CN115594506A - Method for rapidly producing sphere-like boron carbide ceramic powder - Google Patents
Method for rapidly producing sphere-like boron carbide ceramic powder Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 68
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 229910052580 B4C Inorganic materials 0.000 title claims abstract description 54
- 239000000919 ceramic Substances 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 26
- 238000002156 mixing Methods 0.000 claims abstract description 17
- 238000000498 ball milling Methods 0.000 claims abstract description 14
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052796 boron Inorganic materials 0.000 claims abstract description 12
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 12
- 238000007664 blowing Methods 0.000 claims abstract description 10
- 230000006698 induction Effects 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000002347 injection Methods 0.000 claims abstract description 8
- 239000007924 injection Substances 0.000 claims abstract description 8
- 239000011812 mixed powder Substances 0.000 claims abstract description 4
- 238000005507 spraying Methods 0.000 claims abstract description 4
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 24
- 229910052786 argon Inorganic materials 0.000 claims description 12
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical group O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims description 9
- 239000006229 carbon black Substances 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 6
- 239000002006 petroleum coke Substances 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 238000003801 milling Methods 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 abstract description 7
- 238000005469 granulation Methods 0.000 abstract description 6
- 230000003179 granulation Effects 0.000 abstract description 6
- 239000007921 spray Substances 0.000 abstract description 6
- 239000002994 raw material Substances 0.000 abstract description 3
- 238000007751 thermal spraying Methods 0.000 abstract description 3
- 238000001514 detection method Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000004992 fission Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000013332 literature search Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 238000007750 plasma spraying Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
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- 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
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- 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
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
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- 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
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
- C04B35/6265—Thermal treatment of powders or mixtures thereof other than sintering involving reduction or oxidation
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- 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
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
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- 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
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3409—Boron oxide, borates, boric acids, or oxide forming salts thereof, e.g. borax
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- 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
- C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
- C04B2235/422—Carbon
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- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
- C04B2235/422—Carbon
- C04B2235/424—Carbon black
Abstract
The invention discloses a method for rapidly producing spheroidal boron carbide ceramic powder, which comprises the following steps of mixing a carbon source and a boron source according to a mass ratio of 1:2.8, mixing materials, namely putting the mixed powder into a ball mill to be uniformly mixed, wherein the ball milling time is 12-16h, and the rotating speed is 100-300r/min; and taking out the powder after ball milling and mixing, drying, spraying and granulating to obtain powder of 45-100 mu m, blowing the powder into an induction plasma device, performing high-temperature treatment, and collecting to obtain the spheroidal boron carbide powder of 15-25 mu m. The invention provides a method for rapidly preparing boron carbide ceramic powder, which forms spheroidal boron carbide ceramic powder by directly carrying out plasma injection on spray granulation, realizes rapid and efficient preparation of the spheroidal boron carbide ceramic powder, has the advantages of purity higher than 98%, good fluidity, high hardness, convenience for ceramic forming, and can be used in the ceramic field and also be directly used as a thermal spraying raw material.
Description
Technical Field
The invention relates to the technical field of ceramic production, in particular to a method for quickly producing spheroidal boron carbide ceramic powder.
Background
Boron carbide is an important high-temperature wear-resistant material in high-performance ceramic materials, and is used as superhard boron carbide (B4C) ceramic with a third hardness value, due to the characteristics of high Young modulus, low fracture toughness and the like of the boron carbide ceramic, the crystal structure of B4C is an rhombohedra, and due to the fact that B atoms and C atoms in B4C exist in a B-C covalent bond form, the self-diffusion coefficient of B4C is low, grain boundaries are difficult to move, and high-density sintering is difficult to realize.
The boron carbide ceramic has the characteristics of low density, high hardness, high melting point, excellent chemical stability, good neutron absorption interface and the like, and can be widely applied to the aspects of abrasive cutting, coating materials, light armors, nuclear fission control and the like. When the bullet is resisted to impact, compared with other materials, the boron carbide is not easy to generate plastic deformation, the bullet can be passivated or broken by depending on the characteristics of the boron carbide, and cracks can be generated on the surface of the boron carbide to absorb energy generated when the bullet impacts at high speed. The boron carbide material can replace diamond material in some fields, and the production cost is effectively reduced. The alloy can be used as mechanical tools such as boron carbide coating cutters and the like due to the characteristics of high hardness, wear resistance, radiation resistance and the like. The development of the special boron carbide ceramic as one of novel materials also puts new requirements on the preparation of ceramic powder materials, the boron carbide powder is a material guarantee for preparing the ceramic, and the common methods for preparing the boron carbide powder at present comprise a carbothermic reduction method, a self-propagating high-temperature synthesis method, a chemical vapor deposition method, a sol-gel method and the like.
Through the literature search of the prior art, chinese patent with publication No. CN 106744968A discloses a preparation method for preparing high-purity boron carbide powder by a solid phase method. The method has the following defects: the preparation process is complicated, the energy consumption is increased by heating for many times, and the green and high efficiency are not facilitated. The document retrieval also shows that Chinese patent with publication number CN 113548667B discloses a method for rapidly preparing superfine boron carbide powder under low temperature by current assistance, and the defects of the method are as follows: after the current-assisted low-temperature rapid preparation of the superfine boron carbide powder, the grinding, pickling, suction filtration and drying treatment are still carried out, so that the process is complicated and is not beneficial to large-scale production.
Disclosure of Invention
The invention aims to provide a method for quickly producing spheroidal boron carbide ceramic powder to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a method for rapidly producing spheroidal boron carbide ceramic powder comprises the following steps of mixing a carbon source and a boron source according to a mass ratio of 1:2.8, mixing materials, namely putting the mixed powder into a ball mill to be uniformly mixed, wherein the ball milling time is 12-16h, and the rotating speed is 100-300r/min; taking out the powder after ball milling and mixing, drying, spraying and granulating to obtain 45-100 mu m powder, blowing the powder into an induction plasma device, treating at 6000-7000 ℃ by plasma, and collecting to obtain 15-25 mu m spheroidal boron carbide powder.
Preferably, the purity of the carbon source is greater than 99.7% and the purity of the boron source is greater than 98%.
Preferably, the carbon source is one of carbon black and petroleum coke, and the boron source is diboron trioxide.
Preferably, the ball milling medium of the ball mill is absolute ethyl alcohol, and the milling balls are agate balls.
Preferably, the powder injection speed of powder injection entering the induction plasma device is 8-12kg/h, the working gas is argon, and the argon flow is 60-100L/min.
Compared with the prior art, the invention has the following beneficial effects:
the invention provides a method for rapidly preparing boron carbide ceramic powder, which forms spheroidal boron carbide ceramic powder by directly carrying out plasma injection on spray granulation, realizes rapid and efficient preparation of the spheroidal boron carbide ceramic powder, has the advantages of purity higher than 98%, good fluidity, high hardness, convenience for ceramic forming, and can be used in the ceramic field and also be directly used as a thermal spraying raw material.
Drawings
Further details, features and advantages of the invention are disclosed in the following description of exemplary embodiments with reference to the accompanying drawings, in which:
FIG. 1 shows a schematic diagram of the structure of an inductive plasma device of the present invention;
FIG. 2 shows a micro cross-sectional profile of a boron carbide ceramic according to a second embodiment of the present invention;
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below with reference to specific embodiments, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The method for rapidly producing the spheroidal boron carbide ceramic powder comprises the following steps of: 2.8, mixing materials, namely putting the mixed powder into a ball mill to be uniformly mixed, wherein the ball milling time is 12-16h, and the rotating speed is 100-300r/min; and taking out the powder after ball milling and mixing, drying, spraying and granulating to obtain 45-100 mu m powder, blowing the powder into an induction plasma device, treating at 6000-7000 ℃ by plasma, and collecting to obtain 15-25 mu m spheroidal boron carbide powder.
Furthermore, the purity of the carbon source is more than 99.7%, and the purity of the boron source is more than 98%.
Further, the carbon source is one of carbon black and petroleum coke, and the boron source is diboron trioxide.
Furthermore, the ball milling medium of the ball mill is absolute ethyl alcohol, and the milling balls are agate balls.
Furthermore, the powder injection speed of the powder injection entering the induction plasma device is 8-12kg/h, the working gas is argon, and the argon flow is 60-100L/min.
Example 1:
the embodiment provides a method for rapidly preparing boron carbide ceramic powder, which comprises the following steps: selecting carbon black and petroleum coke as carbon sources, boron oxide (B2O 3) as a boron source, mixing according to the mass ratio of 1.
And taking out the powder after ball milling and mixing, drying, carrying out spray granulation to obtain powder of 45-100 mu m, blowing the powder into an induction plasma device, wherein the blowing powder feeding speed is 8kg/h, the working gas is argon, the argon flow is 100L/min, and collecting the obtained spherical-like boron carbide powder of 15-25 mu m after treatment at the temperature of 6000-7000 ℃ by plasma.
The detection proves that the purity of the boron carbide is more than 99%.
Example 2:
the embodiment provides a method for rapidly preparing boron carbide ceramic powder, which comprises the following steps: selecting carbon black and petroleum coke as carbon sources, boron oxide (B2O 3) as a boron source, mixing according to the mass ratio of 1.
And taking out the powder after ball milling and mixing, drying, carrying out spray granulation to obtain powder of 45-100 mu m, blowing the powder into an induction plasma device, wherein the blowing powder feeding speed is 12kg/h, the working gas is argon, the argon flow is 60L/min, and collecting the obtained spherical-like boron carbide powder of 15-25 mu m after treatment at the temperature of 6000-7000 ℃ by plasma.
The detection proves that the purity of the boron carbide is more than 98.6 percent.
Example 3:
the embodiment provides a method for rapidly preparing boron carbide ceramic powder, which comprises the following steps: selecting carbon black and petroleum coke as carbon sources, boron oxide (B2O 3) as a boron source, mixing according to the mass ratio of 1.
And taking out the powder after ball milling and mixing, drying, carrying out spray granulation to obtain powder of 45-100 mu m, blowing the powder into an induction plasma device, wherein the blowing powder feeding speed is 10kg/h, the working gas is argon, the argon flow is 80L/min, and collecting the obtained spherical-like boron carbide powder of 15-25 mu m after treatment at the temperature of 6000-7000 ℃ by plasma.
The detection proves that the purity of the boron carbide is more than 98 percent.
The microscopic cross-sectional topography (SEM) of the boron carbide ceramic obtained in example 2 of the invention is shown in figure 2, and it can be seen that the prepared boron carbide ceramic powder has a uniform structure.
In conclusion, the invention provides a method for rapidly preparing boron carbide ceramic powder, which forms spheroidal boron carbide ceramic powder by direct plasma injection of spray granulation, realizes rapid and efficient preparation of the spheroidal boron carbide ceramic powder, has the purity of more than 98 percent, can be used in the ceramic field and can also be directly used as a thermal spraying raw material, and the rapid plasma spraying method adopted by the invention is more environment-friendly and efficient.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (5)
1. A method for rapidly producing sphere-like boron carbide ceramic powder is characterized by comprising the following steps,
mixing a carbon source and a boron source according to a mass ratio of 1:2.8, mixing materials, namely putting the mixed powder into a ball mill to be uniformly mixed, wherein the ball milling time is 12-16h, and the rotating speed is 100-300r/min;
and taking out the powder after ball milling and mixing, drying, spraying and granulating to obtain 45-100 mu m powder, blowing the powder into an induction plasma device, treating at 6000-7000 ℃ by plasma, and collecting to obtain 15-25 mu m spheroidal boron carbide powder.
2. The method for rapidly producing the sphere-like boron carbide ceramic powder according to claim 1, wherein the purity of the carbon source is more than 99.7%, and the purity of the boron source is more than 98%.
3. The method for rapidly producing the spheroidal boron carbide ceramic powder according to claim 2, wherein the carbon source is one of carbon black and petroleum coke, and the boron source is diboron trioxide.
4. The method for rapidly producing the sphere-like boron carbide ceramic powder according to claim 1, wherein the ball milling medium of the ball mill is absolute ethyl alcohol, and the milling balls are agate balls.
5. The method for rapidly producing the sphere-like boron carbide ceramic powder according to claim 1, wherein the powder injection rate of the powder injected into the induction plasma device is 8-12kg/h, the working gas is argon, and the argon flow is 60-100L/min.
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|---|---|---|---|---|
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2022
- 2022-10-26 CN CN202211327556.2A patent/CN115594506A/en active Pending
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