CN117263691A - B (B) 4 Preparation method of C composite ceramic material - Google Patents
B (B) 4 Preparation method of C composite ceramic material Download PDFInfo
- Publication number
- CN117263691A CN117263691A CN202311190952.XA CN202311190952A CN117263691A CN 117263691 A CN117263691 A CN 117263691A CN 202311190952 A CN202311190952 A CN 202311190952A CN 117263691 A CN117263691 A CN 117263691A
- Authority
- CN
- China
- Prior art keywords
- composite ceramic
- ceramic material
- powder
- preparation
- grinding
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000002131 composite material Substances 0.000 title claims abstract description 66
- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 239000000843 powder Substances 0.000 claims abstract description 33
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims abstract description 28
- 239000011812 mixed powder Substances 0.000 claims abstract description 25
- 238000005245 sintering Methods 0.000 claims abstract description 25
- 238000001035 drying Methods 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 13
- 238000007731 hot pressing Methods 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 11
- 238000000713 high-energy ball milling Methods 0.000 claims abstract description 6
- 238000000227 grinding Methods 0.000 claims description 22
- 239000002245 particle Substances 0.000 claims description 10
- 238000007873 sieving Methods 0.000 claims description 10
- 239000004677 Nylon Substances 0.000 claims description 3
- 229920001778 nylon Polymers 0.000 claims description 3
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 3
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 2
- 239000000919 ceramic Substances 0.000 abstract description 30
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract description 6
- 239000002994 raw material Substances 0.000 abstract description 3
- 239000002002 slurry Substances 0.000 abstract description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 15
- 229910002804 graphite Inorganic materials 0.000 description 15
- 239000010439 graphite Substances 0.000 description 15
- 238000000498 ball milling Methods 0.000 description 12
- 238000010438 heat treatment Methods 0.000 description 12
- 238000000034 method Methods 0.000 description 11
- 239000011268 mixed slurry Substances 0.000 description 8
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 238000005452 bending Methods 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 230000001680 brushing effect Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000005498 polishing Methods 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 241001391944 Commicarpus scandens Species 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000003776 cleavage reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000012938 design process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000001513 hot isostatic pressing Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000005360 mashing Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 230000007017 scission Effects 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/563—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on boron carbide
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/77—Density
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention relates to the field of materials, in particular to a B 4 A preparation method of a C composite ceramic material. First, B is 4 C powder and Al 2 O 3 Mixing the powder according to a proportion, performing high-energy ball milling and mixing in absolute ethyl alcohol, uniformly mixing to obtain slurry, and drying to obtain uniform mixed raw material powder. The mixed powder is then ground and sieved. Then under the protection of flowing Ar atmosphere, carrying out hot-pressing sintering on the mixed powder to generate B 4 C/Al 2 O 3 Composite ceramic blocks. B obtained by the invention 4 C/Al 2 O 3 The composite ceramic has excellent mechanical properties, the preparation method is simple and easy to operate, the preparation period is short, the practicability is strong, and the cost is relatively low.
Description
Technical Field
The invention relates to the field of materials, in particular to a B 4 A preparation method of a C composite ceramic material.
Background
B 4 The C ceramic has high melting point, low density, high hardness and high elastic modulus, and has excellent wear resistance and corrosion resistance, so that the C ceramic has wide application in the fields of aviation, aerospace, military industry, nuclear industry, mechanical manufacturing and the like, and is an important structural ceramic material.
Preparation B 4 The method of C ceramic material mainly has no pressureSintering, hot pressing sintering, hot isostatic pressing sintering, reaction sintering and discharge plasma sintering. B (B) 4 The proportion of the covalent bond C is 94%, and the covalent bond C is a covalent bond compound. At B 4 In the sintering process of the C ceramic, the B-C bond has high covalent bond strength and is not easy to be destroyed, so that the particles are slowly diffused in the sintering process, thereby preparing compact B 4 The C ceramic requires high sintering temperature and long sintering time, and consumes a large amount of energy. And B is 4 C ceramic has lower fracture toughness and B 4 The cost of the raw material powder of C is higher, and the B is limited 4 C ceramic is widely used.
To reduce B 4 The sintering temperature and the production cost of the C ceramic are improved 4 Mechanical properties of C ceramics, obtainable by 4 Adding a second phase into the C ceramic matrix to prepare B 4 C composite ceramic. For this, researchers need to further improve B 4 Component design and preparation process of C ceramic. Developing B with simple process, relatively low sintering temperature, relatively low price and good mechanical property 4 C composite ceramic material, will be to B 4 The wide application of C material has profound effects.
Disclosure of Invention
In view of the problems in the prior art, an object of the present invention is to provide a B 4 Preparation method of C composite ceramic material, and B prepared by method 4 C/Al 2 O 3 The composite ceramic has excellent mechanical properties.
The technical scheme of the invention is as follows:
b (B) 4 The preparation method of the C composite ceramic material comprises the following steps:
step 1, B is 4 C powder and Al 2 O 3 Mixing the powder by wet high-energy ball milling, and drying to obtain mixed powder;
step 2, grinding and sieving the mixed powder;
step 3, hot-pressing and sintering the mixed powder under the protection of flowing Ar atmosphere to obtain B 4 C/Al 2 O 3 A composite ceramic material.
Said B 4 In the step 1, B in the mixed powder is calculated according to the mass ratio 4 C accounts for 60% -90%, al 2 O 3 Accounting for 10 to 40 percent.
Said B 4 Preparation method of C composite ceramic material, in step 1, B 4 The grain diameter of the C powder is less than or equal to 0.5 mu m, al 2 O 3 The grain diameter of the powder is less than or equal to 2.0 mu m.
Said B 4 In the step 1, the materials of a grinding tank and grinding balls of the high-energy ball mill are nylon and silicon carbide respectively, and the high-energy ball mill rotating speed is not lower than 280r/min.
Said B 4 In the step 2, the grinding is carried out by sieving with a sieve of not less than 80 meshes.
Said B 4 In the step 3, the hot-pressing sintering temperature is 1900-1950 ℃, the applied pressure is 30-40 MPa, the pressure is slowly increased from 1500 ℃ to 100-150 ℃ before the target temperature, the applied pressure reaches the maximum value, and the temperature and the pressure are maintained for 1-3 hours at the target temperature.
The design idea of the invention is as follows:
the fracture toughness of the alumina ceramic is higher due to Al 2 O 3 The interaction force between the crystal grains is higher than the strength of the crystal grains, so that the cracks in the alumina ceramic are easy to break through crystals, namely atomic bonds in the unit cells are broken; and Al is 2 O 3 The lattice structure of (a) is a trigonal system, and the lattice parameter isThe surface is easy to have a nanoscale ladder-shaped pattern shape in the fracture process, and the propagation path of the crack is increased, so that the fracture toughness is improved. Thus, al is as follows 2 O 3 Particle addition to B 4 In the C ceramic matrix, can increase B 4 C ceramic fracture toughness.
The invention has the following advantages and beneficial effects:
(1) The invention will B 4 C powder and Al 2 O 3 Mixing the powder by wet high-energy ball milling, and drying to obtain mixed powder; grinding and sieving the mixed powder; under the protection of flowing Ar atmosphere, carrying out hot-pressing sintering on the mixed powder to obtain B 4 C/Al 2 O 3 A composite ceramic material. Thus, by introducing Al with relatively low price and relatively high fracture toughness 2 O 3 On the one hand B can be prepared at relatively low temperatures 4 C ceramic, on the other hand can make B 4 C/Al 2 O 3 The composite ceramic material can obtain excellent mechanical properties, and the performance indexes are as follows: the density is 2.3-2.9 g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the The relative density is 88.9-98.5%; the Vickers hardness is 12-24 GPa; the bending strength is 324-336 MPa; fracture toughness of 3-5 MPa.m 1/2 。
(2) The preparation method provided by the invention is simple and easy to operate, short in preparation period, strong in practicability and relatively low in cost.
Drawings
Other features, objects and advantages of the present invention will become more apparent upon reading of the detailed description of non-limiting embodiments, made with reference to the following drawings.
FIG. 1 is a block diagram of B prepared in example 1 of the present invention 4 C/Al 2 O 3 An X-ray diffraction pattern of the composite ceramic material; in the figure, the abscissa 2θ is the diffraction angle (°), and the ordinate density represents the relative Intensity (a.u.).
FIG. 2 is a diagram of B prepared in example 2 of the present invention 4 C/Al 2 O 3 A field emission Scanning Electron Microscope (SEM) microstructure topography of a cross section of the composite ceramic material.
FIG. 3 is a diagram of B prepared in example 3 of the present invention 4 C/Al 2 O 3 An X-ray diffraction pattern of the composite ceramic material; in the figure, the abscissa 2θ is the diffraction angle (°), and the ordinate density represents the relative Intensity (a.u.).
Detailed Description
Example embodiments will now be described more fully with reference to the accompanying drawings. However, the example embodiments may be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the concept of the example embodiments to those skilled in the art.
In the implementation process, a B is provided 4 The preparation method of the C composite ceramic material comprises the steps of firstly preparing B 4 C powder and Al 2 O 3 Mixing the powder according to a proportion, performing high-energy ball milling and mixing in absolute ethyl alcohol, uniformly mixing to obtain slurry, and drying to obtain uniform mixed raw material powder. The mixed powder is then ground and sieved. Then under the protection of flowing Ar atmosphere, carrying out hot-pressing sintering on the mixed powder to generate the B 4 And C, composite ceramic blocks.
Preferably, the method comprises the following steps:
(1) Will B 4 C powder and Al 2 O 3 Adding the powder into a ball milling tank, and uniformly mixing to obtain mixed slurry; and (5) drying to obtain mixed powder.
In mass ratio, B in the mixed powder 4 C accounts for 60% -90%, al 2 O 3 Accounting for 10 to 40 percent.
Preferably B 4 The particle size of the powder C is less than or equal to 0.5 mu m; preferably Al 2 O 3 The grain diameter of the powder is less than or equal to 2.0 mu m.
Preferably, a QM-BP planetary ball mill is used for high-energy ball milling.
Preferably, the materials of the grinding tank and the grinding balls of the high-energy ball mill are nylon and silicon carbide respectively.
Preferred ball milling parameters are: the ball milling medium is absolute ethyl alcohol; the weight ratio of the ball materials is 3:1; the rotating speed of the ball mill is 280-350 r/min, and the ball milling time is 18-36 h.
The preferred drying process is:
and (3) evaporating and drying the mixed slurry after ball milling at the temperature of between 60 and 70 ℃ for 12 to 24 hours in a constant temperature box, and volatilizing the ball milling medium.
(2) Grinding and sieving the mixed powder.
The preferred sieving process is: grinding and mashing the mixed powder in an agate mortar, and sieving with a sieve of 80-200 meshes.
(3) Under the protection of flowing Ar atmosphere, adopting a hot-pressing sintering system to carry out mixing powderSintering to obtain B 4 C/Al 2 O 3 A composite ceramic material.
Among them, the sintering process is preferable:
firstly, heating from room temperature to 1000 ℃ at a heating rate of 10-15 ℃/min; then the temperature rising rate is regulated to be 5-8 ℃/min, and the temperature is raised from 1000 ℃ to 1900-1950 ℃; the pressure is applied to be 30-40 MPa, the pressure is slowly increased from 1500 ℃ to the maximum value of 100-150 ℃ before the target temperature, and the heat preservation and the pressure maintaining are carried out for 1-3 h, thus obtaining B 4 C/Al 2 O 3 Composite ceramic blocks.
The present invention will be described in more detail with reference to the following examples.
Example 1:
in this embodiment, a B 4 The preparation method of the C composite ceramic material comprises the following steps:
(1) 90g of B having a particle size of 0.3 μm are reacted 4 C powder and 10g of Al having a particle size of 1.5 μm 2 O 3 Placing the powder into a ball milling tank, and adding grinding balls according to the ball material weight ratio of 3:1; ball milling is carried out for 24 hours in absolute ethyl alcohol under the rotating speed of 280r/min, and the mixed slurry is obtained after uniform mixing; and (3) placing the mixed slurry into an electrothermal constant-temperature blast drying oven, and drying at 60 ℃ for 24 hours to obtain mixed powder.
(2) Grinding the mixed powder, and sieving with 80 mesh sieve.
(3) Placing the powder in a graphite mold, uniformly brushing h-BN on the inner wall of the graphite mold, the inside and outside of a sleeve, an upper pressure head, a lower pressure head and the surface of a graphite gasket, and placing graphite paper between the powder and the graphite gasket; firstly, heating from room temperature to 1000 ℃ at a heating rate of 10 ℃/min; then heating from 1000 ℃ to 1950 ℃ at a heating rate of 8 ℃/min; hot pressing sintering temperature is 1950 ℃; the pressure is applied to be 30MPa, and the pressure is slowly increased from 1500 ℃ to 1850 ℃ to reach the maximum value; the sintering time was 1h with flowing Ar. Grinding and polishing the sintered sample to obtain the B of the embodiment of the invention 4 C/Al 2 O 3 A composite ceramic material.
The composite ceramic block prepared in this example 1 was prepared into a test sample and tested to obtain the following test results:
(1) The density of the composite ceramic material is 2.33g/cm 3 ；
(2) The relative density of the composite ceramic material is 88.9%;
(3) The Vickers hardness of the composite ceramic material is 12.4GPa;
(4) The bending strength of the composite ceramic material is 324MPa;
(5) The fracture toughness of the composite ceramic material is 4.99MPa m 1/2 。
As shown in FIG. 1, the composite ceramic material of example 1 has an X-ray diffraction pattern, and the phase composition of the composite material is B 4 C and Al 2 O 3 Indicating that no new phase is generated in the composite ceramic.
Example 2:
in this embodiment, a B 4 The preparation method of the C composite ceramic material comprises the following steps:
(1) 80g of B having a particle size of 0.2 μm were reacted 4 C powder and 20g of Al having a particle size of 1.0 μm 2 O 3 Placing the powder into a ball milling tank, and adding grinding balls according to the ball material weight ratio of 3:1; ball milling is carried out for 24 hours in absolute ethyl alcohol under the rotating speed of 285r/min, and mixed slurry is obtained; and (3) placing the mixed slurry into an electrothermal constant-temperature blast drying oven, and drying at 60 ℃ for 24 hours to obtain mixed powder.
(2) Grinding the mixed powder, and sieving with 80 mesh sieve.
(3) Placing the powder in a graphite mold, uniformly brushing h-BN on the inner wall of the graphite mold, the inside and outside of a sleeve, an upper pressure head, a lower pressure head and the surface of a graphite gasket, and placing graphite paper between the powder and the graphite gasket; firstly, heating from room temperature to 1000 ℃ at a heating rate of 10 ℃/min; then heating from 1000 ℃ to 1950 ℃ at a heating rate of 8 ℃/min, and hot-pressing sintering at 1950 ℃; the pressure is applied to be 30MPa, and the pressure is slowly increased from 1500 ℃ to 1820 ℃ to reach the maximum value; the sintering time was 1h with flowing Ar. Grinding and polishing the sintered sample to obtain the B of the embodiment of the invention 4 C/Al 2 O 3 A composite ceramic material.
The composite ceramic block prepared in this example 2 was prepared into a test sample and tested to obtain the following test results:
(1) The density of the composite ceramic material is 2.61g/cm 3 ；
(2) The relative density of the composite ceramic material is 96.1%;
(3) The Vickers hardness of the composite ceramic material is 22.9GPa;
(4) The bending strength of the composite ceramic material is 325MPa;
(5) The fracture toughness of the composite ceramic material is 3.12MPa m 1/2 。
As shown in fig. 2, the analysis result of the field emission Scanning Electron Microscope (SEM) microstructure map of the cross section of the composite ceramic material of example 2 is as follows:
preparing a composite ceramic block at 1950 ℃; the composite ceramic block is in a crystal-through and crystal-along mixed fracture mode, and the matrix and the second-phase crystal grains show cleavage characteristics; the second phase is tightly combined with the matrix, so that the strengthening and toughening effects of the second phase can be effectively exerted; effectively maintain B under the condition of obviously improving the fracture toughness of the composite ceramic 4 The C ceramic has excellent high hardness and low density, so that the composite ceramic block has excellent mechanical property.
Example 3:
in this embodiment, a B 4 The preparation method of the C composite ceramic material comprises the following steps:
(1) 60g of B having a particle size of 0.1 μm were reacted 4 C powder and 40g of Al having a particle size of 0.5 μm 2 O 3 Placing the powder into a ball milling tank, and adding grinding balls according to the ball material weight ratio of 3:1; ball milling is carried out for 24 hours in absolute ethyl alcohol under the rotating speed of 280r/min, and the mixed slurry is obtained after uniform mixing; and (3) placing the mixed slurry into an electrothermal constant-temperature blast drying oven, and drying at 60 ℃ for 24 hours to obtain mixed powder.
(2) Grinding the mixed powder, and sieving with 80 mesh sieve.
(3) Placing the powder in a graphite mold, uniformly brushing h-BN on the inner wall of the graphite mold, the inside and outside of a sleeve, an upper pressure head, a lower pressure head and the surface of a graphite gasket, and placing graphite paper between the powder and the graphite gasket; firstly, heating from room temperature to 1000 ℃ at a heating rate of 10 ℃/min; then the temperature is raised at a rate of 8 ℃/minThe rate is increased from 1000 ℃ to 1950 ℃ and the hot pressing sintering temperature is 1950 ℃; the pressure is applied to be 30MPa, and the pressure is slowly increased from 1500 ℃ to 1820 ℃ to reach the maximum value; the sintering time was 1h with flowing Ar. Grinding and polishing the sintered sample to obtain the B of the embodiment of the invention 4 C/Al 2 O 3 A composite ceramic material.
The composite ceramic block prepared in this example 3 was prepared into a test sample and tested to obtain the following test results:
(1) The density of the composite ceramic material is 2.90g/cm 3 ；
(2) The relative density of the composite ceramic material is 98.5%;
(3) The Vickers hardness of the composite ceramic material is 23.5GPa;
(4) The bending strength of the composite ceramic material is 336MPa;
(5) The fracture toughness of the composite ceramic material is 4.16MPa m 1/2 。
As shown in FIG. 3, the composite ceramic material of example 3 has an X-ray diffraction pattern, and the phase composition of the composite material is B 4 C and Al 2 O 3 Indicating that no new phase is generated in the composite ceramic.
In summary, embodiments of the invention are B 4 C/Al 2 O 3 Preparation method of composite ceramic material and prepared B 4 C/Al 2 O 3 The composite ceramic material has excellent mechanical properties. The invention uses Al 2 O 3 As an excellent toughening material, the fracture toughness of the alumina ceramic is more than or equal to 4.8 MPa.m 1/2 Can effectively improve B 4 Fracture toughness of C ceramic.
The foregoing is a further detailed description of the invention in connection with the preferred embodiments, and it is not intended that the invention be limited to the specific embodiments described. It will be apparent to those skilled in the art that several simple deductions or substitutions may be made without departing from the spirit of the invention, and these should be considered to be within the scope of the invention.
Claims (6)
1. B (B) 4 The preparation method of the C composite ceramic material is characterized by comprising the following steps:
step 1, B is 4 C powder and Al 2 O 3 Mixing the powder by wet high-energy ball milling, and drying to obtain mixed powder;
step 2, grinding and sieving the mixed powder;
step 3, hot-pressing and sintering the mixed powder under the protection of flowing Ar atmosphere to obtain B 4 C/Al 2 O 3 A composite ceramic material.
2. B according to claim 1 4 The preparation method of the C composite ceramic material is characterized in that in the step 1, B in the mixed powder is calculated according to the mass ratio 4 C accounts for 60% -90%, al 2 O 3 Accounting for 10 to 40 percent.
3. B according to claim 1 4 The preparation method of the C composite ceramic material is characterized in that in the step 1, B 4 The grain diameter of the C powder is less than or equal to 0.5 mu m, al 2 O 3 The grain diameter of the powder is less than or equal to 2.0 mu m.
4. B according to claim 1 4 The preparation method of the C composite ceramic material is characterized in that in the step 1, the materials of a grinding tank and a grinding ball of the high-energy ball mill are nylon and silicon carbide respectively, and the rotating speed of the high-energy ball mill is not lower than 280r/min.
5. B according to claim 1 4 The preparation method of the composite ceramic material is characterized in that in the step 2, the screen mesh with the particle size not less than 80 meshes is adopted after grinding.
6. B according to claim 1 4 The preparation method of the C composite ceramic material is characterized in that in the step 3, the hot-pressing sintering temperature is 1900-1950 ℃, the applied pressure is 30-40 MPa, the pressure is slowly increased from 1500 ℃ to 100-150 ℃ before the target temperature, the applied pressure reaches the maximum value, and the heat preservation and the pressure maintaining are carried out for 1-3 hours at the target temperature。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311190952.XA CN117263691A (en) | 2023-09-15 | 2023-09-15 | B (B) 4 Preparation method of C composite ceramic material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311190952.XA CN117263691A (en) | 2023-09-15 | 2023-09-15 | B (B) 4 Preparation method of C composite ceramic material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN117263691A true CN117263691A (en) | 2023-12-22 |
Family
ID=89213542
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202311190952.XA Pending CN117263691A (en) | 2023-09-15 | 2023-09-15 | B (B) 4 Preparation method of C composite ceramic material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN117263691A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN118637919A (en) * | 2024-08-09 | 2024-09-13 | 东北大学 | Method for preparing ceramic material from boron carbide grinding waste and application of ceramic material |
-
2023
- 2023-09-15 CN CN202311190952.XA patent/CN117263691A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN118637919A (en) * | 2024-08-09 | 2024-09-13 | 东北大学 | Method for preparing ceramic material from boron carbide grinding waste and application of ceramic material |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108484171B (en) | Boron carbide-titanium boride complex phase ceramic material and pressureless sintering preparation method thereof | |
| US11319618B2 (en) | Ti(C,N)-based superhard metal composite material and preparation method thereof | |
| CN110128146B (en) | Multifunctional boron carbide-based multiphase ceramic and reactive hot-pressing sintering preparation method thereof | |
| CN110396632A (en) | A kind of Ti (C, N) based ceramic metal and preparation method thereof with homogeneous ring core structure | |
| CN113817947B (en) | Coarse WC (wolfram carbide) grain reinforced superfine hard alloy and preparation method thereof | |
| CN112500178B (en) | ZrB generated in situ 2 -SiC toughened PcBN cutter and preparation method thereof | |
| CN115180960B (en) | Silicon nitride ceramic sintered body and preparation method thereof | |
| CN109400160A (en) | A kind of composite superhard material and its synthetic method | |
| CN117263691A (en) | B (B) 4 Preparation method of C composite ceramic material | |
| CN109180161B (en) | High-purity titanium silicon carbide/alumina composite material and preparation method thereof | |
| CN111777415B (en) | Boron carbide bulletproof material and preparation method thereof | |
| CN107513651B (en) | A kind of preparation method of titanium particle reinforced magnesium base composite material | |
| CN108411137A (en) | The preparation method of Ultra-fine Grained tungsten carbide base carbide alloy | |
| CN108314455B (en) | Silicon carbide ceramic and preparation method and application thereof | |
| CN115010496A (en) | Controllable B of performance 4 Preparation method of C-diamond composite material | |
| CN110877980A (en) | High-strength silicon carbide/silicon nitride composite ceramic and preparation method thereof | |
| CN113121238B (en) | High-performance boron carbide-based composite ceramic material and preparation method thereof | |
| CN101376931A (en) | Preparation of cemented carbide containing block tabular tungsten carbide crystal grain | |
| CN111995418B (en) | Preparation method of high-strength and high-toughness silicon carbide nanowire reinforced silicon carbide ceramic composite material | |
| CN111254336B (en) | Preparation method of WC-Ni hard alloy | |
| CN113816746A (en) | MAX-phase high-entropy ceramic matrix composite material and preparation method thereof | |
| CN116005084B (en) | W particle-TiB whisker hybridization reinforced titanium-based composite material and preparation method thereof | |
| CN103058660A (en) | High-strength and antioxidation zirconium carbide ceramic material and preparation method thereof | |
| CN113582698A (en) | Preparation method of ZrB2-SiC toughened B4C bulletproof piece | |
| Ovsyannikov et al. | High-hardness ceramics based on boron carbide fullerite derivatives |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |