CN102976620A - Composition for preparing glass fibers and low-dielectric constant glass fibers thereof - Google Patents

Composition for preparing glass fibers and low-dielectric constant glass fibers thereof Download PDF

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CN102976620A
CN102976620A CN2012105193374A CN201210519337A CN102976620A CN 102976620 A CN102976620 A CN 102976620A CN 2012105193374 A CN2012105193374 A CN 2012105193374A CN 201210519337 A CN201210519337 A CN 201210519337A CN 102976620 A CN102976620 A CN 102976620A
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glass
composition
sio
fibers
dielectric constant
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CN102976620B (en
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韩利雄
杜迅
姚远
何建明
陈德全
魏泽聪
彭文杰
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Chongqing international composite Limited by Share Ltd
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Chongqing Polycomp International Corp
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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
    • C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/089—Glass compositions containing silica with 40% to 90% silica, by weight containing boron
    • C03C3/091—Glass compositions containing silica with 40% to 90% silica, by weight containing boron containing aluminium

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Glass Compositions (AREA)

Abstract

The invention discloses a composition for preparing glass fibers and low-dielectric constant glass fibers thereof. The composition for preparing the glass E fibers provided by the invention is mainly composed of the following materials by weight percent: 60.2-65% of SiO2, 10-14% of Al2O3, 23-27% of B2O3 and 0.5-2% of Li2O. The low-dielectric constant glass fibers prepared from the composition have the following advantages: dielectric properties are excellent, at the frequency of 1 MHz, the dielectric constant does not exceed 4.5 and the dielectric loss does not exceed 0.001; simultaneously, the fibers have excellent mechanical properties, and have the elasticity modulus of more than 75 GPa, which is superior to glass D (having the elasticity modulus of about 55 GPa) and also to the common glass E (having the elasticity modulus of about 72 GPa); the fibers have excellent moldability, and the molding temperature does not exceed 1350 DEG C and the molding interval is higher than 80 DEG C; and the fibers also have good thermal stability and the coefficient of thermal expansion of the fibers is about (3.0-3.2)*10<-6>/DEG C, which is equivalent to the glass E level and obviously superior to glass D.

Description

Composition and glass fiber with low dielectric constant thereof for the preparation of glass fibre
Technical field
The present invention relates to composition and glass fibre thereof for the preparation of glass fibre, relate in particular to composition and glass fiber with low dielectric constant thereof for the preparation of glass fiber with low dielectric constant.
Background technology
Modern electronic equipment generally includes the printed circuit board (PCB) of strengthening with glass fibre.The electronics in many modern times such as mobile or fixed radiophone, computer, personal digital assistant (PDA) etc., all has the electronic system of moving under high or ultra high frequency.When glass exposure during in this high frequency or ultra-high frequency elect magnetic field, this glass absorbs at least a portion ability and be hot with the Conversion of energy that absorbs.The energy of the hot form that is absorbed by glass is called the dielectric loss energy.This dielectric loss energy is directly proportional with " specific inductivity " and " tangent of the dielectric loss angle " of glass composition, shown in the following row expression formula:
W=kfv 2ε(tanδ)
Wherein " W " is the dielectric loss energy in the glass, and " k " is constant, and " f " is frequency, " v 2" be potential gradient, " ε " is specific inductivity, " tan δ " is tangent of the dielectric loss angle.Shown in above expression formula, dielectric loss energy " W " is along with the increase of the increase of the specific inductivity of glass and tangent of the dielectric loss angle and/or frequency and increase.
E Glass Fiber, copper coated foil plate (CCL), printed circuit board (pcb) are three upstream and downstream products that closely link to each other, are as close as lips and teeth on the same industrial chain.In recent years, the prosperity of electronic information technology has spurred the increase year after year of the E Glass Fiber market requirement.Simultaneously, be accompanied by the fast development of global electronic information industry, microelectronic industry is constantly pursued high frequency, high is maintained secrecy, high-fidelity and lightweight, and this just requires CCL intensity higher, and specific inductivity and dielectric loss are lower.And CCL mainly is comprised of the moulding resin of using and the glass two portions that play enhancement.Thereby, as the electron glass fiber performance quality of CCL key foundation material, also just directly affect the performance of CCL and even PCB.
The electronic-grade glass of generally using both at home and abroad at present mainly is the E glass fibre, and it consists of: 52 ~ 56% SiO 2, 12 ~ 16% Al 2O 3, 5 ~ 10% B 2O 3, 16 ~ 25% CaO, 0 ~ 5.0% MgO, 3 ~ 5% Na 2O+K 2The advantage such as O, E glass fibre have that workability is good, water-tolerant, price are low, but its specific inductivity is higher, is about 6.7, and dielectric loss is also larger, greater than 10 -3, be difficult to satisfy the requirement of PCB densification and high speed information processing.
In order to reduce the glass fibre specific inductivity, people had developed again D glass fibre afterwards, and it basic composition is: 72 ~ 76% SiO 2, 0 ~ 5% Al 2O 3, 20 ~ 25%B 2O 3, 3 ~ 5% Na 2O+K 2O.The specific inductivity of D glass fibre is about 4.1, and dielectric loss is 8 * 10 -4About, dielectric properties are excellent.But also there are some shortcomings in D glass fibre: (1) with respect to the E glass fibre, D glass fibre has the SiO of high level 2, cause high, the poor performance of holing of D glass fibre enhancement layer pressing plate hardness, be unfavorable for following process; (2) the glass melting temperature of D glass fibre is high, and meltbility is poor, is easy to produce vein and bubble, cause producing the wire-drawing operation difficulty, the problem such as the glass fibre fracture of wire is many in spinning technique, so productivity and workability are all very poor, production cost is very high, is difficult for scale operation; (3) the D glass fibre water tolerance is relatively poor, causes easily peeling off of fiber and resin.
In order to improve the shortcoming of D glass, the researchist has done again many effort.
US Patent No. 6309990 discloses another kind of new dielectric glass fibre, and its composition mainly comprises: SiO 250-60%, B 2O 320-30%, Al 2O 310-20%, CaO0-5%, MgO0-5%, K 2O+Na 2O+Li 2O0-0.5%, TiO 20.5-5%.The specific inductivity of this glass is 4.2-4.8, and dielectric just is being cut to 5-9 * 10 -4(under the 1MHz frequency), mold temperature are 1300-1360 ℃.Should have specific inductivity and the dielectric tangent that comparatively approaches with D glass by low dielectric glass, thermal expansivity is also almost identical, and water tolerance is better, and mold temperature is lower, and production cost and production difficulty have had obvious improvement than D glass.
Application number is that 02810477.3 Chinese patent literature discloses a kind of glass fiber with low dielectric constant, and its classical group becomes: 53% SiO 2, 15.8% Al 2O 3, 19.6% B 2O 3, 0.5% Na 2O+K 2O, 5.3% CaO, 3.9% MgO and 1.2%P 2O 5, this glass fibre has added the P of easy corrosion kiln in order to improve transaction capabilities 2O 5, higher to the kiln specification of quality.
Application number is that 200480006750.4 Chinese patent literature discloses a kind of dielectric glass fibre, and its composition mainly comprises: SiO 250-60%, B 2O 316-25%, Al 2O 310-19%, CaO0-10%, MgO0-10%, K 2O+Na 2O+Li 2O＜2%, TiO 20-3%, ZrO 20.5-1.5%.The specific inductivity of this glass is about 4.6, and the dielectric tangent is about 10 * 10 -4(under the 1MHz frequency), mold temperature are no more than 1350 ℃.This characteristic feature of an invention is to have added in the glass a certain amount of ZrO 2Thereby, obtained between wider shaping area and production efficiency.
Application number is that 200780046066.2 Chinese patent literature discloses a kind of dielectric glass fibre that is applied to electronics, and this glass composition comprises: SiO 260-68%, B 2O 37-13%, Al 2O 39-15%, CaO0-4%, MgO8-15%, K 2O+Na 2O+Li 2O0-2%, TiO 20-2%.The specific inductivity of this glass is 5.4-6, and the dielectric tangent is about 12 * 10 -4(under the 1MHz frequency), mold temperature is less than 1370 ℃.The purpose of this invention is to wish to reduce production costs, thereby has significantly reduced B 2O 3Content, but obviously, this adjustment has also obviously had influence on the dielectric properties of glass fibre.
Application number is that 200780048402.7 Chinese patent literature discloses a kind of glass fiber with low dielectric constant, and it is composed as follows: 52 ~ 60% SiO 2, 11 ~ 16% Al 2O 3, 20 ~ 30% B 2O 3, 4 ~ 8% CaO, the specific inductivity of this glass fibre is 4.5 ~ 5, dielectric loss≤5 * 10 -4But because its CaO content is higher, and does not contain other component, tendency towards devitrification increased greatly when this can cause this glass fibre moulding, was difficult to obtain small diameter fibers.
Application number is that the Chinese patent literature of CN200610166224.5 discloses a kind of glass fiber with low dielectric constant, and it consists of: 50 ~ 60% SiO 2, 6 ~ 9.5% Al 2O 3, 30.5 ~ 35% B 2O 3, 0 ~ 5% CaO, 0 ~ 5% ZnO, 0.5 ~ 5% TiO 2The specific inductivity of this glass fibre is 3.9-4.4, and dielectric loss is 4 * 10 -4~ 8.5 * 10 -4, but the B of this glass fibre 2O 3Content is very high, and B 2O 3Volatilize easily, this is contaminate environment not only, causes easily the composition fluctuation large simultaneously, and corrosion also can increase to kiln, and in addition, this glass fiber strength is inadequate, and easy crystallization, and water tolerance is also relatively poor.
For glass fiber with low dielectric constant, most researchist's attentions concentrates on and reduces its specific inductivity, reduces its moulding difficulty aspect, but constantly pursuit is ultralight ultra-thin along with modern electronic product, and printed circuit board (PCB) (PCB) is also more and more higher to the requirement of intensity own.If it is inadequate to strengthen the glass fibre mechanical property of usefulness, when CCL was more and more less, more and more thinner, the intensity of PCB just can't guarantee certainly, finally also can affect the work-ing life of electronic product.Therefore, for glass fiber with low dielectric constant, not only require its specific inductivity and dielectric loss as far as possible low, its mechanical property also must can satisfy actual needs simultaneously.
Summary of the invention
The present invention solves the inadequate problem of dielectric glass fibre mechanical property in the prior art, and purpose is to provide a kind of glass fiber with low dielectric constant, and it has the dielectric properties close to D glass, and its specific inductivity is no more than 4.5, and dielectric loss is less than 0.001; Its Young's modulus is greater than 75GPa simultaneously.The object of the present invention is achieved like this:
The invention provides a kind of composition for the preparation of glass fibre, mainly the material by following weight percent forms:
SiO 260.4 ~ 65%, Al 2O 310 ~ 14%, B 2O 322 ~ 26% and Li 2O 0.5 ~ 2%.
Preferably, described composition mainly is comprised of the material of following weight percent: SiO 260.6 ~ 63.2%, Al 2O 311 ~ 13.2%, B 2O 324.2 ~ 26% and Li 2O 0.5 ~ 1.5%.
Described composition comprises that also weight percent content is at the CaO below 2%, MgO, ZnO, TiO 2, Fe 2O 3, ZrO 2, Na 2O or K 2O.
Further preferably, described composition be arbitrary in following (1)-(7) shown in:
(1) described composition is comprised of the material of following weight percent: SiO 262%, Al 2O 312.3%, B 2O 324.2% and Li 2O 1%, and surplus is impurity;
(2) described composition is comprised of the material of following weight percent: SiO 260.4%, Al 2O 312.2%, B 2O 326% and Li 2O 1%, and surplus is impurity;
(3) described composition is comprised of the material of following weight percent: SiO 265%, Al 2O 310%, B 2O 322.7% and Li 2O 2%, and surplus is impurity;
(4) described composition is comprised of the material of following weight percent: SiO 261%, Al 2O 311%, B 2O 325.8%, Li 2O 1.2% and TiO 20.8%, surplus is impurity;
(5) described composition is comprised of the material of following weight percent: SiO 263.1%, Al 2O 310.6%, B 2O 324.5% and Li 2O 1.5%, and surplus is impurity;
(6) described composition is comprised of the material of following weight percent: SiO 260.6%, Al 2O 313.2%, B 2O 325% and Li 2O 0.8%, and surplus is impurity;
(7) described composition is comprised of the material of following weight percent: SiO 263.2%, Al 2O 314%, B 2O 322% and Li 2O 0.5%, and surplus is impurity.
The present invention also provides the glass fibre that is prepared by described composition.
The dielectric properties of glass fibre and its chemical constitution are closely related.
SiO 2Be one of main skeleton oxide compound that forms in glass, its field intensity is large, and ion is difficult for polarization, thereby SiO in the glass 2Content is higher, and the glass specific inductivity is less.The specific inductivity of silica glass is minimum, is about 3.75.But SiO in the glass 2During too high levels, the high temperature viscosity of glass can be very large, and refining quality is difficult to guarantee, the wire-drawing shape difficulty.So among the present invention, SiO 2Content is defined as 60.4wt% ~ 65wt%.
Al 2O 3Also be one of skeleton oxide compound that forms in glass, work as Al 2O 3During not enough 10wt%, the mechanical property of glass fibre and water tolerance all can obviously reduce; If but Al 2O 3Too high levels, the high temperature viscosity of glass fibre can enlarge markedly, the wire-drawing shape difficulty, and also specific inductivity also can rise.So among the present invention, Al 2O 3Content is 10wt% ~ 14wt%.
B 2O 3Also be one of skeleton oxide compound that forms in glass, and it there is obvious effect to reducing the glass specific inductivity, therefore, generally all improves B in the glass with low dielectric constant as far as possible 2O 3Content.If but B 2O 3Too high levels, volatile quantity also can be larger when high temperature for it, and this can cause the glass metal uneven components, affects moulding and the stability of glass fibre.So among the present invention, B 2O 3Content be 22wt% ~ 26wt%.
Li 2O and Na 2O, K 2O etc. are all alkalimetal oxide, belong to glass network ectosome ion, but Li +Radius is little, and strength of electric field is large, the successful of not only fluxing, and help to improve the devitrification of glass tendency.So among the present invention, Li 2The content of O is 0.5wt% ~ 2wt%.
The divalent-metal ion oxide compounds such as CaO, MgO, ZnO belong to glass network and adjust body, and to reducing the glass high temperature viscosity, improve the glass ware forming performance certain effect is arranged, but they have negative impact to the glass dielectric properties.TiO 2, Fe 2O 3Deng oxide compound general ubiquity all in raw mineral materials, be difficult to avoid being introduced in the glass as impurity.Therefore among the present invention, allow the existence of these material trace, but its total content must not surpass 2wt%.
The present invention compared with prior art has following advantage:
(1) dielectric glass fibre provided by the present invention has good dielectric properties, and under the 1MHz frequency, specific inductivity is no more than 4.5, and dielectric loss is no more than 0.001.
(2) glass fiber with low dielectric constant provided by the present invention has excellent mechanical property, and its Young's modulus surpasses 75GPa, is much better than D glass (Young's modulus is about 55GPa), also is improved than common E glass (Young's modulus is about 72GPa).
(3) glass fiber with low dielectric constant provided by the present invention has good moulded manufacturability, its mold temperature (temperature when glass viscosity is 1000 pool) (wire-drawing temperature) is no more than 1350 ℃, and (difference of glass ware forming temperature and crystallization ceiling temperature) (being Δ T) is greater than 80 ℃ between shaping area.
(4) glass fiber with low dielectric constant provided by the present invention has good thermostability, and its thermal expansivity is about 3.0-3.2 * 10 -6/ ℃, quite (thermal expansivity is about 3.2 * 10 with the E glass horizontal -6/ ℃), (thermal expansivity is about 5.4 * 10 obviously to be better than D glass -6/ ℃).Thereby, it during for the manufacture of printed circuit board (PCB) dimensional stability better.
The present invention does not have particular restriction to the preparation method of described glass fibre, is preferably the tank furnace method and produces.The typical process flow that the tank furnace method is produced glass fibre is as follows:
After according to component design that various raw material weighing are good, in mixing tank, mix, then add tank furnace by charging machine.In tank furnace, frit obtains stablizing the glass metal of high-quality after fusing under 1300 ℃ ~ 1700 ℃ the condition, clarification, homogenizing.
Above-mentioned glass metal flows out through platinum bushing plate in operation path, formed the glass yarn of diameter 3-24 μ m by the drawing wire machine quick traction, behind spray cooling, treating compound coating, boundling, be wound in spinning cake at drawing wire machine again, namely obtain glass fiber precursor, can be made into various glass fiber products through different aftertreatment technologys again.
Embodiment
Further specify technical scheme of the present invention below by specific embodiment, these embodiment can illustrate and not limit technical scheme of the present invention.
In order to compare with glass fibre of the prior art, present embodiment has provided chemical ingredients and the correlation detection data of common E glass and D glass, sees table 1 for details.
When the composition total content is less than or greater than 100% slightly in the table 1, can be understood as, a small amount of composition that remaining amount is equivalent to impurity or does not analyze, or the acceptable error that occurs in the analytical procedure of taking causes.
Embodiment 1-6:
Prepare glass fibre according to following method:
According to the prescription shown in the table 1, various raw material weighing are good after, in mixing tank, mix, then add tank furnace by charging machine.In tank furnace, frit obtains stablizing the glass metal of high-quality after fusing under 1300 ℃ ~ 1700 ℃ the condition, clarification, homogenizing.
Above-mentioned glass metal flows out through platinum bushing plate in operation path, and the glass yarn by drawing wire machine quick traction formation diameter 3-24 μ m is wound in spinning cake at drawing wire machine again behind spray cooling, treating compound coating, boundling, namely obtain glass fiber.
Comparative example 1-2:
According to the prescription shown in the table 1, prepare the glass fiber of comparative example 1-2 with method same as described above.Comparative example 1 is the E glass fibre, and comparative example 2 is D glass fibre.
The above-mentioned glass fiber for preparing is carried out performance measurement, and performance perameter and the method for mensuration are as follows:
(1) specific inductivity and dielectric loss
Embodiment medium dielectric constant microwave medium and dielectric loss are measured in accordance with the following methods:
By formula rate each raw material is mixed in the rear adding platinum crucible, at 1550 ℃ ~ 1600 ℃ lower insulation 8h, the glass metal of obtain evenly, clarifying; Glass metal is poured on the stainless steel mould of preheating, places in the retort furnace and make sheet glass after the annealing; Sheet glass is made thick about 1.5mm, is about the rectangular sheet of 4mm, wide about 3mm after cutting, grinding, polishing, and after silver electrode is coated on described rectangular sheet surface, at normal temperatures, with the 1MHz frequency specific inductivity and the dielectric loss of sample is measured; Examination criteria ASTM D150.
(2) wire-drawing temperature:
Wire-drawing temperature (T Log η=3) represent that glass viscosity is 10 3Temperature during pool, the temperature of glass metal when being equivalent to the glass fibre moulding is also referred to as the glass fibre mold temperature.Wire-drawing temperature adopts BROOKFIELD high temperature viscosity instrument to detect.
（3）ΔT：
Δ T represents T Log η=3With the difference of devitrification of glass ceiling temperature, be equivalent to the normally temperature range of wire-drawing shape of glass fibre.The devitrification of glass ceiling temperature adopts Orton Model crystallization gradient furnace to detect.
(4) thermal expansivity:
Thermal expansivity is the average thermal linear expansion coefficient of glass fibre between 25 ℃-300 ℃.Adopt ASTM D696 standard detection.Detecting instrument: the German NETZSCH DIL 402PC of company thermal dilatometer.
(5) Young's modulus (GPa):
Young's modulus (GPa) is according to the ASDM2343 standard detection.
The measurement result of above parameter is as shown in table 1:
The prescription of the glass fibre that table 1 embodiment of the invention and comparative example provide and performance perameter
Figure BDA00002535518700061
As can be seen from Table 1, glass fibre provided by the invention has excellent dielectric properties and thermostability, and its specific inductivity and dielectric loss are close to the D glass horizontal, and thermal expansivity can match in excellence or beauty with common E glass; Simultaneously, its wire-drawing temperature and Δ T can be controlled at than in the OK range again, thereby have good moulded manufacturability, can realize in more economical way the production of tank furnace method under present condition; In addition, glass fiber with low dielectric constant good mechanical properties of the present invention (Young's modulus 76-80GPa) obviously is better than D glass (Young's modulus 55GPa), can be the modern electronic product implement thinness and compactness and provides support.Therefore, glass fibre provided by the invention not only goes for conditional electronic level fiberglass Application Areas, also has more advantage at following high-performance electronic product with the glass fibre field.
The above only is preferred implementation of the present invention; should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.

Claims (5)

1. composition for the preparation of glass fibre, mainly the material by following weight percent forms:
SiO 260.4 ~ 65%, Al 2O 310 ~ 14%, B 2O 322 ~ 26% and Li 2O 0.5 ~ 2%.
2. composition according to claim 1, it is characterized in that: described composition mainly is comprised of the material of following weight percent: SiO 260.6 ~ 63.2%, Al 2O 311 ~ 13.2%, B 2O 324.2 ~ 26% and Li 2O 0.5 ~ 1.5%.
3. composition according to claim 1, it is characterized in that: described composition comprises that also weight percent content is at the CaO below 2%, MgO, ZnO, TiO 2, Fe 2O 3, ZrO 2, Na 2O or K 2O.
4. arbitrary described composition according to claim 1-3 is characterized in that: described composition be arbitrary in following (1)-(7) shown in:
(1) described composition is comprised of the material of following weight percent: SiO 262%, Al 2O 312.3%, B 2O 324.2% and Li 2O 1%, and surplus is impurity;
(2) described composition is comprised of the material of following weight percent: SiO 260.4%, Al 2O 312.2%, B 2O 326% and Li 2O 1%, and surplus is impurity;
(3) described composition is comprised of the material of following weight percent: SiO 265%, Al 2O 310%, B 2O 322.7% and Li 2O 2%, and surplus is impurity;
(4) described composition is comprised of the material of following weight percent: SiO 261%, Al 2O 311%, B 2O 325.8%, Li 2O 1.2% and TiO 20.8%, surplus is impurity;
(5) described composition is comprised of the material of following weight percent: SiO 263.1%, Al 2O 310.6%, B 2O 324.5% and Li 2O 1.5%, and surplus is impurity;
(6) described composition is comprised of the material of following weight percent: SiO 260.6%, Al 2O 313.2%, B 2O 325% and Li 2O 0.8%, and surplus is impurity;
(7) described composition is comprised of the material of following weight percent: SiO 263.2%, Al 2O 314%, B 2O 322% and Li 2O 0.5%, and surplus is impurity.
5. the glass fibre that is prepared by arbitrary described composition among the claim 1-4.
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CN103351102A (en) * 2013-06-25 2013-10-16 巨石集团有限公司 Glass fiber composition and low-dielectric constant glass fibers prepared from same
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