CN109704772A - A kind of boron-carbide-based ceramic composite material and preparation method of original position toughening - Google Patents
A kind of boron-carbide-based ceramic composite material and preparation method of original position toughening Download PDFInfo
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- CN109704772A CN109704772A CN201910167454.0A CN201910167454A CN109704772A CN 109704772 A CN109704772 A CN 109704772A CN 201910167454 A CN201910167454 A CN 201910167454A CN 109704772 A CN109704772 A CN 109704772A
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Abstract
The invention discloses the boron-carbide-based ceramic composite materials and preparation method of a kind of toughening in situ, belong to field of material synthesis technology.Each component mass percent is as follows: the molybdenum disilicide of the boron carbide of 65wt%-95wt%, 5wt%-35wt%.The preparation process is as follows: by boron carbide powder and molybdenum silicide powder using dehydrated alcohol as medium, ball milling mixing is sieved and is dried under vacuum condition；By the isometric compression molding of powder, biscuit is made in isostatic cool pressing after vacuum packaging；Boron carbide ceramics composite material will be sintered to obtain under the biscuit vacuum processed.Boron carbide ceramics composite material of the invention has the characteristics that high-compactness and high tenacity, while present device is simple, and it is convenient to operate, and maintains easily and overhauls, and production cost is low, is suitble to large-scale production.
Description
Technical field
The invention belongs to technical field of composite materials, and in particular to the boron-carbide-based ceramic composite material of toughening in situ
Preparation method.
Background technique
Boron carbide ceramics is excellent because having low-density, high rigidity, good wearability and biggish neutron-absorbing interface etc.
It is benign can thus be widely used in bulletproof armour and with the fields such as nuclear screening material.But due to the covalent linkage content of boron carbide compared with
Height, sintering densification are difficult.Though hot pressed sintering can be obtained close to fully dense boron carbide ceramics, its single shape of product and
Expensive expense limits its large-scale application industrially.Though pressureless sintering spends relative moderate and can make all kinds of shapes
Boron carbide ceramics, but its resulting boron carbide ceramics consistency is still relatively low.In addition, the fracture toughness of boron carbide ceramics
It is lower, only about 2.2MPam1/2.Problems above limits further applying for boron carbide ceramics.
Currently, in order to improve the consistency and fracture toughness of sintering gained boron carbide ceramics, silicon carbide and some metal boron
The compound such as additives such as titanium boride, chromium boride and zirconium boride are added in boron carbide to be carbonized as sintering aid service hoisting
The consistency and fracture toughness of boron ceramics.Silicon carbide is introduced in boron carbide by former unreacted mode and metal boride can
So that the distribution of the second phase is more uniform, the consistency and fracture toughness of boron carbide ceramics can be also improved.In addition, addition sintering aid
For example iron, aluminium, silicon, chromium boride etc. are able to achieve liquid-phase sintering, can obtain fine and close boron carbide ceramics composite material.
Summary of the invention
In prior art basis, react in situ raw with boron carbide in pressureless sintering using molybdenum disilicide as sintering aid
At metal boride (molybdenum diboride, five boronations, two molybdenum) and silicon carbide, and it is real using the fusing of molybdenum boride during the sintering process
Existing liquid-phase sintering, is obviously improved the consistency and fracture toughness of gained boron carbide ceramics composite material.
The partial size of the molybdenum disilicide is 0.1 μm -8 μm, and the purity of molybdenum disilicide is 98wt%-99.5wt%, and opposite
In the mixture siccative gross mass, the mass percentage of molybdenum disilicide can be 5wt%-35wt%.
The average grain diameter of the boron carbide can be 0.2 μm -8 μm, and boron carbide powder purity is 95wt%-99.8wt%, and
Relative to the mixture siccative gross mass, the mass percentage of boron carbide can be 65wt%-95wt%.
Method of the invention sequentially includes the following steps:
(1) it weighs, will claim according to the boron-carbide-based ceramic composite material constituent and its mass percent of toughening in situ
Boron carbide, the molybdenum silicide powder taken is put into ball mill, is carried out wet-milling by medium of dehydrated alcohol, is taken slurry after 2h-24h
Out；
(2) at 50 DEG C -130 DEG C in drying 1h-20h in vacuum drying oven, 20-120 mesh is then crossed；
(3) slurry of solids after sieving is packed into mold cavity, it is molded in the inferior Axle mould of 20MPa-120MPa pressure, it protects
The pressure time is 1min-5min；
(4) gained green body is put into Vacuum Package in vacuum packaging bag, is put into cold isostatic press later in 150MP-
Biscuit is made in isostatic cool pressing under 300MPa pressure, dwell time 2min-8min；
(5) biscuit being put into vacuum sintering furnace, vacuum condition Gradient is warming up to 2150 DEG C -2260 DEG C and is sintered,
Furnace cooling after heat preservation 1h-5h；It cut, obtain the boron-carbide-based ceramic composite material of toughening in situ after polishing treatment.
The binder being added during the wet-milling of above-mentioned steps (1) is hydroxypropyl methyl cellulose, accounts for stock quality hundred
Divide than being 0.01wt%-5wt%.
Ball material mass ratio is 3-8, rotational speed of ball-mill 200r/min-600r/min during the wet-milling of above-mentioned steps (1).
The Vacuum packing processes vacuum packaging bag of above-mentioned steps (3) is food pack or rubber bag, is vacuumized and hot
Envelope temporal summation is 10s-20s.
The gradient increased temperature of above-mentioned steps (3) is to rise to 1800 DEG C from room temperature with the heating rate of 20 DEG C/min-30 DEG C/min,
Then 2000 DEG C are risen to from 1800 DEG C with 10 DEG C/min-20 DEG C/min heating rate, is finally risen to 5 DEG C/min-10 DEG C/min
2150℃-2260℃。
The present invention can react in-situ preparation metal boron using molybdenum disilicide as sintering aid in pressureless sintering with boron carbide
Compound (molybdenum diboride, five boronations, two molybdenum) and silicon carbide, and realize that liquid phase is burnt using the fusing of molybdenum boride during the sintering process
Knot, can be obviously improved the consistency of boron-carbide-based ceramic composite material.The silicon carbide toughness of generation is higher than boron carbide, and generates
Molybdenum diboride and five boronations, two molybdenum will lead to the deflection and bridging of crackle since thermal diffusion coefficient and boron carbide mismatch, thus
The toughness of resulting boron-carbide-based ceramic composite material significantly improves.
This method is simple and effective, it is easy to accomplish industrialized production.
Detailed description of the invention
Fig. 1 is a kind of XRD of boron-carbide-based ceramic composite material method for preparing toughening in situ of the embodiment of the present invention 1
Figure.
Fig. 2 is a kind of SEM of boron-carbide-based ceramic composite material method for preparing toughening in situ of the embodiment of the present invention 1
Figure.
Fig. 3 is a kind of process of the technique of boron-carbide-based ceramic composite material method for preparing toughening in situ of the invention
Figure.
Specific embodiment
In order to which the present invention is more clearly understood, below in conjunction with specific example, invention is further described in detail.It answers
Work as understanding, specific implementation case described herein is only used to explain the present invention, be not intended to limit the present invention.
The test method of fracture toughness uses Single edge notch beam in present example, using electronic universal mechanical test
Machine.
Embodiment 1
By average grain diameter be 0.7 μm boron carbide powder 40g, average grain diameter be 2 μm of molybdenum disilicide powder 12g, hydroxypropyls
Mixed powder, is put into 105 DEG C of baking oven by methylcellulose 0.08g, 260g abrading-ball and 40g dehydrated alcohol ball milling mixing 6h
Interior dry 4h, then crosses 40 meshes for powder.Material after sieving is packed into mold cavity, in the inferior Axle mould pressure of 40MPa pressure
Gained green body is put into Vacuum Package in vacuum packaging bag by molding, dwell time 2min, and time 15s is put into cold etc. later
Biscuit is made in isostatic cool pressing, dwell time 3min under 215MPa pressure in static pressure machine.Biscuit is put into furnace and is sintered, with
The heating rate of 30 DEG C/min rises to 1800 DEG C from room temperature, then rises to 2000 DEG C from 1800 DEG C with 20 DEG C/min heating rate,
2200 DEG C finally are risen to 10 DEG C/min, and keeps the temperature 1h, the consistency for obtaining boron carbide ceramics is 95.5%, and fracture toughness is
3.93MPa·m1/2。
It can be seen that obtained boron carbide ceramics composite material mainly by B from Fig. 1 and Fig. 24C、MoB2、Mo2B5、SiC
With five phase composition of C, show that molybdenum disilicide and boron carbide reaction in-situ generate molybdenum boride and silicon carbide.And pass through reaction in-situ
Mode make generate molybdenum boride and silicon carbide be evenly distributed in matrix.Irregular, connection molybdenum boride shape table
Liquid phase is formed in bright sintering process, is filled stomata, is improved the consistency of boron carbide ceramics.Molybdenum boride and boron carbide generated
Thermal expansion coefficient mismatches, and the toughness for improving obtained boron carbide ceramics composite material significantly improves.
Embodiment 2
By average grain diameter be 0.5 μm boron carbide powder 35g, average grain diameter be 1 μm of molybdenum disilicide powder 8.75g, hydroxypropyl
Mixed powder, is put into 105 DEG C of baking by ylmethyl cellulose 0.09g, 175g abrading-ball and 35g dehydrated alcohol ball milling mixing 6h
Dry 5h, then crosses 40 meshes for powder in case.Material after sieving is packed into mold cavity, in the inferior Axle mould of 50MPa pressure
Molded, gained green body is put into Vacuum Package in vacuum packaging bag by dwell time 1min, and time 16s is put into cold later
Biscuit is made in isostatic cool pressing, dwell time 4min under 175MPa pressure in isostatic pressing machine.Biscuit is put into furnace and is sintered,
1800 DEG C are risen to from room temperature with the heating rate of 25 DEG C/min, then rises to 2000 from 1800 DEG C with 20 DEG C/min heating rate
DEG C, 2260 DEG C finally are risen to 10 DEG C/min, and keep the temperature 2h, the consistency for obtaining boron carbide ceramics is 96.3%, fracture toughness
For 3.95MPam1/2。
Embodiment 3
By average grain diameter be 1.5 μm boron carbide powder 35g, average grain diameter be 3 μm of molybdenum disilicide powder 10.05g, hydroxypropyls
Ylmethyl cellulose 0.1g, 270.3g abrading-ball and 45g dehydrated alcohol ball milling mixing 5h, are put into 105 DEG C for mixed powder
Dry 4h, then crosses 40 meshes for powder in baking oven.Material after sieving is packed into mold cavity, it is isometric under 70MPa pressure
Gained green body is put into Vacuum Package in vacuum packaging bag by compression molding, dwell time 1min, and time 14s is put into later
Biscuit is made in isostatic cool pressing, dwell time 2min under 288MPa pressure in cold isostatic press.Biscuit is put into furnace and is burnt
Knot, is risen to 1800 DEG C from room temperature with the heating rate of 30 DEG C/min, is then risen to 20 DEG C/min heating rate from 1800 DEG C
2000 DEG C, 2150 DEG C finally are risen to 5 DEG C/min, and keep the temperature 1h, the consistency for obtaining boron carbide ceramics is 94.5%, is broken tough
Property is 3.65MPam1/2。
Claims (8)
1. a kind of boron-carbide-based ceramic composite material of original position toughening, which is characterized in that the component of the composite material includes two kinds
Substance, the mass percent of each component are as follows: the boron carbide of 65wt%-95wt%, the molybdenum disilicide of 5wt%-35wt%.
2. the boron-carbide-based ceramic composite material of original position toughening according to claim 1, which is characterized in that the carbonization
Boron powder purity is 95wt%-99.8wt%, and average grain diameter is 0.2 μm -8 μm.
3. the boron-carbide-based ceramic composite material of original position toughening according to claim 1, which is characterized in that two silicon
The purity for changing molybdenum is 98wt%-99.5wt%, and average grain diameter is 0.1 μm -8 μm.
4. the preparation method of the boron-carbide-based ceramic composite material of any toughening in situ of claim 1-3, which is characterized in that including
Following steps:
(1) it weighs, will weigh according to the boron-carbide-based ceramic composite material constituent and its mass percent of toughening in situ
Boron carbide, molybdenum silicide powder be put into ball mill, carry out wet-milling by medium of dehydrated alcohol, take out slurry after 2h-24h；
(2) at 50 DEG C -130 DEG C in drying 1h-20h in vacuum drying oven, 20-120 mesh is then crossed；
(3) slurry of solids after sieving is packed into mold cavity, it is molded in the inferior Axle mould of 20MPa-120MPa pressure, when pressure maintaining
Between be 1min-5min；
(4) gained green body is put into Vacuum Package in vacuum packaging bag, is put into cold isostatic press later in 150MP-300MPa
Biscuit is made in isostatic cool pressing under pressure, dwell time 2min-8min；
(5) biscuit is put into vacuum sintering furnace, vacuum condition Gradient is warming up to 2150 DEG C -2260 DEG C and is sintered, heat preservation
Furnace cooling after 1h-5h；It cut, obtain the boron-carbide-based ceramic composite material of toughening in situ after polishing treatment.
5. the preparation method of the boron-carbide-based ceramic composite material of toughening in situ according to claim 4, which is characterized in that step
Suddenly the binder for accounting for stock quality 0.01wt%-5wt% is added during wet-milling described in (1), binder is hydroxypropyl methyl
Cellulose.
6. the preparation method of the boron-carbide-based ceramic composite material of toughening in situ according to claim 4, which is characterized in that step
Suddenly the material mass ratio of wet-milling process ball described in (1) is 3-8, rotational speed of ball-mill 200r/min-600r/min.
7. the preparation method of the boron-carbide-based ceramic composite material of toughening in situ according to claim 4, which is characterized in that step
Suddenly Vacuum packing processes vacuum packaging bag described in (3) is food pack or rubber bag, is vacuumized and heat-sealing temporal summation
For 10s-20s.
8. the preparation method of the boron-carbide-based ceramic composite material of toughening in situ according to claim 4, which is characterized in that step
Suddenly gradient increased temperature described in (3) is to rise to 1800 DEG C from room temperature with the heating rate of 20 DEG C/min-30 DEG C/min, then with 10
DEG C/min-25 DEG C/min heating rate from 1800 DEG C rises to 2000 DEG C, finally with 5 DEG C/min-15 DEG C/min rise to 2150 DEG C-
2260℃。
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| CN110590373A (en) * | 2019-10-28 | 2019-12-20 | 中原工学院 | MoSi prepared by Flashing method2Method for preparing-MoB-SiC three-phase composite material |
| CN111018530A (en) * | 2019-12-18 | 2020-04-17 | 赛福纳米科技(徐州)有限公司 | High-hardness ultra-light ceramic composite material and preparation method thereof |
| CN111825458A (en) * | 2020-07-31 | 2020-10-27 | 中南大学 | High-density boron carbide ceramic material and pressureless sintering preparation method thereof |
| CN113788681A (en) * | 2021-10-12 | 2021-12-14 | 景德镇学院 | Boron carbide light bulletproof material and preparation method thereof |
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Cited By (4)
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