CN115432932B - Glass fiber composition with ultrahigh specific modulus and glass fiber - Google Patents
Glass fiber composition with ultrahigh specific modulus and glass fiber Download PDFInfo
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- 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
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- 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
- C03B37/022—Manufacture of glass fibres or filaments by drawing or extruding, e.g. direct drawing of molten glass from nozzles; Cooling fins therefor from molten glass in which the resultant product consists of different sorts of glass or is characterised by shape, e.g. hollow fibres, undulated fibres, fibres presenting a rough surface
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Abstract
The invention belongs to the technical field of glass fibers, and in particular relates to a glass fiber composite materialA glass fiber composition and glass fiber having an ultra-high specific modulus. The weight percentage of each component is as follows: siO (SiO) 2 :57.0‑61.0％、Al 2 O 3 :17.5‑22.9％、CaO:2.5‑5.9％、MgO:12.1‑16.0％、Fe 2 O 3 :0.2‑0.6％、TiO 2 :0.1‑1.5％、CeO 2 :0.1‑2.0％、La 2 O 3 :0‑1.0％、Li 2 O:0.05‑0.8％、K 2 O:0‑0.8％、Na 2 O0-0.8%. The glass fiber composition of the present invention has a glass density of less than 2.615g/cm 3 The tensile elastic modulus of the glass fiber reaches more than 93.5GPa, and the specific modulus is more than 3.65, so that the glass fiber composite material can be used for large-scale wind power blades, and the quality of the glass fiber composite material is remarkably reduced.
Description
Technical Field
The invention belongs to the technical field of glass fibers, and particularly relates to a glass fiber composition with ultrahigh specific modulus and glass fibers.
Background
Since the 90 th century of the 20 th century, the wind power generation industry rapidly developed due to the influence of energy crisis and environmental protection requirements, the load and weight of wind blades are continuously increased, and high requirements are put on large-size wind blades, so that the wind blades are light-weighted, high-strength and low-cost, and become the development direction of future wind blades.
The specific modulus is the elastic modulus of unit density, and glass fibers and fabrics with high specific modulus are widely applied to wind power blades, and the glass fibers are required to reach high modulus and reduce the density to be lower. The large-size wind power blade manufactured by the glass fiber with high specific modulus can effectively reduce the weight of the blade, can increase the power generation efficiency, can be suitable for low wind speed regions, is the development direction of the glass fiber industry, and becomes a hot spot for research of the glass fiber industry in recent years.
The earliest manufacturers developing high modulus glass fibers were the company Eurasian, U.S., the most representative of which was S-2 glass, which contained about 65% SiO 2 、25％Al 2 O 3 And 10% MgO, the modulus is about 90-92GPa, the melting temperature is as high as 1650 ℃, the forming temperature is 1470 ℃, and the liquid phase temperature is about 1465 ℃. Because the melting temperature is high, the bushing plate can be melted only by an electric kiln with full platinum as the lining, the service life of the bushing plate is greatly shortened due to the higher temperature, the production cost is high, and the absolute modulus of the bushing plate is relatively low, so that the bushing plate is not beneficial to large-scale production.
Chinese patent CN111807707A discloses a high modulus glass fiber composition and glass fiber and composite material containing 8-20% of Y 2 O 3 0-3% SrO,0-2.9% La 2 O 3 . High content rare earth oxide Y 2 O 3 The introduction of the glass fiber improves the raw material cost for producing the high-modulus glass fiber and simultaneously increases the density of the glass fiber. Although the glass fiber can reach higher modulus, the specific modulus is still lower due to the higher density.
In the prior art, the modulus of glass fibers is generally improved by introducing a large amount of rare earth oxide or by adding heavy elements to improve the density of the glass fibers, so that the glass fibers have high production cost and low specific modulus and cannot be widely applied to wind power blades.
In the current high-modulus glass fiber products, the density of the products with the modulus of more than 93GPa is more than 2.62g/cm 3 The specific modulus is less than 3.63, and the high modulus formula has the problems of high crystallization rate and small operation window. In view of the above, there is a need to develop a glass fiber with a low density, a high modulus, a low crystallization tendency and a high specific modulus, which can greatly reduce the mass of the composite material while improving the mechanical properties of the composite material, and can be produced in a large scale.
Disclosure of Invention
The invention aims to provide a glass fiber composition with ultrahigh specific modulus, and the glass fiber prepared by the composition has lower glass density, considerable elastic modulus and lower production cost, and simultaneously has good forming temperature and liquidus temperature, low crystallization rate and suitability for tank furnace and large-scale production; the invention also provides a glass fiber with the ultrahigh specific modulus.
The invention relates to a glass fiber composition with ultrahigh specific modulus, which comprises the following components in percentage by mass:
SiO 2 :57.0-61.0％、Al 2 O 3 :17.5-22.9％、CaO:2.5-5.9％、MgO:12.1-16.0％、Fe 2 O 3 :0.2-0.6％、TiO 2 :0.1-1.5％、CeO 2 :0.1-2.0％、La 2 O 3 :0-1.0％、Li 2 O:0.05-0.8％、K 2 O:0-0.8％、Na 2 0-0.8% of O; wherein, the mass percentage of CaO and MgO satisfies CaO/MgO=0.15-0.45.
Further preferred is:
CeO 2 with TiO 2 The mass percentage of the (B) satisfies the CeO 2 /TiO 2 ≥1.1。
Li 2 O and CeO 2 The mass percentage of (2) satisfies Li 2 O+CeO 2 ≤2.2％。
Al 2 O 3 With MgO (MgO)The mass percentage content satisfies the following Al 2 O 3 +MgO≥32.5％。
The glass fiber composition with the ultrahigh specific modulus does not contain BaO or SrO.
The density of the glass fiber composition with the ultrahigh specific modulus is less than or equal to 2.615g/cm 3 。
The tensile elastic modulus of the glass fiber prepared by the glass fiber composition with the ultrahigh specific modulus is more than or equal to 93.5GPa; the specific modulus of the glass fiber is more than 3.65; the molding temperature of the glass fiber is 1280-1320 ℃; the liquidus temperature of the glass fiber is between 1225 and 1270 ℃.
The glass fiber composition with the ultrahigh specific modulus is prepared from the following raw materials: calcined kaolin, quartz powder, magnesia, quicklime, spodumene, cerium oxide and titanium dioxide.
The particle size of the calcined kaolin is 50-100 mu m, the particle size of the quartz powder is 40-50 mu m, the particle size of the magnesia is 50-100 mu m, the particle size of the quicklime is 100-200 mu m, the particle size of the spodumene is 70-150 mu m, the particle size of the cerium oxide is 40-100 mu m, and the particle size of the titanium pigment is 40-100 mu m.
The invention relates to the use of a glass fiber composition with an ultra-high specific modulus:
(1) The quality of various raw materials required is calculated according to the content of each component in the glass fiber composition with the ultrahigh specific modulus, and the raw materials are weighed and mixed to obtain a batch;
(2) Melting and clarifying the mixed batch at 1450-1550 ℃ to obtain a homogeneous glass liquid;
(3) And drawing the glass liquid at 1280-1320 ℃ to obtain the glass fiber.
The beneficial effects of the invention are as follows:
SiO in the present invention 2 Is a network generator of glass, which forms an irregular continuous network structure with a silicon oxygen tetrahedron structure, the structure has higher bond strength, can effectively improve the mechanical strength, chemical stability and thermal stability of the glass, and can reduce the density of the glass at the same time, but SiO 2 The increased content can increase the high-temperature viscosity of the glassAnd great fiber forming difficulty. On the basis of ensuring that the elastic modulus and the density meet the requirements, the invention can also meet the requirements of fiber forming, and the invention limits SiO in the glass composition 2 The mass percentage is 57.0-61.0%.
Al 2 O 3 Is a network intermediate for forming glass, al 3+ Can abstract non-bridging oxygen to form aluminum oxide tetrahedron to enter into silicon oxygen network, and reconnect broken network, so that the glass structure tends to be compact, the mechanical property and elastic modulus of the glass are improved, but a large amount of Al is introduced 3+ Can promote the crystallization capacity of glass, especially the mass percent of Al 2 O 3 When the content of the cordierite is more than 23%, a large amount of cordierite particles are precipitated on the glass, and the Al is limited in order to adjust the crystallization type in the glass and reduce the crystallization tendency of the cordierite 2 O 3 The mass percentage content ranges from 17.5 percent to 22.9 percent.
CaO is an external network oxide, has an effect of reducing high-temperature viscosity, and can shorten the glass batch property. The introduction of CaO can increase crystal phase competition, effectively inhibit crystallization tendency of cordierite in glass, obviously increase glass density in the glass system, but has little contribution to elastic modulus of the glass, and the mass percent of CaO is limited to be 2.5% -5.9%.
Mg 2+ With Ca 2+ Different, mg 2+ The glass has small radius, high charge, strong polarization capability and strong accumulation effect, and can increase the polymerization degree of a glass network and improve the elastic modulus of glass. Increasing MgO content and also making part of Mg 2+ By [ MgO ] 4 ]Tetrahedra exist and are bonded to [ SiO ] 4 ]The tetrahedron forms a glass structure skeleton, so that the elastic modulus of the glass is obviously improved while the density of the glass is reduced, but excessive MgO can increase the crystallization upper limit temperature and crystallization rate of the glass, and the SiO is reasonably controlled 2 、Al 2 O 3 On the premise of the content, the invention limits the mass percentage content range of MgO to 12.1-16.0%, so as to further ensure the modulus and simultaneously control the Al 2 O 3 The mass percentage of the magnesium alloy and MgO satisfies the following conditions of Al 2 O 3 +MgO≥32.5％。
The influence of CaO and MgO on the elastic modulus, density, crystallization and viscosity of the glass is comprehensively considered, the use proportion of CaO and MgO is regulated, so that the glass achieves the favorable performance indexes of higher elastic modulus, lower density, lower crystallization temperature, crystallization rate and the like, the mass percentage content of CaO is limited to be 2.5-5.9%, and the mass percentage content of CaO and MgO is controlled to meet CaO/MgO=0.15-0.45. The invention does not add BaO and SrO, which can obviously increase the density of the glass, which is not consistent with the purpose of the invention.
The invention simultaneously adds CeO 2 And TiO 2 。TiO 2 Is an intermediate oxide, and a part of TiO in glass formation 2 With titanium oxide tetrahedra [ TiO ] 4 ]Into the network structure, another part is formed by [ TiO ] 6 ]The octahedra are outside the structure. TiO (titanium dioxide) 2 Is a nucleating agent which can increase crystallization tendency of glass when being singly added, and the glass is influenced by reducing atmosphere of batch during melting, tiO 2 Will be converted into Ti 2 O 3 The invention simultaneously adds CeO 2 ，Ti 3+ Will be combined with Ce 4+ React to generate a large amount of Ti 4+ In [ TiO ] 4 ]The form of the titanium oxide tetrahedron enters the network structure, so that the [ TiO ] outside the network structure is reduced 6 ]The number of the titanium oxide octahedrons enhances the interconnection of the structures and can obviously improve the elastic modulus of the glass.
With TiO 2 And CeO 2 The content increase or the use proportion of the two is unreasonable, and TiO 2 Will not easily form [ TiO ] 4 ]Or form excessive [ TiO ] 4 ]Excess titanyl tetrahedra [ TiO 4 ]Will reduce silicon oxygen tetrahedron [ SiO ] 4 ]The quantity gradually reduces the polymerization degree of the glass, influences the structural stability of the glass and reduces the elastic modulus of the glass. With TiO 2 And CeO 2 The increased content also accentuates the color of the glass. The invention defines TiO 2 The mass percentage of the catalyst is in the range of 0.1-1.5 percent, ceO 2 The mass percentage of the CeO is in the range of 0.1-2.0 percent 2 /TiO 2 ≥1.1。
CeO 2 CeO as a strong oxidizer 2 Oxygen evolution by heating at high temperatureAnd in the glass melting process, the gas promotes the discharge of bubbles in the glass liquid. CeO (CeO) 2 Can adjust the oxidation-reduction atmosphere in the kiln and effectively control FeO/Fe 2 O 3 The method improves the heat permeability of the glass liquid, reduces the energy consumption in the glass melting process, is more beneficial to stabilizing the temperature of the large-flow bushing by controlling FeO in the glass liquid, is beneficial to the subsequent wire drawing operation, combines the condition of the wire drawing operation of a high-modulus kiln, and controls Fe 2 O 3 0.2 to 0.6 percent of the weight percentage. CeO (CeO) 2 Can replace sodium sulfate Na in the traditional formula 2 SO 4 SO in the kiln melting process is reduced 2 The generation of gas reduces the SO of volatile gas 2 Corrosion to refractory materials and reduction of SO in flue gas discharged from kiln 2 The content of (3) accords with the national double-carbon policy.
The invention defines Li 2 The mass percentage of O is 0.05-0.8%, and proper amount of Li is added 2 O can reduce the clarifying temperature, forming temperature and crystallization upper limit temperature of the glass, is favorable for the fiber forming operation of glass fiber, and is Li + The radius is small, the electric field intensity is large, the strong accumulation effect is achieved, the compact network skeleton is accumulated, meanwhile, the Li-O bond can connect a discontinuous network structure and Si-O broken bonds in a glass network system, the glass network structure is improved, and the elastic modulus of glass is further enhanced. Li in the glass System of the invention 2 O、CeO 2 Providing more free oxygen, excess Li 2 O、CeO 2 Not only interfere with [ AlO ] 4 ]、[TiO 4 ]And weaken [ SiO ] 4 ]The bridge oxygen in the glass damages the compactness of the structure, reduces the elastic modulus of the glass and promotes crystallization. The invention defines Li 2 O and CeO 2 The mass percentage of (2) satisfies Li 2 O+CeO 2 ≤2.2％。
Na 2 O、K 2 O is not specifically introduced, and is introduced by the mineral raw materials used, and the addition amount of the O and the mineral raw materials is not more than 0.8%. The invention can also add proper amount of La 2 O 3 ，La 2 O 3 Can play a role in regulating viscosity in the glass system, la 2 O 3 The viscosity can be properly increased without affecting the crystallization rate, but the density of the glass is increased due to the excessively high content, and La is limited by the invention 2 O 3 The mass percentage content range of (2)<1.0％。
High content of Y 2 O 3 Can obviously improve the elastic modulus of the glass and inhibit crystallization, when Y 2 O 3 The content of less than 2.0% is not obvious in terms of improving the modulus and inhibiting crystallization, and when the content is higher, the density is obviously increased while the elastic modulus of the glass is improved, which is not consistent with the purpose of the invention. On the premise of not affecting the comprehensive performance of the glass, the invention can add not more than 1.0 percent of Y 2 O 3 Or ZrO (R) 2 、B 2 O 3 、P 2 O 5 。
The invention selects calcined kaolin raw material for the introduction of aluminum in the glass component to further reduce the production cost, and has the primary value of replacing industrial alumina to introduce Al 2 O 3 The cost of ton glass can be greatly reduced, and the kaolin is prepared by calcining solid waste (commonly called coal gangue and low cost) of coal mine in a proper calciner at high temperature; secondly, the main purpose of the calcination of the calcined kaolin is to remove organic carbon, structural water and other impurity minerals in the coal-series kaolin and the coal gangue, so as to greatly reduce COD and loss on ignition, and the calcined kaolin can replace industrial alumina and simultaneously can also give consideration to the controllable COD and gas rate of the batch; and thirdly, in the high-temperature calcination process of the coal-based kaolin, the mineral structure is rearranged, so that the calcined kaolin mainly comprising a stable mullite phase is generated, and compared with corundum, the calcined kaolin has a lower melting point, thereby being very beneficial to reducing the melting energy consumption of batch materials and saving the production cost of ton glass.
The ultra-high specific modulus glass fiber composition of the invention is not added with BaO and SrO components and CeO is added 2 And TiO 2 Simultaneously improves the MgO content and optimizes the SiO 2 、Al 2 O 3 CaO component, and reasonably controlling CeO 2 /TiO 2 CaO/MgO use ratio and Li 2 O+CeO 2 In such an amount that CeO 2 、TiO 2 、MgO、Li 2 O productionBetter synergistic effect is achieved, the elastic modulus of the glass is obviously improved under the condition of low density of the glass, and SiO is enabled to be realized 2 -MgO-Al 2 O 3 The invention also discloses the application of the calcined kaolin raw material in a high-modulus formula of a large tank furnace, which is very beneficial to reducing the melting energy consumption of batch materials and saving the production cost of ton glass.
The glass fiber compositions of the present invention have a density of less than 2.615g/cm 3 The tensile modulus of the glass fiber reaches more than 93.5GPa, and the specific modulus is more than 3.65, so that the glass fiber composite material can be used for large-scale wind power blades, and the quality of the glass fiber composite material is remarkably reduced.
The glass fiber molding temperature is not higher than 1320 ℃, the liquidus temperature is not higher than 1270 ℃, the glass fiber molding temperature and the liquidus temperature are good, the crystallization rate is low, the drawing process requirements are met, and the glass fiber molding device is suitable for tank furnace and large-scale production.
Detailed Description
The invention is further described below with reference to examples.
The tank furnace wire drawing production process of the glass fiber with the ultrahigh specific modulus comprises the following steps:
(1) The quality of various raw materials required is calculated according to the content of each component in the glass fiber composition with the ultrahigh specific modulus, each raw material is weighed and is conveyed to a kiln head stock bin after being uniformly mixed by pneumatic force to obtain a batch, and then the batch is thrown into a large tank furnace at a constant speed by a batch feeder;
(2) Melting and clarifying the mixed batch materials into homogeneous glass liquid at 1450-1550 ℃ in a tank furnace;
(3) Glass liquid is drawn at 1280-1320 ℃ through a discharge spout on a large 4000 Kong Bolao bushing plate to form glass fiber;
(4) The glass fiber is drawn and wound to a wire drawing machine, and a precursor product is formed through high-speed wire drawing.
The components and specifications of the raw materials are as follows:
| raw material name | Oxide designation and content | Particle size |
| Quartz powder | SiO 2 ≥99.0％ | 40-50μm |
| Calcined kaolin | Al 2 O 3 ≥40.0％、SiO 2 ≥53.0％ | 50-100μm |
| Magnesium oxide | MgO≥90％ | 50-100μm |
| Quicklime | CaO≥93％ | 100-200μm |
| Cerium oxide | CeO 2 ≥95％ | 40-100μm |
| Titanium white powder | TiO 2 ≥95％ | 40-100μm |
| Spodumene | Li 2 O≥5.0％、Al 2 O 3 ≥26％、SiO 2 ≥52.0％ | 70-150μm |
The invention adopts the raw materials with different grain size fractions, on one hand, the uniformity of raw material mixing is ensured; on the other hand, the introduction of superfine powder is reduced, which is favorable for the discharge of bubbles in the glass liquid. The invention is suitable for large tank furnaces and is beneficial to improving the production efficiency.
In verifying the overall properties of the glass fibers in the examples and comparative examples, the following parameters were selected:
1) The forming temperature of the glass fiber, i.e., the temperature at which the viscosity of the glass is 1000Poise, can be characterized as the forming temperature of the fiber, and a high temperature viscometer is used to obtain the high temperature viscosity of the glass.
2) The liquidus temperature of glass, i.e., the critical temperature at which glass begins to crystallize, is generally the upper crystallization temperature limit of glass, and the upper crystallization temperature limit of glass is obtained using a crystallization furnace.
3) Delta T, the difference between the forming temperature and the liquidus temperature.
4) Crystallization melting enthalpy: the devitrification dynamics of the glass is researched by a differential thermal analysis method, so that glass devitrification enthalpy parameters are obtained, the smaller the numerical value is, the weaker the devitrification capacity of the glass is, the lower the devitrification rate is, and the devitrification capacity of the glass can be comprehensively characterized.
5) Glass density is measured according to the standard test method of measuring glass density by ASTM C693 buoyancy method;
6) Modulus of elasticity is measured according to ASTM D2343;
7) The specific modulus is the ratio of the modulus to the density of the material (specific modulus = modulus/(density x 9.8)).
Examples 1 to 16
The compositions of the glass fiber compositions having the ultra-high specific moduli in examples 1 to 16 and the glass fiber property data are shown in tables 1, 2.
Comparative examples 1 to 7
The compositions of the glass fiber compositions and the glass fiber property data of comparative examples 1 to 7 are shown in Table 3.
Table 1 data sheets of examples 1-8
Table 2 data sheets of examples 9-16
Table 3 data sheets for comparative examples 1-7
The data in tables 1-3 were analyzed and comparative example 1 is SiO well known in the art 2 -MgO-Al 2 O 3 The ternary system high modulus glass fiber component has lower density and relatively lower modulus, and can not meet the requirements of the invention.
Comparative example 2 and example 15 show that when the lithium content is excessive, li 2 O+CeO 2 When the viscosity is more than 2.2, the viscosity is obviously reduced, crystallization is not reduced but is increased, and the elastic modulus is obviously reduced. From comparative example 3 and example 1, yttrium is used to replace cerium and titanium, the viscosity and crystallization are increased simultaneously, the density is increased, and the modulus is obviously reduced; comparative example 4 increasing the amount of yttrium used, the modulus was increased and the glass density reached 2.675g/cm 3 The density increase is evident. Comparative example 5 and comparative example 6 cerium or titanium alone, comparative example 7 cerium to titanium ratioThe addition is unreasonable, the crystallization temperature is obviously increased, the crystallization capacity is enhanced, and the modulus is reduced.
In addition, siO was used as a material in example 2 2 The content is adjusted to 60.3% from 60.2%, the MgO content is adjusted to 14.3% from 14.4%, and the content of the rest components is unchanged. The modulus is 93.2GPa and the density is 2.610/cm 3 . The experiment shows that when Al 2 O 3 The +MgO content is not in Al 2 O 3 When +MgO is more than or equal to 32.5%, the influence on modulus is large.
Claims (7)
1. A glass fiber composition having an ultra-high specific modulus, characterized by: the weight percentage of each component is as follows:
SiO 2 :57.0-61.0%、Al 2 O 3 :17.5-22.9%、CaO:2.5-5.9%、MgO:12.1-16.0%、Fe 2 O 3 :0.2-0.6%、TiO 2 :0.1-1.5%、CeO 2 :0.1-2.0%、La 2 O 3 :0-1.0%、Li 2 O:0.05-0.8%、K 2 O:0-0.8%、Na 2 O:0-0.8%；
wherein, the mass percentage of CaO and MgO satisfies CaO/MgO=0.15-0.45; ceO (CeO) 2 With TiO 2 The mass percentage of the (B) satisfies the CeO 2 /TiO 2 ≥1.1；Al 2 O 3 The mass percentage of the magnesium alloy and MgO satisfies the following conditions of Al 2 O 3 +MgO≥32.5%。
2. The ultra-high specific modulus glass fiber composition according to claim 1, wherein: li (Li) 2 O and CeO 2 The mass percentage of (2) satisfies Li 2 O+CeO 2 ≤2.2%。
3. The ultra-high specific modulus glass fiber composition according to claim 1, wherein: the density of the glass fiber composition with ultra-high specific modulus is less than or equal to 2.615g/cm 3 。
4. A glass fiber made from the glass fiber composition having an ultra high specific modulus according to any one of claims 1 to 3, wherein: the specific modulus of the glass fiber is more than 3.65.
5. The glass fiber made from the glass fiber composition having an ultra-high specific modulus according to claim 4, wherein: the tensile elastic modulus of the glass fiber is more than or equal to 93.5GPa.
6. The glass fiber made from the glass composition having the ultra-high specific modulus according to claim 4, wherein: the glass fiber has a molding temperature of 1280-1320 ℃.
7. The glass fiber made from the glass composition having the ultra-high specific modulus according to claim 4, wherein: the liquidus temperature of the glass fiber is between 1225 and 1270 ℃.
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