CN103172269B - High-dielectric constant glass fiber and preparation method thereof as well as high-dielectric constant copper-clad laminate - Google Patents
High-dielectric constant glass fiber and preparation method thereof as well as high-dielectric constant copper-clad laminate Download PDFInfo
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- CN103172269B CN103172269B CN201310121691.6A CN201310121691A CN103172269B CN 103172269 B CN103172269 B CN 103172269B CN 201310121691 A CN201310121691 A CN 201310121691A CN 103172269 B CN103172269 B CN 103172269B
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- glass fibre
- glass
- dielectric constant
- compound
- melting
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Classifications
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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
-
- 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
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/062—Glass compositions containing silica with less than 40% silica by weight
Abstract
The invention relates to high-dielectric constant glass fiber which comprises the following compounds in percentage by weight: 30-40% of SiO2, 0-2% of MgO, 3-7% of CaO, 6-10% of SrO, 22-27% of BaO, 0-6% of CeO2, 7-15% of TiO2, 2-5% of ZrO2, 4-22% of Nb2O3, 0-6% of Al2O3 and less than 1% of ZnO, R2O and other compounds, wherein at a condition of 1MHz frequency, the dielectric constant epsilon of the glass fiber is greater than 9.5, and the dielectric loss tan(delta) is less than 0.03. The high-dielectric constant glass fiber provided by the invention has the beneficial effects of excellent dielectric performance and good fiber forming property, and the wire drawing temperature is lower than 1,120 DEG C.
Description
Technical field
The invention belongs to field of new, especially relate to a kind of high-k glass fibre, this high-k glass fibre is used as printed-wiring board (PWB) and strengthens base material, can be used for the printed-wiring board (PWB) field making high-frequency apparatus miniaturization.
Background technology
Along with high-frequency information communication, the such as high speed development of car phone, individual radio communication, satellite communication, cable TV network etc., require electronics and microwave line miniaturization, portability, therefore require printed-wiring board (PWB) miniaturization, the printed-wiring board (PWB) of Large Copacity, miniaturization needs the copper clad laminate adopting specific inductivity high.The copper clad laminate of high-k must use the resin of high-k and the glasscloth of high-k, current prevailing glass fibre is E glass fibre, its specific inductivity only has about 6.5, the requirement of high-k can not be met, although lead glass has high specific inductivity, but due to the problem such as unstable, environmental pollution of lead, cannot meet the need of market equally.In order to solve the problem of high-k glass fibre, Japan and other countries nineteen nineties just begins one's study high-k glass fibre, and has been developed into corresponding high-k glass fibre.Report is not also studied in this respect by China.
Summary of the invention
An object of the present invention is to provide a kind of under 1MHz frequency condition, glass fibre DIELECTRIC CONSTANT ε be greater than 9.5, high-k glass fibre that dielectric loss tan δ is less than 0.03; Another object of the present invention openly a kind ofly has good fiber-forming process performance, and wire-drawing temperature is lower than the preparation method of the high-k glass fibre of 1120 DEG C; Last object of the present invention makes the copper clad laminate of high-k.
Technical scheme of the present invention is as follows:
High-k glass fibre, comprises following compound and makes: SiO
230 ~ 40wt%, MgO 0 ~ 2wt%, CaO 3 ~ 7wt%, SrO 6 ~ 10wt%, BaO 22 ~ 27wt%, CeO
20 ~ 5wt%, TiO
27 ~ 15wt%, ZrO
22 ~ 5wt%, Nb
2o
34 ~ 22wt%, Al
2o
30 ~ 6wt%; ZnO, R
2o and other compound, total amount is less than 1wt%; Under 1MHz frequency condition, glass fibre DIELECTRIC CONSTANT ε is greater than 9.5, dielectric loss tan δ is less than 0.03.
As preferably, high-k glass fibre comprises following compound and makes: SiO
232 ~ 38wt%, MgO0 ~ 2wt%, CaO 4 ~ 6wt%, SrO 7 ~ 8.5wt%, BaO 24 ~ 26wt%, CeO
20 ~ 4.5wt%, TiO
27.5 ~ 14wt%, ZrO
22.5 ~ 4.5wt%, Nb
2o
35 ~ 15wt%, Al
2o
32 ~ 5wt%; ZnO, R
2o and other compound, total amount is less than 1wt%.
The above-mentioned each compound stated is that raw material is hybridly prepared into admixtion by the preparation method of high-k glass fibre, under 1350 DEG C ~ 1450 DEG C temperature condition, frit block is made in melting while stirring, then melting more than 2 hours again at 1280 ~ 1320 DEG C, drawn fiber after temperature is down to 1100 ~ 1120 DEG C.
As preferably, each raw materials of compound is hybridly prepared into admixtion, and load in platinum material crucible, under 1350 DEG C ~ 1450 DEG C temperature condition, melting while stirring, founds 4 hours; Glass is flow on heat-resisting steel sheet and plate, make frit block, then material block is put into fiber drawing furnace, melting more than 2 hours again at 1280 ~ 1320 DEG C, after fiber drawing furnace nozzle plate temperature is down to 1100 ~ 1120 DEG C, start wire drawing, adjustment drawing speed, makes the continuous fibre diameter be drawn into be 8 ~ 9 μm.
The copper clad laminate of high-k, glass fibre is above-mentioned high-k glass fibre.
The oxide content scope determined in the present invention is based on following reason: SiO2, SiO2 glass network formers, its content directly affects strength of glass, recrystallization temperature, high temperature viscosity etc., SiO2 directly affects specific inductivity simultaneously, if content is lower than 30wt% in glass, glass fiber strength reduces, devitrification of glass temperature improves, high temperature viscosity declines, crystallization speed is too fast, is difficult to drawing fiber; If content is higher than 40wt% in glass, be difficult to the glass fibre obtaining high-k, its optimum value is 32 ~ 38wt%.MgO, CaO, SrO, BaO, MgO, CaO, SrO and BaO alkaline earth metal oxide, it is the outer agent of glass network, reduce devitrification of glass temperature for the effect in glass, improve specific inductivity, the increase of ability along with molecular weight from MgO to BaO improving specific inductivity increases progressively successively, when content is too low, glass infusibility, be difficult to into fiber, and specific inductivity is also difficult to reach 9.5, when it is too high, recrystallization temperature not only can not reduce, improve on the contrary, and the high temperature viscosity of glass is too low, be difficult to into fiber, its optimum value is MgO 0 ~ 2wt%, CaO 4 ~ 6wt%, SrO 7 ~ 8.5wt%, BaO 24 ~ 26wt%.TiO2, ZrO2, CeO2, the transition metal oxides such as TiO2, ZrO2, CeO2, play and flux, improve chemical durability of glass, improve the effect such as specific inductivity, but improve recrystallization temperature.When these component contents are too low, be difficult to obtain the good and specific inductivity of chemical stability higher than 9.5 glass fibre; When content is too high, cause recrystallization temperature too high, be difficult to form fiber.Its optimum value is CeO20 ~ 4.5wt%, TiO27.5 ~ 14wt%, ZrO22.5 ~ 4.5wt%.Nb2O3, Nb2O3 effectively can reduce recrystallization temperature in this glass, are conducive to glass smelting and fiberizing, improve the specific inductivity of glass simultaneously.When content is too low, the DeGrain played; When content is too high, recrystallization temperature improves on the contrary, causes fiber to be difficult to shaping.Its optimum value is Nb2O35 ~ 15wt%.Al2O3, adds a small amount of Al2O3 in this glass fibre, improves the difference between fiberizing temperature and recrystallization temperature, is conducive to fiberizing.Its optimum value is 2 ~ 5wt%.Containing other compound such as a small amount of ZnO, R2O in glass, its total amount is less than 1wt%.Glass of the present invention can under more than 1350 DEG C temperature condition, and the pre-assigned glass batch of electricity consumption heating and melting obtains high-k glass.Then glass melting again at 1280 ~ 1320 DEG C, by platinum bushing plate, melten glass lets slip a remark that to be drawn into diameter be 8 ~ 9 μm of continuous fibres.The fiber drawn can need to make the various glass fiber products such as glasscloth, yarn, band according to user.ZnO, R2O, as fusing assistant, can improve founding and drawing process performance of glass.
The invention has the beneficial effects as follows: high-k glass fibre dielectric properties are excellent, DIELECTRIC CONSTANT ε > 9.5, dielectric loss tan δ < 0.03 (test frequency 1MHz); High-k glass fibre has good fiber-forming process performance, and wire-drawing temperature is lower than 1120 DEG C.
Embodiment
Table 1 is the embodiment of high-k glass fibre of the present invention.
By the high-k glass fibre shown in table 1, be made up of following compound: SiO
230 ~ 40wt%, MgO 0 ~ 2wt%, CaO 3 ~ 7wt%, SrO 6 ~ 10wt%, BaO 22 ~ 27wt%, CeO
20 ~ 5wt%, TiO
27 ~ 15wt%, ZrO
22 ~ 5wt%, Nb
2o
34 ~ 22wt%, Al
2o
30 ~ 6wt%, the total content of above-mentioned oxide compound in glass fibre reaches more than 99wt%, containing a small amount of ZnO, R in high-k glass fibre of the present invention
2o and other compound, its total amount is less than 1wt%, and R refers to the alkali metals such as K, Na.Under 1MHz frequency condition, glass fibre DIELECTRIC CONSTANT ε is greater than 9.5, dielectric loss tan δ is less than 0.03.
Table 1
The preparation method of high-k glass fibre, adopt above-mentioned corresponding compound with being raw material, be hybridly prepared into admixtion, be contained in platinum material crucible, under 1350 DEG C ~ 1450 DEG C temperature condition, melting while stirring, found 4 hours, the glass part melted is banished on the mould of preheated dielectric properties test specimens block, and in time sample block is put into annealing furnace, anneal 1 hour under the temperature condition of 450 ~ 550 DEG C, then Temperature fall, takes out sample and tests sample as dielectric properties; Another part glass flows on heat-resisting steel sheet and plate, make frit block, then material block is put into fiber drawing furnace, melting more than 2 hours again at 1280 ~ 1320 DEG C, after fiber drawing furnace nozzle plate temperature is down to 1100 ~ 1120 DEG C, start wire drawing, adjustment drawing speed, makes the continuous fibre diameter be drawn into be 8 ~ 9 μm.The glass sample having surveyed dielectric properties dices, and for measuring glass density, glass density adopts suspension method.
The copper clad laminate of high-k, glass fibre is above-mentioned high-k glass fibre.
Claims (5)
1. high-k glass fibre, is characterized in that comprising following compound makes: SiO
230 ~ 40wt%, MgO 0 ~ 2wt%, CaO 3 ~ 7wt%, SrO 6 ~ 10wt%, BaO 22 ~ 27wt%, CeO
20 ~ 5wt%, TiO
27 ~ 15wt%, ZrO
22 ~ 5wt%, Nb
2o
34 ~ 22wt%, Al
2o
30 ~ 6wt%; ZnO, R
2o and other compound, total amount is less than 1wt%; Under 1MHz frequency condition, glass fibre DIELECTRIC CONSTANT ε is greater than 9.5, dielectric loss tan δ is less than 0.03, and above-mentioned R is alkali metal.
2. high-k glass fibre according to claim 1, is characterized in that comprising following compound makes: SiO
232 ~ 38wt%, MgO 0 ~ 2wt%, CaO 4 ~ 6wt%, SrO 7 ~ 8.5wt%, BaO 24 ~ 26wt%, CeO
20 ~ 4.5wt%, TiO
27.5 ~ 14wt%, ZrO
22.5 ~ 4.5wt%, Nb
2o
35 ~ 15wt%, Al
2o
32 ~ 5wt%; ZnO, R
2o and other compound, total amount is less than 1wt%.
3. the preparation method of high-k glass fibre, it is characterized in that each compound according to claim 1 being that raw material is hybridly prepared into admixtion, under 1350 DEG C ~ 1450 DEG C temperature condition, frit block is made in melting while stirring, then melting more than 2 hours again at 1280 ~ 1320 DEG C, drawn fiber after temperature is down to 1100 ~ 1120 DEG C.
4. the preparation method of high-k glass fibre according to claim 3, is characterized in that each raw materials of compound is hybridly prepared into admixtion, and load in platinum material crucible, under 1350 DEG C ~ 1450 DEG C temperature condition, melting while stirring, founds 4 hours; Glass is flow on heat-resisting steel sheet and plate, make frit block, then material block is put into fiber drawing furnace, melting more than 2 hours again at 1280 ~ 1320 DEG C, after fiber drawing furnace nozzle plate temperature is down to 1100 ~ 1120 DEG C, start wire drawing, adjustment drawing speed, makes the continuous fibre diameter be drawn into be 8 ~ 9 μm.
5. the copper clad laminate of high-k, is characterized in that making with high-k glass fibre according to claim 1.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310121691.6A CN103172269B (en) | 2013-04-09 | 2013-04-09 | High-dielectric constant glass fiber and preparation method thereof as well as high-dielectric constant copper-clad laminate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310121691.6A CN103172269B (en) | 2013-04-09 | 2013-04-09 | High-dielectric constant glass fiber and preparation method thereof as well as high-dielectric constant copper-clad laminate |
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| CN103172269A CN103172269A (en) | 2013-06-26 |
| CN103172269B true CN103172269B (en) | 2015-01-07 |
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| CN105693099A (en) * | 2015-11-06 | 2016-06-22 | 泰山玻璃纤维有限公司 | Glass fiber resistant to chemical corrosion |
| CN105859145B (en) * | 2016-04-07 | 2018-12-04 | 重庆理工大学 | A kind of glass fibre of high dielectric constant |
| CN105731815A (en) * | 2016-04-07 | 2016-07-06 | 重庆理工大学 | High-dielectric-constant glass fiber and preparation method thereof |
| CN107382078B (en) * | 2017-09-07 | 2020-04-17 | 南京玻璃纤维研究设计院有限公司 | High-dielectric-constant low-loss glass fiber |
| CN113135667B (en) * | 2021-04-28 | 2022-09-27 | 泰山玻璃纤维有限公司 | High-dielectric-constant low-dielectric-loss glass fiber |
| CN113135668A (en) * | 2021-04-28 | 2021-07-20 | 泰山玻璃纤维有限公司 | High-dielectric low-loss glass fiber and preparation method thereof |
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| JPS6046945A (en) * | 1983-08-22 | 1985-03-14 | Ohara Inc | Optical glass |
| CN101746951B (en) * | 2008-12-09 | 2012-01-18 | 湖北新华光信息材料有限公司 | Optical glass with negative anomalous dispersion |
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