CN113105118A - Glass composition with low thermal expansion coefficient and glass fiber made from same - Google Patents
Glass composition with low thermal expansion coefficient and glass fiber made from same Download PDFInfo
- Publication number
- CN113105118A CN113105118A CN202110404135.4A CN202110404135A CN113105118A CN 113105118 A CN113105118 A CN 113105118A CN 202110404135 A CN202110404135 A CN 202110404135A CN 113105118 A CN113105118 A CN 113105118A
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- glass composition
- oxide
- glass
- thermal expansion
- low coefficient
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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
- C03C13/00—Fibre or filament compositions
Abstract
The invention discloses a glass composition with a low thermal expansion coefficient, which is characterized by comprising a main body material, a strengthening material and a fluxing material; the main body material comprises silicon oxide, and the weight percentage of the silicon oxide is 55-66% of the glass composition; the strengthening material comprises alumina, and the weight percentage of the alumina is 10-20% of the glass composition; and the fluxing material comprises magnesium oxide, zinc oxide and titanium dioxide; wherein, the weight percentage of the magnesium oxide is 3-12% of the glass composition, the weight percentage of the zinc oxide is 0.01-7% of the glass composition, and the weight percentage of the titanium dioxide is 0.01-6% of the glass composition. The glass composition disclosed by the invention has a lower thermal expansion coefficient and better mass production performance, and meets the severe requirements of future high-end electronic products.
Description
Technical Field
The invention relates to the field of glass manufacturing, in particular to a glass composition with a low thermal expansion coefficient and a glass fiber manufactured by the same.
Background
With the advancement of wired and wireless network technologies and the increasing demand of people for multifunctional, high-speed and high-frequency electronic devices (e.g., smart phones, tablet computers, video game machines, smart watches, servers, fidelity wireless headsets, etc.), various electronic devices with different functions are gradually developed and marketed; in order to increase the operating speed and frequency of electronic devices, it is often necessary to manufacture circuit boards (PCBs) from materials having Low dielectric coefficients (Low Dk) and Low dissipation factors (Low Df) to meet specifications for electrical characteristics.
Since the carrier is an interface between a chip (IC) and a circuit board, compared with a conventional lead frame packaging method, the carrier has significant advantages in terms of transmission speed, performance and volume, and therefore, many high-speed computing chips, such as a Central Processing Unit (CPU), a Graphics Processing Unit (GPU), a Package Antenna (AiP for short) of a mobile phone, a network IC, etc., use the carrier as a basic interface. Therefore, the requirements of manufacturing IC carrier boards and Ball Grid Array (BGA) packages for high-level PCB products are in a high-speed growth period, and in order to meet the product requirements, the materials used in the IC carrier boards and BGA packages need Low Coefficient of Thermal Expansion (CTE) and high fiber strength, and also need to have electrical characteristics such as Low dielectric constant (Low Dk) and Low dissipation factor (Low Df).
Because of its excellent physical properties, glass fibers have become an important raw material indispensable in modern industry, especially "glass fiber yarns" made of electronic grade glass fibers. However, bubbles are generated in the process of converting glass materials from melting to glass, and when the viscosity of the glass is higher, the number of bubbles staying in the glass is larger, so that the finally finished glass fiber has a plurality of hollow fiber structures, which affects the electrical characteristics of the glass fiber, and even may make a circuit board or a carrier board manufactured by replacing the glass fiber unusable.
The thermal expansion coefficient of the traditional E-glass formula reaches 5.4 ppm/DEG C, and the traditional E-glass formula is difficult to meet the requirements of high-order carrier plates. Although D-Glass has a good thermal expansion coefficient which can reach 3.0 ppm/DEG C, the D-Glass has very high melting temperature and viscosity, so that the production is difficult, no method for preparing Glass fiber below 7 mu m by using a D-Glass formula exists, and the application of the D-Glass in a printed circuit board is limited. Thus, the high viscosity also causes difficulty in removing bubbles, resulting in a large amount of hollow fibers existing in the Glass cloth, resulting in the non-durability of the D-Glass printed circuit board.
The current solution in the printed circuit board industry is to use high levels of silicon oxide (SiO)2) Adding alumina (Al)2O3) Glass fiber formulations of (a), for example: T-Glass (one of S-Glass fibers, hereinafter collectively referred to as S-Glass) has a thermal expansion coefficient reduced to 2.8 ppm/DEG C, and the formula can produce ultra-fine fibers and has a thermal expansion coefficient lower than that of E-Glass, but the formula still has the problem of excessively high viscosity, so that the mass production performance of Glass is poor, and the Glass cannot be produced in large quantitiesAnd the cost is too high, so that S-Glass cannot be widely used like E-Glass. At the same time, there is a need in the printed circuit board industry to further reduce the coefficient of thermal expansion based on S-Glass.
Therefore, a glass fiber with a lower thermal expansion coefficient, and a better mass production performance, and a stringent requirement for future high-end electronic products are urgently needed.
Disclosure of Invention
In order to solve the problems of the prior art, the invention discloses a glass composition with low thermal expansion coefficient and a glass fiber manufactured by the same.
Compared with S-Glass and D-Glass fibers in the prior art, the Glass composition disclosed by the invention has better thermal expansion coefficient and viscosity temperature of melting point, so that the problems of low thermal expansion coefficient, overhigh viscosity and poor mass production performance of Glass can be effectively solved.
One of the objects of the present invention is to provide a glass composition with a low coefficient of thermal expansion, comprising a host material, a strengthening material and a fluxing material; wherein the host material comprises silicon oxide (SiO)2) Silicon oxide (SiO)2) Is 55-66% of the glass composition; the reinforcing material includes aluminum oxide (Al)2O3) Said aluminum oxide (Al)2O3) Is 10-20% of the glass composition, the strengthening material being capable of increasing the structural strength of the glass composition; the fluxing material comprises magnesium oxide (MgO), zinc oxide (ZnO) and titanium dioxide (TiO)2)。
Wherein the weight percentage of the magnesium oxide (MgO) accounts for 3-12% of the glass composition, the weight percentage of the zinc oxide (ZnO) accounts for 0.01-7% of the glass composition, and the titanium dioxide (TiO)2) 0.01-6% of the glass composition, the fluxing material being capable of reducing the viscosity temperature of the glass composition by adding zinc oxide (ZnO) and titanium dioxide (TiO)2) And the like, which can lower the thermal expansion coefficient of the glass composition.
It is another object of the present invention to provide a glass fiber, wherein the glass fiber is made from the components of the above glass composition.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention clearer and more fully describe the technical solutions in the embodiments of the present invention, it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all 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.
The invention discloses a glass composition with low thermal expansion coefficient and glass fiber thereof, and the glass composition can be used for manufacturing other glass products besides glass fiber.
The glass composition disclosed by the embodiment of the invention comprises a main body material, a fluxing material and a strengthening material, wherein the main body material comprises silicon oxide (SiO)2) In order to achieve the low coefficient of thermal expansion effect, the amount of silicon oxide in the Glass composition is 55-66% by weight, which is lower than the amount of silicon oxide used in the current S-Glass (S-Glass) (65%), but the Glass composition produced by the present invention has a better coefficient of thermal expansion and a higher viscosity temperature than the current S-Glass (S-Glass).
Because the melting aid material reduces the viscosity of the glass composition when molten because it increases its viscosity temperature when the silica content is high, in one embodiment of the invention, the melting aid material comprises at least magnesium oxide (MgO), zinc oxide (ZnO) and titanium dioxide (TiO)2) Wherein, the magnesium oxide can reduce the melting temperature of the glass composition, is beneficial to the subsequent melting and molding of glass fiber, can prevent crystallization generation and reduce the coefficient of thermal expansion, and can improve the elastic modulus; furthermore, magnesium oxide is an alkaline earth metal oxide and has an interfering influence on the effect of ion exchange properties, and when the content of magnesium oxide is too high, it is not advantageous to reduce the glass compositionAnd a dissipation factor, and increases phase separation of the glass composition, and therefore, the weight percentage of magnesium oxide is 3-12% (more preferably 4-9%) of the glass composition; in addition, a small amount of titanium dioxide (TiO) was added2) The viscosity temperature of the raw materials molten into glass can be reduced, the thermal expansion coefficient of the glass composition can be reduced, and the mechanical property can be increased, but when the content of titanium dioxide is too high, the influence on the color of the glass is large, so that the weight percentage of the titanium dioxide is 0.01-6% of that of the glass composition; the addition of a small amount of zinc oxide (ZnO) can lower the thermal expansion coefficient and lower the melting temperature, and can enhance chemical stability, but when the amount is too high, the elastic modulus is lowered, which is disadvantageous to the glass characteristics, so the weight percentage of zinc oxide is 0.01-7% of the glass composition.
In embodiments of the invention, the strengthening material, which can increase the structural strength of the glass composition, includes at least alumina (Al)2O3) And the alumina is one of the framework oxides forming the glass, when the glass contains a proper amount of alumina, the occurrence of the phenomenon of silicon oxide crystallization (Deviatility) can be inhibited, and the borosilicate glass is prevented from phase separation, so that the chemical strength, the elastic modulus and the hardness of the glass are enhanced. Thus, the alumina is also used to improve the ion exchange performance while at the same time being alumina (Al)2O3) When the content of (b) is decreased, the thermal expansion coefficient is increased and the thermal shock resistance is easily decreased while the dielectric constant is increased with the decrease in the water resistance of the glass composition, and there is a possibility that the ion exchange performance cannot be sufficiently exhibited; when alumina (Al)2O3) When the content exceeds 18%, the devitrified crystals are easily precipitated in the glass, and when the crystallized crystals grow, the glass fibers are drawn at a high temperature and are difficult to be formed in the subsequent production process, and therefore, in this embodiment, the alumina (Al) is used2O3) Is 10-20 wt% of the glass composition (the optimal proportion is
)。
As can be seen from the above, the use of a high silica content alone can achieve a low thermal expansion coefficient of the glass composition, but increases the viscosity temperature, which makes the production difficult and makes it difficult to eliminate bubbles. Therefore, the invention also adds zinc oxide and titanium dioxide, which can reduce the viscosity temperature and further reduce the thermal expansion coefficient to maintain the characteristics of the glass and improve the performance of the glass, and inherits the production yield of the glass fiber step by step.
In other optional embodiments, the glass composition further comprises calcium oxide (CaO), which is a glass network and can lower the melting temperature of the glass fiber produced later, and does not reduce the crystallization resistance, and the calcium oxide permeates the glass fiber with the effect of increasing the elastic modulus compared to other components, but when the content of the calcium oxide is increased (e.g. more than 6%), the dielectric constant of the glass composition is increased, and the thermal expansion coefficient of the glass composition is preferably increased, or the ion exchange performance is easily reduced, so that, in the embodiment, the calcium oxide (CaO) accounts for no more than 5% by weight of the glass composition (preferably, the proportion is 0.1-0.5%) to improve the water resistance of the glass composition. In addition, the glass composition further includes boron oxide (B)2O3) Boron oxide has the functions of reducing the thermal expansion coefficient and the temperature of melting raw materials into glass, and can stabilize the glass to separate out crystals; however, if the content of boron oxide is too high, the elastic modulus and the water resistance will be lowered, and therefore, in this embodiment, the boron oxide (B)2O3) The weight percentage of the glass composition is not more than 15 percent, so as to maintain the glass per se when reducing the viscosity temperature of the glassAnd (4) characteristics.
In other alternative embodiments, other alkali metal oxides, including but not limited to sodium oxide (Na), may be added to the glass composition additive as a Flux (Flux), and may reduce the dielectric loss of the glass composition and glass fibers2O), potassium oxide (K)2O) and/or lithium oxide (Li)2O)。
Wherein, the sodium oxide is the main ion exchange component, and can reduce the viscosity temperature to be beneficial to the subsequent melting and molding of the glass fiber and improve the crystallization resistance; when the content of sodium oxide is too large, the coefficient of thermal expansion will become high; the potassium oxide is also an ion exchange promoting component, is an alkali metal oxide, has a better effect of increasing the stress depth of the compression stress layer, can reduce the viscosity temperature to be beneficial to the subsequent melting and molding of the glass fiber, and can also cause the thermal expansion coefficient to be high when the content of the potassium oxide is excessive; the lithium oxide has the same effect as the common components of the alkali metal oxides, and meanwhile, the improvement of the elastic modulus has positive influence and can promote the melting purification of glass; since the content of the alkali metal oxide is too high, the dielectric loss tangent is required to be high and the water resistance is also deteriorated, and particularly, when sodium oxide and potassium oxide coexist, a mixed alkali oxygen anomalous effect (mixed alkali effect) occurs, whereby the specific resistance of the glass is remarkably increased to exert an influence on the thermal expansion coefficient, and therefore, it is desirable that the content of the alkali metal oxide is not more than 2% based on the total weight of the glass composition. Thus, the glass composition further includes an impurity material comprising iron oxide (Fe)2O3) Since too much impurity material is not favorable for lowering the dielectric constant and dissipation factor of the glass composition, and too little impurity material results in higher raw material cost, the iron oxide (Fe) is used in balancing production cost and product quality2O3) Or other impurity-attributed material, in a total weight percent of 0.05-0.2% of the glass composition.
In the embodiments of the present inventionIn particular, the prior art batch of S-glass A1, S-glass A2 and A3 and A4 is used as a comparative example, and the batch of A5-A8 in a different ratio from the present invention is poured into a ceramic crucible, and is connected to a predetermined temperature (A)
) After a set time is given for complete melting, the glass block is slowly replaced at room temperature, and then the formed glass block is cut into a glass sheet sample with a length of 20mm and a thickness of 2-3mm by a diamond cutter, and the dielectric constant and dissipation factor of the sample are measured by using an RF radio frequency impedance Analyzer and a Thermal Mechanical Analyzer (Thermal Mechanical Analyzer), the test is performed according to ASTM E831, and the Thermal expansion coefficient of the continuous glass sheet sample is measured, and the test results shown in Table 1 are obtained.
Of these, the prior art S-glass A1, S-glass A2 and A3 and A4 are comparative examples, all of which do not contain zinc oxide (ZnO), and some of which do not contain titanium dioxide (TiO) (comparative examples)2) (ii) a A5-A8 are examples of the present invention and all contain zinc oxide (ZnO) and titanium dioxide (TiO)2) From Table 1, it can be seen that the thermal expansion coefficients of the glass compositions of the examples of the present invention are all less than 2.5 ppm/deg.C, much lower than the respective glass samples of the comparative examples, and far beyond the S-glass formulation currently employed in the advanced PCB industry, and the remaining values (e.g.: viscosity temperature, dielectric constant, loss factor) are kept in good standards, and the production yield and the electrical characteristics of the glass fiber can be improved.
All the above-mentioned optional technical solutions can be combined arbitrarily to form the optional embodiments of the present invention, and are not described herein again.
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 invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. A glass composition having a low coefficient of thermal expansion, the glass composition comprising a host material, a strengthening material, and a fluxing material;
the main body material comprises silicon oxide, and the weight percentage of the silicon oxide is 55-66% of the glass composition;
the strengthening material comprises alumina, and the weight percentage of the alumina is 10-20% of the glass composition; and
the fluxing material comprises magnesium oxide, zinc oxide and titanium dioxide;
wherein, the weight percentage of the magnesium oxide is 3-12% of the glass composition, the weight percentage of the zinc oxide is 0.01-7% of the glass composition, and the weight percentage of the titanium dioxide is 0.01-6% of the glass composition.
2. The low coefficient of thermal expansion glass composition of claim 1, further comprising boron oxide, wherein boron oxide comprises no more than 15% by weight of the glass composition.
3. The low coefficient of thermal expansion glass composition of claim 1, further comprising calcium oxide, the calcium oxide comprising no more than 5% by weight of the glass composition, to improve water resistance of the glass composition.
4. The low coefficient of thermal expansion glass composition of claim 1, further comprising at least one alkali metal oxide, wherein the alkali metal oxide comprises no more than 2% of the total weight of the glass composition.
5. The low coefficient of thermal expansion glass composition of claim 4, wherein the alkali metal oxide comprises sodium oxide, potassium oxide, and/or lithium oxide.
6. The low coefficient of thermal expansion glass composition of claim 1, further comprising an impurity material, wherein the impurity material comprises iron oxide, and wherein the weight percent of iron oxide is between 0.05 and 0.2 percent of the glass composition.
7. The low coefficient of thermal expansion glass composition of claim 1, wherein the weight percent of magnesium oxide is 4-9% of the glass composition.
8. The low coefficient of thermal expansion glass composition of claim 1, wherein alumina comprises 13-17% by weight of the glass composition.
9. The low coefficient of thermal expansion glass composition of claim 1, wherein the calcium oxide comprises 0.1 to 0.5 weight percent of the glass composition.
10. A glass fiber made from the low coefficient of thermal expansion glass composition of any of claims 1-9, wherein the coefficient of thermal expansion of the glass composition is less than 2.5ppm/° c.
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| CN202110404135.4A CN113105118A (en) | 2021-04-14 | 2021-04-14 | Glass composition with low thermal expansion coefficient and glass fiber made from same |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113979635A (en) * | 2021-11-23 | 2022-01-28 | 清远忠信世纪电子材料有限公司 | Low-expansion-coefficient glass fiber |
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| CN113979635A (en) * | 2021-11-23 | 2022-01-28 | 清远忠信世纪电子材料有限公司 | Low-expansion-coefficient glass fiber |
| CN113979635B (en) * | 2021-11-23 | 2022-06-10 | 清远忠信世纪电子材料有限公司 | Low-expansion-coefficient glass fiber |
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