CN103145422B - High-hardness ceramic composite material of boron carbide-titanium boride-silicon carbide and preparation method thereof - Google Patents
High-hardness ceramic composite material of boron carbide-titanium boride-silicon carbide and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a high-hardness ceramic composite material of boron carbide-titanium boride-silicon carbide and a preparation method thereof, and belongs to the technical field of a ceramic material. The composite ceramic is prepared from boron carbide, silicon carbide and silicon powder in a hot-pressing sintering manner via reaction. The composite ceramic contains 50-90wt% of boron carbide, 27-5.4wt% of titanium boride and 23-4.6wt% of silicon carbide. The defects of overhigh sintering temperature, and difficulty of improvement of the toughness and the hardness at the same time of the existing boron carbide ceramic are solved; carbon generated by reaction of the boron carbide and the titanium boride is removed by monatomic silicon; and the carbon for reducing the hardness of the base material is converted into hard material silicon carbide which is evenly dispersed, so as to play roles in enhancing the toughness and improving the material hardness. The high-toughness boron carbide composite ceramic can be prepared at low temperature on the premise of not reducing the hardness of a base body.
Description
Technical field
The present invention relates to a kind of ceramic composite and preparation method thereof, relate in particular to high hard ceramic composite of a kind of norbide-titanium boride-silicon carbide and preparation method thereof.
Background technology
Norbide is a kind of superhard material, and its hardness is only second to diamond and cubic boron nitride.In addition, norbide has high-melting-point, low density, excellent wear resistance, fabulous chemical stability and high neutron-absorbing ability, and its application spreads all over nuclear industry, armor facing, the fields such as aviation.But high sintering temperature and low fracture toughness property have had a strong impact on further developing of norbide.In order to address these problems, conventional method is in norbide matrix, to add second-phase material to play the object that reduces sintering temperature and improve toughness.At present, study morely, the good method of effect is in norbide matrix, to introduce titanium boride by reaction sintering.Research shows, adds titanium carbide in norbide, both can utilize the chemical reaction between them to generate non-stoichiometric B
4c
1-xcause the change of norbide lattice parameter, produce textural defect, thereby Accelerative mass transfer process, promote sintering densification, reach the object that reduces sintering temperature, can utilize again the thermal expansivity of reaction product titanium boride do not mate with matrix norbide and produce the tiny crack deflecting effect that unrelieved stress causes, improve the fracture toughness property of norbide.
As adopting, Chinese scholar Tang Jun etc. and foreign scholar L.S.Sigl in norbide, add the method for titanium carbide reaction sintering to prepare norbide-titanium boride composite ceramics of high tenacity.Wherein, Tang Jun etc. are at 2050 ℃, TiB in norbide-titanium boride composite ceramics of preparing under the hot pressing condition of 35MPa
2the particle diameter of particle is generally below 3 μ m; Add 20vol% TiC (corresponding TiB
2for 35vol%) the Fracture Toughness of complex phase ceramic up to 6.3MPam
1/2, compare monomers B
4c improves 75%.But in their research, the carbon that reaction generates is not reasonably processed, and is still present in matrix.Unnecessary carbon can significantly reduce the hardness of matrix, so the hardness of its material only has 21GPa.Therefore, although aforesaid method has reduced sintering temperature and the toughness that has increased material to a certain extent, sacrifice the hardness of material, there is no really to solve the toughness reinforcing problem of high-hardness ceramic.
And for example Chinese scholar Lee likes that the people such as chrysanthemum are with B
4c and Si
3n
4with a small amount of SiC, TiC is raw material, Al
2o
3and Y
2o
3for sintering aid, be 1800-1880 ℃ in sintering temperature, under the hot pressing condition that pressure is 30MP, prepare the ceramic composite take norbide-titanium boride-silicon carbide as principal phase, its fracture toughness property can reach 5.6 MPam
1/2.But the method is used raw material more, reaction process complexity between raw material, centre is mutually various, is difficult to obtain high-purity tri compound pottery.In addition, due to Al
2o
3, Y
2o
3etc. adding of low temperature liquid phase sintering agent, the hardness of material and high-temperature mechanical property are reduced, thereby reduce the use range of material, reduce reliability of material.
Summary of the invention
The shortcoming that the present invention is directed to that existing boron carbide base composite ceramic material sintering temperature is too high, hardness and toughness is difficult to improve simultaneously and high hard ceramic composite of a kind of norbide-titanium boride-silicon carbide and preparation method thereof is provided.The method technique is simple, can at lower temperature, make the high hard ceramic composite of norbide-titanium boride-silicon carbide that toughness and hardness are taken into account.
In order to reach above object, the present invention takes following technical scheme to be achieved:
The high hard ceramic composite of a kind of norbide-titanium boride-silicon carbide, by weight percentage, it is by norbide 50%-90%, titanium boride 27%-5.4%, silicon carbide 23%-4.6% composition.
Press such scheme, the high hard ceramic composite of described norbide-titanium boride-silicon carbide is formed through reaction hot-pressing technology sintering by the ternary mixed powder of raw material norbide, titanium carbide and silicon, described raw material mixed powder by weight percentage, comprise boron carbide powder 60.6%-92%, titanium carbide 4%-23.1%, silica flour 3%-16.3%; Wherein, the mass percent of each raw material is followed reactional equation 2B
4c+2TiC+3Si-B
4c+2TiB
2+ 3SiC, the scope of fluctuating is 2%; The content of silica flour regulates according to the output of the reaction product carbon of norbide and titanium carbide, its objective is and removes product carbon.
Press such scheme, in described mixed powder, boron carbide powder granularity is at 0.5-5 μ m, and purity is greater than 94%; Titanium carbide granularity is at 0.5-5 μ m, and purity is greater than 96%; Silicon particle size is at 0.3-100 μ m, and purity is greater than 98%.
The preparation method of the high hard ceramic composite of above-mentioned norbide-titanium boride-silicon carbide, comprises the following steps:
1. raw materials weighing boron carbide powder 60.6%-92% by weight percentage, titanium carbide 4%-23.1% and silica flour 3%-16.3%, for subsequent use, the mass percent of its Raw is followed reactional equation 2B
4c+2TiC+3Si-B
4c+2TiB
2+ 3SiC, the scope of fluctuating is 2%;
2. load weighted powder is put into the ball grinder of planetary ball mill, added ethanol to carry out batch mixing as dispersion medium, after the removal abrading-ball that then sieves, obtain the ethanolic soln of mixed powder;
3. remove alcohol solvent, obtain moist mixed powder;
4. moist powder is placed in to the vacuum drying oven inner drying 24-48h of 60-100 ℃, grinds, cross the granulation of 100-325 mesh sieve, obtain mixed powder;
5. mixed powder obtained in the previous step is put into graphite jig, between powder and mould, pressure head, separate with graphite paper, insert vacuum or argon gas atmosphere sintering in hot-pressed sintering furnace, apply 20-60MPa pressure, sintering temperature is 1800-2100 ℃, at sintering temperature insulation 30-120min, naturally cooling, can obtain the high hard ceramic composite of norbide-titanium boride-silicon carbide.
Press such scheme, the described step 2. volume of ethanol is less than 2/3rds of ball grinder volume, is greater than 1/3rd of ball grinder volume.
Press such scheme, described step 2. in the rotating speed of planetary ball mill be 50-200 rpm, the material of the ball grinder that adopts and abrading-ball be silicon carbide ball or agate.
Press such scheme, the method that 3. described step removes alcohol solvent is rotary evaporation or suction filtration.
Press such scheme, the described step 5. temperature increasing schedule of middle hot pressed sintering is: 20 ℃/min is warmed up to 1500 ℃, is filled with argon gas (vacuum sintering is applying argon gas not), and insulation 30-60min, is then warmed up to sintering temperature with the speed of 10 ℃/min.
The principle of the invention is: by add titanium carbide in norbide, utilize the chemical reaction between them to generate non-stoichiometric B
4c
1-x, titanium boride and carbon simple substance, cause the change of norbide lattice parameter, produce textural defect, thereby Accelerative mass transfer process reaches the object that reduces sintering temperature; Because the temperature of reaction of silicon and addition product carbon is higher than the temperature of reaction of norbide and titanium carbide, thereby product carbon is carried out with reacting smoothly of silicon.Silicon reacts with carbon not only can remove the carbon that reduces material hardness, can also obtain the third phase material silicon carbide of lightweight, high rigidity.The titanium boride that reaction in－situ generates and silicon carbide purity is high, crystal grain is tiny, be uniformly dispersed, can effectively suppress growing up of norbide crystal grain, is conducive to the generation of refined crystalline strengthening mechanism.In addition, titanium boride does not mate with the thermal expansivity of matrix norbide and produces the tiny crack deflecting effect that unrelieved stress causes, and can improve the fracture toughness property of norbide.So present method can obtain the high hard ceramic composite of norbide-titanium boride-silicon carbide that has high rigidity and high tenacity concurrently at a lower temperature.
Compared with prior art, beneficial effect of the present invention is as follows:
The first, by anti-carbon remaining in ceramic matrix, the hardness of raising body material of removing of original position; Generate the third phase material silicon carbide of lightweight, high rigidity, high tenacity, it is tough that enhancing benefit is played in the generation of silicon carbide, the effect that improves ceramic composite hardness simultaneously.
Second, mechanically resistant material titanium boride and the silicon carbide itself with high rigidity are incorporated in boron carbide superhard stupalith system simultaneously, in improving the fracture toughness property of ceramic composite, do not sacrifice the hardness of ceramic composite, thereby effectively expanded the use range of ceramic composite.
The 3rd, in composite ceramics, second-phase boride and third phase carbide all generate by reaction in－situ, have the advantages that purity is high, crystal grain is tiny, be evenly distributed, can effectively suppress matrix grain grows up, be conducive to the further raising of toughness, thereby effectively improve the work reliability of ceramic composite.
The 4th, this complex phase ceramic is to be obtained by solid state reaction sintering, there is no the participation of liquid phase sintering, and in addition, norbide, titanium boride and silicon carbide are high temperature resistant, corrosion resistant superhard material.Therefore, the ceramic composite that the present invention obtains can be served as high-temperature structural components, is applied to high temperature, the corrosion-resistant condition harshness such as strong, in the high Working environment of mechanical property requirements.
The 5th, sintering temperature is low, technique is simple, workable, product properties stable.
Accompanying drawing explanation
Fig. 1 is the XRD figure of the embodiment of the present invention 1 Raw mixed powder.
Fig. 2 is the XRD figure of the high hard ceramic composite of norbide-titanium boride in the embodiment of the present invention 1-silicon carbide.
Fig. 3 is the SEM secondary electron image (2000 times) of the high hard ceramic composite section of norbide-titanium boride in embodiment 1-silicon carbide.
Fig. 4 is the SEM backscatter images (2000 times) of the high hard ceramic composite section of norbide-titanium boride in embodiment 1-silicon carbide.
Fig. 5 is the SEM secondary electron image (10000 times) of the high hard ceramic composite section of norbide-titanium boride in embodiment 3-silicon carbide.
Fig. 6 is the SEM secondary electron image (40000 times) of the high hard ceramic composite section of norbide-titanium boride in embodiment 3-silicon carbide.
Embodiment
In order to understand better the present invention, further illustrate content of the present invention below in conjunction with accompanying drawing, embodiment, but content of the present invention is not only confined to the following examples.
embodiment 1
The high hard ceramic composite of a kind of norbide-titanium boride-silicon carbide, it is 85%, 8.1%, 6.9% to form by norbide, titanium boride and silicon carbide by mass percent.It is formed through reaction hot-pressing technology sintering by the ternary mixed powder of raw material norbide, titanium carbide and silica flour, described ternary mixed powder by weight percentage, comprise that (purity is 98% to boron carbide powder 88.2%, median size be 0.8 μ m), titanium carbide 6.9%(purity is 97%, median size be 1 μ m), silica flour 4.9%(purity is 99%, median size be 0.6 μ m).
The preparation method of the high hard ceramic composite of norbide-titanium boride described in the present embodiment-silicon carbide, concrete steps comprise:
1. weigh by weight percentage boron carbide powder 88.2%, titanium carbide 6.9%, silica flour 4.9%;
2. load weighted powder is put into the ball grinder of planetary ball mill, add ethanol to carry out batch mixing as dispersion medium, the volume of ethanol is 1/2nd of ball grinder volume, the rotating speed of ball mill is 50 rpm, Ball-milling Time is 6h, the material of the ball grinder that adopts and abrading-ball be agate, then sieve and remove after abrading-ball to obtain the ethanolic soln of mixed powder;
3. adopt the mode of suction filtration to remove alcohol solvent, obtain moist mixed powder;
4. moist powder is placed in to the vacuum drying oven inner drying 48h of 60 ℃, grinds, cross 325 mesh sieve granulations, obtain mixed powder;
5. composite granule obtained in the previous step is put into graphite jig, between powder and mould, pressure head, separate with graphite paper, insert argon gas atmosphere sintering in hot-pressed sintering furnace, apply 30MPa pressure, the temperature increasing schedule of hot pressed sintering is: 20 ℃/min is warmed up to 1500 ℃, be filled with argon gas, insulation 60min, is then warmed up to 1950 ℃ of sintering temperatures with the speed of 10 ℃/min, at sintering temperature insulation 45min, naturally cooling, can obtain the high hard ceramic composite of norbide-titanium boride-silicon carbide.
The performance of the high hard ceramic composite of the norbide-titanium boride that obtains-silicon carbide is as follows: relative density 99.3%, Vickers' hardness 34.1GPa, bending strength 413MPa, fracture toughness property 6.1 MPam
1/2.
embodiment 2
The high hard ceramic composite of a kind of norbide-titanium boride-silicon carbide, it is 90%, 5.4%, 4.6% to form by norbide, titanium boride and silicon carbide by mass percent.It is formed through reaction hot-pressing technology sintering by the ternary mixed powder of raw material norbide, titanium boride and silica flour, the ternary mixed powder of described raw material by weight percentage, comprise that (purity is 96% to boron carbide powder 92.2%, median size be 3 μ m), titanium carbide 4.6%(purity is 97%, median size be 1 μ m), silica flour 3.2%(purity is 99%, median size be 2 μ m).
The preparation method of the high hard ceramic composite of norbide-titanium boride described in the present embodiment-silicon carbide, concrete steps comprise:
1. weigh by weight percentage boron carbide powder 92.2%, titanium carbide 4.6%, silica flour 3.2%;
2. load weighted powder is put into the ball grinder of planetary ball mill, add ethanol to carry out batch mixing as dispersion medium, the volume of ethanol is 2/3rds of ball grinder volume, the rotating speed of ball mill is 100 rpm, Ball-milling Time is 6h, the material of the ball grinder that adopts and abrading-ball be agate, then sieve and remove after abrading-ball to obtain the ethanolic soln of mixed powder;
3. adopt the mode of rotary evaporation to remove alcohol solvent, obtain moist mixed powder;
4. moist powder is placed in to the vacuum drying oven inner drying 36h of 60 ℃, grinds, cross 200 mesh sieve granulations, obtain mixed powder;
5. composite granule obtained in the previous step is put into graphite jig, between powder and mould, pressure head, separate with graphite paper, insert argon gas atmosphere sintering in hot-pressed sintering furnace, apply 30MPa pressure, the temperature increasing schedule of hot pressed sintering is: 20 ℃/min is warmed up to 1500 ℃, be filled with argon gas, insulation 45min, is then warmed up to 1950 ℃ of sintering temperatures with the speed of 10 ℃/min, at sintering temperature insulation 60min, naturally cooling, can obtain the high hard ceramic composite of norbide-titanium boride-silicon carbide.
embodiment 3
The difference of the present embodiment and embodiment 2 is, in the high hard ceramic composite of made norbide-titanium boride-silicon carbide, the mass percent of norbide, titanium boride and silicon carbide is 80%, 10.8%, 9.2%.
embodiment 4
The difference of the present embodiment and embodiment 2 is, in the high hard ceramic composite of made norbide-titanium boride-silicon carbide, the mass percent of norbide, titanium boride and silicon carbide is 70%, 16.2%, 13.8%.
embodiment 5
The difference of the present embodiment and embodiment 2 is, in the high hard ceramic composite of made norbide-titanium boride-silicon carbide, the mass percent of norbide, titanium boride and silicon carbide is 60%, 28%, 12%.
The performance of the high hard ceramic composite of embodiment norbide-titanium boride that 2-5 obtains-silicon carbide is as shown in table 1.
embodiment 6
The high hard ceramic composite of a kind of norbide-titanium boride-silicon carbide, it is 80%, 10.8%, 9.2% to form by norbide, titanium boride and silicon carbide by mass percent.It is formed through reaction hot-pressing technology sintering by the ternary mixed powder of raw material norbide, titanium boride and silica flour, the ternary mixed powder of described raw material by weight percentage, comprise that (purity is 98% to boron carbide powder 84.3%, median size be 0.8 μ m), titanium carbide 9.2%(purity is 97%, median size be 1 μ m), silica flour 6.5%(purity is 99%, median size be 0.6 μ m).
The preparation method of the high hard ceramic composite of norbide-titanium boride described in the present embodiment-silicon carbide, concrete steps comprise:
1. weigh by weight percentage boron carbide powder 84.3.2%, titanium carbide 9.2%, silica flour 6.5%;
2. load weighted powder is put into the ball grinder of planetary ball mill, add ethanol to carry out batch mixing as dispersion medium, the volume of ethanol is 1/2nd of ball grinder volume, the rotating speed of ball mill is 50 rpm, Ball-milling Time is 12h, the material of the ball grinder that adopts and abrading-ball be agate, then sieve and remove after abrading-ball to obtain the ethanolic soln of mixed powder;
3. adopt the mode of suction filtration to remove alcohol solvent, obtain moist mixed powder;
4. moist powder is placed in to the vacuum drying oven inner drying 48h of 60 ℃, grinds, cross 200 mesh sieve granulations, obtain mixed powder;
5. composite granule obtained in the previous step is put into graphite jig, between powder and mould, pressure head, separate with graphite paper, insert argon gas atmosphere sintering in hot-pressed sintering furnace, apply 30MPa pressure, the temperature increasing schedule of hot pressed sintering is: 20 ℃/min is warmed up to 1500 ℃, be filled with argon gas, insulation 60min, is then warmed up to 1850 ℃ of sintering temperatures with the speed of 10 ℃/min, at sintering temperature insulation 90min, naturally cooling, can obtain the high hard ceramic composite of norbide-titanium boride-silicon carbide.
The performance of the high hard ceramic composite of gained norbide-titanium boride-silicon carbide is as follows: relative density 98.6%, Vickers' hardness 31.2GPa, bending strength 401.2MPa, fracture toughness property 6.3 MPam
1/2.
comparative example
Compared with norbide-titanium boride composite ceramics that the prepared high hard ceramic composite of norbide-titanium boride-silicon carbide of present method is prepared by reaction hot-pressing with Tang Jun etc.: in document, the sintering temperature of norbide-titanium boride composite ceramics is 2050 ℃, pressure is 35MPa, adds 20vol% TiC (corresponding TiB
2for 35vol%) the Fracture Toughness of complex phase ceramic be 6.3 MPam
1/2, but its hardness is less than 21GPa; Although add the hardness of the complex phase ceramic of 5% titanium carbide can reach 29GPa, its fracture toughness property only has 4.2 MPam
1/2left and right.Norbide-titanium boride composite ceramics of preparing in document, not only hardness and toughness can not improve simultaneously, the high hard ceramic composite of norbide-titanium boride-silicon carbide that the single-phase maximum value of its hardness and toughness is also prepared lower than the inventive method.
Specifically introduce phase composite, degree of compactness and the microstructure of the high hard ceramic composite of norbide-titanium boride of the present invention-silicon carbide below in conjunction with legend.
Fig. 1 and Fig. 2 are respectively original mixed powder in example 1 and the XRD spectra of obtained ceramic block, and wherein Fig. 1 is the XRD spectra of original powder, and Fig. 2 is the XRD spectra that the inventive method is prepared sample.The diffraction peak that contains obvious norbide, titanium carbide and silicon in spectrogram 1, illustrates that original powder is made up of norbide, titanium carbide and silicon.Spectrogram 2 shows, the diffraction peak of titanium carbide and silicon has not existed, and only has the diffraction peak of norbide, titanium boride and silicon carbide, illustrates in the reaction of sintering process Raw norbide, titanium carbide and silica flour and substantially completes, and generates titanium boride and silicon carbide.Prove that reaction sintering method of the present invention is goods feasible, that can obtain expection.
Fig. 3 and Fig. 4 are respectively SEM secondary electron image and the backscatter images of the high hard ceramic composite sample section of norbide-titanium boride in embodiment 1-silicon carbide.As seen from Figure 3, sample reaches complete densification substantially, does not have leachy existence.And as can be seen from Figure 4, particle diameter is distributed in norbide matrix uniformly at thin brilliant titanium boride and the silicon carbide of 2 μ m left and right, tiny uniform micron order titanium boride and silicon carbide tissue between matrix grain, are formed as seen by reaction in－situ.Tiny equally distributed titanium boride and silicon carbide can effectively improve the toughness reliability of ceramic.
Fig. 5 is the SEM secondary electron phase of the high hard ceramic composite sample section of norbide-titanium boride in embodiment 3-silicon carbide, can be found out by image, and fracture apperance is irregular, has particle to extract phenomenon, and this is the performance along brilliant fracture.The reason that occurs this phenomenon is that the thermal expansivity of titanium boride does not mate with norbide matrix, sample can produce unrelieved stress at phase interface from the process of sintering temperature cool to room temperature, in the time having an effect in crack propagation and residual stress field, crackle is always along the weak link expansion of stress field.So, in the time that crackle runs into boron carbide particles, deflect and detour, so just increase the approach of crack propagation, consume more multipotency, thereby improve the fracture toughness property of ceramic composite.
Fig. 6 is also the SEM secondary electron phase of the high hard ceramic composite sample section of norbide-titanium boride in embodiment 3-silicon carbide, can find out, generated in-situ tiny sheet-shaped silicon carbide (thick 100nm, diameter 1 μ m left and right) interts in norbide matrix.Because the thermal expansivity of norbide and silicon carbide is more or less the same, so micron silicon-carbide particle and matrix that reaction in－situ generates have good consistency, two-phase interface is combined closely.Sheet-shaped silicon carbide interts in matrix, can effectively stop the expansion of crackle in matrix, thereby also can play the effect that increases matrix toughness.
From embodiment 1-6, along with the increase of titanium boride and carborundum content, the density of the high hard combined ceramic products of gained norbide-titanium boride-silicon carbide is the trend of growth, and hardness is in a slight decrease, but its minimum value is also greater than 31GPa; Fracture toughness property is all greater than 6.1 MPam
1/2, and be the trend of growth.Visible, the inventive method can be prepared at a lower temperature has high-compactness, the high hard ceramic composite of norbide-titanium boride-carbonization that high rigidity and high tenacity get both.
Claims (5)
1. a preparation method for the high hard ceramic composite of norbide-titanium boride-silicon carbide, is characterized in that it comprises the following steps:
(1) raw materials weighing boron carbide powder 60.6%-92% by weight percentage, titanium carbide 4%-23.1% and silica flour 3%-16.3%, for subsequent use, the mass percent of its Raw is followed reactional equation 2B
4c+2TiC+3Si-B
4c+2TiB
2+ 3SiC, the scope of fluctuating is 2%;
(2) load weighted powder is put into the ball grinder of planetary ball mill, added ethanolic soln to carry out batch mixing as dispersion medium, then sieve and remove the ethanolic soln that obtains mixed powder after abrading-ball;
(3) remove alcohol solvent, obtain moist mixed powder;
(4) moist powder is placed in to the vacuum drying oven inner drying 24-48h of 60-100 ℃, grinds, cross the granulation of 100-325 mesh sieve, obtain mixed powder;
(5) mixed powder obtained in the previous step is put into graphite jig, between powder and mould, pressure head, separate with graphite paper, insert vacuum or argon gas atmosphere sintering in hot-pressed sintering furnace, apply 20-60MPa pressure, sintering temperature is 1800-2100 ℃, at sintering temperature insulation 30-120min, naturally cooling, can obtain the high hard ceramic composite of norbide-titanium boride-silicon carbide.
2. the preparation method of the high hard ceramic composite of norbide-titanium boride according to claim 1-silicon carbide, is characterized in that the volume of described step (2) ethanol is less than 2/3rds of ball grinder volume, is greater than 1/3rd of ball grinder volume.
3. the preparation method of the high hard ceramic composite of norbide-titanium boride according to claim 1-silicon carbide, it is characterized in that the rotating speed of planetary ball mill is 50-200 rpm in described step (2), the material of the ball grinder that adopts and abrading-ball be silicon carbide or agate.
4. the preparation method of the high hard ceramic composite of norbide-titanium boride according to claim 1-silicon carbide, is characterized in that it is rotary evaporation or suction filtration that described step (3) is removed the method for alcohol solvent.
5. the preparation method of the high hard ceramic composite of norbide-titanium boride according to claim 1-silicon carbide, the temperature increasing schedule that it is characterized in that hot pressed sintering in described step (5) is: 20 ℃/min is warmed up to 1500 ℃, be filled with argon gas, insulation 30-60min, is then warmed up to sintering temperature with the speed of 10 ℃/min; When vacuum sintering is without applying argon gas, 20 ℃/min is warmed up to 1500 ℃, and insulation 30-60min, is then warmed up to sintering temperature with the speed of 10 ℃/min.
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| CN100349824C (en) * | 2006-01-18 | 2007-11-21 | 山东大学 | Boron carbide based bulletproof composite ceramic and preparation method thereof |
| CN102503427B (en) * | 2011-11-10 | 2013-06-05 | 哈尔滨工业大学 | Preparation method of high-toughness boride-carbide composite ceramic |
| CN102603301B (en) * | 2012-03-28 | 2013-06-05 | 无锡职业技术学院 | Preparation method for titanium alloy surface composite ceramic coating |
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| CN111875385A (en) * | 2020-07-17 | 2020-11-03 | 武汉理工大学 | Preparation method of high-strength, high-hardness and low-modulus titanium boride nano multiphase ceramic |
| CN111875385B (en) * | 2020-07-17 | 2022-07-19 | 武汉理工大学 | Preparation method of high-strength, high-hardness and low-modulus titanium boride nano complex phase ceramic |
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