CN111253910A - Preparation method of inorganic polyelectrolyte-silicon oxide composite polishing abrasive particles - Google Patents
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- CN111253910A CN111253910A CN202010192315.6A CN202010192315A CN111253910A CN 111253910 A CN111253910 A CN 111253910A CN 202010192315 A CN202010192315 A CN 202010192315A CN 111253910 A CN111253910 A CN 111253910A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1436—Composite particles, e.g. coated particles
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
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Abstract
The invention discloses a preparation method of inorganic polyelectrolyte-silicon oxide composite polishing abrasive particles, which comprises the following steps: s01: preparing nano silica sol; s02: preparing inorganic polyelectrolyte poly-magnesium-ferrum-aluminum-zinc silicate; s03: dropwise adding the zinc iron aluminum magnesium polysilicate into the nano silica sol at 25 ℃ under the stirring condition, and continuously stirring for 6 hours; and centrifuging and filtering to obtain the inorganic polyelectrolyte-silicon oxide composite polishing abrasive particle solution. The preparation method of the inorganic polyelectrolyte-silicon oxide composite polishing abrasive particles provided by the invention can improve the material removal rate of a sapphire substrate and reduce the surface roughness.
Description
Technical Field
The invention relates to the field of chemical mechanical polishing, in particular to a preparation method of inorganic polyelectrolyte-silicon oxide composite polishing abrasive particles.
Background
Single crystal sapphire has been widely used in the fields of machinery, optics, information, and the like because of its high mechanical strength, good light transmission, and stable chemical properties. Currently, sapphire is the most widely used substrate material for photonic devices, particularly Light Emitting Diodes (LEDs), and with the rapid development of technology, the demand for ultra-smooth and high polishing rates on sapphire surfaces is increasing. However, it is difficult to satisfy the above requirements at the same time due to the high hardness and strong chemical inertness of sapphire. Currently, Chemical Mechanical Polishing (CMP) is considered to be the only globally planarization-capable technique combining chemical and mechanical action, and has wide application in the fields of semiconductors, hard disks, and optics.
CMP depends on many factors, such as abrasive particles, polishing time, polishing rate, additives, etc., wherein abrasive particles are one of the most important factors affecting surface planarization. In order to improve surface quality and increase polishing rate (MRR), researchers have recently studied various types of abrasive particles, such as silica, alumina, ceria, etc., but a single abrasive particle cannot achieve satisfactory polishing results. Among them, silica is most widely used due to its stable chemical properties and excellent dispersibility, but the material removal rate is low and cannot meet industrial requirements in general.
Disclosure of Invention
The invention aims to provide a preparation method of inorganic polyelectrolyte-silicon oxide composite polishing abrasive particles, which can improve the material removal rate of a sapphire substrate and reduce the surface roughness.
In order to achieve the purpose, the invention adopts the following technical scheme: a preparation method of inorganic polyelectrolyte-silicon oxide composite polishing abrasive particles comprises the following steps:
s01: preparing nano silica sol: stirring and heating the silicon dioxide seed crystal solution to 100 ℃, and adjusting the pH to 10; dropwise adding an active silicic acid solution into the silicon dioxide seed crystal solution under the stirring condition, simultaneously adjusting the pH to 10, and keeping the evaporation rate of the solution equal to the dropwise adding rate of silicic acid; cooling to room temperature to obtain nano silica sol;
s02: preparing inorganic polyelectrolyte poly-magnesium-ferrum-aluminum-zinc silicate: dropwise adding sulfuric acid into a sodium silicate solution under the condition of stirring, and adjusting the pH to 4; polymerizing the sulfuric acid and the sodium silicate solution at 25 ℃ for 1 hour, respectively adding magnesium sulfate, ferric chloride (III) hexahydrate, aluminum nitrate nonahydrate and zinc sulfate under the stirring condition, and aging for 24 hours to obtain inorganic polyelectrolyte poly-magnesium-iron-aluminum-zinc silicate;
s03: dropwise adding the zinc iron aluminum magnesium polysilicate into the nano silica sol at 25 ℃ under the stirring condition, and continuously stirring for 6 hours; centrifuging and filtering to obtain inorganic polyelectrolyte-silicon oxide composite polishing abrasive particle solution; wherein the mass ratio of the inorganic polyelectrolyte to the silicon oxide is 0.5-5.0: 100.
further, in step S01, a sodium hydroxide solution with a mass fraction of 1% is used to adjust the pH to 10.
Further, the mass fraction of the nano silica sol silica in the step S01 is 10%.
Further, in the step S01, 0.4mol/L sulfuric acid is added dropwise to the 0.04mol/L sodium silicate solution with stirring.
Further, the method also includes step S04: and adjusting the pH value of the inorganic polyelectrolyte-silicon oxide composite polishing abrasive particle solution to 10, and adding a surfactant to obtain the inorganic polyelectrolyte-silicon oxide composite polishing solution.
The invention has the beneficial effects that: according to the inorganic polyelectrolyte-silicon oxide composite abrasive particle polishing solution prepared by the invention, due to the introduction of cations in an inorganic polymer, the electrostatic repulsion between silicon oxide particles and a workpiece is reduced, so that more effective abrasive particles are in contact with the surface of the workpiece (such as a sapphire wafer) in the polishing process, a soft layer formed through chemical reaction can be quickly removed, the synergistic effect of chemical corrosion and mechanical abrasion is optimal, and the material removal rate is higher; and polishing damage such as scratches and surface damage is small because the silica particles themselves are small in hardness. Therefore, when the novel abrasive particles prepared by the method are used for polishing the sapphire substrate, the material removal rate of the sapphire substrate can be improved, and the surface roughness can be reduced. In addition, the prepared inorganic polyelectrolyte has no toxicity, and the green and environment-friendly concept of the polishing solution is realized.
Drawings
FIG. 1 is a flow chart of a method for preparing inorganic polyelectrolyte-silicon oxide composite polishing abrasive particles according to the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention are described in detail below with reference to the accompanying drawings.
The invention relates to an inorganic polyelectrolyte-silicon oxide composite abrasive particle polishing abrasive particle, which comprises the following preparation steps:
s01: mixing a certain amount of sodium silicate (Na)2SiO3) The solution was passed through a cation exchange resin pretreated with HCl to obtain an active silicic acid solution. The appropriate amount of silica seed solution was then heated to 100 ℃ and stirred, and the pH of the solution was adjusted to 10 with sodium hydroxide. Next, the prepared active silicic acid solution was added dropwise to the above silica seed solution under constant stirring while maintaining the pH of the system at about 10 with a certain amount of NaOH solution. During this process, the evaporation rate of the solution and the dropping rate of the silicic acid were kept equal to maintain a constant liquid level of the system. And after the silicic acid is added dropwise, continuously stirring and cooling to room temperature to obtain the nano silicon dioxide sol.
S02: under the condition of continuous stirring, concentrated sulfuric acid is diluted by a proper amount of water and then is dropwise added into a sodium silicate solution with a certain concentration. Adjusting the pH value of the mixture to 4 by using dilute sulfuric acid or sodium hydroxide, polymerizing for about 1 hour at room temperature, then respectively adding a certain amount of magnesium sulfate, ferric chloride (III) hexahydrate, aluminum nitrate nonahydrate and zinc sulfate while stirring, and aging the mixture for one day to obtain the inorganic polyelectrolyte poly-magnesium-iron-aluminum-zinc silicate.
S03: a certain amount of poly-silicate magnesium iron aluminum zinc is added into the prepared nano-silica sol drop by drop at 25 ℃ under stirring, and the mixture is continuously stirred for 6 hours. And refining the mixed solution by centrifugation, filtration and other modes. By controlling the relative amount of the inorganic electrolyte and the silicon oxide (the mass ratio of the inorganic polyelectrolyte to the silicon oxide (dry weight)) is 0.5-5.0: 100, the inorganic polyelectrolyte-silicon oxide composite polishing abrasive particles with different modification degrees can be obtained.
S04: the polishing solution prepared by the inorganic polyelectrolyte-silicon oxide composite abrasive particles comprises the inorganic polyelectrolyte-silicon oxide composite abrasive particles, a dispersing agent and a surfactant. Wherein the mass percent concentration of the inorganic polyelectrolyte-silicon oxide composite polishing abrasive particles is 10 wt.%; the mass percent concentration of the surfactant sodium dodecyl benzene sulfonate is 0.5 wt.%, and the mass percent concentration of the dispersant sodium hexametaphosphate is 0.03 wt.%; residual water; the sum of the mass percent of the components is 100 percent.
Embodiments of the invention are further illustrated by the following examples.
Example 1
A preparation method of inorganic polyelectrolyte-silicon oxide composite abrasive particles and polishing solution thereof comprises the following steps:
s01: mixing 8 wt.% of sodium silicate (Na)2SiO3) The solution was passed through a cation exchange resin pretreated with HCl to obtain an active silicic acid solution. The 10 wt.% silica seed solution was then heated to 100 ℃ and stirred, the pH of the solution was adjusted to 10 with sodium hydroxide. Next, the prepared active silicic acid solution was added dropwise to the above silica seed solution under constant stirring while maintaining the pH of the system at about 10 using a 1 wt.% NaOH solution. During this process, the evaporation rate of the solution and the dropping rate of the silicic acid were kept equal to maintain a constant liquid level of the system. And after the silicic acid is dropwise added, continuously stirring and cooling to room temperature, and adjusting the mass fraction to 10 wt.% to obtain the nano silicon dioxide sol.
S02: concentrated sulfuric acid is diluted to 0.4mol/L by water and added dropwise into 0.04mol/L sodium silicate solution under the condition of continuous stirring. The pH of the mixture is then adjusted to 4 with dilute sulfuric acid or sodium hydroxide. After polymerization was carried out at room temperature for about 1 hour, 0.08mol of magnesium sulfate, 0.01mol of iron (III) chloride hexahydrate, 0.04mol of aluminum nitrate nonahydrate and 0.01mol of zinc sulfate were added, respectively, and the mixture was aged for one day to obtain an inorganic polyelectrolyte magnesium aluminum zinc polysilicate.
S03: a solution of magnesium iron aluminum zinc polysilicate of 0.5 wt.% relative to the mass of silica was added dropwise to the prepared silica sol at room temperature with stirring and stirred continuously for 6 hours. And refining the mixed solution by centrifuging, filtering and the like to obtain 0.5 wt.% of inorganic polyelectrolyte modified silicon oxide composite polishing abrasive particles.
S04: and (4) adding sodium hydroxide into the solution obtained in the step (S03), controlling the pH value of the solution to be 10, then adding a certain amount of sodium hexametaphosphate dispersant and sodium dodecyl benzene sulfonate surfactant, uniformly stirring, and filtering by using a 1-micron filter element to remove impurities to obtain the polishing solution composition.
The inorganic polyelectrolyte-silicon oxide composite abrasive particle polishing solution composition comprises the following components in percentage by mass:
0.5 wt.% magnesium iron aluminum zinc polysilicate modified silica 10.0 wt.%;
0.03 wt.% sodium hexametaphosphate;
sodium dodecylbenzenesulfonate 0.5 wt.%;
residual water;
the sum of the mass percent of the components is 100 percent.
Example 2
The same as example 1 except that in step S03, the amount of poly (magnesium iron aluminum zinc silicate) was 0.7 wt.% of the silica. Obtaining 0.7 wt.% inorganic polyelectrolyte modified silicon oxide composite polishing abrasive particles and polishing solution thereof.
Example 3
The same as example 1 except that in step S03, the amount of poly (magnesium iron aluminum zinc silicate) was 1.0 wt.% of the silica. Obtaining the 1.0 wt.% inorganic polyelectrolyte modified silicon oxide composite polishing abrasive particles and the polishing solution thereof.
Example 4
The same as example 1 except that in step S03, the amount of poly (magnesium iron aluminum zinc silicate) was 1.5 wt.% of the silica. Obtaining the 1.5 wt.% inorganic polyelectrolyte modified silicon oxide composite polishing abrasive particles and the polishing solution thereof.
Example 5
The same as example 1 except that in step S03, the amount of poly (magnesium iron aluminum zinc silicate) was 3.0 wt.% of the silica. Obtaining the 3.0 wt.% inorganic polyelectrolyte modified silicon oxide composite polishing abrasive particles and the polishing solution thereof.
Example 6
The same as example 1 except that in step S03, the amount of poly (magnesium iron aluminum zinc silicate) was 5.0 wt.% of the silica. To obtain 5.0 wt.% inorganic polyelectrolyte modified silicon oxide composite polishing abrasive particles and polishing solution thereof.
The following comparative examples were made for comparison with the silicon oxide abrasive grains and the polishing liquid thereof which are generally used.
Comparative example
Pure silica abrasive grains and polishing slurry thereof without addition of inorganic polyelectrolyte were prepared in the same manner as in example 1 except that steps S02 and S03 were not performed. The method comprises the following specific steps:
s01: the silica sol is prepared by a seed induced growth method. First, an 8 wt.% sodium silicate (Na2SiO3) solution was passed through a cation exchange resin pretreated with HCl to obtain an active silicic acid solution. The 10 wt.% silica seed solution was then heated to 100 ℃ and stirred, the pH of the solution was adjusted to 10 with sodium hydroxide. Next, the prepared active silicic acid solution was added dropwise to the above silica seed solution under constant stirring while maintaining the pH of the system at about 10 using a 1 wt.% NaOH solution. During this process, the evaporation rate of the solution and the dropping rate of the silicic acid were kept equal to maintain a constant liquid level of the system. After the silicic acid is added dropwise, the mixture is continuously stirred and cooled to room temperature, and the mass fraction is adjusted to 10 wt.%.
S02: and (4) adding sodium hydroxide into the solution obtained in the step (S01), controlling the pH value of the solution to be 10, then adding a certain amount of sodium hexametaphosphate dispersant and sodium dodecyl benzene sulfonate surfactant, uniformly stirring, and filtering by a 1-micron filter element to obtain the polishing solution.
The pure silica sol polishing solution composition comprises the following components in percentage by mass:
10 wt.% silica;
0.03 wt.% sodium hexametaphosphate;
sodium dodecylbenzenesulfonate 0.5 wt.%;
residual water;
the sum of the mass percent of the components is 100 percent.
A polishing test was performed on a sapphire substrate under a constant polishing condition using the polishing liquids of each of examples 1 to 6 and comparative example 1 described above.
The polishing conditions for the polishing test were as follows:
polishing machine: UNIPOL-1502 single side polisher;
workpiece: a sapphire (0001) plane having a diameter of 50.8 mm;
polishing the pad: polyurethane materials, RODEL production;
polishing pressure: 63.2g/cm2；
Rotating speed of a lower disc: 70 rpm;
polishing time: 120 minutes;
after polishing, the sapphire substrate was washed and dried, and the mass before and after polishing was weighed with a precision analytical balance to calculate the polishing rate. Then, the surface of the sample was measured by using (1) mbios XI-100 surface topographer, and the resolution was 0.1 angstrom. The substrate was measured for surface topography and the surface average roughness (Ra) was measured to be 93.5 μm by 93.5. mu.m.
The polishing effect of the polishing solution composition of each example is shown in table 1, and it can be seen from table 1 that after the polishing solution of the silica abrasive grains and the polishing solution of the inorganic polyelectrolyte-silica abrasive grains prepared in examples 1, 2, 3, 4, 5 and 6 polish a sapphire substrate, the polishing rate is improved and the roughness of the sapphire surface is reduced at a lower modification degree (0.5 to 1.5 wt.% of polyelectrolyte in silica) by using the polishing solution of the inorganic polyelectrolyte-silica abrasive grains prepared in the invention.
TABLE 1 polishing Effect of each example polishing solution on sapphire substrates
According to the inorganic polyelectrolyte-silicon oxide composite abrasive particle polishing solution prepared by the invention, due to the introduction of cations in the inorganic polymer, the electrostatic repulsion between silicon oxide particles and a workpiece is reduced, so that more effective abrasive particles are in contact with the surface of the workpiece (such as a sapphire wafer) in the polishing process, a soft layer formed through chemical reaction can be quickly removed, the synergistic effect of chemical corrosion and mechanical wear is optimal, and the material removal rate is higher; and polishing damage such as scratches and surface damage is small because the silica particles themselves are small in hardness. Therefore, when the novel abrasive particles prepared by the method are used for polishing the sapphire substrate, the material removal rate of the sapphire substrate can be improved, and the surface roughness can be reduced. In addition, the prepared inorganic polyelectrolyte has no toxicity, and the green and environment-friendly concept of the polishing solution is realized.
The above description is only a preferred embodiment of the present invention, and the embodiment is not intended to limit the scope of the present invention, so that all equivalent structural changes made by using the contents of the specification and the drawings of the present invention should be included in the scope of the appended claims.
Claims (5)
1. A preparation method of inorganic polyelectrolyte-silicon oxide composite polishing abrasive particles is characterized by comprising the following steps:
s01: preparing nano silica sol: stirring and heating the silicon dioxide seed crystal solution to 100 ℃, and adjusting the pH to 10; dropwise adding an active silicic acid solution into the silicon dioxide seed crystal solution under the stirring condition, simultaneously adjusting the pH to 10, and keeping the evaporation rate of the solution equal to the dropwise adding rate of silicic acid; cooling to room temperature to obtain nano silica sol;
s02: preparing inorganic polyelectrolyte poly-magnesium-ferrum-aluminum-zinc silicate: dropwise adding sulfuric acid into a sodium silicate solution under the condition of stirring, and adjusting the pH to 4; polymerizing the sulfuric acid and the sodium silicate solution at 25 ℃ for 1 hour, respectively adding magnesium sulfate, ferric chloride (III) hexahydrate, aluminum nitrate nonahydrate and zinc sulfate under the stirring condition, and aging for 24 hours to obtain inorganic polyelectrolyte poly-magnesium-iron-aluminum-zinc silicate;
s03: dropwise adding the zinc iron aluminum magnesium polysilicate into the nano silica sol at 25 ℃ under the stirring condition, and continuously stirring for 6 hours; centrifuging and filtering to obtain inorganic polyelectrolyte-silicon oxide composite polishing abrasive particle solution; wherein the mass ratio of the inorganic polyelectrolyte to the silicon oxide is 0.5-5.0: 100.
2. the method of claim 1, wherein the pH of the step S01 is adjusted to 10 by using a 1% sodium hydroxide solution.
3. The method as claimed in claim 1, wherein the nano silica sol silica is present in an amount of 10% by mass in step S01.
4. The method of claim 1, wherein 0.4mol/L sulfuric acid is added dropwise to 0.04mol/L sodium silicate solution with stirring in step S01.
5. The method of claim 1, further comprising step S04 of: and adjusting the pH value of the inorganic polyelectrolyte-silicon oxide composite polishing abrasive particle solution to 10, and adding a surfactant to obtain the inorganic polyelectrolyte-silicon oxide composite polishing solution.
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| CN114525108A (en) * | 2022-02-18 | 2022-05-24 | 太仓硅源纳米材料有限公司 | Silica sol active abrasive particles for chemical mechanical polishing and preparation method thereof |
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