High-abrasion diamond abrasive tool and method for manufacturing the same

By combining nano-cerium oxide-coated diamond particles with FeCoCuSn binder and using self-made high heat-resistant resin, the problems of low bonding strength and insufficient heat resistance of diamond grinding tools were solved, resulting in diamond grinding tools with high grinding performance and long service life.

CN117444867BActive Publication Date: 2026-02-27HONGYUAN SUPER HARD MATERIALS (HENAN) CO LTD
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Patent Information

Application Number
CN202311371656.X
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-10-23
Publication Date
2026-02-27
Estimated Expiration
2043-10-23

AI Technical Summary

Technical Problem

Existing diamond abrasives suffer from problems such as low bonding strength, low grinding efficiency, and short lifespan during grinding. In particular, the insufficient heat resistance when using resin binders leads to easy softening of the abrasives and poor grinding performance.

Method used

High-grindability diamond abrasives are prepared by combining nano-cerium oxide-coated diamond particles with FeCoCuSn binder, along with self-made high-heat-resistant polyaryletherketone modified liquid crystal epoxy resin and liquid crystal epoxide zirconium oxide whiskers, through nitrogen sintering and hot pressing, thereby enhancing the wear resistance, toughness and thermal conductivity of the abrasives.

Benefits of technology

It improves the grinding performance and service life of diamond abrasives, enhances the heat resistance and thermal conductivity of the abrasives, improves grinding efficiency and machining accuracy, and avoids softening of the abrasives and burning of the workpiece at high temperatures.

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Abstract

The present application relates to the field of abrasive tools, and particularly relates to a high-grinding diamond abrasive tool and a preparation method thereof, wherein FeCoCuSn binder is combined with nano cerium oxide coated diamond particles as diamond abrasive, and is added in self-made high-heat-resistant resin; nano diamond is used as a core, cerous nitrate is used as a precursor, and a homogeneous chemical precipitation method is used to coat cerium oxide on the surface of the nano diamond; in order to improve the sintering speed of the iron-based binder, low-melting-point metal tin is introduced into the metal binder; 4-amino-3-methyl phenol and p-xylylene glycol are used to synthesize liquid crystal epoxy monomer as a high-heat-resistant resin matrix, and then amino-terminated heteronaphthalene biphenyl polyarylether ketone is introduced as a curing agent; zirconia whiskers are subjected to hydroxylation, amination and liquid crystal epoxidation, so that the zirconia whiskers can be permanently and firmly attached to the crosslinking network of the abrasive tool.
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Description

TECHNICAL FIELD

[0001] The present application relates to the field of abrasive tools, in particular to a high-grinding diamond abrasive tool and a preparation method thereof. BACKGROUND

[0002] The diamond abrasive tool itself has high wear resistance and high hardness, so that it can realize grinding processing of hard materials and brittle materials, such as being widely used in the processing field of glass, stone, semiconductor, mechanical parts, hard alloy and the like.

[0003] Ordinary diamond has a small size, and when it is applied to prepare an abrasive tool, it usually needs to be mixed with a binder. In the existing market, metal, ceramic and resin are often used as the binder. Compared with metal or ceramic binders, the resin binder has the characteristics of simple process, easy-to-obtain raw materials and the like, and has the advantages of good toughness, not easy to block, and easy to repair the abrasive tool during the grinding process. However, the surface chemical inertness of diamond itself leads to a low bonding strength with the commonly used binder, which easily causes the diamond to fall off and causes the service life of the abrasive tool to rapidly decrease. The existing process often uses phenolic resin as the binder of the resin diamond abrasive tool, but the low heat resistance of the phenolic resin will greatly reduce the grinding efficiency, thereby affecting the service life of the abrasive tool. SUMMARY

[0004] The purpose of the present application is to provide a high-grinding diamond abrasive tool and a preparation method thereof to solve the problems in the prior art.

[0005] In order to solve the above technical problems, the present application provides the following technical scheme:

[0006] A preparation method of a high-grinding diamond abrasive tool, comprising the following steps:

[0007] S1: mixing nano ceria coated diamond particles, FeCoCuSn binder and wetting agent, nitrogen sintering, crushing, granulating, sieving, to obtain diamond abrasive;

[0008] S2: mixing polyaryletherketone modified liquid crystal epoxy resin, diamond abrasive and liquid crystal zirconia whisker to obtain a mixture;

[0009] S3: drying the mixture, injecting into a mold for molding, hot pressing, to obtain a high-grinding diamond abrasive tool.

[0010] Further, the mass ratio of the nano ceria coated diamond particles, the FeCoCuSn binder and the wetting agent is 18:81:1; the wetting agent is one of anhydrous ethanol and polyvinyl alcohol.

[0011] Further, the sieving in step S1 is sieving through a 100-120 mu m sieve, and the working conditions for nitrogen sintering are: a temperature of 700-720 DEG C, and a time of 5-6 h.

[0012] Further, the FeCoCuSn binder is a FeCoCu alloy powder and tin powder compounded at a mass ratio of 9:1.

[0013] Further, the working conditions for hot pressing are: a pressure of 3 MPa, a temperature of 200-230 DEG C, and a holding time of 1-2 h.

[0014] Further, the preparation of the nano cerium oxide coated diamond particles includes the following steps: heating nano diamond powder to 495-505 DEG C for 3-4 h, after cooling, mixing the heat-treated nano diamond powder and deionized water, ultrasonic dispersion for 5-10 min, adding cerium nitrate hexahydrate and hexamethylenetetramine, ultrasonic treatment for 5-10 min, heating to 70-75 DEG C for 1-2 h, centrifugation, washing with deionized water and anhydrous ethanol for 3-5 times in turn, and drying to obtain nano cerium oxide coated diamond particles.

[0015] Further, the polyaryletherketone modified liquid crystal epoxy resin is 12-17 parts by mass, the diamond abrasive is 16-23 parts by mass, and the liquid crystal epoxy zirconia whisker is 1-2 parts by mass.

[0016] Further, the preparation of the liquid crystal epoxy zirconia whisker includes the following steps:

[0017] (1) mixing zirconia whisker and NaOH solution, ultrasonic treatment for 10-20 min, heating to 75-80 DEG C for 10-12 h, cooling, washing with deionized water until neutral, and drying to obtain hydroxylated zirconia whisker; mixing the hydroxylated zirconia whisker and toluene, ultrasonic treatment for 5-10 min, adding ammonia water and gamma-aminopropyltriethoxysilane, heating at 45-50 DEG C for 5-6 h, cooling, washing with anhydrous ethanol for 3-5 times by suction filtration, and drying to obtain amino zirconia whisker;

[0018] (2) mixing liquid crystal epoxy monomer and dimethyl sulfoxide, adding the mixture of amino zirconia whisker and dimethyl sulfoxide, ultrasonic stirring for 20-30 min, heating to 75-80 DEG C for 10-12 h under nitrogen protection, washing with dimethyl sulfoxide and anhydrous ethanol for 3-5 times in turn, suction filtration, and drying to obtain liquid crystal epoxy zirconia whisker.

[0019] Further, the preparation of the polyaryletherketone modified liquid crystal epoxy resin includes the following steps:

[0020] Mix 4-(4-hydroxyphenyl)-2,3-phthalazin-1-one, 4,4'-difluorobenzophenone, potassium carbonate, dimethyl sulfoxide, toluene, heat to 135-140 DEG C for 2-3h under nitrogen atmosphere, heat to 160 DEG C for 10-20min, heat to 170-175 DEG C for 1h, cool to 18-25 DEG C, add 4-aminophenol, potassium carbonate, dimethyl sulfoxide, toluene mixture, heat to 135-140 DEG C for 2-3h, heat to 160 DEG C for 10-20min, heat to 165 DEG C for 2-3h, cool, settle in deionized water, adjust pH to neutral, filter, wash with anhydrous ethanol and deionized water in sequence until the filtrate is neutral, dry to obtain the amino-terminated heteronaphthalene-biphenyl polyaryletherketone; mix the liquid crystal epoxy monomer and the amino-terminated heteronaphthalene-biphenyl polyaryletherketone to obtain the polyaryletherketone modified liquid crystal epoxy resin.

[0021] Further, the preparation of the liquid crystal epoxy monomer comprises the following steps: mixing 4-amino-3-methylphenol, p-xylene glycol, zinc chloride, anhydrous ethanol, heating to 75-80 DEG C for 3-4h under nitrogen atmosphere, cooling, filtering, diluting with anhydrous ethanol, drying to obtain an intermediate; mixing the intermediate, epoxy chloropropane, tetrabutylammonium chloride, dimethyl sulfoxide, heating to 75-80 DEG C for 3-4h under nitrogen atmosphere, then adding sodium hydroxide, distilling under reduced pressure, filtering and washing with deionized water and anhydrous ethanol in sequence for 3-5 times, drying to obtain the liquid crystal epoxy monomer.

[0022] The beneficial effects of the present application are as follows:

[0023] The present application provides a high-grinding diamond tool and a preparation method thereof, which comprises the following steps: mixing FeCoCuSn binder and nano cerium oxide coated diamond particles to form a diamond abrasive, and adding the diamond abrasive into a self-made high-heat-resistant resin, so that the diamond tool has the wear resistance and sharpness of super-hard materials, and has the self-sharpening property of resin materials and the toughness of metal materials, thereby greatly improving the grinding performance of the diamond tool.

[0024] In the present application, metal binder is mixed with diamond to form a diamond abrasive, in order to solve the problems of easy falling off, easy oxidation and easy scratching of the nano diamond during processing, the nano diamond is used as a core, cerium oxide is coated on the surface of the nano diamond by using homogeneous chemical precipitation method with cerium nitrate as a precursor, a low-cost iron-based binder is introduced to strengthen the strength, hardness and wear resistance of the tool, and the iron-based binder also serves as a carbide forming element to increase the holding force of the diamond, and low-melting-point tin is introduced into the metal binder to accelerate alloying in order to improve the sintering speed of the iron-based binder.

[0025] The high-heat-resistant resin is used as the binder of the diamond tool in the application, so that the heat resistance of the tool is greatly improved, the machining precision of the workpiece is better controlled, the grinding efficiency is improved, the tool is prevented from softening and sticking after long-time work, and the problem of workpiece burn caused by poor heat dissipation of the tool is avoided; the 4-amino-3-methyl phenol and the p-phenylenedimethylal are used to synthesize the liquid crystal epoxy monomer with high glass transition temperature, good fracture toughness and high bonding strength as the high-heat-resistant resin matrix, then the amino-terminated heteronaphthalene polyphenyl ether ketone with high heat resistance, good mechanical properties and radiation resistance is introduced as the curing agent, so that the diamond tool is endowed with high strength and high heat resistance, meanwhile, the multiple active sites of the self-made high-heat-resistant resin are beneficial to improving the holding force of the diamond abrasive, thereby prolonging the service life of the diamond tool.

[0026] In order to further enhance the grinding performance of the tool, the zirconia whisker is introduced in the application, in order to improve the problem that the zirconia whisker is easy to fall off during processing, the zirconia whisker is sequentially subjected to hydroxylation, amination and liquid crystal epoxidation in the application, so that it can be permanently and firmly attached to the crosslinked network in the tool, meanwhile, the introduction of the liquid crystal epoxidized zirconia whisker achieves the purpose of low amount filling and rapid heat conduction based on the synergistic effect of intrinsic-filling, so that the heat conduction performance and thermal stability of the tool are greatly improved, thereby improving the grinding performance thereof. DETAILED DESCRIPTION

[0027] The technical solutions in the application will be described clearly and completely in combination with the embodiments of the application. Obviously, the described embodiments are only part of the embodiments of the application, rather than all the embodiments. Based on the embodiments in the application, all the other embodiments obtained by those skilled in the art without creative work belong to the protection scope of the application.

[0028] It should be noted that if the embodiments of the application involve directional indications such as up, down, left, right, front, back and the like, the directional indications are only used to explain the relative position relationship, movement condition and the like between components in a certain posture, and if the certain posture changes, the directional indications also change accordingly. In addition, the technical solutions of each embodiment can be combined with each other, but it must be based on the fact that the technical solutions can be realized by those skilled in the art, and when the combination of the technical solutions appears contradictory or unachievable, it should be considered that the combination of the technical solutions does not exist and is not within the protection scope of the application.

[0029] The technical solutions of the application will be described further in detail in combination with specific embodiments. It should be understood that the following embodiments are only used to explain the application, and are not used to limit the application.

[0030] Embodiment 1: A preparation method of a high-grinding diamond tool, comprising the following steps:

[0031] S1: mixing nano cerium oxide coated diamond particles, FeCoCuSn binder, wetting agent, nitrogen sintering, crushing, granulating, sieving, to obtain diamond abrasive;

[0032] The mass ratio of nano cerium oxide coated diamond particles, FeCoCuSn binder and wetting agent is 18:81:1; the wetting agent is anhydrous ethanol; the working conditions of nitrogen sintering are: temperature is 700℃, time is 6h;

[0033] The sieving in step S1 is 100μm sieving, and the FeCoCuSn binder is a FeCoCu alloy powder compounded with tin powder at a mass ratio of 9:1;

[0034] The preparation of nano cerium oxide coated diamond particles includes the following steps: heating nano diamond powder to 495℃ for 4h, after cooling, mixing 1g of the heat-treated nano diamond powder with 200mL of deionized water, ultrasonic dispersion for 5min, adding 2g of cerium nitrate hexahydrate and 3.2g of hexamethylenetetramine, ultrasonic treatment for 5min, heating to 70℃ for 2h, centrifugation, washing with deionized water and anhydrous ethanol for 3 times respectively, and drying to obtain nano cerium oxide coated diamond particles;

[0035] S2: mixing polyaryletherketone modified liquid crystal epoxy resin, diamond abrasive and liquid crystal epoxy zirconia whisker to obtain a mixture;

[0036] In terms of mass fraction, the polyaryletherketone modified liquid crystal epoxy resin is 12 parts, the diamond abrasive is 16 parts, and the liquid crystal epoxy zirconia whisker is 1 part;

[0037] The preparation of liquid crystal epoxy monomer includes the following steps: mixing 5g of 4-amino-3-methylphenol, 1.25g of p-phenylenedimethylene, 0.75g of zinc chloride and 37mL of anhydrous ethanol, heating to 75℃ for 4h under nitrogen atmosphere, cooling, filtering, diluting with anhydrous ethanol, drying to obtain an intermediate; mixing 2g of the intermediate, 10.8g of epoxy chloropropane, 0.08g of tetrabutylammonium chloride and 2mL of dimethyl sulfoxide under nitrogen atmosphere, heating to 75℃ for 4h, then adding 0.2g of sodium hydroxide, vacuum distillation, filtering with deionized water and anhydrous ethanol for 3 times respectively, and drying to obtain the liquid crystal epoxy monomer;

[0038] The preparation of liquid crystal epoxy zirconia whisker includes the following steps:

[0039] (1) 0.6 g of zirconium oxide whisker, 100 mL of 1 mol / L NaOH solution were mixed, ultrasonic treatment was performed for 10 min, the temperature was increased to 75°C and was kept for 12 h, and then the mixture was cooled, washed with deionized water, and filtered to neutral, and dried to obtain hydroxylated zirconium oxide whisker; 0.3 g of the hydroxylated zirconium oxide whisker, 120 mL of toluene were mixed, ultrasonic treatment was performed for 5 min, 4 drops of ammonia water and 2 mL of γ-aminopropyl triethoxysilane were added dropwise, and the mixture was kept at 45°C for 6 h, and then the mixture was cooled, washed with anhydrous ethanol by filtration for 3 times, and dried to obtain amino zirconium oxide whisker;

[0040] (2) 1.4 g of liquid crystal epoxy monomer, 300 mL of dimethyl sulfoxide were mixed, 1.4 g of the amino zirconium oxide whisker and 300 mL of dimethyl sulfoxide were added, ultrasonic stirring was performed for 20 min, the temperature was increased to 75°C under nitrogen protection and was kept for 12 h, and then the mixture was sequentially washed with dimethyl sulfoxide and anhydrous ethanol for 3 times, filtered by suction, and dried to obtain liquid crystal epoxy zirconium oxide whisker;

[0041] The preparation of the polyaryletherketone modified liquid crystal epoxy resin comprises the following steps:

[0042] 10 mmol of 4-(4-hydroxyphenyl)-2,3-phthalazin-1-one, 12 mmol of 4,4'-difluorobenzophenone, 14 mmol of potassium carbonate, 7.5 mL of dimethyl sulfoxide, and 15 mL of toluene were mixed, the temperature was increased to 135°C under nitrogen atmosphere and was kept for 3 h, the temperature was increased to 160°C and was kept for 10 min, the temperature was increased to 170°C and was kept for 1 h, the temperature was decreased to 18°C, 72 mol of 4-aminophenol, 5 mmol of potassium carbonate, 2.5 mL of dimethyl sulfoxide, and 5 mL of toluene were added, the temperature was increased to 135°C and was kept for 3 h, the temperature was increased to 160°C and was kept for 10 min, the temperature was increased to 165°C and was kept for 2 h, the temperature was decreased, and the mixture was settled in deionized water, the pH was adjusted to neutral, the mixture was filtered by suction, and then the mixture was sequentially washed with anhydrous ethanol and deionized water until the filtrate was neutral, and then the mixture was dried to obtain amino-terminated heterophthalophenyl polyaryletherketone; 2.1 g of liquid crystal epoxy monomer and 1.4 g of the amino-terminated heterophthalophenyl polyaryletherketone were mixed to obtain polyaryletherketone modified liquid crystal epoxy resin;

[0043] S3: The mixture was dried, was put into a mold, and was injection molded to form a high grinding diamond tool, and the hot pressing was performed at a pressure of 3 MPa and a temperature of 200°C for 2 h.

[0044] Example 2: A preparation method of a high grinding diamond tool, comprising the following steps:

[0045] S1: Diamond abrasive was obtained by mixing nano cerium oxide coated diamond particles, FeCoCuSn binder, and wetting agent, nitrogen sintering, crushing, granulating, and sieving;

[0046] The mass ratio of nanometer cerium oxide coated diamond particles, FeCoCuSn binder, and wetting agent is 18:81:1; the wetting agent is anhydrous ethanol; the working conditions of nitrogen sintering are: temperature is 710 DEG C, time is 5.5 h;

[0047] The sieving in step S1 is sieving through a 110 μm sieve, and the FeCoCuSn binder is a FeCoCu alloy powder compounded with tin powder at a mass ratio of 9:1;

[0048] The preparation of nanometer cerium oxide coated diamond particles includes the following steps: heating nanometer diamond powder to 500 DEG C for 3.5 h, after cooling, mixing 1 g of the heat-treated nanometer diamond powder with 200 mL of deionized water, ultrasonic dispersion for 5 min, adding 2 g of cerium nitrate hexahydrate and 3.2 g of hexamethylenetetramine, ultrasonic treatment for 8 min, heating to 72 DEG C for 1.5 h, centrifugation, washing with deionized water and anhydrous ethanol 4 times in turn, and drying to obtain nanometer cerium oxide coated diamond particles;

[0049] S2: mixing the polyaryletherketone modified liquid crystal epoxy resin, the diamond abrasive, and the liquid crystal epoxy zirconia whisker to obtain a mixture;

[0050] In terms of mass fraction, the polyaryletherketone modified liquid crystal epoxy resin is 14 parts, the diamond abrasive is 17 parts, and the liquid crystal epoxy zirconia whisker is 1.5 parts;

[0051] The preparation of the liquid crystal epoxy monomer includes the following steps: mixing 5 g of 4-amino-3-methylphenol, 1.25 g of p-phenylenedimethylaldehyde, 0.75 g of zinc chloride, and 37 mL of anhydrous ethanol, heating to 78 DEG C for 3.5 h under a nitrogen atmosphere, cooling, filtering, diluting with anhydrous ethanol, and drying to obtain an intermediate; mixing 2 g of the intermediate, 10.8 g of epoxy chloropropane, 0.08 g of tetrabutylammonium chloride, and 2 mL of dimethyl sulfoxide under a nitrogen atmosphere, heating to 78 DEG C for 3.5 h, then adding 0.2 g of sodium hydroxide, vacuum distillation, filtering with deionized water and anhydrous ethanol 4 times in turn, and drying to obtain the liquid crystal epoxy monomer

[0052] The preparation of the liquid crystal epoxy zirconia whisker includes the following steps:

[0053] (1) mixing 0.6 g of zirconia whisker and 100 mL of 1 mol / L NaOH solution, ultrasonic treatment for 15 min, heating to 78 DEG C for 11 h, cooling, washing with deionized water until neutral, and drying to obtain hydroxylated zirconia whisker; mixing 0.3 g of the hydroxylated zirconia whisker and 120 mL of toluene, ultrasonic treatment for 8 min, adding 4 drops of ammonia water and 2 mL of γ-aminopropyltriethoxysilane dropwise, heating to 48 DEG C for 5.5 h, cooling, washing with anhydrous ethanol by filtration 4 times, and drying to obtain amino zirconia whisker;

[0054] (2) 1.4 g of liquid crystal epoxy monomer, 300 mL of dimethyl sulfoxide were mixed, and then 1.4 g of amino zirconium oxide whisker mixed with 300 mL of dimethyl sulfoxide was added, and ultrasonic stirring was performed for 25 min. Under the protection of nitrogen, the temperature was raised to 78℃ and kept for 11 h. Then, the mixture was washed with dimethyl sulfoxide and anhydrous ethanol for 4 times, respectively, and then was filtered and dried to obtain the liquid crystal epoxy zirconium oxide whisker;

[0055] The preparation of the polyaryletherketone modified liquid crystal epoxy resin comprises the following steps:

[0056] 10 mmol of 4-(4-hydroxyphenyl)-2,3-phthalazin-1-one, 12 mmol of 4,4'-difluorobenzophenone, 14 mmol of potassium carbonate, 7.5 mL of dimethyl sulfoxide, and 15 mL of toluene were mixed, and then the mixture was heated to 138℃ and kept for 2.5 h. Then, the mixture was heated to 160℃ and kept for 15 min, and then was heated to 173℃ and kept for 1 h. Then, the mixture was cooled to 20℃, and then 72 mol of 4-aminophenol, 5 mmol of potassium carbonate, 2.5 mL of dimethyl sulfoxide, and 5 mL of toluene were added. Then, the mixture was heated to 138℃ and kept for 2.5 h. Then, the mixture was heated to 160℃ and kept for 15 min, and then was heated to 165℃ and kept for 2.5 h. Then, the mixture was cooled and was settled in deionized water. The pH of the mixture was adjusted to neutral. Then, the mixture was filtered and was washed with anhydrous ethanol and deionized water, respectively, until the filtrate was neutral. Then, the mixture was dried to obtain the amino-terminated phthalazinyl biphenyl polyaryletherketone. Then, 2.1 g of liquid crystal epoxy monomer and 1.4 g of the amino-terminated phthalazinyl biphenyl polyaryletherketone were mixed to obtain the polyaryletherketone modified liquid crystal epoxy resin.

[0057] S3: The mixture was dried and was injected into a mold to be molded. Hot pressing was performed at a pressure of 3 MPa and a temperature of 220℃ for 1.5 h to obtain the high-grinding diamond tool.

[0058] Embodiment 3: A method for preparing a high-grinding diamond tool, comprising the following steps:

[0059] S1: Diamond particles coated with nano cerium oxide, FeCoCuSn binder, and wetting agent were mixed, and then were sintered under nitrogen. Then, the mixture was crushed, granulated, and sieved to obtain the diamond abrasive;

[0060] The mass ratio of the diamond particles coated with nano cerium oxide, the FeCoCuSn binder, and the wetting agent was 18:81:1. The wetting agent was anhydrous ethanol. The working conditions of the nitrogen sintering were as follows: the temperature was 720℃, and the time was 5 h.

[0061] In step S1, the sieving was performed through a 120 μm sieve. The FeCoCuSn binder was a FeCoCu alloy powder and tin powder which were compounded at a mass ratio of 9:1.

[0062] The preparation of the nano cerium oxide coated diamond particles comprises the following steps: heating nano diamond powder to 505 DEG C for 3h, after cooling, mixing 1g of the heat-treated nano diamond powder with 200mL of deionized water, ultrasonic dispersion for 10min, adding 2g of cerium nitrate hexahydrate and 3.2g of hexamethylenetetramine, ultrasonic treatment for 10min, heating to 75 DEG C for 1h, centrifugation, washing with deionized water and anhydrous ethanol for 5 times in sequence, drying, and obtaining the nano cerium oxide coated diamond particles;

[0063] S2: mixing the polyaryletherketone modified liquid crystal epoxy resin, the diamond abrasive, and the liquid crystal epoxy zirconia whisker to obtain a mixture;

[0064] The polyaryletherketone modified liquid crystal epoxy resin is 17 parts, the diamond abrasive is 23 parts, and the liquid crystal epoxy zirconia whisker is 2 parts in terms of mass fraction;

[0065] The preparation of the liquid crystal epoxy monomer comprises the following steps: mixing 5g of 4-amino-3-methylphenol, 1.25g of p-phthaldehyde, 0.75g of zinc chloride, and 37mL of anhydrous ethanol, heating to 80 DEG C for 3h under nitrogen atmosphere, cooling, filtering, diluting with anhydrous ethanol, drying, and obtaining an intermediate; mixing 2g of the intermediate, 10.8g of epoxy chloropropane, 0.08g of tetrabutylammonium chloride, and 2mL of dimethyl sulfoxide, adding 0.2g of sodium hydroxide after heating at 80 DEG C for 3h under nitrogen atmosphere, performing vacuum distillation, filtering and washing with deionized water and anhydrous ethanol for 5 times in sequence, and drying to obtain the liquid crystal epoxy monomer;

[0066] The preparation of the liquid crystal epoxy zirconia whisker comprises the following steps:

[0067] (1) mixing 0.6g of zirconia whisker and 100mL of 1mol / L NaOH solution, ultrasonic treatment for 10-20min, heating to 80 DEG C for 10h, cooling, washing with deionized water until neutral, and drying to obtain the hydroxylated zirconia whisker; mixing 0.3g of the hydroxylated zirconia whisker and 120mL of toluene, ultrasonic treatment for 10min, adding 4 drops of ammonia water and 2mL of γ-aminopropyl triethoxysilane, heating at 50 DEG C for 5h, cooling, and performing filtration and washing with anhydrous ethanol for 5 times, and drying to obtain the aminated zirconia whisker;

[0068] (2) mixing 1.4g of the liquid crystal epoxy monomer and 300mL of dimethyl sulfoxide, adding a mixture of 1.4g of the aminated zirconia whisker and 300mL of dimethyl sulfoxide, ultrasonic stirring for 30min, heating to 80 DEG C for 10h under nitrogen protection, washing with dimethyl sulfoxide and anhydrous ethanol for 5 times in sequence, performing filtration and drying to obtain the liquid crystal epoxy zirconia whisker;

[0069] The preparation of the polyaryletherketone modified liquid crystal epoxy resin comprises the following steps:

[0070] Mixing 10 mmol of 4-(4-hydroxyphenyl)-2,3-phthalazin-1-one, 12 mmol of 4,4'-difluorobenzophenone, 14 mmol of potassium carbonate, 7.5 mL of dimethyl sulfoxide, 15 mL of toluene under a nitrogen atmosphere, heating to 140°C for 2 h, heating to 160°C for 20 min, heating to 175°C for 1 h, cooling to 25°C, adding 72 mol of 4-aminophenol, 5 mmol of potassium carbonate, 2.5 mL of dimethyl sulfoxide, 5 mL of toluene, heating to 140°C for 2 h, heating to 160°C for 20 min, heating to 165°C for 3 h, cooling, settling in deionized water, adjusting the pH to neutral, suction filtration, washing with anhydrous ethanol and deionized water in sequence until the filtrate is neutral, drying, to obtain an amino-terminated heteronaphthalene biphenyl polyarylether ketone; mixing 2.1 g of the liquid crystal epoxy monomer and 1.4 g of the amino-terminated heteronaphthalene biphenyl polyarylether ketone to obtain a polyarylether ketone modified liquid crystal epoxy resin;

[0071] S3: drying the mixture, placing it in a mold, and injection molding, hot pressing at a pressure of 3 MPa and a temperature of 230°C for 1 h, to obtain a high-grinding diamond tool.

[0072] Comparative Example 1: using Example 3 as a control group, replacing the nanometer cerium oxide coated diamond particles with nanometer diamond, and the other procedures being normal.

[0073] Comparative Example 2: using Example 3 as a control group, the mass ratio of nanometer cerium oxide coated diamond particles, FeCoCuSn binder, and wetting agent being 20:79:1, and the other procedures being normal.

[0074] Comparative Example 3: using Example 3 as a control group, replacing the polyarylether ketone modified liquid crystal epoxy resin with phenolic resin (9003-35-4: Pandeng (Shanghai) International Trade Co., Ltd.), and the other procedures being normal.

[0075] Comparative Example 4: using Example 3 as a control group, without preparing the amino-terminated heteronaphthalene biphenyl polyarylether ketone, and the other procedures being normal.

[0076] Comparative Example 5: using Example 3 as a control group, replacing the liquid crystal epoxy zirconia whisker with zirconia whisker, and the other procedures being normal.

[0077] Raw material sources:

[0078] FeCoCu alloy powder (8 μm): Beijing Youyan New Material Co., Ltd.; nano-diamond powder (99%, 5 nm): Hubei Yunmagnesium Technology Co., Ltd.; 4-(4-hydroxyphenyl)-2,3-naphthalen-1-one (industrial grade): Dalian Polysciences New Material Co., Ltd.; 4-aminophenol (99%): Wuhan Xinxinjiali Biological Technology Co., Ltd.; tin powder T283639, cerium nitrate hexahydrate C105376, hexamethylenetetramine H431222, 4-amino-3-methylphenol A121773, p-xylylene P105980, zinc chloride Z112527, epichlorohydrin E108182, tetrabutylammonium chloride T101036, zirconia whisker Z431828, gamma-aminopropyltriethoxysilane A107148, dimethyl sulfoxide D103272, 4,4'-difluorobenzophenone M106424: Aldrich reagent; anhydrous ethanol, sodium hydroxide, toluene, ammonia, potassium carbonate, analytical pure: National Pharmaceutical Group Reagent.

[0079] Performance test:

[0080] The sample size was 30 mm x 12 mm x 6 mm; the bending strength was tested on a universal testing machine with a span of 26 mm and a speed of 0.1 mm / min; the thermal conductivity was the resistance to high temperature; the sample was kept at 350°C for 2h, and the bending strength was measured again, and the change rate was used to characterize the resistance to high temperature; the DHM-2 type abrasion ratio tester was used to determine the abrasion ratio of the sample block, and a 200 mm x 25 mm x 32 mm A80k brown corundum grinding wheel (A represents that the grinding wheel material is brown corundum, 80 represents the particle size of the grinding wheel, and k indicates that the hardness of the grinding wheel is medium soft) was used, the grinding wheel linear speed was 35 m / s, the grinding pressure was 2 N, and the sample grinding time was 10 min; the results are shown in Table 1.

[0081] Table 1

[0082]

[0083]

[0084] Comparing Example 3 with Comparative Example 1, the metal binder and diamond are compounded as diamond abrasive in the application, in order to improve the problems of easy falling off, easy oxidation and easy scratching of workpieces during processing of nano-diamond, the nano-diamond is used as the core, cerium nitrate is used as the precursor, and the homogeneous chemical precipitation method is used to coat cerium oxide on the surface of the nano-diamond, so as to improve the performance of the grinding tool.

[0085] Comparing example 3 with comparative example 2, a low-cost iron-based binder is introduced to strengthen the strength, hardness and wear resistance of the abrasive tool, and also acts as a carbide forming element to increase the holding force on the diamond, in order to improve the sintering speed of the iron-based binder, low-melting-point metal tin is introduced into the metal binder to accelerate alloying, and by controlling the coating of nano cerium oxide on the diamond particles, the performance of the abrasive tool is improved.

[0086] Comparing example 3 with comparative examples 3 and 4, the self-made high-heat-resistant resin is used as the binder of the diamond abrasive tool in the application to greatly improve the heat resistance of the abrasive tool, better control the machining precision of the workpiece, improve the grinding efficiency, avoid the softening and sticking of the abrasive tool after long-time work, and avoid the problem of workpiece burning caused by poor heat dissipation of the abrasive tool; the high-heat-resistant resin matrix is synthesized by 4-amino-3-methylphenol and p-phenylenedimethylaldehyde, which has high glass transition temperature, good fracture toughness and high bonding strength, and then the amino-terminated heteronaphthalene biphenyl polyarylether ketone with high heat resistance, good mechanical properties and radiation resistance is introduced as a curing agent, which gives the diamond abrasive tool high strength and high heat resistance, and the multiple active sites of the self-made high-heat-resistant resin are beneficial to improve the holding force on the diamond abrasive, thereby prolonging the service life of the diamond abrasive tool.

[0087] Comparing example 3 with comparative example 5, in order to further enhance the grinding performance of the abrasive tool, zirconia whiskers are introduced in the application, in order to improve the problem that the zirconia whiskers are easy to fall off during processing, the zirconia whiskers are sequentially hydroxylated, aminated and liquid-crystal-epoxidized in the application, so that they can be permanently and firmly attached to the cross-linked network in the abrasive tool, and the introduction of liquid-crystal-epoxidized zirconia whiskers based on the synergistic effect of intrinsic-filling achieves the purpose of low-amount filling and rapid heat conduction, greatly improves the heat conduction performance and thermal stability of the abrasive tool, and thereby improves its grinding performance.

[0088] The above is only an embodiment of the application, and does not limit the patent scope of the application, any equivalent structural transformation made according to the inventive concept of the application, or direct / indirect application in other related technical fields is included in the patent protection scope of the application.

Claims

1. A method for preparing a diamond abrasive with high grindability, characterized in that, Includes the following steps: S1: Mix nano-cerium oxide-coated diamond particles, FeCoCuSn binder, and wetting agent, sinter with nitrogen, crush, granulate, and sieve to obtain diamond abrasive. S2: Mix polyaryletherketone modified liquid crystal epoxy resin, diamond abrasive, and liquid crystal epoxide zirconia whiskers to obtain a mixture; S3: Dry the mixture, put it into a mold for injection molding, and hot press to obtain a diamond abrasive with high abrasiveness. The preparation of polyaryletherketone modified liquid crystal epoxy resin includes the following steps: Mix 4-(4-hydroxyphenyl)-2,3-diazanaphthyl-1-one, 4,4'-difluorobenzophenone, potassium carbonate, dimethyl sulfoxide, and toluene. Under a nitrogen atmosphere, heat to 135-140℃ and hold for 2-3 hours, then heat to 160℃ and hold for 10-20 minutes, then heat to 170-175℃ and hold for 1 hour. Cool to 18-25℃, add a mixture of 4-aminophenol, potassium carbonate, dimethyl sulfoxide, and toluene, and heat again. The mixture is heated to 135-140℃ and held for 2-3 hours, then heated to 160℃ and held for 10-20 minutes, then heated to 165℃ and held for 2-3 hours. After cooling, the mixture is allowed to settle into deionized water, the pH is adjusted to neutral, and the mixture is filtered. It is then washed successively with anhydrous ethanol and deionized water until the filtrate is neutral and dried to obtain amino-terminated heteronaphthyl biphenyl polyaryletherketone. The liquid crystal epoxy monomer and the amino-terminated heteronaphthyl biphenyl polyaryletherketone are mixed to obtain polyaryletherketone modified liquid crystal epoxy resin.

2. The method for preparing a high-grindability diamond abrasive according to claim 1, characterized in that, In step S1, the sieving is done through a 100-120µm sieve. The working conditions for nitrogen sintering are: temperature 700-720℃, time 5-6h.

3. The method for preparing a high-grindability diamond abrasive according to claim 1, characterized in that, The mass ratio of nano-cerium oxide-coated diamond particles, FeCoCuSn binder, and wetting agent is 18:81:1; the wetting agent is either anhydrous ethanol or polyvinyl alcohol.

4. The method for preparing a high-grindability diamond abrasive according to claim 1, characterized in that, The FeCoCuSn binder is obtained by compounding FeCoCu alloy powder and tin powder in a mass ratio of 9:

1.

5. The method for preparing a high-grindability diamond abrasive according to claim 1, characterized in that, The preparation of nano-cerium oxide-coated diamond particles includes the following steps: heating nano-diamond powder to 495-505℃ and holding for 3-4 hours, cooling, mixing the heat-treated nano-diamond powder with deionized water, ultrasonically dispersing for 5-10 minutes, adding cerium nitrate hexahydrate and hexamethylenetetramine, ultrasonically treating for 5-10 minutes, heating to 70-75℃ and holding for 1-2 hours, centrifuging, washing with deionized water and anhydrous ethanol 3-5 times in sequence, and drying to obtain nano-cerium oxide-coated diamond particles.

6. The method for preparing a high-grindability diamond abrasive according to claim 1, characterized in that, By weight, the composition is 12-17 parts of polyaryletherketone modified liquid crystal epoxy resin, 16-23 parts of diamond abrasive, and 1-2 parts of liquid crystal epoxide zirconia whiskers.

7. The method for preparing a high-grindability diamond abrasive according to claim 1, characterized in that, The preparation of liquid crystal epoxide zirconia whiskers includes the following steps: (1) Mix zirconia whiskers with NaOH solution, sonicate for 10-20 min, heat to 75-80℃ and keep warm for 10-12 h, cool, wash with deionized water and filter until neutral, dry to obtain hydroxylated zirconia whiskers; mix hydroxylated zirconia whiskers with toluene, sonicate for 5-10 min, add ammonia and γ-aminopropyltriethoxysilane, keep warm at 45-50℃ for 5-6 h, cool, filter and wash with anhydrous ethanol 3-5 times, dry to obtain aminated zirconia whiskers; (2) Mix liquid crystal epoxy monomer and dimethyl sulfoxide, add a mixture of aminated zirconia whiskers and dimethyl sulfoxide, stir ultrasonically for 20-30 min, heat to 75-80℃ and keep warm for 10-12 h under nitrogen protection, wash with dimethyl sulfoxide and anhydrous ethanol 3-5 times in sequence, filter, dry to obtain liquid crystal epoxide zirconia whiskers.

8. The method for preparing a high-grindability diamond abrasive according to claim 1, characterized in that, The preparation of the liquid crystal epoxy monomer includes the following steps: 4-amino-3-methylphenol, terephthalaldehyde, zinc chloride, and anhydrous ethanol are mixed and heated to 75-80℃ for 3-4 hours under a nitrogen atmosphere. After cooling, the mixture is filtered, diluted with anhydrous ethanol, filtered again, and dried to obtain an intermediate. The intermediate, epichlorohydrin, tetrabutylammonium chloride, and dimethyl sulfoxide are mixed and heated to 75-80℃ for 3-4 hours under a nitrogen atmosphere. Sodium hydroxide is added, and the mixture is distilled under reduced pressure. The mixture is then washed 3-5 times with deionized water and anhydrous ethanol, and dried to obtain the liquid crystal epoxy monomer.

9. A diamond abrasive with high grindability, characterized in that, It is prepared by the preparation method described in any one of claims 1-8.

Citation Information

Patent Citations

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