CN101549958A - Composition for high-performance glass fiber - Google Patents
Composition for high-performance glass fiber Download PDFInfo
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- CN101549958A CN101549958A CNA2009100267596A CN200910026759A CN101549958A CN 101549958 A CN101549958 A CN 101549958A CN A2009100267596 A CNA2009100267596 A CN A2009100267596A CN 200910026759 A CN200910026759 A CN 200910026759A CN 101549958 A CN101549958 A CN 101549958A
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- glass
- glass fibre
- composition
- glass fiber
- percent
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Classifications
-
- 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
- C03C3/095—Glass compositions containing silica with 40% to 90% silica, by weight containing rare earths
-
- 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 relates to a composition for high-performance glass fiber, which comprises 55 to 63 wt percent of SiO2, 23 to 26 wt percent of Al2O3, 11.5 to 14.5 wt percent of MgO, 0.5 to 2.5 wt percent of CeO2, 0 to 0.5 wt percent of LiO2, 0 to 1.5 wt percent of Bi2O3, 0 to 1.5 wt percent of WO3, and the balance of unavoidable impurities; the contents of the Li2O, the Bi2O and the WO3 can not be zero simultaneously. By adopting the composition as a raw material, the high-performance glass fiber can be produced by using a melting furnace and a fiber drawing furnace which are made from the existing fire resisting materials to perform melting and wire drawing. With reduced production difficulty and low cost, the composition has good producibility, is suitable for industrial continuous production and can save energy source, and the produced high-performance glass fiber can be used as the reinforcing material of a resin base composite material and has the advantages of high strength, corrosion resistance, high temperature resistance and light weight.
Description
Technical field
The present invention relates to a kind of composition for high-performance glass fiber, this glass fibre can be used in the advanced composite material field of high strength, high-temperature resistant, high acidproof contour performance requriements, belongs to special glass fibre composition field.
Background technology
Glass fibre is a kind of inorganic fibers of excellent property, strengthens the matrix material that resin can make excellent property with it.The used glass fibre in each field is alkali free glass fibre (E-glass) more than 90% in the world at present, its monofilament tensile strength is between 3038～3430MPa, Young's modulus is about 72000MPa, can not satisfy rocket motor case, missile case, light-duty military weapon far away, aircraft component, wind-power electricity generation, the contour performance composite products of senior sports goods need.Therefore since nineteen sixties, various countries competitively develop out the high strength glass fiber of various compositions, their intensity greatly more than 3920～4580MPa, the matrix material that makes with them, intensity height, light weight mainly are applicable to aspects such as space flight, aviation, military weapon.
The E-glass fiber compound is: SiO
2: 52～66wt%; CaO:16～26wt%; Al
2O
3: 12～16wt%; B
2O
3: 5～10wt%; MgO:0～5wt%; Na
2O+K
2O:0～2wt%; TiO
2: 0～0.8wt%; Fe
2O
3: 0～5wt%; Fluorine: 0～1.0wt%.The characteristics of E-glass are that liquidus temperature is low, are about 1149 ℃, and the service temperature of the production glass fibre of its permission is wide, are about 1038 ℃～1316 ℃.Advantex
TMGlass fiber composition (US5789329): SiO
2: 59～62wt%; CaO:20～24wt%; Al
2O
3: 12～15wt%; MgO:1.0～4.0wt%; Na
2O:0～2wt%; K
2O:0～2wt%; TiO
2: 0～0.9wt%; Fe
2O
3: 0～0.5wt%; Fluorine: 0～0.5wt%; SO
3: 0～0.5wt%.Compare with the E-glass fiber component in the composition design, maximum characteristics are to have removed B
2O
3, owing to contain B
2O
3Expensive raw material price, remove B
2O
3Promptly, do not use B in order to realize the low composition production of glass fibre
2O
3Also improved simultaneously the problem of environmental pollution.Advantex
TMThe temperature of fusion of glass is than E-glass height, and the glass fibre mold temperature is also than E-glass fibre height, so Advantex
TMGlass improves at aspects such as kiln design, smelting technology, fiberizing technology, overcome its found and fiberizing aspect difficulty.
The S-2 that U.S. AGY company produces
TMHigh-strength glass fibre (US3402055), its composition are designed to use in high-intensity application at first, as rocket motor case etc., extensive application are arranged also in bulletproof armour at present.Its composition only is that the oxide compound of silicon, aluminium, magnesium is formed, and its content is SiO
2: 65wt%, Al
2O
3: 25wt%, MgO:10wt%, the characteristics of glass fibre are tensile strength height (4600～4800MPa), but the glass ware forming temperature is higher, and its liquidus temperature is 1471 ℃, and the bushing temperature is up to 1571 ℃, the kiln that needs precious metal materials such as special refractory materials of use and platinum, rhodium to make liner is founded, drawing process condition harshness, the production cost height is difficult to carry out suitability for industrialized production in China.English Patent 1006524, its composition design is reasonable inadequately, its Al
2O
3Not the optimum tight stacking states in glass, Li
2O introducing amount is excessive, has not only improved cost, and has reduced chemical stability, and more toxic substance (Sb has also been introduced in this composition design
2O
3) make finings, both influenced HUMAN HEALTH, easily cause environmental pollution again.Chinese patent application 94111349.3 in order to promote the clarification of glass metal, adds the Fe of certain content in the frit composition in the composition design
2O
3Though, can play clarifying effect, bring the diathermancy of glass poor simultaneously, found problems such as degradation, Fe
2O
3It is painted to introduce the excessive glass fibre that obviously makes, and influences the color of glass fiber applications in matrix material, influences the matrix material outward appearance.In addition, too much Fe
2O
3Also easy and molybdenum electrode generation reduction reaction generates simple substance Fe, causes the platinum bushing to produce intoxication accident.
Summary of the invention
The objective of the invention is to problem at above-mentioned existence, propose a kind of high-performance glass fiber constituent of reasonable composition design, adopt the temperature tolerance and the acid resistance of high-performance glass fiber raising glass fibre in the tensile strength that improves glass fibre of this constituent preparation.
Composition for high-performance glass fiber of the present invention comprises following component:
SiO
2: 55～63wt%, Al
2O
3: 23～26wt%, MgO:11.5～14.5wt%, CeO
2: 0.5～2.5wt%, Li
2O:0～0.5wt%, Bi
2O
3: 0～1.5wt%, WO
3: 0～1.5wt%, the impurity that all the other are introduced for raw material, aforementioned Li
2O, Bi
2O
3, WO
3Content be not zero simultaneously.
In the said components, SiO
2, Al
2O
3, MgO is main component of the present invention, total content in the present invention is 94～98wt%, wherein, SiO
2Be main glass framework ingredient, an amount of raising of its content can improve glass intensity, acid resistance, temperature tolerance, but too high levels can make the high temperature viscosity of glass raise, thus make glass found performance and wire-drawing performance descends, the SiO that the present invention is fit to
2Content is 55～63wt%.Al
2O
3Can improve glass intensity, temperature tolerance, chemical stability, improve the melting properties of admixtion, improve the devitrification behavior of glass, along with Al
2O
3The increase of content, the glass structure densification, glass fiber strength improves thereupon, but surpasses 26% later on because Al
2O
3The change of ligancy makes glass structure lax on the contrary, causes intensity to reduce, and therefore reasonably designs Al
2O
3High-content should not surpass 26%.MgO can reduce the glass fibre forming temperature, prolong the operation life-span of bushing, content is crossed to hang down and can be made the glass melting degradation, and the high temperature viscosity of glass increases, easily make the glass devitrification during too high levels, the MgO content that the present invention is fit to is 11.5～14.5wt%.
Above-mentioned SiO
2-Al
2O
3-MgO system glass glass melting temperature height, high temperature viscosity are big, found, clarification, homogenizing difficulty, thereby cause performance such as glass fiber strength to reduce.For the high temperature viscosity that reduces glass, the glass melting temperature that reduction changes system glass, glass is founded easily, in composition design of the present invention, introduced Li
2O, Bi
2O
3Deng founding modified oxide, Li
2O is a kind of strong fusing assistant, can be under lower temperature and SiO
2Reaction generates silicate, can reduce the glass melting temperature of glass, reduces the viscosity of glass metal, accelerates the speed of founding of glass.But the introducing amount is unsuitable excessive, because excessive Li
2O destroys the siloxane bond structure (Si-O-Si) in the glass structure easily and forms the Si-O-Li key, has so just caused glass micro-crack to increase, strength degradation, and introduce Li
2The raw material of O such as Li
2CO
3Cost an arm and a leg, improved cost significantly, consider also can not too much add from the production cost angle; Bi
2O
3Be used as the fusing assistant of high-strength glass, in founding the high-strength glass process, especially in the glass fibre moulding process, an amount of Bi
2O
3Can guarantee the even of glass smelting, and make glass have suitable viscosity and recrystallization temperature, thereby guarantee the stable of glass fiber wire-drawing technology.In order to ensure the clear quality of glass metal, fully get rid of the bubble in the glass metal, obtain the glass of abundant homogenizing, in composition design of the present invention, introduce CeO
2, WO
3Deng the clarification modified oxide.CeO
2Be the representative species of the abundant rare earth mineral products of china natural resources, nontoxic, contain abundant, output is big, cost is low, it can not only reduce the viscosity of glass, and the reaction of at high temperature appraising at the current rate, and emits O
2, play good clarification, CeO
2Adding, can also improve the glass fibre processability, the producting process difficulty of high-strength glass fibre is reduced.WO
3Claim the surface tension activity agent again, can significantly reduce the surface tension of glass metal, thereby help the clarification of glass.
The CeO that is introduced among the present invention
2, Li
2O, Bi
2O
3, WO
3Total content Deng modified oxide is 2～6wt%, introduces wherein 2～4 kinds usually.Add can make that glass is easy to found behind these modified oxides, homogenizing, clarification and do not reduce the use properties of fiber, can reach and found homogeneous glass and the good purpose of glass diathermancy easily.
Unavoidable impurities is to bring Fe into by raw mineral materials among the present invention
2O
3, Na
2O, K
2Material such as O, CaO, the total content of this type of material should be controlled in the 1.0wt%, otherwise can reduce the diathermancy of glass and the performances such as intensity of glass fibre.Wherein, Fe
2O
3Content be controlled at 0～0.5wt%; Na
2O+K
2The content of O is controlled at 0～0.3wt%; The content of CaO is controlled at 0～0.2wt%;
Contained Fe among the present invention
2O
3Finish by impurities in raw materials and bring into, Fe
2O
3Introduce too much, glass colour is deepened, diathermancy is poor.And the present invention is with Fe
2O
3Content is controlled at below the 0.5wt%, and the diathermancy of glass is better, and the glass fibre color is more shallow.Therefore, thermal source when adopting fusion cast glass of the present invention can be founded with flame heating mode, Electric heating, the thermoelectricity combination is founded, compare with dark glass, increase available and founded means, by the matrix material that this glass fibre is made, the matrix material problem of appearance that also can avoid the dark glass fiber to cause.
Adopt composition for high-performance glass fiber fusion cast glass of the present invention, can adopt conventional flame heating device, electrically heated or thermoelectricity to found, thereby form homogeneous glass in conjunction with heating unit.Stove during fusion cast glass can adopt the melting furnaces of refractory materials silicon oxide, zirconium white-silicon oxide, Zirconia-alumina-silicon oxide, chromic oxide, aluminum oxide, mullite or white afrodite structure to carry out.
When adopting composition for high-performance glass fiber of the present invention to prepare glass fibre, can adopt the melting furnaces path of refractory materials zirconium white-silicon oxide, Zirconia-alumina-silicon oxide, chromic oxide, aluminum oxide, mullite or white afrodite structure to carry out single stage method wire drawing production, perhaps adopt the fiber drawing furnace of above-mentioned refractory materials structure to carry out two step method wire drawing production, promptly adopt high-performance glass fiber constituent fusion cast glass of the present invention earlier, use the glass-pulling glass fibre again.
The glass that adopts composition for high-performance glass fiber of the present invention to found, the viscosity that it is characterized in that melten glass is 10
3Glass fibre mold temperature during dPas is that (viscosity of so-called melten glass is 10 about 1380 ℃
3Glass fibre mold temperature during dPas is about 1380 ℃, be illustrated under the condition of high temperature of melten glass, viscosity is that the temperature of 1000 pools (poise) is about 1380 ℃), glass metal crystallization ceiling temperature is about 1410 ℃, the wire-drawing operation temperature is about 1460 ℃.The present invention has overcome U.S. S-2
TMThe shortcoming of the glass melting temperature height during products production, production unit cost costliness has also overcome S-2
TMThe problem of glass fibre mold temperature height (1471 ℃), wire-drawing operation temperature height drawing process condition harshnesses such as (1571 ℃).
The performance characteristic of above-mentioned high-performance glass fiber is that (nascent state intensity 4600～4800MPa) is higher than Advantex to the intensity height
TM(nascent state intensity 3100～3800MPa), temperature tolerance height (softening point temperature is about 965～970 ℃) are higher than Advantex to glass fibre
TMGlass fibre (softening point temperature is about 916 ℃); Acid resistance height (mass loss rate is 4.38%) is higher than Advantex
TMGlass fibre (mass loss rate is 6.2%).The high-performance glass fiber Hiper-tex of new generation that U.S. OCV company released in 2006
TMProduct (Chinese patent CN101300199A, CN101300200A), its nascent state intensity is 4100～4650MPa, softening temperature is 940～960 ℃.Hiper-tex
TMConstituent in contain MgO, CaO in the alkaline earth metal oxide, total amount is 16～20wt%, acidproof mass loss rate is 5.5%, and high-performance glass fiber constituent of the present invention mainly only contains MgO, content is 11.5～14.5wt%, CaO brings into the impurity form, and content is no more than 0.3wt%, and acidproof mass loss rate is 4.38%.Therefore intensity, temperature tolerance, the acid resistance of high-performance glass fiber of the present invention all are higher than Hiper-tex
TMAnd existing domestic high-strength glass fibre.
With the high-performance glass fiber of the present invention preparation polymer matrix composites as strongthener, intensity height, corrosion-resistant, high temperature resistant, light weight mainly are applicable to fields such as space flight, aviation, boats and ships, weapons, the energy, building, communications and transportation, electronics, environmental protection, wind-power electricity generation, senior sports goods.
Composition for high-performance glass fiber of the present invention has made full use of the china natural resources rich raw mineral materials, raw material source is wide, of high grade, cheap, by adding make that glass is easy to found, homogenizing, clarifying modified oxide, reach and found homogeneous glass and the good purpose of glass diathermancy easily.Adopting composition for high-performance glass fiber of the present invention is raw material, melting furnaces, the fiber drawing furnace of available existing refractory materials structure founded with wire drawing and produced high-performance glass fiber, reduced the production difficulty, cost is low, possesses good producibility, adapt to the serialization production of industry, but and save energy.
Composition for high-performance glass fiber of the present invention, mechanical property, heat resistance, acid resistance all are higher than the strong glass fibre (HS2 of present level
TM, HS4
TM) product.
Embodiment
Embodiments of the invention and S-2
TM, Advantex
TM, Hiper-tex
TM, HS2
TM, HS4
TMThe glass fibre correlation data is as shown in the table:
Chemical constitution by listed each prescription of last table calculates various raw material institute expense, accurately mix after the weighing and be mixed with admixtion, place platinum rhodium to found crucible, in 1510 ℃～1550 ℃ temperature ranges, fusion while stirring, founded 24 hours, obtain clarification, the glass metal of homogenizing, the glass metal that melts is banished on the heat-resisting steel sheet and plate, obtain frit block after the cooling, again the part of the glass that melts is put into single hole platinum rhodium fiber drawing furnace, fusion again under 1440 ℃～1450 ℃, by controlling conventional process for forming glass parameter (liquid level, hot(test)-spot temperature, the bushing temperature, drawing wire machine rotating speed etc.), be drawn into the continuous glass fibre that diameter is 5～22 μ m.Test diameter is the nascent state intensity of the various embodiments described above glass fibre of 7～8 μ m.The resistant glass fiber acid test be adopt diameter be the glass fibre of 10 μ m in 10wt%HCl solution, under 96 ℃ of conditions, soaked 24 hours, measure its rate of weight loss.The testing method of softening temperature is identical with other glass fibre softening temperature testing method, adopts the test of hang spring method.The mensuration of crystallization ceiling temperature, adopt fixed point recrystallization temperature test furnace, furnace for reproduction of fixed points is heated to assigned temperature, behind the insulation 60min, glass to be measured is put into furnace for reproduction of fixed points, and then insulation for some time 30min, taking out, whether have crystal separate out, regulate the furnace for reproduction of fixed points temperature according to observed result if observing under polarizing microscope, test again, finally obtain the crystallization ceiling temperature of glass.The mensuration of high temperature viscosity is to adopt U.S. BROOKFIELD high temperature viscosity instrument to measure.
Claims (10)
1, a kind of composition for high-performance glass fiber is characterized in that comprising:
SiO
2: 55～63wt%, Al
2O
3: 23～26wt%, MgO:11.5～14.5wt%, CeO
2: 0.5～2.5wt%, Li
2O:0～0.5wt%, Bi
2O
3: 0～1.5wt%, WO
3: 0～1.5wt%, all the other are unavoidable impurities; Aforementioned Li
2O, Bi
2O
3, WO
3Content be not zero simultaneously.
2, composition for high-performance glass fiber according to claim 1 is characterized in that described unavoidable impurities is Fe
2O
3, Na
2O, K
2O, CaO, its total content is controlled in the 1.0wt%, wherein:
Fe
2O
3：0～0.5wt％；
Na
2O+K
2O：0～0.3wt％；
CaO：0～0.2wt％；
3, composition for high-performance glass fiber according to claim 1 is characterized in that CeO
2, Li
2O, Bi
2O
3, WO
3The total content of four kinds of modified oxides is 2～6wt%.
4, adopt any glass that described composition for high-performance glass fiber is founded of claim 1 to 3, it is characterized in that to adopt conventional flame heating device, electrically heated or thermoelectricity to found, thereby form homogeneous glass in conjunction with heating unit.
5, glass as claimed in claim 4, the viscosity that it is characterized in that melten glass is 10
3Glass fibre mold temperature during dPas is about 1380 ℃, and the crystallization ceiling temperature is about 1410 ℃, and the wire-drawing operation temperature is about 1460 ℃.
6, as constituent preparation as described in any one of the claim 1 to 3 glass fibre, it is characterized in that by feed glass fiber-forming process parameter, the diameter of glass fibre is controlled at 5 μ m to 22 μ m.
7, glass fibre as claimed in claim 6 is characterized in that glass fibre nascent state intensity is 4600～4800MPa.
8, glass fibre as claimed in claim 6 is characterized in that the glass fibre softening point temperature is 965～970 ℃.
9, glass fibre as claimed in claim 6 is characterized in that glass fibre acid resistance mass loss rate is less than 4.5%.
10, any described glass fibre of claim 6 to 9 has application in the matrix material of high machinery, high corrosion resistance, high heat resistance requirement as strongthener in preparation.
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|---|---|---|---|
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| CN101549958B CN101549958B (en) | 2011-01-26 |
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