CN111607359B - Preparation process of zirconia composite abrasive and grinding fluid - Google Patents
Preparation process of zirconia composite abrasive and grinding fluid Download PDFInfo
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- CN111607359B CN111607359B CN202010441370.4A CN202010441370A CN111607359B CN 111607359 B CN111607359 B CN 111607359B CN 202010441370 A CN202010441370 A CN 202010441370A CN 111607359 B CN111607359 B CN 111607359B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
Abstract
The invention relates to a preparation process and grinding fluid of a novel zirconia composite abrasive, which comprises the steps of firstly preparing an organic precursor sol of the zirconia composite abrasive; granulating the organic precursor sol; and then sintering to obtain the zirconia composite abrasive. The zirconia composite abrasive prepared by the invention is formed by bonding countless tiny zirconia particles through a boroaluminate melt at a crystal boundary, although the macroscopic size is larger, the zirconia composite abrasive is broken along a glass bonding interface in the process of grinding a silicon wafer, the abrasion of the abrasive is micro-crushing abrasion, and the abrasive is continuously broken to generate a large number of new and tiny grinding edges in the grinding process, the composite abrasive has very high self-sharpening performance, and the grinding efficiency is improved by more than 30 percent compared with the alumina abrasive; in addition, the surface of the object to be ground is provided with a large number of fine grinding marks, the surface roughness value of the ground workpiece is lower, stable and consistent grinding amount can be provided in the using process, and the grinding efficiency and the surface quality of the ground workpiece can be effectively considered.
Description
Technical Field
The invention relates to a preparation process and grinding fluid of a zirconia composite abrasive, in particular to a preparation process and grinding fluid of a zirconia composite abrasive for preparing a monocrystalline silicon piece surface processing grinding fluid, belonging to the field of abrasive preparation.
Background
At present, the plane finish machining of monocrystalline silicon in China mainly adopts mechanical grinding, and the common processing method is that a manufacturer purchases sheet-shaped white corundum with the grain diameter of 7-14 microns as a grinding material, and then an aluminum oxide grinding fluid is prepared by using a grinding material, water (or an organic solvent) and a dispersing agent. The double-end-face grinding equipment for the monocrystalline silicon piece adopts a special double-face vertical grinding machine, the upper end face and the lower end face of the grinding machine are respectively provided with a cast iron disc during grinding, the configured alumina grinding liquid is dripped between the cast iron discs and the monocrystalline silicon piece, relative motion is generated between the cast iron discs and the monocrystalline silicon piece during grinding, and at the moment, the white corundum grinding material positioned between the grinding discs and the monocrystalline silicon piece realizes free rolling grinding on the surface of the monocrystalline silicon piece to be processed. The process has a technical bottleneck at present, the polished monocrystalline silicon wafer is required to have as high finish as possible and the surface residual stress is as low as possible along with the development of electronic technology, so that a hard grinding material with a thinner diameter is required, but the grinding efficiency is greatly reduced due to the thinning of the grinding material, and meanwhile, the flatness error of the silicon wafer is increased due to the reduction of the grinding capacity, so that the process is not beneficial to high-precision photoetching. The development of the grinding abrasive which can efficiently grind and remove the machining allowance of the monocrystalline silicon wafer and can obtain a high-finish and low-stress grinding surface has important significance for promoting the development of the semiconductor precision machining technology in China.
Disclosure of Invention
Aiming at the defects of the prior art, one of the purposes of the invention is to provide a preparation process of a zirconia composite abrasive so as to obtain the abrasive with high grinding efficiency and good grinding surface quality; the other object of the present invention is to provide a polishing slurry for surface processing of a single crystal silicon wafer.
In order to solve the technical problems, the technical scheme of the invention is as follows:
a preparation process of a zirconia composite abrasive comprises the following steps:
s1, ZrOCl2Uniformly mixing the powder and absolute ethyl alcohol according to the mass ratio of 1 (8-10) to obtain ZrOCl2The absolute ethyl alcohol solution of (1);
s2, uniformly mixing the absolute ethyl alcohol solution obtained in the step S1 and aluminum isopropoxide according to the mass ratio of (93-95) to (5-7) to obtain a first mixed solution;
s3, mixing the first mixed solution obtained in the step S2 with high-hydroxyl acrylic resin according to the weight ratio of 100: (3-5) uniformly mixing the components in the mass ratio to obtain a second mixed solution;
s4, dropwise adding a borax solution into the second mixed solution obtained in the step S3 while stirring, and stirring at 6000-;
wherein the concentration of the borax solution is 5-7wt%, and the dropping amount of the borax solution is 5-10wt% of the second mixed solution;
s5, taking the organic precursor sol obtained in the S4 as a raw material, and carrying out spray granulation to obtain dry gel particles;
s6, uniformly mixing the dried gel particles obtained in the step S5 and liquid phenolic resin according to the mass ratio of (94-95) to (5-6), transferring the mixture to an atmosphere furnace, heating to 300 ℃ at the speed of 5-8 ℃/min under the inert atmosphere, preserving heat for 0.5-1h, heating to 500 ℃ at the speed of 2-3 ℃/min, preserving heat for 0.5-1h, heating to 800-900 ℃ at the speed of 5-8 ℃/min, preserving heat for 1-2h, and cooling with the furnace to obtain the zirconium oxide composite abrasive.
In the present invention, ZrOCl2The powder is easily dissolved in absolute ethyl alcohol, and ZrOCl is added2Weighing the ZrOCl and absolute ethyl alcohol according to the mass ratio of 1 (8-10), mixing and stirring to obtain ZrOCl2Then in ZrOCl2The absolute ethyl alcohol solution of (2) was added with a specific amount of aluminum isopropoxide to obtain a first mixed solution. A specific amount of high-hydroxyl acrylic resin is added into the first mixed solution, the high-hydroxyl acrylic resin can be used as a temporary adhesive for a subsequent granulation process, meanwhile, the high-hydroxyl acrylic resin can be simultaneously dissolved in solvents with higher polarity, such as ethanol, water and the like, and segregation caused by the addition of an aqueous solution in the subsequent process can be avoided. Subsequently, the borax solution with the amount and the concentration is dripped into the second mixed solution, and ZrOCl is added into the second mixed solution2And isopropanol in an alkaline environment to yield Zr (OH)4、Al(OH)3Mixing the sol, wherein the sol contains a certain amount of sodium borate. Meanwhile, the solution contains a certain amount of high-hydroxyl acrylic resin, and the hydroxyl end of the high-hydroxyl acrylic resin is easy to be adsorbed to high-valence Zr4+And Al3+Surface, further reducing ZrOCl2Hydrolysis rate of aluminum isopropoxide, beneficial to obtaining stable Zr (OH)4、Al(OH)3And mixing the sol.
During spray granulation, the sol liquid sprayed out under the action of surface tension spontaneously forms spherical liquid drops, the spherical liquid drops are quickly dried, the high-hydroxyl acrylic resin in the mixed sol is quickly solidified at a short high temperature, and the micro powder in the dried spherical particles is bonded together to form the spherical particleSpherical dry gel particles of a certain strength consisting essentially of Zr (OH)4、Al(OH)3And Na2B4O7And (3) the composition of the particles.
The dry gel particles are uniformly mixed with a specific amount of liquid phenolic resin, so that the surfaces of the gel particles are coated with a layer of phenolic resin film, and the phenolic resin film is gradually cured and carbonized in the subsequent sintering process. The residual carbon content of the cracked liquid phenolic resin can reach 30-40wt%, so that the cracked phenolic resin can finally form a continuous carbon film on the surface of the spherical composite abrasive, the spherical abrasives are prevented from being adhered to each other in the sintering process, and the sintered abrasives are ensured to be in a single-sphere shape. And (3) heating the dried gel particles covered with the liquid phenolic resin to 300 ℃ at the speed of 5-8 ℃/min in an inert atmosphere, and preserving the temperature for 0.5-1 hour, wherein the liquid phenolic resin on the surfaces of the dried gel particles is gradually cured and cracked in the process, and the high-hydroxyl acrylic resin in the gel particles also starts to crack to release the low-molecular-weight organic gas. Then, the temperature is raised to 500 ℃ at the speed of 2-3 ℃/min, and the temperature is kept for 0.5-1 hour, wherein Zr (OH) in the gel is generated in the process4、Al(OH)3Decomposition into amorphous ZrO2、Al2O3And water vapor, since a large amount of gas is generated, spherical particles can be prevented from being cracked by controlling the rate of temperature rise. Heating to 800-900 deg.C at a rate of 5-8 deg.C/min for 1-2 hr while maintaining Na2B4O7Melt down because of the high amount of Na in the melt+Exhibits basicity, which dissolves highly active amorphous Al2O3And ZrO2And (3) granules. ZrO in spherical composite abrasive2High content of and ZrO2In Na2B4O7Low solubility in the melt, molten Na2B4O7ZrO in spherical composite abrasive2Generates a dynamic dissolution and precipitation mechanism, and facilitates the ZrO2So that a large amount of ZrO can be formed at a relatively low sintering temperature2And (4) microcrystals. Al in spherical composite abrasive2O3Low content of Al2O3In Na2B4O7High solubility in the meltAl in composite abrasives2O3Completely dissolved in Na2B4O7In the melt, Na is formed2O -Al2O3-B2O3A glass system containing a large amount of Al2O3So that it has high strength and a coefficient of expansion lower than Na2B4O7Can be reacted with ZrO2The thermal expansion coefficients of the microcrystals are matched, so that large thermal stress is prevented from being generated at the interface. Sintering the composite abrasive, cooling, and adding Na2O -Al2O3-B2O3ZrO becoming solid from glass2The crystallites are bonded together. When the process is used for preparing the zirconia composite abrasive, ZrO with different diameters can be obtained by regulating and controlling sintering process parameters2Crystallites, ZrO obtained at a higher final sintering temperature for a longer holding time2The larger the crystallite diameter. Optionally, sintering the ZrO2And sieving the composite abrasive to obtain a finished product with the particle size meeting the requirement, and taking the finished product as the abrasive to be mixed into the monocrystalline silicon wafer grinding fluid to grind and process the monocrystalline silicon wafer.
Further, ZrOCl added to absolute ethanol in S1 under the stirring condition of 1000-2Powder is stirred for 1 to 2 hours to obtain ZrOCl2The absolute ethanol solution of (1).
Further, in S2, the anhydrous ethanol solution and the aluminum isopropoxide are mixed under the stirring condition of 1000-2000 r/min, and stirred for 1-2h to obtain a first mixed solution.
Further, in S3, the mixture was stirred for 1 to 2 hours.
Further, in S4, the borax solution is uniformly dripped into the second mixed solution under the stirring condition of 6000-8000 rpm, and the dripping completion time is 10-15 min. The applicant has found, through repeated studies, that the addition of the borax solution must be carried out at a rate such as to prevent ZrOCl2And isopropanol is hydrolyzed too fast to generate gel flocculation, and the generation of flocculation gel can be avoided by controlling the completion time of dripping within 10-15 min.
Further, in S5, spray granulation was performed by a spray granulator having a nozzle with a diameter of 0.1 to 0.15 mm.
Optionally, during spray granulation, the raw material is sprayed into a drying tower of a granulator from a nozzle with a caliber of 0.1-0.15mm under a pressure of 1.0-1.5MPa, and the sol liquid sprayed out under the action of surface tension spontaneously forms spherical droplets, generally, the larger the spraying pressure is, the smaller the nozzle diameter is, the smaller the diameter of the formed spherical droplets is. Preferably, the temperature in the drying tower of the spray granulator is 280-350 ℃ so that the sol droplets sprayed from the nozzles are rapidly dried in the drying tower.
Further, in S6, the inert atmosphere is a nitrogen atmosphere.
Further, after S6, the method further includes the step of sieving the zirconia composite abrasive. The sieving parameters can be set according to requirements, for example, a 320# sieve can be selected, and powder with the particle size of less than 320 meshes below the sieve can be selected as the finished zirconia composite abrasive.
Alternatively, the molecular weight of the high hydroxyl acrylic resin is 3500-4500.
Optionally, the molecular weight of the liquid phenolic resin is 1000-3000.
Optionally, the preparation process of the zirconia composite abrasive includes the following steps:
the method comprises the following steps: preparation of organic precursor sol of zirconium oxide composite abrasive
Firstly, weighing a proper amount of ZrOCl2Powder, then according to ZrOCl2Weighing a proper amount of absolute ethyl alcohol according to the mass ratio of 1 (8-10), pouring the weighed absolute ethyl alcohol into a container, and adding the weighed ZrOCl under the stirring condition of 1000-2Powder is stirred for 1 to 2 hours to obtain ZrOCl2The absolute ethyl alcohol solution of (1);
ZrOCl2Respectively weighing ZrOCl according to the mass ratio of (93-95) to (5-7) of the absolute ethyl alcohol solution to the aluminum isopropoxide2Mixing the anhydrous ethanol solution and the aluminum isopropoxide under the stirring condition of 1000-2000 r/min, and stirring for 1-2 hours to obtain a first mixed solution; weighing high-hydroxyl acrylic resin according to 3-5% of the first mixed solution, and adding the high-hydroxyl acrylic resin into the first mixed solutionAnd stirring the first mixed solution for 1-2 hours to obtain a uniform second mixed solution. Weighing 5-7wt% of borax solution according to 5-10% of the second mixed solution, dropping the borax solution into the resin mixed solution at a constant speed under the stirring condition of 6000-8000 rpm, wherein the dropping completion time is 10-15 minutes, and stirring for 5-8 hours under the stirring condition of 6000-8000 rpm after dropping is completed to obtain organic precursor sol for preparing the zirconia composite abrasive;
step two: granulation of organic precursor sol
Pouring the organic precursor sol of the zirconia composite abrasive prepared in the step one into a material tank of a small-sized spray granulator, spraying the organic precursor sol into a drying tower of the granulator under the pressure of 1.0-1.5MPa, wherein the diameter of a nozzle is 0.1-0.15mm, and controlling the temperature in the drying tower to be 280-350 ℃. Collecting dry gel particles in a spherical shape at a discharge hole of a spray granulator;
step three: sintering of zirconia composite abrasives
Weighing the spherical dry gel particles prepared in the step two and the liquid phenolic resin according to the mass ratio of (94-95) to (5-6), then manually mixing uniformly, pouring the gel particles added with the liquid phenolic resin into a ceramic crucible, filling the ceramic crucible into a controlled atmosphere furnace, heating to 300 ℃ at the speed of 5-8 ℃/min under the nitrogen atmosphere, preserving heat for 0.5-1h, heating to 500 ℃ at the speed of 2-3 ℃/min, preserving heat for 0.5-1h, heating to 800-degree-of-charge 900 ℃ at the speed of 5-8 ℃/min, preserving heat for 1-2h, closing the furnace, and cooling along with the furnace. And (3) passing the sintered composite powder material through a 320# screen mesh in a negative-pressure screening machine, wherein the screened particles are qualified zirconia composite abrasive.
Based on the same inventive concept, the invention also provides grinding fluid which comprises the zirconium oxide composite abrasive prepared by the preparation process.
Optionally, the grinding fluid is prepared from the zirconium oxide composite abrasive, water (or an organic solvent) and a dispersing agent.
The zirconia composite abrasive obtained by the preparation process is mainly formed by bonding numerous tiny zirconia microcrystals, zirconium composite particles are broken along a microcrystal interface in the process of grinding a silicon wafer, the abrasion of the abrasive is micro-crushing abrasion, and a large number of new and fine grinding edges are generated by continuous breakage in the grinding process; on the other hand, the surface of the silicon wafer to be ground is provided with a large number of fine grinding marks, the roughness value of the surface of the ground silicon wafer is lower, and the grinding damage of the surface of the silicon wafer is smaller. The zirconium oxide composite abrasive is used for carrying out plane grinding processing on a silicon wafer, and can effectively give consideration to both grinding efficiency and the surface quality of the ground silicon wafer.
Compared with the prior art, the invention has the following beneficial effects:
conventional Al2O3The grinding material is a single crystal and only has one large cutting edge, and the grinding powder has high grinding efficiency when the single crystal silicon material is ground, but the grinding edge is passivated with the lapse of time, and the grinding efficiency is rapidly reduced. The zirconia composite abrasive is a novel high-performance monocrystalline silicon wafer processing abrasive, and is mainly formed by bonding numerous tiny zirconia particles through a boroaluminate melt at a crystal boundary, although the macroscopic size is larger, the zirconia composite abrasive is broken along a glass bonding interface in the process of grinding a silicon wafer, the abrasion of the abrasive is micro-crushing abrasion, and a large number of new and tiny grinding edges (see figure 1) are generated by continuous breakage in the grinding process, on one hand, the composite abrasive has high self-sharpening performance, and the grinding efficiency is improved by more than 30 percent compared with the alumina abrasive; on the other hand, the surface of the object to be ground is a large number of fine grinding marks, the surface roughness value of the ground workpiece is lower (see fig. 2 and 3), stable and consistent grinding amount can be provided in the using process, and the grinding efficiency and the surface quality of the ground workpiece can be effectively considered.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments are briefly introduced below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without inventive efforts, wherein:
FIG. 1 is a micrograph of a zirconia composite abrasive according to the present invention;
FIG. 2 is a micrograph of a single crystal silicon wafer after grinding with the zirconia composite abrasive of the present invention;
FIG. 3 is a micro-topography of a single crystal silicon wafer ground by a conventional alumina composite abrasive.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
In this embodiment, the preparation process of the zirconia composite abrasive includes the following steps:
the method comprises the following steps: preparation of organic precursor sol of zirconium oxide composite abrasive
Firstly, weighing a proper amount of ZrOCl2Powder, then according to ZrOCl2Weighing a proper amount of absolute ethyl alcohol according to the mass ratio of 1:9, pouring the weighed absolute ethyl alcohol into a container, and adding the weighed ZrOCl under the stirring condition of 1000-2Powder is stirred for 2 hours to obtain ZrOCl2The absolute ethanol solution of (1).
ZrOCl2Respectively weighing ZrOCl in the absolute ethyl alcohol solution and the aluminum isopropoxide according to the mass ratio of 95:52And mixing the anhydrous ethanol solution and the aluminum isopropoxide under the stirring condition of 2000 r/min, and stirring for 1 hour to obtain a first mixed solution. Weighing high-hydroxyl acrylic resin (with the molecular weight of 4000) according to 5% of the mass of the first mixed solution, adding the high-hydroxyl acrylic resin into the first mixed solution, and stirring for 1 hour to obtain a uniform second mixed solution. Weighing 6wt% borax solution according to 5% of the second mixed solution, and dropwise adding the borax solution at uniform speed under the stirring condition of 8000 r/minAnd (3) adding the mixture into the second mixed solution, wherein the dropwise adding time is 10 minutes, and stirring the mixture for 5 hours under the stirring condition of 6000 revolutions per minute after the dropwise adding is finished to obtain the organic precursor sol for preparing the zirconia composite abrasive.
Step two: granulation of organic precursor sol
Pouring the organic precursor sol of the zirconia composite abrasive prepared in the step one into a material tank of a small-sized spray granulator, spraying the organic precursor sol into a drying tower of the granulator under the pressure of 1.5MPa, wherein the diameter of a nozzle is 0.1mm, and the temperature of the drying tower is 350 ℃. Collecting the dry gel particles in a spherical shape at the discharge hole of the spray granulator.
Step three: sintering of zirconia composite abrasives
Weighing the spherical dry gel particles prepared in the step two and the liquid phenolic resin according to the mass ratio of 95:5, then manually mixing uniformly, pouring the gel particles added with the liquid phenolic resin (molecular weight 2000) into a ceramic crucible, loading the ceramic crucible into a controlled atmosphere furnace, heating to 300 ℃ at the speed of 5 ℃/min under the nitrogen atmosphere, preserving heat for 1 hour, heating to 500 ℃ at the speed of 3 ℃/min, preserving heat for 1 hour, heating to 800 ℃ at the speed of 5 ℃/min, preserving heat for 1 hour, closing the furnace, and cooling along with the furnace. The sintered composite powder material passes through a 320# screen mesh in a negative pressure screening machine, and the grains under the screen are qualified zirconia composite abrasive, and the appearance of the zirconia composite abrasive is shown in figure 1. The zirconia composite abrasive obtained in this example was used for grinding a single crystal silicon wafer, and the following ratio of zirconia composite abrasive: polyethylene glycol: deionized water is uniformly mixed according to the mass ratio of 20:5:75 to obtain grinding fluid, the grinding fluid is used for carrying out plane grinding on a monocrystalline silicon double-side grinder with the specification of 16B to a monocrystalline silicon wafer with the diameter of 6 inches, the acceleration of grinding liquid drops is 4L/h, the rotating speed of a grinding disc is 8 m/min, the working pressure of the grinding disc is 1500N, the time required for grinding 50 microns of the monocrystalline silicon wafer is 310 seconds, and the microscopic morphology of the finally obtained monocrystalline silicon wafer is shown in figure 2.
Grinding a monocrystalline silicon wafer by adopting a traditional alumina composite abrasive, wherein the alumina composite abrasive comprises the following components in percentage by weight: polyethylene glycol: deionized water is uniformly mixed according to the mass ratio of 20:5:75 to obtain grinding fluid, the grinding fluid is used for carrying out plane grinding on a monocrystalline silicon double-side grinder with the specification of 16B to a monocrystalline silicon wafer with the diameter of 6 inches, the acceleration of grinding liquid drops is 4L/h, the rotating speed of a grinding disc is 8 m/min, the working pressure of the grinding disc is 1500N, the time required for grinding 50 microns of the monocrystalline silicon wafer is 470 seconds, and the microscopic morphology of the finally obtained monocrystalline silicon wafer is shown in figure 3.
The grinding liquid containing the zirconia composite abrasive is used for grinding the monocrystalline silicon piece, the grinding efficiency is improved by more than 30% compared with that of an alumina abrasive, and as can be seen from the graph 2 and the graph 3, the obtained workpiece is lower in surface roughness and better in surface quality.
The foregoing examples are set forth to illustrate the present invention more clearly and are not to be construed as limiting the scope of the invention, which is defined in the appended claims to which the invention pertains, as modified in all equivalent forms, by those skilled in the art after reading the present invention.
Claims (8)
1. The preparation process of the zirconia composite abrasive is characterized by comprising the following steps of:
s1, ZrOCl2Uniformly mixing the powder and absolute ethyl alcohol according to the mass ratio of 1 (8-10) to obtain ZrOCl2The absolute ethyl alcohol solution of (1);
s2, uniformly mixing the absolute ethyl alcohol solution obtained in the step S1 and aluminum isopropoxide according to the mass ratio of (93-95) to (5-7) to obtain a first mixed solution;
s3, mixing the first mixed solution obtained in the step S2 with high-hydroxyl acrylic resin according to the weight ratio of 100: (3-5) uniformly mixing the components in the mass ratio to obtain a second mixed solution;
s4, dropwise adding the borax solution into the second mixed solution obtained in the step S3 while stirring, and dropwise adding the borax solution into the second mixed solution at a constant speed under the stirring condition of 6000-8000 rpm, wherein the dropwise adding time is 10-15 min; namely, after the dropwise addition is finished, stirring for 5-8h at the speed of 6000-;
wherein the concentration of the borax solution is 5-7wt%, and the dropping amount of the borax solution is 5-10wt% of the second mixed solution;
s5, taking the organic precursor sol obtained in the S4 as a raw material, and carrying out spray granulation to obtain dry gel particles;
s6, uniformly mixing the dried gel particles obtained in the step S5 and liquid phenolic resin according to the mass ratio of (94-95) to (5-6), transferring the mixture to an atmosphere furnace, heating to 300 ℃ at the speed of 5-8 ℃/min under the inert atmosphere, preserving heat for 0.5-1h, heating to 500 ℃ at the speed of 2-3 ℃/min, preserving heat for 0.5-1h, heating to 800-900 ℃ at the speed of 5-8 ℃/min, preserving heat for 1-2h, and cooling with the furnace to obtain the zirconium oxide composite abrasive.
2. The process according to claim 1, wherein ZrOCl is added to the absolute ethanol in S1 under stirring conditions of 1000-2000 rpm2Powder is stirred for 1 to 2 hours to obtain ZrOCl2The absolute ethanol solution of (1).
3. The preparation process as claimed in claim 1, wherein in S2, the anhydrous ethanol solution and the aluminum isopropoxide are mixed under the stirring condition of 1000-2000 rpm, and stirred for 1-2h to obtain the first mixed solution.
4. The process according to claim 1, wherein in S3, stirring is carried out for 1-2h during mixing.
5. The process according to claim 1, wherein in S5, the spray granulation is carried out by a spray granulator having a nozzle diameter of 0.1 to 0.15 mm.
6. The production process according to claim 1, wherein in S6, the inert atmosphere is a nitrogen atmosphere.
7. The process of any one of claims 1-6, further comprising, after S6, the step of sieving the zirconia composite abrasive.
8. A polishing liquid comprising the zirconia composite abrasive produced by the production process according to any one of claims 1 to 7.
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| CN104066808A (en) * | 2012-09-12 | 2014-09-24 | 研磨剂与耐火品研究与开发中心C.A.R.R.D.有限公司 | Agglomerate abrasive grain comprising incorporated hollow microspheres |
| CN107936917A (en) * | 2017-12-13 | 2018-04-20 | 河北思瑞恩新材料科技有限公司 | A kind of micro mist performed polymer formula and preparation method thereof |
| CN109321204A (en) * | 2018-10-24 | 2019-02-12 | 河南省力量钻石股份有限公司 | A kind of more particle agglomeration type abrasive grain bodies, preparation method and applications |
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