CN108609859B - Novel high-modulus glass fiber composition and glass fiber - Google Patents
Novel high-modulus glass fiber composition and glass fiber Download PDFInfo
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Abstract
The invention provides a novel high-modulus glass fiber composition, which comprises the following components: SiO 2253wt％～55.9wt％；Al2O321.1wt％～23.9wt％；SiO2With Al2O376.5 wt% -79 wt% of the total content; al (Al)2O3/SiO2The mass fraction ratio is 0.38-0.45; TiO 22 0.3wt％～1.5wt％；Fe2O30.1wt% -0.5 wt%; CaO 8.2wt% -9.9 wt%; 9.9 to 11.8 weight percent of MgO; the total content of CaO and MgO is 18.8wt% -21.6 wt%; the ratio of the mass fraction of MgO to the mass fraction of CaO is 1.01 to 1.41; na (Na)2O and K2The total content of O is 0.2 to 1.0 weight percent; the total content of other impurity components is not more than 1 wt%. According to the invention, by controlling the specific percentage content of each component, the finally obtained high-modulus glass fiber has extremely high tensile modulus, lower forming temperature and good forming performance.
Description
Technical Field
The invention relates to the technical field of inorganic nonmetallic materials, in particular to a novel high-modulus glass fiber composition and glass fibers.
Background
The glass fiber belongs to an inorganic non-metallic material, has the advantages of high mechanical strength, good electrical insulation, strong heat resistance, stable physical and chemical properties and the like, is widely applied to the fields of aerospace, automobiles, ships, petrifaction, energy sources, electric power, buildings and the like, and is an inorganic fiber reinforced material with the largest application amount at present. The glass fiber is mainly used as a reinforced base material, so that the mechanical property of the glass fiber is particularly important, and along with the development trend that glass fiber composite materials are increasingly large-sized and light-weighted, people put forward higher and higher requirements on the mechanical property of the glass fiber, particularly the tensile modulus.
There are many related studies on the method for improving the strength and modulus of glass fibers. Most typical are S glass and R glass. The basic composition of the S glass is as follows: 65 wt% SiO225 wt% of Al2O310 wt% MgO. The theoretical monofilament strength of the S glass fiber is up to 4500MPa, the elastic modulus exceeds 85GPa, and the mechanical property is very excellent. But the molding temperature of the material exceeds 1470 ℃, and the material is easy to crystallize and has high production difficulty, so that the material cannot be popularized and applied on a large scale. R glass is also a high strength high modulus glass fiber, typically made of SiO2、Al2O3CaO, MgO is generally considered a compromise between manufacturing difficulty and mechanical properties, and is therefore more productive than S glass.
The invention patent application 201710413847.6 provides a high modulus glass fiber composition comprising the following components: SiO 22 50wt％～58wt％；Al2O3 18wt％～24wt％；SiO2With Al2O372.5 wt% -79.5 wt% of the total content; al (Al)2O3/SiO2The mass fraction ratio is 0.34-0.45; TiO 22 0.2wt％～1.5wt％；ZnO 0～2.0wt％；ZrO2 0～2.0wt％；Fe2O30.1wt% -0.6 wt%; 9.2 to 11 weight percent of CaO; 9 to 12 weight percent of MgO; the total content of CaO and MgO is 18.2 wt% -22 wt%; the ratio of the mass fraction of MgO to the mass fraction of CaO is 1.0-1.3; na (Na)2O and K2The total content of O is 0.2 to 1.0 weight percent; the above components amounted to 100%. The glass fiber composition can ensure that the manufactured glass fiber has excellent mechanical property and low viscosity forming property. However, there are the following problems:
the glass fiber composition and the glass fibers thereof have not been formed at a sufficiently low temperature, thereby causing difficulty in reducing the corresponding production cost.
Disclosure of Invention
In view of the above, the present invention provides a novel high modulus glass fiber composition and glass fiber, which can significantly reduce the forming temperature and production cost while ensuring an extremely high tensile modulus.
The invention provides a high modulus glass fiber composition, which comprises the following components:
preferably, the SiO2The content is 53.4wt percent to 55.9wt percent; the Al is2O3The content is 21.4 wt% -23.8 wt%; the SiO2With Al2O3The total content of (A) is 76.5 wt% -79 wt%.
Preferably, the CaO content is 8.4wt% to 9.9 wt%; the MgO content is 10.2wt% -11.8 wt%; the total content of CaO and MgO is 19.5wt% -21.5 wt%; the ratio of the MgO/CaO mass fraction is 1.06-1.39.
Preferably, the Na is2O and K2The total content of O is 0.2 to 0.8 weight percent.
Preferably, the total content of the remaining impurity components is not more than 0.5 wt%.
The invention provides a high modulus glass fiber prepared from the composition of the technical scheme.
Compared with the prior art, the invention provides a high modulus glass fiber composition, which comprises the following components: SiO 2253wt％～55.9wt％；Al2O3 21.1wt％～23.9wt％；SiO2With Al2O376.5 wt% -79 wt% of the total content; al (Al)2O3/SiO2The mass fraction ratio is 0.38-0.45; TiO 22 0.3wt％～1.5wt％；Fe2O30.1wt% -0.5 wt%; CaO 8.2wt% -9.9 wt%; 9.9 to 11.8 weight percent of MgO; the total content of CaO and MgO is 18.8wt% -21.6 wt%; the ratio of the mass fraction of MgO to the mass fraction of CaO is 1.01 to 1.41; na (Na)2O and K2The total content of O is 0.2 to 1.0 weight percent; the total content of other impurity components is not more than 1 wt%. The invention controls the specific percentage content of each component, so that the finally obtained high-modulus glass fiber has extremely high drawing dieVolume, lower molding temperature and lower production cost. Tests prove that the forming temperature of the glass fiber is not more than 1300 ℃, the upper limit temperature of crystallization is lower than 1250 ℃, and the elastic modulus of the glass fiber is more than 95 GPa. In addition, compared with the prior art, the production cost of the invention can be reduced by more than 10%.
Detailed Description
The invention provides a high modulus glass fiber composition and glass fiber, and the technical personnel can use the content in reference to the text and properly improve the technological parameters to realize. It is expressly intended that all such similar substitutes and modifications apparent to those skilled in the art are deemed to be within the scope of the invention. While the methods and applications of this invention have been described in terms of preferred embodiments, it will be apparent to those of ordinary skill in the art that variations and modifications in the methods and applications described herein, as well as other suitable variations and combinations, may be made to implement and use the techniques of this invention without departing from the spirit and scope of the invention.
The invention provides a high modulus glass fiber composition, which comprises the following components:
wherein the silicon dioxide (SiO)2) Is one of the main oxides forming the glass network, which mainly plays a role in improving the mechanical strength, chemical stability and thermal stability of the glass, but too high content increases the viscosity and melting temperature of the glass, resulting in high difficulty in forming glass fibers and high production cost. The invention tests and discovers that SiO2The content is controlled below 55.9 wt%, the tensile modulus of the glass fiber is not greatly influenced, and the forming temperature can be obviously reduced, which is significant for reducing the production difficulty and the production cost of the glass fiber. But if SiO2At a content of less than 53 wt%, the tensile strength of the glass fibers is again too low. Thus, SiO in the glass fiber composition of the present invention2The content is 53 to 55.9 wt%, preferably 53.4 to 55.9 wt%.
Alumina (Al)2O3) Is also formedOne of the main oxides of the glass network, which has a positive effect on the chemical stability and mechanical strength of the glass, in particular on the elastic modulus of the glass. The invention tests and finds that in SiO2-Al2O3In the-CaO-MgO system, Al2O3The content has the greatest influence on the tensile modulus of the glass fiber, and the tensile modulus of the glass fiber almost follows Al2O3The content increase rises parabolically. If glass fibers with tensile modulus of more than 95GPa are to be obtained, Al2O3The content should be more than 21.1 wt%, preferably more than 21.4 wt%. If Al2O3The content exceeding 23.9 wt% causes excessive viscosity of the glass, makes glass fiberization difficult, and is also prone to devitrification problems. Thus, Al in the composition of the invention2O3The content is 21.1 wt% to 23.9 wt%, preferably 21.4 wt% to 23.8 wt%.
In SiO2-Al2O3In the-CaO-MgO system, Al2O3And SiO2The higher the total content of the main body forming the glass network structure, the more complete the glass network structure and the higher the mechanical property of the glass. The invention tests show that Al2O3And SiO2The total content is kept above 76.5 wt%, so that the mechanical properties, particularly the tensile modulus, of the glass fiber can meet the expected requirements. Among them, Al2O3/SiO2The ratio is more closely related to the tensile modulus of the glass fiber, and the mass fraction ratio at least exceeds 0.38, so that the elastic modulus of the glass fiber can reach 95 GPa. But at the same time, if SiO2With Al2O3Total content of (A) or Al2O3/SiO2Too high a proportion also increases the forming temperature and the tendency to devitrify of the glass fibers significantly, making production difficult to accept. Thus, the invention defines SiO2With Al2O3The total content of (A) is 76.5 wt% to 79wt%, preferably 77.2wt% to 79 wt%. Al (Al)2O3/SiO2The mass fraction ratio is 0.38-0.45, and preferably, the Al is2O3/SiO2The mass fraction ratio is 0.39-0.43. This ratio range ensures that the glass fiber has an excellent modulus of elasticity andoptimal melting performance and wire drawing forming performance.
Titanium dioxide (TiO)2) Small ion radius, strong field and certain function of gathering glass network. Thus, the glass contains a small amount of titanium dioxide (TiO)2) The high-temperature fluidity and the crystallization tendency of the glass are improved, and the mechanical property and the corrosion resistance of the glass fiber are improved. However, the content of titanium dioxide should not exceed 1.5 wt.%, otherwise the color of the glass is significantly affected. TiO in the invention2The content of (B) is limited to 0.3wt% to 1.5 wt%.
Due to iron oxide (Fe)2O3) A small amount of Fe widely existing in various mineral raw materials and in glass2O3Entrainment is inevitable and does not exceed 0.5wt% Fe2O3The influence on the performance of the glass fiber is small, and in order to reduce the purchasing cost of mineral raw materials as much as possible, the content of the ferric oxide is limited to 0.1 to 0.5 weight percent.
The calcium oxide (CaO) and the magnesium oxide (MgO) are oxides of the same family, and have the functions of filling network gaps, improving the high-temperature melting performance of the glass and the crystallization tendency of the glass in a glass network structure. But the radius of MgO ions is smaller than that of CaO, the field intensity is larger, so that a higher MgO proportion is beneficial to forming a more compact glass network structure and improving the tensile modulus of the glass. If the content of CaO is too high, the network breaking effect of the CaO in the glass network structure is too strong, and the tensile modulus of the glass is improved. Therefore, the CaO content is limited to 8.2wt% to 9.9wt%, and preferably, the CaO content is 8.4wt% to 9.9wt%, and the MgO content is 9.9wt% to 11.8 wt%, and preferably, 10.2wt% to 11.8 wt%; the total content of CaO and MgO is 18.8wt% to 21.6 wt%, preferably 19.5wt% to 21.5 wt%. The MgO/CaO mass fraction ratio is 1.01-1.41, and preferably, the MgO/CaO mass fraction ratio is 1.06-1.39.
Na2O and K2O as an alkali metal oxide, too high a content impairs the chemical stability and mechanical properties of the aluminosilicate glass, and special addition is generally not recommended. Na in the glass fiber composition of the present invention2O and K2O is the awn used when the mineral raw material impurity form is brought into or adjusted the kiln atmosphereThe nitrate is brought in, and a small amount of the components also have the positive effects of reducing the viscosity of the glass and improving the devitrification tendency of the glass. Therefore, from the viewpoint of the cost of raw materials and the quality of glass fibers, Na is contained in the glass composition of the present invention2O and K2The total O content is limited to 0.2 to 1.0wt%, preferably 0.2 to 0.8%.
In addition to the above components, the present invention is substantially free of other components, such as F, ZnO, ZrO2BaO, SrO, rare earth elements and the like. "substantially free" as used herein means not specifically added and the content of each component is less than 0.1%. Since the glass fiber components are generally introduced through natural minerals, trace elements which are not the main component of the present invention may be introduced as impurities. It is neither practical nor economical to strictly limit the content of these impurities in the present invention to 0 completely. Therefore, from the viewpoint of the raw material cost and the quality of the glass fiber, the total content of impurities in the present invention is limited to not more than 1wt%, and preferably not more than 0.5 wt%.
The invention discovers that Al is prepared by a large number of experiments2O3、SiO2The content range and the relative proportion of MgO and CaO are accurately controlled in a certain specific area, so that the glass fiber has extremely high tensile modulus, and simultaneously, the melt-drawing performance and the crystallization temperature of the glass fiber are in an acceptable range; a small amount of TiO with small ionic radius and large electric field intensity is properly introduced2The glass can further inhibit the crystallization tendency of the glass, and has positive effect on the elastic modulus of the glass. Meanwhile, the invention does not need to add rare earth elements, ZnO and ZrO with higher price2BaO, SrO and the like, can simultaneously realize extremely high tensile modulus and lower molding temperature, and has more advantages in manufacturing cost. Therefore, the glass fiber of the present invention combines extremely high tensile modulus, lower forming temperature and lower production cost by precisely defining the content range and relative proportion of the components. Tests prove that the forming temperature of the glass fiber is not more than 1300 ℃, the upper limit temperature of crystallization is lower than 1250 ℃, and the elastic modulus of the glass fiber is more than 97 GPa. Moreover, compared with the prior art mentioned in the background of the invention, the invention has the advantages that the production cost can be reducedThe reduction is more than 10 percent.
In a preferred embodiment of the present invention, the high modulus glass fiber composition comprises the following components:
the invention also provides a high modulus glass fiber prepared from the composition.
The method for preparing the glass fiber is not particularly limited, and the glass fiber can be prepared by a method well known to those skilled in the art, preferably by a tank furnace method, and can be prepared by the following method:
uniformly mixing various raw materials, putting the mixture into a tank furnace, and melting, clarifying and homogenizing the mixture to obtain molten glass;
and cooling, flowing out and drawing the molten glass to obtain the glass fiber.
Firstly, mixing various raw materials in a mixing tank, and conveying the raw materials to a tank furnace bin after the raw materials are uniformly mixed; then putting the mixture into a tank furnace bin, and melting, clarifying and homogenizing at 1400-1800 ℃ to obtain molten glass;
cooling the molten glass to 1250-1350 ℃, enabling the molten glass to flow out through a platinum bushing plate, and drawing the molten glass into glass wires with the diameter of 3-25 mu m under the traction of a drawing machine;
and carrying out spray cooling on the glass filaments, and coating a sizing agent to obtain the glass fiber.
After obtaining the glass fiber, the glass fiber was subjected to a performance test.
Experimental results show that the forming temperature of the glass fiber is not more than 1300 ℃, the upper limit crystallization temperature is lower than 1250 ℃, and the elastic modulus of the glass fiber is greater than 95 GPa. In addition, compared with the prior art, the production cost of the invention can be reduced by more than 10%.
To further illustrate the present invention, the high modulus glass fiber composition and glass fibers provided by the present invention are described in detail below with reference to the examples.
Example 1
Conveying the raw materials to a mixing tank, uniformly mixing, and conveying the mixture to a tank furnace bin, wherein the content of each raw material is shown in table 1;
putting the mixture in a storage bin of the tank furnace into the tank furnace, melting the mixture into molten glass gradually at a high temperature of more than 1400 ℃ in the tank furnace, clarifying and homogenizing the molten glass, and feeding the stable and high-quality molten glass into a wire drawing operation channel;
cooling the glass liquid in the wire drawing operation channel to a proper temperature, then flowing out through a platinum bushing, rapidly drawing the glass liquid into glass wires with the diameter of 3-25 mu m by a wire drawing machine, and winding the glass wires into wire cakes on the wire drawing machine after the glass wires are subjected to spray cooling, impregnating compound coating and collecting;
all the spinning cakes are dried, spooled or chopped to obtain various types of glass fiber products.
The glass fibers were subjected to performance tests, and the results are shown in table 1, where table 1 shows the formulations and properties of the glass fibers provided in the examples and comparative examples of the present invention.
Examples 2 to 15
The preparation method is the same as the example, except that the content of each raw material is changed, and the specific content is shown in table 1.
The glass fibers were subjected to performance tests, the results of which are shown in table 1, and table 1 is a table of formulations and performance data of the glass fibers provided in examples and comparative examples of the present invention.
Comparative example
Conveying various raw materials to a mixing tank according to a formula shown in table 1, uniformly mixing, and conveying a mixture to a storage bin of a tank furnace, wherein the content of each raw material is shown in table 1;
putting the mixture in a storage bin of the tank furnace into the tank furnace, melting the mixture into molten glass gradually at a high temperature of more than 1400 ℃ in the tank furnace, clarifying and homogenizing the molten glass, and feeding the stable and high-quality molten glass into a wire drawing operation channel;
cooling the glass liquid in the wire drawing operation channel to a proper temperature, then flowing out through a platinum bushing, rapidly drawing the glass liquid into glass wires with the diameter of 3-25 mu m by a wire drawing machine, and winding the glass wires into wire cakes on the wire drawing machine after the glass wires are subjected to spray cooling, impregnating compound coating and collecting;
and drying, winding or chopping all the spinning cakes to obtain the glass fiber.
The glass fibers were subjected to performance tests, the results of which are shown in table 1.
TABLE 1 formulation and Performance data Table for glass fibers provided in examples and comparative examples
TABLE 1 continuation
Table 1 shows the chemical compositions of the glass compositions of the respective examples and comparative examples in terms of mass%. For convenience of calculation, when designing the glass components in table 1, the contents of each component in the table neglect impurity components so that the total content of the introduced components is 100%, and in actual test, there may be slight differences due to instrument errors and trace impurity influences.
The high-temperature viscosity of the glass fiber is detected by a BROOKFIELD high-temperature viscometer produced by ORTON company; the glass liquidus temperature is detected by an Orton Model gradient furnace; the glass softening point is measured by an Orton Model SP-1100 softening point tester;
Tlogη＝3indicates a glass viscosity of 103The temperature at the time of forming the glass fibers corresponds to the temperature of the molten glass at the time of forming the glass fibers, and is also referred to as the glass fiber forming temperature.
TLiquid for treating urinary tract infectionThe liquidus temperature of the glass corresponds to the temperature at which the glass crystallization rate is 0 and also corresponds to the upper limit of the glass crystallization temperature.
Δ T is Tlogη＝3And TLiquid for treating urinary tract infectionDifference of (2)The value is generally used for representing the forming difficulty of the glass fiber, and the glass fiber can be stably drawn and formed when the delta T is more than or equal to 50 ℃.
As can be seen from the above examples and comparative examples, the invention improves the comprehensive properties of the glass fiber by precisely adjusting various components and specific contents thereof.
The above description of the embodiments is only intended to facilitate the understanding of the method of the invention and its core idea. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention.
Claims (2)
1. A novel high modulus glass fiber composition characterized by being selected from any one of the following group of formulations: comprises the following components:
SiO2 55.0wt%、Al2O3 23.6wt%、SiO2with Al2O378.6wt% of Al2O3/SiO2Mass fraction ratio of 0.43, TiO2 0.3wt%、Fe2O30.1wt%, CaO 9.8wt%, MgO 10.4wt%, total content of CaO and MgO 20.2wt%, MgO/CaO mass fraction ratio 1.06, Na2O and K2The total content of O is 0.8 wt%;
SiO2 55.6wt%、Al2O3 22.7wt%、SiO2with Al2O378.3wt% of Al2O3/SiO2Mass fraction ratio of 0.41, TiO2 0.6wt%、Fe2O30.5wt%, CaO 9.6wt%, MgO 10.6wt%, total content of CaO and MgO 20.2wt%, MgO/CaO mass fraction ratio 1.10, Na2O and K2The total content of O is 0.4 wt%;
SiO2 54.5wt%、Al2O3 23.3wt%、SiO2with Al2O3Total content of (3) 77.8wt%, Al2O3/SiO2Mass fraction ratio of 0.43, TiO2 0.7wt%、Fe2O3 0.3wt%、9.4 percent of CaO, 11.2 percent of MgO, 20.6 percent of the total content of CaO and MgO, 1.19 percent of MgO/CaO mass fraction ratio, and Na2O and K2The total content of O is 0.6 wt%;
SiO2 53wt%、Al2O3 23.9wt%、SiO2with Al2O376.9wt% of total Al2O3/SiO2Mass fraction ratio of 0.45, TiO2 1.5wt%、Fe2O30.3wt%, CaO 9.8wt%, MgO 10.7wt%, total content of CaO and MgO 20.5wt%, MgO/CaO mass fraction ratio 1.09, Na2O and K2The total content of O is 0.8 wt%;
SiO2 53.4wt%、Al2O3 23.8wt%、SiO2with Al2O3Total content of (3) 77.2wt%, Al2O3/SiO2Mass fraction ratio of 0.45, TiO2 1.0wt%、Fe2O30.3wt%, CaO 9.8wt%, MgO 10.9wt%, total content of CaO and MgO 20.7wt%, MgO/CaO mass fraction ratio 1.11, Na2O and K2The total content of O is 0.6 wt%;
SiO2 55.5wt%、Al2O3 23.0wt%、SiO2with Al2O378.5wt% of Al2O3/SiO2Mass fraction ratio of 0.41, TiO2 1.0wt%、Fe2O30.3wt%, CaO 8.3wt%, MgO 11.7wt%, CaO and MgO total content 20wt%, MgO/CaO mass fraction ratio 1.41, Na2O and K2The total content of O is 0.6 wt%;
SiO2 55.4wt%、Al2O3 23.1wt%、SiO2with Al2O378.5wt% of Al2O3/SiO2Mass fraction ratio of 0.42, TiO2 0.8wt%、Fe2O30.3wt%, CaO 8.2wt%, MgO 11.6wt%, CaO and MgO total content 19.8wt%, MgO/CaO mass fraction ratio 1.41, Na2O and K2The total content of O is 0.6 wt%;
SiO2 55.3wt%、Al2O3 23.7wt%、SiO2with Al2O3Total content of (9 wt.%), Al2O3/SiO2Mass fraction ratio of 0.43, TiO2 0.8wt%、Fe2O30.3wt%, CaO 9.8wt%, MgO 9.9wt%, total content of CaO and MgO 19.7wt%, MgO/CaO mass fraction ratio 1.01, Na2O and K2The total content of O is 0.2 wt%;
SiO2 55.2wt%、Al2O3 22.7wt%、SiO2with Al2O3Total content of (3) 77.9wt%, Al2O3/SiO2Mass fraction ratio of 0.41, TiO2 1.2wt%、Fe2O30.3wt%, CaO 9.8wt%, MgO 10.2wt%, the total content of CaO and MgO is 20wt%, the ratio of MgO/CaO mass fraction is 1.04, Na2O and K2The total content of O is 0.6 wt%;
SiO2 55.8wt%、Al2O3 22.9wt%、SiO2with Al2O378.7wt% of Al2O3/SiO2Mass fraction ratio of 0.41, TiO2 1.5wt%、Fe2O30.3wt%, CaO 8.4wt%, MgO 10.4wt%, total content of CaO and MgO 18.8wt%, MgO/CaO mass fraction ratio 1.24, Na2O and K2The total content of O is 0.7 wt%; or the like, or, alternatively,
SiO2 55.3wt%、Al2O3 22.8wt%、SiO2with Al2O378.1wt% of Al2O3/SiO2Mass fraction ratio of 0.41, TiO2 1.3wt%、Fe2O30.1wt%, CaO 9.3wt%, MgO 10.2wt%, CaO and MgO total content 19.5wt%, MgO/CaO mass fraction ratio 1.10, Na2O and K2The total O content was 1.0 wt%.
2. A high modulus glass fiber prepared from the composition of claim 1.
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