CN110655087A - Silica colloid and preparation method thereof - Google Patents
Silica colloid and preparation method thereof Download PDFInfo
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- CN110655087A CN110655087A CN201911012164.5A CN201911012164A CN110655087A CN 110655087 A CN110655087 A CN 110655087A CN 201911012164 A CN201911012164 A CN 201911012164A CN 110655087 A CN110655087 A CN 110655087A
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- silicic acid
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- silicon dioxide
- silica
- active silicic
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 132
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 60
- 239000000084 colloidal system Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000000366 colloid method Methods 0.000 title description 2
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 67
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000013078 crystal Substances 0.000 claims abstract description 17
- 239000000203 mixture Substances 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 239000003513 alkali Substances 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 238000005498 polishing Methods 0.000 claims description 35
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 20
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 8
- 235000019353 potassium silicate Nutrition 0.000 claims description 7
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 7
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 5
- 238000005341 cation exchange Methods 0.000 claims description 5
- 239000003729 cation exchange resin Substances 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 150000007529 inorganic bases Chemical class 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims 1
- 150000001768 cations Chemical class 0.000 abstract description 7
- 239000012535 impurity Substances 0.000 abstract description 4
- 229910052751 metal Inorganic materials 0.000 abstract description 4
- 239000002184 metal Substances 0.000 abstract description 4
- 239000003054 catalyst Substances 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 32
- 239000002245 particle Substances 0.000 description 14
- 238000003756 stirring Methods 0.000 description 9
- 229910052594 sapphire Inorganic materials 0.000 description 7
- 239000010980 sapphire Substances 0.000 description 7
- 235000012431 wafers Nutrition 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 3
- 238000007865 diluting Methods 0.000 description 3
- 238000002296 dynamic light scattering Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 230000002572 peristaltic effect Effects 0.000 description 3
- 239000000741 silica gel Substances 0.000 description 3
- 229910002027 silica gel Inorganic materials 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000012452 mother liquor Substances 0.000 description 2
- 150000007530 organic bases Chemical class 0.000 description 2
- 238000003921 particle size analysis Methods 0.000 description 2
- 238000007517 polishing process Methods 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 239000012798 spherical particle Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229940075614 colloidal silicon dioxide Drugs 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000010413 mother solution Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000000206 photolithography Methods 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
- C01B33/141—Preparation of hydrosols or aqueous dispersions
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
- C01B33/141—Preparation of hydrosols or aqueous dispersions
- C01B33/1412—Preparation of hydrosols or aqueous dispersions by oxidation of silicon in basic medium
Abstract
The invention provides a silicon dioxide colloid and a preparation method thereof, wherein the preparation method of the silicon dioxide colloid comprises the following steps: adding an inorganic alkali solution into active silicic acid with the pH of 2-4 according to a certain dropping speed requirement to prepare an alkaline mixture with the pH of 8.5-9.5; heating the alkaline mixture to 90-100 ℃, and preserving the temperature for at least 10min to obtain non-spherical silicon dioxide crystal seeds; heating the non-spherical silicon dioxide seed crystal to boil, and dripping active silicic acid and preserving heat for at least 10min under the condition of ensuring that the pH of the system is 9.0-10.0; naturally cooling to room temperature to obtain the silica colloid, wherein the silica particles in the silica colloid are non-spherical. The new preparation method is simple and effective, can ensure that the silica particles in the silica colloid are non-spherical, and avoids Ca in the silica colloid2+、Mg2+、Al3+And metal cation impurities are added, so that the application range of the catalyst is widened.
Description
Technical Field
The invention relates to a silicon dioxide colloid, in particular to a silicon dioxide colloid used in polishing solution.
Background
With the high development of integrated circuit technology, the surface quality of the substrate material used is more and more demanding. As the size of devices decreases, the depth of focus of optical lithography equipment decreases, requiring flatness of the wafer surface with acceptable resolution on the order of nanometers. To solve this problem, a Chemical Mechanical Polishing (CMP) technique capable of global planarization is one of the important key processes in semiconductor manufacturing. Chemical mechanical polishing utilizes chemical reaction and mechanical polishing to achieve the purpose of planarization, so that the polishing solution plays a central role in the CMP process. As one of the important components of CMP slurry, abrasive particles affect the removal of surface material of a wafer during a CMP process through their hardness, surface chemical activity, surface charging, and the like. Currently, the abrasive particles that are the mainstream in the market are nanoscale silicas, either sintered or amorphous. The sintered silicon dioxide has edges and corners, has higher hardness, has higher removal rate in the polishing process, but is easy to scratch the surface of a wafer; amorphous silica is generally spherical, smooth in edge, less hard, and less damaging to the wafer surface during polishing, but has a problem of low polishing rate (spherical particles are easily rolled during polishing). How to increase the polishing rate of the material without damaging the surface quality is a big problem faced by the CMP polishing solution. The non-spherical silica particles with unique shape, large specific surface and soft texture can simultaneously realize the perfect combination of rapid polishing and high surface quality, are favored by researchers and are prepared by various preparation methods. The preparation methods are roughly divided into two types, one is prepared by using an organic base catalyst to influence the isotropic growth of particles in the preparation process, and for example, the methods are adopted in patents of US6334880B1, US2008/0038996A1 US2009/0223136A1 and US2010/0163786A, CN 1102390837A; another class oneUsually by "cation induction" (e.g. Ca)2+、Mg2+、Al3+) Namely, the method is adopted to prepare by selecting proper divalent or trivalent cations as the morphology control agent, such as patents CN103408027A, CN101402829A, CN101626979A and the like. The organic base is not environment-friendly and is not suitable for large-scale production; the introduction of divalent or trivalent cations can reduce the purity and stability of colloidal silicon dioxide, limiting its use in integrated circuit polishing processes.
Disclosure of Invention
In view of the above-mentioned disadvantages of the prior art, an object of the present invention is to provide a silica colloid and a method for preparing the same, which solve the problems of the prior art.
To achieve the above objects and other related objects, the present invention is achieved by the following technical solutions.
The invention firstly provides a preparation method of silicon dioxide colloid, which comprises the following steps:
adding an inorganic alkali solution into active silicic acid with the pH of 2-4 to prepare an alkaline mixture with the pH of 8.5-9.5;
heating the alkaline mixture to 90-100 ℃, and preserving the temperature for at least 10min to obtain a non-spherical silicon dioxide seed crystal solution;
heating the non-spherical silicon dioxide seed crystal to boil, dripping active silicic acid under the condition of ensuring that the pH of the system is 9.0-10.0, and preserving the temperature for at least 10 min;
naturally cooling to room temperature to obtain the non-spherical silica colloid.
The heat preservation time in the application can be determined according to the reaction condition, and under the general condition, the heat preservation time is not more than 1 h.
According to the technical scheme of the invention, the active silicic acid is obtained by adding a water glass solution into a strong acid type cation exchange resin for cation exchange.
The active silicic acid in this application is a colloidal solution with a silica content of 2.0 wt% to 6.0 wt%, and the most important reason for the ability of silicic acid to nucleate growth into nanoparticles is due to its polymeric nature. The silicic acid molecules can be partially or totally polymerized into a chain or three-dimensional network structure, and the polymerization degree is generally different from dozens to hundreds.
According to the technical scheme of the invention, the content of silicon dioxide in the water glass solution is 3 wt% -6 wt%.
According to the technical scheme of the invention, the inorganic base is one or two selected from potassium hydroxide and sodium hydroxide.
According to the technical scheme of the invention, the concentration of the inorganic alkali solution is 0.5-2.0 wt%. The inorganic base solution in this application is an aqueous solution of an inorganic base.
According to the technical scheme of the invention, the volume ratio of the non-spherical silicon dioxide seed crystal to the dropwise added active silicic acid is 0.1-0.15.
According to the technical scheme of the invention, the speed of dripping the active silicic acid is 7-10 ml/min. In order to ensure that the silicon dioxide particles in the finally obtained silicon dioxide colloid are non-spherical, the speed of dripping the active silicic acid cannot be too fast or too slow, and the particles can only be ensured to grow according to the shape of the non-spherical silicon dioxide seed crystal at a proper speed, and if the dripping speed is too fast, new round seed crystals are easy to form nuclei independently among the silicic acid; if the dropping speed is too slow, the production efficiency is affected.
According to the technical scheme of the invention, the inorganic alkali solution is added into the active silicic acid at the speed of 1.0-5.0ml/min to obtain the alkaline mixture. In order to ensure that the formed silicon dioxide seed crystal is non-spherical, the speed of adding the inorganic alkali solution into the active silicic acid is moderate, and spherical particles are easily generated at an excessively high adding speed; too slow an addition rate can result in instability of the silicic acid, which tends to gel and fail to form silica seeds.
The invention also discloses the non-spherical silicon dioxide colloid prepared by the preparation method.
According to the non-spherical silica colloid, the axial particle size of silica particles in the non-spherical silica colloid is 10-20nm, and the radial particle size is 40-80 nm.
The nonspherical silica colloid has a solid content of 20 to 30 wt%.
The application also discloses the use of the non-spherical silica colloid as described above as a polishing solution in integrated circuits.
The use of the above-mentioned, adjust the pH of said non-spherical silica colloid to 9.5-10.5 and use as polishing solution.
The present application provides a novel silica gel and a method for preparing the same, which is simple and effective, can ensure that silica particles in the silica gel are non-spherical, and can prevent Ca in the silica gel from being present2 +、Mg2+、Al3+Metal cation impurities are waited, so that the application range of the metal cation impurities is widened, and the metal cation impurities are very suitable for being applied to the fields of integrated circuits and the like; in addition, organic alkali is not adopted in the method, so that the environmental protection problem caused in production can be effectively avoided.
Drawings
FIG. 1 shows an electron microscope picture of non-spherical silica particles prepared in example 1 of the present invention.
Detailed Description
The following description of the embodiments of the present invention is provided for illustrative purposes, and other advantages and effects of the present invention will become apparent to those skilled in the art from the present disclosure.
Before the present embodiments are further described, it is to be understood that the scope of the invention is not limited to the particular embodiments described below; it is also to be understood that the terminology used in the examples is for the purpose of describing particular embodiments only, and is not intended to limit the scope of the present invention. Test methods in which specific conditions are not specified in the following examples are generally carried out under conventional conditions or under conditions recommended by the respective manufacturers.
When numerical ranges are given in the examples, it is understood that both endpoints of each of the numerical ranges and any value therebetween can be selected unless the invention otherwise indicated. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In addition to the specific methods, devices, and materials used in the examples, any methods, devices, and materials similar or equivalent to those described in the examples may be used in the practice of the invention in addition to the specific methods, devices, and materials used in the examples, in keeping with the knowledge of one skilled in the art and with the description of the invention.
Example 1
Diluting concentrated water glass with pure water until the content of silicon dioxide is 4 wt%, stirring uniformly, adding into regenerated strong acid type cation exchange resin, and performing cation exchange to obtain active silicic acid. The pH of the activated silicic acid was 2.80 and the silica content was 4 wt%.
1500ml of active silicic acid is added into a reactor, stirring is started, and 1.0 wt% of sodium hydroxide aqueous solution is added into the active silicic acid at a certain speed of 1.0ml/min until the pH value of the solution is 8.5, thus obtaining an alkaline mixture.
The above alkaline mixture was warmed to 100 ℃ and held at 100 ℃ for 0.2 hour to obtain an aspherical silica seed crystal solution.
Taking the non-spherical silicon dioxide seed crystal solution prepared in the above steps as a mother liquor, stirring and heating to boil, adding 15000ml of active silicic acid by a peristaltic pump at the speed of 9ml/min, and dropwise adding 1.0 wt% sodium hydroxide solution to keep the pH value of the whole system at 9.0-10.0. After all the silicic acid is added, continuously preserving the heat for 0.5 hour, and naturally cooling to room temperature to obtain the non-spherical silicon dioxide colloid.
The mean particle diameter of the nonspherical particles was 39.0nm, the polydispersity index PDI was 0.262, the pH was 9.20 and the concentration was 21.25% by weight, as determined by laser particle size analysis (dynamic light scattering). The scanning electron microscope results are shown in FIG. 1.
Example 2
Diluting concentrated water glass with pure water until the content of silicon dioxide is 3 wt%, stirring uniformly, adding into regenerated strong acid type cation exchange resin, and performing cation exchange to obtain active silicic acid. The pH of the active silicic acid was 2.72 and the silica content was 3 wt%.
2000ml of active silicic acid was added to the reactor, stirring was turned on, and 2.0 wt% aqueous potassium hydroxide solution was added to the active silicic acid at a rate of 2.5ml/min to a solution pH of 8.95, to prepare an alkaline mixture.
And (3) heating the alkaline mixture to 95 ℃, and keeping the temperature at 95 ℃ for 0.5 hour to obtain the non-spherical silicon dioxide seed crystal solution.
Taking the non-spherical silicon dioxide seed crystal solution prepared in the above steps as a mother liquor, stirring and heating to boil, adding 20000ml of active silicic acid at a speed of 10ml/min by a peristaltic pump, and dropwise adding 2.0 wt% potassium hydroxide solution to maintain the pH value of the whole system at 9.0-10.0. After all the silicic acid is added, keeping the temperature for 1 hour, and naturally cooling to room temperature to obtain the non-spherical silicon dioxide colloid.
The mean particle diameter of the nonspherical particles measured by means of a laser particle size analyzer (dynamic light scattering method) was 35.4nm, the polydispersity index PDI was 0.280, the pH was 9.24 and the concentration was 20.5% by weight.
Example 3
Diluting concentrated water glass with pure water until the content of silicon dioxide is 6 wt%, stirring uniformly, adding into regenerated strong acid type cation exchange resin, and performing cation exchange to obtain active silicic acid. The pH of the active silicic acid was 3.01 and the silica content was 6 wt%.
1000ml of active silicic acid is added into a reactor, the reactor is started to stir, 0.5 wt% sodium hydroxide solution is added into the active silicic acid at a certain speed of 5.0ml/min until the pH value of the solution is 9.5, and an alkaline mixture is prepared.
And (3) heating the alkaline mixture to 90 ℃, and keeping the temperature at 90 ℃ for 1 hour to obtain the non-spherical silicon dioxide seed crystal solution.
Taking the non-spherical silicon dioxide seed crystal solution prepared in the step as a mother solution, stirring and heating to boil, adding 10000ml of active silicic acid at the speed of 7ml/min through a peristaltic pump, and dropwise adding 0.5 wt% of sodium hydroxide solution to keep the pH value of the whole system at 9.0-10.0. After all the silicic acid is added, continuously preserving the heat for 0.2 hour, and naturally cooling to room temperature to obtain the non-spherical silicon dioxide colloid.
The mean particle diameter of the nonspherical particles was 37.9nm, the polydispersity index PDI was 0.274, the pH was 9.25 and the concentration was 24.8% by weight, as determined by laser particle size analysis (dynamic light scattering).
Example 4
The non-spherical silica colloids prepared in the above examples 1 to 3 were prepared into polishing solutions for rough polishing of sapphire wafers.
The preparation method of the polishing solution comprises the following steps: the non-spherical silica colloid prepared by the invention is diluted by pure water until the content of silica is 20 wt%, the pH value is adjusted to 10.0 by 3 wt% of sodium hydroxide aqueous solution, and 1kg is weighed after being uniformly stirred, thus obtaining the polishing solution.
Polishing experiment: a 2-inch a-phase sapphire sheet was attached to a polishing head by a back film adsorption method. The polishing parameters were set as follows: polishing pressure was 6 psi; the polishing pad rotating speed is 90 rpm; the rotating speed of the polishing sheet is 100 rpm; the flow rate of the polishing solution is 125 ml/min; the polishing time was 30 min. And after finishing each polishing, repairing the polishing pad by using a 4-inch diamond repairing disc for 5 minutes, ultrasonically cleaning the polished sapphire wafer in a cleaning solution for 10 minutes, and drying the polished sapphire wafer by using nitrogen. And observing the surface quality condition of the polished sapphire sheet by a metallographic microscope. The thickness polishing rate was calculated by measuring the difference in mass between before and after the sapphire sheet polishing, and the results are shown in table 1.
TABLE 1 comparative results of polishing experiments
| Sample (I) | Example 1 | Example 2 | Example 3 | Spherical 80nm silica |
| Polishing Rate (nm/min) | 16.45 | 15.90 | 16.30 | 11.93 |
The polishing rate of the nonspherical silica colloid prepared by the invention is at least 33% faster than that of the spherical large-particle-size silica particles (80nm) prepared by the traditional ion exchange method by a polishing rate comparison experiment. The sapphire sheets obtained in examples 1-3 have good surface quality after polishing, and have no obvious defects such as scratches, pits and the like.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (10)
1. The preparation method of the silica colloid is characterized by comprising the following steps:
adding an inorganic alkali solution into active silicic acid with the pH of 2-4 to prepare an alkaline mixture with the pH of 8.5-9.5;
heating the alkaline mixture to 90-100 ℃, and preserving the temperature for at least 10min to obtain a non-spherical silicon dioxide seed crystal solution;
heating the non-spherical silicon dioxide seed crystal to boil, and dripping active silicic acid and preserving heat for at least 10min under the condition of ensuring that the pH of the system is 9.0-10.0;
naturally cooling to room temperature to obtain the non-spherical silica colloid.
2. The preparation method according to claim 1, wherein the active silicic acid is obtained by adding a water glass solution into a strong acid type cation exchange resin for cation exchange.
3. The method according to claim 2, wherein the silica content in the water glass solution is 3 to 6 wt%.
4. The method according to claim 1, wherein the inorganic base is one or two selected from potassium hydroxide and sodium hydroxide.
5. The method according to claim 1, wherein the concentration of the inorganic alkali solution is 0.5 to 2.0 wt%.
6. The method according to claim 1, wherein the volume ratio of the nonspherical silica seed crystal to the dropwise added active silicic acid is 0.1 to 0.15.
7. The production method according to claim 1, wherein the speed of dropping the active silicic acid is 7 to 10 ml/min.
8. The method according to claim 1, wherein the alkali mixture is obtained by adding an inorganic alkali solution to the activated silicic acid at a rate of 1.0 to 5.0 ml/min.
9. A non-spherical silica colloid obtained by the production method according to any one of claims 1 to 8.
10. Use of the non-spherical silica colloid according to claim 9 as a polishing liquid in integrated circuits.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111269695A (en) * | 2020-02-29 | 2020-06-12 | 上海大学 | Peanut-shaped silicon oxide abrasive particles and preparation method and application thereof |
| CN113773806A (en) * | 2021-10-19 | 2021-12-10 | 广东惠尔特纳米科技有限公司 | Nano silicon dioxide abrasive material and preparation method and application thereof |
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| EP1118584A1 (en) * | 2000-01-19 | 2001-07-25 | Oji Paper Co., Ltd. | Dispersion of silica particle agglomerates and process for producing the same |
| CN102390837A (en) * | 2011-08-03 | 2012-03-28 | 南通海迅天恒纳米科技有限公司 | Preparation method of nonspherical nanometer-scale silica sol |
| CN103896287A (en) * | 2012-12-28 | 2014-07-02 | 上海新安纳电子科技有限公司 | Non-spherical silicon dioxide sol and preparation method thereof |
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- 2019-10-23 CN CN201911012164.5A patent/CN110655087A/en active Pending
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| EP1118584A1 (en) * | 2000-01-19 | 2001-07-25 | Oji Paper Co., Ltd. | Dispersion of silica particle agglomerates and process for producing the same |
| CN102390837A (en) * | 2011-08-03 | 2012-03-28 | 南通海迅天恒纳米科技有限公司 | Preparation method of nonspherical nanometer-scale silica sol |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111269695A (en) * | 2020-02-29 | 2020-06-12 | 上海大学 | Peanut-shaped silicon oxide abrasive particles and preparation method and application thereof |
| CN113773806A (en) * | 2021-10-19 | 2021-12-10 | 广东惠尔特纳米科技有限公司 | Nano silicon dioxide abrasive material and preparation method and application thereof |
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