CN111056844A - CNT-B4C-TiB2Complex phase ceramic and preparation method thereof - Google Patents
CNT-B4C-TiB2Complex phase ceramic and preparation method thereof Download PDFInfo
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Abstract
CNT-B4C‑TiB2A complex phase ceramic and a preparation method thereof belong to the technical field of composite material preparation. The CNT-B4C‑TiB2The preparation method of the complex phase ceramic comprises the following steps: s1, mixing the CNT dispersion with B4C、TiO2Mixing with phenolic resin, and stirring to obtain CNT-B4C‑TiO2Compounding the slurry; s2, CNT-B4C‑TiO2Spraying and granulating the composite slurry to obtain CNT-B4C‑TiO2Compounding dry powder; s3, mixing CNT-B4C‑TiO2Laying the composite dry powder in a mould, and compacting and forming; then fired to give CNT-B4C‑TiB2A complex phase ceramic. According to the invention, by adding CNT and adopting a staged sintering process, the toughness and hardness of the prepared complex phase ceramic can be improved while the sintering requirement is reduced.
Description
Technical Field
The invention relates to a technology in the field of composite material preparation, in particular to a CNT-B4C-TiB2A complex phase ceramic and a preparation method thereof.
Background
B4The C ceramic has excellent physical and mechanical properties, such as low density and high strength, and is widely applied to the fields of armor and nuclear energy. B is4C is second only to diamond and cubic boron nitride, is brittle in nature, and is therefore often requiredDifferent additives are needed to improve the sintering and mechanical properties. B is4C-TiB2TiB in composite material2The addition of (2) improves the size and distribution of crystal grains and micro-pores, reduces the porosity, and improves the fracture toughness and the bending strength. However, B4C and TiB2Pressureless reaction sintering is harsh to the sintering temperature, generally not lower than 2100 ℃, and if the temperature is lower than 1800 ℃, the density of the sintered complex phase ceramic is even lower than that of a pressed compact.
The present invention has been made to solve the above-mentioned problems occurring in the prior art.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a CNT-B4C-TiB2The composite ceramic and the preparation method thereof can improve the toughness and hardness of the prepared composite ceramic while reducing the sintering requirement by adding the CNT and adopting a staged sintering process.
The present invention relates to a CNT-B4C-TiB2The preparation method of the complex phase ceramic comprises the following steps:
s1, mixing the CNT dispersion with B4C nano powder and TiO2Mixing the nano powder and phenolic resin, and stirring uniformly to obtain CNT-B4C-TiO2Compounding the slurry;
S2，CNT-B4C-TiO2spraying and granulating the composite slurry to obtain CNT-B4C-TiO2Compounding dry powder;
s3, mixing CNT-B4C-TiO2Laying the composite dry powder in a mould, compacting and forming, and sintering in two stages under a vacuum condition; the first stage is heated to 1500-4C-TiB2A complex phase ceramic.
Preferably, the CNT-B4C-TiO2CNT and B in composite slurry4C nano powder and TiO2The mixing ratio of the nano powder by weight is 1-5: 1-20: 1, CNT-B4C-TiO2The weight proportion of the phenolic resin in the composite slurry is 1-10%.
The present invention relates to a CNT-B4C-TiB2The complex phase ceramic is prepared by the method.
Technical effects
Compared with the prior art, the invention has the following technical effects:
1) the CNT is added into the complex phase ceramic, so that the performance of the complex phase ceramic is improved; by means of B4C、TiO2And CNT in situ Synthesis of CNT-B4C-TiB2Composite materials, in situ Synthesis comprising a two stage reaction, first stage 5B4C+6TiO2＝6TiB2+4B2O3+5C, reaction temperature 1500-2O3+7C＝B4C +6CO, the reaction temperature is 1900-2200 ℃, and the C participating in the reaction in the second stage comprises free carbon and B generated in the reaction in the first stage4The carbon impurities existing in the C nano powder and the carbon supplemented by the carbon nano tube; free carbon generated in the first stage reaction is completely oxidized into CO in the second stage, so that the generation of the free carbon is avoided, and the strength of the complex-phase ceramic is reduced; the high temperature of 1900-2200 ℃ in the second stage increases B relative to the firing temperature of 1500-1700 ℃ in the first stage4C and TiB2The diffusion coefficient accelerates the discharge of CO, and avoids the increase of the porosity and the reduction of the density of the complex phase ceramic caused by the unsmooth discharge of the generated CO, thereby ensuring the toughness and the hardness of the complex phase ceramic;
2) preparation of CNT as dispersion improves the interaction with B4C、TiO2And the compatibility of the phenolic resin ensures the uniform dispersion of the CNT in the complex phase ceramic, thereby ensuring the toughening effect of the complex phase ceramic.
Drawings
FIG. 1 is an SEM photograph of a CNT dispersion of example 1;
FIG. 2 shows CNT-B prepared in example 14C-TiB2XRD pattern of the complex phase ceramic;
FIG. 3 shows CNT-B prepared in example 14C-TiB2SEM photograph of the complex phase ceramic.
Detailed Description
The invention is described in detail below with reference to the drawings and the detailed description.
The embodiment of the invention relates to a CNT-B4C-TiB2The preparation method of the complex phase ceramic comprises the following steps:
s1, mixing the CNT dispersion with B4C nano powder and TiO2Mixing the nano powder and phenolic resin, and stirring uniformly to obtain CNT-B4C-TiO2Compounding the slurry;
S2，CNT-B4C-TiO2spraying and granulating the composite slurry to obtain CNT-B4C-TiO2Compounding dry powder;
s3, mixing CNT-B4C-TiO2Laying the composite dry powder in a mould, compacting and forming, and sintering in two stages under a vacuum condition; the first stage is heated up to 1700 ℃ at the rate of 5-20 ℃/min, the temperature is maintained for 0.5-1h, the second stage is heated up to 2200 ℃ at the rate of 5-20 ℃/min, the temperature is maintained for 1-2h, and the CNT-B is prepared4C-TiB2A complex phase ceramic.
The CNT dispersion is prepared by mixing CNT, PVP (polyvinyl pyrrolidone) and H2And O, mixing, performing ultrasonic treatment, and uniformly stirring to obtain the product.
The CNT-B4C-TiO2CNT and B in composite slurry4C nano powder and TiO2The mixing ratio of the nano powder by weight is 1-5: 1-20: 1, CNT-B4C-TiO2The weight proportion of the phenolic resin in the composite slurry is 1-10%.
The CNT is a whisker multi-wall carbon nanotube, the length of the CNT is 5-20 mu m, and the diameter of the CNT is 50-200 nm.
B is4The grain size of the C nano powder is 100-500 nm.
The TiO is2The grain size of the nano powder is 100-200 nm.
The temperature of the air inlet is 180-200 ℃ and the temperature of the air outlet is 98-110 ℃ in the spray granulation process.
Example 1
This example relates to a CNT-B4C-TiB2The preparation method of the complex phase ceramic comprises the following steps:
S1，CNT-B4C-TiO2preparing composite slurry;
s11, preparing a CNT dispersion liquid;
CNT in weight ratio: PVP: h2Uniformly mixing the raw materials at a ratio of 55:1:400, performing ultrasonic treatment, and uniformly stirring to obtain a CNT dispersion liquid, wherein the CNT is a whisker multi-walled carbon nanotube, the length of the CNT is 5-20 mu m, and the diameter of the CNT is 50-200 nm; the CNT dispersion liquid is detected by a scanning electron microscope to obtain an SEM image shown in figure 1, and the CNT dispersion liquid is found to have good dispersion effect and no agglomeration phenomenon;
s12 preparation of CNT-B4C-TiO2Compounding the slurry;
2.0kg of H was added to the slurry mixing tank2O, 10kg of B with a particle size of 120nm are added in batches4C nanopowder, B4After the C is completely added and stirred uniformly, 0.5kg of TiO with the particle size of 170nm is slowly added from a feeding port2Nanopowder and 5.5kg of CNT dispersion; stirring for 30min, adding 0.3kg phenolic resin, and stirring to obtain CNT-B4C-TiO2Compounding the slurry;
S2，CNT-B4C-TiO2preparing composite dry powder;
CNT-B4C-TiO2spraying and granulating the composite slurry (the air inlet temperature is 200 ℃, the air outlet temperature is 100 ℃) to obtain CNT-B4C-TiO2Compounding dry powder;
S3，CNT-B4C-TiB2preparing complex phase ceramic;
mixing CNT-B4C-TiO2Laying the composite dry powder in a mould, compacting and forming, and firing in two stages under a vacuum condition; the first stage is heated to 1600 ℃ at the speed of 5-20 ℃/min, the temperature is kept for 0.5h, the second stage is heated to 2100 ℃ at the speed of 5-20 ℃/min, the temperature is kept for 1h, and finally the CNT-B is obtained4C-TiB2A complex phase ceramic.
CNT-B prepared by scanning Electron microscope and X-ray diffractometer for this example4C-TiB2And carrying out structural characterization on the complex-phase ceramic to obtain an XRD (X-ray diffraction) pattern shown in figure 2 and an SEM (scanning electron microscope) pattern shown in figure 3. As can be seen from the XRD pattern of FIG. 2, CNT-B4C-TiB2Multiple phase ceramics composed of C, B4C、TiB2Three phases are formed, and no other phases or substances are found. As can be seen from the SEM image of FIG. 3, CNT-B4C-TiB2The composite ceramic has good densification and uniform dispersion of CNT. CNT-B measurement by Archimedes method4C-TiB2The density of the complex phase ceramic is 99.58% of theoretical.
It is to be emphasized that: the above embodiments are only preferred embodiments of the present invention, and are not intended to limit the present invention in any way, and all simple modifications, equivalent changes and modifications made to the above embodiments according to the technical spirit of the present invention are within the scope of the technical solution of the present invention.
Claims (9)
1. CNT-B4C-TiB2The preparation method of the complex phase ceramic is characterized by comprising the following steps:
s1, mixing the CNT dispersion with B4C nano powder and TiO2Mixing the nano powder and phenolic resin, and stirring uniformly to obtain CNT-B4C-TiO2Compounding the slurry;
S2，CNT-B4C-TiO2spraying and granulating the composite slurry to obtain CNT-B4C-TiO2Compounding dry powder;
s3, mixing CNT-B4C-TiO2Laying the composite dry powder in a mould, compacting and forming, and sintering in two stages under a vacuum condition; the first stage is heated to 1500-4C-TiB2A complex phase ceramic.
2. The CNT-B of claim 14C-TiB2The preparation method of the complex phase ceramic is characterized in that the CNT dispersion liquid is prepared by mixing CNT, PVP and H2And O, mixing, performing ultrasonic treatment, and uniformly stirring to obtain the product.
3. The CNT-B of claim 14C-TiB2The preparation method of the complex phase ceramic is characterized in that the CNT-B4C-TiO2CNT and B in composite slurry4C nano powder and TiO2The mixing ratio of the nano powder by weight is 1-5: 1-20: 1, CNT-B4C-TiO2The weight proportion of the phenolic resin in the composite slurry is 1-10%.
4. The CNT-B of claim 34C-TiB2The preparation method of the multiphase ceramic is characterized in that the CNT is a whisker multi-wall carbon nanotube, the length of the CNT is 5-20 mu m, and the diameter of the CNT is 50-200 nm.
5. The CNT-B of claim 34C-TiB2The preparation method of the complex phase ceramic is characterized in that B4The grain size of the C nano powder is 100-500 nm.
6. The CNT-B of claim 34C-TiB2The preparation method of the complex phase ceramic is characterized in that the TiO is2The grain size of the nano powder is 100-200 nm.
7. The CNT-B of claim 14C-TiB2The preparation method of the complex phase ceramic is characterized in that the temperature of an air inlet is 180-200 ℃ and the temperature of an air outlet is 98-110 ℃ in the spray granulation.
8. The CNT-B of claim 14C-TiB2The preparation method of the complex phase ceramic is characterized in that the temperature rise rate of the first stage is 5-20 ℃/min, and the temperature rise rate of the second stage is 5-20 ℃/min.
9. CNT-B4C-TiB2Composite phase ceramics, characterized in that they are obtained by the process according to any one of claims 1 to 8.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1038632A (en) * | 1988-05-26 | 1990-01-10 | 唐化学原料公司 | Make the method and composition that matrix is made norbide/TiB2 composite ceramic powders with norbide |
| CN1582264A (en) * | 2001-11-06 | 2005-02-16 | 独立行政法人产业技术总合研究所 | Boron carbide based sintered compact and method for preparation thereof |
| CN107098703A (en) * | 2017-04-20 | 2017-08-29 | 哈尔滨工业大学 | A kind of TiB2TiC ceramic composites and preparation method thereof |
| CN110282983A (en) * | 2019-07-05 | 2019-09-27 | 河南理工大学 | A kind of high rigidity TiB of no interphase2-B4C ceramic composite preparation method and applications |
-
2019
- 2019-11-28 CN CN201911188019.2A patent/CN111056844A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1038632A (en) * | 1988-05-26 | 1990-01-10 | 唐化学原料公司 | Make the method and composition that matrix is made norbide/TiB2 composite ceramic powders with norbide |
| CN1582264A (en) * | 2001-11-06 | 2005-02-16 | 独立行政法人产业技术总合研究所 | Boron carbide based sintered compact and method for preparation thereof |
| CN107098703A (en) * | 2017-04-20 | 2017-08-29 | 哈尔滨工业大学 | A kind of TiB2TiC ceramic composites and preparation method thereof |
| CN110282983A (en) * | 2019-07-05 | 2019-09-27 | 河南理工大学 | A kind of high rigidity TiB of no interphase2-B4C ceramic composite preparation method and applications |
Non-Patent Citations (2)
| Title |
|---|
| K. SAIRAM等人: "Mechanical properties of HfB2 reinforced B4C matrix ceramics processed by insitu reaction of B4C，HfO2 and CNT", 《SPRINGER INTERNATIONAL PUBLISHING》 * |
| V. SKOROKHOD等人: "High strength-high toughness B4C-TiB2 composites", 《JOURNAL OF MATERIALS SCIENCE LETTERS》 * |
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