CN108892525B - Preparation method of ceramic/ceramic hard bulletproof material - Google Patents

Preparation method of ceramic/ceramic hard bulletproof material Download PDF

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Publication number
CN108892525B
CN108892525B CN201810953436.0A CN201810953436A CN108892525B CN 108892525 B CN108892525 B CN 108892525B CN 201810953436 A CN201810953436 A CN 201810953436A CN 108892525 B CN108892525 B CN 108892525B
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ceramic
bulletproof material
prefabricated part
bulletproof
mixture
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CN108892525A (en
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曹海建
陈红霞
黄晓梅
季涛
杨维维
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Nantong University
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    • C04B35/806
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515Shaped 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
    • C04B35/56Shaped 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
    • C04B35/565Shaped 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 silicon carbide
    • C04B35/571Shaped 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 silicon carbide obtained from Si-containing polymer precursors or organosilicon monomers
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515Shaped 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
    • C04B35/56Shaped 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
    • C04B35/565Shaped 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 silicon carbide
    • C04B35/573Shaped 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 silicon carbide obtained by reaction sintering or recrystallisation
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/48Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins
    • C04B2235/483Si-containing organic compounds, e.g. silicone resins, (poly)silanes, (poly)siloxanes or (poly)silazanes

Abstract

The invention discloses a preparation method of a ceramic/ceramic hard bulletproof material, which comprises a bulletproof material prefabricated part and ceramic resin, wherein the bulletproof material prefabricated part is connected with the ceramic resin, the bulletproof material prefabricated part takes SiC ceramic fiber as a raw material, the bulletproof material prefabricated part is integrally prepared by a three-dimensional weaving process at one time, and the ceramic resin takes polycarbosilane/xylene resin as a matrix; the preparation method of the ceramic/ceramic hard bulletproof material provided by the invention comprises the steps of compounding the bulletproof material prefabricated part and the ceramic resin together, soaking and heating for many times, and finally carrying out heat treatment on the mixture consisting of the bulletproof material prefabricated part and the ceramic resin under the protection of inert gas.

Description

Preparation method of ceramic/ceramic hard bulletproof material
Technical Field
The invention relates to a high-performance fiber technical treatment and production technology, in particular to a preparation method of a ceramic/ceramic hard bulletproof material.
Background
Currently, bulletproof materials are mainly classified into three types, namely soft bulletproof materials, semi-hard bulletproof materials and hard bulletproof materials. The soft bulletproof material is mainly a fiber reinforced composite material prepared by taking high-performance fibers (aramid fibers, ultra-high molecular weight polyethylene fibers and the like) as raw materials, and is mainly used for protecting low-speed bullets (the bullet speed is about 500m/s, and the bullet type is mainly lead bullet). The general structure of the semi-hard bulletproof material is that hard materials (special steel, ceramic plates and the like) and high-performance fiber reinforced composite materials are compounded for use, and the semi-hard bulletproof material is mainly used for protecting high-speed bullets (the bullet speed is about 600m/s, and the bullet type is mainly steel core bullets). The hard bulletproof material mainly takes hard materials (special steel, ceramic plates and the like) as main materials and is mainly used for protecting high-speed and high-energy bullets (the bullet speed is about 700m/s, and the bullet type mainly takes steel core bullets and the like).
However, the development of the bulletproof material with ultrahigh bullet speed (the bullet speed is over 800m/s, and the bullet types comprise steel core bullets, armor piercing bullets and the like) is not very good in China at present. The existing bulletproof material has the problems that the bulletproof material is punctured, a bulletproof ceramic plate is fragile and is broken, and the surface density of the bulletproof material is large to cause heavy weight under the impact of a bullet with ultrahigh bullet speed, and meanwhile, the integrity of the bulletproof material cannot be ensured when the existing bulletproof material is impacted by multiple bullets simultaneously.
Disclosure of Invention
The invention aims to provide a preparation method of a ceramic/ceramic hard bulletproof material, and the bulletproof material prepared by the method has the advantages of light weight, high strength, high hardness, high compression strength, high bulletproof grade and good multiple bulletproof performance, so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
the preparation method of the ceramic/ceramic hard bulletproof material comprises a bulletproof material prefabricated part and ceramic resin, wherein the bulletproof material prefabricated part is connected with the ceramic resin, the bulletproof material prefabricated part takes SiC ceramic fiber as a raw material, the bulletproof material prefabricated part is integrally prepared by a three-dimensional weaving process in one step, and the ceramic resin takes polycarbosilane/xylene resin as a matrix.
Preferably: the bulletproof material prefabricated part is of a three-dimensional orthogonal, three-dimensional angle interlocking and other woven structures, the number of layers of SiC ceramic fibers is 3-15, and the volume content of the fibers is 40-65%.
A preparation method of a ceramic/ceramic hard bulletproof material comprises the following steps:
s1: placing SiC ceramic fibers in three-dimensional weaving equipment, wherein the three-dimensional weaving equipment adopts an integrated forming process to prepare a bulletproof material prefabricated part;
s2: sequentially putting the bulletproof material prefabricated part and ceramic resin into a steel high-pressure-resistant impregnation tank, closing an inlet of the steel high-pressure-resistant impregnation tank, adjusting the pressure in the steel high-pressure-resistant impregnation tank to 0.1-2MPa, and setting the impregnation time to be 5-15 min;
s3: taking out the mixture dipped in the previous step, putting the mixture consisting of the bulletproof material prefabricated part and the ceramic resin into a high-temperature sintering furnace, adjusting the pressure of the high-temperature sintering furnace to 20-30MPa, adjusting the temperature of the high-temperature sintering furnace to 1000-1500 ℃, sintering the mixture consisting of the bulletproof material prefabricated part and the ceramic resin in the high-temperature sintering furnace for 16-20h, and keeping the temperature for 1-1.5h instead of taking out the mixture at the first time after sintering;
s4: repeating the processes of the step S2 and the step S3 for 5-10 times in sequence;
s5: taking out the mixture consisting of the bulletproof material prefabricated part and the ceramic resin, and carrying out heat treatment on the mixture, wherein the heat treatment temperature is controlled to be 1500-2000 ℃, and the heat treatment time is controlled to be 1-1.5 h;
s6: and after the mixture of the bulletproof material prefabricated part and the ceramic resin is naturally cooled, taking out the mixture, and carrying out post-treatment on the mixture.
Preferably: in step S5, the mixture of the bulletproof material preform and the ceramic resin needs to be subjected to heat treatment under protection of inert gas.
Compared with the prior art, the invention has the beneficial effects that:
the preparation method of the ceramic/ceramic hard bulletproof material provided by the invention comprises the steps of compounding the bulletproof material prefabricated part and the ceramic resin together, soaking and heating for many times, and finally carrying out heat treatment on the mixture consisting of the bulletproof material prefabricated part and the ceramic resin under the protection of inert gas.
Detailed Description
The following examples will explain the present invention in detail, however, the present invention is not limited thereto. 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.
In the embodiment of the invention: a method for preparing a ceramic/ceramic hard bulletproof material comprises a bulletproof material prefabricated part and ceramic resin, wherein the bulletproof material prefabricated part is connected with the ceramic resin, the bulletproof material prefabricated part takes SiC ceramic fiber as a raw material, the SiC ceramic fiber takes an organic silicon compound as a raw material to prepare inorganic fiber with a beta-silicon carbide structure through spinning, carbonization or vapor deposition, the strength and the toughness of the SiC ceramic fiber are ensured, the bulletproof material prefabricated part is integrally prepared by adopting a three-dimensional weaving process at one time, the bulletproof material prefabricated part is in a three-dimensional orthogonal, three-dimensional angle interlocking and other woven structures, 3-15 layers of the SiC ceramic fiber have the fiber volume content of 40-65%, the three-dimensional structure in the bulletproof material prefabricated part can enhance the impact resistance, the multiple bulletproof performance and the compression resistance of the bulletproof material, and the ceramic resin takes polycarbosilane/xylene resin as a matrix, when the ceramic/ceramic hard bulletproof material is prepared, the bulletproof material prefabricated part and ceramic resin are required to be compounded together, so that the toughness of the bulletproof material can be enhanced while the hardness of the bulletproof material is ensured, and the bulletproof material can block the impact of high-speed bullets.
A preparation method of a ceramic/ceramic hard bulletproof material comprises the following steps:
the first step is as follows: the SiC ceramic fibers are placed in three-dimensional weaving equipment, the three-dimensional weaving equipment adopts an integrated forming process to prepare a bulletproof material prefabricated part, after the bulletproof material prefabricated part is prepared, the number of the SiC ceramic fibers in the bulletproof material prefabricated part is 3-15, the fiber volume content is 40-65%, and the three-dimensional structure in the bulletproof material prefabricated part can enhance the impact resistance, the multiple bulletproof performance and the compression resistance of the bulletproof material;
the second step is that: the bulletproof material prefabricated part and the ceramic resin are sequentially placed in a steel high-pressure-resistant impregnation tank, after an inlet of the steel high-pressure-resistant impregnation tank is closed, the pressure in the steel high-pressure-resistant impregnation tank is adjusted to be 0.1-2MPa, the impregnation time is set to be 5-15min, the bulletproof material prefabricated part and the ceramic resin are connected more tightly after high-pressure impregnation, and when a bullet flying at a high speed impacts the bulletproof material, the bulletproof material prefabricated part and the ceramic resin cannot be separated;
the third step: taking out the mixture dipped in the previous step, putting the mixture consisting of the bulletproof material prefabricated part and the ceramic resin into a high-temperature sintering furnace, adjusting the pressure of the high-temperature sintering furnace to 20-30MPa, adjusting the temperature of the high-temperature sintering furnace to 1000-1500 ℃, and sintering the mixture consisting of the bulletproof material prefabricated part and the ceramic resin in the high-temperature sintering furnace for 16-20h, namely, the step is the high-temperature sintering of the bulletproof material, so that the bulletproof material has the advantages of enhancing the hardness and the compactness of the bulletproof material, the mixture is not taken out at the first time after the sintering is finished, the heat is preserved for 1-1.5h, and the hardness and the compactness of the mixture consisting of the bulletproof material prefabricated part and the ceramic resin after the heat preservation treatment can be further improved;
the fourth step: repeating the second step and the third step for 5-10 times, namely repeatedly impregnating and sintering the mixture consisting of the bulletproof material prefabricated part and the ceramic resin at high temperature, and further enhancing the hardness and the compactness of the bulletproof material subjected to multiple impregnation and high-temperature sintering;
the fifth step: and taking out the mixture consisting of the bulletproof material prefabricated part and the ceramic resin, and carrying out heat treatment on the mixture, wherein the heat treatment temperature is controlled to be 1500-2000 ℃, and the heat treatment time is controlled to be 1-1.5h, wherein the heat treatment is carried out on the mixture consisting of the bulletproof material prefabricated part and the ceramic resin under the protection of inert gas, and the hardness and the compactness of the bulletproof material after the heat treatment meet the bulletproof requirements.
And a sixth step: and after the mixture of the bulletproof material prefabricated part and the ceramic resin is naturally cooled, taking out the mixture, and carrying out post-treatment on the mixture.
The preparation method of the ceramic/ceramic hard bulletproof material comprises a bulletproof material prefabricated part and ceramic resin, wherein the bulletproof material prefabricated part takes SiC ceramic fiber as a raw material, the SiC ceramic fiber takes an organic silicon compound as a raw material to prepare inorganic fiber with a beta-silicon carbide structure through spinning, carbonization or vapor deposition, the strength and the toughness of the SiC ceramic fiber are ensured, the bulletproof material prefabricated part is integrally prepared by adopting a three-dimensional weaving process, the bulletproof material prefabricated part has a three-dimensional orthogonal, three-dimensional angle interlocking and other woven structures, the number of layers of the SiC ceramic fiber is 3-15, the fiber volume content is 40-65%, the three-dimensional structure in the bulletproof material prefabricated part can enhance the impact resistance, the multiple bulletproof performance and the compression resistance of the bulletproof material, the ceramic resin takes polycarbosilane/xylene resin as a matrix, and the bulletproof material and the ceramic resin are compounded together, thus, the toughness of the bulletproof material can be enhanced while the hardness of the bulletproof material is ensured, so that the bulletproof material can block the impact of high-speed bullets.
The preparation steps of the ceramic/ceramic hard bulletproof material are as follows: firstly, preparing a bulletproof material prefabricated part by an integral forming process, wherein the number of SiC ceramic fiber layers in the bulletproof material prefabricated part is 3-15, the fiber volume content is 40-65%, and the three-dimensional structure in the bulletproof material prefabricated part can enhance the impact resistance, the multiple-shot prevention performance and the compression resistance of the bulletproof material; then the bulletproof material prefabricated part and the ceramic resin are sequentially placed in a steel high-pressure-resistant impregnation tank, the connection is tighter after high-pressure impregnation, and when a bullet flying at high speed impacts the bulletproof material, the situation that the bulletproof material prefabricated part is separated from the ceramic resin cannot occur; then the mixture composed of the preformed part of the bulletproof material and the ceramic resin is placed in a high-temperature sintering furnace for high-temperature sintering, so that the hardness and compactness of the bulletproof material are enhanced, the mixture is not taken out at the first time after sintering, and the heat is preserved for 1-1.5h, so that the hardness and compactness of the bulletproof material are further improved; the impregnation and high-temperature sintering process is repeated for 5-10 times in sequence, and the hardness and the compactness of the bulletproof material subjected to multiple times of impregnation and high-temperature sintering are further enhanced; finally, the mixture of the bulletproof material prefabricated member and the ceramic resin is subjected to heat treatment under the protection of inert gas, and the pottery/pottery hard bulletproof material prepared by the complete process has the advantages of light weight, high strength, high hardness, high compression strength, high bulletproof grade and good multiple bulletproof performance.
In conclusion, the preparation method of the ceramic/ceramic hard bulletproof material provided by the invention firstly prepares the bulletproof material prefabricated part with three-dimensional orthogonality and three-dimensional angle interlocking, the bulletproof material prefabricated part has good impact resistance, multiple bulletproof performance and compression resistance, the ceramic resin and the bulletproof material are compounded together, the bulletproof material compounded together is further soaked for multiple times and is subjected to high temperature, the hardness and the compactness of the bulletproof material can be further enhanced, and finally, the mixture formed by the bulletproof material prefabricated part and the ceramic resin is subjected to heat treatment under the protection of inert gas, and the ceramic/ceramic hard bulletproof material prepared by the complete process has the advantages of light weight, high strength, high hardness, high compression strength, high bulletproof grade and good multiple bulletproof performance, and is suitable for the protection of high-speed bullets.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (3)

1. A preparation method of a ceramic/ceramic hard bulletproof material comprises a bulletproof material prefabricated part and ceramic resin, and is characterized in that: the bulletproof material prefabricated part is connected with ceramic resin, the bulletproof material prefabricated part takes SiC ceramic fiber as a raw material, the bulletproof material prefabricated part is integrally prepared by adopting a three-dimensional weaving process in one step, and the ceramic resin takes polycarbosilane/xylene resin as a matrix;
the method comprises the following steps:
s1: placing SiC ceramic fibers in three-dimensional weaving equipment, wherein the three-dimensional weaving equipment adopts an integrated forming process to prepare a bulletproof material prefabricated part;
s2: sequentially putting the bulletproof material prefabricated part and the polycarbosilane/xylene resin matrix material into a steel high-pressure-resistant impregnation tank, closing an inlet of the steel high-pressure-resistant impregnation tank, adjusting the pressure in the steel high-pressure-resistant impregnation tank to 0.1-2MPa, and setting the impregnation time to be 5-15 min;
s3: taking out the mixture dipped in the previous step, putting the mixture consisting of the bulletproof material prefabricated part and the polycarbosilane/xylene resin matrix material into a high-temperature sintering furnace, adjusting the pressure of the high-temperature sintering furnace to 20-30MPa, adjusting the temperature of the high-temperature sintering furnace to 1000-1500 ℃, sintering the mixture consisting of the bulletproof material prefabricated part and the polycarbosilane/xylene resin matrix material in the high-temperature sintering furnace for 16-20h, and keeping the temperature for 1-1.5h instead of taking out the mixture at the first time after sintering;
s4: repeating the processes of the step S2 and the step S3 for 5-10 times in sequence;
s5: taking out the mixture consisting of the bulletproof material prefabricated part and the polycarbosilane/xylene resin matrix material, and carrying out heat treatment on the mixture, wherein the heat treatment temperature is controlled to be 1500-2000 ℃, and the heat treatment processing time is controlled to be 1-1.5 h;
s6: and after the mixture consisting of the bulletproof material prefabricated part and the polycarbosilane/xylene resin matrix material is naturally cooled, taking out the mixture, and carrying out post-treatment on the mixture.
2. The process for the preparation of a ceramic/ceramic ballistic material according to claim 1, characterized in that: the bulletproof material prefabricated part is of a three-dimensional orthogonal and three-dimensional angle interlocking woven structure, the number of layers of SiC ceramic fibers is 3-15, and the volume content of the fibers is 40-65%.
3. The method of claim 1, wherein the step S5 is performed under inert gas protection while the mixture of the preformed bulletproof material and the polycarbosilane/xylene resin matrix material is being heat treated.
CN201810953436.0A 2018-08-21 2018-08-21 Preparation method of ceramic/ceramic hard bulletproof material Active CN108892525B (en)

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Publication number Priority date Publication date Assignee Title
CN113061047B (en) * 2021-03-19 2022-11-25 南通大学 Ceramic/ceramic bulletproof material and preparation method thereof
CN114644528B (en) * 2022-03-30 2023-01-24 江苏东润安全科技有限公司 Hard material and preparation method and application thereof

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CN107383787A (en) * 2017-08-29 2017-11-24 湖北大地环保设备有限公司 A kind of resin fibre ceramic material and preparation method thereof
CN108253843A (en) * 2017-12-01 2018-07-06 中国航空工业集团公司基础技术研究院 A kind of preparation method of Continuous Fiber Reinforced Silicon Carbide armour

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Publication number Priority date Publication date Assignee Title
US6389594B1 (en) * 2001-08-30 2002-05-21 Israel Military Industries Ltd. Anti-ballistic ceramic articles
US7648757B2 (en) * 2005-01-04 2010-01-19 Rocky Research Penetration resistant composite
CN105906361A (en) * 2016-04-13 2016-08-31 南通大学 Preparation method of carbon or carbon composite bulletproof material
CN105948774A (en) * 2016-04-13 2016-09-21 南通大学 Preparation method for superhard carbon/carbon bulletproof material
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CN107383787A (en) * 2017-08-29 2017-11-24 湖北大地环保设备有限公司 A kind of resin fibre ceramic material and preparation method thereof
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