Environment-friendly high-performance titanium alloy polishing composition as well as preparation method and application thereof

Abstract

The invention discloses an environment-friendly high-performance titanium alloy polishing composition as well as a preparation method and application thereof, and relates to the technical field of metal material surface treatment. According to the environment-friendly high-performance titanium alloy polishing composition, the pH value of a basic system is adjusted to 9.5-10.0 through a pH adjusting agent; the base system comprises the following components in percentage by mass: 10-30% of silica sol, 3-4% of an anti-gel stabilizer (urea or methylurea), 2-3% of a heat transfer improvement and surface defect inhibitor (ethylene glycol or propylene glycol), 0.1-0.2% of a wetting leveling agent, 1-2% of an alcohol amine complexing agent and 0.5-1% of an aminopolycarboxylic acid chelating agent besides water. According to the environment-friendly high-performance titanium alloy polishing composition, on the premise that an oxidizing agent is completely abandoned, perfect balance of high stability, high polishing rate and excellent surface quality is achieved through unique formula design, and the environment-friendly high-performance titanium alloy polishing composition has the advantages of being environmentally friendly and high in safety.

Description

Technical Field

[0001] This invention relates to the field of metal material surface treatment technology, and in particular to an environmentally friendly high-performance titanium alloy polishing composition, its preparation method, and its application. Background Technology

[0002] Titanium and titanium alloys are widely used in aerospace, medical devices, and high-end consumer electronics due to their high strength, low density, excellent corrosion resistance, and biocompatibility. These applications demand extremely high surface quality (such as roughness, gloss, and defect-free properties) from titanium and titanium alloys, making chemical mechanical polishing (CMP) a key technology for achieving ultra-smooth, damage-free surfaces.

[0003] Traditional titanium alloy polishing compositions (i.e., polishing slurries) typically use strong oxidants such as hydrogen peroxide (H2O2) and abrasives such as silica sol as the main components to rapidly generate an easily removable soft oxide film (titanium dioxide) on the surface of titanium and titanium alloys, thereby achieving efficient polishing. However, such polishing slurries have significant drawbacks: (1) Environmental and safety issues: H2O2 is unstable and easily decomposed, and there are risks in its storage and use. Furthermore, the treatment of wastewater containing oxidants is complicated and does not conform to the trend of green manufacturing.

[0004] (2) Stability issues: Polishing slurries using silica sol as an abrasive release a large number of metal cations such as titanium ions (Ti4+) during the polishing process. These cations compress the double layer of silica sol particles, destroying their electrostatic stability mechanism, which can easily lead to gelation of the polishing slurry, causing it to fail and become unusable, resulting in waste and production interruption.

[0005] (3) Surface defects: Titanium and titanium alloys have high surface energy. When the wettability of the polishing liquid is poor, surface defects such as water ripples and orange peel are easily generated, which affect the final smoothness.

[0006] Therefore, developing a titanium alloy polishing composition that is free of oxidants, has excellent anti-gel stability, high polishing rate, and is environmentally friendly has significant industrial application value. Summary of the Invention

[0007] The purpose of this invention is to provide an environmentally friendly, high-performance titanium alloy polishing composition, its preparation method, and its application, thereby solving the aforementioned problems in the prior art. The environmentally friendly, high-performance titanium alloy polishing composition of this invention needs to simultaneously address the following key technical issues: (1) Completely eliminate oxidants such as hydrogen peroxide to achieve environmental friendliness.

[0008] (2) It has extremely strong anti-gelling ability and can maintain high dispersion stability even during long-term storage or use.

[0009] (3) Maintain a high polishing rate to ensure production efficiency.

[0010] (4) It has excellent wetting and spreading properties, avoiding polishing defects such as water ripples on the surface of titanium and titanium alloys.

[0011] (5) Effectively complexes and chelates polishing products to maintain the stability of the polishing process.

[0012] To achieve the above objectives, the present invention provides the following solution: One of the technical solutions of this invention is an environmentally friendly high-performance titanium alloy polishing composition (environmentally friendly means free of oxidants, and high-performance means having performance advantages such as high stability and high polishing rate). The environmentally friendly high-performance titanium alloy polishing composition is a polishing composition in which the pH value of the base system is adjusted to 9.5-10.0 using a pH adjuster. By mass percentage, the base system, in addition to water, includes: 10-30% silica sol, 3-4% anti-gel stabilizer, 2-3% heat transfer improver and surface defect inhibitor, 0.1-0.2% wetting and leveling agent, 1-2% alkanolamine complexing agent, and 0.5-1% amino polycarboxylic acid chelating agent. The heat transfer improvement and surface defect inhibitor include ethylene glycol or propylene glycol; The antigel stabilizer includes urea or methylurea.

[0013] In the environmentally friendly high-performance titanium alloy polishing composition of the present invention, the functions of each component are as follows: Silica sol (abrasive): used as the main mechanical grinding medium.

[0014] Antigel stabilizers (urea or methylurea): By forming a strong hydrogen bond network with water molecules through a large number of amino groups in the molecule, they inhibit the Brownian motion and collision aggregation of silica sol particles, thereby fundamentally delaying the gelation process.

[0015] Heat transfer improvement and surface defect inhibitor (ethylene glycol or propylene glycol): It has the characteristics of high heat capacity, high boiling point, moderate viscosity and non-volatile properties. When mixed with water, it improves the overall heat transfer, reduces local overheating, enhances the heat transfer efficiency and thermal stability of the polishing system, avoids local overheating caused by frictional heat at the interface between the polishing pad and the workpiece, and reduces surface defects caused by thermal stress, thereby obtaining a smooth and low-defect polished surface.

[0016] Wetting and leveling agent: It can rapidly reduce the contact angle of the polishing composition on the surface of hydrophobic titanium and titanium alloys, achieving rapid spreading and leveling, and effectively eliminating water ripples.

[0017] Alkylamine complexing agents: The alkylamine groups in their molecules can react with Ti generated during the initial polishing stage. 4+ When metal ions form soluble complexes, they weaken the surface passivation layer, promote material removal, and improve surface gloss.

[0018] Amino polycarboxylic acid chelating agents: As powerful chelating agents, they can deeply capture the Ti produced after the surface softening of titanium and titanium alloys under alkaline conditions. 4+ Ions improve removal rate.

[0019] pH adjuster: Adjusts the pH of the polishing composition to 9.5-10.0. This alkaline environment is beneficial to the stability of the silica sol and promotes the slight chemical dissolution of titanium.

[0020] The environmentally friendly high-performance titanium alloy polishing composition provided by this invention achieves a perfect balance of high stability, high polishing rate and excellent surface quality through a unique formula design, without completely eliminating oxidants. It is a highly competitive environmentally friendly titanium alloy polishing solution.

[0021] Furthermore, the wetting and leveling agent includes diethylene glycol monobutyl ether or acetylenic diol surfactants (both are nonionic wetting and leveling agents).

[0022] Furthermore, the acetylenic diol surfactant includes acetylenic diol 465 or acetylenic diol 607.

[0023] Furthermore, the alkanolamine complexing agent includes triethanolamine or isopropanolamine.

[0024] Furthermore, the aminopolycarboxylic acid chelating agent includes tetrasodium glutamate diacetate (GLDA) or diammonium ethylenediaminetetraacetate (EDTA-2ammonium).

[0025] Furthermore, the pH adjuster includes an organic base or an inorganic base.

[0026] Furthermore, the organic base includes AMP-95 or tetramethylammonium hydroxide, and the inorganic base includes potassium hydroxide (KOH).

[0027] Furthermore, the silica sol has a silica mass concentration of 30-50%, wherein the silica particle size is 80-150 nm, preferably 100 nm.

[0028] The second technical solution of the present invention: a method for preparing the above-mentioned environmentally friendly high-performance titanium alloy polishing composition, comprising the following steps: Prepare each component according to the composition of the basic system; Mix a portion of water with an antigel stabilizer, a heat transfer improver and surface defect inhibitor, a wetting and leveling agent, an alkanolamine complexing agent and an amino polycarboxylic acid chelating agent, and stir until homogeneous to obtain mixture 1; The silica sol was mixed with the mixture 1 and stirred until homogeneous to obtain mixture 2; Add the remaining water to the mixture 2 and stir until homogeneous to obtain mixture 3; A pH adjuster is added to the mixture 3 until the pH value of the system is 9.5-10.0 to obtain the environmentally friendly high-performance titanium alloy polishing composition.

[0029] Preferably, the specific preparation steps of the mixture 1 include: adding an anti-gel stabilizer, a heat transfer improver and surface defect inhibitor, a wetting and leveling agent, an alkanolamine complexing agent, and an amino polycarboxylic acid chelating agent sequentially to water accounting for 20-30% of the total mass of the base system under stirring conditions of 200-400 rpm. After each component is added, the mixture is stirred until it is completely dissolved and mixed evenly before adding the next component. After the amino polycarboxylic acid chelating agent is added and stirred until it is completely dissolved and mixed evenly, the mixture 1 is obtained.

[0030] Preferably, the specific preparation steps of the mixture 2 include: adding the mixture 1 to the silica sol under stirring at 500-700 rpm, and continuing to stir until the mixture is uniform after the addition is complete.

[0031] Furthermore, after adding a pH adjuster to the mixture 3 to bring the system pH to 9.5-10.0, the process also includes a step of filtering using a 400nm filter bag.

[0032] The third technical solution of the present invention: the application of the above-mentioned environmentally friendly high-performance titanium alloy polishing composition in the chemical mechanical polishing of titanium or titanium alloy surfaces.

[0033] The present invention discloses the following technical effects: (1) Environmentally friendly and highly safe: The environmentally friendly high-performance titanium alloy polishing composition of the present invention is completely free of hazardous oxidants such as H2O2, making production, storage, use and subsequent wastewater treatment safer and more environmentally friendly.

[0034] (2) Excellent anti-gel stability: Through the physical barrier stabilization effect of anti-gel stabilizer (urea or methylurea), the polishing composition can still maintain a fluid state after standing at 40°C for 30 days or after being circulated for more than 48 hours without any signs of gelation, which greatly extends the service life of the polishing composition and the tank management cycle.

[0035] (3) High polishing efficiency: In an alkaline environment, amine complexing agents can continuously soften the surface of titanium and titanium alloys through complexation; while amino polycarboxylic acid chelating agents can complex Ti through strong chelation. 4+ Ions promote the dissociation and removal of the oxide and passivation layers on the surface of titanium alloys, accelerate the dissolution and stripping of surface substances, and, in conjunction with the mechanical action of silica sol, achieve a high material removal rate (i.e., a high polishing rate) that does not depend on oxidants.

[0036] (4) Excellent polished surface quality: The use of wetting and leveling agents ensures that the polishing composition is evenly spread on the surface of complex titanium and titanium alloy workpieces. Combined with the heat transfer improvement and surface defect inhibitor (ethylene glycol or propylene glycol) heat transfer homogenization effect, surface defects such as water ripples, orange peel, and hot spots are effectively avoided.

[0037] (5) Strong synergistic effect of formulation: Each component has a clear function and promotes each other. The synergistic effect of alcohol amine complexing agent and amino polycarboxylic acid chelating agent maintains good surface gloss and high surface removal rate. Heat transfer improvement, surface defect inhibitor and wetting leveling agent together ensure surface quality. Anti-gel stabilizer provides the physical basis for long-term operation of the whole system. Detailed Implementation

[0038] Various exemplary embodiments of the present invention will now be described in detail. This detailed description should not be considered as a limitation of the present invention, but rather as a more detailed description of certain aspects, features, and embodiments of the present invention.

[0039] It should be understood that the terminology used in this invention is merely for describing particular embodiments and is not intended to limit the invention. Furthermore, with respect to numerical ranges in this invention, it should be understood that each intermediate value between the upper and lower limits of the range is also specifically disclosed. Any stated value or intermediate value within a stated range, as well as each smaller range between any other stated value or intermediate value within said range, is also included in this invention. The upper and lower limits of these smaller ranges may be independently included or excluded from the range.

[0040] Unless otherwise stated, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art. While only preferred methods and materials have been described herein, any methods and materials similar or equivalent to those described herein may be used in the implementation or testing of this invention. All references to this specification are incorporated by way of citation to disclose and describe methods and / or materials associated with those references. In the event of any conflict with any incorporated reference, the content of this specification shall prevail.

[0041] Various modifications and variations can be made to the specific embodiments described in this specification without departing from the scope or spirit of the invention, as will be apparent to those skilled in the art. Other embodiments derived from this specification will also be apparent to those skilled in the art. This specification and embodiments are merely exemplary.

[0042] The terms “include,” “including,” “have,” “contain,” etc., used in this article are all open-ended terms, meaning that they include but are not limited to.

[0043] It should be noted that any aspects not described in detail in this invention are conventional practices in the field and are not the focus of this invention.

[0044] Unless otherwise specified, the room temperature mentioned in the following embodiments, comparative examples and test examples of this invention refers to 20-30°C.

[0045] Unless otherwise specified, all raw materials used in the following embodiments, comparative examples and test examples of this invention are commercially available products.

[0046] Example 1 An environmentally friendly, high-performance titanium alloy polishing composition is prepared by the following steps: (1) Prepare the following components as the base system based on a total mass fraction of 100%: 30% silica sol (containing 40wt% silica with an average particle size of 100nm), 4% urea, 2% ethylene glycol, 0.15% acetylacetonate 465, 2% triethanolamine, 0.5% GLDA, and the balance being deionized water.

[0047] (2) Add 25% of the total mass of the basic system of deionized water to the container.

[0048] (3) Under stirring conditions (400 rpm), urea, ethylene glycol, acetylation glycol 465, triethanolamine, and GLDA were added sequentially to deionized water. After each component was added, the mixture was stirred for 5 minutes until it was completely dissolved and homogeneous before adding the next component. After all the GLDA was added and the mixture was stirred for 5 minutes, the mixture 1 was obtained.

[0049] (4) Add silica sol to another container and slowly add mixture 1 to the silica sol while stirring at 700 rpm. After the addition is complete, continue stirring for 30 minutes to ensure that the silica sol is evenly dispersed to obtain mixture 2.

[0050] (5) Add the remaining deionized water to mixture 2. After adding the water, continue stirring for 15 minutes to mix it evenly and obtain mixture 3.

[0051] (6) Using AMP-95 as a pH adjuster, slowly add it to the mixture 3 while monitoring the pH value. Adjust the pH value of the system to 10.0 precisely, and then filter it with a 400nm filter bag to obtain an environmentally friendly high-performance titanium alloy polishing composition.

[0052] Example 2 An environmentally friendly, high-performance titanium alloy polishing composition is prepared by the following steps: (1) Prepare the following components as the base system based on a total mass fraction of 100%: 30% silica sol (containing 40wt% silica with an average particle size of 100nm), 3% urea, 2% propylene glycol, 0.15% acetylacetonate 465, 1% triethanolamine, 0.5% GLDA, and the balance being deionized water.

[0053] (2) Add 25% of the total mass of the basic system of deionized water to the container.

[0054] (3) Under stirring conditions (400 rpm), urea, propylene glycol, acetylation glycol 465, triethanolamine, and GLDA were added sequentially to deionized water. After each component was added, the mixture was stirred for 5 minutes until it was completely dissolved and homogeneous before adding the next component. After all the GLDA was added and the mixture was stirred for 5 minutes, the mixture 1 was obtained.

[0055] (4) Add silica sol to another container and slowly add mixture 1 to the silica sol while stirring at 700 rpm. After the addition is complete, continue stirring for 30 minutes to ensure that the silica sol is evenly dispersed to obtain mixture 2.

[0056] (5) Add the remaining deionized water to mixture 2. After adding the water, continue stirring for 15 minutes to mix it evenly and obtain mixture 3.

[0057] (6) Using AMP-95 as a pH adjuster, slowly add it to the mixture 3 while monitoring the pH value. Adjust the pH value of the system to 10.0 precisely, and then filter it with a 400nm filter bag to obtain an environmentally friendly high-performance titanium alloy polishing composition.

[0058] Example 3 An environmentally friendly, high-performance titanium alloy polishing composition is prepared by the following steps: (1) Prepare the following components as the base system based on a total mass fraction of 100%: 30% silica sol (containing 40wt% silica with an average particle size of 100nm), 4% methylurea, 2% ethylene glycol, 0.15% acetylacetonate 607, 1% triethanolamine, 0.5% GLDA, and the balance being deionized water.

[0059] (2) Add 25% of the total mass of the basic system of deionized water to the container.

[0060] (3) Under stirring conditions (400 rpm), methylurea, ethylene glycol, acetylation glycol 607, triethanolamine, and GLDA were added sequentially to deionized water. After each component was added, the mixture was stirred for 5 minutes until it was completely dissolved and homogeneous before adding the next component. After all the GLDA was added and the mixture was stirred for 5 minutes, the mixture 1 was obtained.

[0061] (4) Add silica sol to another container and slowly add mixture 1 to the silica sol while stirring at 600 rpm. After the addition is complete, continue stirring for 30 minutes to ensure that the silica sol is evenly dispersed to obtain mixture 2.

[0062] (5) Add the remaining deionized water to mixture 2. After adding the water, continue stirring for 15 minutes to mix it evenly and obtain mixture 3.

[0063] (6) Using AMP-95 as a pH adjuster, slowly add it to the mixture 3 while monitoring the pH value. Adjust the pH value of the system to 10.0 precisely, and then filter it with a 400nm filter bag to obtain an environmentally friendly high-performance titanium alloy polishing composition.

[0064] Example 4 An environmentally friendly, high-performance titanium alloy polishing composition is prepared by the following steps: (1) Prepare the following components as the base system based on a total mass fraction of 100%: 30% silica sol (containing 40wt% silica with an average particle size of 100nm), 4% methylurea, 2% propylene glycol, 0.15% acetylacetonate 465, 2% triethanolamine, 0.5% EDTA-2 ammonium, and the balance being deionized water.

[0065] (2) Add 25% of the total mass of the basic system of deionized water to the container.

[0066] (3) Under stirring conditions (400 rpm), methylurea, propylene glycol, acetylacetonate 465, triethanolamine, and EDTA-2 ammonium were added sequentially to deionized water. After each component was added, the mixture was stirred for 5 minutes until it was completely dissolved and homogeneous before adding the next component. After all the EDTA-2 ammonium was added and the mixture was stirred for 5 minutes, the mixture 1 was obtained.

[0067] (4) Add silica sol to another container and slowly add mixture 1 to the silica sol while stirring at 600 rpm. After the addition is complete, continue stirring for 30 minutes to ensure that the silica sol is evenly dispersed to obtain mixture 2.

[0068] (5) Add the remaining deionized water to mixture 2. After adding the water, continue stirring for 15 minutes to mix it evenly and obtain mixture 3.

[0069] (6) KOH is slowly added to the mixture 3 as a pH adjuster, while monitoring the pH value. The pH value of the system is precisely adjusted to 10.0. Then, the mixture is filtered with a 400nm filter bag to obtain an environmentally friendly high-performance titanium alloy polishing composition.

[0070] Comparative Example 1 Same as Example 4, except that the use of methylurea is omitted.

[0071] Comparative Example 2 Same as Example 4, except that the use of propylene glycol is omitted.

[0072] Comparative Example 3 Same as Example 4, except that the use of acetylidene 465 is omitted.

[0073] Comparative Example 4 Same as Example 4, except that the use of triethanolamine is omitted.

[0074] Comparative Example 5 Same as Example 4, except that the use of EDTA-2 ammonium is omitted.

[0075] Comparative Example 6 Same as Example 4, except that the mass of EDTA-2 ammonium is replaced with triethanolamine, that is, the mass content of triethanolamine in the basic system is 2.5%.

[0076] Comparative Example 7 Same as Example 4, except that triethanolamine is replaced by EDTA-2 ammonium by mass, that is, the mass content of EDTA-2 ammonium in the basic system is 2.5%.

[0077] Comparative Example 8 Same as Example 4, except that triethanolamine is replaced by sodium gluconate.

[0078] Comparative Example 9 The preparation steps of a traditional titanium alloy polishing composition containing an oxidant are as follows: (1) Based on a total mass fraction of 100%, prepare the following components as the base system: 30% silica sol (containing 40wt% silica with an average particle size of 100nm), 2% sodium hypochlorite (as an oxidant), 2% glycine (as a chelating agent), 2.5% ethylene glycol, and the remainder deionized water.

[0079] (2) Add 25% of the total mass of the basic system of deionized water to the container.

[0080] (3) Under stirring conditions (400 rpm), sodium hypochlorite, glycine, and ethylene glycol were added sequentially to deionized water. After each component was added, the mixture was stirred for 5 minutes until completely dissolved and homogeneous before adding the next component. After the ethylene glycol was added and stirred for 5 minutes, mixture 1 was obtained.

[0081] (4) Add silica sol to another container and slowly add mixture 1 to the silica sol while stirring at 700 rpm. After the addition is complete, continue stirring for 30 minutes to ensure that the silica sol is evenly dispersed to obtain mixture 2.

[0082] (5) Add the remaining deionized water to mixture 2. After adding the water, continue stirring for 15 minutes to mix it evenly and obtain mixture 3.

[0083] (6) Using AMP-95 as a pH adjuster, slowly add it to the mixture 3 while monitoring the pH value. Adjust the pH value of the system to 10.0 precisely, and then filter it with a 400nm filter bag to obtain the traditional titanium alloy polishing composition containing oxidant.

[0084] Comparative Example 10 The preparation steps of a traditional titanium alloy polishing composition containing an oxidant are as follows: (1) Based on a total mass fraction of 100%, prepare the following components as the base system: 30% silica sol (containing 40wt% silica with an average particle size of 100nm), 3% H2O2 (as an oxidant), 2% glycine (as a chelating agent), 2.5% ethylene glycol, and the remainder deionized water.

[0085] (2) Add 25% of the total mass of the basic system of deionized water to the container.

[0086] (3) Under stirring conditions (400 rpm), add H2O2, glycine, and ethylene glycol to deionized water in sequence. After each component is added, stir for 5 minutes until completely dissolved and mixed before adding the next component. After all the ethylene glycol has been added and stirred for 5 minutes, mixture 1 is obtained.

[0087] (4) Add silica sol to another container and slowly add mixture 1 to the silica sol while stirring at 600 rpm. After the addition is complete, continue stirring for 30 minutes to ensure that the silica sol is evenly dispersed to obtain mixture 2.

[0088] (5) Add the remaining deionized water to mixture 2. After adding the water, continue stirring for 15 minutes to mix it evenly and obtain mixture 3.

[0089] (6) KOH was slowly added to the mixture 3 as a pH adjuster, while monitoring the pH value. The pH value of the system was precisely adjusted to 10.0. Then, the mixture was filtered with a 400 nm filter bag to obtain the traditional titanium alloy polishing composition containing oxidant.

[0090] Test Example 1 Stability test: Stability testing was conducted through accelerated aging tests, with the following specific steps: The titanium alloy polishing compositions prepared in each example and comparative example were placed in an oven at 40°C for accelerated aging tests for 30 days, and the gelation was observed daily.

[0091] Upon observation, the titanium alloy polishing compositions prepared in Examples 1-4 showed no signs of gelation after standing at 40°C for 30 days.

[0092] The titanium alloy polishing composition prepared in Comparative Example 1 showed no obvious gelation phenomenon after standing at 40°C for 10 days. After 10 days, the viscosity of the solution began to increase, and slow gelation occurred.

[0093] The titanium alloy polishing composition prepared in Comparative Example 2 showed no obvious gelation after standing at 40°C for 30 days, but the moisture evaporated significantly.

[0094] The titanium alloy polishing compositions prepared in Comparative Examples 3-8 showed no signs of gelation after standing at 40°C for 30 days.

[0095] In Comparative Example 9, the sodium hypochlorite in the titanium alloy polishing composition decomposed significantly after 12 hours, causing the silica sol system to become viscous and gelled, and the performance of the titanium alloy polishing composition decreased sharply.

[0096] The H2O2 in the titanium alloy polishing composition prepared in Comparative Example 10 decomposed significantly after 24 hours, causing the silica sol system to become viscous and gelled, and the performance of the titanium alloy polishing composition decreased sharply.

[0097] Test Example 2 Polishing test (performed on standard CMP equipment): Using black damping cloth as the polishing pad, the polishing test is conducted under specific pressure. The specific test conditions are as follows: Workpiece: TC4 titanium alloy; Pressure: 3 psi; Polishing head / polishing disc speed: 87 / 93 rpm; Titanium alloy polishing composition (i.e., titanium alloy polishing fluid) flow rate: 80 mL / min; Polishing time: Polishing was performed in 20-minute cycles, using the same batch of titanium alloy polishing composition to continuously polish the same workpiece for 48 hours (i.e., a total of 144 polishing cycles). After each polishing cycle, the surface quality (surface roughness, surface condition, etc.) of the workpiece was inspected and the polishing rate (MRR) was calculated. Simultaneously, the state of the titanium alloy polishing composition after use (e.g., viscosity) was observed. Then, the next polishing cycle was performed until the total polishing time reached 48 hours. Surface roughness was tested using a roughness meter; surface condition was observed using a high-magnification optical microscope, specifically to check for defects. The polishing rate was calculated by measuring the weight loss of the workpiece before and after polishing, with units of nm / min. The calculation formula is as follows: ; In the above formula, m1 is the weight of the workpiece before polishing, and m2 is the weight of the workpiece after polishing. The density of the workpiece ( =4.43g / cm 3), t is the polishing time, and s is the cross-sectional area of ​​the workpiece (s = 300 cm²). 2 ).

[0098] The test results of the titanium alloy polishing compositions prepared in each embodiment and comparative example are as follows: Example 1: Polishing rate: The polishing rate remained basically unchanged within 48 hours of the cycle, with both the first and last polishing rates being 350 nm / min.

[0099] Workpiece surface quality and the state of the titanium alloy polishing composition after use: After the initial 20 minutes of polishing (i.e., the first polishing), there were no visible water ripples, scratches, or other defects on the workpiece surface, and the surface roughness was 10 nm. After 48 hours of cycling, the workpiece surface condition was good, with virtually no change compared to after the first polishing, and the surface roughness was 12 nm. After 48 hours of cycling, the fluidity of the polishing composition remained essentially unchanged, while the viscosity increased slightly, from 10 mPa·s before polishing to 14 mPa·s.

[0100] Example 2: Polishing rate: The polishing rate did not change much within 48 hours of the cycle. The initial polishing rate was 320 nm / min, and the final polishing rate was 300 nm / min.

[0101] Workpiece surface quality and the condition of the titanium alloy polishing composition after use: After the first polishing, the workpiece surface showed no visible water ripples, scratches, or other defects, and the surface roughness was 10 nm. After 48 hours of cycling, the workpiece surface condition was good, showing almost no change compared to after the first polishing, with a surface roughness of 13 nm. After 48 hours of cycling, the fluidity of the polishing composition remained essentially unchanged, while the viscosity increased slightly, from 10 mPa·s before polishing to 14 mPa·s.

[0102] Example 3: Polishing rate: The polishing rate did not change much within 48 hours of the cycle. The initial polishing rate was 340 nm / min, and the final polishing rate was 320 nm / min.

[0103] Workpiece surface quality and the condition of the titanium alloy polishing composition after use: After the first polishing, the workpiece surface showed no visible water ripples, scratches, or other defects, and the surface roughness was 10 nm. After 48 hours of cycling, the workpiece surface condition was good, showing almost no change compared to after the first polishing, with a surface roughness of 12 nm. After 48 hours of cycling, the fluidity of the polishing composition remained essentially unchanged, while the viscosity increased slightly, from 11 mPa·s before polishing to 13 mPa·s.

[0104] Example 4: Polishing rate: The polishing rate remained basically unchanged within 48 hours of the cycle, with both the first and last polishing rates being 300 nm / min.

[0105] Workpiece surface quality and the condition of the titanium alloy polishing composition after use: After the first polishing, the workpiece surface showed no visible water ripples, scratches, or other defects, and the surface roughness was 10 nm. After 48 hours of cycling, the workpiece surface condition was good, showing almost no change compared to after the first polishing, with a surface roughness of 13 nm. After 48 hours of cycling, the fluidity of the polishing composition remained essentially unchanged, while the viscosity increased slightly, from 9 mPa·s before polishing to 13 mPa·s.

[0106] Comparative Example 1: Polishing rate: The initial polishing rate was 310 nm / min. After 12 hours of cycling (i.e., after the 36th cycle), the polishing rate decreased to 200 nm / min. After 48 hours of cycling (i.e. after the final polishing), the polishing rate decreased to 160 nm / min.

[0107] Workpiece surface quality and the state of the titanium alloy polishing composition after use: After the first polishing, the workpiece surface had no visible water ripples, scratches, or other defects, and the surface roughness was 11 nm. After 24 hours of circulation, crystallization began to appear at the nozzle, and scratches appeared on the workpiece surface, at which point the surface roughness was 15 nm. After 48 hours of circulation, the number of scratches on the workpiece surface increased, and the roughness increased to 25 nm. The initial viscosity of the polishing composition (i.e., before polishing) was 10 mPa·s, which increased to 16 mPa·s after 24 hours of circulation, and further increased to 30 mPa·s after 48 hours of circulation.

[0108] Comparative Example 2: Polishing rate: The polishing rate did not change much within 48 hours of the cycle. The initial polishing rate was 320 nm / min, and the final polishing rate was 300 nm / min.

[0109] Workpiece surface quality and the state of the titanium alloy polishing composition after use: After the first polishing, fine water ripples were visible on the workpiece surface, with no scratches or other defects, and the surface roughness was 13 nm. After 24 hours of cycling, the water ripples on the workpiece surface worsened, and the surface roughness was 15 nm. After 48 hours of cycling, the water ripples on the workpiece surface continued to worsen, and the surface roughness increased to 19 nm. Moreover, after 48 hours of cycling, the polishing composition lost approximately 5 wt% of water, and the viscosity increased from 10 mPa·s before polishing to 18 mPa·s.

[0110] Comparative Example 3: Polishing rate: The polishing rate did not change much within 48 hours of the cycle. The initial polishing rate was 330 nm / min, and the final polishing rate was 320 nm / min.

[0111] Workpiece surface quality and the state of the titanium alloy polishing composition after use: After the first polishing, water ripples appeared on the workpiece surface, with a roughness of 13 nm. After 48 hours of cycling, the workpiece surface condition was basically unchanged compared to after the first polishing, with a roughness of 15 nm. After 48 hours of cycling, the viscosity of the polishing composition increased from 11 mPa·s before polishing to 16 mPa·s.

[0112] Comparative Example 4: Polishing rate: The polishing rate did not change much within 48 hours of the cycle. The initial polishing rate was 280 nm / min, and the final polishing rate was 260 nm / min.

[0113] Surface quality of the workpiece and the condition of the titanium alloy polishing composition after use: After the first polishing, fine circular pits appeared on the workpiece surface, with a roughness of 15 nm. After 48 hours of cycling, the surface condition of the workpiece remained essentially unchanged compared to after the first polishing, with a roughness of 17 nm. After 48 hours of cycling, the viscosity of the polishing composition increased from 11 mPa·s before polishing to 15 mPa·s.

[0114] Comparative Example 5: Polishing rate: The initial polishing rate was 230 nm / min, which decreased to 170 nm / min after 24 hours of cycling, and further decreased to 130 nm / min after 48 hours of cycling.

[0115] Workpiece surface quality and the state of the titanium alloy polishing composition after use: After the first polishing, the workpiece surface showed no visible water ripples, scratches, or other defects, and the surface roughness was 10 nm. After 48 hours of cycling, the workpiece surface condition was good, showing almost no change compared to after the first polishing, with a surface roughness of 12 nm. The state of the polishing composition did not change significantly; however, the viscosity of the polishing composition increased from 11 mPa·s before polishing to 14 mPa·s.

[0116] Comparative Example 6: Polishing rate: The initial polishing rate was 200 nm / min. After 24 hours of cycling, the polishing rate decreased to 170 nm / min. After 48 hours of cycling, the polishing rate decreased to 150 nm / min.

[0117] Workpiece surface quality and the condition of the titanium alloy polishing composition after use: After the first polishing, the workpiece surface showed no visible water ripples, scratches, or other defects, and the surface roughness was 10 nm. After 48 hours of cycling, the workpiece surface condition was good, showing almost no change compared to after the first polishing, with a surface roughness of 11 nm. After 48 hours of cycling, the viscosity of the polishing composition increased from 15 mPa·s to 25 mPa·s.

[0118] Comparative Example 7: Polishing rate: The initial polishing rate was 400 nm / min, which decreased to 380 nm / min after 24 hours of cycling, and further decreased to 340 nm / min after 48 hours of cycling.

[0119] Workpiece surface quality and the state of the titanium alloy polishing composition after use: After the first polishing, circular pits appeared on the workpiece surface, with a roughness of 12 nm. After 48 hours of cycling, the workpiece surface condition was basically unchanged compared to after the first polishing, with a roughness of 13 nm. After 48 hours of cycling, the viscosity of the polishing composition increased from 11 mPa·s before polishing to 15 mPa·s.

[0120] Comparative Example 8: Polishing rate: The initial polishing rate was 310 nm / min, which decreased to 250 nm / min after 24 hours of cycling, and further decreased to 200 nm / min after 48 hours of cycling.

[0121] Workpiece surface quality and the condition of the titanium alloy polishing composition after use: After the first polishing, the workpiece surface exhibited obvious orange peel texture, with a surface roughness of 20 nm. After 48 hours of cycling, the orange peel texture became more severe, and the roughness increased to 38 nm. The viscosity of the polishing composition was 11 mPa·s before polishing, increasing to 20 mPa·s after 24 hours of cycling, and further increasing to 40 mPa·s after 48 hours of cycling.

[0122] Comparative Example 9: Polishing rate: The initial polishing rate was 500 nm / min. The polishing rate was relatively stable for the first 10 hours, but it decreased rapidly after 10 hours due to the decomposition of sodium hypochlorite. After 12 hours of cycling, the polishing rate decreased to 380 nm / min, and after 48 hours of cycling, the final polishing rate decreased to 200 nm / min.

[0123] Surface quality of the workpiece and the condition of the titanium alloy polishing composition after use: After the first polishing, the workpiece surface had no visible water ripples, scratches, or other defects, and the roughness was 11 nm. After 48 hours of cycling, severe water ripples appeared on the workpiece surface, and the roughness increased to 30 nm. The viscosity of the polishing composition was 11 mPa·s before polishing, increased to 30 mPa·s after 24 hours of cycling, and increased to 50 mPa·s after 48 hours of cycling.

[0124] Comparative Example 10: Polishing rate: The initial polishing rate was 520 nm / min. The polishing rate was relatively stable for the first 20 hours, but it decreased rapidly after 20 hours due to the decomposition of H2O2. After 24 hours of cycling, the polishing rate decreased to 350 nm / min, and after 48 hours of cycling, the polishing rate decreased to 180 nm / min.

[0125] Surface quality of the workpiece and the condition of the titanium alloy polishing composition after use: After the first polishing, the workpiece surface had no visible water ripples, scratches, or other defects, and the roughness was 11 nm. After 48 hours of cycling, severe water ripples appeared on the workpiece surface, and the roughness increased to 30 nm. The viscosity of the polishing composition was 11 mPa·s before polishing, increased to 20 mPa·s after 24 hours of cycling, and increased to 40 mPa·s after 48 hours of cycling.

[0126] The test results above show that the stability and polished surface quality of the titanium alloy polishing compositions prepared in Examples 1-4 of this invention are significantly better than those prepared in Comparative Examples 1-10, especially better than the traditional oxidant-containing titanium alloy polishing compositions prepared in Comparative Examples 9-10. Furthermore, the traditional oxidant-containing titanium alloy polishing compositions prepared in Comparative Examples 9-10 generate oxidant-containing wastewater after use. Wastewater treatment requires a step of reducing and decomposing the oxidant, resulting in high treatment costs and risks of oxidant corrosion and decomposition during use, leading to poor environmental protection and safety. In contrast, the titanium alloy polishing compositions of this invention, after polishing, mainly produce silica sol wastewater without oxidants, with suspended SiO2, organic additives, and metal ions (TiO2) as the main pollutants. 4+ Al 3+ (etc.) etc. It can be processed through the following steps: (1) destabilization + flocculation sedimentation; (2) solid-liquid separation; (3) supernatant treatment. The processing is simple to operate, low in cost, does not require a pre-decomposition step, and has no oxidation safety risk.

[0127] The embodiments described above are merely preferred embodiments of the present invention and are not intended to limit the scope of the present invention. Various modifications and improvements made by those skilled in the art to the technical solutions of the present invention without departing from the spirit of the present invention should fall within the protection scope defined by the claims of the present invention.

Claims

1. An environmentally friendly, high-performance titanium alloy polishing composition, characterized in that, The environmentally friendly high-performance titanium alloy polishing composition is a polishing composition in which the pH value of the base system is adjusted to 9.5-10.0 by a pH adjuster; In addition to water, the basic system, by mass percentage, comprises: 10-30% silica sol, 3-4% anti-gel stabilizer, 2-3% heat transfer improver and surface defect inhibitor, 0.1-0.2% wetting and leveling agent, 1-2% alkanolamine complexing agent, and 0.5-1% amino polycarboxylic acid chelating agent; The heat transfer improvement and surface defect inhibitor include ethylene glycol or propylene glycol; The antigel stabilizer includes urea or methylurea.

2. The environmentally friendly high-performance titanium alloy polishing composition as described in claim 1, characterized in that, The wetting and leveling agent includes diethylene glycol monobutyl ether or acetylenic diol surfactants.

3. The environmentally friendly high-performance titanium alloy polishing composition as described in claim 1, characterized in that, The alkanolamine complexing agents include triethanolamine or isopropanolamine.

4. The environmentally friendly high-performance titanium alloy polishing composition as described in claim 1, characterized in that, The aminopolycarboxylic acid chelating agents include tetrasodium glutamate diacetate or diammonium ethylenediaminetetraacetate.

5. The environmentally friendly high-performance titanium alloy polishing composition as described in claim 1, characterized in that, The pH adjuster includes organic or inorganic bases.

6. The environmentally friendly high-performance titanium alloy polishing composition as described in claim 1, characterized in that, The silica sol has a silica mass concentration of 30-50%, and the silica particle size is 80-150 nm.

7. A method for preparing an environmentally friendly high-performance titanium alloy polishing composition as described in any one of claims 1-6, characterized in that, Includes the following steps: Prepare each component according to the composition of the basic system; Mix a portion of water with an antigel stabilizer, a heat transfer improver and surface defect inhibitor, a wetting and leveling agent, an alkanolamine complexing agent and an amino polycarboxylic acid chelating agent, and stir until homogeneous to obtain mixture 1; Mix the silica sol and the mixture 1, and stir until homogeneous to obtain mixture 2; Add the remaining water to the mixture 2 and stir until homogeneous to obtain mixture 3; A pH adjuster is added to the mixture 3 until the pH value of the system is 9.5-10.0 to obtain the environmentally friendly high-performance titanium alloy polishing composition.

8. The application of an environmentally friendly high-performance titanium alloy polishing composition as described in any one of claims 1-6 in the chemical mechanical polishing of titanium or titanium alloy surfaces.