CN112194144A - Preparation method of spherical silicon micropowder - Google Patents
Preparation method of spherical silicon micropowder Download PDFInfo
- Publication number
- CN112194144A CN112194144A CN202010952064.7A CN202010952064A CN112194144A CN 112194144 A CN112194144 A CN 112194144A CN 202010952064 A CN202010952064 A CN 202010952064A CN 112194144 A CN112194144 A CN 112194144A
- Authority
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- China
- Prior art keywords
- silicon oxide
- oxide slurry
- nano silicon
- spray tower
- spherical
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 10
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 10
- 239000010703 silicon Substances 0.000 title claims abstract description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 68
- 229910052814 silicon oxide Inorganic materials 0.000 claims abstract description 49
- 239000002002 slurry Substances 0.000 claims abstract description 41
- 239000007921 spray Substances 0.000 claims abstract description 34
- 238000001035 drying Methods 0.000 claims abstract description 28
- 239000005543 nano-size silicon particle Substances 0.000 claims abstract description 27
- 239000007788 liquid Substances 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 11
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 9
- 239000007864 aqueous solution Substances 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims description 20
- 229920000642 polymer Polymers 0.000 claims description 12
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 7
- 238000001354 calcination Methods 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 238000004806 packaging method and process Methods 0.000 abstract description 6
- 238000001694 spray drying Methods 0.000 abstract description 3
- 238000011065 in-situ storage Methods 0.000 abstract description 2
- 239000002245 particle Substances 0.000 abstract description 2
- 235000012239 silicon dioxide Nutrition 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 229920002521 macromolecule Polymers 0.000 abstract 2
- 239000012798 spherical particle Substances 0.000 description 8
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The invention discloses a preparation method of spherical silicon micropowder, which comprises the steps of taking a certain amount of nano silicon oxide aqueous solution, adjusting the nano silicon oxide aqueous solution to nano silicon oxide slurry, adding 0.1-50 parts of macromolecule A and 0.1-10 parts of macromolecule B into the nano silicon oxide slurry, stirring and mixing uniformly to form uniform mixed silicon oxide slurry, feeding the mixed silicon oxide slurry into a drying spray tower to obtain spherical liquid drops, the process improves the physical curing process of the traditional spray drying spheroidization, provides a process combining chemical in-situ curing and physical curing, and the prepared spherical silicon dioxide particles have high sphericity rate, high sphericity, good fluidity, compact structure, high purity and smooth surface, and can meet the requirement of large-scale integrated circuit packaging.
Description
Chinese patent CN200610038823.9 describes a process for preparing spherical silica powder, which comprises spray drying silica sol to obtain microspherical silica gel, performing flame heat treatment, and performing secondary spheroidization to obtain high-purity spherical silica powder.
Disclosure of Invention
The invention aims to provide a preparation method of spherical silicon micropowder so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of spherical silicon micropowder comprises the following steps:
s1, taking 10-500 parts of nano silicon oxide aqueous solution, adjusting the solid content of the nano silicon oxide aqueous solution to 5-80%, and adjusting the pH value to 1-10 to obtain nano silicon oxide slurry A;
s2, adding 0.1-50 parts of polymer A and 0.1-10 parts of polymer B into the nano silicon oxide slurry A, and stirring and mixing uniformly to form uniform mixed silicon oxide slurry;
s3, feeding the prepared mixed silicon oxide slurry into a drying spray tower, atomizing the mixed silicon oxide slurry into spherical liquid drops, and further solidifying the spherical liquid drops to obtain powder;
and S4, calcining the powder in a furnace body, and removing moisture and organic matters in the powder.
Further, the silicon oxide aqueous solution comprises at least one of silica sol, nano silicon oxide slurry B and a mixture of the silica sol and the nano silicon oxide slurry B.
Further, the rotating speed of a centrifugal spray disk of the drying spray tower is 200-1000r/min, and the output pressure of a pressure nozzle of the drying spray tower is 0.1-1 MPa.
Furthermore, the inlet air temperature of the drying spray tower is 80-300 ℃, and the outlet air temperature is 60-250 ℃.
Furthermore, the furnace body is at least one of a kiln furnace, a box furnace, a tunnel furnace and a roller furnace.
Further, in step S4, the furnace body is in 8-36h and the temperature inside the furnace body is raised to 1300 ℃ of 300 and kept for 1-12 h.
Compared with the prior art, the invention has the beneficial effects that:
the process improves the physical curing process of the traditional spray drying spheroidization, provides a process combining chemical in-situ curing and physical curing, has high sphericity rate, high sphericity, good fluidity, compact structure, high purity and smooth surface of the prepared spherical silicon dioxide particles, and can meet the requirement of large-scale integrated circuit packaging.
In addition to the objects, features and advantages described above, other objects, features and advantages of the present invention are also provided. The present invention will be described in further detail with reference to examples.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to 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 derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
the invention provides a technical scheme that: a preparation method of spherical silicon micropowder comprises the following steps: firstly, 10 parts of silica sol is taken, the solid content is adjusted to 25%, and the PH is adjusted to 1, so that nano silicon oxide slurry A is obtained;
then adding 0.1 part of polymer A and 0.1 part of polymer B into the nano silicon oxide slurry A, and stirring and mixing uniformly to form uniform mixed silicon oxide slurry;
then, the prepared mixed silicon oxide slurry is sent into a drying spray tower, the rotating speed of a centrifugal spray disk of the drying spray tower is 200r/min, the output pressure of a pressure nozzle of the drying spray tower is 0.1Mpa, the air inlet temperature of the drying spray tower is 80 ℃, the air outlet temperature of the drying spray tower is 60 ℃, the mixed silicon oxide slurry is atomized into spherical liquid drops, and the spherical liquid drops are further solidified to obtain powder;
and finally, calcining the powder in a kiln, slowly raising the internal temperature of the kiln to 300 ℃ in 8 hours, and preserving heat for 1 hour, so that moisture and organic matters in the powder are removed, the spherical particles are densified, the sphericity rate of the spherical particles is higher than 85%, the sphericity is high, the flowability is good, the structure is compact, the purity is high, the surface is smooth, and the requirement of large-scale integrated circuit packaging can be met.
Example 2:
the invention provides a technical scheme that: a preparation method of spherical silicon micropowder comprises the following steps: firstly, 50 parts of nano silicon oxide slurry B is taken, the solid content is adjusted to 5%, and the PH is adjusted to 3, so that nano silicon oxide slurry A is obtained;
then adding 1 part of polymer A and 0.4 part of polymer B into the nano silicon oxide slurry A, and stirring and mixing uniformly to form uniform mixed silicon oxide slurry;
then, the prepared mixed silicon oxide slurry is sent into a drying spray tower, the rotating speed of a centrifugal spray disk of the drying spray tower is 500r/min, the output pressure of a pressure nozzle of the drying spray tower is 0.4Mpa, the air inlet temperature of the drying spray tower is 120 ℃, the air outlet temperature of the drying spray tower is 150 ℃, the mixed silicon oxide slurry is atomized into spherical liquid drops, and the spherical liquid drops are further solidified to obtain powder;
and finally, calcining the powder in a box type furnace, slowly raising the temperature of the inside of the furnace to 600 ℃ in 12 hours, and preserving the heat for 2 hours, thereby removing the moisture and organic matters in the powder, and densifying the spherical particles, so that the sphericity ratio of the spherical particles is higher than 70%, the sphericity is high, the fluidity is good, the structure is compact, the purity is high, the surface is smooth, and the requirement of large-scale integrated circuit packaging can be met.
Example 3:
the invention provides a technical scheme that: a preparation method of spherical silicon micropowder comprises the following steps: firstly, taking 100 parts of a mixture of silica sol and the nano silicon oxide slurry B, adjusting the solid content of the mixture to 40%, and adjusting the PH value of the mixture to 6 to obtain nano silicon oxide slurry A;
then adding 10 parts of polymer A and 5 parts of polymer B into the nano silicon oxide slurry A, and stirring and mixing uniformly to form uniform mixed silicon oxide slurry;
then, the prepared mixed silicon oxide slurry is sent into a drying spray tower, the rotating speed of a centrifugal spray disk of the drying spray tower is 800r/min, the output pressure of a pressure nozzle of the drying spray tower is 0.8Mpa, the air inlet temperature of the drying spray tower is 200 ℃, the air outlet temperature of the drying spray tower is 200 ℃, the mixed silicon oxide slurry is atomized into spherical liquid drops, and the spherical liquid drops are further solidified to obtain powder;
and finally, calcining the powder in a kiln, slowly raising the internal temperature of the kiln to 800 ℃ in 24 hours, and preserving heat for 8 hours, so that moisture and organic matters in the powder are removed, the spherical particles are densified, the sphericity rate of the spherical particles is higher than 90%, the sphericity degree is high, the flowability is good, the structure is compact, the purity is high, the surface is smooth, and the requirement of large-scale integrated circuit packaging can be met.
Example 4:
the invention provides a technical scheme that: a preparation method of spherical silicon micropowder comprises the following steps: firstly, taking a mixture of 500 parts of silica sol and the nano silicon oxide slurry B, adjusting the solid content of the mixture to 80%, and adjusting the PH to 10 to obtain nano silicon oxide slurry A;
then adding 50 parts of polymer A and 10 parts of polymer B into the nano silicon oxide slurry A, and stirring and mixing uniformly to form uniform mixed silicon oxide slurry;
then, the prepared mixed silicon oxide slurry is sent into a drying spray tower, the rotating speed of a centrifugal spray disk of the drying spray tower is 1000r/min, the output pressure of a pressure nozzle of the drying spray tower is 1Mpa, the air inlet temperature of the drying spray tower is 300 ℃, the air outlet temperature is 250 ℃, the mixed silicon oxide slurry is atomized into spherical liquid drops, and the spherical liquid drops are further solidified to obtain powder;
and finally, calcining the powder in a kiln, slowly raising the internal temperature of the kiln to 1300 ℃ in 36 hours, and preserving the heat for 12 hours, thereby removing the moisture and organic matters in the powder, and densifying the spherical particles, so that the sphericity ratio of the spherical particles is higher than 95%, the sphericity is high, the fluidity is good, the structure is compact, the purity is high, the surface is smooth, and the requirement of large-scale integrated circuit packaging can be met.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (6)
1. The preparation method of the spherical silicon micropowder is characterized by comprising the following steps:
s1, taking 10-500 parts of nano silicon oxide aqueous solution, adjusting the solid content of the nano silicon oxide aqueous solution to 5-80%, and adjusting the pH value to 1-10 to obtain nano silicon oxide slurry A;
s2, adding 0.1-50 parts of polymer A and 0.1-10 parts of polymer B into the nano silicon oxide slurry A, and stirring and mixing uniformly to form uniform mixed silicon oxide slurry;
s3, feeding the prepared mixed silicon oxide slurry into a drying spray tower, atomizing the mixed silicon oxide slurry into spherical liquid drops, and further solidifying the spherical liquid drops to obtain powder;
and S4, calcining the powder in a furnace body, and removing moisture and organic matters in the powder.
2. The method for preparing spherical silica micropowder according to claim 1, characterized by comprising: the silicon oxide aqueous solution at least comprises one of silica sol, nano silicon oxide slurry B and a mixture of the silica sol and the nano silicon oxide slurry B.
3. The method for preparing spherical silica micropowder according to claim 1, characterized by comprising: the rotating speed of a centrifugal spray disk of the drying spray tower is 200-1000r/min, and the output pressure of a pressure nozzle of the drying spray tower is 0.1-1 Mpa.
4. The method for preparing spherical silica micropowder according to claim 1 or 3, characterized in that: the inlet air temperature of the drying spray tower is 80-300 ℃, and the outlet air temperature is 60-250 ℃.
5. The method for preparing spherical silica micropowder according to claim 1, characterized by comprising: the furnace body is at least one of a kiln furnace, a box furnace, a tunnel furnace and a roller furnace.
6. The method for preparing spherical silica micropowder according to claim 1, characterized by comprising: in step S4, the furnace body is in 8-36h and the temperature inside the furnace body is raised to 1300 ℃ of 300-.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010952064.7A CN112194144A (en) | 2020-09-11 | 2020-09-11 | Preparation method of spherical silicon micropowder |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010952064.7A CN112194144A (en) | 2020-09-11 | 2020-09-11 | Preparation method of spherical silicon micropowder |
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| Publication Number | Publication Date |
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| CN112194144A true CN112194144A (en) | 2021-01-08 |
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| CN202010952064.7A Pending CN112194144A (en) | 2020-09-11 | 2020-09-11 | Preparation method of spherical silicon micropowder |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112978740A (en) * | 2021-03-23 | 2021-06-18 | 江苏联瑞新材料股份有限公司 | Preparation method of submicron spherical silicon dioxide micropowder |
| CN115368754A (en) * | 2022-08-12 | 2022-11-22 | 吉安豫顺新材料有限公司 | Spherical low-density silica filler |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6451862B1 (en) * | 1999-11-05 | 2002-09-17 | Asahi Glass Company, Limited | Process for producing a spherical silica gel |
| CN101037206A (en) * | 2006-03-14 | 2007-09-19 | 连云港东海硅微粉有限责任公司 | Production method of high-purity ball-shaped silicon micro powder |
| CN105036146A (en) * | 2015-08-28 | 2015-11-11 | 北京理工大学 | Method for preparing spherical nanometer zirconium silicate powder |
| CN110015666A (en) * | 2019-04-29 | 2019-07-16 | 江苏辉迈粉体科技有限公司 | A kind of preparation method of high-purity Submicron spherical silica micropowder |
| CN110282633A (en) * | 2019-04-29 | 2019-09-27 | 江苏辉迈粉体科技有限公司 | A kind of method of modifying of nano oxidized silicon materials |
-
2020
- 2020-09-11 CN CN202010952064.7A patent/CN112194144A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6451862B1 (en) * | 1999-11-05 | 2002-09-17 | Asahi Glass Company, Limited | Process for producing a spherical silica gel |
| CN101037206A (en) * | 2006-03-14 | 2007-09-19 | 连云港东海硅微粉有限责任公司 | Production method of high-purity ball-shaped silicon micro powder |
| CN105036146A (en) * | 2015-08-28 | 2015-11-11 | 北京理工大学 | Method for preparing spherical nanometer zirconium silicate powder |
| CN110015666A (en) * | 2019-04-29 | 2019-07-16 | 江苏辉迈粉体科技有限公司 | A kind of preparation method of high-purity Submicron spherical silica micropowder |
| CN110282633A (en) * | 2019-04-29 | 2019-09-27 | 江苏辉迈粉体科技有限公司 | A kind of method of modifying of nano oxidized silicon materials |
Non-Patent Citations (1)
| Title |
|---|
| 李俊;蒋述兴;: "球形硅微粉的制备现状" * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112978740A (en) * | 2021-03-23 | 2021-06-18 | 江苏联瑞新材料股份有限公司 | Preparation method of submicron spherical silicon dioxide micropowder |
| CN112978740B (en) * | 2021-03-23 | 2023-11-21 | 江苏联瑞新材料股份有限公司 | Preparation method of submicron spherical silica micropowder |
| CN115368754A (en) * | 2022-08-12 | 2022-11-22 | 吉安豫顺新材料有限公司 | Spherical low-density silica filler |
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Application publication date: 20210108 |
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