CN110713192B - Preparation method of spherical silicon dioxide nanoparticle slurry - Google Patents
Preparation method of spherical silicon dioxide nanoparticle slurry Download PDFInfo
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Abstract
The invention relates to the technical field of preparation of silicon dioxide nanoparticles, in particular to a preparation method of spherical silicon dioxide nanoparticle slurry. The preparation process of the spherical silicon dioxide nano-particle slurry is carried out in a precipitation aging reactor; the precipitation aging reactor comprises a kettle body, wherein a centrifugal mixer is arranged at the upper part of the kettle body, and a liquid distributor is arranged at the center of the centrifugal mixer; the lower part of the kettle body is an aging area; the reactant A and the reactant B enter a liquid distributor through a pipeline, are uniformly mixed and then react, slurry after reaction enters an aging zone for aging, and is continuously discharged under the condition of keeping a certain liquid holding capacity of the aging zone, so that continuous production is formed; and evaporating and concentrating the outflow slurry under reduced pressure to form spherical silicon dioxide nano-particle slurry with the particle size of 10-200 nm. The solid content of the silicon dioxide nano particle slurry obtained by the invention is high, wherein the particle size of the silicon dioxide nano particles is controllable and uniform.
Description
Technical Field
The invention relates to the technical field of preparation of silicon dioxide nanoparticles, in particular to a preparation method of spherical silicon dioxide nanoparticle slurry.
Background
To date, ultra-precise Chemical Mechanical Polishing (CMP) techniques have been the only technique for providing globally planarized surface finishes in Integrated Circuit (IC) and ultra large or very large scale integrated (ULSI) fabrication processes. And silicon dioxide SiO2The sol polishing solution is an important polishing medium in the CMP technology, and is mainly used for rough polishing and fine polishing of silicon substrates and polishing of interlayer media. The silica sol belongs to a colloidal solution, is a dispersion of nano-scale silica particles in water or a solvent, and is odorless and nontoxic.
At present, the effective component of the polishing solution for fine polishing of silicon dioxide is mainly spherical silicon dioxide nano-particle sol, and the following preparation methods are available:
(1) the water glass is used as a raw material, a nano-scale nucleus is formed through ion exchange, and then the nucleus grows into nano-particles in an aqueous solution, so that the colloidal form is basically maintained, and long-term stability can be realized through adjustment. The high-concentration colloidal silicon dioxide can be prepared by adopting different concentration modes, and is convenient to transport and store. The colloidal silicon dioxide is not dried and dehydrated in the preparation process, so that the colloidal silicon dioxide is moderate in hardness, does not scratch a wafer due to the hardness, is low in viscosity and weak in adhesion, is easy to clean after polishing, and is widely used for roughly polishing and finely polishing silicon wafers. However, the method for preparing the large-particle-size colloidal silica has the defects of complex process, difficult growth, non-uniform particles and wide particle size distribution, and cannot meet the requirements of a fine line process.
(2) The sol-gel method takes alkoxy silane as raw material, takes hydrolysis reaction under the action of alkali catalyst, and can prepare the silicon dioxide abrasive with consistent grain diameter and higher purity by controlling hydrolysis conditions. But is mainly used for high-end requirements, such as chip level, due to higher raw material cost. However, the method for producing a silica sol in which alkoxysilane is hydrolyzed under base catalysis to give a synthetic route has the following disadvantages:
a. the reaction is carried out by using a conventional batch reactor, the concentration of a reaction product cannot be higher than about 5 percent, otherwise, a reaction system can generate a viscous phenomenon, so that the production efficiency is lower;
b. when the synthetic route is used for preparing the silica sol, the mixing state of the materials has great influence on the quality of the product. In the reaction process, if the two components cannot be uniformly mixed in a short time, the local reaction concentration is too high, and the uniformity of final product particles is influenced, so that the quality of the product is influenced.
Disclosure of Invention
The invention aims to provide a preparation method of spherical silicon dioxide nanoparticle slurry, which has high solid content, wherein the particle size of silicon dioxide nanoparticles is controllable and uniform.
The preparation method of the spherical silicon dioxide nanoparticle slurry comprises the following steps: the preparation process of the spherical silicon dioxide nano-particle slurry is carried out in a precipitation aging reactor; the precipitation aging reactor comprises a kettle body, wherein a centrifugal mixer arranged on a stirring paddle is arranged at the upper part of the kettle body, and a liquid distributor is arranged at the center of the centrifugal mixer; the lower part of the kettle body is an aging area;
the reactant A and the reactant B enter a liquid distributor positioned in the center of a centrifugal mixer, move from the inside of the centrifugal mixer to the outside along the radial direction under the centrifugal force, the reactant A and the reactant B are uniformly mixed and react under the action of the centrifugal mixer, slurry after reaction enters an aging zone for aging, and is continuously discharged under the condition of keeping a certain liquid retention amount in the aging zone to form continuous production; and (3) the slurry flowing out of the precipitation aging reactor is evaporated and concentrated under reduced pressure to form spherical silicon dioxide nanoparticle slurry with the particle size of 10-200 nm.
Wherein:
the reactant A is alkoxy silane or a mixture of alkoxy silane and a first organic solvent; the molar ratio of alkoxysilane to first organic solvent is from 1:0 to 5, preferably from 1:0 to 2.
The alkoxy silane comprises one or more of methoxy silane, ethoxy silane, propoxy silane or butoxy silane, and preferably tetramethoxy silane or tetraethoxy silane.
The first organic solvent comprises one or more of methanol, ethanol, glycol, propanol, propylene glycol, glycerol or butanol.
The reactant B comprises a base catalyst, water and a second organic solvent; the molar ratio of water to the base catalyst is 1-50: 1; the molar ratio of the second organic solvent to the base catalyst is 1-50: 1.
The alkali catalyst comprises one or more of sodium hydroxide, potassium hydroxide, organic amine, quaternary ammonium base or ammonia water.
The second organic solvent comprises one or more of methanol, ethanol, ethylene glycol, propanol, propylene glycol, glycerol or butanol.
The molar ratio of the alkoxy silane to the base catalyst is 1:0.01-2, preferably 1:0.05-1, more preferably 1: 0.1-0.5.
The temperature of the reactant A, the reactant B, the slurry in the aging area and the slurry flowing out of the precipitation aging reactor are controlled to be 0-60 ℃, preferably 10-50 ℃, and more preferably 20-40 ℃.
The pH value of the slurry flowing out of the precipitation aging reactor is 9-12, and the solid content is controlled to be 5-15wt.%, preferably 13-14 wt.%; the solid content of the spherical silica nanoparticle slurry is 30-40 wt.%.
The preparation process of the spherical silicon dioxide nanoparticle slurry is carried out in a precipitation aging reactor, the precipitation aging reactor comprises a kettle body, the upper part of the kettle body is provided with a centrifugal mixer, the lower part of the kettle body is an aging area, a stirring paddle is arranged in the aging area, the centrifugal mixer is connected with a rotating shaft of the stirring paddle, the top of the rotating shaft is provided with a variable frequency motor, and the variable frequency motor drives the centrifugal mixer and the stirring paddle to rotate together; the center of the centrifugal mixer is provided with a liquid distributor; the liquid distributor is respectively connected with the storage tank A and the storage tank B through a flowmeter; centrifugal pumps are respectively arranged on pipelines connecting the liquid distributor with the storage tank A and the storage tank B. The storage tank A and the storage tank B respectively store a reactant A and a reactant B.
The material of the centrifugal mixer 6 can be metal or high molecular polymer, and the inside of the centrifugal mixer 6 is filled with wire mesh filler.
The reactant A and the reactant B are conveyed by a centrifugal pump, enter a liquid distributor positioned in the center of a centrifugal mixer through a flowmeter along a pipeline, move from the inside to the outside of the centrifugal mixer along the radial direction under the centrifugal force, are uniformly mixed and react under the action of the centrifugal mixer, and slurry after reaction enters an aging zone for aging, and is continuously discharged under the condition of keeping a certain liquid retention amount in the aging zone to form continuous production; and (3) the slurry flowing out of the precipitation aging reactor is subjected to reduced pressure evaporation concentration to remove redundant organic solvent and volatile reactants in the slurry, so as to form spherical silicon dioxide nanoparticle slurry with the particle size of 10-200 nm.
The invention has the following beneficial effects:
(1) according to the invention, the centrifugal mixer is arranged above the interior of the precipitation aging reactor, and the liquid distributor is arranged in the center of the centrifugal mixer, so that the reactant A and the reactant B can be mixed very uniformly in a short time, the reaction is more thorough, and the phenomenon of overhigh local reaction concentration is avoided; and (3) the reacted slurry enters an aging zone for further aging, and the particle size of the silicon dioxide in the obtained spherical silicon dioxide nano-particle slurry is between 10 and 200nm and is uniform through reduced pressure evaporation and concentration.
(2) The invention adopts the centrifugal mixer to mix and react the reactants, so that the ratio of the reactants is always kept consistent in the production process, the two reactants are uniformly mixed, the constancy of the reaction process state and the uniformity of the reaction product are ensured, and the uniformity of the particle size of the silicon dioxide particles is ensured. In addition, the silica particle slurry enters the aging zone, which can further increase the stability of the silica particles. The precipitation aging reactor can avoid the back mixing phenomenon of reactants, thereby avoiding the formation of uneven silicon dioxide particles.
(3) The slurry prepared by the existing batch reaction kettle is easy to crosslink particles formed in the continuous reaction process of one reactant and the other reactant because one reactant is always in a highly excessive state, so that the concentration of a reaction product can only reach about 5 wt%; if the reactant concentration is too high, the reaction slurry becomes more viscous and loses fluidity. The centrifugal mixer is adopted for mixing the reactants, so that the high excessive amount of the reactants is avoided, the crosslinking of the silica particles is avoided, the solid content of slurry in the precipitation aging reactor can reach about 14 wt.%, the solid content of the obtained spherical silica nanoparticle slurry is 30-40wt.%, and the production efficiency is greatly improved.
(4) The centrifugal mixer and the aging zone are coupled together, so that the reacted materials can enter the aging zone in time, and the materials are discharged continuously under the condition of keeping a certain liquid holding capacity of the aging zone, thereby realizing continuous production and improving the yield.
Drawings
FIG. 1 is a schematic diagram of the structure of the apparatus of the present invention;
wherein: 1. a storage tank A; 2. a flowmeter A; 3. a kettle body; 4. a variable frequency motor; 5. a liquid distributor; 6. a centrifugal mixer; 7. a flow meter B; 8. a storage tank B; 9. a centrifugal pump B; 10. a stirring paddle; 11. a centrifugal pump A;
FIG. 2 is a scanning electron micrograph of spherical silica nanoparticles obtained in example 1;
FIG. 3 is a scanning electron micrograph of spherical silica nanoparticles obtained in example 2;
FIG. 4 is a scanning electron micrograph of spherical silica nanoparticles obtained in example 3;
FIG. 5 is a scanning electron micrograph of spherical silica nanoparticles obtained in example 4;
FIG. 6 is a scanning electron micrograph of spherical silica nanoparticles obtained in example 5;
fig. 7 is a scanning electron micrograph of the spherical silica nanoparticles obtained in example 6.
Detailed Description
The present invention is further described below with reference to examples.
Example 1
Reactant A contained 10.156kg tetramethoxysilane and 1100g methanol; reactant B comprised 12.237kg methanol, 5.338kg water and 1178g of 26.2 wt.% aqueous ammonia. The molar ratio of tetramethoxysilane to ammonia in the entire system was 1: 0.27.
The reactant A and the reactant B are respectively stored in a storage tank A and a storage tank B, heated to 50 ℃, conveyed to a precipitation aging reactor at the speed of 93.8g/min and 156.3g/min through a centrifugal pump A and a centrifugal pump B respectively, distributed on a centrifugal mixer through a liquid distributor, and formed into a uniform-concentration mixed state in a very short time under the action of centrifugal force, and reacted. And (3) aging the mixed slurry in an aging region at the lower part of the precipitation aging reactor, keeping the aging temperature at 50 ℃, and continuously discharging to finally form the slurry, wherein the pH value of the slurry is 11.03, and the solid content of the slurry is 13 wt.%. And (3) removing redundant organic solvent and volatile reactants in the slurry through reduced pressure evaporation concentration to obtain spherical silica nanoparticle slurry with the solid content of 40 wt.%. Wherein the spherical silica nanoparticles have a particle size of 40 nm. The scanning electron micrograph of the spherical silica nanoparticles is shown in fig. 2.
Example 2
Reactant A was 10.156kg tetramethoxysilane; reactant B comprised 12.237kg of methanol, 4.287kg of water and 1433g of 26.2 wt.% aqueous ammonia. The molar ratio of tetramethoxysilane to ammonia in the entire system was 1: 0.33.
The reactant A and the reactant B are respectively stored in a storage tank A and a storage tank B, heated to 45 ℃, conveyed to a precipitation aging reactor at the speed of 84.6g/min and 149.6g/min through a centrifugal pump A and a centrifugal pump B, distributed on a centrifugal mixer through a liquid distributor, and formed into a uniform-concentration mixed state in a very short time under the action of centrifugal force, and reacted. And (3) aging the mixed slurry in an aging area at the lower part of the precipitation aging reactor, keeping the aging temperature at 45 ℃, continuously discharging, and finally forming the slurry, wherein the pH value of the slurry is 11.3, and the solid content of the slurry is 14 wt.%. And (3) removing redundant organic solvent and volatile reactants in the slurry through reduced pressure evaporation concentration to obtain spherical silica nanoparticle slurry with the solid content of 40 wt.%. Wherein the spherical silica nanoparticles have a particle size of 50 nm. The scanning electron micrograph of the spherical silica nanoparticles is shown in fig. 3.
Example 3
Reactant A was 10.156kg tetramethoxysilane; reactant B comprised 12.237kg methanol, 4.287kg water and 870g of 26.2 wt.% aqueous ammonia. The molar ratio of tetramethoxysilane to ammonia in the entire system was 1: 0.20.
The reactant A and the reactant B are respectively stored in a storage tank A and a storage tank B, heated to the temperature of 35 ℃, conveyed to a precipitation aging reactor at the speed of 84.6g/min and 149.6g/min through a centrifugal pump A and a centrifugal pump B, distributed on a centrifugal mixer through a liquid distributor, and formed into a uniform-concentration mixed state in a very short time under the action of centrifugal force, and reacted. And (3) aging the mixed slurry in an aging area at the lower part of the precipitation aging reactor, keeping the aging temperature at 35 ℃, continuously discharging, and finally forming the slurry, wherein the pH value of the slurry is 11.1, and the solid content of the slurry is 14 wt.%. And (3) removing redundant organic solvent and volatile reactants in the slurry through reduced pressure evaporation concentration to obtain spherical silica nanoparticle slurry with the solid content of 40 wt.%. Wherein the particle size of the spherical silicon dioxide nano-particles is 60-70 nm. The scanning electron micrograph of the spherical silica nanoparticles is shown in fig. 4.
Example 4
Reactant A was 10.156kg tetramethoxysilane; reactant B comprised 12.237kg methanol, 4.287kg water and 870g of 26.2 wt.% aqueous ammonia. The molar ratio of tetramethoxysilane to ammonia in the entire system was 1: 0.20.
The reactant A and the reactant B are respectively stored in a storage tank A and a storage tank B, are heated to 35 ℃, are conveyed into a precipitation aging reactor at the speed of 169.2g/min and 290g/min through a centrifugal pump A and a centrifugal pump B respectively, are distributed on a centrifugal mixer through a liquid distributor, and form a uniform-concentration mixed state in a very short time under the action of centrifugal force, and react. And (3) aging the mixed slurry in an aging area at the lower part of the precipitation aging reactor, keeping the aging temperature at 35 ℃, continuously discharging, and finally forming the slurry, wherein the pH value of the slurry is 11.1, and the solid content of the slurry is 14 wt.%. And (3) removing redundant organic solvent and volatile reactants in the slurry through reduced pressure evaporation concentration to obtain spherical silica nanoparticle slurry with the solid content of 40 wt.%. Wherein the particle size of the spherical silicon dioxide nano-particles is 70-80 nm. The scanning electron micrograph of the spherical silica nanoparticles is shown in fig. 5.
Example 5
Reactant A was 10.156kg tetramethoxysilane; reactant B comprised 12.237kg methanol, 4.287kg water and 870g of 26.2 wt.% aqueous ammonia. The molar ratio of tetramethoxysilane to ammonia in the entire system was 1: 0.20.
The reactant A and the reactant B are respectively stored in a storage tank A and a storage tank B, heated to 50 ℃, conveyed to a precipitation aging reactor at the speed of 84.6g/min and 149.6g/min through a centrifugal pump A and a centrifugal pump B, distributed on a centrifugal mixer through a liquid distributor, and formed into a uniform-concentration mixed state in a very short time under the action of centrifugal force, and reacted. And (3) aging the mixed slurry in an aging area at the lower part of the precipitation aging reactor, keeping the aging temperature at 50 ℃, and continuously discharging to finally form the slurry, wherein the pH value of the slurry is 10.8, and the solid content of the slurry is 14 wt.%. And (3) removing redundant organic solvent and volatile reactants in the slurry through reduced pressure evaporation concentration to obtain spherical silica nanoparticle slurry with the solid content of 40 wt.%. Wherein the spherical silica nanoparticles have a particle size of 30 nm. The scanning electron micrograph of the spherical silica nanoparticles is shown in fig. 6.
Example 6
The reactant A was 13.900kg of tetraethoxysilane; reactant B comprised 12.237kg ethanol, 4.287kg water and 870g of 26.2 wt.% aqueous ammonia. The molar ratio of tetraethoxysilane to ammonia in the whole system was 1: 0.20.
The reactant A and the reactant B are respectively stored in a storage tank A and a storage tank B, heated to 45 ℃, conveyed to a precipitation aging reactor at the speed of 115.8g/min and 156.3g/min through a centrifugal pump A and a centrifugal pump B respectively, distributed on a centrifugal mixer through a liquid distributor, and formed into a uniform-concentration mixed state in a very short time under the action of centrifugal force, and reacted. And (3) aging the mixed slurry in an aging area at the lower part of the precipitation aging reactor, keeping the aging temperature at 45 ℃, continuously discharging, and finally forming the slurry, wherein the pH value of the slurry is 10.9, and the solid content of the slurry is 14 wt.%. And (3) removing redundant organic solvent and volatile reactants in the slurry through reduced pressure evaporation concentration to obtain spherical silica nanoparticle slurry with the solid content of 40 wt.%. Wherein the spherical silica nanoparticles have a particle size of 100 nm. The scanning electron micrograph of the spherical silica nanoparticles is shown in fig. 7.
The preparation process of the spherical silicon dioxide nanoparticle slurry is carried out in a precipitation aging reactor, as shown in figure 1, the precipitation aging reactor comprises a kettle body 3, a centrifugal mixer 6 is arranged at the upper part of the kettle body 3, an aging area is arranged at the lower part of the kettle body, a stirring paddle 10 is arranged in the aging area, the centrifugal mixer 6 is connected with a rotating shaft of the stirring paddle 10, a variable frequency motor 4 is arranged at the top of the rotating shaft, and the variable frequency motor 4 drives the centrifugal mixer 6 to rotate together with the stirring paddle 10; the center of the centrifugal mixer 6 is provided with a liquid distributor 5; the liquid distributor 5 is respectively connected with a storage tank A1 and a storage tank B8 through a flowmeter A2 and a flowmeter B7; the pipelines of the liquid distributor 5 connected with the storage tank A1 and the storage tank B8 are respectively provided with a centrifugal pump A11 and a centrifugal pump B9. The storage tank a1 and the storage tank B8 store a reactant a and a reactant B, respectively.
The material of the centrifugal mixer 6 can be metal or high molecular polymer, and the inside of the centrifugal mixer 6 is filled with wire mesh filler.
The reactant A and the reactant B are respectively conveyed by a centrifugal pump A11 and a centrifugal pump B9, respectively enter a liquid distributor 5 positioned in the center of a centrifugal mixer 6 through a flow meter A2 and a flow meter B7 along a pipeline, move from the inside to the outside of the centrifugal mixer 6 along the radial direction under the centrifugal force, and are uniformly mixed and then reacted under the action of the centrifugal mixer 6, slurry after reaction enters an aging zone for aging, and is continuously discharged under the condition of keeping a certain liquid amount in the aging zone to form continuous production; and (3) the slurry flowing out of the precipitation aging reactor is subjected to reduced pressure evaporation concentration to remove redundant organic solvent and volatile reactants in the slurry, so as to form spherical silicon dioxide nanoparticle slurry with the particle size of 10-200 nm.
In examples 1 to 6, the rotational speeds of the centrifugal mixers were 800rpm, 1800rpm, 800rpm, and 1000rpm, respectively.
Claims (10)
1. A preparation method of spherical silicon dioxide nanoparticle slurry is characterized by comprising the following steps: the preparation process of the spherical silicon dioxide nano-particle slurry is carried out in a precipitation aging reactor; the precipitation aging reactor comprises a kettle body (3), wherein a centrifugal mixer (6) arranged on a stirring paddle (10) is arranged at the upper part of the kettle body (3), and a liquid distributor (5) is arranged at the center of the centrifugal mixer (6); the lower part of the kettle body (3) is an aging area;
the reactant A and the reactant B enter a liquid distributor (5) positioned in the center of a centrifugal mixer (6), move from the inside to the outside of the centrifugal mixer (6) along the radial direction under the centrifugal force, the reactant A and the reactant B are uniformly mixed and react under the action of the centrifugal mixer (6), the reacted slurry enters an aging zone for aging, and the continuous discharge is realized under the condition of keeping a certain liquid retention amount in the aging zone to form continuous production; the slurry flowing out of the precipitation aging reactor is evaporated and concentrated under reduced pressure to form spherical silicon dioxide nano-particle slurry with the particle size of 10-200 nm;
the reactant A is alkoxy silane or a mixture of alkoxy silane and a first organic solvent;
reactant B includes a base catalyst, water, and a second organic solvent.
2. The method for preparing a spherical silica nanoparticle slurry according to claim 1, characterized in that: the molar ratio of the alkoxysilane to the first organic solvent is 1: 0-5.
3. The method for preparing a spherical silica nanoparticle slurry according to claim 2, characterized in that: the alkoxy silane comprises one or more of methoxy silane, ethoxy silane, propoxy silane or butoxy silane.
4. The method for preparing a spherical silica nanoparticle slurry according to claim 3, characterized in that: the alkoxy silane is tetramethoxy silane or tetraethoxy silane.
5. The method for preparing a spherical silica nanoparticle slurry according to claim 2, characterized in that: the first organic solvent includes one or more of methanol, ethanol, ethylene glycol, propanol, propylene glycol, glycerol, or butanol.
6. The method for preparing a spherical silica nanoparticle slurry according to claim 1, characterized in that: the molar ratio of water to the base catalyst is 1-50: 1; the molar ratio of the second organic solvent to the base catalyst is 1-50: 1.
7. The method for preparing a spherical silica nanoparticle slurry according to claim 6, wherein: the base catalyst comprises one or more of sodium hydroxide, potassium hydroxide, organic amine, quaternary ammonium base or ammonia water.
8. The method for preparing a spherical silica nanoparticle slurry according to claim 6, wherein: the second organic solvent comprises one or more of methanol, ethanol, ethylene glycol, propanol, propylene glycol, glycerol or butanol.
9. The method for preparing a spherical silica nanoparticle slurry according to claim 2 or 6, characterized in that: the molar ratio of the alkoxysilane to the base catalyst is 1: 0.01-2.
10. The method for preparing a spherical silica nanoparticle slurry according to claim 1, characterized in that: the temperature of the reactant A, the reactant B, the slurry in the aging area and the slurry flowing out of the precipitation aging reactor are controlled to be 0-60 ℃; the pH value of slurry flowing out of the precipitation aging reactor is 9-12, and the solid content is controlled to be 5-15 wt.%; the solid content of the spherical silica nanoparticle slurry is 30-40 wt.%.
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