CN110482867B - Low-dielectric glass microsphere for high-frequency high-speed copper-clad plate and preparation method thereof - Google Patents
Low-dielectric glass microsphere for high-frequency high-speed copper-clad plate and preparation method thereof Download PDFInfo
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- CN110482867B CN110482867B CN201910843577.1A CN201910843577A CN110482867B CN 110482867 B CN110482867 B CN 110482867B CN 201910843577 A CN201910843577 A CN 201910843577A CN 110482867 B CN110482867 B CN 110482867B
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- C—CHEMISTRY; METALLURGY
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- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
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Abstract
The invention provides a preparation method of low-dielectric glass microspheres for a high-frequency high-speed copper-clad plate, which comprises the following steps: weighing the following raw materials: 70-85% of SiO210 to 25% of B2O3、0.2～2％Al2O30.5 to 1% of TiO20.1-1% of ZnO and 0.2-1% of CaO, uniformly mixing, adding into a melting furnace for melting, and then quenching the molten glass with water; grinding and grading the water-quenched glass material; spheroidizing the classified glass powder in a balling furnace, and conveying the crushed and classified glass powder into the balling furnace of a flame burner in a gas conveying mode for spheroidizing; sorting is carried out by a classifier. The invention also provides the low dielectric glass microspheres for the high-frequency high-speed copper clad laminate, and the low dielectric glass microspheres for the high-frequency high-speed copper clad laminate prepared by the preparation method. The glass microsphere has the dielectric constant of 3.9-4.2 and the dielectric loss factor of 0.0020-0.0035 when the frequency is 10GHz, the particle size distribution is in different particle size ranges of 0.5-20 mu m, the sphericity is greater than or equal to 99 percent, and the requirement of the filler of the high-frequency and high-speed copper clad laminate for aviation can be met.
Description
Technical Field
The invention relates to an inorganic spherical filler, namely low dielectric glass microspheres, which is widely applied to the technical field of electronic circuit boards and the like, in particular to the field of high-frequency high-speed printed circuit boards; in particular to a low dielectric glass microsphere for a high-frequency high-speed copper-clad plate.
The invention also relates to a preparation method of the low-dielectric glass microspheres for the high-frequency high-speed copper-clad plate.
Background
With the rapid development of the new generation of internet, cloud planning technology and application, the requirements on large-scale data processing and data transmission speed are higher and higher, the frequency of signal processing and transmission is higher and higher, electronic information systems develop towards high frequency and high speed, and the new generation of high-speed routers, high-speed exchangers, communication base stations, high-end servers and the like in the market have great demands on copper clad plates of high-frequency and high-speed lines. The use frequency is upgraded from MHz to GHz frequency band, which promotes the rapid development of high frequency technology application, and the information transmission technology has begun to advance into the high frequency era. The copper-clad plate is used as one of main components of electronic products, is not simply used as a physical support any more, and the requirements of the future market for the copper-clad plate material are lead-free and halogen-free. And its function is required to be applicable to high frequencies. With the function of the copper clad laminate being increasingly explored and used in the electronic industry, the copper clad laminate has been integrated with other electronic devices to form a Printed Circuit Board (PCB), so the copper clad laminate is one of the key materials for improving the product performance of terminal manufacturers. The high frequency and high speed of electronic information products put higher requirements on the high frequency characteristics of the copper-clad plate, and the dielectric constant (Dk) and the loss factor (Df) of the electronic information products are two most important performance indexes concerned in the field of high frequency application.
At present, the copper-clad plate is mainly formed by compounding three materials of organic resin, inorganic glass fiber and inorganic filler, namely, the performance parameters of the copper-clad plate are the comprehensive expression of the three material performance parameters. The organic resin Dk used by the copper-clad plate is generally about 3.9, and the inorganic glass fiber Dk is generally 6.6, so that the inorganic filler used for preparing one of the key materials of the high-frequency high-speed copper-clad plate becomes a key material for adjusting the Dk and Df values of the copper-clad plate. By using the inorganic filler with ultralow Dk and Df values, the low Dk copper-clad plate suitable for high-frequency and high-speed application can be prepared, and the performances of the copper-clad plate such as thermal expansion coefficient, mechanical strength, thermal stability and the like can be improved.
At present, inorganic fillers used in domestic copper-clad plates mainly comprise fused silica powder, E-Glass powder, TFT-Glass powder and the like. The fused silica micropowder is the most main inorganic filler of the existing copper-clad plate, but the fused silica micropowder has high hardness and irregular surface appearance, and the properties bring a lot of difficulties to the preparation and later processing of the copper-clad plate, for example, when the copper-clad plate prepared by the materials is drilled, a drill bit is easy to damage, and the processing cost of the copper-clad plate is increased. Although the hardness of the E-Glass powder and the TFT-Glass powder is smaller than that of the fused silica powder, the dielectric constant (about 6.87 for the E-Glass powder and about 6.5 for the TFT-Glass powder) and the thermal expansion coefficient are large, and the high-performance high-frequency high-speed copper-clad plate is difficult to manufacture. As the inorganic filler is granular powder with irregular polygons, the uniform dispersion and high filling rate can not be realized in the preparation process of the copper-clad plate, so that the prepared copper-clad plate has low yield and high cost.
At present, inorganic filler with low dielectric constant, good mechanical property, chemical property, thermal property and high dispersion filling property is actively researched and developed at home and abroad to meet the performance requirement of the high-frequency high-speed copper-clad plate on the inorganic filler, but the market at home and abroad has no application of the high-performance product at present.
Disclosure of Invention
The invention aims to solve the technical problem of providing low-dielectric glass microspheres which are used for a high-frequency high-speed copper-clad plate and adopt inorganic fillers.
The invention also provides a preparation method of the low-dielectric glass microspheres for the high-frequency high-speed copper-clad plate.
In order to solve the technical problem, the invention provides a preparation method of low dielectric glass microspheres for a high-frequency high-speed copper-clad plate, which comprises the following steps:
a) weighing the following raw materials in percentage by weight:
70-85% of SiO2、10～25% of B2O3、0.2～2％Al2O30.5 to 1% of TiO20.1-1% of ZnO and 0.2-1% of CaO, and uniformly mixing the raw materials;
b) adding the uniformly mixed raw materials in the step a) into a melting furnace for melting, wherein the glass melting temperature is 1580-1650 ℃, and then quenching the melted glass liquid with water;
c) grinding and grading the water-quenched glass material, wherein the particle size of the glass powder is in different size fraction ranges of 0.5-20 mu m;
d) spheroidizing the graded glass powder in a balling furnace, and conveying the crushed and graded glass powder into a flame burner balling furnace for spheroidization in a gas conveying mode, wherein the flame spheroidization temperature is 1450-1500 ℃;
e) and collecting the spheroidized glass microspheres, and then sorting the glass microspheres by a classifier.
In the present invention, the melted glass liquid is water-quenched in the step b) to form a cullet having a size of 5mm or less.
Preferably, in the step c), the pulverizing and classifying is performed by using a jet milling and classifying device or a fine ball milling and pulverizing and classifying device.
Preferably, the spheroidized glass microspheres are collected in the step e) by using a cyclone collector and a bag collector.
The low dielectric glass microsphere prepared by the preparation method has the dielectric constant of 3.9-4.2 and the dielectric loss factor of 0.0020-0.0035 at the frequency of 10GHz, the particle size distribution is in different size ranges of 0.5-20 mu m, and the sphericity is larger than or equal to 99%. The high-dielectric-constant high-density high-frequency high-speed printed circuit board is suitable for industries with high requirements on dielectric constant and dielectric loss factor, such as high-frequency high-density, high-frequency high-speed circuit boards and the like, and provides a reliable high-quality product.
Wherein SiO is2、B2O3And Al2O3Is the main component of the microsphere of the invention and also forms the framework of the glass. At the same time B2O3Also acts as a cosolvent to reduce the viscosity of the glass and promote melting, Al2O3Improve the water resistance of the glass microspheres.
TiO2The present invention is effective for lowering the viscosity of glass to promote melting and lowering the dielectric loss of glass, but if the glass is too low in melting property, the dielectric loss is increased, whereas if the glass is too low in melting property, phase separation is easy and water resistance is poor, and the range of the most preferable selection in the present invention is 0.5 to 1%.
ZnO can improve the water resistance of the glass and reduce the dielectric constant, but the dielectric constant of the glass is increased when the ZnO content is higher than 3.2%, and the optimal selection range of the invention is 0.5-1%.
CaO mainly CaF2Introduced for fluxing, but in excess resulting in SiF4The generation of the CaO is not beneficial to the reduction of the dielectric constant, and the CaO is introduced to improve the chemical stability of the glass and adjust the viscosity, wherein the content of the CaO is not more than 1%.
In order to solve the technical problem, the invention also provides a low dielectric glass microsphere for the high-frequency high-speed copper-clad plate, which is characterized in that: the low-dielectric glass microspheres for the high-frequency high-speed copper-clad plate are prepared by the preparation method for the high-frequency high-speed copper-clad plate low-dielectric glass microspheres.
The low-dielectric-constant glass microspheres for the high-frequency and high-speed copper-clad plate have the dielectric constant of 3.9-4.2 and the dielectric loss factor of 0.0020-0.0035 when the frequency is 10GHz, the particle size distribution is in different size ranges of 0.5-20 mu m, the sphericity is not less than 99 percent, and the requirement of filler of the high-frequency and high-speed copper-clad plate for aviation can be met.
Drawings
FIG. 1 is an optical microscopic image with 100 times magnification of the embodiment of the low-dielectric glass microsphere for the high-frequency high-speed copper-clad plate
FIG. 2 is a 2000 times magnified scanning electron microscope image of the embodiment of the low-dielectric glass microsphere for the high-frequency high-speed copper-clad plate.
Detailed Description
Example one
The preparation method of the low dielectric glass microspheres for the high-frequency high-speed copper-clad plate comprises the following steps:
a) mixing materials: weighing the following raw materials in percentage by weight:
70% SiO225% of B2O3、2％Al2O31% of TiO21% of ZnO and 1% of CaO, and uniformly mixing the raw materials.
b) Melting and water quenching: adding the uniformly mixed raw materials in the step a) into a melting furnace for melting, wherein the glass melting temperature is 1580 ℃, and then quenching the melted glass liquid into cullet with the particle size of less than 5 mm.
c) Crushing and grading: grinding and grading the water-quenched glass material, wherein the grinding and grading adopt airflow grinding and grading equipment or fine ball grinding and grading equipment, and the particle size of the used glass powder is in different particle size ranges of 0.5-20 mu m.
d) Spheroidizing: spheroidizing the graded glass powder in a balling furnace, and conveying the crushed and graded glass powder into a flame burner balling furnace for spheroidizing in a gas conveying mode, wherein the flame spheroidizing temperature is 1450 ℃.
e) Collecting and sorting: collecting the spheroidized microspheres by using a cyclone collector and a cloth bag collector, and sorting the collected microsphere powder by using superfine precise sorting equipment according to requirements.
The shape of the sorted low dielectric glass microspheres for the high-frequency high-speed copper clad laminate is shown in figures 1 and 2, the particle size of the low dielectric glass microspheres for the high-frequency high-speed copper clad laminate is basically concentrated between 1 and 15 mu m, the dielectric constant is 4.1 when the frequency is 10GHz, the dielectric loss factor is 0.0030, the particle size is distributed in different size ranges of 1 to 15 mu m, and the sphericity is larger than or equal to 99%.
Example two
The preparation method of the low dielectric glass microspheres for the high-frequency high-speed copper-clad plate comprises the following steps:
a) mixing materials: weighing the following raw materials in percentage by weight:
80% SiO219% of B2O3、0.2％Al2O30.5% of TiO20.1 percent of ZnO and 0.2 percent of CaO, and the raw materials are mixed evenly.
b) Melting and water quenching: adding the uniformly mixed raw materials in the step a) into a melting furnace for melting, wherein the glass melting temperature is 1620 ℃, and then quenching the melted glass liquid into cullet with the size of less than 5 mm.
c) Crushing and grading: grinding and grading the water-quenched glass material, wherein the grinding and grading adopt airflow grinding and grading equipment or fine ball grinding and grading equipment, and the particle size of the used glass powder is in different particle size ranges of 0.5-20 mu m.
d) Spheroidizing: and spheroidizing the classified glass powder in a balling furnace, and conveying the crushed and classified glass powder into a flame burner balling furnace for spheroidizing in a gas conveying mode, wherein the flame spheroidizing temperature is 1480 ℃.
e) Collecting and sorting: collecting the spheroidized microspheres by using a cyclone collector and a cloth bag collector, and sorting the collected microsphere powder by using superfine precise sorting equipment according to requirements.
The particle size of the low dielectric glass microspheres for the high-frequency high-speed copper-clad plate is basically concentrated between 1 and 15 micrometers, the dielectric constant is 4.0 when the frequency is 10GHz, the dielectric loss factor is 0.0028, the particle size distribution is in different size ranges of 1 to 15 micrometers, and the sphericity is greater than or equal to 99%.
EXAMPLE III
The preparation method of the low dielectric glass microspheres for the high-frequency high-speed copper-clad plate comprises the following steps:
a) mixing materials: weighing the following raw materials in percentage by weight:
85% SiO210% of B2O3、2％Al2O31% of TiO21% of ZnO and 1% of CaO, and uniformly mixing the raw materials.
b) Melting and water quenching: adding the uniformly mixed raw materials in the step a) into a melting furnace for melting, wherein the glass melting temperature is 1650 ℃, and then quenching the melted glass liquid into cullet with the size of less than 5 mm.
c) Crushing and grading: grinding and grading the water-quenched glass material, wherein the grinding and grading adopt airflow grinding and grading equipment or fine ball grinding and grading equipment, and the particle size of the used glass powder is in different particle size ranges of 0.5-20 mu m.
d) Spheroidizing: and spheroidizing the graded glass powder in a balling furnace, and conveying the crushed and graded glass powder into a flame burner balling furnace for spheroidizing in a gas conveying mode, wherein the flame spheroidizing temperature is 1500 ℃.
e) Collecting and sorting: collecting the spheroidized microspheres by using a cyclone collector and a cloth bag collector, and sorting the collected microsphere powder by using superfine precise sorting equipment according to requirements.
The particle size of the low dielectric glass microspheres for the high-frequency high-speed copper-clad plate is basically concentrated between 1 and 15 micrometers, the dielectric constant is 3.9 when the frequency is 10GHz, the dielectric loss factor is 0.0022, the particle size distribution is in different size ranges of 1 to 15 micrometers, and the sphericity is greater than or equal to 99%.
The above description is only three embodiments of the present invention, and it should be noted that, for those skilled in the art, several modifications and improvements can be made without departing from the principle of the present invention, and these should also be considered as falling within the protection scope of the present invention.
Claims (5)
1. A preparation method of low dielectric glass microspheres for a high-frequency high-speed copper-clad plate comprises the following steps:
a) weighing the following raw materials in percentage by weight:
70-85% of SiO210 to 25% of B2O3、0.2～2％Al2O30.5 to 1% of TiO20.1-1% of ZnO and 0.2-1% of CaO, and uniformly mixing the raw materials;
b) adding the uniformly mixed raw materials in the step a) into a melting furnace for melting, wherein the glass melting temperature is 1580-1650 ℃, and then quenching the melted glass liquid with water;
c) grinding and grading the water-quenched glass material, wherein the particle size of the glass powder is in different size fraction ranges of 0.5-20 mu m;
d) spheroidizing the graded glass powder in a balling furnace, and conveying the crushed and graded glass powder into a flame burner balling furnace for spheroidization in a gas conveying mode, wherein the flame spheroidization temperature is 1450-1500 ℃;
e) and collecting the spheroidized glass microspheres, and then sorting the glass microspheres by a classifier.
2. The preparation method of the low-dielectric glass microspheres for the high-frequency high-speed copper-clad plate according to claim 1, which is characterized by comprising the following steps:
and in the step b), the melted glass liquid is quenched into cullet with the size of less than 5 mm.
3. The preparation method of the low-dielectric glass microspheres for the high-frequency high-speed copper-clad plate according to claim 1, which is characterized by comprising the following steps:
and the crushing and grading in the step c) adopt airflow crushing and grading equipment or fine ball milling and crushing and grading equipment.
4. The preparation method of the low-dielectric glass microspheres for the high-frequency high-speed copper-clad plate according to claim 1, which is characterized by comprising the following steps:
the spheroidized glass microspheres in the step e) are firstly subjected to coarse particle collection by a cyclone collector, and then are subjected to fine particle collection by a cloth bag collector.
5. A low dielectric glass microsphere for a high-frequency high-speed copper-clad plate is characterized in that: the low-dielectric glass microspheres for the high-frequency high-speed copper clad laminate, which are prepared by the preparation method for the high-frequency high-speed copper clad laminate low-dielectric glass microspheres according to any one of claims 1 to 4.
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| CN113072303A (en) * | 2021-03-29 | 2021-07-06 | 浙江奕成科技有限公司 | Shape changing method of glass powder for solar cell conductive silver paste |
| CN113277858A (en) * | 2021-05-27 | 2021-08-20 | 江苏联瑞新材料股份有限公司 | Preparation method of spherical ceramic powder for vehicle-mounted copper-clad plate |
| CN113354291B (en) * | 2021-07-05 | 2023-01-31 | 安徽凯盛基础材料科技有限公司 | Hollow glass microsphere for high-frequency high-speed PCB (printed Circuit Board), and preparation method and application thereof |
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| DE2330381A1 (en) * | 1972-06-14 | 1974-01-03 | Du Pont | GLASSES FOR THE MANUFACTURE OF CROSSING DIELECTRICS WITH LOW VALUES |
| CN1186482A (en) * | 1995-06-05 | 1998-07-01 | 日东纺织株式会社 | Low-permittivity glass fibers |
| CN101696089A (en) * | 2009-10-29 | 2010-04-21 | 四川省玻纤集团有限公司 | Glass fiber with low dielectric constant for high frequency high-density circuit board |
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