CN100349824C - Boron carbide based bulletproof composite ceramic and preparation method thereof - Google Patents
Boron carbide based bulletproof composite ceramic and preparation method thereof Download PDFInfo
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- CN100349824C CN100349824C CNB200610042047XA CN200610042047A CN100349824C CN 100349824 C CN100349824 C CN 100349824C CN B200610042047X A CNB200610042047X A CN B200610042047XA CN 200610042047 A CN200610042047 A CN 200610042047A CN 100349824 C CN100349824 C CN 100349824C
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Abstract
The present invention relates to boron carbide based composite bulletproof ceramics and a preparation method thereof, which belongs to the technical field of a protective material. The boron carbide based composite bulletproof ceramics have the following components: 85 to 95 shares of boron carbide, 1 to 15 shares of silicon carbide whisker, 2 to 15 shares of silicon powder and 1 to 5 shares of boride all of which are in weight shares. The powder of the boron carbide, the silicon carbide whisker, the silicon powder and the boride use absolute alcohol as media, are mixed in a ball milling mode, and are dried under a vacuum condition to prepare mixed powder. The mixed powder is added in a graphite mould, and layers are separated by using graphite shims and graphite paper. The mixed powder is sintered in a hot pressing mode, temperature is 1700 to 2000DEG C, and pressure is 30 to 40MPa. The composite bulletproof ceramics of the present invention have the characteristics of low-density, high hardness, high strength and high elastic modulus. The present invention is an ideal ceramic material for the protection of aviation aircrafts and bulletproof clothes.
Description
(1) technical field
The present invention relates to a kind of low density carbonization boryl bulletproof composite ceramic and preparation method thereof, belong to the protective material technical field.
(2) background technology
In order to ensure the safety of aviation aircraft driver and crew in modern war; in the design of aviation aircraft, need high-performance, low-density stupalith to protect; in order to ensure the personnel safety of combatant in anti-terrorism, high-risk activity such as anti-riot, the lightweight bulletproof pottery also becomes the preferred material of preparation high performance ballistic clothing in addition.
The best stupalith that is used for aviation aircraft protection and flak jackets is norbide (B
4C) pottery.At present advanced country such as U.S. has been used for the boron carbide ceramics armour equipment of aircraft such as vertiplane.Boron carbide ceramics is as armor facing material require sintering under high temperature and high pressure.In order to reduce the sintering temperature of norbide, improve density, metallic aluminium, titanium carbide, wolfram varbide, TiB2, aluminum oxide or rare earth oxides etc. such as aluminium have been added in many researchs in norbide, but these technology have all reduced the hardness of boron carbide ceramics to some extent or have improved density.Deng builds hot pressed sintering under 2000~2150 ℃ high temperature such as new grade and has prepared the blast tube that silicon carbide whisker strengthens norbide, referring to Deng Jianxin etc., and " B
4C/SiC
wThe preparation of ceramic sand jet and the research of erosive wear mechanism thereof ", silicate circular, 2004,3,18~20.Chinese patent application CN1552667 discloses " manufacture method of boron carbide ceramics armour material and ceramic armour thereof ", and this boron carbide ceramics armour material is additive and the CeO that chooses any one kind of them by silicon carbide and boron carbide powder, Al-Y
2Or La
2O
3Form, prepare the armour material by being incubated 240~480 minutes sintering in 1750~2050 ℃ of argon gas.Chinese patent application CN1541981 discloses " preparation method of lightweight norbide armor ceramic "; this preparation method boron carbide powder of overflow sorting classifying; by the tablets press granulation; adopt single-phase no auxiliary agent hot pressing and sintering technique, two-way pressurization is carried out hot pressed sintering and has been prepared the norbide armor ceramic in the High Temperature High Pressure vacuum sintering furnace.
In norbide bulletproof ceramic preparation, still exist sintering temperature height, sintering time long at present, be unfavorable for the problem that mass production and product density are big.
(3) summary of the invention
The present invention is directed to the deficiencies in the prior art, boron carbide based bulletproof composite ceramic of a kind of low density high hardness and preparation method thereof is provided.
The present invention is matrix with the norbide, forms silicon hexaboride (SiB by adding boride and silica flour in sintering process
6) do not increase its density with the sintering temperature that reduces boron carbide ceramics; On the other hand by adding silicon carbide whisker (SiC
w) improve intensity, fracture toughness property and the Young's modulus of boron carbide ceramics, prepare a kind of norbide/silicon hexaboride/silicon carbide whisker (B of low density high hardness
4C/SiB
6/ SiC
w) bulletproof composite ceramic.
The component of boron carbide based bulletproof composite ceramic of the present invention is as follows: 85~95 parts of norbides, and 1~15 part of silicon carbide whisker, 2~15 parts of silica flours, 1~5 part of boride is weight part.
Above-mentioned norbide is a boron carbide powder, B
4C content>98%, d
50<3.5 μ m.
Above-mentioned silicon carbide (SiC) diameter of whiskers 0.1~1 μ m, long 30~100 μ m, SiC content>95%.
Described silica flour is d
50The technical pure silica flour of<3 μ m.
Described boride is selected from a kind of of boric acid, boron cash or metal boron.
Bulletproof composite ceramic preparation method of the present invention, step is as follows:
1, by weight, be medium with the dehydrated alcohol for 1~5 part with 85~95 parts of boron carbide powders, 1~15 part of silicon carbide whisker, 2~15 parts of silica flours and boride, ball milling mixes, vacuum condition oven dry down.The preparation mixed powder.
2, above-mentioned mixed powder is joined in the graphite jig, separate with Graphite pad and graphite paper between layer and the layer, the loadings of mixed powder is decided according to the thickness of required bulletproof ceramic.
3, the above-mentioned mould that powder is housed is put in the atmosphere that the hot pressing furnace inherence is protective gas with hydrogen, nitrogen or argon gas or hot pressed sintering in the vacuum, sintering temperature is 1700~2000 ℃, hot pressing pressure is 30~40MPa, and heat-insulation pressure keeping is 20~30 minutes under top temperature; Naturally cooling.
The present invention forms the sintering that silicon hexaboride promotes norbide by adding boride and silicon, reduces sintering temperature, increases the density of sintered compact; By adding the intensity and the toughness of silicon carbide whisker raising norbide; Prepared boron carbide based bulletproof composite ceramic has the characteristics of low density, high rigidity, high strength, high-fracture toughness and high elastic coefficient, and its crystallization phases is norbide, silicon hexaboride and silicon carbide.
The low density of boron carbide based bulletproof composite ceramic of the present invention, high rigidity, high strength, high-fracture toughness and high elastic coefficient characteristic realize by adding boride, silicon and silicon carbide whisker.Compared with prior art, bulletproof composite ceramic of the present invention has the characteristics of low density, high rigidity, high strength and high elastic coefficient, density≤2.6g/cm
3, Vickers' hardness Hv>27GPa, compressive strength>1.8GPa, flexural strength>400MPa, Young's modulus>300GPa, fracture toughness property>4.0MPa.m
1/2Boron carbide based bulletproof composite ceramic of the present invention is the desirable stupalith that is used for aviation aircraft protection and flak jackets.
(4) embodiment
The invention will be further described below in conjunction with embodiment, but be not limited thereto.
Embodiment 1: the component of bulletproof composite ceramic is as follows: 88 parts of boron carbide powders, and 6 parts of silicon carbide whiskers, 5 parts of silica flours, 3 parts of boric acid are weight part.Described boron carbide powder B
4C content>98%, d
50<3.5 μ m.Described silicon carbide (SiC) diameter of whiskers 0.1~1 μ m, long 30~100 μ m, SiC content>95%.Described silica flour is d
50The technical pure silica flour of<3 μ m.
Preparation method's step is as follows:
1, by above-mentioned weight part, be medium with the dehydrated alcohol with boron carbide powder, silicon carbide whisker, silica flour and boric acid, ball milling mixes, vacuum condition oven dry down.The preparation mixed powder.
2, above-mentioned mixed powder layering is joined in the graphite jig, separate with Graphite pad and graphite paper between layer and the layer.
3, the above-mentioned mould that powder is housed is put into hot pressed sintering in the hot pressing furnace, temperature is 1800 ℃, is protective gas with nitrogen; Hot pressing pressure is 40MPa, heat-insulation pressure keeping 30 minutes; Naturally cooling.Getting thickness is the bulletproof composite ceramic of 1cm.
The products obtained therefrom performance is as follows: density 2.5g/cm
3, Vickers' hardness Hv 30GPa, compressive strength 1.8GPa, flexural strength 500MPa, Young's modulus 350GPa, fracture toughness property 4.0MPa.m
1/2
Embodiment 2: as described in embodiment 1, different is that boride is the boron cash.
Embodiment 3: the component of bulletproof composite ceramic is as follows: 95 parts of boron carbide powders, and 15 parts of silicon carbide whiskers, 5 parts of silica flours, 2 parts of metal boron are weight part.
Preparation method's step is as follows:
1, by above-mentioned weight part, be medium with the dehydrated alcohol with boron carbide powder, silicon carbide whisker, silica flour and metal boron, ball milling mixes, vacuum condition oven dry down.The preparation mixed powder.
2, above-mentioned mixed powder is joined in the graphite jig, separate with Graphite pad and graphite paper between layer and the layer.
3, the above-mentioned mould that powder is housed is put into hot pressed sintering in the hot pressing furnace, temperature is 1900 ℃, is protective gas with the argon gas; Hot pressing pressure is 30MPa, heat-insulation pressure keeping 30 minutes; Naturally cooling.Getting thickness is the bulletproof composite ceramic of 0.5cm.
The products obtained therefrom performance is as follows: density 2.55g/cm
3, Vickers' hardness Hv 33GPa, compressive strength 1.8GPa, flexural strength 560MPa, Young's modulus 380GPa, fracture toughness property 5.0MPa.m
1/2
Embodiment 4: as described in embodiment 1, different is that step 3 hot pressed sintering temperature is 1800 ℃ among the preparation method, is protective gas with hydrogen; Hot pressing pressure is 40MPa, and heat-insulation pressure keeping is 20 minutes when top temperature; Naturally cooling.Getting thickness is the bulletproof composite ceramic of 1.2cm.
Claims (6)
1. bulletproof composite ceramic is characterized in that component is as follows: 85~95 parts of norbides, and 1~15 part of silicon carbide whisker, 2~15 parts of silica flours, 1~5 part of boride is weight part.
2. bulletproof composite ceramic as claimed in claim 1 is characterized in that described norbide is a boron carbide powder, B
4C content>98%, d
50<3.5 μ m.
3. bulletproof composite ceramic as claimed in claim 1 is characterized in that described silicon carbide whisker diameter 0.1~1 μ m, long 30~100 μ m, SiC content>95%.
4. bulletproof composite ceramic as claimed in claim 1 is characterized in that described silica flour is d
50The technical pure silica flour of<3 μ m.
5. bulletproof composite ceramic as claimed in claim 1 is characterized in that described boride is selected from a kind of of boric acid, boron cash or metal boron.
6. the preparation method of the described bulletproof composite ceramic of claim 1, step is as follows:
(1) by weight, be medium with the dehydrated alcohol for 1~5 part with 85~95 parts of boron carbide powders, 1~15 part of silicon carbide whisker, 2~15 parts of silica flours and boride, ball milling mixes, vacuum condition oven dry down, preparation mixed powder;
(2) above-mentioned mixed powder is joined in the graphite jig, separate with Graphite pad and graphite paper between layer and the layer, the loadings of mixed powder is decided according to the thickness of required bulletproof ceramic;
(3) the above-mentioned mould that powder is housed is put into hot pressed sintering in the hot pressing furnace, sintering temperature is 1700~2000 ℃, is protective gas with hydrogen, nitrogen or argon gas; Hot pressing pressure is 30~40MPa, heat-insulation pressure keeping 20~30 minutes; Naturally cooling.
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CN102464490B (en) * | 2010-11-17 | 2013-06-12 | 东北大学 | Method for preparing boron-carbide-based ceramic composite material |
CN102672187B (en) * | 2012-05-08 | 2013-08-14 | 哈尔滨工业大学 | Preparation methods of layered titanium matrix composite material |
FR2991981A1 (en) * | 2012-06-15 | 2013-12-20 | Saint Gobain Ct Recherches | SILICON CARBIDE PRODUCT FOR SHIELDING |
CN102786304B (en) * | 2012-07-28 | 2014-02-26 | 贵州木易精细陶瓷有限责任公司 | Preparation method for hot-pressed boron carbide ceramic |
CN103030396B (en) * | 2012-12-21 | 2014-10-01 | 武汉理工大学 | Boron carbide silicon carbide composite ceramic and preparation method thereof |
CN103145422B (en) * | 2013-03-06 | 2014-05-14 | 武汉理工大学 | High-hardness ceramic composite material of boron carbide-titanium boride-silicon carbide and preparation method thereof |
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CN108911773A (en) * | 2018-06-20 | 2018-11-30 | 浙江立泰复合材料股份有限公司 | A kind of preparation method of silicon carbide fibre enhancing boron carbide ceramics material |
CN108997015A (en) * | 2018-08-20 | 2018-12-14 | 宁夏昌杨科技有限公司 | A kind of boron carbide-based bulletproof ceramic composite material and preparation method |
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CN111777415B (en) * | 2020-07-10 | 2022-06-17 | 上海衡益特陶新材料有限公司 | Boron carbide bulletproof material and preparation method thereof |
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CN112723889B (en) * | 2021-02-05 | 2022-09-13 | 武汉理工大学 | High-strength and high-toughness boron carbide-titanium boride-graphene composite ceramic and preparation method thereof |
CN112851355A (en) * | 2021-03-09 | 2021-05-28 | 上海召明实业有限公司 | Pressureless sintering silicon carbide bulletproof ceramic and preparation method thereof |
CN113121237B (en) * | 2021-04-16 | 2023-06-02 | 合肥工业大学 | Boron carbide-based composite ceramic and preparation process thereof |
CN113121238B (en) * | 2021-04-16 | 2023-02-17 | 合肥工业大学 | High-performance boron carbide-based composite ceramic material and preparation method thereof |
CN115403386A (en) * | 2022-08-24 | 2022-11-29 | 佛山国防科技工业技术成果产业化应用推广中心 | Whisker-reinforced boron carbide composite ceramic and preparation method thereof |
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