CN114015359B - Silicon dioxide polishing solution and preparation method thereof - Google Patents
Silicon dioxide polishing solution and preparation method thereof Download PDFInfo
- Publication number
- CN114015359B CN114015359B CN202111331749.0A CN202111331749A CN114015359B CN 114015359 B CN114015359 B CN 114015359B CN 202111331749 A CN202111331749 A CN 202111331749A CN 114015359 B CN114015359 B CN 114015359B
- Authority
- CN
- China
- Prior art keywords
- colloid
- polishing
- silicon dioxide
- silica
- polishing solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- 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 provides a silicon dioxide polishing solution and a preparation method thereof, which are used for solving the technical problems of too fast temperature rise of polishing temperature and low polishing removal rate of the existing silicon dioxide polishing solution in the process of polishing a sapphire sheet. According to the invention, two kinds of silicon dioxide colloids with different particle sizes are selected for compounding, colloid hardness is lower than that of silicon powder hydrolysis method colloid with the same particle size prepared by an ion exchange method, colloid with a large particle size is polished, and the surface of sapphire is repaired and roughness is reduced by colloid with a small particle size; the small-particle-size colloid is adsorbed on the surface of the sapphire sheet and chemically reacts with the sapphire sheet to soften the surface, the large-particle-size colloid removes the softened surface, the polishing rate of the sapphire sheet is improved, and the contact area between the non-spherical particles and the sapphire sheet is larger, so that the chemical action with the sapphire sheet is easier to occur; the mobility of the colloid with small particle size in the polishing solution is stronger than that of the colloid with large particle size, agglomeration caused by aggregation of reaction products is prevented, the polishing temperature is prevented from rising too fast, and the selected cellulose humectant can inhibit crystallization of the polishing solution.
Description
Technical Field
The invention relates to the technical field of grinding and polishing, in particular to a silicon dioxide polishing solution and a preparation method thereof.
Background
With the continuous development of semiconductor technology, more and more LEDs enter the field of lighting. The rapid growth of the LED lighting industry is yet another important force for the expansion of the sapphire application market.
At present, silicon dioxide polishing solution is mostly adopted for polishing a sapphire substrate, and compared with other polishing solutions such as diamond polishing solution, aluminum oxide polishing solution, cerium oxide polishing solution and the like, the silicon dioxide polishing solution can realize lower scratching rate and higher surface quality due to low hardness of abrasive particles, but has some problems in the use process of the silicon dioxide polishing solution, such as too fast temperature rise of the polishing solution, low removal rate, easy crystallization and the like.
In practical application, the problem that the temperature of the polishing solution is too high is very important and easy to ignore, and the problem that the temperature of the polishing solution is too high can bring many problems, such as high surface temperature of the polishing disk, inconsistent chemical and mechanical actions of the polishing solution, fast water evaporation of the polishing solution, fast crystallization of the polishing solution, easy melting of wax attached to the wafer and the like, so that a series of adverse phenomena of orange peel, pits, scratches, chipping, broken wafers and the like can be caused on the surface of the wafer, and the problems are severely limited to the application of the silicon dioxide polishing solution, and some manufacturers such as Berne optics, orude photoelectricity, crystal photoelectricity and the like have selected to use the aluminum oxide polishing solution to polish the sapphire substrate.
In view of the above, there is an urgent need for a silica polishing solution that can improve the polishing temperature and increase the removal rate in order to maintain the applicability of the silica polishing solution.
Disclosure of Invention
The invention provides a silicon dioxide polishing solution and a preparation method thereof, aiming at the technical problems of over-fast temperature rise and low polishing removal rate of the existing silicon dioxide polishing solution in the process of polishing a sapphire sheet, wherein two silicon dioxide colloids with different particle sizes are selected to be compounded with a humectant, a surfactant, a complexing agent and pure water, in the polishing process of the sapphire sheet, the silicon dioxide colloids with small particle sizes are adsorbed on the surface of the sapphire sheet to chemically react with the sapphire to soften the surface of the sapphire, and the silicon dioxide colloids with large particle sizes remove the softened surface of the sapphire, so that the polishing rate of the sapphire sheet can be greatly improved. The mobility of the small-particle-size silica colloid in the polishing solution is stronger than that of the large-particle-size silica colloid, the small-particle-size silica colloid carries adsorbed polishing debris and other substances to pass through gaps among the large-particle-size silica colloids and leave the surfaces of the sapphire wafers and the polishing pad, chemical reaction and substance transportation are accelerated, agglomeration caused by aggregation of reaction products is prevented, the temperature of a processing area is reduced, over-concentration of the temperature is prevented, and the polishing temperature is prevented from rising too fast.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
a silicon dioxide polishing solution comprises silicon dioxide colloid, wherein the silicon dioxide colloid comprises silicon dioxide colloid I and silicon dioxide colloid II, and the particle size of the silicon dioxide colloid I is larger than that of the silicon dioxide colloid II.
Preferably, the silica colloid is non-spherical in shape and the silica colloid has a circularity of less than 0.7. It is to be noted that the cross-sectional shape of the silica gel includes a triangle, a rhombus, a square-like shape, a regular hexagon, and a rectangle-like shape.
Preferably, the particle size of the silica colloid I is 80nm to 120nm, and the particle size of the silica colloid II is 10nm to 40nm.
Preferably, the water-soluble silicon dioxide gel consists of silicon dioxide colloid, humectant, surfactant, complexing agent and water.
Preferably, the mass fraction of the silicon dioxide colloid is 5-50%, the mass fraction of the humectant is 0.01-2%, the mass fraction of the surfactant is 0.001-0.1%, the mass fraction of the complexing agent is 0.01-0.1%, and the mass fraction of the water is 47.8-94.979%.
Preferably, the mass fraction ratio of the silica colloid I to the silica colloid II is (2:1) to (8:1).
Preferably, silica gel I is prepared by an ion exchange method, and silica gel II is prepared by a silica powder hydrolysis method.
Preferably, the humectant is cellulose ether, the complexing agent is ammonium sulfamate, and the surfactant is alkylphenol ethoxylates.
Preferably, the cellulose ethers include sodium carboxymethylcellulose.
The preparation method of the silicon dioxide polishing solution comprises the following steps:
s1, mixing and uniformly stirring a silicon dioxide colloid I and a silicon dioxide colloid II;
s2, adding water for dilution under the stirring state in the step S1;
s3, under the stirring state of the step S2, sequentially dripping a humectant, a surfactant and a complexing agent;
and S4, adjusting the pH value of the suspension obtained in the step S3 to 10-12 to obtain the silicon dioxide polishing solution.
The invention has the beneficial effects that:
1. the silicon dioxide polishing solution prepared by the invention is prepared by compounding two silicon dioxide colloids with different particle sizes, wherein the colloid with a large particle size is prepared by an ion exchange method, the hardness of the colloid is lower than that of the colloid with the same particle size and prepared by a silica powder hydrolysis method, and the colloid mainly plays a polishing role; the small-particle size colloid is prepared by a silicon powder hydrolysis method, the hardness of the small-particle size colloid is higher than that of the colloid prepared by the same-particle size ion exchange method, and the small-particle size colloid plays roles in repairing the surface of the sapphire and reducing the roughness; according to the invention, through compounding of large and small silica colloids, the capabilities of repairing the sapphire surface and reducing the roughness are improved on the basis of ensuring polishing, and the polishing rate of the sapphire wafer can be greatly improved.
2. The silicon dioxide polishing solution prepared by the invention selects the colloid with large particle size and the colloid with small particle size to be compounded according to a certain proportion, and the silicon dioxide colloid with small particle size is absorbed on the surface of the sapphire sheet and sapphire (Al) in the polishing process of the sapphire sheet 2 O 3 ) And chemical reaction is carried out to generate aluminosilicate so as to soften the surface of the sapphire, and the softened sapphire surface is removed by the silica colloid with large particle size, so that the polishing rate of the sapphire sheet can be greatly improved.
3. The small-particle-size silica colloid used in the polishing solution has stronger movement capability in the polishing solution than the large-particle-size silica colloid, and the small-particle-size silica colloid carries adsorbed polishing debris and other substances to pass through gaps among the large-particle-size silica colloids and leave the surfaces of the sapphire wafers and the polishing pad, so that the chemical reaction and the substance transportation are accelerated, the aggregation caused by the aggregation of reaction products is prevented, the temperature of a processing area is reduced, the temperature is prevented from being excessively concentrated, and the polishing temperature is prevented from being heated too fast. Therefore, the compounding of the colloid with large particle size and small particle size can improve the removal rate and effectively control the polishing temperature, so that the temperature of the silicon dioxide polishing solution is maintained in a certain range (35-40 ℃) in the polishing process and is not too high.
4. The silicon dioxide polishing solution prepared by the invention selects the non-spherical silicon dioxide colloid, and compared with the spherical silicon dioxide colloid with the same granularity, the polishing efficiency can be further improved. Spherical silica colloidal particles are mainly subjected to rolling friction, while non-spherical silica colloidal particles are subjected to sliding friction instead of rolling friction, and the contact area between the non-spherical silica colloidal particles and a sapphire sheet is larger than that between the non-spherical silica colloidal particles and spherical particles, so that the non-spherical silica colloidal particles are adhered to the surface of the sapphire sheet and are easier to chemically react with the sapphire sheet. Therefore, the non-spherical silica colloidal particles contribute to an increase in the removal rate by polishing.
5. According to the silicon dioxide polishing solution prepared by the invention, cellulose is selected as a humectant, so that on one hand, colloid can be dispersed, and a colloid system is more stable; on the other hand, the polishing solution can keep moisture and inhibit the crystallization of the polishing solution.
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, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a graph showing the temperature of silica polishing solutions according to examples 3 to 8 of the present invention and comparative examples 1 to 4 as a function of polishing time.
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 obtained by a person skilled in the art without inventive effort based on the embodiments of the present invention, are within the scope of the present invention.
Example 1
A silicon dioxide polishing solution comprises silicon dioxide colloid, wherein the silicon dioxide colloid comprises silicon dioxide colloid I and silicon dioxide colloid II, and the particle size of the silicon dioxide colloid I is larger than that of the silicon dioxide colloid II.
Further, the silicon dioxide polishing solution consists of silicon dioxide colloid, humectant, surfactant, complexing agent and water.
Specifically, the mass fraction of the silica gel is 5-50%, the mass fraction of the humectant is 0.01-2%, the mass fraction of the surfactant is 0.001-0.1%, the mass fraction of the complexing agent is 0.01-0.1%, and the mass fraction of the water is 47.8-94.979%.
It is noted that, in the present embodiment, the kind of water includes pure water or deionized water.
Further, the shape of the silica colloid is non-spherical and the circularity of the silica colloid is less than 0.7; the cross-sectional shape of the silica gel includes triangle, rhombus, square-like, regular hexagon and rectangle-like.
It is worth mentioning that, in the polishing process, the spherical silica colloid particles are mainly subjected to rolling friction, while the non-spherical silica colloid particles are subjected to sliding friction instead of rolling friction, and on the other hand, the non-spherical silica colloid particles are larger in contact area with the sapphire sheet than the spherical particles, are adhered to the surface of the sapphire sheet, and are more prone to have chemical action with the sapphire sheet. Therefore, the non-spherical silica colloidal particles contribute to an increase in polishing removal rate.
Furthermore, the particle size of the silicon dioxide colloid I is 80 nm-120 nm, and the particle size of the silicon dioxide colloid II is 10 nm-40 nm.
It is worth noting that, during the polishing process of the sapphire sheet, the silica colloid with small particle size is adsorbed on the surface of the sapphire sheet and sapphire (Al) 2 O 3 ) And chemical reaction is carried out to generate aluminosilicate so as to soften the surface of the sapphire, and the softened surface of the sapphire is removed by the silica colloid with large particle size, so that the polishing rate of the sapphire sheet can be greatly improved. The mobility of the silicon dioxide colloid with small particle size in the polishing solution is stronger than that of the silicon dioxide colloid with large particle size, and the silicon dioxide colloid with small particle size carriesSubstances such as adsorbed polishing debris and the like pass through gaps among silica colloids with large particle sizes to leave the surfaces of sapphire wafers and polishing pads, so that chemical reaction and substance transportation are accelerated, agglomeration caused by aggregation of reaction products is prevented, the temperature of a processing area is reduced, excessive concentration of temperature is prevented, and the polishing temperature is prevented from rising too fast. Therefore, the compounding of the large-particle-size silica colloid and the small-particle-size silica colloid can improve the removal rate and effectively control the polishing temperature, so that the temperature of the silica polishing solution is maintained within a certain range (35-40 ℃) in the polishing process and is not too high.
Further, the mass fraction ratio of the silica gel I to the silica gel II was (2:1) to (8:1).
Further, the silica gel I is prepared by an ion exchange method, and the silica gel II is prepared by a silica powder hydrolysis method. It is to be noted that the preparation of the silica colloid by the ion exchange method is a process in which small particles formed by polymerization after ion substitution are aggregated on crystal nuclei to form large particles. The silica colloid prepared by the silica powder hydrolysis method is a single colloidal molecule generated by silica powder hydrolysis, the colloidal molecules are freely combined into colloidal particles, new colloidal molecules are gathered on the colloidal particles, the colloidal particles gradually grow to the required size, and the obtained silica colloid is more compact and has higher hardness. Therefore, the hardness of the silica colloid prepared by the ion exchange method is lower than that of the silica colloid prepared by the silica powder hydrolysis method with the same granularity, so that the silica colloid I has low hardness and mainly plays a polishing role in the polishing process, and the silica colloid II has high hardness and plays a role in repairing the surface of the sapphire and reducing the roughness in the polishing process, and therefore, the polishing rate of the sapphire sheet can be greatly improved by compounding the large silica colloid and the small silica colloid.
Further, the humectant is cellulose ether, the complexing agent is ammonium sulfamate, and the surfactant is alkylphenol ethoxylates. More specifically, the cellulose ethers include sodium carboxymethylcellulose. Cellulose ethers are selected as the humectant, so that on one hand, colloid can be dispersed, and the colloid system of the polishing solution is more stable; on the other hand, the polishing solution can keep moisture, inhibit the crystallization of the polishing solution and ensure the polishing effect.
Example 2
A preparation method of silicon dioxide polishing solution comprises the following steps:
and S1, mixing and uniformly stirring the silicon dioxide colloid I and the silicon dioxide colloid II. Specifically, two types of silica colloids with the total mass fraction of 5-50% are mixed and stirred, wherein the particle size of the silica colloid I is 80-120 nm, the particle size of the silica colloid II is 10-40 nm, and the mass fraction ratio of the silica colloid I to the silica colloid II is (2:1) - (8:1).
It is worth noting that, during the polishing process of the sapphire sheet, the silica colloid with small particle size is adsorbed on the surface of the sapphire sheet and sapphire (Al) 2 O 3 ) And chemical reaction is carried out to generate aluminosilicate so as to soften the surface of the sapphire, and the softened sapphire surface is removed by the silica colloid with large particle size, so that the polishing rate of the sapphire sheet can be greatly improved. The mobility of the small-particle-size silicon dioxide colloid in the polishing solution is higher than that of the large-particle-size silicon dioxide colloid, the small-particle-size silicon dioxide colloid carries adsorbed polishing debris and other substances to penetrate through gaps among the large-particle-size silicon dioxide colloids and leave the surfaces of the sapphire wafers and the polishing pad, chemical reaction and substance transportation are accelerated, aggregation caused by aggregation of reaction products is prevented, the temperature of a processing area is reduced, over-concentration of the temperature is prevented, and the polishing temperature is prevented from rising too fast. Therefore, the compounding of the large-particle-size silica colloid and the small-particle-size silica colloid can improve the removal rate and effectively control the polishing temperature, so that the temperature of the silica polishing solution is maintained within a certain range (35-40 ℃) in the polishing process and is not too high.
It is worth noting that the shape of the silica colloid is non-spherical and the circularity of the silica colloid is less than 0.7; the cross-sectional shape of the silica gel includes triangle, rhombus, square-like, regular hexagon and rectangle-like.
It is worth to say that silica gel I is prepared by an ion exchange method, and silica gel II is prepared by a silica powder hydrolysis method. It is to be noted that the preparation of the silica colloid by the ion exchange method is a process in which small particles formed by polymerization after ion substitution are aggregated on crystal nuclei to form large particles. The silica colloid prepared by the silica powder hydrolysis method is a single colloidal molecule generated by silica powder hydrolysis, the colloidal molecules are freely combined into colloidal particles, new colloidal molecules are gathered on the colloidal particles, the colloidal particles gradually grow to the required size, and the obtained silica colloid is more compact and has higher hardness. Therefore, the hardness of the silica colloid prepared by the ion exchange method is lower than that of the silica colloid prepared by the silica powder hydrolysis method with the same granularity, so that the silica colloid I has low hardness and mainly plays a polishing role in the polishing process, and the silica colloid II has high hardness and plays a role in repairing the surface of the sapphire and reducing the roughness in the polishing process, and therefore, the polishing rate of the sapphire sheet can be greatly improved by compounding the large silica colloid and the small silica colloid.
And S2, adding water for dilution under the stirring state in the step S1. Specifically, water with the mass fraction of 47.8% -94.979% is added to the mixed liquid obtained in the step S1 under the stirring state.
It is noted that, in the present embodiment, the kind of water includes pure water or deionized water.
And S3, under the stirring state in the step S2, sequentially dropwise adding the humectant, the surfactant and the complexing agent. Specifically, under a stirring state, 0.01-2% by mass of a humectant, 0.001-0.1% by mass of a surfactant and 0.01-0.1% by mass of a complexing agent are sequentially added dropwise to the mixed solution obtained in the step S2. In this embodiment, the humectant is cellulose ether, the complexing agent is ammonium sulfamate, the surfactant is alkylphenol ethoxylates, the cellulose ether comprises sodium carboxymethylcellulose, and the cellulose ether is used as the humectant, so that on one hand, the colloid can be dispersed, and the colloid system of the polishing solution is more stable; on the other hand, the polishing solution can keep moisture, inhibit the crystallization of the polishing solution and ensure the polishing effect.
And S4, adjusting the pH value of the suspension obtained in the step S3 to 10-12 to obtain the silicon dioxide polishing solution. It is to be noted that the pH adjusting agent used comprises 20% triethanolamine, 20% AMP-95, 20% KOH solution and 25% tetramethylammonium hydroxide solution
Example 3
A silicon dioxide polishing solution comprises the following raw materials:
silica gel having a 120nm cross-sectional shape similar to a rectangle: 40 percent; silica colloid having a cross-sectional shape of 20nm of a quasi-rectangular shape: 10 percent; sodium carboxymethylcellulose: 0.02 percent; surfactant OP-10:0.01 percent; complexing agent ammonium sulfamate: 0.05 percent; water: 49.92%.
According to the raw material of the silica polishing solution in this embodiment, this embodiment provides a method for preparing silica, comprising: slowly adding 20nm silicon dioxide colloid (with the cross section shaped like a rectangle) into 120nm silicon dioxide colloid (with the cross section shaped like a rectangle), uniformly stirring, diluting, then dropwise adding sodium carboxymethylcellulose, a surfactant OP-10 and a complexing agent ammonium sulfamate solution, and adjusting the pH value of the polishing solution to 10.0 by using 20% triethanolamine to obtain the silicon dioxide polishing solution.
In this example, the prepared silica polishing solution was prepared according to the following ratio of 1:1 proportion dilution, polishing 2 inches of C-direction sapphire wafer on a single-side polishing machine, matching with SUBA800 polishing pad, the unit area pressure is 300g/cm < 2 >, and the average removal rate of the wafer can reach 8.5um/h.
Example 4
A silicon dioxide polishing solution comprises the following raw materials:
silica gel with 120nm cross section in the shape of regular hexagon: 40 percent; silica gel having a cross-sectional shape of 40nm of regular hexagon: 5 percent; sodium carboxymethylcellulose: 0.02 percent; surfactant OP-10:0.01 percent; complexing agent ammonium sulfamate: 0.05 percent; water: 54.92%.
According to the raw material of the silica polishing solution in this embodiment, this embodiment provides a method for preparing silica, comprising: slowly adding 40nm silicon dioxide colloid (with the cross section being in the shape of a regular hexagon) into 120nm silicon dioxide colloid (with the cross section being in the shape of a regular hexagon), uniformly stirring, diluting, then dropwise adding sodium carboxymethylcellulose, a surfactant OP-10 and an ammonium sulfamate solution serving as a complexing agent, and adjusting the pH value of the polishing solution to 10.2 by using 20% AMP-95 to obtain the silicon dioxide polishing solution.
In this example, the prepared silica polishing solution was prepared according to the following ratio of 1:1 proportion dilution, polishing 2 inches of C-direction sapphire wafers on a single-side polishing machine, matching with an SUBA800 polishing pad, wherein the unit area pressure is 300g/cm < 2 >, and the average removal rate of the wafers can reach 8.2um/h.
Example 5
A silicon dioxide polishing solution is composed of the following raw materials:
silica gel having a 110nm cross-sectional shape of rhombohedral: 35 percent; silica gel having a 20nm cross-sectional shape of rhombohedral: 7 percent; sodium carboxymethylcellulose: 0.02 percent; surfactant OP-10:0.01 percent; complexing agent ammonium sulfamate: 0.05 percent; water: 57.92%.
According to the raw materials of the silica polishing solution in this embodiment, this embodiment provides a method for preparing silica, comprising: slowly adding 20nm silicon dioxide colloid (with the cross section of a rhombus) into 110nm silicon dioxide colloid (with the cross section of a rhombus), uniformly stirring, diluting, then dropwise adding sodium carboxymethylcellulose, a surfactant OP-10 and an ammonium sulfamate solution serving as a complexing agent, and adjusting the pH value of the polishing solution to 10.5 by using a KOH solution 20 percent to obtain the silicon dioxide polishing solution.
In this example, the prepared silica polishing solution was prepared according to the following ratio of 1:1 proportion dilution, polishing 2 inches of C-direction sapphire wafer on a single-side polishing machine, matching with SUBA800 polishing pad, the unit area pressure is 300g/cm < 2 >, and the average removal rate of the wafer can reach 8.4um/h.
Example 6
A silicon dioxide polishing solution is composed of the following raw materials:
silica colloid having a 100nm cross-sectional shape resembling a square: 27 percent; silica colloid having a cross-sectional shape of 30nm like a square: 9 percent; sodium carboxymethylcellulose: 0.02 percent; surfactant OP-10:0.01 percent; complexing agent ammonium sulfamate: 0.05 percent; water: 63.87 percent.
According to the raw material of the silica polishing solution in this embodiment, this embodiment provides a method for preparing silica, comprising: slowly adding 30nm silicon dioxide colloid (the cross section of which is shaped like a square) into 100nm silicon dioxide colloid (the cross section of which is shaped like a square), uniformly stirring, diluting, then dropwise adding sodium carboxymethylcellulose, a surfactant OP-10 and an ammonium sulfamate solution serving as a complexing agent, and adjusting the pH value of the polishing solution to be 11 by using a 25% tetramethylammonium hydroxide solution to obtain the silicon dioxide polishing solution.
In this example, the prepared silica polishing solution was prepared according to the following ratio of 1:1 proportion dilution, polishing 2 inches of C-direction sapphire wafer on a single-side polishing machine, matching with SUBA800 polishing pad, the unit area pressure is 300g/cm < 2 >, and the average removal rate of the wafer can reach 7.5um/h.
Example 7
A silicon dioxide polishing solution is composed of the following raw materials:
silica gel having a cross-sectional shape of 80nm of a triangle: 20 percent; silica gel having a 10nm cross-sectional shape of triangle: 5 percent; sodium carboxymethylcellulose: 0.015 percent; surfactant OP-10:0.005 percent; complexing agent ammonium sulfamate: 0.08 percent; water: 74.9 percent.
According to the raw material of the silica polishing solution in this embodiment, this embodiment provides a method for preparing silica, comprising: slowly adding 10nm silicon dioxide colloid (with the cross section shaped as a triangle) into 80nm silicon dioxide colloid (with the cross section shaped as a triangle), uniformly stirring, diluting, then dropwise adding sodium carboxymethylcellulose, a surfactant OP-10 and a complexing agent ammonium sulfamate solution, and adjusting the pH value of the polishing solution to 11 by using a 25% tetramethylammonium hydroxide solution to obtain the silicon dioxide polishing solution.
In this example, the prepared silica polishing solution was prepared according to the following ratio of 1:1 proportion dilution, polishing 2 inches of C-direction sapphire wafer on a single-side polishing machine, matching with SUBA800 polishing pad, the unit area pressure is 300g/cm < 2 >, and the average removal rate of the wafer can reach 7.0um/h.
Example 8
A silicon dioxide polishing solution is composed of the following raw materials:
silica gel having a 100nm cross-sectional shape of rhombohedral: 10 percent; silica gel having a 10nm cross-sectional shape of rhombohedral: 2 percent; sodium carboxymethylcellulose: 0.015 percent; surfactant OP-10:0.005 percent; complexing agent ammonium sulfamate: 0.08%; water: 87.9 percent.
According to the raw material of the silica polishing solution in this embodiment, this embodiment provides a method for preparing silica, comprising: slowly adding 10nm silicon dioxide colloid (with the cross section of a rhombus shape) into 100nm silicon dioxide colloid (with the cross section of a rhombus shape), uniformly stirring, diluting, then dropwise adding sodium carboxymethylcellulose, a surfactant OP-10 and a complexing agent ammonium sulfamate solution, and adjusting the pH value of the polishing solution to 10.0 by using 20% triethanolamine to obtain the silicon dioxide polishing solution.
In this example, the prepared silica polishing solution was prepared according to the following ratio of 1:1 proportion dilution, polishing 2 inches of C-direction sapphire wafer on a single-side polishing machine, matching with SUBA800 polishing pad, the unit area pressure is 300g/cm < 2 >, and the average removal rate of the wafer can reach 7.2um/h.
It is noted that, in the above examples 3 to 6, the present invention also provides a comparison of the results of four comparative examples in which the silica colloid used is spherical.
Comparative example 1
A silicon dioxide polishing solution is composed of the following raw materials:
120nm spherical silica colloid: 40 percent; 20nm spherical silica colloid: 10 percent; sodium carboxymethylcellulose: 0.02 percent; surfactant OP-10:0.01 percent; complexing agent ammonium sulfamate: 0.05 percent; water: 49.92%.
According to the raw materials of the above silica polishing liquid in this comparative example, this comparative example provides a method for producing silica, comprising: slowly adding 20nm silicon dioxide colloid (spherical) into 120nm silicon dioxide colloid (spherical), uniformly stirring, diluting, then dropwise adding sodium carboxymethylcellulose, a surfactant OP-10 and a complexing agent ammonium sulfamate solution, and adjusting the pH value of the polishing solution to 10.0 by using 20% triethanolamine to obtain the silicon dioxide polishing solution.
In this comparative example, the silica polishing solution was prepared in accordance with a 1:1 proportion dilution, polishing 2 inches of C-direction sapphire wafer on a single-side polishing machine, matching with SUBA800 polishing pad, the unit area pressure is 300g/cm < 2 >, and the average removal rate of the wafer can reach 6.8um/h.
Comparative example 2
A silicon dioxide polishing solution is composed of the following raw materials:
120nm spherical silica colloid: 40 percent; 40nm spherical silica colloid: 5 percent; sodium carboxymethylcellulose: 0.02 percent; surfactant OP-10:0.01 percent; complexing agent ammonium sulfamate: 0.05 percent; water: 54.92%.
According to the raw materials of the above silica polishing liquid in this comparative example, this comparative example provides a method for producing silica, comprising: slowly adding 40nm silicon dioxide colloid (spherical) into 120nm silicon dioxide colloid (spherical), stirring uniformly, diluting, then dropwise adding sodium carboxymethylcellulose, a surfactant OP-10 and a complexing agent ammonium sulfamate solution, and adjusting the pH value of the polishing solution to 10.2 by using 20% AMP-95 to obtain the silicon dioxide polishing solution.
In this comparative example, a silica polishing solution was prepared in accordance with a 1:1 proportion dilution, polishing 2 inches of C-direction sapphire wafer on a single-side polishing machine, matching with SUBA800 polishing pad, the unit area pressure is 300g/cm < 2 >, and the average removal rate of the wafer can reach 6.4um/h.
Comparative example 3
A silicon dioxide polishing solution is composed of the following raw materials:
110nm spherical silica colloid: 35 percent; 20nm spherical silica colloid: 7 percent; sodium carboxymethylcellulose: 0.02 percent; surfactant OP-10:0.01 percent; complexing agent ammonium sulfamate: 0.05 percent; water: 57.92%.
According to the raw materials of the above silica polishing liquid in this comparative example, this comparative example provides a method for producing silica, comprising: slowly adding 20nm silicon dioxide colloid (spherical) into 110nm silicon dioxide colloid (spherical), stirring uniformly, diluting, then dropwise adding sodium carboxymethylcellulose, a surfactant OP-10 and a complexing agent ammonium sulfamate solution, and adjusting the pH value of the polishing solution to 10.5 by using a 20% KOH solution to obtain the silicon dioxide polishing solution.
In this comparative example, the silica polishing solution was prepared in accordance with a 1:1 proportion dilution, polishing 2 inches of C-direction sapphire wafer on a single-side polishing machine, matching with SUBA800 polishing pad, the unit area pressure is 300g/cm < 2 >, and the average removal rate of the wafer can reach 6.0um/h.
Comparative example 4
A silicon dioxide polishing solution is composed of the following raw materials:
100nm spherical silica colloid: 27 percent; 30nm spherical silica colloid: 9 percent; sodium carboxymethylcellulose: 0.02 percent; surfactant OP-10:0.01 percent; complexing agent ammonium sulfamate: 0.05 percent; water: 63.87 percent.
According to the raw material of the above silica polishing liquid in this comparative example, there is provided a method for producing silica, comprising: slowly adding 30nm silicon dioxide colloid (spherical) into 100nm silicon dioxide colloid (spherical), uniformly stirring, diluting, then dropwise adding sodium carboxymethylcellulose, a surfactant OP-10 and a complexing agent ammonium sulfamate solution, and adjusting the pH value of the polishing solution to 11 by using a 25% tetramethylammonium hydroxide solution to obtain the silicon dioxide polishing solution.
In this comparative example, the silica polishing solution was prepared in accordance with a 1:1 proportion dilution, polishing 2 inches of C-direction sapphire wafer on a single-side polishing machine, matching with SUBA800 polishing pad, the unit area pressure is 300g/cm < 2 >, and the average removal rate of the wafer can reach 6.6um/h.
It is to be noted that, in the present invention, the equipment and process conditions for polishing a sapphire sheet using a silica polishing slurry are as shown in table 1 below.
TABLE 1 Equipment and Process conditions for polishing sapphire wafers with silicon dioxide polishing solution
| Device name | AM-ASL400 single-side polishing machine |
| Matching cushion | SUBA800 polishing pad |
| Paster mode | Wax patch |
| Number of C-direction sapphire sheets processed | 3 sheets/disc (2 in) 33 discs |
| By liquid means | Dropping and circulating |
| State of polishing solution | Natural heating, no water bath heating |
| Polishing time | 2h |
| Liquid consumption amount | 1.5L |
| Dilution ratio | 1:1 |
| Pressure of | 17.67kg |
| Flow rate | 120g/min |
| Main disc rotational speed | 100rpm |
The test results of the silicon dioxide polishing liquids of the above examples and comparative examples of the present invention for polishing sapphire sheets are shown in table 2 below.
Table 2 test results of silicon dioxide polishing solutions of examples and comparative examples polishing sapphire sheets
| Removal Rate (um/h) | Yield (%) | Average temperature (. Degree. C.) of polishing liquid | Cause of failure | |
| Example 3 | 8.5 | 100 | 36.33 | No bad effect |
| Example 4 | 8.2 | 99 | 36.19 | Slight scratch |
| Example 5 | 8.4 | 100 | 36.68 | No bad effect |
| Example 6 | 7.5 | 99 | 36.98 | Slight scratch |
| Example 7 | 7.0 | 99 | 36.74 | Slight scratch |
| Example 8 | 7.2 | 99 | 36.85 | No bad effect |
| Comparative example 1 | 6.8 | 100 | 38.90 | No bad effect |
| Comparative example 2 | 6.4 | 100 | 44.04 | No bad effect |
| Comparative example 3 | 6.0 | 96 | 45.09 | Scratch and orange peel |
| Comparative example 4 | 6.6 | 100 | 40.78 | No bad effect |
As can be seen from table 2, the average removal rate of the sapphire wafers in examples 3 to 8 is greater than that in comparative examples 1 to 4, and from table 2 and fig. 1, the average temperature of the polishing solution and the surface quality of the polished sapphire wafers in examples 3 to 8 are higher than those in comparative examples 1 to 4, because the non-spherical silica colloid is selected in the examples, the polishing efficiency can be further improved compared with that of the spherical silica having the same particle size, the spherical particles are mainly rolling friction during polishing, and the non-spherical particles are mainly rolling friction during polishing: on one hand, sliding friction is used for replacing rolling friction, on the other hand, the contact area of the non-spherical particles and the wafer is larger than that of the spherical particles, the non-spherical particles are adhered to the surface of the wafer, and chemical action is easier to occur between the non-spherical particles and the wafer. Thus, the non-spherical silica particles contribute to an increase in removal rate.
It is noted that, as shown in table 2, example 5 is the most preferred embodiment of the present invention in terms of the average removal rate of the sapphire wafer and the average temperature of the polishing liquid.
The present invention is not limited to the above preferred embodiments, and any modifications, equivalent substitutions, improvements, etc. within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (4)
1. The silicon dioxide polishing solution for sapphire sheet polishing is characterized by comprising silicon dioxide colloid, a humectant, a surfactant, a complexing agent and water;
the silica colloid comprises a silica colloid I and a silica colloid II, and the particle size of the silica colloid I is larger than that of the silica colloid II; the shape of the silica colloid is non-spherical and the circularity of the silica colloid is less than 0.7; the cross section of the silica gel is any one of a triangle, a diamond, a square-like, a regular hexagon and a rectangle-like, the silica gel I is prepared by an ion exchange method, and the silica gel II is prepared by a silica powder hydrolysis method; the particle size of the silicon dioxide colloid I is 80 nm-120 nm, and the particle size of the silicon dioxide colloid II is 10 nm-40 nm;
the mass fraction of the silicon dioxide colloid is 5-50%, the mass fraction of the humectant is 0.01-2%, the mass fraction of the surfactant is 0.001-0.1%, the mass fraction of the complexing agent is 0.01-0.1%, and the mass fraction of the water is 47.8-94.979%;
the mass fraction ratio of the silica gel I to the silica gel II is (2:1) - (8:1);
the humectant is cellulose ether.
2. The silica polishing solution for sapphire sheet polishing of claim 1, wherein the complexing agent is ammonium sulfamate and the surfactant is alkylphenol ethoxylates.
3. The silica polishing solution for sapphire sheet polishing of claim 2, wherein the cellulose ether is sodium carboxymethylcellulose.
4. The silicon dioxide polishing solution for sapphire wafer polishing as set forth in claim 3, wherein the preparation method comprises the steps of:
s1, mixing and uniformly stirring a silicon dioxide colloid I and a silicon dioxide colloid II;
s2, adding water for dilution under the stirring state in the step S1;
s3, under the stirring state in the step S2, sequentially dripping the humectant, the surfactant and the complexing agent;
and S4, adjusting the pH value of the suspension obtained in the step S3 to 10-12 to obtain the silicon dioxide polishing solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111331749.0A CN114015359B (en) | 2021-11-11 | 2021-11-11 | Silicon dioxide polishing solution and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111331749.0A CN114015359B (en) | 2021-11-11 | 2021-11-11 | Silicon dioxide polishing solution and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114015359A CN114015359A (en) | 2022-02-08 |
| CN114015359B true CN114015359B (en) | 2023-03-10 |
Family
ID=80063376
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111331749.0A Active CN114015359B (en) | 2021-11-11 | 2021-11-11 | Silicon dioxide polishing solution and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114015359B (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2003042322A1 (en) * | 2001-11-09 | 2003-05-22 | Silbond Corporation | Abrasive media and aqueous slurries |
| CN104893587A (en) * | 2015-03-09 | 2015-09-09 | 江苏中晶科技有限公司 | Efficient C-oriented sapphire polishing solution and preparation method thereof |
| CN105462504A (en) * | 2015-12-11 | 2016-04-06 | 蓝思科技（长沙）有限公司 | C-direction sapphire polishing solution and preparation method thereof |
| CN107987732A (en) * | 2017-12-19 | 2018-05-04 | 北京航天赛德科技发展有限公司 | A kind of polishing fluid for sapphire plane polishing and preparation method thereof |
| CN108949034A (en) * | 2018-08-17 | 2018-12-07 | 无锡易洁工业介质有限公司 | A kind of sapphire chemical mechanical polishing liquid and preparation method thereof |
| CN111748318A (en) * | 2020-07-28 | 2020-10-09 | 上海大学 | Popcorn-like silica sol, preparation method and application thereof |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008270584A (en) * | 2007-04-23 | 2008-11-06 | Nippon Chem Ind Co Ltd | Polishing composition for semiconductor wafer and polishing processing method |
| JP5602358B2 (en) * | 2007-11-30 | 2014-10-08 | 日揮触媒化成株式会社 | Non-spherical silica sol, method for producing the same, and polishing composition |
| CN103897605A (en) * | 2012-12-27 | 2014-07-02 | 天津西美半导体材料有限公司 | Sapphire substrate polishing solution for single-sided polishing machine |
| JP6495095B2 (en) * | 2014-05-20 | 2019-04-03 | 花王株式会社 | Polishing liquid composition for magnetic disk substrate |
| JP2017119738A (en) * | 2015-12-28 | 2017-07-06 | 花王株式会社 | Polishing liquid composition for sapphire plate nonpolar surface |
| CN112390262A (en) * | 2020-12-22 | 2021-02-23 | 郑州中科新兴产业技术研究院 | Double-particle-size non-spherical silicon dioxide, preparation method and polishing slurry prepared from double-particle-size non-spherical silicon dioxide |
-
2021
- 2021-11-11 CN CN202111331749.0A patent/CN114015359B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2003042322A1 (en) * | 2001-11-09 | 2003-05-22 | Silbond Corporation | Abrasive media and aqueous slurries |
| CN104893587A (en) * | 2015-03-09 | 2015-09-09 | 江苏中晶科技有限公司 | Efficient C-oriented sapphire polishing solution and preparation method thereof |
| CN105462504A (en) * | 2015-12-11 | 2016-04-06 | 蓝思科技（长沙）有限公司 | C-direction sapphire polishing solution and preparation method thereof |
| CN107987732A (en) * | 2017-12-19 | 2018-05-04 | 北京航天赛德科技发展有限公司 | A kind of polishing fluid for sapphire plane polishing and preparation method thereof |
| CN108949034A (en) * | 2018-08-17 | 2018-12-07 | 无锡易洁工业介质有限公司 | A kind of sapphire chemical mechanical polishing liquid and preparation method thereof |
| CN111748318A (en) * | 2020-07-28 | 2020-10-09 | 上海大学 | Popcorn-like silica sol, preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114015359A (en) | 2022-02-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106044786B (en) | Big partial size silica solution of polydispersion and preparation method thereof | |
| US9919962B2 (en) | Polishing agent for synthetic quartz glass substrate | |
| CN102190962B (en) | Polishing composition and utilize the finishing method of said composition | |
| TW500792B (en) | Edge polishing composition | |
| JP2592401B2 (en) | Composition and method for polishing and planarizing a surface | |
| KR101092884B1 (en) | Method for polishing wafer | |
| WO2009021364A1 (en) | The method of controlling scratching of the polished surface of silicon wafer | |
| CN107189693B (en) | Polishing solution for chemical mechanical polishing of A-direction sapphire and preparation method thereof | |
| CN107987732B (en) | Polishing solution for sapphire plane polishing and preparation method thereof | |
| JP6223786B2 (en) | Polishing liquid composition for hard and brittle materials | |
| JP2008290183A (en) | Composition for polishing | |
| JP2006278981A (en) | Abrasive for single crystal surface and polishing method | |
| WO2009021363A1 (en) | Nano silicon dioxide abradant polishing liquid for processing microcrystal glass | |
| JP2012079964A (en) | Polishing liquid composition for semiconductor wafer | |
| CN114231182A (en) | Easy-to-cleave gallium oxide wafer chemical mechanical polishing process, polishing solution and preparation method thereof | |
| JPH11140427A (en) | Polishing liquid and polishing | |
| CN108949034B (en) | Sapphire chemical mechanical polishing solution and preparation method thereof | |
| CN114015359B (en) | Silicon dioxide polishing solution and preparation method thereof | |
| JP2004155913A (en) | Abrasive grain for polishing, manufacturing method therefor, and abrasive | |
| TWI421334B (en) | Slurry composition and use thereof | |
| CN111316399B (en) | Method for manufacturing semiconductor wafer | |
| KR102508181B1 (en) | Polishing composition and polishing method | |
| CN109666410A (en) | Sapphire polishing liquid additive and its preparation method and application | |
| CN1861724A (en) | Nano SiO2 grinding material polishing fluid for electronic glass | |
| CN113755099B (en) | Sapphire chemical mechanical polishing solution and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |