CN113735593B - SiC with adjustable microstructure nws -ZrB 2 -ZrC hybrid ceramic powder and preparation method thereof - Google Patents
SiC with adjustable microstructure nws -ZrB 2 -ZrC hybrid ceramic powder and preparation method thereof Download PDFInfo
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Abstract
The invention relates to SiC with adjustable microstructure nws ‑ZrB 2 The preparation method of the-ZrC hybrid ceramic powder combines a sol-gel method and a template method, carbon fiber powder is uniformly dispersed into borosilicate zirconium sol to obtain composite sol, and SiC nanowires with different microscopic morphologies and ZrC-ZrB are obtained by controlling a high-temperature heat treatment process 2 A hybrid powder. The prepared hybrid powder has the advantages that the SiC nanowires and the ceramic particles are uniformly dispersed, the ceramic particles are fine and uniform, the average particle size is about 100nm or the particle size is distributed between 50-150nm, the microscopic morphology of the SiC nanowires is linear, chain, hexagonal prism or bamboo joint, the diameter is between 100 and 500nm, the length is between 10 and 100 mu m, and therefore ZrC-ZrB is solved 2 The introduction of the SiC nano-wire in the complex phase ceramic powder and the dispersion uniformity problem simultaneously realize the microstructure regulation of the SiC nano-wire.
Description
Technical Field
The invention belongs to the technical field of ceramic materials, and particularly relates to SiC with adjustable microstructure nws -ZrB 2 -ZrC hybrid ceramic powder and a preparation method thereof.
Background
ZrB 2 the-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. Among them, SiC nanowires are widely used for reinforcement and toughening of ceramic materials due to their excellent mechanical properties. Research has shown that SiC fibers with special microstructures, such as bamboo-shaped, chain-shaped and needle-shaped SiC fibers, are used as reinforcement of ceramic materials, compared with SiC fibers with common shapes f (nanopillar) has more excellent reinforcing effect.
The traditional preparation method of the raw material powder of the fiber reinforced ceramic matrix composite material is mainly characterized in that the fiber mixed ceramic powder is added and the mechanical mixing mode is adopted for preparation. The method has the advantages that the dispersion uniformity of the fibers is difficult to solve, the mixing process of the raw material powder can cause harm to the health of a human body, the process is complex, and the production cost is high. The hybrid powder with the uniformly dispersed fibers and ceramic particles is obtained through the in-situ growth of the fibers, and the method becomes an effective way for solving the problem.
Patent "a SiCw-ZrB 2 -ZrC ceramic composite powder and preparation method thereof (application number: 201710157781.9) provide SiCw-ZrB 2 The preparation method of the-ZrC ceramic composite powder comprises the steps of synthesizing an organic high molecular polymer containing boron, silicon and zirconium, and combining a high-temperature cracking process to obtain the SiC whiskers which are uniformly dispersed in ZrB 2 -ZrC ceramic matrix is grown around or uniformly on ZrB 2 -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, high production cost and nonadjustable morphology and scale of the SiC crystal whisker. Patent "a kind of SiC f -ZrB 2 the-ZrC ceramic composite powder and the preparation method thereof (application number: 202010065527.8) adopt an organic template agent to successfully prepare SiC with uniformly dispersed nano-columnar SiC fibers and adjustable length between 10 mu m and 100 mu m by regulating and controlling the preparation process f -ZrB 2 -ZrC ceramic composite powder. And for how to control the microstructure of the SiC nanowire, SiC with adjustable SiC nanowire microstructure is obtained nws -ZrB 2 -ZrC hybrid ceramic powders have not yet formed a feasible manufacturing strategy.
Disclosure of Invention
In order to overcome the disadvantages of the prior art, the invention aims to provide SiC with adjustable microstructure nws -ZrB 2 The preparation method of the-ZrC hybrid ceramic powder combines a sol-gel method and a template method, and SiC nanowires (SiC) with different microscopic morphologies are obtained by synchronous in-situ growth nws ) And ZrC-ZrB 2 Hybrid powder for solving ZrC-ZrB 2 The microstructure of the SiC nanowire is regulated and controlled while the problems of the introduction and the dispersion uniformity of the SiC nanowire in the complex phase ceramic powder are solved.
In order to achieve the purpose, the invention adopts the technical scheme that:
microstructure-adjustable SiC nws -ZrB 2 The preparation method of the-ZrC hybrid ceramic powder comprises the following steps:
preparing boron-silicon-zirconium precursor sol by using zirconium oxychloride, boric acid, tetraethoxysilane and glucose as raw materials, ethanol or deionized water as a solvent and polyethylene glycol as a dispersing agent;
step (2), dispersing carbon fiber powder into the borosilicate zirconium precursor sol, and continuously stirring to obtain a composite sol in which the carbon fiber powder is uniformly dispersed;
step (3), drying the composite sol at 50-90 ℃, and then grinding to obtain dry gel powder;
step (4), placing the dry gel powder in a graphite crucible, and carrying out 1400-1600 ℃ heat treatment under the protection of argon atmosphere to obtain SiC nws -ZrC-ZrB 2 Ceramic composite powder.
In the step (1), zirconium oxychloride ethanol solution with the concentration of 0.1-0.3g/mL, tetraethoxysilane ethanol solution with the concentration of 0.05-2g/mL, glucose aqueous solution with the concentration of 0.2-0.4g/mL and boric acid ethanol solution with the concentration of 0.5-0.1g/mL are respectively prepared, the solutions are respectively measured according to the volume ratio of 1:2.5:1:1 and are uniformly mixed, then, dispersant polyethylene glycol 600 is added according to the volume fraction of 0.5-1.5%, and the borosilicate zirconium precursor sol is obtained by continuously stirring.
The particle size of the carbon fiber powder is 500-1000 meshes, and the length-diameter ratio is 2: 1-10: 1.
In the step (2), carbon fiber powder is added into the boron-silicon-zirconium precursor sol according to the mass fraction of 0.05-1 wt%.
And (3) in the step (2), stirring for 2-5h to obtain the composite sol.
In the step (3), the drying is carried out for 24-48h at 50-90 ℃, and in the step (3), the heat treatment is carried out for 1-4h at 1400-1600 ℃.
When the concentration of ethyl orthosilicate ethanol solution is 0.2-1.5g/mL, the SiC containing bamboo-shaped silicon carbide nano-wires is obtained by heat treatment for 2-3h at 1500 DEG C nws -ZrC-ZrB 2 Hybrid ceramic powder; when the concentration of the ethyl orthosilicate ethanol solution is 0.5-2g/cm 3 Keeping the temperature at 1500 ℃ for 3-4h to obtain SiC containing hexagonal prism-shaped SiC nanowires nws -ZrC-ZrB 2 Hybrid ceramic powder; when the concentration of the ethyl orthosilicate ethanol solution is 1-2g/cm 3 Heat treatment at 1600 deg.c for 2-3 hr to obtain SiC containing chain SiC nano wire nws -ZrC-ZrB 2 Hybrid ceramic powder; when the concentration of the ethyl orthosilicate ethanol solution is 1.5-2g/cm 3 Heat treatment at 1500 deg.c for 1-2 hr to obtain SiC containing linear SiC nanometer wire nws -ZrC-ZrB 2 A hybrid ceramic powder.
The invention also claims the SiC obtained by the preparation nws -ZrB 2 -ZrC hybrid ceramic powder, SiC nws The ceramic particles are uniformly dispersed, the ceramic particles are fine and uniform, and the average particle size is about 100 nm; or the grain diameter is distributed between 50nm and 150nm, SiC nws The micro-morphology of the material is linear, chain, hexagonal prism or bamboo joint, the diameter is between 100 and 500nm, and the length is between 10 and 100 mu m.
Compared with the prior art, the invention uses the low-cost, safe and nontoxic soluble zirconium source, silicon source and 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, further disperses carbon fiber powder into the prepared sol, and utilizes the high viscosity of the sol to enable the carbon fiber powder to be uniformly suspended, thereby solving the problem of dispersion uniformity of the carbon fiber powder; pyrolysis product SiO of silicon source in heat treatment process 2 The carbon fiber powder is used as a nucleating agent to generate a randomly oriented SiC crystal nucleus so as to solve the problem of dispersion uniformity of the nanowires; on one hand, the carbon fiber powder is used as a template agent, the one-dimensional structure of the carbon fiber plays a certain space confinement effect on the growth of the nanowire, and the formed SiC crystal nucleus continuously grows along the direction of the carbon fiber to obtain the one-dimensional silicon carbide nanowire; in addition, at a higher temperature, zirconium oxide in the precursor reacts with a carbon source/boron source to generate CO gas while zirconium carbide/zirconium boride is generated, so that the gas phase saturation required by the growth of the SiC nanowire is regulated and obtained to obtain different shapesThe appearance of the SiC nanowire is improved, thereby effectively solving the problem of preparing SiC nanowire reinforced ZrC-ZrB with different microstructures 2 The 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 invention nws -ZrC-ZrB 2 XRD spectrogram of the ceramic composite powder.
FIG. 2 shows SiC produced in example 1 of the present invention nws -ZrB 2 SEM image of ceramic particles in ZrC hybrid ceramic powder.
FIG. 3 shows SiC produced in example 1 of the present invention nws -ZrB 2 SEM photograph of SiC nanowires in ZrC hybrid ceramic powder.
FIG. 4 shows SiC produced in example 2 of the present invention nws -ZrB 2 SEM photograph of SiC nanowires in ZrC hybrid ceramic powder.
FIG. 5 shows SiC produced in example 3 of the present invention nws -ZrB 2 SEM photograph of SiC nanowires in ZrC hybrid ceramic powder.
FIG. 6 shows SiC produced in example 4 of the present invention nws -ZrB 2 SEM photograph of SiC nanowires in ZrC hybrid ceramic 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.
The invention relates to SiC with adjustable microstructure nws -ZrB 2 The preparation method of the-ZrC hybrid ceramic powder combines a sol-gel method and a template method, carbon fiber powder is uniformly dispersed into borosilicate zirconium sol to obtain composite sol, and SiC nanowires with different microscopic morphologies and ZrC-ZrB are obtained by controlling a high-temperature heat treatment process 2 A hybrid powder. The prepared hybrid powder has the advantages that the SiC nanowires and the ceramic particles are uniformly dispersed, the ceramic particles are fine and uniform, the average particle size is about 100nm or the particle size is distributed between 50-150nm, the microscopic morphology of the SiC nanowires is linear, chain, hexagonal prism or bamboo joint, the diameter is between 100 and 500nm, the length is between 10 and 100 mu m, and therefore ZrC-ZrB is solved 2 The introduction of the SiC nano-wire in the complex phase ceramic powder and the dispersion uniformity problem simultaneously realize the microstructure regulation of the SiC nano-wire.
The following are several embodiments of the invention.
Example 1:
SiC nws -ZrC-ZrB 2 The preparation method of the hybrid ceramic powder comprises the following specific processes:
(1) preparing a zirconium oxychloride ethanol solution with the concentration of 0.15g/mL, an ethyl orthosilicate ethanol solution with the concentration of 0.2g/mL, a glucose aqueous solution with the concentration of 0.3g/mL and a boric acid ethanol solution with the concentration of 0.5g/mL, uniformly mixing the solutions, adding polyethylene glycol 600 with the volume fraction of 0.5%, and continuously stirring for 3 hours to obtain a boron-silicon-zirconium precursor sol;
(2) weighing carbon fiber powder according to 0.05 percent of the mass of the sol, dispersing the carbon fiber powder into the sol prepared in the step 1, and continuously stirring for 2 hours to obtain composite sol in which the carbon fiber powder is uniformly dispersed;
(3) drying the composite sol obtained in the step 2 at 70 ℃ for 48h, and grinding the obtained xerogel for subsequent heat treatment;
(4) carrying out heat treatment on the dry gel powder obtained in the step 3 at 1500 ℃ for 2h under the protection of atmosphere to obtain SiC containing bamboo-shaped silicon carbide nano-wires shown in the attached figure 2 nws -ZrC-ZrB 2 A hybrid ceramic powder. The XRD pattern of the obtained hybrid ceramic powder is shown in figure 1, and the SEM pattern of the ceramic particles is shown in figure 2.
As can be seen from FIG. 1, SiC produced in this example 1 nws -ZrC-ZrB 2 The phase composition of the hybrid ceramic powder is ZrC and ZrB 2 And SiC, the crystallinity is higher, and other impurity phases are not found.
As can be seen from FIG. 2, SiC produced in this example nws -ZrC-ZrB 2 In the hybrid ceramic powder, ceramic particles are uniform and fine, and the average particle size is about 100 nm.
As can be seen from FIG. 3, SiC produced in this example nws -ZrC-ZrB 2 In the hybrid ceramic powder, the SiC nanowires and the ceramic particles are uniformly dispersed, and the appearance of the SiC nanowires isBamboo-like, the diameter is about 100nm, and the length is about 100 um.
Example 2:
SiC nws -ZrC-ZrB 2 The preparation method of the hybrid ceramic powder is the same as that of example 1 except that the following raw material concentrations and heat treatment processes are different.
In this embodiment: in the preparation process of the zirconium borosilicate precursor sol, the concentration of the prepared ethyl orthosilicate ethanol solution is 1g/cm 3 ；
The precursor xerogel is obtained for standby according to the steps in the embodiment 1, the heat treatment temperature is 1500 ℃, and the SiC of the hexagonal prism-shaped SiC nanowire shown in the attached figure 4 is obtained after the heat treatment is carried out for 4 hours nws -ZrC-ZrB 2 The hybrid ceramic powder has the diameter of about 200nm and the length of about 200 um.
Example 3:
SiC nws -ZrC-ZrB 2 The preparation method of the hybrid ceramic powder is the same as that of example 1 except that the following raw material concentrations and heat treatment processes are different.
In this embodiment: in the preparation process of the zirconium borosilicate precursor sol, the concentration of the prepared ethyl orthosilicate ethanol solution is 1.5g/cm 3 ；
The precursor xerogel is obtained for standby according to the steps in the embodiment 1, and the heat treatment temperature is 1600 ℃ for 2h, thus obtaining the SiC of the chain SiC nanowire shown in the attached figure 5 nws -ZrC-ZrB 2 The hybrid ceramic powder has the diameter of about 500nm and the length of about 100 um.
Example 4:
SiC nws -ZrC-ZrB 2 The preparation method of the hybrid ceramic powder is the same as that of example 1 except that the following raw material concentrations and heat treatment processes are different.
In this embodiment: in the preparation process of the zirconium borosilicate precursor sol, the concentration of the prepared ethyl orthosilicate ethanol solution is 2g/cm 3 ；
The precursor xerogel is obtained for standby according to the steps in the embodiment 1, the heat treatment temperature is 1500 ℃, and the SiC of the linear SiC nanowire shown in the attached figure 6 is obtained after the heat treatment is carried out for 2 hours nws -ZrC-ZrB 2 Hybrid ceramic powder about 20 mm in diameter0nm and a length of about 100 um.
Claims (7)
1. SiC with adjustable microstructure nws -ZrB 2 The preparation method of the-ZrC hybrid ceramic powder is characterized by comprising the following steps:
preparing boron-silicon-zirconium precursor sol by using zirconium oxychloride, boric acid, tetraethoxysilane and glucose as raw materials, ethanol or deionized water as a solvent and polyethylene glycol as a dispersing agent;
step (2), adding carbon fiber powder into the boron-silicon-zirconium precursor sol according to the mass fraction of 0.05-1 wt%, and continuously stirring to obtain composite sol in which the carbon fiber powder is uniformly dispersed, wherein the particle size of the carbon fiber powder is 500-1000 meshes, and the length-diameter ratio is 2: 1-10: 1;
step (3), drying the composite sol at 50-90 ℃, and then grinding to obtain dry gel powder;
step (4), placing the dry gel powder in a graphite crucible, and carrying out 1400-1600 ℃ heat treatment under the protection of argon atmosphere to obtain SiC nws -ZrC-ZrB 2 Ceramic composite powder; wherein when the concentration of ethyl orthosilicate ethanol solution is 0.2-1.5g/mL, SiC containing bamboo-shaped silicon carbide nano-wires is obtained by heat treatment for 2-3h at 1500 DEG C nws -ZrC-ZrB 2 Hybrid ceramic powder; when the concentration of the ethyl orthosilicate ethanol solution is 0.5-2g/cm 3 Keeping the temperature at 1500 ℃ for 3-4h to obtain SiC containing hexagonal prism-shaped SiC nanowires nws -ZrC-ZrB 2 Hybrid ceramic powder; when the concentration of the ethyl orthosilicate ethanol solution is 1-2g/cm 3 Heat treatment at 1600 deg.c for 2-3 hr to obtain SiC containing chain SiC nano wire nws -ZrC-ZrB 2 Hybridizing ceramic powder; when the concentration of the ethyl orthosilicate ethanol solution is 1.5-2g/cm 3 Heat treatment at 1500 deg.c for 1-2 hr to obtain SiC containing linear SiC nanometer wire nws -ZrC-ZrB 2 And (3) hybrid ceramic powder.
2. The microstructure tunable SiC of claim 1 nws -ZrB 2 The preparation method of the-ZrC hybrid ceramic powder is characterized in that in the step (1), the concentrations are respectively preparedRespectively measuring the solution according to the volume ratio of 1:2.5:1:1, uniformly mixing, adding a dispersant polyethylene glycol 600 according to the volume fraction of 0.5% -1.5%, and continuously stirring to obtain the zirconium borosilicate precursor sol.
3. Microstructure tunable SiC according to claim 1 nws -ZrB 2 The preparation method of the-ZrC hybrid ceramic powder is characterized in that in the step (2), the composite sol is obtained after stirring for 2-5 hours.
4. Microstructure tunable SiC according to claim 1 nws -ZrB 2 The preparation method of the-ZrC hybrid ceramic powder is characterized in that in the step (3), the powder is dried for 24-48h at 50-90 ℃, and in the step (4), the powder is subjected to heat treatment for 1-4h at 1400-1600 ℃.
5. The microstructure tunable SiC of claim 1 nws -ZrB 2 SiC prepared by preparation method of-ZrC hybrid ceramic powder nws -ZrB 2 -ZrC hybrid ceramic powder.
6. SiC according to claim 5 nws -ZrB 2 -ZrC hybrid ceramic powder characterized in that SiC nws The ceramic particles are uniformly dispersed, the ceramic particles are fine and uniform, and the average particle size is 100 nm; or the particle size distribution is between 50-150 nm.
7. SiC according to claim 6 nws -ZrB 2 -ZrC hybrid ceramic powder characterized in that said SiC nws The micro-morphology of the material is linear, chain, hexagonal prism or bamboo joint, the diameter is between 100 and 500nm, and the length is between 10 and 100 mu m.
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| CN103693984B (en) * | 2011-12-29 | 2015-08-26 | 中国科学院过程工程研究所 | Fibre reinforced complex phase ceramic base friction braking material and preparation method thereof |
| CN103332944B (en) * | 2013-06-08 | 2015-01-21 | 山东工业陶瓷研究设计院有限公司 | Preparation method of Cf-ZrB2/ZrC/SiC composite material |
| CN105237020B (en) * | 2015-08-31 | 2018-08-24 | 中国人民解放军国防科学技术大学 | A kind of fibre reinforced ZrB2- ZrN multiphase ceramic matrix composites and preparation method thereof |
| CN110872198B (en) * | 2018-08-31 | 2022-02-15 | 航天特种材料及工艺技术研究所 | Nanowire toughened ZrB2Preparation method of-ZrC-SiC oxidation resistant coating |
| CN111253161A (en) * | 2020-01-20 | 2020-06-09 | 陕西科技大学 | SiCf-ZrC-ZrB2Ceramic composite powder and preparation method thereof |
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