CN114918024A - Process method for grinding silicon micropowder by airflow - Google Patents
Process method for grinding silicon micropowder by airflow Download PDFInfo
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- CN114918024A CN114918024A CN202210400544.1A CN202210400544A CN114918024A CN 114918024 A CN114918024 A CN 114918024A CN 202210400544 A CN202210400544 A CN 202210400544A CN 114918024 A CN114918024 A CN 114918024A
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- grinding
- powder
- coarse powder
- silicon micropowder
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- 238000000227 grinding Methods 0.000 title claims abstract description 74
- 238000000034 method Methods 0.000 title claims abstract description 65
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 38
- 239000010703 silicon Substances 0.000 title claims abstract description 38
- 230000008569 process Effects 0.000 title claims abstract description 35
- 239000007788 liquid Substances 0.000 claims abstract description 30
- 239000000843 powder Substances 0.000 claims description 54
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000002245 particle Substances 0.000 claims description 16
- 239000011248 coating agent Substances 0.000 claims description 15
- 238000000576 coating method Methods 0.000 claims description 15
- 238000002360 preparation method Methods 0.000 claims description 11
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 8
- 239000005055 methyl trichlorosilane Substances 0.000 claims description 6
- JLUFWMXJHAVVNN-UHFFFAOYSA-N methyltrichlorosilane Chemical compound C[Si](Cl)(Cl)Cl JLUFWMXJHAVVNN-UHFFFAOYSA-N 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 4
- 229910000077 silane Inorganic materials 0.000 claims description 4
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 4
- 229920002554 vinyl polymer Polymers 0.000 claims description 4
- 238000004806 packaging method and process Methods 0.000 abstract description 4
- 230000002209 hydrophobic effect Effects 0.000 abstract description 3
- 238000005253 cladding Methods 0.000 abstract description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 11
- 239000000047 product Substances 0.000 description 8
- 239000000377 silicon dioxide Substances 0.000 description 5
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 4
- 239000011863 silicon-based powder Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 3
- ARGICNMLPHJXTP-UHFFFAOYSA-N [SiH4].C(=C)C(OC(CCC)=NO)C(COC(CCC)=O)OC(CCC)=O Chemical compound [SiH4].C(=C)C(OC(CCC)=NO)C(COC(CCC)=O)OC(CCC)=O ARGICNMLPHJXTP-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005008 domestic process Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- YOBAEOGBNPPUQV-UHFFFAOYSA-N iron;trihydrate Chemical compound O.O.O.[Fe].[Fe] YOBAEOGBNPPUQV-UHFFFAOYSA-N 0.000 description 1
- 238000010902 jet-milling Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000011044 quartzite Substances 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C19/00—Other disintegrating devices or methods
- B02C19/06—Jet mills
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C23/00—Auxiliary methods or auxiliary devices or accessories specially adapted for crushing or disintegrating not provided for in preceding groups or not specially adapted to apparatus covered by a single preceding group
- B02C23/18—Adding fluid, other than for crushing or disintegrating by fluid energy
-
- 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
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- 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
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
- C01P2006/65—Chroma (C*)
Abstract
The invention discloses a process method for air-flow grinding of silicon micropowder, which effectively improves the air-flow grinding efficiency by adding grinding aid liquid, and simultaneously improves the hydrophobic property of the silicon micropowder by adding cladding liquid, so that the silicon micropowder has better waterproof property when being applied in the fields of integrated circuit packaging, copper-clad plate bonding and the like.
Description
Technical Field
The invention relates to a production process of silicon micropowder, in particular to a process method for grinding the silicon micropowder by airflow.
Background
The silica powder is an inorganic material with wide application, has the characteristics of small heat conductivity coefficient, excellent dielectric property, small thermal expansion coefficient, corrosion resistance and the like, and has wide application in the fields of integrated circuit packaging, copper-clad plate bonding and the like.
At present, the domestic process for preparing the silicon micropowder mainly adopts dry ball milling, and other processes are less used. The air flow grinding has the advantages of large crushing strength, fine product granularity, narrow particle size distribution, more regular particle ball shape and the like, and has received more and more attention in the preparation process of the silicon micro powder.
Disclosure of Invention
The invention discloses a process method for grinding silicon micropowder by airflow, which effectively improves the efficiency of airflow grinding by adding grinding aid liquid, and simultaneously improves the hydrophobic property of the silicon micropowder by adding cladding liquid, so that the silicon micropowder has better waterproof property when applied to the fields of integrated circuit packaging, copper-clad plate bonding and the like.
A process method for grinding silicon micropowder by airflow comprises the following specific steps:
(1) coarse powder obtained by preliminary grinding;
(2) grinding the coarse powder in an air flow grinder, and adding grinding aid liquid accounting for 1-2% of the mass of the coarse powder when the grinding starts;
(3) continuously adding a coating liquid accounting for 0.3-0.5% of the mass of the coarse powder 0.5-1h before grinding, and humidifying the powder to ensure that the water content of the powder reaches 0.5-0.8%;
(4) continuously grinding to the target particle size to obtain the silicon micropowder prepared by the jet milling method.
Further, the step (4) is: continuously grinding to the target particle size, washing with pure water with the mass of 3-5 times of the powder, filtering, drying and re-dispersing to obtain the silicon micro powder.
Furthermore, the particle size of the coarse powder in the step (1) is 80-100 meshes.
Further, the preparation method of the grinding aid liquid in the step (2) comprises the following steps: mixing methyl trichlorosilane and vinyl tributyroximo silane according to the volume ratio of 1:4-5, then adding ethanol with the volume multiple of 8-10, and uniformly dispersing to obtain the product.
Further, the preparation method of the coating solution in the step (3) comprises the following steps: dissolving ethyl orthosilicate in ethanol with volume of 3-5 times, and dispersing uniformly to obtain the final product.
Further, the target particle size in the step (4) is 1 to 3 μm.
The invention has the advantages that:
1. according to the invention, the grinding aid liquid is added, so that the air flow grinding efficiency is effectively improved, and meanwhile, the coating liquid is added, so that the hydrophobic property of the silica powder is improved, and the silica powder has better waterproof property when being applied in the fields of integrated circuit packaging, copper-clad plate bonding and the like;
2. and (4) washing with pure water can effectively reduce the Fe content and effectively improve the whiteness of the silicon micro powder.
Detailed Description
Example 1
A process method for grinding silicon micropowder by air flow comprises the following steps:
(1) coarse powder obtained by preliminary grinding;
(2) grinding the coarse powder in an air flow grinder, and adding grinding aid liquid accounting for 1% of the mass of the coarse powder when grinding is started;
the preparation method of the grinding aid liquid comprises the following steps: mixing methyl trichlorosilane and vinyl tributyroximo silane according to the volume ratio of 1:5, then adding ethanol with the volume multiple of 10 times, and uniformly dispersing to obtain the product;
(3) continuously adding a coating liquid accounting for 0.3 percent of the mass of the coarse powder 0.5h before the grinding is finished, and humidifying the powder to ensure that the water content of the powder reaches 0.5 percent;
the preparation method of the coating solution in the step (3) comprises the following steps: dissolving tetraethoxysilane in ethanol with the volume 5 times that of the tetraethoxysilane, and uniformly dispersing to obtain the product;
(4) and continuously grinding to a target particle size, washing with pure water with the mass of 3 times that of the powder, and then filtering, drying and re-dispersing to obtain the silicon micro powder.
Example 2
A process method for grinding silicon micropowder by air flow comprises the following steps:
(1) coarse powder obtained by preliminary grinding;
(2) grinding the coarse powder in an air flow grinder, and adding grinding aid liquid accounting for 1.8% of the mass of the coarse powder when grinding is started;
the preparation method of the grinding aid liquid comprises the following steps: mixing methyl trichlorosilane and vinyl tributyroximo silane according to the volume ratio of 1:4, then adding ethanol with the volume multiple of 8, and uniformly dispersing to obtain the product;
(3) continuously adding a coating liquid with the mass of 0.4% of the coarse powder 1h before grinding is finished, and humidifying the powder to ensure that the water content of the powder reaches 0.6%;
the preparation method of the coating liquid comprises the following steps: dissolving tetraethoxysilane in ethanol with the volume of 4 times of that of the tetraethoxysilane, and uniformly dispersing to obtain the tetraethoxysilane;
(4) and continuously grinding to a target particle size, washing with pure water with the mass of 4 times that of the powder, and then filtering, drying and re-dispersing to obtain the silicon micro powder.
Example 3
A process method for grinding silicon micropowder by airflow comprises the following specific steps:
(1) coarse powder obtained by preliminary grinding;
(2) grinding the coarse powder in an air flow grinder, and adding grinding aid liquid accounting for 2% of the mass of the coarse powder when grinding is started;
the preparation method of the grinding aid liquid comprises the following steps: mixing methyl trichlorosilane and vinyl tributyrinoxime silane according to the volume ratio of 1:4, then adding ethanol with the volume multiple of 8, and uniformly dispersing to obtain the product;
(3) continuously adding a coating liquid accounting for 0.5 percent of the mass of the coarse powder 1 hour before the grinding is finished, and humidifying the powder to ensure that the water content of the powder reaches 0.8 percent;
the preparation method of the coating liquid comprises the following steps: dissolving tetraethoxysilane in 3 times of ethanol, and uniformly dispersing to obtain the product;
(4) continuously grinding the mixture to a target particle size, washing the mixture by pure water with the mass of 5 times of that of the powder, and then filtering, drying and re-dispersing the mixture to obtain the silicon micro powder.
Example 4
A process method for grinding silicon micropowder by airflow, which is characterized in that the step (4) in the process method is not washed by pure water, and comprises the following steps: (4) continuously grinding to a target particle size to obtain the silicon micropowder prepared by an air flow grinding method; the rest is the same as example 2.
Comparative example 1
A process method for grinding silicon micropowder by air current is characterized in that grinding aid and coating liquid are not added in the process method, and the silicon micropowder is directly ground to a target particle size by an air current grinding machine.
Comparative example 2
A process method for grinding silicon micropowder by air flow, which is the same as the process method in the example 2 except that grinding aid liquid is not added.
Comparative example 3
A process for air-milling fine silica powder, which is the same as example 2 except that no coating liquid is added and no humidification is performed.
Comparative example 4
The process method for grinding the silicon micropowder by air flow is the same as the process method in the embodiment 2 except that the coating liquid is not added and then the silicon micropowder is not humidified.
Comparative example 5
The process method for grinding the silicon micropowder by using the airflow is the same as the process method in the example 2, wherein the grinding aid liquid is not added with methyltrichlorosilane.
Comparative example 6
The process method for grinding the silicon micropowder by using the airflow is the same as that in the example 2 except that vinyl tributyrinoxime silane is not added into the grinding aid liquid.
Comparative example 7
A process method for grinding silicon micropowder by air flow is provided, wherein grinding aid and coating liquid are added at the same time when the grinding in the step (2) is started, and the rest is the same as that in the example 2.
Detection and analysis:
using the coarse powder of 100 mesh obtained by coarse grinding of the same raw material as a raw material, the coarse powder of equal weight was processed by the above-described processes of examples and comparative examples to prepare a fine silicon powder having a target particle size of 2.5. mu.m.
1. Grinding time: calculating the time (min) required by grinding each process method to the target particle size;
2. water absorption performance: taking the silicon micro powder prepared by the process method in the embodiment and the comparative example, putting the silicon micro powder into a beaker, adding excessive water, immersing for 5min, and then discharging excessive water; weighing the silicon powder after water absorption (W), then putting the silicon powder into a drying oven at 120 ℃ for drying, weighing the silicon powder again after drying, and calculating the saturated water absorption rate (%);
saturated water absorption (W/W-1) × 100%
3. Whiteness degree: according to GB/T5950-2008 "whiteness measurement method of building materials and nonmetallic mineral products", whiteness (%) of the silicon fine powder prepared by the process method in the above examples and comparative examples is measured by a whiteness meter;
4. content of iron oxide: the content (ppm) of iron oxide in the fine silica powder obtained by the process described in the above examples and comparative examples was measured according to the test method of SN/T0483-1995, part 3.4 of methods for measuring the amount of iron sesquioxide in import and export quartzite (sand) chemical analysis.
And finally: the above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (6)
1. A process method for grinding silicon micropowder by air flow is characterized in that: the process method comprises the following specific steps:
(1) coarse powder obtained by preliminary grinding;
(2) grinding the coarse powder in an air flow grinder, and adding grinding aid liquid accounting for 1-2% of the mass of the coarse powder when grinding is started;
(3) continuously adding a coating liquid accounting for 0.3-0.5% of the mass of the coarse powder 0.5-1h before grinding, and humidifying the powder to ensure that the water content of the powder reaches 0.5-0.8%;
(4) continuously grinding to the target particle size to obtain the silicon micropowder prepared by the air flow grinding method.
2. The process according to claim 1, characterized in that: the step (4) is as follows: continuously grinding to a target particle size, washing with pure water with the mass of 3-5 times of that of the powder, and then filtering, drying and re-dispersing to obtain the silicon micro powder.
3. The process according to claim 1 or 2, characterized in that: the grain diameter of the coarse powder in the step (1) is 80-100 meshes.
4. The process according to claim 1 or 2, characterized in that: the preparation method of the grinding aid liquid in the step (2) comprises the following steps: mixing methyl trichlorosilane and vinyl tributyroximo silane according to the volume ratio of 1:4-5, then adding ethanol with the volume multiple of 8-10, and uniformly dispersing to obtain the product.
5. The process according to claim 1 or 2, characterized in that: the preparation method of the coating solution in the step (3) comprises the following steps: dissolving tetraethoxysilane in ethanol with the volume of 3-5 times of that of the tetraethoxysilane, and uniformly dispersing to obtain the product.
6. The process according to claim 1 or 2, characterized in that: the target particle size in the step (4) is 1-3 μm.
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