A diamond polishing pad and a method of making the same

Abstract

The present application relates to a kind of diamond polishing pad and its preparation method, belong to the technical field of polishing pad.A kind of diamond polishing pad is by grinding base and the grinding layer of being arranged in the surface of grinding base, the grinding layer is by several hexagonal projections, the hexagonal projection is made of grinding material, the grinding material includes the following components: epoxy modified acrylate, polyurethane, modified filler, diamond micro powder, curing agent, silane coupling agent and dispersing agent.The grinding material prepared by the present application strengthens the mechanical properties of matrix by modified filler, gives cutting ability by diamond micro powder, cooperatively improves the hardness, wear resistance and interface bonding stability of polishing pad, guarantees the precision, efficiency of polishing process and the long service life of polishing pad.

Description

Technical Field

[0001] This invention belongs to the technical field of polishing pads, and relates to a diamond grinding and polishing pad and its preparation method. Background Technology

[0002] Diamond polishing pads are a type of chemical mechanical polishing consumable that uses diamond micropowder as the core abrasive. They achieve efficient, low-damage precision machining of hard and brittle materials such as semiconductor wafers, optical lenses, and consumer electronics glass through a three-dimensional polishing unit structure or sintering process. A typical example is the 3M diamond polishing pad, which uses micro-replication technology to construct a three-dimensional structure, allowing for stable control of material removal rate and surface roughness. It requires no additional coolant and boasts advantages such as long lifespan and environmental friendliness, making it widely used in semiconductors, optics, and consumer electronics.

[0003] In traditional polishing pads, the interface between diamond micropowder and the polyurethane matrix is ​​mostly physically interlocked, which is prone to detachment due to mechanical load, resulting in abrasive loss and scratching of the workpiece. At the same time, the poor high temperature resistance leads to a decrease in polishing accuracy. In addition, during the grinding process, high-speed stirring and long-term friction can easily generate internal heat accumulation, which can cause the matrix to soften and affect the processing stability.

[0004] Patent document CN104772693A discloses a diamond abrasive pad for processing superhard ceramics and its preparation method. The abrasive pad includes a diamond material layer, which comprises a square abrasive block layer and a flat layer. The diamond material layer is made of the following raw materials in the following mass percentages: resin binder: 25%-50%, diamond: 5%-20%, molybdenum disulfide: 1%-10%, wollastonite: 20%-50%, and fumed silica: 0.5%-5%. In the patent document, the diamond material layer uses a variety of inorganic abrasives, and then the abrasives are bonded together by the resin binder alone. This simple physical bonding method still poses a risk of diamond abrasive detachment during high-speed grinding or long-term use. In addition, the resin matrix itself has limited heat resistance and is difficult to cope with the continuous high temperature generated in high-precision processing, resulting in poor service life and processing stability of the abrasive pad, which affects the final processing quality. Summary of the Invention

[0005] The purpose of this invention is to provide a diamond grinding and polishing pad and its preparation method. The grinding material obtained by this invention enhances the mechanical properties of the matrix through modified fillers and imparts cutting ability with diamond micro powder, thereby synergistically improving the hardness, wear resistance and interfacial bonding stability of the polishing pad, ensuring the precision and efficiency of the polishing process and the long service life of the polishing pad.

[0006] The objective of this invention can be achieved through the following technical solutions:

[0007] A diamond polishing pad comprises a polishing substrate and a polishing layer disposed on the surface of the polishing substrate. The polishing layer is composed of a plurality of hexagonal protrusions arranged in an interlocking manner. The side length of each hexagonal protrusion is 0.5-2 mm. A groove with a depth of 0.1-0.3 mm is formed between any adjacent hexagonal protrusions. The top and sidewall of each hexagonal protrusion are rounded with a radius of 0.05-0.1 mm. The hexagonal protrusions are made of polishing material. The method for preparing the diamond polishing pad includes placing the polishing substrate in a mold, introducing polishing material into the mold, allowing the polishing material to solidify on the surface of the polishing substrate and form a preset polishing layer structure, ultimately obtaining the diamond polishing pad.

[0008] As a preferred embodiment of the present invention, the grinding layer is composed of a plurality of intersecting hexagonal protrusions, each hexagonal protrusion having a side length of 0.5-2mm. A groove with a depth of 0.1-0.3mm is formed between any adjacent hexagonal protrusions. This structural design can effectively improve the adhesion of abrasive during the grinding process and enhance the fluidity of the grinding fluid on the surface of the grinding layer, thereby improving the grinding and polishing efficiency and the uniformity of surface quality. The apex of the hexagonal protrusion unit is rounded with a radius of 0.05-0.1mm to avoid scratching damage to the surface of the workpiece during the grinding process.

[0009] As a preferred embodiment of the present invention, the grinding material comprises the following components by weight: 40-50 parts of epoxy-modified acrylate, 5-10 parts of polyurethane, 20-30 parts of modified filler, 10-15 parts of diamond micro powder, 5-8 parts of curing agent, 0.5-1 parts of silane coupling agent, and 0.3-0.5 parts of dispersant.

[0010] As a preferred technical solution of the present invention, the curing agent of the present invention is isophorone diamine. Isophorone diamine, as a curing agent in epoxy modified acrylate and polyurethane systems, has good temperature resistance and high toughness after curing, and can effectively avoid coating cracking during grinding.

[0011] As a preferred embodiment of the present invention, the silane coupling agent is one or a combination of two of silane coupling agents KH550, KH560 and KH570. Preferably, the embodiment of the present invention uses silane coupling agent KH560. Silane coupling agent KH560 interacts with the epoxy groups of epoxy-modified acrylate and the amino groups of polyurethane, which can significantly improve the interfacial bonding force between diamond micropowder and the system resin and reduce micropowder shedding.

[0012] As a preferred embodiment of the present invention, the dispersant is one or a combination of dispersant BYK-110 and dispersant BYK-163. Preferably, the present invention uses dispersant BYK-110. Dispersant BYK-110 has excellent compatibility with epoxy-modified acrylate / polyurethane system resin and high dispersion efficiency for diamond micro powder.

[0013] As a preferred embodiment of the present invention, the epoxy-modified acrylate in the present invention is an epoxy-modified acrylate emulsion with a solid content of 46-48%, a viscosity (23℃) of 500-1500 mpa·s, a glass transition temperature of 18-22℃, and a pH value of 7.0-9.0.

[0014] As a preferred embodiment of the present invention, the polyurethane in the present invention is a polyurethane emulsion with a solid content of 39-41%, a pH value of 7.0-8.5, a viscosity (23℃) of 50-800 mPa·s, and an average particle size of 80-120 nm.

[0015] As a preferred embodiment of the present invention, the average particle size of the diamond micro powder is 10 μm.

[0016] As a preferred technical solution of the present invention, the preparation of the abrasive material includes: mixing diamond micro powder, silane coupling agent and dispersant, adding epoxy modified acrylate, polyurethane, modified filler and curing agent, stirring at high speed, degassing under vacuum, pouring into a mold for curing, and thus obtaining the abrasive material.

[0017] As a preferred embodiment of the present invention, the high-speed stirring is performed at a speed of 3000-4000 r / min for 15-20 min, and the curing is performed at 70-80℃ for 2-3 h, followed by heating to 110-120℃ for 1-2 h.

[0018] As a preferred embodiment of the present invention, the method for preparing the modified filler includes the following steps:

[0019] S1. Soak the zirconia fiber in a nitric acid aqueous solution, filter, rinse, and vacuum dry in an oven to obtain pretreated zirconia fiber;

[0020] S2. The pretreated zirconia fiber is placed in a mixture of ammonia and anhydrous ethanol. A silicon source is added dropwise under stirring and heated. The mixture is then filtered, washed, and placed in an oven for vacuum drying to obtain a silica / zirconia fiber composite.

[0021] S3. Spray chitosan solution onto the surface of the silica / zirconia fiber composite and then dry it. After drying, place the product in anhydrous ethanol and ultrasonically disperse it. Slowly add silane coupling agent, heat and stir, rotary evaporate to obtain the solid, and vacuum dry it to obtain the silane modified composite.

[0022] S4. Mix the silane-modified composite, the reactive monomer, and the organic solvent, add the initiator, stir and mix, centrifuge, take the solid, wash, and dry to obtain the modified filler.

[0023] As a preferred embodiment of the present invention, in step S1, the soaking time is 2-3 hours, the rinsing is performed with deionized water until the filtrate is neutral, and the vacuum drying is performed at 80°C to constant weight; the mass ratio of the zirconium oxide fiber to the nitric acid aqueous solution is 1.0-1.2:6.0-6.5, and the mass concentration of the nitric acid aqueous solution is 4%.

[0024] As a preferred embodiment of the present invention, the zirconium oxide fiber has a tetragonal phase crystal structure, a fiber diameter of 5-10 μm, and a fiber length of 1-5 mm.

[0025] As a preferred embodiment of the present invention, in step S2, the stirring speed is 150-200 r / min, the heating treatment is stirring at 110-120℃ and 200-280 r / min for 3-4 hours, the washing is washing three times with anhydrous ethanol, the vacuum drying is vacuum drying at 90℃ to constant weight, the mass ratio of the pretreated zirconia fiber, ammonia, anhydrous ethanol and silicon source is 26-28:5-8:110-120:9-12, the concentration of the ammonia is 18 wt%, and the silicon source is composed of tetraethyl orthosilicate and methyltrimethoxysilane in a mass ratio of 2:3.8-4.2.

[0026] As a preferred embodiment of the present invention, in step S3, the drying is performed at 50°C to constant weight, the ultrasonic dispersion is performed at 300-500W power for 20-30 minutes, the heating and stirring is performed at 60-65°C for 4-5 hours, and the vacuum drying is performed at 80°C to constant weight. The mass ratio of the silica / zirconium oxide fiber composite, chitosan solution, anhydrous ethanol, and silane coupling agent is 2.4-2.8:0.9-1.2:25-30:0.2-0.4, and the silane coupling agent is silane coupling agent A171, vinyltrimethoxysilane.

[0027] As a preferred embodiment of the present invention, the chitosan solution is prepared by mixing chitosan and a 2% (by mass) aqueous acetic acid solution at a ratio of 1g:10mL, wherein the degree of deacetylation of the chitosan is 90-95% and the molecular weight is 200-300kDa.

[0028] As a preferred embodiment of the present invention, in step S4, the stirring and mixing is carried out at a temperature of 65-70°C for 2-3 hours, the washing is carried out with ethyl acetate three times, and the drying is carried out under vacuum at 80°C to constant weight, i.e., azobisisobutyronitrile (AIBN). The organic solvent is ethyl acetate. The mass ratio of the silane-modified complex, the reactive monomer, the organic solvent, and the initiator is 10-12:5-7:50-60:0.25-0.28. The reactive monomer is composed of furanyl acrylate, glycidyl methacrylate, and methacrylate in a mass ratio of 1:0.8-1.2:0.5-1.0. The initiator is AIBN, and the furanyl acrylate is 2-furanyl acrylate.

[0029] The beneficial effects of this invention are:

[0030] The abrasive material prepared by this invention enhances the mechanical properties of the matrix through modified fillers and imparts cutting ability with diamond micro powder, thereby synergistically improving the hardness, wear resistance and interfacial bonding stability of the polishing pad, ensuring the precision and efficiency of the polishing process and the long service life of the polishing pad. Attached Figure Description

[0031] Figure 1 A schematic diagram of the structure of a diamond grinding and polishing pad;

[0032] Figure 2 The images show the FT-IR infrared spectra of the silica / zirconium oxide fiber composite, silane-modified composite, and modified filler in Example 1. Detailed Implementation

[0033] To further illustrate the technical means and effects of the present invention in achieving its intended purpose, the following detailed description of the specific implementation methods, structures, features, and effects of the present invention, in conjunction with embodiments, is provided below.

[0034] like Figure 1 As shown, a diamond polishing pad comprises a polishing substrate 1 and a polishing layer disposed on the surface of the polishing substrate 1. The polishing layer is composed of a plurality of hexagonal protrusions 2, which are arranged in an interlaced manner. The side length of each hexagonal protrusion 2 is 0.5-2 mm. A groove 3 with a depth of 0.1-0.3 mm is formed between any adjacent hexagonal protrusions 2. The top and sidewall of each hexagonal protrusion 2 are rounded with a radius of 0.05-0.1 mm. The hexagonal protrusions 2 are made of polishing material. The preparation method of the diamond polishing pad includes placing the polishing substrate in a mold, introducing polishing material into the mold, allowing the polishing material to solidify on the surface of the polishing substrate and form a preset polishing layer structure, ultimately obtaining the diamond polishing pad.

[0035] Example 1

[0036] The grinding material comprises the following components by weight: 40 parts epoxy-modified acrylate, 5 parts polyurethane, 20 parts modified filler, 10 parts diamond micro powder, 5 parts curing agent, 0.5 parts silane coupling agent, and 0.3 parts dispersant, wherein the curing agent is isophorone diamine, the silane coupling agent is silane coupling agent KH560, and the dispersant is dispersant BYK-110;

[0037] The preparation method of the abrasive material includes the following steps: diamond micro powder, silane coupling agent and dispersant are mixed, epoxy modified acrylate, polyurethane, modified filler and curing agent are added, and the mixture is stirred at 3000 r / min for 15 min. Vacuum degassing is performed, the mixture is poured into a mold, cured at 70℃ for 2 h, and then heated to 110℃ for 1 h to obtain the abrasive material.

[0038] The method for preparing the modified filler includes the following steps:

[0039] S1. Soak the zirconia fiber in a nitric acid aqueous solution for 2 hours, filter to obtain the solid, rinse with deionized water until the filtrate is neutral, place in an oven and vacuum dry at 80°C to constant weight to obtain pretreated zirconia fiber; the mass ratio of zirconia fiber to nitric acid aqueous solution is 1.0:6.0, and the mass concentration of the nitric acid aqueous solution is 4%;

[0040] S2. The pretreated zirconia fiber was placed in a mixture of ammonia and anhydrous ethanol. A silicon source was added dropwise while stirring at 150 rpm. The mixture was then stirred at 110°C and 200 rpm for 3 hours. The solid was filtered, washed three times with anhydrous ethanol, and then vacuum-dried at 90°C to constant weight to obtain a silica / zirconia fiber composite. The mass ratio of the pretreated zirconia fiber, ammonia, anhydrous ethanol, and silicon source was 26:5:110:9. The concentration of the ammonia was 18 wt%. The silicon source consisted of tetraethyl orthosilicate and methyltrimethoxysilane in a mass ratio of 2:3.8.

[0041] S3. After spraying chitosan solution onto the surface of the silica / zirconia fiber composite, the product was dried at 50°C to constant weight. The dried product was placed in anhydrous ethanol and sonicated at 300W for 20 min. Silane coupling agent A171 was slowly added, and the mixture was stirred at 60°C for 4 h. The solid was collected by rotary evaporation and dried under vacuum at 80°C to constant weight to obtain the silane-modified composite. The mass ratio of silica / zirconia fiber composite, chitosan solution, anhydrous ethanol, and silane coupling agent A171 was 2.4:0.9:25:0.2.

[0042] S4. Mix the silane-modified composite, the reactant, and the ethyl acetate organic solvent, add the initiator, stir at 65°C for 2 hours, centrifuge, take the solid, wash it three times with ethyl acetate, and dry it under vacuum at 80°C to constant weight to obtain the modified filler.

[0043] Wherein, the initiator is initiator AIBN, the reaction monomer is composed of 2-furanacrylic acid, glycidyl methacrylate and methacrylate in a mass ratio of 1:0.8:0.5, the furanacrylic acid is 2-furanacrylic acid, and the mass ratio of silane modified complex, reaction monomer, ethyl acetate organic solvent and initiator AIBN is 10:5:50:0.25;

[0044] like Figure 2 As shown, in the infrared spectrum of the silica / zirconia fiber composite, at 1160 cm⁻¹... -1 The absorption peak at 786 cm⁻¹ is attributed to the antisymmetric stretching vibration peak of Si-O-Si. -1 The characteristic peaks at the point are the stretching vibration peaks of Si-O, which indicate that silica has been successfully coated on the surface of zirconia fibers, that is, the silica / zirconia fiber composite has been successfully prepared.

[0045] like Figure 2 As shown in the infrared spectrum of the silane-modified composite, at 1571 cm⁻¹ -1 The characteristic peak at 2896 cm⁻¹ corresponds to the NH bond in the amide II band of chitosan, indicating that chitosan is retained and interacts with the surface of the silica / zirconia fiber composite. -1 and 1408cm -1 The absorption peak at 1307 cm⁻¹ is attributed to the CH groups of the methyl group and the CH groups of the vinyl group in the silane coupling agent A171, while the peak at 1307 cm⁻¹ is attributed to the CH groups of the methyl group and the vinyl group in the silane coupling agent A171. -1 The characteristic peaks at the surface are mainly attributed to the bonding between the silica coated on the surface and the vinyl groups in A171 via Si-C chemical bonds. The above results indicate that the silane coupling agent A171 was successfully grafted onto the composite, and also prove that the silane-modified composite was successfully prepared.

[0046] like Figure 2 As shown in the infrared spectrum of the modified filler, at 1725 cm⁻¹... -1 The nearby absorption peak is mainly attributed to the carbonyl group (C=O), which is direct evidence that the complex has undergone polymerization with all the ester-containing monomers involved in the reaction. Compared to the silane-modified complex, the peak at 2893 cm⁻¹ is significantly higher. -1 The increased intensity and broadening of the CH absorption peak at the point indicates that a large number of methylene and methyl groups have been introduced into the polymer chain, which is a clear sign of surface organication, namely the copolymerization reaction of the silane-modified complex and the reactive monomer, thus enabling the successful preparation of the modified filler.

[0047] Example 2

[0048] The grinding material comprises the following components by weight: 45 parts epoxy-modified acrylate, 8 parts polyurethane, 25 parts modified filler, 12 parts diamond micro powder, 6 parts curing agent, 0.8 parts silane coupling agent, and 0.4 parts dispersant, wherein the curing agent is isophorone diamine, the silane coupling agent is silane coupling agent KH560, and the dispersant is dispersant BYK-110;

[0049] The preparation method of the abrasive material includes the following steps: diamond micro powder, silane coupling agent and dispersant are mixed, epoxy modified acrylate, polyurethane, modified filler and curing agent are added, and the mixture is stirred at 3500 r / min for 18 min. Vacuum degassing is performed, the mixture is poured into a mold, cured at 75℃ for 2.5 h, and then heated to 115℃ for 1.5 h to obtain the final product.

[0050] The method for preparing the modified filler includes the following steps:

[0051] S1. Soak zirconia fibers in nitric acid aqueous solution for 2.5 hours, filter to obtain solid matter, rinse with deionized water until the filtrate is neutral, place in an oven and vacuum dry at 80°C to constant weight to obtain pretreated zirconia fibers; the mass ratio of zirconia fibers to nitric acid aqueous solution is 1.1:6.2, and the mass concentration of the nitric acid aqueous solution is 4%;

[0052] S2. Pretreated zirconia fibers were placed in a mixture of ammonia and anhydrous ethanol. A silicon source was added dropwise while stirring at 180 rpm. The mixture was then stirred at 115°C and 240 rpm for 3.5 hours. The solid was filtered, washed three times with anhydrous ethanol, and then vacuum-dried at 90°C to constant weight to obtain a silica / zirconia fiber composite. The mass ratio of pretreated zirconia fibers, ammonia, anhydrous ethanol, and silicon source was 27:6:115:10. The concentration of the ammonia was 18 wt%, and the silicon source consisted of tetraethyl orthosilicate and methyltrimethoxysilane in a mass ratio of 2:4.

[0053] S3. After spraying chitosan solution onto the surface of the silica / zirconia fiber composite, the product was dried at 50°C to constant weight. The dried product was placed in anhydrous ethanol and sonicated at 400W for 25 min. Silane coupling agent A171 was slowly added, and the mixture was stirred at 62°C for 4.5 h. The solid was collected by rotary evaporation and dried under vacuum at 80°C to constant weight to obtain the silane-modified composite. The mass ratio of silica / zirconia fiber composite, chitosan solution, anhydrous ethanol, and silane coupling agent A171 was 2.6:1:28:0.3.

[0054] S4. Mix the silane-modified composite, the reactant, and the ethyl acetate organic solvent, add the initiator, stir at 68°C for 2.5 h, centrifuge, take the solid, wash it three times with ethyl acetate, and dry it under vacuum at 80°C to constant weight to obtain the modified filler.

[0055] The initiator is AIBN, and the reaction monomer is composed of 2-furanacrylic acid, glycidyl methacrylate and methacrylate in a mass ratio of 1:1:0.8. The furanacrylic acid is 2-furanacrylic acid, and the mass ratio of the silane modified complex, the reaction monomer, ethyl acetate organic solvent and the initiator AIBN is 11:6:55:0.26.

[0056] Example 3

[0057] The grinding material comprises the following components by weight: 50 parts epoxy-modified acrylate, 10 parts polyurethane, 30 parts modified filler, 15 parts diamond micro powder, 8 parts curing agent, 1 part silane coupling agent, and 0.5 parts dispersant, wherein the curing agent is isophorone diamine, the silane coupling agent is silane coupling agent KH560, and the dispersant is dispersant BYK-110;

[0058] The preparation method of the abrasive material includes the following steps: diamond micro powder, silane coupling agent and dispersant are mixed, epoxy modified acrylate, polyurethane, modified filler and curing agent are added, and the mixture is stirred at 4000 r / min for 20 min. Vacuum degassing is performed, the mixture is poured into a mold, cured at 80℃ for 3 h, and then heated to 120℃ for 2 h to obtain the final product.

[0059] The method for preparing the modified filler includes the following steps:

[0060] S1. Soak zirconia fibers in nitric acid aqueous solution for 3 hours, filter to obtain solid matter, rinse with deionized water until the filtrate is neutral, place in an oven and vacuum dry at 80°C to constant weight to obtain pretreated zirconia fibers; the mass ratio of zirconia fibers to nitric acid aqueous solution is 1.2:6.5, and the mass concentration of the nitric acid aqueous solution is 4%;

[0061] S2. The pretreated zirconia fiber was placed in a mixture of ammonia and anhydrous ethanol. A silicon source was added dropwise while stirring at 200 rpm. The mixture was then stirred at 120°C and 280 rpm for 4 hours. The solid was filtered, washed three times with anhydrous ethanol, and then vacuum-dried at 90°C to constant weight to obtain a silica / zirconia fiber composite. The mass ratio of the pretreated zirconia fiber, ammonia, anhydrous ethanol, and silicon source was 28:8:120:12. The concentration of the ammonia was 18 wt%. The silicon source consisted of tetraethyl orthosilicate and methyltrimethoxysilane in a mass ratio of 2:4.2.

[0062] S3. After spraying chitosan solution onto the surface of the silica / zirconia fiber composite, the product was dried at 50°C to constant weight. The dried product was placed in anhydrous ethanol and sonicated at 500W for 30 min. Silane coupling agent A171 was slowly added, and the mixture was stirred at 65°C for 5 h. The solid was collected by rotary evaporation and dried under vacuum at 80°C to constant weight to obtain the silane-modified composite. The mass ratio of silica / zirconia fiber composite, chitosan solution, anhydrous ethanol, and silane coupling agent A171 was 2.8:1.2:30:0.4.

[0063] S4. Mix the silane-modified composite, the reactant and ethyl acetate organic solvent, add the initiator and stir at 70°C for 3 hours. Centrifuge, take the solid and wash it 3 times with ethyl acetate. Dry it under vacuum at 80°C to constant weight to obtain the modified filler.

[0064] The initiator is AIBN, and the reaction monomer is composed of 2-furanacrylic acid, glycidyl methacrylate and methacrylate in a mass ratio of 1:1.2:1.0. The furanacrylic acid is 2-furanacrylic acid, and the mass ratio of the silane modified complex, the reaction monomer, ethyl acetate organic solvent and the initiator AIBN is 12:7:60:0.28.

[0065] Comparative Example 1

[0066] Compared with Example 1, Comparative Example 1 differs in that it uses tetraethyl orthosilicate instead of methyltrimethoxysilane;

[0067] Everything else is the same.

[0068] Comparative Example 2

[0069] The difference between Comparative Example 2 and Example 1 is that Comparative Example 2 does not use chitosan;

[0070] Everything else is the same.

[0071] Comparative Example 3

[0072] Compared with Example 1, Comparative Example 3 differs in that step S3 of Comparative Example 3 does not use a silane coupling agent;

[0073] Everything else is the same.

[0074] Comparative Example 4-5

[0075] Compared with Example 1, Comparative Examples 4-5 differ in the composition of the reactant monomers. The amounts of reactant monomers used in Comparative Examples 4-5 are shown in Table 1; all other aspects are the same.

[0076] Table 1 (Unit: parts by weight)

[0077] 2-Furanacrylic acid glycidyl methacrylate methacrylates Example 3 1 0.8 0.5 Comparative Example 4 0 1.3 1 Comparative Example 5 1.4 0 0.9

[0078] The performance of the abrasive materials prepared in Examples 1-3 and Comparative Examples 1-5 was tested, and the test results are shown in Table 2.

[0079] Table 2 Test Results

[0080]

[0081]

[0082] As can be seen from the test results in Table 2, compared with Comparative Examples 1-5, the abrasive materials prepared by the present invention have better hardness, wear resistance and mechanical strength in Examples 1-3.

[0083] Comparative analysis reveals that this invention utilizes the strong oxidizing properties of nitric acid to generate active functional groups such as hydroxyl and carboxyl groups on the surface of zirconia fibers. Nitric acid etching further forms a micro-nano-scale rough structure, significantly increasing the specific surface area and surface energy of the zirconia fibers, providing ample "anchoring points" for subsequent silicon source loading. Then, using a combination of tetraethyl orthosilicate and methyltrimethoxysilane as the silicon source, due to the difference in their hydrolysis rates, in a system catalyzed by ammonia and dispersed by anhydrous ethanol, the methyl group of methyltrimethoxysilane inhibits excessive condensation of silica, resulting in more uniform pores and better dispersion of the generated silica. Simultaneously, the composite of silica and zirconia fibers reduces self-agglomeration, and the synergistic effect of their high-temperature resistance improves dispersibility, significantly enhancing the wear resistance and mechanical properties of the abrasive material. This invention utilizes the adsorption of hydroxyl groups on the surface of the silica / zirconia fiber composite with the amino and hydroxyl groups of chitosan molecules through hydrogen bonding and electrostatic interactions, allowing chitosan to be adsorbed onto the composite surface and woven into a three-dimensional network structure. This structure is then applied in an ultrasonic-assisted process. With the assistance of this technology, it is easier for silane coupling agents to be grafted onto the surface of the composite, introducing carbon-carbon double bonds. This facilitates free radical copolymerization via an initiator, increasing the bonding strength between the composite and the organic layer. Specifically, this invention utilizes the furan ring structure of furanacrylic acid to impart a rigid framework and thermal stability. Its carboxyl groups can also enhance the interfacial bonding with diamond micropowder and inorganic fillers through polarity. The epoxy groups of glycidyl methacrylate can both undergo ring-opening crosslinking reactions with the matrix (epoxy-modified acrylate, polyurethane) and strengthen the covalent bonding at the inorganic-organic interface. Combined with methacrylate, it regulates the flexibility and compatibility of the copolymer layer, preventing excessive rigidity and embrittlement of the system. Through the synergy of these three factors, a high-hardness, strongly bonded organic layer is constructed on the surface of the inorganic filler (silica / zirconia fiber composite), improving the interfacial bonding and dispersibility of the silica / zirconia fiber composite in the organic system. Ultimately, this enhances the hardness and tensile / tear strength of the abrasive material while reducing its wear.

[0084] The above description is merely a preferred embodiment of the present invention and is not intended to limit the present invention in any way. Although the present invention has been disclosed above with reference to preferred embodiments, it is not intended to limit the present invention. Any person skilled in the art can make some modifications or alterations to the above-disclosed technical content to create equivalent embodiments without departing from the scope of the present invention. Any indirect modifications, equivalent changes, and alterations made to the above embodiments based on the technical essence of the present invention without departing from the scope of the present invention shall still fall within the scope of the present invention.

Claims

1. A diamond grinding and polishing pad, characterized in that, The abrasive comprises a grinding substrate and an abrasive layer disposed on the surface of the grinding substrate. The abrasive layer is composed of a plurality of hexagonal protrusions, which are made of abrasive material. The abrasive material includes the following components: epoxy-modified acrylate, polyurethane, modified filler, diamond powder, curing agent, silane coupling agent and dispersant. The method for preparing the modified filler includes the following steps: S1. Soak the zirconia fiber in a nitric acid aqueous solution, filter, rinse, and vacuum dry in an oven to obtain pretreated zirconia fiber; S2. The pretreated zirconia fiber is placed in a mixture of ammonia and anhydrous ethanol. A silicon source is added dropwise under stirring and heated. The mixture is then filtered, washed, and placed in an oven for vacuum drying to obtain a silica / zirconia fiber composite. S3. Spray chitosan solution onto the surface of the silica / zirconia fiber composite and then dry it. After drying, place the product in anhydrous ethanol and ultrasonically disperse it. Slowly add silane coupling agent, heat and stir, rotary evaporate to obtain the solid, and vacuum dry it to obtain the silane modified composite. S4. Mix the silane-modified composite, the reactive monomer and the organic solvent, add the initiator and stir to mix, centrifuge, take the solid, wash and dry it to obtain the modified filler.

2. The diamond grinding and polishing pad according to claim 1, characterized in that: The polishing layer is composed of several intersecting hexagonal protrusions, each with a side length of 0.5-2mm.

3. The diamond grinding and polishing pad according to claim 1, characterized in that: A groove with a depth of 0.1-0.3 mm is formed between any adjacent hexagonal protrusions, and the top and sidewall of the hexagonal protrusions are connected by a rounded transition with a radius of 0.05-0.1 mm.

4. The diamond grinding and polishing pad according to claim 1, characterized in that, The grinding material comprises the following components by weight: 40-50 parts epoxy-modified acrylate, 5-10 parts polyurethane, 20-30 parts modified filler, 10-15 parts diamond micro powder, 5-8 parts curing agent, 0.5-1 part silane coupling agent, and 0.3-0.5 parts dispersant; The preparation method of the abrasive material includes the following steps: diamond micro powder, silane coupling agent and dispersant are mixed, epoxy modified acrylate, polyurethane, modified filler and curing agent are added and stirred at high speed, vacuum degassing is performed, and the mixture is poured into a mold for curing to obtain the final product.

5. A diamond grinding and polishing pad according to claim 1, characterized in that: In step S1, the soaking time is 2-3 hours, the mass ratio of the zirconium oxide fiber to the nitric acid aqueous solution is 1.0-1.2:6.0-6.5, and the mass concentration of the nitric acid aqueous solution is 4%.

6. A diamond grinding and polishing pad according to claim 1, characterized in that: In step S2, the stirring speed is 150-200 r / min, the heating treatment is carried out at 110-120℃ and 200-280 r / min for 3-4 hours, the mass ratio of the pretreated zirconia fiber, ammonia, anhydrous ethanol and silicon source is 26-28:5-8:110-120:9-12, the concentration of the ammonia is 18 wt%, and the silicon source is composed of tetraethyl orthosilicate and methyltrimethoxysilane in a mass ratio of 2:3.8-4.

2.

7. A diamond grinding and polishing pad according to claim 1, characterized in that: In step S3, the ultrasonic dispersion is performed by ultrasonication at 300-500W power for 20-30 minutes, the heating and stirring is performed by stirring at 60-65℃ for 4-5 hours, and the mass ratio of the silica / zirconia fiber composite, chitosan solution, anhydrous ethanol and silane coupling agent is 2.4-2.8:0.9-1.2:25-30:0.2-0.

4.

8. A diamond grinding and polishing pad according to claim 1, characterized in that: In step S4, the stirring and mixing is carried out at a temperature of 65-70°C for 2-3 hours. The mass ratio of the silane-modified complex, the reactive monomer, the organic solvent, and the initiator is 10-12:5-7:50-60:0.25-0.

28. The reactive monomer is composed of furanyl acrylate, glycidyl methacrylate, and methacrylate in a mass ratio of 1:0.8-1.2:0.5-1.

0.

9. A method for preparing a diamond grinding and polishing pad as described in any one of claims 1 to 8, characterized in that, The preparation method includes using the abrasive material.

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