CN104591542A - High-strength glass fiber containing transition metal oxides and preparation method thereof - Google Patents
High-strength glass fiber containing transition metal oxides and preparation method thereof Download PDFInfo
- Publication number
- CN104591542A CN104591542A CN201410851921.9A CN201410851921A CN104591542A CN 104591542 A CN104591542 A CN 104591542A CN 201410851921 A CN201410851921 A CN 201410851921A CN 104591542 A CN104591542 A CN 104591542A
- Authority
- CN
- China
- Prior art keywords
- glass
- glass fiber
- transition metal
- high strength
- metal oxide
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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
- C03C13/00—Fibre or filament compositions
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
- C03B37/01—Manufacture of glass fibres or filaments
- C03B37/02—Manufacture of glass fibres or filaments by drawing or extruding, e.g. direct drawing of molten glass from nozzles; Cooling fins therefor
- C03B37/025—Manufacture of glass fibres or filaments by drawing or extruding, e.g. direct drawing of molten glass from nozzles; Cooling fins therefor from reheated softened tubes, rods, fibres or filaments, e.g. drawing fibres from preforms
Abstract
The invention relates to a high-strength glass fiber containing transition metal oxides and a preparation method thereof. The high-strength glass fiber comprises the following components in percentage by weight: 55-64 percent of SiO2, 15-21 percent of Al2O3, 9-15 percent of CaO, 5-10 percent of MgO, 1.5-3.5 percent of ZnO, 0.5-3 percent of TiO2 and 0.5-3.5 percent of ZrO2. The preparation method comprises the following steps: (1) calculating the formula, weighing and uniformly mixing; (2) melting; (3) casting into glass blocks or glass strips, and annealing; and (4) drawing with melting. The high-strength glass fiber is prepared by adding the transition metal oxides into the conventional high-strength glass fiber and controlling the total content of silicon oxide and aluminum oxide, so that the prepared glass fiber has high tensile strength and low melting temperature and glass viscosity and has good application prospects.
Description
Technical field
The invention belongs to high strength glass fiber field, particularly a kind of high strength glass fiber containing transition metal oxide and preparation method thereof.
Background technology
Compared with common alkali free glass fibre, high-strength high-modulus glass fiber has the premium propertiess such as tensile strength is high, Young's modulus is high, shock resistance is good, chemical stability is good, fatigue resistance is good, high temperature resistant, the field that space flight, aviation, weapons, naval vessel, chemical industry etc. are harsher to composite property requirement can be widely used in, as missile engine case, aerospace aircraft liner, gun stock, launching gun barrel, bulletproof armour, high pressure vessel, large size fan blade etc.
High strength glass fiber system Main System has SiO
2-Al
2o
3-MgO or SiO
2-Al
2o
3-CaO, although the massfraction of various high strength glass composition is not quite similar, wherein the content of main oxides is as all very high in silicon oxide and alumina content, wherein Al
2o
3content can reach about 25%.
U.S. S-2 high strength glass fiber, its composition is only the oxide compound of silicon, aluminium and magnesium, and content is 65wt%SiO
2, 25wt%Al
2o
3, 10wt%MgO, the advantage of S-2 glass is that tensile strength is high, but glass ware forming temperature is high, its liquidus temperature is up to 1470 DEG C, bushing temperature reaches 1570 DEG C, found inner lining of kiln material require and use special refractory and the precious metal material such as platinum, rhodium, drawing process condition is harsh, and production cost is higher.
France R glass is a kind of high strength glass fiber, is mainly used in Aeronautics and Astronautics and military field.R glass forms primarily of the oxide compound of silicon, aluminium, calcium and magnesium, and its main component is 58 ~ 60wt%SiO
2, 23.5 ~ 25.5wt%Al
2o
3, 5 ~ 6wt%MgO and 9 ~ 11wt%CaO.The liquidus temperature of R glass and mold temperature are higher than 1350 DEG C, and found, wire-drawing temperature is equally very high, therefore the same with S glass, production cost is higher.
The Hiper-tex glass of the 3B glass fibre company production in Europe is based on melting technology, fiberizing and treating compound technology, its fibre strength is made to improve 30%, modulus can improve 17%, and thermal linear expansion coefficient is low by 30%, but there is the problem such as glass melting temperature and production cost height equally.Therefore the production difficulty of high-strength glass fibre is large, and production cost is high, constrains scale operation and the application of high-strength glass fibre.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of high strength glass fiber containing transition metal oxide and preparation method thereof, this glass fibre is by adding transition metal oxide the total content of controlled oxidization silicon and aluminum oxide prepares high-strength glass fibre in conventional high-strength glass fibre, make it have higher tensile strength and lower glass melting temperature and glass viscosity, have a good application prospect.
A kind of high strength glass fiber containing transition metal oxide of the present invention, by weight percentage, composed of the following components: SiO
255 ~ 64%, Al
2o
315 ~ 21%, CaO 9 ~ 15%, MgO 5 ~ 10%, ZnO 1.5 ~ 3.5%, TiO
20.5 ~ 3% and ZrO
20.5 ~ 3.5%.
The present invention adopt the high-strength glass fibre system of technical scheme to be SiO
2-Al
2o
3-CaO-MgO-ZnO-TiO
2-ZrO
2, oxygen-freeization boron and fluorochemical.
Excellent and be conducive to glass fiber wire-drawing and have the glass fibre of high strength in order to prepare vitrifying, glass ingredient described above also must meet following characteristics:
SiO in described glass ingredient
2preferable range: 58 ~ 63%; Al
2o
3preferable range: 17 ~ 20%; SiO
2+ Al
2o
3preferable range 75 ~ 80%.SiO
2be topmost Network former in silicate glass, in glass system, play main skeleton, improve SiO
2content, although enhance glass skeleton structure, the viscosity of glass metal under identical glass melting temperature rises, and founds clarifying temp and raises.Al
2o
3glass can not be formed separately, but vitrifying degree and the increased devitrification resistance of glass can be improved, improve the chemical stability of glass fibre.Al
2o
3content height makes the liquidus line of glass rise equally, therefore in order to both ensure that glass fibre has higher tensile strength, makes again glass fibre glass melting temperature moderate, control SiO
2+ Al
2o
3content 75 ~ 80%.
The preferable range of CaO in described glass ingredient: 10 ~ 14%, in described glass ingredient, the ratio of the preferable range of the preferable range of MgO: 6 ~ 8%, CaO+MgO: 15 ~ 20%, CaO/MgO is greater than 1.2.CaO and MgO is cheap composition conventional in glass.CaO belongs to network-modifying ion, and CaO can reduce the high temperature viscosity of glass metal, but the content increasing CaO can increase the fragility of glass.The increase of content of MgO can promote the phase-splitting of glass, makes the liquidus line of glass increase, and make devitrification of glass be inclined to increases simultaneously.The present invention is preferred CaO and MgO simultaneously, and CaO is greater than MgO, now utilizes two kinds of cationic actings in conjunction and drag effect, improve the melting conditions of glass, reach the effect of clarification and homogenization, improve the chemical stability of glass network compact structure degree and glass.
The preferable range of ZnO in described glass ingredient: 1.5 ~ 2.5%.ZnO is a kind of intermediate oxide.In non-alkali glass, ZnO then exists with zinc oxygen octahedra, enter in the space between silicon-oxy tetrahedron and serve as Network modifier, in ZnO and glass, some component forms eutectic mixture, liquid phase can be formed at a lower temperature, facilitate the melting of bulk glass, play the effect reducing glass high temperature viscosity.The present invention selects the main purpose of ZnO to be improve the melting conditions of glass, plays fluxing action when glass smelting, and meanwhile, ZnO can also reduce the coefficient of expansion of glass, improves the corrosion resistance nature of glass, but the too high tendency towards devitrification that can increase glass of ZnO.
TiO in described glass ingredient
2preferable range: 1 ~ 2%.TiO
2belonging to transition group oxide compound, be generally present in glass network structure with octahedral coordination structure, is network modifying oxide, adds TiO
2the melting conditions of glass can be improved, play fluxing action, but excessive TiO
2crystallization and the tendency towards devitrification of glass can be increased.
ZnO+TiO in described glass ingredient
2preferable range: 2 ~ 4%.Excessive ZnO and TiO
2capital makes the tendency towards devitrification of glass increase, and therefore controls total content and is less than 4%.
ZrO in described glass ingredient
2preferable range: 1 ~ 2.5%.ZrO
2significantly can increase the intensity of glass, thermostability and corrosion resistance nature, but Zr
4+field intensity own is large, if content is high, can produces in glass and gather effect, cause glass phase-separating and crystallization, and ZrO
2content height also can improve the high temperature viscosity of glass.
Oxygen-freeization boron and fluorochemical in described glass ingredient.Boron oxide is good glass-former, glass melting temperature and the high temperature viscosity of glass can be reduced, normally use as solubility promoter, but in high-strength glass fibre is founded, boron oxide self volatilization at high temperature brings adverse influence also to the clarification homogenizing of glass, the use of fluorochemical increases the erosion of refractory materials on the one hand, increase of volatilizing on the other hand, therefore does not use boron oxide and fluorochemical in described glass ingredient.
The preparation method of a kind of high strength glass fiber containing transition metal oxide of the present invention, comprising:
(1) aluminum oxide is introduced by aluminium hydroxide, and CaO, MgO are introduced by respective carbonate, and all the other components are introduced by respective oxide compound, then calculates formula, weighing mixes;
(2) select quartz crucible, found in silicon molybdenum rod furnace, glass melting temperature is 1500 ~ 1550 DEG C, is incubated 4 ~ 5 hours;
(3) glass metal melted is cast into glass block or glass bar, puts into annealing furnace and anneal, furnace cooling after insulation;
(4) by the above-mentioned glass melted melt drawing on glass fiber single filament machine, to obtain final product.
Annealing temperature in described step (3) is 660 ~ 720 DEG C.
Wire-drawing temperature in described step (4) is 1300 ~ 1320 DEG C, and drawing wire machine rotating speed is 1200 ~ 1500r/min.
beneficial effect
The present invention in conventional high-strength glass fibre by adding transition metal oxide the total content of controlled oxidization silicon and aluminum oxide prepares high-strength glass fibre, make it have higher tensile strength and lower glass melting temperature and glass viscosity, have a good application prospect.
Embodiment
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.In addition should be understood that those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within the application's appended claims limited range equally after the content of having read the present invention's instruction.
Embodiment 1
(1) by weight percentage, SiO
261%, Al
2o
318%, CaO 10%, MgO 7%, ZnO 2%, TiO
21% and ZrO
21% weighing mixes;
(2) quartz crucible is selected, and cover lid, found in silicon molybdenum rod furnace, glass melting temperature is 1550 DEG C, is incubated 5 hours;
(3) glass metal melted is cast into glass block or glass bar, puts into annealing furnace and anneal, annealing temperature is 710 DEG C, is incubated furnace cooling after 2 hours;
(4) by the above-mentioned glass melted melt drawing on glass fiber single filament machine, wire-drawing temperature 1320 DEG C, drawing wire machine rotating speed 1200r/min, obtains high strength glass fiber.
Embodiment 2
(1) by weight percentage, SiO
260%, Al
2o
320%, CaO 11%, MgO 5.5%, ZnO 1%, TiO
21% and ZrO
21.5% weighing mixes;
(2) quartz crucible is selected, and cover lid, found in silicon molybdenum rod furnace, glass melting temperature is 1530 DEG C, is incubated 5 hours;
(3) glass metal melted is cast into glass block or glass bar, puts into annealing furnace and anneal, annealing temperature is 690 DEG C, is incubated furnace cooling after 2 hours;
(4) by the above-mentioned glass melted melt drawing on glass fiber single filament machine, wire-drawing temperature 1320 DEG C, drawing wire machine rotating speed 1300r/min, obtains high strength glass fiber.
Embodiment 3
(1) by weight percentage, SiO
260%, Al
2o
318%, CaO 11%, MgO 7%, ZnO 1.5%, TiO
21% and ZrO
21.5% weighing mixes;
(2) quartz crucible is selected, and cover lid, found in silicon molybdenum rod furnace, glass melting temperature is 1540 DEG C, is incubated 4 hours;
(3) glass metal melted is cast into glass block or glass bar, puts into annealing furnace and anneal, annealing temperature is 680 DEG C, is incubated furnace cooling after 2 hours;
(4) by the above-mentioned glass melted melt drawing on glass fiber single filament machine, wire-drawing temperature 1300 DEG C, drawing wire machine rotating speed 1300r/min, obtains high strength glass fiber.
Embodiment 4
(1) by weight percentage, SiO
258%, Al
2o
320%, CaO 10%, MgO 8%, ZnO 1%, TiO
21.5% and ZrO
21.5% weighing mixes;
(2) quartz crucible is selected, and cover lid, found in silicon molybdenum rod furnace, glass melting temperature is 1550 DEG C, is incubated 4 hours;
(3) glass metal melted is cast into glass block or glass bar, puts into annealing furnace and anneal, annealing temperature is 680 DEG C, is incubated furnace cooling after 2 hours;
(4) by the above-mentioned glass melted melt drawing on glass fiber single filament machine, wire-drawing temperature 1300 DEG C, drawing wire machine rotating speed 1400r/min, obtains high strength glass fiber.
Embodiment 5
(1) by weight percentage, SiO
258%, Al
2o
319%, CaO 10.5%, MgO 8%, ZnO1.5%, TiO
21.5% and ZrO
21.5% weighing mixes;
(2) quartz crucible is selected, and cover lid, found in silicon molybdenum rod furnace, glass melting temperature is 1530 DEG C, is incubated 5 hours;
(3) glass metal melted is cast into glass block or glass bar, puts into annealing furnace and anneal, annealing temperature is 670 DEG C, is incubated furnace cooling after 2 hours;
(4) by the above-mentioned glass melted melt drawing on glass fiber single filament machine, wire-drawing temperature 1300 DEG C, drawing wire machine rotating speed 1500r/min, obtains high strength glass fiber.
Embodiment 6
(1) by weight percentage, SiO
258%, Al
2o
318%, CaO 10%, MgO 8.5%, ZnO 1.5%, TiO
21.5% and ZrO
22.5% weighing mixes;
(2) quartz crucible is selected, and cover lid, found in silicon molybdenum rod furnace, glass melting temperature is 1520 DEG C, is incubated 5 hours;
(3) glass metal melted is cast into glass block or glass bar, puts into annealing furnace and anneal, annealing temperature is 670 DEG C, is incubated furnace cooling after 2 hours;
(4) by the above-mentioned glass melted melt drawing on glass fiber single filament machine, wire-drawing temperature 1300 DEG C, drawing wire machine rotating speed 1500r/min, obtains high strength glass fiber.
Chemical durability of glass test sample is the glass block of 50mm × 10mm × 10mm, test condition: the mass loss rate after being incubated 10h respectively in 90 DEG C of deionized waters, 1mol/L sulphuric acid soln and NaOH solution characterizes.
Thermal expansion coefficient of glass α sample
the glass wafer of 6mm × 25mm, density samples is the glass block of 50mm × 10mm × 10mm;
Tensile strength (cN/dtex) is tested, and experiment load measurement scope is 0-3000cN, and clamp distance is 250mm, and draw speed is 100mm/min.
Test the sample after processing, glass composition (weight percent) of embodiment 1-6 and the performance test results see the following form:
Table: fiberglass component and performance
Claims (10)
1., containing a high strength glass fiber for transition metal oxide, it is characterized in that: by weight percentage, composed of the following components: SiO
255 ~ 64%, Al
2o
315 ~ 21%, CaO 9 ~ 15%, MgO 5 ~ 10%, ZnO 1.5 ~ 3.5%, TiO
20.5 ~ 3% and ZrO
20.5 ~ 3.5%.
2. a kind of high strength glass fiber containing transition metal oxide according to claim 1, is characterized in that: described SiO
2weight percent is 58 ~ 63%; Al
2o
3weight percent is 17 ~ 20%.
3. a kind of high strength glass fiber containing transition metal oxide according to claim 1, is characterized in that: described SiO
2, Al
2o
3weight percent sum is 75 ~ 80%.
4. a kind of high strength glass fiber containing transition metal oxide according to claim 1, is characterized in that: described CaO weight percent is 10 ~ 14%; MgO weight percent is 6 ~ 8%.
5. a kind of high strength glass fiber containing transition metal oxide according to claim 1, is characterized in that: described CaO, MgO weight percent sum is 15 ~ 20%; The weight ratio of CaO and MgO is greater than 1.2.
6. a kind of high strength glass fiber containing transition metal oxide according to claim 1, is characterized in that: described ZnO weight percent is 1.5 ~ 2.5%; TiO
2weight percent is 1 ~ 2%; ZrO
2weight percent is 1 ~ 2.5%.
7. a kind of high strength glass fiber containing transition metal oxide according to claim 1, is characterized in that: described ZnO, TiO
2weight percent sum is 2 ~ 4%.
8. a preparation method for the high strength glass fiber containing transition metal oxide as claimed in claim 1, comprising:
(1) aluminum oxide is introduced by aluminium hydroxide, and CaO, MgO are introduced by respective carbonate, and all the other components are introduced by respective oxide compound, then calculates formula, weighing mixes;
(2) select quartz crucible, found in silicon molybdenum rod furnace, glass melting temperature is 1500 ~ 1550 DEG C, is incubated 4 ~ 5 hours;
(3) glass metal melted is cast into glass block or glass bar, puts into annealing furnace and anneal, furnace cooling after insulation;
(4) by the above-mentioned glass melted melt drawing on glass fiber single filament machine, to obtain final product.
9. the preparation method of a kind of high strength glass fiber containing transition metal oxide according to claim 8, is characterized in that: the annealing temperature in described step (3) is 660 ~ 720 DEG C.
10. the preparation method of a kind of high strength glass fiber containing transition metal oxide according to claim 8, it is characterized in that: the wire-drawing temperature in described step (4) is 1300 ~ 1320 DEG C, drawing wire machine rotating speed is 1200 ~ 1500r/min.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107216042A (en) * | 2017-06-05 | 2017-09-29 | 重庆国际复合材料有限公司 | A kind of high-modulus glass fiber composition and glass fibre |
| US11214512B2 (en) | 2017-12-19 | 2022-01-04 | Owens Coming Intellectual Capital, LLC | High performance fiberglass composition |
| CN117534319A (en) * | 2023-11-24 | 2024-02-09 | 中国建筑材料科学研究总院有限公司 | Preparation method and application of ultra-narrow twisted wire area optical fiber image inverter |
| CN117534319B (en) * | 2023-11-24 | 2024-05-14 | 中国建筑材料科学研究总院有限公司 | Preparation method and application of ultra-narrow twisted wire area optical fiber image inverter |
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| CN101597140A (en) * | 2009-07-02 | 2009-12-09 | 重庆国际复合材料有限公司 | A kind of high-strength high-modulus glass fiber |
| CN101838110A (en) * | 2010-05-19 | 2010-09-22 | 巨石集团有限公司 | Composition for preparing high-performance glass fiber by tank furnace production |
| CN103449728A (en) * | 2013-08-23 | 2013-12-18 | 中材科技股份有限公司 | Corrosion-resistant high-strength high-modulus fiber and fabric prepared from fiber |
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2014
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Patent Citations (4)
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| CN101580344A (en) * | 2009-06-29 | 2009-11-18 | 巨石集团有限公司 | High strength glass fiber composition |
| CN101597140A (en) * | 2009-07-02 | 2009-12-09 | 重庆国际复合材料有限公司 | A kind of high-strength high-modulus glass fiber |
| CN101838110A (en) * | 2010-05-19 | 2010-09-22 | 巨石集团有限公司 | Composition for preparing high-performance glass fiber by tank furnace production |
| CN103449728A (en) * | 2013-08-23 | 2013-12-18 | 中材科技股份有限公司 | Corrosion-resistant high-strength high-modulus fiber and fabric prepared from fiber |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107216042A (en) * | 2017-06-05 | 2017-09-29 | 重庆国际复合材料有限公司 | A kind of high-modulus glass fiber composition and glass fibre |
| US11214512B2 (en) | 2017-12-19 | 2022-01-04 | Owens Coming Intellectual Capital, LLC | High performance fiberglass composition |
| CN117534319A (en) * | 2023-11-24 | 2024-02-09 | 中国建筑材料科学研究总院有限公司 | Preparation method and application of ultra-narrow twisted wire area optical fiber image inverter |
| CN117534319B (en) * | 2023-11-24 | 2024-05-14 | 中国建筑材料科学研究总院有限公司 | Preparation method and application of ultra-narrow twisted wire area optical fiber image inverter |
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Application publication date: 20150506 |