CN112759408A - Boron carbide ceramic and preparation method and application thereof - Google Patents

Boron carbide ceramic and preparation method and application thereof Download PDF

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CN112759408A
CN112759408A CN202110002571.9A CN202110002571A CN112759408A CN 112759408 A CN112759408 A CN 112759408A CN 202110002571 A CN202110002571 A CN 202110002571A CN 112759408 A CN112759408 A CN 112759408A
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boron carbide
carbide ceramic
sintering
carbon
ceramic
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CN112759408B (en
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刘媛
薛平
董明
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Suzhou First Element Nano Technology Co ltd
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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
    • 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
    • C04B35/64—Burning or sintering processes
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F41—WEAPONS
    • F41H—ARMOUR; ARMOURED TURRETS; ARMOURED OR ARMED VEHICLES; MEANS OF ATTACK OR DEFENCE, e.g. CAMOUFLAGE, IN GENERAL
    • F41H5/00—Armour; Armour plates
    • F41H5/02—Plate construction
    • F41H5/04—Plate construction composed of more than one layer
    • F41H5/0414—Layered armour containing ceramic material
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F41—WEAPONS
    • F41H—ARMOUR; ARMOURED TURRETS; ARMOURED OR ARMED VEHICLES; MEANS OF ATTACK OR DEFENCE, e.g. CAMOUFLAGE, IN GENERAL
    • F41H5/00—Armour; Armour plates
    • F41H5/02—Plate construction
    • F41H5/04—Plate construction composed of more than one layer
    • F41H5/0414—Layered armour containing ceramic material
    • F41H5/0428—Ceramic layers in combination with additional layers made of fibres, fabrics or plastics
    • 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
    • C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
    • C04B2235/422—Carbon
    • C04B2235/427—Diamond
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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
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/52—Constituents or additives characterised by their shapes
    • C04B2235/5284—Hollow fibers, e.g. nanotubes
    • C04B2235/5288—Carbon nanotubes
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/66—Specific sintering techniques, e.g. centrifugal sintering
    • C04B2235/666—Applying a current during sintering, e.g. plasma sintering [SPS], electrical resistance heating or pulse electric current sintering [PECS]
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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    • 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
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    • 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

Abstract

A boron carbide ceramic and a preparation method and application thereof belong to the technical field of weaponry. The preparation method of the boron carbide ceramic comprises the steps of fully mixing boron carbide powder and carbon nano tubes according to a proportion, compacting and forming, then carrying out flash firing-plasma sintering, and generating nano-diamond in situ by at least part of the carbon nano tubes in the sintering process to obtain the boron carbide ceramic with uniformly distributed nano-carbon tubes and nano-diamond. The boron carbide ceramic prepared by the invention has the characteristics of high toughness, high hardness and high strength, can be used for bulletproof decks, and can resist multiple strikes of armor-piercing bullets and armor-piercing combustion bullets.

Description

Boron carbide ceramic and preparation method and application thereof
Technical Field
The invention relates to a technology in the field of weaponry, in particular to boron carbide ceramic and a preparation method and application thereof.
Background
Boron carbide has excellent performances of low density, high hardness, strength, elastic modulus and the like, and is more and more widely applied in the field of bulletproof armor. But the bending strength and fracture toughness are lower, and the brittleness is higher, so that the further application of the boron carbide ceramic is limited.
Japanese patent JP 5057327B2 (10/24/2012) utilizes Vapor Grown Carbon Fiber (VGCF) and Al2O3As a sintering aid and a toughening agent, the boron carbide ceramic obviously improves various physical indexes (Vickers hardness, bending strength and fracture toughness). However, in practical applications, it is difficult for VGCF or carbon nanotubes to form perfect uniform dispersion and distribution in the ceramic matrix. The non-uniformly dispersed VGCF or carbon nanotubes may cause a decrease in local hardness and bending strength of the ceramic, thereby seriously impairing the ability of the boron carbide ballistic ceramic to withstand multiple strikes by armor-piercing bullets.
The present invention has been made to solve the above-mentioned problems occurring in the prior art.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides the boron carbide ceramic and the preparation method and the application thereof, the defects of the boron carbide ceramic can be overcome, and the prepared composite bulletproof deck has good integral associativity and strong resistance to armor-piercing bullets and armor-piercing combustion bullets.
The invention relates to a preparation method of boron carbide ceramic, which comprises the steps of fully mixing boron carbide powder and carbon nano tubes in proportion, pressing and molding in a sintering device, then carrying out Flash combustion-plasma sintering (Flash-SPS) in an inert gas atmosphere or a vacuum environment, and generating nano diamond in situ by at least part of the carbon nano tubes in the sintering process to obtain the boron carbide ceramic;
the sintering device comprises a mold, an electrode pressure head and a pulse power supply, wherein the mold is annular and comprises a graphite foil, a boron nitride layer and a carbon fiber composite layer which are sequentially arranged from inside to outside; the graphite foil is used for controlling the shape of a product and conducting heat in the electric heating process, so that materials in the die are uniformly heated; the boron nitride layer is used as an electric insulating layer, and current is concentrated in a product area, so that the controllability of an electric heat generation process is ensured; the carbon fiber composite layer is used for high-temperature heat insulation and protects the product based on good thermal shock resistance of the carbon fiber composite layer.
Preferably, the particle size of the boron carbide powder is 0.5-5 μm; the carbon nanotube has a length of 5-20 μm and a diameter of 10-200 nm.
Preferably, the volume ratio of the boron carbide powder to the carbon nano tubes is 100: 5-20.
Preferably, the flash-plasma sintering conditions: the pressure is 80-200MPa, the voltage is 1-20V, the current is 1000-.
Preferably, the resulting nanodiamond has a particle size of 10 to 1000 nm.
The invention also relates to application of the boron carbide ceramic in a bulletproof ceramic composite deck, which can resist multiple strikes of armor-piercing bullets and armor-piercing combustion bullets.
Technical effects
Compared with the prior art, the invention has the following technical effects:
1) the carbon nano tubes are uniformly dispersed and have high difficulty and are easy to agglomerate, and in the flash combustion-plasma sintering process, the agglomerated carbon nano tubes generate nano diamonds in situ under the action of high pressure, high temperature and large current, the conversion ratio (volume ratio) is between 50 and 80 percent, so that the problem of non-uniform distribution of the carbon nano tubes as a reinforcing phase is solved;
2) the nano diamond synthesized by the carbon nano tube in situ can ensure that the reinforcing phase is combined with the boron carbide substrate more tightly, the wettability is better, the contact interface is cleaner, and diamond particles generated in situ are finer and distributed in the substrate to play a role in dispersion strengthening; therefore, the nano-diamond and the unreacted carbon nano-tube cooperatively enhance the boron carbide ceramic, so that the composite material has excellent comprehensive performance, can cut and destroy the incident armor-piercing warhead, weakens the penetrating strength of the armor-piercing warhead on the boron carbide ceramic, and protects the overall strength of the boron carbide ceramic;
3) the boron carbide ceramic has high bending strength and fracture toughness, and can meet the requirement of lightweight high-strength protective armor.
Drawings
FIG. 1a is a schematic diagram of a longitudinal cross-sectional structure of a flash-plasma sintering apparatus according to example 1;
FIG. 1b is a schematic diagram of the cross-sectional structure of a flash-plasma sintering apparatus in accordance with example 1;
FIG. 2 is an SEM photograph of the boron carbide ceramic of example 1;
FIG. 3 is a SAED diagram of the enlarged structure of FIG. 2;
FIG. 4a is a schematic diagram showing a longitudinal sectional structure of a conventional spark plasma sintering apparatus according to comparative example 1;
FIG. 4b is a schematic diagram showing a cross-sectional structure of a conventional spark plasma sintering apparatus according to comparative example 1;
FIG. 5 is an SEM photograph of the boron carbide ceramic of comparative example 1;
FIG. 6 is an SEM photograph of a mixed material in examples of the present invention and comparative examples;
FIG. 7 is a comparison of Raman spectra of boron carbide ceramics of example 1 and comparative example 1.
Detailed Description
The invention is described in detail below with reference to the drawings and the detailed description. The experimental procedures, in which specific conditions are not specified in the examples, were carried out according to the conventional methods and conditions.
Example 1
The boron carbide ceramic is sintered by the device shown in fig. 1a and 1B, a mixed material of boron carbide powder and carbon nano tubes is placed in a sintering die A, and an electrode pressure head B at two ends is pressed tightly, and then sintering is carried out. The sintering container A is provided with a graphite foil A1, a boron nitride layer A2 and a carbon fiber composite layer A3 in the order from the inside to the outside in the radial direction.
The embodiment relates to a flash-plasma sintering process of boron carbide ceramic, which comprises the following steps:
step 1, taking 1.75kg of boron carbide powder with the granularity of 0.5-25 mu m and 0.25kg of carbon nano tube (first element of Suzhou) with the length of 5-20 mu m and the diameter of 10-200nm, fully mixing to prepare a mixed material, wherein the volume ratio of the boron carbide powder to the carbon nano tube in the mixed material reaches 85: 15;
step 2, carrying out flash combustion-plasma sintering on the mixed material to obtain boron carbide ceramic; flash-plasma sintering conditions: the pressure is 80MPa, the direct current pulse voltage is 5V (12ms on, 2ms off), the current is 1000A, the heating rate is 100 ℃/min, the sintering temperature is 1500 ℃, the heat preservation time is 30min, the cooling rate is 10 ℃/min, and the vacuum condition is adopted.
The Vickers hardness of the boron carbide ceramic is 39GPa after testing; the density was 2.495g/cm3(archimedes method); and (3) crushing the ceramic, and testing the theoretical density of the ceramic powder by XRD (X-ray diffraction), wherein the calculated density is 99.5%.
FIG. 2 is an SEM photograph of a flash-plasma sintered boron carbide ceramic in which carbon nanotubes are in a diamond wire frame, and FIG. 3 is a SAED diagram of an enlarged structure in a rectangular wire frame in FIG. 2, and it can be seen that diamond [111] orientation occurs in the lightning plasma sintered product.
Comparative example 1
Sintering boron carbide ceramic by using the conventional plasma sintering device shown in fig. 4a and 4b, placing a mixed material of boron carbide powder and carbon nanotubes in a sintering mold a, pressing by using electrode pressing heads b at two ends, and sintering. The sintering mold a is sequentially provided with a graphite foil a1 and a graphite layer a2 from inside to outside along the radial direction, and the heat conduction effect is achieved.
The present embodiment relates to a general Spark Plasma Sintering (SPS) boron carbide ceramic, comprising the steps of:
step 1, taking 1.75kg of boron carbide powder with the granularity of 0.5-25 mu m and 0.25kg of carbon nano tube (first element of Suzhou) with the length of 5-20 mu m and the diameter of 10-200nm, fully mixing to prepare a mixed material, wherein the volume ratio of the boron carbide powder to the carbon nano tube in the mixed material reaches 85: 15;
step 2, sintering the mixed material by using common discharge plasma to obtain boron carbide ceramic; common discharge plasma sintering conditions: the boron carbide ceramic is prepared under the conditions of 40MPa of pressure, 5V of direct current voltage, 1000A of current, 100 ℃/min of heating rate, 1800 ℃ of sintering temperature, 30min of heat preservation time, 10 ℃/min of cooling rate and vacuum. Through testing, the Vickers hardness of the ceramic is 35 GPa; the density of the boron carbide ceramic is measured by an Archimedes method and is 2.434g/cm3(ii) a And (3) crushing the ceramic, and testing the theoretical density of the ceramic powder by XRD (X-ray diffraction) to calculate that the density is 99.5%.
Fig. 6 is an SEM photograph of the mixed material, from which it can be seen that the carbon nanotubes are relatively uniformly distributed in the boron carbide powder. After sintering, comparing fig. 2 (diamond wire frame, square wire frame) and fig. 5 (oval wire frame), it can be found that the boron carbide ceramic prepared in example 1 has a uniform distribution of the reinforcing phase (carbon nanotubes and nanodiamonds), while the boron carbide ceramic prepared in comparative example 1 has a relatively obvious local agglomeration phenomenon of the reinforcing phase carbon nanotubes; it is inferred that the in-situ generation of nanodiamonds by at least some of the carbon nanotubes in example 1 avoids the local agglomeration of the carbon nanotubes.
FIG. 7 is a graph comparing the Raman spectra of boron carbide ceramics of example 1 and comparative example 1, wherein a is the Raman spectrum of boron carbide ceramics of comparative example 1 and b is the Raman spectrum of boron carbide ceramics of example 1; the boron carbide ceramic of example 1 can be found at 1333cm-1A sharp diamond characteristic peak appears at 1581cm-1Where a broadband raman peak corresponding to the non-diamond carbon phase appears. The results show that part of the carbon nanotubes in the boron carbide ceramic sintered by flash combustion-plasma are converted into nano-diamonds, and the hardness, density and density of the ceramic are obviously improved; it can obviously improve the capability of the bulletproof deck to resist the strike of armor-piercing bullet/armor-piercing burning bullet for multiple times.
It is to be emphasized that: the above embodiments are only preferred embodiments of the present invention, and are not intended to limit the present invention in any way, and all simple modifications, equivalent changes and modifications made to the above embodiments according to the technical spirit of the present invention are within the scope of the technical solution of the present invention.

Claims (7)

1. The preparation method of the boron carbide ceramic is characterized in that boron carbide powder and carbon nano tubes are fully mixed according to a proportion, then the mixture is pressed and molded in a sintering device, and then flash-plasma sintering is carried out in an inert gas atmosphere or a vacuum environment, and nano diamond is generated in situ by at least part of the carbon nano tubes in the sintering process to obtain the boron carbide ceramic;
the sintering device comprises a mold, electrode pressure heads and a pulse power supply, wherein the mold is annular and comprises a graphite foil, a boron nitride layer and a carbon fiber composite layer which are sequentially arranged from inside to outside, the electrode pressure heads are arranged at two ends of the mold and electrically connected with the pulse power supply.
2. The method for preparing boron carbide ceramic according to claim 1, wherein the particle size of the boron carbide powder is 0.5 to 5 μm; the carbon nanotube has a length of 5-20 μm and a diameter of 10-200 nm.
3. The method for preparing boron carbide ceramic according to claim 1, wherein the volume ratio of the boron carbide powder to the carbon nanotubes is 100: 5-20.
4. The method for preparing boron carbide ceramic according to claim 1, wherein the flash-plasma sintering conditions are as follows: the pressure is 80-200MPa, the voltage is 1-20V, the current is 1000-.
5. The method for preparing boron carbide ceramic according to claim 1, wherein the nano-diamond has a particle size of 10 to 1000 nm.
6. A boron carbide ceramic produced by the production method according to any one of claims 1 to 5.
7. The boron carbide ceramic of claim 6 for use in ballistic resistant ceramic composite decks.
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CN114907126A (en) * 2022-04-29 2022-08-16 南京工程学院 Multi-dimensional nanocarbon structure TiB 2 -SiC-B 4 C-structure function integrated composite material and preparation method thereof
CN115448723A (en) * 2022-07-11 2022-12-09 中晶城康资源再生利用技术有限公司 Preparation method and application of boron carbide-based ceramic modified by magnesium-aluminum hydrotalcite
CN115536421A (en) * 2022-12-05 2022-12-30 湖南晶碳新材料有限公司 Process and equipment for producing carbon-carbon product by using processing waste
CN117105665A (en) * 2023-08-21 2023-11-24 扬州北方三山工业陶瓷有限公司 Preparation method of boron carbide ceramic with high thermal shock resistance for nuclear protection
CN117105665B (en) * 2023-08-21 2024-04-12 扬州北方三山工业陶瓷有限公司 Preparation method of boron carbide ceramic with high thermal shock resistance for nuclear protection

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CN115448723A (en) * 2022-07-11 2022-12-09 中晶城康资源再生利用技术有限公司 Preparation method and application of boron carbide-based ceramic modified by magnesium-aluminum hydrotalcite
CN115536421A (en) * 2022-12-05 2022-12-30 湖南晶碳新材料有限公司 Process and equipment for producing carbon-carbon product by using processing waste
CN117105665A (en) * 2023-08-21 2023-11-24 扬州北方三山工业陶瓷有限公司 Preparation method of boron carbide ceramic with high thermal shock resistance for nuclear protection
CN117105665B (en) * 2023-08-21 2024-04-12 扬州北方三山工业陶瓷有限公司 Preparation method of boron carbide ceramic with high thermal shock resistance for nuclear protection

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