CN112174672A - Preparation method of boron carbide composite ceramic plate and bulletproof flashboard - Google Patents
Preparation method of boron carbide composite ceramic plate and bulletproof flashboard Download PDFInfo
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- 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
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- 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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- C04B35/626—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
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- C04B35/62695—Granulation or pelletising
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- 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
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Abstract
The invention provides a preparation method of a boron carbide composite ceramic plate and a boron carbide titanium alloy composite bulletproof flashboard. The preparation method of the boron carbide composite ceramic plate comprises the steps of selecting boron carbide powder as a raw material and a graphene material as a sintering aid, dispersing the graphene material by adopting a high-pressure homogenization process, adding the boron carbide powder and a graphene suspension into a three-roll grinding machine for mixing, granulating and drying to obtain granulated powder, finally filling the granulated powder into a graphite mold in a prefabricated shape, heating in two stages under a vacuum environment, introducing nitrogen while heating in the second stage, rapidly cooling to 2200 ℃ after heat preservation, and preserving the heat for 1-1.5 hours. The preparation method of the boron carbide composite ceramic plate can effectively promote the sintering densification of the boron carbide ceramic, can also avoid the overlarge grain growth of the boron carbide ceramic on a microscopic level, and can effectively improve the fracture toughness of the boron carbide ceramic plate.
Description
Technical Field
The invention relates to the technical field of bulletproof ceramics, in particular to a preparation method of a boron carbide composite ceramic plate. The invention also relates to a bulletproof flashboard applying the composite ceramic plate prepared by the preparation method of the boron carbide composite ceramic plate.
Background
Ceramic materials absorb energy through a process of microfracture. The capacity of the ceramic to absorb energy is related to the hardness and elastic modulus of the ceramic, and the larger the elastic modulus and the hardness of the ceramic, the smaller the density, the higher the anti-elastic energy, and the stronger the capacity of the ceramic to absorb kinetic energy. The high fracture toughness of the ceramic can delay the fracture time of the shot impacting the ceramic, improve the fracture energy consumption and the elastic resistance of the ceramic, and enhance the abrasion and the plough cutting action of the ceramic on the shot, thereby consuming more kinetic energy of the shot and improving the elastic resistance of the ceramic.
The density of boron carbide is the lowest of several commonly used armor ceramics, and the modulus of elasticity is higher, so that the boron carbide becomes the best choice for materials in the fields of military armor, body armor and space. The main problems of boron carbide ceramics are high price (about 10 times of that of aluminum oxide), high brittleness and low fracture toughness, and limit the application of the boron carbide ceramics in the fields of bulletproof armor and bulletproof inserting plates in a whole plate form as bulletproof ceramics. A great deal of research at home and abroad shows that the pure stoichiometric boron carbide is extremely difficult to sinter and densify, and the smaller the particle size of the boron carbide raw material is, the better the sintering and densification of the obtained boron carbide ceramic is mainly due to the fact that the covalent bond content is quite high (more than 90%). The sintering aid can effectively promote sintering densification and avoid overlarge ceramic grain size.
Disclosure of Invention
In view of this, the present invention is directed to a method for preparing a boron carbide composite ceramic plate, so as to improve fracture toughness of the boron carbide ceramic plate.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
a preparation method of a boron carbide composite ceramic plate comprises the following steps:
s1: selecting materials: selecting boron carbide powder with D50 less than 3um as a raw material and a graphene material as a sintering aid;
s2: preparing a graphene suspension: dissolving a dispersing auxiliary agent in water or alcohol to prepare a solution, then adding a graphene material into the solution, and dispersing for 1-24h by adopting a high-pressure homogenization process to obtain a graphene suspension with uniformly dispersed graphene; wherein the mass ratio of the graphene in the dispersion liquid is 1-10%, the sheet diameter D90 of the graphene in the prepared graphene suspension liquid is less than 1 mu m, and the number of layers is less than 10;
s3: adding the boron carbide powder obtained in the step S1 and the graphene suspension prepared in the step S2 into a three-roll grinding machine for mixing and grinding, wherein the roll speed ratio of a slow roll, a medium roll and a fast roll is 1:3:9, the speed of the slow roll is 10-30rpm, and the circular grinding is carried out for 5-8 times;
s4: adding the base material with uniform particle size distribution, good fluidity and moderate moisture content obtained in the step S3 into a granulator for granulation, wherein the particle size is 5-100 mu m, and then drying at the drying temperature of 100 and 110 ℃ to obtain granulated powder;
s5: and (2) filling the granulated powder into a graphite mold with a prefabricated shape, heating to 1000 ℃ in a first stage at the speed of 10-20 ℃/min in a vacuum environment, then heating to 2350 ℃ in a second stage at the speed of 5-15 ℃/min, introducing nitrogen while heating in the second stage, preserving heat for 10-30min, and then quickly cooling to 2200 ℃ and preserving heat for 1-1.5 h.
Further, the graphene material in the step S1 includes one or more of graphene oxide, functionalized graphene or graphene with a D50 of 10 μm to 20 μm.
Further, the dispersant in step S2 includes one or more of BYK-190, SN 5027 and Dego760W, CMC.
Compared with the prior art, the invention has the following advantages:
(1) the preparation method of the boron carbide composite ceramic plate can enable the graphene material to be distributed in the boron carbide ceramic more uniformly, so that the boron carbide ceramic sintering densification can be effectively promoted.
(2) The graphene material is a two-dimensional planar structure, and can be uniformly mixed with boron carbide to avoid the excessive growth of boron carbide ceramic grains on a microscopic layer, so that the fracture toughness of the boron carbide ceramic is effectively improved.
(3) Because the theoretical thickness of the graphene is only 0.37nm, the using amount of the graphene serving as a toughening agent is less than that of other carbon material toughening agents theoretically, and the thickness of the actual commercially available graphene material is below 10 layers after a dispersion process, so that the using amount of the toughening agent can be effectively reduced.
Another object of the present invention is to provide a bulletproof insert plate, which comprises a waterproof layer, a crack stopper layer, a bullet receiving layer, a transition layer, a titanium alloy bulletproof layer and a buffer layer in this order along a bullet receiving direction, wherein the bullet receiving layer is a multi-curved plate made of the boron carbide composite ceramic plate as claimed in claim 1.
Further, the waterproof layer adopts a polyurea nano coating or oxford waterproof cloth with the thickness of 0.5 mm.
Furthermore, the crack-stopping layer is made of aramid woven fabric.
Furthermore, the transition layer is made of aramid woven fabric.
Further, the buffer layer adopts a PE plate.
Further, the material of the bulletproof layer of the titanium alloy plate is Ti5322 or TC4 alloy.
Further, the thickness of the bulletproof layer of the titanium alloy plate is between 0.3 and 17 mm.
Compared with the prior art, the invention has the following advantages:
according to the bulletproof flashboard, the composite ceramic plate is prepared by adopting the preparation method of the boron carbide composite ceramic plate, and is applied to the bulletproof flashboard, so that the toughness of the ceramic can be effectively improved, and a small amount of graphene material is added to effectively guide micro cracks of the ceramic, so that the multi-shot resistance of the composite ceramic plate, namely the bulletproof flashboard, can be improved.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate an embodiment of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
fig. 1 is a schematic structural diagram of a bullet-facing layer prepared by a preparation method of a boron carbide composite ceramic plate according to an embodiment of the invention;
description of reference numerals:
1-boron carbide composite ceramic plate.
Detailed Description
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict.
The present invention will be described in detail below with reference to the embodiments with reference to the attached drawings.
Example one
The embodiment relates to a preparation method of a boron carbide composite ceramic plate, which comprises the following steps:
s1: selecting materials: selecting boron carbide powder with D50 less than 3um as a raw material and a graphene material as a sintering aid;
s2: preparing a graphene suspension: dissolving a dispersing auxiliary agent in water or alcohol to prepare a solution, then adding graphene into the solution, and dispersing for 1-24h by adopting a high-pressure homogenization process to obtain a graphene suspension with uniformly dispersed graphene; wherein the mass ratio of the graphene in the dispersion liquid is 1-10%, the sheet diameter D90 of the graphene in the prepared graphene suspension liquid is less than 1 mu m, and the number of layers is less than 10;
s3: adding the boron carbide powder obtained in the step S1 and the graphene suspension prepared in the step S2 into a three-roll grinding machine for mixing, wherein the roll speed ratio of a slow roll, a medium-speed roll and a fast roll is 1:3:9, the speed of the slow roll is 10-30rpm, and the materials are circularly ground for 5-8 times;
s4: adding the base material with uniform particle size distribution, good fluidity and moderate moisture content obtained in the step S3 into a granulator for granulation, wherein the particle size is 5-100 mu m, and then drying at the drying temperature of 100 and 110 ℃ to obtain granulated powder;
s5: and (2) filling the granulated powder into a graphite mold with a prefabricated shape, heating to 1000 ℃ in a first stage at the speed of 10-20 ℃/min in a vacuum environment, then heating to 2350 ℃ in a second stage at the speed of 5-15 ℃/min, introducing nitrogen while heating in the second stage, preserving heat for 10-30min, and then quickly cooling to 2200 ℃ and preserving heat for 1-1.5 h.
Wherein the graphene material in the step S1 comprises one or more of graphene oxide, functionalized graphene or graphene with D50 of 10-20 μm.
As a preferred embodiment, the dispersant in step S2 includes one or more of BYK-190, SN 5027, Dego760W, CMC. According to the preparation method of the boron carbide composite ceramic plate, the graphene can be dispersed more uniformly through a high-pressure homogenizing process, so that the graphene is in full contact with the boron carbide ceramic, the sintering densification of the boron carbide ceramic can be effectively promoted, meanwhile, the graphene and the boron carbide are mixed more uniformly through a three-roll grinding process, the phenomenon that boron carbide ceramic grains grow too large on a microscopic level can be avoided, and the fracture toughness of the boron carbide ceramic plate can be effectively improved.
Example two
This embodiment relates to a shellproof picture peg, follows and meets bullet direction and include the waterproof layer in proper order, the crack arrest layer, meets bullet layer, the transition layer, the shellproof layer of titanium alloy and buffer layer, and its major structure includes: the bullet facing layer is a multi-curved-surface plate made of the boron carbide composite ceramic plate in the first embodiment. Wherein, the waterproof layer adopts polyurea nanometer coating or oxford waterproof cloth with the thickness of 0.5 mm.
As a further improvement of this embodiment, the crack arrest layer is made of aramid woven fabric.
As a further improvement of this embodiment, the transition layer is made of aramid woven fabric.
As a further improvement of this embodiment, the buffer layer is made of a PE plate.
As a further improvement of this embodiment, the material of the bulletproof layer of the titanium alloy plate is Ti5322 or TC4 alloy.
As a further improvement of the embodiment, the thickness of the bulletproof layer of the titanium alloy plate is between 0.3 and 17 mm.
In addition, the preparation steps of the bulletproof flashboard are as follows:
according to the method, a mold with a certain shape is prefabricated on the size of the boron carbide composite ceramic plate in the step S5 in the embodiment I, and the titanium alloy composite material with the thickness of 0.3-1mm is molded in a rolling mode. The plugboard to be compounded is as follows: placing aramid fabric, ceramic plate, aramid fabric, titanium alloy plate, and PE plate in sequence, preheating in a vacuum autoclave for 0.5-3h at 80-150 deg.C, naturally cooling to room temperature, taking out, bonding with special glue, placing in a pressure container with pressure not less than 8 kg, and pressurizing for 24-48 h.
Compared with a ceramic plate compounded by carbon fiber, graphite and boron carbide in the prior art, the composite ceramic plate prepared by the preparation method in the application is greatly improved in performance, especially in fracture toughness of ceramic. See the data comparison in table one for details:
a first table:
as can be seen from the comparison of the data in the table, the fracture toughness of the composite ceramic plate prepared by the scheme is greatly improved.
In addition, when the composite ceramic plate prepared by the scheme is applied to bulletproof inserts, the specific data are detailed in a table II on the aspect of carrying out bulletproof effect test:
table two:
the data in the table show that the size, the thickness, the weight and the like of the bulletproof insert prepared by the scheme meet the manufacturing standards of WHB906-2015 and WHB917-2015, and the bulletproof insert is numbered and subjected to a gun striking test at the same time, and the result shows that the bulletproof insert can meet the acceptance conditions of WHB906-2015 and WHB917-2015 and has better bulletproof performance.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. A preparation method of a boron carbide composite ceramic plate is characterized by comprising the following steps: the method comprises the following steps:
s1: selecting materials: selecting boron carbide powder with D50 less than 3um as a raw material and a graphene material as a sintering aid;
s2: preparing a graphene suspension: dissolving a dispersing auxiliary agent in water or alcohol to prepare a solution, then adding a graphene material into the solution, and dispersing for 1-24h by adopting a high-pressure homogenization process to obtain a graphene suspension with uniformly dispersed graphene; wherein the mass ratio of the graphene in the dispersion liquid is 1-10%, the sheet diameter D90 of the graphene in the prepared graphene suspension liquid is less than 1 mu m, and the number of layers is less than 10;
s3: adding the boron carbide powder obtained in the step S1 and the graphene suspension prepared in the step S2 into a three-roll grinding machine for mixing, wherein the roll speed ratio of a slow roll, a medium-speed roll and a fast roll is 1:3:9, the speed of the slow roll is 10-30rpm, and the materials are circularly ground for 5-8 times;
s4: adding the base material with uniform particle size distribution, good fluidity and moderate moisture content obtained in the step S3 into a granulator for granulation, wherein the particle size is 5-100 mu m, and then drying at the drying temperature of 100 and 110 ℃ to obtain granulated powder;
s5: and (2) filling the granulated powder into a graphite mold with a prefabricated shape, heating to 1000 ℃ in a first stage at the speed of 10-20 ℃/min in a vacuum environment, then heating to 2350 ℃ in a second stage at the speed of 5-15 ℃/min, introducing nitrogen while heating in the second stage, preserving heat for 10-30min, and then quickly cooling to 2200 ℃ and preserving heat for 1-1.5 h.
2. The method for preparing a boron carbide composite ceramic plate according to claim 1, wherein: the graphene material in the step S1 comprises one or more of graphene oxide, functionalized graphene or graphene with D50 of 10-20 μm.
3. The method for preparing a boron carbide composite ceramic plate according to claim 1, wherein: the dispersant in step S2 includes one or more of BYK-190, SN 5027 and Dego760W, CMC.
4. The utility model provides a bulletproof flashboard, includes waterproof layer, crack arrest layer, meets bullet layer, transition layer, titanium alloy bulletproof layer and buffer layer, its characterized in that in proper order along meeting bullet direction: the ballistic layer is a multi-curved plate made of the boron carbide composite ceramic plate according to claim 1.
5. A ballistic protection panel according to claim 4, wherein: the waterproof layer adopts a polyurea nano coating or oxford waterproof cloth with the thickness of 0.5 mm.
6. A ballistic protection panel according to claim 4, wherein: the crack-stopping layer is made of aramid woven fabric.
7. A ballistic protection panel according to claim 4, wherein: the transition layer is made of aramid woven fabric.
8. A ballistic protection panel according to claim 4, wherein: the buffer layer adopts PE board.
9. A ballistic protection panel according to claim 4, wherein: the material of the bulletproof layer of the titanium alloy plate is Ti5322 or TC4 alloy.
10. A ballistic protection panel according to claim 4, wherein: the thickness of the bulletproof layer of the titanium alloy plate is between 0.3 and 17 mm.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113587728A (en) * | 2021-07-30 | 2021-11-02 | 浙江吉成新材股份有限公司 | Multi-elasticity-resistant multi-curved-surface boron carbide bulletproof plugboard and preparation method thereof |
| CN113788681A (en) * | 2021-10-12 | 2021-12-14 | 景德镇学院 | Boron carbide light bulletproof material and preparation method thereof |
| CN113880596A (en) * | 2021-11-04 | 2022-01-04 | 景德镇华迅特种陶瓷有限公司 | Preparation method of boron carbide individual-soldier plug board ceramic |
| CN114057489A (en) * | 2021-11-08 | 2022-02-18 | 景德镇华迅特种陶瓷有限公司 | Compound preparation method of boron carbide individual soldier plugboard |
| CN114216372A (en) * | 2021-11-23 | 2022-03-22 | 中航装甲科技有限公司 | Graphene composite bulletproof plate and preparation method thereof |
| CN115752097A (en) * | 2022-11-30 | 2023-03-07 | 中硼科技(威海)有限公司 | Boron carbide bulletproof flashboard and preparation method thereof |
| CN116003134A (en) * | 2022-12-09 | 2023-04-25 | 中航装甲科技有限公司 | Boron carbide-based composite material and preparation method and application thereof |
| WO2023113743A3 (en) * | 2021-12-15 | 2023-08-10 | Ondokuz Mayis Universitesi | Functionally graded multiphase new generation hybrid ballistic armour |
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