CN115386301B - CMP polishing solution for gallium oxide single crystal wafer processing and preparation method thereof - Google Patents
CMP polishing solution for gallium oxide single crystal wafer processing and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the technical field of polishing solution production, in particular to CMP polishing solution for gallium oxide single crystal wafer processing and a preparation method thereof; the polishing solution is prepared from the following raw materials in percentage by weight: 45-52% of nano silica sol, 2-4% of nano manganese dioxide, 1.8-2.5% of polyethylene glycol, 1.8-3.0% of polishing auxiliary agent, 0.8-2.5% of pH value regulator, 2.2-2.8% of surfactant, 1.2-1.8% of chelating agent, 0.015-0.025% of polydimethylsilane, 0.03-0.05% of dodecyl trimethyl ammonium chloride, 0.02-0.04% of benzotriazole and the balance of deionized water; the polishing solution prepared by the invention can effectively avoid the situation that the surface of the gallium oxide single crystal wafer is damaged in the polishing process, and can improve the microcosmic conditions such as polishing scratches, surface pressure loss and the like after the surface of the gallium oxide single crystal wafer is polished, reduce the roughness and ensure the polishing quality of the gallium oxide single crystal wafer; furthermore, the polishing solution prepared by the invention has better cleaning performance, antibacterial performance and wear resistance, and effectively improves the quality.
Description
Technical Field
The invention relates to the technical field of polishing solution production, in particular to CMP polishing solution for gallium oxide single crystal wafer processing and a preparation method thereof.
Background
The polishing solution is prepared from various chemical solutions, has important positions in the polishing process, and is reasonably selected, so that the processed wafer surface has no scratches, no pits and easy cleaning. In addition, the polishing solution also has the functions of removing greasy dirt, softening the surface of the wafer to accelerate the grinding, reducing the impact of the grinding tool on the wafer, and enabling the metal product to exceed the original luster. The product has stable performance, no toxicity, no pollution to environment, etc.
At present, the commercially available polishing solution product has good polishing effect on the wafer, so that the surface of the wafer is brighter and more attractive, and the color and luster of the wafer are attractive. However, the surface of the gallium oxide single crystal wafer is mechanically damaged in the polishing treatment process, scratches or damages are formed on the surface of the gallium oxide single crystal wafer, the roughness of the gallium oxide single crystal wafer is increased, and the polishing quality of the gallium oxide single crystal wafer is affected. In addition, the existing polishing solution product has relatively poor cleaning performance and antibacterial performance, so that the service life of the polishing solution product is shortened to a certain extent, and the production cost is increased.
Accordingly, the present invention provides a CMP polishing solution for gallium oxide single-wafer processing and a preparation method thereof, which are used for solving the above-mentioned related technical problems-!
Disclosure of Invention
The invention aims to provide a CMP polishing solution for gallium oxide single crystal wafer processing and a preparation method thereof, wherein the prepared polishing solution can effectively avoid the situation that the surface of the gallium oxide single crystal wafer is damaged in the polishing process, can improve the microscopic conditions such as polishing scratches, surface pressure loss and the like after the surface of the gallium oxide single crystal wafer is polished, reduce the roughness, and ensure the polishing quality of the gallium oxide single crystal wafer. Furthermore, the polishing solution prepared by the invention has better cleaning performance, antibacterial performance and wear resistance, prolongs the service life to a certain extent, and effectively improves the quality.
In order to achieve the above purpose, the present invention provides the following technical solutions:
the CMP polishing solution for gallium oxide single crystal wafer processing is prepared from the following raw materials in percentage by weight: 45-52% of nano silica sol, 2-4% of nano manganese dioxide, 1.8-2.5% of polyethylene glycol, 1.8-3.0% of polishing auxiliary agent, 0.8-2.5% of pH value regulator, 2.2-2.8% of surfactant, 1.2-1.8% of chelating agent, 0.015-0.025% of polydimethylsilane, 0.03-0.05% of dodecyl trimethyl ammonium chloride, 0.02-0.04% of benzotriazole and the balance of deionized water.
Further, the preparation method of the polishing auxiliary agent comprises the following steps: putting the pretreated matrix material into deionized water with the mass being 5-8 times of that of the matrix material, vacuumizing and filling nitrogen for three times, then raising the temperature of the obtained mixed system to 75-85 ℃, sequentially adding 20-30% of acrylamide monomer with the mass being 20-30% of that of the pretreated matrix material and 0.08-0.42% of ammonium persulfate with the mass being 0.08-0.42% of that of the acrylamide monomer into the mixed system at the temperature, and then carrying out heat preservation reaction for 7-10 h at the temperature of 75-85 ℃; after the reaction is finished, centrifugally separating the obtained product components, washing the obtained solid filter material with deionized water for 3-5 times, and finally placing the solid filter material in a drying oven for drying treatment to obtain the polishing auxiliary agent finished product.
Further, the pretreatment process of the substrate material comprises the following steps: adding a matrix material into a proper amount of modified liquid according to the solid-liquid ratio of 0.08-0.15 g/mL, performing ultrasonic dispersion for 20-30 min, adding gamma-methacryloxypropyl trimethoxy silane with the mass of 10-20% of the modified liquid into the modified liquid, and performing heat preservation and stirring reaction for 10-15 h at the temperature of 55-65 ℃; after the reaction is finished, the obtained product components are subjected to centrifugal separation and drying treatment, and then the pretreatment of the matrix material is completed.
Furthermore, the modified liquid is prepared by uniformly dispersing a proper amount of absolute ethyl alcohol with the concentration of 60-75% and nonylphenol polyoxyethylene ether with the mass of 2.5-4.2% and polyhexamethylene biguanide hydrochloride with 10-15% by ultrasound.
Further, the preparation method of the matrix material comprises the following steps:
injecting deionized water with the volume of 20-30 times of that of the polystyrene microsphere emulsion with the concentration of 10-14 g/L into the polystyrene microsphere emulsion, performing ultrasonic dispersion for 20-30 min, adding a proper amount of aluminum nitrate nonahydrate into the obtained mixed solution according to the feeding standard of 0.0073-0.0078 mol/L, uniformly mixing and stirring, adding thiourea with the molar quantity of 50% of aluminum nitrate nonahydrate into the mixed solution, performing magnetic stirring reaction for 2-4 h at the temperature of 60-80 ℃ after uniformly mixing and stirring, and then adjusting the pH value of the mixed solution to 10.8-11.3 by using sodium hydroxide solution with the concentration of 0.1-0.15 mol/L, thereby obtaining a first dispersion liquid for storage and standby;
II, respectively adding a proper amount of nano silicon carbide with the particle size of 10-13 nm and nano molybdenum disulfide with the particle size of 5-8 nm into deionized water according to the dosage ratio of 0.02-0.03 g/mL and 0.015-0.025 g/mL, then adding fatty alcohol polyoxyethylene ether with the mass of 2-4% of that of the deionized water into the deionized water, uniformly dispersing the mixture by ultrasonic waves to prepare second dispersion liquid, and preserving the second dispersion liquid for later use;
III, adding a second dispersion liquid with the volume of 40-50% of that of the first dispersion liquid into the first dispersion liquid, and then magnetically stirring the first dispersion liquid at 50-60 ℃ for reaction for 3-5 h; after the reaction is finished, the obtained product components are subjected to centrifugal separation, washing and drying in sequence, and finally the obtained solid material is the finished product of the matrix material.
Further, the weight percentage of the silicon dioxide particles in the nano silica sol is 35-45%, the particle size of the silicon dioxide particles is 8-12 nm, the particle size of the silicon dioxide micelle particles is less than or equal to 45nm, and the average particle size of the nano manganese dioxide is less than or equal to 55nm.
Further, the surfactant is selected from any one of fatty alcohol polyoxyethylene ether, fatty acid polyoxyethylene ether, octyl phenol polyoxyethylene ether and methyl stearate polyoxyethylene ether.
Further, the pH value regulator is prepared from sodium hydroxide and triethanolamine according to a mass ratio of 1: 2-4.
Further, the chelating agent is any one of disodium edetate, tartaric acid, ethylenediamine tetraacetic acid and hydroxyethyl ethylenediamine triacetic acid.
The preparation method of the CMP polishing solution for processing the gallium oxide single crystal wafer comprises the following steps:
firstly, adding nano manganese dioxide and polishing auxiliary agent into nano silica sol, injecting two thirds of deionized water, mechanically mixing and stirring for 20-40 min, and standing the obtained mixed slurry for later use;
step two, adding polyethylene glycol, a surfactant, a chelating agent, polydimethylsilane, dodecyl trimethyl ammonium chloride, benzotriazole and one third of the amount of pH value regulator into the rest deionized water while stirring, and mixing and stirring the materials at a stirring rate of 150-250 r/min to uniformly disperse the materials in the deionized water, so that the obtained mixed solution is preserved for later use;
and thirdly, slowly adding the mixed solution into the mixed slurry at a feeding rate of 80-120 mL/min while stirring, continuously stirring for 30-50 min at a stirring rate of 180-300 r/min after the mixed solution is added, slowly adding the rest pH value regulator under the stirring condition, and mechanically mixing and stirring for 20-40 min to obtain the finished product of the CMP polishing solution for processing the gallium oxide single crystal wafer.
Compared with the prior art, the invention has the beneficial effects that:
the invention takes polystyrene microsphere emulsion, aluminum nitrate nonahydrate, thiourea and the like as raw materials of a first dispersion liquid; nano silicon carbide, nano molybdenum disulfide, fatty alcohol polyoxyethylene ether and the like are used as raw materials of the second dispersion liquid; and then adding the first dispersion liquid into the second dispersion liquid, and carrying out chemical reaction under the action of magnetic stirring to finally prepare a finished product of the matrix material taking polystyrene microspheres as the inner cores and externally loaded with aluminum oxide, silicon carbide and nano molybdenum disulfide. Then, the substrate is pretreated, so that the substrate is immersed in a modified solution containing nonylphenol polyoxyethylene ether and polyhexamethylene biguanide hydrochloride, and after being uniformly dispersed by ultrasonic, a proper amount of gamma-methacryloxypropyl trimethoxy silane is added into the modified solution. After being uniformly dispersed by ultrasound, the polyhexamethylene biguanide hydrochloride is uniformly dispersed on the surface of a matrix material with a porous microstructure on the surface, and gamma-methacryloxypropyl trimethoxy silane and related groups on the surface of the matrix material are subjected to chemical reaction to form bonds, and a dense three-dimensional network structure is formed on the surface of the matrix material, so that the effective fixation of the polyhexamethylene biguanide hydrochloride dispersed on the surface of the matrix material is finally realized, and the antibacterial property of the matrix material is effectively improved. Meanwhile, due to the existence of the porous microstructure on the surface of the matrix material, the heat dissipation performance of the matrix material is effectively enhanced; the existence of the nano silicon carbide and the nano molybdenum disulfide also effectively improves the wear resistance of the matrix material.
And (3) carrying out grafting reaction between alumina in the pretreated substrate material and an acrylamide monomer under the action of ammonium persulfate, and grafting the acrylamide monomer on the surface of the substrate material through chemical bonds to finally prepare a polishing auxiliary agent finished product. Due to the existence of the acrylamide monomer, the dispersion performance of the prepared polishing auxiliary agent is effectively improved, and the agglomeration phenomenon of the polishing auxiliary agent is reduced. And the acrylamide monomer can play a certain flexible buffering role, so that the situation that the surface of the gallium oxide single crystal wafer is damaged in the polishing process of the gallium oxide single crystal wafer by adopting the polishing solution prepared by the invention can be effectively avoided, and simultaneously, the microcosmic conditions of polishing scratches, surface pressure loss and the like after the surface of the gallium oxide single crystal wafer is polished can be improved, the roughness is reduced, and the polishing quality of the gallium oxide single crystal wafer is ensured.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The CMP polishing solution for gallium oxide single crystal wafer processing is prepared from the following raw materials in percentage by weight: 45% of nano silica sol, 2% of nano manganese dioxide, 1.8% of polyethylene glycol, 1.8% of polishing auxiliary agent, 0.8% of pH value regulator, 2.2% of fatty alcohol polyoxyethylene ether, 1.2% of disodium edetate, 0.015% of polydimethylsilane, 0.03% of dodecyl trimethyl ammonium chloride, 0.02% of benzotriazole and the balance of deionized water.
The preparation method of the polishing auxiliary agent comprises the following steps: putting the pretreated matrix material into deionized water with the mass being 5 times of that of the matrix material, vacuumizing and filling nitrogen for three times, then raising the temperature of the obtained mixed system to 75 ℃, sequentially adding an acrylamide monomer with the mass being 20% of the pretreated matrix material and ammonium persulfate with the mass being 0.08% of the acrylamide monomer into the mixed system at the temperature, and then carrying out heat preservation reaction for 7 hours at the temperature of 75 ℃; after the reaction is finished, the obtained product components are centrifugally separated, the obtained solid filter material is washed for 3 times by deionized water, and finally the solid filter material is placed in a drying oven for drying treatment, so that the polishing auxiliary agent finished product is obtained.
The pretreatment process of the matrix material comprises the following steps: adding a matrix material into a proper amount of modified liquid according to the solid-liquid ratio of 0.08g/mL, performing ultrasonic dispersion for 20min, adding gamma-methacryloxypropyl trimethoxysilane with the mass of 10% of the modified liquid into the modified liquid, and performing heat preservation and stirring reaction for 10h at the temperature of 55 ℃; after the reaction is finished, the obtained product components are subjected to centrifugal separation and drying treatment, and then the pretreatment of the matrix material is completed.
The modified liquid is prepared by uniformly dispersing a proper amount of absolute ethyl alcohol with the concentration of 60 percent, nonylphenol polyoxyethylene ether with the mass of 2.5 percent and polyhexamethylene biguanide hydrochloride with the mass of 10 percent respectively by ultrasonic.
The preparation method of the matrix material comprises the following steps:
injecting deionized water with the volume of 20 times of that of the polystyrene microsphere emulsion with the concentration of 10g/L into the polystyrene microsphere emulsion, performing ultrasonic dispersion for 20min, adding a proper amount of aluminum nitrate nonahydrate into the obtained mixed solution according to the feeding standard of 0.0073mol/L, uniformly mixing and stirring, adding thiourea with the molar quantity of 50% of the aluminum nitrate nonahydrate into the mixed solution, performing magnetic stirring reaction for 2h at 60 ℃ after uniformly mixing and stirring, then adjusting the pH value of the mixed solution to 10.8 by using sodium hydroxide solution with the concentration of 0.1mol/L, and preserving and keeping the obtained first dispersion liquid for later use;
II, respectively adding a proper amount of nano silicon carbide with the particle size of 10nm and nano molybdenum disulfide with the particle size of 5nm into deionized water according to the dosage ratio of 0.02g/mL and 0.015g/mL, then adding fatty alcohol polyoxyethylene ether with the mass of 2% of deionized water into the mixture, and uniformly dispersing the mixture by ultrasonic waves to prepare a second dispersion liquid, and preserving the second dispersion liquid for later use;
III, adding a second dispersion liquid with the volume of 40% of that of the first dispersion liquid into the first dispersion liquid, and magnetically stirring the mixture at 50 ℃ for reaction for 3 hours; after the reaction is finished, the obtained product components are subjected to centrifugal separation, washing and drying in sequence, and finally the obtained solid material is the finished product of the matrix material.
The weight percentage of the silicon dioxide particles in the nano silica sol is 35%, the particle size of the silicon dioxide particles is 8nm, the particle size of the silicon dioxide micelle particles is 45nm, and the average particle size of the nano manganese dioxide is 55nm.
The pH value regulator is prepared from sodium hydroxide and triethanolamine according to a mass ratio of 1:2 are mixed and prepared.
The preparation method of the CMP polishing solution for processing the gallium oxide single crystal wafer comprises the following steps:
firstly, adding nano manganese dioxide and polishing auxiliary agent into nano silica sol, injecting two thirds of deionized water, mechanically mixing and stirring for 20min, and standing the obtained mixed slurry for later use;
step two, adding polyethylene glycol, a surfactant, a chelating agent, polydimethylsilane, dodecyl trimethyl ammonium chloride, benzotriazole and one third of the amount of pH value regulator into the rest deionized water while stirring, and mixing and stirring the materials at a stirring rate of 150r/min to uniformly disperse the materials in the deionized water, so that the obtained mixed solution is preserved for later use;
and thirdly, slowly adding the mixed solution into the mixed slurry at a feeding rate of 80mL/min while stirring, continuously stirring at a stirring rate of 180r/min for 30min after the mixed solution is added, slowly adding the rest pH value regulator under the stirring condition, and mechanically mixing and stirring for 20min to obtain the finished product of the CMP polishing solution for gallium oxide single crystal wafer processing.
Example 2
The preparation method of the CMP polishing solution for gallium oxide single crystal wafer processing provided by the embodiment is basically the same as that of the embodiment 1, and the main difference between the preparation method and the embodiment is that the specific composition and the proportion of the raw materials are different, and the specific composition of the raw materials in the embodiment is as follows:
50% of nano silica sol, 3% of nano manganese dioxide, 2.2% of polyethylene glycol, 2.5% of polishing auxiliary agent, 1.8% of pH value regulator, 2.5% of fatty acid polyoxyethylene ether, 1.5% of ethylenediamine tetraacetic acid, 0.02% of polydimethylsilane, 0.04% of dodecyl trimethyl ammonium chloride, 0.03% of benzotriazole and the balance of deionized water.
The preparation method of the polishing auxiliary agent comprises the following steps: putting the pretreated matrix material into deionized water with the mass being 6 times of that of the matrix material, vacuumizing and filling nitrogen for three times, then raising the temperature of the obtained mixed system to 80 ℃, sequentially adding an acrylamide monomer with the mass being 25% of the pretreated matrix material and ammonium persulfate with the mass being 0.25% of the acrylamide monomer into the mixed system at the temperature, and then carrying out heat preservation reaction for 8 hours at the temperature of 80 ℃; after the reaction is finished, the obtained product components are centrifugally separated, the obtained solid filter material is washed for 4 times by deionized water, and finally the solid filter material is placed in a drying oven for drying treatment, so that the polishing auxiliary agent finished product is obtained.
The pretreatment process of the matrix material comprises the following steps: adding a matrix material into a proper amount of modified liquid according to a solid-liquid ratio of 0.12g/mL, performing ultrasonic dispersion for 25min, adding gamma-methacryloxypropyl trimethoxysilane with the mass of 15% of the modified liquid into the modified liquid, and performing heat preservation and stirring reaction for 12h at the temperature of 60 ℃; after the reaction is finished, the obtained product components are subjected to centrifugal separation and drying treatment, and then the pretreatment of the matrix material is completed.
The modified liquid is prepared by uniformly dispersing a proper amount of absolute ethyl alcohol with the concentration of 70 percent, 3.6 percent of polyoxyethylene nonylphenol ether and 12 percent of polyhexamethylene biguanide hydrochloride by ultrasonic.
The preparation method of the matrix material comprises the following steps:
injecting deionized water with the volume of 25 times of that of the polystyrene microsphere emulsion with the concentration of 12g/L into the polystyrene microsphere emulsion, performing ultrasonic dispersion for 25min, adding a proper amount of aluminum nitrate nonahydrate into the obtained mixed solution according to the feeding standard of 0.0075mol/L, uniformly mixing and stirring, adding thiourea with the molar quantity of 50% of the aluminum nitrate nonahydrate into the mixed solution, performing magnetic stirring reaction for 3h at 70 ℃ after uniformly mixing and stirring, and then adjusting the pH value of the mixed solution to 11.0 by using sodium hydroxide solution with the concentration of 0.12mol/L, wherein the obtained first dispersion is stored and reserved;
II, respectively adding a proper amount of nano silicon carbide with the particle size of 12nm and nano molybdenum disulfide with the particle size of 6nm into deionized water according to the dosage ratio of 0.025g/mL and 0.02g/mL, then adding fatty alcohol polyoxyethylene ether with the mass of 3% of deionized water into the mixture, and uniformly dispersing the mixture by ultrasonic waves to prepare a second dispersion liquid, and preserving the second dispersion liquid for later use;
III, adding 45% of second dispersion liquid into the first dispersion liquid, and magnetically stirring the second dispersion liquid at 55 ℃ for reaction for 4 hours; after the reaction is finished, the obtained product components are subjected to centrifugal separation, washing and drying in sequence, and finally the obtained solid material is the finished product of the matrix material.
The weight percentage of the silicon dioxide particles in the nano silica sol is 40%, the particle size of the silicon dioxide particles is 10nm, the particle size of the silicon dioxide micelle particles is 40nm, and the average particle size of the nano manganese dioxide is 50nm.
The pH value regulator is prepared from sodium hydroxide and triethanolamine according to a mass ratio of 1:3, mixing and preparing.
Example 3
The preparation method of the CMP polishing solution for gallium oxide single crystal wafer processing provided by the embodiment is basically the same as that of the embodiment 1, and the main difference between the preparation method and the embodiment is that the specific composition and the proportion of the raw materials are different, and the specific composition of the raw materials in the embodiment is as follows:
52% of nano silica sol, 4% of nano manganese dioxide, 2.5% of polyethylene glycol, 3.0% of polishing auxiliary agent, 2.5% of pH value regulator, 2.8% of octyl phenol polyoxyethylene ether, 1.8% of hydroxyethyl ethylenediamine triacetic acid, 0.025% of polydimethylsilane, 0.05% of dodecyl trimethyl ammonium chloride, 0.04% of benzotriazole and the balance of deionized water.
The preparation method of the polishing auxiliary agent comprises the following steps: putting the pretreated matrix material into deionized water with the mass being 8 times of that of the matrix material, vacuumizing and filling nitrogen for three times, then raising the temperature of the obtained mixed system to 85 ℃, sequentially adding an acrylamide monomer with the mass being 30% of that of the pretreated matrix material and ammonium persulfate with the mass being 0.42% of that of the acrylamide monomer into the mixed system at the temperature, and then carrying out heat preservation reaction for 10 hours at the temperature of 85 ℃; after the reaction is finished, the obtained product components are centrifugally separated, the obtained solid filter material is washed for 5 times by deionized water, and finally the solid filter material is placed in a drying oven for drying treatment, so that the polishing auxiliary agent finished product is obtained.
The pretreatment process of the matrix material comprises the following steps: adding a matrix material into a proper amount of modified liquid according to a solid-liquid ratio of 0.15g/mL, performing ultrasonic dispersion for 30min, adding gamma-methacryloxypropyl trimethoxysilane with the mass of 20% of the modified liquid into the modified liquid, and performing heat preservation and stirring reaction for 15h at the temperature of 65 ℃; after the reaction is finished, the obtained product components are subjected to centrifugal separation and drying treatment, and then the pretreatment of the matrix material is completed.
The modified liquid is prepared by uniformly dispersing a proper amount of absolute ethyl alcohol with the concentration of 75 percent, 4.2 percent of polyoxyethylene nonylphenol ether and 15 percent of polyhexamethylene biguanide hydrochloride by ultrasonic.
The preparation method of the matrix material comprises the following steps:
injecting deionized water with the volume of 30 times of that of the polystyrene microsphere emulsion with the concentration of 14g/L into the polystyrene microsphere emulsion, performing ultrasonic dispersion for 30min, adding a proper amount of aluminum nitrate nonahydrate into the obtained mixed solution according to the feeding standard of 0.0078mol/L, uniformly mixing and stirring, adding thiourea with the molar quantity of 50% of the aluminum nitrate nonahydrate into the mixed solution, uniformly mixing and stirring, performing magnetic stirring reaction for 4h at 80 ℃, and then adjusting the pH value of the mixed solution to 11.3 by using sodium hydroxide solution with the concentration of 0.15mol/L, wherein the obtained first dispersion is stored and reserved;
II, respectively adding a proper amount of nano silicon carbide with the particle size of 13nm and nano molybdenum disulfide with the particle size of 8nm into deionized water according to the dosage ratio of 0.03g/mL and 0.025g/mL, then adding fatty alcohol polyoxyethylene ether with the mass of 4% of deionized water into the mixture, and uniformly dispersing the mixture by ultrasonic waves to prepare a second dispersion liquid, and preserving the second dispersion liquid for later use;
III, adding a second dispersion liquid with the volume of 50% of that of the first dispersion liquid into the first dispersion liquid, and magnetically stirring the second dispersion liquid at 60 ℃ for reaction for 5 hours; after the reaction is finished, the obtained product components are subjected to centrifugal separation, washing and drying in sequence, and finally the obtained solid material is the finished product of the matrix material.
The weight percentage of the silicon dioxide particles in the nano silica sol is 45%, the particle size of the silicon dioxide particles is 12nm, the particle size of the silicon dioxide micelle particles is 35nm, and the average particle size of the nano manganese dioxide is 45nm.
The pH value regulator is prepared from sodium hydroxide and triethanolamine according to a mass ratio of 1:4, mixing and preparing.
Comparative example 1: the preparation method of the polishing solution and the specific proportion of the raw materials provided in the embodiment are approximately the same as those in embodiment 1, and the main differences are that: the raw materials used in this example do not contain polishing aids;
comparative example 2: the preparation method of the polishing solution and the specific proportion of the raw materials provided in the embodiment are approximately the same as those in embodiment 1, and the main differences are that: in the embodiment, the polishing auxiliary agent is replaced by an equivalent amount of pretreated matrix material;
comparative example 3: the preparation method of the polishing solution and the specific proportion of the raw materials provided in the embodiment are approximately the same as those in embodiment 1, and the main differences are that: in this example, the polishing auxiliary agent is replaced by an equal amount of matrix material;
performance testing
Will be respectively realized by the present inventionPolishing solutions prepared in examples 1 to 3 were designated as experimental examples 1 to 3; the polishing solutions prepared by comparative examples 1 to 3 were referred to as comparative examples 1 to 3; then polishing the gallium oxide single crystal wafer (wafer size is four inches) with each group of polishing liquid samples (chemical mechanical polishing is carried out on the gallium oxide single crystal wafer with Unipol-1502 precision polishing machine), wherein the polishing pressure is set to be 350g/cm 2 The polishing disk rotation speed was set at 60RPM and the slurry flow was set at 20mL/min. After finishing polishing, the surface granularity and scratch condition of the wafer are tested by adopting a surface defect meter (Candela 8520), then the surface roughness is tested by using an atomic ion microscope, meanwhile, the antibacterial performance of the wafer is tested, and the obtained test data are recorded in the following table:
as can be seen from comparison and analysis of related data in the table, the polishing solution prepared by the invention can effectively avoid the situation that the surface of the gallium oxide single crystal wafer is damaged in the polishing process, and can improve microscopic conditions such as polishing scratches, surface pressure loss and the like after the surface of the gallium oxide single crystal wafer is polished, reduce roughness and ensure the polishing quality of the gallium oxide single crystal wafer. Furthermore, the polishing solution prepared by the invention has better cleaning performance, antibacterial performance and wear resistance, prolongs the service life to a certain extent, and effectively improves the quality. Therefore, the polishing solution produced by the invention has wider market prospect and is more suitable for popularization.
In the description of the present specification, the descriptions of the terms "one embodiment," "example," "specific example," and the like, mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The preferred embodiments of the invention disclosed above are intended only to assist in the explanation of the invention. The preferred embodiments are not exhaustive or to limit the invention to the precise form disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best understand and utilize the invention. The invention is limited only by the claims and the full scope and equivalents thereof.
Claims (6)
1. The CMP polishing solution for processing the gallium oxide single crystal wafer is characterized in that: the polishing solution is prepared from the following raw materials in percentage by weight: 45-52% of nano silica sol, 2-4% of nano manganese dioxide, 1.8-2.5% of polyethylene glycol, 1.8-3.0% of polishing auxiliary agent, 0.8-2.5% of pH value regulator, 2.2-2.8% of surfactant, 1.2-1.8% of chelating agent, 0.015-0.025% of polydimethylsilane, 0.03-0.05% of dodecyl trimethyl ammonium chloride, 0.02-0.04% of benzotriazole and the balance of deionized water;
the preparation method of the polishing auxiliary agent comprises the following steps: putting the pretreated matrix material into deionized water with the mass being 5-8 times of that of the matrix material, vacuumizing and filling nitrogen for three times, then raising the temperature of the obtained mixed system to 75-85 ℃, sequentially adding 20-30% of acrylamide monomer with the mass being 20-30% of that of the pretreated matrix material and 0.08-0.42% of ammonium persulfate with the mass being 0.08-0.42% of that of the acrylamide monomer into the mixed system at the temperature, and then carrying out heat preservation reaction for 7-10 h at the temperature of 75-85 ℃; after the reaction is finished, centrifugally separating the obtained product components, washing the obtained solid filter material with deionized water for 3-5 times, and finally placing the solid filter material in a drying oven for drying treatment to obtain a polishing auxiliary agent finished product;
the pretreatment process of the matrix material comprises the following steps: adding a matrix material into a proper amount of modified liquid according to the solid-liquid ratio of 0.08-0.15 g/mL, performing ultrasonic dispersion for 20-30 min, adding gamma-methacryloxypropyl trimethoxy silane with the mass of 10-20% of the modified liquid into the modified liquid, and performing heat preservation and stirring reaction for 10-15 h at the temperature of 55-65 ℃; after the reaction is finished, the obtained product components are subjected to centrifugal separation and drying treatment, and the pretreatment of the matrix material is finished;
the modified liquid is prepared by uniformly dispersing a proper amount of absolute ethyl alcohol with the concentration of 60-75% and nonylphenol polyoxyethylene ether with the mass of 2.5-4.2% and polyhexamethylene biguanide hydrochloride with 10-15% by ultrasound;
the preparation method of the matrix material comprises the following steps:
injecting deionized water with the volume of 20-30 times of that of the polystyrene microsphere emulsion with the concentration of 10-14 g/L into the polystyrene microsphere emulsion, performing ultrasonic dispersion for 20-30 min, adding a proper amount of aluminum nitrate nonahydrate into the obtained mixed solution according to the feeding standard of 0.0073-0.0078 mol/L, uniformly mixing and stirring, adding thiourea with the molar quantity of 50% of aluminum nitrate nonahydrate into the mixed solution, performing magnetic stirring reaction for 2-4 h at the temperature of 60-80 ℃ after uniformly mixing and stirring, and then adjusting the pH value of the mixed solution to 10.8-11.3 by using sodium hydroxide solution with the concentration of 0.1-0.15 mol/L, thereby obtaining a first dispersion liquid for storage and standby;
II, respectively adding a proper amount of nano silicon carbide with the particle size of 10-13 nm and nano molybdenum disulfide with the particle size of 5-8 nm into deionized water according to the dosage ratio of 0.02-0.03 g/mL and 0.015-0.025 g/mL, then adding fatty alcohol polyoxyethylene ether with the mass of 2-4% of that of the deionized water into the deionized water, uniformly dispersing the mixture by ultrasonic waves to prepare second dispersion liquid, and preserving the second dispersion liquid for later use;
III, adding a second dispersion liquid with the volume of 40-50% of that of the first dispersion liquid into the first dispersion liquid, and then magnetically stirring the first dispersion liquid at 50-60 ℃ for reaction for 3-5 h; after the reaction is finished, the obtained product components are subjected to centrifugal separation, washing and drying in sequence, and finally the obtained solid material is the finished product of the matrix material.
2. The CMP polishing liquid for gallium oxide single-wafer processing according to claim 1, wherein: the weight percentage of the silicon dioxide particles in the nano silica sol is 35-45%, the particle size of the silicon dioxide particles is 8-12 nm, the particle size of the silicon dioxide micelle particles is less than or equal to 45nm, and the average particle size of the nano manganese dioxide is less than or equal to 55nm.
3. The CMP polishing liquid for gallium oxide single-wafer processing according to claim 1, wherein: the surfactant is selected from any one of fatty alcohol polyoxyethylene ether, fatty acid polyoxyethylene ether, octyl phenol polyoxyethylene ether and methyl stearate polyoxyethylene ether.
4. The CMP polishing liquid for gallium oxide single-wafer processing according to claim 1, wherein: the pH value regulator is prepared from sodium hydroxide and triethanolamine according to a mass ratio of 1: 2-4.
5. The CMP polishing liquid for gallium oxide single-wafer processing according to claim 1, wherein: the chelating agent is selected from any one of disodium ethylenediamine tetraacetate, tartaric acid, ethylenediamine tetraacetic acid and hydroxyethyl ethylenediamine triacetic acid.
6. The method for preparing a CMP polishing liquid for processing gallium oxide single crystal wafers according to any one of claims 1 to 5, comprising the steps of:
firstly, adding nano manganese dioxide and polishing auxiliary agent into nano silica sol, injecting two thirds of deionized water, mechanically mixing and stirring for 20-40 min, and standing the obtained mixed slurry for later use;
step two, adding polyethylene glycol, a surfactant, a chelating agent, polydimethylsilane, dodecyl trimethyl ammonium chloride, benzotriazole and one third of the amount of pH value regulator into the rest deionized water while stirring, and mixing and stirring the materials at a stirring rate of 150-250 r/min to uniformly disperse the materials in the deionized water, so that the obtained mixed solution is preserved for later use;
and thirdly, slowly adding the mixed solution into the mixed slurry at a feeding rate of 80-120 mL/min while stirring, continuously stirring for 30-50 min at a stirring rate of 180-300 r/min after the mixed solution is added, slowly adding the rest pH value regulator under the stirring condition, and mechanically mixing and stirring for 20-40 min to obtain the finished product of the CMP polishing solution for processing the gallium oxide single crystal wafer.
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| CN105153943A (en) * | 2015-09-10 | 2015-12-16 | 盐城工学院 | Anti-cleavage polishing solution for gallium oxide wafer and preparation method of anti-cleavage polishing solution |
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| CN105153943A (en) * | 2015-09-10 | 2015-12-16 | 盐城工学院 | Anti-cleavage polishing solution for gallium oxide wafer and preparation method of anti-cleavage polishing solution |
| CN109880533A (en) * | 2019-03-26 | 2019-06-14 | 中南大学 | A kind of composite abrasive grain polishing solution and preparation method thereof |
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