CN113277850A - Preparation method of ZrC-TiC composite nano-particle material - Google Patents
Preparation method of ZrC-TiC composite nano-particle material Download PDFInfo
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- C04B35/5622—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on refractory metal carbides based on zirconium or hafnium carbides
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Abstract
The invention discloses a preparation method of a ZrC-TiC composite nano-particle material, which comprises the following steps: step 1, ZrOCl2·8H2Mixing O with water, stirring to obtain a colorless transparent solution A, adding glucose and TBT solution into the colorless transparent solution A, and stirring to obtain a colorless transparent solution B; step 2, mixing tartaric acid with water, and stirring to obtain a colorless transparent solution C; step 3, adding the colorless transparent solution C into the colorless transparent solution B, and stirring to obtain a colorless transparent solution D; step 4, carrying out rotary evaporation on the colorless transparent solution D, stopping the rotary evaporation when the rest 1/3 liquid is in a wall hanging state, and placing the rest liquid in an oven for drying to obtain a ZrC/TiC organic composite precursor; and 5, sintering and cooling the ZrC/TiC organic composite precursor to obtain ZrC/TiC nano particles. The invention solves the problems of pollution and toxicity of products in the production process.
Description
Technical Field
The invention belongs to the technical field of high-temperature ceramic materials, and relates to a preparation method of a ZrC-TiC composite nano-particle material.
Background
The zirconium carbide/titanium carbide (ZrC/TiC) composite ceramic has high melting point, high thermal conductivity, high electrical conductivity, high specific strength, high specific modulus, high hardness, high wear resistance and good chemical stability, so that the zirconium carbide/titanium carbide (ZrC/TiC) composite ceramic has wide application in the field of ultrahigh-temperature structural materials: ultra-high temperature heat insulation coating, high temperature fire-resistant and wear-resistant materials and the like. The preferred method for preparing the precursor is an organic synthesis method, but the method has the defects of high raw material cost, complex preparation process, overlarge toxicity of the precursor, difficult storage of the product and the like. Therefore, the ZrC/TiC ceramic precursor which has the advantages of simple research and preparation process, no pollution in the production process, no toxicity and harm in the product and low cost has very important strategic significance and urgent practical value.
At present, Chinese patent CN104671815A discloses a ZrC-TiC modified C/C-SiC composite material and a preparation method thereof; the method mainly comprises the steps of preparing a low-density C/C composite material by a chemical vapor infiltration method, melting mixed powder of Si, Zr and Ti, infiltrating the mixed powder into the C/C composite material by capillary action, and forming a ceramic phase in pores by high-temperature in-situ reaction to finally obtain the ZrC-TiC modified C/C-SiC composite material.
Chinese patent CN103985842B discloses a method for preparing a ZrC-TiC/SiC double-layer complex phase ceramic coating; firstly preparing slurry containing Ti powder, then coating the slurry on a carbon substrate to obtain a prefabricated coating, and then adopting mixed powder containing Zr powder and Si powder to perform heating evaporation and reaction on the substrate on which the prefabricated coating is formed to obtain the ZrC-TiC/SiC double-layer complex phase ceramic coating.
However, in any carbide composite material, the metal powder is selected to obtain the slurry, the uniform mixing of the nano-scale materials is difficult to realize, the existing mode of preparing the composite material by mixing can be broken through, and meanwhile, the nano-particles with specific morphology are obtained, so that the method becomes the key for further development of the preparation technology of the high-temperature carbide composite material.
Disclosure of Invention
The invention aims to provide a preparation method of a ZrC-TiC composite nano-particle material, which solves the problems of pollution, product toxicity and difficulty in uniform mixing by using metal powder as slurry in the production process of the existing method.
The invention adopts the technical scheme that a preparation method of a ZrC-TiC composite nano-particle material is implemented according to the following steps:
step 3, adding all the colorless transparent solution C obtained in the step 2 into the colorless transparent solution B obtained in the step 1, and stirring and mixing uniformly to obtain a colorless transparent solution D;
step 4, carrying out rotary evaporation on the colorless transparent solution D obtained in the step 3, wherein the colorless transparent solution D is yellow after the rotary evaporation, stopping the rotary evaporation when the residual 1/3 liquid is in a wall hanging state, and drying the residual liquid in an oven to obtain a black ZrC/TiC organic composite precursor solid product;
and 5, placing the ZrC/TiC organic composite precursor solid product obtained in the step 4 into a high-temperature sintering furnace, introducing inert gas for sintering, and then cooling to room temperature along with the furnace to obtain the ZrC/TiC nano-particles of octahedrons and polyhedrons.
The present invention is also characterized in that,
in step 1, ZrOCl2·8H2The mass ratio of the O, the water, the glucose and the TBT solution is 13: 20-50: 4-8: 3.6-7.2.
In the step 2, the mass ratio of the tartaric acid to the water is 0.75-1.5: 5-10.
In step 3, the stirring time is 30 min.
In the step 4, the rotary evaporation pressure is 72-78 mbar, the water bath temperature is 45-52 ℃, the circulating cooling temperature is 5-10 ℃, and the rotary evaporation time is 2-3 hours.
In the step 4, the drying temperature is 60 ℃, and the drying time is 2-3 days.
In the step 5, the sintering temperature is 1400-1500 ℃, the time is 2h, and the heating rate is 2-5 ℃/min.
In step 5, the inert gas is Ar gas.
The preparation method of the ZrC-TiC composite nano-particle material has the beneficial effects that the ZrC/TiC organic composite precursor solid product prepared by the rotary evaporation method is sintered to obtain the ZrC/TiC nano-particles of octahedrons and polyhedrons, the production process is simple, the cost is lower, no pollution is caused, the product is non-toxic and easy to mix uniformly, the requirements of large-scale industrial production are met, and the preparation method is an excellent choice for metal organic precursors in the field of high-temperature materials.
Drawings
FIG. 1 is an X-ray diffraction pattern of ZrC/TiC nano composite particles prepared in example 1 by using the preparation method of ZrC-TiC nano particle material of the invention;
FIG. 2 is a scanning electron microscope micrograph of octahedron and polyhedral ZrC/TiC nanoparticles prepared in example 1 by the preparation method of a ZrC-TiC nanoparticle material of the invention;
FIG. 3 is a TEM image of ZrC/TiC nanoparticles prepared in example 1, using the preparation method of ZrC-TiC nanoparticle material of the invention;
FIG. 4 is a high resolution view of the cladding interface at A in FIG. 3;
FIG. 5 shows the diffraction pattern of ZrC particles obtained in example 1 of the preparation method of a ZrC-TiC nanoparticle material of the present invention;
FIG. 6 shows the diffraction pattern of TiC particles obtained in example 1, which is a method for preparing a ZrC-TiC nano-particle material of the present invention.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The invention provides a preparation method of a ZrC-TiC composite nano-particle material, which is implemented according to the following steps:
wherein ZrOCl2·8H2The mass ratio of the O to the water to the glucose to the TBT solution is 13: 20-50: 4-8: 3.6-7.2;
wherein the mass ratio of tartaric acid to water is 0.75-1.5: 5-10; ZrOCl2·8H2The mass ratio of O to tartaric acid is 13: 075-1.5;
step 3, adding the colorless transparent solution C obtained in the step 2 into the colorless transparent solution B obtained in the step 1, stirring for 30min, and uniformly mixing to obtain a colorless transparent solution D;
step 4, carrying out rotary evaporation on the colorless transparent solution D obtained in the step 3, wherein the pressure of the rotary evaporation is 72-78 mbar, the temperature of a water bath is 45-52 ℃, the circulating cooling temperature is 5-10 ℃, the rotary evaporation time is 2-3 h, the colorless transparent solution D after the rotary evaporation is yellow, stopping the rotary evaporation when the residual 1/3 liquid is in a wall hanging state, placing the residual liquid in an oven for drying, wherein the drying temperature is 60 ℃, and the drying time is 2-3 days, so as to obtain a black ZrC/TiC organic composite precursor solid product;
and 5, placing the ZrC/TiC organic composite precursor solid product obtained in the step 4 into a high-temperature sintering furnace, introducing inert gas (Ar) for sintering at 1400-1500 ℃ for 2h at the heating rate of 2-5 ℃/min, and then cooling to room temperature along with the furnace to obtain the octahedral and polyhedral ZrC/TiC nanoparticles.
Example 1
step 3, adding the colorless transparent solution C obtained in the step 2 into the colorless transparent solution B obtained in the step 1, stirring for 30min, and uniformly mixing to obtain a colorless transparent solution D;
step 4, carrying out rotary evaporation on the colorless transparent solution D obtained in the step 3, wherein the rotary evaporation pressure is 78mbar, the water bath temperature is 45 ℃, the circulating cooling temperature is 5 ℃, the rotary evaporation time is 2 hours, the colorless transparent solution D is yellow after the rotary evaporation, when the residual 1/3 liquid is in a wall hanging state, stopping the rotary evaporation, and placing the residual liquid in an oven for drying, wherein the drying temperature is 60 ℃, and the drying time is 3 days, so as to obtain a black ZrC/TiC organic composite precursor solid product;
and 5, placing the ZrC/TiC organic composite precursor solid product obtained in the step 4 into a high-temperature sintering furnace, introducing inert gas (Ar) for sintering at 1500 ℃ for 2h at the heating rate of 2 ℃/min, and then cooling to room temperature along with the furnace to obtain the octahedral and polyhedral ZrC/TiC nanoparticles.
Example 2
step 3, adding the colorless transparent solution C obtained in the step 2 into the colorless transparent solution B obtained in the step 1, stirring for 30min, and uniformly mixing to obtain a colorless transparent solution D;
step 4, carrying out rotary evaporation on the colorless transparent solution D obtained in the step 3, wherein the rotary evaporation pressure is 75mbar, the water bath temperature is 48 ℃, the circulating cooling temperature is 8 ℃, the rotary evaporation time is 2.5 hours, the colorless transparent solution D is yellow after the rotary evaporation, when the residual 1/3 liquid is in a wall hanging state, stopping the rotary evaporation, and placing the residual liquid in an oven for drying at the drying temperature of 60 ℃ for 2.5 days to obtain a black ZrC/TiC organic composite precursor solid product;
and 5, placing the ZrC/TiC organic composite precursor solid product obtained in the step 4 into a high-temperature sintering furnace, introducing inert gas (Ar) for sintering at 1500 ℃ for 2 hours at the heating rate of 3.5 ℃/min, and then cooling to room temperature along with the furnace to obtain the octahedral and polyhedral ZrC/TiC nanoparticles.
Example 3
step 3, adding the colorless transparent solution C obtained in the step 2 into the colorless transparent solution B obtained in the step 1, stirring for 30min, and uniformly mixing to obtain a colorless transparent solution D;
step 4, carrying out rotary evaporation on the colorless transparent solution D obtained in the step 3, wherein the pressure of the rotary evaporation is 72mbar, the temperature of a water bath is 50 ℃, the circulating cooling temperature is 5 ℃, the rotary evaporation time is 2.5 hours, the colorless transparent solution D is yellow after the rotary evaporation, when the residual 1/3 liquid is in a wall hanging state, stopping the rotary evaporation, and placing the residual liquid in an oven for drying at the drying temperature of 60 ℃ for 2 days to obtain a black ZrC/TiC organic composite precursor solid product;
and 5, placing the ZrC/TiC organic composite precursor solid product obtained in the step 4 into a high-temperature sintering furnace, introducing inert gas (Ar) for sintering at 1400 ℃ for 2h at the heating rate of 5 ℃/min, and then cooling to room temperature along with the furnace to obtain the octahedral and polyhedral ZrC/TiC nanoparticles.
Example 4
step 3, adding the colorless transparent solution C obtained in the step 2 into the colorless transparent solution B obtained in the step 1, stirring for 30min, and uniformly mixing to obtain a colorless transparent solution D;
step 4, carrying out rotary evaporation on the colorless transparent solution D obtained in the step 3, wherein the rotary evaporation pressure is 78mbar, the water bath temperature is 48 ℃, the circulating cooling temperature is 8 ℃, the rotary evaporation time is 2.5h, the colorless transparent solution D is yellow after the rotary evaporation, when the residual 1/3 liquid is in a wall hanging state, stopping the rotary evaporation, and placing the residual liquid in an oven for drying at the drying temperature of 60 ℃ for 3 days to obtain a black ZrC/TiC organic composite precursor solid product;
and 5, placing the ZrC/TiC organic composite precursor solid product obtained in the step 4 into a high-temperature sintering furnace, introducing inert gas (Ar) for sintering at 1450 ℃ for 2h at the heating rate of 3.5 ℃/min, and then cooling to room temperature along with the furnace to obtain the octahedral and polyhedral ZrC/TiC nanoparticles.
Example 5
step 3, adding the colorless transparent solution C obtained in the step 2 into the colorless transparent solution B obtained in the step 1, stirring for 30min, and uniformly mixing to obtain a colorless transparent solution D;
step 4, carrying out rotary evaporation on the colorless transparent solution D obtained in the step 3, wherein the pressure of the rotary evaporation is 75mbar, the water bath temperature is 46 ℃, the circulating cooling temperature is 5 ℃, the rotary evaporation time is 3 hours, the colorless transparent solution D is yellow after the rotary evaporation, when the residual 1/3 liquid is in a wall hanging state, stopping the rotary evaporation, and placing the residual liquid in an oven for drying, wherein the drying temperature is 60 ℃, and the drying time is 3 days, so as to obtain a black ZrC/TiC organic composite precursor solid product;
and 5, placing the ZrC/TiC organic composite precursor solid product obtained in the step 4 into a high-temperature sintering furnace, introducing inert gas (Ar) for sintering at 1400 ℃ for 2h at the heating rate of 2 ℃/min, and then cooling to room temperature along with the furnace to obtain the octahedral and polyhedral ZrC/TiC nanoparticles.
FIG. 1 is an X-ray diffraction pattern (XRD) of ZrC/TiC nanoparticles, from which it can be seen that the nanoparticles have characteristic peaks of ZrC and TiC and show the tendency of Ti to be solid-dissolved in ZrC, and the ZrC/TiC diffraction peak intensity of the ZrC/TiC organic composite precursor solid product obtained by sintering at 1400-1500 ℃ for 2h is high and the crystallinity is good; FIG. 2 is a Scanning Electron Microscope (SEM) of ZrC/TiC nanoparticles, and the ZrC/TiC nanoparticles are found to be in octahedral and polyhedral shapes; FIG. 3 is a TEM image of ZrC/TiC nanoparticles, and shows that the light-colored polyhedral particles are TiC particles, the dark-colored polyhedral particles are ZrC particles, and the composite nanoparticles all present a carbon-coated structure; FIG. 4 is a high resolution view of the cladding interface of FIG. 3A; fig. 5 shows the electron emission pattern of ZrC nanoparticles and fig. 6 shows the electron emission pattern of TiC nanoparticles, and it can be seen from the figures that both ZrC and TiC particles exhibit a single crystal structure.
Claims (8)
1. A preparation method of a ZrC-TiC composite nano-particle material is characterized by comprising the following steps:
step 1, ZrOCl2·8H2Mixing O and water, stirring until the O is completely dissolved to obtain a colorless transparent solution A, sequentially adding glucose and a TBT solution into the colorless transparent solution A, dropwise adding the TBT solution, and uniformly stirring to obtain a colorless transparent solution B;
step 2, mixing tartaric acid with water, stirring and dissolving to obtain a colorless transparent solution C;
step 3, adding the colorless transparent solution C obtained in the step 2 into the colorless transparent solution B obtained in the step 1, and stirring and mixing uniformly to obtain a colorless transparent solution D;
step 4, carrying out rotary evaporation on the colorless transparent solution D obtained in the step 3, wherein the colorless transparent solution D is yellow after the rotary evaporation, stopping the rotary evaporation when the residual 1/3 liquid is in a wall hanging state, and drying the residual liquid in an oven to obtain a black ZrC/TiC organic composite precursor solid product;
and 5, placing the ZrC/TiC organic composite precursor solid product obtained in the step 4 into a high-temperature sintering furnace, introducing inert gas for sintering, and then cooling to room temperature along with the furnace to obtain the ZrC/TiC nano-particles of octahedrons and polyhedrons.
2. The method for preparing ZrC-TiC composite nano-particle material as claimed in claim 1, wherein in the step 1, ZrOCl is adopted2·8H2The mass ratio of the O, the water, the glucose and the TBT solution is 13: 20-50: 4-8: 3.6-7.2.
3. The method for preparing a ZrC-TiC composite nano-particle material as claimed in claim 1, wherein in the step 2, the mass ratio of tartaric acid to water is 0.75-1.5: 5-10.
4. The method for preparing ZrC-TiC composite nano-particle material as claimed in claim 1, wherein in the step 3, the stirring time is 30 min.
5. The preparation method of a ZrC-TiC composite nano-particle material as claimed in claim 1, wherein in the step 4, the pressure of rotary evaporation is 72-78 mbar, the temperature of water bath is 45-52 ℃, the temperature of circulating cooling is 5-10 ℃, and the time of rotary evaporation is 2-3 h.
6. The method for preparing a ZrC-TiC composite nano-particle material as claimed in claim 1, wherein in the step 4, the drying temperature is 60 ℃ and the drying time is 2-3 days.
7. The method for preparing ZrC-TiC composite nano-particle material as claimed in claim 1, wherein in the step 5, the sintering temperature is 1400-1500 ℃, the time is 2h, and the heating rate is 2-5 ℃/min.
8. The method for preparing ZrC-TiC composite nano-particle material as claimed in claim 1, wherein in the step 5, the inert gas is Ar gas.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102530942A (en) * | 2010-12-08 | 2012-07-04 | 中国科学院金属研究所 | Preparation method for synthesizing zirconium carbide powder material by utilizing zirconium-containing organic matter precursor |
| CN111471962A (en) * | 2020-02-21 | 2020-07-31 | 西安理工大学 | Method for preparing ZrC organic precursor by rotary evaporation |
| CN112479711A (en) * | 2020-12-17 | 2021-03-12 | 西安理工大学 | Preparation method of zirconium carbide/hafnium carbide nano composite particles |
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| CN102530942A (en) * | 2010-12-08 | 2012-07-04 | 中国科学院金属研究所 | Preparation method for synthesizing zirconium carbide powder material by utilizing zirconium-containing organic matter precursor |
| CN111471962A (en) * | 2020-02-21 | 2020-07-31 | 西安理工大学 | Method for preparing ZrC organic precursor by rotary evaporation |
| CN112479711A (en) * | 2020-12-17 | 2021-03-12 | 西安理工大学 | Preparation method of zirconium carbide/hafnium carbide nano composite particles |
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| FUPING LI等: "Microstructural features and oxidation resistance of (Ti, Zr)C solid solution nanofibers fabricated using polymeric precursors", 《CERAMICS INTERNATIONAL》 * |
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| MADIS UMALAS等: "Synthesis of ZrC-TiC Blend by Novel Combination of Sol-gel Method and Carbothermal Reduction", 《KEY ENGINEERING MATERIALS》 * |
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