CN117821014A - Self-modified alumina material for polishing and preparation method and application thereof - Google Patents
Self-modified alumina material for polishing and preparation method and application thereof Download PDFInfo
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- CN117821014A CN117821014A CN202311759062.6A CN202311759062A CN117821014A CN 117821014 A CN117821014 A CN 117821014A CN 202311759062 A CN202311759062 A CN 202311759062A CN 117821014 A CN117821014 A CN 117821014A
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- 238000005498 polishing Methods 0.000 title claims abstract description 44
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 239000000463 material Substances 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000000843 powder Substances 0.000 claims abstract description 27
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910002601 GaN Inorganic materials 0.000 claims abstract description 22
- 239000002002 slurry Substances 0.000 claims abstract description 17
- 238000003756 stirring Methods 0.000 claims abstract description 11
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000002253 acid Substances 0.000 claims abstract description 10
- 229910052582 BN Inorganic materials 0.000 claims abstract description 9
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 9
- -1 aluminum compound Chemical class 0.000 claims abstract description 9
- 239000007788 liquid Substances 0.000 claims abstract description 9
- 239000002245 particle Substances 0.000 claims abstract description 8
- 238000001354 calcination Methods 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- 239000002270 dispersing agent Substances 0.000 claims abstract description 5
- 238000001694 spray drying Methods 0.000 claims abstract description 5
- 239000002738 chelating agent Substances 0.000 claims abstract description 4
- 239000007800 oxidant agent Substances 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims description 18
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 10
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 9
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 9
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 8
- 239000004576 sand Substances 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 7
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 6
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 claims description 6
- SMYKVLBUSSNXMV-UHFFFAOYSA-K aluminum;trihydroxide;hydrate Chemical compound O.[OH-].[OH-].[OH-].[Al+3] SMYKVLBUSSNXMV-UHFFFAOYSA-K 0.000 claims description 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 4
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 3
- 239000004471 Glycine Substances 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 3
- 235000001014 amino acid Nutrition 0.000 claims description 3
- 150000001413 amino acids Chemical class 0.000 claims description 3
- 150000001732 carboxylic acid derivatives Chemical class 0.000 claims description 3
- 239000004310 lactic acid Substances 0.000 claims description 3
- 235000014655 lactic acid Nutrition 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 235000006408 oxalic acid Nutrition 0.000 claims description 3
- 239000006174 pH buffer Substances 0.000 claims description 3
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 claims description 3
- 229960004889 salicylic acid Drugs 0.000 claims description 3
- 239000011975 tartaric acid Substances 0.000 claims description 3
- 235000002906 tartaric acid Nutrition 0.000 claims description 3
- GDFIFJMSTFQDLW-UHFFFAOYSA-K O.O.[OH-].[OH-].[OH-].[Al+3] Chemical compound O.O.[OH-].[OH-].[OH-].[Al+3] GDFIFJMSTFQDLW-UHFFFAOYSA-K 0.000 claims description 2
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 claims description 2
- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 claims description 2
- YPUVTLQZHBUGSK-UHFFFAOYSA-K aluminum;trihydroxide;trihydrate Chemical compound O.O.O.[OH-].[OH-].[OH-].[Al+3] YPUVTLQZHBUGSK-UHFFFAOYSA-K 0.000 claims description 2
- 229910001593 boehmite Inorganic materials 0.000 claims description 2
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 claims description 2
- 238000003801 milling Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 238000010979 pH adjustment Methods 0.000 claims 1
- 239000002131 composite material Substances 0.000 abstract description 4
- 230000007547 defect Effects 0.000 abstract description 4
- 230000001590 oxidative effect Effects 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 230000003746 surface roughness Effects 0.000 abstract description 2
- 239000003795 chemical substances by application Substances 0.000 abstract 1
- 239000006179 pH buffering agent Substances 0.000 abstract 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 7
- 239000013078 crystal Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical group OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 3
- 239000005708 Sodium hypochlorite Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- PQRHBEQNPCVBSM-UHFFFAOYSA-M potassium;2-carboxybenzoate;hydrochloride Chemical compound Cl.[K+].OC(=O)C1=CC=CC=C1C([O-])=O PQRHBEQNPCVBSM-UHFFFAOYSA-M 0.000 description 3
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 description 1
- IVLXQGJVBGMLRR-UHFFFAOYSA-N 2-aminoacetic acid;hydron;chloride Chemical compound Cl.NCC(O)=O IVLXQGJVBGMLRR-UHFFFAOYSA-N 0.000 description 1
- QPCDCPDFJACHGM-UHFFFAOYSA-N N,N-bis{2-[bis(carboxymethyl)amino]ethyl}glycine Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(=O)O)CCN(CC(O)=O)CC(O)=O QPCDCPDFJACHGM-UHFFFAOYSA-N 0.000 description 1
- 229920002125 Sokalan® Polymers 0.000 description 1
- AZFNGPAYDKGCRB-XCPIVNJJSA-M [(1s,2s)-2-amino-1,2-diphenylethyl]-(4-methylphenyl)sulfonylazanide;chlororuthenium(1+);1-methyl-4-propan-2-ylbenzene Chemical compound [Ru+]Cl.CC(C)C1=CC=C(C)C=C1.C1=CC(C)=CC=C1S(=O)(=O)[N-][C@@H](C=1C=CC=CC=1)[C@@H](N)C1=CC=CC=C1 AZFNGPAYDKGCRB-XCPIVNJJSA-M 0.000 description 1
- YBCVMFKXIKNREZ-UHFFFAOYSA-N acoh acetic acid Chemical compound CC(O)=O.CC(O)=O YBCVMFKXIKNREZ-UHFFFAOYSA-N 0.000 description 1
- KBKZYWOOZPIUJT-UHFFFAOYSA-N azane;hypochlorous acid Chemical compound N.ClO KBKZYWOOZPIUJT-UHFFFAOYSA-N 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 238000012946 outsourcing Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000007517 polishing process Methods 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 235000019422 polyvinyl alcohol Nutrition 0.000 description 1
- 235000010333 potassium nitrate Nutrition 0.000 description 1
- 239000004323 potassium nitrate Substances 0.000 description 1
- 235000010289 potassium nitrite Nutrition 0.000 description 1
- 239000004304 potassium nitrite Substances 0.000 description 1
- 239000012286 potassium permanganate Substances 0.000 description 1
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- PFUVRDFDKPNGAV-UHFFFAOYSA-N sodium peroxide Chemical compound [Na+].[Na+].[O-][O-] PFUVRDFDKPNGAV-UHFFFAOYSA-N 0.000 description 1
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 description 1
- KHQHQJDNEISKKS-UHFFFAOYSA-M sodium;2-chloroacetic acid;hydroxide Chemical compound [OH-].[Na+].OC(=O)CCl KHQHQJDNEISKKS-UHFFFAOYSA-M 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
Landscapes
- Polishing Bodies And Polishing Tools (AREA)
Abstract
The invention discloses a self-modified alumina material for polishing and a preparation method and application thereof, wherein the preparation method of the self-modified alumina material comprises the following steps: s1, dispersing cubic boron nitride powder in acid liquor, and uniformly stirring and dispersing to obtain slurry; s2, adding aluminum compound powder into the slurry, fully stirring for reaction, then spray-drying to obtain powder, calcining to obtain self-modified alumina powder, and carrying out sanding treatment on the self-modified alumina powder to obtain the powder slurry with the particle size distribution required by polishing liquid, so as to further prepare the polishing liquid, wherein the polishing liquid also contains an oxidant, a pH buffering agent, a pH value adjusting agent, a chelating agent and a dispersing agent. The polishing solution prepared based on the composite alumina material is not only beneficial to improving the removal rate of gallium nitride, but also reduces the surface roughness and further reduces the defects of surface scratches and the like.
Description
Technical Field
The invention relates to the field of inorganic materials and semiconductors, in particular to a self-modified alumina material for polishing, a preparation method and application thereof.
Background
Gallium nitride has the excellent characteristics of large forbidden bandwidth, high saturation electron drift velocity, high breakdown field strength, high thermal conductivity, low dielectric constant, strong radiation resistance and the like, has become a third-generation semiconductor material for replacing Si-based materials, is also an ideal material for high-temperature, high-frequency, high-power and photoelectric integrated circuits and the like, and has great application potential in ultraviolet and laser light emitting diodes.
The gallium nitride is made into a substrate or an electronic component, the GaN wafer is required to be subjected to planarization treatment, the surface of the wafer is required to be ultra-smooth, defect-free and damage-free, and the processing quality and precision of GaN also directly influence the performance of the component. However, because gallium nitride has the characteristics of high hardness, high brittleness, strong chemical inertness and the like, the polishing planarization of gallium nitride is not very challenging, and especially the treatment of Ga surface is always the bottleneck of gallium nitride development.
While less research on polishing gallium nitride in China, china patent 2009101805295 discloses a gallium nitride crystal polishing method, wherein ultraviolet light source irradiation is added during polishing, and a self-made water bath heating system is used for heating polishing liquid, so that the chemical reaction rate in the chemical mechanical polishing process is improved, but the device structure is complex. In 2009, yan huaiyue et al studied the polishing effect of different abrasive particles on gallium nitride under alkaline conditions, and found that the removal rate applicable to 1 μm was maximum, but the surface scratch defects were more. The Hideo Aida published in Mrs Proceedings uses silicon oxide as the abrasive for gallium nitride polishing, the removal rate is only 17nm/h, and the efficiency is low.
Disclosure of Invention
Aiming at the problems of low removal rate, easiness in generating scratches, pits and the like of the gallium nitride polishing solution in the prior art, the invention provides the self-modified aluminum oxide material for polishing and the preparation method and application thereof, and the self-modified aluminum oxide material can obviously improve the removal rate of polishing to more than 190nm/h, has smooth surface, no obvious defects and roughness less than 3nm.
The technical scheme of the invention is as follows:
the invention relates to a preparation method of a self-modified alumina material for polishing, which comprises the following steps:
s1, dispersing cubic boron nitride powder in acid liquor, and uniformly stirring and dispersing to obtain slurry;
s2, adding aluminum compound powder into the slurry obtained in the step S1, fully stirring for reaction, spray-drying to obtain powder, and calcining to obtain the self-modified alumina powder.
Preferably, in the step S1, the particle diameter d50 of the cubic boron nitride powder is 10-100nm, d99 is less than or equal to 300nm, and the cubic boron nitride is used as a crystal nucleus.
Preferably, in the step S1, the acid solution is one or more of hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, citric acid, carboxylic acid, salicylic acid, glycine, oxalic acid, tartaric acid, lactic acid and amino acid, and the pH of the acid solution is 1-6.
Preferably, in step S2, the aluminum compound is one or more of aluminum hydroxide monohydrate, aluminum hydroxide dihydrate, aluminum hydroxide trihydrate, boehmite, pseudo-boehmite, aluminum isopropoxide.
Preferably, in the step S2, aluminum compound powder is added, and the mixture is fully stirred for reaction for 2 to 10 hours; the calcination process comprises the following steps: heating to 400-650 ℃ at a heating rate of 1-10 ℃/min, preserving heat for 1-10h, heating to 1000-1500 ℃ at a heating rate of 1-20 ℃/min, preserving heat for 1-10h, and naturally cooling in a cooling section.
Preferably, the mass ratio of the cubic boron nitride powder to the aluminum compound is 1:10 to 20.
Preferably, the method also comprises sand milling treatment, specifically, the self-modified alumina powder obtained in the step S2 is treated to have the particle size of d50=0.5-2 mu m and the d99 is less than 10 mu m by a sand mill, so as to obtain the self-modified alumina slurry with the solid content of 10-30%.
The invention also relates to a self-modified alumina material for polishing, which is prepared by adopting the preparation method.
The invention also relates to application of the self-modified aluminum oxide material for polishing in preparation of gallium nitride polishing solution.
Preferably, the gallium nitride polishing solution further comprises an oxidant, a pH buffer, a pH value regulator, a chelating agent and a dispersing agent.
Preferably, the oxidant is one or more of Fenton reaction liquid, hydrogen peroxide, sodium peroxide, potassium permanganate, sodium hypochlorite, ammonium hypochlorite, potassium nitrate, potassium nitrite, sodium persulfate and potassium peroxodisulfate;
the pH buffer is one or more of an glycine-hydrochloric acid system, a potassium hydrogen phthalate-hydrochloric acid system, a monochloroacetic acid-sodium hydroxide system and a hexamethylenetetramine-hydrochloric acid system, and an acetic acid-acetate system;
the pH value is adjusted to one or more of hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, citric acid, carboxylic acid, salicylic acid, glycine, oxalic acid, tartaric acid, lactic acid and amino acid;
the chelating agent is EDTA and/or DTPA;
the dispersing agent is any one of polycarboxylic acid compounds, polyvinyl alcohols, polyacrylic acids and phosphoric acid dispersing agents.
The beneficial effects of the invention are as follows:
(1) According to the invention, the gallium nitride polishing solution is prepared based on composite aluminum oxide, and the growth orientation of aluminum oxide crystals is changed on the crystal nucleus based on the cubic crystal form of cubic boron nitride, so that the distribution surface fluffy appearance is formed, and the physical properties of aluminum oxide are changed.
(2) The polishing solution can obviously improve the removal rate of polishing from 90nm/h of common alumina to 190nm/h, has smooth surface, no obvious defect and roughness less than 3nm.
Drawings
The invention is further described below with reference to the accompanying drawings and examples:
FIG. 1 is an SEM image of self-modifying alumina powder of example 1;
fig. 2 is an atomic microscope image of the gallium nitride surface after polishing.
Detailed Description
The objects, technical solutions and advantages of the present invention will become more apparent by the following detailed description of the present invention with reference to the accompanying drawings. It should be understood that the description is only illustrative and is not intended to limit the scope of the invention. In addition, in the following description, descriptions of well-known structures and techniques are omitted so as not to unnecessarily obscure the present invention.
Example 1
(1) Phosphoric acid (mass concentration: 85%) was added to 100kg of pure water, the pH was adjusted to 5.0, and then 2kg of hexagonal boron nitride powder having d50=80 nm and d99=270 nm was added thereto, followed by stirring and dispersion.
(2) Adding 30kg of aluminum hydroxide monohydrate into the slurry obtained in the step (1), fully stirring and reacting for 5 hours, then spray-drying to obtain spherical powder, calcining by using a high-temperature furnace, heating up to a temperature curve of 0-600 ℃, heating up to a temperature of 4 ℃/min, insulating at 600 ℃ for 2 hours, heating up to 600-1100 ℃, heating up to a temperature of 3 ℃/min, insulating at 1100 ℃ for 3 hours, and naturally cooling.
(3) And (3) carrying out sand grinding and grading treatment on the product obtained in the step (2) by using a sand grinder to obtain composite alumina slurry with the particle size distribution of d50=1.2 mu m and d99=8.1 mu m, wherein the solid content is 20%.
(4) Taking 20kg of the slurry obtained in the step (3), regulating the pH of the obtained slurry to 4 by using phosphoric acid (the mass concentration is 85%), then adding 200g of potassium hydrogen phthalate-hydrochloric acid system, adding 0.8kg of sodium hypochlorite, 300g of polycarboxylic acid polymer F38 and 50g of EDTA, and fully stirring for 3 hours to obtain the gallium nitride polishing solution.
Comparative example 1
(1) Phosphoric acid (mass concentration: 85%) was added to 100kg of pure water, the pH was adjusted to 5.0, and the mixture was stirred and dispersed uniformly.
(2) Adding 30kg of aluminum hydroxide monohydrate into the slurry obtained in the step (1), fully stirring and reacting for 5 hours, then spray-drying to obtain spherical powder, calcining by using a high-temperature furnace, heating up to a temperature curve of 0-600 ℃, heating up to a temperature of 4 ℃/min, insulating at 600 ℃ for 2 hours, heating up to 600-1100 ℃, heating up to a temperature of 3 ℃/min, insulating at 1100 ℃ for 3 hours, and naturally cooling.
(3) And (3) carrying out sand grinding and grading treatment on the product obtained in the step (2) by using a sand grinder to obtain composite alumina slurry with the particle size distribution of d50=1.2 mu m and d99=8.1 mu m, wherein the solid content is 20%.
(4) Taking 20kg of the slurry obtained in the step (3), regulating the pH of the obtained slurry to 4 by using phosphoric acid (the mass concentration is 85%), then adding 200g of potassium hydrogen phthalate-hydrochloric acid system, adding 0.8kg of sodium hypochlorite, 300g of polycarboxylic acid polymer F38 and 50g of EDTA, and fully stirring for 3 hours to obtain the gallium nitride polishing solution.
Comparative example 2
Outsourcing samples: anhui crystal grain d50:1.2 μm alumina polishing powder, this sample was used to prepare a polishing liquid according to the formulation of the polishing liquid in example 1.
Polishing comparative experiment
Different samples are used for preparing polishing solutions with the same formula, and the polishing removal rate is compared and verified, and the process is used: OKAMOTO GNX200BH polisher, 5cm of gallium nitride wafer, single-sided polishing, rotation speed of 100rpm, polishing time of 1h, removal rate data as shown in table 1 below:
TABLE 1
| Removal rate (nm/h) | |
| Example 1 | 194 |
| Comparative example 1 | 91 |
| Comparative example 2 | 102 |
From the polishing removal rate data in the table, it can be seen that the removal rate of example 1 is improved by approximately 100% over the conventional product.
Fig. 1 is an SEM image of the self-modified alumina powder in example 1, fig. 2 is an atomic microscope image of the surface of gallium nitride polished by the gallium nitride polishing liquid prepared in example 1, the appearance of the product in fig. 1 is like sphere and fluff, and the surface roughness of the product in fig. 2 is about 3nm, which meets the requirements.
It is to be understood that the above-described embodiments of the present invention are merely illustrative of or explanation of the principles of the present invention and are in no way limiting of the invention. Accordingly, any modification, equivalent replacement, improvement, etc. made without departing from the spirit and scope of the present invention should be included in the scope of the present invention. Furthermore, the appended claims are intended to cover all such changes and modifications that fall within the scope and boundary of the appended claims, or equivalents of such scope and boundary.
Claims (10)
1. The preparation method of the self-modified alumina material for polishing is characterized by comprising the following steps of:
s1, dispersing cubic boron nitride powder in acid liquor, and uniformly stirring and dispersing to obtain slurry;
s2, adding aluminum compound powder into the slurry obtained in the step S1, fully stirring for reaction, spray-drying to obtain powder, and calcining to obtain the self-modified alumina powder.
2. The method according to claim 1, wherein in the step S1, the particle diameter d50 of the cubic boron nitride powder is 10-100nm, and d99 is less than or equal to 300nm.
3. The method according to claim 1, wherein in the step S1, the acid is one or more of hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, citric acid, carboxylic acid, salicylic acid, glycine, oxalic acid, tartaric acid, lactic acid and amino acid, and the pH of the acid is 1-6.
4. The method according to claim 1, wherein in step S2, the aluminum compound is one or more of aluminum hydroxide monohydrate, aluminum hydroxide dihydrate, aluminum hydroxide trihydrate, boehmite, pseudo-boehmite, aluminum isopropoxide.
5. The preparation method according to claim 1, wherein in step S2, aluminum compound powder is added and fully stirred for reaction for 2-10 hours; the calcination process comprises the following steps: heating to 400-650 ℃ at a heating rate of 1-10 ℃/min, preserving heat for 1-10h, heating to 1000-1500 ℃ at a heating rate of 1-20 ℃/min, preserving heat for 1-10h, and naturally cooling in a cooling section.
6. The preparation method according to claim 1, wherein the mass ratio of the cubic boron nitride powder to the aluminum compound is 1:10 to 20.
7. The method according to claim 1, further comprising a sand milling treatment, specifically, the self-modified alumina powder obtained in step S2 is treated to a particle size d50=0.5-2 μm and d99 < 10 μm by a sand mill, to obtain a self-modified alumina slurry.
8. A self-modifying alumina material for polishing, characterized by being produced by the production method according to any one of claims 1 to 7.
9. Use of the self-modifying aluminum oxide material for polishing as claimed in claim 8 for preparing a gallium nitride polishing liquid.
10. The use according to claim 9, wherein the gallium nitride polishing liquid further comprises an oxidizing agent, a pH buffer, a pH adjustment, a chelating agent, a dispersing agent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311759062.6A CN117821014A (en) | 2023-12-20 | 2023-12-20 | Self-modified alumina material for polishing and preparation method and application thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311759062.6A CN117821014A (en) | 2023-12-20 | 2023-12-20 | Self-modified alumina material for polishing and preparation method and application thereof |
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| Publication Number | Publication Date |
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| CN117821014A true CN117821014A (en) | 2024-04-05 |
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| CN202311759062.6A Pending CN117821014A (en) | 2023-12-20 | 2023-12-20 | Self-modified alumina material for polishing and preparation method and application thereof |
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| Country | Link |
|---|---|
| CN (1) | CN117821014A (en) |
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2023
- 2023-12-20 CN CN202311759062.6A patent/CN117821014A/en active Pending
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Inventor after: Wang Zhen Inventor after: Zou Bo Inventor after: Wu Yonglong Inventor after: Dong Ruiwei Inventor before: Wang Zhen Inventor before: Wu Yonglong Inventor before: Dong Ruiwei |