CN107879745B - Ceramic material containing eutectic structure and preparation method thereof - Google Patents
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Abstract
The invention discloses HfB containing eutectic structures2-HfC-SiC ceramic material and a preparation method thereof. The ceramic material comprises HfB in percentage by mass260-70%, HfC 5-15%, and SiC 20-30%. The preparation method comprises the following steps: to HfB2Mixing HfC and SiC raw material powder uniformly by wet ball milling, and drying to obtain HfB2-HfC-SiC mixed powder; putting the mixed powder into a graphite mould, and heating and preserving heat under a vacuum condition; then applying axial load, introducing inert atmosphere, simultaneously heating, preserving heat, performing hot-pressing sintering and preparing HfB2-an HfC-SiC ceramic material; to HfB2And (3) after the HfC-SiC ceramic material is subjected to heat treatment, grinding the superficial layer with pores. The ceramic material prepared by the invention has excellent mechanical properties, and the preparation method has the advantages of simple process, strong controllability and the like.
Description
Technical Field
The invention relates to HfB containing eutectic structures2-HfC-SiC ceramic material and a preparation method thereof, belonging to the field of high temperature resistant material.
Background
HfB2The melting point of the material is higher than 3000 ℃, the material has excellent high temperature resistance, and has unique potential advantages in the aspect of being used as an ultrahigh temperature thermal protection material. NASA studies in the United states found on HfB2HfB prepared by adding SiC2the-SiC complex phase ceramic has good ablation resistance, and an oxide layer generated on the surface of the-SiC complex phase ceramic due to high-temperature ablation can play an effective role in protecting a matrix material. However, when the heat flux density and the mach number reach critical values, the adhesion of the surface oxide layer to the substrate may be reduced, resulting in deterioration of ablation resistance. To address this problem, researchers in NASA have regulated HfB2-a composition of SiC ceramics, to which the addition of HfC improves its ablation resistance. The results show that HfB2The ablation resistance of the-HfC-SiC ceramic is better than that of HfB2-SiC complex phase ceramics [ ball J, et. al., U.S. patent, No.5750450,1998.]. Therefore, HfB2The HfC-SiC ceramic is very promising to be used as a novel ultra-high temperature thermal protection material for hypersonic aircrafts.
It is well known that the microstructure of a material features a diameter shadowThe fine and uniform microstructure is usually beneficial to improving the mechanical property of the material by influencing the mechanical property of the material. Eutectic and hypoeutectic materials generally have very fine tissue structures, and all phases in the eutectic structures are staggered and nested with one another to form a network structure, so that the materials show excellent mechanical properties. It has been shown that eutectic or hypoeutectic ZrB2-SiC ceramic, ZrB2-SiC-B4C ceramics and the like have higher mechanics and fracture toughness. E.g. ZrB having eutectic structure characteristics2The hardness of the-SiC ceramic is up to 24GPa, and the toughness is up to 6.0 MPa.m1/2[Tu R,et.al.,Journal of the Ceramic Societ of Japan 116 431-435 2008.]. Therefore, if it can be in HfB2Eutectic or hypoeutectic structures are prepared in the HfC-SiC ceramic, so that the mechanical property of the material can be further improved.
The high-temperature heat treatment method is one of effective methods for preparing a ceramic material containing a eutectic structure. The method designs the initial composition design and the heat treatment process of the material according to the eutectic composition point and the eutectic temperature of the material to obtain a completely eutectic material or a hypoeutectic material with higher eutectic structure content. Therefore, the HfB is reasonably designed by adopting the high-temperature heat treatment method2Initial composition of HfC-SiC ceramic and thermal treatment process, will enable obtaining HfB containing eutectic structure2-HfC-SiC ceramic expected to further improve HfB2The mechanical property of the-HfC-SiC ceramic is of great significance for promoting the practical application of the material.
Disclosure of Invention
The invention aims to solve the problems that: provided is HfB having a eutectic structure2-HfC-SiC ceramic material and method for preparing the same to further improve HfB2-mechanical properties of HfC-SiC ceramics.
In order to solve the problems, the technical scheme adopted by the invention is as follows:
a ceramic material having a eutectic structure, comprising HfB in a mass percentage260-70%, HfC 5-15%, and SiC 20-30%.
Preferably, the HfB2Eutectic structures contained in the-HfC-SiC ceramic materialThe network structure is formed by mutually interleaving and nesting.
The invention also provides a preparation method of the ceramic material containing the eutectic structure, which is characterized by comprising the following steps of:
step 1): to HfB2Mixing HfC and SiC raw material powder uniformly by wet ball milling, and drying to obtain HfB2-HfC-SiC mixed powder;
step 2): putting the mixed powder obtained in the step 1) into a graphite mold, firstly heating to 1600-1650 ℃ under a vacuum condition, and preserving heat for 15-30 minutes; then applying axial load to enable the sample to bear the pressure of 25-50 MPa, introducing inert atmosphere, simultaneously heating to 1900-2200 ℃, and carrying out heat-pressing sintering for 30-90 minutes to prepare HfB2-an HfC-SiC ceramic material;
step 3): HfB obtained in the step 2)2-subjecting the HfC-SiC ceramic material to a heat treatment: heating to 2450 ℃ in a graphite resistance furnace under inert atmosphere, preserving heat for 5 minutes, cooling to 2200-2400 ℃, preserving heat for 5-30 minutes, stopping heating, cooling the sample to room temperature, and then grinding a superficial layer with pores to obtain HfB containing eutectic structures2-HfC-SiC ceramic material.
Preferably, HfB in said step 1)2The particle size of the raw material powder is 0.5-1.5 mu m, and the mass purity is more than or equal to 98.5%; the particle size of the HfC powder is 0.1-1.5 mu m, and the mass purity is more than or equal to 99%; the grain diameter of the SiC powder is 0.4-1.5 μm, and the mass purity is more than or equal to 99%.
Preferably, ethanol or acetone is used as a ball milling medium for wet ball milling in the step 1), and SiC ceramic balls are used as milling balls.
Preferably, the inert atmosphere in the step 3) is argon with the mass purity of 99.99-99.999%.
Compared with the prior art, the invention has the following beneficial effects:
1. HfB containing eutectic structure prepared by the invention2The HfC-SiC ceramic material has a fine organization structure, all phases in the eutectic structure are mutually staggered and nested to form a network structure, and the material has excellent mechanical properties. The material has strong four-point bending at room temperatureThe degree is obviously higher than that of HfB without eutectic structures prepared by the conventional hot-pressing sintering method2-an HfC-SiC ceramic;
2. the invention provides HfB containing eutectic structure2The preparation method of the-HfC-SiC ceramic material has the advantages of simple process, strong controllability and the like.
Drawings
FIG. 1 is a HfB prepared in example 12-SEM image of fracture micro-topography of HfC-SiC ceramic material;
FIG. 2 shows HfB prepared in example 22-XRD pattern of HfC-SiC ceramic material;
FIG. 3 is HfB prepared in example 32-XRD pattern of HfC-SiC ceramic material.
Detailed Description
In order to make the invention more comprehensible, preferred embodiments are described in detail below with reference to the accompanying drawings.
Example 1
HfB containing eutectic structure2The preparation method of the-HfC-SiC ceramic material comprises the following steps:
to HfB2Mixing 0.5-1.5 mu m (98.5 wt.%), HfC powder (0.1-1.5 mu m (99 wt.%), and SiC powder (0.4-1.5 mu m (99 wt.%) in a mass ratio of 60:15:25, ball-milling and mixing on a roller ball mill at a rotating speed of 200 rpm for 24h by using ethanol as a medium and SiC balls as grinding balls, and performing rotary evaporation to obtain HfB2-HfC-SiC mixed dry powder; the mixed dry powder is put into a graphite mould, and is heated to 1650 ℃ under vacuum condition and is kept warm for 15 minutes. Then, applying axial load to enable the sample to bear 25MPa of pressure, introducing argon with the mass purity of 99.99, and simultaneously heating to 2100 ℃ and preserving the temperature for 45 minutes to obtain HfB through hot-pressing sintering2-an HfC-SiC ceramic; heating the obtained ceramic in a graphite resistance furnace under inert atmosphere to 2450 ℃ and preserving heat for 5 minutes, cooling to 2300 ℃ and preserving heat for 10 minutes, stopping heating, cooling the sample to room temperature, and then grinding the superficial layer with pores to obtain HfB containing eutectic structures2-HfC-SiC ceramic material.
After analysis: prepared HfB2The density of the-HfC-SiC ceramic reaches 99 percent. It is composed ofContains fine eutectic structures, and all phases in the eutectic structures are mutually staggered and nested to form a network structure, as shown in figure 1. HfB having eutectic structure2-HfC-SiC ceramic material and HfB obtained by direct hot-pressing sintering without heat treatment2The room temperature four-point bending strength vs. ratio of the-HfC-SiC ceramic is shown in Table 1. It can be seen that HfB obtained by direct hot-pressing sintering2Compared with HfC-SiC ceramic, HfB containing eutectic structure is obtained by hot-pressing sintering and then heat treatment by adopting the method2-HfC-SiC ceramic having a four-point bending strength at room temperature significantly higher than that of HfB without eutectic structure prepared by conventional hot-press sintering2-HfC-SiC ceramic.
Example 2
HfB containing eutectic structure2The preparation method of the-HfC-SiC ceramic material comprises the following steps:
to HfB2Mixing 0.5-1.5 mu m (98.5 wt.%), HfC powder (0.1-1.5 mu m (99 wt.%), and SiC powder (0.4-1.5 mu m (99 wt.%)) according to a mass ratio of 65:15:20, ball-milling and mixing on a roller ball mill for 24h at a rotating speed of 200 r/min by using ethanol as a medium and SiC balls as grinding balls, and performing rotary evaporation to obtain HfB2-HfC-SiC mixed dry powder; the mixed dry powder is put into a graphite mould, and is heated to 1600 ℃ under the vacuum condition and is kept for 30 minutes. Then, applying axial load to enable the sample to bear 50MPa of pressure, introducing argon with the mass purity of 99.99, and simultaneously heating to 2000 ℃ and preserving heat for 70 minutes to obtain HfB through hot-pressing sintering2-an HfC-SiC ceramic; heating the obtained ceramic in a graphite resistance furnace under inert atmosphere to 2450 ℃ and preserving heat for 5 minutes, cooling to 2250 ℃ and preserving heat for 30 minutes, stopping heating, cooling the sample to room temperature, and then grinding the superficial layer with pores to obtain HfB containing eutectic structures2-HfC-SiC ceramic material.
After analysis: the density of the prepared ceramic material reaches 99.2 percent, and the phase composition of the ceramic material is HfB2HfC, SiC. The XRD pattern of the resulting ceramic material is shown in FIG. 2. The room temperature four-point bending strength of the resulting ceramic material is shown in table 1.
Example 3
HfB containing eutectic structure2-HfC-SiC, the preparation method of the ceramic material comprises the following steps:
to HfB2Mixing 0.5-1.5 mu m (98.5 wt.%), HfC powder (0.1-1.5 mu m (99 wt.%), and SiC powder (0.4-1.5 mu m (99 wt.%)) in a mass ratio of 70:10:20, ball-milling and mixing on a roller ball mill at a rotating speed of 200 rpm for 24h by using ethanol as a medium and SiC balls as grinding balls, and performing rotary evaporation to obtain HfB2-HfC-SiC mixed dry powder; the mixed dry powder is put into a graphite mould, and is heated to 1600 ℃ under the vacuum condition and is kept for 30 minutes. Then, applying axial load to enable the sample to bear 30MPa of pressure, introducing argon with the mass purity of 99.99, and simultaneously heating to 2000 ℃ and preserving heat for 60 minutes to obtain HfB through hot-pressing sintering2-an HfC-SiC ceramic; heating the obtained ceramic in a graphite resistance furnace under inert atmosphere to 2450 ℃ for 5 minutes, cooling to 2350, keeping the temperature for 5 minutes, stopping heating, cooling the sample to room temperature, and then grinding off the superficial layer with pores to obtain HfB containing eutectic structures2-HfC-SiC ceramic material.
After analysis: prepared HfB2The density of the-HfC-SiC ceramic reaches 99.1 percent, and the phase composition of the-HfC-SiC ceramic is HfB2HfC, SiC. The XRD pattern of the resulting ceramic material is shown in FIG. 3. The room temperature four-point bending strength of the resulting ceramic material is shown in table 1.
Example 4
HfB containing eutectic structure2The preparation method of the-HfC-SiC ceramic material comprises the following steps:
to HfB2Mixing 0.5-1.5 mu m (98.5 wt.%), HfC powder (0.1-1.5 mu m (99 wt.%), and SiC powder (0.4-1.5 mu m (99 wt.%) in a mass ratio of 62:10:28, ball-milling and mixing on a roller ball mill at a rotating speed of 200 rpm for 24h by using ethanol as a medium and SiC balls as grinding balls, and performing rotary evaporation to obtain HfB2-HfC-SiC mixed dry powder; the mixed dry powder is put into a graphite mould, and is heated to 1600 ℃ under the vacuum condition and is kept for 30 minutes. Then, applying axial load to enable the sample to bear 30MPa of pressure, introducing argon with the mass purity of 99.99, and simultaneously heating to 2000 ℃ and preserving heat for 60 minutes to obtain HfB through hot-pressing sintering2-an HfC-SiC ceramic; subjecting the obtained ceramic to graphite treatment under inert atmosphereHeating in a resistance furnace to 2450 ℃ and preserving heat for 5 minutes, cooling to 2340 and preserving heat for 5 minutes, stopping heating, cooling the sample to room temperature, and then grinding the superficial layer with pores to obtain HfB containing eutectic structures2-HfC-SiC ceramic material.
After analysis: prepared HfB2The density of the-HfC-SiC ceramic reaches 99%, and the material contains fine eutectic structures, and all phases are uniformly distributed. The room temperature four-point bending strength of the resulting ceramic material is shown in table 1.
Table 1 shows HfB containing eutectic structures prepared in examples 1 to 42-HfC-SiC ceramic and HfB prepared by conventional hot pressing sintering method and free of eutectic structure2Room temperature four-point bending strength comparison of HfC-SiC ceramics.
TABLE 1
Claims (5)
1. A ceramic material having a eutectic structure, comprising HfB in a mass percentage2
60-70%, HfC 5-15% and SiC 20-30%;
the preparation method of the ceramic material containing the eutectic structure comprises the following steps:
step 1): to HfB2Mixing HfC and SiC raw material powder uniformly by wet ball milling, and drying to obtain HfB2-HfC-SiC mixed powder;
step 2): putting the mixed powder obtained in the step 1) into a graphite mold, firstly heating to 1600-1650 ℃ under a vacuum condition, and preserving heat for 15-30 minutes; then applying axial load to enable the sample to bear the pressure of 25-50 MPa, introducing inert atmosphere, simultaneously heating to 1900-2200 ℃, and carrying out heat-pressing sintering for 30-90 minutes to prepare HfB2-an HfC-SiC ceramic material;
step 3): HfB obtained in the step 2)2-subjecting the HfC-SiC ceramic material to a heat treatment: heating to 2450 deg.C in graphite resistance furnace under inert atmosphere, maintaining for 5 min, and coolingHeating is stopped after the temperature is kept for 5-30 minutes at 2200-2400 ℃, and after the sample is cooled to the room temperature, the superficial layer with pores is ground, so that HfB containing eutectic structures is prepared2-HfC-SiC ceramic material.
2. The ceramic material having a eutectic structure of claim 1, wherein said HfB2Eutectic structures contained in the HfC-SiC ceramic material are mutually staggered and nested to form a network structure.
3. The ceramic material having a eutectic structure according to claim 1, wherein HfB in step 1) is2The particle size of the raw material powder is 0.5-1.5 mu m, and the mass purity is more than or equal to 98.5%; the particle size of the HfC powder is 0.1-1.5 mu m, and the mass purity is more than or equal to 99%; the grain diameter of the SiC powder is 0.4-1.5 mu m, and the mass purity is more than or equal to 99%.
4. The ceramic material containing the eutectic structure according to claim 1, wherein the wet ball milling in step 1) is performed with ethanol or acetone as a milling medium, and SiC ceramic balls are used as milling balls.
5. The ceramic material containing the eutectic structure according to claim 1, wherein the inert atmosphere in the step 3) is argon gas having a mass purity of 99.99 to 99.999%.
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| JPH0497952A (en) * | 1990-08-09 | 1992-03-30 | Eagle Ind Co Ltd | Silicon carbide-based composite body |
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| CN103979974A (en) * | 2014-05-14 | 2014-08-13 | 西北工业大学 | Preparation method of C/SiC-HfB2-HfC ultrahigh-temperature ceramic-based composite material |
| CN104529459A (en) * | 2014-12-03 | 2015-04-22 | 武汉理工大学 | B4C-HfB2-SiC ternary high-temperature eutectic composite ceramic material and preparation method |
| US9061947B1 (en) * | 2009-11-02 | 2015-06-23 | Lockheed Martin Corporation | Multiphase eutectic ceramic coatings |
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2017
- 2017-12-08 CN CN201711302894.XA patent/CN107879745B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0385509B1 (en) * | 1989-03-03 | 1994-01-05 | Toray Industries, Inc. | Process for producing ceramic composites |
| JPH0497952A (en) * | 1990-08-09 | 1992-03-30 | Eagle Ind Co Ltd | Silicon carbide-based composite body |
| CN101113096A (en) * | 2006-07-28 | 2008-01-30 | 通用电气公司 | Presintering process for reducing inequality in density of sintered material |
| US9061947B1 (en) * | 2009-11-02 | 2015-06-23 | Lockheed Martin Corporation | Multiphase eutectic ceramic coatings |
| CN103979974A (en) * | 2014-05-14 | 2014-08-13 | 西北工业大学 | Preparation method of C/SiC-HfB2-HfC ultrahigh-temperature ceramic-based composite material |
| CN104529459A (en) * | 2014-12-03 | 2015-04-22 | 武汉理工大学 | B4C-HfB2-SiC ternary high-temperature eutectic composite ceramic material and preparation method |
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