CN111253161A - SiCf-ZrC-ZrB2Ceramic composite powder and preparation method thereof - Google Patents
SiCf-ZrC-ZrB2Ceramic composite powder and preparation method thereof Download PDFInfo
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Abstract
The invention discloses SiCf‑ZrC‑ZrB2Preparing zirconium oxychloride ethanol solution, boric acid ethanol solution, ethyl orthosilicate ethanol solution and glucose water solution respectively, and uniformly mixing the solutions to obtain a zirconium borosilicate precursor solution; drying the target precursor solution, and carrying out heat treatment under the protection of argon atmosphere to obtain the SiC fiber with controllable scale and the uniform and fine ZrC-ZrB2SiC with uniformly dispersed ceramic particlesf‑ZrC‑ZrB2Complex phase ceramic powder. The prepared ceramic powder fiberThe fiber and the ceramic particles are uniformly dispersed, and the length of the fiber can be controllably adjusted between 10um and 100 um; the ceramic particles have fine and uniform particle size and a flat particle size of about 30-50 nm. The method has the advantages of simple and reliable process, safe and nontoxic raw materials, low cost, short preparation period, low formation temperature of the ceramic phase, uniform and fine ceramic particles, uniform distribution of the nanowires and the ceramic particles and controllable nanowire size, and effectively solves the problem of preparing SiC fiber reinforced ZrC-ZrB with different sizes2The preparation of the raw material powder of the ceramic matrix composite and the mixing uniformity problem.
Description
Technical Field
The invention belongs to the technical field of ceramic materials, and particularly relates to SiCf-ZrC-ZrB2Ceramic composite powder and a preparation method thereof.
Background
The ultra-high temperature ceramics mainly comprise high melting point transition metal ceramics, such as boride and carbide ceramics (ZrB)2、ZrC、HfB2And HfC, etc.). ZrB2the-ZrC and other ultrahigh-temperature ceramics have unique excellent performance and wide application prospect in the field of aerospace. In order to improve the inherent brittleness of ceramic materials, the design and preparation of ceramic matrix composites reinforced by second phases such as particles, whiskers, fibers and the like are a necessary trend in the development of ultrahigh temperature ceramics. Wherein, SiC fibers (SiC)fAnd f is the initials of fiber), such as whisker, and nanowires have been widely used in recent years as effective reinforcing and toughening materials.
At present, the fiber reinforced ceramic matrix composite is basically limited to be prepared by a high-temperature sintering method by using external fiber mixed raw material powder, and the method still has the following problems which are difficult to overcome: the fiber and ceramic raw material powder is difficult to be uniformly mixed, so that the material performance shows non-uniformity; the treatment process of the raw material powder can cause harm to human health, for example, the inhalation of the fiber can cause health problems such as cancer and the like; the process is complex and the production cost is high. In addition, the uniformity of the dispersion of the fibers and the ceramic matrix, the particle size and distribution uniformity of the ceramic particles, and the size (such as length, diameter, thickness, etc.) of the fibers directly influence the microstructure uniformity, sintering property, and mechanical properties of the prepared fiber-reinforced ceramic matrix composite.
Patent "a SiCw-ZrB2-ZrC ceramic composite powder and preparation method thereof (application number: 201710157781.9) provide SiCw-ZrB2The preparation method of the-ZrC ceramic composite powder comprises the steps of synthesizing ceramic precursor polymer containing boron, silicon and zirconium; then drying, ball-milling and high-temperature cracking the precursor polymer to obtain SiC whiskers which are uniformly dispersed in ZrB2-ZrC ceramic matrix is grown around or uniformly on ZrB2-a ZrC ceramic matrix surface. The method well solves the problems of introduction and dispersion uniformity of the crystal whisker, but still has the problems of high raw material toxicity, complex preparation process and high production cost. In addition, the particle size of the ceramic particles, the dispersion uniformity of the ceramic phase, and the control of the size of the fibers are still in need of further improvement.
Disclosure of Invention
In order to overcome the disadvantages of the prior art, the invention aims to provide SiCf-ZrC-ZrB2Ceramic composite powder and preparation method thereof, aiming at solving the problem of ZrC-ZrB2Solves the problems of the introduction and the dispersion uniformity of SiC fibers in the complex phase ceramic powder, simultaneously solves the problems of the refinement and the dispersion uniformity of ceramic phase particles, the size control of SiC fibers and the complex and high cost of the existing preparation method, has the characteristics of simple and easily obtained raw materials, safety, no toxicity, simple and easily controlled process and low pyrolysis temperature, has controllable SiC crystal whisker size, and ZrC-ZrB2The ceramic particles are uniform, fine and dispersed uniformly.
In order to achieve the purpose, the invention adopts the technical scheme that:
zirconium oxychloride octahydrate, boric acid, tetraethoxysilane and glucose are taken as initial raw materials, polyethylene glycol 600 is taken as a dispersing agent, absolute ethyl alcohol and deionized water are taken as solvents, and the method specifically comprises the following steps:
dissolving zirconium oxychloride in absolute ethyl alcohol, and uniformly stirring to obtain a zirconium precursor solution;
step (2), dissolving ethyl orthosilicate in absolute ethyl alcohol, and uniformly stirring to obtain a silicon precursor solution;
step (3), adding the silicon precursor solution into a zirconium precursor solution under continuous magnetic stirring, dropwise adding a dispersant polyethylene glycol 600, and uniformly stirring to obtain a silicon-zirconium precursor solution;
step (4), adding an ethanol solution of boric acid and an aqueous solution of glucose into the zirconium-silicon precursor solution, and uniformly stirring to obtain a zirconium-boron-silicon precursor solution, namely a target precursor solution;
and (5) drying the target precursor solution, and carrying out pyrolysis under the protection of argon to obtain SiC fibers (SiC)f) Scale controllable ZrC-ZrB2-SiC complex phase ceramic powder.
Wherein the molar concentration of the zirconium precursor solution is 0.5-1.5mol/L, the molar concentration of the boric acid ethanol solution is 0.5-3mol/L, the molar concentration of the glucose aqueous solution is 1.5-9mol/L, the molar ratio of zirconium oxychloride to tetraethoxysilane is 1:1-1:6, the molar ratio of zirconium oxychloride to boric acid is 1:1-1:4, the molar ratio of zirconium oxychloride to glucose is 1:3-1:5, the volume ratio of tetraethoxysilane to absolute ethyl alcohol in the silicon precursor solution is 1:1-1:4, and the volume ratio of polyethylene glycol 600 to absolute ethyl alcohol in the silicon precursor solution is 0.0025:1-0.005: 1.
The drying temperature is 60-80 ℃, and the drying time is 12-36 h.
The high-temperature cracking temperature is 1400-1600 ℃, and the heat preservation time is 1-4 h.
The invention also claims SiC prepared by the preparation methodf-ZrC-ZrB2Ceramic composite powder.
Compared with the prior art, the invention uses a low-cost, safe and nontoxic soluble zirconium source, a silicon source and a carbon source as raw materials, adopts a liquid phase method to perform hybrid crosslinking on ceramic elements at a molecular level to obtain a precursor with uniformly distributed ceramic elements, can obtain ternary complex phase ceramic powder with uniformly distributed ceramic phases by heat treatment at a lower temperature, and adjusts the gas phase saturation, the diffusion rate of gas molecules and the growth rate of fibers by utilizing the synergistic action among temperature, heat preservation time and the relative content of ceramic components to obtain the SiC fibers with controllable morphology and scale; specifically, in the temperature range (1400 ℃ C. and 1600 ℃ C.) in which the ternary ceramic phase can be generated, under the condition of certain ceramic components, the heat treatment temperature is reduced, the heat preservation time is prolonged, and the axial growth of SiC fibers is facilitated, so that the SiC long fibers are obtained; on the premise of certain heat treatment temperature and heat preservation time, the SiC content in the ceramic component is improved, so that the improvement of gas phase saturation is facilitated, and the formation of SiC long fibers is promoted; under the condition of certain ceramic components and heat preservation time, the diffusion rate of gas molecules is improved and the gas phase saturation is improved by increasing the heat treatment temperature, so that the SiC short fiber is obtained.
The method has the advantages of simple and reliable process, safe and nontoxic raw materials, low cost, short preparation period, low formation temperature of the ceramic phase, uniform and fine ceramic particles, uniform distribution of the nanowires and the ceramic particles and controllable nanowire size, and effectively solves the problem of preparing SiC fiber reinforced ZrC-ZrB with different sizes2The preparation of the raw material powder of the ceramic matrix composite and the mixing uniformity problem.
Drawings
FIG. 1 shows SiC produced in example 1 of the present inventionf-ZrC-ZrB2XRD spectrogram of the ceramic composite powder.
FIG. 2 shows SiC produced in example 1 of the present inventionf-ZrC-ZrB2SEM photograph of the ceramic composite powder.
FIG. 3 shows SiC produced in example 2 of the present inventionf-ZrC-ZrB2XRD spectrogram of the ceramic composite powder.
FIG. 4 shows SiC produced in example 2 of the present inventionf-ZrC-ZrB2SEM photograph of the ceramic composite powder.
FIG. 5 shows SiC produced in example 3 of the present inventionf-ZrC-ZrB2XRD spectrogram of the ceramic composite powder.
FIG. 6 shows SiC produced in example 3 of the present inventionf-ZrC-ZrB2SEM photograph of the ceramic composite powder.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the embodiments of the present invention are not limited thereto.
Example 1:
(1) preparation of zirconium precursor solution: weighing 3.2g of zirconium oxychloride according to the molar weight of 0.01mol for later use, dissolving the zirconium oxychloride in 20mL of absolute ethanol, and uniformly stirring to obtain a zirconium precursor solution;
(2) preparation of a silicon precursor solution: weighing 10.4g of tetraethoxysilane according to the molar ratio of zirconium oxychloride to tetraethoxysilane of 1:5, dissolving the tetraethoxysilane in 15mL of absolute ethyl alcohol, and uniformly stirring to obtain a silicon precursor solution; wherein the volume ratio of the ethyl orthosilicate to the absolute ethyl alcohol is 1: 4;
(3) preparing a silicon-zirconium precursor solution: dropwise adding the silicon precursor solution prepared in the step 2 into the zirconium precursor solution under continuous magnetic stirring, dropwise adding 0.05mL of polyethylene glycol, and uniformly stirring to obtain a silicon-zirconium precursor solution;
(4) preparing a zirconium borosilicate precursor solution: 2.5g of boric acid and 9g of glucose are weighed according to the molar ratio of zirconium to boron being 1:4 and the molar ratio of zirconium to carbon being 1:5, respectively dissolved in 30mL of absolute ethanol and 10mL of deionized water, and are dropwise added into the silicon-zirconium precursor solution obtained in the step 3, and the target precursor solution is obtained after uniform stirring.
(5)SiCf-ZrC-ZrB2Preparing composite powder: placing the target precursor solution obtained in the step (4) in a forced air drying oven, and keeping the temperature at 80 ℃ for 12h for drying; then placing the mixture in a graphite crucible, and keeping the temperature of 1600 ℃ for 2h under the argon atmosphere to obtain SiCf-ZrC-ZrB2Ceramic composite powder.
As can be seen from FIG. 1, the phase composition of the composite ceramic powder prepared in this example is pure ZrC and ZrB2And SiC, the crystallization degree is high, and other impurity phases are not found.
As can be seen from FIG. 2, the composite ceramic powder prepared in this example has uniformly dispersed whiskers, a uniform size of about 10 μm, a uniform and fine ceramic phase, and a uniform particle size of about 50 nm.
Example 2:
(1) preparation of zirconium precursor solution: weighing 6.4g of zirconium oxychloride according to the molar weight of 0.02mol for later use, dissolving the zirconium oxychloride in 30mL of absolute ethanol, and uniformly stirring to obtain a zirconium precursor solution;
(2) preparation of a silicon precursor solution: weighing 16.6g of tetraethoxysilane according to the molar ratio of zirconium oxychloride to tetraethoxysilane of 1:4, dissolving the tetraethoxysilane in 15mL of absolute ethyl alcohol, and uniformly stirring to obtain a silicon precursor solution;
(3) preparing a silicon-zirconium precursor solution: dropwise adding the silicon precursor solution prepared in the step 2 into the zirconium precursor solution under continuous magnetic stirring, dropwise adding 0.05mL of polyethylene glycol, and uniformly stirring to obtain a silicon-zirconium precursor solution;
(4) preparing a zirconium borosilicate precursor solution: weighing 2.5g of boric acid and 14.4g of glucose according to the molar ratio of zirconium to boron being 1:2 and the molar ratio of zirconium to carbon being 1:4, respectively dissolving the boric acid and the glucose in 20mL of absolute ethyl alcohol and 10mL of deionized water, dropwise adding the solution into the silicon-zirconium precursor solution obtained in the step 3, and uniformly stirring the solution to obtain a target precursor solution;
(5)SiCf-ZrC-ZrB2preparing composite powder: placing the target precursor solution obtained in the step (4) in a forced air drying oven, and keeping the temperature at 60 ℃ for 36h for drying; then placing the mixture in a graphite crucible, and preserving heat for 1.5 hours at 1500 ℃ under the argon atmosphere to obtain SiCf-ZrC-ZrB2Ceramic composite powder.
As can be seen from FIG. 3, the phase composition of the composite ceramic powder prepared in this example is pure ZrC and ZrB2And SiC, the crystallization degree is high, and other impurity phases are not found.
As can be seen from FIG. 4, the composite ceramic powder prepared in this example has uniformly dispersed whiskers, uniform size of about 60 μm, uniform and fine ceramic phase, uniform particle size, and average particle size of about 40 nm.
Example 3:
(1) preparation of zirconium precursor solution: weighing 3.2g of zirconium oxychloride according to the molar weight of 0.01mol for later use, dissolving the zirconium oxychloride in 20mL of absolute ethanol, and uniformly stirring to obtain a zirconium precursor solution;
(2) preparation of a silicon precursor solution: weighing 8.32g of tetraethoxysilane according to the molar ratio of zirconium oxychloride to tetraethoxysilane of 1:4, dissolving the tetraethoxysilane in 10mL of absolute ethyl alcohol, and uniformly stirring to obtain a silicon precursor solution; wherein the volume ratio of the ethyl orthosilicate to the absolute ethyl alcohol is 1: 3;
(3) preparing a silicon-zirconium precursor solution: dropwise adding the silicon precursor solution prepared in the step 2 into the zirconium precursor solution under continuous magnetic stirring, dropwise adding 0.05mL of polyethylene glycol, and uniformly stirring to obtain a silicon-zirconium precursor solution;
(4) preparing a zirconium borosilicate precursor solution: weighing l.8g of boric acid and 7.2g of glucose according to the molar ratio of zirconium to boron of 1:3 and the molar ratio of zirconium to carbon of 1:4, respectively dissolving the boric acid and the glucose in 30mL of absolute ethanol and 15mL of deionized water, dropwise adding the solution into the silicon-zirconium precursor solution obtained in the step (3), and uniformly stirring to obtain the target precursor solution.
(5)SiCf-ZrC-ZrB2Preparing composite powder: placing the target precursor solution obtained in the step (4) in a forced air drying oven, and keeping the temperature at 70 ℃ for 24h for drying; then placing the mixture in a graphite crucible, and preserving heat for 2 hours at 1500 ℃ under the argon atmosphere to obtain SiCf-ZrC-ZrB2Ceramic composite powder.
As can be seen from FIG. 5, the phase composition of the composite ceramic powder prepared in this example is pure ZrC and ZrB2And SiC, the crystallization degree is high, and other impurity phases are not found.
As can be seen from fig. 6, the composite ceramic powder prepared in this example has uniformly dispersed whiskers, a uniform size of about 100um, a uniform and fine ceramic phase, and a uniform particle size of about 30 nm.
In conclusion, the ceramic powder fiber prepared by the invention is uniformly dispersed with the ceramic particles, and the length of the fiber is within the range of 10-100 um; the ceramic particles have fine and uniform particle size and a flat particle size of about 30-50 nm.
Claims (5)
1. SiCf-ZrC-ZrB2The preparation method of the ceramic composite powder is characterized by comprising the following steps:
dissolving zirconium oxychloride in absolute ethyl alcohol, and uniformly stirring to obtain a zirconium precursor solution;
step (2), dissolving ethyl orthosilicate in absolute ethyl alcohol, and uniformly stirring to obtain a silicon precursor solution;
step (3), adding the silicon precursor solution into a zirconium precursor solution under continuous magnetic stirring, dropwise adding a dispersant polyethylene glycol 600, and uniformly stirring to obtain a silicon-zirconium precursor solution;
step (4), adding an ethanol solution of boric acid and an aqueous solution of glucose into the zirconium-silicon precursor solution, and uniformly stirring to obtain a zirconium-boron-silicon precursor solution, namely a target precursor solution;
and (5) drying the target precursor solution, and carrying out pyrolysis under the protection of argon to obtain SiCf-ZrC-ZrB2-ceramic composite powder.
2. SiC according to claim 1f-ZrC-ZrB2The preparation method of the ceramic composite powder is characterized in that the molar concentration of the zirconium precursor solution is 0.5-1.5mol/L, the molar concentration of the boric acid ethanol solution is 0.5-3mol/L, the molar concentration of the glucose aqueous solution is 1.5-9mol/L, the molar ratio of zirconium oxychloride to tetraethoxysilane is 1:1-1:6, the molar ratio of zirconium oxychloride to boric acid is 1:1-1:4, the molar ratio of zirconium oxychloride to glucose is 1:3-1:5, the volume ratio of tetraethoxysilane to absolute ethyl alcohol in the silicon precursor solution is 1:1-1:4, and the volume ratio of polyethylene glycol 600 to absolute ethyl alcohol in the silicon precursor solution is 0.0025:1-0.005: 1.
3. SiC according to claim 1f-ZrC-ZrB2The preparation method of the ceramic composite powder is characterized in that the drying temperature is 60-80 ℃, and the drying time is 12-36 h.
4. SiC according to claim 1f-ZrC-ZrB2The preparation method of the ceramic composite powder is characterized in that the high-temperature cracking temperature is 1400-1600 ℃, and the heat preservation time is 1-4 h.
5. SiC produced by the production method according to any one of claims 1 to 4f-ZrC-ZrB2Ceramic composite powder.
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Cited By (2)
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| CN113735593A (en) * | 2021-09-30 | 2021-12-03 | 陕西科技大学 | Microstructure-adjustable SiCnws-ZrB2-ZrC hybrid ceramic powder and preparation method thereof |
| CN113800935A (en) * | 2021-09-27 | 2021-12-17 | 陕西科技大学 | Preparation method of in-situ synthesized SiC (nw, np) -ZrB2-ZrC modified carbon/carbon composite material |
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