CN118438342B - A core-shell abrasive polishing disc capable of changing the motion state of abrasive, preparation method and application thereof - Google Patents
A core-shell abrasive polishing disc capable of changing the motion state of abrasive, preparation method and application thereof Download PDFInfo
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- CN118438342B CN118438342B CN202410526205.7A CN202410526205A CN118438342B CN 118438342 B CN118438342 B CN 118438342B CN 202410526205 A CN202410526205 A CN 202410526205A CN 118438342 B CN118438342 B CN 118438342B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B37/00—Lapping machines or devices; Accessories
- B24B37/11—Lapping tools
- B24B37/20—Lapping pads for working plane surfaces
- B24B37/24—Lapping pads for working plane surfaces characterised by the composition or properties of the pad materials
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24D—TOOLS FOR GRINDING, BUFFING OR SHARPENING
- B24D11/00—Constructional features of flexible abrasive materials; Special features in the manufacture of such materials
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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
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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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/304—Mechanical treatment, e.g. grinding, polishing, cutting
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Abstract
The invention relates to a core-shell abrasive polishing disc capable of changing the motion state of an abrasive, a preparation method and application thereof. In the course of rough machining, core-shell abrasive is uniformly fixed in the grinding and polishing disk, the holding force of matrix on core-shell abrasive is large, the matrix has large material removing capacity on workpiece, and can quickly implement flattening machining of workpiece, according to the machining process, the colloid shell of core-shell abrasive is dissolved by adding organic solvent grinding and polishing liquid on the surface of grinding and polishing disk to form pores, and internal abrasive can be locally moved freely in the pores so as to implement the conceivability of abrasive on workpiece surface machining, obtain high-quality machining surface and at the same time can prevent waste of free abrasive. The coarse and fine machining process circulation of the workpiece is realized through the addition of the organic solvent and the trimming of the polishing disc, so that the polishing machining procedure is shortened, and the machining efficiency and the surface quality are improved.
Description
Technical Field
The invention relates to the technical field of grinding and polishing. In particular to a core-shell abrasive polishing disc capable of changing abrasive motion state, a preparation method and application thereof.
Background
For processing hard and brittle material workpieces such as semiconductors and glass, the workpiece is generally required to undergo cutting, grinding, polishing and other procedures, and the processing efficiency and the processing surface quality such as surface roughness, surface/subsurface damage, lattice dislocation and the like of the workpiece are often required to adjust the processing procedures according to the processing progress so as to realize the removal of high-efficiency materials to obtain high-quality processing surfaces.
Currently, in the grinding and polishing stages, the abrasive is generally classified into three forms of a fixed abrasive, a semi-fixed abrasive and a free abrasive according to the state of the abrasive in the grinding and polishing. A fixed abrasive disk is a solid body of abrasive material in which the abrasive material is bonded to a base material, and during processing, the workpiece is removed by the abrasive material from the disk surface. The matrix in the fixed abrasive polishing disc has high holding force on the abrasive, can realize the rapid planarization processing of the surface of the workpiece, but is easy to cause the damage of the surface/subsurface of the workpiece, and meanwhile, the fixed abrasive is easy to grind down due to the lack of elasticity in the process of contacting with the workpiece, so that the polishing disc needs to be timely trimmed, and the service life is reduced. The semi-solid abrasive polishing disc generally adopts a special consolidation agent to consolidate the abrasive, so that the abrasive can move in a certain space or a certain range, the processing surface quality can be improved while higher processing efficiency is ensured, but the conversion from efficient planarization processing to high-quality surface processing cannot be realized according to the processing progress. The free abrasive is added into the solution, and the abrasive is removed from the workpiece material by dripping the polishing liquid onto the polishing disc, so that the surface can be processed with high quality, but the processing efficiency is low, the waste of the abrasive material is easily caused, the abrasive is harmful to the environment, the abrasive is agglomerated due to lack of control of the abrasive in the polishing process, and the polishing uniformity of the workpiece is affected to a certain extent.
Currently, in the grinding and polishing stage, it is generally divided into rough and fine machining processes, in which a planarized machined surface is efficiently obtained with a large mechanical removal force, and in which a high quality surface is flexibly obtained with a reduced mechanical removal force. In the course of rough to fine machining, machining parameters such as a machining disc, an abrasive and the like often need to be replaced, and the machining parameters have complex machining procedures and high use cost. Therefore, if the conversion from rough machining to finish machining can be quickly realized on the same polishing disc, the machining efficiency is greatly improved, and the machining cost is reduced.
The present patent (CN 109475995B) discloses a polishing body for CMP, which stores polishing particles through a plurality of air holes communicating in a longitudinal direction, and the polishing particles can be maintained in the air holes during polishing to achieve stable polishing performance. However, the control form of the grinding body on the grinding material is not changeable, the performance cannot be changed according to the processing process, the processing efficiency is low, and the efficient material removal cannot be realized.
The present patent (CN 103897202A) discloses a preparation method and application of a polystyrene/silicon oxide core-shell type nano composite abrasive, wherein polystyrene is used as an inner core, silicon oxide is used as an outer shell, and the polystyrene has higher elasticity and buffering effect on polishing pressure, so that excessive mechanical damage of the silicon oxide abrasive to a workpiece is reduced, and scratches and damage are effectively reduced. However, the core-shell abrasive is used for free abrasive, and is not applied to a polishing disc or a polishing pad, and the particle size of the silica abrasive serving as an outer layer is smaller, so that the material removal rate of composite abrasive processing is lower.
The method has the advantages that the existing workpiece processing has the problems that the surface/subsurface damage of the workpiece is easy to cause in the processing of the fixed abrasive, the processing uniformity of the free abrasive is poor, the utilization rate of the abrasive is low, the process from rough processing to finish processing is complicated, and the like in grinding and polishing.
Disclosure of Invention
Aiming at the problems existing in the prior art, the application discloses a core-shell abrasive polishing disc capable of changing the motion state of an abrasive, a preparation method and application thereof, and solves the problems that the surface/subsurface damage of a workpiece is easily caused by the processing of a fixed abrasive, the processing uniformity of free abrasive is poor, the utilization rate of the abrasive is low, the process from rough processing to finish processing is complicated, and the like in the grinding and polishing by changing the application mode of the abrasive in the polishing process.
The core-shell abrasive polishing disc capable of changing the abrasive motion state, the preparation method and the application thereof have extremely important significance in reducing the cost in polishing and processing and improving the processing efficiency and the surface quality.
Based on the polishing disc, the invention provides a core-shell abrasive polishing disc capable of changing the motion state of an abrasive, which is used for flattening, grinding and polishing of semiconductors and glass workpieces, and the substrate of the polishing disc is selected from one of epoxy resin base, ceramic base and polyurethane base.
Further, the core-shell abrasive consists of an abrasive inner layer and a polymer organic colloid outer layer wrapping the abrasive, wherein the core-shell abrasive and the abrasive inner layer are granular, the grain size of the core-shell abrasive is 0.1-20 mu m, the grain size of the abrasive inner layer of the core-shell abrasive is 0.1-16 mu m, and the thickness of the polymer organic colloid outer layer is 0.05-4 mu m.
Further, the inner layer abrasive is selected from one of diamond, silicon carbide, alumina, cerium oxide and silicon dioxide, and the outer layer of the polymer organic colloid is selected from one of polystyrene, polymethyl methacrylate and benzoguanamine formaldehyde.
Furthermore, uniform air holes are formed in the polishing disc, the diameters of the air holes are 10-100 mu m, abrasive dust generated during processing can be stored, and excessive abrasive dust is prevented from blocking the holes where the abrasive is located, so that the concession of the abrasive in finish processing is prevented from being influenced.
The invention also provides a method for preparing the core-shell abrasive polishing disc capable of changing the motion state of the abrasive, which comprises the following steps:
S1, adding polyvinyl alcohol into a three-neck flask containing deionized water, heating in a water bath to 100 ℃, and continuously stirring for 1-2 hours at 400-600 r/min to obtain a polyvinyl alcohol aqueous solution with a mass fraction of 2-4%, adding sodium oleate particles with a particle size of 1 mu m into the polyvinyl alcohol aqueous solution, controlling the mass fraction of sodium oleate to be 3-6%, and continuously stirring at a speed of 400-600 r/min for 1-2 hours to obtain a substance A;
S2, adding a grinding material and polystyrene with the mass fraction of 5-20% into a dichloromethane solvent with the mass fraction of 20-30%, controlling the mass ratio of the grinding material to the polystyrene to the dichloromethane to be 1:2-4:20-25, and stirring in a water bath at 20-50 ℃ for 1-2 hours until the polystyrene and the grinding material are completely mixed, wherein the obtained substance is denoted as B;
S3, dropwise adding the substance B prepared in the step S2 into the substance A prepared in the step S1 at a speed of 1-1.5 mL/min to form emulsion, placing the emulsion in an environment of 25-30 ℃ and stirring at a speed of 450-600 r/min, preserving heat for 15-20 h, evaporating the organic solvent, keeping the remainder as C after the organic solvent is completely evaporated, centrifuging the substance C at 7000-800 r/min for 10-20 min, washing the precipitate with deionized water for 3-5 times, wherein the mass ratio of the deionized water to the substance B is 1:2-4, and placing the precipitate in a drying oven at 30-50 ℃ for 2h to obtain the abrasive/polystyrene core-shell abrasive;
S4, taking 4.9-9.9% of the core-shell abrasive material prepared in the step S3 according to the mass percentage, taking a polishing disc matrix preparation formula according to the corresponding mass percentage, mixing abrasive particles and the matrix formula, and solidifying and forming;
and S5, demolding the polishing disc blank formed by curing in the step S4, and finishing the polishing disc on a polishing machine by using a 100-1000-mesh grinding wheel for 5-20 min to obtain higher flatness on the surface of the polishing disc, so that the core-shell abrasive polishing disc capable of changing the abrasive motion state for polishing processing can be obtained, and the abrasive is fixedly arranged in the polishing disc.
Further, when the substrate of the polishing disc is selected from epoxy resin, the specific procedure of S4 is as follows:
Taking 4.9-9.9% of the core-shell abrasive material prepared in the step S3 by mass percent, taking 70-74% of liquid epoxy resin by mass percent, taking 0.1% of pore-forming agent by mass percent, wherein the pore-forming agent is one of calcium carbonate, plastic balls and hollow microspheres, mixing the three materials, stirring for 30-1 h at 1000-1200 r/min, adding 20-21% of curing agent by mass percent, mixing at the same speed, stirring for 5-10 min to obtain a mixture, pouring the mixture into a polishing disc die, standing and curing at 23-26 ℃, and keeping for 10-12 h.
Further, the curing agent is one of aniline curing agent, alcohol amine curing agent, polyamide curing agent and the like which are commonly used for curing epoxy resin, and preferably, the curing agent is one of ethylenediamine, cyclohexylamine and polyamide ester.
Further, when the substrate of the polishing disc is selected from polyurethane groups, the specific procedure of S4 is as follows:
taking 4.9-9.9% of core-shell abrasive material prepared in the step S3 by mass percent, taking 65-70% of polyurethane prepolymer by mass percent, taking 20-25% of hydroxypropyl silicone oil by mass percent, taking 0.001% of stannous octoate by mass percent, taking 0.1% of pore-forming agent by mass percent, wherein the pore-forming agent is selected from one of calcium carbonate, plastic balls and hollow microspheres, mixing and performing ultrasonic dispersion at 80 ℃, mechanically stirring at 600r/min for reacting for 12min, adding chain-extending cross-linking agent MOCA at 1-2% by mass percent, stirring at 1300r/min for 30S at 80 ℃ to obtain a mixture, pouring the mixture into a preheated polytetrafluoroethylene mould, applying 2kg pressure to the mould, and curing at 110 ℃ for 16 h.
The invention also provides an application of the core-shell abrasive polishing disc capable of changing the abrasive motion state in workpiece grinding and polishing, comprising the following steps:
The method comprises the following steps of SS1, dropwise adding deionized water polishing liquid to the surface of a core-shell abrasive fixed polishing disc at the speed of 3-4 mL/min in a rough machining stage, enabling a workpiece to be in contact with the core-shell abrasive fixed polishing disc capable of changing the abrasive motion state and realizing relative motion, solidifying the abrasive in the polishing disc at the moment and removing materials on the surface of the workpiece, wherein the rough machining stage is adopted;
SS2, when the surface roughness of a workpiece is reduced to 1-20 nm through rough machining, dropwise adding grinding liquid containing 15-20% of organic solvent to the surface of a core-shell abrasive grinding disc capable of changing the motion state of the abrasive at the speed of 3-4 mL/min, dissolving a colloid shell of the core-shell abrasive on the surface of the grinding disc by the organic solvent, enabling the abrasive inside to freely move in a limited space pore generated by dissolving the shell, further playing roles of avoiding free abrasive loss and waste, improving abrasive yield and reducing damage to the surface of the workpiece, realizing the finish machining of the workpiece, and finishing the finish machining stage when the surface roughness of the workpiece is reduced to 0.1-1 nm;
And SS3, finishing the polished core-shell abrasive polishing disc capable of changing the abrasive motion state by using a 100-1000-mesh finishing grinding wheel, setting the rotation speed of the polishing disc according to the diameter of the polishing disc, determining the finishing time by using a polishing disc matrix material, removing the surface layer of the polishing disc where free abrasive exists, and reserving the plane where the core-shell abrasive which is not dissolved in the shell exists so as to realize disc surface abrasive state conversion.
Further, the organic solvent added to SS2 is selected from one of limonene, methylene chloride, methanol, and the like.
Compared with the prior art, the invention has the beneficial effects that:
1. The invention provides a core-shell abrasive polishing disc capable of changing abrasive motion state, which comprises a core-shell abrasive, wherein the core-shell abrasive consists of an inner abrasive layer and an outer colloid wrapping the abrasive, and the core-shell abrasive is uniformly distributed in the polishing disc.
2. In the rough machining process, the core-shell abrasive is uniformly fixed in the polishing disc, the holding force of the matrix on the core-shell abrasive is large, the abrasive has larger mechanical removing force on the surface of the workpiece, and the planarization machining of the workpiece can be rapidly realized.
3. According to the processing progress, the conversion from rough processing to finish processing is realized by adding an organic solvent polishing liquid into the polishing disc, the organic solvent solution can dissolve the colloid of the organic shell, the colloid shell of the core-shell abrasive is dissolved to form pores, the internal abrasive can do local free movement in the limited space pores generated by the colloid dissolution, the waste of free abrasive is avoided, the concessibility of the abrasive on the surface of a workpiece is improved, and the damage of the abrasive on the surface of the workpiece is reduced or even eliminated, so that the high-quality processing surface is obtained.
4. The pore-forming agent is added in the preparation process to enable the polishing disc to have pores for storing abrasive dust generated in the polishing process, so that excessive abrasive dust is prevented from entering pores where the abrasive is located to prevent local free movement of the abrasive, and the conceivability of the abrasive in finish machining is reduced.
5. The polishing disc can realize the conversion of rough and finish machining procedures of workpieces in one disc, effectively shortens the grinding and polishing machining procedures, greatly improves the machining efficiency, the abrasive utilization rate, the machining uniformity and the surface quality of the workpieces, and reduces the machining cost.
Drawings
FIG. 1 is a schematic illustration of a core-shell abrasive disk application step for changing the abrasive motion;
FIG. 2 is a schematic illustration of rough machining of a workpiece by a core-shell abrasive disk with changeable abrasive motion;
FIG. 3 is a schematic illustration of the finishing of a workpiece by a core-shell abrasive disk with a changeable abrasive motion.
Wherein, the polishing agent comprises a 1-core-shell abrasive, a 2-material removing layer, a 3-workpiece, a 4-abrasive inner layer, a 5-macromolecule organic colloid, a 6-polishing solution, a 7-polishing disc matrix and 8-pores.
Detailed Description
The invention will be further described with reference to the following specific embodiments, but the examples are not intended to limit the invention in any way. Raw materials reagents used in the examples of the present invention are conventionally purchased raw materials reagents unless otherwise specified.
Examples 1-5 are core-shell abrasive polishing discs with epoxy resin based and changeable abrasive motion state, and the types, particle sizes and grinding fluids of the abrasives in examples 1-5 are different, see table 1:
table 1 examples 1-5 partial parameter summary tables
Example 1
This example describes the formulation and preparation of a core-shell abrasive, further describes the method of preparing a polishing disc using the core-shell abrasive, and further describes an application of the polishing disc.
1.1A core-shell abrasive material comprises the following specific steps:
S1, adding polyvinyl alcohol into a three-neck flask containing deionized water, heating in a water bath to 100 ℃, continuously stirring at 600r/min for 2 hours until the polyvinyl alcohol is completely dissolved to obtain a polyvinyl alcohol aqueous solution with the mass fraction of 3 percent, adding sodium oleate particles with the particle size of 1 mu m into the polyvinyl alcohol aqueous solution, controlling the mass fraction of sodium oleate to be 3 percent, and continuously stirring at 600r/min for 2 hours to obtain a substance A;
S2, adding a diamond abrasive with the grain diameter of 5 mu m and 10% of polystyrene into 20% of methylene dichloride solvent, wherein the mass ratio of the diamond abrasive to the polystyrene to the methylene dichloride solvent is 1:2:20, and stirring in a water bath at 40 ℃ for 2 hours until the polystyrene and the diamond are completely mixed and dissolved, wherein the obtained substance is denoted as B;
And S3, dropwise adding the substance B prepared in the step S2 into the substance A prepared in the step S1 at a speed of 1mL/min by using a syringe to form emulsion, placing the emulsion in a water bath kettle at a temperature of 30 ℃ and stirring at a speed of 600r/min, preserving heat for 20h, evaporating an organic solvent, marking the residual substance as C, centrifuging the substance C at 8000r/min for 20min, washing the precipitate with deionized water for 5 times, wherein the mass ratio of the dosage of the deionized water to the substance B is 1-4, and placing the precipitate in a drying oven at a temperature of 50 ℃ for 2h to obtain the diamond/polystyrene core-shell abrasive.
1.2 Method for preparing core-shell abrasive polishing disc with epoxy resin base and changeable abrasive motion state, comprising the following specific steps:
(1) Taking 9.8% of core-shell abrasive material prepared by 1.1% by mass, taking 70% of liquid epoxy resin by mass, taking 0.1% of hollow microspheres by mass, mixing the three, stirring for 30min at 1000r/min, adding 20% by mass of curing agent ethylenediamine, mixing, stirring for 5min at the same speed to obtain a mixture, pouring the mixture into a grinding and polishing disc mold, standing and curing at 25 ℃, and keeping for 2h;
(2) Demolding the polishing disc blank formed by curing in the step (1), and then finishing the polishing disc on a polishing machine by using a 500-mesh grinding wheel for 15min to ensure that the surface of the polishing disc obtains higher flatness, thus obtaining the core-shell abrasive polishing disc which is used for polishing and can change the abrasive motion state, wherein the abrasive is fixedly arranged in the polishing disc.
1.3 A core-shell abrasive polishing disc for processing a workpiece of a hard and brittle material, the abrasive motion state of which can be changed, the application of the polishing disc comprising the following steps:
SS1, dropwise adding deionized water polishing liquid to the surface of a core-shell abrasive fixed polishing disc at the speed of 4mL/min, enabling a workpiece to be in contact with the core-shell abrasive polishing disc capable of changing the abrasive motion state and realizing relative motion, wherein the polishing time is 20min;
And SS2, setting the rotation speed of the polishing disc to be 100r/min, and using a 500-mesh dressing grinding wheel to dress the polished core-shell abrasive polishing disc capable of changing the abrasive motion state for 10min.
Example 2
2.1 Formulation and preparation of core-shell abrasive referring to 1.1 of example 1, the difference is that the diamond abrasive particle size in this example S2 is 1 μm.
2.2 Method for preparing core-shell abrasive polishing disc with epoxy resin based capable of changing abrasive motion state, the specific steps refer to 1.2 of example 1, and the difference is that (1) in this example is 9.8% of the core-shell abrasive prepared by 2.1 by mass percent.
2.3 A core-shell abrasive polishing disc for hard and brittle material workpiece processing with changeable abrasive motion state, the polishing application step of which is referred to 1.3 of example 1.
Example 3
3.1 Method for preparing core-shell abrasive polishing disc with epoxy resin based changeable abrasive motion state, the specific steps refer to 1.2 of example 1, wherein (1) in this example 9.8% of diamond abrasive is taken by mass percent, and the abrasive particle size is 5 μm.
3.2 A core-shell abrasive polishing disc for processing workpieces of brittle and hard material with changeable abrasive motion, the polishing application procedure of which is described in example 1, 1.3.
Example 4
4.1 Method for preparing core-shell abrasive polishing disc with epoxy resin based changeable abrasive motion state, the specific steps refer to 1.2 of example 1, wherein (1) in this example 9.8% of diamond abrasive is taken by mass percent, and the abrasive particle size is 1 μm.
4.2 A core-shell abrasive polishing disc for hard and brittle material workpiece processing with changeable abrasive motion state, the polishing application step of which is referred to 1.3 of example 1.
Example 5
5.1 Formulation and preparation of a core-shell abrasive specific procedures are described in example 1, 1.1.
5.2 Method for preparing core-shell abrasive polishing disc with epoxy resin based capable of changing abrasive motion state, the specific steps refer to 1.2 of example 1, and the difference is that (1) in this example is 9.8% of core-shell abrasive prepared by 5.1 by mass percent.
5.3 A core-shell abrasive polishing disc which is used for processing hard and brittle material workpieces and can change the abrasive motion state, wherein the polishing application steps are as follows:
SS1, dropwise adding deionized water polishing liquid to the surface of a core-shell abrasive fixed polishing disc at the speed of 4mL/min, enabling a workpiece to be in contact with the core-shell abrasive fixed polishing disc capable of changing the motion state of the abrasive and realizing relative motion, wherein the abrasive is fixed in the polishing disc and realizes material removal on the surface of the workpiece, and the polishing time is 10min;
SS2, dripping polishing liquid containing 20% of limonene on the surface of a core-shell abrasive polishing disc capable of changing the abrasive motion state at the speed of 4mL/min, wherein the polishing time is 10min;
And SS3, setting the rotation speed of the polishing disc to be 100r/min, using a 500-mesh finishing grinding wheel to finish the polished core-shell abrasive polishing disc capable of changing the abrasive motion state for 10min, removing the surface layer of the polishing disc where free abrasive exists, and reserving the plane where the core-shell abrasive which is not dissolved in the shell exists.
The mass change of the workpiece before and after grinding was weighed with a precision electronic balance (precision: 0.1 mg) to calculate the material removal rate, and the surface roughness and the morphology change of the workpiece before and after grinding were measured with a white light interferometer (ContourGT-X3). The polishing was performed on a KD15BX single-sided grinder using the polishing pad of this example, and the polished workpiece was a 2-inch 4H-SiC cut piece manufactured by Blu-ray semiconductor Co., ltd. In Beijing, with an initial surface roughness of 80.+ -. 6nm and an initial thickness of 400.+ -.25. Mu.m.
The grinding processing of the 4H-SiC workpiece is realized through relative rotation, the grinding pressure is 200kPa, the rotating speed is 60r/min, the workpiece grinding time is set to be 0-10min and 10-20min, and the workpiece material removal rate and the surface roughness are detected after grinding.
Polishing tests were performed on the polishing plates of the different applications of examples 1-5 using the above polishing conditions, and the test results are shown in Table 2:
Table 2 examples 1-5 polishing test results on polishing discs
As can be seen from comparative examples 3 and 4 in Table 2, the 5 μm large-grain diamond consolidated polishing disc has a high material removal rate in the polishing process, which can reach 55.88nm/min, but has a poor effect of reducing the surface roughness of the wafer, the surface roughness reduction efficiency is obviously deteriorated in the stage of 10-20min, the 1 μm small-grain diamond consolidated polishing disc can effectively reduce the surface roughness in the polishing process, the polishing time can be reduced to Ra 3.2nm for 20min, but the material removal rate is lower, which is only 41.4% of that of the large-grain diamond polishing disc.
As can be seen from comparison of examples 1 and 2, the material removal rate of the large-particle-size core-shell abrasive fixed polishing disc in the polishing process is higher and can reach 54.32nm/min, while the small-particle-size core-shell abrasive fixed polishing disc can obtain better wafer surface quality and can reach Ra 2.2nm.
It can be seen from comparative examples 1 and 3, comparative examples 2 and 4 that the grinding effect of diamond with the same particle size and core-shell diamond consolidated disk is about the same in the case that the core-shell abrasive shell is not dissolved, and the larger particle size core-shell abrasive consolidated disk has higher material removal rate, and the lower particle size core-shell abrasive consolidated disk can obtain better lens surface quality.
As can be seen from a comparison of examples 1 and 5, the polishing disc allows the wafer to achieve a lower surface roughness, reaching Ra 1.2nm, after dissolution of the core shell abrasive colloid shell.
As can be seen from comparison of examples 2 and 5, the large-particle-size core-shell abrasive consolidated polishing disc has higher material removal rate, and the surface roughness of the wafer can be effectively reduced by dissolving the colloid shell of the shell abrasive, so that the large-particle-size abrasive has better surface quality than the small-particle-size abrasive in the polishing process.
Examples 6 to 10
Examples 6 to 10 are core-shell abrasive polishing discs with polyurethane base and changeable abrasive motion state, and the types, particle sizes and grinding fluids of the abrasives in examples 6 to 10 are different, see table 3:
TABLE 3 Induction of parameters for examples 6-10 section
Example 6
This example describes the formulation and preparation of a core-shell abrasive, further describes the method of preparing a polishing disc using the core-shell abrasive, and further describes an application of the polishing disc.
6.1 Formulation and preparation of a core-shell abrasive specific procedures are described in example 1, 1.1.
6.2, The method for preparing the polyurethane-based core-shell abrasive polishing disc capable of changing the motion state of the abrasive comprises the following specific steps:
(1) Taking 8.2% of core-shell abrasive material prepared in the step 6.1 by mass percent, taking 68.4% of polyurethane prepolymer by mass percent, taking 21.6% of hydroxypropyl silicone oil by mass percent, taking 0.001% of stannous octoate by mass percent, taking 0.1% of hollow microspheres by mass percent, mixing and performing ultrasonic dispersion at 80 ℃, mechanically stirring at 600r/min for reacting for 12min, adding 1.7% of chain-extending cross-linking agent MOCA by mass percent, stirring at 1300r/min for 30s at 80 ℃ to obtain a mixture, pouring the mixture into a preheated polytetrafluoroethylene mould, applying 2kg pressure to the mould, and curing at 110 ℃ for 16 h;
(2) Demolding the polishing disc blank solidified and molded in the step S4, and then finishing the polishing disc on a polishing machine by using a 500-mesh grinding wheel for 10min to ensure that the surface of the polishing disc obtains higher flatness, thus obtaining the core-shell abrasive polishing disc which is used for polishing and processing and can change the abrasive motion state, wherein the abrasive is fixedly arranged in the polishing disc.
6.3 A core-shell abrasive polishing disc for processing a workpiece of a hard and brittle material, the polishing application of which comprises the following steps:
SS1, dropwise adding deionized water polishing liquid to the surface of a core-shell abrasive fixed polishing disc at the speed of 4mL/min, enabling a workpiece to be in contact with the core-shell abrasive polishing disc capable of changing the abrasive motion state and realizing relative motion, wherein the polishing time is 60min;
and SS2, setting the rotation speed of the polishing disc to be 100r/min, and finishing the polished core-shell abrasive polishing disc capable of changing the abrasive motion state for 10min by using a 500-mesh finishing grinding wheel.
Example 7
7.1 Formulation and preparation of a core-shell abrasive specific procedures are described in example 2, 2.1.
7.2 Method for preparing polyurethane-based core-shell abrasive polishing disc capable of changing abrasive motion state, the specific procedure is 6.2 of example 6, except that (1) in this example, the core-shell abrasive obtained by 7.1 is used.
7.3 A core-shell abrasive polishing disc for hard and brittle material workpiece processing with changeable abrasive motion state, the polishing application step of which is described in example 6, 6.3.
Example 8
8.1 Method for preparing polyurethane-based core-shell abrasive polishing disc capable of changing abrasive motion state, referring to 6.2 of example 6, in specific steps, 9.8% of diamond abrasive is taken according to mass percentage in the example (1), and the abrasive particle size is 5 μm.
8.2 A core-shell abrasive polishing disc for hard and brittle material workpiece processing with changeable abrasive motion state, the polishing application step of which is described in example 6, 6.3.
Example 9
9.1 Method for preparing polyurethane-based core-shell abrasive polishing disc capable of changing abrasive motion state, referring to 6.2 of example 6, in specific steps, (1) 9.8% diamond abrasive is taken by mass percent in this example, and abrasive particle size is 1 μm.
9.2A core-shell abrasive polishing disc for workpiece processing of hard and brittle materials with changeable abrasive motion state, the polishing application step of which is described in example 6, 6.3.
Example 10
10.1 Formulation and preparation of a core-shell abrasive specific procedures are described in example 1, 1.1.
10.2 Method for preparing polyurethane-based core-shell abrasive polishing disc capable of changing abrasive motion state, the specific procedure is 6.2 of example 6, except that (1) in this example, 10.1 of the core-shell abrasive is taken.
10.3 A core-shell abrasive polishing disc which is used for processing hard and brittle material workpieces and can change the motion state of the abrasive, wherein the polishing application steps are as follows:
SS1, dropwise adding deionized water polishing liquid to the surface of a core-shell abrasive fixed polishing disc at the speed of 4mL/min, enabling a workpiece to be in contact with the core-shell abrasive fixed polishing disc capable of changing the motion state of the abrasive and realizing relative motion, wherein the abrasive is fixed in the polishing disc and realizes material removal on the surface of the workpiece, and the polishing time is 30min;
SS2, dripping polishing liquid containing 20% of limonene on the surface of a core-shell abrasive polishing disc capable of changing the abrasive motion state at the speed of 4mL/min, wherein the polishing time is 30min;
And SS3, setting the rotation speed of the polishing disc to be 100r/min, using a 500-mesh finishing grinding wheel to finish the polished core-shell abrasive polishing disc capable of changing the abrasive motion state for 10min, removing the surface layer of the polishing disc where free abrasive exists, and reserving the plane where the core-shell abrasive which is not dissolved in the shell exists.
The experimental detection method adopted is the same as that of examples 1 to 5, and will not be described here again. The polished workpiece was a 2 inch 4H-SiC cut piece produced by Beijing Tiankogakuda blue semiconductor Co., ltd, with an original surface roughness of 2.+ -. 0.3nm and an initial thickness of 350.+ -. 25. Mu.m.
The 4H-SiC workpiece is polished by relative rotation, the polishing solution is deionized water or limonene solution, the polishing pressure is 40kPa, the workpiece rotating speed is 40r/min, the polishing disk rotating speed is 40r/min, the workpiece polishing time is set to 0-30min and 30-60min, and the workpiece material removal rate and the surface roughness are detected after polishing.
Polishing tests were performed on the polishing plates of the different applications of examples 6-10 using the polishing conditions described above, and the test results are shown in Table 4:
table 4 results of polishing test on polishing discs of examples 6 to 10
As can be seen from the comparison of the examples 8 and 9 in Table 4, the 5 μm large grain diameter diamond consolidated polishing disc has a higher material removal rate in the polishing process, which can reach 43.75nm/min, but the effect of reducing the surface roughness of the wafer is poor, the surface roughness reduction efficiency is obviously deteriorated in the stage of 30-60min, the 1 μm small grain diameter diamond consolidated polishing disc can effectively reduce the surface roughness in the polishing process, the polishing time can be reduced to Ra 0.432nm in 60min, but the material removal rate is lower, which is only 54.8% of that of the large grain diameter diamond polishing disc.
As can be seen from comparison of examples 6 and 7, the material removal rate of the large-particle-size core-shell abrasive fixed polishing disc in the polishing process is higher and can reach 46.11nm/min, while the small-particle-size core-shell abrasive fixed polishing disc can obtain better wafer surface quality and can reach Ra 0.466nm.
As can be seen from comparative examples 6 and 8, and comparative examples 7 and 9, the polishing effect of the diamond and core-shell diamond consolidated disk of the same particle size is about the same in the case where the core-shell abrasive shell is insoluble, and the larger particle size core-shell abrasive consolidated disk has a higher material removal rate, and the lower particle size core-shell abrasive consolidated disk can achieve better lens surface quality.
As can be seen from a comparison of examples 6 and 10, the polishing disc allows the wafer to achieve a lower surface roughness, up to Ra 0.357nm, after dissolution of the core-shell abrasive colloid shell.
As can be seen from comparison of examples 7 and 10, the large-particle-size core-shell abrasive consolidated disk has a higher material removal rate, and the surface roughness of the wafer can be effectively reduced by dissolving the colloidal shell of the shell abrasive, so that the large-particle-size abrasive has better surface quality than the small-particle-size abrasive in the polishing process.
As can be seen from the above examples, core-shell abrasive polishing discs that change the state of abrasive motion can be used for efficient conversion from rough to finish. The workpiece material removal rate is higher before the organic solvent is added dropwise, and the surface roughness is rapidly reduced after the organic solvent is added dropwise.
In the examples, the core-shell abrasive was dissolved in the polystyrene shell by dropping a limonene organic solvent to convert from rough machining to finish machining, and the abrasive inside the particles was converted from a solidified state to a state free from the pores in the limited space.
The core-shell abrasive polishing disc capable of changing the abrasive motion state has the function of controlling the abrasive application mode of the polishing disc in the polishing process, and the advantages that the polishing disc can avoid waste of free abrasive and obtain higher processing efficiency and better polishing effect are shown.
The above examples illustrate only a few embodiments of the invention, which are described in detail and are not to be construed as limiting the scope of the invention. It should be noted that it is possible for a person skilled in the art to make several variants and modifications without departing from the inventive concept, which fall within the scope of protection of the present invention.
Claims (7)
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| US6659846B2 (en) * | 2001-09-17 | 2003-12-09 | Agere Systems, Inc. | Pad for chemical mechanical polishing |
| JP2004074330A (en) * | 2002-08-13 | 2004-03-11 | Ebara Corp | Fixed abrasive polishing tool, and method for manufacturing the same |
| JP4039214B2 (en) * | 2002-11-05 | 2008-01-30 | Jsr株式会社 | Polishing pad |
| KR20110030957A (en) * | 2009-09-18 | 2011-03-24 | 주식회사 동진쎄미켐 | Polishing pads containing core-shell type particles |
| CN103862354B (en) * | 2014-03-24 | 2015-12-09 | 南京航空航天大学 | Processing method of ultra-thin single crystal germanium wafer |
| CN105238354B (en) * | 2015-11-04 | 2019-01-01 | 华侨大学 | A kind of stone soft shell abrasive compound and its preparation method and application |
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