CN114105646A - Preparation method of in-situ SiC-BN (C) -Ti (C, N) nanocrystalline complex phase ceramic - Google Patents
Preparation method of in-situ SiC-BN (C) -Ti (C, N) nanocrystalline complex phase ceramic Download PDFInfo
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Abstract
A preparation method of in-situ SiC-BN (C) -Ti (C, N) nanocrystalline complex phase ceramic relates to a mechanical alloying combined reaction hot pressing sintering technology. The method aims to solve the problem that the mechanical property, reliability and damage resistance of the existing ceramic material are deteriorated due to the addition of a lubricating phase in the preparation of the ceramic material. The method comprises the following steps: H-BN powder, graphite, cubic silicon powder and Ti powder are ball-milled to prepare SiBCN-xwt% Ti powder, and hot pressed and sintered. The method 2 comprises the following steps: preparing NB21 mixed powder, adding cubic silicon powder, h-BN powder and graphite to obtain SiBCN-xwt% NB21 powder, and carrying out hot-pressing sintering in a furnace. The method 3 comprises the following steps: TiN and TiB2Adding cubic silicon powder, h-BN powder and graphite after ball milling, continuously ball milling to obtain amorphous/nanocrystalline composite powder, and carrying out hot-pressing sintering in a furnace. By mechanical alloyingThe hot-pressing sintering technology is used for preparing ceramics with excellent mechanical and tribological properties and high-temperature oxidation resistance; is suitable for preparing nanocrystalline complex phase ceramics.
Description
Technical Field
The invention relates to a mechanical alloying combined reaction hot-pressing sintering technology, in particular to a preparation method of in-situ SiC-BN (C) -Ti (C, N) nanocrystalline complex phase ceramic.
Background
The SiC-based ceramic material has been widely used in the field of high-temperature friction due to its high toughness, superior high-temperature oxidation resistance, excellent friction and wear resistance, good creep resistance, ablation resistance, thermal shock resistance and the like. However, when the ceramic material is used at the temperature of more than 1500 ℃ for a long time, the high-temperature strength, the thermal stability and the oxidation resistance of the material are reduced sharply, and the friction coefficient and the wear rate under the dry friction condition are larger. Therefore, the research and preparation of the high-temperature-resistant structure/lubricating function integrated material which can be used for a long time at the temperature of more than 1500 ℃ is one of the urgent requirements of the development of the modern aerospace technology. The problems encountered in practical engineering are that the addition of the lubricating phase damages the continuity and uniformity of the ceramic phase to cause the deterioration of mechanical properties thereof, and the deterioration of reliability and damage resistance causes the failure to meet the practical requirements of applications in the high-tech field. Ti (C, N) has the characteristics of high melting point, high hardness, good corrosion resistance and oxidation resistance and the like, is widely applied to the fields of structural materials and friction, and graphite and boron nitride also have the advantages of small friction coefficient and the like and are used as common lubricants.
Disclosure of Invention
The invention aims to solve the problem that the mechanical property, reliability and damage resistance of the existing ceramic material are deteriorated due to the addition of a lubricating phase in the preparation of the ceramic material, and provides a preparation method of in-situ SiC-BN (C) -Ti (C, N) nanocrystalline complex phase ceramic.
The preparation method of the in-situ SiC-BN (C) -Ti (C, N) nanocrystalline complex phase ceramic is realized by the following steps:
firstly, weighing h-BN powder, amorphous graphite and cubic silicon powder according to the molar ratio of 1 (1-4) to 2; then weighing Ti powder according to SiBCN-xwt% Ti, wherein x is 0.1-30;
secondly, ball-milling the weighed h-BN powder, amorphous graphite, cubic silicon powder and Ti powder in a high-energy ball mill for 20-30 hours to obtain SiBCN-xwt% Ti composite powder;
and thirdly, placing the SiBCN-xwt% Ti composite powder in a hot-pressing sintering furnace, performing reaction sintering under the protection of nitrogen, wherein the sintering temperature is 1800-2000 ℃, the sintering pressure is 40-80 MPa, the heat preservation time is 30-60 min, then cooling to 1200 ℃ at the speed of 20K/min, and then cooling along with the furnace to complete the preparation of the in-situ SiC-BN (C) -Ti (C, N) nanocrystalline composite ceramic.
The preparation method of the in-situ SiC-BN (C) -Ti (C, N) nanocrystalline complex phase ceramic can be realized by the following steps:
firstly, weighing Ti powder and boron nitride powder according to a molar ratio of 3:2, and then ball-milling for 30 hours in a high-energy ball mill to obtain NB21 mixed powder;
weighing cubic silicon powder, h-BN powder and amorphous graphite according to the molar ratio of 2:3: 1; then weighing the mixed powder of NB21 according to SiBCN-xwt% NB21, wherein x is 0.1-30;
thirdly, ball-milling the weighed mixed powder of the cubic silicon powder, the h-BN powder, the amorphous graphite and the NB21 in a high-energy ball mill for 20-24 hours to obtain SiBCN-xwt% NB21 composite powder;
fourthly, placing the SiBCN-xwt% NB21 composite powder in a hot-pressing sintering furnace, performing reaction sintering under the protection of nitrogen, wherein the sintering temperature is 1700-2000 ℃, the sintering pressure is 60-80 MPa, the heat preservation time is 30-120 min, then cooling to 1200 ℃ at the speed of 20K/min, and then cooling along with the furnace to obtain the SiC-BN (C) -Ti (C, N) nanocrystalline composite ceramic, namely completing the preparation of the in-situ SiC-BN (C) -Ti (C, N) nanocrystalline composite ceramic.
The preparation method of the in-situ SiC-BN (C) -Ti (C, N) nanocrystalline complex phase ceramic can be realized by the following steps:
firstly, weighing hard TiN and TiB according to the molar ratio of 2:12Then ball-milling for 30h in a high-energy ball mill to obtain mixed powder;
weighing cubic silicon powder, h-BN powder and amorphous graphite according to the molar ratio of 2:1:3 to obtain a substance A, adding the substance A into the mixed powder obtained in the step one according to the mass ratio, and then carrying out ball milling in a high-energy ball mill for 20 hours to obtain amorphous/nanocrystalline composite powder; the mass ratio of the mixed powder to the substance A is (70-95) to (5-30);
and thirdly, placing the amorphous/nanocrystalline composite powder in a hot-pressing sintering furnace, performing reactive sintering under the protection of nitrogen, wherein the sintering temperature is 1900 ℃, the sintering pressure is 60-80 MPa, the heat preservation time is 30-60 min, then cooling to 1200 ℃ at the speed of 20K/min, and then cooling along with the furnace, thus completing the preparation of the in-situ SiC-BN (C) -Ti (C, N) nanocrystalline composite ceramic.
The invention adopts a mechanical alloying technology, can prepare SiC-based ceramic materials with different components and different micro-nano tissue structures by changing the raw materials and the molar ratio thereof, and provides possibility for preparing nanocrystalline complex phase ceramic materials with special purposes or excellent performance.
The invention adopts a mechanical alloying combined hot-pressing sintering technology to prepare SiC-BN (C) -Ti (C, N) nanocrystalline complex phase ceramic with excellent mechanical and tribological properties and high-temperature oxidation resistance, the prepared special tissue structure with a turbulent layer-shaped amorphous nanocrystalline BN (C) phase wrapping nanocrystalline SiC and Ti (C, N) phase crystal grains can prevent the abnormal growth of the SiC and Ti (C, N) phase crystal grains, the bending strength of the prepared composite ceramic reaches 210-394 MPa, the elastic modulus is 150-185 GPa, the Vickers hardness is 1.5-4.7 GPa, and the fracture toughness reaches 3-3.95 GPa cm1/2The bulk density is 2.85g/cm3The problems that the mechanical property is poor due to the fact that the continuity and the uniformity of the ceramic phase are damaged by adding the lubricating phase, and the application in the high technical field cannot be met due to the fact that the reliability and the damage resistance are poor are solved.
The method is suitable for preparing the in-situ SiC-BN (C) -Ti (C, N) nanocrystalline complex phase ceramic.
Drawings
FIG. 1 is an SEM image of a SiBCN-15 wt% Ti composite powder in example 1;
FIG. 2 is a partially enlarged view of a SiBCN-15 wt% Ti composite powder in example 1;
FIG. 3 is a TEM (see part a) and HTEM (see parts b and c) of SiBCN-15 wt% Ti composite powder in example 1;
FIG. 4 is a sectional view of the element plane of bulk ceramic of the in-situ SiC-BN (C) -Ti (C, N) nanocrystalline composite ceramic of example 1, wherein a represents HAADF; b to h represent corresponding Si, B, C, N, Ti and O element distribution maps;
FIG. 5 is a ball-milling XRD pattern of Ti powder and boron nitride powder in example 2;
FIG. 6 is an XRD pattern of the SiC-BN (C) -Ti (C, N) nanocrystalline complex phase ceramic of example 2;
FIG. 7 is a TEM analysis of the SiC-BN (C) -Ti (C, N) nanocrystalline complex phase ceramic of example 2, wherein a represents the bright field image morphology, b represents the STEM morphology, and C and d represent the corresponding HRTEM images;
FIG. 8 is a block ceramic diffraction ring diagram of the SiC-BN (C) -Ti (C, N) nanocrystalline composite ceramic of example 2;
FIG. 9 is a graph showing the mechanical properties of the SiC-BN (C) -Ti (C, N) nanocrystalline composite ceramic of example 2, wherein a represents flexural strength, b represents fracture toughness, C represents Vickers hardness, and d represents elastic modulus;
FIG. 10 is a crack propagation diagram of the SiC-BN (C) -Ti (C, N) nanocrystalline composite ceramic of example 3.
Detailed Description
The technical solution of the present invention is not limited to the following specific embodiments, but includes any combination of the specific embodiments.
The first embodiment is as follows: the preparation method of the in-situ SiC-BN (C) -Ti (C, N) nanocrystalline composite ceramic of the embodiment is realized by the following steps:
firstly, weighing h-BN powder, amorphous graphite and cubic silicon powder according to the molar ratio of 1 (1-4) to 2; then weighing Ti powder according to SiBCN-xwt% Ti, wherein x is 0.1-30;
secondly, ball-milling the weighed h-BN powder, amorphous graphite, cubic silicon powder and Ti powder in a high-energy ball mill for 20-30 hours to obtain SiBCN-xwt% Ti composite powder;
and thirdly, placing the SiBCN-xwt% Ti composite powder in a hot-pressing sintering furnace, performing reaction sintering under the protection of nitrogen, wherein the sintering temperature is 1800-2000 ℃, the sintering pressure is 40-80 MPa, the heat preservation time is 30-60 min, then cooling to 1200 ℃ at the speed of 20K/min, and then cooling along with the furnace to complete the preparation of the in-situ SiC-BN (C) -Ti (C, N) nanocrystalline composite ceramic.
In the embodiment, the h-BN powder, the amorphous graphite, the cubic silicon powder and the Ti powder are subjected to full solid-state amorphization after ball milling, and the whole process is carried out under the protection of high-purity argon, so that the five component elements are fully mixed at the atomic scale to reach an amorphous state.
The second embodiment is as follows: the difference between the first embodiment and the second embodiment is that the h-BN powder, the amorphous graphite and the cubic silicon powder are weighed according to the molar ratio of 1:3:2 in the first step. Other steps and parameters are the same as those in the first embodiment.
The third concrete implementation mode: the difference between the embodiment and the first or second embodiment is that in the second step, silicon nitride grinding balls with the grain diameter of 1.85cm are adopted for ball milling, the ball-material ratio is 20:1, the rotating speed of a main disc is 350r/min, the rotating speed of a planetary disc is 700r/min, and the ball mill has a rest for 10min every 50 min. Other steps and parameters are the same as those in the first or second embodiment.
The fourth concrete implementation mode: the difference between the present embodiment and one of the first to third embodiments is that, in the third step, when the sintering temperature is less than 1200 ℃, the temperature rising speed is 25K/min; when the sintering temperature is higher than 1200 ℃, the heating rate is 20K/min. Other steps and parameters are the same as those in one of the first to third embodiments.
The fifth concrete implementation mode: the preparation method of the in-situ SiC-BN (C) -Ti (C, N) nanocrystalline composite ceramic in the embodiment can be realized by the following steps:
firstly, weighing Ti powder and boron nitride powder according to a molar ratio of 3:2, and then ball-milling for 30 hours in a high-energy ball mill to obtain NB21 mixed powder;
weighing cubic silicon powder, h-BN powder and amorphous graphite according to the molar ratio of 2:3: 1; then weighing the mixed powder of NB21 according to SiBCN-xwt% NB21, wherein x is 0.1-30;
thirdly, ball-milling the weighed mixed powder of the cubic silicon powder, the h-BN powder, the amorphous graphite and the NB21 in a high-energy ball mill for 20-24 hours to obtain SiBCN-xwt% NB21 composite powder;
fourthly, placing the SiBCN-xwt% NB21 composite powder in a hot-pressing sintering furnace, performing reaction sintering under the protection of nitrogen, wherein the sintering temperature is 1700-2000 ℃, the sintering pressure is 60-80 MPa, the heat preservation time is 30-120 min, then cooling to 1200 ℃ at the speed of 20K/min, and then cooling along with the furnace to obtain the SiC-BN (C) -Ti (C, N) nanocrystalline composite ceramic, namely completing the preparation of the in-situ SiC-BN (C) -Ti (C, N) nanocrystalline composite ceramic.
The sixth specific implementation mode: the difference between the embodiment and the fifth embodiment is that silicon nitride grinding balls with the particle size of 1.85cm are adopted for ball milling in the first step and the third step, the ball-material ratio is 20:1, the rotating speed of a main disc is 350r/min, the rotating speed of a planetary disc is 700r/min, and the ball mill has a rest for 10min every 50min of operation. The other steps and parameters are the same as those in the fifth embodiment.
The seventh embodiment: the difference between the fifth embodiment and the sixth embodiment is that in the fourth step, when the sintering temperature is less than 1200 ℃, the temperature rise speed is 25K/min; when the sintering temperature is higher than 1200 ℃, the heating rate is 20K/min. Other steps and parameters are the same as in one of the fifth or sixth embodiments.
The specific implementation mode is eight: the preparation method of the in-situ SiC-BN (C) -Ti (C, N) nanocrystalline composite ceramic in the embodiment can be realized by the following steps:
firstly, weighing hard TiN and TiB according to the molar ratio of 2:12Then ball-milling for 30h in a high-energy ball mill to obtain mixed powder;
weighing cubic silicon powder, h-BN powder and amorphous graphite according to the molar ratio of 2:1:3 to obtain a substance A, adding the substance A into the mixed powder obtained in the step one according to the mass ratio, and then carrying out ball milling in a high-energy ball mill for 20 hours to obtain amorphous/nanocrystalline composite powder; the mass ratio of the mixed powder to the substance A is (70-95) to (5-30);
and thirdly, placing the amorphous/nanocrystalline composite powder in a hot-pressing sintering furnace, performing reactive sintering under the protection of nitrogen, wherein the sintering temperature is 1900 ℃, the sintering pressure is 60-80 MPa, the heat preservation time is 30-60 min, then cooling to 1200 ℃ at the speed of 20K/min, and then cooling along with the furnace, thus completing the preparation of the in-situ SiC-BN (C) -Ti (C, N) nanocrystalline composite ceramic.
The specific implementation method nine: the difference between the embodiment and the eighth embodiment is that silicon nitride grinding balls with the particle size of 1.85cm are adopted for ball milling in the first step and the second step, the ball-material ratio is 20:1, the rotating speed of a main disc is 350r/min, the rotating speed of a planetary disc is 700r/min, and the ball mill has a rest for 10min every 50 min. The other steps and parameters are the same as those in the eighth embodiment.
The detailed implementation mode is ten: the difference between the present embodiment and the eighth or ninth embodiment is that the mass ratio of the mixed powder to the substance a in the second step is 80: 20. Other steps and parameters are the same as those in the eighth or ninth embodiment.
The concrete implementation mode eleven: the eighth embodiment is different from the eighth embodiment to the tenth embodiment in that, in the third step, when the sintering temperature is less than 1200 ℃, the temperature rise speed is 25K/min; when the sintering temperature is higher than 1200 ℃, the heating rate is 20K/min. Other steps and parameters are the same as those in one of the eighth to the tenth embodiments.
The beneficial effects of the present invention are demonstrated by the following examples:
example 1:
the preparation method of the in-situ SiC-BN (C) -Ti (C, N) nanocrystalline complex phase ceramic is realized by the following steps:
firstly, weighing h-BN powder, amorphous graphite and cubic silicon powder according to a molar ratio of 1:3: 2; then weighing Ti powder according to SiBCN-xwt% Ti, wherein x is 15;
secondly, ball-milling the weighed h-BN powder, amorphous graphite, cubic silicon powder and Ti powder in a high-energy ball mill for 20 hours to obtain SiBCN-15 wt% Ti composite powder;
and thirdly, placing the SiBCN-15 wt% Ti composite powder in a hot-pressing sintering furnace, performing reaction sintering under the protection of nitrogen, wherein the sintering temperature is 1800-2000 ℃, the sintering pressure is 40-80 MPa, the heat preservation time is 30-60 min, then cooling to 1200 ℃ at the speed of 20K/min, and then cooling along with the furnace to complete the preparation of the in-situ SiC-BN (C) -Ti (C, N) nanocrystalline composite ceramic.
In the second step of this embodiment, silicon nitride grinding balls with a particle size of 1.85cm are used for ball milling, the ball-to-material ratio is 20:1, the rotation speed of the main disc is 350r/min, the rotation speed of the planetary disc is 700r/min, and the ball mill has a rest for 10min every 50 min.
In the third step of this embodiment, when the sintering temperature is less than 1200 ℃, the temperature rising speed is 25K/min; when the sintering temperature is higher than 1200 ℃, the heating rate is 20K/min.
In the SEM picture (shown in figure 1) and the partial enlarged picture (shown in figure 2) of the SiBCN-15 wt% Ti composite powder prepared in the embodiment, the size of the composite powder particles is 50-200 nm, and the hard agglomeration phenomenon of the powder due to the welding action can be obviously found; TEM (see part a in FIG. 3) and HTEM (see part b and part c in FIG. 3) of SiBCN-15 wt% Ti composite powder, and TEM observation of the composite powder shows that larger particles are also present in the composite powder, and the particles are formed by agglomeration of smaller powder particles. FIG. 3(a) is an HRTEM of the powder, and after a large amount of HRTEM observation of the powder, the powder particles are basically amorphized, only a few Ti (C, N) nanocrystals exist, and the nanocrystal size is 6-10 nm.
The bulk ceramic element surface of the in-situ SiC-BN (C) -Ti (C, N) nanocrystalline composite ceramic obtained in the embodiment is divided into sections, which can be seen in a part A of HAADF in FIG. 4; the distribution of Si, B, C, N, Ti and O elements in the sections B to h of FIG. 4 shows that the elements are uniformly distributed in the composite material.
Example 2:
the preparation method of the in-situ SiC-BN (C) -Ti (C, N) nanocrystalline complex phase ceramic is realized by the following steps:
firstly, weighing Ti powder and boron nitride powder according to a molar ratio of 3:2, and then ball-milling for 30 hours in a high-energy ball mill to obtain NB21 mixed powder;
weighing cubic silicon powder, h-BN powder and amorphous graphite according to the molar ratio of 2:3: 1; then weighing the mixed powder of NB21 according to SiBCN-xwt% NB21, wherein x is 15;
thirdly, ball-milling the weighed mixed powder of the cubic silicon powder, the h-BN powder, the amorphous graphite and the NB21 in a high-energy ball mill for 20 hours to obtain SiBCN-15 wt% NB21 composite powder;
fourthly, placing the SiBCN-15 wt% NB21 composite powder in a hot-pressing sintering furnace, carrying out reaction sintering under the protection of nitrogen, wherein the sintering temperature is 1700 ℃, the sintering pressure is 70MPa, the heat preservation time is 60min, then cooling to 1200 ℃ at the speed of 20K/min, and then cooling along with the furnace to obtain the SiC-BN (C) -Ti (C, N) nanocrystalline composite ceramic, namely completing the preparation of the in-situ SiC-BN (C) -Ti (C, N) nanocrystalline composite ceramic.
In the first step and the third step of the present embodiment, silicon nitride grinding balls with a particle size of 1.85cm are adopted for ball milling, the ball-material ratio is 20:1, the rotation speed of the main disc is 350r/min, the rotation speed of the planetary disc is 700r/min, and the ball mill has a rest of 10min every 50 min.
In the fourth step of this example, when the sintering temperature is less than 1200 ℃, the temperature rise rate is 25K/min; when the sintering temperature is higher than 1200 ℃, the heating rate is 20K/min.
In the ball milling XRD patterns of Ti powder and boron nitride powder in the first step of this example, it can be seen from fig. 5 that the BN peak substantially disappears after about 1 hour, the Ti peak gradually disappears, and a steamed bun-like amorphous peak is finally formed after 30 hours of high-energy ball milling.
The XRD spectrum (see fig. 6) of the obtained SiC-BN (C) -Ti (C, N) nanocrystalline composite ceramic in this example shows that after hot press sintering, the ceramic mainly consists of SiC, BN (C) and Ti (C, N), and the content of Ti (C, N) phase increases gradually with the increase of Ti content.
TEM analysis of the SiC-BN (C) -Ti (C, N) nanocrystalline composite ceramic obtained in the embodiment is respectively shown in a part of bright field image morphology in FIG. 7 a; fig. 7 b is a STEM profile; HRTEM corresponding to sections c and d in fig. 7; from fig. 7, it is evident that there are lamellar bn (C) phases with a grain size of 20-100 nm, the bn (C) phase contains many stacking faults and many atomic dislocation rows are observed at high resolution, the turbulent lamellar bn (C) phase wraps the Ti (C, N) phase and the SiC phase, and this special structure can prevent abnormal growth of Ti (C, N) phase and SiC phase particles, so that the composite material has excellent mechanical and oxidation resistance properties; ti (C, N) phase is uniformly distributed in the composite material, and the grain size of the Ti (C, N) phase is about 30 nm; the SiC crystal grain size is also small, about 30nm, and it can be observed from fig. 7 that a stacking fault exists on the SiC crystal grain.
The diffraction rings of the bulk ceramic of the SiC-bn (C) -Ti (C, N) nanocrystalline composite ceramic obtained in this example are shown in fig. 8, and fig. 8 is a series of diffraction rings obtained by selective electron diffraction of the portion b in fig. 7, which indicates that the grain size of the composite material is fine and is nanocrystalline, and some of the rings are differentiated, indicating that some grains begin to develop to coarsen.
The mechanical properties of the SiC-BN (C) -Ti (C, N) nanocrystalline multiphase ceramic obtained in the example can be seen from the graph in FIG. 9(a, b, C and d), the bending strength reaches 394MPa, the elastic modulus reaches 178.3GPa, the Vickers hardness reaches 4.7GPa, and the fracture toughness reaches 3.95GPa cm1/2The bulk density is 2.85g/cm3(ii) a The composite material has excellent mechanical properties, and the introduction of the nanocrystalline can effectively improve the mechanical properties of the SiBCN ceramic.
Example 3:
the preparation method of the in-situ SiC-BN (C) -Ti (C, N) nanocrystalline complex phase ceramic can be realized by the following steps:
firstly, weighing hard TiN and TiB according to the molar ratio of 2:12Then ball-milling for 30h in a high-energy ball mill to obtain mixed powder;
weighing cubic silicon powder, h-BN powder and amorphous graphite according to the molar ratio of 2:1:3 to obtain a substance A, adding the substance A into the mixed powder obtained in the step one according to the mass ratio, and then carrying out ball milling in a high-energy ball mill for 20 hours to obtain amorphous/nanocrystalline composite powder; the mass ratio of the mixed powder to the substance A is 80: 20;
and thirdly, placing the amorphous/nanocrystalline composite powder in a hot-pressing sintering furnace, performing reactive sintering under the protection of nitrogen, wherein the sintering temperature is 1900 ℃, the sintering pressure is 60-80 MPa, the heat preservation time is 30-60 min, then cooling to 1200 ℃ at the speed of 20K/min, and then cooling along with the furnace, thus completing the preparation of the in-situ SiC-BN (C) -Ti (C, N) nanocrystalline composite ceramic.
In the first step and the second step of the present embodiment, silicon nitride grinding balls with a particle size of 1.85cm are adopted for ball milling, the ball-material ratio is 20:1, the rotation speed of the main disc is 350r/min, the rotation speed of the planetary disc is 700r/min, and the ball mill has a rest for 10min every 50 min.
In the third step of this embodiment, when the sintering temperature is less than 1200 ℃, the temperature rising speed is 25K/min; when the sintering temperature is higher than 1200 ℃, the heating rate is 20K/min.
The crack propagation pattern of the SiC-BN (C) -Ti (C, N) nanocrystalline composite ceramic obtained in the embodiment can show the deflection of the crack from figure 10, which shows that the fine crystal grains in the composite material enhance the toughness of the composite material and are beneficial to improving the mechanical property of the composite material.
Claims (10)
1. The preparation method of the in-situ SiC-BN (C) -Ti (C, N) nanocrystalline complex phase ceramic is characterized by comprising the following steps:
firstly, weighing h-BN powder, amorphous graphite and cubic silicon powder according to the molar ratio of 1 (1-4) to 2; then weighing Ti powder according to SiBCN-xwt% Ti, wherein x is 0.1-30;
secondly, ball-milling the weighed h-BN powder, amorphous graphite, cubic silicon powder and Ti powder in a high-energy ball mill for 20-30 hours to obtain SiBCN-xwt% Ti composite powder;
and thirdly, placing the SiBCN-xwt% Ti composite powder in a hot-pressing sintering furnace, performing reaction sintering under the protection of nitrogen, wherein the sintering temperature is 1800-2000 ℃, the sintering pressure is 40-80 MPa, the heat preservation time is 30-60 min, then cooling to 1200 ℃ at the speed of 20K/min, and then cooling along with the furnace to complete the preparation of the in-situ SiC-BN (C) -Ti (C, N) nanocrystalline composite ceramic.
2. The method for preparing the in-situ SiC-BN (C) -Ti (C, N) nanocrystalline multiphase ceramic according to claim 1, wherein in the step one, h-BN powder, amorphous graphite and cubic silicon powder are weighed according to a molar ratio of 1:3: 2.
3. The method for preparing in-situ SiC-BN (C) -Ti (C, N) nanocrystalline composite ceramic according to claim 1, wherein in the second step, silicon nitride grinding balls with the grain diameter of 1.85cm are adopted for the ball milling, the ball-material ratio is 20:1, the rotating speed of a main disc is 350r/min, the rotating speed of a planetary disc is 700r/min, and the ball mill is rested for 10min every 50 min.
4. The method for preparing in-situ SiC-BN (C) -Ti (C, N) nanocrystalline composite ceramic according to claim 1, characterized in that in the third step, when the sintering temperature is less than 1200 ℃, the heating rate is 25K/min; when the sintering temperature is higher than 1200 ℃, the heating rate is 20K/min.
5. The preparation method of the in-situ SiC-BN (C) -Ti (C, N) nanocrystalline complex phase ceramic is characterized by comprising the following steps:
firstly, weighing Ti powder and boron nitride powder according to a molar ratio of 3:2, and then ball-milling for 30 hours in a high-energy ball mill to obtain NB21 mixed powder;
weighing cubic silicon powder, h-BN powder and amorphous graphite according to the molar ratio of 2:3: 1; then weighing the mixed powder of NB21 according to SiBCN-xwt% NB21, wherein x is 0.1-30;
thirdly, ball-milling the weighed mixed powder of the cubic silicon powder, the h-BN powder, the amorphous graphite and the NB21 in a high-energy ball mill for 20-24 hours to obtain SiBCN-xwt% NB21 composite powder;
fourthly, placing the SiBCN-xwt% NB21 composite powder in a hot-pressing sintering furnace, performing reaction sintering under the protection of nitrogen, wherein the sintering temperature is 1700-2000 ℃, the sintering pressure is 60-80 MPa, the heat preservation time is 30-120 min, then cooling to 1200 ℃ at the speed of 20K/min, and then cooling along with the furnace to obtain the SiC-BN (C) -Ti (C, N) nanocrystalline composite ceramic, namely completing the preparation of the in-situ SiC-BN (C) -Ti (C, N) nanocrystalline composite ceramic.
6. The method for preparing in-situ SiC-BN (C) -Ti (C, N) nanocrystalline multiphase ceramic according to claim 5, wherein in the first and third steps, silicon nitride grinding balls with the grain diameter of 1.85cm are adopted for ball milling, the ball-material ratio is 20:1, the rotating speed of a main disc is 350r/min, the rotating speed of a planetary disc is 700r/min, and the ball mill is rested for 10min every 50 min.
7. The method for preparing in-situ SiC-BN (C) -Ti (C, N) nanocrystalline composite ceramic according to claim 5, characterized in that in the fourth step, when the sintering temperature is less than 1200 ℃, the heating rate is 25K/min; when the sintering temperature is higher than 1200 ℃, the heating rate is 20K/min.
8. The preparation method of the in-situ SiC-BN (C) -Ti (C, N) nanocrystalline complex phase ceramic is characterized by comprising the following steps:
firstly, weighing hard TiN and TiB according to the molar ratio of 2:12Then ball-milling for 30h in a high-energy ball mill to obtainMixing the powder with the mixture;
weighing cubic silicon powder, h-BN powder and amorphous graphite according to the molar ratio of 2:1:3 to obtain a substance A, adding the substance A into the mixed powder obtained in the step one according to the mass ratio, and then carrying out ball milling in a high-energy ball mill for 20 hours to obtain amorphous/nanocrystalline composite powder; the mass ratio of the mixed powder to the substance A is (70-95) to (5-30);
and thirdly, placing the amorphous/nanocrystalline composite powder in a hot-pressing sintering furnace, performing reactive sintering under the protection of nitrogen, wherein the sintering temperature is 1900 ℃, the sintering pressure is 60-80 MPa, the heat preservation time is 30-60 min, then cooling to 1200 ℃ at the speed of 20K/min, and then cooling along with the furnace, thus completing the preparation of the in-situ SiC-BN (C) -Ti (C, N) nanocrystalline composite ceramic.
9. The method for preparing in-situ SiC-BN (C) -Ti (C, N) nanocrystalline composite ceramic according to claim 8, wherein the mass ratio of the mixed powder to the A substance in the second step is 80: 20.
10. The method for preparing in-situ SiC-BN (C) -Ti (C, N) nanocrystalline composite ceramic according to claim 8, characterized in that in the third step, when the sintering temperature is less than 1200 ℃, the heating rate is 25K/min; when the sintering temperature is higher than 1200 ℃, the heating rate is 20K/min.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116023150A (en) * | 2023-01-19 | 2023-04-28 | 天津大学 | High-temperature-resistant transition metal carbide (nitride)/silicon-boron-carbon-nitrogen composite ceramic aerogel and preparation method thereof |
| CN116693303A (en) * | 2023-03-31 | 2023-09-05 | 江苏东浦精细陶瓷科技股份有限公司 | TiN-Si 3 N 4 Near net shape forming method for composite material |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1056859A (en) * | 1990-05-30 | 1991-12-11 | 中国建筑材料科学研究院高技术陶瓷研究所 | Titanium carbonitride-titanium boride ceramics is made in reaction hot-pressing |
| CN101367511A (en) * | 2008-08-06 | 2009-02-18 | 燕山大学 | Method for preparing non-stoichiometry ratio nano TiNx with reaction ball milling method |
| CN101445370A (en) * | 2008-12-24 | 2009-06-03 | 哈尔滨工业大学 | Method for preparing TiN/TiB2 composite material |
| CN101870586A (en) * | 2010-07-07 | 2010-10-27 | 哈尔滨工业大学 | Amorphous and nanocrystalline Si-B-C-N ceramic composite material and preparation method thereof |
-
2021
- 2021-12-20 CN CN202111562121.1A patent/CN114105646B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1056859A (en) * | 1990-05-30 | 1991-12-11 | 中国建筑材料科学研究院高技术陶瓷研究所 | Titanium carbonitride-titanium boride ceramics is made in reaction hot-pressing |
| CN101367511A (en) * | 2008-08-06 | 2009-02-18 | 燕山大学 | Method for preparing non-stoichiometry ratio nano TiNx with reaction ball milling method |
| CN101445370A (en) * | 2008-12-24 | 2009-06-03 | 哈尔滨工业大学 | Method for preparing TiN/TiB2 composite material |
| CN101870586A (en) * | 2010-07-07 | 2010-10-27 | 哈尔滨工业大学 | Amorphous and nanocrystalline Si-B-C-N ceramic composite material and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 张聪: "碳氮化法合成Si-B-C-N和Si-Ti-C-N复合陶瓷粉末的研究", 《中国优秀博硕士学位论文全文数据库(硕士)工程科技Ⅰ辑》 * |
| 李建林等: "高能球磨过程中Ti与BN的反应", 《金属学报》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116023150A (en) * | 2023-01-19 | 2023-04-28 | 天津大学 | High-temperature-resistant transition metal carbide (nitride)/silicon-boron-carbon-nitrogen composite ceramic aerogel and preparation method thereof |
| CN116023150B (en) * | 2023-01-19 | 2024-01-23 | 天津大学 | High-temperature-resistant transition metal carbide (nitride)/silicon-boron-carbon-nitrogen composite ceramic aerogel and preparation method thereof |
| CN116693303A (en) * | 2023-03-31 | 2023-09-05 | 江苏东浦精细陶瓷科技股份有限公司 | TiN-Si 3 N 4 Near net shape forming method for composite material |
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