CN113881348A - Composite alumina polishing solution and preparation method and application thereof - Google Patents
Composite alumina polishing solution and preparation method and application thereof Download PDFInfo
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- CN113881348A CN113881348A CN202111298074.4A CN202111298074A CN113881348A CN 113881348 A CN113881348 A CN 113881348A CN 202111298074 A CN202111298074 A CN 202111298074A CN 113881348 A CN113881348 A CN 113881348A
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- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
Abstract
The invention discloses a composite alumina polishing solution and a preparation method and application thereof, wherein the preparation method comprises the following steps: mixing aluminum hydroxide and lanthanum oxide according to a certain mass ratio; calcining the mixture to obtain a calcined material mixed by aluminum oxide and lanthanum oxide, and controlling the calcined material to lose 25-40% of the mass; adding the fired material into deionized water for mixing; ball milling to obtain ball grinding material; adding multi-silicon-based functional silane with the mass ratio of 0.5-5% of the calcined material into the ball-milled material, uniformly mixing, aging at 150 ℃ for 20-60 minutes, and filtering by adopting a filter bag with the aperture of 2 mu m; and adding a dispersing agent, a lubricant, a surfactant, an ionic stabilizer, a thickening agent, a pH value regulator and deionized water into the obtained material, and mixing to obtain the composite alumina polishing solution. The polishing solution prepared by the invention can greatly improve the cutting amount, realize low loss and high yield on the premise of ensuring high surface quality of the object to be polished and no scratch on the surface.
Description
Technical Field
The invention belongs to the technical field of semiconductor polishing, and particularly relates to a composite aluminum oxide polishing solution, and a preparation method and application thereof.
Background
Many semiconductor materials, particularly semiconductor wafer substrates and epitaxial wafers, require polishing to achieve the required flatness. Silicon dioxide polishing solutions are used in the mainstream market for polishing conventional semiconductor materials. However, with the advance of technology, the use of new semiconductor materials such as silicon carbide, gallium nitride, etc. is becoming more widespread. The traditional silicon dioxide polishing solution can not completely meet the original process requirements, particularly the requirements on the cutting rate. Therefore, there is a need for a polishing solution that can meet the requirements of high cutting rate and high surface quality of semiconductor materials such as silicon carbide and gallium nitride.
Disclosure of Invention
In order to solve the technical problems, the invention provides the composite alumina polishing solution and the preparation method and the application thereof.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a preparation method of composite alumina polishing solution comprises the following steps:
(1) mixing aluminum hydroxide and lanthanum oxide according to a certain mass ratio;
(2) calcining the mixture at the temperature of 1000-1200 ℃ for 1-6 hours to obtain a calcined material mixed by aluminum oxide and lanthanum oxide, and controlling the mass loss of 25-40% after calcination;
(3) adding deionized water into the fired material, and mixing, wherein the mass ratio of the fired material to the deionized water is (30-45): (55-70); ball milling until D50 is between 300 and 500nm to obtain ball milling material;
(4) adding multi-silicon-based functional silane with the mass ratio of 5-25% of the burned material into the ball-milled material, uniformly mixing, aging at 150 ℃ for 20-60 minutes, and filtering by adopting a filter bag with the aperture of 2 mu m;
(5) and adding a dispersing agent, a lubricating agent, a surfactant, an ionic stabilizer, a thickening agent, a pH value regulator and deionized water into the obtained material, and mixing to obtain the composite alumina polishing solution with the solid content of 5-25% and the pH value of 7-8.
In the scheme, in the step (1), the mass ratio of the aluminum hydroxide to the lanthanum oxide is (95-99.5): (0.5-5).
In the above scheme, in the step (4), the multi-silicon-based functional silane is aminosilane or ureido silane.
In the scheme, in the step (5), the addition amount of the dispersing agent accounts for 0.1-1% of the burnt material in percentage by mass; the dispersing agent is one or a combination of more of triphosphates, triethylhexyl phosphoric acid, methyl amyl alcohol, polyalcohols, polyethers, polyacrylic acids, fatty acid polyesters, sodium dodecyl sulfate, stearic acid monoglyceride, oxidized polyethylene wax and sodium methylene dinaphthalene sulfonate.
In the above embodiment, in the step (5), the lubricant is added in an amount of 5 to 10% by mass based on the burned material, and the lubricant is selected from one or a combination of more of glycerol, polypropylene glycol and polybutylene glycol.
In the above scheme, in the step (5), the addition amount of the surfactant accounts for 0.5-1.5% of the burnt material by mass percent, and the surfactant is a nonionic surfactant.
In the scheme, in the step (5), the addition amount of the ionic stabilizer accounts for 0.01-0.5% of the burnt material by mass percentage; the ionic stabilizer is selected from one or more of HPMA, inorganic soluble salts and organic acids.
In the scheme, in the step (5), the addition amount of the thickening agent accounts for 0.5-2% of the burnt material by mass percentage; the thickening agent is one or more of carboxymethyl cellulose, methyl cellulose, sodium starch phosphate, sodium polyacrylate, polyoxyethylene, carbomer and inorganic salt.
A composite alumina polishing solution prepared by the preparation method of any one of the above.
The composite alumina polishing solution is applied to polishing of silicon carbide and gallium nitride semiconductor materials.
Through the technical scheme, the preparation method of the composite aluminum oxide polishing solution provided by the invention has the following beneficial effects:
1. according to the invention, a small amount of lanthanum oxide is added into aluminum hydroxide, so that the gradient of the calcination curve of the aluminum hydroxide is reduced, and the calcination parameters are conveniently and accurately controlled, thereby improving the product quality.
2. According to the invention, after the mixture is calcined, the ball grinding material with D50 of 300-500nm is prepared, then the multi-silicon-based functional silane is added, after mixing, the composite structure of Al-O-Si-functional group is formed after aging, on one hand, the composite structure can provide enough hardness for the powder, and the cutting rate is dozens of times higher than that of the conventional silica sol; on the other hand, the functional group can form stable connection with a surfactant in the polishing solution through an ionic bond, the electronic potential of the composite alumina abrasive particles is changed, and the dispersibility, the discreteness and the cleanability of the polishing powder are improved, so that the cutting rate is improved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below.
FIG. 1 is a schematic view showing the microstructure of the surface of alumina ball abrasive grains prepared in example 1 of the present invention;
fig. 2 is an atomic force electron microscope image of a local surface of a silicon carbide wafer to which the polishing solution prepared in example 1 of the present invention is applied: (a) is a magnification of 250 times, (b) is a magnification of 500 times, (c) is a magnification of 1000 times, and (c) is a partial region of (b), (b) is a partial region of (a); (d) is a cross section diagram of atomic force microscope scanning, which is a cross section of 45-degree oblique lines on the diagram (c);
FIG. 3 is an atomic force electron microscope (500 times magnified) image of a local surface of a GaN wafer to which the polishing solution prepared in example 1 of the present invention is applied;
FIG. 4 is an atomic force electron microscope (2000 times magnification) image of a part of the surface of a silicon carbide wafer to which the polishing liquids prepared in example 1 and comparative example 2 of the present invention were applied, wherein (a) is example 1, and (b) is comparative example 2.
Detailed Description
The technical solution in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention.
The invention provides a preparation method of composite alumina polishing solution, which comprises the following steps:
(1) a mixture of 990 g of aluminum hydroxide (from Shandong of middle aluminum Co., Ltd.) and 10 g of lanthanum oxide (from Baotou New Source rare earth high New Material Co., Ltd.) was used;
(2) calcining the mixture obtained in the step (1) at the temperature of 1000-;
(3) adding 600 g of deionized water into 400 g of the calcined material obtained in the step (2), and performing ball milling until D50 is 300-500nm to obtain a ball grinding material, wherein the microstructure of the ball grinding material is shown in figure 1, and the arc line in figure 1 is the surface of the prepared alumina grinding material particle;
(4) adding 20 g of gamma-aminopropyltriethoxysilane (gamma-APS, which is available from Dow chemical) into 500 g (with the solid content of 40%) of the ball milling material obtained in the step (3), uniformly mixing, and aging at 150 ℃ for 20 minutes; the microstructure of the ball grinding material is shown in figure 1, and the arc line in figure 1 is the surface of the prepared alumina ball grinding material particle; filtering the aged slurry through a filter bag with the specification of 2 mu m;
(5) dispersing a dispersing agent (ammonium polyacrylate, trade name Darvin821A, available from Van-Deberg mineral Co., Ltd., and sodium lauryl sulfate, available from Shanghai Haohnhong biomedical science and technology Co., Ltd.), wherein the addition amounts of the ammonium polyacrylate and the sodium lauryl sulfate respectively account for 0.15% of the calcined material (200 g), namely 0.3 g, and 0.75% of the calcined material, namely 1.5 g, in mass percent, dispersing in 30 g of deionized water, and then adding the material obtained in the step (4) for mixing;
(6) adding a lubricant (glycerol, Shandong Xingqi chemical engineering science and technology Co., Ltd.), wherein the addition amount of the glycerol accounts for 10 percent of the burnt material (200 g), namely 20 g;
(7) adding a surfactant (Pluronic L43, purchased from Basff), wherein the addition amount of Pluronic L43 accounts for 1 percent of the burnt material (200 g), namely 2 g;
(8) adding an ion stabilizer (ammonium sulfate, purchased from national pharmaceutical group reagent company), wherein the addition amount of the ammonium sulfate accounts for 0.5 percent of the burnt material (200 g), namely 1 g;
(9) adding polyoxyethylene thickening agent (carboxyvinyl resin, trade name CARBOPOL, available from Noveon Inc. Cleveland, USA), wherein the adding amount of the CARBOPOL accounts for 1.25% of the burnt material (200 g), namely 2.5 g;
(10) a pH adjuster (potassium hydroxide, available from pharmaceutical company, national group agents) was added to adjust the pH to between 7 and 8.
(11) The remaining portion of 422.7 g of deionized water was added to give a post-preparation solids content of 20%.
(12) And filtering the prepared slurry through a filter bag with the specification of 2 mu m to prepare the composite aluminum oxide polishing solution.
Example 2
The only difference from example 1 is that in step (4) gamma-ureidopropyltrimethoxysilane (trade name gamma-UPS, available from Dow chemical) was added in place of gamma-aminopropyltriethoxysilane (gamma-APS) in an amount of 10% of the post-combustion charge.
Example 3
The only difference from example 1 is that the thickener is added to 0.5% methylcellulose (available from Shanghai Merlan Biotech Co., Ltd.) in place of CARBOPOL in the calcined batch.
Comparative example 1
The only difference from example 1 is that step (4) does not add any silicon-based functional silane.
Comparative example 2
The same as example 1 except that the ball-milled material prepared in steps (1) (2) (3) was replaced with silica sol (500nm, available from NOAH Chemicals, texas, usa), and then steps (4) to (12) were continued.
Examples of the applications
The polishing solutions prepared in examples 1 to 3 and comparative examples 1 to 2 were used for polishing silicon carbide and gallium nitride wafers (20 cm in diameter). The specific process comprises the following steps: polishing tests (process technical parameters: rotation speed: 200rpm, polishing time: 1 hour) were carried out on a Speedfam 800 single-side flat polisher, and the properties shown in table 1 below were measured.
TABLE 1 cut Rate for different examples and comparative examples
| Cutting Rate nm/h (silicon carbide) | Cutting Rate nm/h (gallium nitride) | |
| Example 1 | 1778 | 452 |
| Example 2 | 1633 | 771 |
| Example 3 | 1698 | 493 |
| Comparative example 1 | 980 | 215 |
| Comparative example 2 | 125 | 56 |
As can be seen from Table 1, examples 1-3 all achieved high stock removal rates on both SiC and GaN wafers after the aluminum oxide was silane treated (composite alumina); the cutting rate of the alumina without silane treatment of comparative example 1 was about 1/3 lower, while the cutting rate of the conventional silica polishing solution of comparative example 2 was only 1/10.
The polishing solution obtained in example 1 of the present invention is applied to local surface polishing of a silicon carbide wafer, and the effect is shown in fig. 2(a), fig. 2(b), fig. 2(c), and fig. 2(d), and it can be seen from the figure that the polishing solution prepared in example 1 of the present invention has smooth silicon carbide surface without any pits and protrusions after polishing the silicon carbide wafer.
The polishing solution obtained in embodiment 1 of the present invention is applied to local surface polishing of a gallium nitride wafer, and the effect is shown in fig. 3. As can be seen from fig. 3, after the polishing solution prepared in example 1 of the present invention polishes a gan wafer, the gan surface is smooth without any pits or protrusions.
The polishing solutions prepared in example 1 and comparative example 2 of the present invention were applied to the local surface polishing of silicon carbide wafers, and the effects are shown in fig. 4(a) and fig. 4(b), where it can be seen that after the polishing with the conventional silica polishing solution of comparative example 2, pits and projections were left on the surface of the silicon carbide wafer, whereas after the polishing with the composite polishing solution of example 1 of the present invention, pits and projections were not left on the surface of the silicon carbide wafer.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. The preparation method of the composite aluminum oxide polishing solution is characterized by comprising the following steps:
(1) mixing aluminum hydroxide and lanthanum oxide according to a certain mass ratio;
(2) calcining the mixture at the temperature of 1000-1200 ℃ for 1-6 hours to obtain a calcined material mixed by aluminum oxide and lanthanum oxide, and controlling the mass loss of 25-40% after calcination;
(3) adding deionized water into the fired material, and mixing, wherein the mass ratio of the fired material to the deionized water is (30-45): (55-70); ball milling until D50 is between 300 and 500nm to obtain ball milling material;
(4) adding multi-silicon-based functional silane with the mass ratio of 5-25% of the burned material into the ball-milled material, uniformly mixing, aging at 150 ℃ for 20-60 minutes, and filtering by adopting a filter bag with the aperture of 2 mu m;
(5) and adding a dispersing agent, a lubricating agent, a surfactant, an ionic stabilizer, a thickening agent, a pH value regulator and deionized water into the obtained material, and mixing to obtain the composite alumina polishing solution with the solid content of 5-25% and the pH value of 7-8.
2. The method for preparing the composite aluminum oxide polishing solution according to claim 1, wherein in the step (1), the mass ratio of the aluminum hydroxide to the lanthanum oxide is (95-99.5): (0.5-5).
3. The method for preparing the composite alumina polishing solution according to claim 1, wherein in the step (4), the multi-silicon-based functional silane is aminosilane or ureido silane.
4. The method for preparing the composite alumina polishing solution according to claim 1, wherein in the step (5), the addition amount of the dispersant accounts for 0.1-1% of the calcined material in terms of mass percentage; the dispersing agent is one or a combination of more of triphosphates, triethylhexyl phosphoric acid, methyl amyl alcohol, polyalcohols, polyethers, polyacrylic acids, fatty acid polyesters, sodium dodecyl sulfate, stearic acid monoglyceride, oxidized polyethylene wax and sodium methylene dinaphthalene sulfonate.
5. The method of claim 1, wherein in step (5), the lubricant is added in an amount of 5-10% by mass based on the fired material, and the lubricant is selected from one or more of glycerol, polypropylene glycol, and polybutylene glycol.
6. The method for preparing a composite alumina polishing solution according to claim 1, wherein in the step (5), the addition amount of the surfactant is 0.5-1.5% of the calcined material by mass percentage, and the surfactant is a nonionic surfactant.
7. The method for preparing the composite alumina polishing solution according to claim 1, wherein in the step (5), the addition amount of the ionic stabilizer accounts for 0.01 to 0.5 percent of the calcined material in terms of mass percentage; the ionic stabilizer is selected from one or more of HPMA, inorganic soluble salts and organic acids.
8. The method for preparing the composite alumina polishing solution according to claim 1, wherein in the step (5), the addition amount of the thickener is 0.5-2% of the calcined material by mass percentage; the thickening agent is one or more of carboxymethyl cellulose, methyl cellulose, sodium starch phosphate, sodium polyacrylate, polyoxyethylene, carbomer and inorganic salt.
9. A composite alumina polishing liquid prepared by the preparation method according to any one of claims 1 to 8.
10. Use of the composite alumina polishing slurry according to claim 9 for polishing silicon carbide and gallium nitride semiconductor materials.
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