CN111303667A - Modification method of superfine composite silica micropowder for high-end copper-clad plate - Google Patents
Modification method of superfine composite silica micropowder for high-end copper-clad plate Download PDFInfo
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- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
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- 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
- C01B33/181—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by a dry process
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- C08L61/04—Condensation polymers of aldehydes or ketones with phenols only
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
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Abstract
The invention relates to a method for modifying superfine composite silica powder for a high-end copper-clad plate, which comprises the following steps: putting quartz fragments and quartz sand into a continuously operated ball mill according to the mass ratio of 5:1, wherein a grinding medium is an alumina ball; adjusting the induced air flux to be 1-1.5 ten thousand cubic meters per hour, and separating by a high-speed classifier to obtain large-particle silicon micro powder with non-uniform particle size distribution; sieving the coarse powder by a guarantee sieve to prepare 1-3 micron horn-shaped silicon micro powder coarse powder; step two, pouring 1-3 micron angular silicon micropowder coarse powder into a reaction vessel, igniting, melting and spheroidizing; selecting the spheroidized silicon micropowder, the amino triethoxysilane and the hexamethyldisilazane in the two steps according to the mass ratio of 1: 0.002-0.03: mixing the mixture with anhydrous chloroform in a ratio of 0.01, reacting for 4-24 hours at 100-130 ℃, cooling, centrifuging, and drying in vacuum to obtain the modified superfine silicon powder. The invention effectively enhances the compatibility of the silicon micropowder and the phenolic resin in the processing process of the copper-clad plate.
Description
Technical Field
The invention belongs to the field of materials for manufacturing integrated circuits, and particularly relates to a modification method of superfine composite silicon powder for a high-end copper-clad plate.
Background
With more and more electronic information products in China gradually being in the front of the world, the integrated circuit market in China is continuously increased, the composite silicon micropowder is used as an important epoxy molding compound filler for packaging the integrated circuit, the composite silicon micropowder has huge market space, and the market demand of the silicon micropowder for the copper-clad plate at present is increased at the speed of 15-20% every year.
The silicon micropowder for the copper-clad plate in the prior art has the following problems: silica powder is an inorganic filler, and has poor compatibility with organic polymer resin and is difficult to disperse when being mixed for use, so that the heat resistance and the moisture resistance of materials such as integrated circuit packages, substrates and the like filled with the traditional silica powder are poor, and the reliability and the stability of products are influenced.
Aiming at the problems, the invention provides a modification method of superfine composite silica powder for a high-end copper-clad plate, and the scheme is generated by the method.
Disclosure of Invention
The invention aims to provide a modification method of superfine composite silica powder for a high-end copper-clad plate, so that the compatibility of the silica powder and phenolic resin is effectively enhanced in the processing process of the copper-clad plate.
In order to achieve the purpose, the invention specifically provides the following technical scheme: a modification method of superfine composite silica powder for a high-end copper-clad plate comprises the following steps: putting quartz fragments and quartz sand into a continuously operated ball mill according to the mass ratio of 5:1, wherein a grinding medium is an alumina ball; adjusting the induced air flux to be 1-1.5 ten thousand cubic meters per hour, and separating by a high-speed classifier to obtain large-particle silicon micro powder with non-uniform particle size distribution; sieving the coarse powder by a guarantee sieve to prepare 1-3 micron angular silica micropowder coarse powder with D100 less than 10 microns;
step two, pouring 1-3 micron angular silicon micropowder coarse powder into a reaction vessel, igniting, melting and spheroidizing;
selecting the spheroidized silicon micropowder, the amino triethoxysilane and the hexamethyldisilazane in the two steps according to the mass ratio of 1: 0.002-0.03: mixing the mixture with anhydrous chloroform in a ratio of 0.01, reacting for 4-24 hours at 100-130 ℃, cooling, centrifuging, and drying in vacuum to obtain the modified superfine silicon powder.
Further, the diameter of the quartz sand is 0.4-0.6 mm. Further, SiO of the quartz chips2The content is higher than 99%. Further, the guarantee sieve is 90-160 microns. Further, the reaction container is filled with a mixed gas of natural gas and oxygen. Further, after cooling, centrifugal separation, chloroform washing for 3 times, and vacuum drying at 60 ℃ for 12 hours to prepare the modified superfine silicon powder.
The principle of the invention is as follows: in the aspect of the processing performance of the silicon micropowder, in order to improve the problem of interface bonding between the silicon micropowder and an organic polymer material and improve the application performance of the silicon micropowder, the surface modification of the silicon micropowder is generally required. The silane coupling agent can improve the lipophilicity of the surface of the silicon micropowder and is the most commonly used silicon micropowder surface modifier. In addition, the silane coupling agent can also improve the wettability of the high polymer material on the surface of the silicon micropowder, and the high polymer material and the silicon micropowder filler are firmly combined through a covalent bond through a functional group reaction, so that the performance of the copper-clad plate is improved. However, the products produced by the conventional silane coupling agent modification method do not achieve the ideal effect, and the main reasons are that the structure and the performance of the silane coupling agent are not clear, the understanding of the action mechanism of the silane coupling agent and the silica micropowder is not thorough, and the matching with downstream products is not fully considered. The invention aims to solve the technical problem of the prior art and provides a surface modification method for silica powder for phenolic aldehyde copper-clad plate filler. The compatibility of the silicon micropowder and the phenolic resin is effectively enhanced in the processing process of the copper-clad plate, so that the expansion coefficient, hydrophobicity and water absorption of the finished copper-clad plate are effectively reduced and the heat resistance and toughness of the plate are improved in the application process of the finished copper-clad plate.
Compared with the prior art, the invention has the following effects:
(1) after the surface of the superfine silicon powder is subjected to alkylation modification, the compatibility with several shifts is improved, and the increase of the filling amount of the silicon powder is realized.
(2) The finished copper clad laminate effectively reduces the expansion coefficient, hydrophobicity and water absorption and improves the heat resistance and toughness of the board in the application process, thereby improving the use reliability of the circuit substrate and reducing the cost.
(3) The spherical silicon micropowder is prepared by melting treatment, and the composite interface effect is enhanced.
(4) Methyl is introduced on the surface of the silicon micro powder through surface modification, and when the silicon micro powder is used as a filler, the silicon micro powder has better compatibility with resin; the modified amino can be better combined with phenolic resin, and the toughness and the strength of the circuit substrate are improved.
(5) The method is green and environment-friendly in the process of producing the superfine silicon powder, and has no secondary pollution.
Drawings
FIG. 1 is a scanning electron microscope photograph of a modified ultrafine silica powder prepared in example four; FIG. 2 is a scanning electron microscope photograph of the modified ultrafine silica powder prepared in example six.
Detailed Description
The following embodiments are described in detail to illustrate the technical solutions of the present invention, and the following embodiments are only used to illustrate the technical solutions of the present invention more clearly, and the protection scope of the present invention is not limited thereby.
The first embodiment is as follows:
(1) mixing SiO2The quartz chips with the content of more than 99 percent and the quartz sand with the thickness of about 0.5 mm are put into a continuously operating ball mill according to the mass ratio of 5:1, and the grinding medium is alumina balls (0.1-1.0 mm). Adjusting the induced air flux to about 1.5 ten thousand cubic meters per hour, and separating by a high-speed classifier to obtain large-particle silicon micro powder with non-uniform particle size distribution. Sieving with a 150-micron sieve to obtain 1-3-micron coarse angular silica powder D100<10 microns.
(2) Pouring 1-3 micron angular silicon micropowder coarse powder into a reaction vessel filled with a mixed gas of natural gas and oxygen, and igniting, melting and spheroidizing.
(3) Selecting 2 steps of spheroidized silicon micropowder, 4-aminobutyltriethoxysilane and hexamethyldisilazane according to the mass ratio of 1: 0.002: mixing with anhydrous chloroform at a ratio of 0.01, reacting at 100 deg.C for 12 hr, cooling, centrifuging, washing with chloroform for 3 times, and vacuum drying at 60 deg.C for 12 hr to obtain modified superfine silicon powder.
Example two:
(1) mixing SiO2The quartz chips with the content of more than 99 percent and the quartz sand with the thickness of about 0.5 mm are put into a continuously operating ball mill according to the mass ratio of 5:1, and the grinding medium is alumina balls (0.1-1.0 mm). Adjusting the induced air flux to be about 1 ten thousand cubic meters per hour, and separating by a high-speed classifier to obtain large-particle silicon micro powder with non-uniform particle size distribution. Sieving with a 100-micron sieve to obtain 1-3 micron coarse powder of angle-type silicon micropowder D100<10 microns.
(2) Pouring 1-3 micron angular silicon micropowder coarse powder into a reaction vessel filled with a mixed gas of natural gas and oxygen, and igniting, melting and spheroidizing.
(3) Selecting the spheroidized silicon powder, 3-aminopropyl triethoxysilane and hexamethyldisilazane in the step 2 according to the mass ratio of 1: 0.01: mixing with anhydrous chloroform at a ratio of 0.01, reacting at 120 deg.C for 12 hr, cooling, centrifuging, washing with chloroform for 3 times, and vacuum drying at 60 deg.C for 12 hr to obtain modified superfine silicon powder.
Example three:
(1) mixing SiO2The quartz chips with the content of more than 99 percent and the quartz sand with the thickness of about 0.5 mm are put into a continuously operating ball mill according to the mass ratio of 5:1, and the grinding medium is alumina balls (0.1-1.0 mm). Adjusting the induced air flux to about 1.2 ten thousand cubic meters per hour, and separating by a high-speed classifier to obtain large-particle silicon micro powder with non-uniform particle size distribution. Sieving with a 130-micron sieve to obtain 1-3-micron coarse angular silicon powder D100<10 microns.
(2) Pouring 1-3 micron angular silicon micropowder coarse powder into a reaction vessel filled with a mixed gas of natural gas and oxygen, and igniting, melting and spheroidizing.
(3) Selecting the spheroidized silicon micropowder, 6-aminohexyltriethoxysilane and hexamethyldisilazane in the step 2 according to the mass ratio of 1: 0.03: mixing with anhydrous chloroform at a ratio of 0.01, reacting at 130 deg.C for 4 hr, cooling, centrifuging, washing with chloroform for 3 times, and vacuum drying at 60 deg.C for 12 hr to obtain modified superfine silicon powder.
With reference to fig. 1, the fourth embodiment:
(1) mixing SiO2Adding quartz chips with the content higher than 99% and quartz sand with the content of about 0.5 mm into the mixture according to the mass ratio of 5:1The ball mill is continuously operated, and the grinding medium is alumina balls (0.1-1.0 mm). Adjusting the induced air flux to about 1.5 ten thousand cubic meters per hour, and separating by a high-speed classifier to obtain large-particle silicon micro powder with non-uniform particle size distribution. Sieving with a 150-micron sieve to obtain 1-3-micron coarse angular silica powder D100<10 microns.
(2) Pouring 1-3 micron angular silicon micropowder coarse powder into a reaction vessel filled with a mixed gas of natural gas and oxygen, and igniting, melting and spheroidizing.
(3) Selecting the spheroidized silicon powder, 4-aminobutyltriethoxysilane and hexamethyldisilazane in the step 2 according to the mass ratio of 1: 0.008: mixing with anhydrous chloroform at a ratio of 0.01, reacting at 110 deg.C for 8 hr, cooling, centrifuging, washing with chloroform for 3 times, and vacuum drying at 60 deg.C for 12 hr to obtain modified superfine silicon powder.
Example five:
(1) mixing SiO2The quartz chips with the content of more than 99 percent and the quartz sand with the thickness of about 0.5 mm are put into a continuously operating ball mill according to the mass ratio of 5:1, and the grinding medium is alumina balls (0.1-1.0 mm). Adjusting the induced air flux to be about 1 ten thousand cubic meters per hour, and separating by a high-speed classifier to obtain large-particle silicon micro powder with non-uniform particle size distribution. Sieving with a 150-micron sieve to obtain 1-3-micron coarse angular silica powder D100<10 microns.
(2) Pouring 1-3 micron angular silicon micropowder coarse powder into a reaction vessel filled with a mixed gas of natural gas and oxygen, and igniting, melting and spheroidizing.
(3) Selecting the spheroidized silicon powder, 5-aminopentyltriethoxysilane and hexamethyldisilazane in the step 2 according to the mass ratio of 1: 0.02: mixing with anhydrous chloroform at a ratio of 0.01, reacting at 100 deg.C for 24 hr, cooling, centrifuging, washing with chloroform for 3 times, and vacuum drying at 60 deg.C for 12 hr to obtain modified superfine silicon powder.
In conjunction with fig. 2, example six:
(1) mixing SiO2The quartz chips with the content of more than 99 percent and the quartz sand with the thickness of about 0.5 mm are put into a continuously operating ball mill according to the mass ratio of 5:1, and the grinding medium is alumina balls (0.1-1.0 mm). Adjusting induced draft flux at about 1.2 million cubic meters per hour, passing through a high speed classifierSeparating to obtain large-particle silicon micropowder with non-uniform particle size distribution. Sieving with a 150-micron sieve to obtain 1-3-micron coarse angular silica powder D100<10 microns.
(2) Pouring 1-3 micron angular silicon micropowder coarse powder into a reaction vessel filled with a mixed gas of natural gas and oxygen, and igniting, melting and spheroidizing.
(3) Selecting the spheroidized silicon powder, 4-aminobutyltriethoxysilane and hexamethyldisilazane in the step 2 according to the mass ratio of 1: 0.01: mixing with anhydrous chloroform at a ratio of 0.01, reacting at 115 deg.C for 16 hr, cooling, centrifuging, washing with chloroform for 3 times, and vacuum drying at 60 deg.C for 12 hr to obtain modified superfine silicon powder.
Application of the results of the experiments
Evaluation system: 150 ℃ phenolic aldehyde curing system
The addition amount of the filler is as follows: 35 percent of
TABLE 1 comparison of the overall Properties of the sheets
From the test results, the products of examples two and four are excellent in stability, dielectric properties, strength and other properties.
Through detection and test, the modified silica micropowder produced by the method provided by the invention can effectively enhance the compatibility of the silica micropowder and phenolic resin in the processing process of the copper-clad plate, so that the expansion coefficient, hydrophobicity and water absorption of the finished copper-clad plate can be effectively reduced in the application process, the heat resistance and toughness of the plate can be improved, the use stability of the plate can be further improved, and the cost can be reduced.
Claims (6)
1. A modification method of superfine composite silica powder for a high-end copper-clad plate is characterized by comprising the following steps: putting quartz fragments and quartz sand into a continuously operated ball mill according to the mass ratio of 5:1, wherein a grinding medium is an alumina ball; adjusting the induced air flux to be 1-1.5 ten thousand cubic meters per hour, and separating by a high-speed classifier to obtain large-particle silicon micro powder with non-uniform particle size distribution; sieving the coarse powder by a guarantee sieve to prepare 1-3 micron angular silica micropowder coarse powder with D100 less than 10 microns;
step two, pouring 1-3 micron angular silicon micropowder coarse powder into a reaction vessel, igniting, melting and spheroidizing;
selecting the spheroidized silicon micropowder, the amino triethoxysilane and the hexamethyldisilazane in the two steps according to the mass ratio of 1: 0.002-0.03: mixing the mixture with anhydrous chloroform in a ratio of 0.01, reacting for 4-24 hours at 100-130 ℃, cooling, centrifuging, and drying in vacuum to obtain the modified superfine silicon powder.
2. The method for modifying the superfine composite silica powder for the high-end copper-clad plate according to claim 1, which is characterized in that: the diameter of the quartz sand is 0.4-0.6 mm.
3. The method for modifying the superfine composite silica powder for the high-end copper-clad plate according to claim 1, which is characterized in that: SiO of the quartz chips2The content is higher than 99%.
4. The method for modifying the superfine composite silica powder for the high-end copper-clad plate according to claim 1, which is characterized in that: the guarantee sieve is 90-160 microns.
5. The method for modifying the superfine composite silica powder for the high-end copper-clad plate according to claim 1, which is characterized in that: the reaction vessel is filled with a mixed gas of natural gas and oxygen.
6. The method for modifying the superfine composite silica powder for the high-end copper-clad plate according to claim 1, which is characterized in that: cooling, centrifuging, washing with chloroform for 3 times, and vacuum drying at 60 deg.C for 12 hr to obtain modified superfine silicon powder.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114874644A (en) * | 2022-04-21 | 2022-08-09 | 吉安豫顺新材料有限公司 | Preparation method of coated spherical silicon micro powder |
| WO2023020222A1 (en) * | 2021-08-16 | 2023-02-23 | 广东生益科技股份有限公司 | Resin composition and use thereof |
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|---|---|---|---|---|
| CN101280125A (en) * | 2008-05-27 | 2008-10-08 | 阮建军 | Production method of superfine silicon powder for electronic grade low-heat expansion coefficient copper clad laminate |
| CN103613956A (en) * | 2013-11-25 | 2014-03-05 | 连云港东海硅微粉有限责任公司 | Preparation method of mechanochemical modified silica micropowder |
| CN106255315A (en) * | 2016-07-28 | 2016-12-21 | 江苏联瑞新材料股份有限公司 | A kind of preparation method of ic substrate electron level superfine composite silicon powder |
| CN108083286A (en) * | 2018-01-05 | 2018-05-29 | 江苏联瑞新材料股份有限公司 | A kind of preparing spherical SiO 2 micro mist and its preparation method and application |
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2020
- 2020-02-21 CN CN202010107841.8A patent/CN111303667A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101280125A (en) * | 2008-05-27 | 2008-10-08 | 阮建军 | Production method of superfine silicon powder for electronic grade low-heat expansion coefficient copper clad laminate |
| CN103613956A (en) * | 2013-11-25 | 2014-03-05 | 连云港东海硅微粉有限责任公司 | Preparation method of mechanochemical modified silica micropowder |
| CN106255315A (en) * | 2016-07-28 | 2016-12-21 | 江苏联瑞新材料股份有限公司 | A kind of preparation method of ic substrate electron level superfine composite silicon powder |
| CN108083286A (en) * | 2018-01-05 | 2018-05-29 | 江苏联瑞新材料股份有限公司 | A kind of preparing spherical SiO 2 micro mist and its preparation method and application |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2023020222A1 (en) * | 2021-08-16 | 2023-02-23 | 广东生益科技股份有限公司 | Resin composition and use thereof |
| CN114874644A (en) * | 2022-04-21 | 2022-08-09 | 吉安豫顺新材料有限公司 | Preparation method of coated spherical silicon micro powder |
| CN114874644B (en) * | 2022-04-21 | 2023-07-25 | 吉安豫顺新材料有限公司 | Preparation method of coated spherical silicon micropowder |
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Application publication date: 20200619 |