CN108191252A - A kind of doping Gd2O3Dielectric glass fibre and preparation method thereof - Google Patents
A kind of doping Gd2O3Dielectric glass fibre and preparation method thereof Download PDFInfo
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- CN108191252A CN108191252A CN201810265430.4A CN201810265430A CN108191252A CN 108191252 A CN108191252 A CN 108191252A CN 201810265430 A CN201810265430 A CN 201810265430A CN 108191252 A CN108191252 A CN 108191252A
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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
- C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
- C03C25/10—Coating
Abstract
The present invention provides one kind to have low-k and dieleetric glass fibre.The glass fibre is by adding rare earth oxide Gd2O3To optimize its dielectric properties and high-temperature behavior to be suitable for large-scale industrial production, and describe preparation method in detail.The glass fiber compound includes（In terms of weight %）SiO254 ~ 63%, Al2O38 ~ 21%, B2O314 ~ 26%, CaO+MgO 6 ~ 14%, Na2O+K2O 0 ~ 1, Gd2O30.5~7%.Glass fibre according to the present invention is suitble to do the reinforcing material of printed circuit board.Its dielectric properties is better than E glass, has preferable dielectric properties when frequency is 1MHz, dielectric constant is between 4.17 ~ 4.57, and dielectric loss is up to 6.32 × 10‑3~8.74×10‑3Between.
Description
Technical field
The present invention relates to a kind of rare earth doped oxide Gd2O3Dielectric glass fibre, which glues with high temperature
It spends low, is conducive to large-scale industrial production and can be used as the reinforcing material of printed circuit board.
Background technology
With the development of information industry, electronic product is towards micromation, lightening development, this is to operativeness of printed circuit boards
Propose higher requirement.Chief component wherein in printed circuit board is covers copper aluminium sheet, wherein covering copper aluminium sheet
Performance can directly influence the performance of electronics and IT products.Presently, there are main problem be still that dielectric properties are poor, by closing
It is formula：
（1）
V in formula：Signal velocity；K：Constant；ε：Printed circuit board dielectric constant；C：The light velocity
（2）
P：Power attenuation；U2：Forcing voltage；tanα：Printed circuit board dielectric loss；ω：Angular speed；C：The light velocity
Understand that dielectric constant and dielectric loss cross conference and influence the spread speed of signal and make signal intensity attenuation weak.By with
Upper analysis understands that we need to drop the dielectric constant and dielectric loss of low lying copper aluminium sheet.
Mainly include glass fibre and resin base covering copper aluminium sheet dielectric matrix, wherein resin-based dielectric constant exists
2.1 ~ 3.3, dielectric loss is 2 × 10-4~ 0.005, and commonly used glass fibre is mainly E glass in domestic and international circuit board at present
Glass fiber and D glass fibre.
Wherein, the composition of E glass fibres is：52% ~ 56% SiO2, the Al of l2% ~ 16%2O3, 5% ~ 10% B2O3, 16% ~
25% CaO, 0 ~ 5.0% Mg.With 3% ~ 5% Na2O+K2O.E glass fibres have that machinability is good, water-tolerant, price are low
The advantages that, but its dielectric constant is higher, is 6.7 or so, and its dielectric loss is larger, more than 10-3, it is impossible to meet densification
With the requirement of high speed information processing.
The composition of D glass fibre is：72% ~ 76% SiO2, 0% ~ 5% A12O3, 20% ~ 25% B2O3With 3% ~ 5% Na2O
+K2O.Its dielectric constant is 4.1 or so, and dielectric loss is 8 × 10-4Left and right, but D glass fibre has the disadvantages that：(1) phase
For E glass fibres, D glass fibre has the SiO of high level2, lead to the drilling of D glass fibre enhancing laminate
Can be poor, it is unfavorable for following process；(2) glass softening point of D glass fibre is high, and meltbility is poor, it is easy to vein and bubble are generated,
Cause to generate the problems such as wire-drawing operation is difficult, and glass fibre fracture of wire is more in spinning technique, therefore productivity and workability are all very
Difference, production cost is very high, is not easy to mass produce；(3) D glass fibre has very high melting temperature and wire-drawing temperature, generally
It is very harsh to kiln quality requirement at 1400 DEG C or more, furnace service life can be reduced；(4) D glass fibre water resistance is poor, holds
Easily cause the stripping of fiber and resin.
For case above, many researchs have also been made both at home and abroad.The patent 96194439.0 of Nitto Boseki Co. Ltd. is situated between
The dielectric glass fibre dielectric constant to continue fails to reach 4.2 hereinafter, still will appear in use higher in 4.2-4.8
Dielectric loss, while when corresponding ingredient examination in research process described according to its specification is molten, the glass of gained does not also obtain
Performance and processing performance described in the patent, and the viscosity of glass metal larger is unfavorable for industrialized production.U.S. PPG
The patent CN102531401A of Ohio Industrial Company is described reduces glass in the case where ensureing glass fibre dielectric properties
Forming temperature it is minimum can drop to 1244 DEG C, which meets the large-scale industrial production of glass, but shortcoming exists
It is more than 5.5 in dielectric constant is higher, and which introduce F elements, the introducings of F elements can in production cause environment serious
Harm.The patent CN102503153A of domestic Chongqing Polycomp International Co., Ltd describes a kind of glass with low dielectric constant
Fiber, dielectric constant can reach 4.1 ~ 4.5, but the forming temperature of its glass fibre is unfavorable for this at 1300 DEG C or so
The industrialized production of glass fibre.
Invention content
In view of this, the technical problem to be solved in the present invention is to provide a kind of dielectric glass fibre, and the present invention provides
Dielectric glass fibre have good craftsmanship and operability, relatively low dielectric constant and dielectric loss.
The present invention provides a kind of glass fibre with excellent dielectric performance, in terms of weight %, including following components：
SiO254 ~ 63%, Al2O38 ~ 21%, B2O314 ~ 26%, CaO+MgO 6 ~ 14%, Na2O+K2O 0 ~ 1, Gd2O3 0.5~7%。
Preferably, including：SiO258 ~ 60%, Al2O314 ~ 18%, B2O3 16~24%。
Preferably, including：CaO+MgO 4.5~12%.
Preferably, including：CaO 3.5 ~ 6%, MgO 3 ~ 6%.
Preferably, including：Na2O 0.1 ~ 0.7%, K2O 0.1~0.7%。
Preferably, including：Gd2O3Content is less than 5%.
Preferably, including：Gd2O3Content is less than 3%.
Main technological means is by introducing gadolinium oxide in glass ingredient in the present invention（Gd2O3）, and Gd2O3's
Introduce the high temperature viscosity that can significantly reduce glass fibre, the dielectric properties for improving glass.Rare earth Gd2O3With larger field
Strong and its radius is larger, can link multiple non-bridging oxygens and play the role of net mending, make its attached compared with conference additionally, due to its field strength
The bridging oxygen key of near and coupled group, which shifts, makes bridging oxygen key key weaken by force.It is understood based on above analysis：At high temperature,
Gd2O3Net mending key and be affected by it the bridging oxygen key easy fracture to shift, batch meltable generation can be made glass metal and to drop
The high temperature viscosity of low glass metal；In low temperature, Gd2O3Net mending effect play main function, on the one hand make the network structure of glass
Densification inhibits the movement of alkali metal and alkaline-earth metal, another aspect Gd2O3Link non-bridging oxygen can greatly reduce non-bridging oxygen
Polarization, so rare earth Gd2O3Addition can improve the dielectric properties of glass.Wherein Gd2O3If introduce it is excessive, can be due to
Its radius compared with havoc glass network structure, so Gd2O3It to add in right amount.Optimal restriction Gd in the present invention2O3Content is small
In 5%.
SiO2、B2O3、Al2O3In formation body of the glass kind as glass, the network structure of glass is formed and performance rises
Critical effect is arrived.Wherein SiO2It is the main body to form skeleton, if suitable addition SiO2It can be with the knot of oxygen-octahedron
Structure forms irregular contiguous network structure, which has higher key strong, be not easy to polarize under the action of external electric field, also not
It is also easy to produce the losses such as conductance and relaxation, suitable addition SiO2Have to the dielectric constant and dielectric loss that reduce glass brighter
Aobvious effect.SiO2During less than 50%, the dielectric properties of glass are poor.But SiO2Too high levels can cause the fusing point of glass it is high,
Viscosity of glass metal is excessive to cause fusing is difficult, energy consumption is excessive to be unfavorable for industrialized production.SiO2During more than 60%, glass smelting is stranded
Easy fracture when hardly possible, wire drawing.If in addition contain excessive SiO in glass ingredient2It can be because containing limited alkali metal oxygen in ingredient
The free oxygen that compound and alkaline earth oxide are provided is limited and increases glass containing non-bridging oxygen with each oxygen-octahedron
Dielectric constant and dielectric loss.In order to not only meet the needs of glass dielectric performance but also production needs can be met, in the present invention most
Excellent restriction SiO2Content 58% ~ 60%.
B2O3Itself it is Network former, glass can be individually formed.Boron atom can partly replace silicon in silicate glass
Atomic building network structure.B2O3Addition introduce B3+B-O is formed, the bond energy of the key is big compared with Si-O bond energys, in glass can be with
Play the role of stabilized glass network structure and to limit oxonium ion polarized.Therefore appropriate addition B2O3Jie of glass can be optimized
Electrical property.In addition, B2O3Have the function of to reduce high temperature viscosity and fluxing in glass, the high temperature viscosity of glass can be caused to drop
It is low in favor of save cost, conducive to industrial production.In addition B2O3There is low temperature thickening, make the compact structure of glass.But
With B2O3The devitrification range of the increase glass of content increases, in addition B2O3It is volatile to can cause environmental pollution, in production process
In should strictly control dosage.Optimal restriction B in the present invention2O3Content 16% ~ 24%.
Al2O3Although not being glass former, it can have an impact the network structure of glass and then to glass
Stability plays an important role.Al2O3Suitable addition can reduce the tendency towards devitrification of glass, improve chemical stability, improve
Thermal stability, and Al2O3Addition can mitigate erosion of the glass metal to refractory material.Al2O3Excessive addition causes glass
Fluid viscosity is excessive to make glass be more easy to crystallization, and due to Al instead3+Ionic polarizability it is larger, if Al2O3Glass can excessively be made
Poor dielectric performance.Optimal restriction Al in the present invention2O3Content 14 ~ 18%.
The bridging oxygen key that the addition of divalent alkaline-earth metal oxide CaO, MgO can destroy glass is easy to the viscosity reduction of glass
The production of glass, but the addition of alkaline earth oxide can be destroyed the dielectric properties of glass, therefore in the present invention
Optimal restriction CaO+MgO contents 4.5 ~ 12%.Again since MgO substitutions CaO can be improved the dielectric properties of glass, but MgO
Excessively it will appear split-phase, so MgO and CaO additive amounts are appropriate.Optimal restriction CaO content 3.5 ~ 6% in the present invention, at this
Optimal restriction content of MgO 3 ~ 6% in invention.
Alkali metal oxide Na2O and K2O can be used as fluxing agent and fining agent to use addition, Na2O and K2O is a small amount of to be added
The high temperature viscosity that glass can be made by adding significantly reduces, but when its content be more than 1% when glass dielectric constant and dielectric loss can significantly increase
Add.Therefore to accomplish the minimum of alkali metal additive amount as possible.Optimal restriction Na in the present invention2O+K2O contents 0 ~ 1, wherein
Na2O contents 0.1 ~ 0.7%, K2O content 0.1 ~ 0.7%.
The preparation method of dielectric glass fibre of the present invention, including step once：
Step 1: it is matched according to raw material components, raw material needed for preparation, and by feedstock Particle size requirement（≤1.5mm）Carry out powder
Broken processing, will be machined to satisfactory raw material and be mixed into batch in proportion to be placed in uniform batch mixing in blending tank；
Step 2: it is 1590 ~ 1630 DEG C of kilns that the raw material obtained by step 1 is sent into hot(test)-spot temperature through furnace hopper, spiral feeder
It is melted in pond, clarification homogenizing, needs in the environment to keep the temperature glass metal 3 ~ 6h in the process in favor of clarification homogenizing；
Step 3: the good glass metal of clarification homogenizing flows through platinum of the temperature at 1290 ~ 1350 DEG C in operation path in step 2
Bushing and passing through, which is let slip a remark, outflow liquid glass fiber and passes through cooling gas and cooling water is cooled down to obtain glass fibre.Herein
The leakage hole number of platinum bushing plate can be between 1000 ~ 2000 in the process；
Step 4: by coated glass fiber size obtained by step 3, and ensure glass fibre by controlling wire drawing machine rotating speed
Parameter to be drawn into silk.Wire drawing machine revolution is adjustable at 2500 ~ 3000 turns, 5 ~ 10 μm of gained glass fiber diameter.
Embodiment
The present invention will be illustrated by following serial specific embodiment, however it will be understood by those skilled in the art that according to this
The principle of invention is expected many other embodiments.
Embodiment 1 ~ 7
The raw material of the present invention can not only be prepared into glass but also can be prepared into glass fibre.The method for preparing glass is to melt raw material
The glass metal melted is cast, is annealed；The method for preparing glass fibre is on the basis of drawing process by manufactured glass metal
Upper carry out wire drawing.Since certain test events can not directly use glass fibre, in order to be more convenient the items of test glass fibre
Performance, therefore the glass for preparing same recipe is detected.
Remarks：
1）Dielectric properties：Dielectric using Keysight E4990A precise impedances analyzers determination sample under 1MHz frequencies is normal
Number and dielectric loss；
2）Glass forming temperature：It is detected using BROOKFIELD high-temperature viscosimeters, it is glass to take the temperature value corresponding to Lg3.0
Forming temperature；
3）Liquidus temperature：Liquidus temperature is detected using SKL-8-12-14 tubular type gradient resistances stove.
Raw material is weighed according to the composition of raw materials of the following table 1, is prepared into glass sample, the preparation method of glass is as follows：It will prepare
Glass raw material be uniformly mixed and be placed in platinum crucible, melting temperature is carried out in lift thermal gradient furnace and is maintained at 1450 DEG C about
3h causes glass metal to clarify bubble-free.The glass metal clarified is poured on to the liter of the atmosphere on graphite jig and at 600 ~ 700 DEG C
2h annealing is kept the temperature in drop formula thermal gradient furnace to eliminate inside glass stress.Then glass blocks is cooled to room temperature.Glass is cut into 10
Then by glass polishing, glass blocks surface is cleared up, and be put into vacuum drying with alcohol for the normal glass block of mm × 10 mm × 5mm
Case is dried.With Keysight E4990A precise impedances analyzers under 1MHz frequencies the dielectric constant of determination sample and Jie
Electrical loss, dielectric constant and dielectric loss can directly be read.
Table 1
| Embodiment | 1 | 2 | 3 | 4 | 5 | 6 | E glass | D glass |
| SiO2 | 58.41 | 58.15 | 59.36 | 59.13 | 59.29 | 59.06 | 53.90 | 72.50 |
| Al2O3 | 15.86 | 16.50 | 15.28 | 14.02 | 14.21 | 17.54 | 14.80 | 1.50 |
| B2O3 | 15.73 | 15.36 | 16.36 | 18.20 | 17.23 | 21.40 | 7.90 | 21.50 |
| CaO | 4.79 | 4.45 | 4.87 | 4.25 | 4.13 | 4.96 | 22.80 | 0.5 |
| MgO | 4.21 | 4.54 | 4.13 | 4.03 | 4.14 | 4.04 | 0.35 | 0.5 |
| Na2O+K2O | 1 | 1 | 1 | 1 | 1 | 1 | 0.1 | 3.5 |
| Gd2O3 | 0.5 | 1.5 | 2.5 | 4 | 6 | 7 | 0 | 0 |
Above-mentioned glass is tested for the property, as a result referring to table 2.Wherein,T lonη=3For glass fibre forming temperature,T LiquidRepresent glass
The glass recrystallization temperature upper limit；△ T are the difference of glass forming temperature and devitrification of glass temperature upper limit.
The glass properties tables of data that 2 embodiment of table is provided with comparative example
| Sample | 1 | 2 | 3 | 4 | 5 | 6 | E glass | D glass |
| Dielectric constant 1MHz | 4.32 | 4.17 | 4.23 | 4.27 | 4.42 | 4.57 | 6.80 | 4.20 |
| Dielectric loss × 10-3 | 6.71 | 6.32 | 6.54 | 7.86 | 6.85 | 8.74 | 90.00 | 10.00 |
| T lonη=3（℃） | 1244 | 1256 | 1254 | 1233 | 1220 | 1216 | 1206 | 1422 |
| T Liquid（℃） | 1187 | 1175 | 1191 | 1163 | 1159 | 1123 | 1098 | 1265 |
| △T（℃） | 57 | 81 | 63 | 70 | 61 | 95 | 108 | 157 |
As shown in Table 2, glass provided by the invention has that preferably dielectric properties, forming temperature be low and glass forming temperature and a glass
The difference of glass liquidus temperature is all much larger than 50 DEG C, it is ensured that in drawing process is not in crystallization.The present invention provides
The dielectric constant minimum of glass can reach 4.17 dielectric properties for being much better than E glass, and dielectric properties and D glass dielectrics
It can be close.And the forming temperature of the glass is minimum up to 1216 DEG C, and glass forming temperature temperature is relatively low compared with D glass.
It can be by adding rare earth oxide Gd from glass sample provided by the invention2O3Come to the dielectric properties of glass and
High-temperature behavior has an impact.Rare earth Gd2O3Appropriate addition can be such that the dielectric constant of glass and dielectric loss significantly drops
It is low.It can be run counter to desire if excessive addition so that the dielectric constant and dielectric loss of glass increase.In addition, rare earth element adds
Can also the high temperature viscosity of glass be generated certain influence by adding, and the addition of rare earth element can reduce the forming temperature of glass, this
So that the glass with excellent dielectric performance puts into production.
The condition of the invention that can be provided simultaneously with excellent dielectric properties and can be easy to produce is understood by more than comparative analysis.
It can be widely used in printed circuit board as reinforcing material.
Finally it should be noted that：Obviously, above-described embodiment is just for the sake of clearly demonstrating the application example, so
And it is not intended to limit the embodiments.For the those of ordinary skill in the field, may be used also on the basis of the above description
To make other various forms of variations or variation.There is no necessity and possibility to exhaust all the enbodiments.And thus institute
Among the obvious changes or variations amplified out are still in the protection domain of the application type.
Claims (10)
1. a kind of dielectric glass fibre, it is characterised in that including rare earth Gd2O3。
2. dielectric glass fibre according to claim 1, it is characterised in that comprising following components, in terms of weight %：
SiO254 ~ 63%, Al2O38 ~ 21%, B2O314 ~ 26%, CaO+MgO 6 ~ 14%, Na2O+K2O 0 ~ 1%, Gd2O3 0.5~
7%。
3. dielectric glass fibre according to claim 2, it is characterized in that frequency is the dielectric constant of 1MHz at room temperature
（Dk）It is 4.17 ~ 4.57.
4. dielectric glass fibre according to claim 2, it is characterized in that frequency is the dielectric loss of 1MHz at room temperature
（Df）It is 6.32 × 10-3~8.74×10-3。
5. dielectric glass fibre according to claim 2, be characterized under 1000 pool viscosity no more than 1260 DEG C into
Type temperature TF。
6. glass fibre according to claim 2, which is characterized in that % by weight is counted, Gd2O3Content is less than 5%.
7. glass fibre according to claim 2, which is characterized in that % by weight is counted, Gd2O3Content is less than 3%.
8. the glass fibre with more excellent dielectric properties according to described in claim 1-7, is characterized in terms of weight %, comprising：
SiO258 ~ 60%, Al2O314 ~ 18%, B2O316 ~ 24%, CaO+MgO 4.5 ~ 12%, Na2O+K2O 0 ~ 1%, Gd2O3 0.5~3%。
9. the glass fibre with more excellent dielectric properties according to described in claim 1-8, is characterized in terms of weight %, comprising：
CaO 3.5 ~ 6%, MgO 3 ~ 6%, Na2O 0.1 ~ 0.7%, K2O 0.1~0.7%。
10. the dielectric glass fibre according to described in claim 1 ~ 9, is characterized in that：The method step is as follows：
Step 1: being matched according to raw material components, raw material needed for preparation, and processing is crushed by feedstock Particle size requirement, it will
Be machined to satisfactory raw material in proportion uniform batch mixing to be mixed into batch；
Step 2: by the raw material obtained by step 1 through being sent into hot(test)-spot temperature to be melted, being clarified in 1570 ~ 1610 DEG C of kiln ponds
Change；
Step 3: the good glass metal of clarification homogenizing flows through platinum of the temperature at 1270 ~ 1320 DEG C in operation path in step 2
Bushing and passing through, which is let slip a remark, outflow liquid glass fiber and passes through cooling gas and cooling water is cooled down to obtain glass fibre；
Step 4: by coated glass fiber size obtained by step 3, and ensure glass fibre by controlling wire drawing machine rotating speed
Parameter（5 ~ 10 μm of diameter）To be drawn into silk.
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| CN201810265430.4A CN108191252A (en) | 2018-03-28 | 2018-03-28 | A kind of doping Gd2O3Dielectric glass fibre and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115304282A (en) * | 2022-09-09 | 2022-11-08 | 清远忠信世纪电子材料有限公司 | Low-dielectric-constant glass fiber containing lanthanum oxide |
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| CN115304282A (en) * | 2022-09-09 | 2022-11-08 | 清远忠信世纪电子材料有限公司 | Low-dielectric-constant glass fiber containing lanthanum oxide |
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