CN108193325B - Zirconium-containing high-temperature-resistant silicon carbide fiber and preparation method thereof - Google Patents
Zirconium-containing high-temperature-resistant silicon carbide fiber and preparation method thereof Download PDFInfo
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- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
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- D01F9/20—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products
- D01F9/24—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- D01D5/08—Melt spinning methods
- D01D5/084—Heating filaments, threads or the like, leaving the spinnerettes
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Abstract
The invention relates to zirconium-containing high-temperature-resistant silicon carbide fiber and a preparation method thereof. The preparation method comprises the following steps: s101: dissolving yttrium oxide in ethanol, heating and uniformly stirring to obtain a first solution; s102: mixing the first solution and the nano zirconium oxide dispersion liquid and stirring uniformly to obtain a second solution; s103: dissolving polycarbosilane in xylene, adding the second solution, stirring, and heating until the solvent is completely volatilized to obtain a powdery product; s104: carrying out melt spinning and non-melting treatment on the powdery product to obtain a cross-linked fiber bundle; s105: and sintering the cross-linked fiber bundle at high temperature in an inert atmosphere, and then cooling to room temperature to obtain the silicon carbide fiber. In the preparation process of the silicon carbide fiber, the zirconium oxide and the yttrium oxide are introduced, and the silicon carbide fiber with high strength and stable performance at high temperature is prepared by utilizing the phase change volume expansion of the zirconium oxide and the high-temperature fluidity of the yttrium oxide, so that the silicon carbide fiber has good application prospect in the high-temperature fields of aerospace and the like.
Description
Technical Field
The invention relates to the technical field of high-performance fibers, in particular to zirconium-containing high-temperature-resistant silicon carbide fibers and a preparation method thereof.
Background
The silicon carbide (SiC) fiber is a ceramic fiber with high strength, high modulus and excellent high temperature resistance. Based on excellent physical mechanics and high temperature resistance, the silicon carbide fiber has very wide application prospect in the national defense advanced fields of aviation, aerospace, weaponry and the like; therefore, it is also a prohibited product of western countries for our country. Based on the method, the preparation technology of the silicon carbide fiber is researched, the blockade of foreign technologies is broken, the autonomous production of the silicon carbide fiber is realized, the research and application level of advanced composite materials and weaponry in China is certainly improved, and the method is also an important guarantee for improving the military strength and comprehensive strength in China.
In the traditional technology, Polycarbosilane (PCS) is mainly used as a precursor, and the SiC fiber is prepared by melt spinning, non-melting treatment and high-temperature sintering processes, however, the performance of the SiC fiber is very sensitive to the high-temperature treatment temperature, generally, the size of β -SiC microcrystal in the SiC fiber grows up along with the increase of the temperature under the high-temperature condition, and obvious holes and microcracks appear in the fiber, so that the fiber strength is sharply reduced.
Based on this, it is important to provide a novel method for preparing silicon carbide fiber.
Disclosure of Invention
The zirconium-containing high-temperature-resistant silicon carbide fiber has the advantages of high strength, stable high-temperature performance and the like, can be used in an environment with the temperature of over 1200 ℃, and basically keeps the performance unchanged, so that a good application prospect in the high-temperature field is shown.
Therefore, the invention provides the following technical scheme:
in a first aspect, the present invention provides a method for preparing zirconium-containing silicon carbide fiber, comprising the following steps: s101: dissolving yttrium oxide in ethanol, heating and uniformly stirring to obtain a first solution; s102: mixing the first solution and the nano zirconia dispersion liquid and uniformly stirring to obtain a second solution; s103: dissolving polycarbosilane in xylene to obtain a third solution; the preferable softening point of the polycarbosilane is 240-280 ℃, and the molecular weight of the polycarbosilane is 2500-3200; then adding the second solution into the third solution, uniformly stirring, and heating the uniformly stirred solution until the solvent is completely volatilized to obtain a powdery product; in the specific operation process, heating and stirring are carried out until the solvent is completely volatilized; s104: carrying out melt spinning and non-melting treatment on the powdery product to obtain a cross-linked fiber bundle; wherein the melt spinning is specifically as follows: the powder product was placed in a melt spinning cylinder at N2Or heating to 280-300 ℃ in Ar atmosphere for 2-4 h, then pressurizing to 2-4 MPa, and enabling the melt to flow out through a filter screen and a spinneret plate to obtain a fiber bundle; the non-melting treatment specifically comprises the following steps: putting the fiber bundle into a silk disc in an air environment, heating to 180-200 ℃ for 1-2 h, preserving heat for 2-4 h, and then N2Or heating to 420-460 ℃ for 2-3 h under Ar atmosphere, and preserving heat for 6-8 h. S105: crosslinking the fibersAnd sintering the bundles at high temperature in an inert atmosphere, and then cooling to room temperature to obtain the zirconium-containing silicon carbide fiber. Specifically, the preparation method of the nano zirconia dispersion liquid comprises the following steps: adding a certain amount of nano zirconia into deionized water, wherein the mass ratio of the nano zirconia to the deionized water is (1-10): 3000; and then adding 0.03-0.5 wt% of isopropanol or PEG as a dispersing agent, adjusting the pH value of the solution to about 10 by using NaOH, ultrasonically oscillating for 30min, and then magnetically stirring for 1-2 h to obtain the nano zirconium oxide dispersion liquid.
Preferably, in S101, the mass ratio of yttrium oxide to ethanol is 1: (5-10), the heating temperature is 40-45 ℃, the stirring speed is 200-300 r/min, and the stirring time is 30-40 min.
Preferably, in S102, the volume ratio of the first solution to the nano zirconia dispersion is 1: (10-20), the stirring speed is 200-300 r/min, and the stirring time is 90-120 min.
Preferably, in S103, the mass ratio of polycarbosilane to xylene is 1: (5-10), wherein the volume ratio of the third solution to the second solution is (5-10): 1, the stirring speed is 300-400 r/min.
Preferably, in S105, the inert gas is N2And/or Ar, and the flow rate of the inert gas is 100-200 ml/min.
Preferably, in S105, the step of sintering at a high temperature and then cooling to room temperature specifically includes: heating to 1000-1200 ℃ at the speed of 100-200 ℃/h, and preserving heat for 2-4 h; then heating to 1700-1800 ℃ at the speed of 500-600 ℃/h, and preserving heat for 0.5-1 h; and then cooling to room temperature at a speed of 100-200 ℃/h.
In a second aspect, the zirconium-containing silicon carbide fiber prepared by the method is adopted.
In a third aspect, the invention provides a zirconium-containing silicon carbide fiber for use in high temperature applications such as aerospace, and particularly in environments above 1200 ℃.
The technical scheme provided by the invention has the following advantages:
(1) the applicant has found through a great deal of research that: the zirconium-containing high-temperature-resistant silicon carbide fiber provided by the invention has the advantages of high strength, stable high-temperature performance and the like, can be used in an environment with the temperature of more than 1200 ℃, and has basically unchanged performance, thereby having good application prospect in the high-temperature field.
(2) In the preparation process of the SiC fiber provided by the invention, zirconia and yttria are introduced in a physical blending mode, the growth of β -SiC microcrystal grains is inhibited by utilizing the volume expansion generated by the transformation of zirconia at high temperature, and surface cracks in the sintering process of the silicon carbide fiber are healed by utilizing a ceramic phase with good fluidity formed by the sintering aid yttria at high temperature, so that the silicon carbide fiber with high strength and stable high-temperature performance is prepared.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Detailed Description
Hereinafter, embodiments of the present invention will be described in detail. The following examples are only for illustrating the technical solutions of the present invention more clearly, and therefore are only examples, and the protection scope of the present invention is not limited thereby.
The experimental procedures in the following examples are conventional unless otherwise specified.
The test materials used in the following examples were purchased from a conventional reagent store unless otherwise specified.
In the quantitative tests in the following examples, three replicates were set, and the data are the mean or the mean ± standard deviation of the three replicates.
The invention provides a preparation method of zirconium-containing silicon carbide fiber, which comprises the following steps:
s101: dissolving yttrium oxide in ethanol, heating to 40-50 ℃, and uniformly stirring to obtain a first solution. Wherein the mass ratio of yttrium oxide to ethanol is 1: (5-10), the heating temperature is 40-45 ℃, the stirring speed is 200-300 r/min, and the stirring time is 30-40 min.
S102: and mixing the first solution and the nano zirconium oxide dispersion liquid and uniformly stirring to obtain a second solution. Wherein the volume ratio of the first solution to the nano zirconia dispersion is 1: (10-20), the stirring speed is 200-300 r/min, and the stirring time is 90-120 min. The preparation method of the nano zirconia dispersion liquid comprises the following steps: mixing nano zirconia and deionized water according to the ratio of (1-10): 3000, adding 0.03-0.5 wt% of isopropanol or PEG as a dispersing agent, adjusting the pH value of the solution to about 10 by using NaOH, ultrasonically shaking for 30min, and then magnetically stirring for 1-2 h to obtain the nano-zirconia dispersion liquid.
S103: dissolving polycarbosilane in xylene to obtain a third solution; and adding the second solution into the third solution, uniformly stirring, heating the uniformly stirred solution to 60-80 ℃, and continuously stirring until the solvent is completely volatilized to obtain a powdery product. Wherein the mass ratio of polycarbosilane to xylene is 1: (5-10), wherein the volume ratio of the third solution to the second solution is (5-10): 1, the stirring speed is 300-400 r/min.
S104: and carrying out melt spinning and non-melting treatment on the powdery product to obtain the crosslinked fiber bundle. Wherein the melt spinning is specifically as follows: the powder product was placed in a melt spinning cylinder at N2Or heating to 280-300 ℃ in Ar atmosphere for 2-4 h, then pressurizing to 2-4 MPa, and enabling the melt to flow out through a filter screen and a spinneret plate to obtain a fiber bundle; the non-melting treatment specifically comprises the following steps: putting the fiber bundle into a silk disc in an air environment, heating to 180-200 ℃ for 1-2 h, preserving heat for 2-4 h, and then N2Or heating to 420-460 ℃ for 2-3 h under Ar atmosphere, and preserving heat for 6-8 h.
S105: and (3) placing the cross-linked fiber bundle in a sintering furnace, sintering at high temperature in an inert atmosphere, and then cooling to room temperature to obtain the zirconium-containing silicon carbide fiber. Wherein the inert gas is N2And/or Ar, wherein the flow rate of the inert gas is 100-200 ml/min; the high-temperature sintering and then the cooling to the room temperature specifically comprise the following steps: heating to 1000-1200 ℃ at the speed of 100-200 ℃/h, and preserving heat for 2-4 h; then heating to 1700-1800 ℃ at the speed of 500-600 ℃/h, and preserving heat for 0.5-1 h; and then cooling to room temperature at a speed of 100-200 ℃/h.
The following description is made with reference to specific embodiments:
example one
The embodiment provides a preparation method of zirconium-containing silicon carbide fiber, which comprises the following steps:
s101: dissolving yttrium oxide powder in ethanol. Wherein the mass ratio of the yttrium oxide to the ethanol is 1: 5. Heating to 40 deg.C, stirring at 200r/min for 40min to obtain a first solution.
S102: and mixing the first solution and the nano zirconium oxide dispersion liquid and uniformly stirring to obtain a second solution. Wherein the volume ratio of the first solution to the nano zirconia dispersion is 1:10, the stirring speed is 200r/min, and the stirring time is 90 min. The preparation method of the nano zirconia dispersion liquid comprises the following steps: mixing nano zirconia and deionized water according to the weight ratio of 1: 3000, then adding 0.03 wt% of isopropanol serving as a dispersing agent, adjusting the pH value of the solution to 10 by using NaOH, ultrasonically oscillating for 30min, and then magnetically stirring for 2h to obtain the nano-zirconia dispersion liquid.
S103: dissolving polycarbosilane in xylene to obtain a third solution; and adding the second solution into the third solution, uniformly stirring, heating the uniformly stirred solution to 80 ℃, and stirring at the speed of 400r/min until the solvent is completely volatilized to obtain a powdery product. Wherein the mass ratio of polycarbosilane to xylene is 1: and 5, the volume ratio of the third solution to the second solution is 5: 1.
s104: the powder product was placed in a melt spinning cylinder at N2Heating to 280 ℃ in the atmosphere for 2h, then pressurizing to 4MPa, and enabling the melt to flow out through a filter screen and a spinneret plate to obtain a fiber bundle; putting the fiber bundle into a silk disc in an air environment, heating to 200 ℃ for 2h, preserving the heat for 4h, and then N2And heating to 420 ℃ in the atmosphere for 2h, and preserving the heat for 6h to obtain the crosslinked fiber bundle.
S105: the cross-linked fiber bundle was placed in a sintering furnace at a flow rate of 100ml/min of N2Raising the temperature to 1000 ℃ at the speed of 100 ℃/h under the atmosphere, and preserving the temperature for 4 h; then heating to 1700 ℃ at the speed of 500 ℃/h, and preserving heat for 0.5 h; then cooling to room temperature at the speed of 100 ℃/h to obtain the zirconium-containing silicon carbide fiber.
Example two
The embodiment provides a preparation method of zirconium-containing silicon carbide fiber, which comprises the following steps:
s101: dissolving yttrium oxide powder in ethanol. Wherein the mass ratio of the yttrium oxide to the ethanol is 1: 10. Heating to 50 deg.C, stirring at 200r/min for 40min to obtain a first solution.
S102: and mixing the first solution and the nano zirconium oxide dispersion liquid and uniformly stirring to obtain a second solution. Wherein the volume ratio of the first solution to the nano zirconia dispersion is 1: 15, the stirring speed is 300r/min, and the stirring time is 120 min. The preparation method of the nano zirconia dispersion liquid comprises the following steps: mixing nano zirconia and deionized water according to the weight ratio of 10: 3000, then adding 0.5 wt% of isopropanol as a dispersing agent, adjusting the pH value of the solution to 10 by using NaOH, ultrasonically oscillating for 30min, and then magnetically stirring for 1h to obtain the nano-zirconia dispersion liquid.
S103: dissolving polycarbosilane in xylene to obtain a third solution; and adding the second solution into the third solution, uniformly stirring, heating the uniformly stirred solution to 60 ℃, and stirring at the speed of 400r/min until the solvent is completely volatilized to obtain a powdery product. Wherein the mass ratio of polycarbosilane to xylene is 1:10, the volume ratio of the third solution to the second solution is 10: 1.
s104: the powder product was placed in a melt spinning cylinder at N2Heating to 300 ℃ in the atmosphere for 4h, then pressurizing to 2MPa, and enabling the melt to flow out through a filter screen and a spinneret plate to obtain a fiber bundle; putting the fiber bundle into a silk disc in an air environment, heating to 180 ℃ for 1h, preserving the heat for 2h, and then N2And heating to 460 ℃ in the atmosphere for 3h, and preserving the heat for 8h to obtain the crosslinked fiber bundle.
S105: placing the crosslinked fiber bundle in a sintering furnace, heating to 1200 ℃ at the speed of 200 ℃/h under the Ar atmosphere with the flow of 200ml/min, and preserving the heat for 2 h; then heating to 1800 ℃ at the speed of 600 ℃/h, and keeping the temperature for 1 h; then cooling to room temperature at the speed of 200 ℃/h to obtain the zirconium-containing silicon carbide fiber.
Comparative example 1
The comparative example is based on example two, and is formed by changing the relevant parameter settings. Specifically, the present comparative example provides a method for preparing zirconium-containing silicon carbide fiber, comprising the steps of:
s1: dissolving polycarbosilane in xylene to obtain a third solution; and adding the nano zirconium oxide dispersion liquid into the third solution, uniformly stirring, heating the uniformly stirred solution to 60 ℃, and stirring at the speed of 400r/min until the solvent is completely volatilized to obtain a powdery product. Wherein the mass ratio of polycarbosilane to xylene is 1:10, the volume ratio of the third solution to the nano zirconia dispersion is 10: 1. the preparation method of the nano zirconia dispersion liquid comprises the following steps: mixing nano zirconia and deionized water according to the weight ratio of 10: 3000, then adding 0.5 wt% of isopropanol as a dispersing agent, adjusting the pH value of the solution to 10 by using NaOH, ultrasonically oscillating for 30min, and then magnetically stirring for 1h to obtain the nano-zirconia dispersion liquid.
S2: the powder product was placed in a melt spinning cylinder at N2Heating to 300 ℃ in the atmosphere for 4h, then pressurizing to 2MPa, and enabling the melt to flow out through a filter screen and a spinneret plate to obtain a fiber bundle; putting the fiber bundle into a silk disc in an air environment, heating to 180 ℃ for 1h, preserving the heat for 2h, and then N2And heating to 460 ℃ in the atmosphere for 3h, and preserving the heat for 8h to obtain the crosslinked fiber bundle.
S3: placing the crosslinked fiber bundle in a sintering furnace, heating to 1200 ℃ at the speed of 200 ℃/h under the Ar atmosphere with the flow of 200ml/min, and preserving the heat for 2 h; then heating to 1800 ℃ at the speed of 600 ℃/h, and keeping the temperature for 1 h; then cooling to room temperature at the speed of 200 ℃/h to obtain the zirconium-containing silicon carbide fiber.
In addition, in order to better highlight the advantages of the technical scheme of the invention, the room temperature strength and the elastic modulus of the zirconium-containing silicon carbide fiber of each example and the comparative example are measured, and in addition, the strength retention rate of each zirconium-containing silicon carbide fiber after 10 hours of working in the environment of 1200 ℃ is measured, and the specific results are shown in table 1.
TABLE 1 tabulated performance of the zirconium-containing silicon carbide fibers of the examples
| Strength at room temperature/GPa | Modulus of elasticity/GPa | Strength retention% | |
| Example one | 3.3 | 218 | 98 |
| Example two | 3.2 | 220 | 95 |
| Comparative example 1 | 2.6 | 198 | 71 |
Of course, other than those exemplified in examples one and two, the weight percentages of other raw material components, the respective conditions and parameters in the production process, and the like are also possible.
The zirconium-containing high-temperature-resistant silicon carbide fiber provided by the invention has the advantages of high strength, stable high-temperature performance and the like, can be used in an environment with the temperature of more than 1200 ℃, and basically keeps the performance unchanged, so that a good application prospect in the high-temperature field is shown.
In the description of the present invention, it is to be understood that the terms "first", "second" and the like are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implying any number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.
Claims (5)
1. The preparation method of the zirconium-containing silicon carbide fiber is characterized by comprising the following steps of:
s101: dissolving yttrium oxide in ethanol, heating and uniformly stirring to obtain a first solution;
s102: mixing the first solution with the nano zirconia dispersion liquid and uniformly stirring to obtain a second solution;
s103: dissolving polycarbosilane in xylene to obtain a third solution; adding the second solution into the third solution, uniformly stirring, and heating the uniformly stirred solution until the solvent is completely volatilized to obtain a powdery product;
s104: carrying out melt spinning and non-melting treatment on the powdery product to obtain a cross-linked fiber bundle;
s105: sintering the cross-linked fiber bundle at high temperature in an inert atmosphere, and then cooling to room temperature to obtain the zirconium-containing silicon carbide fiber;
in the step S101, the mass ratio of the yttrium oxide to the ethanol is 1: (5-10), heating at 40-45 ℃, stirring at a speed of 200-300 r/min, and stirring for 30-40 min;
in S102, the volume ratio of the first solution to the nano zirconia dispersion is 1: (10-20), wherein the stirring speed is 200-300 r/min, and the stirring time is 90-120 min;
in the step S103, the mass ratio of the polycarbosilane to the xylene is 1: (5-10), wherein the volume ratio of the third solution to the second solution is (5-10): 1, stirring at a speed of 300-400 r/min;
in S105, the sintering at high temperature, and then cooling to room temperature specifically includes: heating to 1000-1200 ℃ at the speed of 100-200 ℃/h, and preserving heat for 2-4 h; then heating to 1700-1800 ℃ at the speed of 500-600 ℃/h, and preserving heat for 0.5-1 h; and then cooling to room temperature at a speed of 100-200 ℃/h.
2. The method of preparing zirconium-containing silicon carbide fiber according to claim 1, wherein:
in the step S105, the inert gas is N2And/or Ar, wherein the flow rate of the inert gas is 100-200 m L/min.
3. The zirconium-containing silicon carbide fiber prepared by the method according to any one of claims 1 to 2.
4. Use of the zirconium-containing silicon carbide fiber according to claim 3 in high temperature applications.
5. Use of the zirconium-containing silicon carbide fiber of claim 3 in an environment above 1200 ℃.
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| CN109761610B (en) * | 2019-01-28 | 2021-12-24 | 江西嘉捷信达新材料科技有限公司 | Silicon carbide fiber and preparation method and application thereof |
| CN109809820B (en) * | 2019-01-28 | 2021-11-02 | 江西嘉捷信达新材料科技有限公司 | Zirconium carbide and silicon carbide nano composite fiber reinforced silicon carbide fiber and preparation method thereof |
| CN109811429B (en) * | 2019-01-28 | 2021-07-27 | 江西嘉捷信达新材料科技有限公司 | Silicon carbide fiber containing nano aluminum nitride and metal nickel, and preparation method and application thereof |
| CN109608201A (en) * | 2019-01-28 | 2019-04-12 | 江西嘉捷信达新材料科技有限公司 | Silicon carbide/boron nitride fiber and its preparation method and application |
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| CN106757525A (en) * | 2016-12-12 | 2017-05-31 | 浙江嘉华晶体纤维有限公司 | A kind of production method of crystal fibre |
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