CN108640687A - A kind of boron carbide/carborundum composite-phase ceramic and preparation method thereof - Google Patents
A kind of boron carbide/carborundum composite-phase ceramic and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of boron carbide/carborundum composite-phase ceramics and preparation method thereof, belong to armor facing field of material technology.The regulation and control that the present invention passes through selection and each component content to ingredient in boron carbide/carborundum composite-phase ceramic, the bullet-proof ceramic that a kind of density is low, elasticity modulus is high, bending strength is high and fracture toughness is high is obtained, disclosure satisfy that modern armoring lightweight, high performance demand；In addition, being fired using pressureless sintering method in the preparation process of boron carbide/carborundum composite-phase ceramic of the present invention, compared with previous sintering method, this method can reduce cost, production efficiency is improved, is sintered and high-compactness ceramics is made, and suitable for producing in enormous quantities.
Description
Technical field
It is burnt present invention relates particularly to a kind of lightweight, boron carbide/carborundum composite-phase ceramic of high-strength tenacity and using without pressure
The method that knot technique is sintered preparation belongs to armor facing field of material technology.
Background technology
With the development of armor technology, the requirement to armour material not only needs good anti-bullet barrier propterty, subtracts to it
It is important to ask also higher and higher.It can be on the basis of not reducing barrier propterty further using the novel armour material of light high performance
The weight for reducing tank and panzer etc., significantly promotes its mobility.As important armor facing material, ceramics can be
Erosion, passivation and broken body, have excellent anti-penetration properties in impact process.
In current existing various bulletproof ceramics, boron carbide (B4C) ceramics have minimum proportion, highest hardness and
Elasticity modulus is material most hard in addition to diamond, cubic boron nitride, is the anti-bullet pottery of first choice of modern lightweight bullet resistant material
Ceramic material.But the fracture toughness and bending strength of B4C ceramics are relatively low, only 1~2MPam1/2With 100~260MPa, this pole
The big application for limiting B4C ceramics.In addition, B4C ceramics covalent bond accountings reach 94%, fusing point is up to 2350 DEG C, and sintering is extremely
Difficulty, traditional B4C ceramics mainly by hot pressed sintering be made, but hot-press sintering equipment it is complicated, it is expensive, be not easy
Control；And hot-pressed product shape is single, and hot pressed sintering ceramics are not easy to realize that large-scale production, low production efficiency directly contribute life
It is high to produce cost, this severely limits the commercial Applications of boron carbide ceramics.
Such as Chinese invention patent application (application number：201510807372.X the applying date：2015.11.19 one kind) is disclosed
The preparation method of pressureless sintering boron carbide ceramics, this approach includes the following steps：By boron carbide powder (D50 >=2 μm) 70~
80wt%, 4~8wt% of carbon dust, oxidation yttrium powder 0.7~2wt%, tri- kinds of raw materials are put into ball mill mixing container, add bonding
Agent, dispersant and deionized water carry out ball milling slurrying, obtain the slurry that solid concentration is 25~45wt%；Slurry is spray-dried
Pelletizing is made in comminutor；Pelletizing is depressed into life using dry-pressing formed or cold isostatic compaction technique in 100~200MPa
Base；It puts the green body into vacuum drying oven, using vacuum or normal pressure-sintered mode, 0.5~5h is kept the temperature at 2000~2300 DEG C, is obtained
Boron carbide ceramics.The boron carbide ceramics density being prepared reaches 2.40g/cm3, consistency can reach 96% or more, fracture
3.0~3.5MPam of toughness1/2, 22~24GPa of Vickers hardness.
As that studies boron carbide ceramics gos deep into, researcher has developed boron carbide-based complex phase ceramic or boron carbide-based multiple
Condensation material.Such as Chinese invention patent application (application number：201110079294.8 the applying date：2011.03.31) disclose a kind of carbon
Change boron carbon/silicon carbide ceramic matrix composite and preparation method thereof.The boron carbide carbon/silicon carbide ceramic matrix composite is mixed by boron carbide carbon
It is formed by alloy infiltration reaction-sintered after closing powder precast body degreasing；Wherein, in the boron carbide carbon mixed powder precast body
Including 85~98wt% of boron carbide, 1.0~14.0wt% of carbon and the pre-formed organic adhesive used, the alloy is by silicon
12.5~95wt%, 5~87.5wt% of aluminium are constituted.But the density of prepared boron carbide carbon/silicon carbide ceramic matrix composite compared with
Height, mechanical property is poor, cannot meet modern armoring lightweight, high performance demand.
Invention content
In view of this, one of the objects of the present invention is to provide a kind of boron carbide/carborundum composite-phase ceramics, by ingredient
Selection and each component content regulation and control, obtain that a kind of density is low, elasticity modulus is high, bending strength is high and fracture toughness is high
Bullet-proof ceramic, disclosure satisfy that modern armoring lightweight, high performance demand；
The second object of the present invention is to provide a kind of preparation method of boron carbide/carborundum composite-phase ceramic, and previous
Hot-pressing sintering method is different, and the present invention is fired using pressureless sintering method, can reduce cost, improves production efficiency, sintering system
High-compactness ceramics are obtained, and suitable for producing in enormous quantities.
The purpose of the present invention is what is be achieved through the following technical solutions.
A kind of boron carbide/carborundum composite-phase ceramic, the raw material gross mass to prepare the complex phase ceramic are institute in terms of 100%
The mass percent stated the composition of raw material and respectively formed is as follows：Boron carbide powder 56%~90%, carborundum powder 5%~30%,
Carbon dust 0.5%~5%, alumina powder 0~5%, boronation zirconium powder 0~5% and REO (rare earth oxide) 0.5%~5%；Its
In, the preferred CeO of REO2、Y2O3Or La2O3。
In the complex phase ceramic raw material, the granularity of boron carbide powder is (0.5~1.0) μm, purity >=96%；Carborundum powder
Granularity be (0.3~0.8) μm, purity >=96%.
A kind of preparation method of boron carbide/carborundum composite-phase ceramic of the present invention, steps are as follows for the method：
Batch mixing ball milling：By in raw material each ingredient and deionized water be added in ball grinder, in 200r/min~600r/
Ball milling 4h~12h under min rotating speeds, obtains uniformly mixed slurry；Wherein, per 100g raw materials in be added 200mL~400mL go from
Sub- water is as grinding aid；
Mist projection granulating：First uniformly mixed slurry is uniformly mixed with polyvinyl alcohol (PVA) aqueous solution as bonding agent,
It sprays into granulation tower again, good particle shape, good fluidity, particle is obtained by controlling atomisation pressure, inlet air temperature, leaving air temp
The moderate pelletizing of narrow distribution range, moisture；Wherein, the mass fraction of polyvinyl alcohol (PVA) aqueous solution is 1%~5%, air inlet
150 DEG C~180 DEG C of temperature, 80 DEG C~130 DEG C, atomisation pressure 0.05MPa~0.5MPa of leaving air temp, the particle size of pelletizing
It is 20 μm~200 μm；
It is dry-pressing formed：Pelletizing is placed in mold, pressurize 0.5min~5min under the pressure of 150MPa~200MPa,
Demoulding, obtains green compact；
Pressureless sintering：It puts the green body into non-pressure sintering furnace, is sintered under vacuum condition or argon gas atmosphere protection；
Wherein, 500 DEG C~900 DEG C first are warming up to the speed of 5 DEG C/min~10 DEG C/min, keep the temperature 15min~60min, then with 5 DEG C/
The speed of min~15 DEG C/min continues to be warming up to 1500 DEG C~1900 DEG C, then again with the speed of 5 DEG C/min~20 DEG C/min after
It is continuous to be warming up to 2050 DEG C~2250 DEG C, 30min~120min is kept the temperature, is then first cooled down with the speed of 5 DEG C/min~15 DEG C/min
It to 1900 DEG C~1500 DEG C, then natural cooling or is quickly cooled down, obtains boron carbide/carborundum composite-phase ceramic.
Advantageous effect：
(1) it is low to obtain a kind of density by the regulation and control of constituent in ceramic material and each component content by the present invention
(2.5g/cm3~2.8g/cm3), elasticity modulus high (380GPa~420GPa), Vickers hardness high (>=26GPa), bending strength it is high
(400MPa~550MPa) and fracture toughness height (5.0MPam1/2~6.9MPam1/2) bullet-proof ceramic, disclosure satisfy that existing
Generation armoring lightweight, high performance demand；
(2) present invention is fired using pressureless sintering method, and compared with previous sintering method, this method has cost
The advantages of low, efficient, suitable for being prepared on a large scale, and prepared product consistency is high.
Specific implementation mode
With reference to specific embodiment, the invention will be further elaborated.
In following embodiment：
Respectively refer to Archimedes's drainage in national standard GB/T 25995-2010, in national standard GB/T22315-2008
Lash method, the three-point bending method in national standard GB/T6569-2006 and the Single edge notch beam in national standard GB/T23806-2009
The density of prepared bullet-proof ceramic, elasticity modulus, bending strength and fracture toughness are tested.
Embodiment 1
A kind of boron carbide/carborundum composite-phase ceramic, the raw material gross mass to prepare the complex phase ceramic are institute in terms of 100%
The mass percent stated the composition of raw material and respectively formed is as follows：Boron carbide powder (granularity is 0.6 μm, purity 97%)
85%, carborundum powder (granularity be 0.6 μm, purity 97%) 12%, carbon dust 1% and cerium oxide powder 2%, preparation process is such as
Under：
Batch mixing ball milling：By in raw material each ingredient and deionized water be added in ball grinder, under 400r/min rotating speeds
Ball milling 6h obtains uniformly mixed slurry；Wherein, 300mL deionized waters are added as grinding aid in every 100g raw materials；
Mist projection granulating：Uniformly mixed slurry is uniformly mixed with the PVA aqueous solutions that mass fraction is 2% first, then is sprayed into
In granulation tower, the pelletizing that particle size is 150 μm is obtained；Wherein, 160 DEG C of the inlet air temperature of granulation tower, leaving air temp 100
DEG C, atomisation pressure 0.1MPa；
It is dry-pressing formed：Pelletizing is placed in sintered-carbide die, is pressed by the way of Bidirectional-pressure,
Under 150MPa pressure after pressurize 30s, demoulding obtains green compact；
Pressureless sintering：It puts the green body into non-pressure sintering furnace, is sintered under argon gas atmosphere protection, wherein first with 7
DEG C/speed of min is warming up to 500 DEG C, keep the temperature 30min, then continue with the speed of 15 DEG C/min to be warming up to 1700 DEG C, then again with
The speed of 10 DEG C/min is continuously heating to 2150 DEG C, keeps the temperature 60min, is then first cooled to 1500 DEG C with the speed of 10 DEG C/min,
Natural cooling again obtains boron carbide/carborundum composite-phase ceramic.
By test it is found that the consistency of boron carbide/carborundum composite-phase ceramic prepared by the present embodiment is 98%, density
For 2.56g/cm3, elasticity modulus 390GPa, Vickers hardness 29GPa, bending strength 540MPa, fracture toughness is
6.2MPa·m1/2。
Embodiment 2
A kind of boron carbide/carborundum composite-phase ceramic, the raw material gross mass to prepare the complex phase ceramic are institute in terms of 100%
The mass percent stated the composition of raw material and respectively formed is as follows：Boron carbide powder (granularity is 0.8 μm, purity 97%)
80%, carborundum powder (granularity be 0.8 μm, purity 97%) 15%, carbon dust 2%, boronation zirconium powder 1% and cerium oxide powder 2%,
Its preparation process is as follows：
Batch mixing ball milling：By in raw material each ingredient and deionized water be added in ball grinder, under 400r/min rotating speeds
Ball milling 10h obtains uniformly mixed slurry；Wherein, 300mL deionized waters are added as grinding aid in every 100g raw materials；
Mist projection granulating：Uniformly mixed slurry is uniformly mixed with the PVA aqueous solutions that mass fraction is 5% first, then is sprayed into
In granulation tower, the pelletizing that particle size is 150 μm is obtained；Wherein, 160 DEG C of the inlet air temperature of granulation tower, leaving air temp 120
DEG C, atomisation pressure 0.3MPa；
It is dry-pressing formed：Pelletizing is placed in sintered-carbide die, is pressed by the way of Bidirectional-pressure,
Under 150MPa pressure after pressurize 3min, demoulding obtains green compact；
Pressureless sintering：It puts the green body into non-pressure sintering furnace, is sintered under argon gas atmosphere protection, wherein first with 5
DEG C/speed of min is warming up to 900 DEG C, keep the temperature 30min, then continue with the speed of 15 DEG C/min to be warming up to 1700 DEG C, then again with
The speed of 10 DEG C/min is continuously heating to 2100 DEG C, keeps the temperature 60min, is then first cooled to 1500 DEG C with the speed of 5 DEG C/min, then
Natural cooling obtains boron carbide/carborundum composite-phase ceramic.
By test it is found that the consistency of boron carbide/carborundum composite-phase ceramic prepared by the present embodiment is 98%, density
For 2.70g/cm3, elasticity modulus 400GPa, Vickers hardness 27GPa, bending strength 480MPa, fracture toughness is
5.8MPa·m1/2。
Embodiment 3
A kind of boron carbide/carborundum composite-phase ceramic, the raw material gross mass to prepare the complex phase ceramic are institute in terms of 100%
The mass percent stated the composition of raw material and respectively formed is as follows：Boron carbide powder (granularity is 0.8 μm, purity 97%)
70%, carborundum powder (granularity is 0.5 μm, purity 97%) 15%, carbon dust 5%, alumina powder 4%, 2% He of boronation zirconium powder
Cerium oxide powder 4%, preparation process is as follows：
Batch mixing ball milling：By in raw material each ingredient and deionized water be added in ball grinder, under 400r/min rotating speeds
Ball milling 6h obtains uniformly mixed slurry；Wherein, 300mL deionized waters are added as grinding aid in every 100g raw materials；
Mist projection granulating：Uniformly mixed slurry is uniformly mixed with the PVA aqueous solutions that mass fraction is 3% first, then is sprayed into
In granulation tower, the pelletizing that particle size is 100 μm is obtained；Wherein, 180 DEG C of the inlet air temperature of granulation tower, leaving air temp 120
DEG C, atomisation pressure 0.2MPa；
It is dry-pressing formed：Pelletizing is placed in sintered-carbide die, is pressed by the way of Bidirectional-pressure,
Under 200MPa pressure after pressurize 2min, demoulding obtains green compact；
Pressureless sintering：It puts the green body into non-pressure sintering furnace, is sintered in argon gas atmosphere protectiveness, wherein first with 10
DEG C/speed of min is warming up to 900 DEG C, keep the temperature 30min, then continue with the speed of 10 DEG C/min to be warming up to 1700 DEG C, then again with
The speed of 5 DEG C/min is continuously heating to 2150 DEG C, keeps the temperature 60min, is then first cooled to 1500 DEG C with the speed of 7 DEG C/min, then
Natural cooling obtains boron carbide/carborundum composite-phase ceramic.
By test it is found that the consistency of boron carbide/carborundum composite-phase ceramic prepared by the present embodiment is 97%, density
For 2.78g/cm3, elasticity modulus 390GPa, Vickers hardness 26GPa, bending strength 410MPa, fracture toughness is
5.0MPa·m1/2。
The present invention includes but not limited to above example, it is every carried out under the spirit and principles in the present invention it is any etc.
With replacement or local improvement, all will be regarded as within protection scope of the present invention.
Claims (7)
1. a kind of boron carbide/carborundum composite-phase ceramic, it is characterised in that：Raw material gross mass to prepare the complex phase ceramic is
100% meter, the composition of the raw material and the mass percent respectively formed are as follows：Boron carbide powder 56%~90%, carborundum powder
5%~30%, carbon dust 0.5%~5%, alumina powder 0~5%, boronation zirconium powder 0~5% and rare earth oxide 0.5%~
5%.
2. a kind of boron carbide/carborundum composite-phase ceramic according to claim 1, it is characterised in that：Rare earth oxide is
CeO2、Y2O3Or La2O3。
3. a kind of boron carbide/carborundum composite-phase ceramic according to claim 1, it is characterised in that：The boron carbide powder
Granularity is (0.5~1.0) μm, purity >=96%.
4. a kind of boron carbide/carborundum composite-phase ceramic according to claim 1, it is characterised in that：The carborundum powder
Granularity is (0.3~0.8) μm, purity >=96%.
5. a kind of preparation method of such as Claims 1 to 4 any one of them boron carbide/carborundum composite-phase ceramic, feature exist
In：Steps are as follows for the method,
Batch mixing ball milling：By in raw material each ingredient and deionized water be added in ball grinder, be uniformly mixed obtain slurry；
Mist projection granulating：Slurry is uniformly mixed with polyvinyl alcohol water solution first, then sprays into granulation tower and is granulated, obtains particle
The pelletizing that size is 20 μm~200 μm；
It is dry-pressing formed：Pelletizing is placed in mold, pressurize 0.5min~5min under the pressure of 150MPa~200MPa, is taken off
Mould obtains green compact；
Pressureless sintering：It puts the green body into non-pressure sintering furnace, is sintered under vacuum condition or argon gas atmosphere protection；Its
In, 500 DEG C~900 DEG C first are warming up to the speed of 5 DEG C/min~10 DEG C/min, keeps the temperature 15min~60min, then with 5 DEG C/min
The speed of~15 DEG C/min continues to be warming up to 1500 DEG C~1900 DEG C, is then continued again with the speed of 5 DEG C/min~20 DEG C/min
2050 DEG C~2250 DEG C are warming up to, 30min~120min is kept the temperature, is then first cooled to the speed of 5 DEG C/min~15 DEG C/min
1900 DEG C~1500 DEG C, then natural cooling or be quickly cooled down, obtain boron carbide/carborundum composite-phase ceramic.
6. a kind of preparation method of boron carbide/carborundum composite-phase ceramic according to claim 5, it is characterised in that：Batch mixing
In mechanical milling process, ball milling 4h~12h, obtains slurry under 200r/min~600r/min rotating speeds；Wherein, add in every 100g raw materials
Enter 200mL~400mL deionized waters.
7. a kind of preparation method of boron carbide/carborundum composite-phase ceramic according to claim 5, it is characterised in that：Spraying
In granulation process, 150 DEG C~180 DEG C of inlet air temperature, 80 DEG C~130 DEG C, atomisation pressure 0.05MPa~0.5MPa of leaving air temp,
The mass fraction of polyvinyl alcohol water solution is 1%~5%.
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| CN111423233A (en) * | 2020-05-27 | 2020-07-17 | 陕西科技大学 | Silicon carbide reinforced boron carbide-based ceramic material and preparation method thereof |
| CN112079642A (en) * | 2020-08-17 | 2020-12-15 | 沈阳中钛装备制造有限公司 | Boron carbide spray granulation powder and preparation method and application thereof |
| CN112209718A (en) * | 2020-09-03 | 2021-01-12 | 沈阳中钛装备制造有限公司 | Boron carbide-based multiphase ceramic and preparation method and device thereof |
| CN113666750A (en) * | 2021-08-16 | 2021-11-19 | 中硼科技(威海)有限公司 | Light high-performance boron carbide-based bulletproof ceramic and preparation method thereof |
| CN114591086A (en) * | 2022-03-31 | 2022-06-07 | 中国兵器工业第五二研究所烟台分所有限责任公司 | Nano powder modified silicon carbide-boron carbide composite ceramic and preparation method thereof |
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| CN115572878A (en) * | 2022-09-30 | 2023-01-06 | 蒋孟瑶 | Hard alloy material and preparation method and application thereof |
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| CN113666750A (en) * | 2021-08-16 | 2021-11-19 | 中硼科技(威海)有限公司 | Light high-performance boron carbide-based bulletproof ceramic and preparation method thereof |
| CN114621024A (en) * | 2022-03-23 | 2022-06-14 | 山东华屹科创纳米材料有限公司 | High-purity toughened boron carbide foamed ceramic and preparation method thereof |
| CN114591086A (en) * | 2022-03-31 | 2022-06-07 | 中国兵器工业第五二研究所烟台分所有限责任公司 | Nano powder modified silicon carbide-boron carbide composite ceramic and preparation method thereof |
| CN115572878A (en) * | 2022-09-30 | 2023-01-06 | 蒋孟瑶 | Hard alloy material and preparation method and application thereof |
| CN117185817A (en) * | 2023-09-08 | 2023-12-08 | 兰溪泛翌精细陶瓷有限公司 | High-performance boron carbide composite material and preparation method thereof |
| CN117185817B (en) * | 2023-09-08 | 2024-04-09 | 兰溪泛翌精细陶瓷有限公司 | High-performance boron carbide composite material and preparation method thereof |
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