CN103979970B - A kind of high tenacity pressureless sintering boron carbide bulletproof material and preparation method thereof - Google Patents
A kind of high tenacity pressureless sintering boron carbide bulletproof material and preparation method thereof Download PDFInfo
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- CN103979970B CN103979970B CN201410139407.2A CN201410139407A CN103979970B CN 103979970 B CN103979970 B CN 103979970B CN 201410139407 A CN201410139407 A CN 201410139407A CN 103979970 B CN103979970 B CN 103979970B
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Abstract
The present invention relates to a kind of high tenacity pressureless sintering boron carbide bulletproof material and preparation method thereof, belong to field of material synthesis technology.Described bullet resistant material comprises the moiety of following mass percent: norbide: 70-95%, TiC:0.5-15%, α-SiC:1-15%, carbon black: 0-2%.Its preparation method is: take raw material, and the norbide taken, TiC, α-SiC, carbon black are put into ball mill, is that medium carries out wet-milling, screen cloth with deionized water; Carry out mist projection granulating, screening again; Green compact are made by dry-pressing formed for slurry; Biscuit after processing is sintered under argon shield, obtained liquid phase sintering boron carbide bulletproof material after mill processing, polished finish.The volume density of bullet resistant material of the present invention reaches 2.50-2.59g/cm
3, the performance such as hardness, bending strength, fracture toughness property, Young's modulus of material is good.
Description
Technical field
The present invention relates to a kind of high tenacity pressureless sintering boron carbide bulletproof material and preparation method thereof, belong to field of material synthesis technology.
Background technology
Along with the extensive development of modern war destructive weapon, previous bullet resistant material can not meet the performance requriements that bullet resistant material possesses.The bullet resistant material seeking superior performance has great defense strategy meaning.There is easy quilt attack as early stage bullet resistant material and wear in metal group material, the shortcomings such as shellproof coefficient is low, and the density of metal is large, optionally can not increase again its thickness, otherwise the fight capability of soldier can decline by straight line.And stupalith has that intensity is high, hardness is large, high temperature resistant, anti-oxidant, high temperature creep property is little, excellent in abrasion resistance under high temperature, the excellent over-all properties such as thermal expansivity is little, density is low, it is all obviously better than metallic substance, macromolecular material and matrix material thereof in shellproof energy-absorbing effect, wear effects, kinetic effect etc., and actual application is obtained in military project protection, become one of leading greatly material of three in armor facing.The research of countries in the world to Ceramic Composite bullet resistant material is all paid much attention to, this research mainly concentrates on ceramic-metal compound, pottery-aspect such as polyester thin slice compound, steel-ceramic-steel compound, these matrix materials all belong to stratified composite macroscopically, namely there is sharp interface between layers and occur between each layer physicals sudden change stratified composite.By ceramic-metal composite material that is ceramic and metal composite, although have lot of advantages, but when internal stress increases, the destruction of material can be caused, and its density is because the existence of metal is relative to also not having advantage stupalith on armoring bullet resistant material.On the other hand, although pottery meets the requirement of bullet resistant material to lightweight with the matrix material of polyester thin slice, the inter-laminar stress that the sudden change due to material behavior causes is concentrated, is easily caused the unfavorable factors such as slabbing destruction.It is good that pottery and the bullet resistant material of aluminum oxide have sintering character, technical maturity, and product size is stablized, the low and advantages such as abundant raw material of production cost, but its bulletproof ability is lower slightly, and density is comparatively large, can not meet high performance ballistic requirements.
And norbide is a kind of superhard material, have that lightweight, wear resisting property are good, resistance to chemical attack, the premium properties such as splendid ballisticperformances and high neutron absorption performance.Can be applicable in the bullet resistant materials such as the armour of the nozzle of sandblast machine, sealing element, bullet-proof vest and aircraft.Owing to there being the covalent linkage of about 93% in the crystalline structure of norbide, make the sintering of boron carbide material very difficult.Usually will could obtain finer and close boron carbide material at 2300 DEG C of hot pressed sinterings, in addition, norbide is a kind of material be highly brittle, and the fracture toughness property of pure norbide only has 2.2MPam
1/2, due to above-mentioned shortcoming, limit the widespread use of norbide.
At present, both at home and abroad to the sintering character improving boron carbide material, directly add TiB by adopting
2, SiC, C, Al
2o
3and the method for metal Ti, Al etc., make sintering temperature be reduced to 1700-1800 DEG C, but the hardness of material but drops to below 30Gpa, fracture toughness property is only 2.5-3.2MPam
1/2, and complex process, cost is high.
Summary of the invention
The present invention is directed to the above-mentioned problems in the prior art, the high tenacity pressureless sintering boron carbide bulletproof material that a kind of hardness is high, folding strength is large, fracture toughness property is good is provided, and relates to the preparation method of this high tenacity pressureless sintering boron carbide bulletproof material.
For achieving the above object, the present invention by the following technical solutions, a kind of high tenacity pressureless sintering boron carbide bulletproof material, described bullet resistant material comprises the moiety of following mass percent: norbide: 70-95%, TiC:0.5-15%, α-SiC:1-15%, carbon black: 0-2%.
The boron carbide particles that the present invention is large with hardness, density is little is matrix, utilize particle strengthening and toughening mechanism to make bullet resistant material, and pass through moiety and the mass percent thereof of reasonable compatibility bullet resistant material, make material have density little, ballistic performance is good, and cost performance height waits overall merit.After sintering, the thing phase composite of bullet resistant material of the present invention is mainly B
4c, SiC, TiB
2, wherein B
4c and SiC is principal crystalline phase, and the TiC in raw material disappears substantially.In reaction sintering process, resultant can stop growing up of matrix grain thus reach the effect of strengthening matrix.Higher sintering temperature makes the reaction of formation cenotype carry out smoothly, generates more TiB
2, the SiC in raw material is rack-like Structural assignments, is distributed in principal crystalline phase B
4around C, play connection, calking and the effect of strengthening crystal boundary; The toughening mechanism of long bar-shaped SiC crystalline phase is similar to fiber or whisker, mainly plays deviation and bridging effect to crackle; TiC and B
4the rod shape TiB that C produces
2also the performance SiC and the TiB that improve material is conducive to
2.SiC and TiB
2be uniformly distributed in B
4around C matrix, B can be limited
4the abnormal growth of C crystal grain.Newly born phase grain-size is little, because the TiB that reaction generates
2many with SiC, the new crystal boundary of generation is also more, and crystal boundary energy is higher, and the resistance that crack propagation is subject to is larger, so material of the present invention can significantly improve flexural strength and fracture toughness property.The strict proportioning controlled between its raw material in bullet resistant material of the present invention, by the synergy between each raw material, make in material, to there is more disperse phase, when the interface cohesion of disperse phase and matrix phase is strengthened, during Materials Fracture will there is tension fracture in toughness reinforcing particle, and this will effectively improve the toughness of material.In crack propagation process, as run into the obstruction of subparticle, namely producing particle " pinning " effect, crack propagation hindered or deflects.In addition, produce deflection, bifurcated when the existence of tiny crack makes lead crack expand, lead crack also can be made to expand and consume more energy, therefore, bill of material of the present invention reveals high toughness, hardness, and the ballistic performance of material is good.
In above-mentioned high tenacity pressureless sintering boron carbide bulletproof material, as preferably, described bullet resistant material comprises the moiety of following mass percent: norbide: 75-90%, TiC:2-12%, α-SiC:2-12%, carbon black: 1-2%.
In above-mentioned high tenacity pressureless sintering boron carbide bulletproof material, further preferably, described bullet resistant material comprises the moiety of following mass percent: norbide: 83%, TiC:8%, α-SiC:8%, carbon black: 1%.
In addition, the purity of raw material and particle diameter also very important on the impact of material property.The purity of selected raw material is higher, and impurity is fewer, and the grain-boundary strength of generation is higher, and the performance of material is better.Within the specific limits, the particle diameter of raw material is less, and the temperature generating high tenacity with no pressure is lower, is more conducive to the sintering promoting product.If but the particle diameter of raw material is too little, easily reunites, impact is dispersed, makes weave construction uneven, thus the performance of harm product.
In above-mentioned high tenacity pressureless sintering boron carbide bulletproof material, as preferably, the purity of described norbide is 99.0-99.9%, and median size is 1-3.5 micron.If norbide particle diameter is too thick, biscuit density does not reach requirement, i.e. not easily compacting, and material internal pore is more, and crack propagation accelerates, and material property declines, especially hardness, and firing temperature is higher simultaneously, can the serious waste energy.If norbide particle diameter is too thin, easily reunite, weave construction is uneven, reduces product performance equally.
In above-mentioned high tenacity pressureless sintering boron carbide bulletproof material, as preferably, the purity of described TiC is 99.0-99.8%, and median size is 2.0-4.5 micron.
In above-mentioned high tenacity pressureless sintering boron carbide bulletproof material, as preferably, the purity of described α-SiC is 99.0-99.8%, and median size is 1-5 micron.
Second object of the present invention is the preparation method providing a kind of above-mentioned high tenacity pressureless sintering boron carbide bulletproof material, and described preparation method comprises the steps:
S1, take high tenacity pressureless sintering boron carbide bulletproof material composi and mass percent thereof as described in the appended claim 1, the norbide taken, TiC, α-SiC, carbon black are put into ball mill, be that medium carries out wet-milling with deionized water, after wet-milling 1-3h, slurry passed through 120 object screen clothes;
S2, the slip after sieving is carried out mist projection granulating by mist projection granulating tower, by the slurry after granulation by for subsequent use after 60 mesh sieves;
S3, loaded in mold cavity by the slurry after above-mentioned granulation, dry-pressing formed under the pressure of 25-100MPa, the dwell time is 5s-20s, makes green compact;
S4, according to drawing dimensional requirement, green compact to be processed; the biscuit processed is put into non-pressure sintering furnace, and under argon shield, gradient increased temperature sinters to 2150-2250 DEG C; furnace cooling after insulation 1-3h, obtained liquid phase sintering boron carbide bulletproof material after mill processing, polished finish.
Raw material first takes by the preparation process of bullet resistant material of the present invention carries out wet-milling, wet-milling can make final material fineness evenly, the energy expenditure of unit weight product is low, do not have dust to fly field, noise is less, then by spray-dired agglomeration technique, slurry drying is directly made to become granulated powders, the operation such as devaporation, pulverizing can be economized, by dry-pressing formed after sieving, sinter finally by gradient increased temperature, the bullet resistant material that obtained toughness is higher.
In the preparation method of above-mentioned high tenacity pressureless sintering boron carbide bulletproof material, in the process of wet-milling described in step S1, add the adhesive phenolic resin accounting for stock quality 5-15%.Resol can make binding agent on the one hand, for forming of green body provides cohesiveness, otherwise can not carry out dry-pressing formed; Resol residual on the other hand can be residual in the product with the form of carbon, i.e. recarburization, contributes to activated sintering.
In the preparation method of above-mentioned high tenacity pressureless sintering boron carbide bulletproof material, described in step S2, during mist projection granulating, the inlet temperature of prilling tower is 180-230 DEG C, temperature out is 85-120 DEG C, take away pump rotating speed: 45-90r/min, atomizing disk rotating speed 14000r/min.
In the preparation method of above-mentioned high tenacity pressureless sintering boron carbide bulletproof material, gradient increased temperature described in step S5 is rise to 400 DEG C of insulation 20-60min with the heat-up rate of 2-5 DEG C/min from room temperature, 600 DEG C of insulation 20-30min are risen to from 400 DEG C again with the heat-up rate of 2-5 DEG C/min, then rise to 1400 DEG C of insulation 20-30min with the heat-up rate of 8-15 DEG C/min from 600 DEG C, finally rise to 2150-2250 DEG C of insulation 1h-3h with the heat-up rate of 8-20 DEG C/min from 1400 DEG C.From room temperature, temperature rise rate is more slowly and respectively 400 DEG C and 600 DEG C of insulations, mainly because make moisture and adhesive phenolic resin fully evaporate in base substrate when low temperature, thus avoid making base substrate occur a large amount of pore even cracking phenomena, cause product performance decline or scrap.
Compared with prior art, the present invention is by the composition of reasonable compatibility high tenacity pressureless sintering bullet resistant material, the boron carbide particles that, density large with hardness is little is matrix, particle strengthening and toughening mechanism is utilized to make bullet resistant material, reduce the volume density of material, improve the ballistic performance of material, make the volume density of material reach 2.50-2.59g/cm
3, improve the hardness, bending strength, fracture toughness property, Young's modulus etc. of material, make the Shore hardness of material reach 120-130HS, folding strength reaches 470-490MPa, and fracture toughness property reaches 5.8-6.8MPam
1/2, Young's modulus reaches 430-460MPa.
Embodiment
In order to make technical problem solved by the invention, technical scheme and beneficial effect clearly understand, below in conjunction with specific embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
Table 1: the moiety of high tenacity pressureless sintering boron carbide bulletproof material and mass percent, particle diameter, purity in embodiment 1-3
Embodiment 1
Take high tenacity pressureless sintering boron carbide bulletproof material composi and mass percent thereof as described in table 1 embodiment 1, the norbide taken, TiC, α-SiC, carbon black are put into ball mill, be that medium carries out wet-milling with deionized water, add the adhesive phenolic resin accounting for stock quality 5-15% in wet-milling process, after wet-milling 1-3h, slurry is passed through 120 object screen clothes;
Slip after sieving is carried out mist projection granulating by mist projection granulating tower, during mist projection granulating, the inlet temperature of prilling tower is 180-230 DEG C, and temperature out is 85-120 DEG C, take away pump rotating speed: 45-90r/min, atomizing disk rotating speed 14000r/min, by the slurry after granulation by for subsequent use after 60 mesh sieves;
Loaded in mold cavity by slurry after above-mentioned granulation, dry-pressing formed under the pressure of 25-100MPa, the dwell time is 5s-20s, makes green compact;
According to drawing dimensional requirement, green compact are processed, the biscuit processed is put into non-pressure sintering furnace, under argon shield, 400 DEG C of insulation 20-60min are risen to from room temperature with the heat-up rate of 2-5 DEG C/min, 600 DEG C of insulation 20-30min are risen to from 400 DEG C again with the heat-up rate of 2-5 DEG C/min, then 1400 DEG C of insulation 20-30min are risen to the heat-up rate of 8-15 DEG C/min from 600 DEG C, finally rise to 2150-2250 DEG C with the heat-up rate of 8-20 DEG C/min from 1400 DEG C to sinter, furnace cooling be incubated 1h-3h at 2150-2250 DEG C after, through mill processing, obtained liquid phase sintering boron carbide bulletproof material after polished finish.
Embodiment 2
Take high tenacity pressureless sintering boron carbide bulletproof material composi and mass percent thereof as described in table 1 embodiment 1, the norbide taken, TiC, α-SiC, carbon black are put into ball mill, be that medium carries out wet-milling with deionized water, add the adhesive phenolic resin accounting for stock quality 5-15% in wet-milling process, after wet-milling 1-3h, slurry is passed through 120 object screen clothes;
Slip after sieving is carried out mist projection granulating by mist projection granulating tower, during mist projection granulating, the inlet temperature of prilling tower is 180-230 DEG C, and temperature out is 85-120 DEG C, take away pump rotating speed: 45-90r/min, atomizing disk rotating speed 14000r/min, by the slurry after granulation by for subsequent use after 60 mesh sieves;
Loaded in mold cavity by slurry after above-mentioned granulation, dry-pressing formed under the pressure of 25-100MPa, the dwell time is 5s-20s, makes green compact;
According to drawing dimensional requirement, green compact are processed, the biscuit processed is put into non-pressure sintering furnace, under argon shield, 400 DEG C of insulation 20-60min are risen to from room temperature with the heat-up rate of 2-5 DEG C/min, 600 DEG C of insulation 20-30min are risen to from 400 DEG C again with the heat-up rate of 2-5 DEG C/min, then 1400 DEG C of insulation 20-30min are risen to the heat-up rate of 8-15 DEG C/min from 600 DEG C, finally rise to 2150-2250 DEG C with the heat-up rate of 8-20 DEG C/min from 1400 DEG C to sinter, furnace cooling be incubated 1h-3h at 2150-2250 DEG C after, through mill processing, obtained liquid phase sintering boron carbide bulletproof material after polished finish.
Embodiment 3
Take high tenacity pressureless sintering boron carbide bulletproof material composi and mass percent thereof as described in table 1 embodiment 1, the norbide taken, TiC, α-SiC, carbon black are put into ball mill, be that medium carries out wet-milling with deionized water, add the adhesive phenolic resin accounting for stock quality 5-15% in wet-milling process, after wet-milling 1-3h, slurry is passed through 120 object screen clothes;
Slip after sieving is carried out mist projection granulating by mist projection granulating tower, during mist projection granulating, the inlet temperature of prilling tower is 180-230 DEG C, and temperature out is 85-120 DEG C, take away pump rotating speed: 45-90r/min, atomizing disk rotating speed 14000r/min, by the slurry after granulation by for subsequent use after 60 mesh sieves;
Loaded in mold cavity by slurry after above-mentioned granulation, dry-pressing formed under the pressure of 25-100MPa, the dwell time is 5s-20s, makes green compact;
According to drawing dimensional requirement, green compact are processed, the biscuit processed is put into non-pressure sintering furnace, under argon shield, 400 DEG C of insulation 20-60min are risen to from room temperature with the heat-up rate of 2-5 DEG C/min, 600 DEG C of insulation 20-30min are risen to from 400 DEG C again with the heat-up rate of 2-5 DEG C/min, then 1400 DEG C of insulation 20-30min are risen to the heat-up rate of 8-15 DEG C/min from 600 DEG C, finally rise to 2150-2250 DEG C with the heat-up rate of 8-20 DEG C/min from 1400 DEG C to sinter, furnace cooling be incubated 1h-3h at 2150-2250 DEG C after, through mill processing, obtained liquid phase sintering boron carbide bulletproof material after polished finish.
High tenacity pressureless sintering boron carbide bulletproof material obtained in embodiment of the present invention 1-3 is carried out performance test, and test result is as shown in table 2.
Table 2: the performance test results of high tenacity pressureless sintering boron carbide bulletproof material obtained in embodiment of the present invention 1-3
Wherein, comparative example is the general silicon carbide ceramics adopting reaction sintering to produce at present.
In sum, high tenacity pressureless sintering boron carbide bulletproof material of the present invention is by the composition of reasonable compatibility high tenacity pressureless sintering bullet resistant material, reduce the volume density of material, improve the ballistic performance of material, especially the dimensional precision etc. of the hardness of material, bending strength, fracture toughness property, Young's modulus and material.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (8)
1. a high tenacity pressureless sintering boron carbide bulletproof material, it is characterized in that, the raw material of the following mass percent of described bullet resistant material consists of: norbide: 70-95%, TiC:0.5-15%, α-SiC:1-15%, carbon black: 0-2%, the purity of described norbide is 99.0-99.9%, and the median size of norbide is 1.5-3 micron.
2. high tenacity pressureless sintering boron carbide bulletproof material according to claim 1, it is characterized in that, the raw material of the following mass percent of described bullet resistant material consists of: norbide: 75-90%, TiC:2-12%, α-SiC:2-12%, carbon black: 1-2%.
3. high tenacity pressureless sintering boron carbide bulletproof material according to claim 1 and 2, it is characterized in that, the raw material of the following mass percent of described bullet resistant material consists of: norbide: 83%, TiC:8%, α-SiC:8%, carbon black: 1%.
4. high tenacity pressureless sintering boron carbide bulletproof material according to claim 1 and 2, is characterized in that, the purity of described TiC is 99.0-99.8%, and median size is 2.0-4.5 micron.
5. high tenacity pressureless sintering boron carbide bulletproof material according to claim 1 and 2, is characterized in that, the purity of described α-SiC is 99.0-99.8%, and median size is 1-5 micron.
6. a preparation method for high tenacity pressureless sintering boron carbide bulletproof material, is characterized in that, described preparation method comprises the steps:
S1, take high tenacity pressureless sintering boron carbide bulletproof material composi and mass percent thereof as described in the appended claim 1, the norbide taken, TiC, α-SiC, carbon black are put into ball mill, be that medium carries out wet-milling with deionized water, after wet-milling 1-3h, slurry passed through 120 object screen clothes;
S2, the slip after sieving is carried out mist projection granulating by mist projection granulating tower, by the powder after granulation by for subsequent use after 60 mesh sieves;
S3, the powder obtained by step S2 load in mold cavity, and dry-pressing formed under the pressure of 25-100MPa, the dwell time is 5s-20s, makes green compact;
S4, according to drawing dimensional requirement, green compact to be processed, the biscuit processed is put into non-pressure sintering furnace, and under argon shield, gradient increased temperature sinters to 2150-2250 DEG C, furnace cooling after insulation 1-3h, obtained liquid phase sintering boron carbide bulletproof material after mill processing, polished finish;
Wherein, the adhesive phenolic resin accounting for stock quality 5-15% is added in the process of wet-milling described in step S1.
7. the preparation method of high tenacity pressureless sintering boron carbide bulletproof material according to claim 6, it is characterized in that, described in step S2, during mist projection granulating, the inlet temperature of prilling tower is 180-230 DEG C, temperature out is 85-120 DEG C, take away pump rotating speed: 45-90r/min, atomizing disk rotating speed 14000r/min.
8. the preparation method of high tenacity pressureless sintering boron carbide bulletproof material according to claim 6, it is characterized in that, gradient increased temperature described in step S4 is rise to 400 DEG C of insulation 20-60min with the heat-up rate of 2-5 DEG C/min from room temperature, 600 DEG C of insulation 20-30min are risen to from 400 DEG C again with the heat-up rate of 2-5 DEG C/min, then rise to 1400 DEG C of insulation 20-30min with the heat-up rate of 8-15 DEG C/min from 600 DEG C, finally rise to 2150-2250 DEG C of insulation 1h-3h with the heat-up rate of 8-20 DEG C/min from 1400 DEG C.
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| CN108640687B (en) * | 2018-05-29 | 2021-02-05 | 北京理工大学 | Boron carbide/silicon carbide composite ceramic and preparation method thereof |
| CN109467436B (en) * | 2018-12-19 | 2022-03-11 | 中国兵器科学研究院宁波分院 | Boron carbide ceramic ball and preparation method thereof |
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| CN102757224A (en) * | 2012-07-31 | 2012-10-31 | 中国科学院上海硅酸盐研究所 | Method for preparing dense boron carbide matrix ceramic material by sintering |
| CN103145422A (en) * | 2013-03-06 | 2013-06-12 | 武汉理工大学 | High-hardness ceramic composite material of boron carbide-titanium boride-silicon carbide and preparation method thereof |
| CN103641480A (en) * | 2013-12-13 | 2014-03-19 | 宁波东联密封件有限公司 | High-tenacity boron carbide composite material and preparation method thereof |
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| CN102757224A (en) * | 2012-07-31 | 2012-10-31 | 中国科学院上海硅酸盐研究所 | Method for preparing dense boron carbide matrix ceramic material by sintering |
| CN103145422A (en) * | 2013-03-06 | 2013-06-12 | 武汉理工大学 | High-hardness ceramic composite material of boron carbide-titanium boride-silicon carbide and preparation method thereof |
| CN103641480A (en) * | 2013-12-13 | 2014-03-19 | 宁波东联密封件有限公司 | High-tenacity boron carbide composite material and preparation method thereof |
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