CN110421494B - Resin metal composite mirror grinding wheel based on sol-gel method and preparation method thereof - Google Patents
Resin metal composite mirror grinding wheel based on sol-gel method and preparation method thereof Download PDFInfo
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- CN110421494B CN110421494B CN201910716714.5A CN201910716714A CN110421494B CN 110421494 B CN110421494 B CN 110421494B CN 201910716714 A CN201910716714 A CN 201910716714A CN 110421494 B CN110421494 B CN 110421494B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24D—TOOLS FOR GRINDING, BUFFING OR SHARPENING
- B24D18/00—Manufacture of grinding tools or other grinding devices, e.g. wheels, not otherwise provided for
- B24D18/0009—Manufacture of grinding tools or other grinding devices, e.g. wheels, not otherwise provided for using moulds or presses
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24D—TOOLS FOR GRINDING, BUFFING OR SHARPENING
- B24D3/00—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents
- B24D3/02—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents the constituent being used as bonding agent
- B24D3/20—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents the constituent being used as bonding agent and being essentially organic
- B24D3/28—Resins or natural or synthetic macromolecular compounds
- B24D3/32—Resins or natural or synthetic macromolecular compounds for porous or cellular structure
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24D—TOOLS FOR GRINDING, BUFFING OR SHARPENING
- B24D3/00—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents
- B24D3/34—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents characterised by additives enhancing special physical properties, e.g. wear resistance, electric conductivity, self-cleaning properties
- B24D3/342—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents characterised by additives enhancing special physical properties, e.g. wear resistance, electric conductivity, self-cleaning properties incorporated in the bonding agent
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24D—TOOLS FOR GRINDING, BUFFING OR SHARPENING
- B24D3/00—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents
- B24D3/34—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents characterised by additives enhancing special physical properties, e.g. wear resistance, electric conductivity, self-cleaning properties
- B24D3/346—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents characterised by additives enhancing special physical properties, e.g. wear resistance, electric conductivity, self-cleaning properties utilised during polishing, or grinding operation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24D—TOOLS FOR GRINDING, BUFFING OR SHARPENING
- B24D7/00—Bonded abrasive wheels, or wheels with inserted abrasive blocks, designed for acting otherwise than only by their periphery, e.g. by the front face; Bushings or mountings therefor
- B24D7/02—Wheels in one piece
Abstract
The invention discloses a preparation method of a resin metal composite mirror grinding wheel based on a sol-gel method, and belongs to the field of precision machining, grinding and polishing. In the preparation process, adding water-soluble resin into polyvinyl alcohol glue to obtain mixed glue, and then adding the mixed glue into diamond micro powder, water-resistant aluminum nitride micro powder, electrolytic copper powder, filler and additive to prepare a suspension by dispersing and mixing to prepare slurry; and pouring the slurry into a grinding wheel die to prepare the grinding wheel, and shaping and finishing the grinding wheel. The mirror grinding wheel prepared by the polyvinyl alcohol and water-soluble resin mixed glue hydrosol gel has the characteristics of uniform diamond distribution and through capillary micropores, soluble aluminum nitride with a waterproof coating is added, after the waterproof coating of aluminum nitride particles on the surface layer of the mirror grinding wheel is ground, the aluminum nitride is hydrolyzed, the strength is reduced, the mirror grinding wheel has the effect of self-sharpening of the surface layer, and the aluminum nitride waterproof coating inside the mirror grinding wheel is protected, so that the stability of the internal strength of the mirror grinding wheel is ensured.
Description
Technical Field
The invention belongs to the field of precision machining grinding and polishing, and relates to a resin metal composite mirror grinding wheel based on a sol-gel method and a preparation method thereof.
Background
The mirror grinding refers to the mirror grinding, wherein the surface roughness Ra of the ground workpiece is not more than 0.01 mu m, and the mirror grinding can be used for clearly imaging if light is mirror-like. The mirror surface grinding mainly comprises the steps that abrasive particle micro-blades remove the allowance of the surface of a workpiece, and meanwhile, the abrasive material becomes dull due to abrasion, so that the friction, extrusion, calendaring and polishing effects are generated on the surface of the workpiece. Therefore, two measures are generally adopted for realizing mirror surface grinding, firstly, a grinding wheel of fine grinding materials is adopted, an elastic grinding wheel of rubber bonding agents is used for extrusion polishing, and the mirror surface is achieved, and the mirror surface grinding only needs five procedures of rough grinding, finish grinding, semi-finish grinding, ultra-precision grinding and mirror surface grinding to achieve mirror surface processing; one is to use coarse-grained grinding material to carry out dressing, and through slow dressing, the cutting edge of the grinding material is trimmed to be flat, the flatter the surface of the grinding wheel is, the lower the roughness after grinding is. The primary reason for achieving a mirror surface with this approach is the excision by the microedges.
The traditional grinding wheel manufacturing method comprises powder mixing → sieving → drying → pressing → sintering, the problem of phase agglomeration is easy to occur, and how to reduce the internal defects of the abrasive grain grinding tool and ensure the uniformity of the grinding tool tissue is the first problem to be compelled, because the uniformity of the internal tissue directly influences the polishing performance. Meanwhile, the traditional grinding tool has the problem that the grinding tool is passivated after being used for a long time, so that the mirror surface grinding wheel needs to be designed to have the self-sharpening function.
The invention patent with the publication number of 106944939B discloses a self-sharpening superhard superfine grinding tool pellet added with soluble resin materials and a preparation method thereof, the soluble resin materials on the surface layer of the grinding tool are dissolved by grinding fluid, pores are formed among binding agents, and the purposes of reducing the strength of the binding agents and the holding force of the binding agents on surrounding abrasive particles are achieved, so that the purpose of automatically and controllably sharpening the grinding tool on line is achieved, but the method is easy to dissolve the resin generated inside the pellet, so that swelling is caused, and the strength is reduced; the invention patent with the publication number of 104944956A discloses a preparation method of a polycrystalline nano-diamond grinding tool based on gel reaction, and the method adopts polyacrylonitrile for gelling, has high hardness and is suitable for a grinding stage; the invention patent publication 108081159a discloses a method for forming a polyvinyl acetal resin abrasive organogel that is not suitable for aqueous systems, and that is not carbonized to form capillary pores with a single resin.
In order to solve the problems of phase agglomeration, capillary pore formation and self-sharpening of the diamond mirror grinding wheel, the invention adopts composite resin gel molding, one resin is sintered and cured, and the other resin is carbonized to generate capillary micropores; the hydrolyzable filler of the water-resistant coating is added, so that in the grinding process, surface friction, wiping of the water-resistant coating, filler hydrolysis, reduction of bonding strength and falling of passivated abrasive particles are realized, the filler in the grinding wheel cannot hydrolyze under the protection of the water-resistant coating, and the strength of a matrix is ensured.
Disclosure of Invention
According to the invention, the mirror grinding wheel is manufactured by using the polyvinyl alcohol (PVA) and the water-soluble resin liquid gel, so that the problem of uneven powder forming and dispersing is avoided. Firstly, forming a gel biscuit by utilizing the physical gelling capacity of PVA, solidifying the water-soluble resin after sintering, carbonizing the PVA, wherein the sintering and solidifying temperature of the water-soluble resin is also the PVA carbonizing temperature, and generating a large number of capillary micropores after carbonizing the PVA, compared with a hole generated by directly adding a pore-forming agent in powder molding, the capillary micropores generated in the mirror grinding wheel by the method are through micropores and have strong water absorption capacity; because the capillary micropores in the mirror grinding wheel have water absorption capacity, the aluminum nitride coated with the water-resistant nano silicon dioxide coating in the mirror grinding wheel can avoid direct hydrolysis, and the strength of the mirror grinding wheel matrix is maintained.
In order to achieve the purpose, the invention adopts the following technical scheme:
step 1: preparing water-resistant aluminum nitride powder with a silicon dioxide film layer on the surface;
step 2: dispersing diamond powder, water-resistant aluminum nitride powder, electrolytic copper powder, a filler and an additive in water to prepare a suspension;
and step 3: under the condition of 90 ℃ water bath, dissolving polyvinyl alcohol in a mixed solvent of water and ethanol to obtain polyvinyl alcohol glue, adding water-soluble resin liquid into the polyvinyl alcohol glue to obtain mixed glue, wherein the weight ratio of the polyvinyl alcohol glue to the water-soluble resin liquid in the mixed glue is 1: 1-6; adding the mixed glue into the suspension prepared in the step 2, and stirring while adding to obtain glue-containing slurry;
and 4, step 4: pouring the slurry containing the rubber into a grinding wheel mold, freezing for 1-3 hours at the temperature of-25 to-15 ℃, naturally drying for 5-10 hours after thawing, taking out a blank from the grinding wheel mold, performing densification treatment, drying for 24-48 hours at the temperature of 45-65 ℃, sintering, and cooling to obtain a grinding wheel semi-finished product with micro pores;
and 5: and (4) carrying out grinding wheel dressing on the grinding wheel semi-finished product obtained in the step (4) on a grinding machine, then installing the dressed grinding wheel semi-finished product on the grinding machine, adding grinding fluid into a machining area, adding the grinding fluid to carry out grinding working surface dressing on the grinding wheel, wherein the flow rate of the grinding fluid is 100-500 ml/min, and preparing the mirror surface grinding wheel.
Further, the step 1 specifically comprises:
mixing 1-10 parts by weight of aluminum nitride powder and 50 parts by weight of absolute ethyl alcohol, heating to 40 ℃ under the condition of water bath, and uniformly stirring to obtain an aluminum nitride ethyl alcohol dispersion liquid; dropwise adding 3-6 parts of tetraethoxysilane diluted by 30 parts of absolute ethyl alcohol, 4-6 parts of ammonia water diluted by 30 parts of absolute ethyl alcohol and 5 parts of water into the aluminum nitride ethanol dispersion liquid at the dropping speed of 1-2 drops/second, then carrying out gel reaction for 6 hours at the temperature of 35-45 ℃, carrying out vacuum filtration, washing the product for 3 times by using the absolute ethyl alcohol, naturally drying the obtained product for 12-24 hours at the room temperature, then calcining for 2 hours at the temperature of 300 ℃, cooling and then sieving by using a 200-mesh sieve to obtain the water-resistant aluminum nitride powder with the silicon dioxide film layer on the surface. The aluminum nitride can be hydrolyzed in water, the hydrolysis speed of the aluminum nitride can be adjusted under alkaline or acidic conditions, the aluminum nitride in the grinding wheel can be prevented from being hydrolyzed by coating a layer of silicon dioxide, and the aluminum nitride on the surface layer can be hydrolyzed under friction conditions.
Further, the step 2 specifically comprises:
adding 5-10 parts by weight of 0.5-5 micron diamond powder, 1-3 parts by weight of water-resistant aluminum nitride powder, 10-30 parts by weight of 200-1000 mesh electrolytic copper powder, 5-10 parts by weight of filler and 1-5 parts by weight of additive into 20-50 parts by weight of water, and dispersing by using a planetary ball mill, wherein a dispersion medium is zirconia microspheres to prepare a suspension; the filler is any one or more of copper-coated graphite, talcum powder, cryolite, cerium oxide, aluminum oxide powder, calcium carbonate, calcium oxide, zinc oxide, barium sulfate, magnesium oxide and molybdenum disulfide; the additive comprises a wetting agent, a dispersing agent, an organic silicon defoaming agent and a dimethyl silicon oil release agent, wherein the addition amount of the wetting agent is 0.1-1 wt% of the dry weight of the sizing agent, the addition amount of the dispersing agent is 0.1-1.5 wt% of the dry weight of the sizing agent, the addition amount of the organic silicon defoaming agent is 0.1-1 wt% of the dry weight of the sizing agent, the addition amount of the dimethyl silicon oil release agent is 0.1-1 wt% of the dry weight of the sizing agent, the wetting agent is any one of alkyl sulfate, sulfonate, fatty acid ester sulfate, carboxylic acid soap and phosphate ester anionic surfactant or polyoxyethylene alkylphenol ether, polyoxyethylene fatty alcohol ether and polyoxyethylene polyoxypropylene segmented copolymer nonionic surfactant, and the dispersing agent is phosphate ester dispersing agent, ethoxy compound dispersing agent, polyacrylate dispersing agent, polyester dispersing agent, polyether dispersing agent, polyoxyethylene polyoxypropylene segmented copolymer nonionic surfactant, and dimethyl, Any one of polyolefin dispersant, sodium carbonate, sodium orthophosphate or herring oil.
Further, in the step 3, the weight ratio of water to ethanol in the polyvinyl alcohol glue is 3-10: 1, and the solid content of polyvinyl alcohol is 5-15 wt%; the water-soluble resin is one or more of water-soluble epoxy resin, water-soluble polyimide resin or water-soluble phenolic resin, and the solid content of the water-soluble resin liquid is 40-60 wt%; the dry weight of the mixed glue is 5-15 wt% of the dry weight of the glue-containing slurry.
Further, the grinding wheel die in the step 4 is cylindrical or circular; the densification treatment is cold isostatic pressing, and the pressure is 5-50 MPa; and the sintering is specifically to place the blank in an oven, firstly heat up to 75 ℃ and preserve heat for 1 hour, then heat up to 115 ℃ and preserve heat for 1.5 hours, then heat up to 150-180 ℃ and preserve heat for 1 hour, finally heat up to 180-230 ℃ and preserve heat for 30min, the polyvinyl alcohol glue is thermally decomposed to form uniform capillary micropores, the water-soluble resin is solidified, and the grinding wheel semi-finished product with the micro pores is obtained after cooling.
Further, in the step 5, the ceramic bond grinding wheel with the granularity of 60-100 is adopted for the grinding wheel dressing, and redundant rim charge of the semi-finished grinding wheel product obtained in the step 4 is removed, so that the size precision of the semi-finished grinding wheel product reaches 0.01-0.05 mm.
In addition, the mirror surface grinding wheel in the step 5 comprises an end surface grinding wheel and an external grinding wheel, if the end surface of the trimmed semi-finished grinding wheel is used as a grinding wheel grinding working surface, the end surface of the semi-finished grinding wheel is installed on a grinding wheel base to carry out end surface mirror surface grinding, the end surface grinding wheel is obtained, and the feed rate of the end surface mirror surface grinding is 0.002 mm/min; if the excircle surface of the trimmed grinding wheel semi-finished product is used as a grinding working surface of the grinding wheel, and the center hole of the grinding wheel semi-finished product is arranged on a grinding wheel spindle for excircle mirror surface grinding, the excircle grinding wheel is obtained, wherein the back bite of the excircle mirror surface grinding is 0.001-0.005 mm, the transverse feed is 0.2-0.5 mm/min, and the longitudinal feed is 10-20 m/min;
the grinding fluid is added to finish the grinding working surface of the grinding wheel, and the method specifically comprises the following steps: firstly, using a ceramic bond grinding wheel with the granularity of 100-400 # as a dressing grinding wheel, removing the thickness of 0.1mm of the grinding working surface of the grinding wheel, then dressing for 2 times by using the cutting depth of 0.02mm, then dressing for 3 times by using the cutting depth of 0.01mm, and finally reciprocating for 2 times without cutting depth and idle stroke, wherein the feeding speed of the dressing grinding wheel is 20-30 mm/min; the effective abrasive particles on the surface of the grinding wheel form a plurality of semi-passive micro-blades with equal height through fine finishing, only fine abrasive dust is cut off during grinding, and a proper friction polishing effect is achieved;
the flow rate of the grinding fluid is 100-500 ml/min, and the grinding fluid is acidic grinding fluid, alkaline grinding fluid or water; the acid grinding fluid and the alkaline grinding fluid are respectively prepared by adding an acid pH regulator or an alkaline pH regulator into water, wherein the acid pH regulator is dilute hydrochloric acid or acetic acid, the pH value regulating range is 2-6, the alkaline pH regulator is potassium hydroxide, ammonia water or sodium carbonate, and the pH value regulating range is 8-12. The dissolving capacity of the soluble aluminum nitride filler is improved, and the size processing is finished and the polishing is carried out for two minutes.
The invention also discloses the resin metal composite mirror grinding wheel prepared by the method.
The invention has the beneficial effects that:
the mirror grinding wheel has high requirements on the uniformity of the internal tissue structure of the grinding wheel and the self-sharpening property of the grinding wheel, and the traditional powder dry pressing sand paper manufacturing method is easy to cause particle agglomeration, particularly the agglomeration of fine-grained grinding materials, and the agglomerated particles are far larger than the grain diameter of the actual grinding materials, so that the surface of a workpiece is scratched in the grinding process; according to the traditional manufacturing method of the gel casting grinding wheel, glue is directly used as a bonding agent to solidify grinding materials, micropores are generated by adding a pore-forming agent, most of the pores generated after the pore-forming agent is gasified are closed, the connectivity is poor, polishing liquid cannot permeate, the thickness of a water film in a polishing area is caused, the adsorption potential energy is low, the friction force is low, a sufficient heat source cannot be generated to promote mechanochemical action, and the polishing efficiency is low. According to the invention, through the dispersion and mixing of the slurry, the dispersion uniformity of each material of the grinding wheel is improved, and the agglomeration of particles is prevented; forming a blank body by adding gel resin, and forming a through capillary micropore after sintering; water-soluble resin is added and sintered to be used as a grinding wheel bonding agent for solidifying the grinding material; the self-sharpening performance of the grinding wheel is improved by adding the hydrolysable filler with the surface water-resistant function.
The grinding wheel is manufactured by mixed liquid gel of polyvinyl alcohol and water-soluble resin, so that the internal defects of the grinding wheel are reduced, and the uniformity of the grinding wheel tissue is ensured. The two resins have different functions in the process of forming the grinding wheel, firstly, a gel biscuit is formed by utilizing the low-temperature physical gelling capacity of polyvinyl alcohol, the polyvinyl alcohol is sintered and carbonized at high temperature, meanwhile, the water-soluble resin is solidified to be used as a grinding wheel binding agent, a large number of capillary micropores are generated after the polyvinyl alcohol is carbonized, compared with holes generated by adding a pore-forming agent in direct powder forming, the pores generated in the pill piece by the method are closed pores, and the capillary micropores generated in the pill piece are through micropores, have strong water absorption capacity, and are beneficial to improving friction force, storing polishing solution and removing chips.
The traditional grinding wheel improves self-sharpening property by adding 'soluble', 'decomposable' or 'electrolytic' filler, which can swell and can not ensure selective self-sharpening of surface materials, and has the defect of complex process. The aluminum nitride soluble powder filler with the water-resistant nano silicon dioxide coating coated on the surface is added, silicon dioxide on the surface of aluminum nitride on the surface layer of the grinding wheel is abraded, the aluminum nitride is hydrolyzed by grinding fluid, the surface bonding strength is reduced, the passivated abrasive falls off, new abrasive is exposed, and the self-sharpening property is maintained; because the capillary micropores in the grinding wheel have water absorption capacity, the aluminum nitride coated with the water-resistant nano silicon dioxide coating in the grinding wheel can avoid direct hydrolysis and maintain the strength of the grinding wheel matrix, and therefore, the grinding wheel has the advantages of stable internal structure and good surface self-sharpening property. The dissolving capacity of the grinding fluid to aluminum nitride can be adjusted by adjusting the pH value of the acidic or alkaline grinding fluid, the stable self-sharpening property of the grinding tool is kept, and the grinding efficiency is improved.
Drawings
FIG. 1 is a schematic view of the internal structure of a mirror grinding wheel by a sol-gel method;
FIG. 2 SEM surface topography of the mirror-grinding wheel prepared in example 1;
FIG. 3 is a schematic view of the end face grinding principle;
FIG. 4 is a white light interference pattern of the surface of the silicon planar lens after mirror grinding in the embodiment 1;
FIG. 5 is a surface laser interference profile after mirror grinding of the silicon flat lens in embodiment 1;
FIG. 6 is a white light interference topography of the surface of a silicon flat mirror ground by a hot press molding grinding wheel;
FIG. 7 is a graph of material removal rate versus time for two grinding wheels on a workpiece;
FIG. 8 is a graph showing the relationship between the pH value of the grinding fluid and the wear rate of the grinding wheel.
Detailed Description
The invention provides a resin metal composite mirror grinding wheel based on a sol-gel method and a preparation method thereof, wherein the schematic diagram of the internal structure of the sol-gel mirror grinding wheel is shown in figure 1. The grinding wheel is manufactured by using PVA and water-soluble resin liquid gel, the problem of uneven powder forming and dispersion is avoided, a gel biscuit is formed by utilizing the physical gel capability of the PVA, sintering and carbonization are carried out, the sintering and curing temperature of the water-soluble resin is also the carbonization temperature of the PVA, a large number of through capillary micropores are generated after the PVA is carbonized, the gel biscuit has good water absorption capability, and an aluminum nitride soluble powder filler with a water-resistant nano silicon dioxide coating coated on the surface is added, silicon dioxide on the surface of aluminum nitride on the surface layer of the grinding wheel is worn, the aluminum nitride is hydrolyzed by grinding liquid, the surface bonding strength is reduced, the passivated grinding material falls off, and new grinding material is exposed; the aluminum nitride coated with the water-resistant nano silicon dioxide coating in the grinding wheel can avoid direct hydrolysis, maintain the strength of the mirror surface grinding wheel matrix, effectively reduce the consumption of the grinding materials, and improve the service life and the utilization rate of the grinding materials in the polishing tool.
Example 1
In this example, a mirror-surface grinding wheel having fine pores was prepared, and a silicon flat lens was mirror-surface ground on an end-face grinding machine.
Step 1: preparation of aluminum nitride powder with water-resistant film layer on surface
Mixing 100g of aluminum nitride powder with the average grain diameter of 1 micron and 1kg of absolute ethyl alcohol by weight, uniformly stirring, and heating to 40 ℃ under the condition of water bath to obtain an aluminum nitride ethanol dispersion liquid; simultaneously adding 80g of tetraethyl orthosilicate (TEOS) diluted by 600g of absolute ethyl alcohol, 100g of ammonia water diluted by 600g of absolute ethyl alcohol and 100g of water into an aluminum nitride ethanol dispersion liquid, controlling the dropping speed to be 2 drops/second, after the dropping is finished, reacting for 6 hours under the condition of 40 ℃ water bath, stopping the reaction, carrying out vacuum filtration, washing the product for 3 times by using absolute ethyl alcohol, naturally drying the obtained product for 12 hours at room temperature, calcining for 2 hours at 300 ℃ after the drying, cooling, and sieving by using a 200-mesh sieve to obtain aluminum nitride powder coated by silicon dioxide, wherein the silicon dioxide has water resistance, so that the aluminum nitride powder with a water-resistant film layer on the surface is obtained;
step 2: a suspension is prepared. According to weight, 300g of diamond powder with the particle size of 2.5 microns, 100g of silicon dioxide coated aluminum nitride powder, 500g of electrolytic copper powder with the particle size of 400 meshes, 50g of copper-coated graphite, 50g of cryolite powder, 80g of zinc oxide, 150g of barium sulfate, 70g of aluminum oxide powder, 15g of polyoxyethylene alkylphenol ether wetting agent, 20g of polyethylene imine, 10g of organic silicon defoamer and 10g of dimethyl silicone oil release agent are added into 1200g of water, the mixture is dispersed by using a planetary ball mill after mixing, and zirconium oxide microspheres with the particle size of 3mm are selected as dispersion media to prepare suspension.
And step 3: preparing a sizing agent containing glue: under the condition of 90 ℃ water bath, 10g of polyvinyl alcohol is dissolved in a mixed solvent of 80g of water and 10g of ethanol to obtain 100g of polyvinyl alcohol glue with the solid content of 10 wt%; adding 300g of water-soluble polyimide resin liquid with the solid content of 40 wt% into the polyvinyl alcohol glue to obtain 400g of mixed glue, adding the mixed glue into the suspension prepared in the step 2 while stirring, and dispersing for 1 hour by using a planetary ball mill after mixing and stirring to obtain glue-containing slurry;
and 4, step 4: preparing a mirror grinding wheel semi-finished product with micro pores. Pouring 100g of the prepared slurry containing the glue into a circular mold with the diameter of 55mm, freezing at the temperature of-15 ℃ for 2 hours, naturally drying for 10 hours after thawing, taking out a blank from the mold, cold isostatic pressing under 30MPa, baking at 45 deg.C for 24 hr, the temperature of the grinding wheel blank is raised to 230 ℃ for sintering, the temperature rise curve is that the temperature is raised to 75 ℃ firstly and is preserved for 1 hour, and then heating to 115 ℃ and preserving heat for 1.5 hours, heating to 180 ℃ and preserving heat for 1 hour, finally heating to 230 ℃ and preserving heat for 30 minutes, thermally decomposing the polyvinyl alcohol glue to form uniform capillary micropores, curing the water-soluble polyimide resin to obtain a mirror grinding wheel semi-finished product with micro pores, wherein the surface topography of the prepared sol-gel mirror grinding wheel SEM is shown in figure 2, and the diamond, the filler and the electrolytic copper powder are uniformly distributed in the mirror grinding wheel. The obtained polyimide binding agent mirror grinding wheel has tensile strength up to 25MPa, hardness up to 60 (Shore hardness) and elongation at break up to 150%.
And 5: and (5) repairing the grinding wheel. Adopting a ceramic bond grinding wheel with the granularity of 100 to shape the semi-finished product of the mirror grinding wheel, removing redundant rim charge, and enabling the size precision of the grinding wheel to reach 0.01 mm;
step 6: and (5) dressing a grinding wheel. Adhering the trimmed mirror surface grinding wheel semi-finished product on a grinding wheel seat, and mounting the grinding wheel seat on a grinding wheel spindle of a milling and grinding machine for grinding wheel trimming to obtain an end surface grinding wheel; the grinding wheel dressing specifically comprises the steps of firstly using a ceramic bond corundum grinding wheel with the granularity of 150 # as a dressing grinding wheel, removing the thickness of 0.1mm of the working surface of the mirror surface grinding wheel, then using the cutting depth of 0.02mm for dressing twice, then using the cutting depth of 0.01mm for dressing three times, and finally performing reciprocating twice without a cutting depth idle stroke, wherein the transverse feeding speed of the dressing grinding wheel is 20mm/min during finishing, effective abrasive particles on the surface of the grinding wheel form a plurality of semi-passive micro-blades with equal height through fine dressing, only cutting fine abrasive dust during grinding, and having proper friction polishing effect, and enough grinding fluid or other cooling fluid must be used for washing on the contact point of the mirror surface grinding wheel and the dressing grinding wheel during grinding to wash away the grinding wheel dust in time so as not to influence the grinding quality;
and 7: and (5) carrying out mirror grinding processing on the silicon plane lens. Firstly, a silicon plane lens with the diameter of 50mm is finely ground by a diamond bronze grinding wheel with the granularity of 15 microns, the flatness reaches 1 micron, the surface roughness reaches 25nm, then the silicon plane lens is subjected to mirror grinding by using the end face grinding wheel, the schematic diagram of end face grinding processing is shown in figure 3, the rotating speed of a grinding wheel spindle is 7654rpm, the rotating speed of a workpiece spindle is 356rpm, the feeding amount is controlled at 0.002mm/min, the grinding depth is 50 microns, the grinding process is two minutes, the grinding fluid is alkaline grinding fluid, the dissolving capacity of soluble aluminum nitride filler is improved by adding alkaline pH regulator sodium carbonate into water and adjusting the pH value to 9, during grinding, the cutting fluid is sufficient, the flow rate of the grinding fluid is controlled at 300ml/min, and a good filtering device is arranged to prevent scratching the surface of the workpiece, after the size processing is finished, the grinding process is two minutes, a white light interference pattern of the surface of the silicon plane lens after the mirror face grinding, the surface roughness reaches 6.063nm, the surface has micro-cutting traces, fig. 5 is a surface laser interference surface profile after the mirror surface of the silicon plane lens is ground, the flatness PV value reaches below 1.5 wavelengths, the grinding load does not exceed 25% by detecting the power of the milling and grinding machine in the grinding process, which shows that the sol-gel mirror surface grinding wheel has good self-sharpening performance and can realize high flatness processing of the ground workpiece.
Example 2
Polishing contrast test: the silicon plane mirror head is ground by using a powder mixing-hot press molding method prepared by a traditional method, the surface topography of the silicon plane mirror head obtained by grinding is shown in fig. 6, the surface topography and the surface topography of the silicon plane mirror head in the example 1 are compared, the fine cut marks on the surface of the silicon plane mirror head obtained by polishing in the example 1 are uniform, the surface roughness of the silicon plane mirror head prepared by adopting a hot press molding method is 10.77nm, and the definition of the mirror grinding is that the surface roughness is less than 10nm after grinding, so that the requirement of the mirror grinding is difficult to meet, meanwhile, the appearance of coarse scratches on the surface is observed, which indicates that the dry powder mixing-hot press molding method cannot realize the uniform dispersion among materials with different densities, and the agglomeration phenomenon of powder particles is easy to occur when the mirror grinding wheel with fine granularity.
Meanwhile, the gel grinding wheel and the hot press molding grinding wheel are subjected to a durability comparison experiment, the grinding process parameters are consistent, a graph showing that the material removal rate of the two grinding wheels to a workpiece changes along with time after the two grinding wheels are used for a period of time is observed, as shown in fig. 7, the gel grinding wheel added with the hydrolysable aluminum nitride still keeps a high material removal rate after the gel grinding wheel is used for a period of time, and the surface of the hot press molding grinding wheel is passivated, so that the material removal rate is reduced.
Example 3
The mirror-surface grinding wheel obtained in example 1 was ground in grinding liquids having different pH values (7, 8, 9, 10, 11, 12, and 13), sodium carbonate was used as an acid pH adjuster, and the wear rate of the grinding tool was observed as shown in fig. 8, in accordance with other grinding parameters. As can be seen from the figure, the wear rate of the grinding wheel is improved along with the increase of the pH value, so that the pH value is adjusted according to the passivation degree of the grinding wheel in the using process in consideration of the service life of the grinding wheel, and the wear of the grinding wheel is controlled while the grinding wheel is sharpened. For the aluminum nitride of the water-resistant coating in the grinding wheel obtained in example 1, when the material removal rate is high, the pH of the grinding fluid can be controlled below 9 to slow down the abrasion of the grinding wheel, and when the material removal rate is reduced, an alkali pH regulator sodium carbonate can be added, and the pH is controlled above 10 to quickly sharpen the surface.
Example 4
Two comparative experiments were carried out in substantially the same manner as in example 1, except that in experiment 1, the particle size of the diamond abrasive in step 2 was changed to 1 μm, the grinding load was increased by more than 30% by detecting the power of the milling machine, and the surface of the silicon flat lens was also scratched by the previous fine grinding process, and the roughness was inferior to that of example 1 because the abrasive particle size was decreased and the grinding efficiency was decreased.
Example 5
The operation was substantially the same as that of example 1, except that 0, 50, 100, 150, 200, 250, and 300g of aluminum nitride powder having a water-resistant coating was added to prepare a gel mirror-surface grinding wheel, and a silicon mirror was ground, and experiments showed that the more the amount of the aluminum nitride powder filler was added, the more the abrasion of the wheel became remarkable, the too fast wear rate of the wheel became unfavorable for the high-precision surface profile processing, the higher the flatness PV value, and the lower the durability of the wheel without the aluminum nitride powder filler, and the glaze phenomenon appeared after 1 hour of grinding.
Example 6
The operation was substantially the same as in example 1, except that the amount of 10 wt% PVA glue in the mixed glue in step 3 was increased to 200g, and since PVA was carbonized after sintering, a large number of capillary pores having good water absorption capacity were generated, friction was enhanced, removal efficiency was improved, but wear rate was also improved.
As a comparative experiment, the operation was substantially the same as that of example 1 except that the water-soluble polyimide resin solution was added to 500g, the amount of the resin binder in the grinding wheel was increased after curing, the abrasion resistance was improved, the effect of aluminum nitride as a hydrolyzable filler was reduced, the surface was glazed after 5 hours of use, and the removal force was reduced.
Example 7
The operation is basically the same as that of the embodiment 1, except that the water-soluble polyimide resin is changed into the water-soluble phenolic resin, in the step 4, the sintering temperature is changed into 180 ℃, the sintering temperature rise curve is that the temperature is firstly raised to 75 ℃ and preserved for 1 hour, then raised to 115 ℃ and preserved for 1.5 hours, then raised to 150 ℃ and preserved for 1 hour, and finally raised to 180 ℃ and preserved for 30 minutes, so that the phenolic resin binding agent mirror grinding wheel is obtained, the tensile strength of the obtained mirror grinding wheel reaches 22MPa, the hardness reaches 56 (Shore hardness), and the mirror effect below 10nm can be achieved by grinding the silicon plane lens.
Claims (8)
1. A preparation method of a resin metal composite mirror grinding wheel based on a sol-gel method is characterized by comprising the following steps:
step 1: preparing water-resistant aluminum nitride powder with a silicon dioxide film layer on the surface;
step 2: dispersing diamond powder, water-resistant aluminum nitride powder, electrolytic copper powder, a filler and an additive in water to prepare a suspension;
and step 3: under the condition of 90 ℃ water bath, dissolving polyvinyl alcohol in a mixed solvent of water and ethanol to obtain polyvinyl alcohol glue, adding water-soluble resin liquid into the polyvinyl alcohol glue to obtain mixed glue, wherein the weight ratio of the polyvinyl alcohol glue to the water-soluble resin liquid in the mixed glue is 1: 1-6; adding the mixed glue into the suspension prepared in the step 2, and stirring while adding to obtain glue-containing slurry;
and 4, step 4: pouring the slurry containing the rubber into a grinding wheel mold, freezing for 1-3 hours at the temperature of-25 to-15 ℃, naturally drying for 5-10 hours after thawing, taking out a blank from the grinding wheel mold, performing densification treatment, drying for 24-48 hours at the temperature of 45-65 ℃, sintering, and cooling to obtain a grinding wheel semi-finished product with micro pores;
and 5: and (4) carrying out grinding wheel dressing on the grinding wheel semi-finished product obtained in the step (4) on a grinding machine, then installing the dressed grinding wheel semi-finished product on the grinding machine, adding grinding fluid to carry out grinding wheel grinding working surface dressing, wherein the flow rate of the grinding fluid is 100-500 ml/min, and preparing the mirror surface grinding wheel.
2. The method for preparing the resin metal composite mirror grinding wheel based on the sol-gel method according to claim 1, wherein the step 1 specifically comprises:
mixing 1-10 parts by weight of aluminum nitride powder and 50 parts by weight of absolute ethyl alcohol, and uniformly stirring at 40 ℃ to obtain an aluminum nitride ethanol dispersion liquid; dropwise adding 3-6 parts of tetraethoxysilane diluted by 30 parts of absolute ethyl alcohol, 4-6 parts of ammonia water diluted by 30 parts of absolute ethyl alcohol and 5 parts of water into the aluminum nitride ethanol dispersion liquid at the dropping speed of 1-2 drops/second, then carrying out gel reaction for 6 hours at the temperature of 35-45 ℃, carrying out vacuum filtration, washing the product for 3 times by using the absolute ethyl alcohol, naturally drying the obtained product for 12-24 hours at the room temperature, then calcining for 2 hours at the temperature of 300 ℃, cooling and then sieving by using a 200-mesh sieve to obtain the water-resistant aluminum nitride powder with the silicon dioxide film layer on the surface.
3. The method for preparing the resin metal composite mirror grinding wheel based on the sol-gel method according to claim 1, wherein the step 2 specifically comprises:
adding 5-10 parts by weight of 0.5-5 micron diamond powder, 1-3 parts by weight of water-resistant aluminum nitride powder, 10-30 parts by weight of 200-1000 mesh electrolytic copper powder, 5-10 parts by weight of filler and 1-5 parts by weight of additive into 20-50 parts by weight of water, and dispersing by using a planetary ball mill, wherein a dispersion medium is zirconia microspheres to prepare a suspension; the filler is any one or more of copper-coated graphite, talcum powder, cryolite, cerium oxide, aluminum oxide powder, calcium carbonate, calcium oxide, zinc oxide, barium sulfate, magnesium oxide and molybdenum disulfide; the additive is prepared by mixing a wetting agent, a dispersing agent, an organic silicon defoaming agent and a dimethyl silicon oil release agent, wherein the addition amount of the wetting agent is 0.1-1 wt% of the dry weight of the paste containing the glue, the addition amount of the dispersing agent is 0.1-1.5 wt% of the dry weight of the paste containing the glue, the addition amount of the organic silicon defoaming agent is 0.1-1 wt% of the dry weight of the paste containing the glue, the addition amount of the dimethyl silicon oil release agent is 0.1-1 wt% of the dry weight of the paste containing the glue, the wetting agent is any one of alkyl sulfate, sulfonate, fatty acid ester sulfate, carboxylic acid soap and phosphate ester anionic surfactant or polyoxyethylene alkylphenol ether, polyoxyethylene fatty alcohol ether and polyoxyethylene polyoxypropylene segmented copolymer nonionic surfactant, and the dispersing agent is phosphate ester dispersing agent, ethoxy compound dispersing agent, polyacrylate dispersing agent, polyester dispersing agent, any one of polyether type dispersant, polyolefin type dispersant, sodium carbonate, sodium orthophosphate or herring oil.
4. The method for preparing the resin metal composite mirror grinding wheel based on the sol-gel method according to claim 1, wherein the weight ratio of water to ethanol in the polyvinyl alcohol glue in the step 3 is 3-10: 1, and the solid content of polyvinyl alcohol is 5-15 wt%; the water-soluble resin solution is one or more of water-soluble epoxy resin solution, water-soluble polyimide resin solution or water-soluble phenolic resin solution, and the solid content of the water-soluble resin solution is 40-60 wt%; the dry weight of the mixed glue accounts for 5-15 wt% of the dry weight of the glue-containing slurry.
5. The method for preparing a resin metal composite mirror grinding wheel based on the sol-gel method according to claim 1, wherein the grinding wheel mold in the step 4 is cylindrical or circular; the densification treatment is cold isostatic pressing, and the pressure is 5-50 MPa; the sintering is specifically that the blank body is placed in an oven, the temperature is firstly raised to 75 ℃ and is preserved for 1 hour, then the temperature is raised to 115 ℃ and is preserved for 1.5 hours, then the temperature is raised to 150-180 ℃ and is preserved for 1 hour, and finally the temperature is raised to 180-230 ℃ and is preserved for 30 min.
6. The method for preparing the resin metal composite mirror grinding wheel based on the sol-gel method according to claim 1, wherein in the step 5, the wheel dressing is performed by using a ceramic bond grinding wheel with a grain size of 60-100, and excess rim charge of the semi-finished grinding wheel obtained in the step 4 is removed, so that the dimensional accuracy of the semi-finished grinding wheel reaches 0.01-0.05 mm.
7. The method for preparing a resin metal composite mirror grinding wheel based on the sol-gel method according to claim 1, wherein the mirror grinding wheel in step 5 comprises an end face grinding wheel and an external grinding wheel, and if the end face of the semi-finished product of the grinding wheel after dressing is used as a grinding working face of the grinding wheel, the end face of the semi-finished product of the grinding wheel is installed on a grinding wheel base for end face grinding, the end face grinding wheel is obtained, and the feeding amount of the end face mirror grinding is 0.002 mm/min; if the excircle surface of the trimmed grinding wheel semi-finished product is used as a grinding working surface of the grinding wheel, and the center hole of the grinding wheel semi-finished product is arranged on a grinding wheel spindle for excircle mirror surface grinding, the excircle grinding wheel is obtained, wherein the back bite of the excircle mirror surface grinding is 0.001-0.005 mm, the transverse feed is 0.2-0.5 mm/min, and the longitudinal feed is 10-20 m/min;
the grinding fluid is added to finish the grinding working surface of the grinding wheel, and the method specifically comprises the following steps: firstly, using a ceramic bond grinding wheel with the granularity of 100-400 # as a dressing grinding wheel, removing the thickness of 0.1mm of the grinding working surface of the grinding wheel, then dressing for 2 times by using the cutting depth of 0.02mm, then dressing for 3 times by using the cutting depth of 0.01mm, and finally reciprocating for 2 times without cutting depth and idle stroke, wherein the feeding speed of the dressing grinding wheel is 20-30 mm/min;
the flow rate of the grinding fluid is 100-500 ml/min, the grinding fluid is acidic grinding fluid, alkaline grinding fluid or water, the acidic grinding fluid and the alkaline grinding fluid are respectively prepared by adding an acidic pH regulator or an alkaline pH regulator into water, the acidic pH regulator is dilute hydrochloric acid or acetic acid, the pH value regulating range is 2-6, the alkaline pH regulator is potassium hydroxide, ammonia water or sodium carbonate, and the pH value regulating range is 8-12.
8. A resin metal composite mirror grinding wheel produced by the method according to any one of claims 1 to 7.
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