diamonds fixed on the base to trim the polishing pad surface. The fixation of diamonds in the dresser includes electroplating method, brazing method, metal sintering method and the like. The present application uses the electroplating method to fix the diamonds on the base of the dresser.

[0039] Electroplating is a process of plating a thin layer of other metal or alloy on the surface of certain metal by using electrolysis, which is a process of attaching a metal film to the surface of a metal or other material part by using electrolysis. In electroplating, the plating layer metal or other insoluble material is used as the anode, and the workpiece to be plated is used as the cathode. The cations of the plating layer metal are reduced on the surface of the workpiece to be plated to form a plating layer. In order to exclude the interference of other cations and make the plating layer uniform and firm, a solution containing the cations of the plating layer metal is used as the electroplating solution to keep the concentration of the cations of the plating layer metal unchanged.

[0040] In the process of iron plating, trivalent iron ions in the iron plating solution with pH value greater than 3 are easily combined with hydroxyl ions to precipitate in the form of iron hydroxide, and the adsorption of iron hydroxide on the surface of the cathode will result in rough surface of the iron plating layer and deterioration of mechanical properties. If the pH value of the iron plating solution is less than 3, the hydrogen evolution side reaction in the electroplating process is serious, and the hydrogen evolved permeates into the plating layer and the substrate to cause hydrogen embrittlement, resulting in poor performance of the plating layer. If the hydrogen evolved stays on the surface of the part in the form of bubbles, it will cause pores and pits in the plating layer.

[0041] <iron plating solution>

[0042] The present application provides an iron plating solution for manufacturing a polishing pad conditioner. In the process of electroplating, elemental iron is precipitated from the iron plating solution to the substrate of the conditioner with a pure iron or carbon steel substrate as the cathode, and holds the diamonds arranged on the substrate. In the embodiment, the specific components of the iron plating solution include: oxalate complexes of trivalent iron ions, pH buffers, chlorinated salt auxiliary reagents, stress relievers, and wetting agents; and the pH of the iron plating solution is 3.0-3.8. The iron plating process is completed under acidic conditions, which can avoid passivation of the iron anode.

[0043] The iron plating solution in the embodiment of the present application uses oxalate complexes of trivalent iron ions. The oxalate complexes of trivalent iron ions are one or more of the complexes formed by ammonium ferric oxalate, soluble trivalent iron salts and ammonium oxalate. The use of high-valence iron ions eliminates the problem of oxidation of the iron plating solution. At the same time, the electroplating solution is stable, and there is no problem of iron hydroxide precipitation.

[0044] The effect of ammonium oxalate in plating is very important. Ammonium oxalate is combined with trivalent iron ions to form ammonium iron oxalate (III) complex, which has very good stability, and can prevent the generation of iron hydroxide precipitate in the iron plating solution with pH greater than 3. The solubility of ferrous oxalate is 0.03g / 100g, and ferrous oxalate is a yellow precipitate in water and is insoluble in water. In the implementation process, no yellow substance was observed, indicating that no ammonium ferrous oxalate precipitate was generated in the iron plating process. Further, after the reduction of trivalent iron to divalent iron on the surface of the cathode, the divalent iron can be quickly reduced to elemental iron. Although citric acid can complex trivalent iron, the complex formed has too large a stability constant, and the iron ion reduction potential is much more negative than that of the oxalate complex, which exacerbates hydrogen evolution and increases the internal stress of the plating layer.

[0045] In the embodiment of the present application, the molar ratio of the ammonium oxalate to the soluble trivalent iron salt is at least 3.1:1, and when the coordination reaction occurs, it can generate trisoxalate iron complex ions [Fe(C2O4)3] 3-Preferably, the molar ratio of the ammonium oxalate to the soluble ferric salt is 3.1-6:1; more preferably, the molar ratio of the ammonium oxalate to the soluble ferric salt is 3.1-5:1.

[0046] The soluble ferric salt in the embodiment of the present application is one or more of ferric chloride, ferric sulfate, and ferric sulfamate, or other soluble ferric salts.

[0047] The iron concentration in the iron plating solution is closely related to the plating speed, and a high concentration requires a large current density and a fast plating speed, while a low concentration results in a slow plating speed. However, a too high concentration will affect the dispersion ability of the plating solution. Therefore, the iron supply mode of the ferric ammonium oxalate (III) complex is adopted in the embodiment, and the iron concentration in the iron plating solution is set to 0.3-0.5 mol / L; preferably, the concentration of the ferric ammonium oxalate is 0.4 mol / L.

[0048] In order to prevent the pH of the iron plating solution from being increased due to the gas (e.g. hydrogen) generated in the iron electroplating operation, affecting the performance of the plated layer. The pH buffer agent plays a great role in the stability of the pH value in the electroplating process. Considering the stability and economy of the iron plating solution, the concentration of the pH buffer agent is 0.4-0.7 mol / L; the pH buffer agent is boric acid, and the content of the boric acid is 24.73-43.28 g / L in terms of mass concentration. Preferably, the concentration of the boric acid is 0.45-0.6 mol / L. More preferably, the concentration of the boric acid is 0.5 mol / L. The pH buffer agent can also be a polyacid having a buffering effect, which does not form a precipitate or complex with the ferric ion.

[0049] The concentration of the chlorinated salt auxiliary agent in the embodiment of the present application is 0.2-0.7 mol / L. Preferably, the concentration of the chlorinated salt auxiliary agent is 0.4-0.7 mol / L. More preferably, the concentration of the chlorinated salt auxiliary agent is 0.5-0.6 mol / L. The chlorinated salt auxiliary agent is one or more of manganese chloride, ammonium chloride, and sodium chloride. The addition of manganese chloride, ammonium chloride, and sodium chloride increases the conductivity of the solution and promotes the anode dissolution. With the increase of the content, the brittleness of the plated layer will increase, and therefore, they should not be added too much.

[0050] Coating internal stress is a kind of balance force caused by stress in the process of metal electrodeposition due to the influence of operating conditions and plating solution composition. Since it is not caused by external force, it is called internal stress. From the micro perspective, the coating internal stress is also the accumulation of abnormal electrodeposition in the process of metal electrodeposition when the metal is far away from the lattice crystallization. When the accumulated micro internal stress reaches a certain value, it will cause the coating to peel off or even crack in the release process. If the force is not enough to destroy the coating and release, it will show internal stress and release when induced, which will show the brittleness of the coating. The concentration of the stress reliever in the embodiment of the application is 0.01-0.025 mol / L; preferably, the concentration of the stress reliever is 0.01-0.02 mol / L; more preferably, the concentration of the stress reliever is 0.015 mol / L. In the electroplating process, the commonly used stress relievers are: naphthalene sulfonic acid, p-toluenesulfonamide, saccharin, etc. The stress reliever in the embodiment of the application is one or more of sodium o-benzoyl sulfonamide, sodium p-toluenesulfonamide and sodium p-toluenesulfinate.

[0051] The most basic requirement of the electroplating wetting agent is to better reduce the interfacial tension between the electrode and the plating solution interface, so that the plating solution can spread on the electrode surface to achieve the purpose of uniform plating, and it has certain salt resistance, acid and alkali resistance and temperature resistance to the plating solution, and makes the coating better adhere to the substrate and reduces the porosity. The wetting agent in the embodiment is one or more of sodium dodecyl sulfate and methylene bis naphthalene sulfonic acid sodium. The concentration of the wetting agent is 0.35-1.4 mmol / L; preferably, the concentration of the wetting agent is 0.35-1.25 mmol / L; preferably, the concentration of the wetting agent is 0.5-1.0 mmol / L; more preferably, the concentration of the wetting agent is 0.5 mmol / L. Most preferably, 1.0 mmol / L of sodium dodecyl sulfate can be used.

[0052] <Preparation method of iron plating solution>

[0053] The application provides a preparation method of an iron plating solution for manufacturing a polishing pad trimmer, which comprises the following steps:

[0054] S1, a pH buffer and a chlorinated salt auxiliary reagent are added to deionized water, heated to 60-80 DEG C, and stirred until completely dissolved, then the pH is adjusted to 3 to obtain a first solution;

[0055] S2, ammonium ferric oxalate and / or soluble trivalent iron salt and ammonium oxalate are added to the first solution, and stirred until completely dissolved to obtain a second solution;

[0056] S3, adding a stress reliever and a wetting agent into the second solution, then supplementing deionized water to a preset volume, adjusting a pH value range to 3.0-3.8, and obtaining a plating iron solution.

[0057] The pH value is adjusted by using dilute sulfuric acid, and if the pH value is adjusted to be low, 5% sodium hydroxide solution can be used to adjust the pH value to be within the range of 3.0-3.8.

[0058] In the embodiment, the volume of the deionized water added in step S1 is 2 / 3 of the preset volume.

[0059] The embodiment of the application adopts a step-by-step adding method, and can prevent the plating iron solution from generating precipitates.

[0060] <Plating process of the plating iron solution>

[0061] The application provides a plating process of a plating iron solution for manufacturing a polishing pad trimmer, which comprises the following steps:

[0062] S1, pre-treatment of an iron or carbon steel base body of the trimmer before plating;

[0063] In the application, the pre-treatment of the base body before plating comprises chemical degreasing, rust removal by dilute hydrochloric acid immersion, electrochemical degreasing, electrochemical activation, and distilled water rinsing, so as to enhance the bonding strength between the plating layer and the base body.

[0064] In the pre-treatment step of the base body before plating, chemical degreasing is firstly performed. The base body is immersed in a degreasing agent or detergent solution and is carefully scrubbed with cotton yarn and sawdust, and then is cleaned with water. If only a local area of the base body needs to be plated, insulation treatment needs to be performed on the non-plating surface. The insulation treatment can be performed in the form of waterproof electrician tape wrapping or insulating paint coating. After insulation, the plating surface needs to be rust-removed, and the base body can be immersed in 10wt% dilute hydrochloric acid for 1-1.5 min.

[0065] After the rust removal of the base body, electrochemical degreasing is performed. The base body subjected to the rust removal treatment is connected to a cathode of a direct current power supply, and a lead plate is connected to an anode and is powered for 2-3 min. Then, the base body is switched to an anode, i.e., the base body is connected to the anode, and the lead plate is connected to the cathode and is powered for 1-2 min, so as to remove the oil film on the plating surface. Finally, the base body is rinsed with clean water. The current density for the degreasing is 3-8 A / dm 2 , and the electrolyte formula is: sodium hydroxide 16-40 g / L, sodium carbonate 30-50 g / L, sodium phosphate 10-20 g / L, and sodium silicate 5-12 g / L.

[0066] After the electrochemical degreasing of the base body, electrochemical activation needs to be performed, so as to ensure the bonding strength between the plating iron layer and the base body. The electrochemical activation uses 25-40% sulfuric acid solution as the electrolyte, the base body subjected to the electrochemical degreasing treatment is connected to an anode of a direct current power supply, and a lead plate is connected to a cathode, and the current is 10-20 A / dm 2The substrate is rinsed with clean water after the current density is activated for 1.5 min.

[0067] S2, the substrate is charged into the iron plating solution after the above-mentioned pre-plating treatment. The substrate is used as a cathode, and a pure iron plate is used as an anode. The plating temperature is 30-40℃, the pH of the iron plating solution is 3.0-3.8, the current density is 0.5-2.0 A / dm 2 .

[0068] Preferably, the pH of the iron plating solution is 3.0-3.8.

[0069] Preferably, the plating temperature of the iron plating solution is kept at 30-35℃.

[0070] Specifically, the current waveform can be one of direct current, single pulse current or double pulse current.

[0071] When pulse plating is used, the duty cycle of the pulse current is 5-50%, and the peak current is 1.0-4.0 A / dm 2 .

[0072] Preferably, the current waveform is pulse current, and the duty cycle is 20%-30%, and the average current density is 0.8-1.2 A / dm 2 .

[0073] After the plating is completed, the diamond tool is rinsed with clean water to remove the residual plating solution on the surface of the diamond tool. If necessary, the diamond tool can be subjected to anti-rust treatment with mineral oil or lubricating grease after being cleaned.

[0074] <Polishing pad conditioner>

[0075] The present application provides a polishing pad conditioner, the roughness Ra of the plating layer of the conditioner is 0.3-0.5 μm. The polishing pad prepared by the plating process of the present application has a flat plating layer, the height of the diamond blade can be better controlled, the damage to the polishing pad is small during cutting, the service life of the polishing pad can be prolonged, and the service life of the polishing pad conditioner can also be prolonged.

[0076] The advantages, features and methods of achieving the present application will be more apparent in light of the embodiments described in detail hereinafter.

[0077] <Example 1>

[0078] An iron plating solution for manufacturing a polishing pad conditioner, the components of which include: 0.4 mol / L of ferric ammonium oxalate, 0.5 mol / L of boric acid, 0.5 mol / L of ammonium chloride, 0.015 mol / L of sodium o-benzoylsulfonamide, and 0.5 mmol / L of sodium dodecyl sulfate; the pH of the iron plating solution is between 3.0 and 3.8.

[0079] <Example 2>

[0080] An iron plating solution for manufacturing a polishing pad conditioner, the composition of which includes: 0.3 mol / L of ferric chloride, 1.0 mol / L of ammonium oxalate, 0.45 mol / L of boric acid, 0.4 mol / L of sodium chloride, 0.01 mol / L of sodium p-toluenesulfonamide, 0.7 mmol / L of sodium methylene bisnaphthalene sulfonate; the pH of the iron plating solution is between 3.0 and 3.8.

[0081] <Example 3>

[0082] An iron plating solution for manufacturing a polishing pad conditioner, the composition of which includes: 0.5 mol / L of ferric sulfate, 1.6 mol / L of ammonium oxalate, 0.6 mol / L of boric acid, 0.6 mol / L of manganese chloride, 0.025 mol / L of sodium p-toluenesulfinate, 1.4 mmol / L of sodium methylene bisnaphthalene sulfonate; the pH of the iron plating solution is between 3.0 and 3.8.

[0083] <Example 4>

[0084] An iron plating solution for manufacturing a polishing pad conditioner, the composition of which includes: 0.45 mol / L of ferric ammonium oxalate, 0.7 mol / L of boric acid, 0.7 mol / L of ammonium chloride, 0.02 mol / L of sodium o-benzoylsulfonamide, 1.0 mmol / L of sodium dodecyl sulfate; the pH of the iron plating solution is between 3.0 and 3.8.

[0085] <Example 5>

[0086] An iron plating solution for manufacturing a polishing pad conditioner, the composition of which includes: 0.35 mol / L of ferric sulfamate, 1.1 mol / L of ammonium oxalate, 0.5 mol / L of boric acid, 0.6 mol / L of sodium chloride, 0.015 mol / L of sodium p-toluenesulfinate, 0.7 mmol / L of sodium methylene bisnaphthalene sulfonate; the pH of the iron plating solution is between 3.0 and 3.8.

[0087] <Example 6>

[0088] An iron plating solution for manufacturing a polishing pad conditioner, the composition of which includes: 0.3 mol / L of ferric sulfate, 1.3 mol / L of ammonium oxalate, 0.4 mol / L of boric acid, 0.3 mol / L of manganese chloride, 0.01 mol / L of sodium p-toluenesulfonamide, 0.35 mmol / L of sodium dodecyl sulfate; the pH of the iron plating solution is between 3.0 and 3.8.

[0089] <Example 7>

[0090] The embodiment provides a preparation method of a plating iron solution for manufacturing a polishing pad conditioner, and the plating iron solution prepared by the preparation method has the component content shown in Table 1. The preparation method comprises the following steps:

[0091] S1, boric acid and ammonium chloride are added into deionized water, heated to 60 DEG C, and stirred until completely dissolved, then diluted sulfuric acid is used to adjust the pH to 3 to obtain a first solution;

[0092] S2, ammonium ferric oxalate is added into the first solution, and stirred until completely dissolved to obtain a second solution;

[0093] S3, sodium o-benzoylsulfonamide and sodium dodecyl sulfate are dissolved and then added into the second solution, and then deionized water is supplemented to a preset volume, and a 5wt% sodium hydroxide solution is used to adjust the pH value in the range of 3.0-3.8 to obtain the plating iron solution.

[0094] The volume of the deionized water added in step S1 is 2 / 3 of the preset volume.

[0095] <Embodiment 8>

[0096] The embodiment provides a preparation method of a plating iron solution for manufacturing a polishing pad conditioner, and the plating iron solution prepared by the preparation method has the component content shown in Table 2. The preparation method comprises the following steps:

[0097] S1, boric acid and sodium chloride are added into deionized water, heated to 70 DEG C, and stirred until completely dissolved, then diluted sulfuric acid is used to adjust the pH to 3 to obtain a first solution;

[0098] S2, ferric chloride and ammonium oxalate are added into the first solution, and stirred until completely dissolved to obtain a second solution;

[0099] S3, sodium p-toluenesulfonamide and sodium methylene bisnaphthalene sulfonate are dissolved and then added into the second solution, and then deionized water is supplemented to a preset volume, and a 5wt% sodium hydroxide solution is used to adjust the pH value in the range of 3.0-3.8 to obtain the plating iron solution.

[0100] The volume of the deionized water added in step S1 is 2 / 3 of the preset volume.

[0101] <Embodiment 9>

[0102] In the embodiment, the electroplating process of the conditioner base body is implemented by using the plating iron solution in Embodiment 1, and the electroplating process comprises the following steps:

[0103] S1, conditioner base body pretreatment, comprising chemical degreasing by using a detergent, rust removal by soaking in dilute hydrochloric acid, electrochemical degreasing, electrochemical activation, and water rinsing.

[0104] S2, the dresser base after the above-mentioned pre-plating treatment, charged into the iron plating solution. The base is used as the cathode, and a pure iron plate is used as the anode. The plating process parameters used are: plating solution temperature, 35°C; pulse current parameters, duty cycle 30%, average current density 1.2 A / dm 2 After the dresser base is electroplated for 20 minutes, sanding is performed using the sand-embedding method; the sand is removed after 1 hour of sand embedding, and then the plating is thickened to embed the diamonds to 70% of the diamond particle size. The electroplated diamond dresser with a pure iron plating layer is obtained after cleaning in the tank. The micrograph of the dresser base after the iron plating and embedding of the diamonds is shown in Figure 1 , and the crystal is fine and the surface is smooth.

[0105] <Example 10>

[0106] The plating process of this example is the same as that of Example 8, except that the dresser base after the above-mentioned pre-plating treatment is charged into the iron plating solution of Example 2. The plating process parameters used are: plating solution temperature, 30°C; pulse current parameters, duty cycle 35%, average current density 1.5 A / dm 2 .

[0107] <Example 11>

[0108] The plating process of this example is the same as that of Example 8, except that the dresser base after the above-mentioned pre-plating treatment is charged into the iron plating solution of Example 3. The plating process parameters used are: plating solution temperature, 40°C; pulse current parameters, duty cycle 25%, average current density 1.0 A / dm 2 .

[0109] <Comparative Example 1>

[0110] This comparative example provides an iron plating solution for manufacturing a dresser for a polishing pad, and the contents of the components in the iron plating solution are as shown in Example 1. The difference is that the pH of the iron plating solution is about 4.5.

[0111] <Comparative Example 2>

[0112] This comparative example provides an iron plating solution for manufacturing a dresser for a polishing pad, and the contents of the components in the iron plating solution are as shown in Example 1. The difference is that the pH of the iron plating solution is about 6.

[0113] <Comparative Example 3>

[0114] The plating process of this comparative example is the same as that of Example 9, except that the plating process parameters used are: plating solution temperature, room temperature; pulse current parameters, duty cycle 30%, average current density 3 A / dm 2 .

[0115] <Comparative Example 4>

[0116] The plating process of the present comparative example is the same as that of Example 9, except that the plating process parameters used are: plating solution temperature, 50°C; pulse current parameters, duty cycle 30%, average current density 3 A / dm 2 .

[0117] <Test Example 1>

[0118] The plating iron solutions of Examples 1-6 and Comparative Examples 1-2 were left to stand at room temperature, and the color and turbidity of the plating iron solutions were observed. The observation results are shown in Table 1.

[0119] Table 1 Stability of plating iron solution

[0120]

[0121]

[0122] As can be seen from Table 1, the plating iron solutions of Examples 1-6 were stable, and there was no phenomenon of generation of iron hydroxide precipitate. As can be seen from the comparison between Example 1 and Comparative Examples 1-2, the pH of the plating iron solution affects the generation of precipitate.

[0123] <Test Example 2>

[0124] The roughness Ra, Rz of the dresser working surface coating layer of Examples 9-11 and Comparative Examples 3-4 was measured using a VK-X3000 from KEYENCE, under the conditions of objective 20x, and the test results are shown in Table 2.

[0125] Table 2 Roughness of dresser working surface

[0126] Number Ra / μm Rz / μm Example 9 0.423 4.267 Example 10 0.468 4.984 Example 11 0.325 3.725 Comparative Example 3 0.712 6.799 Comparative Example 4 0.557 5.632

[0127] In Table 2, the roughness of Examples 9-11 shows that the dresser surface prepared using the plating process of the present application is smooth.

[0128] As can be seen from the comparison between Example 9 and Comparative Examples 3-4, a plating solution temperature that is too high or too low has an effect on the roughness of the dresser surface.

[0129] Although embodiments of the present application have been disclosed as above, it is not limited only to the use listed in the specification and embodiments, and it can be fully applied to various fields suitable for the present application, and further modifications can be easily made by those skilled in the art, and therefore the present application is not limited to specific details and the examples shown and described herein, without departing from the general concept defined by the claims and the equivalent scope.

Claims

1. A plating solution for manufacturing polishing pad dressers, characterized in that, include: Oxalic acid complexes of ferric ions, pH buffers, chloride salt auxiliary reagents, stress relievers, wetting agents; The pH of the iron plating solution is 3.0-3.8; The oxalate complex of the ferric ion is one or more of the following: a complex formed from ammonium ferric oxalate, a complex formed from soluble ferric salts and ammonium oxalate; the chloride salt auxiliary reagent is one or more of the following: ammonium chloride, manganese chloride, and sodium chloride; the stress reliever is one or more of the following: sodium o-benzoylsulfonylimide, sodium p-toluenesulfonamide, and sodium p-toluenesulfinate; and the wetting agent is one or more of the following: sodium dodecyl sulfate and sodium methylene bisnaphthalenesulfonate.

2. The iron plating solution for manufacturing a polishing pad dresser as described in claim 1, characterized in that, The iron concentration in the plating solution is 0.3-0.5 mol / L; The concentration of the pH buffer is 0.4-0.7 mol / L; The concentration of the chloride salt auxiliary reagent is 0.2-0.7 mol / L; The concentration of the stress reliever is 0.01-0.025 mol / L; The concentration of the wetting agent is 0.35-1.4 mmol / L.

3. The iron plating solution for manufacturing a polishing pad dresser as described in claim 1, characterized in that, The soluble ferric salt is one or more of ferric chloride, ferric sulfate, and ferric aminosulfonate.

4. The iron plating solution for manufacturing a polishing pad dresser as described in claim 1 or 3, characterized in that, The molar ratio of ammonium oxalate to the soluble ferric salt is at least 3.1:

1.

5. The iron plating solution for manufacturing a polishing pad dresser as described in claim 1, characterized in that, The pH buffer is boric acid.

6. The method for preparing the iron plating solution for manufacturing a polishing pad dresser as described in any one of claims 1 to 5, characterized in that, Includes the following steps: S1. Add pH buffer and chloride salt auxiliary reagent to deionized water, heat to 60-80℃, stir until completely dissolved, and adjust pH to 3 to obtain the first solution; S2. Add the oxalic acid complex of ferric ions to the first solution and stir until completely dissolved to obtain the second solution; S3. Add stress reliever and wetting agent to the second solution, then add deionized water to the preset volume, and adjust the pH value to 3.0-3.8 to obtain the iron plating solution; The volume of deionized water added in step S1 is 2 / 3 of the preset volume.

7. An electroplating process for the iron plating solution as described in any one of claims 1 to 5 or the iron plating solution prepared by the preparation method as described in claim 6, characterized in that, Includes the following steps: Using the substrate of the plating device as the cathode and a pure iron plate as the anode, the electroplating temperature is 30-40℃, the pH of the iron plating solution is 3.0-3.8, and the current density is 0.5-2.0 A / dm³. 2 .

8. The electroplating process as described in claim 7, characterized in that, The current waveform is one of direct current, single-pulse current, or double-pulse current. When pulse electroplating is used, the duty cycle of the pulse current is 5%-50%, and the peak current is 1.0-4.0 A / dm. 2 .

9. A polishing pad dresser, prepared by the electroplating process as described in claim 7, wherein the roughness Ra of the coating of the dresser is 0.3-0.5 μm.

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