CN114394834A - Preparation method of boron carbide-based nano composite powder - Google Patents
Preparation method of boron carbide-based nano composite powder Download PDFInfo
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- CN114394834A CN114394834A CN202210159935.9A CN202210159935A CN114394834A CN 114394834 A CN114394834 A CN 114394834A CN 202210159935 A CN202210159935 A CN 202210159935A CN 114394834 A CN114394834 A CN 114394834A
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- 229910052580 B4C Inorganic materials 0.000 title claims abstract description 42
- 239000000843 powder Substances 0.000 title claims abstract description 34
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000002114 nanocomposite Substances 0.000 title claims description 7
- 150000003839 salts Chemical class 0.000 claims abstract description 23
- 239000002245 particle Substances 0.000 claims abstract description 21
- 239000002131 composite material Substances 0.000 claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 238000002156 mixing Methods 0.000 claims abstract description 17
- 239000000463 material Substances 0.000 claims description 21
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 20
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 20
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 10
- 238000000227 grinding Methods 0.000 claims description 10
- 239000011780 sodium chloride Substances 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 5
- 239000007795 chemical reaction product Substances 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000011033 desalting Methods 0.000 claims description 5
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 2
- 229910033181 TiB2 Inorganic materials 0.000 abstract description 26
- QYEXBYZXHDUPRC-UHFFFAOYSA-N B#[Ti]#B Chemical compound B#[Ti]#B QYEXBYZXHDUPRC-UHFFFAOYSA-N 0.000 abstract description 14
- 238000000034 method Methods 0.000 abstract description 14
- 238000005245 sintering Methods 0.000 abstract description 8
- 230000002349 favourable effect Effects 0.000 abstract description 4
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 230000007547 defect Effects 0.000 abstract description 2
- 238000009792 diffusion process Methods 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 230000001788 irregular Effects 0.000 abstract description 2
- 239000000376 reactant Substances 0.000 abstract description 2
- 230000035484 reaction time Effects 0.000 abstract description 2
- 238000013329 compounding Methods 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 238000001878 scanning electron micrograph Methods 0.000 description 6
- 239000000919 ceramic Substances 0.000 description 4
- 239000000654 additive Substances 0.000 description 3
- 238000001144 powder X-ray diffraction data Methods 0.000 description 3
- 238000005299 abrasion Methods 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- 208000012868 Overgrowth Diseases 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- 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
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- 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
- 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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- 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
- C04B2235/38—Non-oxide ceramic constituents or additives
- C04B2235/3804—Borides
- C04B2235/3813—Refractory metal borides
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- 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
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
- C04B2235/5454—Particle size related information expressed by the size of the particles or aggregates thereof nanometer sized, i.e. below 100 nm
Abstract
The invention discloses boron carbide-based composite powder and a preparation method thereof, wherein a molten salt method is adopted, and B is obtained by optimized raw material proportion and granularity selection and reasonable process condition design4C‑TiB2Composite powder of TiB2Nanoscale flaky particles are uniformly attached to B4The surface of the irregular particles is superior to the uniformity of the traditional mechanical mixing method; TiB2Is nano-scale flaky particles, has high sintering activity, is beneficial to forming a sintering neck at a lower temperature and overcomes the defect of B4C is a disadvantage of being difficult to sinter; the mass ratio of the prepared powder TiB2：（TiB2+B4C) And 5% -15%. The molten salt method is favorable for the diffusion of reactants, so that the products are uniformly distributed; the reaction temperature is reduced, the reaction time is shortened, the energy consumption is low and the efficiency is high; is favorable for the growth and development of the anisotropic structure. In preparation B4C‑TiB2In the process of compounding the powder, the solubility is removed by washingThe salt is recycled, and the process is environment-friendly and green.
Description
Technical Field
The invention relates to a ceramic composite material and a preparation method thereof, in particular to boron carbide-based composite powder and a preparation method thereof.
Background
Boron carbide (B)4C) As an important structural ceramic material, the high-hardness low-density high-strength ceramic material has high hardness, low density and high resistanceHigh temperature, abrasion resistance, excellent neutron absorption capacity and the like, and is widely applied to the fields of abrasion-resistant devices, bulletproof armor, aerospace, nuclear industry and the like.
However, B4More than 93% of material bonding property of C atom layer belongs to high-stability covalent bond, which results in high-density single-phase B4The sintering conditions of C are harsh, and the sintering temperature still needs to reach 2000 ℃ particularly under the condition of confining pressure. In order to increase the compactness of the material without affecting the excellent physical and mechanical properties of the material itself, additives are often used to improve the sinterability of B4C, to increase the surface energy and to prevent the overgrowth of grains, such as metallic Al, metallic Mo, elemental C, hexagonal boron nitride (h-BN), titanium diboride (TiB)2) And the like. Wherein, TiB2Has high melting point (2980 ℃), high material hardness (25-32 GPa), and moderate density (4.52 g/cm)3) And the conductive performance is good, and the like, and the additive used as the composite material can effectively improve the B content and improve the B content4The toughness of the C matrix can also be improved4The conductive property of C, thereby improving B4Processability of C (let B4C ceramics can be processed by an electric discharge process), and thus TiB2Is B4C composite ceramic excellent additive phase.
For particle dispersed toughened composites, if the matrix grains have a fine, uniform microstructure; the added phase crystal grains have nanometer sizes and are uniformly dispersed, so that the mechanical property of a final product can be improved. However, TiB2Nanopowders are difficult to prepare, expensive and poorly sinterable. Using micron-sized TiB2Ceramic powder added directly to B4The method of mixing and sintering the C powder requires high sintering temperature, and the obtained composite material has low density, coarse grain structure and uneven distribution, so that the product cannot achieve the expected excellent performance.
In order to solve the problems, the invention provides a method for preparing boron carbide-based composite powder by a molten salt method.
Disclosure of Invention
The invention aims to provide a preparation method of boron carbide-based composite powder.
The invention is realized by the following steps: a boron carbide-based composite powder and a preparation method thereof, 1) reacting material TiO2、B4C. Mixing carbon powder and molten salt, wherein the mass ratio of the reaction materials to the molten salt is 1:2-1: 5; the mass ratio of the reaction materials is TiO2：B4C：C= 160：472-2696：12；
2) Fully grinding and uniformly mixing in a grinding device, placing in a high-purity alumina crucible, and reacting for 5-8h at 1000-1200 ℃ in Ar atmosphere;
3) and fully washing the reaction product with deionized water, drying and desalting to obtain the boron carbide-based nano composite powder.
Further, the TiO2The grain diameter is 5-100 nm; b is4The grain diameter of C is 0.5-5 μm; the particle size of the carbon powder is as follows: 0.005-1.0 μm.
Further, the mass ratio of the reaction materials is preferably TiO2：B4C：C=160：611-1306:12。
Further, the molten salt is a mixture of KCl and NaCl, and the molar ratio of the KCl to the NaCl is 1: 1.
Further, the molten salt was dried at 120 ℃ for 12h before mixing with the reaction mass.
Compared with the prior art, the invention has the beneficial effects that:
preparation process of the invention gives B4C-TiB2Composite powder of TiB2Nanoscale flaky particles are uniformly attached to B4C, the surface of the irregular particles is uniformly distributed and is superior to the uniformity of the traditional mechanical mixing method; TiB2Is nano-scale flaky particles, has high sintering activity, is beneficial to forming a sintering neck at a lower temperature and overcomes the defect of B4C is a disadvantage of being difficult to sinter; the mass ratio of the prepared powder TiB2：（TiB2+B4C) And 5% -15%. The molten salt method is favorable for the diffusion of reactants, so that the products are uniformly distributed; the reaction temperature is reduced, the reaction time is shortened, the energy consumption is low and the efficiency is high; is favorable for the growth and development of the anisotropic structure. In preparation B4C-TiB2In the process of composite powder, soluble substances are removed by water washingAnd (4) the salt is recycled, and the process is environment-friendly and green.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are required to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is an SEM photograph of powder of example 1.
FIG. 2 is the powder XRD pattern of example 1.
FIG. 3 is an SEM image of powder of example 2.
FIG. 4 is the powder XRD pattern of example 2.
FIG. 5 is an SEM image of powder of example 3.
FIG. 6 is the powder XRD pattern of example 3.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings of the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
Example 1:
1) TiO reacting the reaction material2、B4C. Mixing carbon powder and molten salt, drying the molten salt at 120 ℃ for 12h before mixing the molten salt with the reaction material, wherein the mass ratio of the materials is TiO2：B4C: c: (KCl + NaCl) =160:2696:12:11472, molar ratio KCl: NaCl =1:1, TiO2Average particle diameter of 10nm, B4The average grain diameter of C is 1.5 μm, and the average grain diameter of carbon powder is: 0.015 μm.
2) Fully grinding and uniformly mixing in a grinding device, placing in a high-purity alumina crucible, and reacting for 6h at 1200 ℃ in Ar atmosphere;
3) fully washing the reaction product with deionized water, drying and desalting to obtain boron carbide-based nano composite powder with the powder mass ratio of TiB2：（TiB2+B4C) And = 5%. Fig. 1 and 2 are a SEM image and an XRD image of the powder of example 1, respectively. As can be seen from the SEM image, the nanoscale flaky particles are uniformly adhered to the irregularities B4The surface of the C particles is analyzed by XRD phase, and the nano-scale flaky particles are TiB2。
Example 2:
1) TiO reacting the reaction material2、B4C. Mixing carbon powder and molten salt, drying the molten salt at 120 ℃ for 12h before mixing the molten salt with the reaction material, wherein the mass ratio of the materials is TiO2：B4C: c: (KCl + NaCl) =160:843:12:4059, molar ratio KCl: NaCl =1:1, TiO2Average particle diameter of 10nm, B4The average grain diameter of C is 1.5 μm, and the average grain diameter of carbon powder is: 0.010 μm.
2) Fully grinding and uniformly mixing in a grinding device, placing in a high-purity alumina crucible, and reacting for 6h at 1100 ℃ in Ar atmosphere;
3) fully washing the reaction product with deionized water, drying and desalting to obtain boron carbide-based nano composite powder with the powder mass ratio of TiB2：（TiB2+B4C) And = 15%. Fig. 3 and 4 are SEM and XRD charts of the powder of example 2, respectively. As can be seen from the SEM image, the nanoscale flaky particles are uniformly adhered to the irregularities B4The surface of the C particles is analyzed by XRD phase, and the nano-scale flaky particles are TiB2。
Example 3:
1) TiO reacting the reaction material2、B4C. Mixing carbon powder and molten salt, drying the molten salt at 120 ℃ for 12h before mixing the molten salt with the reaction material, wherein the mass ratio of the materials is TiO2：B4C: c: (KCl + NaCl) =160:1306:12:5912, molar ratio KCl: NaCl =1:1, TiO2Average particle diameter of 10nm, B4The average grain diameter of C is 1.5 μm, and the average grain diameter of carbon powder is: 0.010 μm.
2) Fully grinding and uniformly mixing in a grinding device, placing in a high-purity alumina crucible, and reacting for 6h at 1000 ℃ in Ar atmosphere;
3) fully washing the reaction product with deionized water, drying and desalting to obtain boron carbide-based nano composite powder with the powder mass ratio of TiB2：（TiB2+B4C) = 10%. Fig. 5 and 6 are SEM and XRD charts of the powder of example 3, respectively. As can be seen from the SEM image, the nanoscale flaky particles are uniformly adhered to the irregularities B4The surface of the C particles is analyzed by XRD phase, and the nano-scale flaky particles are TiB2。
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (5)
1. A boron carbide-based composite powder and a preparation method thereof are characterized in that:
1) TiO reacting the reaction material2、B4C. Mixing carbon powder and molten salt, wherein the mass ratio of the reaction materials to the molten salt is 1:2-1: 5; the mass ratio of the reaction materials is TiO2：B4C：C= 160：472-2696：12；
2) Fully grinding and uniformly mixing in a grinding device, placing in a high-purity alumina crucible, and reacting for 5-8h at 1000-1200 ℃ in Ar atmosphere;
3) and fully washing the reaction product with deionized water, drying and desalting to obtain the boron carbide-based nano composite powder.
2. The boron carbide-based composite powder according to claim 1, characterized in that: the TiO is2The grain diameter is 5-100 nm; b is4The grain diameter of C is 0.5-5 μm; the particle size of the carbon powder is as follows: 0.005-1.0 μm.
3. The boron carbide-based composite powder according to claim 1, and the boron carbide-based composite powderThe preparation method is characterized by comprising the following steps: the mass ratio of the reaction materials is TiO2：B4C：C=160：611-1306:12。
4. The boron carbide-based composite powder according to claim 3, characterized in that: the molten salt is a mixture of KCl and NaCl, and the molar ratio of KCl to NaCl is 1: 1.
5. The boron carbide-based composite powder according to claim 1, characterized in that: the molten salt was dried at 120 ℃ for 12h before being mixed with the reaction mass.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116813363A (en) * | 2023-05-15 | 2023-09-29 | 北京航空航天大学 | Antioxidant SiC f /SiC-HfB 2 Preparation method of composite material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116813363A (en) * | 2023-05-15 | 2023-09-29 | 北京航空航天大学 | Antioxidant SiC f /SiC-HfB 2 Preparation method of composite material |
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