CN112979168A - High-elasticity-modulus glass fiber composition and preparation method thereof - Google Patents
High-elasticity-modulus glass fiber composition and preparation method thereof Download PDFInfo
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- 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
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
- C03C3/095—Glass compositions containing silica with 40% to 90% silica, by weight containing rare earths
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Abstract
The invention discloses a high-elasticity-modulus glass fiber composition and a preparation method thereof, belonging to the technical field of inorganic nonmetallic materials. The high-elasticity-modulus glass fiber composition consists of the following components: SiO 22、Al2O3、CaO、MgO、Ce2O3、Yb2O3、ZrO2、BaO、R2O; the R is2O is Na2O、K2O and Li2A mixture of O. The invention is on SiO2And Al2O3In the network formed, by limiting the amount of each substance added, CaO/Al in particular2O3MgO and Ce2O3/Yb2O3The weight ratio of (a) to (b) makes it difficult for each ion to move in the network by utilizing a synergistic effect between each ion, thereby improving the elastic modulus and the tensile strength.
Description
Technical Field
The invention relates to the technical field of inorganic nonmetallic materials, in particular to a high-elasticity-modulus glass fiber composition and a preparation method thereof.
Background
Glass fiber (Fiberglass) is an inorganic non-metallic material with excellent performance, has good insulativity, strong heat resistance, good corrosion resistance and high mechanical strength, but is brittle and has poor wear resistance. The hair-care fiber is made of six kinds of ores of pyrophyllite, quartz sand, limestone, dolomite, borocalcite and boromagnesite through the processes of high-temperature melting, wire drawing, winding, weaving and the like, wherein the diameter of each monofilament ranges from several micrometers to twenty micrometers, the monofilament is equivalent to 1/20-1/5 of one hair, and each bundle of fiber precursor consists of hundreds of even thousands of monofilaments. Glass fibers are commonly used in various fields of national economy, such as reinforcing materials, electrical insulating materials, thermal insulating materials, and circuit substrates in composite materials. In the application process of the glass fiber, along with the continuous increase of the size of the composite material product, people put higher and higher requirements on the mechanical property, especially the elastic modulus of the glass fiber.
In the prior art, there are many methods for improving the elastic modulus of glass fiber, such as S glass, and the basic composition 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.
The prior publications mostly increase the modulus of elasticity of glass fibers by adding different substances, such as: patent document CN108751728A discloses a high modulus glass fiber composition produced based on basalt. The composition comprises the following components in percentage by weight: SiO 22：53.0-60.0％；Al2O3：24.5-28.0％；MgO：8.0-15.0％；Fe2O3：1.5-5.5％；TiO2：2.0-4.0％；0＜CaO≤5.0％；0＜Na2O≤1.5％；0＜K2O is less than or equal to 0.5 percent. The invention is prepared by utilizing basalt mineral raw materials and conventional glass fiber mineral raw materials, and introduces Fe with a certain proportion2O3The components enable the glass fiber to have the characteristics of high strength, high modulus and the like which are peculiar to the basalt glass fiber. But Fe2O3The existence of (2) easily causes phase separation of glass, so that the stability is poor and the mechanical strength is poor; and the content of titanium dioxide is higher, so that the color of the glass is darker, and the application of the glass is limited.
Patent document CN107216042A discloses a high modulus glass fiber composition comprising the following components: SiO 2250wt％-58wt％；Al2O3 18wt％-24wt％；SiO2With Al2O372.5 to 79.5 weight percent 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％；Fe2O30.1 wt% -0.6 wt%; 9.2 to 11 weight percent of CaO; 9-12 wt% of MgO; the total content of CaO and MgO is 18.2 wt% -22 wt%; the ratio of MgO/CaO in mass fraction is 1.0-1.3; na (Na)2O、K2O and Li2The total content of O is 0.2 to 1.0 weight percent; the above components amounted to 100%. However, too high a content of magnesium oxide increases the tendency of the glass to devitrify.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a high-elasticity modulus glass fiber composition and a preparation method thereof; the glass fiber composition can effectively reduce the crystallization rate of glass, has higher elastic modulus reaching 105GPa on the basis of ensuring higher tensile strength, and is suitable for large-scale production.
In order to solve the technical problems, the invention provides the following technical scheme:
on one hand, the invention provides a high-elasticity modulus glass fiber composition which comprises the following components in percentage by weight:
SiO2 54-57wt％；
Al2O3 14-18wt％；
CaO 12-18wt％；
MgO 5-10.5wt％；
Ce2O3 1-4.2wt％；
Yb2O3 0.5-3.5wt％；
ZrO2 0.2-0.5wt％；
BaO 0.1-0.5wt％；
R2O 0.7-1.0wt％。
preferably, the glass fiber composition with high elastic modulus comprises the following components in percentage by weight:
SiO2 55-56wt％；
Al2O3 15-18wt％；
CaO 14-16wt％；
MgO 6-8wt％；
Ce2O3 2.3-4.2wt％；
Yb2O3 1-3.5wt％；
ZrO2 0.2-0.5wt％；
BaO 0.3-0.5wt％；
R2O 0.8-0.9wt％。
further, said R2O is Na2O、K2O and Li2A mixture of O; wherein Li2O stands for R250-60% of the total weight of O.
Further, the CaO and Al2O3The weight ratio of MgO to MgO is 1:0.88-1.5: 0.33-0.78; ce2O3And Yb2O3The weight ratio of (A) to (B) is 1: 0.12-0.94.
Preferably, the CaO and Al are2O3The weight ratio of MgO to MgO is 1:1-1.5: 0.5-0.78; ce2O3And Yb2O3The weight ratio is 1: 0.8-0.94.
On the other hand, the invention also provides a preparation method of the high-elasticity-modulus glass fiber composition, which comprises the steps of weighing raw materials in proportion, putting the raw materials into a glass melting furnace, carrying out vitrification and melting treatment, and then carrying out spinning forming to obtain the glass fiber.
Preferably, the melting temperature is 1300-.
Preferably, the spinning temperature is 1200-1300 ℃, and the temperature difference Delta T between the spinning temperature and the liquid phase temperature is 30-80 ℃.
Compared with the prior art, the invention has the following beneficial effects:
SiO in the invention2The framework main body for forming glass is a network forming object, and in order to improve the modulus of glass fiber, SiO is reduced to a certain extent2In order to ensure chemical stability and mechanical strength, SiO is limited2The content is 54-57%.
Al2O3The addition of (2) has an influence on the crystallization tendency, stability and mechanical strength of the glass fiber, and the stability and mechanical strength of the glass fiber can be improved when the addition amount is higher, but the crystallization rate is increased, the melting difficulty is improved, the viscosity is increased, and the difficulty in the glass melting process is increased.
In order to adjust the viscosity of the glass and the crystallization of the glass, certain content of CaO and MgO is added, and CaO and Al are subjected to crystallization2O3The weight ratio of (a) to (b), reducing the viscosity of the glass; meanwhile, the crystallization tendency can be effectively reduced and the strength can be improved to a certain extent by adjusting the proportion of the dosage of CaO and MgO. Further, Ce2O3、Yb2O3、ZrO2BaO and the like are good fluxes, and can reduce the difficulty in melting to some extent.
The invention is on SiO2And Al2O3The network is formed by introducing calcium, magnesium, cerium, ytterbium, zirconium, barium and the like, and by limiting the addition amount of each substance, particularly CaO/Al2O3MgO and Ce2O3/Yb2O3The weight ratio of (A) to (B) is utilized, and the synergistic effect among ions is utilized, so that the network is more compact, and the ions are difficult to move in the network, thereby improving the elastic modulus and the tensile strength and reducing the crystallization tendency.
Detailed Description
In order to make the technical problems, technical solutions and advantages to be solved by the present invention clearer, the following detailed description is given with reference to specific embodiments.
In the present invention, the materials and reagents used are not specifically described, and are commercially available.
The invention provides a high-elasticity modulus glass fiber composition and a preparation method thereof, and specific examples are as follows.
Example 1
Weighing the raw materials according to the formula of the example 1 in the table 1, putting the raw materials into a glass melting furnace, carrying out vitrification and melting treatment at 1300-1300 ℃ and then carrying out spinning forming at the temperature of 1200-1300 ℃ to obtain the glass fiber. And the performance of the prepared glass fiber is tested, and the results are shown in table 2.
Examples 2 to 8
Weighing the raw materials according to the formulas of the examples 2-8 in the table 1, putting the raw materials into a glass melting furnace, carrying out vitrification and melting treatment at 1300 ℃ and 1400 ℃, and then carrying out spinning forming at the temperature of 1200 ℃ and 1300 ℃ to obtain the glass fiber. And the performance of the prepared glass fiber is tested, and the results are shown in table 2.
To further illustrate the beneficial effects of the present application, a comparative example was constructed as follows, using example 3 as an example only, for reasons of space.
Comparative example 1
Replacement of Yb2O3 with the same amount of La2O3The other conditions were the same as in example 3.
Comparative example 2
Replacement of Yb2O3 with an equivalent amount of Y2O3The other conditions were the same as in example 3.
Comparative examples 3 to 7
Weighing the raw materials according to the formulas of comparative examples 3-7 in the table 1, putting the raw materials into a glass melting furnace, carrying out vitrification and 1400 ℃ melting treatment, and then carrying out spinning forming at the temperature of 1200 ℃ and 1300 ℃ to obtain the glass fiber.
The glass fibers prepared in comparative examples 1 to 7 were subjected to property tests, and the results are shown in Table 2.
TABLE 1
| Serial number | SiO2 | Al2O3 | CaO | MgO | Ce2O3 | Yb2O3 | ZrO2 | BaO | Na2O | K2O | Li2O |
| Example 1 | 54 | 17 | 18 | 6 | 1.8 | 1.7 | 0.5 | 0.2 | 0.2 | 0.2 | 0.4 |
| Example 2 | 57 | 16 | 12 | 9.3 | 3 | 1 | 0.4 | 0.5 | 0.2 | 0.12 | 0.48 |
| Example 3 | 55 | 15 | 14 | 7 | 4.2 | 3.5 | 0.3 | 0.1 | 0.3 | 0.15 | 0.45 |
| Example 4 | 56 | 14 | 16 | 7 | 3.9 | 1.6 | 0.2 | 0.3 | 0.2 | 0.3 | 0.5 |
| Example 5 | 56 | 18 | 12 | 8 | 4.1 | 0.5 | 0.4 | 0.2 | 0.1 | 0.3 | 0.4 |
| Example 6 | 55 | 15 | 16 | 10.5 | 1 | 0.7 | 0.4 | 0.4 | 0.2 | 0.25 | 0.55 |
| Example 7 | 57 | 16 | 14 | 5 | 3.4 | 3 | 0.3 | 0.3 | 0.2 | 0.2 | 0.6 |
| Example 8 | 56 | 15 | 15 | 8 | 2.3 | 2 | 0.5 | 0.4 | 0.2 | 0.16 | 0.44 |
| Comparative example 1 | 55 | 15 | 14 | 7 | 4.2 | -- | 0.3 | 0.1 | 0.3 | 0.15 | 0.45 |
| Comparative example 2 | 55 | 15 | 14 | 7 | 4.2 | -- | 0.3 | 0.1 | 0.3 | 0.15 | 0.45 |
| Comparative example 3 | 55 | 15 | 14 | 7 | 7.7 | -- | 0.3 | 0.1 | 0.3 | 0.15 | 0.45 |
| Comparative example 4 | 55 | 15 | 14 | 7 | 4.2 | 3.5 | 0.3 | 0.1 | 0.3 | 0.3 | 0.3 |
| Comparative example 5 | 55 | 15 | 17.5 | 3.5 | 4.2 | 3.5 | 0.3 | 0.1 | 0.3 | 0.15 | 0.45 |
| Comparative example 6 | 55 | 19 | 10 | 7 | 4.2 | 3.5 | 0.3 | 0.1 | 0.3 | 0.15 | 0.45 |
| Comparative example 7 | 55 | 11.6 | 17.4 | 7 | 4.2 | 3.5 | 0.3 | 0.1 | 0.3 | 0.15 | 0.45 |
TABLE 2
| Serial number | Fiber forming temperature,. degree.C | Liquidus temperature,. degree.C | △T，℃ | Modulus of elasticity, GPa | Tensile strength, MPa |
| Example 1 | 1334 | 1294 | 40 | 101.4 | 2146 |
| Example 2 | 1326 | 1273 | 53 | 103.5 | 2253 |
| Example 3 | 1319 | 1284 | 35 | 104.3 | 2284 |
| Example 4 | 1337 | 1292 | 45 | 102.4 | 2137 |
| Example 5 | 1357 | 1279 | 78 | 101.6 | 2168 |
| Example 6 | 1336 | 1287 | 49 | 102.7 | 2156 |
| Example 7 | 1341 | 1267 | 74 | 102.9 | 2179 |
| Example 8 | 1316 | 1268 | 48 | 105.6 | 2210 |
| Comparative example 1 | 1322 | 1267 | 55 | 91.5 | 1846 |
| Comparative example 2 | 1346 | 1235 | 111 | 94.4 | 1792 |
| Comparative example 3 | 1317 | 1249 | 68 | 92.6 | 1922 |
| Comparative example 4 | 1329 | 1257 | 72 | 98.6 | 1934 |
| Comparative example 5 | 1336 | 1268 | 68 | 87.5 | 1846 |
| Comparative example 6 | 1342 | 1264 | 78 | 92.7 | 1857 |
| Comparative example 7 | 1325 | 1256 | 69 | 82.6 | 1916 |
Note: the value of Delta T: the difference between the forming temperature and the liquidus temperature indicates the temperature range of the wire drawing.
As can be seen from tables 1 and 2, the invention successfully prepares the glass fiber with high elastic modulus, and the elastic modulus can reach 105GPa at most. At the same time, by SiO2、Al2O3、Ce2O3、Yb2O3、ZrO2And the glass fiber has lower forming temperature and liquidus temperature due to the synergistic effect of BaO and the like, and is convenient to prepare.
Yb in the present invention was compared with comparative examples 1 to 32O3Respectively replaced by La2O3Or Y2O3、Ce2O3The resulting composition showed little difference between the glass fiber forming temperature and the liquidus temperature as compared with the examples, but the elastic modulus was much lower than that of the glass fiber of the present invention and the tensile strength. This is probably because the difference between the ionic radii of Yb ions and La, Y and Ce ions is large, and Yb can enter SiO well2And Al2O3The formed network prevents ions from moving in the network, so that the network has higher elastic modulus and higher tensile strength.
As can be seen from the data in Table 2, the present inventionCaO/Al in specified proportion range2O3MgO and Ce2O3/Yb2O3In a weight ratio of (A) and R2Li in O2The proportion of the O used can obtain the glass fiber with larger elastic modulus and stability.
Reduction of Li in comparative example 42Amount of O to R233% of O, the elastic modulus of the obtained glass fiber is reduced by 5.25% compared with that of the glass fiber obtained in the embodiment 3 of the invention, and the tensile strength is also reduced by 15.3%; this is because Li2The O amount can greatly accelerate the melting of the glass, improve the chemical stability, the surface tension and the crystallization capacity of the glass, ensure that all components in the glass fiber are uniformly distributed and have higher elastic modulus and higher tensile strength.
In comparative examples 3 to 7, CaO/Al was adjusted2O3The ratio of CaO and MgO is within the range of the present invention, and the elastic modulus and tensile strength of the obtained glass fiber are greatly different from those of the glass fiber of the present invention of example 3 because CaO and Al are in the specific ratio range2O3And the three substances act synergistically with MgO, so that the viscosity in the glass melting process can be reduced, the crystallization tendency is effectively reduced, and the strength is improved to a certain extent.
In conclusion, the present invention is on SiO2And Al2O3The network is formed by introducing calcium, magnesium, cerium, ytterbium, zirconium, barium and the like, and by limiting the addition amount of each substance, particularly CaO/Al2O3MgO and Ce2O3/Yb2O3The weight ratio of (a) to (b) is such that the network is more compact and the movement of ions in the network is difficult by utilizing the synergistic effect between the ions, thereby improving the elastic modulus and tensile strength.
The foregoing is a preferred embodiment of the present invention, and it will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the principles of the invention and are intended to be within the scope of the invention.
Claims (7)
1. The high-elasticity-modulus glass fiber composition is characterized by comprising the following components in percentage by weight:
SiO2 54-57wt％；
Al2O3 14-18wt％；
CaO 12-18wt％；
MgO 5-10.5wt％；
Ce2O3 1-4.2wt％；
Yb2O3 0.5-3.5wt％；
ZrO2 0.2-0.5wt％；
BaO 0.1-0.5wt％；
R2O 0.7-1.0wt％；
the R is2O is Na2O、K2O and Li2A mixture of O; wherein Li2O stands for R250-60% of the total weight of O.
2. The high elastic modulus glass fiber composition according to claim 1, which is composed of the following components in percentage by weight:
SiO2 55-56wt％；
Al2O3 15-18wt％；
CaO 14-16wt％；
MgO 6-8wt％；
Ce2O3 2.3-4.2wt％；
Yb2O3 1-3.5wt％；
ZrO2 0.2-0.5wt％；
BaO 0.3-0.5wt％；
R2O 0.8-0.9wt％。
3. the high elastic modulus glass fiber of claim 1 or 2The vitamin composition is characterized in that the CaO and the Al are2O3The weight ratio of MgO to MgO is 1:0.88-1.5: 0.33-0.78; ce2O3And Yb2O3The weight ratio of (A) to (B) is 1: 0.12-0.94.
4. The high elastic modulus glass fiber composition of claim 3, wherein said CaO, Al2O3The weight ratio of MgO to MgO is 1:1-1.5: 0.5-0.78; ce2O3And Yb2O3The weight ratio is 1: 0.8-0.94.
5. The method for preparing the glass fiber composition with high elastic modulus as claimed in any one of claims 1 to 4, wherein the glass fiber is obtained by weighing raw materials in proportion, putting the raw materials into a glass melting furnace, carrying out vitrification and melting treatment, and then carrying out spinning molding.
6. The method for preparing a glass fiber composition with high elastic modulus as claimed in claim 5, wherein the melting temperature is 1300-1400 ℃.
7. The method for preparing a glass fiber composition with high elastic modulus as claimed in claim 6, wherein the spinning temperature is 1200 ℃ and 1300 ℃, and the temperature difference Δ T between the spinning temperature and the liquidus temperature is 30-80 ℃.
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