CN105174732A - High-strength glass fiber as well as preparation method and applications thereof - Google Patents
High-strength glass fiber as well as preparation method and applications thereof Download PDFInfo
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- CN105174732A CN105174732A CN201510579963.6A CN201510579963A CN105174732A CN 105174732 A CN105174732 A CN 105174732A CN 201510579963 A CN201510579963 A CN 201510579963A CN 105174732 A CN105174732 A CN 105174732A
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Abstract
The invention relates to a high-strength glass fiber with excellent mechanical properties as well as a preparation method and applications thereof. The high-strength glass fiber is mainly prepared from the following raw materials in percentage by weight: 55-60% of silica sand, 20-23% of calcined alumina, 7-10% of blast furnace slag, 5-9% of CaO, and 8-10% of MgO. The high-strength glass fiber can be used as an ideal reinforced base material of high-performance composite materials, and widely applied to the fields of windmill blades and space shuttles and the like with higher specific strength and specific elastic modulus requirements.
Description
Technical field
The invention belongs to fibre technology field, relate to high strength glass fiber of a kind of excellent in mechanical performance and its production and use.
Background technology
The most frequently used glass composition for the manufacture of continuous glass fibre precursor is non-alkali glass, strengthens with it the matrix material that resin can obtain excellent property.But along with the expanding day of alkali free glass fibre Application Areas, with regard to the mechanical property that alkali free glass fibre is current, it can not meet the requirement of light-duty military weapon, aerospace parts, special purpose trolley part and field of wind power generation far away, all needs to seek to be applicable to having the matrix material that more high strength, erosion resistance and high thermal resistance good quality are light.
This matrix material can be made to meet the requirements at the higher level in these fields by improving fortifying fibre.
For above situation, scientific research institution of many enterprises has carried out large quantity research, to improve glass fibre mechanics mechanical property by every means.As United States Patent (USP) 3402055, its tensile strength is significantly increased than alkali free glass fibre, but its liquidus temperature is up to more than 1471 DEG C, bushing temperatures as high 1571 DEG C, production difficulty is very large, adds the erosion of glass metal to kiln refractory materials, shortens the life-span of platinum bushing plate, substantially increase its production cost, be therefore difficult to apply.As Chinese patent 94111349.3, in order to improve the crystallization property of glass, relatively large introduces Fe
2o
4, but Fe
2o
3introduce the melting properties that the excessive diathermancy that can reduce glass metal affects glass metal, and obviously make glass fibre painted, too much Fe
2o
3also be easily reduced to fe by molybdenum electrode, cause platinum bushing plate to produce intoxication accident.
In view of the above circumstances, for meeting military, electronics and the industry needs such as civilian, the invention describes one both comparatively can increase substantially mechanics mechanical property by alkali free glass fibre, and had the reinforcing glass fiber compared with high performance-price ratio.
CN102786223A discloses a kind of high strength glass fiber composition, and described high strength glass fiber major ingredient is: 56-65wt%SiO
2, 18.5-25.8wt%Al
2o
3, 11.5-23.0wt%RO (RO is CaO, MgO, SrO and BaO sum), 0.1-1.0wt%CeO
2and 0.1-0.8wt%Li
2o.But the specific tenacity of described fiber and also need to improve further than Young's modulus and could meet its application requiring in the field such as air vane, space shuttle.
Summary of the invention
The object of the invention is to, for above-mentioned Problems existing, propose a kind of high strength glass fiber and its production and use, the fiberization temperature of described glass fibre is low, and tensile strength, temperature tolerance, erosion resistance and acid resistance are all higher.
For reaching this object, the present invention by the following technical solutions:
On the one hand, the invention provides a kind of high strength glass fiber, described glass fibre weight percentage prepares primarily of following raw material:
Calcined polishing aluminum oxide is the high-purity mangesium oxide aluminum feedstock adopting " Bayer process " obtained, obtains alpha-alumina powder through the temperature lower calcination of 950-1200 DEG C; Water ratio≤1.0%, iron level≤0.15%; The compound of fluorine and boron is not all contained in described each component;
The blast furnace slag adopted in formula material is the product after steel-making, could use after steps of processing;
1) blast furnace slag adopted is through high temperature (1300 DEG C) above chilling (shrend); In this blast furnace slag, the content of Fe is less than or equal to 0.3%, and not objectionable constituent such as boracic and fluorine completely;
2) carry out after adopting equipment for removing ferric ion to remove ferrous contaminants to the blast furnace slag of chilling grinding reach 300 orders full by granularity requirements, then in homogenizing bin, carry out homogenizing.
In described glass fibre, the weight percentage sum of each raw material is 100%.
Described glass fibre weight percentage contains 55-60% silica sand, as 55%, 56%, 57%, 58%, 59% or 60% etc.; 20-23% calcined alumina, as 20%, 21%, 22% or 23% etc.; 7-10% blast furnace slag, as 7%, 8%, 9% or 10% etc.; 5-9%CaO, as 5%, 6%, 7%, 8% or 9% etc., with 8-10%MgO, as 8%, 9% or 10% etc.
High strength glass fiber of the present invention is by introducing containing Fe
2o
3lower Calcined polishing aluminum oxide replacement agalmatolite reduces impurity introducing and ensure that the purity changing glass ingredient, remains the mechanical strength of said composition most possibly, also improves the diathermancy of glass metal simultaneously, reduce energy consumption, stably manufactured.The present invention, by using appropriate blast furnace slag, introduces about 6-12% according to specific needs, reaches the object reducing fusing difficulty and reduce energy consumption.
This glass formula, on the basis of traditional silicon, aluminium, magnesium TERNARY GLASS, makes it be in high-temperature stable compositing area by the blend proportion of adjustment silicon, aluminium, magnesium, and ensure that the mechanics mechanical property of final fiber by adjustment proportions.
Described high strength glass fiber weight percentage mainly comprises following component:
Wherein RO is CaO, MgO, SrO and BaO sum.
Described high strength glass fiber composition also comprises 0.1%-0.15%CeO
2, as 0.11%, 0.12%, 0.13%, 0.14% or 0.15% etc.
Preferably, described glass fibre also comprises ZnO, TiO of being no more than 2wt%
2, ZrO
2, Fe
2o
3, Y
2o
3, MnO
2.
The weight percentage sum of described CaO and MgO is not less than 17%, is not more than 19%; And MgO/ (CaO+MgO) >=0.25, MgO/ (CaO+MgO)≤0.7.
Described SiO
2with Al
2o
3weight percentage sum be not less than 82%.
In order to effectively improve the tensile strength of fiber of glass fibre, acid resistance, temperature tolerance and erosion resistance, improving the melting properties of admixtion, improving the devitrification behavior of glass, by SiO in whole glass ingredient
2get about 60-62wt%, Al
2o
3get 20-25%wt%, sum of the two is not less than 82wt%.Simultaneously in order to reduce fiberization temperature and the high-temperature viscosity of glass fibre, extend the work-ing life of platinum bushing plate, the content of MgO that the present invention is applicable to is 8-10%%.
Above-mentioned SiO
2-Al
2o
3the glass melting temperature of-MgO system is high, clarifies poor and wire-drawing operation difficult, for the feature of this glass composition, adopts fluorite and boron compound as fusing assistant in conventional fiber glass, but fluorine wherein and the equal highly volatile of boron very harmful to air.Completely not fluorine-containing and boron in the present invention, thus reduce the destruction to bulk glass bond structure.
For the feature of this glass composition, introduce chemical composition in glass composition of the present invention single, Fe
2o
3the Calcined polishing aluminum oxide that content is lower replaces a certain amount of agalmatolite, both the use pressure of pyrophyllite deposit had been reduced, the unnecessary impurity in glass can be reduced again, improve the diathermancy of glass metal, effectively reduce the fiberization temperature of glass metal, reduce the use pressure of passage temperature and kiln, and significantly improve the color of glass fibre, alleviate the corrosion to platinum bushing plate, extend the work-ing life of bushing.
Calcined polishing aluminum oxide is by bauxite (Al
2o
3h
2o and Al
2o
33H
2o) with high temperature hydrogen sodium hydroxide solution dipping after pulverizing, sodium aluminate solution is obtained; Cross and filter to remove residue, filtrate lowered the temperature and add aluminum hydroxide crystals, through stirring for a long time, sodium aluminate solution can divide and parses aluminum hydroxide precipitation; Precipitate and separate is out cleaned, then at the temperature lower calcination of 950-1200 DEG C, just obtains alpha-alumina powder (mother liquor reusable edible).
Clear up problems to improve glass metal further, add be greater than 1% and be less than 0.15% CeO
2used in combination with the blast furnace slag through calcining, reach good clarifying effect.CeO
2when addition is greater than 0.15%, there is no obvious effect, and after usage quantity is less than 1%, the trend that not only cost obviously raises but also clarifying effect does not increase further.Cerium oxide is the oxide compound that appraises at the current rate, and cerium dioxide pyrolytic decomposition goes out oxygen, and it is more from isolated oxygen its Chemical bond key that temperature often raises 1 degree Celsius of energy, and clarification is larger.And the solubility with temperature of oxygen raises and reduces, thus produce clarification.Formula of the present invention needs higher glass melting temperature, and cerium oxide is suitable finings.Release the oxygen of nascent state in the reaction simultaneously, also can by iron (Fe at a low price
2+) be oxidized to ferric oxide, reduce glass coloring further, because trivalent Fe
3+tinting strength be only equivalent to Fe
2+1/10, so in use, the usage quantity of blast furnace slag can be increased.Cerium oxide also serves the effect of glass chemistry discoloring agent in this formula, and cerium oxide has higher oxidation potential, so better than traditional finings, use simultaneously have splendid combination with the blast furnace slag through calcining.
Due to CeO
2under high temperature, valence state changes and releases oxygen, and on the one hand can play the effect of clarification by stirred glass liquid, oxidizing atmosphere can make blast furnace slag better balance its reductibility on the other hand.
Because this glass formula more common alkali free glass fibre clarification processing temperature rises about 140 DEG C, in order to solve fusing and clear up problems, the energy distribution ratio that first design modifying electricity fusing-aid is shared in whole fusing; Steady and continuous can producing on the kiln not having electricity fusing-aid of common E glass.And the production of this glass formula, electricity fusing-aid becomes requisite assembly.Electricity fusing-aid is the mode adopting electrode directly to insert glass liquid heating, and capacity usage ratio is high, and the temperature of glass liquid of ate electrode up to more than 1700 DEG C, can have good effect to the fusing of pressure glass metal.The electricity fusing-aid power of increase melting area and settling section and energy input can improve the job stabilization of this glass formula effectively.The too low meeting of electricity fusing-aid energy input ratio causes glass melting slow, easily produces and do not melt raw material calculus completely during wire drawing, makes the flow of wire-drawing operation can not operation at full capacity, can not meet quantity-produced requirement; The too high meeting of electricity fusing-aid energy input ratio causes temperature of glass liquid wayward and all temperature of glass liquid is not too high, accelerate the erosion of kiln refractory materials, and more blub can be produced, simulation and the actual adjustment of kiln is founded through laboratory repeatedly, finally determine electricity fusing-aid energy input ratio between 20%-35% according to the thawing settling time of this formula admixtion, the energy consumption input of melting area accounts for the glass that the whole 60-85% founding kiln energy input can obtain fine melting rate and clarification.Electricity fusing-aid power input melting area accounts for the 40-60% of total electricity fusing-aid power, settling section 30-35%, and melting area and settling section electricity fusing-aid power summation are no less than 72%; Electricity fusing-aid electric current is not higher than 420A, and voltage is not higher than 120V, and electrode adopts water cycle cooling, and watercooling jacket temperature can not more than 800 DEG C.Direct wire-drawing shape on the suitable platinum rhodium bushing of E glass can produced after this glass compositions melt homogenizing.
The fibrosis performance of glass composition of the present invention comprises: fiberization temperature, liquidus temperature and Δ T.Fiberization temperature is defined as the temperature that viscosity is 1000 pools; Reduce fiberization temperature, flow attachment work-ing life can be increased, be easy to produce, greatly reduce production cost.Liquidus temperature is defined as the top temperature of balance between the liquid phase of matrix cystal with it of glass, forms crystal, fiberizing is interrupted lower than being easy to during this temperature.Another fibrosis performance is Δ T, is defined as the difference of fiberization temperature and liquidus temperature, and larger Δ T is conducive to fiberizing, reduces the control overflow to process facility, is easy to control to reduce production cost.
The admixtion of glass of the present invention preferably comprises above institute determinant and makes fiber and have fiberization temperature lower than about 1300 DEG C, and at least about the Δ T of 70 DEG C.Fiber prepared by this glass composition has the tensile strength of fiber exceeding alkali free glass fibre more than 20%.
This glass ingredient is owing to removing the very strong fluorine-containing mineral of fluxing capabilities completely, and the fusing clarification of glass becomes more difficult, explores and parameter simulation use Fe through great many of experiments
2o
3the lower Calcined polishing aluminum oxide of content, as a kind of main raw material, effectively can improve the melting capacity of glass metal.Add CeO
2mainly consider clearing up problems of high-viscosity glass liquid in the design.Steel-making byproduct-the blast furnace slag meanwhile with greater activity also substantially improves fusing and the clarification of this glass as a kind of main raw material.
In the present invention, in addition to the aforementioned ingredients, the TiO of total amount 2wt% is at the most introduced
2, SrO, ZnO, Fe
2o
3, P
2o
5, MnO
2, ZrO
2, Cr
2o
3, Y
2o
3deng composition, the introducing of these compositions plays improvement result energetically to glass high-temperature stability, also further increases the tensile strength of glass fibre.
The tensile strength of described glass fibre is for being not less than 6400MP, and Young's modulus is not less than 110GPa.
Present invention also offers the preparation method of described glass fibre, described glass fibre prepares through melt drawing.
Carry out in the described common refractory tank furnace be melted in electricity fusing-aid structure, electricity fusing-aid accounts for more than 20% of energy input total amount; The energy consumption input of melting area accounts for the whole 60-85% founding kiln energy input.
Preferably, the fiberization temperature of described wire drawing is not higher than 1350 DEG C.
Preferably, the difference Δ T of described fiberization temperature and crystallization ceiling temperature is not less than 80 DEG C.
Described wire drawing adopts the direct wire-drawing operation of common platinum rhodium bushing to produce.
Present invention also offers the purposes of described glass fibre, it is applied to defence and military, electronic application or civilian industry.
Enhancing base material containing glass fibre of the present invention is applicable to require to use in the application of higher and low weight at strength and stiffness, comprises defence and military, electronic application, civilian industry and other association areas.
Compared with prior art, beneficial effect of the present invention is:
The fiberization temperature of glass fibre provided by the invention is low, tensile strength is not less than 6400MP, Young's modulus is not less than 110GPa, and temperature tolerance, erosion resistance and acid resistance are all higher, be applicable to the high field of strength and stiffness requirement and defence and military, electronic application, civilian industry and other association areas.
Embodiment
Following according to case study on implementation, the present invention is described in detail, and the embodiment glass composition listed in table 1 is all the compositions based on the claims in the present invention.
Embodiment 1
Through remove the aluminum oxide after impurity fully calcined at about 1100 DEG C after, control moisture within 1.0%, iron level is 0.15%, Task-size Controlling 200 orders full by;
From the blast furnace slag of steel-making blast furnace through more than 1300 DEG C high-temperature quenchings, carry out iron removal system process, detection control iron level is less than or equal to 0.3%, with Raymond mill, granularity (300 orders full by) required for producing to glass fibre, add a certain amount of oxidative compound according to the oxidation-reduction quality of the blast furnace slag detected while grinding to be in harmonious proportion, e.g., vitriol (about 1 ton of blast furnace slag adds 1 to 10Kg oxidative compound).
Take 200Kg Calcined polishing aluminum oxide, blast furnace slag that 100Kg grinding is good, detect its composition, according to formula calculation, add the raw mineral materialss such as 90Kg magnesium oxide, 60Kg unslaked lime, 550Kg silica sand and be mixed with the admixtion about 1 ton of composition as table 1, add the CeO being not more than total dosage weight ratio 1% in addition
2as finings, in the tank furnace of electricity fusing-aid structure, melting is founded, and the glass uniform glass liquid through fully clarifying is delivered directly to wire drawing on platinum rhodium bushing through passage and makes glass fibre.
Embodiment 2
As embodiment 1, take 230Kg Calcined polishing aluminum oxide, blast furnace slag that 70Kg grinding is good, detect its composition, according to formula calculation, add 80Kg magnesium oxide, the raw mineral materialss such as 50Kg unslaked lime, 570Kg silica sand are mixed with the admixtion about 1 ton of composition as table 1, and in tank furnace, melting is carried out founding drawn glass fiber.
Embodiment 3
As embodiment 1 takes 200Kg Calcined polishing aluminum oxide, blast furnace slag that 70Kg grinding is good, detect its composition, according to formula calculation, add 80Kg magnesium oxide, 50Kg unslaked lime, the raw mineral materialss such as 600Kg silica sand are mixed with the admixtion about 1 ton of composition as table 1, and in tank furnace, melting is carried out founding drawn glass fiber.
Embodiment 4
As embodiment 1 takes 210Kg Calcined polishing aluminum oxide, blast furnace slag that 70Kg grinding is good, detect its composition, according to formula calculation, add 100Kg magnesium oxide, the raw mineral materialss such as 50Kg unslaked lime, 570Kg silica sand are mixed with the admixtion about 1 ton of composition as table 1, and in tank furnace, melting is carried out founding drawn glass fiber.
Embodiment 5
As embodiment 1 takes 200Kg Calcined polishing aluminum oxide, blast furnace slag that 70Kg grinding is good, detect its composition, according to formula calculation, add 90Kg magnesium oxide, the raw mineral materialss such as 90Kg unslaked lime, 550Kg silica sand are mixed with the admixtion about 1 ton of composition as table 1, and in tank furnace, melting is carried out founding drawn glass fiber.
Detect the tensile strength of the glass fibre that embodiment 1-5 obtains, Young's modulus, liquidus temperature, fiberization temperature, density and △ T, result is as shown in table 1.
Table 1
Glass fiber single filament intensity of the present invention, apparently higher than E glass fibre with abroad without boron floride-free glass fibre, all improves more than 60%, and Young's modulus improves more than 30%.
Comparative example 1-5
Described comparative example is the embodiment 1-5 in CN102786223A.
Applicant states; the foregoing is only the specific embodiment of the present invention; but protection scope of the present invention is not limited thereto; person of ordinary skill in the field should understand; anyly belong to those skilled in the art in the technical scope that the present invention discloses; the change that can expect easily or replacement, all drop within protection scope of the present invention and open scope.
Claims (10)
1. a high strength glass fiber, is characterized in that, described glass fibre weight percentage prepares primarily of following raw material:
Calcined polishing aluminum oxide is the high-purity mangesium oxide aluminum feedstock adopting " Bayer process " obtained, obtains alpha-alumina powder through the temperature lower calcination of 950-1200 DEG C; Water ratio≤1.0%, iron level≤0.15%; The compound of fluorine and boron is not all contained in described each component;
The blast furnace slag adopted in formula material is the product after steel-making, could use after steps of processing;
1) blast furnace slag adopted is through high temperature (1300 DEG C) above chilling (shrend); In this blast furnace slag, the content of Fe is less than or equal to 0.3%, and not objectionable constituent such as boracic and fluorine completely;
2) carry out after adopting equipment for removing ferric ion to remove ferrous contaminants to the blast furnace slag of chilling grinding reach 300 orders full by granularity requirements, then in homogenizing bin, carry out homogenizing.
2. glass fibre as claimed in claim 1, it is characterized in that, the weight that described high strength glass fiber accounts for by each component mainly comprises following component:
Wherein RO is CaO, MgO, SrO and BaO sum.
3., as power requires the glass fibre as described in 1 or 2, it is characterized in that, described high strength glass fiber composition also comprises 0.1%-0.15%CeO
2;
Preferably, described glass fibre also comprises ZnO, TiO of being no more than 2wt%
2, ZrO
2, Fe
2o
3, Y
2o
3, MnO
2.
4., as power requires the glass fibre as described in one of 1-3, it is characterized in that, the weight percentage sum of described CaO and MgO is not less than 17%, is not more than 19%; And MgO/ (CaO+MgO) >=0.25, MgO/ (CaO+MgO)≤0.7.
5., as power requires the glass fibre as described in one of 1-4, it is characterized in that, described SiO
2with Al
2o
3weight percentage sum be not less than 82%.
6. the glass fibre as described in one of claim 1-5, is characterized in that, the tensile strength of described glass fibre is for being not less than 4400MP, and Young's modulus is not less than 90GPa.
7. the preparation method of the glass fibre as described in one of claim 1-6, is characterized in that, described glass fiber compound prepares through melt drawing.
8. preparation method as claimed in claim 7, is characterized in that, described in be melted in electricity fusing-aid structure common refractory tank furnace in carry out, electricity fusing-aid accounts for more than 20% of energy input total amount; The energy consumption input of melting area accounts for the whole 60-85% founding kiln energy input;
Preferably, the fiberization temperature of described wire drawing is not higher than 1350 DEG C;
Preferably, the difference Δ T of described fiberization temperature and crystallization ceiling temperature is not less than 80 DEG C.
9. preparation method as claimed in claim 7 or 8, is characterized in that, described wire drawing adopts the direct wire-drawing operation of common platinum rhodium bushing to produce.
10. the purposes of the glass fibre as described in one of claim 1-6, it is applied to air vane or space shuttle field.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111018358A (en) * | 2020-01-02 | 2020-04-17 | 泰山玻璃纤维邹城有限公司 | Alkali-free superfine glass fiber formula |
| CN113912384A (en) * | 2021-12-01 | 2022-01-11 | 泉州市龙亘耐火保温材料有限公司 | Superfine ceramic fiber cotton and production method thereof |
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| US20120163987A1 (en) * | 2010-12-22 | 2012-06-28 | Agy Holding Corporation | High strength glass composition and fibers |
| CN102786223A (en) * | 2012-08-28 | 2012-11-21 | 泰山玻璃纤维有限公司 | High-strength glass fiber composition |
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| CN111018358A (en) * | 2020-01-02 | 2020-04-17 | 泰山玻璃纤维邹城有限公司 | Alkali-free superfine glass fiber formula |
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| CN113912384A (en) * | 2021-12-01 | 2022-01-11 | 泉州市龙亘耐火保温材料有限公司 | Superfine ceramic fiber cotton and production method thereof |
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Application publication date: 20151223 |