CN108484171B - Boron carbide-titanium boride complex phase ceramic material and pressureless sintering preparation method thereof - Google Patents
Boron carbide-titanium boride complex phase ceramic material and pressureless sintering preparation method thereof Download PDFInfo
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Abstract
The invention relates to a boron carbide-titanium boride complex phase ceramic material and a pressureless sintering preparation method thereof, belonging to the technical field of structural ceramics. The composite ceramic comprises the following components in percentage by mass based on 100% of the total mass of the composite ceramic raw material: 50-80% of boron carbide powder, 10-30% of titanium boride powder, 3-20% of amorphous carbon powder and 5-30% of silicon powder. The method comprises the following steps: mixing the raw materials, adding the mixture into a medium solution, and performing ball milling and mixing to obtain mixed slurry; drying the mixed slurry, grinding and sieving to obtain powder; carrying out compression molding on the powder, and carrying out cold isostatic pressing to obtain a green body; and sintering the green body at high temperature and no pressure under vacuum or protective gas to obtain the ceramic material. The toughness of the material is obviously improved, the production cost is greatly reduced, and the material can be widely applied to the fields of nuclear power, light armor protection and the like.
Description
Technical Field
The invention relates to a boron carbide-titanium boride complex phase ceramic material and a pressureless sintering preparation method thereof, belonging to the technical field of structural ceramics.
Background
Boron carbide (B)4C) Ceramics have lower density, higher hardness (second to cubic boron nitride and diamond), wear resistance and good neutron absorption cross section characteristics, and are widely used in the fields of light armor protection, nuclear energy, wear-resistant parts and the like.
Boron carbide is a ceramic material with strong covalent bonds, the covalent bonds account for 93.94 percent, and the self-diffusion coefficient is low, so that pure boron carbide is difficult to realize sintering densification. The most important prerequisite for pressureless sintering to prepare pure boron carbide is the use of ultrafine powders with particle size less than 3 μm, protective atmosphere and high temperature (2300 ℃). The relative density of the product obtained by sintering boron carbide at 2300 ℃ under normal pressure is usually lower than 80%, the mechanical property index of the product is lower, and the phenomena of abnormal growth of crystal grains and surface melting are easy to occur. These severely limit the range of applications for boron carbide. So that various assistants such as C, SiC, TiC and TiB are introduced2，ZrB2，CrB2，W2B5，BN，Al2O3And some metals and the like to increase the degree of densification of the boron carbide.
Although much research is done on the preparation technology of boron carbide composite materials at home and abroad, the prepared boron carbide ceramic material has little improvement on toughness, complex production equipment and high cost, and the popularization and the application of the boron carbide ceramic material are seriously restricted.
Disclosure of Invention
In view of the above, the present invention aims to provide a boron carbide-titanium boride complex phase ceramic material and a pressureless sintering preparation method thereof, which realizes the preparation of the boron carbide-titanium boride complex phase ceramic material with low cost and high toughness.
In order to achieve the above object, the technical solution of the present invention is as follows.
The boron carbide-titanium boride complex phase ceramic material comprises the following components in percentage by mass based on 100% of the total mass of the complex phase ceramic raw material:
preferably, the purity of the boron carbide powder is more than or equal to 90 percent, and the average grain diameter is D50≤10μm。
Preferably, the purity of the titanium boride powder is more than or equal to 95 percent, and the average grain diameter is D50≤10μm。
Preferably, the purity of the amorphous carbon powder is not less than 96%, and the particle size range is 50 nm-3 μm.
Preferably, the purity of the silicon powder is more than or equal to 96%, and the particle size range is 50 nm-3 μm.
A pressureless sintering preparation method of boron carbide-titanium boride complex phase ceramic material comprises the following steps:
(1) adding boron carbide powder, titanium boride powder, amorphous carbon powder and silicon powder into ball milling equipment, then adding the mixture into a medium solution, carrying out ball milling mixing, and fully stirring and mixing for 2-48 h at the rotating speed of 50-400 r/min to obtain mixed slurry; wherein the mass ratio of the medium solution to the raw material is more than or equal to 1: 1;
(2) drying the mixed slurry, grinding, and sieving with a 60-100 mesh sieve to obtain powder;
(3) carrying out compression molding on the powder, carrying out cold isostatic pressing at the pressure of 100-500 MPa, and maintaining the pressure for 5-30 min to obtain a green body;
(4) and (3) carrying out high-temperature pressureless sintering on the green body under vacuum or protective gas at the temperature of 1900-2300 ℃ for 0.5-3 h to obtain the boron carbide-titanium boride complex phase ceramic material.
Preferably, the medium solution is absolute ethyl alcohol or deionized water.
Preferably, the ball milling equipment is a vertical or horizontal ball mill; during ball milling and material mixing, the ball material ratio is 1-30: 1.
preferably, the mixed slurry is dried by rotary evaporation and then dried in vacuum for 12-36 hours.
Preferably, the protective gas is inert gas or nitrogen with the purity of more than 99.999 percent.
Has the advantages that:
1. the raw materials adopted by the invention are coarse-particle boron carbide powder and titanium boride powder, the cost of the raw materials is reduced, a small amount of carbon powder and silicon powder are added as auxiliary agents, a pressureless sintering process capable of large-scale production is adopted, the toughness of the prepared boron carbide-titanium boride complex phase ceramic material is obviously improved, the production cost is greatly reduced, and the boron carbide-titanium boride complex phase ceramic material can be widely applied to the fields of nuclear power, light armor protection and the like. TiB2As diffusing particles with B4Between C and the substrateThe thermal expansion coefficients are not matched, a plurality of micro cracks are formed, the energy absorption capacity is improved, and the fracture toughness is obviously improved. The addition of C can effectively improve the densification degree of boron carbide, C is used as an additive, and B is prepared by pressureless sintering at 2150 DEG C4The relative density of C reaches 96.4%. The addition of a small amount of Si is very effective for improving the sintering capability of the boron carbide, and the boron carbide matrix can also provide a C source to react with the Si to form second-phase SiC, which is beneficial to improving the mechanical property of the boron carbide.
2. The invention simultaneously converts TiB into2The C and Si components are introduced into a boron carbide complex phase ceramic material system, a small amount of new silicon carbide phases are generated through in-situ reaction, and the silicon carbide improves the toughness of the complex phase ceramic by inhibiting the growth of crystal grains of boron carbide and titanium boride. The titanium boride with higher hardness and toughness is introduced into a boron carbide complex phase ceramic material system, so that the fracture toughness of the complex phase ceramic is improved without reducing the hardness of the complex phase ceramic. In the complex phase ceramic material, the generated laminated graphite promotes the sintering process, is in a residual stress field of boron carbide and titanium boride, causes deflection, bridging and the like of cracks, and obviously improves the toughness of the complex phase ceramic.
3. In the method, the amorphous carbon powder and the silicon powder auxiliary agent with small particle sizes have high surface energy, good particle agglomeration effect can be realized, the particle size distribution of agglomerated particles is uniform after sieving, and the compression molding can be well realized, so that a binder is not required to be added in the molding process, the glue discharging process is omitted, holes generated by glue discharging in a sample are avoided, and the sintering time is shortened.
4. The method has the advantages of simple and convenient process operation, low cost of raw materials and production and easy realization of industrial production.
Drawings
FIG. 1 is an X-ray diffraction pattern of a complex phase ceramic material prepared in example 1 of the present invention;
FIG. 2 is a scanning electron microscope image of the fracture morphology of the complex phase ceramic material prepared in example 1 of the present invention;
FIG. 3 is an X-ray diffraction pattern of a complex phase ceramic material prepared in example 2 of the present invention;
FIG. 4 is a scanning electron microscope image of the fracture morphology of the complex phase ceramic material prepared in example 2 of the present invention;
FIG. 5 is an X-ray diffraction pattern of a complex phase ceramic material prepared in example 3 of the present invention;
FIG. 6 is a scanning electron microscope image of the fracture morphology of the complex phase ceramic material prepared in example 3 of the present invention.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
The following tests were carried out on the products prepared in the examples:
x-ray diffraction (XRD) test: polishing the surface of the obtained product to a surface roughness of less than or equal to 0.5 μm by using an X-ray diffractometer (XRD, Rigaku Ultima III, Japan, Cu-K alpha).
Scanning Electron Microscope (SEM) testing: fracture morphology surface of the product, field emission scanning electron microscope (FESEM, FEI Quanta FEG250, USA).
Example 1
B4C-TiB2The pressureless sintering preparation method of the complex phase ceramic material comprises the following steps:
(1) 50g of boron carbide powder (the purity is more than or equal to 90 percent, D)5010 μm), titanium boride powder 10g (purity is not less than 99%, D)5010 μm), amorphous carbon powder 10g (purity not less than 99%, D)50500nm), 30g of silicon powder (purity is more than or equal to 96 percent, D)501 μm), and 200ml of absolute ethyl alcohol; putting the mixture into a nylon tank, and carrying out ball milling on a planetary ball mill (ball-material ratio is 1:1), wherein the rotating speed of the ball mill is 450r/min, and the ball milling time is 48 h; obtaining mixed slurry;
(2) drying the mixed slurry on a rotary evaporator, and then drying for 12 hours in an oven; grinding by a mortar, and sieving by a 100-mesh sieve to obtain powder;
(3) dry pressing the powder in a graphite mould for molding, and carrying out cold isostatic pressing treatment under the pressure of 500MPa for 5min to obtain a green body;
(4) and (3) sintering the green body in a graphite vacuum sintering furnace at 2100 ℃ for 30min to obtain a final product.
The XRD results of the final product are shown in FIG. 1, and the phase composition of the final product is as follows: b is4C、TiB2And SiC, the characteristic peak of SiC is higher, the characteristic peak of Si is not present, the Si is completely reacted, C and Si in the raw material are reacted to generate SiC, and the surplus Si and B4C, reacting to generate SiC; indicating that the final product is B4C-TiB2A complex phase ceramic material.
The SEM result of the final product is shown in FIG. 2, the final product has lath-shaped SiC phase, and the product has compact structure, and the fracture mode has a mixed mode of crystal-through fracture and crystal-along fracture.
And (3) performance testing: the relative density of the final product is up to 92.5% measured by an Archimedes drainage method; the bending strength of the final product is up to 300MPa measured by adopting a GBT6569-2006 fine ceramic bending strength test method; the fracture toughness of the final product measured by adopting a GBT 23806-2009 fine ceramic fracture toughness test method-unilateral pre-crack beam (SEPB) method reaches 4.2MPam1/2(ii) a The Vickers hardness of the final product reaches 28GPa measured by adopting a Vickers hardness test method of GBT16534-1996 engineering ceramics.
Example 2
B4C-TiB2The pressureless sintering preparation method of the complex phase ceramic material comprises the following steps:
(1) 80g of boron carbide powder (the purity is more than or equal to 99 percent, D)503 μm), titanium boride powder 10g (purity is not less than 95%, D)5010 μm), amorphous carbon powder 5g (purity not less than 96%, D)503 μm), 5g of silicon powder (purity not less than 96%, D)503 μm), 30ml of absolute ethyl alcohol; putting the mixture into a nylon tank, and carrying out ball milling on a planetary ball mill (ball-material ratio is 10:1), wherein the rotating speed of the ball mill is 80r/min, and the ball milling time is 12 h; obtaining mixed slurry;
(2) drying the mixed slurry on a rotary evaporator, and then drying for 36h in an oven; grinding by a mortar, and sieving by a 60-mesh sieve to obtain powder;
(3) dry pressing the powder in a graphite mould for molding, and carrying out cold isostatic pressing treatment under the pressure of 100MPa for 30min to obtain a green body;
(4) and (3) sintering the green body in a graphite vacuum sintering furnace at the sintering temperature of 2150 ℃ for 2h to obtain a final product.
The XRD results of the final product are shown in FIG. 3, and the phase composition of the final product is as follows: b is4C、TiB2And SiC and graphite show that SiC is generated by the reaction of C and Si in the raw materials, and the redundant amorphous carbon powder exists in the form of graphite; indicating that the final product is B4C-TiB2A complex phase ceramic material.
The SEM result of the final product is shown in FIG. 4, and the final product has lath-shaped SiC phase and smaller size; meanwhile, laminated graphite phase exists; the fracture modes of the samples are mixed fracture modes of transcrystalline and intergranular.
And (3) performance testing: the relative density of the final product is measured to reach 98.6 percent by adopting an Archimedes drainage method; the bending strength of the final product reaches 353MPa measured by adopting a GBT6569-2006 fine ceramic bending strength test method; the fracture toughness of the final product measured by adopting a GBT 23806-2009 fine ceramic fracture toughness test method-unilateral pre-crack beam (SEPB) method reaches 5.11MPam1/2(ii) a The Vickers hardness of the final product reaches 33GPa measured by adopting a Vickers hardness test method of GBT16534-1996 engineering ceramics.
Example 3
B4C-TiB2The pressureless sintering preparation method of the complex phase ceramic material comprises the following steps:
(1) 60g of boron carbide powder (purity is more than or equal to 96 percent, D)505 μm), 30g of titanium boride powder (purity is more than or equal to 95 percent, D)503 μm), amorphous carbon powder 3g (purity not less than 99%, D)50300nm), 7g of silicon powder (purity is more than or equal to 99 percent, D)50500nm), and 200ml of absolute ethyl alcohol; putting the mixture into a nylon tank, and carrying out ball milling on a planetary ball mill (ball-material ratio is 1:1), wherein the rotating speed of the ball mill is 300r/min, and the ball milling time is 8 h; obtaining mixed slurry;
(2) drying the mixed slurry on a rotary evaporator, and then drying for 24 hours in an oven; grinding by a mortar, and sieving by a 80-mesh sieve to obtain powder;
(3) dry pressing the powder in a graphite mould for molding, and carrying out cold isostatic pressing treatment under the pressure of 300MPa for 20min to obtain a green body;
(4) and (3) sintering the green body in a graphite vacuum sintering furnace at the sintering temperature of 1900 ℃ for 3 hours to obtain a final product.
The XRD results of the final product are shown in fig. 5, and the phase composition of the final product is: b is4C、TiB2And SiC, which shows that SiC is generated by the reaction of C and Si in the raw materials and no redundant Si and C residues are left; indicating that the final product is B4C-TiB2A complex phase ceramic material.
The SEM result of the final product is shown in FIG. 6, and the final product has lath-shaped SiC phase with small size; the fracture mode is a mixed mode of transcrystalline and intergranular fracture.
And (3) performance testing: the relative density of the final product is up to 94% measured by an Archimedes drainage method; the bending strength of the final product is measured to reach 320MPa by adopting a GBT6569-2006 fine ceramic bending strength test method; the fracture toughness of the final product measured by adopting a GBT 23806-2009 fine ceramic fracture toughness test method-unilateral pre-crack beam (SEPB) method reaches 4.8MPam1/2(ii) a The Vickers hardness of the final product reaches 30GPa measured by a Vickers hardness test method of GBT16534-1996 engineering ceramics.
The invention includes, but is not limited to, the above embodiments, and any equivalent substitutions or partial modifications made under the spirit and principle of the invention are deemed to be within the scope of the invention.
Claims (9)
1. A boron carbide-titanium boride complex phase ceramic material is characterized in that: the composite ceramic comprises the following components in percentage by mass based on 100% of the total mass of the composite ceramic raw material:
the complex phase ceramic raw material is prepared by a pressureless sintering method, and the method comprises the following steps:
(1) adding boron carbide powder, titanium boride powder, amorphous carbon powder and silicon powder into ball milling equipment, then adding the mixture into a medium solution, carrying out ball milling mixing, and fully stirring and mixing for 2-48 h at the rotating speed of 50-400 r/min to obtain mixed slurry; wherein the mass ratio of the medium solution to the raw material is more than or equal to 1: 1;
(2) drying the mixed slurry, grinding, and sieving with a 60-100 mesh sieve to obtain powder;
(3) carrying out compression molding on the powder, carrying out cold isostatic pressing at the pressure of 100-500 MPa, and maintaining the pressure for 5-30 min to obtain a green body;
(4) and (3) carrying out high-temperature pressureless sintering on the green body under vacuum or protective gas, wherein the temperature is 1900-2300 ℃, and the heat preservation time is 0.5-3 h, so as to obtain the boron carbide-titanium boride complex phase ceramic material.
2. The boron carbide-titanium boride composite ceramic material of claim 1 wherein: the purity of the boron carbide powder is more than or equal to 90 percent, and the average grain diameter is D50≤10μm。
3. The boron carbide-titanium boride composite ceramic material of claim 1 wherein: the purity of the titanium boride powder is more than or equal to 95 percent, and the average grain diameter is D50≤10μm。
4. The boron carbide-titanium boride composite ceramic material of claim 1 wherein: the purity of the amorphous carbon powder is more than or equal to 96 percent, and the particle size range is 50 nm-3 mu m.
5. The boron carbide-titanium boride composite ceramic material of claim 1 wherein: the purity of the silicon powder is more than or equal to 96 percent, and the particle size range is 50 nm-3 mu m.
6. The boron carbide-titanium boride composite ceramic material of claim 1 wherein: the medium solution is absolute ethyl alcohol or deionized water.
7. The boron carbide-titanium boride composite ceramic material of claim 1 wherein: the ball milling equipment is a vertical or horizontal ball mill; during ball milling and material mixing, the ball material ratio is 1-30: 1.
8. the boron carbide-titanium boride composite ceramic material of claim 1 wherein: and after the mixed slurry is subjected to rotary evaporation drying, performing vacuum drying for 12-36 h.
9. The boron carbide-titanium boride composite ceramic material of claim 1 wherein: the protective gas is inert gas or nitrogen with the purity of more than 99.999 percent.
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