CN101830703B - Carbon fiber reinforced boron carbide composite material and preparation method thereof - Google Patents
Carbon fiber reinforced boron carbide composite material and preparation method thereof Download PDFInfo
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- CN101830703B CN101830703B CN2010101398802A CN201010139880A CN101830703B CN 101830703 B CN101830703 B CN 101830703B CN 2010101398802 A CN2010101398802 A CN 2010101398802A CN 201010139880 A CN201010139880 A CN 201010139880A CN 101830703 B CN101830703 B CN 101830703B
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- boron carbide
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Abstract
The invention relates to a carbon fiber reinforced boron carbide composite material and a preparation method thereof. The preparation method comprises the following steps of: preparing a carbon fiber preform by adopting a needling, puncturing or three-dimensional weaving process; and depositing boron carbide matrix in the porous carbon fiber preform by osmosis to form the compact carbon fiber reinforced boron carbide composite material. Aiming at a certain specific application environment, a boron carbide coat can be deposited on the surface of a sample by adopting the same chemical vapor osmosis process. The carbon fiber reinforced boron carbide-based composite material manufactured by the method has the characteristics of good mechanical property, toughness superior to that of the traditional sintered boron carbide, compact structure, light weight, abrasion resistance and high hardness, and is suitable to be applied to a high-temperature light structural component.
Description
Technical field
The invention belongs to chemical industry and field of materials, be specifically related to a kind of carbon fiber reinforced boron carbide composite material and preparation method thereof.
Background technology
Norbide is a kind of special cermacis of excellent property, and its density is 2.4-2.5g/cm
3, fusing point is greater than 2400 ℃, and Vickers' hardness be only second to diamond and cubic boron nitride, and hot hardness is better than diamond and cubic boron nitride greater than 3000, therefore is particularly suitable for structured material parts such as lightweight high temperature nozzle, lightweight bulletproof plate armour.Simultaneously, norbide is widely used in the nucleus screening parts because having high neutron-absorption cross-section.
The preparation method that boron carbide ceramics is commonly used is traditional powder sintered manufacturing process, promptly prepares boron carbide powder earlier, adds the mixed compression moulding of powder with other again; High temperature hot pressing or pressureless sintering then, high to sintering process and equipment requirements, it is reported; Can only obtain 80% specific density in 2300 ℃ of sintering under the normal pressure; And be easy to occur abnormal grain and grow up and the surface melting phenomenon, be difficult to obtain complicated shape goods such as large size goods and curved surface, and mechanical property is bad.Simultaneously, norbide is the very strong stupalith of covalent linkage, and toughness is merely 2.2MPam
1/2, this big limitations its application.
Three aspects are mainly concentrated in the research of boron carbide ceramics both at home and abroad at present, the one, reduce sintering temperature.As help burning component such as SiC, Al through adding
2O
3, TiB
2Wait and reduce the norbide sintering temperature, increase density.The 2nd, increase toughness, mainly adopt composite means, as adding TiB
2Particle adds co-sinterings such as staple fibre.The 3rd, the optimization of sintering process.Comprise sintering process such as doping pressureless sintering, HIP sintering, microwave sintering, explosion forming and reaction sintering.
Summary of the invention
The objective of the invention is deficiency, a kind of boron carbide composite material and preparation method thereof is provided to boron carbide ceramics conventional sintering forming technology.Adopt the boron carbide composite material of this method preparation, owing to adopt charcoal fiber reinforcement precast body and chemical gas phase low temperature osmotic technology, the plasticity of material is good, mechanical property is good, has overcome the fragility of conventional sintering norbide, is suitable for as the high rigid structure parts of lightweight.
The technical scheme that the present invention uses may further comprise the steps:
(1) adopt acupuncture, puncture and three dimensional knitting method to produce charcoal fiber reinforcement precast body;
(2) precast body in the step (1) is cut into preset shape, be placed on behind the weighing in the chemical vapor deposition stove, be evacuated to below the 50Pa, be warming up to 800-1300 ℃ of infiltration temperature, insulation baking in 30 minutes precast body about 300 ℃ with 10 ℃/min speed.
(3) in cvd furnace, feed a kind of in propylene or the methane simultaneously, add boron trichloride gas, hydrogen and argon gas, the volume ratio of hydrogen, boron trichloride and propylene or methane is 20: 3-10: 1-2, Ar gas remains on 200sccm.Reaction pressure is controlled at 600-2000Pa, and the reactive infiltration time changes according to the precast body variation in thickness, general each 20-50 hour.
(4) off-response gas, goods are taken out in the cooling blowing out, remove fine and close epidermis, cleaning-drying.
(5) repeating step (2) (3) (4) reaches 2.0-2.3g/cm up to the goods global density
3Till.
(6), can the sample in the step (5) be utilized the identical processing condition deposition one deck norbide top coat of step (3) (4) to some specific application environment.
The charcoal fiber preform that the described acupuncture of above-mentioned steps (1) is produced is meant x-y to adopting charcoal cloth or not having latitude cloth and charcoal fibrous reticulum tire shop layer alternately, and z is to the charcoal fiber preform with needling process introducing charcoal fiber; The charcoal fiber preform that the described puncture of step (1) is produced is meant x-y to adopting charcoal cloth or not having latitude cloth shop layer, and z is to the charcoal fiber preform with charcoal fibrous bundle puncture braiding; The charcoal fiber preform that the described 3 D weaving of step (1) is produced is meant the charcoal fiber preform by the three-dimensional four-way weaving preparation of 22 ° of braid angles.The charcoal fiber comprises T300, T700 or similar charcoal fiber.
The described preset shape of above-mentioned steps (2) comprises tabular, cylindric, cylindric, curved surface shape, coniform.
The present invention compares with the conventional sintering technology of preparing and has the following advantages:
(1) the brand-new technology that combines of the present invention's mode of on the boron carbide ceramics Composite Preparation, having adopted the high strength carbon fibre precast body to add chemical vapor infiltration first also is to have prepared the boron carbide ceramics matrix material with good mechanical property and brand new of stability first.Adopt high-strength carbon fibre (C
f) precast body is as toughness reinforcing skeleton, preparation temperature is lower than 1300 ℃, can not damage the mechanical property of charcoal fiber; Adopt the fiber reinforced reinforcement boron carbide-based composite material of continuous charcoal, can suppress the volume effect of ceramic defective to greatest extent, extract the consumption energy-to-break, thereby strengthen toughness reinforcingly, overcome the weakness of the big and poor reliability of its fragility through crack deflection and expansion, fiber.High-strength carbon fibre can weave or be processed into complicated shape arbitrarily such as curved surface, tubular, taper, compares sintering process, can make the goods of complicated shape; The norbide crystal grain that chemical vapor infiltration obtains is tiny, than the B of prepared by other
4The C pottery has higher purity and hardness.
(2) low for equipment requirements, technical process is simple, and control is convenient.
(3) the precast body shape can weave arbitrarily, therefore can prepare the goods of any complicated shape.
(4) preparation temperature is low, and the goods crackle is few, and internal stress is little.
(5) can select precast body fibre content and weaving manner as requested for use, the designability of matrix material is good.
Description of drawings
Fig. 1 is the manufacturing process synoptic diagram of carbon fiber reinforced boron carbide composite material of the present invention.
Embodiment
Embodiment 1
(1) the x-y face adopts alternately shop layer of no latitude cloth and charcoal fibrous reticulum tire, is 0 °, 90 ° between adjacent layers, and z forms accurate three-dimensional structure needle-punched carbon fiber precast body, precast body density 0.5g/cm to introducing needling fiber
3
(2) referring to Fig. 1; Plate tensile sample with the precast body cut growth (60-200mm) in the step (1) * wide (60-200mm) * thick (10-60mm); Put in the cvd furnace behind the weighing; The stove vacuum is extracted into below the 50Pa, is warming up to 1100 ℃ with the speed of 10 ℃/min, and wherein 300 ℃ of following bakers are 30 minutes.Feed hydrogen, boron trichloride and propylene gas with 10: 5: 1 ratios, Ar gas remains on 200sccm.Furnace pressure is adjusted at 1000Pa during infiltration, penetration time 30 hours.The cooling of stopping the supple of gas or steam is taken out the samples weighing detection after closing stove, removes the fine and close exterior skin of sample, puts into stove behind the cleaning-drying again and continues the infiltration density, carries out 3-5 time repeatedly, reaches 2-2.3g/cm up to the sample global density
3Till.
(3) after the sample cutting, the epoxy resin for cold edge, the diamond sand table polishes polishing.The matrix material pattern of under opticmicroscope, observing is as shown in Figure 2.The C for preparing with this understanding
f/ B
4C, three-point bending strength 300-400MPa, Vickers' hardness is greater than 2000, and fracture toughness property is greater than 5MPam
1/2, tensile strength shows as non-brittle fracture greater than 150MPa, and certain pseudo-plasticity is arranged.
Embodiment 2
(1) the x-y face adopts the no latitude cloth of T300 charcoal fibrage, and z forms three-dimensional thin puncture precast body, the precast body density 0.6g/cm of compiling to adopting T700 charcoal fiber puncture braiding
3
(2) precast body in the step (1) is cut into the disk sample of Φ (60-150mm) * 30mm, put into cvd furnace behind the weighing, the stove vacuum is extracted into below the 50Pa, is warming up to 1000 ℃ with the speed of 10 ℃/min, and wherein 300 ℃ of following bakers are 30 minutes.Feed hydrogen, boron trichloride and methane gas with 10: 4: 1 ratios, Ar gas remains on 200sccm.Furnace pressure is adjusted at 600Pa during infiltration, penetration time 30 hours.The cooling of stopping the supple of gas or steam is taken out the samples weighing detection after closing stove, removes the fine and close exterior skin of sample, puts into stove behind the cleaning-drying again and continues the infiltration density, carries out 2-3 time repeatedly, reaches 2-2.3g/cm up to the sample global density
3Till.The C for preparing with this understanding
f/ B
4C, three-point bending strength 300-350MPa, Vickers' hardness is greater than 2000, and fracture toughness property is greater than 5MPam
1/2, tensile strength shows as non-brittle fracture greater than 150MPa, and certain pseudo-plasticity is arranged.
Embodiment 3
(1) adopt the braiding of T300 charcoal fibre three-dimensional four-way, 22 ° of braid angles are formed the 3 D weaving precast body, be shaped as circular, precast body density 0.8g/cm
3
(2) precast body in the step (1) is processed into the ring specimen of external diameter Φ 90 wall thickness 30mm, puts into cvd furnace behind the weighing, the stove vacuum is extracted into below the 50Pa, is warming up to 900 ℃ with the speed of 10 ℃/min, and wherein 300 ℃ of following bakers are 30 minutes.Feed hydrogen, boron trichloride and propylene gas with 10: 5: 1 ratios, Ar gas remains on 200sccm.Furnace pressure is adjusted at 1000Pa during infiltration, penetration time 30 hours.The cooling of stopping the supple of gas or steam is taken out the samples weighing detection after closing stove, removes the fine and close exterior skin of sample, puts into stove behind the cleaning-drying again and continues the infiltration density, carries out 2-3 time repeatedly, reaches 2-2.3g/cm up to the sample global density
3Till.
(3) with behind the sample cleaning-drying in the step (2); Put into cvd furnace again, the condition of (2) prepares the boron carbide coating of the about 20 μ m of a bed thickness, densification, the three-point bending strength 300-350MPa of sample set by step; The surface Vickers' hardness is greater than 2200, and fracture toughness property is greater than 5MPam
1/2, tensile strength is greater than 200MPa.The anti-ablation of sample is anti-oxidant, can be used as high temperature nozzle.
It should be noted; The examples of implementation that above-mentioned practical implementation example disclosed by the invention is just listed in order to be expressly understood principle of the present invention; Under the unactual situation that deviates from spirit of the present invention and principle; Can do many improvement and change to above-mentioned embodiment, all these improvement and change all are included in the scope of the present disclosure and receive the protection of claim.
Claims (5)
1. the preparation method of a carbon fiber reinforced boron carbide composite material is characterized in that, may further comprise the steps:
(1) adopt acupuncture, puncture and three dimensional knitting method to produce charcoal fiber reinforcement precast body;
(2) precast body in the step (1) is cut into preset shape, be placed on behind the weighing in the chemical vapor deposition stove, be evacuated to below the 50Pa, be warming up to 800-1300 ℃ of infiltration temperature, at 300 ℃ of insulations baking in 30 minutes precast body with 10 ℃/min speed;
(3) in cvd furnace, feed a kind of in propylene or the methane simultaneously, add boron trichloride gas, hydrogen and argon gas, the volume ratio of hydrogen, boron trichloride and propylene or methane is 20: 3-10: 1-2, and Ar gas remains on 200sccm; Reaction pressure is controlled at 600-2000Pa, each 20-50 of reactive infiltration time hour;
(4) off-response gas, goods are taken out in the cooling blowing out, remove fine and close epidermis, cleaning-drying;
(5) repeating step (2) (3) (4) reaches 2.0-2.3g/cm up to the goods global density
3Till.
2. the preparation method of carbon fiber reinforced boron carbide composite material according to claim 1; It is characterized in that; The charcoal fiber preform that the described acupuncture of step (1) is produced; Be meant x-y to adopting charcoal cloth or not having latitude cloth and charcoal fibrous reticulum tire shop layer alternately, z is to the charcoal fiber preform with needling process introducing charcoal fiber; The charcoal fiber preform that the described puncture of step (1) is produced is meant x-y to adopting charcoal cloth or not having latitude cloth shop layer, and z is to the charcoal fiber preform with charcoal fibrous bundle puncture braiding; The charcoal fiber preform that the described 3 D weaving of step (1) is produced is meant the charcoal fiber preform by the three-dimensional four-way weaving preparation of 22 ° of braid angles.
3. the preparation method of carbon fiber reinforced boron carbide composite material according to claim 1 and 2 is characterized in that, the described used charcoal fiber of charcoal fiber reinforcement precast body of producing comprises T300 or T700.
4. the preparation method of carbon fiber reinforced boron carbide composite material according to claim 1 is characterized in that, the described preset shape of step (2) comprises tabular, cylindric, cylindric, curved surface shape, coniform.
5. a carbon fiber reinforced boron carbide composite material is characterized in that, described matrix material is prepared by the described method of claim 1.
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| JPH0881261A (en) * | 1994-09-09 | 1996-03-26 | Hitachi Ltd | Highly heat-conductive carbon fiber/boron carbide composite material |
| CN1718560A (en) * | 2005-06-29 | 2006-01-11 | 中国人民解放军国防科学技术大学 | Carbon-fiber reinforced silicon carbide composite material antioxidation coating layer and its preparation method |
| CN101503305B (en) * | 2009-02-03 | 2012-01-04 | 西北工业大学 | Process for preparing self-sealing silicon carbide ceramic based composite material |
| CN101671193A (en) * | 2009-10-21 | 2010-03-17 | 淄博高新区联创科技服务中心 | Carbon fiber/boron carbide composite ceramic and preparation method thereof |
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