CN102886942B - Layered composite boron carbide ceramic material and its preparation method - Google Patents
Layered composite boron carbide ceramic material and its preparation method Download PDFInfo
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Abstract
A layered composite boron carbide ceramic material and its preparation method belong to the technical field of materials. The layered composite boron carbide ceramic material is prepared from a base layer of a B4C ceramic layer and a composite layer to form a gradient distribution material, wherein a double-layer composite boron carbide ceramic material is composed of Al/B4C-B4C, and a three-layer composite boron carbide ceramic material is composed of Al/B4C-TiB2/B4C-B4C. The preparation method comprises three steps of burdening forming, hot-pressing presintering and vacuum infiltration. The layered composite ceramic material is light in weight; the matrix of each layer is B4C; and the layers of the material are combined very well. Through the composition of the multiple layers, shock resistance of the material is greatly raised. Based on a single boron carbide material, fracture toughness of the material provided by the invention is raised. The layered composite boron carbide ceramic material has a wide application prospect in the field of bullet resistant materials.
Description
Technical field
The invention belongs to technical field of ceramic material, be specifically related to a kind of stratiform compound carbonizing boryl ceramic material and preparation method thereof.
Background technology
Boron carbide has the advantages that low, the antiacid caustic corrosion ability of density is good, neutron-absorbing ability is strong, but also there is the hardness of superelevation, particularly its constant high temperature hardness is that other materials is incomparable, is one of ceramic material adapting to the demands such as bullet resistant material lightweight high rigidity.
The good combination properties such as ceramic material 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, thermal coefficient of expansion is little, density is low, it is all obviously better than metal material, macromolecular material and composite thereof at aspects such as shellproof energy-absorbing effect, wear effects, kinetic effects, and obtained actual application in military project protection, become one of greatly leading material of three in armor facing.Countries in the world are all paid much attention to the research of Ceramic Composite bullet resistant material, this research mainly concentrates on the aspects such as ceramic-metal is compound, pottery-polyester thin slice is compound, steel-ceramic-steel is compound, these composites all belong to the laminar composite in macroscopic view, have between layers the laminar composite that physical property sudden change occurs between sharp interface and each layer.The ceramic-metal composite material being formed by pottery and metal composite, although there is lot of advantages, but in the time that internal stress increases, can cause the destruction of material, and its density due to the relative ceramic material of existence of metal for not having advantage on armoring bullet resistant material yet.On the other hand, although pottery meets the requirement of bullet resistant material to lightweight with the composite of polyester thin slice, because the unfavorable factors such as slabbing destruction are concentrated, easily caused to the inter-laminar stress that the sudden change of material behavior causes.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of stratiform compound carbonizing boryl ceramic material and preparation method thereof is provided, this laminar composite quality is light, and hardness and intensity are high.
A kind of stratiform compound carbonizing boryl ceramic material, its main points are by base layer B
4c ceramic layer and composite bed form, wherein base layer B
4the composition of C ceramic layer is 94.5wt%B
4c, 2.5wt% titanium valve and 3wt% carbon black; Composite bed consists of Al/B
4c aluminized coating or Al/B
4c aluminized coating and TiB
2/ B
4c intermediate layer; Described Al/B
4c aluminized coating is made after vacuum infiltration aluminium by porous boron carbide pre-burning body layer, and the aluminium of infiltration accounts for the 20wt% of whole aluminized coating quality; Described TiB
2/ B
4c intermediate layer is by B
4c and TiB
2powder is B in mass ratio
4c:TiB
2=7:3 batching obtains after hot-forming and infiltration;
Porous boron carbide pre-burning body layer be respectively 4.4 μ m and 260 μ m by average grain diameter two kinds of boron carbide powders in mass ratio 7:3 mix, form through hot pressing pre-burning.
As the B of stratiform compound carbonizing boryl ceramic material
4when C ceramic layer is stress surface, its hardness is 33.0-34.2GPa, and fracture toughness is 4.8-6.0MPam
1/2, bending strength is 266.0-275.0MPa; As the Al/B of stratiform compound carbonizing boryl ceramic material
4when C aluminized coating is stress surface, its hardness is 72.5HRA, and fracture toughness is 5.8-6.1MPam
1/2, bending strength is 88.0-168.4MPa.
The preparation method of a kind of stratiform compound carbonizing of the present invention boryl ceramic material carries out according to the following steps:
(1) base layer and composite bed are proportionally prepared burden, B
4the boron carbide powder that C ceramic matrix layer raw material is 4.4 μ m by average grain diameter accounts for raw material total amount 94.5 wt%, and average grain diameter is that to account for raw material total amount 2.5wt% and average grain diameter be that the carbon black of 0.8 μ m accounts for raw material total amount 3wt% and prepares burden to the titanium valve of 48 μ m; In composite bed, porous boron carbide pre-burning body layer raw material is the B of 260 μ m by particle diameter
4c powder and particle diameter are the B of 4.4 μ m
4c powder quality is prepared burden than 7:3; After having prepared burden, carry out ball mill mixing, to B
4c ceramic matrix layer raw material carries out wet ball-milling 6h, and ball-milling medium is absolute ethyl alcohol, and ball milling ball is Si
3n
4ball is then dried 18h in 60 DEG C in baking oven; Two kinds of varigrained boron carbide powder ball milling of porous boron carbide pre-burning body layer to composite bed are dry mixed 4h, and ball-milling medium is spring-like iron wire, the powder being mixed respectively; To mix the successively compression molding under 5.5 ~ 6MPa pressure jointly of two-layer powder, obtain two-layer compound powder;
Or B
4the boron carbide powder that C ceramic matrix layer raw material is 4.4 μ m by average grain diameter accounts for raw material total amount 94.5 wt%, and average grain diameter is that to account for raw material total amount 2.5wt% and average grain diameter be that the carbon black of 0.8 μ m accounts for raw material total amount 3wt% and prepares burden to the titanium valve of 48 μ m; In composite bed, porous boron carbide pre-burning body layer Raw is the B of 260 μ m by particle diameter
4c powder and particle diameter are the B of 4.4 μ m
4c powder quality is prepared burden than 7:3, B
4c/TiB
2intermediate layer is B in mass ratio
4c:TiB
2=7:3 prepares burden, the average grain diameter 4.4 μ m of boron carbide powder, TiB
2the average grain diameter of powder is 5 μ m; After having prepared burden, carry out ball mill mixing, to B
4the TiB of C ceramic matrix layer raw material and composite bed
2/ B
4c intermediate layer raw material carries out wet ball-milling 6h, and ball-milling medium is absolute ethyl alcohol, and ball milling ball is Si
3n
4ball is then dried 18h in 60 DEG C in baking oven; Two kinds of varigrained boron carbide powder ball milling of porous boron carbide pre-burning body layer to composite bed are dry mixed 4h, and ball-milling medium is spring-like iron wire, obtains the each layer of powder mixing respectively; By the base layer powder mixing and the successively compression molding under 5.5 ~ 6MPa pressure jointly of composite bed powder, obtain three layers of composite granule;
(2) hot pressing pre-burning
The stratiform composite granule of compression molding is placed in to hot-pressed sintering furnace, be evacuated to lower than 30Pa, be warming up to 1500 DEG C of insulation 30～80min with the heating rate of 5～8 DEG C/min, then be warming up to 1860～1920 DEG C with the heating rate of 4～7 DEG C/min, pressure remains on 28 MPa, insulation 30～50min, obtains the boron carbide-based loose structure pre-burning of stratiform body;
(3) vacuum infiltration aluminium
Boron carbide-based bilayer loose structure pre-burning body is placed in to vacuum melting furnace, Al alloy block is placed in to the boron carbide-based porous pre-burning of stratiform body top, carry out vacuum infiltration aluminium, being evacuated to vacuum is 5～10Pa, and energising is warming up to 700 DEG C, insulation 30 min, be warming up to again at 1000～1080 DEG C and be incubated 70 ~ 120min, the heating rate of whole process is 200 DEG C/h, controls constant temperature precision within the scope of ± 5 DEG C, obtains stratiform compound carbonizing boryl ceramic material.
The purity of all boron carbide powders of the present invention is all 99%, described TiB
2the purity of powder is 98%
Aluminium alloy of the present invention is commercial aluminum alloy, and the trade mark is 5083,5086,5A12 or 7005.
Compared with current studied bulletproof ceramic composite, the invention has the beneficial effects as follows:
(1) stratiform compound carbonizing boryl ceramic material quality of the present invention is light, can greatly improve the impact resistance of material by MULTILAYER COMPOSITE, can alleviate greatly the weight of bullet resistant material;
(2) stratiform compound carbonizing boryl ceramic material of the present invention improves 2.14～2.78 times of fracture toughnesses on the basis of single boron carbide material, makes the application of boron carbide ceramics material more extensive;
(3) each layer of matrix of stratiform compound carbonizing boryl ceramic material of the present invention is B
4, so the combination between layers of bullet resistant material is very intact, there is not the performance sudden change of obvious interlayer, so can well avoid the phenomenon of slabbing in C.
Detailed description of the invention
Embodiment 1:
(1) forming ingredient
Base layer B
4the boron carbide powder that C ceramic layer raw material is 4.4 μ m by average grain diameter accounts for raw material total amount 94.5 wt%, and average grain diameter is that to account for raw material total amount 2.5wt% and average grain diameter be that the carbon black of 0.8 μ m accounts for raw material total amount 3wt% and prepares burden to the titanium valve of 48 μ m; Composite bed porous boron carbide pre-burning body layer Raw is the B of 260 μ m by average grain diameter
4c powder and average grain diameter are the B of 4.4 μ m
4c powder quality is prepared burden than 7:3; The purity of all boron carbide powders is all 99%; To base layer B
4c ceramic layer raw material wet ball-milling 6h, ball-milling medium is absolute ethyl alcohol, ball milling ball is Si
3n
4ball, then in baking oven in 60 DEG C dry 18h, two kinds of varigrained boron carbide powder ball milling of composite bed porous boron carbide pre-burning body layer are dry mixed to 4h, ball-milling medium is spring-like iron wire, obtains the two-layer powder mixing respectively; By two-layer composite granule after mixing respectively, successively compression molding under 5.5MPa pressure, obtains two-layer compound powder;
(2) hot pressing pre-burning
The two-layer compound powder of compression molding is placed in to hot-pressed sintering furnace, be evacuated to lower than 30Pa, be warming up to 1500 DEG C of insulations 60 minutes with the heating rate of 5～8 DEG C/min, and then be warming up to 1860 DEG C with the heating rate of 4～7 DEG C/min, pressure remains 28 MPa, and insulation 50min obtains double-deck boron carbide-based loose structure pre-burning body;
(3) vacuum infiltration
Boron carbide-based bilayer loose structure pre-burning body is placed in to vacuum melting furnace, Al alloy block is placed in to double-deck boron carbide-based porous pre-burning body top, carry out vacuum infiltration aluminium, be evacuated to 5Pa, energising is warming up to 700 DEG C, be incubated 30 min, be warming up to again 1000 DEG C, insulation 120 min, the heating rate of whole process is 200 DEG C/h, control constant temperature precision within the scope of ± 5 DEG C, obtain Al/B
4c-B
4the double-deck boron-carbide-based ceramic composite material of C.
After testing, work as B
4when C ceramic layer is stress surface, its hardness is 33GPa, fracture toughness 4.8MPam
1/2, bending strength 275.0MPa, this result has improved 2.18 times than the fracture toughness of single boron carbide material; Work as Al/B
4when C aluminized coating is stress surface, its hardness is 72.5HRA, fracture toughness 5.8MPam
1/2, bending strength 168.4MPa, this result has improved 2.64 times than the fracture toughness of single boron carbide material.
Embodiment 2:
(1) forming ingredient
Base layer B
4the boron carbide powder that C ceramic layer raw material is 4.4 μ m by average grain diameter accounts for raw material total amount 94.5 wt%, and average grain diameter is that to account for raw material total amount 2.5wt% and average grain diameter be that the carbon black of 0.8 μ m accounts for raw material total amount 3wt% and prepares burden to the titanium valve of 48 μ m; Composite bed porous boron carbide pre-burning body layer Raw is the B of 260 μ m by average grain diameter
4c powder and average grain diameter are the B of 4.4 μ m
4c powder quality is prepared burden than 7:3, B
4c/TiB
2intermediate layer is B in mass ratio
4c:TiB
2=7:3 prepares burden, the average grain diameter 4.4 μ m of boron carbide powder, TiB
2the average grain diameter of powder is 5 μ m; The purity of all boron carbide powders is all 99%, described TiB
2the purity of powder is 98%; By base layer B
4the B of C ceramic layer raw material and composite bed
4c/TiB
2intermediate layer raw material puts into respectively that nylon ball grinder ball milling is wet closes 6h, and ball-milling medium is absolute ethyl alcohol, and ball milling ball is Si
3n
4ball, then in baking oven in 100 DEG C of dry 12h; Two kinds of varigrained boron carbide powder ball millings of the porous boron carbide pre-burning body layer to composite bed are dry mixed 4h, and ball-milling medium is spring-like iron wire; Powder after each layer is mixed, successively compression molding under 6MPa pressure, obtains three layers of composite granule;
(2) hot pressing pre-burning
The two-layer compound powder of compression molding is placed in to hot-pressed sintering furnace, be evacuated to lower than 30Pa, be warming up to 1500 DEG C of insulation 60min with the heating rate of 5～8 DEG C/min, then be warming up to 1920 DEG C with the heating rate of 4～7 DEG C/min, pressure remains on 28 MPa, insulation 30min, obtains three layers of boron carbide-based loose structure pre-burning body;
(3) vacuum infiltration
Three layers of boron carbide-based loose structure pre-burning body are placed in to vacuum melting furnace, Al alloy block is placed in to three layers of boron carbide-based porous pre-burning body top, carry out vacuum infiltration aluminium, be evacuated to 10Pa, energising is warming up to 700 DEG C, be incubated 30 min, be warming up to again 1080 DEG C, insulation 70 min, the heating rate of whole process is 200 DEG C/h, control constant temperature precision within the scope of ± 5 DEG C, obtain Al/B
4c-TiB
2/ B
4c-B
4tri-layers of boron-carbide-based ceramic composite material of C.
After testing, work as B
4when C ceramic layer is stress surface, its hardness is 34.2 GPa; Fracture toughness 6.0MPam
1/2; Bending strength 266.0MPa, this result has improved 2.73 times than the fracture toughness of single boron carbide material; Work as Al/B
4when C aluminized coating is stress surface, its hardness is 72.5HRA, and its fracture toughness is 6.1MPam
1/2, bending strength 88.0MPa, this result has improved 2.78 times than the fracture toughness of single boron carbide material.
Claims (5)
1. a stratiform compound carbonizing boryl ceramic material, is characterized in that by B
4c ceramic matrix layer and composite bed form, wherein B
4the composition of C ceramic matrix layer is 94.5wt%B
4c, 2.5wt% titanium valve and 3wt% carbon black; Composite bed consists of Al/B
4c aluminized coating or Al/B
4c aluminized coating and TiB
2/ B
4c intermediate layer; Described Al/B
4c aluminized coating is made after vacuum infiltration aluminium by porous boron carbide pre-burning body layer, the aluminium infiltrating accounts for the 20wt% of whole aluminized coating quality, described porous boron carbide pre-burning body layer be respectively 4.4 μ m and 260 μ m by particle mean size two kinds of boron carbide powders in mass ratio 7:3 mix, form through hot pressing pre-burning; Described TiB
2/ B
4c intermediate layer is by B
4c and TiB
2powder is B in mass ratio
4c:TiB
2=7:3 batching obtains after hot-forming and infiltration; As the B of stratiform compound carbonizing boryl ceramic material
4when C ceramic matrix layer is stress surface, its hardness is 33.0-34.2GPa, and fracture toughness is 4.8-6.0MPam
1/2, bending strength is 266-275.0MPa; As the Al/B of stratiform compound carbonizing boryl ceramic material
4when C aluminized coating is stress surface, its hardness is 72.5HRA, and fracture toughness is 5.8-6.1MPam
1/2, bending strength is 88.0-168.4MPa.
2. the preparation method of a kind of stratiform compound carbonizing boryl ceramic material as claimed in claim 1, is characterized in that carrying out according to the following steps:
(1) base layer and composite bed are proportionally prepared burden, B
4the boron carbide powder that C ceramic matrix layer raw material is 4.4 μ m by average grain diameter accounts for raw material total amount 94.5wt%, and average grain diameter is that to account for raw material total amount 2.5wt% and average grain diameter be that the carbon black of 0.8 μ m accounts for raw material total amount 3wt% and prepares burden to the titanium valve of 48 μ m; In composite bed, porous boron carbide pre-burning body layer raw material is the B of 260 μ m by particle diameter
4c powder and particle diameter are the B of 4.4 μ m
4c powder quality is prepared burden than 7:3; After having prepared burden, carry out ball mill mixing, to B
4c ceramic matrix layer raw material carries out wet ball-milling 6h, and ball-milling medium is absolute ethyl alcohol, and ball milling ball is Si
3n
4ball is then dried 18h in 60 DEG C in baking oven; Two kinds of varigrained boron carbide powder ball milling of porous boron carbide pre-burning body layer to composite bed are dry mixed 4h, and ball-milling medium is spring-like iron wire, the powder being mixed respectively; To mix the successively compression molding under 5.5～6MPa pressure jointly of two-layer powder, obtain two-layer compound powder;
(2) the two-layer compound powder of compression molding is placed in to hot-pressed sintering furnace, be evacuated to lower than 30Pa, be warming up to 1500 DEG C of insulation 30～80min with the heating rate of 5～8 DEG C/min, then be warming up to 1860～1920 DEG C with the heating rate of 4～7 DEG C/min, pressure remains on 28MPa, insulation 30～50min, obtains double-deck boron carbide-based loose structure pre-burning body;
(3) boron carbide-based bilayer loose structure pre-burning body is placed in to vacuum melting furnace, Al alloy block is placed in to double-deck boron carbide-based porous pre-burning body top, carry out vacuum infiltration aluminium, being evacuated to vacuum is 5～10Pa, and energising is warming up to 700 DEG C, insulation 30min, be warming up to again at 1000～1080 DEG C and be incubated 70～120min, the heating rate of whole process is 200 DEG C/h, controls constant temperature precision within the scope of ± 5 DEG C, obtains two-layer compound boron carbide base ceramic material.
3. the preparation method of a kind of stratiform compound carbonizing boryl ceramic material as claimed in claim 1, is characterized in that carrying out according to the following steps:
(1) base layer and composite bed are proportionally prepared burden, B
4the boron carbide powder that C ceramic matrix layer raw material is 4.4 μ m by average grain diameter accounts for raw material total amount 94.5wt%, and average grain diameter is that to account for raw material total amount 2.5wt% and average grain diameter be that the carbon black of 0.8 μ m accounts for raw material total amount 3wt% and prepares burden to the titanium valve of 48 μ m; In composite bed, porous boron carbide pre-burning body layer Raw is the B of 260 μ m by particle diameter
4c powder and particle diameter are the B of 4.4 μ m
4c powder quality is prepared burden than 7:3, B
4c/TiB
2intermediate layer is B in mass ratio
4c:TiB
2=7:3 prepares burden, the average grain diameter 4.4 μ m of boron carbide powder, TiB
2the average grain diameter of powder is 5 μ m; After having prepared burden, carry out ball mill mixing, to B
4the TiB of C ceramic matrix layer raw material and composite bed
2/ B
4c intermediate layer raw material carries out wet ball-milling 6h, and ball-milling medium is absolute ethyl alcohol, and ball milling ball is Si
3n
4ball is then dried 18h in 60 DEG C in baking oven; Two kinds of varigrained boron carbide powder ball milling of porous boron carbide pre-burning body layer to composite bed are dry mixed 4h, and ball-milling medium is spring-like iron wire, obtains the each layer of powder mixing respectively; By the base layer powder mixing and the successively compression molding under 5.5～6MPa pressure jointly of composite bed powder, obtain three layers of composite granule;
(2) three layers of composite granule of compression molding are placed in to hot-pressed sintering furnace, be evacuated to lower than 30Pa, be warming up to 1500 DEG C of insulation 30～80min with the heating rate of 5～8 DEG C/min, then be warming up to 1860～1920 DEG C with the heating rate of 4～7 DEG C/min, pressure remains on 28MPa, insulation 30～50min, obtains three layers of boron carbide-based loose structure pre-burning body;
(3) three layers of boron carbide-based loose structure pre-burning body are placed in to vacuum melting furnace, Al alloy block is placed in to three layers of boron carbide-based porous pre-burning body top, carry out vacuum infiltration aluminium, being evacuated to vacuum is 5～10Pa, and energising is warming up to 700 DEG C, insulation 30min, be warming up to again at 1000～1080 DEG C and be incubated 70～120min, the heating rate of whole process is 200 DEG C/h, controls constant temperature precision within the scope of ± 5 DEG C, obtains three layers of compound carbonizing boryl ceramic material.
4. according to the preparation method of a kind of stratiform compound carbonizing boryl ceramic material described in claim 2 or 3, it is characterized in that the purity of described all boron carbide powders is all 99%, described TiB
2the purity of powder is 98%.
5. according to the preparation method of a kind of stratiform compound carbonizing boryl ceramic material described in claim 2 or 3, it is characterized in that described aluminium alloy is commercial aluminum alloy, the trade mark is 5083,5086,5A12 or 7005.
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| CN104018022B (en) * | 2014-05-28 | 2016-07-20 | 成都西顿硬质合金有限公司 | The preparation method of boron carbide-based microstructure composite |
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| CN108467272A (en) * | 2018-03-21 | 2018-08-31 | 浙江立泰复合材料股份有限公司 | A kind of preparation method of boron carbide/silicon carbide stratiform composite ceramic material |
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| CN111578784B (en) * | 2020-04-20 | 2022-05-13 | 哈尔滨工业大学 | SiC and aluminum alloy composite integral bulletproof plate |
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